Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_section_title 'Robust Chiral Zirconium Alkoxide Initiators' _publ_contact_author_name 'Matthew G. Davidson' _publ_contact_author_address ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; _publ_contact_author_email m.g.davidson@bath.ac.uk loop_ _publ_author_name _publ_author_address M.Davidson ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; A.Chmura ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; D.Cousins ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; M.Jones ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; M.Lunn ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; M.Mahon ;Department of Chemistry University of Bath Claverton Down Bath BA2 7AY UK ; data_1H _database_code_depnum_ccdc_archive 'CCDC 665065' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H13 Cl2 N O' _chemical_formula_weight 294.16 _chemical_absolute_configuration ad 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' 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 'C 2' _symmetry_int_tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 21.2540(2) _cell_length_b 9.08200(10) _cell_length_c 15.6400(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.2910(10) _cell_angle_gamma 90.00 _cell_volume 2772.95(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36069 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.458 _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_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ccd _diffrn_measurement_method 'nonius kappa ccd' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25570 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 27.57 _reflns_number_total 6089 _reflns_number_gt 5506 _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^)+(0.0335P)^2^+0.8911P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 6089 _refine_ls_number_parameters 369 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _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 Cl1 Cl 0.83440(2) 0.19669(5) 0.67038(3) 0.03533(12) Uani 1 1 d . . . Cl3 Cl 1.03226(3) -0.13747(6) 0.65352(4) 0.04426(14) Uani 1 1 d . . . Cl4 Cl 1.15317(2) 0.36674(6) 0.81917(4) 0.03875(13) Uani 1 1 d . . . Cl2 Cl 0.96852(3) 0.66881(6) 0.86656(4) 0.05060(16) Uani 1 1 d . . . O2 O 1.03204(7) 0.50745(15) 0.68014(10) 0.0327(3) Uani 1 1 d . . . O1 O 0.95159(7) 0.03164(15) 0.79767(10) 0.0303(3) Uani 1 1 d . . . N2 N 0.90946(8) 0.50235(18) 0.54958(10) 0.0281(3) Uani 1 1 d . . . N1 N 1.06836(8) 0.00636(19) 0.93392(10) 0.0293(4) Uani 1 1 d . . . C3 C 0.90765(10) 0.4216(2) 0.77577(13) 0.0271(4) Uani 1 1 d . . . C1 C 0.95651(9) 0.1763(2) 0.81580(12) 0.0245(4) Uani 1 1 d . . . C16 C 1.03167(9) 0.3600(2) 0.67082(12) 0.0254(4) Uani 1 1 d . . . C10 C 1.17424(9) -0.1057(2) 0.94177(12) 0.0271(4) Uani 1 1 d . . . C25 C 0.81025(9) 0.6259(2) 0.55393(12) 0.0246(4) Uani 1 1 d . . . C2 C 0.90440(9) 0.2715(2) 0.76103(13) 0.0257(4) Uani 1 1 d . . . C18 C 1.08796(10) 0.1252(2) 0.72543(14) 0.0269(4) Uani 1 1 d . . . C26 C 0.75370(9) 0.5516(2) 0.55625(12) 0.0287(4) Uani 1 1 d . . . H26 H 0.7350 0.4709 0.5154 0.034 Uiso 1 1 calc R . . C20 C 0.97787(10) 0.1310(2) 0.59718(13) 0.0283(4) Uani 1 1 d . . . H20 H 0.9406 0.0802 0.5516 0.034 Uiso 1 1 calc R . . C6 C 1.01319(9) 0.2386(2) 0.88920(13) 0.0272(4) Uani 1 1 d . . . C5 C 1.01653(9) 0.3899(2) 0.90432(13) 0.0299(4) Uani 1 1 d . . . H5 H 1.0548 0.4314 0.9536 0.036 Uiso 1 1 calc R . . C30 C 0.83727(10) 0.7434(2) 0.61476(13) 0.0295(4) Uani 1 1 d . . . H30 H 0.8762 0.7946 0.6145 0.035 Uiso 1 1 calc R . . C28 C 0.75142(10) 0.7106(2) 0.67699(13) 0.0347(5) Uani 1 1 d . . . H28 H 0.7315 0.7396 0.7191 0.042 Uiso 1 1 calc R . . C21 C 0.97672(9) 0.2845(2) 0.60276(13) 0.0251(4) Uani 1 1 d . . . C24 C 0.85893(10) 0.6942(3) 0.43438(13) 0.0364(5) Uani 1 1 d . . . H24A H 0.8794 0.6518 0.3937 0.055 Uiso 1 1 calc R . . H24B H 0.8908 0.7650 0.4770 0.055 Uiso 1 1 calc R . . H24C H 0.8162 0.7445 0.3964 0.055 Uiso 1 1 calc R . . C11 C 1.22634(10) -0.0042(2) 0.95533(13) 0.0343(4) Uani 1 1 d . . . H11 H 1.2336 0.0742 0.9984 0.041 Uiso 1 1 calc R . . C4 C 0.96423(10) 0.4797(2) 0.84767(13) 0.0302(4) Uani 1 1 d . . . C15 C 1.16429(11) -0.2181(2) 0.87814(14) 0.0356(5) Uani 1 1 d . . . H15 H 1.1286 -0.2874 0.8680 0.043 Uiso 1 1 calc R . . C17 C 1.08659(9) 0.2773(2) 0.73121(13) 0.0263(4) Uani 1 1 d . . . C22 C 0.91549(9) 0.3640(2) 0.54181(12) 0.0285(4) Uani 1 1 d . . . C19 C 1.03315(10) 0.0537(2) 0.65782(14) 0.0295(4) Uani 1 1 d . . . C29 C 0.80775(11) 0.7859(2) 0.67561(13) 0.0334(5) Uani 1 1 d . . . H29 H 0.8261 0.8668 0.7164 0.040 Uiso 1 1 calc R . . C12 C 1.26776(11) -0.0177(3) 0.90589(15) 0.0431(6) Uani 1 1 d . . . H12 H 1.3034 0.0516 0.9154 0.052 Uiso 1 1 calc R . . C14 C 1.20581(13) -0.2310(3) 0.82889(15) 0.0443(6) Uani 1 1 d . . . H14 H 1.1985 -0.3088 0.7854 0.053 Uiso 1 1 calc R . . C7 C 1.06932(10) 0.1440(2) 0.94920(13) 0.0298(4) Uani 1 1 d . . . C8 C 1.12557(9) -0.0909(2) 0.99155(13) 0.0300(4) Uani 1 1 d . . . H8 H 1.1054 -0.1906 0.9910 0.036 Uiso 1 1 calc R . . C27 C 0.72417(10) 0.5939(2) 0.61751(13) 0.0339(5) Uani 1 1 d . . . H27 H 0.6854 0.5427 0.6183 0.041 Uiso 1 1 calc R . . C9 C 1.16046(11) -0.0450(3) 1.09298(13) 0.0398(5) Uani 1 1 d . . . H9A H 1.1262 -0.0363 1.1200 0.060 Uiso 1 1 calc R . . H9B H 1.1831 0.0503 1.0970 0.060 Uiso 1 1 calc R . . H9C H 1.1946 -0.1192 1.1273 0.060 Uiso 1 1 calc R . . C23 C 0.84397(9) 0.5721(2) 0.49020(12) 0.0288(4) Uani 1 1 d . . . H23 H 0.8138 0.4969 0.4464 0.035 Uiso 1 1 calc R . . C13 C 1.25759(12) -0.1309(3) 0.84300(16) 0.0468(6) Uani 1 1 d . . . H13 H 1.2862 -0.1398 0.8096 0.056 Uiso 1 1 calc R . . H7 H 1.1053(10) 0.196(2) 0.9998(13) 0.025(5) Uiso 1 1 d . . . H22 H 0.8790(11) 0.298(3) 0.4993(16) 0.040(6) Uiso 1 1 d . . . H18 H 1.1245(11) 0.069(2) 0.7686(14) 0.032(6) Uiso 1 1 d . . . H3 H 0.8732(11) 0.484(2) 0.7381(14) 0.033(6) Uiso 1 1 d . . . H2 H 0.9893(18) 0.538(4) 0.632(2) 0.093(11) Uiso 1 1 d . . . H1 H 0.9945(15) -0.009(3) 0.841(2) 0.073(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0243(2) 0.0333(3) 0.0386(2) -0.0031(2) 0.00199(18) -0.0033(2) Cl3 0.0389(3) 0.0264(3) 0.0576(3) -0.0069(3) 0.0085(2) 0.0057(2) Cl4 0.0230(2) 0.0390(3) 0.0457(3) -0.0097(2) 0.00445(19) -0.0035(2) Cl2 0.0488(3) 0.0281(3) 0.0553(3) -0.0077(3) -0.0003(3) 0.0014(2) O2 0.0282(7) 0.0247(7) 0.0424(8) -0.0013(6) 0.0109(6) -0.0018(6) O1 0.0253(7) 0.0256(7) 0.0365(7) 0.0005(6) 0.0083(6) 0.0015(6) N2 0.0254(8) 0.0302(9) 0.0272(8) 0.0027(7) 0.0089(6) 0.0029(7) N1 0.0236(8) 0.0347(9) 0.0298(8) 0.0060(7) 0.0107(7) 0.0047(7) C3 0.0238(10) 0.0288(10) 0.0282(9) 0.0039(8) 0.0098(8) 0.0036(8) C1 0.0243(9) 0.0258(10) 0.0277(9) 0.0034(8) 0.0147(7) 0.0001(8) C16 0.0243(9) 0.0260(9) 0.0290(9) -0.0007(8) 0.0138(7) 0.0003(8) C10 0.0228(9) 0.0301(10) 0.0249(8) 0.0069(8) 0.0058(7) 0.0075(7) C25 0.0232(9) 0.0243(9) 0.0210(8) 0.0037(7) 0.0029(7) 0.0047(7) C2 0.0202(9) 0.0299(10) 0.0260(9) 0.0011(8) 