# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'G Erker' 'Roland Frohlich' 'Gerald Kehr' 'Tulay Tumay' _publ_contact_author_name 'Gerhard Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Ring-Closing Metathesis of Sterically Congested Functionalized Zirconocenes - Ethene Polymerization Catalysts Derived from Related Bridged and Open Metallocenes ; # Attachment 'erk5007.cif' data_erk5007 _database_code_depnum_ccdc_archive 'CCDC 735244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Cl2 Zr' _chemical_formula_weight 484.63 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 6.7351(1) _cell_length_b 10.0317(2) _cell_length_c 18.8814(4) _cell_angle_alpha 75.096(1) _cell_angle_beta 87.165(1) _cell_angle_gamma 79.401(2) _cell_volume 1211.76(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2938 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8219 _exptl_absorpt_correction_T_max 0.9048 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11034 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.90 _reflns_number_total 5695 _reflns_number_gt 4716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CollecT (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. Group C6A-C7A-C8A refined split positions using PART command and geometrical restraints (SADI). ; _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^+0.8234P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5695 _refine_ls_number_parameters 260 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.14545(3) 0.43086(3) 0.261943(12) 0.03386(9) Uani 1 1 d . A . Cl1 Cl -0.13956(10) 0.46874(10) 0.34414(4) 0.0623(2) Uani 1 1 d . . . Cl2 Cl -0.06079(11) 0.37751(9) 0.17402(4) 0.0566(2) Uani 1 1 d . . . C1A C 0.1649(4) 0.6526(3) 0.15483(14) 0.0401(6) Uani 1 1 d D A . C2A C 0.0514(4) 0.6964(3) 0.21181(15) 0.0464(6) Uani 1 1 d . A . H2A H -0.0868 0.7358 0.2094 0.056 Uiso 1 1 calc R . . C3A C 0.1768(5) 0.6722(3) 0.27347(15) 0.0509(7) Uani 1 1 d . . . C4A C 0.3660(4) 0.6055(3) 0.25562(16) 0.0487(7) Uani 1 1 d . A . H4A H 0.4798 0.5765 0.2863 0.058 Uiso 1 1 calc R . . C5A C 0.3585(4) 0.5888(3) 0.18390(15) 0.0408(6) Uani 1 1 d . . . H5A H 0.4643 0.5431 0.1596 0.049 Uiso 1 1 calc R A . C6A C 0.138(4) 0.717(5) 0.3428(13) 0.0773(16) Uani 0.351(8) 1 d PD A 1 H6AA H 0.0741 0.8165 0.3305 0.093 Uiso 0.351(8) 1 calc PR A 1 H6AB H 0.0418 0.6639 0.3722 0.093 Uiso 0.351(8) 1 calc PR A 1 C7A C 0.319(3) 0.7010(17) 0.3887(7) 0.090(2) Uani 0.351(8) 1 d PD A 1 H7A H 0.4275 0.7468 0.3707 0.108 Uiso 0.351(8) 1 calc PR A 1 C8A C 0.319(6) 0.622(2) 0.4536(10) 0.137(4) Uani 0.351(8) 1 d PD A 1 H8AA H 0.2086 0.5773 0.4705 0.165 Uiso 0.351(8) 1 calc PR A 1 H8AB H 0.4302 0.6087 0.4845 0.165 Uiso 0.351(8) 1 calc PR A 1 C6C C 0.104(2) 0.725(3) 0.3412(6) 0.0773(16) Uani 0.649(8) 1 d PD A 2 H6CA H 0.1153 0.8239 0.3315 0.093 Uiso 0.649(8) 1 calc PR A 2 H6CB H -0.0386 0.7180 0.3495 0.093 Uiso 0.649(8) 1 calc PR A 2 C7C C 0.2190(13) 0.6464(9) 0.4091(4) 0.090(2) Uani 0.649(8) 1 d PD A 2 H7C H 0.2104 0.5510 0.4267 0.108 Uiso 0.649(8) 1 calc PR A 2 C8C C 0.329(3) 0.6965(15) 0.4460(7) 0.137(4) Uani 0.649(8) 1 d PD A 2 H8CA H 0.3419 0.7913 0.4306 0.165 Uiso 0.649(8) 1 calc PR A 2 H8CB H 0.3956 0.6384 0.4884 0.165 Uiso 0.649(8) 1 calc PR A 2 C9A C 0.1053(5) 0.6927(3) 0.07456(16) 0.0556(8) Uani 1 1 d . . . C10A C -0.1237(6) 0.7245(5) 0.0639(2) 0.0815(12) Uani 1 1 d . A . H10A H -0.1541 0.7515 0.0119 0.122 Uiso 1 1 calc R . . H10B H -0.1820 0.8006 0.0856 0.122 Uiso 1 1 calc R . . H10C H -0.1801 0.6417 0.0873 0.122 Uiso 1 1 calc R . . C11A C 0.1876(7) 0.8318(4) 0.04149(19) 0.0820(12) Uani 1 1 d . A . H11A H 0.3320 0.8157 0.0498 0.123 Uiso 1 1 calc R . . H11B H 0.1208 0.9035 0.0649 0.123 Uiso 1 1 calc R . . H11C H 0.1609 0.8624 -0.0108 0.123 Uiso 1 1 calc R . . C12A C 0.2060(6) 0.5890(4) 0.03285(17) 0.0693(10) Uani 1 1 d . A . H12A H 0.3509 0.5723 0.0400 0.104 Uiso 1 