# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2213 data_azrs20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 Cl Si Zr' _chemical_formula_weight 502.30 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6955(4) _cell_length_b 12.4482(6) _cell_length_c 20.4091(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.1940(10) _cell_angle_gamma 90.00 _cell_volume 2462.67(19) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8871 _exptl_absorpt_correction_T_max 0.9700 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17993 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.34 _reflns_number_total 5689 _reflns_number_gt 4560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0419P)^2^+0.7821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5689 _refine_ls_number_parameters 273 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.119 _refine_ls_shift/su_mean 0.003 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 Zr Zr 0.20576(2) 0.778462(16) 0.143643(9) 0.02635(7) Uani 1 1 d . . . Si Si -0.11009(6) 0.68345(5) 0.15849(3) 0.03120(14) Uani 1 1 d . . . Cl Cl 0.30785(8) 0.92491(5) 0.20830(3) 0.05165(17) Uani 1 1 d . . . C1 C -0.2007(3) 0.5711(2) 0.11507(13) 0.0447(6) Uani 1 1 d . . . H1A H -0.2222 0.5150 0.1462 0.067 Uiso 1 1 calc R . . H1B H -0.1416 0.5422 0.0816 0.067 Uiso 1 1 calc R . . H1C H -0.2854 0.5976 0.0948 0.067 Uiso 1 1 calc R . . C2 C -0.2410(3) 0.7312(2) 0.21793(14) 0.0491(6) Uani 1 1 d . . . H2A H -0.3228 0.7556 0.1941 0.074 Uiso 1 1 calc R . . H2B H -0.2028 0.7900 0.2436 0.074 Uiso 1 1 calc R . . H2C H -0.2653 0.6726 0.2469 0.074 Uiso 1 1 calc R . . C11 C -0.0371(2) 0.79136(17) 0.10386(10) 0.0296(4) Uani 1 1 d . . . C12 C 0.0416(2) 0.77154(17) 0.04577(10) 0.0305(4) Uani 1 1 d . . . C13 C 0.1237(2) 0.86277(18) 0.03279(10) 0.0321(5) Uani 1 1 d . . . C14 C 0.0990(2) 0.94048(17) 0.08192(11) 0.0334(5) Uani 1 1 d . . . C15 C 0.0006(2) 0.89759(17) 0.12523(11) 0.0321(5) Uani 1 1 d . . . C21 C 0.0603(2) 0.64404(17) 0.19792(10) 0.0290(4) Uani 1 1 d . . . C22 C 0.1646(2) 0.58137(17) 0.16621(10) 0.0298(4) Uani 1 1 d . . . C23 C 0.2936(2) 0.59966(18) 0.19782(11) 0.0335(5) Uani 1 1 d . . . C24 C 0.2734(2) 0.6729(2) 0.24960(11) 0.0357(5) Uani 1 1 d . . . C25 C 0.1311(2) 0.70098(18) 0.24988(10) 0.0321(5) Uani 1 1 d . . . C32 C 0.0238(3) 0.6803(2) -0.00166(12) 0.0406(5) Uani 1 1 d . . . H32A H -0.0309 0.7041 -0.0393 0.061 Uiso 1 1 calc R . . H32B H -0.0227 0.6213 0.0196 0.061 Uiso 1 1 calc R . . H32C H 0.1136 0.6567 -0.0160 0.061 Uiso 1 1 calc R . . C33 C 0.2092(3) 0.8819(2) -0.02653(11) 0.0426(6) Uani 1 1 d . . . H33A H 0.1585 0.9273 -0.0572 0.064 Uiso 1 1 calc R . . H33B H 0.2295 0.8137 -0.0472 0.064 Uiso 1 1 calc R . . H33C H 0.2947 0.9170 -0.0135 0.064 Uiso 1 1 calc R . . C34 C 0.1588(3) 1.05148(19) 0.08332(13) 0.0467(6) Uani 1 1 d . . . H34A H 0.2562 1.0480 0.0737 0.070 Uiso 1 1 calc R . . H34B H 0.1473 1.0826 0.1264 0.070 Uiso 1 1 calc R . . H34C H 0.1116 1.0957 0.0508 0.070 Uiso 1 1 calc R . . C35 C -0.0598(3) 0.9610(2) 0.18047(12) 0.0453(6) Uani 1 1 d . . . H35A H -0.0787 0.9133 0.2168 0.068 Uiso 1 1 calc R . . H35B H -0.1450 0.9947 0.1655 0.068 Uiso 1 1 calc R . . H35C H 0.0052 1.0159 0.1947 0.068 Uiso 1 1 calc R . . C42 C 0.1429(3) 0.49350(19) 0.11623(12) 0.0398(5) Uani 1 1 d . . . H42A H 0.2089 0.5016 0.0815 0.060 Uiso 1 1 calc R . . H42B H 0.0500 0.4982 0.0979 0.060 Uiso 1 1 calc R . . H42C H 0.1557 0.4241 0.1372 0.060 Uiso 1 1 calc R . . C43 C 0.4243(3) 0.5395(2) 0.18523(14) 0.0482(6) Uani 1 1 d . . . H43A H 0.5027 0.5819 0.2003 0.072 Uiso 1 1 calc R . . H43B H 0.4316 0.5260 0.1386 0.072 Uiso 1 1 calc R . . H43C H 0.4233 0.4716 0.2086 0.072 Uiso 1 1 calc R . . C44 C 0.3809(3) 0.7065(3) 0.29992(13) 0.0519(7) Uani 1 1 d . . . H44A H 0.3850 0.6540 0.3350 0.078 Uiso 1 1 calc R . . H44B H 0.3566 0.7761 0.3177 0.078 Uiso 1 1 calc R . . H44C H 0.4701 0.7111 0.2795 0.078 Uiso 1 1 calc R . . C45 C 0.0695(3) 0.7710(2) 0.30177(12) 0.0433(6) Uani 1 1 d . . . H45A H 0.0570 0.7292 0.3413 0.065 Uiso 1 1 calc R . . H45B H -0.0191 0.7981 0.2862 0.065 Uiso 1 1 calc R . . H45C H 0.1308 0.8308 0.3112 0.065 Uiso 1 1 calc R . . C51 C 0.3835(2) 0.7399(2) 0.07545(12) 0.0390(5) Uani 1 1 d . . . C52 C 0.3927(3) 0.6602(2) 0.02795(14) 0.0500(7) Uani 1 1 d . . . H52A H 0.3234 0.6075 0.0256 0.060 Uiso 1 1 calc R . . C53 C 0.4999(3) 0.6549(3) -0.01620(15) 0.0618(8) Uani 1 1 d . . . H53A H 0.5013 0.5996 -0.0476 0.074 Uiso 1 1 calc R . . C54 C 0.6034(3) 0.7297(3) -0.01424(18) 0.0688(10) Uani 1 1 d . . . H54A H 0.6745 0.7275 -0.0448 0.083 Uiso 1 1 calc R . . C55 C 0.6015(3) 0.8082(3) 0.03341(17) 0.0657(9) Uani 1 1 d . . . H55A H 0.6738 0.8584 0.0364 0.079 Uiso 1 1 calc R . . C56 C 0.4938(3) 0.8136(2) 0.07685(14) 0.0505(7) Uani 1 1 d . . . H56A H 0.4943 0.8685 0.1085 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.02940(11) 0.02692(11) 0.02272(11) -0.00005(8) 0.00036(7) -0.00466(8) Si 0.0278(3) 0.0328(3) 0.0331(3) 0.0013(3) 0.0029(2) -0.0024(2) Cl 0.0666(4) 0.0453(4) 0.0425(4) -0.0063(3) -0.0106(3) -0.0199(3) C1 0.0375(13) 0.0424(13) 0.0538(16) 0.0016(12) -0.0057(11) -0.0102(10) C2 0.0398(14) 0.0590(17) 0.0490(16) 0.0051(13) 0.0127(11) 0.0015(12) C11 0.0291(10) 0.0311(11) 0.0285(11) 0.0005(9) -0.0006(8) 0.0031(8) C12 0.0335(11) 0.0326(11) 0.0251(10) -0.0014(9) -0.0027(8) 0.0014(9) C13 0.0378(11) 0.0329(11) 0.0257(10) 0.0058(9) 0.0003(9) 0.0018(9) C14 0.0422(12) 0.0284(11) 0.0294(11) 0.0043(9) -0.0003(9) 0.0016(9) C15 0.0407(12) 0.0269(10) 0.0288(11) -0.0006(9) 0.0009(9) 0.0038(9) C21 0.0334(11) 0.0283(10) 0.0256(10) 0.0059(8) 0.0039(8) -0.0043(8) C22 0.0340(11) 0.0266(10) 0.0289(11) 0.0047(8) 0.0027(8) 0.0001(8) C23 0.0345(11) 0.0359(12) 0.0301(11) 0.0091(9) 0.0001(9) 0.0007(9) C24 0.0369(12) 0.0436(13) 0.0265(11) 0.0093(10) -0.0031(9) -0.0061(10) C25 0.0399(12) 0.0341(11) 0.0223(10) 0.0050(8) 0.0018(8) -0.0032(9) C32 0.0503(14) 0.0411(13) 0.0304(12) -0.0086(10) -0.0013(10) -0.0034(11) C33 0.0513(14) 0.0491(14) 0.0274(11) 0.0067(11) 0.0050(10) -0.0013(12) C34 0.0606(16) 0.0297(12) 0.0499(15) 0.0048(11) 0.0021(12) -0.0059(11) C35 0.0624(16) 0.0342(12) 0.0398(13) -0.0033(11) 0.0114(12) 0.0069(11) C42 0.0461(13) 0.0315(11) 0.0419(13) -0.0027(10) 0.0044(11) -0.0023(10) C43 0.0384(13) 0.0529(15) 0.0532(16) 0.0104(13) -0.0005(11) 0.0092(11) C44 0.0482(15) 0.0725(19) 0.0344(13) 0.0052(13) -0.0118(11) -0.0075(13) C45 0.0539(15) 0.0472(14) 0.0290(12) -0.0035(11) 0.0065(10) -0.0029(12) C51 0.0351(12) 0.0450(13) 0.0370(13) 0.0129(11) 0.0070(10) 0.0035(10) C52 0.0484(15) 0.0505(16) 0.0516(16) 0.0040(13) 0.0134(12) 0.0043(12) C53 0.0665(19) 0.0648(19) 0.0552(18) 0.0059(15) 0.0250(15) 0.0181(16) C54 0.0563(18) 0.076(2) 0.076(2) 0.0245(19) 0.0356(17) 0.0161(16) C55 0.0457(16) 0.074(2) 0.078(2) 0.0246(18) 0.0165(15) -0.0051(15) C56 0.0414(14) 0.0563(16) 0.0541(16) 0.0119(13) 0.0052(12) -0.0021(12) _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 Zr C51 2.288(2) . ? Zr Cl 2.4475(6) . ? Zr C21 2.4661(19) . ? Zr C11 2.480(2) . ? Zr C25 2.494(2) . ? Zr C15 2.503(2) . ? Zr C12 2.529(2) . ? Zr C22 2.530(2) . ? Zr C14 2.583(2) . ? Zr C24 2.603(2) . ? Zr C13 2.603(2) . ? Zr C23 2.620(2) . ? Si C1 1.866(2) . ? Si C2 1.871(2) . ? Si C21 1.887(2) . ? Si C11 1.893(2) . ? C11 C15 1.437(3) . ? C11 C12 1.444(3) . ? C12 C13 1.415(3) . ? C12 C32 1.499(3) . ? C13 C14 1.417(3) . ? C13 C33 1.500(3) . ? C14 C15 1.418(3) . ? C14 C34 1.499(3) . ? C15 C35 1.505(3) . ? C21 C25 1.438(3) . ? C21 C22 1.441(3) . ? C22 C23 1.414(3) . ? C22 C42 1.507(3) . ? C23 C24 1.412(3) . ? C23 C43 1.499(3) . ? C24 C25 1.424(3) . ? C24 C44 1.507(3) . ? C25 C45 1.505(3) . ? C51 C52 1.391(4) . ? C51 C56 1.409(4) . ? C52 C53 1.391(3) . ? C53 C54 1.369(5) . ? C54 C55 1.379(5) . ? C55 C56 1.386(4) . ? 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 C51 Zr Cl 100.55(7) . . ? C51 Zr C21 125.14(8) . . ? Cl Zr C21 119.46(5) . . ? C51 Zr C11 122.43(8) . . ? Cl Zr C11 119.93(5) . . ? C21 Zr C11 69.09(7) . . ? C51 Zr C25 133.10(8) . . ? Cl Zr C25 86.60(5) . . ? C21 Zr C25 33.70(7) . . ? C11 Zr C25 91.09(7) . . ? C51 Zr C15 129.73(8) . . ? Cl Zr C15 87.18(5) . . ? C21 Zr C15 90.54(7) . . ? C11 Zr C15 33.53(7) . . ? C25 Zr C15 96.64(7) . . ? C51 Zr C12 88.96(8) . . ? Cl Zr C12 133.78(5) . . ? C21 Zr C12 88.58(7) . . ? C11 Zr C12 33.50(7) . . ? C25 Zr C12 118.96(7) . . ? C15 Zr C12 54.32(7) . . ? C51 Zr C22 91.76(8) . . ? Cl Zr C22 133.46(5) . . ? C21 Zr C22 33.50(7) . . ? C11 Zr C22 88.28(7) . . ? C25 Zr C22 54.33(7) . . ? C15 Zr C22 118.29(7) . . ? C12 Zr C22 90.66(7) . . ? C51 Zr C14 99.59(8) . . ? Cl Zr C14 80.49(6) . . ? C21 Zr C14 121.45(7) . . ? C11 Zr C14 54.66(7) . . ? C25 Zr C14 127.25(7) . . ? C15 Zr C14 32.33(7) . . ? C12 Zr C14 53.29(7) . . ? C22 Zr C14 141.53(7) . . ? C51 Zr C24 102.67(8) . . ? Cl Zr C24 80.56(6) . . ? C21 Zr C24 54.61(7) . . ? C11 Zr C24 121.73(7) . . ? C25 Zr C24 32.35(7) . . ? C15 Zr C24 127.57(7) . . ? C12 Zr C24 141.49(7) . . ? C22 Zr C24 52.92(7) . . ? C14 Zr C24 153.00(7) . . ? C51 Zr C13 77.08(8) . . ? Cl Zr C13 106.33(5) . . ? C21 Zr C13 119.78(7) . . ? C11 Zr C13 54.44(7) . . ? C25 Zr C13 145.33(7) . . ? C15 Zr C13 53.36(7) . . ? C12 Zr C13 31.96(7) . . ? C22 Zr C13 120.17(7) . . ? C14 Zr C13 31.71(7) . . ? C24 Zr C13 173.07(7) . . ? C51 Zr C23 80.56(7) . . ? Cl Zr C23 106.32(6) . . ? C21 Zr C23 54.39(7) . . ? C11 Zr C23 119.43(7) . . ? C25 Zr C23 53.28(7) . . ? C15 Zr C23 144.79(7) . . ? C12 Zr C23 119.87(7) . . ? C22 Zr C23 31.82(7) . . ? C14 Zr C23 173.08(7) . . ? C24 Zr C23 31.37(7) . . ? C13 Zr C23 143.14(7) . . ? C1 Si C2 103.11(12) . . ? C1 Si C21 114.01(11) . . ? C2 Si C21 113.93(11) . . ? C1 Si C11 115.50(11) . . ? C2 Si C11 115.09(11) . . ? C21 Si C11 95.79(9) . . ? C15 C11 C12 105.73(18) . . ? C15 C11 Si 124.76(16) . . ? C12 C11 Si 124.94(16) . . ? C15 C11 Zr 74.14(12) . . ? C12 C11 Zr 75.14(12) . . ? Si C11 Zr 97.21(9) . . ? C13 C12 C11 108.99(18) . . ? C13 C12 C32 123.0(2) . . ? C11 C12 C32 127.1(2) . . ? C13 C12 Zr 76.90(13) . . ? C11 C12 Zr 71.36(12) . . ? C32 C12 Zr 126.70(16) . . ? C12 C13 C14 108.13(18) . . ? C12 C13 C33 126.9(2) . . ? C14 C13 C33 124.6(2) . . ? C12 C13 Zr 71.13(12) . . ? C14 C13 Zr 73.35(12) . . ? C33 C13 Zr 126.97(16) . . ? C13 C14 C15 108.05(19) . . ? C13 C14 C34 124.9(2) . . ? C15 C14 C34 126.9(2) . . ? C13 C14 Zr 74.93(12) . . ? C15 C14 Zr 70.73(12) . . ? C34 C14 Zr 124.03(17) . . ? C14 C15 C11 109.10(18) . . ? C14 C15 C35 123.2(2) . . ? C11 C15 C35 127.5(2) . . ? C14 C15 Zr 76.94(13) . . ? C11 C15 Zr 72.34(12) . . ? C35 C15 Zr 121.26(16) . . ? C25 C21 C22 105.62(19) . . ? C25 C21 Si 125.91(16) . . ? C22 C21 Si 124.42(16) . . ? C25 C21 Zr 74.22(11) . . ? C22 C21 Zr 75.67(11) . . ? Si C21 Zr 97.80(8) . . ? C23 C22 C21 109.27(19) . . ? C23 C22 C42 122.4(2) . . ? C21 C22 C42 127.4(2) . . ? C23 C22 Zr 77.60(12) . . ? C21 C22 Zr 70.83(11) . . ? C42 C22 Zr 126.94(15) . . ? C24 C23 C22 108.09(19) . . ? C24 C23 C43 125.5(2) . . ? C22 C23 C43 125.8(2) . . ? C24 C23 Zr 73.66(13) . . ? C22 C23 Zr 70.58(12) . . ? C43 C23 Zr 128.37(15) . . ? C23 C24 C25 108.1(2) . . ? C23 C24 C44 125.8(2) . . ? C25 C24 C44 125.8(2) . . ? C23 C24 Zr 74.97(12) . . ? C25 C24 Zr 69.62(12) . . ? C44 C24 Zr 125.79(16) . . ? C24 C25 C21 108.90(19) . . ? C24 C25 C45 123.0(2) . . ? C21 C25 C45 127.9(2) . . ? C24 C25 Zr 78.03(12) . . ? C21 C25 Zr 72.08(11) . . ? C45 C25 Zr 120.96(15) . . ? C52 C51 C56 114.7(2) . . ? C52 C51 Zr 129.35(18) . . ? C56 C51 Zr 115.58(19) . . ? C51 C52 C53 123.1(3) . . ? C54 C53 C52 120.4(3) . . ? C53 C54 C55 118.8(3) . . ? C54 C55 C56 120.4(3) . . ? C55 C56 C51 122.5(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.329 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.061 data_hbs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 N Zr' _chemical_formula_weight 478.81 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' '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 8.7032(7) _cell_length_b 9.6822(8) _cell_length_c 15.8118(12) _cell_angle_alpha 89.3260(10) _cell_angle_beta 79.892(2) _cell_angle_gamma 70.0910(10) _cell_volume 1231.66(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9554 _exptl_absorpt_correction_T_max 0.9774 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6631 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5018 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5018 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 1.007 _refine_ls_shift/su_mean 0.005 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 Zr Zr 0.29509(4) -0.24428(3) 0.26639(2) 0.03171(12) Uani 1 1 d . . . N N 0.4811(4) -0.1524(4) 0.2394(2) 0.0464(7) Uani 1 1 d . . . C1 C 0.4670(5) -0.0470(4) 0.1893(2) 0.0470(9) Uani 1 1 d . . . C2 C 0.6002(7) 0.0219(8) 0.1663(4) 0.0788(16) Uani 1 1 d . . . H2A H 0.538(8) 0.142(8) 0.169(4) 0.14(3) Uiso 1 1 d . . . H2B H 0.692(6) -0.026(5) 0.199(3) 0.069(14) Uiso 1 1 d . . . H2C H 0.647(6) 0.001(5) 0.109(3) 0.073(15) Uiso 1 1 d . . . C11 C 0.4500(6) -0.5161(4) 0.2367(3) 0.0636(12) Uani 1 1 d . . . C12 C 0.2871(5) -0.4957(4) 0.2236(2) 0.0496(10) Uani 1 1 d . . . C13 C 0.2610(5) -0.4101(4) 0.1520(2) 0.0412(8) Uani 1 1 d . . . C14 C 0.4067(5) -0.3801(4) 0.1184(2) 0.0472(9) Uani 1 1 d . . . C15 C 0.5245(5) -0.4477(5) 0.1703(3) 0.0629(12) Uani 1 1 d . . . C21 C 0.1785(5) -0.2742(4) 0.4220(2) 0.0449(9) Uani 1 1 d . . . C22 C 0.0421(5) -0.1829(5) 0.3864(2) 0.0568(11) Uani 1 1 d . . . C23 C 0.0682(6) -0.0484(5) 0.3696(2) 0.0587(12) Uani 1 1 d . . . C24 C 0.2178(6) -0.0573(4) 0.3922(2) 0.0525(10) Uani 1 1 d . . . C25 C 0.2867(5) -0.1978(4) 0.4241(2) 0.0429(8) Uani 1 1 d . . . C31 C 0.5403(9) -0.6155(6) 0.3002(4) 0.124(3) Uani 1 1 d . . . H31A H 0.6224 -0.7034 0.2698 0.186 Uiso 1 1 calc R . . H31B H 0.4612 -0.6429 0.3420 0.186 Uiso 1 1 calc R . . H31C H 0.5953 -0.5640 0.3296 0.186 Uiso 1 1 calc R . . C32 C 0.1688(8) -0.5684(6) 0.2677(3) 0.0900(18) Uani 1 1 d . . . H32A H 0.0572 -0.4967 0.2803 0.135 Uiso 1 1 calc R . . H32B H 0.2025 -0.6075 0.3210 0.135 Uiso 1 1 calc R . . H32C H 0.1705 -0.6479 0.2304 0.135 Uiso 1 1 calc R . . C33 C 0.1087(6) -0.3740(5) 0.1115(3) 0.0701(13) Uani 1 1 d . . . H33A H 0.1091 -0.4619 0.0825 0.105 Uiso 1 1 calc R . . H33B H 0.1088 -0.2992 0.0701 0.105 Uiso 1 1 calc R . . H33C H 0.0099 -0.3377 0.1557 0.105 Uiso 1 1 calc R . . C34 C 0.4369(7) -0.3034(5) 0.0375(3) 0.0816(16) Uani 1 1 d . . . H34A H 0.5019 -0.2425 0.0458 0.122 Uiso 1 1 calc R . . H34B H 0.3313 -0.2422 0.0236 0.122 Uiso 1 1 calc R . . H34C H 0.4970 -0.3759 -0.0093 0.122 Uiso 1 1 calc R . . C35 C 0.7027(6) -0.4540(7) 0.1536(5) 0.124(3) Uani 1 1 d . . . H35A H 0.7717 -0.5431 0.1193 0.186 Uiso 1 1 calc R . . H35B H 0.7401 -0.4542 0.2079 0.186 Uiso 1 1 calc R . . H35C H 0.7112 -0.3690 0.1227 0.186 Uiso 1 1 calc R . . C41 C 0.1867(8) -0.4160(5) 0.4654(3) 0.0864(17) Uani 1 1 d . . . H41A