0.0081(8) -0.0008(7) C18 0.0229(9) 0.0287(11) 0.0288(9) 0.0006(8) 0.0100(8) 0.0037(8) C26 0.0253(9) 0.0279(9) 0.0258(9) -0.0015(8) 0.0025(7) -0.0021(8) C20 0.0257(10) 0.0305(11) 0.0274(9) -0.0045(8) 0.0091(8) 0.0000(8) C6 0.0229(9) 0.0351(12) 0.0254(9) 0.0031(8) 0.0113(8) 0.0032(8) C5 0.0253(9) 0.0346(12) 0.0267(9) -0.0025(8) 0.0072(7) -0.0018(8) C30 0.0283(10) 0.0281(10) 0.0270(9) 0.0054(8) 0.0054(8) -0.0011(8) C28 0.0369(11) 0.0381(11) 0.0302(9) 0.0019(9) 0.0144(8) 0.0094(10) C21 0.0243(9) 0.0289(10) 0.0228(9) -0.0018(8) 0.0101(7) 0.0008(8) C24 0.0353(10) 0.0430(12) 0.0318(9) 0.0090(10) 0.0141(8) 0.0071(10) C11 0.0305(11) 0.0375(11) 0.0334(10) 0.0030(9) 0.0110(8) 0.0038(9) C4 0.0304(10) 0.0268(10) 0.0314(10) -0.0011(8) 0.0102(8) 0.0009(8) C15 0.0363(11) 0.0337(11) 0.0325(10) 0.0046(9) 0.0089(9) 0.0063(9) C17 0.0182(9) 0.0329(11) 0.0279(9) -0.0050(8) 0.0093(7) -0.0046(8) C22 0.0278(9) 0.0323(10) 0.0243(8) -0.0008(9) 0.0089(7) 0.0031(9) C19 0.0315(10) 0.0264(10) 0.0322(10) -0.0040(8) 0.0142(8) 0.0020(8) C29 0.0395(12) 0.0252(10) 0.0285(10) -0.0007(8) 0.0060(9) 0.0037(9) C12 0.0292(11) 0.0544(15) 0.0472(12) 0.0116(11) 0.0165(10) 0.0018(10) C14 0.0570(15) 0.0452(14) 0.0317(11) 0.0030(10) 0.0185(11) 0.0194(11) C7 0.0252(10) 0.0375(12) 0.0249(9) 0.0006(8) 0.0080(8) -0.0010(8) C8 0.0256(9) 0.0331(11) 0.0307(9) 0.0071(8) 0.0106(8) 0.0064(8) C27 0.0278(10) 0.0401(12) 0.0316(10) 0.0053(9) 0.0093(8) 0.0005(9) C9 0.0349(11) 0.0571(15) 0.0288(10) 0.0115(10) 0.0141(9) 0.0153(10) C23 0.0253(9) 0.0316(10) 0.0242(9) 0.0024(8) 0.0040(7) 0.0047(8) C13 0.0454(12) 0.0604(16) 0.0444(12) 0.0151(13) 0.0282(10) 0.0211(13) _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 Cl1 C2 1.7371(19) . ? Cl3 C19 1.737(2) . ? Cl4 C17 1.7364(19) . ? Cl2 C4 1.739(2) . ? O2 C16 1.347(2) . ? O2 H2 0.97(3) . ? O1 C1 1.339(2) . ? O1 H1 0.97(3) . ? N2 C22 1.274(3) . ? N2 C23 1.476(2) . ? N1 C7 1.271(3) . ? N1 C8 1.485(2) . ? C3 C2 1.379(3) . ? C3 C4 1.386(3) . ? C3 H3 0.93(2) . ? C1 C2 1.399(3) . ? C1 C6 1.413(3) . ? C16 C17 1.395(3) . ? C16 C21 1.408(3) . ? C10 C15 1.382(3) . ? C10 C11 1.391(3) . ? C10 C8 1.527(3) . ? C25 C26 1.391(3) . ? C25 C30 1.393(3) . ? C25 C23 1.520(3) . ? C18 C19 1.387(3) . ? C18 C17 1.386(3) . ? C18 H18 0.95(2) . ? C26 C27 1.391(3) . ? C26 H26 0.9500 . ? C20 C19 1.375(3) . ? C20 C21 1.398(3) . ? C20 H20 0.9500 . ? C6 C5 1.391(3) . ? C6 C7 1.469(3) . ? C5 C4 1.381(3) . ? C5 H5 0.9500 . ? C30 C29 1.386(3) . ? C30 H30 0.9500 . ? C28 C27 1.377(3) . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C21 C22 1.464(3) . ? C24 C23 1.521(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C15 C14 1.387(3) . ? C15 H15 0.9500 . ? C22 H22 1.00(2) . ? C29 H29 0.9500 . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C14 C13 1.376(4) . ? C14 H14 0.9500 . ? C7 H7 0.98(2) . ? C8 C9 1.520(3) . ? C8 H8 1.0000 . ? C27 H27 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C23 H23 1.0000 . ? C13 H13 0.9500 . ? 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 C16 O2 H2 104(2) . . ? C1 O1 H1 104.7(19) . . ? C22 N2 C23 117.95(16) . . ? C7 N1 C8 121.49(16) . . ? C2 C3 C4 118.83(18) . . ? C2 C3 H3 121.4(13) . . ? C4 C3 H3 119.8(13) . . ? O1 C1 C2 120.00(16) . . ? O1 C1 C6 122.36(16) . . ? C2 C1 C6 117.64(18) . . ? O2 C16 C17 119.61(16) . . ? O2 C16 C21 122.24(16) . . ? C17 C16 C21 118.14(18) . . ? C15 C10 C11 119.02(18) . . ? C15 C10 C8 119.39(18) . . ? C11 C10 C8 121.51(18) . . ? C26 C25 C30 118.71(17) . . ? C26 C25 C23 119.84(16) . . ? C30 C25 C23 121.34(16) . . ? C3 C2 C1 122.21(18) . . ? C3 C2 Cl1 119.55(15) . . ? C1 C2 Cl1 118.23(15) . . ? C19 C18 C17 118.93(19) . . ? C19 C18 H18 119.8(13) . . ? C17 C18 H18 121.2(13) . . ? C27 C26 C25 120.93(18) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C19 C20 C21 119.81(19) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C5 C6 C1 120.25(17) . . ? C5 C6 C7 119.69(17) . . ? C1 C6 C7 120.06(18) . . ? C4 C5 C6 120.03(17) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C29 C30 C25 120.41(18) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C27 C28 C29 120.27(18) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C20 C21 C16 120.20(18) . . ? C20 C21 C22 118.97(18) . . ? C16 C21 C22 120.67(18) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C12 C11 C10 119.9(2) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C5 C4 C3 121.03(19) . . ? C5 C4 Cl2 119.98(15) . . ? C3 C4 Cl2 118.98(15) . . ? C10 C15 C14 120.8(2) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C18 C17 C16 121.72(18) . . ? C18 C17 Cl4 119.10(16) . . ? C16 C17 Cl4 119.11(15) . . ? N2 C22 C21 121.44(18) . . ? N2 C22 H22 124.9(13) . . ? C21 C22 H22 113.4(13) . . ? C20 C19 C18 121.20(19) . . ? C20 C19 Cl3 119.34(15) . . ? C18 C19 Cl3 119.38(15) . . ? C30 C29 C28 120.09(19) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C13 C14 C15 120.0(2) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N1 C7 C6 120.44(18) . . ? N1 C7 H7 125.4(12) . . ? C6 C7 H7 114.2(12) . . ? N1 C8 C9 114.51(16) . . ? N1 C8 C10 107.48(14) . . ? C9 C8 C10 114.02(16) . . ? N1 C8 H8 106.8 . . ? C9 C8 H8 106.8 . . ? C10 C8 H8 106.8 . . ? C28 C27 C26 119.59(19) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C23 C24 108.36(15) . . ? N2 C23 C25 107.28(14) . . ? C24 C23 C25 113.69(16) . . ? N2 C23 H23 109.1 . . ? C24 C23 H23 109.1 . . ? C25 C23 H23 109.1 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 N2 0.97(3) 1.70(3) 2.599(2) 152(3) . O1 H1 N1 0.97(3) 1.67(3) 2.563(2) 151(3) . _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.200 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.062 #===END data_(R2)2Ti(OiPr)2 _database_code_depnum_ccdc_archive 'CCDC 665066' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H46 N2 O6 Ti' _chemical_formula_weight 674.67 _chemical_absolute_configuration ad 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 'C 2' _symmetry_int_tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 19.9450(2) _cell_length_b 9.4060(2) _cell_length_c 11.1810(2) _cell_angle_alpha 90.0000 _cell_angle_beta 122.9800(10) _cell_angle_gamma 90.0000 _cell_volume 1759.58(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12553 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description yellow _exptl_crystal_colour block _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 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.291 _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_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius Kappa CCD' _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 15092 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3973 _reflns_number_gt 3658 _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^)+(0.0506P)^2^+0.6639P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 3973 _refine_ls_number_parameters 221 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.5000 0.70257(4) 1.0000 0.02062(12) Uani 1 2 d S . . O2 O 