1 calc R . . H12B H 0.1756 0.6264 -0.0189 0.104 Uiso 1 1 calc R . . H12C H 0.1561 0.5015 0.0506 0.104 Uiso 1 1 calc R . . C1B C 0.3672(4) 0.1909(3) 0.26370(15) 0.0441(6) Uani 1 1 d D . . C2B C 0.2143(5) 0.1652(3) 0.31728(17) 0.0514(7) Uani 1 1 d . A . H2B H 0.1110 0.1150 0.3148 0.062 Uiso 1 1 calc R . . C3B C 0.2403(4) 0.2259(3) 0.37436(15) 0.0489(7) Uani 1 1 d . . . C4B C 0.4025(4) 0.2977(3) 0.35474(14) 0.0428(6) Uani 1 1 d . A . H4B H 0.4511 0.3512 0.3820 0.051 Uiso 1 1 calc R . . C5B C 0.4807(4) 0.2762(3) 0.28699(14) 0.0392(6) Uani 1 1 d . A . H5B H 0.5904 0.3128 0.2617 0.047 Uiso 1 1 calc R . . C6B C 0.1275(5) 0.2069(4) 0.44649(17) 0.0693(10) Uani 1 1 d D A . H6BA H 0.1245 0.2892 0.4657 0.083 Uiso 1 1 calc R . . H6BB H -0.0122 0.1991 0.4386 0.083 Uiso 1 1 calc R . . C7B C 0.2256(6) 0.0790(5) 0.5009(2) 0.0915(14) Uani 1 1 d D . . H7B H 0.2514 -0.0045 0.4855 0.110 Uiso 1 1 calc R A . C8B C 0.2778(8) 0.0703(7) 0.5651(2) 0.127(2) Uani 1 1 d D A . H8BA H 0.2556 0.1506 0.5834 0.152 Uiso 1 1 calc R . . H8BB H 0.3390 -0.0165 0.5949 0.152 Uiso 1 1 calc R . . C9B C 0.4248(6) 0.1213(3) 0.20106(18) 0.0612(8) Uani 1 1 d . A . C10B C 0.2594(9) 0.0475(5) 0.1850(3) 0.1031(16) Uani 1 1 d . . . H10D H 0.2223 -0.0153 0.2300 0.155 Uiso 1 1 calc R A . H10E H 0.3088 -0.0059 0.1496 0.155 Uiso 1 1 calc R . . H10F H 0.1420 0.1167 0.1653 0.155 Uiso 1 1 calc R . . C11B C 0.6171(9) 0.0124(5) 0.2254(3) 0.123(2) Uani 1 1 d . . . H11D H 0.5882 -0.0574 0.2689 0.185 Uiso 1 1 calc R A . H11E H 0.7220 0.0586 0.2363 0.185 Uiso 1 1 calc R . . H11F H 0.6625 -0.0329 0.1864 0.185 Uiso 1 1 calc R . . C12B C 0.4723(6) 0.2256(4) 0.13110(19) 0.0694(9) Uani 1 1 d . . . H12D H 0.5181 0.1763 0.0937 0.104 Uiso 1 1 calc R A . H12E H 0.5774 0.2730 0.1407 0.104 Uiso 1 1 calc R . . H12F H 0.3516 0.2940 0.1143 0.104 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 0.02396(12) 0.04420(15) 0.03194(13) -0.00648(10) -0.00020(8) -0.00672(9) Cl1 0.0313(3) 0.0965(6) 0.0521(4) -0.0144(4) 0.0078(3) -0.0024(4) Cl2 0.0477(4) 0.0826(6) 0.0463(4) -0.0142(4) -0.0067(3) -0.0301(4) C1A 0.0422(14) 0.0382(14) 0.0361(13) -0.0040(11) -0.0032(10) -0.0048(11) C2A 0.0456(15) 0.0449(16) 0.0402(15) -0.0058(12) -0.0041(11) 0.0079(12) C3A 0.071(2) 0.0421(15) 0.0382(15) -0.0113(12) -0.0081(13) -0.0043(14) C4A 0.0515(16) 0.0399(15) 0.0533(17) -0.0016(13) -0.0176(13) -0.0146(12) C5A 0.0355(13) 0.0378(14) 0.0464(15) -0.0051(11) 0.0037(11) -0.0081(10) C6A 0.125(5) 0.057(3) 0.049(2) -0.022(2) -0.002(3) -0.001(5) C7A 0.130(7) 0.104(6) 0.047(3) -0.032(4) -0.003(3) -0.031(4) C8A 0.175(7) 0.168(14) 0.094(5) -0.082(8) -0.023(5) -0.018(12) C6C 0.125(5) 0.057(3) 0.049(2) -0.022(2) -0.002(3) -0.001(5) C7C 0.130(7) 0.104(6) 0.047(3) -0.032(4) -0.003(3) -0.031(4) C8C 0.175(7) 0.168(14) 0.094(5) -0.082(8) -0.023(5) -0.018(12) C9A 0.069(2) 0.0581(19) 0.0352(15) -0.0032(13) -0.0086(13) -0.0097(15) C10A 0.077(3) 0.100(3) 0.055(2) -0.006(2) -0.0300(18) 0.004(2) C11A 0.129(4) 0.060(2) 0.050(2) 0.0045(17) -0.009(2) -0.021(2) C12A 0.091(3) 0.079(2) 0.0403(17) -0.0163(17) 0.0030(17) -0.021(2) C1B 0.0474(15) 0.0374(14) 0.0436(15) -0.0059(12) 0.0051(11) -0.0052(11) C2B 0.0532(17) 0.0410(16) 0.0562(18) -0.0001(13) 0.0061(13) -0.0179(13) C3B 0.0424(15) 0.0532(17) 0.0387(15) 0.0057(13) 0.0058(11) -0.0028(12) C4B 0.0352(13) 0.0495(16) 0.0374(14) -0.0040(12) -0.0029(10) -0.0007(11) C5B 0.0298(12) 0.0410(14) 0.0397(14) -0.0027(11) 0.0035(10) -0.0002(10) C6B 0.061(2) 0.083(3) 0.0442(18) 0.0085(17) 0.0167(15) -0.0045(18) C7B 0.084(3) 0.100(3) 0.057(2) 0.015(2) 0.026(2) 0.011(2) C8B 0.115(4) 0.167(5) 0.052(3) 0.005(3) 0.010(2) 0.044(4) C9B 0.080(2) 0.0485(18) 0.057(2) -0.0214(15) 0.0043(16) -0.0049(16) C10B 0.154(5) 0.083(3) 0.100(3) -0.050(3) 0.021(3) -0.057(3) C11B 0.156(5) 0.095(3) 0.100(4) -0.048(3) -0.014(3) 0.060(3) C12B 0.077(2) 0.083(3) 0.055(2) -0.0281(18) 0.0140(17) -0.019(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 Cl2 2.4353(7) . ? Zr1 Cl1 2.4450(7) . ? Zr1 C4B 2.469(3) . ? Zr1 C4A 2.474(3) . ? Zr1 C5A 2.484(2) . ? Zr1 C5B 2.484(2) . ? Zr1 C3A 2.533(3) . ? Zr1 C2A 2.557(3) . ? Zr1 C3B 2.559(3) . ? Zr1 C2B 2.563(3) . ? Zr1 C1B 2.582(3) . ? Zr1 C1A 2.612(2) . ? C1A C2A 1.405(4) . ? C1A C5A 1.412(4) . ? C1A C9A 1.519(4) . ? C2A C3A 1.416(4) . ? C2A H2A 0.9400 . ? C3A C4A 1.394(4) . ? C3A C6A 1.489(10) . ? C3A C6C 1.531(7) . ? C4A C5A 1.411(4) . ? C4A H4A 0.9400 . ? C5A H5A 0.9400 . ? C6A C7A 1.486(10) . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C7A C8A 1.277(10) . ? C7A H7A 0.9400 . ? C8A H8AA 0.9400 . ? C8A H8AB 0.9400 . ? C6C C7C 1.488(10) . ? C6C H6CA 0.9800 . ? C6C H6CB 0.9800 . ? C7C C8C 1.286(9) . ? C7C H7C 0.9400 . ? C8C H8CA 0.9400 . ? C8C H8CB 0.9400 . ? C9A C12A 1.507(5) . ? C9A C10A 1.529(5) . ? C9A C11A 1.564(5) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C10A H10C 0.9700 . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C11A H11C 0.9700 . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C12A H12C 0.9700 . ? C1B C5B 1.406(4) . ? C1B C2B 1.418(4) . ? C1B C9B 1.522(4) . ? C2B C3B 1.400(4) . ? C2B H2B 0.9400 . ? C3B C4B 1.401(4) . ? C3B C6B 1.512(4) . ? C4B C5B 1.412(4) . ? C4B H4B 0.9400 . ? C5B H5B 0.9400 . ? C6B C7B 1.488(5) . ? C6B H6BA 0.9800 . ? C6B H6BB 0.9800 . ? C7B C8B 1.256(6) . ? C7B H7B 0.9400 . ? C8B H8BA 0.9400 . ? C8B H8BB 0.9400 . ? C9B C12B 1.520(5) . ? C9B C10B 1.528(5) . ? C9B C11B 1.537(6) . ? C10B H10D 0.9700 . ? C10B H10E 0.9700 . ? C10B H10F 0.9700 . ? C11B H11D 0.9700 . ? C11B H11E 0.9700 . ? C11B H11F 0.9700 . ? C12B H12D 0.9700 . ? C12B H12E 0.9700 . ? C12B H12F 0.9700 . ? 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 Cl2 Zr1 Cl1 93.34(3) . . ? Cl2 Zr1 C4B 136.50(7) . . ? Cl1 Zr1 C4B 98.71(6) . . ? Cl2 Zr1 C4A 134.75(7) . . ? Cl1 Zr1 C4A 110.03(8) . . ? C4B Zr1 C4A 79.01(9) . . ? Cl2 Zr1 C5A 103.69(7) . . ? Cl1 Zr1 C5A 133.24(7) . . ? C4B Zr1 C5A 97.90(9) . . ? C4A Zr1 C5A 33.07(9) . . ? Cl2 Zr1 C5B 114.80(7) . . ? Cl1 Zr1 C5B 130.32(6) . . ? C4B Zr1 C5B 33.13(9) . . ? C4A Zr1 C5B 79.08(9) . . ? C5A Zr1 C5B 80.83(8) . . ? Cl2 Zr1 C3A 126.69(7) . . ? Cl1 Zr1 C3A 80.76(8) . . ? C4B Zr1 C3A 96.55(10) . . ? C4A Zr1 C3A 32.30(10) . . ? C5A Zr1 C3A 54.07(10) . . ? C5B Zr1 C3A 108.48(10) . . ? Cl2 Zr1 C2A 94.45(7) . . ? Cl1 Zr1 C2A 82.77(7) . . ? C4B Zr1 C2A 128.38(9) . . ? C4A Zr1 C2A 53.20(9) . . ? C5A Zr1 C2A 53.13(9) . . ? C5B Zr1 C2A 130.73(9) . . ? C3A Zr1 C2A 32.30(9) . . ? Cl2 Zr1 C3B 113.26(8) . . ? Cl1 Zr1 C3B 78.09(7) . . ? C4B Zr1 C3B 32.29(9) . . ? C4A Zr1 C3B 109.29(9) . . ? C5A Zr1 C3B 129.91(9) . . ? C5B Zr1 C3B 53.78(8) . . ? C3A Zr1 C3B 116.98(10) . . ? C2A Zr1 C3B 146.90(10) . . ? Cl2 Zr1 C2B 84.79(8) . . ? Cl1 Zr1 C2B 93.04(7) . . ? C4B Zr1 C2B 53.11(10) . . ? C4A Zr1 C2B 129.78(10) . . ? C5A Zr1 C2B 131.16(9) . . ? C5B Zr1 C2B 53.09(9) . . ? C3A Zr1 C2B 148.00(10) . . ? C2A Zr1 C2B 175.70(9) . . ? C3B Zr1 C2B 31.72(10) . . ? Cl2 Zr1 C1B 85.21(7) . . ? Cl1 Zr1 C1B 125.01(6) . . ? C4B Zr1 C1B 53.84(9) . . ? C4A Zr1 C1B 109.16(9) . . ? C5A Zr1 C1B 99.88(9) . . ? C5B Zr1 C1B 32.15(9) . . ? C3A Zr1 C1B 140.27(10) . . ? C2A Zr1 C1B 152.21(9) . . ? C3B Zr1 C1B 53.26(9) . . ? C2B Zr1 C1B 32.00(9) . . ? Cl2 Zr1 C1A 82.22(6) . . ? Cl1 Zr1 C1A 112.35(6) . . ? C4B Zr1 C1A 129.20(8) . . ? C4A Zr1 C1A 53.39(8) . . ? C5A Zr1 C1A 32.06(8) . . ? C5B Zr1 C1A 111.43(8) . . ? C3A Zr1 C1A 53.21(9) . . ? C2A Zr1 C1A 31.52(8) . . ? C3B Zr1 C1A 161.48(9) . . ? C2B Zr1 C1A 151.99(9) . . ? C1B Zr1 C1A 121.77(8) . . ? C2A C1A C5A 106.3(2) . . ? C2A C1A C9A 126.2(2) . . ? C5A C1A C9A 126.4(3) . . ? C2A C1A Zr1 72.07(15) . . ? C5A C1A Zr1 68.96(14) . . ? C9A C1A Zr1 133.02(19) . . ? C1A C2A C3A 109.6(2) . . ? C1A C2A Zr1 76.41(15) . . ? C3A C2A Zr1 72.94(16) . . ? C1A C2A H2A 125.2 . . ? C3A C2A H2A 125.2 . . ? Zr1 C2A H2A 117.3 . . ? C4A C3A C2A 106.7(3) . . ? C4A C3A C6A 122.5(8) . . ? C2A C3A C6A 130.6(8) . . ? C4A C3A C6C 131.0(5) . . ? C2A C3A C6C 122.2(5) . . ? C6A C3A C6C 8.5(12) . . ? C4A C3A Zr1 71.53(16) . . ? C2A C3A Zr1 74.76(17) . . ? C6A C3A Zr1 124(2) . . ? C6C C3A Zr1 122.6(11) . . ? C3A C4A C5A 108.8(2) . . ? C3A C4A Zr1 76.17(17) . . ? C5A C4A Zr1 73.82(15) . . ? C3A C4A H4A 125.6 . . ? C5A C4A H4A 125.6 . . ? Zr1 C4A H4A 116.4 . . ? C4A C5A C1A 108.3(2) . . ? C4A C5A Zr1 73.11(15) . . ? C1A C5A Zr1 78.99(15) . . ? C4A C5A H5A 125.8 . . ? C1A C5A H5A 125.8 . . ? Zr1 C5A H5A 114.3 . . ? C7A C6A C3A 115.9(12) . . ? C7A C6A H6AA 108.3 . . ? C3A C6A H6AA 108.3 . . ? C7A C6A H6AB 108.3 . . ? C3A C6A H6AB 108.3 . . ? H6AA C6A H6AB 107.4 . . ? C8A C7A C6A 117(3) . . ? C8A C7A H7A 121.4 . . ? C6A C7A H7A 121.4 . . ? C7A C8A H8AA 120.0 . . ? C7A C8A H8AB 120.0 . . ? H8AA C8A H8AB 120.0 . . ? C7C C6C C3A 114.0(9) . . ? C7C C6C H6CA 108.7 . . ? C3A C6C H6CA 108.7 . . ? C7C C6C H6CB 108.7 . . ? C3A C6C H6CB 108.7 . . ? H6CA C6C H6CB 107.6 . . ? C8C C7C C6C 126.2(14) . . ? C8C C7C H7C 116.9 . . ? C6C C7C H7C 116.9 . . ? C7C C8C H8CA 120.0 . . ? C7C C8C H8CB 120.0 . . ? H8CA C8C H8CB 120.0 . . ? C12A C9A C1A 113.7(3) . . ? C12A C9A C10A 111.4(3) . . ? C1A C9A C10A 112.5(3) . . ? C12A C9A C11A 106.6(3) . . ? C1A C9A C11A 104.3(3) . . ? C10A C9A C11A 107.7(3) . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C9A C11A H11A 109.5 . . ? C9A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C9A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? C9A C12A H12A 109.5 . . ? C9A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C9A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C5B C1B C2B 106.1(2) . . ? C5B C1B C9B 125.2(3) . . ? C2B C1B C9B 127.9(3) . . ? C5B C1B Zr1 70.07(14) . . ? C2B C1B Zr1 73.26(16) . . ? C9B C1B Zr1 129.4(2) . . ? C3B C2B C1B 109.7(3) . . ? C3B C2B Zr1 73.96(16) . . ? C1B C2B Zr1 74.74(16) . . ? C3B C2B H2B 125.1 . . ? C1B C2B H2B 125.1 . . ? Zr1 C2B H2B 117.9 . . ? C2B C3B C4B 107.0(2) . . ? C2B C3B C6B 126.5(3) . . ? C4B C3B C6B 126.3(3) . . ? C2B C3B Zr1 74.32(16) . . ? C4B C3B Zr1 70.34(14) . . ? C6B C3B Zr1 124.7(2) . . ? C3B C4B C5B 108.4(3) . . ? C3B C4B Zr1 77.37(15) . . ? C5B C4B Zr1 74.01(14) . . ? C3B C4B H4B 125.8 . . ? C5B C4B H4B 125.8 . . ? Zr1 C4B H4B 115.0 . . ? C1B C5B C4B 108.7(2) . . ? C1B C5B Zr1 77.78(15) . . ? C4B C5B Zr1 72.86(14) . . ? C1B C5B H5B 125.7 . . ? C4B C5B H5B 125.7 . . ? Zr1 C5B H5B 115.7 . . ? C7B C6B C3B 111.0(3) . . ? C7B C6B H6BA 109.4 . . ? C3B C6B H6BA 109.4 . . ? C7B C6B H6BB 109.4 . . ? C3B C6B H6BB 109.4 . . ? H6BA C6B H6BB 108.0 . . ? C8B C7B C6B 127.2(5) . . ? C8B C7B H7B 116.4 . . ? C6B C7B H7B 116.4 . . ? C7B C8B H8BA 120.0 . . ? C7B C8B H8BB 120.0 . . ? H8BA C8B H8BB 120.0 . . ? C12B C9B C1B 112.0(3) . . ? C12B C9B C10B 108.8(3) . . ? C1B C9B C10B 112.0(3) . . ? C12B C9B C11B 108.3(4) . . ? C1B C9B C11B 106.4(3) . . ? C10B C9B C11B 109.2(4) . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C9B C11B H11D 109.5 . . ? C9B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C9B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C9B C12B H12D 109.5 . . ? C9B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C9B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Zr1 C1A C2A 111.87(16) . . . . ? Cl1 Zr1 C1A C2A 21.45(17) . . . . ? C4B Zr1 C1A C2A -101.70(18) . . . . ? C4A Zr1 C1A C2A -77.52(18) . . . . ? C5A Zr1 C1A C2A -116.2(2) . . . . ? C5B Zr1 C1A C2A -134.48(16) . . . . ? C3A Zr1 C1A C2A -36.92(17) . . . . ? C3B Zr1 C1A C2A -100.2(3) . . . . ? C2B Zr1 C1A C2A 174.99(19) . . . . ? C1B Zr1 C1A C2A -168.72(16) . . . . ? Cl2 Zr1 C1A C5A -131.94(16) . . . . ? Cl1 Zr1 C1A C5A 137.64(15) . . . . ? C4B Zr1 C1A C5A 14.5(2) . . . . ? C4A Zr1 C1A C5A 38.67(16) . . . . ? C5B Zr1 C1A C5A -18.28(18) . . . . ? C3A Zr1 