H 0.1423 -0.3949 0.5263 0.130 Uiso 1 1 calc R . . H41B H 0.3014 -0.4815 0.4574 0.130 Uiso 1 1 calc R . . H41C H 0.1217 -0.4627 0.4401 0.130 Uiso 1 1 calc R . . C42 C -0.1139(6) -0.2131(8) 0.3765(3) 0.110(2) Uani 1 1 d . . . H42A H -0.1049 -0.3114 0.3942 0.165 Uiso 1 1 calc R . . H42B H -0.1270 -0.2055 0.3167 0.165 Uiso 1 1 calc R . . H42C H -0.2097 -0.1418 0.4121 0.165 Uiso 1 1 calc R . . C43 C -0.0584(8) 0.0909(6) 0.3465(3) 0.122(3) Uani 1 1 d . . . H43A H -0.1180 0.1514 0.3984 0.184 Uiso 1 1 calc R . . H43B H -0.1362 0.0659 0.3180 0.184 Uiso 1 1 calc R . . H43C H -0.0021 0.1448 0.3082 0.184 Uiso 1 1 calc R . . C44 C 0.2872(9) 0.0657(6) 0.3909(3) 0.112(2) Uani 1 1 d . . . H44A H 0.2841 0.1102 0.3356 0.167 Uiso 1 1 calc R . . H44B H 0.4013 0.0268 0.3999 0.167 Uiso 1 1 calc R . . H44C H 0.2211 0.1393 0.4362 0.167 Uiso 1 1 calc R . . C45 C 0.4470(6) -0.2519(7) 0.4582(3) 0.0843(16) Uani 1 1 d . . . H45A H 0.5343 -0.2338 0.4173 0.126 Uiso 1 1 calc R . . H45B H 0.4770 -0.3566 0.4664 0.126 Uiso 1 1 calc R . . H45C H 0.4328 -0.2001 0.5127 0.126 Uiso 1 1 calc R . . C51 C 0.1943(4) -0.0579(4) 0.1778(2) 0.0364(8) Uani 1 1 d . . . C52 C 0.3107(4) 0.0144(4) 0.1540(2) 0.0393(8) Uani 1 1 d . . . C53 C 0.2791(6) 0.1314(4) 0.0994(2) 0.0583(11) Uani 1 1 d . . . H53A H 0.3585 0.1773 0.0836 0.070 Uiso 1 1 calc R . . C54 C 0.1323(7) 0.1799(5) 0.0686(3) 0.0668(13) Uani 1 1 d . . . H54A H 0.1105 0.2601 0.0330 0.080 Uiso 1 1 calc R . . C55 C 0.0191(6) 0.1117(5) 0.0899(3) 0.0594(11) Uani 1 1 d . . . H55A H -0.0801 0.1435 0.0678 0.071 Uiso 1 1 calc R . . C56 C 0.0489(5) -0.0052(4) 0.1442(2) 0.0469(9) Uani 1 1 d . . . H56A H -0.0320 -0.0499 0.1587 0.056 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 Zr 0.03582(19) 0.02975(17) 0.02775(18) 0.00494(11) -0.00615(12) -0.00890(12) N 0.0405(17) 0.0541(19) 0.0446(18) -0.0035(15) -0.0077(14) -0.0162(15) C1 0.046(2) 0.053(2) 0.044(2) -0.0054(18) 0.0014(17) -0.0244(18) C2 0.066(3) 0.105(5) 0.082(4) 0.002(4) -0.003(3) -0.055(3) C11 0.087(3) 0.0287(19) 0.062(3) -0.0040(18) -0.034(3) 0.007(2) C12 0.075(3) 0.0313(18) 0.044(2) 0.0040(16) -0.010(2) -0.0215(19) C13 0.055(2) 0.0342(18) 0.0365(19) 0.0010(15) -0.0121(17) -0.0156(16) C14 0.061(2) 0.038(2) 0.039(2) -0.0082(16) 0.0058(19) -0.0198(18) C15 0.048(2) 0.057(3) 0.072(3) -0.030(2) -0.003(2) -0.005(2) C21 0.065(2) 0.050(2) 0.0237(17) 0.0080(15) -0.0049(17) -0.0275(19) C22 0.038(2) 0.092(3) 0.036(2) 0.000(2) 0.0009(17) -0.021(2) C23 0.062(3) 0.057(3) 0.032(2) 0.0013(18) -0.0011(19) 0.009(2) C24 0.085(3) 0.040(2) 0.0289(19) -0.0017(16) 0.003(2) -0.024(2) C25 0.047(2) 0.056(2) 0.0266(18) 0.0063(16) -0.0104(16) -0.0178(18) C31 0.174(6) 0.053(3) 0.117(5) -0.004(3) -0.089(5) 0.026(4) C32 0.163(5) 0.073(3) 0.057(3) 0.009(3) -0.001(3) -0.079(4) C33 0.083(3) 0.065(3) 0.071(3) -0.001(2) -0.039(3) -0.026(3) C34 0.133(5) 0.066(3) 0.045(2) -0.008(2) 0.026(3) -0.052(3) C35 0.035(3) 0.126(5) 0.187(7) -0.087(5) 0.009(3) -0.010(3) C41 0.156(5) 0.065(3) 0.048(3) 0.021(2) -0.008(3) -0.055(3) C42 0.061(3) 0.204(7) 0.069(4) -0.028(4) 0.008(3) -0.060(4) C43 0.126(5) 0.103(4) 0.050(3) -0.006(3) -0.003(3) 0.067(4) C44 0.218(7) 0.082(4) 0.054(3) -0.017(3) 0.020(4) -0.097(5) C45 0.068(3) 0.139(5) 0.055(3) 0.013(3) -0.033(3) -0.037(3) C51 0.0418(19) 0.0353(18) 0.0283(17) 0.0014(14) -0.0040(15) -0.0096(15) C52 0.048(2) 0.0415(19) 0.0293(18) 0.0014(15) -0.0010(15) -0.0192(16) C53 0.089(3) 0.052(2) 0.042(2) 0.0104(19) -0.005(2) -0.037(2) C54 0.101(4) 0.050(2) 0.047(3) 0.020(2) -0.025(3) -0.018(3) C55 0.073(3) 0.052(2) 0.047(2) 0.0073(19) -0.031(2) -0.004(2) C56 0.045(2) 0.049(2) 0.042(2) 0.0061(17) -0.0134(17) -0.0078(17) _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 Zr N 2.079(3) . ? Zr C51 2.298(3) . ? Zr C11 2.521(4) . ? Zr C25 2.524(3) . ? Zr C24 2.544(4) . ? Zr C22 2.544(4) . ? Zr C21 2.545(3) . ? Zr C15 2.549(4) . ? Zr C13 2.553(3) . ? Zr C23 2.560(4) . ? Zr C14 2.560(3) . ? Zr C12 2.561(4) . ? N C1 1.270(5) . ? C1 C52 1.490(5) . ? C1 C2 1.515(6) . ? C11 C15 1.413(7) . ? C11 C12 1.415(6) . ? C11 C31 1.514(6) . ? C12 C13 1.400(5) . ? C12 C32 1.509(6) . ? C13 C14 1.410(5) . ? C13 C33 1.506(5) . ? C14 C15 1.407(6) . ? C14 C34 1.499(5) . ? C15 C35 1.507(6) . ? C21 C25 1.386(5) . ? C21 C22 1.419(6) . ? C21 C41 1.513(5) . ? C22 C23 1.410(6) . ? C22 C42 1.517(6) . ? C23 C24 1.384(6) . ? C23 C43 1.512(6) . ? C24 C25 1.414(5) . ? C24 C44 1.507(6) . ? C25 C45 1.507(5) . ? C51 C56 1.391(5) . ? C51 C52 1.415(5) . ? C52 C53 1.397(5) . ? C53 C54 1.376(6) . ? C54 C55 1.357(6) . ? C55 C56 1.394(5) . ? 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 N Zr C51 75.99(12) . . ? N Zr C11 103.55(15) . . ? C51 Zr C11 132.12(13) . . ? N Zr C25 88.03(12) . . ? C51 Zr C25 122.51(12) . . ? C11 Zr C25 105.18(13) . . ? N Zr C24 78.07(13) . . ? C51 Zr C24 90.10(12) . . ? C11 Zr C24 137.36(14) . . ? C25 Zr C24 32.41(12) . . ? N Zr C22 130.91(13) . . ? C51 Zr C22 98.91(13) . . ? C11 Zr C22 114.00(17) . . ? C25 Zr C22 53.15(12) . . ? C24 Zr C22 52.93(14) . . ? N Zr C21 119.63(12) . . ? C51 Zr C21 129.09(12) . . ? C11 Zr C21 93.52(14) . . ? C25 Zr C21 31.73(11) . . ? C24 Zr C21 53.02(11) . . ? C22 Zr C21 32.39(13) . . ? N Zr C15 78.47(13) . . ? C51 Zr C15 106.06(15) . . ? C11 Zr C15 32.36(15) . . ? C25 Zr C15 124.43(14) . . ? C24 Zr C15 147.17(15) . . ? C22 Zr C15 145.90(16) . . ? C21 Zr C15 124.00(15) . . ? N Zr C13 119.49(12) . . ? C51 Zr C13 84.80(12) . . ? C11 Zr C13 53.08(13) . . ? C25 Zr C13 146.62(12) . . ? C24 Zr C13 159.55(14) . . ? C22 Zr C13 108.29(13) . . ? C21 Zr C13 116.97(11) . . ? C15 Zr C13 52.75(13) . . ? N Zr C23 102.37(14) . . ? C51 Zr C23 76.97(12) . . ? C11 Zr C23 145.08(16) . . ? C25 Zr C23 52.88(13) . . ? C24 Zr C23 31.47(14) . . ? C22 Zr C23 32.09(14) . . ? C21 Zr C23 53.03(12) . . ? C15 Zr C23 176.96(15) . . ? C13 Zr C23 128.33(14) . . ? N Zr C14 87.67(12) . . ? C51 Zr C14 78.88(12) . . ? C11 Zr C14 53.47(14) . . ? C25 Zr C14 156.25(13) . . ? C24 Zr C14 163.79(11) . . ? C22 Zr C14 140.12(13) . . ? C21 Zr C14 142.94(12) . . ? C15 Zr C14 31.97(14) . . ? C13 Zr C14 32.00(11) . . ? C23 Zr C14 150.60(14) . . ? N Zr C12 131.57(13) . . ? C51 Zr C12 115.70(12) . . ? C11 Zr C12 32.32(14) . . ? C25 Zr C12 115.92(12) . . ? C24 Zr C12 143.07(12) . . ? C22 Zr C12 95.18(14) . . ? C21 Zr C12 90.18(12) . . ? C15 Zr C12 53.14(14) . . ? C13 Zr C12 31.76(11) . . ? C23 Zr C12 125.85(15) . . ? C14 Zr C12 53.13(11) . . ? C1 N Zr 120.6(3) . . ? N C1 C52 118.6(3) . . ? N C1 C2 122.6(4) . . ? C52 C1 C2 118.7(4) . . ? C15 C11 C12 107.9(4) . . ? C15 C11 C31 125.0(5) . . ? C12 C11 C31 126.3(5) . . ? C15 C11 Zr 74.9(2) . . ? C12 C11 Zr 75.4(2) . . ? C31 C11 Zr 123.8(3) . . ? C13 C12 C11 107.4(3) . . ? C13 C12 C32 124.1(4) . . ? C11 C12 C32 128.0(4) . . ? C13 C12 Zr 73.82(19) . . ? C11 C12 Zr 72.3(2) . . ? C32 C12 Zr 126.2(3) . . ? C12 C13 C14 109.2(3) . . ? C12 C13 C33 124.5(4) . . ? C14 C13 C33 125.8(4) . . ? C12 C13 Zr 74.4(2) . . ? C14 C13 Zr 74.3(2) . . ? C33 C13 Zr 123.8(3) . . ? C15 C14 C13 107.2(3) . . ? C15 C14 C34 126.1(4) . . ? C13 C14 C34 126.5(4) . . ? C15 C14 Zr 73.6(2) . . ? C13 C14 Zr 73.7(2) . . ? C34 C14 Zr 122.7(3) . . ? C14 C15 C11 108.3(4) . . ? C14 C15 C35 125.2(5) . . ? C11 C15 C35 126.4(5) . . ? C14 C15 Zr 74.4(2) . . ? C11 C15 Zr 72.7(2) . . ? C35 C15 Zr 122.1(3) . . ? C25 C21 C22 107.8(3) . . ? C25 C21 C41 125.9(4) . . ? C22 C21 C41 125.3(4) . . ? C25 C21 Zr 73.29(19) . . ? C22 C21 Zr 73.78(19) . . ? C41 C21 Zr 127.5(3) . . ? C23 C22 C21 107.3(4) . . ? C23 C22 C42 124.6(5) . . ? C21 C22 C42 127.8(5) . . ? C23 C22 Zr 74.6(2) . . ? C21 C22 Zr 73.8(2) . . ? C42 C22 Zr 122.3(3) . . ? C24 C23 C22 108.5(3) . . ? C24 C23 C43 124.9(5) . . ? C22 C23 C43 125.8(5) . . ? C24 C23 Zr 73.6(2) . . ? C22 C23 Zr 73.4(2) . . ? C43 C23 Zr 127.3(3) . . ? C23 C24 C25 108.0(3) . . ? C23 C24 C44 126.0(5) . . ? C25 C24 C44 125.8(5) . . ? C23 C24 Zr 74.9(2) . . ? C25 C24 Zr 73.0(2) . . ? C44 C24 Zr 122.3(3) . . ? C21 C25 C24 108.4(3) . . ? C21 C25 C45 126.1(4) . . ? C24 C25 C45 125.5(4) . . ? C21 C25 Zr 75.0(2) . . ? C24 C25 Zr 74.6(2) . . ? C45 C25 Zr 118.7(3) . . ? C56 C51 C52 116.2(3) . . ? C56 C51 Zr 134.0(3) . . ? C52 C51 Zr 109.9(2) . . ? C53 C52 C51 121.0(3) . . ? C53 C52 C1 124.2(3) . . ? C51 C52 C1 114.9(3) . . ? C54 C53 C52 120.4(4) . . ? C55 C54 C53 119.9(4) . . ? C54 C55 C56 120.4(4) . . ? C51 C56 C55 122.2(4) . . ? _diffrn_measured_fraction_theta_max 0.822 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.822 _refine_diff_density_max 0.469 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.071 data_hyo10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H43 Si Zr' _chemical_formula_weight 583.00 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8990(10) _cell_length_b 11.497(2) _cell_length_c 13.928(2) _cell_angle_alpha 74.670(10) _cell_angle_beta 79.250(10) _cell_angle_gamma 86.970(10) _cell_volume 1501.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method ? _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 0.427 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6098 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5130 _reflns_number_observed 4625 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+0.9547P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0054(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5130 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_obs 0.0401 _refine_ls_wR_factor_all 0.1127 _refine_ls_wR_factor_obs 0.1079 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.063 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.063 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr Zr 0.26727(3) 0.26358(2) -0.21422(2) 0.03008(12) Uani 1 d . . Si Si 0.22444(9) 0.45554(9) -0.42932(7) 0.0452(2) Uani 1 d . . C1 C 0.1880(4) 0.4208(4) -0.5455(3) 0.0713(12) Uani 1 d . . H1A H 0.1829(4) 0.3351(4) -0.5347(3) 0.107 Uiso 1 calc R . H1B H 0.2604(4) 0.4526(4) -0.6015(3) 0.107 Uiso 1 calc R . H1C H 0.1021(4) 0.4570(4) -0.5603(3) 0.107 Uiso 1 calc R . C2 C 0.2308(4) 0.6239(3) -0.4636(3) 0.0704(12) Uani 1 d . . H2A H 0.2493(4) 0.6502(3) -0.4074(3) 0.106 Uiso 1 calc R . H2B H 0.1441(4) 0.6563(3) -0.4799(3) 0.106 Uiso 1 calc R . H2C H 0.3023(4) 0.6518(3) -0.5210(3) 0.106 Uiso 1 calc R . C11 C 0.3839(3) 0.3817(3) -0.3831(2) 0.0387(7) Uani 1 d . . C12 C 0.4279(3) 0.2611(3) -0.3792(2) 0.0399(7) Uani 1 d . . C13 C 0.5167(3) 0.2253(3) -0.3084(2) 0.0399(7) Uani 1 d . . C14 C 0.5293(3) 0.3233(3) -0.2663(2) 0.0407(7) Uani 1 d . . C15 C 0.4477(3) 0.4193(3) -0.3123(2) 0.0386(7) Uani 1 d . . C21 C 0.0975(3) 0.3855(3) -0.3113(2) 0.0379(6) Uani 1 d . . C22 C 0.0500(3) 0.2631(3) -0.2842(2) 0.0365(6) Uani 1 d . . C23 C 0.0029(3) 0.2268(3) -0.1783(2) 0.0389(7) Uani 1 d . . C24 C 0.0183(3) 0.3260(3) -0.1390(2) 0.0402(7) Uani 1 d . . C25 C 0.0763(3) 0.4224(3) -0.2189(2) 0.0389(7) Uani 1 d . . C32 C 0.4035(4) 0.1833(3) -0.4467(3) 0.0539(9) Uani 1 d . . H32A H 0.3401(4) 0.2233(3) -0.4893(3) 0.081 Uiso 1 calc R . H32B H 0.3658(4) 0.1072(3) -0.4056(3) 0.081 Uiso 1 calc R . H32C H 0.4890(4) 0.1700(3) -0.4879(3) 0.081 Uiso 1 calc R . C33 C 0.6025(4) 0.1122(3) -0.2918(3) 0.0551(9) Uani 1 d . . H33A H 0.6535(4) 0.1099(3) -0.2390(3) 0.083 Uiso 1 calc R . H33B H 0.6652(4) 0.1115(3) -0.3532(3) 0.083 Uiso 1 calc R . H33C H 0.5436(4) 0.0430(3) -0.2725(3) 0.083 Uiso 1 calc R . C34 C 0.6280(4) 0.3262(4) -0.1981(3) 0.0564(9) Uani 1 d . . H34A H 0.6687(4) 0.2479(4) -0.1783(3) 0.085 Uiso 1 calc R . H34B H 0.5800(4) 0.3485(4) -0.1389(3) 0.085 Uiso 1 calc R . H34C H 0.6987(4) 0.3842(4) -0.2330(3) 0.085 Uiso 1 calc R . C35 C 0.4515(4) 0.5451(3) -0.2987(3) 0.0541(9) Uani 1 d . . H35A H 0.3888(4) 0.5961(3) -0.3361(3) 0.081 Uiso 1 calc R . H35B H 0.5430(4) 0.5768(3) -0.3232(3) 0.081 Uiso 1 calc R . H35C H 0.4253(4) 0.5425(3) -0.2283(3) 0.081 Uiso 1 calc R . C42 C 0.0262(4) 0.1920(3) -0.3554(3) 0.0544(9) Uani 1 d . . H42A H 0.0668(4) 0.2332(3) -0.4233(3) 0.082 Uiso 1 calc R . H42B H -0.0708(4) 0.1835(3) -0.3513(3) 0.082 Uiso 1 calc R . H42C H 0.0675(4) 0.1136(3) -0.3373(3) 0.082 Uiso 1 calc R . C43 C -0.0673(4) 0.1103(3) -0.1195(3) 0.0527(9) Uani 1 d . . H43A H -0.0643(4) 0.0576(3) -0.1631(3) 0.079 Uiso 1 calc R . H43B H -0.1614(4) 0.1261(3) -0.0936(3) 0.079 Uiso 1 calc R . H43C H -0.0213(4) 0.0726(3) -0.0643(3) 0.079 Uiso 1 calc R . C44 C -0.0394(4) 0.3343(4) -0.0333(3) 0.0608(10) Uani 1 d . . H44A H -0.0730(4) 0.2567(4) 0.0075(3) 0.091 Uiso 1 calc R . H44B H -0.1135(4) 0.3918(4) -0.0350(3) 0.091 Uiso 1 calc R . H44C H 0.0314(4) 0.3598(4) -0.0048(3) 0.091 Uiso 1 calc R . C45 C 0.0900(4) 0.5464(3) -0.2050(3) 0.0564(9) Uani 1 d . . H45A H 0.1318(4) 0.5993(3) -0.2680(3) 0.085 Uiso 1 calc R . H45B H 0.1463(4) 0.5423(3) -0.1550(3) 0.085 Uiso 1 calc R . H45C H 0.0006(4) 0.5768(3) -0.1830(3) 0.085 Uiso 1 calc R . C51 C 0.2893(3) 0.2944(3) -0.0611(2) 0.0444(7) Uani 1 d . . C52 C 0.3357(4) 0.3937(3) -0.0370(3) 0.0548(9) Uani 1 d . . H52A H 0.3714(4) 0.4592(3) -0.0892(3) 0.066 Uiso 1 calc R . C53 C 0.3305(4) 0.3982(4) 0.0623(3) 0.0686(12) Uani 1 d . . H53A H 0.3616(4) 0.4665(4) 0.0753(3) 0.082 Uiso 1 calc R . C54 C 0.2800(5) 0.3030(5) 0.1411(3) 0.0730(12) Uani 1 d . . H54A H 0.2773(5) 0.3059(5) 0.2075(3) 0.088 Uiso 1 calc R . C55 C 0.2336(4) 0.2033(4) 0.1212(3) 0.0635(10) Uani 1 d . . H55A H 0.1996(4) 0.1379(4) 0.1742(3) 0.076 Uiso 1 calc R . C56 C 0.2374(4) 0.2001(3) 0.0228(3) 0.0521(8) Uani 1 d . . H56A H 0.2038(4) 0.1319(3) 0.0113(3) 0.063 Uiso 1 calc R . C61 C 0.2828(3) 0.0556(3) -0.1788(2) 0.0401(7) Uani 1 d . . C62 C 0.3662(3) 0.0024(3) -0.1086(3) 0.0478(8) Uani 1 d . . H62A H 0.4012(3) 0.0510(3) -0.0753(3) 0.057 Uiso 1 calc R . C63 C 0.3995(4) -0.1191(3) -0.0860(3) 0.0573(9) Uani 1 d . . H63A H 0.4549(4) -0.1504(3) -0.0381(3) 0.069 Uiso 1 calc R . C64 C 0.3511(4) -0.1932(3) -0.1342(3) 0.0645(11) Uani 1 d . . H64A H 0.3738(4) -0.2747(3) -0.1199(3) 0.077 Uiso 1 calc R . C65 C 0.2685(5) -0.1453(3) -0.2038(4) 0.0666(11) Uani 1 d . . H65A H 0.2343(5) -0.1947(3) -0.2369(4) 0.080 Uiso 1 calc R . C66 C 0.2357(4) -0.0242(3) -0.2251(3) 0.0521(8) Uani 1 d . . H66A H 0.1795(4) 0.0058(3) -0.2727(3) 0.063 Uiso 1 calc R . C71 C 0.1236(8) -0.0488(6) -0.4799(5) 0.099(2) Uani 1 d . . H71A H 0.2079(8) -0.0816(6) -0.4660(5) 0.119 Uiso 1 calc R . C72 C 0.1190(7) 0.0472(6) -0.5620(5) 0.099(2) Uani 1 d . . H72A H 0.2002(7) 0.0787(6) -0.6043(5) 0.118 Uiso 1 calc R . C73 C -0.0039(8) 0.0968(5) -0.5821(5) 0.099(2) Uani 1 d . . H73A H -0.0068(8) 0.1627(5) -0.6374(5) 0.119 Uiso 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 Zr 0.0292(2) 0.0287(2) 0.0316(2) -0.00791(11) -0.00336(11) -0.00065(11) Si 0.0375(5) 0.0480(5) 0.0395(5) 0.0037(4) -0.0035(4) 0.0036(4) C1 0.053(2) 0.114(4) 0.038(2) -0.005(2) -0.009(2) 0.009(2) C2 0.054(2) 0.051(2) 0.081(3) 0.021(2) -0.004(2) 0.005(2) C11 0.034(2) 0.038(2) 0.0358(15) -0.0007(12) 