0.45025(8) 0.58062(15) 0.84958(14) 0.0275(3) Uani 1 1 d . . . N1 N 0.44327(10) 0.88267(18) 0.83050(16) 0.0224(3) Uani 1 1 d . . . C1 C 0.37466(17) 0.5083(3) 0.7811(3) 0.0452(6) Uani 1 1 d . . . H1 H 0.3401 0.5671 0.8012 0.054 Uiso 1 1 calc R . . H11 H 0.3493(14) 0.995(3) 0.696(2) 0.031(6) Uiso 1 1 d . . . O1 O 0.40780(7) 0.73388(14) 1.00599(12) 0.0238(3) Uani 1 1 d . . . C2 C 0.38364(16) 0.3696(3) 0.8506(3) 0.0547(7) Uani 1 1 d . . . H2A H 0.4142 0.3048 0.8292 0.082 Uiso 1 1 calc R . . H2B H 0.3307 0.3290 0.8148 0.082 Uiso 1 1 calc R . . H2C H 0.4119 0.3830 0.9540 0.082 Uiso 1 1 calc R . . O3 O 0.11835(9) 1.01474(17) 0.70746(18) 0.0382(4) Uani 1 1 d . . . C3 C 0.33503(17) 0.5080(4) 0.6272(3) 0.0646(9) Uani 1 1 d . . . H3A H 0.3233 0.6060 0.5917 0.097 Uiso 1 1 calc R . . H3B H 0.2851 0.4540 0.5843 0.097 Uiso 1 1 calc R . . H3C H 0.3700 0.4637 0.6015 0.097 Uiso 1 1 calc R . . C4 C 0.33807(11) 0.8029(2) 0.93504(19) 0.0220(4) Uani 1 1 d . . . C5 C 0.28183(11) 0.7810(2) 0.9712(2) 0.0252(4) Uani 1 1 d . . . H5 H 0.2940 0.7173 1.0464 0.030 Uiso 1 1 calc R . . C6 C 0.20845(12) 0.8505(2) 0.8994(2) 0.0264(4) Uani 1 1 d . . . H6 H 0.1711 0.8340 0.9256 0.032 Uiso 1 1 calc R . . C7 C 0.18986(11) 0.9441(2) 0.7896(2) 0.0270(4) Uani 1 1 d . . . C8 C 0.24550(11) 0.9690(2) 0.7538(2) 0.0256(4) Uani 1 1 d . . . H8 H 0.2332 1.0345 0.6799 0.031 Uiso 1 1 calc R . . C9 C 0.31934(11) 0.8993(2) 0.82486(19) 0.0226(4) Uani 1 1 d . . . C10 C 0.05620(14) 0.9797(3) 0.7273(3) 0.0490(6) Uani 1 1 d . . . H10A H 0.0469 0.8769 0.7164 0.074 Uiso 1 1 calc R . . H10B H 0.0072 1.0295 0.6562 0.074 Uiso 1 1 calc R . . H10C H 0.0713 1.0085 0.8232 0.074 Uiso 1 1 calc R . . C11 C 0.37282(12) 0.9311(2) 0.7778(2) 0.0241(4) Uani 1 1 d . . . C12 C 0.48785(11) 0.9363(2) 0.7652(2) 0.0256(4) Uani 1 1 d . . . H12 H 0.5274 0.8611 0.7815 0.031 Uiso 1 1 calc R . . C13 C 0.53565(13) 1.0672(2) 0.8472(2) 0.0342(5) Uani 1 1 d . . . H13A H 0.4990 1.1425 0.8374 0.051 Uiso 1 1 calc R . . H13B H 0.5669 1.1004 0.8089 0.051 Uiso 1 1 calc R . . H13C H 0.5718 1.0429 0.9482 0.051 Uiso 1 1 calc R . . C14 C 0.43404(11) 0.9581(2) 0.6045(2) 0.0239(4) Uani 1 1 d . . . C15 C 0.40599(14) 1.0910(2) 0.5423(2) 0.0356(5) Uani 1 1 d . . . H15 H 0.4201 1.1729 0.6010 0.043 Uiso 1 1 calc R . . C16 C 0.35734(15) 1.1048(3) 0.3947(2) 0.0421(6) Uani 1 1 d . . . H16 H 0.3377 1.1959 0.3535 0.051 Uiso 1 1 calc R . . C17 C 0.33762(14) 0.9880(3) 0.3084(2) 0.0368(5) Uani 1 1 d . . . H17 H 0.3049 0.9982 0.2077 0.044 Uiso 1 1 calc R . . C18 C 0.36522(14) 0.8565(2) 0.3678(2) 0.0377(5) Uani 1 1 d . . . H18 H 0.3516 0.7752 0.3085 0.045 Uiso 1 1 calc R . . C19 C 0.41318(13) 0.8422(2) 0.5151(2) 0.0331(5) Uani 1 1 d . . . H19 H 0.4321 0.7506 0.5553 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0179(2) 0.0249(2) 0.0172(2) 0.000 0.00828(16) 0.000 O2 0.0252(7) 0.0302(8) 0.0239(7) -0.0054(6) 0.0112(6) -0.0038(6) N1 0.0231(8) 0.0263(8) 0.0196(7) 0.0005(6) 0.0128(7) -0.0010(6) C1 0.0381(14) 0.0464(14) 0.0336(13) -0.0057(11) 0.0081(11) -0.0149(11) O1 0.0209(6) 0.0301(8) 0.0195(6) 0.0023(5) 0.0105(5) 0.0005(5) C2 0.0412(14) 0.0457(15) 0.0648(18) 0.0085(13) 0.0209(13) -0.0099(11) O3 0.0259(7) 0.0371(8) 0.0546(10) 0.0110(7) 0.0240(7) 0.0091(6) C3 0.0432(15) 0.100(2) 0.0352(13) -0.0038(14) 0.0111(12) -0.0280(16) C4 0.0204(9) 0.0261(9) 0.0178(8) -0.0029(7) 0.0092(7) -0.0006(7) C5 0.0259(9) 0.0290(10) 0.0225(9) -0.0024(8) 0.0145(8) -0.0026(8) C6 0.0264(9) 0.0288(10) 0.0289(10) -0.0054(8) 0.0183(8) -0.0027(8) C7 0.0233(9) 0.0245(10) 0.0325(10) -0.0025(8) 0.0147(8) 0.0026(8) C8 0.0258(9) 0.0251(9) 0.0263(9) 0.0019(8) 0.0143(8) 0.0016(8) C9 0.0213(9) 0.0259(9) 0.0194(8) -0.0017(7) 0.0104(7) -0.0002(7) C10 0.0302(11) 0.0441(14) 0.0784(18) 0.0145(13) 0.0333(13) 0.0083(10) C11 0.0228(10) 0.0273(10) 0.0214(9) 0.0037(8) 0.0115(8) 0.0026(8) C12 0.0253(9) 0.0303(10) 0.0223(9) 0.0054(8) 0.0137(8) 0.0031(8) C13 0.0297(10) 0.0406(12) 0.0284(10) 0.0041(9) 0.0132(9) -0.0050(9) C14 0.0238(9) 0.0286(9) 0.0233(9) 0.0045(7) 0.0154(8) 0.0028(8) C15 0.0484(13) 0.0277(10) 0.0278(10) 0.0040(8) 0.0188(10) 0.0032(10) C16 0.0568(15) 0.0329(11) 0.0300(11) 0.0124(9) 0.0193(11) 0.0065(11) C17 0.0379(11) 0.0478(13) 0.0239(10) 0.0052(9) 0.0161(9) 0.0014(10) C18 0.0424(12) 0.0375(13) 0.0301(11) -0.0060(9) 0.0177(10) 0.0015(10) C19 0.0374(11) 0.0278(10) 0.0317(11) 0.0047(8) 0.0173(9) 0.0051(9) _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 1.8200(14) . ? Ti1 O2 1.8200(14) 2_657 ? Ti1 O1 1.8991(12) . ? Ti1 O1 1.8991(12) 2_657 ? Ti1 N1 2.3253(17) 2_657 ? Ti1 N1 2.3253(16) . ? O2 C1 1.437(3) . ? N1 C11 1.276(3) . ? N1 C12 1.512(2) . ? C1 C3 1.451(3) . ? C1 C2 1.479(4) . ? C1 H1 1.0000 . ? O1 C4 1.336(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C7 1.376(2) . ? O3 C10 1.412(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.399(2) . ? C4 C9 1.407(3) . ? C5 C6 1.391(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C8 C9 1.399(3) . ? C8 H8 0.9500 . ? C9 C11 1.454(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.98(2) . ? C12 C13 1.521(3) . ? C12 C14 1.524(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.381(3) . ? C14 C15 1.391(3) . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 C17 1.372(3) . ? C16 H16 0.9500 . ? C17 C18 1.370(3) . ? C17 H17 0.9500 . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? 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 101.86(9) . 2_657 ? O2 Ti1 O1 94.53(6) . . ? O2 Ti1 O1 96.69(6) 2_657 . ? O2 Ti1 O1 96.69(6) . 2_657 ? O2 Ti1 O1 94.53(6) 2_657 2_657 ? O1 Ti1 O1 162.16(8) . 2_657 ? O2 Ti1 N1 172.30(6) . 2_657 ? O2 Ti1 N1 85.83(6) 2_657 2_657 ? O1 Ti1 N1 84.79(5) . 2_657 ? O1 Ti1 N1 82.23(5) 2_657 2_657 ? O2 Ti1 N1 85.83(6) . . ? O2 Ti1 N1 172.30(6) 2_657 . ? O1 Ti1 N1 82.23(5) . . ? O1 Ti1 N1 84.79(5) 2_657 . ? N1 Ti1 N1 86.48(8) 2_657 . ? C1 O2 Ti1 132.60(15) . . ? C11 N1 C12 116.58(16) . . ? C11 N1 Ti1 124.15(13) . . ? C12 N1 Ti1 118.93(11) . . ? O2 C1 C3 111.7(2) . . ? O2 C1 C2 110.2(2) . . ? C3 C1 C2 117.0(3) . . ? O2 C1 H1 105.7 . . ? C3 C1 H1 105.7 . . ? C2 C1 H1 105.7 . . ? C4 O1 Ti1 140.32(11) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 O3 C10 117.53(17) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O1 C4 C5 119.76(16) . . ? O1 C4 C9 121.84(16) . . ? C5 C4 C9 118.39(17) . . ? C6 C5 C4 121.43(18) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C5 119.93(17) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? O3 C7 C6 125.27(17) . . ? O3 C7 C8 115.28(18) . . ? C6 C7 C8 119.44(18) . . ? C7 C8 C9 121.12(18) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 119.67(16) . . ? C8 C9 C11 116.81(17) . . ? C4 C9 C11 123.51(17) . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C9 126.87(18) . . ? N1 C11 H11 119.9(13) . . ? C9 C11 H11 113.2(13) . . ? N1 C12 C13 108.61(15) . . ? N1 C12 C14 113.11(15) . . ? C13 C12 C14 114.22(16) . . ? N1 C12 H12 106.8 . . ? C13 C12 H12 106.8 . . ? C14 C12 H12 106.