# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hiroyuki Kawaguchi' _publ_contact_author_email HKAWA@CHEM.TITECH.AC.JP _publ_section_title ; Synthesis and structures of zirconium(IV) complexes supported by 2,6-di-adamantylaryloxide ligands and formation of arene-bridged dizirconium complexes with an inverse sandwich structure ; loop_ _publ_author_name 'Hiroyuki Kawaguchi' 'Yutaka Ishida' 'Tsukasa Matsuo' 'Takahito Watanabe' # Attachment 'KawaguchiCIF-B911082H.txt' data_[Ar(Me)O]Li(THF)2 _database_code_depnum_ccdc_archive 'CCDC 735063' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H51 Li O3' _chemical_formula_sum 'C35 H51 Li O3' _chemical_formula_weight 526.70 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' Li Li -0.0003 0.0001 '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 18.930(15) _cell_length_b 12.889(8) _cell_length_c 12.831(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.611(12) _cell_angle_gamma 90.00 _cell_volume 3015(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3821 _cell_measurement_theta_min 3.1147 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9722 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 11462 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3395 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0805P)^2^+2.6799P] 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 3395 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.2075 _refine_ls_wR_factor_gt 0.2017 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _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 C1 C 0.5000 -0.10510(18) 0.7500 0.0314(5) Uani 1 2 d S . . C2 C 0.56768(9) -0.16237(14) 0.77820(16) 0.0373(4) Uani 1 1 d . . . C3 C 0.56500(11) -0.26972(16) 0.7781(2) 0.0651(8) Uani 1 1 d . . . H1 H 0.6099 -0.3071 0.7983 0.078 Uiso 1 1 calc R . . C4 C 0.5000 -0.3252(2) 0.7500 0.0888(16) Uani 1 2 d S . . C5 C 0.64169(9) -0.10589(13) 0.80813(14) 0.0325(4) Uani 1 1 d . . . C6 C 0.64916(9) -0.03754(14) 0.90904(14) 0.0349(4) Uani 1 1 d . . . H2 H 0.6077 0.0120 0.8955 0.042 Uiso 1 1 calc R . . H3 H 0.6469 -0.0818 0.9711 0.042 Uiso 1 1 calc R . . C7 C 0.70745(10) -0.18147(16) 0.83535(18) 0.0459(5) Uani 1 1 d . . . H4 H 0.7045 -0.2261 0.8969 0.055 Uiso 1 1 calc R . . H5 H 0.7051 -0.2269 0.7723 0.055 Uiso 1 1 calc R . . C8 C 0.65001(10) -0.03787(16) 0.71274(15) 0.0386(4) Uani 1 1 d . . . H6 H 0.6482 -0.0825 0.6493 0.046 Uiso 1 1 calc R . . H7 H 0.6087 0.0118 0.6925 0.046 Uiso 1 1 calc R . . C9 C 0.72185(10) 0.02275(16) 0.93726(15) 0.0415(5) Uani 1 1 d . . . H8 H 0.7247 0.0679 1.0016 0.050 Uiso 1 1 calc R . . C10 C 0.78076(10) -0.12278(18) 0.86477(19) 0.0508(6) Uani 1 1 d . . . H9 H 0.8220 -0.1739 0.8818 0.061 Uiso 1 1 calc R . . C11 C 0.72267(11) 0.02214(18) 0.74303(16) 0.0470(5) Uani 1 1 d . . . H10 H 0.7260 0.0668 0.6808 0.056 Uiso 1 1 calc R . . C12 C 0.78568(11) -0.05455(18) 0.96312(17) 0.0498(6) Uani 1 1 d . . . H11 H 0.8329 -0.0166 0.9821 0.060 Uiso 1 1 calc R . . H12 H 0.7834 -0.0980 1.0257 0.060 Uiso 1 1 calc R . . C13 C 0.78667(11) -0.0547(2) 0.76943(19) 0.0587(6) Uani 1 1 d . . . H13 H 0.8338 -0.0165 0.7886 0.070 Uiso 1 1 calc R . . H14 H 0.7851 -0.0986 0.7055 0.070 Uiso 1 1 calc R . . C14 C 0.72616(11) 0.08988(17) 0.84104(16) 0.0461(5) Uani 1 1 d . . . H15 H 0.6849 0.1399 0.8241 0.055 Uiso 1 1 calc R . . H16 H 0.7726 0.1297 0.8596 0.055 Uiso 1 1 calc R . . C15 C 0.5000 -0.4432(3) 0.7500 0.149(3) Uani 1 2 d S . . H17 H 0.5507 -0.4685 0.7719 0.223 Uiso 0.50 1 calc PR . . H18 H 0.4758 -0.4685 0.6771 0.223 Uiso 0.50 1 calc PR . . H19 H 0.4736 -0.4685 0.8010 0.223 Uiso 0.50 1 calc PR . . O1 O 0.5000 -0.00417(12) 0.7500 0.0340(4) Uani 1 2 d S . . Li1 Li 0.4697(4) 0.1221(5) 0.7388(6) 0.0479(16) Uani 0.50 1 d P . . O2 O 0.4712(2) 0.2112(2) 0.8584(4) 0.0593(9) Uani 0.50 1 d P . 1 C16 C 0.4846(3) 0.3193(4) 0.8576(6) 0.0776(18) Uani 0.50 1 d P A 1 H20 H 0.4466 0.3577 0.8819 0.093 Uiso 0.50 1 calc PR A 1 H21 H 0.4831 0.3424 0.7835 0.093 Uiso 0.50 1 calc PR A 1 C17 C 0.5573(5) 0.3396(6) 0.9312(8) 0.104(3) Uani 0.50 1 d P A 1 H22 H 0.5543 0.3941 0.9842 0.125 Uiso 0.50 1 calc PR A 1 H23 H 0.5919 0.3626 0.8902 0.125 Uiso 0.50 1 calc PR A 1 C18 C 0.5823(4) 0.2380(5) 0.9883(6) 0.0746(18) Uani 0.50 1 d P A 1 H24 H 0.6032 0.2483 1.0671 0.090 Uiso 0.50 1 calc PR A 1 H25 H 0.6190 0.2031 0.9581 0.090 Uiso 0.50 1 calc PR A 1 C19 C 0.5111(4) 0.1771(6) 0.9644(6) 0.0565(17) Uani 0.50 1 d P A 1 H26 H 0.5206 0.1016 0.9650 0.068 Uiso 0.50 1 calc PR A 1 H27 H 0.4836 0.1929 1.0182 0.068 Uiso 0.50 1 calc PR A 1 O3 O 0.45983(19) 0.2051(3) 0.6114(3) 0.0654(10) Uani 0.50 1 d P . 2 C20 C 0.5202(5) 0.2021(9) 0.5593(11) 0.088(3) Uani 0.50 1 d P . 2 H28 H 0.5673 0.1850 0.6122 0.105 Uiso 0.50 1 calc PR . 2 H29 H 0.5104 0.1506 0.4998 0.105 Uiso 0.50 1 calc PR . 2 C21 C 0.5210(3) 0.3079(6) 0.5177(5) 0.083(2) Uani 0.50 1 d P B 2 H30 H 0.5431 0.3094 0.4560 0.100 Uiso 0.50 1 calc PR B 2 H31 H 0.5489 0.3551 0.5750 0.100 Uiso 0.50 1 calc PR B 2 C22 C 0.4426(3) 0.3376(5) 0.4828(6) 0.0703(15) Uani 0.50 1 d P B 2 H32 H 0.4209 0.3190 0.4059 0.084 Uiso 0.50 1 calc PR B 2 H33 H 0.4368 0.4131 0.4915 0.084 Uiso 0.50 1 calc PR B 2 C23 C 0.4066(3) 0.2785(5) 0.5538(5) 0.0545(12) Uani 0.50 1 d P B 2 H34 H 0.3918 0.3258 0.6049 0.065 Uiso 0.50 1 calc PR B 2 H35 H 0.3624 0.2423 0.5100 0.065 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0283(12) 0.0258(11) 0.0376(12) 0.000 0.0046(9) 0.000 C2 0.0261(8) 0.0293(9) 0.0514(11) -0.0002(7) 0.0018(7) 0.0012(6) C3 0.0294(10) 0.0301(10) 0.121(2) -0.0011(11) -0.0043(12) 0.0059(8) C4 0.0393(17) 0.0241(14) 0.181(5) 0.000 -0.008(2) 0.000 C5 0.0235(8) 0.0334(9) 0.0381(9) 0.0010(7) 0.0039(6) 0.0003(6) C6 0.0310(9) 0.0407(10) 0.0308(8) 0.0047(7) 0.0049(7) -0.0038(7) C7 0.0275(9) 0.0441(11) 0.0605(12) -0.0003(9) 0.0021(8) 0.0062(8) C8 0.0318(9) 0.0511(11) 0.0313(9) -0.0004(8) 0.0056(7) 0.0009(8) C9 0.0376(10) 0.0494(11) 0.0331(9) -0.0001(8) 0.0022(7) -0.0104(8) C10 0.0256(9) 0.0618(13) 0.0610(13) 0.0065(10) 0.0048(8) 0.0058(9) C11 0.0361(10) 0.0686(14) 0.0370(10) 0.0111(9) 0.0109(8) -0.0088(9) C12 0.0306(9) 0.0636(14) 0.0469(11) 0.0114(10) -0.0040(8) -0.0085(9) C13 0.0313(10) 0.0907(18) 0.0565(13) -0.0012(12) 0.0161(9) -0.0026(11) C14 0.0363(10) 0.0502(11) 0.0474(11) 0.0067(9) 0.0036(8) -0.0147(8) C15 0.053(2) 0.0225(16) 0.334(10) 0.000 -0.012(4) 0.000 O1 0.0282(8) 0.0251(8) 0.0461(10) 0.000 0.0054(7) 0.000 Li1 0.049(3) 0.031(3) 0.062(4) 0.007(3) 0.011(3) 0.005(3) O2 0.065(2) 0.0322(15) 0.073(2) -0.0018(16) 0.0044(19) -0.0031(14) C16 0.069(3) 0.031(2) 0.110(5) -0.001(2) -0.013(3) 0.002(2) C17 0.084(5) 0.073(4) 0.129(7) 0.042(5) -0.017(5) -0.024(4) C18 0.082(4) 0.069(4) 0.061(4) 0.006(3) -0.001(3) 0.001(3) C19 0.081(5) 0.046(3) 0.052(3) -0.002(2) 0.034(4) -0.010(3) O3 0.060(2) 0.0565(19) 0.086(2) 0.0356(18) 0.0313(19) 0.0219(16) C20 0.065(6) 0.094(8) 0.114(9) 0.016(7) 0.042(6) 0.030(5) C21 0.046(3) 0.119(5) 0.085(4) 0.057(4) 0.018(3) 0.017(3) C22 0.056(3) 0.076(4) 0.080(4) 0.024(3) 0.020(3) 0.015(3) C23 0.046(3) 0.054(3) 0.061(3) 0.011(3) 0.010(2) 0.008(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 C1 O1 1.301(3) . ? C1 C2 1.438(2) 2_656 ? C1 C2 1.438(2) . ? C2 C3 1.385(3) . ? C2 C5 1.533(2) . ? C3 C4 1.384(3) . ? C3 H1 0.9500 . ? C4 C3 1.384(3) 2_656 ? C4 C15 1.521(4) . ? C5 C6 1.541(3) . ? C5 C7 1.545(3) . ? C5 C8 1.548(3) . ? C6 C9 1.536(3) . ? C6 H2 0.9900 . ? C6 H3 0.9900 . ? C7 C10 1.536(3) . ? C7 H4 0.9900 . ? C7 H5 0.9900 . ? C8 C11 1.534(3) . ? C8 H6 0.9900 . ? C8 H7 0.9900 . ? C9 C14 1.528(3) . ? C9 C12 1.532(3) . ? C9 H8 1.0000 . ? C10 C12 1.520(3) . ? C10 C13 1.534(3) . ? C10 H9 1.0000 . ? C11 C14 1.518(3) . ? C11 C13 1.530(3) . ? C11 H10 1.0000 . ? C12 H11 0.9900 . ? C12 H12 0.9900 . ? C13 H13 0.9900 . ? C13 H14 0.9900 . ? C14 H15 0.9900 . ? C14 H16 0.9900 . ? C15 H17 0.9800 . ? C15 H18 0.9800 . ? C15 H19 0.9800 . ? O1 Li1 1.719(7) . ? O1 Li1 1.719(7) 2_656 ? Li1 O2 1.911(9) . ? Li1 O3 1.920(8) . ? O2 C16 1.416(6) . ? O2 C19 1.435(9) . ? C16 C17 1.468(8) . ? C16 H20 0.9900 . ? C16 H21 0.9900 . ? C17 C18 1.513(9) . ? C17 H22 0.9900 . ? C17 H23 0.9900 . ? C18 C19 1.518(11) . ? C18 H24 0.9900 . ? C18 H25 0.9900 . ? C19 H26 0.9900 . ? C19 H27 0.9900 . ? O3 C23 1.434(6) . ? O3 C20 1.471(11) . ? C20 C21 1.465(12) . ? C20 H28 0.9900 . ? C20 H29 0.9900 . ? C21 C22 1.480(7) . ? C21 H30 0.9900 . ? C21 H31 0.9900 . ? C22 C23 1.486(8) . ? C22 H32 0.9900 . ? C22 H33 0.9900 . ? C23 H34 0.9900 . ? C23 H35 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 C1 C2 120.89(11) . 2_656 ? O1 C1 C2 120.89(11) . . ? C2 C1 C2 118.2(2) 2_656 . ? C3 C2 C1 118.87(17) . . ? C3 C2 C5 120.36(16) . . ? C1 C2 C5 120.76(16) . . ? C4 C3 C2 123.08(19) . . ? C4 C3 H1 118.5 . . ? C2 C3 H1 118.5 . . ? C3 C4 C3 117.8(3) 2_656 . ? C3 C4 C15 121.08(14) 2_656 . ? C3 C4 C15 121.08(14) . . ? C2 C5 C6 110.66(14) . . ? C2 C5 C7 112.56(16) . . ? C6 C5 C7 106.52(14) . . ? C2 C5 C8 110.58(14) . . ? C6 C5 C8 109.56(15) . . ? C7 C5 C8 106.79(15) . . ? C9 C6 C5 111.16(15) . . ? C9 C6 H2 109.4 . . ? C5 C6 H2 109.4 . . ? C9 C6 H3 109.4 . . ? C5 C6 H3 109.4 . . ? H2 C6 H3 108.0 . . ? C10 C7 C5 111.39(17) . . ? C10 C7 H4 109.3 . . ? C5 C7 H4 109.3 . . ? C10 C7 H5 109.3 . . ? C5 C7 H5 109.3 . . ? H4 C7 H5 108.0 . . ? C11 C8 C5 111.12(15) . . ? C11 C8 H6 109.4 . . ? C5 C8 H6 109.4 . . ? C11 C8 H7 109.4 . . ? C5 C8 H7 109.4 . . ? H6 C8 H7 108.0 . . ? C14 C9 C12 109.45(17) . . ? C14 C9 C6 109.58(15) . . ? C12 C9 C6 109.04(17) . . ? C14 C9 H8 109.6 . . ? C12 C9 H8 109.6 . . ? C6 C9 H8 109.6 . . ? C12 C10 C13 109.2(2) . . ? C12 C10 C7 109.78(17) . . ? C13 C10 C7 109.92(17) . . ? C12 C10 H9 109.3 . . ? C13 C10 H9 109.3 . . ? C7 C10 H9 109.3 . . ? C14 C11 C13 109.48(17) . . ? C14 C11 C8 109.64(16) . . ? C13 C11 C8 109.4(2) . . ? C14 C11 H10 109.4 . . ? C13 C11 H10 109.4 . . ? C8 C11 H10 109.4 . . ? C10 C12 C9 109.14(16) . . ? C10 C12 H11 109.9 . . ? C9 C12 H11 109.9 . . ? C10 C12 H12 109.9 . . ? C9 C12 H12 109.9 . . ? H11 C12 H12 108.3 . . ? C11 C13 C10 108.88(16) . . ? C11 C13 H13 109.9 . . ? C10 C13 H13 109.9 . . ? C11 C13 H14 109.9 . . ? C10 C13 H14 109.9 . . ? H13 C13 H14 108.3 . . ? C11 C14 C9 110.12(19) . . ? C11 C14 H15 109.6 . . ? C9 C14 H15 109.6 . . ? C11 C14 H16 109.6 . . ? C9 C14 H16 109.6 . . ? H15 C14 H16 108.2 . . ? C4 C15 H17 109.5 . . ? C4 C15 H18 109.5 . . ? H17 C15 H18 109.5 . . ? C4 C15 H19 109.5 . . ? H17 C15 H19 109.5 . . ? H18 C15 H19 109.5 . . ? C1 O1 Li1 161.3(2) . . ? C1 O1 Li1 161.3(2) . 2_656 ? O1 Li1 O2 124.7(4) . . ? O1 Li1 O3 123.6(4) . . ? O2 Li1 O3 109.0(4) . . ? C16 O2 C19 105.0(4) . . ? C16 O2 Li1 123.3(5) . . ? C19 O2 Li1 117.9(4) . . ? O2 C16 C17 108.0(5) . . ? O2 C16 H20 110.1 . . ? C17 C16 H20 110.1 . . ? O2 C16 H21 110.1 . . ? C17 C16 H21 110.1 . . ? H20 C16 H21 108.4 . . ? C16 C17 C18 105.9(5) . . ? C16 C17 H22 110.5 . . ? C18 C17 H22 110.5 . . ? C16 C17 H23 110.5 . . ? C18 C17 H23 110.5 . . ? H22 C17 H23 108.7 . . ? C17 C18 C19 101.8(5) . . ? C17 C18 H24 111.4 . . ? C19 C18 H24 111.4 . . ? C17 C18 H25 111.4 . . ? C19 C18 H25 111.4 . . ? H24 C18 H25 109.3 . . ? O2 C19 C18 104.2(6) . . ? O2 C19 H26 110.9 . . ? C18 C19 H26 110.9 . . ? O2 C19 H27 110.9 . . ? C18 C19 H27 110.9 . . ? H26 C19 H27 108.9 . . ? C23 O3 C20 107.9(5) . . ? C23 O3 Li1 134.5(4) . . ? C20 O3 Li1 117.5(5) . . ? C21 C20 O3 103.1(7) . . ? C21 C20 H28 111.2 . . ? O3 C20 H28 111.2 . . ? C21 C20 H29 111.2 . . ? O3 C20 H29 111.2 . . ? H28 C20 H29 109.1 . . ? C20 C21 C22 104.1(5) . . ? C20 C21 H30 110.9 . . ? C22 C21 H30 110.9 . . ? C20 C21 H31 110.9 . . ? C22 C21 H31 110.9 . . ? H30 C21 H31 109.0 . . ? C21 C22 C23 105.6(4) . . ? C21 C22 H32 110.6 . . ? C23 C22 H32 110.6 . . ? C21 C22 H33 110.6 . . ? C23 C22 H33 110.6 . . ? H32 C22 H33 108.7 . . ? O3 C23 C22 106.2(4) . . ? O3 C23 H34 110.5 . . ? C22 C23 H34 110.5 . . ? O3 C23 H35 110.5 . . ? C22 C23 H35 110.5 . . ? H34 C23 H35 108.7 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.319 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.036 #===END data_ZrCl2[OAr(Me)]2 _database_code_depnum_ccdc_archive 'CCDC 735064' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H70 Cl2 O2 Zr, 0.5(C6 H14)' _chemical_formula_sum 'C57 H77 Cl2 O2 Zr' _chemical_formula_weight 956.31 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.960(2) _cell_length_b 19.240(4) _cell_length_c 41.699(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9596(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23673 _cell_measurement_theta_min 3.0863 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4072 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9070 _exptl_absorpt_correction_T_max 0.9483 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 71788 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10746 _reflns_number_gt 10412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+16.7161P] 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 10746 _refine_ls_number_parameters 644 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.465 _refine_ls_restrained_S_all 1.465 _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 0.25488(2) 