C1A C5A 79.27(18) . . . . ? C2A Zr1 C1A C5A 116.2(2) . . . . ? C3B Zr1 C1A C5A 16.0(4) . . . . ? C2B Zr1 C1A C5A -68.8(2) . . . . ? C1B Zr1 C1A C5A -52.52(19) . . . . ? Cl2 Zr1 C1A C9A -11.3(3) . . . . ? Cl1 Zr1 C1A C9A -101.7(3) . . . . ? C4B Zr1 C1A C9A 135.1(3) . . . . ? C4A Zr1 C1A C9A 159.3(3) . . . . ? C5A Zr1 C1A C9A 120.7(3) . . . . ? C5B Zr1 C1A C9A 102.4(3) . . . . ? C3A Zr1 C1A C9A -160.1(3) . . . . ? C2A Zr1 C1A C9A -123.2(3) . . . . ? C3B Zr1 C1A C9A 136.6(3) . . . . ? C2B Zr1 C1A C9A 51.8(4) . . . . ? C1B Zr1 C1A C9A 68.1(3) . . . . ? C5A C1A C2A C3A 5.2(3) . . . . ? C9A C1A C2A C3A -163.3(3) . . . . ? Zr1 C1A C2A C3A 66.0(2) . . . . ? C5A C1A C2A Zr1 -60.78(18) . . . . ? C9A C1A C2A Zr1 130.7(3) . . . . ? Cl2 Zr1 C2A C1A -67.26(15) . . . . ? Cl1 Zr1 C2A C1A -160.07(16) . . . . ? C4B Zr1 C2A C1A 104.52(17) . . . . ? C4A Zr1 C2A C1A 78.19(18) . . . . ? C5A Zr1 C2A C1A 36.53(15) . . . . ? C5B Zr1 C2A C1A 61.21(19) . . . . ? C3A Zr1 C2A C1A 115.8(3) . . . . ? C3B Zr1 C2A C1A 145.08(17) . . . . ? C2B Zr1 C2A C1A -146.8(12) . . . . ? C1B Zr1 C2A C1A 20.9(3) . . . . ? Cl2 Zr1 C2A C3A 176.93(17) . . . . ? Cl1 Zr1 C2A C3A 84.12(17) . . . . ? C4B Zr1 C2A C3A -11.3(2) . . . . ? C4A Zr1 C2A C3A -37.62(18) . . . . ? C5A Zr1 C2A C3A -79.27(19) . . . . ? C5B Zr1 C2A C3A -54.6(2) . . . . ? C3B Zr1 C2A C3A 29.3(3) . . . . ? C2B Zr1 C2A C3A 97.4(13) . . . . ? C1B Zr1 C2A C3A -94.9(2) . . . . ? C1A Zr1 C2A C3A -115.8(3) . . . . ? C1A C2A C3A C4A -3.4(3) . . . . ? Zr1 C2A C3A C4A 64.9(2) . . . . ? C1A C2A C3A C6A 170(3) . . . . ? Zr1 C2A C3A C6A -121(3) . . . . ? C1A C2A C3A C6C 172.5(13) . . . . ? Zr1 C2A C3A C6C -119.2(13) . . . . ? C1A C2A C3A Zr1 -68.3(2) . . . . ? Cl2 Zr1 C3A C4A -117.66(16) . . . . ? Cl1 Zr1 C3A C4A 155.08(17) . . . . ? C4B Zr1 C3A C4A 57.27(18) . . . . ? C5A Zr1 C3A C4A -37.76(16) . . . . ? C5B Zr1 C3A C4A 25.53(19) . . . . ? C2A Zr1 C3A C4A -113.8(3) . . . . ? C3B Zr1 C3A C4A 83.59(18) . . . . ? C2B Zr1 C3A C4A 74.2(2) . . . . ? C1B Zr1 C3A C4A 19.5(2) . . . . ? C1A Zr1 C3A C4A -77.84(18) . . . . ? Cl2 Zr1 C3A C2A -3.8(2) . . . . ? Cl1 Zr1 C3A C2A -91.08(17) . . . . ? C4B Zr1 C3A C2A 171.11(17) . . . . ? C4A Zr1 C3A C2A 113.8(3) . . . . ? C5A Zr1 C3A C2A 76.08(18) . . . . ? C5B Zr1 C3A C2A 139.37(17) . . . . ? C3B Zr1 C3A C2A -162.57(16) . . . . ? C2B Zr1 C3A C2A -171.94(17) . . . . ? C1B Zr1 C3A C2A 133.39(18) . . . . ? C1A Zr1 C3A C2A 36.00(16) . . . . ? Cl2 Zr1 C3A C6A 125.1(9) . . . . ? Cl1 Zr1 C3A C6A 37.8(9) . . . . ? C4B Zr1 C3A C6A -60.0(9) . . . . ? C4A Zr1 C3A C6A -117.3(10) . . . . ? C5A Zr1 C3A C6A -155.0(10) . . . . ? C5B Zr1 C3A C6A -91.7(9) . . . . ? C2A Zr1 C3A C6A 128.9(10) . . . . ? C3B Zr1 C3A C6A -33.7(9) . . . . ? C2B Zr1 C3A C6A -43.0(10) . . . . ? C1B Zr1 C3A C6A -97.7(9) . . . . ? C1A Zr1 C3A C6A 164.9(10) . . . . ? Cl2 Zr1 C3A C6C 115.0(5) . . . . ? Cl1 Zr1 C3A C6C 27.7(5) . . . . ? C4B Zr1 C3A C6C -70.1(5) . . . . ? C4A Zr1 C3A C6C -127.3(6) . . . . ? C5A Zr1 C3A C6C -165.1(5) . . . . ? C5B Zr1 C3A C6C -101.8(5) . . . . ? C2A Zr1 C3A C6C 118.8(6) . . . . ? C3B Zr1 C3A C6C -43.8(5) . . . . ? C2B Zr1 C3A C6C -53.1(6) . . . . ? C1B Zr1 C3A C6C -107.8(5) . . . . ? C1A Zr1 C3A C6C 154.8(5) . . . . ? C2A C3A C4A C5A 0.1(3) . . . . ? C6A C3A C4A C5A -174(3) . . . . ? C6C C3A C4A C5A -175.2(15) . . . . ? Zr1 C3A C4A C5A 67.23(19) . . . . ? C2A C3A C4A Zr1 -67.1(2) . . . . ? C6A C3A C4A Zr1 119(3) . . . . ? C6C C3A C4A Zr1 117.5(15) . . . . ? Cl2 Zr1 C4A C3A 90.38(19) . . . . ? Cl1 Zr1 C4A C3A -26.28(18) . . . . ? C4B Zr1 C4A C3A -121.64(18) . . . . ? C5A Zr1 C4A C3A 114.7(2) . . . . ? C5B Zr1 C4A C3A -155.40(18) . . . . ? C2A Zr1 C4A C3A 37.62(16) . . . . ? C3B Zr1 C4A C3A -110.23(17) . . . . ? C2B Zr1 C4A C3A -138.43(17) . . . . ? C1B Zr1 C4A C3A -166.92(16) . . . . ? C1A Zr1 C4A C3A 77.22(17) . . . . ? Cl2 Zr1 C4A C5A -24.3(2) . . . . ? Cl1 Zr1 C4A