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 117.85(18) . . ? C19 C14 C12 119.25(17) . . ? C15 C14 C12 122.89(18) . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 119.9(2) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C14 C19 C18 121.6(2) . . ? C14 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.441 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.069 #===END data_(R1)Zr(OiPr)2 _database_code_depnum_ccdc_archive 'CCDC 665067' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 N2 O4 Zr' _chemical_formula_weight 657.94 _chemical_absolute_configuration ad 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 17.6960(2) _cell_length_b 10.4180(3) _cell_length_c 18.2880(3) _cell_angle_alpha 90 _cell_angle_beta 101.4880(10) _cell_angle_gamma 90 _cell_volume 3303.98(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 88079 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.373 _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_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius Kappa CCD' _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 68318 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15063 _reflns_number_gt 11657 _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^)+(0.0893P)^2^+1.3472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 15063 _refine_ls_number_parameters 803 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.62929(2) 0.68358(3) -0.16639(2) 0.03323(15) Uani 1 1 d . . . O1 O 0.55640(18) 0.8376(3) -0.18374(19) 0.0414(8) Uani 1 1 d . . . N1 N 0.6962(2) 0.8346(3) -0.2348(2) 0.0300(8) Uani 1 1 d . . . C1 C 0.5606(2) 0.9655(4) -0.1893(2) 0.0329(9) Uani 1 1 d . . . H7 H 0.708(3) 1.010(5) -0.262(3) 0.030(12) Uiso 1 1 d . . . H22 H 0.575(3) 0.529(5) -0.383(3) 0.037(13) Uiso 1 1 d . . . H43 H 0.792(3) 0.546(5) 0.267(2) 0.033(12) Uiso 1 1 d . . . H58 H 0.925(3) 0.025(5) 0.378(3) 0.035(12) Uiso 1 1 d . . . Zr2 Zr 0.87884(2) 0.22103(3) 0.17284(2) 0.03200(14) Uani 1 1 d . . . O2 O 0.70680(17) 0.5495(3) -0.18860(16) 0.0359(7) Uani 1 1 d . . . N2 N 0.57458(18) 0.6213(3) -0.29412(18) 0.0284(7) Uani 1 1 d . . . C2 C 0.5069(2) 1.0430(4) -0.1626(2) 0.0362(10) Uani 1 1 d . . . H2 H 0.4687 1.0043 -0.1400 0.043 Uiso 1 1 calc R . . O3 O 0.55701(19) 0.5696(3) -0.13266(18) 0.0425(8) Uani 1 1 d . . . N3 N 0.80944(19) 0.3686(4) 0.24019(19) 0.0316(8) Uani 1 1 d . . . C3 C 0.5095(3) 1.1753(5) -0.1691(2) 0.0410(11) Uani 1 1 d . . . H3 H 0.4728 1.2265 -0.1508 0.049 Uiso 1 1 calc R . . O4 O 0.6924(2) 0.7411(4) -0.07454(17) 0.0495(8) Uani 1 1 d . . . N4 N 0.93026(18) 0.1373(3) 0.29655(17) 0.0272(7) Uani 1 1 d . . . C4 C 0.5646(3) 1.2343(5) -0.2018(2) 0.0401(10) Uani 1 1 d . . . H4 H 0.5652 1.3250 -0.2069 0.048 Uiso 1 1 calc R . . O5 O 0.95508(16) 0.3726(3) 0.19979(18) 0.0373(7) Uani 1 1 d . . . C5 C 0.6183(3) 1.1595(5) -0.2268(2) 0.0376(10) Uani 1 1 d . . . H5 H 0.6565 1.1997 -0.2488 0.045 Uiso 1 1 calc R . . O6 O 0.79808(18) 0.0886(3) 0.18784(16) 0.0357(7) Uani 1 1 d . . . C6 C 0.6180(2) 1.0239(4) -0.2206(2) 0.0300(9) Uani 1 1 d . . . O7 O 0.94998(19) 0.1088(3) 0.13575(16) 0.0390(7) Uani 1 1 d . . . C7 C 0.6800(2) 0.9541(5) -0.2441(2) 0.0333(9) Uani 1 1 d . . . O8 O 0.82039(19) 0.2940(3) 0.08343(17) 0.0439(8) Uani 1 1 d . . . C8 C 0.7681(2) 0.7888(5) -0.2576(2) 0.0349(10) Uani 1 1 d . . . H8 H 0.7590 0.6973 -0.2735 0.042 Uiso 1 1 calc R . . C9 C 0.8312(3) 0.7882(6) -0.1874(3) 0.0464(12) Uani 1 1 d . . . H9A H 0.8394 0.8757 -0.1678 0.070 Uiso 1 1 calc R . . H9B H 0.8792 0.7557 -0.1996 0.070 Uiso 1 1 calc R . . H9C H 0.8157 0.7327 -0.1497 0.070 Uiso 1 1 calc R . . C10 C 0.7893(2) 0.8605(4) -0.3229(2) 0.0352(9) Uani 1 1 d . . . C11 C 0.8504(3) 0.9456(5) -0.3154(3) 0.0433(11) Uani 1 1 d . . . H11 H 0.8809 0.9607 -0.2672 0.052 Uiso 1 1 calc R . . C12 C 0.8682(3) 1.0098(5) -0.3767(3) 0.0543(13) Uani 1 1 d . . . H12 H 0.9104 1.0679 -0.3702 0.065 Uiso 1 1 calc R . . C13 C 0.8245(4) 0.9886(6) -0.4461(3) 0.0578(14) Uani 1 1 d . . . H13 H 0.8365 1.0321 -0.4880 0.069 Uiso 1 1 calc R . . C14 C 0.7636(4) 0.9048(7) -0.4557(3) 0.0640(17) Uani 1 1 d . . . H14 H 0.7330 0.8912 -0.5040 0.077 Uiso 1 1 calc R . . C15 C 0.7463(3) 0.8393(6) -0.3939(3) 0.0491(12) Uani 1 1 d . . . H15 H 0.7048 0.7798 -0.4008 0.059 Uiso 1 1 calc R . . C16 C 0.7222(2) 0.4718(4) -0.2400(2) 0.0293(9) Uani 1 1 d . . . C17 C 0.7896(3) 0.3955(5) -0.2252(3) 0.0400(10) Uani 1 1 d . . . H17 H 0.8235 0.4013 -0.1781 0.048 Uiso 1 1 calc R . . C18 C 0.8066(3) 0.3120(5) -0.2791(3) 0.0428(11) Uani 1 1 d . . . H18 H 0.8516 0.2602 -0.2681 0.051 Uiso 1 1 calc R . . C19 C 0.7586(3) 0.3040(5) -0.3485(3) 0.0407(10) Uani 1 1 d . . . H19 H 0.7708 0.2475 -0.3853 0.049 Uiso 1 1 calc R . . C20 C 0.6929(2) 0.3784(4) -0.3641(2) 0.0333(9) Uani 1 1 d . . . H20 H 0.6600 0.3720 -0.4118 0.040 Uiso 1 1 calc R . . C21 C 0.6733(2) 0.4634(4) -0.3113(2) 0.0285(8) Uani 1 1 d . . . C22 C 0.6023(2) 0.5367(4) -0.3324(2) 0.0295(8) Uani 1 1 d . . . C23 C 0.4970(2) 0.6768(5) -0.3288(2) 0.0380(10) Uani 1 1 d . . . H23 H 0.4947 0.7654 -0.3082 0.046 Uiso 1 1 calc R . . C24 C 0.4365(3) 0.5976(7) -0.3016(3) 0.0634(17) Uani 1 1 d . . . H24A H 0.4381 0.5092 -0.3195 0.095 Uiso 1 1 calc R . . H24B H 0.3854 0.6343 -0.3208 0.095 Uiso 1 1 calc R . . H24C H 0.4468 0.5980 -0.2469 0.095 Uiso 1 1 calc R . . C25 C 0.4848(2) 0.6889(5) -0.4129(2) 0.0357(10) Uani 1 1 d . . . C26 C 0.5310(3) 0.7728(5) -0.4422(3) 0.0465(11) Uani 1 1 d . . . H26 H 0.5669 0.8247 -0.4095 0.056 Uiso 1 1 calc R . . C27 C 0.5259(3) 0.7831(6) -0.5191(3) 0.0600(15) Uani 1 1 d . . . H27 H 0.5597 0.8389 -0.5384 0.072 Uiso 1 1 calc R . . C28 C 0.4717(3) 0.7120(7) -0.5670(3) 0.0620(17) Uani 1 1 d . . . H28 H 0.4678 0.7187 -0.6194 0.074 Uiso 1 1 calc R . . C29 C 0.4233(4) 0.6317(6) -0.5385(3) 0.0630(16) Uani 1 1 d . . . H29 H 0.3858 0.5824 -0.5711 0.076 Uiso 1 1 calc R . . C30 C 0.4294(3) 0.6225(5) -0.4615(3) 0.0501(13) Uani 1 1 d . . . H30 H 0.3944 0.5692 -0.4423 0.060 Uiso 1 1 calc R . . C31 C 0.5099(3) 0.5224(5) -0.0851(3) 0.0441(11) Uani 1 1 d . . . H31 H 0.4671 0.4710 -0.1155 0.053 Uiso 1 1 calc R . . C32 C 0.4751(4) 0.6361(7) -0.0511(3) 0.0713(19) Uani 1 1 d . . . H32A H 0.5162 0.6842 -0.0187 0.107 Uiso 1 1 calc R . . H32B H 0.4382 0.6049 -0.0217 0.107 Uiso 1 1 calc R . . H32C H 0.4485 0.6923 -0.0911 0.107 Uiso 1 1 calc R . . C33 C 0.5557(3) 0.4366(5) -0.0264(3) 0.0537(13) Uani 1 1 d . . . H33A H 0.5756 0.3633 -0.0504 0.081 Uiso 1 1 calc R . . H33B H 0.5225 0.4056 0.0068 0.081 Uiso 1 1 calc R . . H33C H 0.5989 0.4851 0.0027 0.081 Uiso 1 1 calc R . . C34 C 0.7312(3) 0.7982(6) -0.0077(3) 0.0586(15) Uani 1 1 d . . . H34 H 0.7879 0.7897 -0.0053 0.070 Uiso 1 1 calc R . . C35 C 0.7121(5) 0.9341(6) -0.0103(4) 0.088(2) Uani 1 1 d . . . H35A H 0.7225 0.9716 -0.0564 0.132 Uiso 1 1 calc R . . H35B H 0.7436 0.9776 0.0328 0.132 Uiso 1 1 calc R . . H35C H 0.6574 0.9448 -0.0089 0.132 Uiso 1 1 calc R . . C36 C 0.7121(5) 0.7320(6) 0.0579(3) 0.084(2) Uani 1 1 d . . . H36A H 0.6571 0.7432 0.0581 0.126 