0.148263(16) 0.108857(7) 0.01973(8) Uani 1 1 d . . . Cl1 Cl 0.18050(8) 0.24530(5) 0.08161(2) 0.0360(2) Uani 1 1 d . . . Cl2 Cl 0.11136(7) 0.06539(5) 0.10149(2) 0.0377(2) Uani 1 1 d . . . O1 O 0.25381(18) 0.17831(10) 0.15286(5) 0.0192(4) Uani 1 1 d . . . O2 O 0.37466(17) 0.10741(11) 0.08474(5) 0.0193(4) Uani 1 1 d . . . C1 C 0.2657(3) 0.21987(15) 0.17958(7) 0.0183(6) Uani 1 1 d . . . C2 C 0.1810(3) 0.21658(16) 0.20367(7) 0.0201(6) Uani 1 1 d . . . C3 C 0.1907(3) 0.26323(17) 0.22907(8) 0.0260(7) Uani 1 1 d . . . H1 H 0.1347 0.2626 0.2452 0.031 Uiso 1 1 calc R . . C4 C 0.2776(3) 0.31052(18) 0.23204(8) 0.0304(8) Uani 1 1 d . . . C5 C 0.3594(3) 0.30958(17) 0.20881(8) 0.0259(7) Uani 1 1 d . . . H2 H 0.4210 0.3404 0.2111 0.031 Uiso 1 1 calc R . . C6 C 0.3573(3) 0.26592(16) 0.18196(7) 0.0202(6) Uani 1 1 d . . . C7 C 0.0818(3) 0.16498(15) 0.20349(8) 0.0205(6) Uani 1 1 d . . . C8 C 0.0012(3) 0.17712(18) 0.17512(8) 0.0273(7) Uani 1 1 d . . . H3 H -0.0292 0.2249 0.1763 0.033 Uiso 1 1 calc R . . H4 H 0.0428 0.1726 0.1547 0.033 Uiso 1 1 calc R . . C9 C 0.0109(3) 0.17231(19) 0.23448(9) 0.0329(8) Uani 1 1 d . . . H5 H 0.0593 0.1643 0.2534 0.040 Uiso 1 1 calc R . . H6 H -0.0187 0.2203 0.2359 0.040 Uiso 1 1 calc R . . C10 C 0.1248(3) 0.08905(17) 0.20246(9) 0.0309(8) Uani 1 1 d . . . H7 H 0.1691 0.0818 0.1827 0.037 Uiso 1 1 calc R . . H8 H 0.1741 0.0804 0.2211 0.037 Uiso 1 1 calc R . . C11 C -0.0959(3) 0.1246(2) 0.17564(10) 0.0388(9) Uani 1 1 d . . . H9 H -0.1456 0.1325 0.1567 0.047 Uiso 1 1 calc R . . C12 C -0.0868(3) 0.1209(2) 0.23525(10) 0.0390(9) Uani 1 1 d . . . H10 H -0.1301 0.1275 0.2555 0.047 Uiso 1 1 calc R . . C13 C 0.0262(4) 0.03765(19) 0.20313(11) 0.0419(10) Uani 1 1 d . . . H11 H 0.0557 -0.0109 0.2021 0.050 Uiso 1 1 calc R . . C14 C -0.1630(3) 0.1341(2) 0.20672(11) 0.0452(10) Uani 1 1 d . . . H12 H -0.1932 0.1819 0.2078 0.054 Uiso 1 1 calc R . . H13 H -0.2265 0.1011 0.2071 0.054 Uiso 1 1 calc R . . C15 C -0.0402(4) 0.0470(2) 0.23423(11) 0.0467(11) Uani 1 1 d . . . H14 H -0.1022 0.0130 0.2351 0.056 Uiso 1 1 calc R . . H15 H 0.0091 0.0390 0.2530 0.056 Uiso 1 1 calc R . . C16 C -0.0497(4) 0.0504(2) 0.17477(11) 0.0455(11) Uani 1 1 d . . . H16 H -0.1123 0.0168 0.1752 0.055 Uiso 1 1 calc R . . H17 H -0.0074 0.0432 0.1546 0.055 Uiso 1 1 calc R . . C17 C 0.4569(3) 0.27616(16) 0.15860(7) 0.0207(6) Uani 1 1 d . . . C18 C 0.2826(4) 0.3608(2) 0.25989(9) 0.0482(11) Uani 1 1 d . . . H18 H 0.2949 0.3350 0.2798 0.072 Uiso 1 1 calc R . . H19 H 0.2120 0.3865 0.2613 0.072 Uiso 1 1 calc R . . H20 H 0.3443 0.3936 0.2566 0.072 Uiso 1 1 calc R . . C19 C 0.4590(3) 0.23043(17) 0.12827(8) 0.0239(7) Uani 1 1 d . . . H21 H 0.3904 0.2390 0.1156 0.029 Uiso 1 1 calc R . . H22 H 0.4593 0.1809 0.1347 0.029 Uiso 1 1 calc R . . C20 C 0.4588(3) 0.35254(18) 0.14681(8) 0.0263(7) Uani 1 1 d . . . H23 H 0.3905 0.3619 0.1341 0.032 Uiso 1 1 calc R . . H24 H 0.4586 0.3841 0.1656 0.032 Uiso 1 1 calc R . . C21 C 0.5672(3) 0.26110(19) 0.17689(8) 0.0284(7) Uani 1 1 d . . . H25 H 0.5698 0.2898 0.1966 0.034 Uiso 1 1 calc R . . H26 H 0.5688 0.2116 0.1834 0.034 Uiso 1 1 calc R . . C22 C 0.5624(3) 0.24532(19) 0.10722(9) 0.0306(8) Uani 1 1 d . . . H27 H 0.5605 0.2146 0.0879 0.037 Uiso 1 1 calc R . . C23 C 0.5618(3) 0.36761(19) 0.12623(9) 0.0306(8) Uani 1 1 d . . . H28 H 0.5609 0.4174 0.1194 0.037 Uiso 1 1 calc R . . C24 C 0.6701(3) 0.2771(2) 0.15607(9) 0.0335(8) Uani 1 1 d . . . H29 H 0.7396 0.2681 0.1687 0.040 Uiso 1 1 calc R . . C25 C 0.5603(3) 0.3209(2) 0.09663(9) 0.0336(8) Uani 1 1 d . . . H30 H 0.4920 0.3300 0.0839 0.040 Uiso 1 1 calc R . . H31 H 0.6262 0.3309 0.0830 0.040 Uiso 1 1 calc R . . C26 C 0.6669(3) 0.3535(2) 0.14565(9) 0.0343(8) Uani 1 1 d . . . H32 H 0.6681 0.3838 0.1648 0.041 Uiso 1 1 calc R . . H33 H 0.7338 0.3642 0.1325 0.041 Uiso 1 1 calc R . . C27 C 0.6684(3) 0.2300(2) 0.12655(10) 0.0369(9) Uani 1 1 d . . . H34 H 0.6692 0.1807 0.1332 0.044 Uiso 1 1 calc R . . H35 H 0.7353 0.2389 0.1132 0.044 Uiso 1 1 calc R . . C28 C 0.4830(2) 0.08789(15) 0.07741(7) 0.0181(6) Uani 1 1 d . . . C29 C 0.5298(2) 0.10983(16) 0.04794(7) 0.0198(6) Uani 1 1 d . . . C30 C 0.6461(3) 0.10387(18) 0.04521(8) 0.0252(7) Uani 1 1 d . . . H36 H 0.6808 0.1196 0.0260 0.030 Uiso 1 1 calc R . . C31 C 0.7128(3) 0.07622(18) 0.06911(8) 0.0259(7) Uani 1 1 d . . . C32 C 0.6604(3) 0.04625(17) 0.09516(8) 0.0240(7) Uani 1 1 d . . . H37 H 0.7052 0.0227 0.1105 0.029 Uiso 1 1 calc R . . C33 C 0.5444(3) 0.04876(15) 0.10009(7) 0.0196(6) Uani 1 1 d . A . C34 C 0.4600(2) 0.13823(15) 0.01977(7) 0.0190(6) Uani 1 1 d . . . C35 C 0.3600(3) 0.08906(17) 0.01271(8) 0.0247(7) Uani 1 1 d . . . H38 H 0.3886 0.0422 0.0072 0.030 Uiso 1 1 calc R . . H39 H 0.3130 0.0848 0.0322 0.030 Uiso 1 1 calc R . . C36 C 0.4168(3) 0.21228(16) 0.02654(8) 0.0222(6) Uani 1 1 d . . . H40 H 0.3725 0.2123 0.0466 0.027 Uiso 1 1 calc R . . H41 H 0.4811 0.2440 0.0295 0.027 Uiso 1 1 calc R . . C37 C 0.5295(3) 0.14249(17) -0.01149(7) 0.0217(6) Uani 1 1 d . . . H42 H 0.5935 0.1743 -0.0082 0.026 Uiso 1 1 calc R . . H43 H 0.5597 0.0959 -0.0167 0.026 Uiso 1 1 calc R . . C38 C 0.2889(3) 0.11653(19) -0.01503(8) 0.0280(7) Uani 1 1 d . . . H44 H 0.2242 0.0846 -0.0187 0.034 Uiso 1 1 calc R . . C39 C 0.3439(3) 0.23844(18) -0.00131(8) 0.0279(7) Uani 1 1 d . . . H45 H 0.3151 0.2859 0.0038 0.034 Uiso 1 1 calc R . . C40 C 0.4585(3) 0.16861(17) -0.03965(8) 0.0243(7) Uani 1 1 d . . . H46 H 0.5060 0.1707 -0.0594 0.029 Uiso 1 1 calc R . . C41 C 0.2453(3) 0.18922(19) -0.00666(8) 0.0313(8) Uani 1 1 d . . . H47 H 0.1979 0.2069 -0.0243 0.038 Uiso 1 1 calc R . . H48 H 0.1991 0.1869 0.0130 0.038 Uiso 1 1 calc R . . C42 C 0.4146(3) 0.24164(17) -0.03201(8) 0.0280(7) Uani 1 1 d . . . H49 H 0.3684 0.2589 -0.0500 0.034 Uiso 1 1 calc R . . H50 H 0.4780 0.2740 -0.0290 0.034 Uiso 1 1 calc R . . C43 C 0.3606(3) 0.11969(18) -0.04550(8) 0.0283(7) Uani 1 1 d . . . H51 H 0.3886 0.0727 -0.0509 0.034 Uiso 1 1 calc R . . H52 H 0.3151 0.1367 -0.0637 0.034 Uiso 1 1 calc R . . C44 C 0.8386(3) 0.0764(2) 0.06705(10) 0.0419(10) Uani 1 1 d . . . H53 H 0.8693 0.1049 0.0844 0.063 Uiso 1 1 calc R . . H54 H 0.8618 0.0958 0.0463 0.063 Uiso 1 1 calc R . . H55 H 0.8666 0.0288 0.0690 0.063 Uiso 1 1 calc R . . C45 C 0.4928(3) 0.00299(16) 0.12640(8) 0.0197(6) Uani 1 1 d . . . C46 C 0.4020(5) -0.0415(3) 0.10889(14) 0.0167(11) Uani 0.50 1 d P A 1 H56 H 0.3442 -0.0105 0.0997 0.020 Uiso 0.50 1 calc PR A 1 H57 H 0.4369 -0.0679 0.0911 0.020 Uiso 0.50 1 calc PR A 1 C47 C 0.4451(5) 0.0410(3) 0.15420(14) 0.0158(11) Uani 0.50 1 d P A 1 H58 H 0.3886 0.0748 0.1466 0.019 Uiso 0.50 1 calc PR A 1 H59 H 0.5051 0.0671 0.1653 0.019 Uiso 0.50 1 calc PR A 1 C48 C 0.5823(5) -0.0494(3) 0.13875(15) 0.0200(12) Uani 0.50 1 d P A 1 H60 H 0.6156 -0.0746 0.1204 0.024 Uiso 0.50 1 calc PR A 1 H61 H 0.6428 -0.0240 0.1499 0.024 Uiso 0.50 1 calc PR A 1 C49 C 0.3481(6) -0.0917(3) 0.13266(17) 0.0209(13) Uani 0.50 1 d P A 1 H62 H 0.2874 -0.1183 0.1216 0.025 Uiso 0.50 1 calc PR A 1 C50 C 0.3910(7) -0.0098(4) 0.17750(19) 0.0209(16) Uani 0.50 1 d P A 1 H63 H 0.3575 0.0165 0.1958 0.025 Uiso 0.50 1 calc PR A 1 C51 C 0.5280(9) -0.1013(5) 0.1618(2) 0.0226(19) Uani 0.50 1 d P A 1 H64 H 0.5867 -0.1341 0.1697 0.027 Uiso 0.50 1 calc PR A 1 C52 C 0.299(2) -0.0516(13) 0.1603(7) 0.026(4) Uani 0.50 1 d P A 1 H65 H 0.2637 -0.0841 0.1757 0.031 Uiso 0.50 1 calc PR A 1 H66 H 0.2406 -0.0195 0.1523 0.031 Uiso 0.50 1 calc PR A 1 C53 C 0.4801(9) -0.0614(5) 0.1904(2) 0.028(2) Uani 0.50 1 d P A 1 H67 H 0.5404 -0.0357 0.2016 0.033 Uiso 0.50 1 calc PR A 1 H68 H 0.4454 -0.0940 0.2059 0.033 Uiso 0.50 1 calc PR A 1 C54 C 0.4368(9) -0.1429(5) 0.1453(3) 0.024(2) Uani 0.50 1 d P A 1 H69 H 0.4023 -0.1758 0.1606 0.029 Uiso 0.50 1 calc PR A 1 H70 H 0.4687 -0.1699 0.1273 0.029 Uiso 0.50 1 calc PR A 1 C55 C 0.3636(5) 0.0110(3) 0.13429(16) 0.0236(13) Uani 0.50 1 d P A 2 H71 H 0.3490 0.0594 0.1413 0.028 Uiso 0.50 1 calc PR A 2 H72 H 0.3200 0.0028 0.1145 0.028 Uiso 0.50 1 calc PR A 2 C56 C 0.5096(6) -0.0727(3) 0.11792(16) 0.0248(14) Uani 0.50 1 d P A 2 H73 H 0.5902 -0.0807 0.1139 0.030 Uiso 0.50 1 calc PR A 2 H74 H 0.4690 -0.0827 0.0977 0.030 Uiso 0.50 1 calc PR A 2 C57 C 0.5503(6) 0.0166(4) 0.16033(16) 0.0286(15) Uani 0.50 1 d P A 2 H75 H 0.6324 0.0125 0.1580 0.034 Uiso 0.50 1 calc PR A 2 H76 H 0.5331 0.0645 0.1675 0.034 Uiso 0.50 1 calc PR A 2 C58 C 0.3220(18) -0.0400(11) 0.1609(7) 0.024(4) Uani 0.50 1 d P A 2 H77 H 0.2400 -0.0335 0.1646 0.029 Uiso 0.50 1 calc PR A 2 C59 C 0.4701(10) -0.1241(6) 0.1437(3) 0.027(2) Uani 0.50 1 d P A 2 H78 H 0.4851 -0.1727 0.1365 0.032 Uiso 0.50 1 calc PR A 2 C60 C 0.5091(9) -0.0359(5) 0.1862(3) 0.029(2) Uani 0.50 1 d P A 2 H79 H 0.5495 -0.0274 0.2068 0.035 Uiso 0.50 1 calc PR A 2 C61 C 0.3848(8) -0.0258(5) 0.1911(2) 0.0295(19) Uani 0.50 1 d P A 2 H80 H 0.3583 -0.0576 0.2082 0.035 Uiso 0.50 1 calc PR A 2 H81 H 0.3703 0.0225 0.1982 0.035 Uiso 0.50 1 calc PR A 2 C62 C 0.3453(6) -0.1141(4) 0.1487(2) 0.0285(15) Uani 0.50 1 d P A 2 H82 H 0.3174 -0.1484 0.1644 0.034 Uiso 0.50 1 calc PR A 2 H83 H 0.3054 -0.1217 0.1282 0.034 Uiso 0.50 1 calc PR A 2 C63 C 0.5324(10) -0.1100(6) 0.1746(2) 0.031(2) Uani 0.50 1 d P A 2 H84 H 0.6136 -0.1161 0.1711 0.037 Uiso 0.50 1 calc PR A 2 H85 H 0.5084 -0.1436 0.1912 0.037 Uiso 0.50 1 calc PR A 2 C64 C 0.4473(4) 0.4949(2) 0.00955(10) 0.0420(10) Uani 1 1 d . . . H86 H 0.3827 0.4968 -0.0053 0.050 Uiso 1 1 calc R . . H87 H 0.4396 0.5339 0.0249 0.050 Uiso 1 1 calc R . . C65 C 0.4420(4) 0.4271(2) 0.02814(12) 0.0499(11) Uani 1 1 d . . . H88 H 0.5025 0.4266 0.0443 0.060 Uiso 1 1 calc R . . H89 H 0.4553 0.3880 0.0132 0.060 Uiso 1 1 calc R . . C66 C 0.3307(4) 0.4160(2) 0.04495(12) 0.0527(12) Uani 1 1 d . . . H90 H 0.3183 0.4536 0.0605 0.079 Uiso 1 1 calc R . . H91 H 0.3316 0.3713 0.0562 0.079 Uiso 1 1 calc R . . H92 H 0.2703 0.4161 0.0291 0.079 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 0.01444(13) 0.02779(15) 0.01694(13) -0.00552(12) -0.00126(12) 0.00574(12) Cl1 0.0346(5) 0.0430(5) 0.0305(4) 0.0021(4) -0.0028(4) 0.0199(4) Cl2 0.0269(4) 0.0477(5) 0.0384(5) -0.0170(4) 0.0001(4) -0.0066(4) O1 0.0183(10) 0.0227(10) 0.0166(10) -0.0037(8) 0.0020(9) -0.0007(9) O2 0.0165(10) 0.0223(11) 0.0192(10) -0.0002(9) 0.0018(8) 0.0046(9) C1 0.0207(16) 0.0181(13) 0.0160(14) -0.0016(11) -0.0018(12) 0.0036(12) C2 0.0236(16) 0.0208(15) 0.0160(14) 0.0003(12) -0.0004(12) 0.0036(12) C3 0.0321(18) 0.0288(17) 0.0173(15) -0.0027(13) 0.0060(14) -0.0008(14) C4 0.040(2) 0.0316(18) 0.0195(16) -0.0067(13) 0.0016(15) -0.0054(15) C5 0.0295(18) 0.0266(17) 0.0216(16) -0.0026(13) -0.0015(14) -0.0062(14) C6 0.0236(16) 0.0201(15) 0.0170(15) 0.0016(12) -0.0007(12) 0.0009(12) C7 0.0224(16) 0.0181(15) 0.0212(15) 0.0017(11) 0.0053(13) 0.0011(12) C8 0.0239(17) 0.0306(17) 0.0274(18) 0.0041(14) 0.0022(14) 0.0003(14) C9 0.034(2) 0.037(2) 0.0273(19) -0.0008(15) 0.0133(16) -0.0033(16) C10 0.0332(19) 0.0235(17) 0.036(2) 0.0045(14) 0.0084(16) 0.0037(14) C11 0.0249(18) 0.052(2) 0.039(2) 0.0029(18) 0.0012(16) -0.0103(17) C12 0.037(2) 0.043(2) 0.037(2) 0.0006(17) 0.0201(18) -0.0073(17) C13 0.046(2) 0.0205(17) 0.059(3) 0.0030(17) 0.016(2) -0.0036(16) C14 0.0237(19) 0.051(3) 0.061(3) -0.001(2) 0.0095(19) -0.0068(17) C15 0.048(3) 0.042(2) 0.050(3) 0.0146(19) 0.014(2) -0.0120(19) C16 0.044(2) 0.042(2) 0.051(3) -0.0135(19) 0.016(2) -0.0209(19) C17 0.0192(15) 0.0242(15) 0.0187(15) -0.0021(12) -0.0015(12) -0.0029(12) C18 0.063(3) 0.052(3) 0.029(2) -0.0208(18) 0.0123(19) -0.018(2) C19 0.0201(16) 0.0298(17) 0.0219(16) -0.0032(13) -0.0002(13) -0.0040(13) C20 0.0235(16) 0.0279(17) 0.0276(17) 0.0022(14) 0.0008(14) -0.0020(14) C21 0.0273(18) 0.0346(19) 0.0233(17) 0.0005(14) -0.0082(14) -0.0008(15) C22 0.0219(16) 0.042(2) 0.0284(18) -0.0100(16) 0.0040(15) -0.0062(15) C23 0.0273(18) 0.0299(18) 0.0345(19) 0.0016(15) 0.0019(15) -0.0062(14) C24 0.0178(16) 0.045(2) 0.038(2) -0.0040(17) -0.0068(15) 0.0009(15) C25 0.0246(18) 0.049(2) 0.0271(18) 0.0035(16) 0.0027(15) -0.0097(16) C26 0.0251(18) 0.041(2) 0.037(2) -0.0065(17) 0.0011(15) -0.0116(16) C27 0.0218(18) 0.040(2) 0.049(2) -0.0086(18) 0.0036(17) 0.0009(15) C28 0.0162(14) 0.0156(14) 0.0224(15) -0.0026(11) 0.0015(12) 0.0044(11) C29 0.0185(14) 0.0186(14) 0.0222(15) -0.0016(12) 0.0005(12) 0.0023(12) C30 0.0195(15) 0.0316(17) 0.0244(16) 0.0003(14) 0.0053(13) 0.0023(14) C31 0.0167(15) 0.0325(18) 0.0286(17) -0.0040(14) 0.0019(13) 0.0063(13) C32 0.0196(16) 0.0250(16) 0.0274(17) -0.0015(13) -0.0054(13) 0.0063(13) C33 0.0208(15) 0.0167(14) 0.0214(15) -0.0027(11) -0.0017(12) 0.0023(12) C34 0.0175(14) 0.0210(15) 0.0183(14) -0.0003(12) 0.0024(12) -0.0003(12) C35 0.0254(16) 0.0260(17) 0.0227(16) 0.0008(13) 0.0037(13) -0.0063(13) C36 0.0231(16) 0.0209(15) 0.0226(16) -0.0021(12) -0.0019(13) 0.0013(13) C37 0.0202(15) 0.0247(15) 0.0203(15) 0.0004(13) 0.0024(12) -0.0022(13) C38 0.0236(16) 0.0362(19) 0.0241(17) 0.0003(14) -0.0020(13) -0.0107(14) C39 0.0311(18) 0.0253(17) 0.0274(18) 0.0001(14) -0.0032(15) 0.0079(14) C40 0.0266(17) 0.0287(17) 0.0177(15) 0.0004(12) 0.0040(13) -0.0044(13) C41 0.0217(16) 0.049(2) 0.0233(17) 0.0004(15) -0.0032(15) 0.0042(16) C42 0.0346(19) 0.0248(17) 0.0247(17) 