0.0013(12) -0.0009(12) C12 0.034(2) 0.045(2) 0.036(2) -0.0079(13) 0.0031(12) 0.0007(13) C13 0.0292(15) 0.042(2) 0.042(2) -0.0054(13) 0.0030(12) 0.0015(12) C14 0.0310(15) 0.042(2) 0.043(2) -0.0060(13) 0.0012(12) -0.0031(13) C15 0.0310(15) 0.035(2) 0.044(2) -0.0053(12) 0.0024(12) -0.0043(12) C21 0.0325(15) 0.037(2) 0.041(2) -0.0076(12) -0.0053(12) 0.0052(12) C22 0.0322(15) 0.038(2) 0.040(2) -0.0101(12) -0.0107(12) 0.0030(12) C23 0.0276(14) 0.041(2) 0.043(2) -0.0040(13) -0.0019(12) -0.0019(12) C24 0.0313(15) 0.045(2) 0.041(2) -0.0109(13) -0.0012(12) 0.0043(13) C25 0.034(2) 0.035(2) 0.046(2) -0.0125(13) -0.0028(13) 0.0037(12) C32 0.060(2) 0.057(2) 0.046(2) -0.020(2) -0.004(2) 0.002(2) C33 0.041(2) 0.050(2) 0.066(2) -0.010(2) 0.002(2) 0.011(2) C34 0.043(2) 0.067(2) 0.059(2) -0.013(2) -0.014(2) -0.002(2) C35 0.049(2) 0.039(2) 0.069(2) -0.010(2) -0.003(2) -0.0060(15) C42 0.055(2) 0.057(2) 0.060(2) -0.021(2) -0.027(2) 0.000(2) C43 0.041(2) 0.048(2) 0.059(2) 0.002(2) -0.004(2) -0.0089(15) C44 0.053(2) 0.076(3) 0.049(2) -0.020(2) 0.005(2) 0.009(2) C45 0.054(2) 0.041(2) 0.075(2) -0.023(2) -0.003(2) 0.005(2) C51 0.038(2) 0.056(2) 0.043(2) -0.0199(14) -0.0051(13) -0.0014(14) C52 0.052(2) 0.057(2) 0.061(2) -0.025(2) -0.011(2) -0.004(2) C53 0.064(3) 0.081(3) 0.081(3) -0.053(3) -0.017(2) 0.000(2) C54 0.072(3) 0.108(4) 0.051(2) -0.040(2) -0.016(2) 0.010(3) C55 0.068(3) 0.075(3) 0.046(2) -0.015(2) -0.007(2) 0.005(2) C56 0.050(2) 0.056(2) 0.053(2) -0.023(2) -0.003(2) -0.003(2) C61 0.038(2) 0.031(2) 0.047(2) -0.0085(13) -0.0011(13) 0.0011(12) C62 0.043(2) 0.049(2) 0.051(2) -0.015(2) -0.0037(15) -0.0011(15) C63 0.047(2) 0.057(2) 0.056(2) 0.001(2) -0.003(2) 0.009(2) C64 0.066(3) 0.034(2) 0.085(3) -0.006(2) -0.007(2) 0.005(2) C65 0.073(3) 0.041(2) 0.093(3) -0.027(2) -0.020(2) 0.001(2) C66 0.057(2) 0.041(2) 0.061(2) -0.014(2) -0.016(2) -0.001(2) C71 0.129(5) 0.093(4) 0.108(4) -0.070(4) -0.048(4) 0.041(4) C72 0.128(5) 0.086(4) 0.101(4) -0.063(4) -0.016(4) 0.013(4) C73 0.154(6) 0.078(4) 0.081(3) -0.047(3) -0.032(4) 0.030(4) _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 Zr C51 2.303(3) . ? Zr C61 2.313(3) . ? Zr C11 2.485(3) . ? Zr C21 2.492(3) . ? Zr C22 2.523(3) . ? Zr C15 2.529(3) . ? Zr C12 2.545(3) . ? Zr C25 2.555(3) . ? Zr C23 2.607(3) . ? Zr C24 2.633(3) . ? Zr C14 2.636(3) . ? Zr C13 2.644(3) . ? Si C1 1.867(4) . ? Si C2 1.869(4) . ? Si C21 1.889(3) . ? Si C11 1.891(3) . ? C11 C12 1.422(4) . ? C11 C15 1.429(4) . ? C12 C13 1.409(4) . ? C12 C32 1.514(5) . ? C13 C14 1.421(5) . ? C13 C33 1.505(4) . ? C14 C15 1.416(4) . ? C14 C34 1.492(5) . ? C15 C35 1.511(4) . ? C21 C25 1.434(4) . ? C21 C22 1.437(4) . ? C22 C23 1.416(4) . ? C22 C42 1.498(4) . ? C23 C24 1.415(4) . ? C23 C43 1.501(4) . ? C24 C25 1.404(4) . ? C24 C44 1.503(4) . ? C25 C45 1.505(4) . ? C51 C52 1.394(5) . ? C51 C56 1.404(5) . ? C52 C53 1.389(5) . ? C53 C54 1.367(6) . ? C54 C55 1.368(6) . ? C55 C56 1.373(5) . ? C61 C66 1.394(5) . ? C61 C62 1.394(5) . ? C62 C63 1.385(5) . ? C63 C64 1.368(6) . ? C64 C65 1.370(6) . ? C65 C66 1.379(5) . ? C71 C72 1.370(8) . ? C71 C73 1.375(9) 2_554 ? C72 C73 1.361(9) . ? C73 C71 1.375(9) 2_554 ? 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 C51 Zr C61 100.91(12) . . ? C51 Zr C11 125.67(11) . . ? C61 Zr C11 117.60(11) . . ? C51 Zr C21 119.53(11) . . ? C61 Zr C21 123.81(11) . . ? C11 Zr C21 69.22(10) . . ? C51 Zr C22 128.06(11) . . ? C61 Zr C22 91.34(11) . . ? C11 Zr C22 89.69(10) . . ? C21 Zr C22 33.30(10) . . ? C51 Zr C15 92.96(11) . . ? C61 Zr C15 128.83(10) . . ? C11 Zr C15 33.10(10) . . ? C21 Zr C15 88.55(10) . . ? C22 Zr C15 117.63(10) . . ? C51 Zr C12 136.15(11) . . ? C61 Zr C12 85.04(10) . . ? C11 Zr C12 32.82(10) . . ? C21 Zr C12 90.07(10) . . ? C22 Zr C12 94.77(10) . . ? C15 Zr C12 53.50(10) . . ? C51 Zr C25 86.61(11) . . ? C61 Zr C25 137.11(10) . . ? C11 Zr C25 89.25(10) . . ? C21 Zr C25 32.98(10) . . ? C22 Zr C25 53.73(10) . . ? C15 Zr C25 92.28(10) . . ? C12 Zr C25 118.17(10) . . ? C51 Zr C23 98.83(11) . . ? C61 Zr C23 84.41(10) . . ? C11 Zr C23 120.51(10) . . ? C21 Zr C23 54.08(10) . . ? C22 Zr C23 32.00(10) . . ? C15 Zr C23 141.79(10) . . ? C12 Zr C23 125.01(10) . . ? C25 Zr C23 52.71(10) . . ? C51 Zr C24 75.92(11) . . ? C61 Zr C24 109.42(10) . . ? C11 Zr C24 119.59(10) . . ? C21 Zr C24 53.43(10) . . ? C22 Zr C24 52.56(10) . . ? C15 Zr C24 121.73(10) . . ? C12 Zr C24 143.10(10) . . ? C25 Zr C24 31.37(9) . . ? C23 Zr C24 31.33(10) . . ? C51 Zr C14 83.95(11) . . ? C61 Zr C14 100.94(10) . . ? C11 Zr C14 53.67(10) . . ? C21 Zr C14 119.40(10) . . ? C22 Zr C14 143.00(10) . . ? C15 Zr C14 31.74(10) . . ? C12 Zr C14 52.46(10) . . ? C25 Zr C14 121.90(10) . . ? C23 Zr C14 173.45(9) . . ? C24 Zr C14 146.07(10) . . ? C51 Zr C13 107.34(11) . . ? C61 Zr C13 76.47(10) . . ? C11 Zr C13 53.32(10) . . ? C21 Zr C13 120.16(10) . . ? C22 Zr C13 124.60(10) . . ? C15 Zr C13 52.42(10) . . ? C12 Zr C13 31.43(10) . . ? C25 Zr C13 141.62(10) . . ? C23 Zr C13 149.94(10) . . ? C24 Zr C13 172.88(9) . . ? C14 Zr C13 31.22(10) . . ? C1 Si C2 103.7(2) . . ? C1 Si C21 113.5(2) . . ? C2 Si C21 114.8(2) . . ? C1 Si C11 115.4(2) . . ? C2 Si C11 113.1(2) . . ? C21 Si C11 96.83(13) . . ? C12 C11 C15 106.4(3) . . ? C12 C11 Si 126.1(2) . . ? C15 C11 Si 123.5(2) . . ? C12 C11 Zr 75.9(2) . . ? C15 C11 Zr 75.1(2) . . ? Si C11 Zr 97.05(12) . . ? C13 C12 C11 109.1(3) . . ? C13 C12 C32 122.2(3) . . ? C11 C12 C32 128.3(3) . . ? C13 C12 Zr 78.2(2) . . ? C11 C12 Zr 71.3(2) . . ? C32 C12 Zr 123.1(2) . . ? C12 C13 C14 108.1(3) . . ? C12 C13 C33 126.5(3) . . ? C14 C13 C33 124.6(3) . . ? C12 C13 Zr 70.4(2) . . ? C14 C13 Zr 74.1(2) . . ? C33 C13 Zr 128.9(2) . . ? C15 C14 C13 107.4(3) . . ? C15 C14 C34 127.8(3) . . ? C13 C14 C34 124.2(3) . . ? C15 C14 Zr 70.0(2) . . ? C13 C14 Zr 74.7(2) . . ? C34 C14 Zr 127.6(2) . . ? C14 C15 C11 108.9(3) . . ? C14 C15 C35 122.9(3) . . ? C11 C15 C35 127.4(3) . . ? C14 C15 Zr 78.3(2) . . ? C11 C15 Zr 71.8(2) . . ? C35 C15 Zr 124.4(2) . . ? C25 C21 C22 106.1(3) . . ? C25 C21 Si 125.2(2) . . ? C22 C21 Si 124.4(2) . . ? C25 C21 Zr 75.9(2) . . ? C22 C21 Zr 74.5(2) . . ? Si C21 Zr 96.88(12) . . ? C23 C22 C21 108.8(3) . . ? C23 C22 C42 123.6(3) . . ? C21 C22 C42 126.6(3) . . ? C23 C22 Zr 77.3(2) . . ? C21 C22 Zr 72.2(2) . . ? C42 C22 Zr 126.0(2) . . ? C24 C23 C22 107.6(3) . . ? C24 C23 C43 125.5(3) . . ? C22 C23 C43 126.5(3) . . ? C24 C23 Zr 75.3(2) . . ? C22 C23 Zr 70.7(2) . . ? C43 C23 Zr 125.3(2) . . ? C25 C24 C23 108.8(3) . . ? C25 C24 C44 125.0(3) . . ? C23 C24 C44 125.5(3) . . ? C25 C24 Zr 71.3(2) . . ? C23 C24 Zr 73.3(2) . . ? C44 C24 Zr 129.2(2) . . ? C24 C25 C21 108.7(3) . . ? C24 C25 C45 122.1(3) . . ? C21 C25 C45 128.5(3) . . ? C24 C25 Zr 77.4(2) . . ? C21 C25 Zr 71.1(2) . . ? C45 C25 Zr 125.0(2) . . ? C52 C51 C56 114.6(3) . . ? C52 C51 Zr 131.2(3) . . ? C56 C51 Zr 114.0(2) . . ? C53 C52 C51 122.3(4) . . ? C54 C53 C52 120.4(4) . . ? C53 C54 C55 119.4(4) . . ? C54 C55 C56 119.9(4) . . ? C55 C56 C51 123.4(4) . . ? C66 C61 C62 114.2(3) . . ? C66 C61 Zr 130.2(2) . . ? C62 C61 Zr 115.1(2) . . ? C63 C62 C61 123.2(3) . . ? C64 C63 C62 120.1(4) . . ? C63 C64 C65 118.9(3) . . ? C64 C65 C66 120.3(4) . . ? C65 C66 C61 123.2(4) . . ? C72 C71 C73 120.2(6) . 2_554 ? C73 C72 C71 120.3(7) . . ? C72 C73 C71 119.6(6) . 2_554 ? _refine_diff_density_max 0.726 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.070 data_phcs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 Cl Zr' _chemical_formula_weight 474.21 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' '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 8.4788(4) _cell_length_b 16.1860(8) _cell_length_c 17.4483(9) _cell_angle_alpha 89.9190(10) _cell_angle_beta 85.4150(10) _cell_angle_gamma 83.0840(10) _cell_volume 2369.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8919 _exptl_absorpt_correction_T_max 0.8919 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17064 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.38 _reflns_number_total 10126 _reflns_number_gt 8196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0647P)^2^+1.2028P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10126 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.005 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 0.46022(3) 0.780840(16) 0.359490(15) 0.02647(9) Uani 1 1 d . . . Zr2 Zr 0.92415(3) 0.288849(17) 0.156161(15) 0.02699(9) Uani 1 1 d . . . Cl1 Cl 0.20202(10) 0.73589(7) 0.40252(6) 0.0565(3) Uani 1 1 d . . . Cl2 Cl 0.65821(11) 0.27040(6) 0.21344(7) 0.0621(3) Uani 1 1 d . . . C11 C 0.3695(5) 0.8840(4) 0.4662(3) 0.093(2) Uani 1 1 d . . . C12 C 0.4697(11) 0.9267(2) 0.4124(3) 0.099(3) Uani 1 1 d . . . C13 C 0.6192(7) 0.8875(3) 0.4144(2) 0.0716(15) Uani 1 1 d . . . C14 C 0.6216(5) 0.8286(3) 0.4652(3) 0.0592(12) Uani 1 1 d . . . C15 C 0.4731(6) 0.8223(3) 0.4980(2) 0.0601(12) Uani 1 1 d . . . C21 C 0.5402(4) 0.62489(18) 0.34422(18) 0.0357(7) Uani 1 1 d . . . C22 C 0.6838(4) 0.66055(19) 0.34260(18) 0.0362(7) Uani 1 1 d . . . C23 C 0.6970(3) 0.70917(19) 0.27566(17) 0.0330(7) Uani 1 1 d . . . C24 C 0.5622(3) 0.70111(19) 0.23395(17) 0.0317(6) Uani 1 1 d . . . C25 C 0.4636(3) 0.65011(18) 0.27702(18) 0.0323(6) Uani 1 1 d . . . C31 C 0.1975(7) 0.9091(9) 0.4887(8) 0.360(12) Uani 1 1 d . . . H31A H 0.1505 0.8618 0.5108 0.539 Uiso 1 1 calc R . . H31B H 0.1437 0.9277 0.4436 0.539 Uiso 1 1 calc R . . H31C H 0.1861 0.9539 0.5262 0.539 Uiso 1 1 calc R . . C32 C 0.414(2) 1.0069(4) 0.3753(5) 0.334(11) Uani 1 1 d . . . H32A H 0.5004 1.0241 0.3414 0.501 Uiso 1 1 calc R . . H32B H 0.3813 1.0492 0.4146 0.501 Uiso 1 1 calc R . . H32C H 0.3247 0.9995 0.3457 0.501 Uiso 1 1 calc R . . C33 C 0.7679(13) 0.9190(7) 0.3743(4) 0.235(7) Uani 1 1 d . . . H33A H 0.7904 0.9685 0.4005 0.352 Uiso 1 1 calc R . . H33B H 0.7494 0.9322 0.3213 0.352 Uiso 1 1 calc R . . H33C H 0.8581 0.8761 0.3756 0.352 Uiso 1 1 calc R . . C34 C 0.7725(9) 0.7874(5) 0.4987(5) 0.189(5) Uani 1 1 d . . . H34A H 0.8534 0.7711 0.4573 0.284 Uiso 1 1 calc R . . H34B H 0.7483 0.7386 0.5275 0.284 Uiso 1 1 calc R . . H34C H 0.8115 0.8264 0.5326 0.284 Uiso 1 1 calc R . . C35 C 0.4315(15) 0.7672(6) 0.5628(3) 0.205(6) Uani 1 1 d . . . H35A H 0.4881 0.7119 0.5536 0.308 Uiso 1 1 calc R . . H35B H 0.3176 0.7641 0.5669 0.308 Uiso 1 1 calc R . . H35C H 0.4618 0.7895 0.6103 0.308 Uiso 1 1 calc R . . C41 C 0.4860(6) 0.5639(2) 0.4029(3) 0.0624(11) Uani 1 1 d . . . H41A H 0.5356 0.5083 0.3889 0.094 Uiso 1 1 calc R . . H41B H 0.3711 0.5656 0.4047 0.094 Uiso 1 1 calc R . . H41C H 0.5165 0.5787 0.4531 0.094 Uiso 1 1 calc R . . C42 C 0.8170(5) 0.6323(3) 0.3921(3) 0.0627(12) Uani 1 1 d . . . H42A H 0.8683 0.5781 0.3746 0.094 Uiso 1 1 calc R . . H42B H 0.7743 0.6287 0.4451 0.094 Uiso 1 1 calc R . . H42C H 0.8944 0.6720 0.3886 0.094 Uiso 1 1 calc R . . C43 C 0.8421(4) 0.7481(3) 0.2465(2) 0.0544(10) Uani 1 1 d . . . H43A H 0.8950 0.7662 0.2897 0.082 Uiso 1 1 calc R . . H43B H 0.8105 0.7957 0.2149 0.082 Uiso 1 1 calc R . . H43C H 0.9145 0.7077 0.2160 0.082 Uiso 1 1 calc R . . C44 C 0.5423(5) 0.7265(2) 0.15268(19) 0.0495(9) Uani 1 1 d . . . H44A H 0.6068 0.7708 0.1394 0.074 Uiso 1 1 calc R . . H44B H 0.4312 0.7460 0.1470 0.074 Uiso 1 1 calc R . . H44C H 0.5761 0.6792 0.1187 0.074 Uiso 1 1 calc R . . C45 C 0.3153(4) 0.6223(2) 0.2502(2) 0.0518(10) Uani 1 1 d . . . H45A H 0.3436 0.5781 0.2123 0.078 Uiso 1 1 calc R . . H45B H 0.2533 0.6688 0.2273 0.078 Uiso 1 1 calc R . . H45C H 0.2527 0.6019 0.2936 0.078 Uiso 1 1 calc R . . C51 C 0.3780(4) 0.8658(2) 0.26172(18) 0.0383(7) Uani 1 1 d . . . C52 C 0.4743(5) 0.9099(2) 0.2116(2) 0.0493(9) Uani 1 1 d . . . H52A H 0.5830 0.9077 0.2195 0.059 Uiso 1 1 calc R . . C53 C 0.4167(6) 0.9567(2) 0.1505(3) 0.0661(12) Uani 1 1 d . . . H53A H 0.4858 0.9849 0.1180 0.079 Uiso 1 1 calc R . . C54 C 0.2562(7) 0.9614(3) 0.1381(3) 0.0723(14) Uani 1 1 d . . . H54A H 0.2156 0.9932 0.0973 0.087 Uiso 1 1 calc R . . C55 C 0.1587(6) 0.9199(3) 0.1851(3) 0.0697(14) Uani 1 1 d . . . H55A H 0.0502 0.9229 0.1764 0.084 Uiso 1 1 calc R . . C56 C 0.2163(4) 0.8728(2) 0.2462(2) 0.0500(9) Uani 1 1 d . . . H56A H 0.1452 0.8449 0.2779 0.060 Uiso 1 1 calc R . . C61 C 1.1628(4) 0.18437(19) 0.11052(19) 0.0379(7) Uani 1 1 d . . . C62 C 1.1398(4) 0.1707(2) 0.1890(2) 0.0416(8) Uani 1 1 d . . . C63 C 0.9930(5) 0.1409(2) 0.2041(2) 0.0495(9) Uani 1 1 d . . . C64 C 0.9243(4) 0.1335(2) 0.1332(3) 0.0547(11) Uani 1 1 d . . . C65 C 1.0334(4) 0.1615(2) 0.0746(2) 0.0423(8) Uani 1 1 d . . . C71 C 0.9615(5) 0.3709(2) 0.03337(18) 0.0515(10) Uani 1 1 d . . . C72 C 0.7943(5) 0.3746(2) 0.0534(2) 0.0497(9) Uani 1 1 d . . . C73 C 0.7612(4) 0.4240(2) 0.1194(2) 0.0493(9) Uani 1 1 d . . . C74 C 0.8990(5) 0.4491(2) 0.1420(2) 0.0436(8) Uani 1 1 d . . . C75 C 1.0244(4) 0.4169(2) 0.0908(2) 0.0417(8) Uani 1 1 d . . . C81 C 1.3205(5) 0.2031(3) 0.0700(3) 0.0658(12) Uani 1 1 d . . . H81A H 1.3940 0.1522 0.0650 0.099 Uiso 1 1 calc R . . H81B H 1.3655 0.2436 0.0998 0.099 Uiso 1 1 calc R . . H81C H 1.3023 0.2252 0.0193 0.099 Uiso 1 1 calc R . . C82 C 1.2662(6) 0.1699(3) 0.2454(3) 0.0665(12) Uani 1 1 d . . . H82A H 1.3220 0.1142 0.2481 0.100 Uiso 1 1 calc R . . H82B H 1.2166 0.1870 0.2958 0.100 Uiso 1 1 calc R . . H82C H 1.3414 0.2081 0.2283 0.100 Uiso 1 1 calc R . . C83 C 0.9297(7) 0.1135(3) 0.2817(3) 0.0864(18) Uani 1 1 d . . . H83A H 0.9820 0.0586 0.2926 0.130 Uiso 1 1 calc R . . H83B H 0.8158 0.1116 0.2819 0.130 Uiso 1 1 calc R . . H83C H 0.9504 0.1526 0.3206 0.130 Uiso 1 1 calc R . . C84 C 0.7783(6) 0.0934(3) 0.1198(4) 0.104(2) Uani 1 1 d . . . H84A H 0.8076 0.0342 0.1110 0.156 Uiso 1 1 calc R . . H84B H 0.7302 0.1180 0.0752 0.156 Uiso 1 1 calc R . . H84C H 0.7026 0.1021 0.1646 0.156 Uiso 1 1 calc R . . C85 C 1.0240(7) 0.1461(3) -0.0109(3) 0.0846(17) Uani 1 1 d . . . H85A H 1.1123 0.1679 -0.0398 0.127 Uiso 1 1 calc R . . H85B H 0.9242 0.1739 -0.0268 0.127 Uiso 1 1 calc R . . H85C H 1.0295 0.0868 -0.0205 0.127 Uiso 1 1 calc R . . C91 C 1.0452(8) 0.3438(3) -0.0430(3) 0.103(2) Uani 1 1 d . . . H91A H 1.0545 0.3921 -0.0753 0.155 Uiso 1 1 calc R . . H91B H 0.9845 0.3058 -0.0677 0.155 Uiso 1 1 calc R . . H91C H 1.1507 0.3160 -0.0355 0.155 Uiso 1 1 calc R . . C92 C 0.6707(7) 0.3401(4) 0.0086(4) 0.0949(19) Uani 1 1 d . . . H92A H 0.6490 0.2868 0.0297 0.142 Uiso 1 1 calc R . . H92B H 0.7108 0.3329 -0.0449 0.142 Uiso 1 1 calc R . . H92C H 0.5734 0.3785 0.0123 0.142 Uiso 1 1 calc R . . C93 C 0.5947(6) 0.4554(3) 0.1561(4) 0.0935(19) Uani 1 1 d . . . H93A H 0.6025 0.4732 0.2086 0.140 Uiso 1 1 calc R . . H93B H 0.5276 0.4109 0.1561 0.140 Uiso 1 1 calc R . . H93C H 0.5484 0.5019 0.1269 0.140 Uiso 1 1 calc R . . C94 C 0.9063(7) 0.5109(2) 0.2061(3) 0.0777(15) Uani 1 1 d . . . H94A H 0.8553 0.5650 0.1919 0.117 Uiso 1 1 calc R . . H94B H 1.0167 0.5149 0.2148 0.117 Uiso 1 1 calc R . . H94C H 0.8514 0.4925 0.2528 0.117 Uiso 1 