Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # Attachment 'Xray.cif' # 1. SUBMISSION DETAILS _publ_contact_author ; Matthew G. Davidson University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_contact_author_phone '# 44 1225 38 4467' _publ_contact_author_fax '# 44 1225 82 6231' _publ_contact_author_email m.g.davidson@bath.ac.uk _publ_contact_letter ; ; #================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Group(IV) complexes of amine bisphenolates and their application to the ring opening polymerisation of cyclic esters ; loop_ _publ_author_name _publ_author_address 'Matthew G Davidson' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Matthew D Jones' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Amanda J Chmura' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Matthew Lunn' ; Johnson Matthey PO Box 1 Belasis Avenue Billingham, TS23 1LB ; 'Mary F. Mahon' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_contact_author_name 'Matthew G. Davidson' #========================================================= data_Ti(1a)2 _database_code_depnum_ccdc_archive 'CCDC 284362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 N2 O4 Ti, 4(C H2 Cl2)' _chemical_formula_sum 'C42 H54 Cl8 N2 O4 Ti' _chemical_formula_weight 982.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.6050(3) _cell_length_b 14.5310(3) _cell_length_c 17.5150(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.1740(10) _cell_angle_gamma 90.00 _cell_volume 4645.40(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21644 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 25.06 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kapp CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21644 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4086 _reflns_number_gt 3731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+25.6918P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4086 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.18377(6) 0.2500 0.0244(3) Uani 1 2 d S . . O1 O -0.07244(14) 0.27558(18) 0.24830(15) 0.0302(6) Uani 1 1 d . . . N1 N 0.00765(16) 0.1842(2) 0.38058(18) 0.0264(7) Uani 1 1 d . . . C1 C -0.08136(19) 0.3438(3) 0.2982(2) 0.0278(8) Uani 1 1 d . . . Cl2 Cl 0.28463(8) 0.23548(10) 0.24575(9) 0.0650(4) Uani 1 1 d . . . O2 O 0.07322(14) 0.09308(18) 0.27327(15) 0.0318(6) Uani 1 1 d . . . C2 C -0.0966(2) 0.4341(3) 0.2721(2) 0.0314(8) Uani 1 1 d . . . Cl3 Cl 0.27734(7) 0.30252(11) 0.40213(8) 0.0627(4) Uani 1 1 d . . . C3 C -0.1038(2) 0.5011(3) 0.3277(2) 0.0352(9) Uani 1 1 d . . . H3 H -0.1139 0.5627 0.3109 0.042 Uiso 1 1 calc R . . Cl4 Cl 0.53443(9) 0.33584(15) 0.13679(10) 0.0789(5) Uani 1 1 d . . . C4 C -0.0967(2) 0.4811(3) 0.4059(3) 0.0370(9) Uani 1 1 d . . . Cl5 Cl 0.44005(19) 0.18847(17) 0.14955(18) 0.0768(11) Uani 0.715(8) 1 d P A 1 C5 C -0.0825(2) 0.3900(3) 0.4304(2) 0.0357(9) Uani 1 1 d . . . H5 H -0.0779 0.3748 0.4839 0.043 Uiso 1 1 calc R . . C6 C -0.0751(2) 0.3214(3) 0.3768(2) 0.0304(8) Uani 1 1 d . . . C7 C -0.1050(2) 0.4576(3) 0.1873(2) 0.0393(10) Uani 1 1 d . . . H7A H -0.0591 0.4445 0.1699 0.059 Uiso 1 1 calc R . . H7B H -0.1169 0.5230 0.1797 0.059 Uiso 1 1 calc R . . H7C H -0.1445 0.4205 0.1571 0.059 Uiso 1 1 calc R . . C8 C -0.1059(3) 0.5555(4) 0.4642(3) 0.0500(12) Uani 1 1 d . . . H8A H -0.0931 0.6154 0.4449 0.075 Uiso 1 1 calc R . . H8B H -0.0736 0.5424 0.5143 0.075 Uiso 1 1 calc R . . H8C H -0.1569 0.5567 0.4712 0.075 Uiso 1 1 calc R . . C9 C -0.0621(2) 0.2226(3) 0.4000(2) 0.0309(8) Uani 1 1 d . . . H9A H -0.1040 0.1853 0.3734 0.037 Uiso 1 1 calc R . . H9B H -0.0598 0.2170 0.4568 0.037 Uiso 1 1 calc R . . C10 C 0.0708(2) 0.2387(3) 0.4225(2) 0.0310(8) Uani 1 1 d . . . H10A H 0.0733 0.2334 0.4787 0.046 Uiso 1 1 calc R . . H10B H 0.0644 0.3035 0.4070 0.046 Uiso 1 1 calc R . . H10C H 0.1162 0.2152 0.4094 0.046 Uiso 1 1 calc R . . C11 C 0.0149(2) 0.0873(3) 0.4099(2) 0.0302(8) Uani 1 1 d . . . H11A H -0.0258 0.0503 0.3802 0.036 Uiso 1 1 calc R . . H11B H 0.0098 0.0869 0.4652 0.036 Uiso 1 1 calc R . . C12 C 0.0870(2) 0.0421(3) 0.4035(2) 0.0314(8) Uani 1 1 d . . . C13 C 0.1286(2) -0.0039(3) 0.4668(3) 0.0372(9) Uani 1 1 d . . . H13 H 0.1135 -0.0028 0.5156 0.045 Uiso 1 1 calc R . . C14 C 0.1919(2) -0.0512(3) 0.4596(3) 0.0403(10) Uani 1 1 d . . . C15 C 0.2123(2) -0.0522(3) 0.3872(3) 0.0392(10) Uani 1 1 d . . . H15 H 0.2545 -0.0861 0.3813 0.047 Uiso 1 1 calc R . . C16 C 0.1732(2) -0.0053(3) 0.3231(2) 0.0324(9) Uani 1 1 d . . . C17 C 0.1102(2) 0.0437(3) 0.3325(2) 0.0292(8) Uani 1 1 d . . . C18 C 0.1956(2) -0.0060(3) 0.2450(3) 0.0395(10) Uani 1 1 d . . . H18A H 0.2446 -0.0330 0.2503 0.059 Uiso 1 1 calc R . . H18B H 0.1963 0.0571 0.2256 0.059 Uiso 1 1 calc R . . H18C H 0.1605 -0.0427 0.2083 0.059 Uiso 1 1 calc R . . C19 C 0.2368(3) -0.1023(4) 0.5288(3) 0.0554(13) Uani 1 1 d . . . H19A H 0.2329 -0.0701 0.5771 0.083 Uiso 1 1 calc R . . H19B H 0.2882 -0.1045 0.5235 0.083 Uiso 1 1 calc R . . H19C H 0.2180 -0.1652 0.5305 0.083 Uiso 1 1 calc R . . C20 C 0.2434(3) 0.2215(4) 0.3276(3) 0.0567(14) Uani 1 1 d . . . H20A H 0.2529 0.1584 0.3484 0.068 Uiso 1 1 calc R . . H20B H 0.1897 0.2292 0.3115 0.068 Uiso 1 1 calc R . . C21 C 0.4452(4) 0.3078(6) 0.1482(5) 0.0417(18) Uani 0.715(8) 1 d P A 1 H21A H 0.4355 0.3337 0.1975 0.050 Uiso 0.715(8) 1 calc PR A 1 H21B H 0.4087 0.3330 0.1045 0.050 Uiso 0.715(8) 1 calc PR A 1 Cl5' Cl 0.3913(5) 0.2209(5) 0.1055(4) 0.078(3) Uani 0.285(8) 1 d P A 2 C21' C 0.479(4) 0.280(3) 0.163(3) 0.18(3) Uani 0.285(8) 1 d P A 2 H21C H 0.4620 0.3181 0.2024 0.215 Uiso 0.285(8) 1 calc PR A 2 H21D H 0.5076 0.2289 0.1925 0.215 Uiso 0.285(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0234(5) 0.0215(5) 0.0304(5) 0.000 0.0107(4) 0.000 O1 0.0303(14) 0.0294(14) 0.0311(14) -0.0034(11) 0.0069(11) 0.0064(11) N1 0.0230(15) 0.0241(16) 0.0353(17) 0.0034(13) 0.0134(13) 0.0032(12) C1 0.0214(17) 0.0276(19) 0.035(2) -0.0045(15) 0.0078(14) 0.0023(14) Cl2 0.0635(8) 0.0556(8) 0.0834(10) -0.0012(7) 0.0331(7) -0.0133(6) O2 0.0306(14) 0.0299(14) 0.0383(15) 0.0040(11) 0.0149(11) 0.0093(11) C2 0.0253(18) 0.0261(19) 0.042(2) -0.0035(16) 0.0051(16) 0.0045(15) Cl3 0.0459(7) 0.0804(10) 0.0602(8) 0.0116(7) 0.0062(6) -0.0045(6) C3 0.0273(19) 0.029(2) 0.048(2) -0.0054(17) 0.0035(17) 0.0057(16) Cl4 0.0534(8) 0.1082(14) 0.0754(10) -0.0058(9) 0.0137(7) 0.0004(8) C4 0.0240(19) 0.037(2) 0.048(2) -0.0154(19) 0.0026(17) 0.0050(16) Cl5 0.098(2) 0.0563(13) 0.0803(19) -0.0101(12) 0.0288(17) -0.0158(13) C5 0.0262(19) 0.047(2) 0.035(2) -0.0091(18) 0.0068(16) 0.0047(17) C6 0.0219(18) 0.034(2) 0.036(2) -0.0034(16) 0.0080(15) 0.0042(15) C7 0.041(2) 0.034(2) 0.044(2) 0.0041(18) 0.0109(19) 0.0090(18) C8 0.044(3) 0.049(3) 0.054(3) -0.021(2) 0.005(2) 0.009(2) C9 0.0253(18) 0.035(2) 0.036(2) -0.0004(16) 0.0148(15) 0.0039(16) C10 0.0279(19) 0.034(2) 0.0310(19) 0.0012(16) 0.0057(15) 0.0002(16) C11 0.0277(19) 0.0279(19) 0.039(2) 0.0057(16) 0.0151(16) 0.0009(15) C12 0.0250(18) 0.0287(19) 0.042(2) 0.0026(16) 0.0103(16) 0.0002(15) C13 0.031(2) 0.039(2) 0.043(2) 0.0043(18) 0.0117(17) -0.0019(18) C14 0.030(2) 0.041(2) 0.049(2) 0.0046(19) 0.0034(18) -0.0010(18) C15 0.0223(19) 0.039(2) 0.056(3) 0.001(2) 0.0083(18) -0.0002(17) C16 0.0219(18) 0.030(2) 0.046(2) -0.0024(17) 0.0091(16) -0.0025(15) C17 0.0251(18) 0.0260(19) 0.038(2) -0.0011(16) 0.0093(15) -0.0018(15) C18 0.029(2) 0.041(2) 0.050(2) -0.0051(19) 0.0134(18) 0.0037(18) C19 0.039(2) 0.064(3) 0.061(3) 0.011(3) 0.006(2) 0.012(2) C20 0.034(2) 0.068(3) 0.067(3) 0.019(3) 0.007(2) -0.011(2) C21 0.031(3) 0.034(4) 0.058(4) 0.001(3) 0.003(3) 0.008(3) Cl5' 0.097(6) 0.066(4) 0.076(5) -0.026(3) 0.032(4) -0.028(4) C21' 0.33(8) 0.05(2) 0.13(3) -0.01(2) -0.04(4) -0.04(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 Ti1 O2 1.882(3) 2 ? Ti1 O2 1.882(3) . ? Ti1 O1 1.892(3) 2 ? Ti1 O1 1.892(3) . ? Ti1 N1 2.264(3) . ? Ti1 N1 2.264(3) 2 ? Cl2 C20 1.764(5) . ? Cl3 C20 1.780(6) . ? Cl4 C21' 1.45(6) . ? Cl4 C21 1.757(7) . ? Cl5 C21 1.737(8) . ? O1 C1 1.352(4) . ? O2 C17 1.337(5) . ? C1 C6 1.397(6) . ? C1 C2 1.401(5) . ? N1 C10 1.487(5) . ? N1 C11 1.496(5) . ? N1 C9 1.510(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C17 1.393(6) . ? C12 C13 1.394(6) . ? C12 C11 1.517(5) . ? C17 C16 1.408(5) . ? C5 C6 1.394(6) . ? C5 C4 1.402(6) . ? C5 H5 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C2 C3 1.402(6) . ? C2 C7 1.501(6) . ? C3 C4 1.381(6) . ? C3 H3 0.9500 . ? C4 C8 1.519(6) . ? C13 C14 1.391(6) . ? C13 H13 0.9500 . ? C16 C15 1.392(6) . ? C16 C18 1.505(6) . ? C15 C14 1.391(6) . ? C15 H15 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C9 C6 1.500(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C14 C19 1.525(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? Cl5' C21' 1.95(6) . ? C21' H21C 0.9900 . ? C21' H21D 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 O2 Ti1 O2 91.13(17) 2 . ? O2 Ti1 O1 168.58(11) 2 2 ? O2 Ti1 O1 90.39(12) . 2 ? O2 Ti1 O1 90.39(12) 2 . ? O2 Ti1 O1 168.58(11) . . ? O1 Ti1 O1 90.35(17) 2 . ? O2 Ti1 N1 97.00(11) 2 . ? O2 Ti1 N1 83.22(11) . . ? O1 Ti1 N1 94.42(11) 2 . ? O1 Ti1 N1 85.36(11) . . ? O2 Ti1 N1 83.22(11) 2 2 ? O2 Ti1 N1 97.00(11) . 2 ? O1 Ti1 N1 85.36(11) 2 2 ? O1 Ti1 N1 94.42(11) . 2 ? N1 Ti1 N1 179.69(16) . 2 ? C21' Cl4 C21 25(2) . . ? C1 O1 Ti1 133.0(2) . . ? C17 O2 Ti1 141.7(2) . . ? O1 C1 C6 118.0(3) . . ? O1 C1 C2 121.2(3) . . ? C6 C1 C2 120.8(3) . . ? C10 N1 C11 108.8(3) . . ? C10 N1 C9 108.8(3) . . ? C11 N1 C9 107.1(3) . . ? C10 N1 Ti1 112.9(2) . . ? C11 N1 Ti1 109.2(2) . . ? C9 N1 Ti1 109.9(2) . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C17 C12 C13 119.8(4) . . ? C17 C12 C11 119.4(3) . . ? C13 C12 C11 120.8(4) . . ? O2 C17 C12 120.0(3) . . ? O2 C17 C16 119.6(3) . . ? C12 C17 C16 120.4(4) . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? N1 C11 C12 113.8(3) . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C1 C2 C3 117.6(4) . . ? C1 C2 C7 120.8(3) . . ? C3 C2 C7 121.6(4) . . ? C4 C3 C2 122.7(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C8 121.1(4) . . ? C5 C4 C8 120.4(4) . . ? C14 C13 C12 121.0(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C16 C17 118.0(4) . . ? C15 C16 C18 122.4(4) . . ? C17 C16 C18 119.6(4) . . ? C14 C15 C16 122.5(4) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C6 C9 N1 113.1(3) . . ? C6 C9 H9A 109.0 . . ? N1 C9 H9A 109.0 . . ? C6 C9 H9B 109.0 . . ? N1 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C9 122.2(4) . . ? C1 C6 C9 117.9(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C14 C13 118.2(4) . . ? C15 C14 C19 121.1(4) . . ? C13 C14 C19 120.7(4) . . ? Cl2 C20 Cl3 111.8(3) . . ? Cl2 C20 H20A 109.3 . . ? Cl3 C20 H20A 109.3 . . ? Cl2 C20 H20B 109.3 . . ? Cl3 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Cl5 C21 Cl4 106.8(4) . . ? Cl5 C21 H21A 110.4 . . ? Cl4 C21 H21A 110.4 . . ? Cl5 C21 H21B 110.4 . . ? Cl4 C21 H21B 110.4 . . ? H21A C21 H21B 108.6 . . ? Cl4 C21' Cl5' 131(3) . . ? Cl4 C21' H21C 104.4 . . ? Cl5' C21' H21C 104.4 . . ? Cl4 C21' H21D 104.5 . . ? Cl5' C21' H21D 104.5 . . ? H21C C21' H21D 105.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.389 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.115 #===END data_Zr(1a)2 _database_code_depnum_ccdc_archive 'CCDC 284363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 N2 O4 Zr, 4(C H2 Cl2) ' _chemical_formula_sum 'C42 H54 Cl8 N2 O4 Zr' _chemical_formula_weight 1025.69 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.8020(2) _cell_length_b 14.4540(2) _cell_length_c 17.7450(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.9820(10) _cell_angle_gamma 90.00 _cell_volume 4734.14(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4315 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8093 _diffrn_reflns_av_R_equivalents 0.0095 _diffrn_reflns_av_sigmaI/netI 0.0196 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4144 _reflns_number_gt 3898 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+12.8575P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4144 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.5000 0.17261(2) 0.2500 0.01715(11) Uani 1 2 d S . . Cl1 Cl 0.21262(5) 0.22076(6) 0.25008(6) 0.0572(2) Uani 1 1 d . . . O1 O 0.42360(9) 0.07646(11) 0.21776(9) 0.0240(4) Uani 1 1 d . . . N1 N 0.48924(10) 0.17782(13) 0.11277(11) 0.0193(4) Uani 1 1 d . . . C1 C 0.38498(12) 0.03177(16) 0.15682(13) 0.0215(5) Uani 1 1 d . . . Cl2 Cl 0.22307(5) 0.29864(7) 0.10018(5) 0.0571(2) Uani 1 1 d . . . O2 O 0.57532(9) 0.27011(11) 0.24376(9) 0.0241(4) Uani 1 1 d . . . C2 C 0.32261(12) -0.01778(17) 0.16463(14) 0.0245(5) Uani 1 1 d . . . Cl3 Cl -0.06378(7) 0.18515(7) 0.15185(6) 0.0689(3) Uani 1 1 d . . . C3 C 0.28380(13) -0.06196(18) 0.09964(16) 0.0307(6) Uani 1 1 d . . . H3 H 0.2420 -0.0968 0.1043 0.037 Uiso 1 1 calc R . . Cl4 Cl 0.03509(5) 0.33433(7) 0.13893(5) 0.0550(2) Uani 1 1 d . . . C4 C 0.30403(14) -0.05692(19) 0.02823(16) 0.0324(6) Uani 1 1 d . . . C5 C 0.36638(13) -0.00683(18) 0.02267(15) 0.0280(5) Uani 1 1 d . . . H5 H 0.3806 -0.0018 -0.0257 0.034 Uiso 1 1 calc R . . C6 C 0.40807(12) 0.03582(16) 0.08651(14) 0.0224(5) Uani 1 1 d . . . C7 C 0.30057(14) -0.02312(19) 0.24146(15) 0.0302(6) Uani 1 1 d . . . H7A H 0.2550 -0.0576 0.2366 0.045 Uiso 1 1 calc R . . H7B H 0.2939 0.0395 0.2600 0.045 Uiso 1 1 calc R . . H7C H 0.3384 -0.0548 0.2780 0.045 Uiso 1 1 calc R . . C8 C 0.26026(16) -0.1047(3) -0.04162(18) 0.0491(8) Uani 1 1 d . . . H8A H 0.2809 -0.1660 -0.0474 0.074 Uiso 1 1 calc R . . H8B H 0.2617 -0.0676 -0.0875 0.074 Uiso 