Uiso 1 1 calc R . . H36B H 0.7428 0.7687 0.1037 0.126 Uiso 1 1 calc R . . H36C H 0.7237 0.6403 0.0555 0.126 Uiso 1 1 calc R . . C37 C 0.9469(2) 0.5001(4) 0.1995(2) 0.0311(9) Uani 1 1 d . . . C38 C 1.0007(2) 0.5777(5) 0.1731(2) 0.0361(10) Uani 1 1 d . . . H38 H 1.0418 0.5390 0.1547 0.043 Uiso 1 1 calc R . . C39 C 0.9943(2) 0.7100(5) 0.1738(2) 0.0380(10) Uani 1 1 d . . . H39 H 1.0309 0.7611 0.1555 0.046 Uiso 1 1 calc R . . C40 C 0.9350(3) 0.7694(5) 0.2010(2) 0.0386(10) Uani 1 1 d . . . H40 H 0.9315 0.8603 0.2023 0.046 Uiso 1 1 calc R . . C41 C 0.8813(3) 0.6940(4) 0.2259(2) 0.0368(10) Uani 1 1 d . . . H41 H 0.8404 0.7341 0.2440 0.044 Uiso 1 1 calc R . . C42 C 0.8854(2) 0.5586(4) 0.2252(2) 0.0308(9) Uani 1 1 d . . . C43 C 0.8229(2) 0.4900(4) 0.2478(2) 0.0319(9) Uani 1 1 d . . . C44 C 0.7366(3) 0.3216(5) 0.2603(2) 0.0369(10) Uani 1 1 d . . . H44 H 0.7456 0.2300 0.2759 0.044 Uiso 1 1 calc R . . C45 C 0.6748(3) 0.3210(6) 0.1890(3) 0.0508(13) Uani 1 1 d . . . H45A H 0.6664 0.4088 0.1698 0.076 Uiso 1 1 calc R . . H45B H 0.6265 0.2871 0.1999 0.076 Uiso 1 1 calc R . . H45C H 0.6917 0.2668 0.1515 0.076 Uiso 1 1 calc R . . C46 C 0.7124(2) 0.3917(5) 0.3252(2) 0.0374(10) Uani 1 1 d . . . C47 C 0.6503(3) 0.4732(6) 0.3163(3) 0.0518(13) Uani 1 1 d . . . H47 H 0.6209 0.4879 0.2676 0.062 Uiso 1 1 calc R . . C48 C 0.6292(4) 0.5350(6) 0.3767(3) 0.0635(16) Uani 1 1 d . . . H48 H 0.5857 0.5903 0.3695 0.076 Uiso 1 1 calc R . . C49 C 0.6722(4) 0.5146(6) 0.4465(3) 0.0659(17) Uani 1 1 d . . . H49 H 0.6585 0.5564 0.4882 0.079 Uiso 1 1 calc R . . C50 C 0.7346(4) 0.4348(7) 0.4571(3) 0.0675(18) Uani 1 1 d . . . H50 H 0.7644 0.4223 0.5058 0.081 Uiso 1 1 calc R . . C51 C 0.7549(3) 0.3715(6) 0.3966(3) 0.0556(14) Uani 1 1 d . . . H51 H 0.7977 0.3147 0.4043 0.067 Uiso 1 1 calc R . . C52 C 0.7786(2) 0.0057(4) 0.2363(2) 0.0320(9) Uani 1 1 d . . . C53 C 0.7098(3) -0.0627(5) 0.2182(3) 0.0408(10) Uani 1 1 d . . . H53 H 0.6766 -0.0492 0.1712 0.049 Uiso 1 1 calc R . . C54 C 0.6892(3) -0.1504(5) 0.2679(3) 0.0474(12) Uani 1 1 d . . . H54 H 0.6425 -0.1972 0.2541 0.057 Uiso 1 1 calc R . . C55 C 0.7360(3) -0.1709(5) 0.3377(3) 0.0428(11) Uani 1 1 d . . . H55 H 0.7213 -0.2305 0.3717 0.051 Uiso 1 1 calc R . . C56 C 0.8037(3) -0.1032(5) 0.3566(2) 0.0379(10) Uani 1 1 d . . . H56 H 0.8365 -0.1177 0.4037 0.045 Uiso 1 1 calc R . . C57 C 0.8256(2) -0.0122(4) 0.3071(2) 0.0298(9) Uani 1 1 d . . . C58 C 0.8996(2) 0.0500(4) 0.3312(2) 0.0310(9) Uani 1 1 d . . . C59 C 1.0668(3) 0.0818(6) 0.3106(3) 0.0478(12) Uani 1 1 d . . . H59A H 1.0606 -0.0018 0.3332 0.072 Uiso 1 1 calc R . . H59B H 1.1197 0.1125 0.3279 0.072 Uiso 1 1 calc R . . H59C H 1.0564 0.0731 0.2561 0.072 Uiso 1 1 calc R . . C60 C 1.0105(2) 0.1774(5) 0.3329(2) 0.0344(10) Uani 1 1 d . . . H60 H 1.0204 0.2624 0.3112 0.041 Uiso 1 1 calc R . . C61 C 1.0191(3) 0.1963(5) 0.4170(2) 0.0388(11) Uani 1 1 d . . . C62 C 0.9693(3) 0.2797(5) 0.4428(3) 0.0498(12) Uani 1 1 d . . . H62 H 0.9331 0.3273 0.4078 0.060 Uiso 1 1 calc R . . C63 C 0.9711(3) 0.2955(6) 0.5187(3) 0.0619(15) Uani 1 1 d . . . H63 H 0.9360 0.3525 0.5352 0.074 Uiso 1 1 calc R . . C64 C 1.0239(4) 0.2283(7) 0.5695(3) 0.0618(16) Uani 1 1 d . . . H64 H 1.0247 0.2368 0.6214 0.074 Uiso 1 1 calc R . . C65 C 1.0761(4) 0.1480(6) 0.5451(3) 0.0662(17) Uani 1 1 d . . . H65 H 1.1133 0.1023 0.5801 0.079 Uiso 1 1 calc R . . C66 C 1.0738(3) 0.1344(5) 0.4687(3) 0.0526(13) Uani 1 1 d . . . H66 H 1.1107 0.0814 0.4522 0.063 Uiso 1 1 calc R . . C67 C 0.9868(3) 0.0669(5) 0.0786(2) 0.0401(10) Uani 1 1 d . . . H67 H 1.0338 0.0167 0.1012 0.048 Uiso 1 1 calc R . . C68 C 0.9336(4) -0.0179(6) 0.0247(3) 0.0634(16) Uani 1 1 d . . . H68A H 0.9144 -0.0874 0.0522 0.095 Uiso 1 1 calc R . . H68B H 0.9618 -0.0544 -0.0114 0.095 Uiso 1 1 calc R . . H68C H 0.8900 0.0329 -0.0017 0.095 Uiso 1 1 calc R . . C69 C 1.0108(3) 0.1816(5) 0.0374(3) 0.0489(12) Uani 1 1 d . . . H69A H 0.9651 0.2319 0.0155 0.073 Uiso 1 1 calc R . . H69B H 1.0365 0.1517 -0.0023 0.073 Uiso 1 1 calc R . . H69C H 1.0465 0.2353 0.0724 0.073 Uiso 1 1 calc R . . C70 C 0.7801(3) 0.3684(5) 0.0228(3) 0.0413(11) Uani 1 1 d . . . H70 H 0.7355 0.4118 0.0384 0.050 Uiso 1 1 calc R . . C71 C 0.7500(4) 0.2785(6) -0.0412(3) 0.0662(17) Uani 1 1 d . . . H71A H 0.7933 0.2329 -0.0554 0.099 Uiso 1 1 calc R . . H71B H 0.7226 0.3279 -0.0839 0.099 Uiso 1 1 calc R . . H71C H 0.7147 0.2163 -0.0257 0.099 Uiso 1 1 calc R . . C72 C 0.8324(3) 0.4690(5) 0.0006(3) 0.0577(14) Uani 1 1 d . . . H72A H 0.8533 0.5227 0.0439 0.087 Uiso 1 1 calc R . . H72B H 0.8030 0.5226 -0.0392 0.087 Uiso 1 1 calc R . . H72C H 0.8748 0.4272 -0.0174 0.087 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 0.0384(2) 0.0347(3) 0.0287(2) -0.00610(17) 0.01166(18) -0.00648(17) O1 0.0455(18) 0.0311(17) 0.0538(19) -0.0135(14) 0.0251(15) -0.0102(13) N1 0.0301(18) 0.030(2) 0.0308(18) -0.0045(15) 0.0080(15) -0.0014(14) C1 0.028(2) 0.041(2) 0.030(2) -0.0058(18) 0.0070(17) -0.0019(17) Zr2 0.0351(2) 0.0347(3) 0.0278(2) 0.00594(17) 0.01011(17) 0.00732(17) O2 0.0386(17) 0.0411(17) 0.0276(15) -0.0008(13) 0.0058(13) -0.0010(13) N2 0.0244(16) 0.0317(19) 0.0298(17) -0.0017(15) 0.0070(13) 0.0033(13) C2 0.029(2) 0.042(3) 0.038(2) -0.010(2) 0.0079(18) -0.0028(17) O3 0.0502(19) 0.0424(19) 0.0384(17) -0.0008(14) 0.0177(15) -0.0105(15) N3 0.0243(17) 0.046(2) 0.0249(17) 0.0002(16) 0.0065(14) 0.0043(15) C3 0.033(2) 0.053(3) 0.036(2) -0.011(2) 0.0034(18) 0.006(2) O4 0.0541(19) 0.059(2) 0.0354(16) -0.0161(16) 0.0080(14) -0.0123(17) N4 0.0232(16) 0.0305(17) 0.0264(16) -0.0009(14) 0.0018(13) 0.0003(13) C4 0.044(2) 0.036(2) 0.040(2) 0.002(2) 0.0065(19) 0.007(2) O5 0.0329(15) 0.0323(16) 0.0487(18) 0.0061(14) 0.0126(13) 0.0057(12) C5 0.041(2) 0.040(3) 0.032(2) 0.0046(19) 0.0077(18) 0.003(2) O6 0.0382(16) 0.0388(17) 0.0284(15) 0.0023(13) 0.0026(13) 0.0012(13) C6 0.034(2) 0.028(2) 0.029(2) -0.0027(16) 0.0071(17) 0.0001(16) O7 0.0497(18) 0.0374(18) 0.0330(16) 0.0044(13) 0.0155(14) 0.0128(14) C7 0.029(2) 0.047(3) 0.025(2) 0.0000(18) 0.0066(17) -0.0073(19) O8 0.0480(19) 0.052(2) 0.0326(16) 0.0113(15) 0.0110(14) 0.0139(15) C8 0.030(2) 0.042(3) 0.035(2) 0.0011(19) 0.0128(18) 0.0018(18) C9 0.031(2) 0.071(3) 0.040(2) 0.011(2) 0.0122(19) 0.005(2) C10 0.034(2) 0.040(2) 0.034(2) 0.0001(18) 0.0154(18) 0.0064(18) C11 0.040(2) 0.046(3) 0.048(3) -0.003(2) 0.016(2) -0.006(2) C12 0.062(3) 0.044(3) 0.067(4) -0.001(3) 0.038(3) -0.002(2) C13 0.074(4) 0.055(3) 0.053(3) 0.008(3) 0.033(3) 0.010(3) C14 0.066(4) 0.098(5) 0.030(3) -0.001(3) 0.015(2) 0.014(3) C15 0.040(3) 0.071(4) 0.038(2) -0.007(2) 0.013(2) -0.001(2) C16 0.031(2) 0.029(2) 0.029(2) 0.0024(16) 0.0070(17) -0.0014(17) C17 0.034(2) 0.045(3) 0.039(2) 0.006(2) 0.0027(19) 0.0018(19) C18 0.035(2) 0.048(3) 0.046(3) 0.008(2) 0.010(2) 0.013(2) C19 0.039(2) 0.045(3) 0.041(2) 0.001(2) 0.015(2) 0.008(2) C20 0.035(2) 0.034(2) 0.033(2) -0.0022(18) 0.0105(17) 0.0002(17) C21 0.0238(19) 0.032(2) 0.031(2) 0.0035(16) 0.0070(16) 0.0028(15) C22 0.031(2) 0.030(2) 