1 calc R . . C95 C 1.1939(5) 0.4379(3) 0.0841(4) 0.0879(18) Uani 1 1 d . . . H95A H 1.2101 0.4724 0.0393 0.132 Uiso 1 1 calc R . . H95B H 1.2672 0.3870 0.0788 0.132 Uiso 1 1 calc R . . H95C H 1.2134 0.4678 0.1299 0.132 Uiso 1 1 calc R . . C01 C 1.0206(5) 0.3356(2) 0.26481(19) 0.0446(8) Uani 1 1 d . . . C02 C 0.9190(7) 0.3490(3) 0.3322(2) 0.0660(13) Uani 1 1 d . . . H02A H 0.8166 0.3320 0.3342 0.079 Uiso 1 1 calc R . . C03 C 0.9695(9) 0.3881(3) 0.3979(3) 0.092(2) Uani 1 1 d . . . H03A H 0.9011 0.3968 0.4430 0.110 Uiso 1 1 calc R . . C04 C 1.1216(11) 0.4129(3) 0.3940(4) 0.106(3) Uani 1 1 d . . . H04A H 1.1544 0.4402 0.4364 0.127 Uiso 1 1 calc R . . C05 C 1.2220(8) 0.3987(3) 0.3307(3) 0.0862(18) Uani 1 1 d . . . H05A H 1.3251 0.4147 0.3293 0.103 Uiso 1 1 calc R . . C06 C 1.1726(6) 0.3601(2) 0.2677(3) 0.0596(11) Uani 1 1 d . . . H06A H 1.2454 0.3498 0.2243 0.072 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 0.02582(15) 0.02734(15) 0.02561(15) -0.00664(11) 0.00122(10) -0.00266(11) Zr2 0.02333(15) 0.02839(15) 0.02899(16) -0.00243(11) 0.00313(10) -0.00550(11) Cl1 0.0363(5) 0.0683(6) 0.0637(6) -0.0216(5) 0.0201(4) -0.0173(4) Cl2 0.0363(5) 0.0613(6) 0.0861(7) -0.0067(5) 0.0253(5) -0.0149(4) C11 0.030(2) 0.138(5) 0.108(4) -0.107(4) -0.015(2) 0.017(2) C12 0.221(8) 0.0216(18) 0.058(3) -0.0124(18) -0.086(4) 0.018(3) C13 0.109(4) 0.071(3) 0.043(2) -0.026(2) 0.014(2) -0.057(3) C14 0.056(2) 0.056(2) 0.064(3) -0.038(2) -0.018(2) 0.0063(19) C15 0.101(4) 0.059(2) 0.0276(18) -0.0088(16) -0.0026(19) -0.038(2) C21 0.0430(18) 0.0268(15) 0.0359(16) -0.0042(12) -0.0003(13) 0.0002(13) C22 0.0398(17) 0.0318(15) 0.0356(16) -0.0115(13) -0.0078(13) 0.0044(13) C23 0.0261(14) 0.0359(16) 0.0357(16) -0.0128(13) 0.0033(12) -0.0027(12) C24 0.0298(15) 0.0339(15) 0.0299(15) -0.0114(12) -0.0006(11) 0.0016(12) C25 0.0282(15) 0.0300(15) 0.0382(16) -0.0135(12) -0.0006(12) -0.0032(12) C31 0.036(3) 0.52(2) 0.51(2) -0.484(19) -0.036(6) 0.045(6) C32 0.81(3) 0.035(3) 0.171(8) -0.036(4) -0.313(14) 0.075(8) C33 0.311(13) 0.321(13) 0.112(6) -0.123(7) 0.104(7) -0.281(12) C34 0.139(6) 0.191(8) 0.227(9) -0.166(8) -0.123(6) 0.095(6) C35 0.426(17) 0.196(9) 0.035(3) 0.005(4) -0.002(5) -0.215(11) C41 0.077(3) 0.040(2) 0.069(3) 0.0111(19) 0.003(2) -0.007(2) C42 0.064(3) 0.057(2) 0.065(3) -0.022(2) -0.033(2) 0.021(2) C43 0.0360(19) 0.060(2) 0.067(3) -0.015(2) 0.0091(17) -0.0157(17) C44 0.063(2) 0.053(2) 0.0301(17) -0.0122(15) -0.0043(15) 0.0051(18) C45 0.0356(18) 0.052(2) 0.069(3) -0.0269(19) -0.0057(16) -0.0081(16) C51 0.0437(18) 0.0332(16) 0.0374(17) -0.0115(13) -0.0113(14) 0.0037(14) C52 0.064(2) 0.0377(18) 0.048(2) 0.0002(16) -0.0152(17) -0.0074(17) C53 0.107(4) 0.039(2) 0.058(3) 0.0082(18) -0.030(2) -0.016(2) C54 0.108(4) 0.045(2) 0.067(3) 0.005(2) -0.050(3) 0.007(2) C55 0.070(3) 0.061(3) 0.079(3) -0.016(2) -0.043(3) 0.017(2) C56 0.047(2) 0.047(2) 0.054(2) -0.0133(17) -0.0161(17) 0.0094(16) C61 0.0339(16) 0.0305(15) 0.0462(19) 0.0031(13) 0.0017(13) 0.0049(13) C62 0.051(2) 0.0292(16) 0.0446(19) 0.0031(14) -0.0074(15) -0.0008(14) C63 0.064(2) 0.0294(16) 0.052(2) 0.0057(15) 0.0132(18) -0.0034(16) C64 0.0350(19) 0.0260(16) 0.104(3) -0.0122(19) -0.0091(19) -0.0064(14) C65 0.049(2) 0.0338(16) 0.0413(18) -0.0082(14) -0.0087(15) 0.0085(15) C71 0.084(3) 0.0361(17) 0.0255(16) 0.0106(13) 0.0125(16) 0.0171(18) C72 0.053(2) 0.048(2) 0.052(2) 0.0111(17) -0.0278(17) -0.0073(17) C73 0.0388(19) 0.0404(19) 0.064(2) 0.0055(17) 0.0023(16) 0.0105(15) C74 0.064(2) 0.0281(16) 0.0378(18) 0.0021(13) -0.0025(16) -0.0033(15) C75 0.0325(17) 0.0425(18) 0.052(2) 0.0232(15) -0.0051(14) -0.0095(14) C81 0.044(2) 0.057(2) 0.089(3) 0.012(2) 0.019(2) 0.0056(19) C82 0.073(3) 0.056(2) 0.072(3) 0.006(2) -0.034(2) 0.008(2) C83 0.109(4) 0.062(3) 0.081(3) 0.026(3) 0.040(3) -0.010(3) C84 0.053(3) 0.060(3) 0.202(7) -0.046(4) -0.011(3) -0.018(2) C85 0.133(5) 0.059(3) 0.056(3) -0.023(2) -0.035(3) 0.028(3) C91 0.180(6) 0.064(3) 0.045(2) 0.014(2) 0.045(3) 0.036(3) C92 0.105(4) 0.084(4) 0.108(4) 0.005(3) -0.071(4) -0.020(3) C93 0.051(3) 0.085(4) 0.132(5) 0.015(3) 0.021(3) 0.026(3) C94 0.145(5) 0.035(2) 0.054(3) -0.0066(18) -0.017(3) -0.005(3) C95 0.044(2) 0.085(3) 0.140(5) 0.062(3) -0.013(3) -0.023(2) C01 0.067(2) 0.0328(17) 0.0342(17) 0.0052(13) -0.0084(16) -0.0049(16) C02 0.113(4) 0.047(2) 0.035(2) -0.0003(17) 0.000(2) -0.002(2) C03 0.185(7) 0.049(3) 0.037(2) 0.0044(19) -0.008(3) 0.006(3) C04 0.209(8) 0.045(3) 0.074(4) 0.011(3) -0.083(5) -0.012(4) C05 0.132(5) 0.057(3) 0.082(4) 0.012(3) -0.072(4) -0.020(3) C06 0.081(3) 0.043(2) 0.063(3) 0.0102(18) -0.039(2) -0.016(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 C51 2.289(3) . ? Zr1 Cl1 2.4505(9) . ? Zr1 C11 2.514(3) . ? Zr1 C15 2.523(3) . ? Zr1 C21 2.542(3) . ? Zr1 C13 2.547(4) . ? Zr1 C23 2.547(3) . ? Zr1 C22 2.549(3) . ? Zr1 C12 2.549(4) . ? Zr1 C25 2.557(3) . ? Zr1 C14 2.557(4) . ? Zr1 C24 2.578(3) . ? Zr2 C01 2.288(4) . ? Zr2 Cl2 2.4440(8) . ? Zr2 C72 2.509(3) . ? Zr2 C71 2.538(3) . ? Zr2 C65 2.543(3) . ? Zr2 C64 2.547(3) . ? Zr2 C63 2.551(3) . ? Zr2 C61 2.552(3) . ? Zr2 C73 2.553(3) . ? Zr2 C75 2.565(3) . ? Zr2 C62 2.579(3) . ? Zr2 C74 2.589(3) . ? C11 C15 1.394(8) . ? C11 C12 1.447(9) . ? C11 C31 1.487(6) . ? C12 C13 1.351(8) . ? C12 C32 1.491(7) . ? C13 C14 1.299(7) . ? C13 C33 1.534(8) . ? C14 C15 1.356(6) . ? C14 C34 1.529(7) . ? C15 C35 1.486(7) . ? C21 C22 1.407(5) . ? C21 C25 1.421(4) . ? C21 C41 1.505(5) . ? C22 C23 1.412(5) . ? C22 C42 1.504(5) . ? C23 C24 1.422(4) . ? C23 C43 1.502(4) . ? C24 C25 1.417(4) . ? C24 C44 1.493(5) . ? C25 C45 1.494(4) . ? C51 C52 1.402(5) . ? C51 C56 1.410(5) . ? C52 C53 1.393(5) . ? C53 C54 1.387(7) . ? C54 C55 1.353(7) . ? C55 C56 1.397(6) . ? C61 C62 1.390(5) . ? C61 C65 1.393(5) . ? C61 C81 1.525(5) . ? C62 C63 1.393(5) . ? C62 C82 1.510(5) . ? C63 C64 1.420(6) . ? C63 C83 1.502(5) . ? C64 C65 1.433(6) . ? C64 C84 1.500(6) . ? C65 C85 1.523(5) . ? C71 C75 1.423(5) . ? C71 C72 1.427(6) . ? C71 C91 1.499(5) . ? C72 C73 1.392(5) . ? C72 C92 1.514(6) . ? C73 C74 1.369(5) . ? C73 C93 1.532(5) . ? C74 C75 1.385(5) . ? C74 C94 1.512(5) . ? C75 C95 1.512(5) . ? C01 C06 1.398(6) . ? C01 C02 1.402(5) . ? C02 C03 1.429(7) . ? C03 C04 1.393(9) . ? C04 C05 1.342(9) . ? C05 C06 1.384(6) . ? 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 C51 Zr1 Cl1 98.16(9) . . ? C51 Zr1 C11 96.09(19) . . ? Cl1 Zr1 C11 79.52(13) . . ? C51 Zr1 C15 126.83(13) . . ? Cl1 Zr1 C15 85.52(11) . . ? C11 Zr1 C15 32.14(18) . . ? C51 Zr1 C21 123.80(10) . . ? Cl1 Zr1 C21 82.23(8) . . ? C11 Zr1 C21 138.1(2) . . ? C15 Zr1 C21 109.30(13) . . ? C51 Zr1 C13 93.57(16) . . ? Cl1 Zr1 C13 131.63(10) . . ? C11 Zr1 C13 52.56(15) . . ? C15 Zr1 C13 51.19(13) . . ? C21 Zr1 C13 127.56(17) . . ? C51 Zr1 C23 92.57(11) . . ? Cl1 Zr1 C23 131.57(7) . . ? C11 Zr1 C23 146.04(12) . . ? C15 Zr1 C23 123.81(14) . . ? C21 Zr1 C23 53.43(10) . . ? C13 Zr1 C23 94.23(14) . . ? C51 Zr1 C22 123.94(11) . . ? Cl1 Zr1 C22 113.04(8) . . ? C11 Zr1 C22 133.40(15) . . ? C15 Zr1 C22 101.90(14) . . ? C21 Zr1 C22 32.09(10) . . ? C13 Zr1 C22 97.96(17) . . ? C23 Zr1 C22 32.17(10) . . ? C51 Zr1 C12 76.47(12) . . ? Cl1 Zr1 C12 108.5(2) . . ? C11 Zr1 C12 33.2(2) . . ? C15 Zr1 C12 52.76(14) . . ? C21 Zr1 C12 156.41(15) . . ? C13 Zr1 C12 30.73(19) . . ? C23 Zr1 C12 119.9(2) . . ? C22 Zr1 C12 128.70(19) . . ? C51 Zr1 C25 92.09(11) . . ? Cl1 Zr1 C25 78.91(7) . . ? C11 Zr1 C25 157.81(17) . . ? C15 Zr1 C25 139.90(12) . . ? C21 Zr1 C25 32.37(10) . . ? C13 Zr1 C25 147.47(14) . . ? C23 Zr1 C25 53.50(9) . . ? C22 Zr1 C25 53.30(10) . . ? C12 Zr1 C25 166.98(15) . . ? C51 Zr1 C14 122.71(14) . . ? Cl1 Zr1 C14 115.93(12) . . ? C11 Zr1 C14 51.78(13) . . ? C15 Zr1 C14 30.96(14) . . ? C21 Zr1 C14 106.13(12) . . ? C13 Zr1 C14 29.50(16) . . ? C23 Zr1 C14 96.36(11) . . ? C22 Zr1 C14 84.35(11) . . ? C12 Zr1 C14 50.37(14) . . ? C25 Zr1 C14 136.73(11) . . ? C51 Zr1 C24 74.13(10) . . ? Cl1 Zr1 C24 107.48(7) . . ? C11 Zr1 C24 168.5(2) . . ? C15 Zr1 C24 154.47(14) . . ? C21 Zr1 C24 53.16(10) . . ? C13 Zr1 C24 120.87(12) . . ? C23 Zr1 C24 32.21(9) . . ? C22 Zr1 C24 53.01(10) . . ? C12 Zr1 C24 135.97(19) . . ? C25 Zr1 C24 32.04(10) . . ? C14 Zr1 C24 128.54(11) . . ? C01 Zr2 Cl2 97.05(10) . . ? C01 Zr2 C72 127.48(12) . . ? Cl2 Zr2 C72 88.34(10) . . ? C01 Zr2 C71 118.02(13) . . ? Cl2 Zr2 C71 121.17(10) . . ? C72 Zr2 C71 32.85(13) . . ? C01 Zr2 C65 127.94(12) . . ? Cl2 Zr2 C65 109.16(9) . . ? C72 Zr2 C65 98.18(12) . . ? C71 Zr2 C65 85.71(11) . . ? C01 Zr2 C64 120.33(14) . . ? Cl2 Zr2 C64 79.83(9) . . ? C72 Zr2 C64 112.07(14) . . ? C71 Zr2 C64 113.53(14) . . ? C65 Zr2 C64 32.71(13) . . ? C01 Zr2 C63 87.98(13) . . ? Cl2 Zr2 C63 83.04(9) . . ? C72 Zr2 C63 144.35(13) . . ? C71 Zr2 C63 138.58(11) . . ? C65 Zr2 C63 53.37(11) . . ? C64 Zr2 C63 32.35(14) . . ? C01 Zr2 C61 98.55(12) . . ? Cl2 Zr2 C61 131.89(8) . . ? C72 Zr2 C61 115.97(12) . . ? C71 Zr2 C61 90.02(11) . . ? C65 Zr2 C61 31.74(11) . . ? C64 Zr2 C61 53.11(11) . . ? C63 Zr2 C61 52.52(11) . . ? C01 Zr2 C73 98.34(13) . . ? Cl2 Zr2 C73 78.12(9) . . ? C72 Zr2 C73 31.92(13) . . ? C71 Zr2 C73 52.78(11) . . ? C65 Zr2 C73 130.09(12) . . ? C64 Zr2 C73 137.36(13) . . ? C63 Zr2 C73 160.71(13) . . ? C61 Zr2 C73 142.76(11) . . ? C01 Zr2 C75 85.67(12) . . ? Cl2 Zr2 C75 129.55(8) . . ? C72 Zr2 C75 53.55(12) . . ? C71 Zr2 C75 32.39(12) . . ? C65 Zr2 C75 108.06(12) . . ? C64 Zr2 C75 140.41(14) . . ? C63 Zr2 C75 147.32(12) . . ? C61 Zr2 C75 96.86(11) . . ? C73 Zr2 C75 51.83(11) . . ? C01 Zr2 C62 76.05(12) . . ? Cl2 Zr2 C62 113.21(8) . . ? C72 Zr2 C62 147.29(12) . . ? C71 Zr2 C62 119.90(11) . . ? C65 Zr2 C62 52.54(11) . . ? C64 Zr2 C62 52.82(12) . . ? C63 Zr2 C62 31.50(12) . . ? C61 Zr2 C62 31.43(10) . . ? C73 Zr2 C62 167.67(12) . . ? C75 Zr2 C62 116.25(11) . . ? C01 Zr2 C74 75.17(12) . . ? Cl2 Zr2 C74 100.98(9) . . ? C72 Zr2 C74 52.64(12) . . ? C71 Zr2 C74 52.60(11) . . ? C65 Zr2 C74 137.41(11) . . ? C64 Zr2 C74 164.41(14) . . ? C63 Zr2 C74 163.00(13) . . ? C61 Zr2 C74 126.98(11) . . ? C73 Zr2 C74 30.87(12) . . ? C75 Zr2 C74 31.17(11) . . ? C62 Zr2 C74 137.38(12) . . ? C15 C11 C12 105.0(4) . . ? C15 C11 C31 128.4(9) . . ? C12 C11 C31 126.2(10) . . ? C15 C11 Zr1 74.3(2) . . ? C12 C11 Zr1 74.8(2) . . ? C31 C11 Zr1 121.6(3) . . ? C13 C12 C11 106.4(4) . . ? C13 C12 C32 129.3(10) . . ? C11 C12 C32 123.4(9) . . ? C13 C12 Zr1 74.6(2) . . ? C11 C12 Zr1 72.1(2) . . ? C32 C12 Zr1 126.6(3) . . ? C14 C13 C12 110.1(5) . . ? C14 C13 C33 124.7(8) . . ? C12 C13 C33 124.2(8) . . ? C14 C13 Zr1 75.6(2) . . ? C12 C13 Zr1 74.7(3) . . ? C33 C13 Zr1 125.6(3) . . ? C13 C14 C15 111.1(4) . . ? C13 C14 C34 124.4(6) . . ? C15 C14 C34 122.8(6) . . ? C13 C14 Zr1 74.9(3) . . ? C15 C14 Zr1 73.2(2) . . ? C34 C14 Zr1 131.2(3) . . ? C14 C15 C11 107.2(4) . . ? C14 C15 C35 126.3(7) . . ? C11 C15 C35 126.1(7) . . ? C14 C15 Zr1 75.9(2) . . ? C11 C15 Zr1 73.6(2) . . ? C35 C15 Zr1 122.2(3) . . ? C22 C21 C25 108.1(3) . . ? C22 C21 C41 125.6(3) . . ? C25 C21 C41 126.0(3) . . ? C22 C21 Zr1 74.20(17) . . ? C25 C21 Zr1 74.37(17) . . ? C41 C21 Zr1 122.0(2) . . ? C21 C22 C23 108.5(3) . . ? C21 C22 C42 123.9(3) . . ? C23 C22 C42 125.7(3) . . ? C21 C22 Zr1 73.71(17) . . ? C23 C22 Zr1 73.87(17) . . ? C42 C22 Zr1 130.9(2) . . ? C22 C23 C24 107.7(3) . . ? C22 C23 C43 125.5(3) . . ? C24 C23 C43 125.8(3) . . ? C22 C23 Zr1 73.96(16) . . ? C24 C23 Zr1 75.08(15) . . ? C43 C23 Zr1 125.8(2) . . ? C25 C24 C23 108.0(3) . . ? C25 C24 C44 124.6(3) . . ? C23 C24 C44 126.3(3) . . ? C25 C24 Zr1 73.14(15) . . ? C23 C24 Zr1 72.71(15) . . ? C44 C24 Zr1 129.2(2) . . ? C24 C25 C21 107.6(3) . . ? C24 C25 C45 124.4(3) . . ? C21 C25 C45 127.7(3) . . ? C24 C25 Zr1 74.82(16) . . ? C21 C25 Zr1 73.26(16) . . ? C45 C25 Zr1 122.5(2) . . ? C52 C51 C56 114.9(3) . . ? C52 C51 Zr1 126.6(3) . . ? C56 C51 Zr1 118.4(3) . . ? C53 C52 C51 123.2(4) . . ? C54 C53 C52 119.4(5) . . ? C55 C54 C53 119.5(4) . . ? C54 C55 C56 121.3(4) . . ? C55 C56 C51 121.8(4) . . ? C62 C61 C65 109.1(3) . . ? C62 C61 C81 123.9(4) . . ? C65 C61 C81 125.7(3) . . ? C62 C61 Zr2 75.38(18) . . ? C65 C61 Zr2 73.79(18) . . ? C81 C61 Zr2 127.3(2) . . ? C61 C62 C63 108.5(3) . . ? C61 C62 C82 125.3(4) . . ? C63 C62 C82 125.0(4) . . ? C61 C62 Zr2 73.19(18) . . ? C63 C62 Zr2 73.1(2) . . ? C82 C62 Zr2 129.7(2) . . ? C62 C63 C64 108.3(3) . . ? C62 C63 C83 124.6(4) . . ? C64 C63 C83 126.8(4) . . ? C62 C63 Zr2 75.37(19) . . ? C64 C63 Zr2 73.7(2) . . ? C83 C63 Zr2 121.9(3) . . ? C63 C64 C65 106.6(3) . . ? C63 C64 C84 127.1(5) . . ? C65 C64 C84 125.8(5) . . ? C63 C64 Zr2 74.0(2) . . ? C65 C64 Zr2 73.51(18) . . ? C84 C64 Zr2 124.1(3) . . ? C61 C65 C64 107.5(3) . . ? C61 C65 C85 127.3(4) . . ? C64 C65 C85 123.4(4) . . ? C61 C65 Zr2 74.47(18) . . ? C64 C65 Zr2 73.79(18) . . ? C85 C65 Zr2 129.4(2) . . ? C75 C71 C72 106.7(3) . . ? C75 C71 C91 125.9(5) . . ? C72 C71 C91 125.7(5) . . ? C75 C71 Zr2 74.86(18) . . ? C72 C71 Zr2 72.48(19) . . ? C91 C71 Zr2 129.9(3) . . ? C73 C72 C71 106.7(3) . . ? C73 C72 C92 125.2(4) . . ? C71 C72 C92 127.8(4) . . ? C73 C72 Zr2 75.8(2) . . ? C71 C72 Zr2 74.67(19) . . ? C92 C72 Zr2 120.0(3) . . ? C74 C73 C72 110.0(3) . . ? C74 C73 C93 124.0(4) . . ? C72 C73 C93 125.7(4) . . ? C74 C73 Zr2 76.0(2) . . ? C72 C73 Zr2 72.3(2) . . ? C93 C73 Zr2 124.2(3) . . ? C73 C74 C75 108.6(3) . . ? C73 C74 C94 124.5(4) . . ? C75 C74 C94 126.4(4) . . ? C73 C74 Zr2 73.1(2) . . ? C75 C74 Zr2 73.44(19) . . ? C94 C74 Zr2 125.7(2) . . ? C74 C75 C71 108.0(3) . . ? C74 C75 C95 128.2(4) . . ? C71 C75 C95 122.7(4) . . ? C74 C75 Zr2 75.39(19) . . ? C71 C75 Zr2 72.75(18) . . ? C95 C75 Zr2 126.6(2) . . ? C06 C01 C02 115.9(4) . . ? C06 C01 Zr2 124.3(3) . . ? C02 C01 Zr2 119.5(3) . . ? C01 C02 C03 120.8(5) . . ? C04 C03 C02 118.9(5) . . ? C05 C04 C03 121.1(5) . . ? C04 C05 C06 119.5(6) . . ? C05 C06 C01 123.7(5) . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 0.855 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.091 data_zrcs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H38 Si Zr' _chemical_formula_weight 493.89 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4751(10) _cell_length_b 13.9980(13) _cell_length_c 16.7840(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.838(2) _cell_angle_gamma 90.00 _cell_volume 2417.