1 1 calc R . . H8C H 0.2099 -0.1115 -0.0350 0.074 Uiso 1 1 calc R . . C9 C 0.47936(13) 0.08081(16) 0.08174(14) 0.0227(5) Uani 1 1 d . . . H9A H 0.5189 0.0418 0.1101 0.027 Uiso 1 1 calc R . . H9B H 0.4846 0.0818 0.0273 0.027 Uiso 1 1 calc R . . C10 C 0.42782(13) 0.23576(17) 0.07453(13) 0.0236(5) Uani 1 1 d . . . H10A H 0.4255 0.2347 0.0189 0.035 Uiso 1 1 calc R . . H10B H 0.4348 0.2995 0.0933 0.035 Uiso 1 1 calc R . . H10C H 0.3825 0.2114 0.0862 0.035 Uiso 1 1 calc R . . C11 C 0.55877(13) 0.21365(17) 0.09288(14) 0.0239(5) Uani 1 1 d . . . H11A H 0.5995 0.1749 0.1190 0.029 Uiso 1 1 calc R . . H11B H 0.5561 0.2073 0.0369 0.029 Uiso 1 1 calc R . . C12 C 0.57439(12) 0.31308(17) 0.11519(14) 0.0232(5) Uani 1 1 d . . . C13 C 0.58293(12) 0.33704(16) 0.19282(14) 0.0219(5) Uani 1 1 d . . . C14 C 0.59808(13) 0.42846(17) 0.21668(15) 0.0258(5) Uani 1 1 d . . . C15 C 0.60398(13) 0.49441(18) 0.16089(16) 0.0308(6) Uani 1 1 d . . . H15 H 0.6139 0.5567 0.1764 0.037 Uiso 1 1 calc R . . C16 C 0.59584(13) 0.47239(19) 0.08340(16) 0.0313(6) Uani 1 1 d . . . C17 C 0.58074(13) 0.38112(19) 0.06130(15) 0.0288(6) Uani 1 1 d . . . H17 H 0.5747 0.3649 0.0086 0.035 Uiso 1 1 calc R . . C18 C 0.60430(17) 0.5457(2) 0.02496(19) 0.0455(8) Uani 1 1 d . . . H18A H 0.6554 0.5505 0.0209 0.068 Uiso 1 1 calc R . . H18B H 0.5876 0.6053 0.0412 0.068 Uiso 1 1 calc R . . H18C H 0.5754 0.5287 -0.0251 0.068 Uiso 1 1 calc R . . C19 C 0.60692(15) 0.45347(19) 0.30010(16) 0.0353(6) Uani 1 1 d . . . H19A H 0.6257 0.5167 0.3079 0.053 Uiso 1 1 calc R . . H19B H 0.6410 0.4105 0.3308 0.053 Uiso 1 1 calc R . . H19C H 0.5599 0.4496 0.3160 0.053 Uiso 1 1 calc R . . C20 C 0.25739(17) 0.2169(3) 0.1714(2) 0.0492(8) Uani 1 1 d . . . H20A H 0.3097 0.2286 0.1898 0.059 Uiso 1 1 calc R . . H20B H 0.2521 0.1541 0.1486 0.059 Uiso 1 1 calc R . . C21 C -0.05354(17) 0.3050(2) 0.14796(18) 0.0437(7) Uani 1 1 d . . . H21A H -0.0645 0.3333 0.1953 0.052 Uiso 1 1 calc R . . H21B H -0.0883 0.3301 0.1036 0.052 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 Zr1 0.01845(17) 0.01579(17) 0.01721(17) 0.000 0.00341(12) 0.000 Cl1 0.0646(5) 0.0409(5) 0.0727(6) 0.0028(4) 0.0303(5) 0.0094(4) O1 0.0260(8) 0.0235(9) 0.0231(8) -0.0020(7) 0.0061(7) -0.0062(7) N1 0.0190(9) 0.0185(10) 0.0211(10) -0.0016(8) 0.0053(8) -0.0011(8) C1 0.0200(11) 0.0173(11) 0.0261(12) -0.0019(9) 0.0020(9) 0.0006(9) Cl2 0.0451(4) 0.0762(6) 0.0469(5) -0.0049(4) 0.0010(4) 0.0078(4) O2 0.0285(9) 0.0223(9) 0.0202(8) 0.0017(7) 0.0017(7) -0.0058(7) C2 0.0187(11) 0.0200(12) 0.0344(13) -0.0007(10) 0.0042(10) 0.0026(9) Cl3 0.0930(8) 0.0526(5) 0.0633(6) -0.0071(4) 0.0207(5) -0.0223(5) C3 0.0193(12) 0.0281(13) 0.0435(15) -0.0038(11) 0.0026(11) -0.0024(10) Cl4 0.0434(4) 0.0679(6) 0.0522(5) 0.0077(4) 0.0054(4) -0.0076(4) C4 0.0250(13) 0.0333(14) 0.0360(15) -0.0089(12) -0.0016(11) -0.0010(11) C5 0.0258(12) 0.0300(13) 0.0277(13) -0.0048(10) 0.0038(10) 0.0025(10) C6 0.0222(12) 0.0180(11) 0.0268(12) -0.0032(9) 0.0038(9) 0.0007(9) C7 0.0245(12) 0.0304(14) 0.0368(14) 0.0029(11) 0.0087(11) -0.0021(11) C8 0.0350(16) 0.064(2) 0.0453(18) -0.0192(16) -0.0015(13) -0.0128(15) C9 0.0247(12) 0.0207(12) 0.0238(12) -0.0051(9) 0.0071(9) -0.0003(9) C10 0.0239(12) 0.0245(12) 0.0219(12) 0.0015(10) 0.0030(9) 0.0008(10) C11 0.0222(12) 0.0281(13) 0.0235(12) -0.0003(10) 0.0101(9) -0.0019(10) C12 0.0183(11) 0.0262(13) 0.0255(12) 0.0015(10) 0.0049(9) -0.0030(9) C13 0.0171(11) 0.0221(12) 0.0263(12) 0.0039(9) 0.0036(9) -0.0022(9) C14 0.0197(11) 0.0232(12) 0.0339(13) -0.0005(10) 0.0038(10) -0.0039(9) C15 0.0216(12) 0.0217(13) 0.0477(16) 0.0045(11) 0.0034(11) -0.0033(10) C16 0.0207(12) 0.0313(14) 0.0401(15) 0.0150(12) 0.0011(11) -0.0039(10) C17 0.0219(12) 0.0369(15) 0.0269(13) 0.0068(11) 0.0030(10) -0.0054(11) C18 0.0394(16) 0.0421(17) 0.0523(18) 0.0241(15) 0.0015(14) -0.0079(13) C19 0.0381(15) 0.0277(14) 0.0406(16) -0.0081(12) 0.0089(12) -0.0086(12) C20 0.0320(15) 0.059(2) 0.0547(19) -0.0094(16) 0.0044(14) 0.0117(15) C21 0.0408(17) 0.0487(18) 0.0415(17) 0.0008(14) 0.0070(13) 0.0044(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 Zr1 O1 2.0022(16) . ? Zr1 O1 2.0022(16) 2_655 ? Zr1 O2 2.0158(16) . ? Zr1 O2 2.0158(16) 2_655 ? Zr1 N1 2.4061(19) 2_655 ? Zr1 N1 2.4061(19) . ? Cl2 C20 1.760(4) . ? Cl4 C21 1.756(3) . ? Cl1 C20 1.764(3) . ? Cl3 C21 1.746(3) . ? O2 C13 1.350(3) . ? O1 C1 1.347(3) . ? N1 C10 1.482(3) . ? N1 C9 1.505(3) . ? N1 C11 1.509(3) . ? C13 C12 1.400(3) . ? C13 C14 1.400(3) . ? C2 C3 1.396(4) . ? C2 C1 1.403(3) . ? C2 C7 1.501(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C1 C6 1.398(3) . ? C6 C5 1.393(3) . ? C6 C9 1.507(3) . ? C14 C15 1.394(4) . ? C14 C19 1.502(4) . ? C5 C4 1.397(4) . ? C5 H5 0.9500 . ? C3 C4 1.393(4) . ? C3 H3 0.9500 . ? C17 C16 1.390(4) . ? C17 C12 1.393(3) . ? C17 H17 0.9500 . ? C12 C11 1.505(3) . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C4 C8 1.517(4) . ? C16 C18 1.512(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 O1 92.09(10) . 2_655 ? O1 Zr1 O2 160.53(6) . . ? O1 Zr1 O2 91.59(7) 2_655 . ? O1 Zr1 O2 91.59(7) . 2_655 ? O1 Zr1 O2 160.53(6) 2_655 2_655 ? O2 Zr1 O2 91.28(10) . 2_655 ? O1 Zr1 N1 103.20(6) . 2_655 ? O1 Zr1 N1 79.34(6) 2_655 2_655 ? O2 Zr1 N1 96.27(6) . 2_655 ? O2 Zr1 N1 81.20(6) 2_655 2_655 ? O1 Zr1 N1 79.34(6) . . ? O1 Zr1 N1 103.20(6) 2_655 . ? O2 Zr1 N1 81.20(6) . . ? O2 Zr1 N1 96.27(6) 2_655 . ? N1 Zr1 N1 176.41(9) 2_655 . ? C13 O2 Zr1 134.66(14) . . ? C1 O1 Zr1 144.09(15) . . ? C10 N1 C9 109.14(18) . . ? C10 N1 C11 109.46(18) . . ? C9 N1 C11 106.64(17) . . ? C10 N1 Zr1 112.89(14) . . ? C9 N1 Zr1 108.77(13) . . ? C11 N1 Zr1 109.74(13) . . ? O2 C13 C12 118.3(2) . . ? O2 C13 C14 121.0(2) . . ? C12 C13 C14 120.6(2) . . ? C3 C2 C1 117.8(2) . . ? C3 C2 C7 122.4(2) . . ? C1 C2 C7 119.8(2) . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C1 C6 119.0(2) . . ? O1 C1 C2 119.9(2) . . ? C6 C1 C2 121.1(2) . . ? C5 C6 C1 119.0(2) . . ? C5 C6 C9 121.0(2) . . ? C1 C6 C9 119.9(2) . . ? C15 C14 C13 118.0(2) . . ? C15 C14 C19 121.8(2) . . ? C13 C14 C19 120.2(2) . . ? C6 C5 C4 121.4(2) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C4 C3 C2 122.5(2) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C16 C17 C12 121.1(2) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C17 C12 C13 119.5(2) . . ? C17 C12 C11 122.1(2) . . ? C13 C12 C11 118.4(2) . . ? C16 C15 C14 122.5(2) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? C12 C11 N1 113.61(19) . . ? C12 C11 H11A 108.8 . . ? N1 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? N1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N1 C9 C6 115.52(19) . . ? N1 C9 H9A 108.4 . . ? C6 C9 H9A 108.4 . . ? N1 C9 H9B 108.4 . . ? C6 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C3 C4 C5 118.0(2) . . ? C3 C4 C8 121.3(3) . . ? C5 C4 C8 120.7(3) . . ? C17 C16 C15 118.3(2) . . ? C17 C16 C18 120.9(3) . . ? C15 C16 C18 120.8(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Cl3 C21 Cl4 110.88(18) . . ? Cl3 C21 H21A 109.5 . . ? Cl4 C21 H21A 109.5 . . ? Cl3 C21 H21B 109.5 . . ? Cl4 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Cl2 C20 Cl1 112.45(17) . . ? Cl2 C20 H20A 109.1 . . ? Cl1 C20 H20A 109.1 . . ? Cl2 C20 H20B 109.1 . . ? Cl1 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.734 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.067 #===END data_Hf(1a)2 _database_code_depnum_ccdc_archive 'CCDC 284364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C38 H46 Hf N2 O4), C6 H14, C7 ' _chemical_formula_sum 'C89 H106 Hf2 N4 O8' _chemical_formula_weight 1716.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.63600(10) _cell_length_b 12.72600(10) _cell_length_c 14.74600(10) _cell_angle_alpha 97.3500(10) _cell_angle_beta 96.4400(10) _cell_angle_gamma 118.2500(10) _cell_volume 2030.69(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52791 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.51 _exptl_crystal_description diamond _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 2.611 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonis kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38403 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 30.52 _reflns_number_total 12228 _reflns_number_gt 11048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+1.1974P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12228 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Hf1 Hf 0.209987(8) 0.242380(8) 0.252522(6) 0.02080(4) Uani 1 1 d . . . O1 O 0.27925(16) 0.36466(15) 0.37281(11) 0.0254(4) Uani 1 1 d . . . N1 N 0.24934(18) 0.41979(18) 0.19664(13) 0.0217(4) Uani 1 1 d . . . C1 C 0.3001(2) 0.4761(2) 0.41075(16) 0.0229(4) Uani 1 1 d . . . O2 O 0.16073(17) 0.16851(15) 0.11539(11) 0.0286(4) Uani 1 1 d . . . N2 N 0.14426(19) 0.05158(18) 0.29628(14) 0.0237(4) Uani 1 1 d . . . C2 C 0.2724(2) 0.5438(2) 0.35514(16) 0.0232(4) Uani 1 1 d . . . O3 O 0.03987(16) 0.20036(16) 0.26673(12) 0.0278(4) Uani 1 1 d . . . C3 C 0.3000(2) 0.6619(2) 0.39427(19) 0.0290(5) Uani 1 1 d . . . H3 H 0.2819 0.7082 0.3559 0.035 Uiso 1 1 calc R . . O4 O 0.36933(15) 0.24162(16) 0.25773(13) 0.0275(4) Uani 1 1 d . . . C4 C 0.3532(2) 0.7133(2) 0.48762(19) 0.0319(6) Uani 1 1 d . . . C5 C 0.3776(2) 0.6435(2) 0.54241(18) 0.0320(6) Uani 1 1 d . . . H5 H 0.4133 0.6775 0.6066 0.038 Uiso 1 1 calc R . . C6 C 0.3515(2) 0.5246(2) 0.50637(16) 0.0262(5) Uani 1 1 d . . . C7 C 0.3775(3) 0.4504(3) 0.56718(18) 0.0341(6) Uani 1 1 d . . . H7A H 0.4250 0.5021 0.6284 0.051 Uiso 1 1 calc R . . H7B H 0.4246 0.4174 0.5380 0.051 Uiso 1 1 calc R . . H7C H 0.3001 0.3831 0.5748 0.051 Uiso 1 1 calc R . . C8 C 0.3816(3) 0.8413(3) 0.5283(2) 0.0476(8) Uani 1 1 d . . . H8A H 0.4080 0.8922 0.4818 0.071 Uiso 1 1 calc R . . H8B H 0.4471 0.8757 0.5838 0.071 Uiso 1 1 calc R . . H8C H 0.3079 0.8390 0.5455 0.071 Uiso 1 1 calc R . . C9 C 0.2042(2) 0.4892(2) 0.25599(16) 0.0250(5) Uani 1 1 d . . . H9A H 0.2078 0.5558 0.2259 0.030 Uiso 1 1 calc R . . H9B H 0.1170 0.4336 0.2566 0.030 Uiso 1 1 calc R . . C10 C 0.3817(2) 0.4984(2) 0.19864(18) 0.0267(5) Uani 1 1 d . . . H10A H 0.4100 0.4540 0.1579 0.040 Uiso 1 1 calc R . . H10B H 0.4277 0.5207 0.2626 0.040 Uiso 1 1 calc R . . H10C H 0.3949 0.5724 0.1768 0.040 Uiso 1 1 calc R . . C11 C 0.1782(2) 0.3895(2) 0.09944(16) 0.0271(5) Uani 1 1 d . . . H11A H 0.0899 0.3400 0.0998 0.033 Uiso 1 1 calc R . . H11B H 0.1916 0.4663 0.0811 0.033 Uiso 1 1 calc R . . C12 C 0.2105(2) 0.3215(2) 0.02708(16) 0.0250(5) Uani 1 1 d . . . C13 C 0.2477(2) 0.3649(2) -0.05212(17) 0.0292(5) Uani 1 1 d . . . H13 H 0.2600 0.4430 -0.0584 0.035 Uiso 1 1 calc R . . C14 C 0.2674(2) 0.2960(2) -0.12227(17) 0.0309(5) Uani 1 1 d . . . C15 C 0.2496(2) 0.1825(2) -0.11109(17) 0.0316(6) Uani 1 1 d . . . H15 H 0.2625 0.1348 -0.1589 0.038 Uiso 1 1 calc R . . C16 C 0.2135(2) 0.1357(2) -0.03215(17) 0.0290(5) Uani 1 1 d . . . C17 C 0.1951(2) 0.2076(2) 0.03734(16) 0.0249(5) Uani 1 1 d . . . C18 C 0.1899(3) 0.0105(3) -0.0228(2) 0.0421(7) Uani 1 1 d . . . H18A H 0.2374 0.0159 0.0367 0.063 Uiso 1 1 calc R . . H18B H 0.2146 -0.0237 -0.0743 0.063 Uiso 1 1 calc R . . H18C H 0.1024 -0.0424 -0.0246 0.063 Uiso 1 1 calc R . . C19 C 0.3005(3) 0.3412(3) -0.2107(2) 0.0435(7) Uani 1 1 d . . . H19A H 0.3542 0.3129 -0.2341 0.065 Uiso 1 1 calc R . . H19B H 0.3431 0.4305 -0.1973 0.065 Uiso 1 1 calc R . . H19C H 0.2257 0.3094 -0.2579 0.065 Uiso 1 1 calc R . . C20 C -0.0575(2) 0.1215(2) 0.29732(16) 0.0238(5) Uani 1 1 d . . . C21 C -0.1682(2) 0.1222(2) 0.27977(17) 0.0272(5) Uani 1 1 d . . . C22 C -0.2687(2) 0.0356(2) 0.31003(18) 0.0302(5) Uani 1 1 d . . . H22 H -0.3446 0.0347 0.2979 0.036 Uiso 1 1 calc R . . C23 C -0.2613(3) -0.0497(2) 0.35758(18) 0.0311(5) Uani 1 1 d . . . C24 C -0.1492(2) -0.0459(2) 0.37564(17) 0.0291(5) Uani 1 1 d . . . H24 H -0.1423 -0.1027 0.4083 0.035 Uiso 1 1 calc R . . C25 C -0.0464(2) 0.0390(2) 0.34714(16) 0.0264(5) Uani 1 1 d . . . C26 C -0.1755(3) 0.2170(2) 0.23275(19) 0.0321(5) Uani 1 1 d . . . H26A H -0.2597 0.2027 0.2238 0.048 Uiso 1 1 calc R . . H26B H -0.1517 0.2122 0.1720 0.048 Uiso 1 1 calc R . . H26C H -0.1201 0.2982 0.2717 0.048 Uiso 1 1 calc R . . C27 C -0.3727(3) -0.1410(3) 0.3890(2) 0.0427(7) Uani 1 1 d . . . H27A H -0.3997 -0.0977 0.4321 0.064 Uiso 1 1 calc R . . H27B H -0.3518 -0.1939 0.4207 0.064 Uiso 1 1 calc R . . H27C H -0.4388 -0.1907 0.3347 0.064 Uiso 1 1 calc R . . C28 C 0.0766(2) 0.0489(2) 0.37451(17) 0.0282(5) Uani 1 1 d . . . H28A H 0.0651 -0.0211 0.4031 0.034 Uiso 1 1 calc R . . H28B H 0.1285 0.1241 0.4228 0.034 Uiso 1 1 calc R . . C29 C 0.0623(2) -0.0531(2) 0.21764(17) 0.0279(5) Uani 1 1 d . . . H29A H 0.1086 -0.0558 0.1692 0.042 Uiso 1 1 calc R . . H29B H -0.0063 -0.0431 0.1915 0.042 Uiso 1 1 calc R . . H29C H 0.0308 -0.1293 0.2405 0.042 Uiso 1 1 calc R . . C30 C 0.2517(2) 0.0377(2) 0.33332(18) 0.0300(5) Uani 1 1 d . . . H30A H 0.3029 0.1041 0.3883 0.036 Uiso 1 1 calc R . . H30B H 0.2209 -0.0406 0.3544 0.036 Uiso 1 1 calc R . . C31 C 0.3299(2) 0.0406(2) 0.26355(19) 0.0294(5) Uani 1 1 d . . . C32 C 0.3900(2) 0.1476(2) 0.22941(18) 0.0282(5) Uani 1 1 d . . . C33 C 0.4684(2) 0.1568(2) 0.1672(2) 0.0319(5) Uani 1 1 d . . . C34 C 0.4824(3) 0.0562(3) 0.1387(2) 0.0366(6) Uani 1 1 d . . . H34 H 0.5350 0.0615 0.0961 0.044 Uiso 1 1 calc R . . C35 C 0.4223(3) -0.0520(3) 0.1701(2) 0.0381(6) Uani 1 1 d . . . C36 C 0.3470(3) -0.0576(2) 0.2330(2) 0.0346(6) Uani 1 1 d . . . H36 H 0.3060 -0.1303 0.2559 0.041 Uiso 1 1 calc R . . C37 C 0.4393(3) -0.1593(3) 0.1363(3) 0.0503(8) Uani 1 1 d . . . H37A H 0.5173 -0.1303 0.1150 0.075 Uiso 1 1 calc R . . H37B H 0.3719 -0.2159 0.0846 0.075 Uiso 1 1 calc R . . H37C H 0.4399 -0.2013 0.1875 0.075 Uiso 1 1 calc R . . C38 C 0.5333(3) 0.2731(3) 0.1324(2) 0.0442(7) Uani 1 1 d . . . H38A H 0.4737 0.2819 0.0901 0.066 Uiso 1 1 calc R . . H38B H 0.5951 0.2705 0.0989 0.066 Uiso 1 1 calc R . . H38C H 0.5734 0.3426 0.1854 0.066 Uiso 1 1 calc R . . C42 C -0.0076(3) 0.4367(3) 0.4929(2) 0.0450(7) Uani 1 1 d . . . H42A H -0.0946 0.3767 0.4657 0.054 Uiso 1 1 calc R . . H42B H 0.0418 0.4303 0.4471 0.054 Uiso 1 1 calc R . . C43 C 0.0298(3) 0.4033(3) 0.5805(3) 0.0525(8) Uani 1 1 d . . . H43A H -0.0195 0.4095 0.6264 0.063 Uiso 1 1 calc R . . H43B H 0.1169 0.4627 0.6076 0.063 Uiso 1 1 calc R . . C44 C 0.0131(4) 0.2753(3) 0.5640(4) 0.0736(13) Uani 1 1 d . . . H44A H -0.0733 0.2157 0.5382 0.110 Uiso 1 1 calc R . . H44B H 0.0383 0.2585 0.6233 0.110 Uiso 1 1 calc R . . H44C H 0.0635 0.2692 0.5200 0.110 Uiso 1 1 calc R . . C51 C 0.9880(10) 0.5406(10) 0.0784(7) 0.156(4) Uani 1 1 d . . 