0.026(2) 0.0020(16) 0.0017(16) -0.0013(16) C23 0.032(2) 0.044(3) 0.036(2) -0.005(2) 0.0015(17) 0.010(2) C24 0.029(3) 0.113(5) 0.049(3) 0.015(3) 0.009(2) 0.013(3) C25 0.031(2) 0.037(3) 0.038(2) -0.001(2) 0.0048(18) 0.0127(19) C26 0.048(3) 0.044(3) 0.044(3) 0.008(2) 0.001(2) 0.007(2) C27 0.061(3) 0.064(4) 0.057(3) 0.020(3) 0.015(3) 0.015(3) C28 0.067(3) 0.072(4) 0.043(3) 0.010(3) 0.002(3) 0.032(3) C29 0.065(4) 0.066(4) 0.047(3) -0.006(3) -0.014(3) 0.011(3) C30 0.052(3) 0.049(3) 0.043(3) -0.004(2) -0.006(2) 0.003(2) C31 0.043(3) 0.051(3) 0.039(2) 0.005(2) 0.011(2) -0.004(2) C32 0.062(4) 0.091(5) 0.069(4) 0.028(4) 0.033(3) 0.039(3) C33 0.067(3) 0.050(3) 0.047(3) 0.008(2) 0.016(3) 0.003(3) C34 0.048(3) 0.074(4) 0.054(3) -0.026(3) 0.010(2) -0.004(3) C35 0.145(7) 0.044(3) 0.060(4) -0.003(3) -0.015(4) -0.008(4) C36 0.143(6) 0.058(4) 0.041(3) -0.009(3) -0.005(3) 0.013(4) C37 0.027(2) 0.033(2) 0.033(2) 0.0091(17) 0.0036(16) 0.0059(16) C38 0.026(2) 0.048(3) 0.034(2) 0.008(2) 0.0074(17) 0.0033(18) C39 0.036(2) 0.038(3) 0.037(2) 0.005(2) 0.0020(18) -0.010(2) C40 0.045(3) 0.034(2) 0.037(2) -0.0009(19) 0.007(2) -0.0003(19) C41 0.040(2) 0.036(3) 0.034(2) -0.0049(18) 0.0072(18) 0.0012(19) C42 0.029(2) 0.040(2) 0.0229(19) 0.0020(17) 0.0036(16) 0.0005(17) C43 0.031(2) 0.034(2) 0.031(2) -0.0013(18) 0.0068(17) 0.0051(18) C44 0.036(2) 0.043(3) 0.035(2) -0.0040(19) 0.0117(19) -0.0056(19) C45 0.030(2) 0.081(4) 0.043(3) -0.013(3) 0.010(2) -0.005(2) C46 0.035(2) 0.045(3) 0.036(2) 0.000(2) 0.0146(19) -0.0017(19) C47 0.046(3) 0.064(3) 0.049(3) -0.002(3) 0.020(2) 0.007(2) C48 0.074(4) 0.059(4) 0.069(4) 0.002(3) 0.042(3) 0.014(3) C49 0.082(4) 0.075(4) 0.055(3) -0.016(3) 0.047(3) -0.010(3) C50 0.071(4) 0.104(5) 0.033(3) -0.002(3) 0.021(3) -0.013(4) C51 0.043(3) 0.088(4) 0.040(3) 0.005(3) 0.018(2) 0.003(3) C52 0.029(2) 0.038(2) 0.028(2) -0.0042(18) 0.0043(17) 0.0007(18) C53 0.030(2) 0.053(3) 0.037(2) -0.011(2) 0.0025(18) -0.0065(19) C54 0.038(2) 0.051(3) 0.054(3) -0.011(2) 0.013(2) -0.013(2) C55 0.044(3) 0.045(3) 0.044(3) -0.003(2) 0.018(2) -0.012(2) C56 0.038(2) 0.044(3) 0.033(2) -0.0021(19) 0.0111(18) -0.0028(19) C57 0.030(2) 0.032(2) 0.029(2) -0.0054(17) 0.0092(17) -0.0023(16) C58 0.033(2) 0.032(2) 0.027(2) 0.0015(17) 0.0044(17) 0.0002(17) C59 0.028(2) 0.065(3) 0.052(3) 0.001(3) 0.011(2) -0.002(2) C60 0.029(2) 0.038(2) 0.035(2) 0.0083(19) 0.0025(17) -0.0047(18) C61 0.037(2) 0.035(3) 0.040(2) 0.003(2) -0.0048(19) -0.0124(19) C62 0.049(3) 0.053(3) 0.042(3) -0.007(2) -0.004(2) 0.003(2) C63 0.055(3) 0.077(4) 0.052(3) -0.018(3) 0.005(3) -0.003(3) C64 0.079(4) 0.067(4) 0.034(2) -0.007(3) -0.002(2) -0.029(3) C65 0.079(4) 0.056(3) 0.050(3) 0.004(3) -0.019(3) -0.007(3) C66 0.058(3) 0.044(3) 0.049(3) 0.002(2) -0.007(2) 0.001(2) C67 0.042(3) 0.044(3) 0.036(2) -0.001(2) 0.010(2) 0.010(2) C68 0.099(5) 0.048(3) 0.046(3) -0.006(3) 0.021(3) -0.017(3) C69 0.048(3) 0.053(3) 0.045(2) 0.005(2) 0.008(2) -0.004(2) C70 0.040(2) 0.046(3) 0.035(2) 0.009(2) 0.0017(19) 0.013(2) C71 0.077(4) 0.056(3) 0.052(3) 0.014(3) -0.019(3) -0.016(3) C72 0.064(3) 0.050(3) 0.054(3) 0.021(3) 0.001(3) 0.006(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 Zr1 O4 1.918(3) . ? Zr1 O3 1.934(3) . ? Zr1 O1 2.044(3) . ? Zr1 O2 2.054(3) . ? Zr1 N2 2.432(3) . ? Zr1 N1 2.457(4) . ? O1 C1 1.339(5) . ? N1 C7 1.281(6) . ? N1 C8 1.493(5) . ? C1 C6 1.401(6) . ? C1 C2 1.406(6) . ? Zr2 O8 1.910(3) . ? Zr2 O7 1.937(3) . ? Zr2 O6 2.044(3) . ? Zr2 O5 2.072(3) . ? Zr2 N4 2.426(3) . ? Zr2 N3 2.448(4) . ? O2 C16 1.310(5) . ? N2 C22 1.283(5) . ? N2 C23 1.508(5) . ? C2 C3 1.385(7) . ? C2 H2 0.9500 . ? O3 C31 1.408(6) . ? N3 C43 1.289(6) . ? N3 C44 1.492(5) . ? C3 C4 1.385(7) . ? C3 H3 0.9500 . ? O4 C34 1.408(6) . ? N4 C58 1.288(5) . ? N4 C60 1.502(5) . ? C4 C5 1.376(6) . ? C4 H4 0.9500 . ? O5 C37 1.336(5) . ? C5 C6 1.417(6) . ? C5 H5 0.9500 . ? O6 C52 1.331(5) . ? C6 C7 1.451(6) . ? O7 C67 1.407(5) . ? C7 H7 0.87(5) . ? O8 C70 1.423(5) . ? C8 C10 1.518(6) . ? C8 C9 1.524(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.383(6) . ? C10 C15 1.385(6) . ? C11 C12 1.395(7) . ? C11 H11 0.9500 . ? C12 C13 1.366(8) . ? C12 H12 0.9500 . ? C13 C14 1.371(9) . ? C13 H13 0.9500 . ? C14 C15 1.405(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.413(6) . ? C16 C21 1.416(5) . ? C17 C18 1.392(7) . ? C17 H17 0.9500 . ? C18 C19 1.382(7) . ? C18 H18 0.9500 . ? C19 C20 1.380(6) . ? C19 H19 0.9500 . ? C20 C21 1.403(6) . ? C20 H20 0.9500 . ? C21 C22 1.455(5) . ? C22 H22 0.96(5) . ? C23 C24 1.511(7) . ? C23 C25 1.516(6) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.372(7) . ? C25 C26 1.376(7) . ? C26 C27 1.395(7) . ? C26 H26 0.9500 . ? C27 C28 1.379(9) . ? C27 H27 0.9500 . ? C28 C29 1.372(9) . ? C28 H28 0.9500 . ? C29 C30 1.393(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C33 1.505(7) . ? C31 C32 1.523(8) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.455(9) . ? C34 C36 1.480(9) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.406(6) . ? C37 C42 1.407(6) . ? C38 C39 1.383(7) . ? C38 H38 0.9500 . ? C39 C40 1.393(7) . ? C39 H39 0.9500 . ? C40 C41 1.378(6) . ? C40 H40 0.9500 . ? C41 C42 1.413(6) . ? C41 H41 0.9500 . ? C42 C43 1.444(6) . ? C43 H43 0.92(5) . ? C44 C46 1.525(6) . ? C44 C45 1.525(6) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.373(7) . ? C46 C51 1.388(7) . ? C47 C48 1.392(8) . ? C47 H47 0.9500 . ? C48 C49 1.366(9) . ? C48 H48 0.9500 . ? C49 C50 1.365(9) . ? C49 H49 0.9500 . ? C50 C51 1.394(8) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.392(6) . ? C52 C57 1.405(6) . ? C53 C54 1.388(7) . ? C53 H53 0.9500 . ? C54 C55 1.393(7) . ? C54 H54 0.9500 . ? C55 C56 1.374(6) . ? C55 H55 0.9500 . ? C56 C57 1.416(6) . ? C56 H56 0.9500 . ? C57 C58 1.450(6) . ? C58 H58 0.93(5) . ? C59 C60 1.522(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.528(6) . ? C60 H60 1.0000 . ? C61 C66 1.372(7) . ? C61 C62 1.384(7) . ? C62 C63 1.393(7) . ? C62 H62 0.9500 . ? C63 C64 1.372(8) . ? C63 H63 0.9500 . ? C64 C65 1.385(9) . ? C64 H64 0.9500 . ? C65 C66 1.397(8) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.505(7) . ? C67 C69 1.518(7) . ? C67 H67 1.0000 . ? 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 C72 1.505(7) . ? C70 C71 1.510(7) . ? C70 H70 1.0000 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zr1 O3 102.66(14) . . ? O4 Zr1 O1 97.47(15) . . ? O3 Zr1 O1 95.44(13) . . ? O4 Zr1 O2 95.19(14) . . ? O3 Zr1 O2 98.94(14) . . ? O1 Zr1 O2 158.27(12) . . ? O4 Zr1 N2 167.24(14) . . ? O3 Zr1 N2 88.89(12) . . ? O1 Zr1 N2 86.68(12) . . ? O2 Zr1 N2 77.44(11) . . ? O4 Zr1 N1 89.45(13) . . ? O3 Zr1 N1 166.47(13) . . ? O1 Zr1 N1 76.79(12) . . ? O2 Zr1 N1 85.76(12) . . ? N2 Zr1 N1 79.71(11) . . ? C1 O1 Zr1 138.6(3) . . ? C7 N1 C8 117.0(4) . . ? C7 N1 Zr1 124.9(3) . . ? C8 N1 Zr1 117.5(3) . . ? O1 C1 C6 121.2(4) . . ? O1 C1 C2 119.5(4) . . ? C6 C1 C2 119.2(4) . . ? O8 Zr2 O7 102.68(13) . . ? O8 Zr2 O6 96.30(13) . . ? O7 Zr2 O6 99.20(14) . . ? O8 Zr2 O5 96.66(14) . . ? O7 Zr2 O5 96.07(13) . . ? O6 Zr2 O5 157.26(12) . . ? O8 Zr2 N4 168.50(13) . . ? O7 Zr2 N4 87.73(12) . . ? O6 Zr2 N4 76.98(11) . . ? O5 Zr2 N4 86.94(12) . . ? O8 Zr2 N3 86.57(13) . . ? O7 Zr2 N3 168.97(13) . . ? O6 Zr2 N3 85.54(12) . . ? O5 Zr2 N3 76.68(12) . . ? N4 Zr2 N3 83.63(11) . . ? C16 O2 Zr1 143.6(3) . . ? C22 N2 C23 116.7(3) . . ? C22 N2 Zr1 125.8(3) . . ? C23 N2 Zr1 117.2(2) . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C31 O3 Zr1 157.2(3) . . ? C43 N3 C44 116.5(4) . . ? C43 N3 Zr2 124.7(3) . . ? C44 N3 Zr2 117.6(3) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C34 O4 Zr1 171.7(4) . . ? C58 N4 C60 115.6(3) . . ? C58 N4 Zr2 126.6(3) . . ? C60 N4 Zr2 117.3(2) . . ? C5 C4 C3 119.0(5) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C37 O5 Zr2 133.8(3) . . ? C4 C5 C6 121.6(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C52 O6 Zr2 143.9(3) . . ? C1 C6 C5 118.7(4) . . ? C1 C6 C7 123.8(4) . . ? C5 C6 C7 117.5(4) . . ? C67 O7 Zr2 151.2(3) . . ? N1 C7 C6 127.6(4) . . ? N1 C7 H7 125(3) . . ? C6 C7 H7 107(3) . . ? C70 O8 Zr2 170.5(3) . . ? N1 C8 C10 114.8(4) . . ? N1 C8 C9 106.8(3) . . ? C10 C8 C9 114.2(4) . . ? N1 C8 H8 106.8 . . ? C10 C8 H8 106.8 . . ? C9 C8 H8 106.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.9(4) . . ? C11 C10 C8 123.3(4) . . ? C15 C10 C8 118.9(4) . . ? C10 C11 C12 121.7(5) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.4(5) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.8(5) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 120.7(5) . . ? C10 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? O2 C16 C17 119.9(4) . . ? O2 C16 C21 121.5(4) . . ? C17 C16 C21 118.6(4) . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 120.5(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.6(4) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 121.7(4) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C20 C21 C16 118.9(4) . . ? C20 C21 C22 117.8(4) . . ? C16 C21 C22 123.3(4) . . ? N2 C22 C21 128.3(4) . . ? N2 C22 H22 114(3) . . ? C21 C22 H22 117(3) . . ? N2 C23 C24 107.3(4) . . ? N2 C23 C25 113.0(3) . . ? C24 C23 C25 114.4(4) . . ? N2 C23 H23 107.3 . . ? C24 C23 H23 107.3 . . ? C25 C23 H23 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 118.1(4) . . ? C30 C25 C23 123.7(5) . . ? C26 C25 C23 118.2(4) . . ? C25 C26 C27 121.1(5) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 119.8(6) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 119.8(6) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C25 C30 C29 121.5(6) . . ? C25 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? O3 C31 C33 110.3(4) . . ? O3 C31 C32 108.5(4) . . ? C33 C31 C32 112.0(4) . . ? O3 C31 H31 108.7 . . ? C33 C31 H31 108.7 . . ? C32 C31 H31 108.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O4 C34 C35 108.3(5) . . ? O4 C34 C36 110.9(5) . . ? C35 C34 C36 113.0(6) . . ? O4 C34 H34 108.2 . . ? C35 C34 H34 108.2 . . ? C36 C34 H34 108.2 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O5 C37 C38 119.5(4) . . ? O5 C37 C42 121.3(4) . . ? C38 C37 C42 119.2(4) . . ? C39 C38 C37 120.5(4) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C38 C39 C40 121.0(4) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 118.9(4) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 121.7(4) . . ? C40 C41 H41 119.1 . . ? C42 C41 H41 119.1 . . ? C37 C42 C41 118.7(4) . . ? C37 C42 C43 124.6(4) . . ? C41 C42 C43 116.6(4) . . ? N3 C43 C42 126.2(4) . . ? N3 C43 H43 124(3) . . ? C42 C43 H43 110(3) . . ? N3 C44 C46 115.1(4) . . ? N3 C44 C45 107.4(3) . . ? C46 C44 C45 113.7(4) . . ? N3 C44 H44 106.7 . . ? C46 C44 H44 106.7 . . ? C45 C44 H44 106.7 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 118.4(5) . . ? C47 C46 C44 123.1(4) . . ? C51 C46 C44 118.5(4) . . ? C46 C47 C48 121.9(5) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C49 C48 C47 118.8(6) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C50 C49 C48 120.7(5) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 120.3(5) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C46 C51 C50 119.9(5) . . ? C46 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? O6 C52 C53 120.2(4) . . ? O6 C52 C57 121.0(4) . . ? C53 C52 C57 118.7(4) . . ? C54 C53 C52 120.8(4) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C55 121.1(4) . . ? C53 C54 H54 119.5 . . ? C55 C54 H54 119.5 . . ? C56 C55 C54 118.7(4) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? C55 C56 C57 121.3(4) . . ? C55 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C52 C57 C56 119.4(4) . . ? C52 C57 C58 123.7(4) . . ? C56 C57 C58 116.8(4) . . ? N4 C58 C57 127.5(4) . . ? N4 C58 H58 119(3) . . ? C57 C58 H58 114(3) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N4 C60 C59 108.1(4) . . ? N4 C60 C61 112.2(3) . . ? C59 C60 C61 114.5(4) . . ? N4 C60 H60 107.2 . . ? C59 C60 H60 107.2 . . ? C61 C60 H60 107.2 . . ? C66 C61 C62 118.0(5) . . ? C66 C61 C60 123.2(5) . . ? C62 C61 C60 118.7(4) . . ? C61 C62 C63 121.6(5) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C64 C63 C62 119.5(6) . . ? C64 C63 H63 120.3 . . ? C62 C63 H63 120.3 . . ? C63 C64 C65 119.9(5) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C64 C65 C66 119.7(5) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C61 C66 C65 121.2(6) . . ? C61 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? O7 C67 C68 110.3(4) . . ? O7 C67 C69 110.0(4) . . ? C68 C67 C69 109.8(4) . . ? O7 C67 H67 108.9 . . ? C68 C67 H67 108.9 . . ? C69 C67 H67 108.9 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O8 C70 C72 110.5(4) . . ? O8 C70 C71 108.1(4) . . ? C72 C70 C71 111.4(4) . . ? O8 C70 H70 109.0 . . ? C72 C70 H70 109.0 . . ? C71 C70 H70 109.0 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.752 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.086 #===END data_R3ZrOiPr2 _database_code_depnum_ccdc_archive 'CCDC 665068' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 N2 O4 Zr' _chemical_formula_sum 'C38 H46 N2 O4 Zr' _chemical_formula_weight 685.99 _chemical_absolute_configuration ad 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_int_tables_number 5 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 18.8930(4) _cell_length_b 9.5550(2) _cell_length_c 11.1310(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.8440(10) _cell_angle_gamma 90.00 _cell_volume 1725.20(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22020 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.360 _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_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Nonius Kappa CCD' _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 17062 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3924 _reflns_number_gt 3894 _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^)+(0.0415P)^2^+0.6809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 3924 _refine_ls_number_parameters 212 