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8603 _exptl_absorpt_correction_T_max 0.9501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17852 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5587 _reflns_number_gt 3670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00036(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5587 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.43578(3) 0.52708(2) 0.246867(18) 0.02388(9) Uani 1 1 d . . . C1 C 0.6372(3) 0.5326(2) 0.32624(17) 0.0284(7) Uani 1 1 d . . . C2 C 0.7404(3) 0.4679(2) 0.34152(19) 0.0343(7) Uani 1 1 d . . . H2A H 0.7279 0.4060 0.3196 0.041 Uiso 1 1 calc R . . C3 C 0.8603(3) 0.4910(2) 0.3876(2) 0.0367(8) Uani 1 1 d . . . H3A H 0.9271 0.4452 0.3967 0.044 Uiso 1 1 calc R . . C4 C 0.8814(3) 0.5812(3) 0.41990(19) 0.0369(8) Uani 1 1 d . . . H4A H 0.9631 0.5979 0.4502 0.044 Uiso 1 1 calc R . . C5 C 0.7813(3) 0.6469(2) 0.40741(19) 0.0328(8) Uani 1 1 d . . . H5A H 0.7949 0.7080 0.4305 0.039 Uiso 1 1 calc R . . C6 C 0.6609(3) 0.6239(2) 0.36119(18) 0.0273(7) Uani 1 1 d . . . C7 C 0.5559(3) 0.7001(2) 0.3445(2) 0.0343(8) Uani 1 1 d . . . H7A H 0.5726 0.7409 0.3002 0.041 Uiso 1 1 calc R . . H7B H 0.5614 0.7403 0.3929 0.041 Uiso 1 1 calc R . . C8 C 0.4170(3) 0.6596(2) 0.3219(2) 0.0358(8) Uani 1 1 d . . . H8A H 0.3585 0.7062 0.2902 0.043 Uiso 1 1 calc R . . H8B H 0.3831 0.6431 0.3707 0.043 Uiso 1 1 calc R . . Si Si 0.29648(9) 0.38687(6) 0.09967(5) 0.0290(2) Uani 1 1 d . . . C11 C 0.3968(3) 0.4987(2) 0.09835(18) 0.0265(7) Uani 1 1 d . . . C12 C 0.3497(3) 0.5942(2) 0.10833(18) 0.0290(7) Uani 1 1 d . . . C13 C 0.4570(3) 0.6547(2) 0.13663(19) 0.0329(8) Uani 1 1 d . . . C14 C 0.5714(3) 0.5993(2) 0.14547(19) 0.0328(8) Uani 1 1 d . . . C15 C 0.5358(3) 0.5045(2) 0.12250(18) 0.0296(8) Uani 1 1 d . . . C21 C 0.2960(3) 0.3836(2) 0.21181(18) 0.0264(7) Uani 1 1 d . . . C22 C 0.2228(3) 0.4466(2) 0.25378(19) 0.0282(7) Uani 1 1 d . . . C23 C 0.2840(3) 0.4533(2) 0.33600(18) 0.0289(7) Uani 1 1 d . . . C24 C 0.3952(3) 0.3948(2) 0.34796(19) 0.0291(7) Uani 1 1 d . . . C25 C 0.4036(3) 0.3515(2) 0.27280(19) 0.0267(7) Uani 1 1 d . . . C32 C 0.2139(3) 0.6322(2) 0.0833(2) 0.0401(9) Uani 1 1 d . . . H32A H 0.1904 0.6683 0.1277 0.060 Uiso 1 1 calc R . . H32B H 0.1538 0.5794 0.0695 0.060 Uiso 1 1 calc R . . H32C H 0.2097 0.6736 0.0365 0.060 Uiso 1 1 calc R . . C33 C 0.4477(4) 0.7615(2) 0.1421(2) 0.0477(10) Uani 1 1 d . . . H33A H 0.5323 0.7874 0.1654 0.072 Uiso 1 1 calc R . . H33B H 0.3858 0.7781 0.1761 0.072 Uiso 1 1 calc R . . H33C H 0.4190 0.7878 0.0882 0.072 Uiso 1 1 calc R . . C34 C 0.7082(3) 0.6370(3) 0.1672(2) 0.0455(10) Uani 1 1 d . . . H34A H 0.7396 0.6528 0.1180 0.068 Uiso 1 1 calc R . . H34B H 0.7638 0.5887 0.1972 0.068 Uiso 1 1 calc R . . H34C H 0.7092 0.6938 0.2004 0.068 Uiso 1 1 calc R . . C35 C 0.6338(3) 0.4271(3) 0.1166(2) 0.0427(9) Uani 1 1 d . . . H35A H 0.5909 0.3654 0.1123 0.064 Uiso 1 1 calc R . . H35B H 0.7016 0.4283 0.1647 0.064 Uiso 1 1 calc R . . H35C H 0.6718 0.4378 0.0689 0.064 Uiso 1 1 calc R . . C42 C 0.0910(3) 0.4898(2) 0.2221(2) 0.0396(9) Uani 1 1 d . . . H42A H 0.0265 0.4594 0.2482 0.059 Uiso 1 1 calc R . . H42B H 0.0683 0.4802 0.1640 0.059 Uiso 1 1 calc R . . H42C H 0.0935 0.5577 0.2339 0.059 Uiso 1 1 calc R . . C43 C 0.2290(3) 0.5026(2) 0.4016(2) 0.0410(9) Uani 1 1 d . . . H43A H 0.1701 0.4596 0.4222 0.061 Uiso 1 1 calc R . . H43B H 0.1822 0.5594 0.3796 0.061 Uiso 1 1 calc R . . H43C H 0.2992 0.5205 0.4454 0.061 Uiso 1 1 calc R . . C44 C 0.4806(3) 0.3733(2) 0.42845(19) 0.0404(9) Uani 1 1 d . . . H44A H 0.4906 0.4305 0.4616 0.061 Uiso 1 1 calc R . . H44B H 0.5651 0.3522 0.4199 0.061 Uiso 1 1 calc R . . H44C H 0.4410 0.3234 0.4557 0.061 Uiso 1 1 calc R . . C45 C 0.5024(3) 0.2755(2) 0.2632(2) 0.0391(8) Uani 1 1 d . . . H45A H 0.5650 0.3016 0.2332 0.059 Uiso 1 1 calc R . . H45B H 0.4584 0.2215 0.2339 0.059 Uiso 1 1 calc R . . H45C H 0.5470 0.2548 0.3163 0.059 Uiso 1 1 calc R . . C51 C 0.1303(3) 0.3929(3) 0.0357(2) 0.0429(9) Uani 1 1 d . . . H51A H 0.1370 0.4091 -0.0195 0.064 Uiso 1 1 calc R . . H51B H 0.0797 0.4412 0.0571 0.064 Uiso 1 1 calc R . . H51C H 0.0879 0.3313 0.0363 0.064 Uiso 1 1 calc R . . C52 C 0.3705(4) 0.2801(2) 0.0599(2) 0.0447(9) Uani 1 1 d . . . H52A H 0.4514 0.2642 0.0959 0.067 Uiso 1 1 calc R . . H52B H 0.3876 0.2940 0.0062 0.067 Uiso 1 1 calc R . . H52C H 0.3111 0.2265 0.0567 0.067 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 Zr 0.02272(16) 0.02276(16) 0.02616(16) 0.00112(15) 0.00457(11) -0.00028(15) C1 0.0291(17) 0.0283(17) 0.0285(17) 0.0049(15) 0.0072(13) -0.0008(15) C2 0.0318(19) 0.0335(19) 0.0375(19) -0.0029(16) 0.0061(14) -0.0033(16) C3 0.0266(19) 0.046(2) 0.037(2) 0.0058(16) 0.0046(15) 0.0044(15) C4 0.027(2) 0.051(2) 0.031(2) -0.0013(16) 0.0018(15) -0.0073(16) C5 0.032(2) 0.035(2) 0.0307(19) -0.0008(14) 0.0064(15) -0.0081(15) C6 0.0291(19) 0.0273(18) 0.0272(18) 0.0014(13) 0.0097(14) -0.0024(13) C7 0.038(2) 0.0270(19) 0.038(2) -0.0030(14) 0.0067(16) 0.0013(14) C8 0.031(2) 0.033(2) 0.045(2) 0.0011(16) 0.0117(16) 0.0032(15) Si 0.0305(5) 0.0270(5) 0.0281(5) -0.0011(4) 0.0022(4) 0.0004(4) C11 0.0282(18) 0.0283(18) 0.0229(17) 0.0033(12) 0.0048(13) 0.0006(12) C12 0.0325(19) 0.0276(18) 0.0267(18) 0.0075(13) 0.0049(14) 0.0004(14) C13 0.042(2) 0.0293(19) 0.0282(19) 0.0060(14) 0.0074(15) -0.0023(15) C14 0.036(2) 0.038(2) 0.0251(18) 0.0042(14) 0.0089(15) -0.0070(15) C15 0.0284(18) 0.036(2) 0.0257(18) 0.0014(13) 0.0089(14) 0.0013(13) C21 0.0236(17) 0.0231(17) 0.0316(18) -0.0005(13) 0.0031(14) -0.0040(13) C22 0.0234(17) 0.0274(19) 0.0340(19) 0.0045(13) 0.0061(14) -0.0045(12) C23 0.0310(18) 0.0297(19) 0.0281(18) 0.0005(13) 0.0111(14) -0.0075(13) C24 0.0307(19) 0.0261(18) 0.0295(18) 0.0051(14) 0.0035(14) -0.0088(14) C25 0.0289(18) 0.0200(17) 0.0315(19) 0.0054(13) 0.0063(14) -0.0026(13) C32 0.040(2) 0.035(2) 0.043(2) 0.0069(16) 0.0044(17) 0.0062(16) C33 0.065(3) 0.029(2) 0.046(2) 0.0082(16) 0.005(2) -0.0052(18) C34 0.037(2) 0.058(3) 0.043(2) 0.0033(18) 0.0126(17) -0.0157(18) C35 0.034(2) 0.052(2) 0.046(2) -0.0018(18) 0.0149(17) 0.0095(17) C42 0.031(2) 0.047(2) 0.041(2) 0.0033(16) 0.0060(15) 0.0049(15) C43 0.040(2) 0.049(2) 0.038(2) -0.0056(15) 0.0168(17) -0.0088(16) C44 0.044(2) 0.043(2) 0.031(2) 0.0094(16) -0.0023(16) -0.0043(17) C45 0.040(2) 0.030(2) 0.045(2) 0.0033(15) -0.0011(17) 0.0062(15) C51 0.042(2) 0.047(2) 0.036(2) 0.0000(16) -0.0026(17) -0.0057(17) C52 0.059(3) 0.034(2) 0.041(2) -0.0039(16) 0.0091(19) 0.0041(17) _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 Zr C8 2.271(3) . ? Zr C1 2.275(3) . ? Zr C11 2.481(3) . ? Zr C21 2.490(3) . ? Zr C12 2.513(3) . ? Zr C22 2.521(3) . ? Zr C15 2.526(3) . ? Zr C25 2.530(3) . ? Zr C23 2.594(3) . ? Zr C24 2.600(3) . ? Zr C13 2.611(3) . ? Zr C14 2.617(3) . ? C1 C2 1.397(4) . ? C1 C6 1.409(4) . ? C2 C3 1.383(4) . ? C3 C4 1.375(5) . ? C4 C5 1.380(4) . ? C5 C6 1.389(4) . ? C6 C7 1.520(4) . ? C7 C8 1.541(4) . ? Si C52 1.864(3) . ? Si C51 1.867(3) . ? Si C21 1.884(3) . ? Si C11 1.888(3) . ? C11 C15 1.438(4) . ? C11 C12 1.445(4) . ? C12 C13 1.416(4) . ? C12 C32 1.503(4) . ? C13 C14 1.412(4) . ? C13 C33 1.501(4) . ? C14 C15 1.413(4) . ? C14 C34 1.506(4) . ? C15 C35 1.508(4) . ? C21 C22 1.437(4) . ? C21 C25 1.445(4) . ? C22 C23 1.411(4) . ? C22 C42 1.509(4) . ? C23 C24 1.408(4) . ? C23 C43 1.502(4) . ? C24 C25 1.417(4) . ? C24 C44 1.503(4) . ? C25 C45 1.513(4) . ? 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 C8 Zr C1 79.35(12) . . ? C8 Zr C11 132.25(11) . . ? C1 Zr C11 123.58(10) . . ? C8 Zr C21 132.96(11) . . ? C1 Zr C21 127.23(11) . . ? C11 Zr C21 69.83(10) . . ? C8 Zr C12 98.86(11) . . ? C1 Zr C12 131.40(10) . . ? C11 Zr C12 33.63(10) . . ? C21 Zr C12 89.43(10) . . ? C8 Zr C22 99.77(10) . . ? C1 Zr C22 136.01(10) . . ? C11 Zr C22 89.71(10) . . ? C21 Zr C22 33.33(9) . . ? C12 Zr C22 92.45(10) . . ? C8 Zr C15 130.78(11) . . ? C1 Zr C15 90.29(10) . . ? C11 Zr C15 33.38(10) . . ? C21 Zr C15 91.17(10) . . ? C12 Zr C15 54.16(10) . . ? C22 Zr C15 119.36(10) . . ? C8 Zr C25 132.08(11) . . ? C1 Zr C25 94.07(10) . . ? C11 Zr C25 90.88(10) . . ? C21 Zr C25 33.44(10) . . ? C12 Zr C25 119.09(10) . . ? C22 Zr C25 53.88(10) . . ? C15 Zr C25 96.30(10) . . ? C8 Zr C23 83.06(10) . . ? C1 Zr C23 106.10(10) . . ? C11 Zr C23 120.86(10) . . ? C21 Zr C23 54.42(9) . . ? C12 Zr C23 122.02(10) . . ? C22 Zr C23 31.99(10) . . ? C15 Zr C23 145.23(10) . . ? C25 Zr C23 52.99(9) . . ? C8 Zr C24 100.28(11) . . ? C1 Zr C24 83.64(10) . . ? C11 Zr C24 121.70(10) . . ? C21 Zr C24 54.45(10) . . ? C12 Zr C24 142.74(10) . . ? C22 Zr C24 52.93(10) . . ? C15 Zr C24 126.45(10) . . ? C25 Zr C24 32.03(9) . . ? C23 Zr C24 31.46(9) . . ? C8 Zr C13 82.04(12) . . ? C1 Zr C13 101.47(11) . . ? C11 Zr C13 54.37(10) . . ? C21 Zr C13 120.60(10) . . ? C12 Zr C13 32.02(10) . . ? C22 Zr C13 122.14(10) . . ? C15 Zr C13 52.88(10) . . ? C25 Zr C13 144.93(10) . . ? C23 Zr C13 145.49(10) . . ? C24 Zr C13 174.74(10) . . ? C8 Zr C14 99.15(11) . . ? C1 Zr C14 79.09(10) . . ? C11 Zr C14 54.21(10) . . ? C21 Zr C14 121.67(10) . . ? C12 Zr C14 52.99(10) . . ? C22 Zr C14 142.74(10) . . ? C15 Zr C14 31.84(10) . . ? C25 Zr C14 126.41(10) . . ? C23 Zr C14 174.70(10) . . ? C24 Zr C14 151.05(11) . . ? C13 Zr C14 31.34(10) . . ? C2 C1 C6 116.2(3) . . ? C2 C1 Zr 133.3(2) . . ? C6 C1 Zr 110.3(2) . . ? C3 C2 C1 122.7(3) . . ? C4 C3 C2 119.8(3) . . ? C3 C4 C5 119.4(3) . . ? C4 C5 C6 121.0(3) . . ? C5 C6 C1 120.9(3) . . ? C5 C6 C7 119.4(3) . . ? C1 C6 C7 119.7(3) . . ? C6 C7 C8 113.9(3) . . ? C7 C8 Zr 105.13(19) . . ? C52 Si C51 103.63(17) . . ? C52 Si C21 114.70(15) . . ? C51 Si C21 113.47(15) . . ? C52 Si C11 112.99(15) . . ? C51 Si C11 114.63(15) . . ? C21 Si C11 97.93(13) . . ? C15 C11 C12 105.4(3) . . ? C15 C11 Si 125.4(2) . . ? C12 C11 Si 124.2(2) . . ? C15 C11 Zr 75.01(17) . . ? C12 C11 Zr 74.39(17) . . ? Si C11 Zr 96.18(12) . . ? C13 C12 C11 109.0(3) . . ? C13 C12 C32 122.1(3) . . ? C11 C12 C32 128.4(3) . . ? C13 C12 Zr 77.83(18) . . ? C11 C12 Zr 71.98(17) . . ? C32 C12 Zr 123.2(2) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 C33 127.1(3) . . ? C12 C13 C33 124.0(3) . . ? C14 C13 Zr 74.54(18) . . ? C12 C13 Zr 70.15(17) . . ? C33 C13 Zr 128.5(2) . . ? C13 C14 C15 108.2(3) . . ? C13 C14 C34 125.7(3) . . ? C15 C14 C34 125.8(3) . . ? C13 C14 Zr 74.13(17) . . ? C15 C14 Zr 70.53(17) . . ? C34 C14 Zr 125.9(2) . . ? C14 C15 C11 109.3(3) . . ? C14 C15 C35 123.0(3) . . ? C11 C15 C35 127.4(3) . . ? C14 C15 Zr 77.64(17) . . ? C11 C15 Zr 71.61(16) . . ? C35 C15 Zr 122.5(2) . . ? C22 C21 C25 105.1(3) . . ? C22 C21 Si 125.2(2) . . ? C25 C21 Si 124.6(2) . . ? C22 C21 Zr 74.52(17) . . ? C25 C21 Zr 74.79(16) . . ? Si C21 Zr 96.00(12) . . ? C23 C22 C21 109.5(3) . . ? C23 C22 C42 122.3(3) . . ? C21 C22 C42 127.6(3) . . ? C23 C22 Zr 76.84(17) . . ? C21 C22 Zr 72.15(16) . . ? C42 C22 Zr 124.3(2) . . ? C24 C23 C22 108.2(3) . . ? C24 C23 C43 125.7(3) . . ? C22 C23 C43 125.5(3) . . ? C24 C23 Zr 74.52(16) . . ? C22 C23 Zr 71.17(16) . . ? C43 C23 Zr 126.9(2) . . ? C23 C24 C25 108.1(3) . . ? C23 C24 C44 125.5(3) . . ? C25 C24 C44 126.1(3) . . ? C23 C24 Zr 74.02(17) . . ? C25 C24 Zr 71.25(16) . . ? C44 C24 Zr 125.9(2) . . ? C24 C25 C21 109.1(3) . . ? C24 C25 C45 123.6(3) . . ? C21 C25 C45 126.9(3) . . ? C24 C25 Zr 76.72(17) . . ? C21 C25 Zr 71.78(16) . . ? C45 C25 Zr 123.3(2) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 0.380 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.080 data_zrms10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 N2 Si Zr' _chemical_formula_weight 547.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4411(5) _cell_length_b 10.2964(6) _cell_length_c 14.6641(8) _cell_angle_alpha 83.5780(10) _cell_angle_beta 78.9870(10) _cell_angle_gamma 74.4950(10) _cell_volume 1345.53(13) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9112 _exptl_absorpt_correction_T_max 0.9541 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10239 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.21 _reflns_number_total 5989 _reflns_number_gt 5095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0561P)^2^+1.4446P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5989 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 4.365 _refine_ls_shift/su_mean 0.016 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 Zr Zr 0.74373(3) 0.70364(3) 0.753655(19) 0.03441(11) Uani 1 1 d . . . N1 N 0.7887(4) 0.8667(3) 0.8216(2) 0.0597(8) Uani 1 1 d . . . N2 N 0.9570(4) 0.6843(4) 0.8224(2) 0.0605(8) Uani 1 1 d . . . H2A H 1.0361 0.6184 0.8259 0.073 Uiso 1 1 calc R . . C11 C 0.8303(3) 0.5810(3) 0.6067(2) 0.0353(6) Uani 1 1 d . . . C12 C 0.7262(3) 0.7049(3) 0.5815(2) 0.0389(6) Uani 1 1 d . . . C13 C 0.7871(4) 0.8155(3) 0.5853(2) 0.0422(7) Uani 1 1 d . . . C14 C 0.9285(4) 0.7641(3) 0.6123(2) 0.0424(7) Uani 1 1 d . . . C15 C 0.9562(3) 0.6211(3) 0.6242(2) 0.0387(6) Uani 1 1 d . . . C21 C 0.6938(3) 0.4732(3) 0.7774(2) 0.0352(6) Uani 1 1 d . . . C22 C 0.5498(3) 0.5656(3) 0.8011(2) 0.0414(7) Uani 1 1 d . . . C23 C 0.5463(4) 0.6267(3) 0.8834(2) 0.0447(7) Uani 1 1 d . . . C24 C 0.6847(4) 0.5754(3) 0.9128(2) 0.0437(7) Uani 1 1 d . . . C25 C 0.7749(3) 0.4802(3) 0.8492(2) 0.0383(6) Uani 1 1 d . . . C32 C 0.5904(4) 0.7181(4) 0.5383(3) 0.0534(8) Uani 1 1 d . . . H32A H 0.5146 0.7981 0.5591 0.080 Uiso 1 1 calc R . . H32B H 0.5520 0.6389 0.5569 0.080 Uiso 1 1 calc R . . H32C H 0.6170 0.7259 0.4710 0.080 Uiso 1 1 calc R . . C33 C 0.7216(5) 0.9594(4) 0.5554(3) 0.0607(10) Uani 1 1 d . . . H33A H 0.7609 1.0183 0.5853 0.091 Uiso 1 1 calc R . . H33B H 0.6140 0.9804 0.5731 0.091 Uiso 1 1 calc R . . H33C H 0.7475 0.9727 0.4884 0.091 Uiso 1 1 calc R . . C34 C 1.0353(5) 0.8460(4) 0.6186(3) 0.0606(10) Uani 1 1 d . . . H34A H 1.1081 0.7953 0.6564 0.091 Uiso 1 1 calc R . . H34B H 0.9810 0.9298 0.6469 0.091 Uiso 1 1 calc R . . H34C H 1.0860 0.8660 0.5567 0.091 Uiso 1 1 calc R . . C35 C 1.1038(4) 0.5291(4) 0.6414(3) 0.0509(8) Uani 1 1 d . . . H35A H 1.1683 0.5828 0.6524 0.076 Uiso 1 1 calc R . . H35B H 1.1504 0.4773 0.5874 0.076 Uiso 1 1 calc R . . H35C H 1.0875 0.4680 0.6955 0.076 Uiso 1 1 calc R . . C42 C 0.4144(4) 0.5747(4) 0.7581(3) 0.0560(9) Uani 1 1 d . . . H42A H 0.3887 0.4885 0.7683 0.084 Uiso 1 1 calc R . . H42B H 0.4360 0.5973 0.6917 0.084 Uiso 1 1 calc R . . H42C H 0.3315 0.6441 0.7865 0.084 Uiso 1 1 calc R . . C43 C 0.4148(5) 0.7203(4) 0.9380(3) 0.0656(11) Uani 1 1 d . . . H43A H 0.3354 0.7507 0.9013 0.098 Uiso 1 1 calc R . . H43B H 0.4445 0.7976 0.9528 0.098 Uiso 1 1 calc R . . H43C H 0.3797 0.6728 0.9953 0.098 Uiso 1 1 calc R . . C44 C 0.7236(5) 0.6066(4) 1.0017(2) 0.0623(10) Uani 1 1 d . . . H44A H 0.6682 0.5659 1.0546 0.093 Uiso 1 1 calc R . . H44B H 0.6980 0.7037 1.0062 0.093 Uiso 1 1 calc R . . H44C H 0.8297 0.5704 1.0015 0.093 Uiso 1 1 calc R . . C45 C 0.9248(4) 0.3903(4) 0.8634(3) 0.0526(8) Uani 1 1 d . . . H45A H 1.0012 0.4109 0.8138 0.079 Uiso 1 1 calc R . . H45B H 0.9235 0.2965 0.8626 0.079 Uiso 1 1 calc R . . H45C H 0.9460 0.4056 0.9229 0.079 Uiso 1 1 calc R . . C51 C 0.9424(5) 0.2687(4) 0.6479(3) 0.0601(10) Uani 1 1 d . . . H51A H 0.9104 0.1899 0.6775 0.090 Uiso 1 1 calc R . . H51B H 1.0176 0.2843 0.6791 0.090 Uiso 1 1 calc R . . H51C H 0.9839 0.2538 0.5830 0.090 Uiso 1 1 calc R . . C52 C 0.6462(5) 0.3690(4) 0.5960(3) 0.0582(9) Uani 1 1 d . . . H52A H 0.5590 0.4439 0.5929 0.087 Uiso 1 1 calc R . . H52B H 0.6160 0.2922 0.6306 0.087 Uiso 1 1 calc R . . H52C H 0.6943 