1 C52 C 0.9207(5) 0.4270(6) 0.0397(6) 0.097(2) Uani 1 1 d . A 1 C53 C 0.9166(11) 0.3591(10) -0.0482(13) 0.227(9) Uani 1 1 d . . 1 C57 C 1.015(2) 0.624(3) 0.1473(15) 0.223(15) Uani 0.50 1 d P . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.02354(5) 0.01812(5) 0.01896(5) 0.00372(3) 0.00078(3) 0.00965(4) O1 0.0346(9) 0.0211(8) 0.0180(7) 0.0000(6) -0.0015(6) 0.0140(7) N1 0.0262(10) 0.0213(9) 0.0196(9) 0.0041(7) 0.0040(7) 0.0135(8) C1 0.0215(10) 0.0221(11) 0.0221(10) 0.0022(8) 0.0046(8) 0.0089(9) O2 0.0387(10) 0.0235(8) 0.0170(7) 0.0017(6) 0.0018(7) 0.0115(8) N2 0.0269(10) 0.0236(10) 0.0217(9) 0.0075(7) 0.0037(8) 0.0128(8) C2 0.0251(11) 0.0232(11) 0.0220(10) 0.0031(8) 0.0065(8) 0.0124(9) O3 0.0278(9) 0.0287(9) 0.0310(9) 0.0129(7) 0.0081(7) 0.0150(7) C3 0.0321(13) 0.0230(12) 0.0347(13) 0.0051(9) 0.0118(10) 0.0150(10) O4 0.0206(8) 0.0246(8) 0.0335(9) -0.0012(7) 0.0036(7) 0.0103(7) C4 0.0309(13) 0.0246(12) 0.0370(14) -0.0018(10) 0.0126(11) 0.0119(10) C5 0.0275(12) 0.0348(14) 0.0253(12) -0.0045(10) 0.0052(10) 0.0114(11) C6 0.0218(11) 0.0329(13) 0.0201(10) 0.0015(9) 0.0054(8) 0.0113(10) C7 0.0360(14) 0.0437(16) 0.0214(11) 0.0066(10) 0.0022(10) 0.0194(12) C8 0.0511(19) 0.0310(15) 0.0519(19) -0.0088(13) 0.0132(15) 0.0168(14) C9 0.0303(12) 0.0253(12) 0.0252(11) 0.0056(9) 0.0040(9) 0.0185(10) C10 0.0259(12) 0.0249(12) 0.0281(12) 0.0061(9) 0.0043(9) 0.0117(10) C11 0.0328(13) 0.0323(13) 0.0202(11) 0.0056(9) 0.0003(9) 0.0203(11) C12 0.0266(11) 0.0291(12) 0.0191(10) 0.0039(8) -0.0003(8) 0.0150(10) C13 0.0314(13) 0.0291(12) 0.0240(11) 0.0052(9) 0.0015(9) 0.0133(10) C14 0.0250(12) 0.0340(13) 0.0228(11) 0.0030(9) 0.0038(9) 0.0068(10) C15 0.0258(12) 0.0361(14) 0.0231(11) -0.0024(10) 0.0027(9) 0.0101(11) C16 0.0294(12) 0.0265(12) 0.0230(11) -0.0021(9) -0.0032(9) 0.0109(10) C17 0.0236(11) 0.0261(12) 0.0193(10) 0.0017(8) -0.0020(8) 0.0098(9) C18 0.061(2) 0.0325(15) 0.0311(14) -0.0019(11) 0.0008(13) 0.0254(14) C19 0.0447(17) 0.0418(16) 0.0278(13) 0.0056(11) 0.0126(12) 0.0078(13) C20 0.0283(12) 0.0227(11) 0.0184(10) 0.0027(8) 0.0052(8) 0.0114(9) C21 0.0302(12) 0.0254(12) 0.0250(11) 0.0007(9) 0.0053(9) 0.0141(10) C22 0.0289(12) 0.0316(13) 0.0279(12) -0.0009(10) 0.0090(10) 0.0141(11) C23 0.0356(14) 0.0285(13) 0.0252(12) 0.0019(9) 0.0138(10) 0.0119(11) C24 0.0384(14) 0.0268(12) 0.0224(11) 0.0062(9) 0.0122(10) 0.0148(11) C25 0.0321(12) 0.0258(12) 0.0225(11) 0.0048(9) 0.0060(9) 0.0152(10) C26 0.0314(13) 0.0298(13) 0.0380(14) 0.0056(10) 0.0048(11) 0.0181(11) C27 0.0422(16) 0.0401(16) 0.0413(16) 0.0099(12) 0.0222(13) 0.0134(13) C28 0.0350(13) 0.0305(13) 0.0208(11) 0.0097(9) 0.0049(9) 0.0168(11) C29 0.0315(12) 0.0235(11) 0.0273(12) 0.0042(9) 0.0042(10) 0.0130(10) C30 0.0326(13) 0.0316(13) 0.0285(12) 0.0113(10) 0.0001(10) 0.0180(11) C31 0.0271(12) 0.0279(12) 0.0337(13) 0.0050(10) -0.0009(10) 0.0158(10) C32 0.0245(11) 0.0251(12) 0.0325(13) 0.0011(9) -0.0026(9) 0.0132(10) C33 0.0260(12) 0.0290(13) 0.0388(14) 0.0045(10) 0.0031(10) 0.0135(10) C34 0.0309(13) 0.0363(15) 0.0421(15) -0.0014(11) 0.0041(11) 0.0191(12) C35 0.0325(14) 0.0302(14) 0.0499(17) -0.0033(12) -0.0042(12) 0.0197(12) C36 0.0307(13) 0.0256(13) 0.0472(16) 0.0069(11) -0.0018(11) 0.0159(11) C37 0.0458(18) 0.0379(17) 0.071(2) -0.0029(15) 0.0031(16) 0.0287(15) C38 0.0402(16) 0.0398(16) 0.058(2) 0.0151(14) 0.0203(14) 0.0203(14) C42 0.0386(16) 0.0439(17) 0.058(2) 0.0197(15) 0.0155(14) 0.0212(14) C43 0.0493(19) 0.0474(19) 0.064(2) 0.0208(16) 0.0148(17) 0.0233(16) C44 0.069(3) 0.042(2) 0.101(3) 0.024(2) -0.008(2) 0.0245(19) C51 0.165(8) 0.168(8) 0.157(7) -0.043(6) -0.092(6) 0.145(7) C52 0.059(3) 0.086(4) 0.152(6) 0.058(4) -0.015(3) 0.040(3) C53 0.152(9) 0.122(7) 0.36(2) -0.005(11) -0.155(12) 0.085(7) C57 0.24(2) 0.28(3) 0.190(18) -0.117(19) -0.137(18) 0.24(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 Hf1 O1 1.9974(15) . ? Hf1 O3 1.9981(18) . ? Hf1 O2 2.0093(16) . ? Hf1 O4 2.0109(17) . ? Hf1 N1 2.3514(19) . ? Hf1 N2 2.369(2) . ? O1 C1 1.343(3) . ? N1 C10 1.482(3) . ? N1 C11 1.501(3) . ? N1 C9 1.504(3) . ? C1 C2 1.392(3) . ? C1 C6 1.408(3) . ? O2 C17 1.347(3) . ? N2 C29 1.490(3) . ? N2 C30 1.502(3) . ? N2 C28 1.506(3) . ? C2 C3 1.397(3) . ? C2 C9 1.501(3) . ? O3 C20 1.340(3) . ? C3 C4 1.386(4) . ? C3 H3 0.9500 . ? O4 C32 1.366(3) . ? C4 C5 1.387(4) . ? C4 C8 1.513(4) . ? C5 C6 1.401(4) . ? C5 H5 0.9500 . ? C6 C7 1.500(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.500(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.390(3) . ? C12 C17 1.398(3) . ? C13 C14 1.390(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 C19 1.515(4) . ? C15 C16 1.399(4) . ? C15 H15 0.9500 . ? C16 C17 1.399(3) . ? C16 C18 1.505(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.398(4) . ? C20 C25 1.405(3) . ? C21 C22 1.398(4) . ? C21 C26 1.501(4) . ? C22 C23 1.398(4) . ? C22 H22 0.9500 . ? C23 C24 1.388(4) . ? C23 C27 1.512(4) . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C28 1.502(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.497(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.394(4) . ? C31 C32 1.403(4) . ? C32 C33 1.399(4) . ? C33 C34 1.393(4) . ? C33 C38 1.506(4) . ? C34 C35 1.392(4) . ? C34 H34 0.9500 . ? C35 C36 1.386(4) . ? C35 C37 1.513(4) . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C42 C43 1.505(5) . ? C42 C42 1.513(6) 2_566 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.524(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C51 C57 1.260(18) . ? C51 C52 1.286(9) . ? C51 C53 1.446(18) 2_765 ? C52 C53 1.444(18) . ? C53 C51 1.446(18) 2_765 ? C53 C57 1.77(3) 2_765 ? C57 C53 1.77(3) 2_765 ? 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 Hf1 O3 90.72(7) . . ? O1 Hf1 O2 161.59(7) . . ? O3 Hf1 O2 94.05(8) . . ? O1 Hf1 O4 90.24(7) . . ? O3 Hf1 O4 162.42(8) . . ? O2 Hf1 O4 90.53(8) . . ? O1 Hf1 N1 79.96(7) . . ? O3 Hf1 N1 94.31(7) . . ? O2 Hf1 N1 81.95(7) . . ? O4 Hf1 N1 103.14(7) . . ? O1 Hf1 N2 104.92(7) . . ? O3 Hf1 N2 79.99(7) . . ? O2 Hf1 N2 93.43(7) . . ? O4 Hf1 N2 82.80(7) . . ? N1 Hf1 N2 172.44(6) . . ? C1 O1 Hf1 141.77(15) . . ? C10 N1 C11 109.52(19) . . ? C10 N1 C9 109.70(18) . . ? C11 N1 C9 105.65(18) . . ? C10 N1 Hf1 111.77(14) . . ? C11 N1 Hf1 111.36(14) . . ? C9 N1 Hf1 108.64(14) . . ? O1 C1 C2 119.9(2) . . ? O1 C1 C6 119.8(2) . . ? C2 C1 C6 120.3(2) . . ? C17 O2 Hf1 135.70(15) . . ? C29 N2 C30 108.95(19) . . ? C29 N2 C28 109.48(19) . . ? C30 N2 C28 107.20(18) . . ? C29 N2 Hf1 112.46(14) . . ? C30 N2 Hf1 111.10(15) . . ? C28 N2 Hf1 107.49(14) . . ? C1 C2 C3 119.4(2) . . ? C1 C2 C9 121.5(2) . . ? C3 C2 C9 118.9(2) . . ? C20 O3 Hf1 143.05(16) . . ? C4 C3 C2 121.6(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C32 O4 Hf1 129.57(15) . . ? C3 C4 C5 118.1(2) . . ? C3 C4 C8 120.5(3) . . ? C5 C4 C8 121.4(3) . . ? C4 C5 C6 122.3(2) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C7 121.4(2) . . ? C1 C6 C7 120.5(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 N1 116.11(19) . . ? C2 C9 H9A 108.3 . . ? N1 C9 H9A 108.3 . . ? C2 C9 H9B 108.3 . . ? N1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N1 114.96(19) . . ? C12 C11 H11A 108.5 . . ? N1 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? N1 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C13 C12 C17 119.4(2) . . ? C13 C12 C11 121.9(2) . . ? C17 C12 C11 118.5(2) . . ? C14 C13 C12 121.2(2) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 118.2(2) . . ? C15 C14 C19 121.1(3) . . ? C13 C14 C19 120.6(3) . . ? C14 C15 C16 122.6(2) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 C17 117.7(2) . . ? C15 C16 C18 121.9(2) . . ? C17 C16 C18 120.4(2) . . ? O2 C17 C12 118.3(2) . . ? O2 C17 C16 120.9(2) . . ? C12 C17 C16 120.8(2) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 C21 120.1(2) . . ? O3 C20 C25 119.1(2) . . ? C21 C20 C25 120.8(2) . . ? C22 C21 C20 118.2(2) . . ? C22 C21 C26 121.8(2) . . ? C20 C21 C26 120.0(2) . . ? C21 C22 C23 122.2(3) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C22 118.0(2) . . ? C24 C23 C27 121.9(3) . . ? C22 C23 C27 120.0(3) . . ? C23 C24 C25 121.8(2) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C24 C25 C20 118.9(2) . . ? C24 C25 C28 121.0(2) . . ? C20 C25 C28 120.0(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 N2 115.44(19) . . ? C25 C28 H28A 108.4 . . ? N2 C28 H28A 108.4 . . ? C25 C28 H28B 108.4 . . ? N2 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? N2 C29 H29A 109.5 . . ? N2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 N2 113.7(2) . . ? C31 C30 H30A 108.8 . . ? N2 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? N2 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C36 C31 C32 119.2(3) . . ? C36 C31 C30 122.6(2) . . ? C32 C31 C30 118.2(2) . . ? O4 C32 C33 121.1(2) . . ? O4 C32 C31 118.5(2) . . ? C33 C32 C31 120.4(2) . . ? C34 C33 C32 118.2(3) . . ? C34 C33 C38 122.2(3) . . ? C32 C33 C38 119.6(2) . . ? C33 C34 C35 122.6(3) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? C36 C35 C34 117.9(2) . . ? C36 C35 C37 121.5(3) . . ? C34 C35 C37 120.7(3) . . ? C35 C36 C31 121.7(3) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C42 C42 114.3(4) . 2_566 ? C43 C42 H42A 108.7 . . ? C42 C42 H42A 108.7 2_566 . ? C43 C42 H42B 108.7 . . ? C42 C42 H42B 108.7 2_566 . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 113.1(3) . . ? C42 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C42 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C57 C51 C52 147(3) . . ? C57 C51 C53 81.1(19) . 2_765 ? C52 C51 C53 131.5(12) . 2_765 ? C51 C52 C53 131.1(9) . . ? C52 C53 C51 97.4(9) . 2_765 ? C52 C53 C57 142.3(15) . 2_765 ? C51 C53 C57 44.9(11) 2_765 2_765 ? C51 C57 C53 54.0(13) . 2_765 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.968 _refine_diff_density_min -1.975 _refine_diff_density_rms 0.132 #===END data_Zr(1b)2 _database_code_depnum_ccdc_archive 'CCDC 284365' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H94 N2 O4 Zr, 2(C7 H8)' _chemical_formula_sum 'C76 H110 N2 O4 Zr' _chemical_formula_weight 1206.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8630(4) _cell_length_b 15.1170(5) _cell_length_c 20.9790(8) _cell_angle_alpha 91.993(2) _cell_angle_beta 103.472(2) _cell_angle_gamma 103.426(2) _cell_volume 3543.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44520 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 22.465 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18613 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 22.48 _reflns_number_total 9022 _reflns_number_gt 7058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+1.6993P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9022 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Zr1 Zr 0.04487(3) 0.30310(3) 0.256556(18) 0.02887(17) Uani 1 1 d . . . O1 O -0.0975(2) 0.3563(2) 0.24957(13) 0.0329(7) Uani 1 1 d . . . N1 N 0.0369(3) 0.3151(2) 0.36955(16) 0.0310(8) Uani 1 1 d . . . C1 C -0.0083(4) 0.3955(3) 0.3836(2) 0.0320(10) Uani 1 1 d . . . H1A H 0.0406 0.4499 0.3692 0.038 Uiso 1 1 calc R . . H1B H 0.0037 0.4059 0.4318 0.038 Uiso 1 1 calc R . . O2 O 0.1791(2) 0.2462(2) 0.29848(12) 0.0330(7) Uani 1 1 d . . . N2 N 0.0695(3) 0.2956(2) 0.14640(16) 0.0310(8) Uani 1 1 d . . . C2 C 0.1621(4) 0.3333(3) 0.4121(2) 0.0339(10) Uani 1 1 d . . . H2A H 0.2127 0.3854 0.3964 0.041 Uiso 1 1 calc R . . H2B H 0.1611 0.3520 0.4577 0.041 Uiso 1 1 calc R . . O3 O -0.0619(2) 0.1790(2) 0.22165(13) 0.0325(7) Uani 1 1 d . . . C3 C 0.0489(4) 0.1998(3) 0.1181(2) 0.0350(10) Uani 1 1 d . . . H3A H 0.1080 0.1718 0.1462 0.042 Uiso 1 1 calc R . . H3B H 0.0661 0.2018 0.0741 0.042 Uiso 1 1 calc R . . O4 O 0.1513(2) 0.4273(2) 0.25465(13) 0.0338(7) Uani 1 1 d . . . C4 C 0.1976(4) 0.3407(3) 0.1488(2) 0.0341(10) Uani 1 1 d . . . H4A H 0.2494 0.3139 0.1827 0.041 Uiso 1 1 calc R . . H4B H 0.2129 0.3253 0.1058 0.041 Uiso 1 1 calc R . . C5 C -0.0372(4) 0.2312(3) 0.3874(2) 0.0358(10) Uani 1 1 d . . . H5A H -0.0379 0.2392 0.4338 0.054 Uiso 1 1 calc R . . H5B H -0.0036 0.1794 0.3802 0.054 Uiso 1 1 calc R . . H5C H -0.1191 0.2196 0.3599 0.054 Uiso 1 1 calc R . . C6 C -0.0128(4) 0.3415(3) 0.1023(2) 0.0381(11) Uani 1 1 d . . . H6A H -0.0010 0.3374 0.0577 0.057 Uiso 1 1 calc R . . H6B H 0.0044 0.4059 0.1189 0.057 Uiso 1 1 calc R . . H6C H -0.0959 0.3113 0.1014 0.057 Uiso 1 1 calc R . . C11 C -0.1757(4) 0.3734(3) 0.2825(2) 0.0308(10) Uani 1 1 d . . . C12 C -0.2931(4) 0.3777(3) 0.2510(2) 0.0325(10) Uani 1 1 d . . . C13 C -0.3668(4) 0.3931(3) 0.2913(2) 0.0387(11) Uani 1 1 d . . . H13A H -0.4460 0.3956 0.2704 0.046 Uiso 1 1 calc R . . C14 C -0.3328(4) 0.4048(3) 0.3596(2) 0.0374(11) Uani 1 1 d . . . C15 C -0.2148(4) 0.4025(3) 0.3884(2) 0.0375(11) Uani 1 1 d . . . H15A H -0.1868 0.4114 0.4350 0.045 Uiso 1 1 calc R . . C16 C -0.1379(4) 0.3878(3) 0.35120(19) 0.0320(10) Uani 1 1 d . . . C17 C -0.3356(4) 0.3725(3) 0.1753(2) 0.0374(11) Uani 1 1 d . . . C18 C -0.4155(4) 0.4215(3) 0.4024(2) 0.0415(11) Uani 1 1 d . . . C21 C 0.2274(4) 0.2138(3) 0.35533(19) 0.0324(10) Uani 1 1 d . . . C22 C 0.2833(4) 0.1402(3) 0.3565(2) 0.0357(10) Uani 1 1 d . . . C23 C 0.3289(4) 0.1137(3) 0.4182(2) 0.0399(11) Uani 1 1 d . . . H23A H 0.3680 0.0653 0.4202 0.048 Uiso 1 1 calc R . . C24 C 0.3207(4) 0.1540(3) 0.4772(2) 0.0408(11) Uani 1 1 d . . . C25 C 0.2648(4) 0.2245(3) 0.4744(2) 0.0372(11) Uani 1 1 d . . . H25A H 0.2573 0.2527 0.5139 0.045 Uiso 1 1 calc R . . C26 C 0.2189(4) 0.2548(3) 0.4138(2) 0.0345(10) Uani 1 1 d . . . C27 C 0.2958(4) 0.0936(3) 0.2934(2) 0.0389(11) Uani 1 1 d . . . C28 C 0.3771(5) 0.1201(4) 0.5436(2) 0.0493(13) Uani 1 1 d . . . C31 C -0.1201(4) 0.1232(3) 0.16596(19) 0.0305(10) Uani 1 1 d . . . C32 C -0.2218(4) 0.0531(3) 0.1624(2) 0.0325(10) Uani 1 1 d . . . C33 C -0.2789(4) 0.0039(3) 0.1006(2) 0.0366(11) Uani 1 1 d . . . H33A H -0.3497 -0.0428 0.0972 0.044 Uiso 1 1 calc R . . C34 C -0.2375(4) 0.0200(3) 0.0440(2) 0.0364(11) Uani 1 1 d . . . C35 C -0.1323(4) 0.0880(3) 0.0510(2) 0.0383(11) Uani 1 1 d . . . H35A H -0.1008 0.1003 0.0137 0.046 Uiso 1 1 calc R . . C36 C -0.0725(4) 0.1381(3) 0.1106(2) 0.0326(10) Uani 1 1 d . . . C37 C -0.2665(4) 0.0262(3) 0.2243(2) 0.0361(11) Uani 1 1 d . . . C38 C -0.3004(4) -0.0342(3) -0.0235(2) 0.0434(12) Uani 1 1 d . . . C41 C 0.2107(4) 0.4831(3) 0.2170(2) 0.0342(10) Uani 1 1 d . . . C42 C 0.2461(4) 0.5790(3) 0.2311(2) 0.0366(11) Uani 1 1 d . . . C43 C 0.3112(4) 0.6272(3) 0.1911(2) 0.0413(11) Uani 1 1 d . . . H43A H 0.3377 0.6917 0.2006 0.050 Uiso 1 1 calc R . . C44 C 0.3409(4) 0.5882(3) 0.1378(2) 0.0396(11) Uani 1 1 d . . . C45 C 0.2980(4) 0.4947(3) 0.1240(2) 0.0378(11) Uani 1 1 d . . . H45A H 0.3121 0.4656 0.0868 0.045 Uiso 1 1 calc R . . C46 C 0.2348(4) 0.4423(3) 0.1633(2) 0.0327(10) Uani 1 1 d . . . C47 C 0.2093(4) 0.6271(3) 0.2854(2) 0.0393(11) Uani 1 1 d . . . C48 C 0.4181(5) 0.6484(4) 0.0984(3) 0.0554(14) Uani 1 1 d . . . C49 C -0.4659(4) 0.3798(4) 0.1527(2) 0.0564(14) Uani 1 1 d . . . H49A H -0.4896 0.3759 0.1045 0.085 Uiso 1 1 calc R . . H49B H -0.4727 0.4384 0.1709 0.085 Uiso 1 1 calc R . . H49C H -0.5183 0.3297 0.1683 0.085 Uiso 1 1 calc R . . C50 C -0.2542(4) 0.4522(3) 0.1517(2) 0.0468(12) Uani 1 1 d . . . H50A H -0.1709 0.4480 0.1659 0.070 Uiso 1 1 calc R . . H50B H -0.2616 0.5101 0.1707 0.070 Uiso 1 1 calc R . . H50C H -0.2779 0.4494 0.1036 0.070 Uiso 1 1 calc R . . C51 C -0.3297(4) 0.2817(3) 0.1441(2) 0.0442(12) Uani 1 1 d . . . H51A H -0.2477 0.2745 0.1576 0.066 Uiso 1 1 calc R . . H51B H -0.3535 0.2807 0.0960 0.066 Uiso 1 1 calc R . . H51C H -0.3840 0.2316 0.1585 0.066 Uiso 1 1 calc R . . C52 C -0.5382(4) 0.4274(4) 0.3614(3) 0.0565(14) Uani 1 1 d . . . H52A H -0.5281 0.4783 0.3339 0.085 Uiso 1 1 calc R . . H52B H -0.5880 0.4376 0.3909 0.085 Uiso 1 1 calc R . . H52C H -0.5770 0.3702 0.3333 0.085 Uiso 1 1 calc R . . C53 C -0.3582(5) 0.5100(5) 0.4473(3) 0.0752(19) Uani 1 1 d . . . H53A H -0.3455 0.5614 0.4205 0.113 Uiso 1 1 calc R . . H53B H -0.2812 0.5059 0.4752 0.113 Uiso 1 1 calc R . . H53C H -0.4111 0.5194 0.4751 0.113 Uiso 1 1 calc R . . C54 C -0.4356(5) 0.3406(5) 0.4455(3) 0.0665(17) Uani 1 1 d . . . H54A H -0.3583 0.3352 0.4722 0.100 Uiso 1 1 calc R . . H54B H -0.4753 0.2838 0.4170 0.100 Uiso 1 1 calc R . . H54C H -0.4860 0.3516 0.4744 0.100 Uiso 1 1 calc R . . C55 C 0.3671(4) 0.1647(4) 0.2574(2) 0.0446(12) Uani 1 1 d . . . H55A H 0.4467 0.1918 0.2861 0.067 Uiso 1 1 calc R . . H55B H 0.3248 0.2128 0.2461 0.067 Uiso 1 1 calc R . . H55C H 0.3751 0.1349 0.2170 0.067 Uiso 1 1 calc R . . C56 C 0.1700(4) 0.0502(3) 0.2493(2) 0.0464(12) Uani 1 1 d . . . H56A H 0.1258 0.0052 0.2728 0.070 Uiso 1 1 calc R . . H56B H 0.1770 0.0200 0.2088 0.070 Uiso 1 1 calc R . . H56C H 0.1271 0.0979 0.2381 0.070 Uiso 1 1 calc R . . C57 C 0.3607(5) 0.0173(4) 0.3066(2) 0.0510(13) Uani 1 1 d . . . H57A H 0.4415 0.0427 0.3345 0.076 Uiso 1 1 calc R . . H57B H 0.3658 -0.0103 0.2647 0.076 Uiso 1 1 calc R . . H57C H 0.3164 -0.0293 0.3290 0.076 Uiso 1 1 calc R . . C58 C 0.3654(6) 0.1768(4) 0.6024(2) 0.0669(17) Uani 1 1 d . . . H58A H 0.4016 0.1539 0.6433 0.100 Uiso 1 1 calc R . . H58B H 0.2806 0.1721 0.5998 0.100 Uiso 1 1 calc R . . H58C H 0.4065 0.2409 0.6018 0.100 Uiso 1 1 calc R . . C59 C 0.3146(6) 0.0198(4) 0.5455(3) 0.0702(17) Uani 1 1 d . . . H59A H 0.3502 -0.0016 0.5872 0.105 Uiso 1 1 calc R . . H59B H 0.3243 -0.0171 0.5088 0.105 Uiso 1 1 calc R . . H59C H 0.2292 0.0141 0.5418 0.105 Uiso 1 1 calc R . . C60 C 0.5099(5) 0.1290(4) 0.5492(2) 0.0609(15) Uani 1 1 d . . . H60A H 0.5457 0.1075 0.5909 0.091 Uiso 1 1 calc R . . H60B H 0.5499 0.1931 0.5479 0.091 Uiso 1 1 calc R . . H60C H 0.5194 0.0920 0.5124 0.091 Uiso 1 1 calc R . . C61 C -0.1628(4) 0.0040(3) 0.2747(2) 0.0454(12) Uani 1 1 d . . . H61A H -0.1887 -0.0137 0.3145 0.068 Uiso 1 1 calc R . . H61B H -0.0950 0.0579 0.2860 0.068 Uiso 1 1 calc R . . H61C H -0.1383 -0.0466 0.2558 0.068 Uiso 1 1 calc R . . C62 C -0.3085(4) 0.1043(3) 0.2530(2) 0.0433(12) Uani 1 1 d . . . H62A H -0.3363 0.0859 0.2922 0.065 Uiso 1 1 calc R . . H62B H -0.3741 0.1178 0.2200 0.065 Uiso 1 1 calc R . . H62C H -0.2418 0.1589 0.2652 0.065 Uiso 1 1 calc R . . C63 C -0.3703(5) -0.0587(4) 0.2098(2) 0.0534(13) Uani 1 1 d . . . H63A H -0.3953 -0.0734 0.2503 0.080 Uiso 1 1 calc R . . H63B H -0.3448 -0.1101 0.1929 0.080 Uiso 1 1 calc R . . H63C H -0.4374 -0.0472 0.1767 0.080 Uiso 1 1 calc R . . C64 C -0.2118(5) -0.0803(4) -0.0459(2) 0.0524(13) Uani 1 1 d . . . H64A H -0.1891 -0.1234 -0.0144 0.079 Uiso 1 1 calc R . . H64B H -0.1402 -0.0337 -0.0479 0.079 Uiso 1 1 calc R . . H64C H -0.2494 -0.1132 -0.0895 0.079 Uiso 1 1 calc R . . C65 C -0.3359(5) 0.0326(4) -0.0741(2) 0.0573(14) Uani 1 1 d . . . H65A H -0.3761 -0.0015 -0.1171 0.086 Uiso 1 1 calc R . . H65B H -0.2640 0.0776 -0.0778 0.086 Uiso 1 1 calc R . . H65C H -0.3903 0.0642 -0.0596 0.086 Uiso 1 1 calc R . . C66 C -0.4114(5) -0.1077(4) -0.0212(3) 0.0630(16) Uani 1 1 d . . . H66A H -0.3889 -0.1504 0.0107 0.095 Uiso 1 1 calc R . . H66B H -0.4472 -0.1410 -0.0649 0.095 Uiso 1 1 calc R . . H66C H -0.4695 -0.0791 -0.0079 0.095 Uiso 1 1 calc R . . C67 C 0.2539(5) 0.7317(3) 0.2894(3) 0.0542(13) Uani 1 1 d . . . H67A H 0.2205 0.7533 0.2473 0.081 Uiso 1 1 calc R . . H67B H 0.3414 0.7487 0.2988 0.081 Uiso 1 1 calc R . . H67C H 0.2282 0.7598 0.3246 0.081 Uiso 1 1 calc R . . C68 C 0.2641(5) 0.5971(4) 0.3527(2) 0.0477(12) Uani 1 1 d . . . H68A H 0.2375 0.5306 0.3520 0.072 Uiso 1 1 calc R . . H68B H 0.2382 0.6264 0.3873 0.072 Uiso 1 1 calc R . . H68C H 0.3516 0.6153 0.3617 0.072 Uiso 1 1 calc R . . C69 C 0.0717(4) 0.6037(4) 0.2711(2) 0.0458(12) Uani 1 1 d . . . H69A H 0.0407 0.5373 0.2683 0.069 Uiso 1 1 calc R . . H69B H 0.0391 0.6263 0.2293 0.069 Uiso 1 1 calc R . . H69C H 0.0479 0.6327 0.3067 0.069 Uiso 1 1 calc R . . C70 C 0.5394(7) 0.6915(6) 0.1459(4) 0.109(3) Uani 1 1 d . . . H70A H 0.5912 0.7305 0.1225 0.164 Uiso 1 1 calc R . . H70B H 0.5768 0.6432 0.1636 0.164 Uiso 1 1 calc R . . H70C H 0.5280 0.7283 0.1822 0.164 Uiso 1 1 calc R . . C71 C 0.3617(10) 0.7203(7) 0.0703(6) 0.161(5) Uani 1 1 d . . . H71A H 0.2844 0.6921 0.0397 0.241 Uiso 1 1 calc R . . H71B H 0.4138 0.7588 0.0468 0.241 Uiso 1 1 calc R . . H71C H 0.3493 0.7579 0.1059 0.241 Uiso 1 1 calc R . . C72 C 0.4458(5) 0.5942(4) 0.0451(3) 0.0629(15) Uani 1 1 d . . . H72A H 0.3716 0.5658 0.0120 0.094 Uiso 1 1 calc R . . H72B H 0.4830 0.5466 0.0643 0.094 Uiso 1 1 calc R . . H72C H 0.5008 0.6349 0.0243 0.094 Uiso 1 1 calc R . . C81 C 0.0452(8) 0.2381(5) -0.1028(4) 0.076(5) Uani 0.475(10) 1 d PG A 1 C82 C 0.1642(7) 0.2814(6) -0.0739(4) 0.049(4) Uani 0.475(10) 1 d PG A 1 H82 H 0.2247 0.2494 -0.0728 0.059 Uiso 0.475(10) 1 calc PR A 1 C83 C 0.1947(7) 0.3715(6) -0.0468(4) 0.060(4) Uani 0.475(10) 1 d PG A 1 H83 H 0.2760 0.4011 -0.0270 0.072 Uiso 0.475(10) 1 calc PR A 1 C84 C 0.1062(9) 0.4183(5) -0.0484(4) 0.068(5) Uani 0.475(10) 1 d PG A 1 H84 H 0.1270 0.4798 -0.0299 0.082 Uiso 0.475(10) 1 calc PR A 1 C85 C -0.0128(8) 0.3749(7) -0.0773(4) 0.058(4) Uani 0.475(10) 1 d PG A 1 H85 H -0.0732 0.4069 -0.0785 0.070 Uiso 0.475(10) 1 calc PR A 1 C86 C -0.0432(6) 0.2848(7) -0.1045(4) 0.064(6) Uani 0.475(10) 1 d PG A 1 H86 H -0.1245 0.2552 -0.1242 0.077 Uiso 0.475(10) 1 calc PR A 1 C87 C 0.0185(13) 0.1298(6) -0.1334(7) 0.114(9) Uani 0.475(10) 1 d PG A 1 H87A H 0.0875 0.1209 -0.1486 0.170 Uiso 0.475(10) 1 calc PR A 1 H87B H -0.0526 0.1158 -0.1704 0.170 Uiso 0.475(10) 1 calc PR A 1 H87C H 0.0049 0.0892 -0.0991 0.170 Uiso 0.475(10) 1 calc PR A 1 C91 C 0.0381(7) 0.3233(5) -0.0849(3) 0.055(3) Uani 0.525(10) 1 d PG A 2 C92 C -0.0617(6) 0.2505(6) -0.1072(3) 0.059(4) Uani 0.525(10) 1 d PG A 2 H92 H -0.1395 0.2592 -0.1103 0.071 Uiso 0.525(10) 1 calc PR A 2 C93 C -0.0476(8) 0.1650(5) -0.1249(3) 0.072(4) Uani 0.525(10) 1 d PG A 2 H93 H -0.1157 0.1153 -0.1401 0.086 Uiso 0.525(10) 1 calc PR A 2 C94 C 0.0663(10) 0.1523(5) -0.1202(3) 0.084(6) Uani 0.525(10) 1 d PG A 2 H94 H 0.0760 0.0939 -0.1323 0.101 Uiso 0.525(10) 1 calc PR A 2 C95 C 0.1661(7) 0.2251(7) -0.0979(4) 0.127(9) Uani 0.525(10) 1 d PG A 2 H95 H 0.2439 0.2164 -0.0948 0.152 Uiso 0.525(10) 1 calc PR A 2 C96 C 0.1520(6) 0.3106(6) -0.0803(4) 0.102(8) Uani 0.525(10) 1 d PG A 2 H96 H 0.2202 0.3603 -0.0650 0.122 Uiso 0.525(10) 1 calc PR A 2 C97 C 0.0295(12) 0.4188(5) -0.0647(3) 0.078(6) Uani 0.525(10) 1 d PG A 2 H97A H -0.0518 0.4163 -0.0607 0.117 Uiso 0.525(10) 1 calc PR A 2 H97B H 0.0481 0.4595 -0.0982 0.117 Uiso 0.525(10) 1 calc PR A 2 H97C H 0.0866 0.4419 -0.0223 0.117 Uiso 0.525(10) 1 calc PR A 2 C101 C 0.1136(7) 0.2815(5) 0.6519(3) 0.104(3) Uani 1 1 d R . . C102 C 0.0772(7) 0.3435(5) 0.6077(3) 0.134(5) Uani 1 1 d R . . H102 H 0.1263 0.4033 0.6092 0.161 Uiso 1 1 calc R . . C103 C -0.029(2) 0.3157(16) 0.5633(8) 0.216(15) Uani 1 1 d . . . H103 H -0.0555 0.3590 0.5354 0.259 Uiso 1 1 calc R . . C104 C -0.0994(19) 0.2323(19) 0.5558(9) 0.210(13) Uani 1 1 d . . . H104 H -0.1726 0.2154 0.5228 0.252 Uiso 1 1 calc R . . C105 C -0.0649(12) 0.1750(10) 0.5949(6) 0.147(4) Uani 1 1 d . . . H105 H -0.1141 0.1146 0.5899 0.177 Uiso 1 1 calc R . . C106 C 0.0354(9) 0.1958(6) 0.6418(4) 0.095(2) Uani 1 1 d . . . H106 H 0.0547 0.1504 0.6696 0.115 Uiso 1 1 calc R . . C107 C 0.2138(11) 0.3060(10) 0.7033(7) 0.199(7) Uani 1 1 d . . . H10A H 0.1901 0.3143 0.7444 0.298 Uiso 1 1 calc R . . H10B H 0.2656 0.3633 0.6958 0.298 Uiso 1 1 calc R . . H10C H 0.2571 0.2578 0.7064 0.298 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 Zr1 0.0320(3) 0.0359(3) 0.0204(2) 0.00565(17) 0.00871(17) 0.00900(19) O1 0.0349(16) 0.0405(18) 0.0251(15) 0.0068(13) 0.0100(13) 0.0097(14) N1 0.033(2) 0.039(2) 0.0239(18) 0.0062(16) 0.0091(15) 0.0107(17) C1 0.038(2) 0.035(3) 0.024(2) 0.0028(19) 0.0084(19) 0.010(2) O2 0.0374(17) 0.0424(18) 0.0221(15) 0.0067(13) 0.0097(12) 0.0126(14) N2 0.034(2) 0.037(2) 0.0252(18) 0.0078(16) 0.0108(15) 0.0092(16) C2 0.033(2) 0.044(3) 0.024(2) 0.0034(19) 0.0043(18) 0.011(2) O3 0.0355(16) 0.0410(18) 0.0217(15) 0.0060(13) 0.0101(12) 0.0073(14) C3 0.041(3) 0.037(3) 0.029(2) 0.003(2) 0.014(2) 0.009(2) O4 0.0369(17) 0.0366(17) 0.0283(15) 0.0040(13) 0.0104(13) 0.0071(14) C4 0.038(3) 0.042(3) 0.026(2) 0.0069(19) 0.0158(19) 0.010(2) C5 0.043(3) 0.039(3) 0.025(2) 0.0040(19) 0.011(2) 0.008(2) C6 0.043(3) 0.048(3) 0.028(2) 0.010(2) 0.011(2) 0.015(2) C11 0.028(2) 0.038(3) 0.030(2) 0.0076(19) 0.0122(19) 0.0082(19) C12 0.032(2) 0.036(3) 0.030(2) 0.0080(19) 0.0094(19) 0.008(2) C13 0.034(3) 0.044(3) 0.039(3) 0.010(2) 0.009(2) 0.011(2) C14 0.036(3) 0.044(3) 0.034(3) 0.002(2) 0.012(2) 0.011(2) C15 0.041(3) 0.045(3) 0.026(2) 0.001(2) 0.009(2) 0.010(2) C16 0.033(2) 0.039(3) 0.028(2) 0.0042(19) 0.0113(19) 0.011(2) C17 0.035(2) 0.048(3) 0.030(2) 0.010(2) 0.0062(19) 0.013(2) C18 0.032(3) 0.057(3) 0.037(3) -0.004(2) 0.013(2) 0.009(2) C21 0.036(2) 0.041(3) 0.022(2) 0.0105(19) 0.0083(18) 0.011(2) C22 0.041(3) 0.039(3) 0.031(2) 0.007(2) 0.010(2) 0.015(2) C23 0.044(3) 0.047(3) 0.036(3) 0.015(2) 0.015(2) 0.021(2) C24 0.045(3) 0.055(3) 0.026(2) 0.011(2) 0.009(2) 0.018(2) C25 0.040(3) 0.050(3) 0.024(2) 0.005(2) 0.0101(19) 0.014(2) C26 0.037(2) 0.045(3) 0.026(2) 0.006(2) 0.0110(19) 0.015(2) C27 0.048(3) 0.044(3) 0.029(2) 0.003(2) 0.010(2) 0.018(2) C28 0.063(3) 0.063(3) 0.032(3) 0.017(2) 0.014(2) 0.032(3) C31 0.034(2) 0.035(2) 0.021(2) 0.0024(19) 0.0047(18) 0.009(2) C32 0.034(2) 0.033(2) 0.031(2) 0.0050(19) 0.0088(19) 0.007(2) C33 0.036(3) 0.036(3) 0.038(3) 0.005(2) 0.012(2) 0.006(2) C34 0.040(3) 0.040(3) 0.030(2) -0.001(2) 0.011(2) 0.010(2) C35 0.042(3) 0.047(3) 0.028(2) 0.002(2) 0.012(2) 0.013(2) C36 0.034(2) 0.037(3) 0.027(2) 0.0037(19) 0.0090(19) 0.009(2) C37 0.041(3) 0.038(3) 0.027(2) 0.009(2) 0.010(2) 0.003(2) C38 0.041(3) 0.052(3) 0.033(3) -0.007(2) 0.007(2) 0.008(2) C41 0.030(2) 0.046(3) 0.029(2) 0.012(2) 0.0102(19) 0.010(2) C42 0.042(3) 0.040(3) 0.030(2) 0.005(2) 0.011(2) 0.013(2) C43 0.049(3) 0.037(3) 0.041(3) 0.009(2) 0.015(2) 0.011(2) C44 0.041(3) 0.042(3) 0.040(3) 0.014(2) 0.018(2) 0.008(2) C45 0.043(3) 0.045(3) 0.031(2) 0.008(2) 0.017(2) 0.013(2) C46 0.033(2) 0.040(3) 0.028(2) 0.007(2) 0.0118(19) 0.009(2) C47 0.052(3) 0.035(3) 0.033(2) 0.001(2) 0.014(2) 0.011(2) C48 0.065(4) 0.050(3) 0.064(3) 