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.0000 0.133000(9) 0.0000 0.02288(8) Uani 1 2 d S . . O1 O 0.10557(8) 0.17651(14) -0.00091(14) 0.0264(3) Uani 1 1 d . . . N1 N 0.06253(11) 0.3178(2) 0.17434(19) 0.0216(3) Uani 1 1 d . . . C1 C 0.17665(12) 0.2447(2) 0.06848(19) 0.0229(4) Uani 1 1 d . . . O2 O 0.04446(11) 0.00230(18) 0.15467(17) 0.0310(4) Uani 1 1 d . . . C2 C 0.19312(11) 0.3386(2) 0.17751(19) 0.0228(4) Uani 1 1 d . . . C3 C 0.26994(12) 0.4083(2) 0.2477(2) 0.0252(4) Uani 1 1 d . . . H3 H 0.2806 0.4719 0.3207 0.030 Uiso 1 1 calc R . . C4 C 0.33005(12) 0.3874(2) 0.2140(2) 0.0278(4) Uani 1 1 d . . . C5 C 0.31193(12) 0.2944(2) 0.1050(2) 0.0294(4) Uani 1 1 d . . . H5 H 0.3520 0.2787 0.0791 0.035 Uiso 1 1 calc R . . C6 C 0.23751(13) 0.2247(2) 0.0338(2) 0.0280(4) Uani 1 1 d . . . H6 H 0.2274 0.1623 -0.0398 0.034 Uiso 1 1 calc R . . C7 C 0.41357(13) 0.4569(3) 0.2945(3) 0.0376(5) Uani 1 1 d . . . H7A H 0.4141 0.5226 0.3625 0.056 Uiso 1 1 calc R . . H7B H 0.4246 0.5077 0.2293 0.056 Uiso 1 1 calc R . . H7C H 0.4561 0.3855 0.3437 0.056 Uiso 1 1 calc R . . C8 C 0.13538(12) 0.3681(2) 0.2237(2) 0.0238(4) Uani 1 1 d . . . H8 H 0.1583(16) 0.437(3) 0.301(3) 0.033(6) Uiso 1 1 d . . . C9 C 0.01416(12) 0.3748(2) 0.2370(2) 0.0235(4) Uani 1 1 d . . . H9 H -0.0272 0.3016 0.2235 0.028 Uiso 1 1 calc R . . C10 C -0.03412(13) 0.5009(2) 0.1505(2) 0.0299(4) Uani 1 1 d . . . H10A H 0.0043 0.5740 0.1581 0.045 Uiso 1 1 calc R . . H10B H -0.0689 0.5368 0.1853 0.045 Uiso 1 1 calc R . . H10C H -0.0689 0.4731 0.0523 0.045 Uiso 1 1 calc R . . C11 C 0.06597(12) 0.4031(2) 0.3935(2) 0.0239(4) Uani 1 1 d . . . C12 C 0.08608(18) 0.5357(3) 0.4501(3) 0.0410(6) Uani 1 1 d . . . H12 H 0.0672 0.6146 0.3897 0.049 Uiso 1 1 calc R . . C13 C 0.13349(19) 0.5560(3) 0.5938(3) 0.0484(7) Uani 1 1 d . . . H13 H 0.1466 0.6483 0.6305 0.058 Uiso 1 1 calc R . . C14 C 0.16156(14) 0.4431(3) 0.6835(2) 0.0370(5) Uani 1 1 d . . . H14 H 0.1937 0.4568 0.7818 0.044 Uiso 1 1 calc R . . C15 C 0.14236(17) 0.3103(3) 0.6284(3) 0.0441(6) Uani 1 1 d . . . H15 H 0.1619 0.2315 0.6890 0.053 Uiso 1 1 calc R . . C16 C 0.09464(16) 0.2909(2) 0.4850(2) 0.0393(5) Uani 1 1 d . . . H16 H 0.0813 0.1985 0.4486 0.047 Uiso 1 1 calc R . . C17 C 0.08504(15) -0.1189(3) 0.2303(2) 0.0345(5) Uani 1 1 d . . . H17 H 0.0433 -0.1798 0.2344 0.041 Uiso 1 1 calc R . . C18 C 0.1495(2) -0.0820(4) 0.3775(3) 0.0677(10) Uani 1 1 d . . . H18A H 0.1855 -0.0089 0.3763 0.102 Uiso 1 1 calc R . . H18B H 0.1824 -0.1652 0.4249 0.102 Uiso 1 1 calc R . . H18C H 0.1228 -0.0478 0.4276 0.102 Uiso 1 1 calc R . . C19 C 0.12053(15) -0.1995(3) 0.1578(3) 0.0419(6) Uani 1 1 d . . . H19A H 0.0760 -0.2289 0.0652 0.063 Uiso 1 1 calc R . . H19B H 0.1494 -0.2823 0.2134 0.063 Uiso 1 1 calc R . . H19C H 0.1594 -0.1401 0.1474 0.063 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 0.02616(12) 0.02000(11) 0.02042(11) 0.000 0.01048(8) 0.000 O1 0.0259(6) 0.0272(7) 0.0252(7) -0.0050(5) 0.0125(5) 0.0005(5) N1 0.0246(8) 0.0198(9) 0.0218(8) -0.0007(7) 0.0129(7) 0.0015(7) C1 0.0240(9) 0.0241(9) 0.0193(9) 0.0034(7) 0.0103(7) 0.0035(7) O2 0.0349(8) 0.0262(9) 0.0285(8) 0.0066(7) 0.0139(7) 0.0038(7) C2 0.0229(9) 0.0223(9) 0.0219(9) 0.0008(7) 0.0106(7) 0.0014(7) C3 0.0255(9) 0.0256(9) 0.0237(9) 0.0015(7) 0.0121(7) 0.0012(8) C4 0.0258(9) 0.0288(10) 0.0295(10) 0.0085(8) 0.0146(8) 0.0038(8) C5 0.0276(9) 0.0359(11) 0.0296(10) 0.0088(8) 0.0184(8) 0.0090(8) C6 0.0305(10) 0.0313(10) 0.0234(9) 0.0008(8) 0.0147(8) 0.0057(8) C7 0.0280(10) 0.0454(13) 0.0408(12) 0.0006(10) 0.0186(10) -0.0018(10) C8 0.0252(9) 0.0237(9) 0.0226(9) -0.0012(7) 0.0124(7) 0.0002(7) C9 0.0238(9) 0.0228(9) 0.0259(9) -0.0033(7) 0.0143(8) -0.0007(7) C10 0.0304(10) 0.0293(10) 0.0302(10) -0.0023(8) 0.0157(8) 0.0032(8) C11 0.0255(9) 0.0259(9) 0.0239(9) -0.0038(7) 0.0153(7) -0.0019(7) C12 0.0614(15) 0.0245(10) 0.0324(12) -0.0041(9) 0.0206(11) 0.0007(11) C13 0.0679(17) 0.0335(14) 0.0355(13) -0.0118(10) 0.0206(12) 0.0012(12) C14 0.0338(11) 0.0498(14) 0.0260(10) -0.0086(10) 0.0144(9) -0.0011(10) C15 0.0526(14) 0.0392(13) 0.0294(11) 0.0054(10) 0.0130(10) 0.0007(11) C16 0.0504(13) 0.0255(11) 0.0318(11) -0.0013(8) 0.0137(10) -0.0049(10) C17 0.0388(12) 0.0332(12) 0.0337(11) 0.0113(9) 0.0202(10) 0.0122(10) C18 0.0629(19) 0.088(3) 0.0294(13) -0.0016(14) 0.0074(12) 0.0339(18) C19 0.0382(12) 0.0386(13) 0.0493(14) -0.0012(11) 0.0228(11) 0.0072(10) _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 O2 1.9355(16) 2 ? Zr1 O2 1.9355(16) . ? Zr1 O1 2.0425(14) . ? Zr1 O1 2.0425(14) 2 ? Zr1 N1 2.4350(19) . ? Zr1 N1 2.4350(19) 2 ? O1 C1 1.327(2) . ? N1 C8 1.285(3) . ? N1 C9 1.507(2) . ? C1 C6 1.401(3) . ? C1 C2 1.410(3) . ? O2 C17 1.405(3) . ? C2 C3 1.413(3) . ? C2 C8 1.453(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.398(3) . ? C4 C7 1.511(3) . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.99(3) . ? C9 C10 1.520(3) . ? C9 C11 1.522(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.379(3) . ? C11 C16 1.383(3) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.378(4) . ? C13 H13 0.9500 . ? C14 C15 1.374(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.498(4) . ? C17 C19 1.501(3) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 O2 Zr1 O2 99.63(10) 2 . ? O2 Zr1 O1 96.11(6) 2 . ? O2 Zr1 O1 98.98(7) . . ? O2 Zr1 O1 98.98(7) 2 2 ? O2 Zr1 O1 96.11(6) . 2 ? O1 Zr1 O1 156.51(8) . 2 ? O2 Zr1 N1 171.41(7) 2 . ? O2 Zr1 N1 86.97(6) . . ? O1 Zr1 N1 77.31(6) . . ? O1 Zr1 N1 85.67(6) 2 . ? O2 Zr1 N1 86.97(6) 2 2 ? O2 Zr1 N1 171.41(7) . 2 ? O1 Zr1 N1 85.67(6) . 2 ? O1 Zr1 N1 77.31(6) 2 2 ? N1 Zr1 N1 87.03(8) . 2 ? C1 O1 Zr1 142.79(12) . . ? C8 N1 C9 115.93(17) . . ? C8 N1 Zr1 126.01(14) . . ? C9 N1 Zr1 117.98(12) . . ? O1 C1 C6 120.06(18) . . ? O1 C1 C2 121.64(17) . . ? C6 C1 C2 118.30(18) . . ? C17 O2 Zr1 156.81(16) . . ? C1 C2 C3 119.11(17) . . ? C1 C2 C8 123.65(18) . . ? C3 C2 C8 117.24(17) . . ? C4 C3 C2 122.47(19) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 117.26(19) . . ? C3 C4 C7 122.0(2) . . ? C5 C4 C7 120.65(19) . . ? C6 C5 C4 121.93(18) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 120.93(19) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C2 127.57(19) . . ? N1 C8 H8 121.2(15) . . ? C2 C8 H8 111.2(15) . . ? N1 C9 C10 107.62(16) . . ? N1 C9 C11 114.01(16) . . ? C10 C9 C11 114.13(16) . . ? N1 C9 H9 106.9 . . ? C10 C9 H9 106.9 . . ? C11 C9 H9 106.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 117.6(2) . . ? C12 C11 C9 123.46(19) . . ? C16 C11 C9 118.94(18) . . ? C11 C12 C13 121.3(2) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.0(2) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 121.5(2) . . ? C11 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O2 C17 C18 110.5(2) . . ? O2 C17 C19 110.95(19) . . ? C18 C17 C19 111.9(2) . . ? O2 C17 H17 107.8 . . ? C18 C17 H17 107.8 . . ? C19 C17 H17 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.376 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.072 #===END