0.0040(13) -0.0053(15) -0.0015(14) C43 0.0322(18) 0.0324(18) 0.0203(16) -0.0036(13) 0.0007(14) -0.0063(15) C44 0.0176(18) 0.063(3) 0.045(2) 0.003(2) 0.0023(16) 0.0086(17) C45 0.0178(15) 0.0191(14) 0.0222(16) -0.0011(12) -0.0030(12) 0.0034(12) C46 0.018(3) 0.015(3) 0.017(3) 0.000(2) 0.000(2) 0.001(2) C47 0.019(3) 0.014(3) 0.014(3) 0.000(2) -0.003(2) 0.004(2) C48 0.019(3) 0.023(3) 0.019(3) 0.003(2) -0.001(2) 0.009(2) C49 0.023(3) 0.017(3) 0.023(3) 0.006(3) -0.004(3) -0.004(3) C50 0.026(4) 0.019(4) 0.017(4) 0.002(3) 0.002(4) 0.009(3) C51 0.024(4) 0.024(4) 0.020(5) 0.007(4) 0.002(5) 0.013(3) C52 0.025(9) 0.026(8) 0.027(5) 0.005(5) -0.005(5) -0.006(5) C53 0.034(6) 0.027(5) 0.022(4) 0.006(4) -0.003(4) 0.004(4) C54 0.028(6) 0.014(5) 0.031(4) 0.006(4) 0.000(4) -0.003(4) C55 0.023(3) 0.024(3) 0.023(3) 0.000(3) -0.001(3) 0.004(3) C56 0.022(3) 0.029(3) 0.024(3) -0.001(3) 0.001(3) 0.004(3) C57 0.031(4) 0.032(4) 0.023(3) -0.005(3) -0.007(3) -0.003(3) C58 0.020(9) 0.019(7) 0.032(6) 0.001(5) 0.008(7) 0.008(7) C59 0.032(7) 0.016(6) 0.032(5) 0.002(4) 0.005(5) 0.000(4) C60 0.028(5) 0.035(6) 0.025(5) -0.005(4) -0.004(4) 0.006(4) C61 0.029(4) 0.031(5) 0.029(5) 0.003(4) 0.001(4) 0.005(3) C62 0.030(4) 0.024(4) 0.031(4) 0.000(3) 0.002(3) -0.003(3) C63 0.034(4) 0.032(5) 0.026(6) 0.007(5) 0.003(5) 0.006(4) C64 0.052(3) 0.033(2) 0.040(2) -0.0022(17) -0.014(2) 0.0118(19) C65 0.053(3) 0.039(2) 0.058(3) 0.009(2) -0.017(2) 0.001(2) C66 0.052(3) 0.050(3) 0.056(3) -0.005(2) -0.012(2) -0.009(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 Zr1 O2 1.919(2) . ? Zr1 O1 1.924(2) . ? Zr1 Cl1 2.3597(10) . ? Zr1 Cl2 2.3629(10) . ? O1 C1 1.379(3) . ? O2 C28 1.384(3) . ? C1 C6 1.413(4) . ? C1 C2 1.428(4) . ? C2 C3 1.393(4) . ? C2 C7 1.547(4) . ? C3 C4 1.387(5) . ? C3 H1 0.9500 . ? C4 C5 1.378(5) . ? C4 C18 1.513(5) . ? C5 C6 1.400(4) . ? C5 H2 0.9500 . ? C6 C17 1.551(4) . ? C7 C8 1.544(5) . ? C7 C10 1.549(4) . ? C7 C9 1.553(4) . ? C8 C11 1.540(5) . ? C8 H3 0.9900 . ? C8 H4 0.9900 . ? C9 C12 1.531(5) . ? C9 H5 0.9900 . ? C9 H6 0.9900 . ? C10 C13 1.539(5) . ? C10 H7 0.9900 . ? C10 H8 0.9900 . ? C11 C16 1.531(6) . ? C11 C14 1.535(6) . ? C11 H9 1.0000 . ? C12 C14 1.520(6) . ? C12 C15 1.527(6) . ? C12 H10 1.0000 . ? C13 C16 1.511(6) . ? C13 C15 1.531(6) . ? C13 H11 1.0000 . ? C14 H12 0.9900 . ? C14 H13 0.9900 . ? C15 H14 0.9900 . ? C15 H15 0.9900 . ? C16 H16 0.9900 . ? C16 H17 0.9900 . ? C17 C19 1.541(4) . ? C17 C20 1.550(4) . ? C17 C21 1.551(4) . ? C18 H18 0.9800 . ? C18 H19 0.9800 . ? C18 H20 0.9800 . ? C19 C22 1.543(4) . ? C19 H21 0.9900 . ? C19 H22 0.9900 . ? C20 C23 1.529(5) . ? C20 H23 0.9900 . ? C20 H24 0.9900 . ? C21 C24 1.537(5) . ? C21 H25 0.9900 . ? C21 H26 0.9900 . ? C22 C25 1.520(5) . ? C22 C27 1.530(5) . ? C22 H27 1.0000 . ? C23 C26 1.520(5) . ? C23 C25 1.527(5) . ? C23 H28 1.0000 . ? C24 C27 1.528(5) . ? C24 C26 1.534(5) . ? C24 H29 1.0000 . ? C25 H30 0.9900 . ? C25 H31 0.9900 . ? C26 H32 0.9900 . ? C26 H33 0.9900 . ? C27 H34 0.9900 . ? C27 H35 0.9900 . ? C28 C33 1.414(4) . ? C28 C29 1.414(4) . ? C29 C30 1.400(4) . ? C29 C34 1.542(4) . ? C30 C31 1.383(5) . ? C30 H36 0.9500 . ? C31 C32 1.380(5) . ? C31 C44 1.508(5) . ? C32 C33 1.404(4) . ? C32 H37 0.9500 . ? C33 C45 1.536(4) . ? C34 C36 1.541(4) . ? C34 C37 1.548(4) . ? C34 C35 1.553(4) . ? C35 C38 1.530(5) . ? C35 H38 0.9900 . ? C35 H39 0.9900 . ? C36 C39 1.537(4) . ? C36 H40 0.9900 . ? C36 H41 0.9900 . ? C37 C40 1.534(4) . ? C37 H42 0.9900 . ? C37 H43 0.9900 . ? C38 C41 1.533(5) . ? C38 C43 1.534(5) . ? C38 H44 1.0000 . ? C39 C41 1.528(5) . ? C39 C42 1.535(5) . ? C39 H45 1.0000 . ? C40 C43 1.522(5) . ? C40 C42 1.534(5) . ? C40 H46 1.0000 . ? C41 H47 0.9900 . ? C41 H48 0.9900 . ? C42 H49 0.9900 . ? C42 H50 0.9900 . ? C43 H51 0.9900 . ? C43 H52 0.9900 . ? C44 H53 0.9800 . ? C44 H54 0.9800 . ? C44 H55 0.9800 . ? C45 C47 1.485(6) . ? C45 C56 1.512(7) . ? C45 C48 1.559(6) . ? C45 C46 1.563(6) . ? C45 C55 1.588(7) . ? C45 C57 1.595(7) . ? C46 C49 1.528(9) . ? C46 H56 0.9900 . ? C46 H57 0.9900 . ? C47 C50 1.523(9) . ? C47 H58 0.9900 . ? C47 H59 0.9900 . ? C48 C51 1.529(11) . ? C48 H60 0.9900 . ? C48 H61 0.9900 . ? C49 C52 1.51(3) . ? C49 C54 1.539(14) . ? C49 H62 1.0000 . ? C50 C52 1.54(3) . ? C50 C53 1.553(13) . ? C50 H63 1.0000 . ? C51 C54 1.518(15) . ? C51 C53 1.533(15) . ? C51 H64 1.0000 . ? C52 H65 0.9900 . ? C52 H66 0.9900 . ? C53 H67 0.9900 . ? C53 H68 0.9900 . ? C54 H69 0.9900 . ? C54 H70 0.9900 . ? C55 C58 1.56(2) . ? C55 H71 0.9900 . ? C55 H72 0.9900 . ? C56 C59 1.535(12) . ? C56 H73 0.9900 . ? C56 H74 0.9900 . ? C57 C60 1.558(11) . ? C57 H75 0.9900 . ? C57 H76 0.9900 . ? C58 C61 1.49(3) . ? C58 C62 1.54(2) . ? C58 H77 1.0000 . ? C59 C63 1.514(17) . ? C59 C62 1.519(14) . ? C59 H78 1.0000 . ? C60 C61 1.513(14) . ? C60 C63 1.530(16) . ? C60 H79 1.0000 . ? C61 H80 0.9900 . ? C61 H81 0.9900 . ? C62 H82 0.9900 . ? C62 H83 0.9900 . ? C63 H84 0.9900 . ? C63 H85 0.9900 . ? C64 C64 1.505(9) 5_665 ? C64 C65 1.518(6) . ? C64 H86 0.9900 . ? C64 H87 0.9900 . ? C65 C66 1.520(6) . ? C65 H88 0.9900 . ? C65 H89 0.9900 . ? C66 H90 0.9800 . ? C66 H91 0.9800 . ? C66 H92 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 O1 128.90(9) . . ? O2 Zr1 Cl1 110.68(7) . . ? O1 Zr1 Cl1 102.65(7) . . ? O2 Zr1 Cl2 101.41(7) . . ? O1 Zr1 Cl2 108.78(7) . . ? Cl1 Zr1 Cl2 101.39(4) . . ? C1 O1 Zr1 160.78(19) . . ? C28 O2 Zr1 157.88(19) . . ? O1 C1 C6 120.0(3) . . ? O1 C1 C2 118.0(3) . . ? C6 C1 C2 121.9(3) . . ? C3 C2 C1 116.6(3) . . ? C3 C2 C7 118.7(3) . . ? C1 C2 C7 124.7(3) . . ? C4 C3 C2 123.5(3) . . ? C4 C3 H1 118.2 . . ? C2 C3 H1 118.2 . . ? C5 C4 C3 117.5(3) . . ? C5 C4 C18 121.3(3) . . ? C3 C4 C18 121.2(3) . . ? C4 C5 C6 123.9(3) . . ? C4 C5 H2 118.1 . . ? C6 C5 H2 118.1 . . ? C5 C6 C1 116.5(3) . . ? C5 C6 C17 114.4(3) . . ? C1 C6 C17 129.1(3) . . ? C8 C7 C2 112.7(3) . . ? C8 C7 C10 109.2(3) . . ? C2 C7 C10 110.5(3) . . ? C8 C7 C9 106.4(3) . . ? C2 C7 C9 110.9(3) . . ? C10 C7 C9 106.9(3) . . ? C11 C8 C7 111.2(3) . . ? C11 C8 H3 109.4 . . ? C7 C8 H3 109.4 . . ? C11 C8 H4 109.4 . . ? C7 C8 H4 109.4 . . ? H3 C8 H4 108.0 . . ? C12 C9 C7 112.1(3) . . ? C12 C9 H5 109.2 . . ? C7 C9 H5 109.2 . . ? C12 C9 H6 109.2 . . ? C7 C9 H6 109.2 . . ? H5 C9 H6 107.9 . . ? C13 C10 C7 110.6(3) . . ? C13 C10 H7 109.5 . . ? C7 C10 H7 109.5 . . ? C13 C10 H8 109.5 . . ? C7 C10 H8 109.5 . . ? H7 C10 H8 108.1 . . ? C16 C11 C14 108.7(3) . . ? C16 C11 C8 109.8(3) . . ? C14 C11 C8 109.1(3) . . ? C16 C11 H9 109.7 . . ? C14 C11 H9 109.7 . . ? C8 C11 H9 109.7 . . ? C14 C12 C15 110.6(4) . . ? C14 C12 C9 109.4(3) . . ? C15 C12 C9 108.8(3) . . ? C14 C12 H10 109.3 . . ? C15 C12 H10 109.3 . . ? C9 C12 H10 109.3 . . ? C16 C13 C15 109.4(4) . . ? C16 C13 C10 110.0(3) . . ? C15 C13 C10 109.7(3) . . ? C16 C13 H11 109.3 . . ? C15 C13 H11 109.3 . . ? C10 C13 H11 109.3 . . ? C12 C14 C11 109.1(3) . . ? C12 C14 H12 109.9 . . ? C11 C14 H12 109.9 . . ? C12 C14 H13 109.9 . . ? C11 C14 H13 109.9 . . ? H12 C14 H13 108.3 . . ? C12 C15 C13 108.8(3) . . ? C12 C15 H14 109.9 . . ? C13 C15 H14 109.9 . . ? C12 C15 H15 109.9 . . ? C13 C15 H15 109.9 . . ? H14 C15 H15 108.3 . . ? C13 C16 C11 110.5(3) . . ? C13 C16 H16 109.6 . . ? C11 C16 H16 109.6 . . ? C13 C16 H17 109.6 . . ? C11 C16 H17 109.6 . . ? H16 C16 H17 108.1 . . ? C19 C17 C20 106.3(3) . . ? C19 C17 C6 117.1(3) . . ? C20 C17 C6 109.3(3) . . ? C19 C17 C21 106.4(3) . . ? C20 C17 C21 108.7(3) . . ? C6 C17 C21 108.7(3) . . ? C4 C18 H18 109.5 . . ? C4 C18 H19 109.5 . . ? H18 C18 H19 109.5 . . ? C4 C18 H20 109.5 . . ? H18 C18 H20 109.5 . . ? H19 C18 H20 109.5 . . ? C17 C19 C22 112.0(3) . . ? C17 C19 H21 109.2 . . ? C22 C19 H21 109.2 . . ? C17 C19 H22 109.2 . . ? C22 C19 H22 109.2 . . ? H21 C19 H22 107.9 . . ? C23 C20 C17 111.7(3) . . ? C23 C20 H23 109.3 . . ? C17 C20 H23 109.3 . . ? C23 C20 H24 109.3 . . ? C17 C20 H24 109.3 . . ? H23 C20 H24 107.9 . . ? C24 C21 C17 111.5(3) . . ? C24 C21 H25 109.3 . . ? C17 C21 H25 109.3 . . ? C24 C21 H26 109.3 . . ? C17 C21 H26 109.3 . . ? H25 C21 H26 108.0 . . ? C25 C22 C27 110.5(3) . . ? C25 C22 C19 109.2(3) . . ? C27 C22 C19 109.2(3) . . ? C25 C22 H27 109.3 . . ? C27 C22 H27 109.3 . . ? C19 C22 H27 109.3 . . ? C26 C23 C25 109.6(3) . . ? C26 C23 C20 109.5(3) . . ? C25 C23 C20 109.4(3) . . ? C26 C23 H28 109.4 . . ? C25 C23 H28 109.4 . . ? C20 C23 H28 109.4 . . ? C27 C24 C26 109.8(3) . . ? C27 C24 C21 109.0(3) . . ? C26 C24 C21 109.4(3) . . ? C27 C24 H29 109.5 . . ? C26 C24 H29 109.5 . . ? C21 C24 H29 109.5 . . ? C22 C25 C23 109.1(3) . . ? C22 C25 H30 109.9 . . ? C23 C25 H30 109.9 . . ? C22 C25 H31 109.9 . . ? C23 C25 H31 109.9 . . ? H30 C25 H31 108.3 . . ? C23 C26 C24 110.0(3) . . ? C23 C26 H32 109.7 . . ? C24 C26 H32 109.7 . . ? C23 C26 H33 109.7 . . ? C24 C26 H33 109.7 . . ? H32 C26 H33 108.2 . . ? C24 C27 C22 108.8(3) . . ? C24 C27 H34 109.9 . . ? C22 C27 H34 109.9 . . ? C24 C27 H35 109.9 . . ? C22 C27 H35 109.9 . . ? H34 C27 H35 108.3 . . ? O2 C28 C33 118.9(3) . . ? O2 C28 C29 118.8(3) . . ? C33 C28 C29 122.3(3) . . ? C30 C29 C28 116.1(3) . . ? C30 C29 C34 120.4(3) . . ? C28 C29 C34 123.6(3) . . ? C31 C30 C29 123.1(3) . . ? C31 C30 H36 118.5 . . ? C29 C30 H36 118.5 . . ? C32 C31 C30 117.8(3) . . ? C32 C31 C44 119.9(3) . . ? C30 C31 C44 122.3(3) . . ? C31 C32 C33 123.3(3) . . ? C31 C32 H37 118.3 . . ? C33 C32 H37 118.3 . . ? C32 C33 C28 115.7(3) . . ? C32 C33 C45 118.8(3) . . ? C28 C33 C45 125.1(3) . . ? C36 C34 C29 111.7(2) . . ? C36 C34 C37 106.6(2) . . ? C29 C34 C37 111.7(2) . . ? C36 C34 C35 109.9(2) . . ? C29 C34 C35 110.2(2) . . ? C37 C34 C35 106.6(2) . . ? C38 C35 C34 111.1(3) . . ? C38 C35 H38 109.4 . . ? C34 C35 H38 109.4 . . ? C38 C35 H39 109.4 . . ? C34 C35 H39 109.4 . . ? H38 C35 H39 108.0 . . ? C39 C36 C34 110.7(3) . . ? C39 C36 H40 109.5 . . ? C34 C36 H40 109.5 . . ? C39 C36 H41 109.5 . . ? C34 C36 H41 109.5 . . ? H40 C36 H41 108.1 . . ? C40 C37 C34 111.4(3) . . ? C40 C37 H42 109.3 . . ? C34 C37 H42 109.3 . . ? C40 C37 H43 109.3 . . ? C34 C37 H43 109.3 . . ? H42 C37 H43 108.0 . . ? C35 C38 C41 109.4(3) . . ? C35 C38 C43 109.2(3) . . ? C41 C38 C43 110.0(3) . . ? C35 C38 H44 109.4 . . ? C41 C38 H44 109.4 . . ? C43 C38 H44 109.4 . . ? C41 C39 C42 109.1(3) . . ? C41 C39 C36 110.2(3) . . ? C42 C39 C36 109.3(3) . . ? C41 C39 H45 109.4 . . ? C42 C39 H45 109.4 . . ? C36 C39 H45 109.4 . . ? C43 C40 C42 109.6(3) . . ? C43 C40 C37 110.2(3) . . ? C42 C40 C37 109.3(3) . . ? C43 C40 H46 109.2 . . ? C42 C40 H46 109.2 . . ? C37 C40 H46 109.2 . . ? C39 C41 C38 109.6(3) . . ? C39 C41 H47 109.7 . . ? C38 C41 H47 109.7 . . ? C39 C41 H48 109.7 . . ? C38 C41 H48 109.7 . . ? H47 C41 H48 108.2 . . ? C40 C42 C39 109.0(3) . . ? C40 C42 H49 109.9 . . ? C39 C42 H49 109.9 . . ? C40 C42 H50 109.9 . . ? C39 C42 H50 109.9 . . ? H49 C42 H50 108.3 . . ? C40 C43 C38 108.8(3) . . ? C40 C43 H51 109.9 . . ? C38 C43 H51 109.9 . . ? C40 C43 H52 109.9 . . ? C38 C43 H52 109.9 . . ? H51 C43 H52 108.3 . . ? C31 C44 H53 109.5 . . ? C31 C44 H54 109.5 . . ? H53 C44 H54 109.5 . . ? C31 C44 H55 109.5 . . ? H53 C44 H55 109.5 . . ? H54 C44 H55 109.5 . . ? C47 C45 C56 135.1(4) . . ? C47 C45 C33 115.4(3) . . ? C56 C45 C33 109.4(3) . . ? C47 C45 C48 109.0(4) . . ? C56 C45 C48 50.4(4) . . ? C33 C45 C48 109.3(3) . . ? C47 C45 C46 111.6(4) . . ? C56 C45 C46 57.1(3) . . ? C33 C45 C46 105.0(3) . . ? C48 C45 C46 106.1(4) . . ? C47 C45 C55 54.3(3) . . ? C56 C45 C55 105.8(4) . . ? C33 C45 C55 118.9(3) . . ? C48 C45 C55 131.6(4) . . ? C46 C45 C55 58.3(3) . . ? C47 C45 C57 52.6(4) . . ? C56 C45 C57 107.9(4) . . ? C33 C45 C57 111.5(3) . . ? C48 C45 C57 61.1(4) . . ? C46 C45 C57 143.5(4) . . ? C55 C45 C57 102.7(4) . . ? C49 C46 C45 109.7(5) . . ? C49 C46 H56 109.7 . . ? C45 C46 H56 109.7 . . ? C49 C46 H57 109.7 . . ? C45 C46 H57 109.7 . . ? H56 C46 H57 108.2 . . ? C45 C47 C50 110.2(5) . . ? C45 C47 H58 109.6 . . ? C50 C47 H58 109.6 . . ? C45 C47 H59 109.6 . . ? C50 C47 H59 109.6 . . ? H58 C47 H59 108.1 . . ? C51 C48 C45 109.7(5) . . ? C51 C48 H60 109.7 . . ? C45 C48 H60 109.7 . . ? C51 C48 H61 109.7 . . ? C45 C48 H61 109.7 . . ? H60 C48 H61 108.2 . . ? C52 C49 C46 109.7(10) . . ? C52 C49 C54 109.6(13) . . ? C46 C49 C54 109.6(6) . . ? C52 C49 H62 109.3 . . ? C46 C49 H62 109.3 . . ? C54 C49 H62 109.3 . . ? C47 C50 C52 110.0(11) . . ? C47 C50 C53 109.9(7) . . ? C52 C50 C53 108.6(12) . . ? C47 C50 H63 109.4 . . ? C52 C50 H63 109.4 . . ? C53 C50 H63 109.4 . . ? C54 C51 C48 111.4(7) . . ? C54 C51 C53 110.4(9) . . ? C48 C51 C53 108.8(8) . . ? C54 C51 H64 108.7 . . ? C48 C51 H64 108.7 . . ? C53 C51 H64 108.7 . . ? C49 C52 C50 110.2(15) . . ? C49 C52 H65 109.6 . . ? C50 C52 H65 109.6 . . ? C49 C52 H66 109.6 . . ? C50 C52 H66 109.6 . . ? H65 C52 H66 108.1 . . ? C51 C53 C50 107.8(8) . . ? C51 C53 H67 110.1 . . ? C50 C53 H67 110.1 . . ? C51 C53 H68 110.1 . . ? C50 C53 H68 110.1 . . ? H67 C53 H68 108.5 . . ? C51 C54 C49 108.2(8) . . ? C51 C54 H69 110.1 . . ? C49 C54 H69 110.1 . . ? C51 C54 H70 110.1 . . ? C49 C54 H70 110.1 . . ? H69 C54 H70 108.4 . . ? C58 C55 C45 113.3(10) . . ? C58 C55 H71 108.9 . . ? C45 C55 H71 108.9 . . ? C58 C55 H72 108.9 . . ? C45 C55 H72 108.9 . . ? H71 C55 H72 107.7 . . ? C45 C56 C59 114.5(6) . . ? C45 C56 H73 108.6 . . ? C59 C56 H73 108.6 . . ? C45 C56 H74 108.6 . . ? C59 C56 H74 108.6 . . ? H73 C56 H74 107.6 . . ? C60 C57 C45 111.9(6) . . ? C60 C57 H75 109.2 . . ? C45 C57 H75 109.2 . . ? C60 C57 H76 109.2 . . ? C45 C57 H76 109.2 . . ? H75 C57 H76 107.9 . . ? C61 C58 C62 110.9(17) . . ? C61 C58 C55 109.0(13) . . ? C62 C58 C55 106.8(16) . . ? C61 C58 H77 110.0 . . ? C62 C58 H77 110.0 . . ? C55 C58 H77 110.0 . . ? C63 C59 C62 110.2(10) . . ? C63 C59 C56 109.2(8) . . ? C62 C59 C56 108.5(9) . . ? C63 C59 H78 109.7 . . ? C62 C59 H78 109.7 . . ? C56 C59 H78 109.7 . . ? C61 C60 C63 109.9(8) . . ? C61 C60 C57 108.7(8) . . ? C63 C60 C57 109.1(8) . . ? C61 C60 H79 109.7 . . ? C63 C60 H79 109.7 . . ? C57 C60 H79 109.7 . . ? C58 C61 C60 110.9(11) . . ? C58 C61 H80 109.5 . . ? C60 C61 H80 109.5 . . ? C58 C61 H81 109.5 . . ? C60 C61 H81 109.5 . . ? H80 C61 H81 108.0 . . ? C59 C62 C58 109.9(10) . . ? C59 C62 H82 109.7 . . ? C58 C62 H82 109.7 . . ? C59 C62 H83 109.7 . . ? C58 C62 H83 109.7 . . ? H82 C62 H83 108.2 . . ? C59 C63 C60 110.3(9) . . ? C59 C63 H84 109.6 . . ? C60 C63 H84 109.6 . . ? C59 C63 H85 109.6 . . ? C60 C63 H85 109.6 . . ? H84 C63 H85 108.1 . . ? C64 C64 C65 114.7(4) 5_665 . ? C64 C64 H86 108.6 5_665 . ? C65 C64 H86 108.6 . . ? C64 C64 H87 108.6 5_665 . ? C65 C64 H87 108.6 . . ? H86 C64 H87 107.6 . . ? C64 C65 C66 113.1(4) . . ? C64 C65 H88 109.0 . . ? C66 C65 H88 109.0 . . ? C64 C65 H89 109.0 . . ? C66 C65 H89 109.0 . . ? H88 C65 H89 107.8 . . ? C65 C66 H90 109.5 . . ? C65 C66 H91 109.5 . . ? H90 C66 H91 109.5 . . ? C65 C66 H92 109.5 . . ? H90 C66 H92 109.5 . . ? H91 C66 H92 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.356 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.060 #===END data_Zr(CH2Ph)2[OAr(Me)]2 _database_code_depnum_ccdc_archive 'CCDC 735065' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H84 O2 Zr, C6 H14' _chemical_formula_sum 'C74 H98 O2 Zr' _chemical_formula_weight 1110.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.234(4) _cell_length_b 14.511(4) _cell_length_c 20.732(7) _cell_angle_alpha 70.337(18) _cell_angle_beta 76.384(18) _cell_angle_gamma 71.853(18) _cell_volume 2991.9(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7985 _cell_measurement_theta_min 3.0088 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9511 _exptl_absorpt_correction_T_max 0.9773 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 23883 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13133 _reflns_number_gt 10835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0779P)^2^+2.3491P] 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 13133 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Zr1 Zr 0.51081(3) 0.68158(2) 0.736234(15) 0.02333(10) Uani 1 1 d . . . O1 O 0.51714(18) 0.60637(14) 0.67384(10) 0.0228(4) Uani 1 1 d . . . O2 O 0.34785(18) 0.74793(15) 0.77751(10) 0.0237(4) Uani 1 1 d . . . C1 C 0.6122(3) 0.5797(3) 0.82736(17) 0.0342(7) Uani 1 1 d . . . H1 H 0.5726 0.5227 0.8521 0.041 Uiso 1 1 calc R . . H2 H 0.7020 0.5514 0.8106 0.041 Uiso 1 1 calc R . . C2 C 0.6046(3) 0.6384(2) 0.87533(17) 0.0315(7) Uani 1 1 d . . . C3 C 0.5098(4) 0.6434(3) 0.9312(2) 0.0507(10) Uani 1 1 d . . . H3 H 0.4485 0.6060 0.9413 0.061 Uiso 1 1 calc R . . C4 C 0.5039(4) 0.7041(4) 0.9733(2) 0.0631(13) Uani 1 1 d . . . H4 H 0.4380 0.7077 1.0114 0.076 Uiso 1 1 calc R . . C5 C 0.5922(5) 0.7578(3) 0.9596(3) 0.0591(12) Uani 1 1 d . . . H5 H 0.5874 0.7984 0.9883 0.071 Uiso 1 1 calc R . . C6 C 0.6863(5) 0.7534(3) 0.9055(2) 0.0600(12) Uani 1 1 d . . . H6 H 0.7480 0.7903 0.8963 0.072 Uiso 1 1 calc R . . C7 C 0.6925(4) 0.6951(3) 0.8636(2) 0.0471(9) Uani 1 1 d . . . H7 H 0.7585 0.6932 0.8254 0.057 Uiso 1 1 calc R . . C8 C 0.6324(3) 0.7916(2) 0.67786(17) 0.0308(7) Uani 1 1 d . . . H8 H 0.5806 0.8540 0.6494 0.037 Uiso 1 1 calc R . . H9 H 0.6639 0.8102 0.7113 0.037 Uiso 1 1 calc R . . C9 C 0.7419(3) 0.7453(2) 0.63217(17) 0.0292(6) Uani 1 1 d . . . C10 C 0.7420(3) 0.7695(3) 0.56102(17) 0.0336(7) Uani 1 1 d . . . H10 H 0.6726 0.8191 0.5407 0.040 Uiso 1 1 calc R . . C11 C 0.8413(3) 0.7226(3) 0.51946(18) 0.0400(8) Uani 1 1 d . . . H11 H 0.8393 0.7402 0.4712 0.048 Uiso 1 1 calc R . . C12 C 0.9434(3) 0.6503(3) 0.54786(19) 0.0404(8) Uani 1 1 d . . . H12 H 1.0108 0.6173 0.5195 0.048 Uiso 1 1 calc R . . C13 C 0.9462(3) 0.6267(3) 0.61777(19) 0.0384(8) Uani 1 1 d . . . H13 H 1.0167 0.5782 0.6375 0.046 Uiso 1 1 calc R . . C14 C 0.8467(3) 0.6733(3) 0.65951(18) 0.0340(7) Uani 1 1 d . . . H14 H 0.8500 0.6559 0.7076 0.041 Uiso 1 1 calc R . . C15 C 0.4700(3) 0.5606(2) 0.64046(14) 0.0212(5) Uani 1 1 d . . . C16 C 0.5220(3) 0.4548(2) 0.64860(15) 0.0230(6) Uani 1 1 d . . . C17 C 0.4570(3) 0.4063(2) 0.62594(16) 0.0272(6) Uani 1 1 d . . . H15 H 0.4871 0.3353 0.6328 0.033 Uiso 1 1 calc R . . C18 C 0.3496(3) 0.4579(2) 0.59365(16) 0.0279(6) Uani 1 1 d . . . C19 C 0.3126(3) 0.5622(2) 0.57953(16) 0.0264(6) Uani 1 1 d . . . H16 H 0.2438 0.5984 0.5542 0.032 Uiso 1 1 calc R . . C20 C 0.3714(3) 0.6170(2) 0.60069(15) 0.0229(6) Uani 1 1 d . . . C21 C 0.6476(3) 0.3951(2) 0.67736(15) 0.0231(6) Uani 1 1 d . . . C22 C 0.7534(3) 0.4471(2) 0.63323(18) 0.0328(7) Uani 1 1 d . . . H17 H 0.7604 0.4496 0.5842 0.039 Uiso 1 1 calc R . . H18 H 0.7314 0.5174 0.6359 0.039 Uiso 1 1 calc R . . C23 C 0.6406(3) 0.3851(2) 0.75398(16) 0.0311(7) Uani 1 1 d . . . H19 H 0.5769 0.3476 0.7819 0.037 Uiso 1 1 calc R . . H20 H 0.6134 0.4532 0.7610 0.037 Uiso 1 1 calc R . . C24 C 0.6882(3) 0.2858(2) 0.67114(19) 0.0348(7) Uani 1 1 d . . . H21 H 0.6236 0.2494 0.6995 0.042 Uiso 1 1 calc R . . H22 H 0.6931 0.2881 0.6223 0.042 Uiso 1 1 calc R . . C25 C 0.8814(3) 0.3886(3) 0.6594(2) 0.0420(8) Uani 1 1 d . . . H23 H 0.9478 0.4243 0.6311 0.050 Uiso 1 1 calc R . . C26 C 0.7702(3) 0.3289(3) 0.77863(18) 0.0392(8) Uani 1 1 d . . . H24 H 0.7639 0.3255 0.8283 0.047 Uiso 1 1 calc R . . C27 C 0.8173(3) 0.2283(2) 0.69542(19) 0.0380(8) Uani 1 1 d . . . H25 H 0.8408 0.1585 0.6904 0.046 Uiso 1 1 calc R . . C28 C 0.8708(3) 0.3840(3) 0.7348(2) 0.0459(9) Uani 1 1 d . . . H26 H 0.8475 0.4534 0.7393 0.055 Uiso 1 1 calc R . . H27 H 0.9535 0.3478 0.7513 0.055 Uiso 1 1 calc R . . C29 C 0.8077(3) 0.2213(3) 0.77149(19) 0.0419(8) Uani 1 1 d . . . H28 H 0.8902 0.1837 0.7879 0.050 Uiso 1 1 calc R . . H29 H 0.7433 0.1847 0.7999 0.050 Uiso 1 1 calc R . . C30 C 0.9185(3) 0.2819(3) 0.6523(2) 0.0444(9) Uani 1 1 d . . . H30 H 0.9266 0.2847 0.6031 0.053 Uiso 1 1 calc R . . H31 H 1.0012 0.2444 0.6684 0.053 Uiso 1 1 calc R . . C31 C 0.2785(4) 0.4032(3) 0.5721(2) 0.0419(8) Uani 1 1 d . . . H32 H 0.3078 0.4057 0.5233 0.063 Uiso 1 1 calc R . . H33 H 0.1877 0.4358 0.5784 0.063 Uiso 1 1 calc R . . H34 H 0.2939 0.3325 0.6006 0.063 Uiso 1 1 calc R . . C32 C 0.3294(3) 0.7331(2) 0.57010(14) 0.0223(6) Uani 1 1 d . . . C33 C 0.3883(3) 0.7973(2) 0.59325(16) 0.0301(6) Uani 1 1 d . . . H35 H 0.4818 0.7735 0.5849 0.036 Uiso 1 1 calc R . . H36 H 0.3619 0.7884 0.6436 0.036 Uiso 1 1 calc R . . C34 C 0.1839(3) 0.7741(2) 0.58471(17) 0.0320(7) Uani 1 1 d . . . H37 H 0.1418 0.7351 0.5704 0.038 Uiso 1 1 calc R . . H38 H 0.1573 0.7651 0.6350 0.038 Uiso 1 1 calc R . . C35 C 0.3701(3) 0.7533(2) 0.49143(16) 0.0324(7) Uani 1 1 d . . . H39 H 0.3344 0.7128 0.4745 0.039 Uiso 1 1 calc R . . H40 H 0.4635 0.7312 0.4815 0.039 Uiso 1 1 calc R . . C36 C 0.3471(4) 0.9115(2) 0.55353(18) 0.0372(8) Uani 1 1 d . . . H41 H 0.3874 0.9512 0.5692 0.045 Uiso 1 1 calc R . . C37 C 0.1426(3) 0.8865(3) 0.54546(19) 0.0397(8) Uani 1 1 d . . . H42 H 0.0483 0.9107 0.5552 0.048 Uiso 1 1 calc R . . C38 C 0.3253(4) 0.8662(3) 0.45220(17) 0.0393(8) Uani 1 1 d . . . H43 H 0.3512 0.8761 0.4013 0.047 Uiso 1 1 calc R . . C39 C 0.3882(4) 0.9248(3) 0.47649(18) 0.0414(8) Uani 1 1 d . . . H44 H 0.4813 0.9001 0.4669 0.050 Uiso 1 1 calc R . . H45 H 0.3642 0.9975 0.4509 0.050 Uiso 1 1 calc R . . C40 C 0.2035(4) 0.9470(3) 0.5690(2) 0.0443(9) Uani 1 1 d . . . H46 H 0.1773 0.9380 0.6193 0.053 Uiso 1 1 calc R . . H47 H 0.1751 1.0198 0.5446 0.053 Uiso 1 1 calc R . . C41 C 0.1828(3) 0.8995(3) 0.46827(19) 0.0419(8) Uani 1 1 d . . . H48 H 0.1441 0.8586 0.4534 0.050 Uiso 1 1 calc R . . H49 H 0.1526 0.9714 0.4423 0.050 Uiso 1 1 calc R . . C42 C 0.2194(3) 0.7911(2) 0.78106(14) 0.0226(6) Uani 1 1 d . . . C43 C 0.1743(3) 0.8967(2) 0.77324(16) 0.0262(6) Uani 1 1 d . A . C44 C 0.0493(3) 0.9407(2) 0.76144(19) 0.0343(7) Uani 1 1 d . . . H50 H 0.0178 1.0117 0.7541 0.041 Uiso 1 1 calc R . . C45 C -0.0319(3) 0.8868(2) 0.75975(18) 0.0341(7) Uani 1 1 d . . . C46 C 0.0127(3) 0.7829(2) 0.77615(17) 0.0306(7) Uani 1 1 d . . . H51 H -0.0437 0.7445 0.7784 0.037 Uiso 1 1 calc R . . C47 C 0.1360(3) 0.7306(2) 0.78967(15) 0.0243(6) Uani 1 1 d . . . C48 C 0.2533(3) 0.9651(2) 0.77599(16) 0.0259(6) Uani 1 1 d . . . C49 C 0.3115(6) 0.9172(4) 0.8446(3) 0.0228(12) Uani 0.50 1 d P A 1 H52 H 0.2431 0.9143 0.8847 0.027 Uiso 0.50 1 calc PR A 1 H53 H 0.3631 0.8474 0.8468 0.027 Uiso 0.50 1 calc PR A 1 C50 C 0.1665(11) 1.0709(8) 0.7807(6) 0.040(3) Uani 0.50 1 d P A 1 H54 H 0.1211 1.1038 0.7400 0.048 Uiso 0.50 1 calc PR A 1 H55 H 0.1027 1.0624 0.8229 0.048 Uiso 0.50 1 calc PR A 1 C51 C 0.3521(8) 0.9765(6) 0.7153(4) 0.0332(16) Uani 0.50 1 d P A 1 H56 H 0.3124 1.0081 0.6725 0.040 Uiso 0.50 1 calc PR A 1 H57 H 0.4074 0.9091 0.7134 0.040 Uiso 0.50 1 calc PR A 1 C52 C 0.3950(7) 0.9824(5) 0.8468(5) 0.0280(14) Uani 0.50 1 d P A 1 H58 H 0.4384 0.9496 0.8889 0.034 Uiso 0.50 1 calc PR A 1 C53 C 0.2457(16) 1.1373(11) 0.7831(7) 0.037(3) Uani 0.50 1 d P A 1 H59 H 0.1902 1.2060 0.7837 0.045 Uiso 0.50 1 calc PR A 1 C54 C 0.4317(11) 1.0425(8) 0.7194(5) 0.0413(18) Uani 0.50 1 d P A 1 H60 H 0.5003 1.0486 0.6787 0.050 Uiso 0.50 1 calc PR A 1 C55 C 0.4880(12) 0.9970(8) 0.7855(7) 0.035(2) Uani 0.50 1 d P A 1 H61 H 0.5481 0.9309 0.7846 0.043 Uiso 0.50 1 calc PR A 1 H62 H 0.5366 1.0417 0.7882 0.043 Uiso 0.50 1 calc PR A 1 C56 C 0.3069(10) 1.0872(9) 0.8504(7) 0.040(3) Uani 0.50 1 d P A 1 H63 H 0.3563 1.1302 0.8546 0.048 Uiso 0.50 1 calc PR A 1 H64 H 0.2404 1.0791 0.8912 0.048 Uiso 0.50 1 calc PR A 1 C57 C 0.3473(13) 1.1464(9) 0.7210(6) 0.048(2) Uani 0.50 1 d P A 1 H65 H 0.3988 1.1894 0.7231 0.058 Uiso 0.50 1 calc PR A 1 H66 H 0.3078 1.1790 0.6782 0.058 Uiso 0.50 1 calc PR A 1 C58 C 0.3792(9) 0.9131(6) 0.8088(5) 0.051(2) Uani 0.50 1 d P A 2 H67 H 0.3582 0.8734 0.8572 0.061 Uiso 0.50 1 calc PR A 2 H68 H 0.4349 0.8650 0.7832 0.061 Uiso 0.50 1 calc PR A 2 C59 C 0.1751(10) 1.0436(9) 0.8117(6) 0.047(3) Uani 0.50 1 d P A 2 H69 H 0.1467 1.0088 0.8603 0.056 Uiso 0.50 1 calc PR A 2 H70 H 0.0986 1.0808 0.7891 0.056 Uiso 0.50 1 calc PR A 2 C60 C 0.3018(8) 1.0263(7) 0.7000(4) 0.0363(17) Uani 0.50 1 d P A 2 H71 H 0.3591 0.9782 0.6749 0.044 Uiso 0.50 1 calc PR A 2 H72 H 0.2286 1.0640 0.6747 0.044 Uiso 0.50 1 calc PR A 2 C61 C 0.4518(16) 0.9847(10) 0.8085(9) 0.063(5) Uani 0.50 1 d P A 2 H73 H 0.5287 0.9465 0.8315 0.075 Uiso 0.50 1 calc PR A 2 C62 C 0.2443(15) 1.1217(13) 0.8115(7) 0.038(3) Uani 0.50 1 d P A 2 H74 H 0.1860 1.1707 0.8364 0.046 Uiso 0.50 1 calc PR A 2 C63 C 0.3718(11) 1.1003(11) 0.7012(4) 0.041(2) Uani 0.50 1 d P A 2 H75 H 0.3996 1.1378 0.6526 0.050 Uiso 0.50 1 calc PR A 2 C64 C 0.4878(9) 1.0441(8) 0.7377(8) 0.051(3) Uani 0.50 1 d P A 2 H76 H 0.5479 0.9986 0.7114 0.061 Uiso 0.50 1 calc PR A 2 H77 H 0.5309 1.0934 0.7389 0.061 Uiso 0.50 1 calc PR A 2 C65 C 0.3610(14) 1.0642(12) 0.8482(6) 0.060(4) Uani 0.50 1 d P A 2 H78 H 0.3343 1.0282 0.8969 0.072 Uiso 0.50 1 calc PR A 2 H79 H 0.4068 1.1124 0.8483 0.072 Uiso 0.50 1 calc PR A 2 C66 C 0.2835(11) 1.1765(8) 0.7390(8) 0.045(2) Uani 0.50 1 d P A 2 H80 H 0.3279 1.2262 0.7380 0.054 Uiso 0.50 1 calc PR A 2 H81 H 0.2079 1.2136 0.7155 0.054 Uiso 0.50 1 calc PR A 2 C67 C -0.1647(3) 0.9381(3) 0.7417(2) 0.0493(10) Uani 1 1 d . . . H82 H -0.2107 0.8868 0.7503 0.074 Uiso 1 1 calc R . . H83 H -0.1598 0.9771 0.6927 0.074 Uiso 1 1 calc R . . H84 H -0.2094 0.9837 0.7704 0.074 Uiso 1 1 calc R . . C68 C 0.1613(3) 0.6143(2) 0.81574(15) 0.0233(6) Uani 1 1 d . . . C69 C 0.1382(3) 0.5724(2) 0.76153(16) 0.0313(7) Uani 1 1 d . . . H85 H 0.0532 0.6085 0.7480 0.038 Uiso 1 1 calc R . . H86 H 0.2018 0.5846 0.7196 0.038 Uiso 1 1 calc R . . C70 C 0.2938(3) 0.5544(2) 0.83518(17) 0.0302(7) Uani 1 1 d . . . H87 H 0.3118 0.5790 0.8701 0.036 Uiso 1 1 calc R . . H88 H 0.3581 0.5665 0.7936 0.036 Uiso 1 1 calc R . . C71 C 0.0650(3) 0.5889(2) 0.88219(17) 0.0317(7) Uani 1 1 d . . . H89 H 0.0810 0.6125 0.9182 0.038 Uiso 1 1 calc R . . H90 H -0.0218 0.6255 0.8718 0.038 Uiso 1 1 calc R . . C72 C 0.1475(3) 0.4580(3) 0.79074(18) 0.0349(7) Uani 1 1 d . . . H91 H 0.1320 0.4330 0.7548 0.042 Uiso 1 1 calc R . . C73 C 0.3040(3) 0.4397(2) 0.86462(18) 0.0353(7) Uani 1 1 d . . . H92 H 0.3907 0.4032 0.8769 0.042 Uiso 1 1 calc R . . C74 C 0.0743(3) 0.4753(3) 0.91010(18) 0.0374(8) Uani 1 1 d . . . H93 H 0.0095 0.4625 0.9522 0.045 Uiso 1 1 calc R . . C75 C 0.0481(3) 0.4396(3) 0.85431(19) 0.0396(8) Uani 1 1 d . . . H94 H 0.0509 0.3667 0.8722 0.048 Uiso 1 1 calc R . . H95 H -0.0373 0.4772 0.8419 0.048 Uiso 1 1 calc R . . C76 C 0.2791(3) 0.4024(3) 0.80984(18) 0.0373(8) Uani 