C5A -140.93(15) . . . . ? C4B Zr1 C4A C5A 123.70(18) . . . . ? C5B Zr1 C4A C5A 89.94(17) . . . . ? C3A Zr1 C4A C5A -114.7(2) . . . . ? C2A Zr1 C4A C5A -77.04(17) . . . . ? C3B Zr1 C4A C5A 135.11(16) . . . . ? C2B Zr1 C4A C5A 106.92(18) . . . . ? C1B Zr1 C4A C5A 78.43(17) . . . . ? C1A Zr1 C4A C5A -37.43(15) . . . . ? C3A C4A C5A C1A 3.1(3) . . . . ? Zr1 C4A C5A C1A 71.90(18) . . . . ? C3A C4A C5A Zr1 -68.8(2) . . . . ? C2A C1A C5A C4A -5.1(3) . . . . ? C9A C1A C5A C4A 163.4(3) . . . . ? Zr1 C1A C5A C4A -67.91(17) . . . . ? C2A C1A C5A Zr1 62.83(19) . . . . ? C9A C1A C5A Zr1 -128.7(3) . . . . ? Cl2 Zr1 C5A C4A 162.51(15) . . . . ? Cl1 Zr1 C5A C4A 54.37(19) . . . . ? C4B Zr1 C5A C4A -55.54(18) . . . . ? C5B Zr1 C5A C4A -84.04(17) . . . . ? C3A Zr1 C5A C4A 36.85(17) . . . . ? C2A Zr1 C5A C4A 77.27(18) . . . . ? C3B Zr1 C5A C4A -60.3(2) . . . . ? C2B Zr1 C5A C4A -102.40(19) . . . . ? C1B Zr1 C5A C4A -110.06(17) . . . . ? C1A Zr1 C5A C4A 113.2(2) . . . . ? Cl2 Zr1 C5A C1A 49.34(16) . . . . ? Cl1 Zr1 C5A C1A -58.80(18) . . . . ? C4B Zr1 C5A C1A -168.71(16) . . . . ? C4A Zr1 C5A C1A -113.2(2) . . . . ? C5B Zr1 C5A C1A 162.79(17) . . . . ? C3A Zr1 C5A C1A -76.32(17) . . . . ? C2A Zr1 C5A C1A -35.90(15) . . . . ? C3B Zr1 C5A C1A -173.45(15) . . . . ? C2B Zr1 C5A C1A 144.43(16) . . . . ? C1B Zr1 C5A C1A 136.77(16) . . . . ? C4A C3A C6A C7A 6(5) . . . . ? C2A C3A C6A C7A -166.7(18) . . . . ? C6C C3A C6A C7A -179(25) . . . . ? Zr1 C3A C6A C7A 95(4) . . . . ? C3A C6A C7A C8A -120(3) . . . . ? C4A C3A C6C C7C -28(3) . . . . ? C2A C3A C6C C7C 157.5(11) . . . . ? C6A C3A C6C C7C -34(20) . . . . ? Zr1 C3A C6C C7C 65.6(18) . . . . ? C3A C6C C7C C8C 116.2(18) . . . . ? C2A C1A C9A C12A -156.1(3) . . . . ? C5A C1A C9A C12A 37.5(4) . . . . ? Zr1 C1A C9A C12A -56.9(4) . . . . ? C2A C1A C9A C10A -28.3(4) . . . . ? C5A C1A C9A C10A 165.4(3) . . . . ? Zr1 C1A C9A C10A 71.0(4) . . . . ? C2A C1A C9A C11A 88.2(4) . . . . ? C5A C1A C9A C11A -78.1(4) . . . . ? Zr1 C1A C9A C11A -172.6(2) . . . . ? Cl2 Zr1 C1B C5B 157.56(15) . . . . ? Cl1 Zr1 C1B C5B -111.71(14) . . . . ? C4B Zr1 C1B C5B -38.14(15) . . . . ? C4A Zr1 C1B C5B 21.61(17) . . . . ? C5A Zr1 C1B C5B 54.47(16) . . . . ? C3A Zr1 C1B C5B 10.7(2) . . . . ? C2A Zr1 C1B C5B 67.1(3) . . . . ? C3B Zr1 C1B C5B -78.58(17) . . . . ? C2B Zr1 C1B C5B -114.6(2) . . . . ? C1A Zr1 C1B C5B 79.78(17) . . . . ? Cl2 Zr1 C1B C2B -87.82(17) . . . . ? Cl1 Zr1 C1B C2B 2.9(2) . . . . ? C4B Zr1 C1B C2B 76.48(18) . . . . ? C4A Zr1 C1B C2B 136.23(18) . . . . ? C5A Zr1 C1B C2B 169.09(18) . . . . ? C5B Zr1 C1B C2B 114.6(2) . . . . ? C3A Zr1 C1B C2B 125.32(19) . . . . ? C2A Zr1 C1B C2B -178.28(19) . . . . ? C3B Zr1 C1B C2B 36.04(17) . . . . ? C1A Zr1 C1B C2B -165.60(16) . . . . ? Cl2 Zr1 C1B C9B 37.9(3) . . . . ? Cl1 Zr1 C1B C9B 128.6(2) . . . . ? C4B Zr1 C1B C9B -157.8(3) . . . . ? C4A Zr1 C1B C9B -98.1(3) . . . . ? C5A Zr1 C1B C9B -65.2(3) . . . . ? C5B Zr1 C1B C9B -119.7(3) . . . . ? C3A Zr1 C1B C9B -109.0(3) . . . . ? C2A Zr1 C1B C9B -52.6(4) . . . . ? C3B Zr1 C1B C9B 161.7(3) . . . . ? C2B Zr1 C1B C9B 125.7(3) . . . . ? C1A Zr1 C1B C9B -39.9(3) . . . . ? C5B C1B C2B C3B -3.5(3) . . . . ? C9B C1B C2B C3B 166.4(3) . . . . ? Zr1 C1B C2B C3B -66.3(2) . . . . ? C5B C1B C2B Zr1 62.80(18) . . . . ? C9B C1B C2B Zr1 -127.3(3) . . . . ? Cl2 Zr1 C2B C3B -154.44(17) . . . . ? Cl1 Zr1 C2B C3B -61.36(16) . . . . ? C4B Zr1 C2B C3B 37.25(16) . . . . ? C4A Zr1 C2B C3B 58.0(2) . . . . ? C5A Zr1 C2B C3B 101.91(18) . . . . ? C5B Zr1 C2B C3B 79.03(18) . . . . ? C3A Zr1 C2B C3B 16.0(3) . . . . ? C2A Zr1 C2B C3B -74.5(13) . . . . ? C1B Zr1 C2B C3B 116.3(3) . . . . ? C1A Zr1 C2B C3B 143.01(19) . . . . ? Cl2 Zr1 C2B C1B 89.31(17) . . . . ? Cl1 Zr1 C2B C1B -177.62(17) . . . . ? C4B Zr1 C2B C1B -79.00(18) . . . . ? C4A Zr1 C2B C1B -58.2(2) . . . . ? C5A Zr1 C2B C1B -14.3(2) . . . . ? C5B Zr1 C2B C1B -37.23(16) . . . . ? C3A