0.015(3) 0.043(3) 0.008(3) C49 0.051(3) 0.089(4) 0.034(3) 0.011(3) 0.005(2) 0.028(3) C50 0.056(3) 0.051(3) 0.036(3) 0.014(2) 0.010(2) 0.019(3) C51 0.047(3) 0.053(3) 0.031(2) 0.003(2) 0.007(2) 0.011(2) C52 0.048(3) 0.072(4) 0.060(3) 0.008(3) 0.027(3) 0.024(3) C53 0.053(3) 0.088(5) 0.084(4) -0.035(4) 0.030(3) 0.010(3) C54 0.055(3) 0.107(5) 0.045(3) 0.017(3) 0.023(3) 0.021(3) C55 0.052(3) 0.060(3) 0.030(2) 0.005(2) 0.017(2) 0.024(3) C56 0.060(3) 0.046(3) 0.033(3) 0.001(2) 0.011(2) 0.013(2) C57 0.070(3) 0.057(3) 0.036(3) 0.004(2) 0.012(2) 0.036(3) C58 0.096(5) 0.093(5) 0.029(3) 0.020(3) 0.016(3) 0.054(4) C59 0.095(5) 0.078(4) 0.048(3) 0.033(3) 0.020(3) 0.035(4) C60 0.070(4) 0.080(4) 0.037(3) 0.014(3) 0.002(3) 0.036(3) C61 0.056(3) 0.051(3) 0.034(3) 0.018(2) 0.016(2) 0.016(2) C62 0.045(3) 0.055(3) 0.036(3) 0.012(2) 0.020(2) 0.012(2) C63 0.058(3) 0.054(3) 0.043(3) 0.011(2) 0.017(2) -0.002(3) C64 0.058(3) 0.059(3) 0.039(3) -0.007(2) 0.014(2) 0.014(3) C65 0.060(3) 0.076(4) 0.034(3) -0.002(3) 0.003(2) 0.022(3) C66 0.053(3) 0.072(4) 0.050(3) -0.025(3) 0.011(3) -0.005(3) C67 0.076(4) 0.041(3) 0.049(3) 0.001(2) 0.024(3) 0.011(3) C68 0.055(3) 0.049(3) 0.036(3) 0.001(2) 0.013(2) 0.007(2) C69 0.052(3) 0.053(3) 0.039(3) 0.005(2) 0.019(2) 0.020(3) C70 0.102(6) 0.104(6) 0.107(6) -0.030(5) 0.071(5) -0.046(5) C71 0.230(11) 0.148(8) 0.231(11) 0.155(9) 0.198(10) 0.134(9) C72 0.074(4) 0.067(4) 0.058(3) 0.021(3) 0.042(3) 0.010(3) C81 0.053(10) 0.117(15) 0.043(7) 0.012(8) 0.010(6) -0.004(9) C82 0.069(10) 0.037(8) 0.049(7) 0.011(6) 0.021(7) 0.022(7) C83 0.063(9) 0.056(9) 0.059(8) 0.006(6) 0.032(7) -0.007(7) C84 0.079(11) 0.079(11) 0.047(8) 0.014(7) 0.036(8) -0.003(9) C85 0.098(12) 0.036(10) 0.037(7) -0.004(6) 0.014(7) 0.013(9) C86 0.026(8) 0.094(14) 0.047(9) 0.010(8) 0.001(7) -0.026(8) C87 0.084(15) 0.121(19) 0.096(15) -0.013(12) 0.015(11) -0.041(13) C91 0.088(10) 0.052(8) 0.034(6) 0.027(6) 0.023(6) 0.023(7) C92 0.074(10) 0.040(8) 0.062(9) 0.006(6) 0.021(7) 0.006(7) C93 0.055(8) 0.081(10) 0.072(8) 0.006(7) 0.018(7) 0.001(7) C94 0.142(18) 0.042(8) 0.095(12) 0.024(8) 0.062(11) 0.038(11) C95 0.087(11) 0.111(16) 0.24(2) 0.103(16) 0.103(14) 0.065(12) C96 0.060(11) 0.084(14) 0.18(2) 0.079(14) 0.046(12) 0.030(10) C97 0.121(17) 0.041(10) 0.059(9) -0.011(7) 0.030(10) -0.009(10) C101 0.101(6) 0.121(8) 0.105(7) -0.019(6) 0.043(5) 0.047(6) C102 0.240(14) 0.107(7) 0.149(10) 0.070(7) 0.161(10) 0.102(9) C103 0.35(4) 0.36(3) 0.092(12) 0.130(18) 0.148(18) 0.30(3) C104 0.174(16) 0.44(4) 0.069(8) -0.005(18) 0.039(9) 0.17(2) C105 0.156(11) 0.215(14) 0.089(8) -0.005(8) 0.042(8) 0.072(10) C106 0.140(8) 0.088(6) 0.085(6) 0.027(5) 0.046(5) 0.060(6) C107 0.148(10) 0.263(17) 0.173(12) -0.117(11) 0.039(9) 0.047(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O3 2.008(3) . ? Zr1 O1 2.011(3) . ? Zr1 O4 2.012(3) . ? Zr1 O2 2.021(3) . ? Zr1 N1 2.397(3) . ? Zr1 N2 2.398(3) . ? O1 C11 1.342(5) . ? N1 C5 1.480(6) . ? N1 C1 1.483(5) . ? N1 C2 1.502(5) . ? C1 C16 1.504(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C21 1.358(5) . ? N2 C3 1.489(5) . ? N2 C6 1.493(5) . ? N2 C4 1.502(5) . ? C2 C26 1.492(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C31 1.355(5) . ? C3 C36 1.493(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C41 1.365(5) . ? C4 C46 1.496(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C16 1.400(6) . ? C11 C12 1.414(6) . ? C12 C13 1.399(6) . ? C12 C17 1.543(6) . ? C13 C14 1.387(6) . ? C13 H13A 0.9500 . ? C14 C15 1.398(6) . ? C14 C18 1.531(6) . ? C15 C16 1.380(6) . ? C15 H15A 0.9500 . ? C17 C51 1.523(7) . ? C17 C50 1.534(7) . ? C17 C49 1.539(6) . ? C18 C53 1.527(7) . ? C18 C52 1.533(6) . ? C18 C54 1.553(8) . ? C21 C26 1.391(6) . ? C21 C22 1.419(6) . ? C22 C23 1.393(6) . ? C22 C27 1.531(6) . ? C23 C24 1.395(6) . ? C23 H23A 0.9500 . ? C24 C25 1.377(6) . ? C24 C28 1.556(6) . ? C25 C26 1.399(6) . ? C25 H25A 0.9500 . ? C27 C57 1.527(6) . ? C27 C56 1.541(7) . ? C27 C55 1.541(7) . ? C28 C60 1.526(7) . ? C28 C58 1.529(7) . ? C28 C59 1.531(8) . ? C31 C32 1.394(6) . ? C31 C36 1.408(6) . ? C32 C33 1.410(6) . ? C32 C37 1.546(6) . ? C33 C34 1.394(6) . ? C33 H33A 0.9500 . ? C34 C35 1.394(6) . ? C34 C38 1.543(6) . ? C35 C36 1.383(6) . ? C35 H35A 0.9500 . ? C37 C63 1.522(7) . ? C37 C61 1.535(6) . ? C37 C62 1.538(6) . ? C38 C66 1.525(7) . ? C38 C64 1.535(7) . ? C38 C65 1.546(7) . ? C41 C46 1.383(6) . ? C41 C42 1.412(6) . ? C42 C43 1.385(6) . ? C42 C47 1.530(6) . ? C43 C44 1.398(6) . ? C43 H43A 0.9500 . ? C44 C45 1.382(7) . ? C44 C48 1.539(7) . ? C45 C46 1.388(6) . ? C45 H45A 0.9500 . ? C47 C67 1.539(7) . ? C47 C69 1.540(6) . ? C47 C68 1.541(6) . ? C48 C71 1.475(9) . ? C48 C72 1.504(7) . ? C48 C70 1.530(9) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C81 C87 1.6676 . ? C82 C83 1.3900 . ? C82 H82 0.9500 . ? C83 C84 1.3900 . ? C83 H83 0.9500 . ? C84 C85 1.3900 . ? C84 H84 0.9500 . ? C85 C86 1.3900 . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 C97 1.5222 . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C101 C107 1.373(12) . ? C101 C106 1.383(11) . ? C101 C102 1.4092(11) . ? C102 C103 1.35(2) . ? C102 H102 0.9500 . ? C103 C104 1.32(3) . ? C103 H103 0.9500 . ? C104 C105 1.28(2) . ? C104 H104 0.9500 . ? C105 C106 1.320(14) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 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 O3 Zr1 O1 91.16(11) . . ? O3 Zr1 O4 157.87(11) . . ? O1 Zr1 O4 91.11(11) . . ? O3 Zr1 O2 90.57(11) . . ? O1 Zr1 O2 158.16(11) . . ? O4 Zr1 O2 95.42(11) . . ? O3 Zr1 N1 103.25(11) . . ? O1 Zr1 N1 79.09(11) . . ? O4 Zr1 N1 98.80(12) . . ? O2 Zr1 N1 79.33(11) . . ? O3 Zr1 N2 79.92(11) . . ? O1 Zr1 N2 104.16(11) . . ? O4 Zr1 N2 78.18(11) . . ? O2 Zr1 N2 97.57(11) . . ? N1 Zr1 N2 175.52(11) . . ? C11 O1 Zr1 143.5(2) . . ? C5 N1 C1 110.4(3) . . ? C5 N1 C2 109.3(3) . . ? C1 N1 C2 106.0(3) . . ? C5 N1 Zr1 112.3(2) . . ? C1 N1 Zr1 110.1(2) . . ? C2 N1 Zr1 108.5(2) . . ? N1 C1 C16 115.3(3) . . ? N1 C1 H1A 108.5 . . ? C16 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? C16 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C21 O2 Zr1 142.3(2) . . ? C3 N2 C6 109.0(3) . . ? C3 N2 C4 105.8(3) . . ? C6 N2 C4 110.6(3) . . ? C3 N2 Zr1 112.2(2) . . ? C6 N2 Zr1 111.1(2) . . ? C4 N2 Zr1 108.0(2) . . ? C26 C2 N1 115.3(4) . . ? C26 C2 H2A 108.5 . . ? N1 C2 H2A 108.5 . . ? C26 C2 H2B 108.5 . . ? N1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C31 O3 Zr1 144.0(3) . . ? N2 C3 C36 117.4(3) . . ? N2 C3 H3A 108.0 . . ? C36 C3 H3A 108.0 . . ? N2 C3 H3B 108.0 . . ? C36 C3 H3B 108.0 . . ? H3A C3 H3B 107.2 . . ? C41 O4 Zr1 144.8(3) . . ? C46 C4 N2 116.3(3) . . ? C46 C4 H4A 108.2 . . ? N2 C4 H4A 108.2 . . ? C46 C4 H4B 108.2 . . ? N2 C4 H4B 108.2 . . ? H4A C4 H4B 107.4 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C11 C16 117.8(3) . . ? O1 C11 C12 123.2(4) . . ? C16 C11 C12 119.0(4) . . ? C13 C12 C11 117.3(4) . . ? C13 C12 C17 121.2(4) . . ? C11 C12 C17 121.4(4) . . ? C14 C13 C12 124.9(4) . . ? C14 C13 H13A 117.6 . . ? C12 C13 H13A 117.6 . . ? C13 C14 C15 115.7(4) . . ? C13 C14 C18 123.7(4) . . ? C15 C14 C18 120.5(4) . . ? C16 C15 C14 122.0(4) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? C15 C16 C11 121.0(4) . . ? C15 C16 C1 120.2(4) . . ? C11 C16 C1 118.5(4) . . ? C51 C17 C50 110.4(4) . . ? C51 C17 C49 107.1(4) . . ? C50 C17 C49 108.9(4) . . ? C51 C17 C12 110.6(3) . . ? C50 C17 C12 107.9(4) . . ? C49 C17 C12 111.9(4) . . ? C53 C18 C14 110.2(4) . . ? C53 C18 C52 108.7(4) . . ? C14 C18 C52 112.5(4) . . ? C53 C18 C54 109.0(5) . . ? C14 C18 C54 108.6(4) . . ? C52 C18 C54 107.8(4) . . ? O2 C21 C26 117.3(4) . . ? O2 C21 C22 122.6(4) . . ? C26 C21 C22 120.1(4) . . ? C23 C22 C21 116.6(4) . . ? C23 C22 C27 121.4(4) . . ? C21 C22 C27 122.0(4) . . ? C22 C23 C24 123.9(4) . . ? C22 C23 H23A 118.0 . . ? C24 C23 H23A 118.0 . . ? C25 C24 C23 118.1(4) . . ? C25 C24 C28 122.3(4) . . ? C23 C24 C28 119.6(4) . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C21 C26 C25 120.9(4) . . ? C21 C26 C2 119.7(4) . . ? C25 C26 C2 119.5(4) . . ? C57 C27 C22 112.8(4) . . ? C57 C27 C56 107.3(4) . . ? C22 C27 C56 108.9(4) . . ? C57 C27 C55 107.9(4) . . ? C22 C27 C55 109.5(4) . . ? C56 C27 C55 110.4(4) . . ? C60 C28 C58 108.1(4) . . ? C60 C28 C59 109.4(4) . . ? C58 C28 C59 109.2(5) . . ? C60 C28 C24 109.2(4) . . ? C58 C28 C24 111.4(4) . . ? C59 C28 C24 109.4(4) . . ? O3 C31 C32 122.7(4) . . ? O3 C31 C36 116.9(4) . . ? C32 C31 C36 120.3(4) . . ? C31 C32 C33 117.3(4) . . ? C31 C32 C37 121.7(4) . . ? C33 C32 C37 120.9(4) . . ? C34 C33 C32 123.7(4) . . ? C34 C33 H33A 118.2 . . ? C32 C33 H33A 118.2 . . ? C35 C34 C33 116.6(4) . . ? C35 C34 C38 120.0(4) . . ? C33 C34 C38 123.4(4) . . ? C36 C35 C34 122.0(4) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C35 C36 C31 119.8(4) . . ? C35 C36 C3 119.8(4) . . ? C31 C36 C3 120.0(4) . . ? C63 C37 C61 107.5(4) . . ? C63 C37 C62 107.9(4) . . ? C61 C37 C62 110.7(4) . . ? C63 C37 C32 112.2(4) . . ? C61 C37 C32 107.6(4) . . ? C62 C37 C32 110.8(3) . . ? C66 C38 C64 108.6(4) . . ? C66 C38 C34 112.5(4) . . ? C64 C38 C34 108.4(4) . . ? C66 C38 C65 109.4(4) . . ? C64 C38 C65 108.7(4) . . ? C34 C38 C65 109.1(4) . . ? O4 C41 C46 117.4(4) . . ? O4 C41 C42 122.2(4) . . ? C46 C41 C42 120.4(4) . . ? C43 C42 C41 116.3(4) . . ? C43 C42 C47 121.8(4) . . ? C41 C42 C47 121.8(4) . . ? C42 C43 C44 124.9(4) . . ? C42 C43 H43A 117.6 . . ? C44 C43 H43A 117.6 . . ? C45 C44 C43 116.2(4) . . ? C45 C44 C48 123.4(4) . . ? C43 C44 C48 120.3(4) . . ? C44 C45 C46 121.5(4) . . ? C44 C45 H45A 119.3 . . ? C46 C45 H45A 119.3 . . ? C41 C46 C45 120.5(4) . . ? C41 C46 C4 120.2(4) . . ? C45 C46 C4 119.2(4) . . ? C42 C47 C67 112.2(4) . . ? C42 C47 C69 109.3(4) . . ? C67 C47 C69 107.7(4) . . ? C42 C47 C68 109.6(4) . . ? C67 C47 C68 107.2(4) . . ? C69 C47 C68 110.9(4) . . ? C71 C48 C72 110.2(6) . . ? C71 C48 C70 110.1(7) . . ? C72 C48 C70 105.1(5) . . ? C71 C48 C44 111.2(5) . . ? C72 C48 C44 112.8(4) . . ? C70 C48 C44 107.1(5) . . ? C17 C49 H49A 109.5 . . ? C17 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C17 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C17 C50 H50A 109.5 . . ? C17 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C17 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C17 C51 H51A 109.5 . . ? C17 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C17 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C18 C52 H52A 109.5 . . ? C18 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C18 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C18 C53 H53A 109.5 . . ? C18 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C18 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C18 C54 H54A 109.5 . . ? C18 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C18 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C27 C55 H55A 109.5 . . ? C27 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C27 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C27 C56 H56A 109.5 . . ? C27 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C27 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C27 C57 H57A 109.5 . . ? C27 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C27 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C28 C58 H58A 109.5 . . ? C28 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C28 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C28 C59 H59A 109.5 . . ? C28 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C28 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C28 C60 H60A 109.5 . . ? C28 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C28 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C37 C61 H61A 109.5 . . ? C37 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C37 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C37 C62 H62A 109.5 . . ? C37 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C37 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C37 C63 H63A 109.5 . . ? C37 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C37 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C38 C64 H64A 109.5 . . ? C38 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C38 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C38 C65 H65A 109.5 . . ? C38 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C38 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C38 C66 H66A 109.5 . . ? C38 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C38 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C47 C67 H67A 109.5 . . ? C47 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C47 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C47 C68 H68A 109.5 . . ? C47 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C47 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C47 C69 H69A 109.5 . . ? C47 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C47 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C48 C70 H70A 109.5 . . ? C48 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C48 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C48 C71 H71A 109.5 . . ? C48 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C48 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C48 C72 H72A 109.5 . . ? C48 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C48 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C82 C81 C86 120.0 . . ? C82 C81 C87 116.1 . . ? C86 C81 C87 123.9 . . ? C83 C82 C81 120.0 . . ? C83 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C82 C83 C84 120.0 . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C83 C84 C85 120.0 . . ? C83 C84 H84 120.0 . . ? C85 C84 H84 120.0 . . ? C84 C85 C86 120.0 . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C81 120.0 . . ? C85 C86 H86 120.0 . . ? C81 C86 H86 120.0 . . ? C92 C91 C96 120.0 . . ? C92 C91 C97 122.9 . . ? C96 C91 C97 117.1 . . ? C93 C92 C91 120.0 . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95 120.0 . . ? C94 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C107 C101 C106 122.8(9) . . ? C107 C101 C102 122.7(8) . . ? C106 C101 C102 114.3(5) . . ? C103 C102 C101 118.2(10) . . ? C103 C102 H102 120.9 . . ? C101 C102 H102 120.9 . . ? C104 C103 C102 124.5(18) . . ? C104 C103 H103 117.8 . . ? C102 C103 H103 117.8 . . ? C105 C104 C103 117(2) . . ? C105 C104 H104 121.3 . . ? C103 C104 H104 121.3 . . ? C104 C105 C106 123.3(18) . . ? C104 C105 H105 118.3 . . ? C106 C105 H105 118.3 . . ? C105 C106 C101 122.3(9) . . ? C105 C106 H106 118.9 . . ? C101 C106 H106 118.9 . . ? C101 C107 H10A 109.5 . . ? C101 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C101 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.600 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.108 #===END data_Ti(1c)(OPr)2 _database_code_depnum_ccdc_archive 'CCDC 284366' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H65 N O4 Ti, 0.5(C6 H14)' _chemical_formula_sum 'C46 H72 N O4 Ti' _chemical_formula_weight 750.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.33900(10) _cell_length_b 9.63900(10) _cell_length_c 27.3100(3) _cell_angle_alpha 86.7660(10) _cell_angle_beta 81.4570(10) _cell_angle_gamma 68.4520(10) _cell_volume 2261.22(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 44815 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35306 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 27.59 _reflns_number_total 10208 _reflns_number_gt 8980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+1.0545P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10208 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.017 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.60657(3) 0.30392(3) 0.245438(9) 0.01944(8) Uani 1 1 d . A . O1 O 0.59465(12) 0.17863(12) 0.29846(4) 0.0256(2) Uani 1 1 d . . . N1 N 0.85898(13) 0.12959(13) 0.23045(4) 0.0176(2) Uani 1 1 d . . . C1 C 0.92386(17) 0.09470(17) 0.27827(5) 0.0212(3) Uani 1 1 d . . . H1A H 0.9207 0.1887 0.2921 0.025 Uiso 1 1 calc R . . H1B H 1.0344 0.0286 0.2714 0.025 Uiso 1 1 calc R . . O2 O 0.60827(12) 0.24871(11) 0.18111(4) 0.0227(2) Uani 1 1 d . . . C2 C 0.84898(16) -0.00704(15) 0.21089(5) 0.0194(3) Uani 1 1 d . . . H2A H 0.7737 -0.0374 0.2341 0.023 Uiso 1 1 calc R . . H2B H 0.9517 -0.0886 0.2099 0.023 Uiso 1 1 calc R . . O3 O 0.40967(13) 0.42955(12) 0.25473(4) 0.0310(3) Uani 1 1 d . . . C3 C 0.95830(16) 0.19385(16) 0.19510(5) 0.0201(3) Uani 1 1 d . . . H3A H 0.9587 0.2843 0.2105 0.024 Uiso 1 1 calc R . . H3B H 0.9078 0.2262 0.1649 0.024 Uiso 1 1 calc R . . O4 O 0.70285(14) 0.42988(12) 0.25424(5) 0.0315(3) Uani 1 1 d . . . C4 C 0.2758(2) 0.5586(2) 0.25860(9) 0.0498(5) Uani 1 1 d . . . H4 H 0.2772 0.6188 0.2871 0.060 Uiso 1 1 calc R . . C5 C 0.2798(4) 0.6506(3) 0.21112(13) 0.0813(9) Uani 1 1 d . . . H5A H 0.3802 0.6634 0.2041 0.122 Uiso 1 1 calc R . . H5B H 0.1961 0.7486 0.2155 0.122 Uiso 1 1 calc R . . H5C H 0.2658 0.5985 0.1835 0.122 Uiso 1 1 calc R . . C6 C 0.1359(3) 0.5169(5) 0.26904(16) 0.1023(13) Uani 1 1 d . . . H6A H 0.1296 0.4624 0.2407 0.153 Uiso 1 1 calc R . . H6B H 0.0426 0.6074 0.2747 0.153 Uiso 1 1 calc R . . H6C H 0.1434 0.4536 0.2986 0.153 Uiso 1 1 calc R . . C7 C 0.6579(4) 0.5836(3) 0.26243(19) 0.0442(10) Uani 0.628(7) 1 d P A 2 H7 H 0.5429 0.6338 0.2634 0.053 Uiso 0.628(7) 1 calc PR A 2 C8 C 0.7436(6) 0.6435(5) 0.2185(3) 0.0702(17) Uani 0.628(7) 1 d P A 2 H8A H 0.8559 0.5892 0.2167 0.105 Uiso 0.628(7) 1 calc PR A 2 H8B H 0.7203 0.7500 0.2233 0.105 Uiso 0.628(7) 1 calc PR A 2 H8C H 0.7090 0.6293 0.1876 0.105 Uiso 0.628(7) 1 calc PR A 2 C9 C 0.7054(7) 0.6009(6) 0.3114(2) 0.087(2) Uani 0.628(7) 1 d P A 2 H9A H 0.6490 0.5602 0.3379 0.131 Uiso 0.628(7) 1 calc PR A 2 H9B H 0.6806 0.7068 0.3177 0.131 Uiso 0.628(7) 1 calc PR A 2 H9C H 0.8174 0.5468 0.3106 0.131 Uiso 0.628(7) 1 calc PR A 2 C11 C 0.84264(17) 0.02116(16) 0.31728(5) 0.0207(3) Uani 1 1 d . . . C12 C 0.68070(17) 0.06989(16) 0.32710(5) 0.0210(3) Uani 1 1 d . . . C13 C 0.60719(17) 0.00733(17) 0.36629(5) 0.0227(3) Uani 1 1 d . . . C14 C 0.70339(19) -0.10163(17) 0.39487(6) 0.0257(3) Uani 1 1 d . . . H14 H 0.6559 -0.1440 0.4217 0.031 Uiso 1 1 calc R . . C15 C 0.86606(19) -0.15233(17) 0.38631(6) 0.0264(3) Uani 1 1 d . . . C16 C 0.93337(18) -0.09001(17) 0.34674(5) 0.0237(3) Uani 1 1 d . . . H16 H 1.0434 -0.1236 0.3395 0.028 Uiso 1 1 calc R . . C17 C 0.42831(18) 0.06045(19) 0.37768(6) 0.0276(3) Uani 1 1 d . . . C18 C 0.9623(2) -0.2702(2) 0.42082(7) 0.0375(4) Uani 1 1 d . . . C21 C 0.80038(16) 0.01120(15) 0.15996(5) 0.0184(3) Uani 1 1 d . . . C22 C 0.68287(16) 0.14170(15) 0.14671(5) 0.0186(3) Uani 1 1 d . . . C23 C 0.64308(16) 0.15979(16) 0.09835(5) 0.0194(3) Uani 1 1 d . . . C24 C 0.72110(17) 0.04117(16) 0.06539(5) 0.0217(3) Uani 1 1 d . . . H24 H 0.6956 0.0519 0.0326 0.026 Uiso 1 1 calc R . . C25 C 0.83441(17) -0.09211(16) 0.07804(5) 0.0212(3) Uani 1 1 d . . . C26 C 0.87252(16) -0.10380(15) 0.12584(5) 0.0200(3) Uani 1 1 d . . . H26 H 0.9499 -0.1928 0.1354 0.024 Uiso 1 1 calc R . . C27 C 0.51777(17) 0.30429(17) 0.08282(6) 0.0235(3) Uani 1 1 d . . . C28 C 0.91365(19) -0.22349(17) 0.04203(6) 0.0264(3) Uani 1 1 d . . . C31 C 1.12578(16) 0.09354(16) 0.17944(5) 0.0208(3) Uani 1 1 d . . . C32 C 1.16941(18) 0.01351(18) 0.13519(6) 0.0267(3) Uani 1 1 d . . . H32 H 1.0924 0.0180 0.1154 0.032 Uiso 1 1 calc R . . C33 C 1.3243(2) -0.0728(2) 0.11975(6) 0.0335(4) Uani 1 1 d . . . H33 H 1.3522 -0.1272 0.0897 0.040 Uiso 1 1 calc R . . C34 C 1.43783(19) -0.0796(2) 0.14816(7) 0.0343(4) Uani 1 1 d . . . H34 H 1.5436 -0.1385 0.1376 0.041 Uiso 1 1 calc R . . C35 C 1.39685(18) -0.0004(2) 0.19186(6) 0.0308(3) Uani 1 1 d . . . H35 H 1.4745 -0.0051 0.2115 0.037 Uiso 1 1 calc R . . C36 C 1.24213(18) 0.08626(18) 0.20727(6) 0.0249(3) Uani 1 1 d . . . H36 H 1.2153 0.1413 0.2372 0.030 Uiso 1 1 calc R . . C37 C 0.3610(2) 0.0338(3) 0.33253(7) 0.0412(4) Uani 1 1 d . . . H37A H 0.4019 -0.0731 0.3250 0.062 Uiso 1 1 calc R . . H37B H 0.3908 0.0883 0.3039 0.062 Uiso 1 1 calc R . . H37C H 0.2474 0.0692 0.3399 0.062 Uiso 1 1 calc R . . C38 C 0.3603(2) 0.2269(2) 0.39080(7) 0.0392(4) Uani 1 1 d . . . H38A H 0.2468 0.2597 0.3978 0.059 Uiso 1 1 calc R . . H38B H 0.3891 0.2842 0.3629 0.059 Uiso 1 1 calc R . . H38C H 0.4016 0.2429 0.4201 0.059 Uiso 1 1 calc R . . C39 C 0.3764(2) -0.0249(2) 0.42139(7) 0.0402(4) Uani 1 1 d . . . H39A H 0.4156 -0.0084 0.4511 0.060 Uiso 1 1 calc R . . H39B H 0.4179 -0.1317 0.4138 0.060 Uiso 1 1 calc R . . H39C H 0.2627 0.0108 0.4273 0.060 Uiso 1 1 calc R . . C40 C 0.9190(4) -0.2111(4) 0.47348(8) 0.0807(10) Uani 1 1 d . . . H40A H 0.9802 -0.2861 0.4955 0.121 Uiso 1 1 calc R . . H40B H 0.8081 -0.1895 0.4842 0.121 Uiso 1 1 calc R . . H40C H 0.9410 -0.1195 0.4748 0.121 Uiso 1 1 calc R . . C41 C 0.9284(3) -0.4144(3) 0.41851(12) 0.0667(7) Uani 1 1 d . . . H41A H 0.9890 -0.4894 0.4406 0.100 Uiso 1 1 calc R . . H41B H 0.9571 -0.4524 0.3845 0.100 Uiso 1 1 calc R . . H41C H 0.8173 -0.3931 0.4289 0.100 Uiso 1 1 calc R . . C42 C 1.1369(2) -0.3126(3) 0.40574(8) 0.0481(5) Uani 1 1 d . . . H42A H 1.1643 -0.2242 0.4071 0.072 Uiso 1 1 calc R . . H42B H 1.1658 -0.3522 0.3719 0.072 Uiso 1 1 calc R . . H42C H 1.1927 -0.3888 0.4285 0.072 Uiso 1 1 calc R . . C43 C 0.4952(2) 0.3003(2) 0.02856(6) 0.0329(4) Uani 1 1 d . . . H43A H 0.5928 0.2891 0.0072 0.049 Uiso 1 1 calc R . . H43B H 0.4138 0.3934 0.0203 0.049 Uiso 1 1 calc R . . H43C H 0.4645 0.2158 0.0235 0.049 Uiso 1 1 calc R . . C44 C 0.5665(2) 0.43820(18) 0.08885(6) 0.0309(3) Uani 1 1 d . . . H44A H 0.5762 0.4472 0.1237 0.046 Uiso 1 1 calc R . . H44B H 0.4876 0.5297 0.0783 0.046 Uiso 1 1 calc R . . H44C H 0.6666 0.4228 0.0684 0.046 Uiso 1 1 calc R . . C45 C 0.36063(18) 0.32609(19) 0.11452(7) 0.0312(4) Uani 1 1 d . . . H45A H 0.3299 0.2415 0.1096 0.047 Uiso 1 1 calc R . . H45B H 0.2817 0.4185 0.1046 0.047 Uiso 1 1 calc R . . H45C H 0.3701 0.3321 0.1495 0.047 Uiso 1 1 calc R . . C46 C 0.8509(3) -0.3468(2) 0.05858(9) 0.0571(6) Uani 1 1 d . . . H46A H 0.8981 -0.4303 0.0353 0.086 Uiso 1 1 calc R . . H46B H 0.7378 -0.3079 0.0593 0.086 Uiso 1 1 calc R . . H46C H 0.8767 -0.3813 0.0917 0.086 Uiso 1 1 calc R . . C47 C 1.0901(2) -0.2805(2) 0.04144(8) 0.0451(5) Uani 1 1 d . . . H47A H 1.1151 -0.3128 0.0748 0.068 Uiso 1 1 calc R . . H47B H 1.1284 -0.2003 0.0305 0.068 Uiso 1 1 calc R . . H47C H 1.1396 -0.3649 0.0186 0.068 Uiso 1 1 calc R . . C48 C 0.8835(3) -0.1796(2) -0.01129(7) 0.0457(5) Uani 1 1 d . . . H48A H 0.9201 -0.0981 -0.0220 0.069 Uiso 1 1 calc R . . H48B H 0.7718 -0.1468 -0.0130 0.069 Uiso 1 1 calc R . . H48C H 0.9393 -0.2658 -0.0330 0.069 Uiso 1 1 calc R . . C51 C 0.7675(5) 0.2611(4) 0.42753(13) 0.0998(12) Uani 1 1 d . . . H51A H 0.7149 0.2989 0.3984 0.150 Uiso 1 1 calc R . . H51B H 0.8137 0.1520 0.4262 0.150 Uiso 1 1 calc R . . H51C H 0.8494 0.3016 0.4280 0.150 Uiso 1 1 calc R . . C52 C 0.6513(5) 0.3085(4) 0.47379(12) 0.0857(10) Uani 1 1 d . . . H52A H 0.5775 0.2559 0.4750 0.103 Uiso 1 1 calc R . . H52B H 0.7073 0.2759 0.5029 0.103 Uiso 1 1 calc R . . C53 C 0.5599(4) 0.4733(4) 0.47802(10) 0.0781(9) Uani 1 1 d . . . H53A H 0.6344 0.5246 0.4776 0.094 Uiso 1 1 calc R . . H53B H 0.5079 0.5055 0.4481 0.094 Uiso 1 1 calc R . . C7' C 0.7083(9) 0.5477(7) 0.2843(3) 0.0418(17) Uani 0.372(7) 1 d P A 1 H7' H 0.8127 0.5077 0.2959 0.050 Uiso 0.372(7) 1 calc PR A 1 C9' C 0.5917(9) 0.5779(7) 0.3306(2) 0.056(2) Uani 0.372(7) 1 d P A 1 H9'1 H 0.6068 0.6502 0.3512 0.084 Uiso 0.372(7) 1 calc PR A 1 H9'2 H 0.6062 0.4848 0.3491 0.084 Uiso 0.372(7) 1 calc PR A 1 H9'3 H 0.4864 0.6185 0.3216 0.084 Uiso 0.372(7) 1 calc PR A 1 C8' C 0.7055(9) 0.6791(7) 0.2542(3) 0.0533(19) Uani 0.372(7) 1 d P A 1 H8'1 H 0.7939 0.6508 0.2277 0.080 Uiso 0.372(7) 1 calc PR A 1 H8'2 H 0.7124 0.7553 0.2751 0.080 Uiso 0.372(7) 1 calc PR A 1 H8'3 H 0.6084 0.7192 0.2398 0.080 Uiso 0.372(7) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01913(14) 0.01614(13) 0.01933(14) 0.00061(9) -0.00076(10) -0.00287(10) O1 0.0207(5) 0.0275(5) 0.0230(5) 0.0068(4) -0.0008(4) -0.0040(4) N1 0.0180(5) 0.0184(5) 0.0164(5) 0.0019(4) -0.0021(4) -0.0071(4) C1 0.0207(7) 0.0253(7) 0.0180(7) 0.0029(5) -0.0047(5) -0.0087(6) O2 0.0214(5) 0.0203(5) 0.0208(5) -0.0009(4) -0.0035(4) -0.0008(4) C2 0.0193(6) 0.0153(6) 0.0211(7) 0.0018(5) -0.0040(5) -0.0034(5) O3 0.0261(6) 0.0249(6) 0.0310(6) 0.0007(5) -0.0002(5) 0.0022(5) C3 0.0183(6) 0.0216(7) 0.0205(7) 0.0042(5) -0.0024(5) -0.0081(5) O4 0.0355(6) 0.0220(5) 0.0374(6) -0.0053(5) -0.0007(5) -0.0117(5) C4 0.0258(9) 0.0424(11) 0.0681(14) -0.0185(10) -0.0048(9) 0.0048(8) C5 0.082(2) 0.0383(13) 0.107(2) 0.0199(14) -0.0370(18) 0.0039(13) C6 0.0315(13) 0.119(3) 0.149(3) -0.034(3) 0.0104(16) -0.0228(15) C7 0.0400(18) 0.0149(14) 0.081(3) -0.0047(15) -0.0296(19) -0.0045(12) C8 0.064(3) 0.047(2) 0.112(5) 0.035(3) -0.031(3) -0.032(2) C9 0.080(4) 0.086(3) 0.097(4) -0.062(3) -0.005(3) -0.025(3) C11 0.0228(7) 0.0220(7) 0.0165(6) 0.0009(5) -0.0019(5) -0.0078(6) C12 0.0235(7) 0.0209(7) 0.0168(6) 0.0007(5) -0.0026(5) -0.0063(6) C13 0.0251(7) 0.0248(7) 0.0184(7) -0.0014(5) -0.0005(6) -0.0101(6) C14 0.0319(8) 0.0261(7) 0.0189(7) 0.0034(6) -0.0004(6) -0.0120(6) C15 0.0309(8) 0.0253(7) 0.0211(7) 0.0047(6) -0.0049(6) -0.0081(6) C16 0.0233(7) 0.0242(7) 0.0217(7) 0.0018(6) -0.0041(6) -0.0063(6) C17 0.0246(7) 0.0351(8) 0.0229(7) 0.0005(6) 0.0013(6) -0.0123(6) C18 0.0355(9) 0.0387(9) 0.0308(9) 0.0169(7) -0.0064(7) -0.0065(8) C21 0.0162(6) 0.0184(6) 0.0203(7) 0.0018(5) -0.0022(5) -0.0065(5) C22 0.0160(6) 0.0181(6) 0.0204(7) -0.0002(5) -0.0007(5) -0.0053(5) C23 0.0160(6) 0.0202(7) 0.0219(7) 0.0040(5) -0.0030(5) -0.0070(5) C24 0.0220(7) 0.0258(7) 0.0193(7) 0.0015(5) -0.0036(5) -0.0111(6) C25 0.0205(7) 0.0218(7) 0.0228(7) -0.0022(5) -0.0003(5) -0.0099(6) C26 0.0178(6) 0.0171(6) 0.0243(7) 0.0008(5) -0.0024(5) -0.0057(5) C27 0.0219(7) 0.0225(7) 0.0242(7) 0.0053(6) -0.0060(6) -0.0053(6) C28 0.0295(8) 0.0235(7) 0.0253(8) -0.0055(6) 0.0004(6) -0.0094(6) C31 0.0192(7) 0.0230(7) 0.0205(7) 0.0043(5) -0.0015(5) -0.0092(5) C32 0.0252(8) 0.0345(8) 0.0225(7) 0.0001(6) -0.0004(6) -0.0145(6) C33 0.0308(8) 0.0371(9) 0.0299(8) -0.0063(7) 0.0071(7) -0.0124(7) C34 0.0205(7) 0.0352(9) 0.0398(10) 0.0033(7) 0.0044(7) -0.0053(7) C35 0.0207(7) 0.0385(9) 0.0331(9) 0.0089(7) -0.0059(6) -0.0110(7) C36 0.0230(7) 0.0311(8) 0.0221(7) 0.0037(6) -0.0026(6) -0.0123(6) C37 0.0341(9) 0.0647(13) 0.0313(9) -0.0001(9) -0.0055(7) -0.0250(9) C38 0.0299(9) 0.0379(10) 0.0404(10) -0.0039(8) 0.0072(7) -0.0054(7) C39 0.0333(9) 0.0515(11) 0.0350(9) 0.0075(8) 0.0045(7) -0.0190(8) C40 0.0834(19) 0.090(2) 0.0267(11) 0.0103(11) -0.0132(11) 0.0177(16) C41 0.0521(13) 0.0418(12) 0.102(2) 0.0361(13) -0.0177(13) -0.0143(10) C42 0.0394(10) 0.0541(12) 0.0446(11) 0.0234(10) -0.0156(9) -0.0095(9) C43 0.0316(8) 0.0355(9) 0.0288(8) 0.0079(7) -0.0126(7) -0.0068(7) C44 0.0351(9) 0.0231(7) 0.0338(9) 0.0073(6) -0.0072(7) -0.0098(7) C45 0.0192(7) 0.0312(8) 0.0361(9) 0.0089(7) -0.0045(6) -0.0020(6) C46 0.0844(17) 0.0409(11) 0.0533(13) -0.0217(10) 0.0209(12) -0.0397(12) C47 0.0324(9) 0.0461(11) 0.0446(11) -0.0199(9) -0.0013(8) 0.0014(8) C48 0.0574(12) 0.0415(10) 0.0288(9) -0.0112(8) -0.0055(8) -0.0054(9) C51 0.141(3) 0.098(3) 0.085(2) -0.027(2) -0.005(2) -0.074(3) C52 0.126(3) 0.098(2) 0.0679(18) 0.0139(17) -0.0360(19) -0.075(2) C53 0.108(3) 0.097(2) 0.0588(16) 0.0115(15) -0.0172(15) -0.071(2) C7' 0.042(3) 0.028(3) 0.058(4) -0.011(3) -0.004(3) -0.015(3) C9' 0.078(5) 0.052(4) 0.041(3) -0.023(3) 0.000(3) -0.027(3) C8' 0.062(4) 0.032(3) 0.070(5) 0.004(3) -0.006(4) -0.023(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 Ti1 O3 1.7812(11) . ? Ti1 O4 1.7999(12) . ? Ti1 O1 1.8497(11) . ? Ti1 O2 1.8602(10) . ? Ti1 N1 2.3301(12) . ? O1 C12 1.3533(17) . ? N1 C2 1.4876(17) . ? N1 C1 1.4904(17) . ? N1 C3 1.5049(18) . ? C1 C11 1.511(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C22 1.3487(16) . ? C2 C21 1.5078(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C4 1.399(2) . ? C3 C31 1.5169(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C7 1.405(3) . ? O4 C7' 1.459(6) . ? C4 C6 1.487(4) . ? C4 C5 1.532(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.506(7) . ? C7 C8 1.547(7) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.397(2) . ? C11 C16 1.397(2) . ? C12 C13 1.412(2) . ? C13 C14 1.394(2) . ? C13 C17 1.544(2) . ? C14 C15 1.401(2) . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 C18 1.538(2) . ? C16 H16 0.9500 . ? C17 C39 1.531(2) . ? C17 C38 1.534(2) . ? C17 C37 1.538(2) . ? C18 C40 1.519(3) . ? C18 C42 1.525(3) . ? C18 C41 1.541(3) . ? C21 C26 1.3901(19) . ? C21 C22 1.4035(19) . ? C22 C23 1.409(2) . ? C23 C24 1.399(2) . ? C23 C27 1.5404(19) . ? C24 C25 1.396(2) . ? C24 H24 0.9500 . ? C25 C26 1.391(2) . ? C25 C28 1.534(2) . ? C26 H26 0.9500 . ? C27 C43 1.532(2) . ? C27 C45 1.538(2) . ? C27 C44 1.542(2) . ? C28 C46 1.527(3) . ? C28 C48 1.531(2) . ? C28 C47 1.531(2) . ? C31 C36 1.395(2) . ? C31 C32 1.396(2) . ? C32 C33 1.392(2) . ? C32 H32 0.9500 . ? C33 C34 1.385(3) . ? C33 H33 0.9500 . ? C34 C35 1.380(3) . ? C34 H34 0.9500 . ? C35 C36 1.391(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C51 C52 1.509(5) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.503(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C53 1.485(6) 2_666 ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C7' C8' 1.465(9) . ? C7' C9' 1.506(9) . ? C7' H7' 1.0000 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 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 O3 Ti1 O4 99.70(6) . . ? O3 Ti1 O1 97.72(5) . . ? O4 Ti1 O1 114.76(5) . . ? O3 Ti1 O2 96.94(5) . . ? O4 Ti1 O2 118.24(5) . . ? O1 Ti1 O2 121.15(5) . . ? O3 Ti1 N1 176.28(5) . . ? O4 Ti1 N1 83.76(5) . . ? O1 Ti1 N1 81.97(4) . . ? O2 Ti1 N1 80.13(4) . . ? C12 O1 Ti1 143.66(10) . . ? C2 N1 C1 109.66(11) . . ? C2 N1 C3 112.69(11) . . ? C1 N1 C3 108.91(11) . . ? C2 N1 Ti1 107.26(8) . . ? C1 N1 Ti1 108.44(8) . . ? C3 N1 Ti1 109.79(8) . . ? N1 C1 C11 115.86(12) . . ? N1 C1 H1A 108.3 . . ? C11 C1 H1A 108.3 . . ? N1 C1 H1B 108.3 . . ? C11 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? C22 O2 Ti1 143.42(9) . . ? N1 C2 C21 114.24(11) . . ? N1 C2 H2A 108.7 . . ? C21 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C21 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 O3 Ti1 163.28(13) . . ? N1 C3 C31 117.26(11) . . ? N1 C3 H3A 108.0 . . ? C31 C3 H3A 108.0 . . ? N1 C3 H3B 108.0 . . ? C31 C3 H3B 108.0 . . ? H3A C3 H3B 107.2 . . ? C7 O4 C7' 32.4(3) . . ? C7 O4 Ti1 136.27(18) . . ? C7' O4 Ti1 147.1(3) . . ? O3 C4 C6 109.5(2) . . ? O3 C4 C5 108.62(18) . . ? C6 C4 C5 113.5(3) . . ? O3 C4 H4 108.3 . . ? C6 C4 H4 108.4 . . ? C5 C4 H4 108.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C9 107.1(4) . . ? O4 C7 C8 106.2(3) . . ? C9 C7 C8 112.7(4) . . ? O4 C7 H7 110.2 . . ? C9 C7 H7 110.2 . . ? C8 C7 H7 110.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 C16 119.78(13) . . ? C12 C11 C1 121.76(13) . . ? C16 C11 C1 118.24(13) . . ? O1 C12 C11 118.97(13) . . ? O1 C12 C13 120.22(13) . . ? C11 C12 C13 120.81(13) . . ? C14 C13 C12 116.93(14) . . ? C14 C13 C17 121.69(14) . . ? C12 C13 C17 121.37(13) . . ? C13 C14 C15 123.78(14) . . ? C13 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C16 C15 C14 117.32(14) . . ? C16 C15 C18 122.74(15) . . ? C14 C15 C18 119.92(14) . . ? C15 C16 C11 121.37(14) . . ? C15 C16 H16 119.3 . . ? C11 C16 H16 119.3 . . ? C39 C17 C38 107.96(14) . . ? C39 C17 C37 107.37(15) . . ? C38 C17 C37 109.79(15) . . ? C39 C17 C13 111.70(14) . . ? C38 C17 C13 109.99(13) . . ? C37 C17 C13 109.97(13) . . ? C40 C18 C42 109.0(2) . . ? C40 C18 C15 109.40(16) . . ? C42 C18 C15 112.69(15) . . ? C40 C18 C41 109.8(2) . . ? C42 C18 C41 106.51(18) . . ? C15 C18 C41 109.35(17) . . ? C26 C21 C22 119.69(13) . . ? C26 C21 C2 119.28(12) . . ? C22 C21 C2 121.02(12) . . ? O2 C22 C21 118.89(12) . . ? O2 C22 C23 120.70(12) . . ? C21 C22 C23 120.41(13) . . ? C24 C23 C22 117.31(13) . . ? C24 C23 C27 121.68(13) . . ? C22 C23 C27 121.01(13) . . ? C25 C24 C23 123.55(13) . . ? C25 C24 H24 118.2 . . ? C23 C24 H24 118.2 . . ? C26 C25 C24 117.18(13) . . ? C26 C25 C28 120.06(13) . . ? C24 C25 C28 122.75(13) . . ? C21 C26 C25 121.79(13) . . ? C21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C43 C27 C45 107.31(13) . . ? C43 C27 C23 112.05(13) . . ? C45 C27 C23 109.92(12) . . ? C43 C27 C44 107.48(13) . . ? C45 C27 C44 110.41(13) . . ? C23 C27 C44 109.64(12) . . ? C46 C28 C48 108.66(17) . . ? C46 C28 C47 110.55(17) . . ? C48 C28 C47 106.64(15) . . ? C46 C28 C25 108.55(13) . . ? C48 C28 C25 112.41(14) . . ? C47 C28 C25 110.03(13) . . ? C36 C31 C32 118.09(14) . . ? C36 C31 C3 120.82(13) . . ? C32 C31 C3 120.96(13) . . ? C33 C32 C31 120.84(15) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.14(15) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.78(15) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.15(15) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 120.99(15) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C17 C37 H37A 109.5 . . ? C17 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C17 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C17 C38 H38A 109.5 . . ? C17 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C17 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C17 C39 H39A 109.5 . . ? C17 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C17 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C18 C40 H40A 109.5 . . ? C18 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C18 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C18 C41 H41A 109.5 . . ? C18 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C18 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C18 C42 H42A 109.5 . . ? C18 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C18 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C27 C43 H43A 109.5 . . ? C27 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C27 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C27 C44 H44A 109.5 . . ? C27 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C27 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C27 C45 H45A 109.5 . . ? C27 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C27 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C28 C46 H46A 109.5 . . ? C28 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C28 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C28 C47 H47A 109.5 . . ? C28 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C28 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C28 C48 H48A 109.5 . . ? C28 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C28 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C51 115.0(3) . . ? C53 C52 H52A 108.5 . . ? C51 C52 H52A 108.5 . . ? C53 C52 H52B 108.5 . . ? C51 C52 H52B 108.5 . . ? H52A C52 H52B 107.5 . . ? C53 C53 C52 117.7(3) 2_666 . ? C53 C53 H53A 107.9 2_666 . ? C52 C53 H53A 107.9 . . ? C53 C53 H53B 107.9 2_666 . ? C52 C53 H53B 107.9 . . ? H53A C53 H53B 107.2 . . ? O4 C7' C8' 111.2(6) . . ? O4 C7' C9' 112.4(5) . . ? C8' C7' C9' 115.4(6) . . ? O4 C7' H7' 105.7 . . ? C8' C7' H7' 105.7 . . ? C9' C7' H7' 105.7 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.441 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.124 #===END data_Ti(1d)(OPr)2 _database_code_depnum_ccdc_archive 'CCDC 284367' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H67 N O4 Ti' _chemical_formula_sum 'C47 H67 N O4 Ti' _chemical_formula_weight 757.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1670(2) _cell_length_b 22.1960(3) _cell_length_c 18.0800(4) _cell_angle_alpha 90.0000 _cell_angle_beta 98.7180(10) _cell_angle_gamma 90.0000 _cell_volume 4429.58(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 742760 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 28.70 _exptl_crystal_description cubic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa CCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37110 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0775 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9971 _reflns_number_gt 7131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+2.9906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9971 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ti1 Ti 0.96470(3) 0.236739(16) 0.29559(2) 0.01943(10) Uani 1 1 d . A . O1 O 0.95574(12) 0.30991(6) 0.24600(8) 0.0256(3) Uani 1 1 d . . . O2 O 1.00046(12) 0.16883(6) 0.24515(8) 0.0240(3) Uani 1 1 d . . . O3 O 0.80664(12) 0.22281(6) 0.29100(8) 0.0272(3) Uani 1 1 d . . . O4 O 1.00922(13) 0.23218(7) 0.39612(8) 0.0272(3) Uani 1 1 d . . . N1 N 1.17510(14) 0.25522(7) 0.29755(9) 0.0194(4) Uani 1 1 d . . . C1 C 1.19650(18) 0.28353(9) 0.22589(11) 0.0217(4) Uani 1 1 d . A . H1A H 1.1668 0.2556 0.1845 0.026 Uiso 1 1 calc R . . H1B H 1.2850 0.2880 0.2271 0.026 Uiso 1 1 calc R . . C2 C 1.23880(17) 0.19571(9) 0.30553(11) 0.0216(4) Uani 1 1 d . A . H2A H 1.2177 0.1750 0.3503 0.026 Uiso 1 1 calc R . . H2B H 1.3273 0.2029 0.3141 0.026 Uiso 1 1 calc R . . C3 C 1.21827(17) 0.29478(9) 0.36390(11) 0.0223(4) Uani 1 1 d . A . H3A H 1.2002 0.2739 0.4093 0.027 Uiso 1 1 calc R . . H3B H 1.1694 0.3322 0.3586 0.027 Uiso 1 1 calc R . . C4 C 0.6926(3) 0.19335(17) 0.2689(2) 0.0262(10) Uani 0.713(9) 1 d P A 1 H4 H 0.7003 0.1661 0.2258 0.031 Uiso 0.713(9) 1 calc PR A 1 C7 C 0.9623(2) 0.20465(13) 0.45651(13) 0.0399(6) Uani 1 1 d . A . H7 H 0.8718 0.2066 0.4466 0.048 Uiso 1 1 calc R . . C8 C 1.0066(3) 0.23890(18) 0.52693(15) 0.0723(10) Uani 1 1 d . . . H8A H 1.0945 0.2338 0.5398 0.108 Uiso 1 1 calc R A . H8B H 0.9667 0.2235 0.5678 0.108 Uiso 1 1 calc R . . H8C H 0.9876 0.2818 0.5191 0.108 Uiso 1 1 calc R . . C9 C 1.0015(3) 0.13882(14) 0.4603(2) 0.0699(10) Uani 1 1 d . . . H9A H 0.9684 0.1185 0.4135 0.105 Uiso 1 1 calc R A . H9B H 0.9711 0.1190 0.5022 0.105 Uiso 1 1 calc R . . H9C H 1.0901 0.1365 0.4676 0.105 Uiso 1 1 calc R . . C11 C 1.01729(17) 0.35419(9) 0.21648(11) 0.0217(4) Uani 1 1 d . A . C12 C 1.13819(18) 0.34391(9) 0.20839(11) 0.0208(4) Uani 1 1 d . . . C13 C 1.20158(18) 0.38842(9) 0.17617(11) 0.0231(4) Uani 1 1 d . A . H13 H 1.2837 0.3813 0.1708 0.028 Uiso 1 1 calc R . . C14 C 1.14852(19) 0.44279(9) 0.15166(11) 0.0242(5) Uani 1 1 d . . . C15 C 1.02796(19) 0.45135(9) 0.16035(11) 0.0247(5) Uani 1 1 d . A . H15 H 0.9902 0.4883 0.1437 0.030 Uiso 1 1 calc R . . C16 C 0.95944(18) 0.40861(9) 0.19222(11) 0.0227(4) Uani 1 1 d . . . C21 C 1.08716(17) 0.14266(9) 0.21116(11) 0.0197(4) Uani 1 1 d . A . C22 C 1.20819(17) 0.15477(9) 0.23865(11) 0.0197(4) Uani 1 1 d . . . C23 C 1.29903(18) 0.12692(9) 0.20598(11) 0.0226(4) Uani 1 1 d . A . H23 H 1.3814 0.1354 0.2247 0.027 Uiso 1 1 calc R . . C24 C 1.27185(17) 0.08702(9) 0.14657(11) 0.0214(4) Uani 1 1 d . . . C25 C 1.14889(17) 0.07730(9) 0.11957(11) 0.0219(4) Uani 1 1 d . A . H25 H 1.1288 0.0508 0.0783 0.026 Uiso 1 1 calc R . . C26 C 1.05458(17) 0.10424(9) 0.14981(11) 0.0193(4) Uani 1 1 d . . . C31 C 1.35121(18) 0.31275(9) 0.37747(11) 0.0218(4) Uani 1 1 d . . . C32 C 1.38456(19) 0.36505(10) 0.34520(12) 0.0261(5) Uani 1 1 d . A . H32 H 1.3247 0.3875 0.3139 0.031 Uiso 1 1 calc R . . C33 C 1.5046(2) 0.38630(10) 0.35719(12) 0.0304(5) Uani 1 1 d . . . H33 H 1.5254 0.4218 0.3327 0.037 Uiso 1 1 calc R A . C34 C 1.59102(19) 0.35588(10) 0.40392(12) 0.0304(5) Uani 1 1 d . A . H34 H 1.6721 0.3703 0.4117 0.036 Uiso 1 1 calc R . . C35 C 1.56151(19) 0.30322(10) 0.44093(11) 0.0264(5) Uani 1 1 d . . . C36 C 1.44057(18) 0.28029(9) 0.42738(11) 0.0222(4) Uani 1 1 d . A . C37 C 1.6507(2) 0.27263(11) 0.49136(12) 0.0323(5) Uani 1 1 d . A . H37 H 1.7308 0.2882 0.5008 0.039 Uiso 1 1 calc R . . C38 C 1.6237(2) 0.22141(11) 0.52645(12) 0.0355(6) Uani 1 1 d . . . H38 H 1.6852 0.2009 0.5590 0.043 Uiso 1 1 calc R A . C39 C 1.5044(2) 0.19860(11) 0.51455(12) 0.0341(5) Uani 1 1 d . A . H39 H 1.4855 0.1631 0.5398 0.041 Uiso 1 1 calc R . . C40 C 1.4159(2) 0.22731(10) 0.46683(11) 0.0276(5) Uani 1 1 d . . . H40 H 1.3359 0.2115 0.4598 0.033 Uiso 1 1 calc R A . C41 C 1.2234(2) 0.49007(10) 0.11621(12) 0.0307(5) Uani 1 1 d . A . C42 C 1.3358(2) 0.50686(11) 0.17199(15) 0.0419(6) Uani 1 1 d . . . H42A H 1.3107 0.5226 0.2179 0.063 Uiso 1 1 calc R A . H42B H 1.3823 0.5377 0.1499 0.063 Uiso 1 1 calc R . . H42C H 1.3862 0.4710 0.1839 0.063 Uiso 1 1 calc R . . C43 C 1.2626(3) 0.46272(13) 0.04554(15) 0.0507(7) Uani 1 1 d . . . H43A H 1.3122 0.4269 0.0592 0.076 Uiso 1 1 calc R A . H43B H 1.3099 0.4924 0.0221 0.076 Uiso 1 1 calc R . . H43C H 1.1906 0.4514 0.0102 0.076 Uiso 1 1 calc R . . C44 C 1.1513(2) 0.54762(11) 0.09392(15) 0.0417(6) Uani 1 1 d . . . H44A H 1.0799 0.5378 0.0574 0.062 Uiso 1 1 calc R A . H44B H 1.2024 0.5763 