1 1 d . . . H96 H 0.3433 0.4142 0.7681 0.045 Uiso 1 1 calc R . . H97 H 0.2861 0.3288 0.8278 0.045 Uiso 1 1 calc R . . C77 C 0.2046(4) 0.4194(3) 0.92931(18) 0.0403(8) Uani 1 1 d . . . H98 H 0.2108 0.3459 0.9478 0.048 Uiso 1 1 calc R . . H99 H 0.2201 0.4427 0.9656 0.048 Uiso 1 1 calc R . . C78 C 1.1446(7) 0.7394(7) 1.0091(4) 0.133(3) Uani 1 1 d . . . H100 H 1.2130 0.7680 0.9783 0.199 Uiso 1 1 calc R . . H101 H 1.1657 0.6667 1.0142 0.199 Uiso 1 1 calc R . . H102 H 1.1343 0.7500 1.0546 0.199 Uiso 1 1 calc R . . C79 C 1.0178(8) 0.7930(7) 0.9776(4) 0.132(3) Uani 1 1 d . . . H103 H 1.0361 0.7921 0.9286 0.158 Uiso 1 1 calc R . . H104 H 0.9579 0.7503 1.0019 0.158 Uiso 1 1 calc R . . C80 C 0.9525(9) 0.8948(7) 0.9786(3) 0.129(4) Uani 1 1 d . . . H105 H 1.0072 0.9399 0.9495 0.155 Uiso 1 1 calc R . . H106 H 0.9406 0.8985 1.0266 0.155 Uiso 1 1 calc R . . C81 C 0.8216(7) 0.9358(6) 0.9531(4) 0.109(3) Uani 1 1 d . . . H107 H 0.8322 0.9259 0.9069 0.131 Uiso 1 1 calc R . . H108 H 0.7643 0.8947 0.9850 0.131 Uiso 1 1 calc R . . C82 C 0.7612(10) 1.0412(7) 0.9481(4) 0.133(4) Uani 1 1 d . . . H109 H 0.8128 1.0839 0.9125 0.160 Uiso 1 1 calc R . . H110 H 0.7557 1.0536 0.9930 0.160 Uiso 1 1 calc R . . C83 C 0.6343(8) 1.0691(6) 0.9299(4) 0.119(3) Uani 1 1 d . . . H111 H 0.6375 1.0439 0.8910 0.178 Uiso 1 1 calc R . . H112 H 0.6024 1.1429 0.9166 0.178 Uiso 1 1 calc R . . H113 H 0.5777 1.0391 0.9698 0.178 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 0.01915(14) 0.02290(15) 0.02969(16) -0.01058(11) -0.00330(10) -0.00460(10) O1 0.0202(9) 0.0211(10) 0.0299(11) -0.0107(8) -0.0062(8) -0.0034(8) O2 0.0190(9) 0.0222(10) 0.0295(11) -0.0073(8) -0.0025(8) -0.0056(8) C1 0.0284(16) 0.0363(18) 0.0400(18) -0.0148(15) -0.0101(13) -0.0028(13) C2 0.0316(16) 0.0296(16) 0.0338(17) -0.0091(13) -0.0158(13) -0.0002(13) C3 0.0370(19) 0.075(3) 0.045(2) -0.025(2) -0.0076(16) -0.0116(19) C4 0.047(2) 0.089(4) 0.054(3) -0.038(3) -0.013(2) 0.005(2) C5 0.068(3) 0.050(3) 0.069(3) -0.033(2) -0.032(2) 0.004(2) C6 0.082(3) 0.052(3) 0.060(3) -0.012(2) -0.032(2) -0.025(2) C7 0.051(2) 0.054(2) 0.045(2) -0.0152(18) -0.0130(17) -0.0186(19) C8 0.0254(15) 0.0355(17) 0.0360(17) -0.0140(14) 0.0013(12) -0.0139(13) C9 0.0222(14) 0.0309(16) 0.0370(17) -0.0104(13) 0.0022(12) -0.0140(12) C10 0.0278(15) 0.0368(18) 0.0362(17) -0.0088(14) -0.0012(13) -0.0127(13) C11 0.0370(18) 0.055(2) 0.0308(17) -0.0122(16) 0.0038(14) -0.0222(16) C12 0.0288(16) 0.048(2) 0.046(2) -0.0211(17) 0.0074(14) -0.0133(15) C13 0.0233(15) 0.0410(19) 0.050(2) -0.0135(16) 0.0011(14) -0.0108(14) C14 0.0252(15) 0.0433(19) 0.0351(17) -0.0102(15) -0.0013(12) -0.0144(14) C15 0.0203(13) 0.0202(13) 0.0234(13) -0.0078(11) -0.0021(10) -0.0048(10) C16 0.0237(13) 0.0195(13) 0.0239(14) -0.0062(11) -0.0043(11) -0.0019(11) C17 0.0305(15) 0.0190(14) 0.0314(16) -0.0068(12) -0.0060(12) -0.0044(12) C18 0.0283(15) 0.0260(15) 0.0316(16) -0.0081(12) -0.0068(12) -0.0084(12) C19 0.0229(14) 0.0269(15) 0.0295(15) -0.0076(12) -0.0074(11) -0.0040(12) C20 0.0212(13) 0.0205(13) 0.0232(14) -0.0036(11) -0.0012(10) -0.0045(11) C21 0.0216(13) 0.0172(13) 0.0288(15) -0.0064(11) -0.0065(11) -0.0006(10) C22 0.0237(15) 0.0266(16) 0.0410(18) -0.0052(14) -0.0033(13) -0.0024(12) C23 0.0263(15) 0.0331(17) 0.0304(16) -0.0099(13) -0.0066(12) 0.0000(13) C24 0.0384(18) 0.0222(15) 0.0445(19) -0.0119(14) -0.0190(15) 0.0036(13) C25 0.0193(15) 0.0368(19) 0.058(2) -0.0040(17) -0.0039(14) -0.0025(13) C26 0.0334(17) 0.042(2) 0.0351(18) -0.0122(15) -0.0147(14) 0.0079(15) C27 0.0378(18) 0.0200(15) 0.050(2) -0.0103(15) -0.0163(15) 0.0090(13) C28 0.0277(17) 0.038(2) 0.075(3) -0.0224(19) -0.0224(17) 0.0045(14) C29 0.0374(18) 0.0330(18) 0.041(2) 0.0032(15) -0.0137(15) 0.0013(15) C30 0.0321(18) 0.041(2) 0.045(2) -0.0108(17) -0.0042(15) 0.0098(15) C31 0.047(2) 0.0289(17) 0.058(2) -0.0135(16) -0.0241(18) -0.0079(15) C32 0.0225(13) 0.0180(13) 0.0240(14) -0.0053(11) -0.0024(10) -0.0035(11) C33 0.0350(16) 0.0244(15) 0.0301(16) -0.0045(12) -0.0079(13) -0.0076(13) C34 0.0249(15) 0.0277(16) 0.0364(17) -0.0042(13) -0.0043(12) -0.0025(12) C35 0.0345(16) 0.0312(17) 0.0286(16) -0.0070(13) -0.0029(13) -0.0071(13) C36 0.050(2) 0.0252(16) 0.0373(18) -0.0064(14) -0.0110(15) -0.0100(15) C37 0.0293(16) 0.0335(18) 0.044(2) -0.0033(15) -0.0070(14) 0.0014(14) C38 0.049(2) 0.0399(19) 0.0235(16) -0.0033(14) -0.0019(14) -0.0126(16) C39 0.049(2) 0.0362(19) 0.0371(19) -0.0019(15) -0.0038(15) -0.0189(16) C40 0.058(2) 0.0243(17) 0.042(2) -0.0076(15) -0.0055(17) -0.0017(16) C41 0.044(2) 0.0328(18) 0.041(2) -0.0002(15) -0.0182(16) -0.0012(15) C42 0.0186(12) 0.0238(14) 0.0220(13) -0.0045(11) -0.0019(10) -0.0037(11) C43 0.0258(14) 0.0215(14) 0.0303(15) -0.0054(12) -0.0043(11) -0.0067(11) C44 0.0273(15) 0.0242(15) 0.050(2) -0.0089(14) -0.0118(14) -0.0025(12) C45 0.0238(15) 0.0294(16) 0.0458(19) -0.0051(14) -0.0108(13) -0.0040(12) C46 0.0227(14) 0.0282(15) 0.0402(18) -0.0053(13) -0.0067(12) -0.0087(12) C47 0.0211(13) 0.0240(14) 0.0263(14) -0.0066(12) -0.0027(11) -0.0050(11) C48 0.0245(14) 0.0186(14) 0.0343(16) -0.0066(12) -0.0084(12) -0.0032(11) C49 0.025(3) 0.015(3) 0.029(3) -0.009(2) -0.003(2) -0.005(2) C50 0.036(4) 0.021(4) 0.062(7) -0.001(4) -0.025(5) -0.002(3) C51 0.053(5) 0.030(4) 0.025(4) -0.006(3) 0.000(3) -0.027(4) C52 0.039(4) 0.014(3) 0.036(4) -0.003(3) -0.019(3) -0.006(3) C53 0.045(7) 0.021(5) 0.048(8) -0.010(7) -0.016(8) -0.004(4) C54 0.039(5) 0.038(5) 0.048(5) -0.011(4) 0.006(4) -0.022(5) C55 0.052(6) 0.022(5) 0.042(7) -0.004(6) -0.010(5) -0.026(4) C56 0.033(5) 0.023(4) 0.066(7) -0.023(4) -0.005(5) -0.003(4) C57 0.067(7) 0.028(6) 0.053(7) 0.008(5) -0.016(6) -0.034(5) C58 0.055(5) 0.031(4) 0.075(6) -0.003(4) -0.040(5) -0.013(4) C59 0.038(5) 0.052(8) 0.066(7) -0.041(6) 0.019(5) -0.025(5) C60 0.051(5) 0.036(4) 0.029(4) -0.011(4) 0.003(3) -0.024(4) C61 0.090(13) 0.043(6) 0.055(9) 0.037(7) -0.038(8) -0.052(8) C62 0.033(6) 0.040(8) 0.049(8) -0.032(7) 0.008(8) -0.010(6) C63 0.060(6) 0.046(6) 0.030(4) -0.015(4) 0.007(4) -0.035(5) C64 0.024(4) 0.055(6) 0.091(9) -0.050(7) 0.011(5) -0.014(4) C65 0.086(10) 0.094(14) 0.027(4) -0.016(6) -0.007(6) -0.062(9) C66 0.046(6) 0.022(5) 0.068(7) -0.012(5) -0.022(5) -0.002(4) C67 0.0290(18) 0.0349(19) 0.079(3) -0.0046(19) -0.0220(18) -0.0028(15) C68 0.0224(13) 0.0221(14) 0.0253(14) -0.0045(11) -0.0038(11) -0.0077(11) C69 0.0328(16) 0.0339(17) 0.0286(16) -0.0071(13) -0.0027(12) -0.0135(13) C70 0.0274(15) 0.0254(15) 0.0370(17) -0.0044(13) -0.0061(12) -0.0093(12) C71 0.0319(16) 0.0302(16) 0.0317(16) -0.0081(13) 0.0015(13) -0.0114(13) C72 0.0412(18) 0.0330(17) 0.0370(18) -0.0149(14) -0.0032(14) -0.0151(14) C73 0.0356(17) 0.0239(16) 0.0435(19) -0.0033(14) -0.0085(14) -0.0082(13) C74 0.0412(19) 0.0330(17) 0.0348(18) -0.0069(14) 0.0067(14) -0.0171(15) C75 0.0407(19) 0.0347(18) 0.045(2) -0.0063(15) -0.0012(15) -0.0208(15) C76 0.0379(18) 0.0280(17) 0.0427(19) -0.0104(15) 0.0018(14) -0.0091(14) C77 0.053(2) 0.0269(17) 0.0364(19) 0.0004(14) -0.0080(16) -0.0136(15) C78 0.121(6) 0.211(9) 0.099(5) -0.021(6) -0.013(5) -0.116(7) C79 0.165(8) 0.160(8) 0.120(6) -0.076(6) 0.051(6) -0.123(7) C80 0.194(9) 0.183(8) 0.073(4) -0.056(5) 0.039(5) -0.155(8) C81 0.128(6) 0.141(6) 0.106(5) -0.080(5) 0.041(4) -0.092(5) C82 0.222(10) 0.159(8) 0.062(4) -0.017(4) 0.000(5) -0.140(8) C83 0.113(6) 0.151(7) 0.095(5) -0.043(5) 0.029(4) -0.060(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.9307(19) . ? Zr1 O2 1.931(2) . ? Zr1 C1 2.266(3) . ? Zr1 C8 2.271(3) . ? O1 C15 1.379(3) . ? O2 C42 1.378(3) . ? C1 C2 1.486(4) . ? C1 H1 0.9900 . ? C1 H2 0.9900 . ? C2 C3 1.381(5) . ? C2 C7 1.402(5) . ? C3 C4 1.412(6) . ? C3 H3 0.9500 . ? C4 C5 1.369(7) . ? C4 H4 0.9500 . ? C5 C6 1.353(7) . ? C5 H5 0.9500 . ? C6 C7 1.381(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.493(4) . ? C8 H8 0.9900 . ? C8 H9 0.9900 . ? C9 C14 1.396(4) . ? C9 C10 1.396(5) . ? C10 C11 1.386(5) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C13 1.378(5) . ? C12 H12 0.9500 . ? C13 C14 1.387(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.410(4) . ? C15 C16 1.427(4) . ? C16 C17 1.399(4) . ? C16 C21 1.544(4) . ? C17 C18 1.394(4) . ? C17 H15 0.9500 . ? C18 C19 1.385(4) . ? C18 C31 1.506(4) . ? C19 C20 1.399(4) . ? C19 H16 0.9500 . ? C20 C32 1.547(4) . ? C21 C23 1.531(4) . ? C21 C22 1.549(4) . ? C21 C24 1.549(4) . ? C22 C25 1.543(4) . ? C22 H17 0.9900 . ? C22 H18 0.9900 . ? C23 C26 1.541(4) . ? C23 H19 0.9900 . ? C23 H20 0.9900 . ? C24 C27 1.537(4) . ? C24 H21 0.9900 . ? C24 H22 0.9900 . ? C25 C28 1.518(6) . ? C25 C30 1.522(5) . ? C25 H23 1.0000 . ? C26 C28 1.528(6) . ? C26 C29 1.534(5) . ? C26 H24 1.0000 . ? C27 C30 1.517(5) . ? C27 C29 1.526(5) . ? C27 H25 1.0000 . ? C28 H26 0.9900 . ? C28 H27 0.9900 . ? C29 H28 0.9900 . ? C29 H29 0.9900 . ? C30 H30 0.9900 . ? C30 H31 0.9900 . ? C31 H32 0.9800 . ? C31 H33 0.9800 . ? C31 H34 0.9800 . ? C32 C35 1.538(4) . ? C32 C33 1.540(4) . ? C32 C34 1.549(4) . ? C33 C36 1.556(4) . ? C33 H35 0.9900 . ? C33 H36 0.9900 . ? C34 C37 1.532(4) . ? C34 H37 0.9900 . ? C34 H38 0.9900 . ? C35 C38 1.543(5) . ? C35 H39 0.9900 . ? C35 H40 0.9900 . ? C36 C39 1.517(5) . ? C36 C40 1.524(5) . ? C36 H41 1.0000 . ? C37 C40 1.517(5) . ? C37 C41 1.520(5) . ? C37 H42 1.0000 . ? C38 C41 1.511(5) . ? C38 C39 1.518(5) . ? C38 H43 1.0000 . ? C39 H44 0.9900 . ? C39 H45 0.9900 . ? C40 H46 0.9900 . ? C40 H47 0.9900 . ? C41 H48 0.9900 . ? C41 H49 0.9900 . ? C42 C47 1.418(4) . ? C42 C43 1.421(4) . ? C43 C44 1.392(4) . ? C43 C48 1.544(4) . ? C44 C45 1.387(4) . ? C44 H50 0.9500 . ? C45 C46 1.380(5) . ? C45 C67 1.518(4) . ? C46 C47 1.399(4) . ? C46 H51 0.9500 . ? C47 C68 1.543(4) . ? C48 C51 1.470(8) . ? C48 C59 1.501(11) . ? C48 C49 1.556(7) . ? C48 C50 1.562(12) . ? C48 C58 1.574(8) . ? C48 C60 1.588(8) . ? C49 C52 1.543(9) . ? C49 H52 0.9900 . ? C49 H53 0.9900 . ? C50 C53 1.52(2) . ? C50 H54 0.9900 . ? C50 H55 0.9900 . ? C51 C54 1.532(12) . ? C51 H56 0.9900 . ? C51 H57 0.9900 . ? C52 C55 1.443(13) . ? C52 C56 1.550(11) . ? C52 H58 1.0000 . ? C53 C57 1.505(17) . ? C53 C56 1.550(18) . ? C53 H59 1.0000 . ? C54 C55 1.502(16) . ? C54 C57 1.518(15) . ? C54 H60 1.0000 . ? C55 H61 0.9900 . ? C55 H62 0.9900 . ? C56 H63 0.9900 . ? C56 H64 0.9900 . ? C57 H65 0.9900 . ? C57 H66 0.9900 . ? C58 C61 1.506(14) . ? C58 H67 0.9900 . ? C58 H68 0.9900 . ? C59 C62 1.56(2) . ? C59 H69 0.9900 . ? C59 H70 0.9900 . ? C60 C63 1.525(12) . ? C60 H71 0.9900 . ? C60 H72 0.9900 . ? C61 C64 1.465(14) . ? C61 C65 1.60(2) . ? C61 H73 1.0000 . ? C62 C66 1.478(15) . ? C62 C65 1.535(19) . ? C62 H74 1.0000 . ? C63 C64 1.524(14) . ? C63 C66 1.534(13) . ? C63 H75 1.0000 . ? C64 H76 0.9900 . ? C64 H77 0.9900 . ? C65 H78 0.9900 . ? C65 H79 0.9900 . ? C66 H80 0.9900 . ? C66 H81 0.9900 . ? C67 H82 0.9800 . ? C67 H83 0.9800 . ? C67 H84 0.9800 . ? C68 C70 1.541(4) . ? C68 C69 1.548(4) . ? C68 C71 1.552(4) . ? C69 C72 1.542(4) . ? C69 H85 0.9900 . ? C69 H86 0.9900 . ? C70 C73 1.544(4) . ? C70 H87 0.9900 . ? C70 H88 0.9900 . ? C71 C74 1.531(4) . ? C71 H89 0.9900 . ? C71 H90 0.9900 . ? C72 C75 1.520(5) . ? C72 C76 1.521(5) . ? C72 H91 1.0000 . ? C73 C76 1.522(5) . ? C73 C77 1.538(5) . ? C73 H92 1.0000 . ? C74 C77 1.509(5) . ? C74 C75 1.533(5) . ? C74 H93 1.0000 . ? C75 H94 0.9900 . ? C75 H95 0.9900 . ? C76 H96 0.9900 . ? C76 H97 0.9900 . ? C77 H98 0.9900 . ? C77 H99 0.9900 . ? C78 C79 1.571(11) . ? C78 H100 0.9800 . ? C78 H101 0.9800 . ? C78 H102 0.9800 . ? C79 C80 1.435(11) . ? C79 H103 0.9900 . ? C79 H104 0.9900 . ? C80 C81 1.551(11) . ? C80 H105 0.9900 . ? C80 H106 0.9900 . ? C81 C82 1.446(11) . ? C81 H107 0.9900 . ? C81 H108 0.9900 . ? C82 C83 1.460(10) . ? C82 H109 0.9900 . ? C82 H110 0.9900 . ? C83 H111 0.9800 . ? C83 H112 0.9800 . ? C83 H113 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr1 O2 118.96(8) . . ? O1 Zr1 C1 110.53(10) . . ? O2 Zr1 C1 104.63(11) . . ? O1 Zr1 C8 105.81(10) . . ? O2 Zr1 C8 111.90(10) . . ? C1 Zr1 C8 104.10(13) . . ? C15 O1 Zr1 156.45(17) . . ? C42 O2 Zr1 154.42(18) . . ? C2 C1 Zr1 109.8(2) . . ? C2 C1 H1 109.7 . . ? Zr1 C1 H1 109.7 . . ? C2 C1 H2 109.7 . . ? Zr1 C1 H2 109.7 . . ? H1 C1 H2 108.2 . . ? C3 C2 C7 117.0(3) . . ? C3 C2 C1 122.5(3) . . ? C7 C2 C1 120.5(3) . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.5(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.7(4) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 122.4(4) . . ? C6 C7 H7 118.8 . . ? C2 C7 H7 118.8 . . ? C9 C8 Zr1 110.6(2) . . ? C9 C8 H8 109.5 . . ? Zr1 C8 H8 109.5 . . ? C9 C8 H9 109.5 . . ? Zr1 C8 H9 109.5 . . ? H8 C8 H9 108.1 . . ? C14 C9 C10 117.4(3) . . ? C14 C9 C8 121.0(3) . . ? C10 C9 C8 121.5(3) . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 119.3(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 121.3(3) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? O1 C15 C20 120.4(2) . . ? O1 C15 C16 118.1(2) . . ? C20 C15 C16 121.4(3) . . ? C17 C16 C15 116.9(3) . . ? C17 C16 C21 119.9(2) . . ? C15 C16 C21 123.1(2) . . ? C18 C17 C16 122.7(3) . . ? C18 C17 H15 118.7 . . ? C16 C17 H15 118.7 . . ? C19 C18 C17 117.7(3) . . ? C19 C18 C31 120.6(3) . . ? C17 C18 C31 121.6(3) . . ? C18 C19 C20 123.4(3) . . ? C18 C19 H16 118.3 . . ? C20 C19 H16 118.3 . . ? C19 C20 C15 116.9(3) . . ? C19 C20 C32 114.9(2) . . ? C15 C20 C32 127.8(2) . . ? C23 C21 C16 113.5(2) . . ? C23 C21 C22 110.2(3) . . ? C16 C21 C22 108.8(2) . . ? C23 C21 C24 106.2(2) . . ? C16 C21 C24 111.1(2) . . ? C22 C21 C24 106.8(2) . . ? C25 C22 C21 110.5(3) . . ? C25 C22 H17 109.6 . . ? C21 C22 H17 109.6 . . ? C25 C22 H18 109.6 . . ? C21 C22 H18 109.6 . . ? H17 C22 H18 108.1 . . ? C21 C23 C26 111.0(3) . . ? C21 C23 H19 109.4 . . ? C26 C23 H19 109.4 . . ? C21 C23 H20 109.4 . . ? C26 C23 H20 109.4 . . ? H19 C23 H20 108.0 . . ? C27 C24 C21 111.2(3) . . ? C27 C24 H21 109.4 . . ? C21 C24 H21 109.4 . . ? C27 C24 H22 109.4 . . ? C21 C24 H22 109.4 . . ? H21 C24 H22 108.0 . . ? C28 C25 C30 109.8(3) . . ? C28 C25 C22 109.7(3) . . ? C30 C25 C22 109.7(3) . . ? C28 C25 H23 109.2 . . ? C30 C25 H23 109.2 . . ? C22 C25 H23 109.2 . . ? C28 C26 C29 109.3(3) . . ? C28 C26 C23 110.3(3) . . ? C29 C26 C23 109.0(3) . . ? C28 C26 H24 109.4 . . ? C29 C26 H24 109.4 . . ? C23 C26 H24 109.4 . . ? C30 C27 C29 109.9(3) . . ? C30 C27 C24 110.6(3) . . ? C29 C27 C24 109.2(3) . . ? C30 C27 H25 109.1 . . ? C29 C27 H25 109.1 . . ? C24 C27 H25 109.1 . . ? C25 C28 C26 109.6(3) . . ? C25 C28 H26 109.7 . . ? C26 C28 H26 109.7 . . ? C25 C28 H27 109.7 . . ? C26 C28 H27 109.7 . . ? H26 C28 H27 108.2 . . ? C27 C29 C26 108.5(3) . . ? C27 C29 H28 110.0 . . ? C26 C29 H28 110.0 . . ? C27 C29 H29 110.0 . . ? C26 C29 H29 110.0 . . ? H28 C29 H29 108.4 . . ? C27 C30 C25 108.8(3) . . ? C27 C30 H30 109.9 . . ? C25 C30 H30 109.9 . . ? C27 C30 H31 109.9 . . ? C25 C30 H31 109.9 . . ? H30 C30 H31 108.3 . . ? C18 C31 H32 109.5 . . ? C18 C31 H33 109.5 . . ? H32 C31 H33 109.5 . . ? C18 C31 H34 109.5 . . ? H32 C31 H34 109.5 . . ? H33 C31 H34 109.5 . . ? C35 C32 C33 106.7(2) . . ? C35 C32 C20 105.5(2) . . ? C33 C32 C20 117.1(2) . . ? C35 C32 C34 108.8(2) . . ? C33 C32 C34 106.6(2) . . ? C20 C32 C34 111.8(2) . . ? C32 C33 C36 111.5(2) . . ? C32 C33 H35 109.3 . . ? C36 C33 H35 109.3 . . ? C32 C33 H36 109.3 . . ? C36 C33 H36 109.3 . . ? H35 C33 H36 108.0 . . ? C37 C34 C32 111.0(3) . . ? C37 C34 H37 109.4 . . ? C32 C34 H37 109.4 . . ? C37 C34 H38 109.4 . . ? C32 C34 H38 109.4 . . ? H37 C34 H38 108.0 . . ? C32 C35 C38 112.0(3) . . ? C32 C35 H39 109.2 . . ? C38 C35 H39 109.2 . . ? C32 C35 H40 109.2 . . ? C38 C35 H40 109.2 . . ? H39 C35 H40 107.9 . . ? C39 C36 C40 110.1(3) . . ? C39 C36 C33 109.1(3) . . ? C40 C36 C33 108.3(3) . . ? C39 C36 H41 109.8 . . ? C40 C36 H41 109.8 . . ? C33 C36 H41 109.8 . . ? C40 C37 C41 110.0(3) . . ? C40 C37 C34 109.6(3) . . ? C41 C37 C34 109.1(3) . . ? C40 C37 H42 109.4 . . ? C41 C37 H42 109.4 . . ? C34 C37 H42 109.4 . . ? C41 C38 C39 111.2(3) . . ? C41 C38 C35 108.8(3) . . ? C39 C38 C35 107.5(3) . . ? C41 C38 H43 109.8 . . ? C39 C38 H43 109.8 . . ? C35 C38 H43 109.8 . . ? C36 C39 C38 109.9(3) . . ? C36 C39 H44 109.7 . . ? C38 C39 H44 109.7 . . ? C36 C39 H45 109.7 . . ? C38 C39 H45 109.7 . . ? H44 C39 H45 108.2 . . ? C37 C40 C36 109.7(3) . . ? C37 C40 H46 109.7 . . ? C36 C40 H46 109.7 . . ? C37 C40 H47 109.7 . . ? C36 C40 H47 109.7 . . ? H46 C40 H47 108.2 . . ? C38 C41 C37 110.2(3) . . ? C38 C41 H48 109.6 . . ? C37 C41 H48 109.6 . . ? C38 C41 H49 109.6 . . ? C37 C41 H49 109.6 . . ? H48 C41 H49 108.1 . . ? O2 C42 C47 119.6(2) . . ? O2 C42 C43 118.8(2) . . ? C47 C42 C43 121.5(2) . . ? C44 C43 C42 116.4(3) . . ? C44 C43 C48 118.4(3) . . ? C42 C43 C48 125.2(3) . . ? C45 C44 C43 123.8(3) . . ? C45 C44 H50 118.1 . . ? C43 C44 H50 118.1 . . ? C46 C45 C44 117.0(3) . . ? C46 C45 C67 120.7(3) . . ? C44 C45 C67 122.3(3) . . ? C45 C46 C47 124.0(3) . . ? C45 C46 H51 118.0 . . ? C47 C46 H51 118.0 . . ? C46 C47 C42 116.0(3) . . ? C46 C47 C68 115.5(2) . . ? C42 C47 C68 128.4(2) . . ? C51 C48 C59 127.9(6) . . ? C51 C48 C43 110.7(4) . . ? C59 C48 C43 111.5(5) . . ? C51 C48 C49 111.4(5) . . ? C59 C48 C49 82.6(6) . . ? C43 C48 C49 108.1(3) . . ? C51 C48 C50 110.4(6) . . ? C59 C48 C50 24.1(5) . . ? C43 C48 C50 110.8(5) . . ? C49 C48 C50 105.3(5) . . ? C51 C48 C58 77.0(6) . . ? C59 C48 C58 107.6(6) . . ? C43 C48 C58 118.1(3) . . ? C49 C48 C58 34.7(4) . . ? C50 C48 C58 123.7(5) . . ? C51 C48 C60 29.5(4) . . ? C59 C48 C60 105.7(6) . . ? C43 C48 C60 110.5(3) . . ? C49 C48 C60 133.6(4) . . ? C50 C48 C60 84.0(5) . . ? C58 C48 C60 102.5(5) . . ? C52 C49 C48 108.8(5) . . ? C52 C49 H52 109.9 . . ? C48 C49 H52 109.9 . . ? C52 C49 H53 109.9 . . ? C48 C49 H53 109.9 . . ? H52 C49 H53 108.3 . . ? C53 C50 C48 110.1(9) . . ? C53 C50 H54 109.6 . . ? C48 C50 H54 109.6 . . ? C53 C50 H55 109.6 . . ? C48 C50 H55 109.6 . . ? H54 C50 H55 108.2 . . ? C48 C51 C54 110.2(6) . . ? C48 C51 H56 109.6 . . ? C54 C51 H56 109.6 . . ? C48 C51 H57 109.6 . . ? C54 C51 H57 109.6 . . ? H56 C51 H57 108.1 . . ? C55 C52 C49 111.7(7) . . ? C55 C52 C56 108.4(9) . . ? C49 C52 C56 107.5(6) . . ? C55 C52 H58 109.7 . . ? C49 C52 H58 109.7 . . ? C56 C52 H58 109.7 . . ? C57 C53 C50 110.1(11) . . ? C57 C53 C56 109.9(12) . . ? C50 C53 C56 107.9(10) . . ? C57 C53 H59 109.6 . . ? C50 C53 H59 109.6 . . ? C56 C53 H59 109.6 . . ? C55 C54 C57 107.1(8) . . ? C55 C54 C51 109.8(7) . . ? C57 C54 C51 109.5(9) . . ? C55 C54 H60 110.1 . . ? C57 C54 H60 110.1 . . ? C51 C54 H60 110.1 . . ? C52 C55 C54 113.5(11) . . ? C52 C55 H61 108.9 . . ? C54 C55 H61 108.9 . . ? C52 C55 H62 108.9 . . ? C54 C55 H62 108.9 . . ? H61 C55 H62 107.7 . . ? C52 C56 C53 108.2(10) . . ? C52 C56 H63 110.1 . . ? C53 C56 H63 110.1 . . ? C52 C56 H64 110.1 . . ? C53 C56 H64 110.1 . . ? H63 C56 H64 108.4 . . ? C53 C57 C54 110.1(9) . . ? C53 C57 H65 109.6 . . ? C54 C57 H65 109.6 . . ? C53 C57 H66 109.6 . . ? C54 C57 H66 109.6 . . ? H65 C57 H66 108.2 . . ? C61 C58 C48 114.9(8) . . ? C61 C58 H67 108.5 . . ? C48 C58 H67 108.5 . . ? C61 C58 H68 108.5 . . ? C48 C58 H68 108.5 . . ? H67 C58 H68 107.5 . . ? C48 C59 C62 114.9(9) . . ? C48 C59 H69 108.5 . . ? C62 C59 H69 108.5 . . ? C48 C59 H70 108.5 . . ? C62 C59 H70 108.5 . . ? H69 C59 H70 107.5 . . ? C63 C60 C48 111.6(6) . . ? C63 C60 H71 109.3 . . ? C48 C60 H71 109.3 . . ? C63 C60 H72 109.3 . . ? C48 C60 H72 109.3 . . ? H71 C60 H72 108.0 . . ? C64 C61 C58 110.9(12) . . ? C64 C61 C65 106.3(10) . . ? C58 C61 C65 108.6(12) . . ? C64 C61 H73 110.3 . . ? C58 C61 H73 110.3 . . ? C65 C61 H73 110.3 . . ? C66 C62 C65 110.1(12) . . ? C66 C62 C59 108.9(10) . . ? C65 C62 C59 108.5(12) . . ? C66 C62 H74 109.7 . . ? C65 C62 H74 109.7 . . ? C59 C62 H74 109.7 . . ? C64 C63 C60 110.6(10) . . ? C64 C63 C66 109.3(7) . . ? C60 C63 C66 109.9(8) . . ? C64 C63 H75 109.0 . . ? C60 C63 H75 109.0 . . ? C66 C63 H75 109.0 . . ? C61 C64 C63 110.8(9) . . ? C61 C64 H76 109.5 . . ? C63 C64 H76 109.5 . . ? C61 C64 H77 109.5 . . ? C63 C64 H77 109.5 . . ? H76 C64 H77 108.1 . . ? C62 C65 C61 109.0(10) . . ? C62 C65 H78 109.9 . . ? C61 C65 H78 109.9 . . ? C62 C65 H79 109.9 . . ? C61 C65 H79 109.9 . . ? H78 C65 H79 108.3 . . ? C62 C66 C63 109.2(10) . . ? C62 C66 H80 109.8 . . ? C63 C66 H80 109.8 . . ? C62 C66 H81 109.8 . . ? C63 C66 H81 109.8 . . ? H80 C66 H81 108.3 . . ? C45 C67 H82 109.5 . . ? C45 C67 H83 109.5 . . ? H82 C67 H83 109.5 . . ? C45 C67 H84 109.5 . . ? H82 C67 H84 109.5 . . ? H83 C67 H84 109.5 . . ? C70 C68 C47 117.0(2) . . ? C70 C68 C69 106.9(2) . . ? C47 C68 C69 110.8(2) . . ? C70 C68 C71 106.6(2) . . ? C47 C68 C71 107.0(2) . . ? C69 C68 C71 108.2(2) . . ? C72 C69 C68 111.0(3) . . ? C72 C69 H85 109.4 . . ? C68 C69 H85 109.4 . . ? C72 C69 H86 109.4 . . ? C68 C69 H86 109.4 . . ? H85 C69 H86 108.0 . . ? C68 C70 C73 111.8(2) . . ? C68 C70 H87 109.3 . . ? C73 C70 H87 109.3 . . ? C68 C70 H88 109.3 . . ? C73 C70 H88 109.3 . . ? H87 C70 H88 107.9 . . ? C74 C71 C68 111.9(3) . . ? C74 C71 H89 109.2 . . ? C68 C71 H89 109.2 . . ? C74 C71 H90 109.2 . . ? C68 C71 H90 109.2 . . ? H89 C71 H90 107.9 . . ? C75 C72 C76 110.1(3) . . ? C75 C72 C69 109.3(3) . . ? C76 C72 C69 109.4(3) . . ? C75 C72 H91 109.3 . . ? C76 C72 H91 109.3 . . ? C69 C72 H91 109.3 . . ? C76 C73 C77 108.9(3) . . ? C76 C73 C70 108.7(3) . . ? C77 C73 C70 110.0(3) . . ? C76 C73 H92 109.7 . . ? C77 C73 H92 109.7 . . ? C70 C73 H92 109.7 . . ? C77 C74 C71 109.5(3) . . ? C77 C74 C75 110.6(3) . . ? C71 C74 C75 108.9(3) . . ? C77 C74 H93 109.3 . . ? C71 C74 H93 109.3 . . ? C75 C74 H93 109.3 . . ? C72 C75 C74 109.2(3) . . ? C72 C75 H94 109.8 . . ? C74 C75 H94 109.8 . . ? C72 C75 H95 109.8 . . ? C74 C75 H95 109.8 . . ? H94 C75 H95 108.3 . . ? C72 C76 C73 109.9(3) . . ? C72 C76 H96 109.7 . . ? C73 C76 H96 109.7 . . ? C72 C76 H97 109.7 . . ? C73 C76 H97 109.7 . . ? H96 C76 H97 108.2 . . ? C74 C77 C73 109.2(3) . . ? C74 C77 H98 109.8 . . ? C73 C77 H98 109.8 . . ? C74 C77 H99 109.8 . . ? C73 C77 H99 109.8 . . ? H98 C77 H99 108.3 . . ? C79 C78 H100 109.5 . . ? C79 C78 H101 109.5 . . ? H100 C78 H101 109.5 . . ? C79 C78 H102 109.5 . . ? H100 C78 H102 109.5 . . ? H101 C78 H102 109.5 . . ? C80 C79 C78 120.1(7) . . ? C80 C79 H103 107.3 . . ? C78 C79 H103 107.3 . . ? C80 C79 H104 107.3 . . ? C78 C79 H104 107.3 . . ? H103 C79 H104 106.9 . . ? C79 C80 C81 115.5(6) . . ? C79 C80 H105 108.4 . . ? C81 C80 H105 108.4 . . ? C79 C80 H106 108.4 . . ? C81 C80 H106 108.4 . . ? H105 C80 H106 107.5 . . ? C82 C81 C80 115.5(6) . . ? C82 C81 H107 108.4 . . ? C80 C81 H107 108.4 . . ? C82 C81 H108 108.4 . . ? C80 C81 H108 108.4 . . ? H107 C81 H108 107.5 . . ? C81 C82 C83 110.7(7) . . ? C81 C82 H109 109.5 . . ? C83 C82 H109 109.5 . . ? C81 C82 H110 109.5 . . ? C83 C82 H110 109.5 . . ? H109 C82 H110 108.1 . . ? C82 C83 H111 109.5 . . ? C82 C83 H112 109.5 . . ? H111 C83 H112 109.5 . . ? C82 C83 H113 109.5 . . ? H111 C83 H113 109.5 . . ? H112 C83 H113 109.5 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.798 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.074 #===END data_[Ar(Me)O]2Zr=NAd(THF) _database_code_depnum_ccdc_archive 'CCDC 735066' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H93 N O3 Zr' _chemical_formula_sum 'C68 H93 N O3 Zr' _chemical_formula_weight 1063.65 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.66(3) _cell_length_b 15.44(4) _cell_length_c 17.16(5) _cell_angle_alpha 83.04(18) _cell_angle_beta 83.19(18) _cell_angle_gamma 64.15(11) _cell_volume 2750(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5256 _cell_measurement_theta_min 3.0910 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9518 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_method dtintegrate.ref _diffrn_detector_area_resol_mean 14.6199 _diffrn_reflns_number 21701 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11905 _reflns_number_gt 10107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0485P)^2^+4.0855P] 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 11905 _refine_ls_number_parameters 660 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1275 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.66231(3) 0.767992(18) 0.723095(15) 0.01944(8) Uani 1 1 d . . . N1 N 0.6895(2) 0.87642(17) 0.68791(14) 0.0253(5) Uani 1 1 d . . . O1 O 0.64726(18) 0.76246(14) 0.83983(11) 0.0221(4) Uani 1 1 d . . . O2 O 0.71690(18) 0.64797(13) 0.66154(10) 0.0198(4) Uani 1 1 d . . . O3 O 0.46384(19) 0.82159(13) 0.68188(12) 0.0246(4) Uani 1 1 d . . . C1 C 0.6805(3) 0.76879(19) 0.91224(16) 0.0222(6) Uani 1 1 d . . . C2 C 0.5798(3) 0.8157(2) 0.96995(16) 0.0256(6) Uani 1 1 d . . . C3 C 0.6141(3) 0.8120(2) 1.04637(18) 0.0342(7) Uani 1 1 d . . . H1 H 0.5481 0.8423 1.0856 0.041 Uiso 1 1 calc R . . C4 C 0.7403(3) 0.7661(2) 1.06802(18) 0.0342(7) Uani 1 1 d . . . C5 C 0.8358(3) 0.7279(2) 1.00965(17) 0.0319(7) Uani 1 1 d . . . H2 H 0.9222 0.7010 1.0227 0.038 Uiso 1 1 calc R . . C6 C 0.8106(3) 0.7272(2) 0.93056(16) 0.0242(6) Uani 1 1 d . . . C7 C 0.4375(3) 0.8632(2) 0.95253(16) 0.0235(6) Uani 1 1 d . . . C8 C 0.4089(3) 0.9384(2) 0.88094(18) 0.0282(6) Uani 1 1 d . . . H3 H 0.4645 0.9079 0.8344 0.034 Uiso 1 1 calc R . . H4 H 0.4280 0.9920 0.8920 0.034 Uiso 1 1 calc R . . C9 C 0.3953(3) 0.7851(2) 0.93857(19) 0.0293(6) Uani 1 1 d . . . H5 H 0.4475 0.7497 0.8930 0.035 Uiso 1 1 calc R . . H6 H 0.4111 0.7382 0.9854 0.035 Uiso 1 1 calc R . . C10 C 0.3496(3) 0.9174(2) 1.02282(19) 0.0338(7) Uani 1 1 d . . . H7 H 0.3635 0.8719 1.0704 0.041 Uiso 1 1 calc R . . H8 H 0.3724 0.9694 1.0334 0.041 Uiso 1 1 calc R . . C11 C 0.2660(3) 0.9790(2) 0.86264(19) 0.0350(7) Uani 1 1 d . . . H9 H 0.2506 1.0250 0.8145 0.042 Uiso 1 1 calc R . . C12 C 0.2536(3) 0.8275(2) 0.9229(2) 0.0359(7) Uani 1 1 d . . . H10 H 0.2309 0.7741 0.9141 0.043 Uiso 1 1 calc R . . C13 C 0.2071(3) 0.9618(2) 1.0058(2) 0.0349(7) Uani 1 1 d . . . H11 H 0.1537 0.9967 1.0520 0.042 Uiso 1 1 calc R . . C14 C 0.1824(4) 1.0325(2) 0.9329(2) 0.0421(8) Uani 1 1 d . . . H12 H 0.2031 1.0862 0.9416 0.050 Uiso 1 1 calc R . . H13 H 0.0911 1.0599 0.9223 0.050 Uiso 1 1 calc R . . C15 C 0.2311(3) 0.8970(3) 0.8494(2) 0.0411(8) Uani 1 1 d . . . H14 H 0.1402 0.9241 0.8378 0.049 Uiso 1 1 calc R . . H15 H 0.2842 0.8622 0.8039 0.049 Uiso 1 1 calc R . . C16 C 0.1698(3) 0.8814(3) 0.9924(2) 0.0403(8) Uani 1 1 d . . . H16 H 0.1822 0.8363 1.0402 0.048 Uiso 1 1 calc R . . H17 H 0.0787 