Zr1 C2B C1B -100.2(2) . . . . ? C2A Zr1 C2B C1B 169.2(12) . . . . ? C3B Zr1 C2B C1B -116.3(3) . . . . ? C1A Zr1 C2B C1B 26.8(3) . . . . ? C1B C2B C3B C4B 3.6(3) . . . . ? Zr1 C2B C3B C4B -63.17(19) . . . . ? C1B C2B C3B C6B -171.3(3) . . . . ? Zr1 C2B C3B C6B 121.9(3) . . . . ? C1B C2B C3B Zr1 66.8(2) . . . . ? Cl2 Zr1 C3B C2B 27.89(18) . . . . ? Cl1 Zr1 C3B C2B 116.40(17) . . . . ? C4B Zr1 C3B C2B -115.0(3) . . . . ? C4A Zr1 C3B C2B -136.32(18) . . . . ? C5A Zr1 C3B C2B -106.19(19) . . . . ? C5B Zr1 C3B C2B -76.66(18) . . . . ? C3A Zr1 C3B C2B -170.55(17) . . . . ? C2A Zr1 C3B C2B 172.40(17) . . . . ? C1B Zr1 C3B C2B -36.37(16) . . . . ? C1A Zr1 C3B C2B -117.2(3) . . . . ? Cl2 Zr1 C3B C4B 142.90(16) . . . . ? Cl1 Zr1 C3B C4B -128.59(18) . . . . ? C4A Zr1 C3B C4B -21.3(2) . . . . ? C5A Zr1 C3B C4B 8.8(2) . . . . ? C5B Zr1 C3B C4B 38.36(16) . . . . ? C3A Zr1 C3B C4B -55.5(2) . . . . ? C2A Zr1 C3B C4B -72.6(2) . . . . ? C2B Zr1 C3B C4B 115.0(3) . . . . ? C1B Zr1 C3B C4B 78.64(18) . . . . ? C1A Zr1 C3B C4B -2.2(4) . . . . ? Cl2 Zr1 C3B C6B -96.0(3) . . . . ? Cl1 Zr1 C3B C6B -7.5(3) . . . . ? C4B Zr1 C3B C6B 121.1(4) . . . . ? C4A Zr1 C3B C6B 99.8(3) . . . . ? C5A Zr1 C3B C6B 130.0(3) . . . . ? C5B Zr1 C3B C6B 159.5(3) . . . . ? C3A Zr1 C3B C6B 65.6(3) . . . . ? C2A Zr1 C3B C6B 48.5(4) . . . . ? C2B Zr1 C3B C6B -123.9(4) . . . . ? C1B Zr1 C3B C6B -160.2(3) . . . . ? C1A Zr1 C3B C6B 119.0(3) . . . . ? C2B C3B C4B C5B -2.3(3) . . . . ? C6B C3B C4B C5B 172.7(3) . . . . ? Zr1 C3B C4B C5B -68.15(18) . . . . ? C2B C3B C4B Zr1 65.8(2) . . . . ? C6B C3B C4B Zr1 -119.2(3) . . . . ? Cl2 Zr1 C4B C3B -53.6(2) . . . . ? Cl1 Zr1 C4B C3B 50.69(18) . . . . ? C4A Zr1 C4B C3B 159.6(2) . . . . ? C5A Zr1 C4B C3B -173.17(18) . . . . ? C5B Zr1 C4B C3B -113.6(2) . . . . ? C3A Zr1 C4B C3B 132.30(18) . . . . ? C2A Zr1 C4B C3B 138.34(18) . . . . ? C2B Zr1 C4B C3B -36.56(17) . . . . ? C1B Zr1 C4B C3B -76.67(19) . . . . ? C1A Zr1 C4B C3B 179.12(16) . . . . ? Cl2 Zr1 C4B C5B 60.03(18) . . . . ? Cl1 Zr1 C4B C5B 164.33(14) . . . . ? C4A Zr1 C4B C5B -86.81(17) . . . . ? C5A Zr1 C4B C5B -59.53(17) . . . . ? C3A Zr1 C4B C5B -114.06(17) . . . . ? C2A Zr1 C4B C5B -108.02(17) . . . . ? C3B Zr1 C4B C5B 113.6(2) . . . . ? C2B Zr1 C4B C5B 77.08(17) . . . . ? C1B Zr1 C4B C5B 36.97(15) . . . . ? C1A Zr1 C4B C5B -67.24(19) . . . . ? C2B C1B C5B C4B 2.0(3) . . . . ? C9B C1B C5B C4B -168.2(3) . . . . ? Zr1 C1B C5B C4B 66.96(18) . . . . ? C2B C1B C5B Zr1 -65.0(2) . . . . ? C9B C1B C5B Zr1 124.8(3) . . . . ? C3B C4B C5B C1B 0.2(3) . . . . ? Zr1 C4B C5B C1B -70.25(18) . . . . ? C3B C4B C5B Zr1 70.42(19) . . . . ? Cl2 Zr1 C5B C1B -24.77(16) . . . . ? Cl1 Zr1 C5B C1B 93.67(16) . . . . ? C4B Zr1 C5B C1B 114.2(2) . . . . ? C4A Zr1 C5B C1B -159.25(17) . . . . ? C5A Zr1 C5B C1B -125.70(16) . . . . ? C3A Zr1 C5B C1B -172.81(15) . . . . ? C2A Zr1 C5B C1B -145.48(15) . . . . ? C3B Zr1 C5B C1B 76.82(17) . . . . ? C2B Zr1 C5B C1B 37.05(15) . . . . ? C1A Zr1 C5B C1B -115.99(15) . . . . ? Cl2 Zr1 C5B C4B -138.93(14) . . . . ? Cl1 Zr1 C5B C4B -20.49(19) . . . . ? C4A Zr1 C5B C4B 86.59(17) . . . . ? C5A Zr1 C5B C4B 120.14(17) . . . . ? C3A Zr1 C5B C4B 73.03(17) . . . . ? C2A Zr1 C5B C4B 100.36(17) . . . . ? C3B Zr1 C5B C4B -37.34(16) . . . . ? C2B Zr1 C5B C4B -77.11(17) . . . . ? C1B Zr1 C5B C4B -114.2(2) . . . . ? C1A Zr1 C5B C4B 129.85(16) . . . . ? C2B C3B C6B C7B 85.6(4) . . . . ? C4B C3B C6B C7B -88.4(4) . . . . ? Zr1 C3B C6B C7B -178.4(3) . . . . ? C3B C6B C7B C8B 128.5(5) . . . . ? C5B C1B C9B C12B -51.9(4) . . . . ? C2B C1B C9B C12B 140.1(3) . . . . ? Zr1 C1B C9B C12B 40.4(4) . . . . ? C5B C1B C9B C10B -174.5(3) . . . . ? C2B C1B C9B C10B 17.5(5) . . . . ? Zr1 C1B C9B C10B -82.2(4) . . . . ? C5B C1B C9B C11B 66.3(4) . . . . ? C2B C1B C9B C11B -101.8(4) . . . . ? Zr1 C1B C9B C11B 158.