0.3448 0.5335 0.087 Uiso 1 1 calc R . . C61 C 0.5440(4) 0.8974(3) 0.7590(2) 0.0467(7) Uani 1 1 d . . . C62 C 0.4089(4) 0.9154(4) 0.7269(3) 0.0606(10) Uani 1 1 d . . . H62A H 0.3921 0.8420 0.7016 0.073 Uiso 1 1 calc R . . C63 C 0.2989(5) 1.0354(5) 0.7305(4) 0.0830(15) Uani 1 1 d . . . H63A H 0.2100 1.0423 0.7083 0.100 Uiso 1 1 calc R . . C64 C 0.3213(6) 1.1446(6) 0.7668(5) 0.104(2) Uani 1 1 d . . . H64A H 0.2467 1.2262 0.7704 0.124 Uiso 1 1 calc R . . C65 C 0.4526(7) 1.1344(5) 0.7979(4) 0.0873(16) Uani 1 1 d . . . H65A H 0.4684 1.2097 0.8214 0.105 Uiso 1 1 calc R . . C66 C 0.5632(4) 1.0122(4) 0.7946(3) 0.0565(9) Uani 1 1 d . . . C71 C 0.7473(8) 1.1029(6) 0.8523(5) 0.106(2) Uani 1 1 d . . . H71A H 0.8426 1.0877 0.8681 0.128 Uiso 1 1 calc R . . H71B H 0.6827 1.1900 0.8540 0.128 Uiso 1 1 calc R . . C72 C 0.7039(6) 1.0007(4) 0.8272(3) 0.0685(11) Uani 1 1 d . . . C81 C 0.9883(6) 0.8620(6) 0.9131(4) 0.0909(16) Uani 1 1 d . . . H81A H 1.0591 0.7912 0.9422 0.136 Uiso 1 1 calc R . . H81B H 0.9122 0.9094 0.9608 0.136 Uiso 1 1 calc R . . H81C H 1.0398 0.9250 0.8760 0.136 Uiso 1 1 calc R . . C82 C 0.9179(5) 0.8018(4) 0.8524(3) 0.0573(9) Uani 1 1 d . . . Si Si 0.77905(10) 0.41947(8) 0.65563(6) 0.03820(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.03769(16) 0.02881(15) 0.03539(16) -0.00395(10) -0.00488(11) -0.00622(10) N1 0.065(2) 0.065(2) 0.0571(19) -0.0104(15) -0.0156(15) -0.0228(16) N2 0.0550(18) 0.065(2) 0.065(2) -0.0041(16) -0.0185(15) -0.0158(15) C11 0.0375(14) 0.0349(14) 0.0328(14) -0.0057(11) -0.0068(11) -0.0056(11) C12 0.0415(15) 0.0386(15) 0.0356(14) -0.0001(12) -0.0114(12) -0.0058(12) C13 0.0515(18) 0.0372(15) 0.0351(15) 0.0015(12) -0.0031(13) -0.0111(13) C14 0.0472(17) 0.0448(17) 0.0370(15) -0.0052(13) 0.0007(13) -0.0190(14) C15 0.0357(14) 0.0435(16) 0.0364(15) -0.0063(12) -0.0042(12) -0.0089(12) C21 0.0383(14) 0.0292(13) 0.0405(15) 0.0004(11) -0.0119(12) -0.0103(11) C22 0.0360(15) 0.0404(16) 0.0487(17) 0.0031(13) -0.0088(13) -0.0128(12) C23 0.0452(17) 0.0426(17) 0.0433(17) -0.0010(13) 0.0012(13) -0.0129(13) C24 0.0556(19) 0.0435(17) 0.0342(15) -0.0002(12) -0.0065(13) -0.0179(14) C25 0.0426(15) 0.0345(14) 0.0398(15) 0.0037(12) -0.0128(12) -0.0116(12) C32 0.0529(19) 0.054(2) 0.055(2) 0.0036(16) -0.0257(16) -0.0067(16) C33 0.081(3) 0.0402(18) 0.054(2) 0.0091(16) -0.0054(19) -0.0122(17) C34 0.064(2) 0.063(2) 0.063(2) -0.0086(18) 0.0028(18) -0.0375(19) C35 0.0348(16) 0.060(2) 0.057(2) -0.0090(16) -0.0087(14) -0.0072(14) C42 0.0373(17) 0.063(2) 0.070(2) 0.0029(18) -0.0154(16) -0.0138(15) C43 0.059(2) 0.064(2) 0.061(2) -0.0105(19) 0.0156(18) -0.0098(19) C44 0.087(3) 0.066(2) 0.0387(18) -0.0050(17) -0.0098(18) -0.028(2) C45 0.054(2) 0.0502(19) 0.054(2) 0.0023(16) -0.0261(16) -0.0055(15) C51 0.072(2) 0.0367(17) 0.064(2) -0.0113(16) -0.0132(19) 0.0050(16) C52 0.071(2) 0.057(2) 0.060(2) -0.0118(17) -0.0233(19) -0.0283(19) C61 0.0461(17) 0.0391(16) 0.0454(17) -0.0010(13) -0.0011(14) 0.0002(13) C62 0.0466(19) 0.055(2) 0.070(2) 0.0019(18) -0.0142(17) 0.0039(16) C63 0.059(3) 0.075(3) 0.098(4) -0.004(3) -0.023(2) 0.018(2) C64 0.086(4) 0.072(3) 0.123(5) -0.013(3) -0.022(3) 0.039(3) C65 0.109(4) 0.051(2) 0.085(3) -0.021(2) -0.009(3) 0.011(2) C66 0.064(2) 0.0455(19) 0.050(2) -0.0067(15) -0.0033(17) -0.0004(16) C71 0.142(5) 0.075(3) 0.116(5) -0.035(3) -0.019(4) -0.041(4) C72 0.094(3) 0.052(2) 0.060(2) -0.0178(18) 0.000(2) -0.023(2) C81 0.104(4) 0.100(4) 0.094(4) -0.015(3) -0.052(3) -0.040(3) C82 0.071(2) 0.060(2) 0.0486(19) -0.0082(17) -0.0068(17) -0.0297(19) Si 0.0443(4) 0.0313(4) 0.0418(4) -0.0060(3) -0.0146(4) -0.0078(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N1 2.216(3) . ? Zr C61 2.348(3) . ? Zr N2 2.372(3) . ? Zr C11 2.508(3) . ? Zr C21 2.514(3) . ? Zr C15 2.519(3) . ? Zr C25 2.533(3) . ? Zr C22 2.557(3) . ? Zr C12 2.560(3) . ? Zr C14 2.577(3) . ? Zr C24 2.589(3) . ? Zr C13 2.611(3) . ? N1 C82 1.359(5) . ? N1 C72 1.400(5) . ? N2 C82 1.269(5) . ? C11 C15 1.432(4) . ? C11 C12 1.447(4) . ? C11 Si 1.883(3) . ? C12 C13 1.417(5) . ? C12 C32 1.504(4) . ? C13 C14 1.412(5) . ? C13 C33 1.496(4) . ? C14 C15 1.422(4) . ? C14 C34 1.498(5) . ? C15 C35 1.509(4) . ? C21 C25 1.432(4) . ? C21 C22 1.441(4) . ? C21 Si 1.891(3) . ? C22 C23 1.413(5) . ? C22 C42 1.507(4) . ? C23 C24 1.402(5) . ? C23 C43 1.505(5) . ? C24 C25 1.418(4) . ? C24 C44 1.510(5) . ? C25 C45 1.508(4) . ? C51 Si 1.869(4) . ? C52 Si 1.865(3) . ? C61 C62 1.402(5) . ? C61 C66 1.411(5) . ? C62 C63 1.384(5) . ? C63 C64 1.377(8) . ? C64 C65 1.376(8) . ? C65 C66 1.403(6) . ? C66 C72 1.467(6) . ? C71 C72 1.337(6) . ? C81 C82 1.480(5) . ? 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 Zr C61 68.66(13) . . ? N1 Zr N2 54.68(12) . . ? C61 Zr N2 123.22(13) . . ? N1 Zr C11 140.06(11) . . ? C61 Zr C11 119.09(11) . . ? N2 Zr C11 107.24(11) . . ? N1 Zr C21 145.26(11) . . ? C61 Zr C21 119.96(11) . . ? N2 Zr C21 105.67(11) . . ? C11 Zr C21 68.89(10) . . ? N1 Zr C15 109.75(11) . . ? C61 Zr C15 130.60(11) . . ? N2 Zr C15 77.09(11) . . ? C11 Zr C15 33.11(9) . . ? C21 Zr C15 89.82(10) . . ? N1 Zr C25 114.15(11) . . ? C61 Zr C25 131.31(11) . . ? N2 Zr C25 75.43(11) . . ? C11 Zr C25 90.18(10) . . ? C21 Zr C25 32.97(9) . . ? C15 Zr C25 95.65(10) . . ? N1 Zr C22 131.76(12) . . ? C61 Zr C22 87.36(11) . . ? N2 Zr C22 126.77(11) . . ? C11 Zr C22 88.11(10) . . ? C21 Zr C22 32.99(10) . . ? C15 Zr C22 117.42(11) . . ? C25 Zr C22 53.33(10) . . ? N1 Zr C12 126.15(11) . . ? C61 Zr C12 86.29(11) . . ? N2 Zr C12 128.87(11) . . ? C11 Zr C12 33.17(9) . . ? C21 Zr C12 88.59(10) . . ? C15 Zr C12 53.65(9) . . ? C25 Zr C12 118.02(10) . . ? C22 Zr C12 91.33(10) . . ? N1 Zr C14 85.81(11) . . ? C61 Zr C14 102.21(11) . . ? N2 Zr C14 78.71(11) . . ? C11 Zr C14 54.46(10) . . ? C21 Zr C14 120.91(10) . . ? C15 Zr C14 32.37(10) . . ? C25 Zr C14 126.32(10) . . ? C22 Zr C14 141.46(10) . . ? C12 Zr C14 52.92(10) . . ? N1 Zr C24 91.55(11) . . ? C61 Zr C24 103.04(11) . . ? N2 Zr C24 76.82(11) . . ? C11 Zr C24 120.88(10) . . ? C21 Zr C24 54.18(10) . . ? C15 Zr C24 126.18(10) . . ? C25 Zr C24 32.11(10) . . ? C22 Zr C24 52.67(10) . . ? C12 Zr C24 141.49(10) . . ? C14 Zr C24 151.67(11) . . ? N1 Zr C13 94.90(12) . . ? C61 Zr C13 77.53(11) . . ? N2 Zr C13 108.63(11) . . ? C11 Zr C13 54.20(10) . . ? C21 Zr C13 119.58(10) . . ? C15 Zr C13 53.11(10) . . ? C25 Zr C13 144.16(10) . . ? C22 Zr C13 120.86(10) . . ? C12 Zr C13 31.79(10) . . ? C14 Zr C13 31.59(10) . . ? C24 Zr C13 173.24(10) . . ? C82 N1 C72 131.4(4) . . ? C82 N1 Zr 101.4(2) . . ? C72 N1 Zr 127.2(3) . . ? C82 N2 Zr 96.8(3) . . ? C15 C11 C12 105.5(3) . . ? C15 C11 Si 124.7(2) . . ? C12 C11 Si 125.1(2) . . ? C15 C11 Zr 73.88(16) . . ? C12 C11 Zr 75.39(16) . . ? Si C11 Zr 96.93(12) . . ? C13 C12 C11 109.1(3) . . ? C13 C12 C32 122.7(3) . . ? C11 C12 C32 127.0(3) . . ? C13 C12 Zr 76.11(18) . . ? C11 C12 Zr 71.45(16) . . ? C32 C12 Zr 128.6(2) . . ? C14 C13 C12 108.0(3) . . ? C14 C13 C33 125.7(3) . . ? C12 C13 C33 125.9(3) . . ? C14 C13 Zr 72.86(17) . . ? C12 C13 Zr 72.10(17) . . ? C33 C13 Zr 126.1(2) . . ? C13 C14 C15 108.1(3) . . ? C13 C14 C34 125.4(3) . . ? C15 C14 C34 126.3(3) . . ? C13 C14 Zr 75.55(17) . . ? C15 C14 Zr 71.58(17) . . ? C34 C14 Zr 122.8(2) . . ? C14 C15 C11 109.3(3) . . ? C14 C15 C35 123.6(3) . . ? C11 C15 C35 126.7(3) . . ? C14 C15 Zr 76.05(17) . . ? C11 C15 Zr 73.01(16) . . ? C35 C15 Zr 122.9(2) . . ? C25 C21 C22 105.3(3) . . ? C25 C21 Si 125.7(2) . . ? C22 C21 Si 124.2(2) . . ? C25 C21 Zr 74.22(16) . . ? C22 C21 Zr 75.14(16) . . ? Si C21 Zr 96.49(12) . . ? C23 C22 C21 109.0(3) . . ? C23 C22 C42 124.3(3) . . ? C21 C22 C42 125.6(3) . . ? C23 C22 Zr 76.25(18) . . ? C21 C22 Zr 71.87(16) . . ? C42 C22 Zr 127.9(2) . . ? C24 C23 C22 108.4(3) . . ? C24 C23 C43 123.9(3) . . ? C22 C23 C43 127.4(3) . . ? C24 C23 Zr 73.50(18) . . ? C22 C23 Zr 72.05(17) . . ? C43 C23 Zr 125.0(2) . . ? C23 C24 C25 107.9(3) . . ? C23 C24 C44 125.4(3) . . ? C25 C24 C44 126.5(3) . . ? C23 C24 Zr 75.22(18) . . ? C25 C24 Zr 71.75(17) . . ? C44 C24 Zr 123.4(2) . . ? C24 C25 C21 109.3(3) . . ? C24 C25 C45 123.9(3) . . ? C21 C25 C45 126.4(3) . . ? C24 C25 Zr 76.14(17) . . ? C21 C25 Zr 72.81(16) . . ? C45 C25 Zr 123.1(2) . . ? C62 C61 C66 115.4(3) . . ? C62 C61 Zr 127.6(3) . . ? C66 C61 Zr 116.9(3) . . ? C63 C62 C61 123.5(4) . . ? C64 C63 C62 119.3(5) . . ? C65 C64 C63 120.0(4) . . ? C64 C65 C66 120.3(5) . . ? C65 C66 C61 121.4(4) . . ? C65 C66 C72 120.7(4) . . ? C61 C66 C72 117.9(3) . . ? C71 C72 N1 125.8(5) . . ? C71 C72 C66 125.5(5) . . ? N1 C72 C66 108.5(3) . . ? N2 C82 N1 106.9(3) . . ? N2 C82 C81 129.5(4) . . ? N1 C82 C81 123.5(4) . . ? N2 C82 Zr 56.7(2) . . ? N1 C82 Zr 50.41(19) . . ? C81 C82 Zr 171.5(3) . . ? C52 Si C51 103.18(19) . . ? C52 Si C11 115.26(16) . . ? C51 Si C11 113.21(17) . . ? C52 Si C21 112.76(16) . . ? C51 Si C21 115.38(16) . . ? C11 Si C21 97.62(13) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.985 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.073 data_zcs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Zr' _chemical_formula_weight 439.77 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2338(5) _cell_length_b 13.7292(7) _cell_length_c 17.2395(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.5760(10) _cell_angle_gamma 90.00 _cell_volume 2333.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8316 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16414 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.26 _reflns_number_total 5335 _reflns_number_gt 4679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0542P)^2^+2.7627P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5335 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.795 _refine_ls_shift/su_mean 0.013 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 Zr Zr 0.80859(2) 0.966945(16) 0.224109(13) 0.02849(10) Uani 1 1 d . . . H1 H 0.934(3) 1.068(2) 0.2429(17) 0.034(7) Uiso 1 1 d . . . C1 C 0.6817(3) 0.9977(3) 0.31067(19) 0.0530(8) Uani 1 1 d . . . C2 C 0.7304(5) 1.0832(4) 0.3477(3) 0.0742(12) Uani 1 1 d . . . H2A H 0.798(5) 1.114(4) 0.340(3) 0.10(2) Uiso 1 1 d . . . C3 C 0.6747(10) 1.1293(5) 0.4036(3) 0.117(3) Uani 1 1 d . . . H3A H 0.727(4) 1.196(3) 0.432(3) 0.071(12) Uiso 1 1 d . . . C4 C 0.5710(11) 1.0892(9) 0.4237(4) 0.151(5) Uani 1 1 d . . . H4A H 0.526(8) 1.113(5) 0.466(5) 0.18(3) Uiso 1 1 d . . . C5 C 0.5174(6) 1.0039(9) 0.3892(4) 0.127(3) Uani 1 1 d . . . H5A H 0.448(6) 0.972(4) 0.398(4) 0.11(2) Uiso 1 1 d . . . C6 C 0.5722(5) 0.9569(5) 0.3328(3) 0.0772(14) Uani 1 1 d . . . H6A H 0.546(5) 0.901(4) 0.312(3) 0.091(19) Uiso 1 1 d . . . C11 C 0.5832(3) 1.0088(5) 0.1269(2) 0.0926(19) Uani 1 1 d . . . C12 C 0.6460(3) 0.9358(2) 0.08821(18) 0.0529(8) Uani 1 1 d . . . C13 C 0.7570(3) 0.9812(3) 0.07285(17) 0.0500(7) Uani 1 1 d . . . C14 C 0.7666(5) 1.0733(3) 0.1000(2) 0.0675(11) Uani 1 1 d . . . C15 C 0.6668(6) 1.0926(3) 0.1325(2) 0.0818(16) Uani 1 1 d . . . C21 C 0.8540(3) 0.7932(2) 0.2713(2) 0.0491(7) Uani 1 1 d . . . C22 C 0.9316(3) 0.8083(2) 0.21610(18) 0.0471(7) Uani 1 1 d . . . C23 C 1.0321(3) 0.8775(2) 0.2497(2) 0.0484(7) Uani 1 1 d . . . C24 C 1.0182(3) 0.9041(2) 0.32567(19) 0.0498(7) Uani 1 1 d . . . C25 C 0.9096(3) 0.8513(2) 0.33995(18) 0.0496(7) Uani 1 1 d . . . C31 C 0.4491(5) 0.9932(10) 0.1438(4) 0.261(8) Uani 1 1 d . . . H31A H 0.4451 1.0309 0.1907 0.392 Uiso 1 1 calc R . . H31B H 0.4380 0.9246 0.1540 0.392 Uiso 1 1 calc R . . H31C H 0.3772 1.0139 0.0977 0.392 Uiso 1 1 calc R . . C32 C 0.5848(7) 0.8387(4) 0.0583(3) 0.158(4) Uani 1 1 d . . . H32A H 0.4922 0.8480 0.0260 0.237 Uiso 1 1 calc R . . H32B H 0.5852 0.7971 0.1038 0.237 Uiso 1 1 calc R . . H32C H 0.6375 0.8084 0.0257 0.237 Uiso 1 1 calc R . . C33 C 0.8439(6) 0.9408(6) 0.0218(3) 0.134(3) Uani 1 1 d . . . H33A H 0.8327 0.9807 -0.0260 0.201 Uiso 1 1 calc R . . H33B H 0.8163 0.8745 0.0060 0.201 Uiso 1 1 calc R . . H33C H 0.9384 0.9414 0.0526 0.201 Uiso 1 1 calc R . . C34 C 0.8685(9) 1.1474(6) 0.0870(4) 0.196(5) Uani 1 1 d . . . H34A H 0.8540 1.1586 0.0297 0.294 Uiso 1 1 calc R . . H34B H 0.9597 1.1230 0.1097 0.294 Uiso 1 1 calc R . . H34C H 0.8569 1.2081 0.1132 0.294 Uiso 1 1 calc R . . C35 C 0.6295(12) 1.1878(5) 0.1663(3) 0.256(7) Uani 1 1 d . . . H35A H 0.7058 1.2104 0.2091 0.385 Uiso 1 1 calc R . . H35B H 0.5519 1.1775 0.1875 0.385 Uiso 1 1 calc R . . H35C H 0.6072 1.2363 0.1239 0.385 Uiso 1 1 calc R . . C41 C 0.7451(5) 0.7174(3) 0.2643(4) 0.0980(18) Uani 1 1 d . . . H41A H 0.7789 0.6655 0.3026 0.147 Uiso 1 1 calc R . . H41B H 0.7202 0.6910 0.2101 0.147 Uiso 1 1 calc R . . H41C H 0.6662 0.7470 0.2757 0.147 Uiso 1 1 calc R . . C42 C 0.9256(6) 0.7449(3) 0.1438(3) 0.0979(18) Uani 1 1 d . . . H42A H 0.9681 0.6827 0.1615 0.147 Uiso 1 1 calc R . . H42B H 0.9733 0.7767 0.1092 0.147 Uiso 1 1 calc R . . H42C H 0.8317 0.7346 0.1143 0.147 Uiso 1 1 calc R . . C43 C 1.1436(4) 0.9110(4) 0.2132(3) 0.0897(16) Uani 1 1 d . . . H43A H 1.1485 0.9816 0.2145 0.135 Uiso 1 1 calc R . . H43B H 1.1239 0.8888 0.1578 0.135 Uiso 1 1 calc R . . H43C H 1.2296 0.8841 0.2438 0.135 Uiso 1 1 calc R . . C44 C 1.1116(6) 0.9693(3) 0.3858(3) 0.099(2) Uani 1 1 d . . . H44A H 1.0584 1.0133 0.4091 0.148 Uiso 1 1 calc R . . H44B H 1.1672 1.0067 0.3590 0.148 Uiso 1 1 calc R . . H44C H 1.1695 0.9300 0.4280 0.148 Uiso 1 1 calc R . . C45 C 0.8725(6) 0.8462(4) 0.4188(3) 0.103(2) Uani 1 1 d . . . H45A H 0.9384 0.8064 0.4566 0.154 Uiso 1 1 calc R . . H45B H 0.7831 0.8174 0.4100 0.154 Uiso 1 1 calc R . . H45C H 0.8721 0.9113 0.4406 0.154 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 Zr 0.02807(14) 0.02745(14) 0.02928(14) 0.00093(8) 0.00655(9) 0.00140(8) C1 0.0478(17) 0.074(2) 0.0390(15) 0.0160(15) 0.0154(13) 0.0245(16) C2 0.081(3) 0.080(3) 0.054(2) 0.012(2) 0.005(2) 0.021(2) C3 0.184(7) 0.104(4) 0.048(3) 0.002(3) 0.004(3) 0.070(5) C4 0.195(9) 0.215(10) 0.053(3) 0.035(4) 0.050(4) 0.153(8) C5 0.072(3) 0.249(9) 0.078(4) 0.085(5) 0.051(3) 0.077(5) C6 0.056(2) 0.120(4) 0.057(2) 0.034(3) 0.0177(18) 0.016(2) C11 0.0282(15) 0.216(6) 0.0337(16) 0.042(3) 0.0080(13) 0.038(2) C12 0.0595(19) 0.0439(15) 0.0401(15) 0.0105(13) -0.0129(14) -0.0168(14) C13 0.0415(15) 0.078(2) 0.0308(13) 0.0080(14) 0.0099(12) 0.0070(14) C14 0.088(3) 0.054(2) 0.0443(18) 0.0164(16) -0.0094(18) -0.022(2) C15 0.121(4) 0.058(2) 0.0431(19) -0.0030(16) -0.018(2) 0.046(3) C21 0.0464(16) 0.0297(13) 0.069(2) 0.0131(13) 0.0121(14) 0.0030(11) C22 0.0553(17) 0.0395(14) 0.0436(15) 0.0011(12) 0.0082(13) 0.0209(13) C23 0.0341(14) 0.0477(16) 0.0640(19) 0.0199(14) 0.0142(13) 0.0136(12) C24 0.0479(16) 0.0361(14) 0.0524(17) 0.0062(13) -0.0095(13) 0.0097(12) C25 0.0646(19) 0.0459(16) 0.0413(15) 0.0169(12) 0.0192(14) 0.0240(14) C31 0.032(2) 0.68(2) 0.076(4) 0.125(8) 0.014(2) 0.045(6) C32 0.209(7) 0.070(3) 0.111(4) 0.033(3) -0.103(4) -0.070(4) C33 0.109(4) 0.252(8) 0.055(3) 0.050(4) 0.044(3) 0.093(5) C34 0.254(9) 0.173(7) 0.098(4) 0.079(4) -0.062(5) -0.161(7) C35 0.480(17) 0.156(6) 0.063(3) -0.027(4) -0.048(6) 0.234(9) C41 0.070(3) 0.047(2) 0.168(5) 0.034(3) 0.015(3) -0.0145(19) C42 0.141(4) 0.077(3) 0.060(2) -0.014(2) 0.001(3) 0.066(3) C43 0.049(2) 0.104(3) 0.127(4) 0.053(3) 0.042(2) 0.024(2) C44 0.101(4) 0.060(2) 0.089(3) 0.000(2) -0.055(3) 0.005(2) C45 0.147(5) 0.116(4) 0.063(2) 0.053(3) 0.060(3) 0.077(4) _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 Zr H1 1.85(3) . ? Zr C1 2.266(3) . ? Zr C15 2.519(3) . ? Zr C12 2.520(3) . ? Zr C21 2.523(3) . ? Zr C13 2.525(3) . ? Zr C11 2.527(3) . ? Zr C23 2.529(3) . ? Zr C24 2.529(3) . ? Zr C14 2.530(3) . ? Zr C22 2.538(3) . ? Zr C25 2.543(3) . ? C1 C2 1.365(6) . ? C1 C6 1.394(6) . ? C2 C3 1.396(8) . ? C3 C4 1.321(13) . ? C4 C5 1.361(13) . ? C5 C6 1.403(9) . ? C11 C15 1.422(7) . ? C11 C12 1.446(7) . ? C11 C31 1.492(6) . ? C12 C13 1.383(5) . ? C12 C32 1.504(5) . ? C13 C14 1.341(5) . ? C13 C33 1.515(5) . ? C14 C15 1.318(7) . ? C14 C34 1.516(6) . ? C15 C35 1.521(6) . ? C21 C22 1.409(5) . ? C21 C25 1.414(5) . ? C21 C41 1.505(5) . ? C22 C23 1.406(5) . ? C22 C42 1.507(5) . ? C23 C24 1.403(5) . ? C23 C43 1.515(5) . ? C24 C25 1.404(5) . ? C24 C44 1.502(5) . ? C25 C45 1.508(4) . ? 