0.0717 0.062 Uiso 1 1 calc R . . H44C H 1.1255 0.5657 0.1384 0.062 Uiso 1 1 calc R . . C45 C 0.82461(19) 0.41878(10) 0.19708(12) 0.0279(5) Uani 1 1 d . A . C46 C 0.7818(2) 0.48175(11) 0.17059(14) 0.0368(6) Uani 1 1 d . . . H46A H 0.6958 0.4863 0.1748 0.055 Uiso 1 1 calc R A . H46B H 0.7931 0.4871 0.1183 0.055 Uiso 1 1 calc R . . H46C H 0.8292 0.5121 0.2017 0.055 Uiso 1 1 calc R . . C47 C 0.8011(2) 0.41168(12) 0.27818(14) 0.0396(6) Uani 1 1 d . . . H47A H 0.8526 0.4399 0.3105 0.059 Uiso 1 1 calc R A . H47B H 0.8200 0.3703 0.2950 0.059 Uiso 1 1 calc R . . H47C H 0.7158 0.4203 0.2808 0.059 Uiso 1 1 calc R . . C48 C 0.7496(2) 0.37265(11) 0.14600(15) 0.0429(6) Uani 1 1 d . . . H48A H 0.7756 0.3318 0.1615 0.064 Uiso 1 1 calc R A . H48B H 0.7618 0.3792 0.0941 0.064 Uiso 1 1 calc R . . H48C H 0.6636 0.3775 0.1499 0.064 Uiso 1 1 calc R . . C49 C 1.36886(17) 0.05294(10) 0.11168(12) 0.0246(5) Uani 1 1 d . A . C50 C 1.3534(2) -0.01511(10) 0.12351(13) 0.0314(5) Uani 1 1 d . . . H50A H 1.3635 -0.0238 0.1772 0.047 Uiso 1 1 calc R A . H50B H 1.4145 -0.0372 0.1008 0.047 Uiso 1 1 calc R . . H50C H 1.2723 -0.0276 0.1001 0.047 Uiso 1 1 calc R . . C51 C 1.3557(2) 0.06617(11) 0.02733(12) 0.0316(5) Uani 1 1 d . . . H51A H 1.2745 0.0544 0.0032 0.047 Uiso 1 1 calc R A . H51B H 1.4166 0.0432 0.0054 0.047 Uiso 1 1 calc R . . H51C H 1.3675 0.1093 0.0196 0.047 Uiso 1 1 calc R . . C52 C 1.49765(19) 0.07060(12) 0.14691(14) 0.0377(6) Uani 1 1 d . . . H52A H 1.5094 0.1139 0.1402 0.056 Uiso 1 1 calc R A . H52B H 1.5564 0.0481 0.1226 0.056 Uiso 1 1 calc R . . H52C H 1.5095 0.0611 0.2005 0.056 Uiso 1 1 calc R . . C53 C 0.92061(17) 0.09117(9) 0.12023(11) 0.0204(4) Uani 1 1 d . A . C54 C 0.85192(19) 0.15017(10) 0.09672(12) 0.0294(5) Uani 1 1 d . . . H54A H 0.8906 0.1706 0.0585 0.044 Uiso 1 1 calc R A . H54B H 0.8539 0.1765 0.1404 0.044 Uiso 1 1 calc R . . H54C H 0.7676 0.1408 0.0763 0.044 Uiso 1 1 calc R . . C55 C 0.86300(18) 0.05972(10) 0.18204(12) 0.0264(5) Uani 1 1 d . . . H55A H 0.7783 0.0500 0.1631 0.040 Uiso 1 1 calc R A . H55B H 0.8666 0.0866 0.2253 0.040 Uiso 1 1 calc R . . H55C H 0.9074 0.0225 0.1971 0.040 Uiso 1 1 calc R . . C56 C 0.90577(19) 0.05021(11) 0.05178(12) 0.0312(5) Uani 1 1 d . . . H56A H 0.9427 0.0693 0.0119 0.047 Uiso 1 1 calc R A . H56B H 0.8194 0.0434 0.0343 0.047 Uiso 1 1 calc R . . H56C H 0.9457 0.0115 0.0651 0.047 Uiso 1 1 calc R . . C4' C 0.6893(7) 0.2178(5) 0.3086(6) 0.031(3) Uani 0.287(9) 1 d P A 2 H4' H 0.6842 0.2451 0.3521 0.038 Uiso 0.287(9) 1 calc PR A 2 C5 C 0.5985(2) 0.24085(12) 0.24273(15) 0.0415(6) Uani 0.713(9) 1 d P A 1 H5A H 0.5904 0.2682 0.2842 0.062 Uiso 0.713(9) 1 calc PR A 1 H5B H 0.5204 0.2214 0.2257 0.062 Uiso 0.713(9) 1 calc PR A 1 H5C H 0.6237 0.2637 0.2014 0.062 Uiso 0.713(9) 1 calc PR A 1 C6 C 0.6614(2) 0.15593(12) 0.33190(14) 0.0408(6) Uani 0.713(9) 1 d P A 1 H6A H 0.7297 0.1294 0.3503 0.061 Uiso 0.713(9) 1 calc PR A 1 H6B H 0.5897 0.1315 0.3143 0.061 Uiso 0.713(9) 1 calc PR A 1 H6C H 0.6444 0.1823 0.3725 0.061 Uiso 0.713(9) 1 calc PR A 1 C5' C 0.5985(2) 0.24085(12) 0.24273(15) 0.0415(6) Uani 0.287(9) 1 d P A 2 H5'1 H 0.6184 0.2825 0.2314 0.062 Uiso 0.287(9) 1 calc PR A 2 H5'2 H 0.5165 0.2393 0.2558 0.062 Uiso 0.287(9) 1 calc PR A 2 H5'3 H 0.6024 0.2155 0.1988 0.062 Uiso 0.287(9) 1 calc PR A 2 C6' C 0.6614(2) 0.15593(12) 0.33190(14) 0.0408(6) Uani 0.287(9) 1 d P A 2 H6'1 H 0.6987 0.1266 0.3019 0.061 Uiso 0.287(9) 1 calc PR A 2 H6'2 H 0.5734 0.1500 0.3242 0.061 Uiso 0.287(9) 1 calc PR A 2 H6'3 H 0.6936 0.1503 0.3850 0.061 Uiso 0.287(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.01798(17) 0.01801(19) 0.0227(2) -0.00169(16) 0.00440(14) -0.00136(15) O1 0.0207(7) 0.0219(8) 0.0348(9) 0.0054(6) 0.0057(6) -0.0010(6) O2 0.0201(7) 0.0229(8) 0.0297(8) -0.0083(6) 0.0066(6) -0.0023(6) O3 0.0192(7) 0.0269(9) 0.0361(9) -0.0031(7) 0.0067(6) -0.0030(6) O4 0.0274(8) 0.0310(9) 0.0237(8) 0.0000(7) 0.0058(6) -0.0039(6) N1 0.0219(8) 0.0160(9) 0.0201(9) -0.0030(7) 0.0025(7) -0.0007(7) C1 0.0209(10) 0.0222(11) 0.0229(11) -0.0028(9) 0.0059(8) -0.0032(8) C2 0.0179(10) 0.0211(11) 0.0251(11) -0.0015(9) 0.0016(8) -0.0010(8) C3 0.0222(10) 0.0215(11) 0.0226(11) -0.0051(9) 0.0019(8) -0.0013(8) C4 0.0229(16) 0.026(2) 0.031(2) -0.0039(17) 0.0069(14) -0.0057(13) C7 0.0279(12) 0.0631(18) 0.0304(13) 0.0062(12) 0.0105(10) 0.0005(12) C8 0.0571(19) 0.132(3) 0.0278(15) -0.0116(18) 0.0064(13) 0.006(2) C9 0.066(2) 0.061(2) 0.085(2) 0.0368(18) 0.0155(18) -0.0019(17) C11 0.0231(10) 0.0198(11) 0.0217(11) -0.0012(8) 0.0018(8) -0.0045(8) C12 0.0240(10) 0.0192(11) 0.0192(10) -0.0036(8) 0.0027(8) -0.0018(8) C13 0.0237(10) 0.0236(12) 0.0225(11) -0.0037(9) 0.0049(8) -0.0045(9) C14 0.0313(11) 0.0209(11) 0.0208(11) -0.0020(9) 0.0051(9) -0.0042(9) C15 0.0303(11) 0.0190(11) 0.0244(11) -0.0002(9) 0.0026(9) 0.0003(9) C16 0.0234(10) 0.0222(11) 0.0223(11) -0.0019(9) 0.0024(8) -0.0011(8) C21 0.0181(9) 0.0182(11) 0.0234(10) -0.0007(8) 0.0047(8) 0.0005(8) C22 0.0215(10) 0.0157(10) 0.0213(10) -0.0014(8) 0.0009(8) -0.0015(8) C23 0.0182(10) 0.0221(11) 0.0266(11) -0.0001(9) 0.0003(8) -0.0021(8) C24 0.0173(10) 0.0211(11) 0.0256(11) -0.0016(9) 0.0030(8) 0.0007(8) C25 0.0232(10) 0.0206(11) 0.0215(10) -0.0047(9) 0.0022(8) -0.0010(8) C26 0.0183(10) 0.0179(11) 0.0214(10) 0.0013(8) 0.0015(8) -0.0023(8) C31 0.0233(10) 0.0211(11) 0.0212(11) -0.0071(9) 0.0036(8) -0.0028(8) C32 0.0291(11) 0.0221(12) 0.0259(12) -0.0031(9) 0.0005(9) -0.0015(9) C33 0.0335(12) 0.0266(12) 0.0312(12) -0.0007(10) 0.0050(10) -0.0101(10) C34 0.0245(11) 0.0360(14) 0.0302(12) -0.0053(10) 0.0026(9) -0.0096(10) C35 0.0262(11) 0.0309(13) 0.0218(11) -0.0069(9) 0.0020(8) -0.0019(9) C36 0.0253(10) 0.0221(11) 0.0192(10) -0.0062(8) 0.0029(8) -0.0014(8) C37 0.0268(11) 0.0402(15) 0.0281(12) -0.0050(11) -0.0017(9) -0.0006(10) C38 0.0376(13) 0.0430(15) 0.0236(12) -0.0026(11) -0.0031(10) 0.0072(11) C39 0.0481(14) 0.0292(13) 0.0240(12) 0.0019(10) 0.0023(10) 0.0010(11) C40 0.0316(12) 0.0275(13) 0.0233(11) -0.0042(9) 0.0032(9) -0.0043(9) C41 0.0363(13) 0.0256(12) 0.0320(12) 0.0033(10) 0.0114(10) -0.0039(10) C42 0.0381(14) 0.0327(14) 0.0553(16) 0.0054(12) 0.0087(12) -0.0112(11) C43 0.073(2) 0.0445(17) 0.0424(15) 0.0039(13) 0.0324(14) -0.0076(14) C44 0.0460(15) 0.0306(14) 0.0499(16) 0.0126(12) 0.0120(12) -0.0057(11) C45 0.0235(11) 0.0260(12) 0.0340(12) 0.0042(10) 0.0034(9) 0.0024(9) C46 0.0304(12) 0.0341(14) 0.0465(15) 0.0100(11) 0.0075(10) 0.0085(10) C47 0.0364(13) 0.0387(15) 0.0480(15) 0.0109(12) 0.0199(11) 0.0122(11) C48 0.0260(12) 0.0377(15) 0.0618(17) -0.0016(13) -0.0038(11) -0.0027(11) C49 0.0177(10) 0.0264(12) 0.0293(12) -0.0062(9) 0.0018(8) 0.0018(8) C50 0.0307(12) 0.0281(13) 0.0344(13) -0.0029(10) 0.0022(10) 0.0080(10) C51 0.0280(12) 0.0357(14) 0.0329(12) -0.0010(10) 0.0107(9) 0.0041(10) C52 0.0200(11) 0.0443(15) 0.0480(15) -0.0173(12) 0.0031(10) 0.0038(10) C53 0.0164(9) 0.0205(11) 0.0235(11) -0.0038(9) 0.0008(8) -0.0011(8) C54 0.0243(11) 0.0331(13) 0.0302(12) 0.0025(10) 0.0019(9) 0.0049(9) C55 0.0223(11) 0.0237(12) 0.0343(12) -0.0011(9) 0.0075(9) -0.0046(9) C56 0.0216(11) 0.0386(14) 0.0325(13) -0.0122(10) 0.0008(9) -0.0031(10) C4' 0.022(4) 0.039(6) 0.036(6) -0.005(5) 0.015(4) -0.001(4) C5 0.0242(12) 0.0444(16) 0.0543(16) 0.0061(13) 0.0005(11) -0.0042(11) C6 0.0340(13) 0.0399(15) 0.0481(16) 0.0048(12) 0.0049(11) -0.0122(11) C5' 0.0242(12) 0.0444(16) 0.0543(16) 0.0061(13) 0.0005(11) -0.0042(11) C6' 0.0340(13) 0.0399(15) 0.0481(16) 0.0048(12) 0.0049(11) -0.0122(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.7815(14) . ? Ti1 O4 1.8129(14) . ? Ti1 O2 1.8368(14) . ? Ti1 O1 1.8505(14) . ? Ti1 N1 2.3801(16) . ? O1 C11 1.355(2) . ? O2 C21 1.354(2) . ? O3 C4' 1.399(8) . ? O3 C4 1.434(3) . ? O4 C7 1.419(3) . ? N1 C1 1.491(2) . ? N1 C2 1.497(2) . ? N1 C3 1.506(2) . ? C1 C12 1.503(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C22 1.510(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C31 1.521(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C6 1.493(4) . ? C4 C5 1.513(4) . ? C4 H4 1.0000 . ? C7 C8 1.501(4) . ? C7 C9 1.524(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.399(3) . ? C11 C16 1.408(3) . ? C12 C13 1.393(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 C41 1.540(3) . ? C15 C16 1.397(3) . ? C15 H15 0.9500 . ? C16 C45 1.538(3) . ? C21 C22 1.394(3) . ? C21 C26 1.403(3) . ? C22 C23 1.393(3) . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 C25 1.403(3) . ? C24 C49 1.533(3) . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C26 C53 1.538(3) . ? C31 C32 1.375(3) . ? C31 C36 1.434(3) . ? C32 C33 1.407(3) . ? C32 H32 0.9500 . ? C33 C34 1.361(3) . ? C33 H33 0.9500 . ? C34 C35 1.410(3) . ? C34 H34 0.9500 . ? C35 C37 1.418(3) . ? C35 C36 1.429(3) . ? C36 C40 1.424(3) . ? C37 C38 1.358(3) . ? C37 H37 0.9500 . ? C38 C39 1.411(3) . ? C38 H38 0.9500 . ? C39 C40 1.367(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C44 1.531(3) . ? C41 C42 1.532(3) . ? C41 C43 1.537(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.530(3) . ? C45 C47 1.536(3) . ? C45 C48 1.539(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C52 1.533(3) . ? C49 C51 1.538(3) . ? C49 C50 1.539(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C56 1.524(3) . ? C53 C55 1.539(3) . ? C53 C54 1.544(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C4' H4' 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 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 O3 Ti1 O4 98.99(6) . . ? O3 Ti1 O2 97.06(6) . . ? O4 Ti1 O2 113.87(7) . . ? O3 Ti1 O1 98.59(6) . . ? O4 Ti1 O1 121.42(7) . . ? O2 Ti1 O1 118.66(6) . . ? O3 Ti1 N1 178.20(6) . . ? O4 Ti1 N1 82.80(6) . . ? O2 Ti1 N1 81.98(6) . . ? O1 Ti1 N1 80.60(6) . . ? C11 O1 Ti1 146.56(13) . . ? C21 O2 Ti1 143.29(13) . . ? C4' O3 C4 37.3(4) . . ? C4' O3 Ti1 163.5(5) . . ? C4 O3 Ti1 157.5(2) . . ? C7 O4 Ti1 135.90(14) . . ? C1 N1 C2 108.61(15) . . ? C1 N1 C3 111.86(15) . . ? C2 N1 C3 110.35(15) . . ? C1 N1 Ti1 110.33(11) . . ? C2 N1 Ti1 107.64(11) . . ? C3 N1 Ti1 107.97(11) . . ? N1 C1 C12 115.93(16) . . ? N1 C1 H1A 108.3 . . ? C12 C1 H1A 108.3 . . ? N1 C1 H1B 108.3 . . ? C12 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? N1 C2 C22 114.04(16) . . ? N1 C2 H2A 108.7 . . ? C22 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C22 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N1 C3 C31 117.92(16) . . ? N1 C3 H3A 107.8 . . ? C31 C3 H3A 107.8 . . ? N1 C3 H3B 107.8 . . ? C31 C3 H3B 107.8 . . ? H3A C3 H3B 107.2 . . ? O3 C4 C6 109.9(3) . . ? O3 C4 C5 108.4(3) . . ? C6 C4 C5 113.3(3) . . ? O3 C4 H4 108.4 . . ? C6 C4 H4 108.4 . . ? C5 C4 H4 108.4 . . ? O4 C7 C8 108.8(2) . . ? O4 C7 C9 108.1(2) . . ? C8 C7 C9 113.1(3) . . ? O4 C7 H7 109.0 . . ? C8 C7 H7 109.0 . . ? C9 C7 H7 109.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O1 C11 C12 118.57(18) . . ? O1 C11 C16 120.60(17) . . ? C12 C11 C16 120.80(18) . . ? C13 C12 C11 119.18(19) . . ? C13 C12 C1 119.28(18) . . ? C11 C12 C1 121.20(18) . . ? C14 C13 C12 122.07(19) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 117.15(19) . . ? C13 C14 C41 119.56(19) . . ? C15 C14 C41 123.29(19) . . ? C14 C15 C16 123.61(19) . . ? C14 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C15 C16 C11 117.19(18) . . ? C15 C16 C45 121.74(18) . . ? C11 C16 C45 120.99(18) . . ? O2 C21 C22 118.50(17) . . ? O2 C21 C26 120.14(17) . . ? C22 C21 C26 121.36(17) . . ? C23 C22 C21 119.49(18) . . ? C23 C22 C2 121.03(17) . . ? C21 C22 C2 119.42(17) . . ? C24 C23 C22 121.50(18) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 117.04(18) . . ? C23 C24 C49 123.18(17) . . ? C25 C24 C49 119.76(17) . . ? C26 C25 C24 123.77(18) . . ? C26 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C25 C26 C21 116.78(17) . . ? C25 C26 C53 122.41(17) . . ? C21 C26 C53 120.77(17) . . ? C32 C31 C36 118.92(18) . . ? C32 C31 C3 118.25(18) . . ? C36 C31 C3 122.60(18) . . ? C31 C32 C33 122.0(2) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C34 C33 C32 119.9(2) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.7(2) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C37 120.7(2) . . ? C34 C35 C36 119.77(19) . . ? C37 C35 C36 119.6(2) . . ? C40 C36 C35 117.26(19) . . ? C40 C36 C31 124.14(18) . . ? C35 C36 C31 118.57(19) . . ? C38 C37 C35 121.1(2) . . ? C38 C37 H37 119.4 . . ? C35 C37 H37 119.4 . . ? C37 C38 C39 120.0(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.3(2) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C39 C40 C36 121.7(2) . . ? C39 C40 H40 119.2 . . ? C36 C40 H40 119.2 . . ? C44 C41 C42 108.4(2) . . ? C44 C41 C43 108.4(2) . . ? C42 C41 C43 109.6(2) . . ? C44 C41 C14 112.42(18) . . ? C42 C41 C14 109.50(18) . . ? C43 C41 C14 108.52(18) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C47 107.58(19) . . ? C46 C45 C16 112.21(18) . . ? C47 C45 C16 110.46(17) . . ? C46 C45 C48 107.70(19) . . ? C47 C45 C48 110.4(2) . . ? C16 C45 C48 108.47(18) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C52 C49 C24 112.32(17) . . ? C52 C49 C51 107.82(18) . . ? C24 C49 C51 110.26(17) . . ? C52 C49 C50 108.12(18) . . ? C24 C49 C50 109.02(17) . . ? C51 C49 C50 109.23(18) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C56 C53 C26 112.03(16) . . ? C56 C53 C55 108.25(17) . . ? C26 C53 C55 108.95(16) . . ? C56 C53 C54 107.09(17) . . ? C26 C53 C54 110.62(16) . . ? C55 C53 C54 109.86(16) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O3 C4' H4' 107.4 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.288 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.083 #===END