0.9094 0.9813 0.048 Uiso 1 1 calc R . . C17 C 0.7711(4) 0.7600(3) 1.1526(2) 0.0469(9) Uani 1 1 d . . . H18 H 0.7526 0.7093 1.1835 0.070 Uiso 1 1 calc R . . H19 H 0.7187 0.8221 1.1748 0.070 Uiso 1 1 calc R . . H20 H 0.8618 0.7447 1.1539 0.070 Uiso 1 1 calc R . . C18 C 0.9310(3) 0.6791(2) 0.87485(16) 0.0223(6) Uani 1 1 d . . . C19 C 1.0123(3) 0.7380(2) 0.86564(19) 0.0321(7) Uani 1 1 d . . . H21 H 0.9622 0.8034 0.8409 0.039 Uiso 1 1 calc R . . H22 H 1.0324 0.7452 0.9183 0.039 Uiso 1 1 calc R . . C20 C 0.9076(3) 0.6668(2) 0.79045(16) 0.0244(6) Uani 1 1 d . . . H23 H 0.8559 0.6296 0.7941 0.029 Uiso 1 1 calc R . . H24 H 0.8579 0.7313 0.7642 0.029 Uiso 1 1 calc R . . C21 C 1.0154(3) 0.5771(2) 0.91095(18) 0.0287(6) Uani 1 1 d . . . H25 H 1.0343 0.5821 0.9646 0.034 Uiso 1 1 calc R . . H26 H 0.9676 0.5369 0.9157 0.034 Uiso 1 1 calc R . . C22 C 1.1377(3) 0.6878(3) 0.8148(2) 0.0372(8) Uani 1 1 d . . . H27 H 1.1869 0.7277 0.8094 0.045 Uiso 1 1 calc R . . C23 C 1.0323(3) 0.6149(2) 0.74009(17) 0.0299(7) Uani 1 1 d . . . H28 H 1.0125 0.6078 0.6868 0.036 Uiso 1 1 calc R . . C24 C 1.1413(3) 0.5275(2) 0.86152(19) 0.0347(7) Uani 1 1 d . . . H29 H 1.1932 0.4624 0.8876 0.042 Uiso 1 1 calc R . . C25 C 1.2166(3) 0.5895(3) 0.8540(2) 0.0412(8) Uani 1 1 d . . . H30 H 1.2361 0.5966 0.9069 0.049 Uiso 1 1 calc R . . H31 H 1.2984 0.5576 0.8223 0.049 Uiso 1 1 calc R . . C26 C 1.1088(3) 0.6759(3) 0.73232(19) 0.0392(8) Uani 1 1 d . . . H32 H 1.0588 0.7402 0.7058 0.047 Uiso 1 1 calc R . . H33 H 1.1898 0.6439 0.7000 0.047 Uiso 1 1 calc R . . C27 C 1.1110(3) 0.5158(2) 0.77975(19) 0.0348(7) Uani 1 1 d . . . H34 H 1.1915 0.4826 0.7472 0.042 Uiso 1 1 calc R . . H35 H 1.0626 0.4761 0.7850 0.042 Uiso 1 1 calc R . . C28 C 0.7128(3) 0.58191(18) 0.61695(15) 0.0184(5) Uani 1 1 d . . . C29 C 0.7365(3) 0.58860(18) 0.53357(15) 0.0191(5) Uani 1 1 d . . . C30 C 0.7172(3) 0.5250(2) 0.48973(16) 0.0236(6) Uani 1 1 d . . . H36 H 0.7316 0.5302 0.4340 0.028 Uiso 1 1 calc R . . C31 C 0.6779(3) 0.4550(2) 0.52427(17) 0.0247(6) Uani 1 1 d . . . C32 C 0.6634(3) 0.44600(19) 0.60567(17) 0.0227(6) Uani 1 1 d . . . H37 H 0.6386 0.3976 0.6302 0.027 Uiso 1 1 calc R . . C33 C 0.6833(3) 0.50487(19) 0.65394(16) 0.0199(5) Uani 1 1 d . . . C34 C 0.7871(3) 0.65970(19) 0.48968(15) 0.0193(5) Uani 1 1 d . . . C35 C 0.6865(3) 0.76533(19) 0.49316(16) 0.0222(6) Uani 1 1 d . . . H38 H 0.6100 0.7743 0.4674 0.027 Uiso 1 1 calc R . . H39 H 0.6601 0.7801 0.5488 0.027 Uiso 1 1 calc R . . C36 C 0.8219(3) 0.6427(2) 0.40065(16) 0.0240(6) Uani 1 1 d . . . H40 H 0.8860 0.5752 0.3950 0.029 Uiso 1 1 calc R . . H41 H 0.7445 0.6521 0.3756 0.029 Uiso 1 1 calc R . . C37 C 0.9111(3) 0.64806(19) 0.52531(16) 0.0217(6) Uani 1 1 d . . . H42 H 0.8919 0.6595 0.5819 0.026 Uiso 1 1 calc R . . H43 H 0.9772 0.5810 0.5209 0.026 Uiso 1 1 calc R . . C38 C 0.7407(3) 0.8351(2) 0.45167(16) 0.0245(6) Uani 1 1 d . . . H44 H 0.6747 0.9031 0.4562 0.029 Uiso 1 1 calc R . . C39 C 0.8757(3) 0.7120(2) 0.35845(16) 0.0258(6) Uani 1 1 d . . . H45 H 0.8979 0.6983 0.3018 0.031 Uiso 1 1 calc R . . C40 C 0.9637(3) 0.7182(2) 0.48355(16) 0.0242(6) Uani 1 1 d . . . H46 H 1.0418 0.7094 0.5085 0.029 Uiso 1 1 calc R . . C41 C 0.8616(3) 0.8210(2) 0.49069(18) 0.0271(6) Uani 1 1 d . . . H47 H 0.8947 0.8672 0.4647 0.032 Uiso 1 1 calc R . . H48 H 0.8394 0.8338 0.5469 0.032 Uiso 1 1 calc R . . C42 C 0.7751(3) 0.8158(2) 0.36403(17) 0.0288(6) Uani 1 1 d . . . H49 H 0.6980 0.8256 0.3386 0.035 Uiso 1 1 calc R . . H50 H 0.8090 0.8610 0.3367 0.035 Uiso 1 1 calc R . . C43 C 0.9976(3) 0.6984(2) 0.39619(18) 0.0293(6) Uani 1 1 d . . . H51 H 1.0642 0.6316 0.3912 0.035 Uiso 1 1 calc R . . H52 H 1.0315 0.7435 0.3687 0.035 Uiso 1 1 calc R . . C44 C 0.6566(3) 0.3885(2) 0.47475(19) 0.0336(7) Uani 1 1 d . . . H53 H 0.7386 0.3345 0.4615 0.050 Uiso 1 1 calc R . . H54 H 0.6186 0.4247 0.4262 0.050 Uiso 1 1 calc R . . H55 H 0.5988 0.3637 0.5046 0.050 Uiso 1 1 calc R . . C45 C 0.6838(3) 0.47860(18) 0.74383(16) 0.0198(5) Uani 1 1 d . . . C46 C 0.5749(3) 0.55645(19) 0.79130(17) 0.0259(6) Uani 1 1 d . . . H56 H 0.5808 0.6188 0.7792 0.031 Uiso 1 1 calc R . . H57 H 0.4915 0.5648 0.7754 0.031 Uiso 1 1 calc R . . C47 C 0.6661(3) 0.3840(2) 0.76619(17) 0.0256(6) Uani 1 1 d . . . H58 H 0.5820 0.3935 0.7508 0.031 Uiso 1 1 calc R . . H59 H 0.7331 0.3311 0.7368 0.031 Uiso 1 1 calc R . . C48 C 0.8150(3) 0.4602(2) 0.77245(16) 0.0236(6) Uani 1 1 d . . . H60 H 0.8839 0.4066 0.7448 0.028 Uiso 1 1 calc R . . H61 H 0.8302 0.5187 0.7587 0.028 Uiso 1 1 calc R . . C49 C 0.5817(3) 0.5286(2) 0.88053(18) 0.0327(7) Uani 1 1 d . . . H62 H 0.5111 0.5812 0.9095 0.039 Uiso 1 1 calc R . . C50 C 0.6743(3) 0.3552(2) 0.85510(18) 0.0294(7) Uani 1 1 d . . . H63 H 0.6649 0.2935 0.8672 0.035 Uiso 1 1 calc R . . C51 C 0.8204(3) 0.4346(2) 0.86245(17) 0.0293(7) Uani 1 1 d . . . H64 H 0.9045 0.4255 0.8791 0.035 Uiso 1 1 calc R . . C52 C 0.7114(4) 0.5153(2) 0.90589(18) 0.0357(8) Uani 1 1 d . . . H65 H 0.7208 0.5764 0.8936 0.043 Uiso 1 1 calc R . . H66 H 0.7150 0.4989 0.9634 0.043 Uiso 1 1 calc R . . C53 C 0.8042(3) 0.3410(2) 0.88116(19) 0.0336(7) Uani 1 1 d . . . H67 H 0.8081 0.3224 0.9384 0.040 Uiso 1 1 calc R . . H68 H 0.8744 0.2883 0.8533 0.040 Uiso 1 1 calc R . . C54 C 0.5661(3) 0.4343(2) 0.89963(19) 0.0353(7) Uani 1 1 d . . . H69 H 0.5690 0.4162 0.9570 0.042 Uiso 1 1 calc R . . H70 H 0.4826 0.4431 0.8837 0.042 Uiso 1 1 calc R . . C55 C 0.7067(3) 0.9655(2) 0.68116(17) 0.0258(6) Uani 1 1 d . . . C56 C 0.6494(3) 1.0293(2) 0.60665(17) 0.0261(6) Uani 1 1 d . . . H71 H 0.6914 0.9935 0.5595 0.031 Uiso 1 1 calc R . . H72 H 0.5570 1.0458 0.6088 0.031 Uiso 1 1 calc R . . C57 C 0.6389(4) 1.0240(2) 0.75296(19) 0.0374(8) Uani 1 1 d . . . H73 H 0.6741 0.9845 0.8017 0.045 Uiso 1 1 calc R . . H74 H 0.5465 1.0403 0.7559 0.045 Uiso 1 1 calc R . . C58 C 0.8505(3) 0.9439(2) 0.6780(2) 0.0323(7) Uani 1 1 d . . . H75 H 0.8881 0.9033 0.7258 0.039 Uiso 1 1 calc R . . H76 H 0.8962 0.9071 0.6317 0.039 Uiso 1 1 calc R . . C59 C 0.6685(3) 1.1223(2) 0.60063(19) 0.0318(7) Uani 1 1 d . . . H77 H 0.6315 1.1628 0.5519 0.038 Uiso 1 1 calc R . . C60 C 0.6574(4) 1.1179(3) 0.7469(2) 0.0450(9) Uani 1 1 d . . . H78 H 0.6118 1.1550 0.7936 0.054 Uiso 1 1 calc R . . C61 C 0.8691(3) 1.0376(2) 0.6724(2) 0.0383(8) Uani 1 1 d . . . H79 H 0.9623 1.0213 0.6699 0.046 Uiso 1 1 calc R . . C62 C 0.8118(3) 1.0985(2) 0.5972(2) 0.0381(8) Uani 1 1 d . . . H80 H 0.8568 1.0623 0.5506 0.046 Uiso 1 1 calc R . . H81 H 0.8228 1.1590 0.5923 0.046 Uiso 1 1 calc R . . C63 C 0.6013(4) 1.1787(2) 0.6720(2) 0.0416(8) Uani 1 1 d . . . H82 H 0.5087 1.1957 0.6744 0.050 Uiso 1 1 calc R . . H83 H 0.6121 1.2393 0.6677 0.050 Uiso 1 1 calc R . . C64 C 0.8008(4) 1.0937(3) 0.7444(2) 0.0479(10) Uani 1 1 d . . . H84 H 0.8122 1.1540 0.7411 0.057 Uiso 1 1 calc R . . H85 H 0.8374 1.0544 0.7929 0.057 Uiso 1 1 calc R . . C65 C 0.3981(3) 0.9186(2) 0.6445(2) 0.0348(7) Uani 1 1 d . . . H86 H 0.4445 0.9267 0.5940 0.042 Uiso 1 1 calc R . . H87 H 0.3912 0.9677 0.6793 0.042 Uiso 1 1 calc R . . C66 C 0.2659(3) 0.9287(2) 0.6307(2) 0.0378(8) Uani 1 1 d . . . H88 H 0.2024 0.9640 0.6726 0.045 Uiso 1 1 calc R . . H89 H 0.2389 0.9645 0.5793 0.045 Uiso 1 1 calc R . . C67 C 0.2764(4) 0.8279(2) 0.6319(2) 0.0423(8) Uani 1 1 d . . . H90 H 0.2104 0.8194 0.6698 0.051 Uiso 1 1 calc R . . H91 H 0.2651 0.8145 0.5791 0.051 Uiso 1 1 calc R . . C68 C 0.4067(3) 0.7623(2) 0.6562(3) 0.0474(10) Uani 1 1 d . . . H92 H 0.4016 0.7156 0.6999 0.057 Uiso 1 1 calc R . . H93 H 0.4600 0.7257 0.6115 0.057 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 0.02681(15) 0.01742(13) 0.01449(14) -0.00191(9) -0.00144(10) -0.00968(10) N1 0.0308(13) 0.0193(11) 0.0259(13) -0.0015(9) -0.0046(10) -0.0103(10) O1 0.0233(10) 0.0262(10) 0.0168(10) -0.0043(7) -0.0022(8) -0.0097(8) O2 0.0257(10) 0.0174(9) 0.0156(9) -0.0029(7) -0.0004(7) -0.0084(8) O3 0.0271(11) 0.0181(9) 0.0275(11) -0.0012(8) -0.0039(8) -0.0084(8) C1 0.0318(15) 0.0226(13) 0.0148(13) -0.0031(10) -0.0039(11) -0.0131(12) C2 0.0335(16) 0.0277(14) 0.0152(14) -0.0027(11) -0.0017(11) -0.0126(12) C3 0.0393(18) 0.0407(18) 0.0204(16) -0.0086(13) 0.0002(13) -0.0141(15) C4 0.047(2) 0.0387(17) 0.0177(15) -0.0043(12) -0.0068(13) -0.0177(15) C5 0.0378(18) 0.0379(17) 0.0204(15) -0.0014(12) -0.0115(13) -0.0143(14) C6 0.0301(15) 0.0277(14) 0.0170(14) -0.0017(11) -0.0055(11) -0.0134(12) C7 0.0295(15) 0.0238(13) 0.0169(14) -0.0052(10) 0.0017(11) -0.0111(12) C8 0.0305(16) 0.0232(14) 0.0261(16) -0.0025(11) 0.0058(12) -0.0088(12) C9 0.0292(16) 0.0251(14) 0.0327(17) -0.0054(12) 0.0062(13) -0.0119(12) C10 0.0351(17) 0.0347(17) 0.0265(17) -0.0102(13) 0.0084(13) -0.0109(14) C11 0.0303(17) 0.0321(16) 0.0271(17) 0.0020(13) 0.0052(13) -0.0020(13) C12 0.0303(17) 0.0373(17) 0.044(2) -0.0098(15) 0.0019(14) -0.0173(14) C13 0.0313(17) 0.0348(17) 0.0304(17) -0.0067(13) 0.0087(13) -0.0082(14) C14 0.0383(19) 0.0307(17) 0.043(2) -0.0013(15) 0.0080(16) -0.0052(15) C15 0.0265(17) 0.055(2) 0.0349(19) -0.0085(16) -0.0031(14) -0.0101(16) C16 0.0284(17) 0.0426(19) 0.045(2) -0.0027(16) 0.0075(15) -0.0140(15) C17 0.059(2) 0.055(2) 0.0233(18) -0.0054(15) -0.0116(16) -0.0178(19) C18 0.0224(14) 0.0253(14) 0.0205(14) 0.0002(11) -0.0057(11) -0.0108(11) C19 0.0382(18) 0.0385(17) 0.0283(16) 0.0043(13) -0.0101(13) -0.0242(15) C20 0.0221(14) 0.0288(14) 0.0201(14) -0.0023(11) -0.0038(11) -0.0081(12) C21 0.0298(16) 0.0312(15) 0.0242(16) 0.0053(12) -0.0071(12) -0.0127(13) C22 0.0361(18) 0.053(2) 0.0329(18) 0.0053(15) -0.0054(14) -0.0306(17) C23 0.0256(15) 0.0434(18) 0.0165(14) -0.0017(12) -0.0051(11) -0.0102(13) C24 0.0276(16) 0.0341(16) 0.0315(17) 0.0051(13) -0.0067(13) -0.0039(13) C25 0.0256(16) 0.066(2) 0.0293(18) 0.0040(16) -0.0062(13) -0.0184(16) C26 0.0315(17) 0.054(2) 0.0274(17) 0.0054(15) 0.0017(13) -0.0166(16) C27 0.0259(16) 0.0365(17) 0.0338(18) -0.0066(14) -0.0030(13) -0.0045(13) C28 0.0202(13) 0.0158(12) 0.0175(13) -0.0044(9) -0.0015(10) -0.0052(10) C29 0.0196(13) 0.0192(12) 0.0165(13) -0.0028(10) -0.0027(10) -0.0057(10) C30 0.0304(15) 0.0244(14) 0.0164(14) -0.0064(10) -0.0010(11) -0.0110(12) C31 0.0260(15) 0.0231(13) 0.0258(15) -0.0078(11) -0.0035(12) -0.0093(12) C32 0.0242(14) 0.0203(13) 0.0253(15) -0.0043(11) 0.0001(11) -0.0110(11) C33 0.0196(13) 0.0181(12) 0.0208(14) -0.0024(10) -0.0019(10) -0.0066(10) C34 0.0208(13) 0.0198(12) 0.0143(13) -0.0038(10) -0.0003(10) -0.0054(10) C35 0.0216(13) 0.0214(13) 0.0176(14) -0.0007(10) -0.0027(10) -0.0036(11) C36 0.0291(15) 0.0242(14) 0.0145(14) -0.0037(10) -0.0018(11) -0.0070(12) C37 0.0240(14) 0.0220(13) 0.0151(13) -0.0009(10) -0.0028(10) -0.0059(11) C38 0.0294(15) 0.0175(12) 0.0208(14) 0.0009(10) -0.0007(11) -0.0055(11) C39 0.0310(16) 0.0289(15) 0.0136(13) -0.0022(11) 0.0033(11) -0.0103(12) C40 0.0218(14) 0.0280(14) 0.0212(14) -0.0017(11) -0.0036(11) -0.0088(12) C41 0.0325(16) 0.0250(14) 0.0236(15) 0.0001(11) 0.0002(12) -0.0133(12) C42 0.0327(16) 0.0276(15) 0.0211(15) 0.0042(11) -0.0043(12) -0.0091(13) C43 0.0256(15) 0.0336(16) 0.0250(16) -0.0031(12) 0.0041(12) -0.0106(13) C44 0.0404(18) 0.0360(17) 0.0313(17) -0.0107(13) -0.0057(14) -0.0200(15) C45 0.0239(14) 0.0170(12) 0.0173(13) -0.0021(10) 0.0019(10) -0.0082(10) C46 0.0296(15) 0.0169(13) 0.0251(15) 0.0009(11) 0.0044(12) -0.0066(11) C47 0.0346(16) 0.0202(13) 0.0246(15) -0.0002(11) -0.0020(12) -0.0146(12) C48 0.0272(15) 0.0211(13) 0.0217(14) -0.0017(11) -0.0023(11) -0.0094(11) C49 0.0450(19) 0.0207(14) 0.0230(16) -0.0020(11) 0.0105(13) -0.0087(13) C50 0.0398(18) 0.0170(13) 0.0283(16) 0.0023(11) 0.0019(13) -0.0113(12) C51 0.0386(17) 0.0270(15) 0.0232(15) 0.0038(12) -0.0102(13) -0.0143(13) C52 0.063(2) 0.0279(15) 0.0171(15) 0.0005(12) -0.0027(14) -0.0206(16) C53 0.047(2) 0.0220(14) 0.0256(16) 0.0060(12) -0.0075(14) -0.0104(14) C54 0.0437(19) 0.0306(16) 0.0279(17) 0.0036(13) 0.0073(14) -0.0164(14) C55 0.0349(16) 0.0225(14) 0.0239(15) 0.0000(11) -0.0066(12) -0.0153(12) C56 0.0290(15) 0.0242(14) 0.0264(15) 0.0006(11) -0.0050(12) -0.0126(12) C57 0.059(2) 0.0347(17) 0.0256(17) -0.0047(13) 0.0048(15) -0.0277(17) C58 0.0334(17) 0.0276(15) 0.0385(18) 0.0026(13) -0.0131(14) -0.0139(13) C59 0.0373(18) 0.0236(14) 0.0347(17) 0.0067(12) -0.0076(14) -0.0143(13) C60 0.072(3) 0.0358(18) 0.036(2) -0.0154(15) 0.0059(18) -0.0306(19) C61 0.0352(18) 0.0371(18) 0.051(2) 0.0035(15) -0.0149(16) -0.0224(15) C62 0.043(2) 0.0368(18) 0.043(2) 0.0062(15) -0.0038(15) -0.0272(16) C63 0.051(2) 0.0226(15) 0.055(2) -0.0022(15) -0.0057(17) -0.0189(15) C64 0.078(3) 0.0394(19) 0.045(2) 0.0021(16) -0.024(2) -0.038(2) C65 0.0284(16) 0.0208(14) 0.051(2) 0.0076(13) -0.0114(14) -0.0074(12) C66 0.0365(18) 0.0311(16) 0.046(2) 0.0072(14) -0.0150(15) -0.0142(14) C67 0.044(2) 0.0350(18) 0.053(2) 0.0059(16) -0.0219(17) -0.0200(16) C68 0.039(2) 0.0229(15) 0.088(3) -0.0052(17) -0.0262(19) -0.0142(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 N1 1.854(5) . ? Zr1 O1 1.984(6) . ? Zr1 O2 2.059(5) . ? Zr1 O3 2.261(6) . ? N1 C55 1.463(5) . ? O1 C1 1.371(5) . ? O2 C28 1.366(4) . ? O3 C65 1.458(5) . ? O3 C68 1.475(4) . ? C1 C6 1.424(6) . ? C1 C2 1.428(6) . ? C2 C3 1.403(6) . ? C2 C7 1.543(6) . ? C3 C4 1.400(6) . ? C3 H1 0.9500 . ? C4 C5 1.376(6) . ? C4 C17 1.517(6) . ? C5 C6 1.424(6) . ? C5 H2 0.9500 . ? C6 C18 1.542(6) . ? C7 C9 1.540(5) . ? C7 C8 1.543(6) . ? C7 C10 1.552(6) . ? C8 C11 1.559(6) . ? C8 H3 0.9900 . ? C8 H4 0.9900 . ? C9 C12 1.533(6) . ? C9 H5 0.9900 . ? C9 H6 0.9900 . ? C10 C13 1.545(6) . ? C10 H7 0.9900 . ? C10 H8 0.9900 . ? C11 C14 1.532(6) . ? C11 C15 1.536(6) . ? C11 H9 1.0000 . ? C12 C15 1.521(7) . ? C12 C16 1.525(6) . ? C12 H10 1.0000 . ? C13 C14 1.522(6) . ? C13 C16 1.531(6) . ? C13 H11 1.0000 . ? C14 H12 0.9900 . ? C14 H13 0.9900 . ? C15 H14 0.9900 . ? C15 H15 0.9900 . ? C16 H16 0.9900 . ? C16 H17 0.9900 . ? C17 H18 0.9800 . ? C17 H19 0.9800 . ? C17 H20 0.9800 . ? C18 C21 1.545(6) . ? C18 C20 1.553(6) . ? C18 C19 1.560(5) . ? C19 C22 1.540(6) . ? C19 H21 0.9900 . ? C19 H22 0.9900 . ? C20 C23 1.535(6) . ? C20 H23 0.9900 . ? C20 H24 0.9900 . ? C21 C24 1.530(6) . ? C21 H25 0.9900 . ? C21 H26 0.9900 . ? C22 C25 1.511(6) . ? C22 C26 1.542(6) . ? C22 H27 1.0000 . ? C23 C27 1.521(6) . ? C23 C26 1.541(6) . ? C23 H28 1.0000 . ? C24 C27 1.536(6) . ? C24 C25 1.543(6) . ? C24 H29 1.0000 . ? C25 H30 0.9900 . ? C25 H31 0.9900 . ? C26 H32 0.9900 . ? C26 H33 0.9900 . ? C27 H34 0.9900 . ? C27 H35 0.9900 . ? C28 C29 1.424(6) . ? C28 C33 1.434(5) . ? C29 C30 1.412(5) . ? C29 C34 1.542(5) . ? C30 C31 1.393(5) . ? C30 H36 0.9500 . ? C31 C32 1.384(6) . ? C31 C44 1.523(5) . ? C32 C33 1.407(5) . ? C32 H37 0.9500 . ? C33 C45 1.546(6) . ? C34 C35 1.542(5) . ? C34 C36 1.557(6) . ? C34 C37 1.566(5) . ? C35 C38 1.539(5) . ? C35 H38 0.9900 . ? C35 H39 0.9900 . ? C36 C39 1.535(5) . ? C36 H40 0.9900 . ? C36 H41 0.9900 . ? C37 C40 1.533(5) . ? C37 H42 0.9900 . ? C37 H43 0.9900 . ? C38 C42 1.540(6) . ? C38 C41 1.550(6) . ? C38 H44 1.0000 . ? C39 C42 1.524(5) . ? C39 C43 1.551(6) . ? C39 H45 1.0000 . ? C40 C41 1.521(5) . ? C40 C43 1.537(6) . ? C40 H46 1.0000 . ? C41 H47 0.9900 . ? C41 H48 0.9900 . ? C42 H49 0.9900 . ? C42 H50 0.9900 . ? C43 H51 0.9900 . ? C43 H52 0.9900 . ? C44 H53 0.9800 . ? C44 H54 0.9800 . ? C44 H55 0.9800 . ? C45 C46 1.543(6) . ? C45 C48 1.557(6) . ? C45 C47 1.559(5) . ? C46 C49 1.541(6) . ? C46 H56 0.9900 . ? C46 H57 0.9900 . ? C47 C50 1.538(6) . ? C47 H58 0.9900 . ? C47 H59 0.9900 . ? C48 C51 1.549(6) . ? C48 H60 0.9900 . ? C48 H61 0.9900 . ? C49 C54 1.537(5) . ? C49 C52 1.543(6) . ? C49 H62 1.0000 . ? C50 C54 1.523(6) . ? C50 C53 1.545(6) . ? C50 H63 1.0000 . ? C51 C53 1.529(5) . ? C51 C52 1.531(6) . ? C51 H64 1.0000 . ? C52 H65 0.9900 . ? C52 H66 0.9900 . ? C53 H67 0.9900 . ? C53 H68 0.9900 . ? C54 H69 0.9900 . ? C54 H70 0.9900 . ? C55 C57 1.541(6) . ? C55 C56 1.541(6) . ? C55 C58 1.555(6) . ? C56 C59 1.536(5) . ? C56 H71 0.9900 . ? C56 H72 0.9900 . ? C57 C60 1.544(6) . ? C57 H73 0.9900 . ? C57 H74 0.9900 . ? C58 C61 1.543(5) . ? C58 H75 0.9900 . ? C58 H76 0.9900 . ? C59 C63 1.519(7) . ? C59 C62 1.540(6) . ? C59 H77 1.0000 . ? C60 C63 1.526(7) . ? C60 C64 1.542(7) . ? C60 H78 1.0000 . ? C61 C64 1.528(7) . ? C61 C62 1.535(7) . ? C61 H79 1.0000 . ? C62 H80 0.9900 . ? C62 H81 0.9900 . ? C63 H82 0.9900 . ? C63 H83 0.9900 . ? C64 H84 0.9900 . ? C64 H85 0.9900 . ? C65 C66 1.524(6) . ? C65 H86 0.9900 . ? C65 H87 0.9900 . ? C66 C67 1.505(6) . ? C66 H88 0.9900 . ? C66 H89 0.9900 . ? C67 C68 1.488(6) . ? C67 H90 0.9900 . ? C67 H91 0.9900 . ? C68 H92 0.9900 . ? C68 H93 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 N1 Zr1 O1 106.53(19) . . ? N1 Zr1 O2 125.50(19) . . ? O1 Zr1 O2 122.85(19) . . ? N1 Zr1 O3 97.69(19) . . ? O1 Zr1 O3 108.0(2) . . ? O2 Zr1 O3 88.40(17) . . ? C55 N1 Zr1 165.7(2) . . ? C1 O1 Zr1 155.1(2) . . ? C28 O2 Zr1 161.81(18) . . ? C65 O3 C68 106.9(3) . . ? C65 O3 Zr1 121.6(2) . . ? C68 O3 Zr1 126.6(2) . . ? O1 C1 C6 121.4(3) . . ? O1 C1 C2 117.7(3) . . ? C6 C1 C2 120.8(3) . . ? C3 C2 C1 117.2(3) . . ? C3 C2 C7 120.0(3) . . ? C1 C2 C7 122.7(3) . . ? C4 C3 C2 123.6(3) . . ? C4 C3 H1 118.2 . . ? C2 C3 H1 118.2 . . ? C5 C4 C3 117.6(3) . . ? C5 C4 C17 121.1(4) . . ? C3 C4 C17 121.2(4) . . ? C4 C5 C6 122.9(4) . . ? C4 C5 H2 118.6 . . ? C6 C5 H2 118.6 . . ? C1 C6 C5 117.6(3) . . ? C1 C6 C18 127.8(3) . . ? C5 C6 C18 114.6(3) . . ? C9 C7 C2 109.8(3) . . ? C9 C7 C8 109.3(3) . . ? C2 C7 C8 113.0(3) . . ? C9 C7 C10 106.4(3) . . ? C2 C7 C10 112.0(3) . . ? C8 C7 C10 106.0(3) . . ? C7 C8 C11 110.8(3) . . ? C7 C8 H3 109.5 . . ? C11 C8 H3 109.5 . . ? C7 C8 H4 109.5 . . ? C11 C8 H4 109.5 . . ? H3 C8 H4 108.1 . . ? C12 C9 C7 112.4(3) . . ? C12 C9 H5 109.1 . . ? C7 C9 H5 109.1 . . ? C12 C9 H6 109.1 . . ? C7 C9 H6 109.1 . . ? H5 C9 H6 107.9 . . ? C13 C10 C7 111.5(3) . . ? C13 C10 H7 109.3 . . ? C7 C10 H7 109.3 . . ? C13 C10 H8 109.3 . . ? C7 C10 H8 109.3 . . ? H7 C10 H8 108.0 . . ? C14 C11 C15 109.1(3) . . ? C14 C11 C8 108.4(3) . . ? C15 C11 C8 110.9(3) . . ? C14 C11 H9 109.5 . . ? C15 C11 H9 109.5 . . ? C8 C11 H9 109.5 . . ? C15 C12 C16 109.4(4) . . ? C15 C12 C9 108.7(3) . . ? C16 C12 C9 110.6(3) . . ? C15 C12 H10 109.4 . . ? C16 C12 H10 109.4 . . ? C9 C12 H10 109.4 . . ? C14 C13 C16 109.1(4) . . ? C14 C13 C10 110.6(3) . . ? C16 C13 C10 109.6(3) . . ? C14 C13 H11 109.2 . . ? C16 C13 H11 109.2 . . ? C10 C13 H11 109.2 . . ? C13 C14 C11 108.9(3) . . ? C13 C14 H12 109.9 . . ? C11 C14 H12 109.9 . . ? C13 C14 H13 109.9 . . ? C11 C14 H13 109.9 . . ? H12 C14 H13 108.3 . . ? C12 C15 C11 109.5(3) . . ? C12 C15 H14 109.8 . . ? C11 C15 H14 109.8 . . ? C12 C15 H15 109.8 . . ? C11 C15 H15 109.8 . . ? H14 C15 H15 108.2 . . ? C12 C16 C13 108.7(3) . . ? C12 C16 H16 109.9 . . ? C13 C16 H16 109.9 . . ? C12 C16 H17 109.9 . . ? C13 C16 H17 109.9 . . ? H16 C16 H17 108.3 . . ? C4 C17 H18 109.5 . . ? C4 C17 H19 109.5 . . ? H18 C17 H19 109.5 . . ? C4 C17 H20 109.5 . . ? H18 C17 H20 109.5 . . ? H19 C17 H20 109.5 . . ? C6 C18 C21 109.5(3) . . ? C6 C18 C20 116.2(3) . . ? C21 C18 C20 106.7(3) . . ? C6 C18 C19 110.2(3) . . ? C21 C18 C19 107.1(3) . . ? C20 C18 C19 106.8(3) . . ? C22 C19 C18 111.2(3) . . ? C22 C19 H21 109.4 . . ? C18 C19 H21 109.4 . . ? C22 C19 H22 109.4 . . ? C18 C19 H22 109.4 . . ? H21 C19 H22 108.0 . . ? C23 C20 C18 112.7(3) . . ? C23 C20 H23 109.1 . . ? C18 C20 H23 109.1 . . ? C23 C20 H24 109.1 . . ? C18 C20 H24 109.1 . . ? H23 C20 H24 107.8 . . ? C24 C21 C18 112.4(3) . . ? C24 C21 H25 109.1 . . ? C18 C21 H25 109.1 . . ? C24 C21 H26 109.1 . . ? C18 C21 H26 109.1 . . ? H25 C21 H26 107.9 . . ? C25 C22 C19 109.4(3) . . ? C25 C22 C26 109.4(4) . . ? C19 C22 C26 110.3(3) . . ? C25 C22 H27 109.2 . . ? C19 C22 H27 109.2 . . ? C26 C22 H27 109.2 . . ? C27 C23 C20 110.0(3) . . ? C27 C23 C26 109.2(3) . . ? C20 C23 C26 108.3(3) . . ? C27 C23 H28 109.8 . . ? C20 C23 H28 109.8 . . ? C26 C23 H28 109.8 . . ? C21 C24 C27 108.6(3) . . ? C21 C24 C25 109.5(3) . . ? C27 C24 C25 110.2(3) . . ? C21 C24 H29 109.5 . . ? C27 C24 H29 109.5 . . ? C25 C24 H29 109.5 . . ? C22 C25 C24 109.3(3) . . ? C22 C25 H30 109.8 . . ? C24 C25 H30 109.8 . . ? C22 C25 H31 109.8 . . ? C24 C25 H31 109.8 . . ? H30 C25 H31 108.3 . . ? C23 C26 C22 109.6(3) . . ? C23 C26 H32 109.8 . . ? C22 C26 H32 109.8 . . ? C23 C26 H33 109.8 . . ? C22 C26 H33 109.8 . . ? H32 C26 H33 108.2 . . ? C23 C27 C24 109.4(3) . . ? C23 C27 H34 109.8 . . ? C24 C27 H34 109.8 . . ? C23 C27 H35 109.8 . . ? C24 C27 H35 109.8 . . ? H34 C27 H35 108.2 . . ? O2 C28 C29 121.0(3) . . ? O2 C28 C33 120.0(3) . . ? C29 C28 C33 119.0(3) . . ? C30 C29 C28 118.5(3) . . ? C30 C29 C34 118.8(3) . . ? C28 C29 C34 122.7(3) . . ? C31 C30 C29 123.1(3) . . ? C31 C30 H36 118.5 . . ? C29 C30 H36 118.5 . . ? C32 C31 C30 117.3(3) . . ? C32 C31 C44 121.3(3) . . ? C30 C31 C44 121.4(3) . . ? C31 C32 C33 123.4(3) . . ? C31 C32 H37 118.3 . . ? C33 C32 H37 118.3 . . ? C32 C33 C28 118.3(3) . . ? C32 C33 C45 118.7(3) . . ? C28 C33 C45 122.8(3) . . ? C35 C34 C29 111.7(3) . . ? C35 C34 C36 106.0(3) . . ? C29 C34 C36 112.1(3) . . ? C35 C34 C37 109.0(3) . . ? C29 C34 C37 110.6(3) . . ? C36 C34 C37 107.1(3) . . ? C38 C35 C34 110.8(3) . . ? C38 C35 H38 109.5 . . ? C34 C35 H38 109.5 . . ? C38 C35 H39 109.5 . . ? C34 C35 H39 109.5 . . ? H38 C35 H39 108.1 . . ? C39 C36 C34 111.4(3) . . ? C39 C36 H40 109.3 . . ? C34 C36 H40 109.3 . . ? C39 C36 H41 109.3 . . ? C34 C36 H41 109.3 . . ? H40 C36 H41 108.0 . . ? C40 C37 C34 112.2(3) . . ? C40 C37 H42 109.2 . . ? C34 C37 H42 109.2 . . ? C40 C37 H43 109.2 . . ? C34 C37 H43 109.2 . . ? H42 C37 H43 107.9 . . ? C35 C38 C42 109.5(3) . . ? C35 C38 C41 110.1(3) . . ? C42 C38 C41 109.6(3) . . ? C35 C38 H44 109.2 . . ? C42 C38 H44 109.2 . . ? C41 C38 H44 109.2 . . ? C42 C39 C36 109.5(3) . . ? C42 C39 C43 109.5(3) . . ? C36 C39 C43 110.5(3) . . ? C42 C39 H45 109.1 . . ? C36 C39 H45 109.1 . . ? C43 C39 H45 109.1 . . ? C41 C40 C37 108.8(3) . . ? C41 C40 C43 109.6(3) . . ? C37 C40 C43 109.2(3) . . ? C41 C40 H46 109.8 . . ? C37 C40 H46 109.8 . . ? C43 C40 H46 109.8 . . ? C40 C41 C38 109.9(3) . . ? C40 C41 H47 109.7 . . ? C38 C41 H47 109.7 . . ? C40 C41 H48 109.7 . . ? C38 C41 H48 109.7 . . ? H47 C41 H48 108.2 . . ? C39 C42 C38 108.4(3) . . ? C39 C42 H49 110.0 . . ? C38 C42 H49 110.0 . . ? C39 C42 H50 110.0 . . ? C38 C42 H50 110.0 . . ? H49 C42 H50 108.4 . . ? C40 C43 C39 109.1(3) . . ? C40 C43 H51 109.9 . . ? C39 C43 H51 109.9 . . ? C40 C43 H52 109.9 . . ? C39 C43 H52 109.9 . . ? H51 C43 H52 108.3 . . ? C31 C44 H53 109.5 . . ? C31 C44 H54 109.5 . . ? H53 C44 H54 109.5 . . ? C31 C44 H55 109.5 . . ? H53 C44 H55 109.5 . . ? H54 C44 H55 109.5 . . ? C46 C45 C33 113.3(3) . . ? C46 C45 C48 109.6(3) . . ? C33 C45 C48 109.7(3) . . ? C46 C45 C47 105.6(3) . . ? C33 C45 C47 111.6(3) . . ? C48 C45 C47 106.8(3) . . ? C49 C46 C45 111.4(3) . . ? C49 C46 H56 109.3 . . ? C45 C46 H56 109.3 . . ? C49 C46 H57 109.3 . . ? C45 C46 H57 109.3 . . ? H56 C46 H57 108.0 . . ? C50 C47 C45 111.3(3) . . ? C50 C47 H58 109.4 . . ? C45 C47 H58 109.4 . . ? C50 C47 H59 109.4 . . ? C45 C47 H59 109.4 . . ? H58 C47 H59 108.0 . . ? C51 C48 C45 112.0(3) . . ? C51 C48 H60 109.2 . . ? C45 C48 H60 109.2 . . ? C51 C48 H61 109.2 . . ? C45 C48 H61 109.2 . . ? H60 C48 H61 107.9 . . ? C54 C49 C46 109.2(3) . . ? C54 C49 C52 110.0(3) . . ? C46 C49 C52 109.7(3) . . ? C54 C49 H62 109.3 . . ? C46 C49 H62 109.3 . . ? C52 C49 H62 109.3 . . ? C54 C50 C47 109.0(3) . . ? C54 C50 C53 109.7(3) . . ? C47 C50 C53 110.6(3) . . ? C54 C50 H63 109.2 . . ? C47 C50 H63 109.2 . . ? C53 C50 H63 109.2 . . ? C53 C51 C52 109.3(3) . . ? C53 C51 C48 107.9(3) . . ? C52 C51 C48 109.8(3) . . ? C53 C51 H64 109.9 . . ? C52 C51 H64 109.9 . . ? C48 C51 H64 109.9 . . ? C51 C52 C49 109.8(3) . . ? C51 C52 H65 109.7 . . ? C49 C52 H65 109.7 . . ? C51 C52 H66 109.7 . . ? C49 C52 H66 109.7 . . ? H65 C52 H66 108.2 . . ? C51 C53 C50 109.8(3) . . ? C51 C53 H67 109.7 . . ? C50 C53 H67 109.7 . . ? C51 C53 H68 109.7 . . ? C50 C53 H68 109.7 . . ? H67 C53 H68 108.2 . . ? C50 C54 C49 108.6(3) . . ? C50 C54 H69 110.0 . . ? C49 C54 H69 110.0 . . ? C50 C54 H70 110.0 . . ? C49 C54 H70 110.0 . . ? H69 C54 H70 108.4 . . ? N1 C55 C57 110.2(3) . . ? N1 C55 C56 111.0(3) . . ? C57 C55 C56 107.9(3) . . ? N1 C55 C58 111.4(3) . . ? C57 C55 C58 107.6(3) . . ? C56 C55 C58 108.6(3) . . ? C59 C56 C55 110.2(3) . . ? C59 C56 H71 109.6 . . ? C55 C56 H71 109.6 . . ? C59 C56 H72 109.6 . . ? C55 C56 H72 109.6 . . ? H71 C56 H72 108.1 . . ? C55 C57 C60 110.7(3) . . ? C55 C57 H73 109.5 . . ? C60 C57 H73 109.5 . . ? C55 C57 H74 109.5 . . ? C60 C57 H74 109.5 . . ? H73 C57 H74 108.1 . . ? C61 C58 C55 111.6(3) . . ? C61 C58 H75 109.3 . . ? C55 C58 H75 109.3 . . ? C61 C58 H76 109.3 . . ? C55 C58 H76 109.3 . . ? H75 C58 H76 108.0 . . ? C63 C59 C56 109.7(3) . . ? C63 C59 C62 108.8(3) . . ? C56 C59 C62 110.6(3) . . ? C63 C59 H77 109.3 . . ? C56 C59 H77 109.3 . . ? C62 C59 H77 109.3 . . ? C63 C60 C64 109.8(4) . . ? C63 C60 C57 109.0(3) . . ? C64 C60 C57 110.2(3) . . ? C63 C60 H78 109.3 . . ? C64 C60 H78 109.3 . . ? C57 C60 H78 109.3 . . ? C64 C61 C62 109.8(4) . . ? C64 C61 C58 109.6(3) . . ? C62 C61 C58 108.3(3) . . ? C64 C61 H79 109.7 . . ? C62 C61 H79 109.7 . . ? C58 C61 H79 109.7 . . ? C61 C62 C59 109.6(3) . . ? C61 C62 H80 109.8 . . ? C59 C62 H80 109.7 . . ? C61 C62 H81 109.8 . . ? C59 C62 H81 109.7 . . ? H80 C62 H81 108.2 . . ? C59 C63 C60 109.8(3) . . ? C59 C63 H82 109.7 . . ? C60 C63 H82 109.7 . . ? C59 C63 H83 109.7 . . ? C60 C63 H83 109.7 . . ? H82 C63 H83 108.2 . . ? C61 C64 C60 108.7(3) . . ? C61 C64 H84 109.9 . . ? C60 C64 H84 109.9 . . ? C61 C64 H85 109.9 . . ? C60 C64 H85 109.9 . . ? H84 C64 H85 108.3 . . ? O3 C65 C66 105.4(3) . . ? O3 C65 H86 110.7 . . ? C66 C65 H86 110.7 . . ? O3 C65 H87 110.7 . . ? C66 C65 H87 110.7 . . ? H86 C65 H87 108.8 . . ? C67 C66 C65 106.7(3) . . ? C67 C66 H88 110.4 . . ? C65 C66 H88 110.4 . . ? C67 C66 H89 110.4 . . ? C65 C66 H89 110.4 . . ? H88 C66 H89 108.6 . . ? C68 C67 C66 105.9(3) . . ? C68 C67 H90 110.6 . . ? C66 C67 H90 110.6 . . ? C68 C67 H91 110.6 . . ? C66 C67 H91 110.6 . . ? H90 C67 H91 108.7 . . ? O3 C68 C67 108.2(3) . . ? O3 C68 H92 110.1 . . ? C67 C68 H92 110.1 . . ? O3 C68 H93 110.1 . . ? C67 C68 H93 110.1 . . ? H92 C68 H93 108.4 . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.921 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.076 #===END