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 H1 Zr C1 103.7(9) . . ? H1 Zr C15 81.5(9) . . ? C1 Zr C15 87.10(15) . . ? H1 Zr C12 122.8(9) . . ? C1 Zr C12 106.96(13) . . ? C15 Zr C12 53.70(12) . . ? H1 Zr C21 126.3(9) . . ? C1 Zr C21 93.01(12) . . ? C15 Zr C21 151.02(14) . . ? C12 Zr C21 99.06(11) . . ? H1 Zr C13 93.7(9) . . ? C1 Zr C13 131.89(11) . . ? C15 Zr C13 51.25(13) . . ? C12 Zr C13 31.83(11) . . ? C21 Zr C13 112.06(12) . . ? H1 Zr C11 114.2(9) . . ? C1 Zr C11 79.16(11) . . ? C15 Zr C11 32.73(17) . . ? C12 Zr C11 33.30(15) . . ? C21 Zr C11 119.01(18) . . ? C13 Zr C11 52.90(11) . . ? H1 Zr C23 77.5(9) . . ? C1 Zr C23 128.86(11) . . ? C15 Zr C23 141.63(17) . . ? C12 Zr C23 114.86(12) . . ? C21 Zr C23 53.48(10) . . ? C13 Zr C23 98.42(11) . . ? C11 Zr C23 148.00(14) . . ? H1 Zr C24 73.5(9) . . ? C1 Zr C24 97.90(11) . . ? C15 Zr C24 155.02(16) . . ? C12 Zr C24 144.26(11) . . ? C21 Zr C24 53.55(10) . . ? C13 Zr C24 130.14(11) . . ? C11 Zr C24 172.11(16) . . ? C23 Zr C24 32.22(11) . . ? H1 Zr C14 70.7(9) . . ? C1 Zr C14 116.90(15) . . ? C15 Zr C14 30.27(16) . . ? C12 Zr C14 52.54(10) . . ? C21 Zr C14 142.45(13) . . ? C13 Zr C14 30.77(13) . . ? C11 Zr C14 52.43(14) . . ? C23 Zr C14 111.59(14) . . ? C24 Zr C14 134.60(13) . . ? H1 Zr C22 108.7(9) . . ? C1 Zr C22 125.19(12) . . ? C15 Zr C22 139.85(11) . . ? C12 Zr C22 90.98(11) . . ? C21 Zr C22 32.32(11) . . ? C13 Zr C22 88.84(10) . . ? C11 Zr C22 122.46(17) . . ? C23 Zr C22 32.21(11) . . ? C24 Zr C22 53.41(10) . . ? C14 Zr C22 115.03(14) . . ? H1 Zr C25 102.3(9) . . ? C1 Zr C25 77.48(10) . . ? C15 Zr C25 164.58(15) . . ? C12 Zr C25 130.67(11) . . ? C21 Zr C25 32.41(11) . . ? C13 Zr C25 141.95(11) . . ? C11 Zr C25 140.25(15) . . ? C23 Zr C25 53.27(10) . . ? C24 Zr C25 32.13(11) . . ? C14 Zr C25 164.84(14) . . ? C22 Zr C25 53.41(10) . . ? C2 C1 C6 115.9(4) . . ? C2 C1 Zr 105.4(3) . . ? C6 C1 Zr 138.6(4) . . ? C1 C2 C3 123.1(6) . . ? C4 C3 C2 119.8(7) . . ? C3 C4 C5 120.2(6) . . ? C4 C5 C6 120.6(7) . . ? C1 C6 C5 120.3(7) . . ? C15 C11 C12 105.0(3) . . ? C15 C11 C31 132.1(8) . . ? C12 C11 C31 122.4(7) . . ? C15 C11 Zr 73.33(19) . . ? C12 C11 Zr 73.07(17) . . ? C31 C11 Zr 124.1(3) . . ? C13 C12 C11 105.4(3) . . ? C13 C12 C32 128.5(5) . . ? C11 C12 C32 125.2(5) . . ? C13 C12 Zr 74.32(17) . . ? C11 C12 Zr 73.63(18) . . ? C32 C12 Zr 125.4(2) . . ? C14 C13 C12 110.2(3) . . ? C14 C13 C33 123.2(5) . . ? C12 C13 C33 125.9(5) . . ? C14 C13 Zr 74.80(19) . . ? C12 C13 Zr 73.85(17) . . ? C33 C13 Zr 125.4(2) . . ? C15 C14 C13 110.2(4) . . ? C15 C14 C34 124.7(6) . . ? C13 C14 C34 124.7(6) . . ? C15 C14 Zr 74.4(2) . . ? C13 C14 Zr 74.43(19) . . ? C34 C14 Zr 123.0(3) . . ? C14 C15 C11 109.2(3) . . ? C14 C15 C35 129.7(7) . . ? C11 C15 C35 121.0(7) . . ? C14 C15 Zr 75.3(2) . . ? C11 C15 Zr 73.9(2) . . ? C35 C15 Zr 120.7(3) . . ? C22 C21 C25 108.0(3) . . ? C22 C21 C41 126.0(4) . . ? C25 C21 C41 125.4(4) . . ? C22 C21 Zr 74.42(16) . . ? C25 C21 Zr 74.58(16) . . ? C41 C21 Zr 124.0(2) . . ? C23 C22 C21 107.7(3) . . ? C23 C22 C42 126.4(4) . . ? C21 C22 C42 124.6(4) . . ? C23 C22 Zr 73.52(16) . . ? C21 C22 Zr 73.26(16) . . ? C42 C22 Zr 129.0(2) . . ? C24 C23 C22 108.3(3) . . ? C24 C23 C43 125.8(4) . . ? C22 C23 C43 125.7(4) . . ? C24 C23 Zr 73.90(16) . . ? C22 C23 Zr 74.26(16) . . ? C43 C23 Zr 121.8(2) . . ? C23 C24 C25 108.2(3) . . ? C23 C24 C44 126.5(4) . . ? C25 C24 C44 125.0(4) . . ? C23 C24 Zr 73.89(16) . . ? C25 C24 Zr 74.51(16) . . ? C44 C24 Zr 122.6(2) . . ? C24 C25 C21 107.7(3) . . ? C24 C25 C45 125.8(4) . . ? C21 C25 C45 125.9(4) . . ? C24 C25 Zr 73.36(16) . . ? C21 C25 Zr 73.00(16) . . ? C45 C25 Zr 126.1(2) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.822 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.069 data_phs10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Zr' _chemical_formula_weight 515.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3667(10) _cell_length_b 16.3096(18) _cell_length_c 34.803(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.765(2) _cell_angle_gamma 90.00 _cell_volume 5310.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.431 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9187 _exptl_absorpt_correction_T_max 0.9187 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39000 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12213 _reflns_number_gt 10511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0245P)^2^+9.2855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00003(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12213 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1141 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.202 _refine_ls_shift/su_max 0.034 _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 0.38194(3) 0.703895(17) 0.078147(8) 0.02406(8) Uani 1 1 d . . . C11 C 0.2997(4) 0.5640(2) 0.05322(11) 0.0383(8) Uani 1 1 d . . . C12 C 0.3609(4) 0.6045(2) 0.02194(10) 0.0362(7) Uani 1 1 d . . . C13 C 0.5096(4) 0.6104(2) 0.03037(10) 0.0368(7) Uani 1 1 d . . . C14 C 0.5394(4) 0.5766(2) 0.06683(11) 0.0406(8) Uani 1 1 d . . . C15 C 0.4109(4) 0.5458(2) 0.08064(10) 0.0414(8) Uani 1 1 d . . . C21 C 0.1240(4) 0.7526(2) 0.06196(10) 0.0394(8) Uani 1 1 d . . . C22 C 0.2117(4) 0.8195(2) 0.05251(11) 0.0401(8) Uani 1 1 d . . . C23 C 0.2799(4) 0.8496(2) 0.08674(11) 0.0403(8) Uani 1 1 d . . . C24 C 0.2324(4) 0.8025(2) 0.11777(10) 0.0391(8) Uani 1 1 d . . . C25 C 0.1373(4) 0.7417(2) 0.10244(10) 0.0369(7) Uani 1 1 d . . . C31 C 0.1530(5) 0.5260(3) 0.05350(16) 0.0666(14) Uani 1 1 d . . . H31A H 0.1609 0.4670 0.0508 0.100 Uiso 1 1 calc R . . H31B H 0.0936 0.5478 0.0323 0.100 Uiso 1 1 calc R . . H31C H 0.1100 0.5388 0.0776 0.100 Uiso 1 1 calc R . . C32 C 0.2879(5) 0.6225(3) -0.01657(11) 0.0614(12) Uani 1 1 d . . . H32A H 0.3362 0.5934 -0.0365 0.092 Uiso 1 1 calc R . . H32B H 0.2913 0.6810 -0.0215 0.092 Uiso 1 1 calc R . . H32C H 0.1890 0.6048 -0.0165 0.092 Uiso 1 1 calc R . . C33 C 0.6197(5) 0.6311(3) 0.00173(15) 0.0636(13) Uani 1 1 d . . . H33A H 0.6996 0.6590 0.0148 0.095 Uiso 1 1 calc R . . H33B H 0.5772 0.6665 -0.0181 0.095 Uiso 1 1 calc R . . H33C H 0.6531 0.5810 -0.0099 0.095 Uiso 1 1 calc R . . C34 C 0.6868(5) 0.5678(3) 0.08550(16) 0.0722(16) Uani 1 1 d . . . H34A H 0.7418 0.5296 0.0708 0.108 Uiso 1 1 calc R . . H34B H 0.6797 0.5474 0.1115 0.108 Uiso 1 1 calc R . . H34C H 0.7338 0.6208 0.0862 0.108 Uiso 1 1 calc R . . C35 C 0.3968(7) 0.4880(3) 0.11409(14) 0.0753(16) Uani 1 1 d . . . H35A H 0.3045 0.4960 0.1251 0.113 Uiso 1 1 calc R . . H35B H 0.4721 0.4991 0.1335 0.113 Uiso 1 1 calc R . . H35C H 0.4045 0.4319 0.1052 0.113 Uiso 1 1 calc R . . C41 C 0.0102(4) 0.7157(3) 0.03516(13) 0.0593(12) Uani 1 1 d . . . H41A H -0.0726 0.7515 0.0336 0.089 Uiso 1 1 calc R . . H41B H -0.0171 0.6625 0.0448 0.089 Uiso 1 1 calc R . . H41C H 0.0472 0.7094 0.0098 0.089 Uiso 1 1 calc R . . C42 C 0.2058(5) 0.8611(3) 0.01368(13) 0.0646(13) Uani 1 1 d . . . H42A H 0.2049 0.8199 -0.0064 0.097 Uiso 1 1 calc R . . H42B H 0.2890 0.8960 0.0117 0.097 Uiso 1 1 calc R . . H42C H 0.1198 0.8941 0.0109 0.097 Uiso 1 1 calc R . . C43 C 0.3675(5) 0.9276(2) 0.09070(15) 0.0577(12) Uani 1 1 d . . . H43A H 0.3057 0.9729 0.0970 0.087 Uiso 1 1 calc R . . H43B H 0.4117 0.9390 0.0666 0.087 Uiso 1 1 calc R . . H43C H 0.4412 0.9208 0.1110 0.087 Uiso 1 1 calc R . . C44 C 0.2576(5) 0.8246(3) 0.15940(12) 0.0553(11) Uani 1 1 d . . . H44A H 0.3530 0.8471 0.1635 0.083 Uiso 1 1 calc R . . H44B H 0.2484 0.7760 0.1751 0.083 Uiso 1 1 calc R . . H44C H 0.1878 0.8651 0.1665 0.083 Uiso 1 1 calc R . . C45 C 0.0409(4) 0.6888(3) 0.12534(13) 0.0557(11) Uani 1 1 d . . . H45A H 0.0739 0.6893 0.1522 0.084 Uiso 1 1 calc R . . H45B H 0.0426 0.6330 0.1156 0.084 Uiso 1 1 calc R . . H45C H -0.0560 0.7099 0.1229 0.084 Uiso 1 1 calc R . . C51 C 0.4640(4) 0.6784(2) 0.14101(9) 0.0360(7) Uani 1 1 d . . . C52 C 0.6024(4) 0.6977(2) 0.15505(12) 0.0472(9) Uani 1 1 d . . . H52A H 0.6654 0.7226 0.1383 0.057 Uiso 1 1 calc R . . C53 C 0.6508(5) 0.6816(3) 0.19286(14) 0.0638(13) Uani 1 1 d . . . H53A H 0.7438 0.6972 0.2012 0.077 Uiso 1 1 calc R . . C54 C 0.5647(6) 0.6433(3) 0.21803(12) 0.0651(14) Uani 1 1 d . . . H54A H 0.5978 0.6324 0.2435 0.078 Uiso 1 1 calc R . . C55 C 0.4302(5) 0.6212(3) 0.20550(11) 0.0577(12) Uani 1 1 d . . . H55A H 0.3704 0.5939 0.2223 0.069 Uiso 1 1 calc R . . C56 C 0.3807(4) 0.6388(2) 0.16814(11) 0.0450(9) Uani 1 1 d . . . H56A H 0.2867 0.6235 0.1605 0.054 Uiso 1 1 calc R . . C61 C 0.5470(4) 0.78766(19) 0.05059(10) 0.0366(7) Uani 1 1 d . . . C62 C 0.5404(4) 0.8144(2) 0.01218(12) 0.0461(9) Uani 1 1 d . . . H62A H 0.4678 0.7933 -0.0046 0.055 Uiso 1 1 calc R . . C63 C 0.6358(5) 0.8705(3) -0.00218(13) 0.0550(11) Uani 1 1 d . . . H63A H 0.6254 0.8876 -0.0280 0.066 Uiso 1 1 calc R . . C64 C 0.7453(5) 0.9009(2) 0.02127(14) 0.0567(11) Uani 1 1 d . . . H64A H 0.8114 0.9380 0.0116 0.068 Uiso 1 1 calc R . . C65 C 0.7571(5) 0.8769(3) 0.05858(14) 0.0573(11) Uani 1 1 d . . . H65A H 0.8320 0.8973 0.0748 0.069 Uiso 1 1 calc R . . C66 C 0.6588(5) 0.8219(2) 0.07298(12) 0.0483(9) Uani 1 1 d . . . H66A H 0.6685 0.8073 0.0991 0.058 Uiso 1 1 calc R . . Zr2 Zr 0.93112(3) 0.194847(17) 0.163080(8) 0.02414(8) Uani 1 1 d . . . C111 C 1.0114(3) 0.2266(2) 0.09432(9) 0.0350(7) Uani 1 1 d . . . C112 C 0.9069(4) 0.2854(2) 0.10241(9) 0.0339(7) Uani 1 1 d . . . C113 C 0.7734(3) 0.2442(2) 0.10484(9) 0.0309(7) Uani 1 1 d . . . C114 C 0.7973(3) 0.1597(2) 0.09826(9) 0.0318(7) Uani 1 1 d . . . C115 C 0.9449(4) 0.1487(2) 0.09206(9) 0.0335(7) Uani 1 1 d . . . C121 C 1.1954(4) 0.1779(3) 0.18172(11) 0.0455(9) Uani 1 1 d . . . C122 C 1.1548(5) 0.2582(3) 0.19338(16) 0.0653(15) Uani 1 1 d . . . C123 C 1.0632(5) 0.2463(3) 0.22484(14) 0.0642(15) Uani 1 1 d . . . C124 C 1.0466(4) 0.1624(3) 0.22975(11) 0.0511(10) Uani 1 1 d . . . C125 C 1.1284(4) 0.1225(2) 0.20475(11) 0.0442(9) Uani 1 1 d . . . C131 C 1.1555(4) 0.2460(3) 0.07906(12) 0.0557(11) Uani 1 1 d . . . H13A H 1.1441 0.2606 0.0521 0.084 Uiso 1 1 calc R . . H13B H 1.2170 0.1983 0.0819 0.084 Uiso 1 1 calc R . . H13C H 1.1983 0.2915 0.0934 0.084 Uiso 1 1 calc R . . C132 C 0.9322(4) 0.3764(2) 0.09948(12) 0.0469(9) Uani 1 1 d . . . H13D H 1.0079 0.3925 0.1180 0.070 Uiso 1 1 calc R . . H13E H 0.8452 0.4056 0.1049 0.070 Uiso 1 1 calc R . . H13F H 0.9599 0.3898 0.0737 0.070 Uiso 1 1 calc R . . C133 C 0.6288(4) 0.2826(2) 0.10822(11) 0.0425(8) Uani 1 1 d . . . H13G H 0.5698 0.2709 0.0852 0.064 Uiso 1 1 calc R . . H13H H 0.6392 0.3415 0.1112 0.064 Uiso 1 1 calc R . . H13I H 0.5838 0.2602 0.1305 0.064 Uiso 1 1 calc R . . C134 C 0.6805(4) 0.0971(2) 0.09164(10) 0.0421(8) Uani 1 1 d . . . H13J H 0.6458 0.0989 0.0649 0.063 Uiso 1 1 calc R . . H13K H 0.6026 0.1092 0.1081 0.063 Uiso 1 1 calc R . . H13L H 0.7179 0.0429 0.0976 0.063 Uiso 1 1 calc R . . C135 C 1.0145(5) 0.0712(3) 0.07882(12) 0.0530(10) Uani 1 1 d . . . H13M H 0.9520 0.0250 0.0830 0.080 Uiso 1 1 calc R . . H13N H 1.1046 0.0632 0.0933 0.080 Uiso 1 1 calc R . . H13O H 1.0319 0.0755 0.0516 0.080 Uiso 1 1 calc R . . C141 C 1.3155(5) 0.1581(5) 0.15601(17) 0.111(3) Uani 1 1 d . . . H14A H 1.3953 0.1354 0.1713 0.166 Uiso 1 1 calc R . . H14B H 1.3458 0.2078 0.1434 0.166 Uiso 1 1 calc R . . H14C H 1.2828 0.1185 0.1367 0.166 Uiso 1 1 calc R . . C142 C 1.2192(8) 0.3378(4) 0.1805(3) 0.158(5) Uani 1 1 d . . . H14D H 1.3087 0.3475 0.1949 0.236 Uiso 1 1 calc R . . H14E H 1.1536 0.3825 0.1849 0.236 Uiso 1 1 calc R . . H14F H 1.2366 0.3346 0.1533 0.236 Uiso 1 1 calc R . . C143 C 1.0161(9) 0.3128(6) 0.2519(2) 0.172(5) Uani 1 1 d . . . H14G H 0.9217 0.2999 0.2605 0.258 Uiso 1 1 calc R . . H14H H 1.0131 0.3650 0.2385 0.258 Uiso 1 1 calc R . . H14I H 1.0832 0.3161 0.2739 0.258 Uiso 1 1 calc R . . C144 C 0.9643(6) 0.1216(5) 0.26112(14) 0.109(3) Uani 1 1 d . . . H14J H 0.9097 0.0759 0.2503 0.163 Uiso 1 1 calc R . . H14K H 0.8998 0.1611 0.2719 0.163 Uiso 1 1 calc R . . H14L H 1.0309 0.1018 0.2812 0.163 Uiso 1 1 calc R . . C145 C 1.1689(6) 0.0320(3) 0.20622(19) 0.092(2) Uani 1 1 d . . . H14M H 1.2532 0.0247 0.2232 0.139 Uiso 1 1 calc R . . H14N H 1.1889 0.0133 0.1806 0.139 Uiso 1 1 calc R . . H14O H 1.0904 0.0005 0.2158 0.139 Uiso 1 1 calc R . . C151 C 0.8276(4) 0.0682(2) 0.17171(10) 0.0363(8) Uani 1 1 d . . . C152 C 0.6909(4) 0.0634(2) 0.18557(11) 0.0430(8) Uani 1 1 d . . . H15A H 0.6453 0.1124 0.1922 0.052 Uiso 1 1 calc R . . C153 C 0.6181(5) -0.0100(3) 0.19008(12) 0.0507(10) Uani 1 1 d . . . H15B H 0.5264 -0.0098 0.1999 0.061 Uiso 1 1 calc R . . C154 C 0.6803(5) -0.0829(2) 0.18023(12) 0.0529(11) Uani 1 1 d . . . H15C H 0.6322 -0.1328 0.1835 0.064 Uiso 1 1 calc R . . C155 C 0.8129(5) -0.0816(2) 0.16560(12) 0.0517(10) Uani 1 1 d . . . H15D H 0.8548 -0.1311 0.1581 0.062 Uiso 1 1 calc R . . C156 C 0.8876(4) -0.0081(2) 0.16154(11) 0.0440(9) Uani 1 1 d . . . H15E H 0.9795 -0.0094 0.1519 0.053 Uiso 1 1 calc R . . C161 C 0.7818(4) 0.2878(2) 0.19100(10) 0.0385(8) Uani 1 1 d . . . C162 C 0.7892(5) 0.3738(2) 0.18412(12) 0.0491(9) Uani 1 1 d . . . H16A H 0.8611 0.3935 0.1686 0.059 Uiso 1 1 calc R . . C163 C 0.6958(5) 0.4299(2) 0.19918(12) 0.0520(10) Uani 1 1 d . . . H16B H 0.7033 0.4858 0.1930 0.062 Uiso 1 1 calc R . . C164 C 0.5928(5) 0.4042(3) 0.22294(12) 0.0530(10) Uani 1 1 d . . . H16C H 0.5289 0.4421 0.2330 0.064 Uiso 1 1 calc R . . C165 C 0.5839(5) 0.3220(3) 0.23195(12) 0.0528(10) Uani 1 1 d . . . H16D H 0.5146 0.3037 0.2486 0.063 Uiso 1 1 calc R . . C166 C 0.6774(4) 0.2664(2) 0.21639(11) 0.0447(9) Uani 1 1 d . . . H16E H 0.6697 0.2110 0.2234 0.054 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 0.02547(14) 0.02247(14) 0.02408(14) -0.00019(11) -0.00036(10) -0.00084(11) C11 0.0417(19) 0.0261(15) 0.048(2) -0.0100(14) 0.0095(15) -0.0109(14) C12 0.0446(19) 0.0302(16) 0.0335(17) -0.0085(14) -0.0004(14) -0.0057(14) C13 0.0382(18) 0.0274(16) 0.0457(19) -0.0112(14) 0.0114(15) -0.0053(13) C14 0.0410(19) 0.0260(16) 0.054(2) -0.0144(15) -0.0062(16) 0.0074(14) C15 0.063(2) 0.0243(16) 0.0371(18) -0.0010(14) 0.0069(17) 0.0014(15) C21 0.0277(17) 0.048(2) 0.0413(19) 0.0017(16) -0.0043(14) 0.0097(15) C22 0.0354(18) 0.0414(19) 0.0434(19) 0.0109(16) 0.0006(14) 0.0130(15) C23 0.0367(19) 0.0271(16) 0.057(2) 0.0022(15) 0.0003(16) 0.0112(14) C24 0.0392(18) 0.0365(18) 0.0415(18) -0.0063(15) 0.0013(14) 0.0125(15) C25 0.0286(17) 0.0417(19) 0.0406(19) 0.0029(15) 0.0038(14) 0.0072(14) C31 0.051(3) 0.047(2) 0.104(4) -0.018(2) 0.024(3) -0.021(2) C32 0.080(3) 0.067(3) 0.035(2) -0.010(2) -0.013(2) 0.000(2) C33 0.067(3) 0.046(2) 0.082(3) -0.021(2) 0.042(3) -0.012(2) C34 0.053(3) 0.061(3) 0.100(4) -0.036(3) -0.026(3) 0.026(2) C35 0.141(5) 0.031(2) 0.055(3) 0.0115(19) 0.016(3) 0.005(3) C41 0.038(2) 0.073(3) 0.065(3) -0.006(2) -0.0168(19) 0.004(2) C42 0.064(3) 0.072(3) 0.057(3) 0.032(2) -0.001(2) 0.020(2) C43 0.062(3) 0.0252(17) 0.088(3) -0.0104(19) 0.017(2) 0.0119(17) C44 0.065(3) 0.053(2) 0.048(2) -0.0154(19) 0.0038(19) 0.019(2) C45 0.039(2) 0.069(3) 0.060(3) 0.007(2) 0.0154(18) 0.000(2) C51 0.0458(19) 0.0313(16) 0.0304(16) -0.0034(13) -0.0035(14) 0.0117(14) C52 0.055(2) 0.0325(18) 0.053(2) 0.0024(17) -0.0091(18) 0.0035(17) C53 0.072(3) 0.045(2) 0.071(3) -0.011(2) -0.036(3) 0.013(2) C54 0.104(4) 0.052(3) 0.037(2) -0.0041(19) -0.021(2) 0.036(3) C55 0.085(3) 0.056(3) 0.0327(19) 0.0074(18) 0.011(2) 0.030(2) C56 0.047(2) 0.051(2) 0.0370(19) 0.0021(16) 0.0015(16) 0.0148(17) C61 0.0441(19) 0.0210(15) 0.0459(19) -0.0036(13) 0.0150(15) -0.0007(13) C62 0.050(2) 0.0385(19) 0.051(2) 0.0019(17) 0.0090(17) -0.0003(17) C63 0.069(3) 0.044(2) 0.053(2) 0.0141(19) 0.020(2) 0.003(2) C64 0.061(3) 0.035(2) 0.077(3) 0.002(2) 0.030(2) -0.0110(18) C65 0.062(3) 0.042(2) 0.069(3) -0.009(2) 0.013(2) -0.0178(19) C66 0.065(3) 0.0355(19) 0.045(2) -0.0026(16) 0.0145(19) -0.0095(18) Zr2 0.02362(14) 0.02381(14) 0.02475(14) 0.00075(11) -0.00126(10) 0.00020(11) C111 0.0288(16) 0.0465(19) 0.0296(16) 0.0091(14) 0.0023(13) -0.0042(14) C112 0.0357(17) 0.0324(16) 0.0331(16) 0.0120(13) -0.0020(13) -0.0039(13) C113 0.0281(16) 0.0378(17) 0.0265(15) 0.0071(13) -0.0037(12) -0.0003(13) C114 0.0341(17) 0.0371(17) 0.0238(15) 0.0034(13) -0.0019(12) -0.0054(13) C115 0.0351(17) 0.0401(18) 0.0252(15) 0.0005(13) 0.0010(13) 0.0009(14) C121 0.0251(16) 0.069(3) 0.0419(19) 0.0034(18) -0.0072(14) 0.0056(16) C122 0.048(2) 0.042(2) 0.100(4) 0.026(2) -0.050(3) -0.0213(19) C123 0.050(3) 0.078(3) 0.061(3) -0.041(2) -0.033(2) 0.028(2) C124 0.039(2) 0.082(3) 0.0314(18) 0.0039(19) -0.0122(15) -0.004(2) C125 0.0392(19) 0.042(2) 0.049(2) 0.0073(17) -0.0191(16) -0.0005(16) C131 0.035(2) 0.081(3) 0.052(2) 0.016(2) 0.0083(17) -0.007(2) C132 0.051(2) 0.039(2) 0.050(2) 0.0163(17) -0.0073(17) -0.0115(17) C133 0.0320(17) 0.050(2) 0.045(2) 0.0054(17) -0.0055(15) 0.0060(15) C134 0.047(2) 0.044(2) 0.0349(18) 0.0041(15) -0.0105(15) -0.0122(16) C135 0.065(3) 0.052(2) 0.043(2) -0.0076(18) 0.0080(19) 0.011(2) C141 0.045(3) 0.219(9) 0.067(3) 0.030(4) 0.003(2) 0.045(4) C142 0.135(6) 0.090(5) 0.233(9) 0.092(5) -0.135(6) -0.082(5) C143 0.142(6) 0.202(9) 0.160(7) -0.151(7) -0.110(6) 0.110(6) C144 0.061(3) 0.223(9) 0.041(3) 0.038(4) -0.008(2) -0.019(4) C145 0.091(4) 0.047(3) 0.133(5) 0.007(3) -0.067(4) 0.008(3) C151 0.0433(19) 0.0304(16) 0.0339(17) 0.0067(13) -0.0131(14) -0.0076(14) C152 0.053(2) 0.0339(18) 0.042(2) -0.0014(15) -0.0037(16) -0.0020(16) C153 0.051(2) 0.050(2) 0.050(2) 0.0055(19) 0.0033(18) -0.0124(19) C154 0.066(3) 0.0340(19) 0.057(2) 0.0086(18) -0.012(2) -0.0163(18) C155 0.071(3) 0.0283(18) 0.054(2) 0.0009(16) -0.017(2) 0.0036(18) C156 0.052(2) 0.0386(19) 0.041(2) 0.0060(16) -0.0063(16) 0.0026(16) C161 0.0422(19) 0.0377(18) 0.0349(17) -0.0076(14) -0.0058(14) 0.0094(15) C162 0.057(2) 0.045(2) 0.047(2) -0.0029(18) 0.0078(18) 0.0031(18) C163 0.070(3) 0.0343(19) 0.051(2) -0.0061(17) -0.001(2) 0.0099(19) C164 0.053(2) 0.048(2) 0.057(2) -0.019(2) -0.0012(19) 0.0136(19) C165 0.053(2) 0.053(2) 0.053(2) -0.0137(19) 0.0134(19) -0.0020(19) C166 0.057(2) 0.0344(18) 0.042(2) -0.0053(15) 0.0026(17) 0.0018(17) _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 C61 2.306(3) . ? Zr1 C51 2.321(3) . ? Zr1 C12 2.541(3) . ? Zr1 C11 2.546(3) . ? Zr1 C25 2.556(3) . ? Zr1 C24 2.577(3) . ? Zr1 C21 2.580(3) . ? Zr1 C23 2.584(3) . ? Zr1 C14 2.588(3) . ? Zr1 C13 2.591(3) . ? Zr1 C15 2.594(3) . ? Zr1 C22 2.599(3) . ? C11 C15 1.410(5) . ? C11 C12 1.417(5) . ? C11 C31 1.508(5) . ? C12 C13 1.413(5) . ? C12 C32 1.504(5) . ? C13 C14 1.399(5) . ? C13 C33 1.506(5) . ? C14 C15 1.410(5) . ? C14 C34 1.504(5) . ? C15 C35 1.508(5) . ? C21 C22 1.414(5) . ? C21 C25 1.420(5) . ? C21 C41 1.507(5) . ? C22 C23 1.413(5) . ? C22 C42 1.511(5) . ? C23 C24 1.414(5) . ? C23 C43 1.517(5) . ? C24 C25 1.419(5) . ? C24 C44 1.501(5) . ? C25 C45 1.506(5) . ? C51 C52 1.399(5) . ? C51 C56 1.410(5) . ? C52 C53 1.396(6) . ? C53 C54 1.370(7) . ? C54 C55 1.362(7) . ? C55 C56 1.389(5) . ? C61 C66 1.392(5) . ? C61 C62 1.405(5) . ? C62 C63 1.389(5) . ? C63 C64 1.372(7) . ? C64 C65 1.356(6) . ? C65 C66 1.395(5) . ? Zr2 C151 2.307(3) . ? Zr2 C161 2.309(3) . ? Zr2 C122 2.521(4) . ? Zr2 C121 2.543(3) . ? Zr2 C124 2.567(4) . ? Zr2 C123 2.569(4) . ? Zr2 C112 2.578(3) . ? Zr2 C113 2.579(3) . ? Zr2 C125 2.579(3) . ? Zr2 C114 2.592(3) . ? Zr2 C115 2.593(3) . ? Zr2 C111 2.595(3) . ? C111 C112 1.408(5) . ? C111 C115 1.416(5) . ? C111 C131 1.508(5) . ? C112 C113 1.425(4) . ? C112 C132 1.508(5) . ? C113 C114 1.418(5) . ? C113 C133 1.502(5) . ? C114 C115 1.420(5) . ? C114 C134 1.505(5) . ? C115 C135 1.505(5) . ? C121 C125 1.378(6) . ? C121 C122 1.429(6) . ? C121 C141 1.506(6) . ? C122 C123 1.437(7) . ? C122 C142 1.508(6) . ? C123 C124 1.388(7) . ? C123 C143 1.515(7) . ? C124 C125 1.354(6) . ? C124 C144 1.520(6) . ? C125 C145 1.523(6) . ? C151 C152 1.393(5) . ? C151 C156 1.418(5) . ? C152 C153 1.390(5) . ? C153 C154 1.374(6) . ? C154 C155 1.365(6) . ? C155 C156 1.398(5) . ? C161 C166 1.394(5) . ? C161 C162 1.425(5) . ? C162 C163 1.385(5) . ? C163 C164 1.366(6) . ? C164 C165 1.381(6) . ? C165 C166 1.388(5) . ? 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 C61 Zr1 C51 107.46(13) . . ? C61 Zr1 C12 94.96(12) . . ? C51 Zr1 C12 128.38(11) . . ? C61 Zr1 C11 125.93(11) . . ? C51 Zr1 C11 103.98(12) . . ? C12 Zr1 C11 32.35(11) . . ? C61 Zr1 C25 128.61(11) . . ? C51 Zr1 C25 89.59(12) . . ? C12 Zr1 C25 111.80(12) . . ? C11 Zr1 C25 93.88(12) . . ? C61 Zr1 C24 104.20(12) . . ? C51 Zr1 C24 76.79(11) . . ? C12 Zr1 C24 141.86(11) . . ? C11 Zr1 C24 125.33(12) . . ? C25 Zr1 C24 32.11(11) . . ? C61 Zr1 C21 111.49(12) . . ? C51 Zr1 C21 121.68(12) . . ? C12 Zr1 C21 89.50(12) . . ? C11 Zr1 C21 86.36(12) . . ? C25 Zr1 C21 32.09(11) . . ? C24 Zr1 C21 52.91(11) . . ? C61 Zr1 C23 76.25(12) . . ? C51 Zr1 C23 99.40(12) . . ? C12 Zr1 C23 131.34(12) . . ? C11 Zr1 C23 139.08(12) . . ? C25 Zr1 C23 52.93(12) . . ? C24 Zr1 C23 31.81(12) . . ? C21 Zr1 C23 52.74(12) . . ? C61 Zr1 C14 90.78(12) . . ? C51 Zr1 C14 80.47(12) . . ? C12 Zr1 C14 52.73(11) . . ? C11 Zr1 C14 52.76(11) . . ? C25 Zr1 C14 140.41(12) . . ? C24 Zr1 C14 155.64(12) . . ? C21 Zr1 C14 138.45(12) . . ? C23 Zr1 C14 166.43(12) . . ? C61 Zr1 C13 75.07(11) . . ? C51 Zr1 C13 110.93(12) . . ? C12 Zr1 C13 31.94(11) . . ? C11 Zr1 C13 52.81(11) . . ? C25 Zr1 C13 143.45(11) . . ? C24 Zr1 C13 172.19(12) . . ? C21 Zr1 C13 119.83(12) . . ? C23 Zr1 C13 143.16(12) . . ? C14 Zr1 C13 31.35(12) . . ? C61 Zr1 C15 122.12(12) . . ? C51 Zr1 C15 76.17(11) . . ? C12 Zr1 C15 52.80(11) . . ? C11 Zr1 C15 31.83(12) . . ? C25 Zr1 C15 108.84(12) . . ? C24 Zr1 C15 131.42(12) . . ? C21 Zr1 C15 114.12(13) . . ? C23 Zr1 C15 161.63(12) . . ? C14 Zr1 C15 31.58(12) . . ? C13 Zr1 C15 52.09(11) . . ? C61 Zr1 C22 80.80(12) . . ? C51 Zr1 C22 128.56(12) . . ? C12 Zr1 C22 100.09(12) . . ? C11 Zr1 C22 111.23(13) . . ? C25 Zr1 C22 52.66(11) . . ? C24 Zr1 C22 52.43(11) . . ? C21 Zr1 C22 31.69(12) . . ? C23 Zr1 C22 31.63(12) . . ? C14 Zr1 C22 150.97(12) . . ? C13 Zr1 C22 120.08(12) . . ? C15 Zr1 C22 142.55(13) . . ? C15 C11 C12 107.8(3) . . ? C15 C11 C31 123.5(4) . . ? C12 C11 C31 126.8(4) . . ? C15 C11 Zr1 75.96(19) . . ? C12 C11 Zr1 73.61(18) . . ? C31 C11 Zr1 128.8(3) . . ? C13 C12 C11 107.7(3) . . ? C13 C12 C32 125.0(4) . . ? C11 C12 C32 126.3(4) . . ? C13 C12 Zr1 75.97(19) . . ? C11 C12 Zr1 74.04(19) . . ? C32 C12 Zr1 125.2(3) . . ? C14 C13 C12 108.2(3) . . ? C14 C13 C33 125.1(4) . . ? C12 C13 C33 125.3(4) . . ? C14 C13 Zr1 74.22(19) . . ? C12 C13 Zr1 72.09(19) . . ? C33 C13 Zr1 130.1(2) . . ? C13 C14 C15 108.3(3) . . ? C13 C14 C34 124.6(4) . . ? C15 C14 C34 126.8(4) . . ? C13 C14 Zr1 74.43(19) . . ? C15 C14 Zr1 74.45(19) . . ? C34 C14 Zr1 121.9(2) . . ? C14 C15 C11 108.0(3) . . ? C14 C15 C35 126.4(4) . . ? C11 C15 C35 124.4(4) . . ? C14 C15 Zr1 73.97(19) . . ? C11 C15 Zr1 72.21(19) . . ? C35 C15 Zr1 129.3(3) . . ? C22 C21 C25 107.6(3) . . ? C22 C21 C41 124.4(4) . . ? C25 C21 C41 126.2(4) . . ? C22 C21 Zr1 74.92(19) . . ? C25 C21 Zr1 73.02(18) . . ? C41 C21 Zr1 129.7(3) . . ? C23 C22 C21 108.5(3) . . ? C23 C22 C42 126.4(4) . . ? C21 C22 C42 123.9(4) . . ? C23 C22 Zr1 73.59(18) . . ? C21 C22 Zr1 73.39(19) . . ? C42 C22 Zr1 128.9(3) . . ? C22 C23 C24 108.0(3) . . ? C22 C23 C43 126.1(4) . . ? C24 C23 C43 125.1(4) . . ? C22 C23 Zr1 74.8(2) . . ? C24 C23 Zr1 73.81(19) . . ? C43 C23 Zr1 125.5(2) . . ? C23 C24 C25 107.9(3) . . ? C23 C24 C44 124.5(4) . . ? C25 C24 C44 126.7(4) . . ? C23 C24 Zr1 74.38(19) . . ? C25 C24 Zr1 73.14(19) . . ? C44 C24 Zr1 127.0(2) . . ? C24 C25 C21 108.0(3) . . ? C24 C25 C45 125.7(3) . . ? C21 C25 C45 124.8(3) . . ? C24 C25 Zr1 74.76(19) . . ? C21 C25 Zr1 74.89(19) . . ? C45 C25 Zr1 127.4(3) . . ? C52 C51 C56 113.8(3) . . ? C52 C51 Zr1 123.2(3) . . ? C56 C51 Zr1 123.0(3) . . ? C53 C52 C51 122.7(4) . . ? C54 C53 C52 120.9(4) . . ? C55 C54 C53 118.7(4) . . ? C54 C55 C56 120.5(4) . . ? C55 C56 C51 123.4(4) . . ? C66 C61 C62 113.9(3) . . ? C66 C61 Zr1 120.4(3) . . ? C62 C61 Zr1 125.5(3) . . ? C63 C62 C61 123.2(4) . . ? C64 C63 C62 120.0(4) . . ? C65 C64 C63 119.3(4) . . ? C64 C65 C66 120.3(4) . . ? C61 C66 C65 123.3(4) . . ? C151 Zr2 C161 105.45(14) . . ? C151 Zr2 C122 131.18(12) . . ? C161 Zr2 C122 93.59(16) . . ? C151 Zr2 C121 106.21(13) . . ? C161 Zr2 C121 124.46(13) . . ? C122 Zr2 C121 32.77(15) . . ? C151 Zr2 C124 81.92(13) . . ? C161 Zr2 C124 89.55(13) . . ? C122 Zr2 C124 53.20(14) . . ? C121 Zr2 C124 52.02(13) . . ? C151 Zr2 C123 111.84(16) . . ? C161 Zr2 C123 73.15(12) . . ? C122 Zr2 C123 32.77(17) . . ? C121 Zr2 C123 53.04(13) . . ? C124 Zr2 C123 31.37(16) . . ? C151 Zr2 C112 126.77(11) . . ? C161 Zr2 C112 86.41(12) . . ? C122 Zr2 C112 98.40(13) . . ? C121 Zr2 C112 108.50(12) . . ? C124 Zr2 C112 151.03(13) . . ? C123 Zr2 C112 121.19(16) . . ? C151 Zr2 C113 98.84(11) . . ? C161 Zr2 C113 77.88(11) . . ? C122 Zr2 C113 129.31(12) . . ? C121 Zr2 C113 138.41(11) . . ? C124 Zr2 C113 167.18(13) . . ? C123 Zr2 C113 142.19(14) . . ? C112 Zr2 C113 32.09(10) . . ? C151 Zr2 C125 79.13(12) . . ? C161 Zr2 C125 119.74(13) . . ? C122 Zr2 C125 52.70(12) . . ? C121 Zr2 C125 31.21(13) . . ? C124 Zr2 C125 30.51(13) . . ? C123 Zr2 C125 51.40(13) . . ? C112 Zr2 C125 139.02(12) . . ? C113 Zr2 C125 162.28(12) . . ? C151 Zr2 C114 74.12(11) . . ? C161 Zr2 C114 103.56(11) . . ? C122 Zr2 C114 144.30(15) . . ? C121 Zr2 C114 128.45(12) . . ? C124 Zr2 C114 154.97(13) . . ? C123 Zr2 C114 173.66(15) . . ? C112 Zr2 C114 52.71(10) . . ? C113 Zr2 C114 31.83(10) . . ? C125 Zr2 C114 133.74(12) . . ? C151 Zr2 C115 84.53(12) . . ? C161 Zr2 C115 130.60(11) . . ? C122 Zr2 C115 116.06(16) . . ? C121 Zr2 C115 96.84(12) . . ? C124 Zr2 C115 139.78(13) . . ? C123 Zr2 C115 148.05(14) . . ? C112 Zr2 C115 52.55(11) . . ? C113 Zr2 C115 52.72(11) . . ? C125 Zr2 C115 109.63(12) . . ? C114 Zr2 C115 31.80(10) . . ? C151 Zr2 C111 116.17(12) . . ? C161 Zr2 C111 117.73(12) . . ? C122 Zr2 C111 91.84(15) . . ? C121 Zr2 C111 86.29(11) . . ? C124 Zr2 C111 138.28(12) . . ? C123 Zr2 C111 123.87(16) . . ? C112 Zr2 C111 31.58(11) . . ? C113 Zr2 C111 52.64(10) . . ? C125 Zr2 C111 112.23(12) . . ? C114 Zr2 C111 52.48(10) . . ? C115 Zr2 C111 31.68(11) . . ? C112 C111 C115 108.3(3) . . ? C112 C111 C131 124.8(3) . . ? C115 C111 C131 124.6(4) . . ? C112 C111 Zr2 73.54(18) . . ? C115 C111 Zr2 74.09(18) . . ? C131 C111 Zr2 132.1(2) . . ? C111 C112 C113 108.1(3) . . ? C111 C112 C132 123.0(3) . . ? C113 C112 C132 127.5(3) . . ? C111 C112 Zr2 74.88(18) . . ? C113 C112 Zr2 73.99(17) . . ? C132 C112 Zr2 127.7(2) . . ? C114 C113 C112 107.6(3) . . ? C114 C113 C133 124.6(3) . . ? C112 C113 C133 127.3(3) . . ? C114 C113 Zr2 74.58(18) . . ? C112 C113 Zr2 73.91(17) . . ? C133 C113 Zr2 123.6(2) . . ? C113 C114 C115 108.0(3) . . ? C113 C114 C134 124.4(3) . . ? C115 C114 C134 126.6(3) . . ? C113 C114 Zr2 73.59(18) . . ? C115 C114 Zr2 74.16(18) . . ? C134 C114 Zr2 126.9(2) . . ? C111 C115 C114 107.9(3) . . ? C111 C115 C135 125.1(3) . . ? C114 C115 C135 126.3(3) . . ? C111 C115 Zr2 74.23(19) . . ? C114 C115 Zr2 74.04(18) . . ? C135 C115 Zr2 125.3(2) . . ? C125 C121 C122 107.5(4) . . ? C125 C121 C141 125.4(5) . . ? C122 C121 C141 125.5(5) . . ? C125 C121 Zr2 75.8(2) . . ? C122 C121 Zr2 72.8(2) . . ? C141 C121 Zr2 128.1(3) . . ? C121 C122 C123 105.6(4) . . ? C121 C122 C142 126.1(6) . . ? C123 C122 C142 127.3(6) . . ? C121 C122 Zr2 74.5(2) . . ? C123 C122 Zr2 75.4(2) . . ? C142 C122 Zr2 124.3(3) . . ? C124 C123 C122 107.5(4) . . ? C124 C123 C143 126.3(7) . . ? C122 C123 C143 125.4(7) . . ? C124 C123 Zr2 74.3(2) . . ? C122 C123 Zr2 71.8(2) . . ? C143 C123 Zr2 127.6(3) . . ? C125 C124 C123 109.0(4) . . ? C125 C124 C144 125.0(5) . . ? C123 C124 C144 125.7(5) . . ? C125 C124 Zr2 75.2(2) . . ? C123 C124 Zr2 74.4(2) . . ? C144 C124 Zr2 122.2(3) . . ? C124 C125 C121 110.2(4) . . ? C124 C125 C145 126.3(5) . . ? C121 C125 C145 122.3(5) . . ? C124 C125 Zr2 74.3(2) . . ? C121 C125 Zr2 73.0(2) . . ? C145 C125 Zr2 129.2(3) . . ? C152 C151 C156 114.7(3) . . ? C152 C151 Zr2 119.7(3) . . ? C156 C151 Zr2 125.4(3) . . ? C153 C152 C151 123.5(4) . . ? C154 C153 C152 120.1(4) . . ? C155 C154 C153 118.9(4) . . ? C154 C155 C156 121.3(4) . . ? C155 C156 C151 121.4(4) . . ? C166 C161 C162 113.2(3) . . ? C166 C161 Zr2 124.1(3) . . ? C162 C161 Zr2 122.7(3) . . ? C163 C162 C161 123.3(4) . . ? C164 C163 C162 120.3(4) . . ? C163 C164 C165 119.1(4) . . ? C164 C165 C166 120.0(4) . . ? C165 C166 C161 124.0(4) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.653 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.071