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.482 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.067 # Attachment 'erk5009.cif' data_erk5009 _database_code_depnum_ccdc_archive 'CCDC 735245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Cl2 Zr' _chemical_formula_weight 484.63 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.4863(3) _cell_length_b 6.6869(1) _cell_length_c 20.7792(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.909(1) _cell_angle_gamma 90.00 _cell_volume 2470.26(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2938 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8508 _exptl_absorpt_correction_T_max 0.9674 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12058 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2942 _reflns_number_gt 2570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.3046P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2942 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.0000 0.80991(4) 0.2500 0.02836(10) Uani 1 2 d S . . Cl1 Cl 0.09003(3) 1.06246(8) 0.23620(3) 0.04347(15) Uani 1 1 d . . . C1 C -0.10926(13) 0.6787(3) 0.15422(11) 0.0378(5) Uani 1 1 d . . . C2 C -0.07016(13) 0.8206(3) 0.12545(11) 0.0394(5) Uani 1 1 d . . . H2 H -0.0897 0.9439 0.1068 0.047 Uiso 1 1 calc R . . C3 C 0.00235(13) 0.7478(3) 0.12922(11) 0.0363(5) Uani 1 1 d . . . C4 C 0.01046(13) 0.5655(3) 0.16379(10) 0.0359(5) Uani 1 1 d . . . H4 H 0.0540 0.4857 0.1751 0.043 Uiso 1 1 calc R . . C5 C -0.05824(13) 0.5220(3) 0.17878(11) 0.0362(5) Uani 1 1 d . . . H5 H -0.0681 0.4077 0.2013 0.043 Uiso 1 1 calc R . . C6 C 0.05767(15) 0.8380(4) 0.09625(12) 0.0471(6) Uani 1 1 d . . . H6A H 0.0513 0.9835 0.0938 0.057 Uiso 1 1 calc R . . H6B H 0.1090 0.8090 0.1231 0.057 Uiso 1 1 calc R . . C7 C 0.04614(17) 0.7548(4) 0.02714(13) 0.0536(7) Uani 1 1 d . . . H7 H -0.0031 0.7574 -0.0014 0.064 Uiso 1 1 calc R . . C8 C 0.0977(2) 0.6801(5) 0.00340(16) 0.0761(10) Uani 1 1 d . . . H8A H 0.1478 0.6746 0.0302 0.091 Uiso 1 1 calc R . . H8B H 0.0854 0.6313 -0.0407 0.091 Uiso 1 1 calc R . . C9 C -0.19325(14) 0.6735(4) 0.14953(14) 0.0535(7) Uani 1 1 d . . . C10 C -0.22774(17) 0.5155(6) 0.09597(18) 0.0856(11) Uani 1 1 d . . . H10A H -0.2817 0.5095 0.0896 0.128 Uiso 1 1 calc R . . H10B H -0.2057 0.3858 0.1105 0.128 Uiso 1 1 calc R . . H10C H -0.2175 0.5517 0.0541 0.128 Uiso 1 1 calc R . . C11 C -0.23111(16) 0.8748(5) 0.12730(17) 0.0727(9) Uani 1 1 d . . . H11A H -0.2845 0.8644 0.1233 0.109 Uiso 1 1 calc R . . H11B H -0.2239 0.9115 0.0843 0.109 Uiso 1 1 calc R . . H11C H -0.2090 0.9762 0.1602 0.109 Uiso 1 1 calc R . . C12 C -0.20698(16) 0.6092(5) 0.21581(15) 0.0639(8) Uani 1 1 d . . . H12A H -0.1860 0.7084 0.2499 0.096 Uiso 1 1 calc R . . H12B H -0.1830 0.4811 0.2293 0.096 Uiso 1 1 calc R . . H12C H -0.2606 0.5974 0.2103 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.03160(16) 0.02248(14) 0.03407(16) 0.000 0.01418(11) 0.000 Cl1 0.0465(3) 0.0313(3) 0.0597(4) -0.0052(2) 0.0264(3) -0.0095(2) C1 0.0376(12) 0.0420(12) 0.0353(11) -0.0010(9) 0.0126(9) -0.0068(10) C2 0.0430(13) 0.0398(12) 0.0361(11) 0.0082(9) 0.0119(10) 0.0026(10) C3 0.0422(13) 0.0366(11) 0.0328(11) 0.0001(8) 0.0149(10) -0.0051(9) C4 0.0416(12) 0.0341(11) 0.0341(11) -0.0042(9) 0.0138(9) 0.0009(9) C5 0.0464(13) 0.0303(10) 0.0335(11) -0.0013(8) 0.0138(9) -0.0088(9) C6 0.0527(15) 0.0522(14) 0.0438(13) 0.0011(11) 0.0259(12) -0.0107(11) C7 0.0568(16) 0.0680(16) 0.0394(13) 0.0051(12) 0.0188(12) -0.0085(13) C8 0.074(2) 0.101(3) 0.0601(19) -0.0262(18) 0.0295(17) -0.0120(19) C9 0.0337(13) 0.0707(18) 0.0563(16) -0.0035(13) 0.0129(11) -0.0077(12) C10 0.0473(18) 0.121(3) 0.085(2) -0.033(2) 0.0123(17) -0.0277(19) C11 0.0395(16) 0.102(2) 0.073(2) 0.0122(19) 0.0087(14) 0.0143(16) C12 0.0445(16) 0.0786(19) 0.078(2) 0.0021(17) 0.0323(15) -0.0112(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr Cl1 2.4425(5) . ? Zr Cl1 2.4425(5) 2 ? Zr C4 2.471(2) . ? Zr C4 2.471(2) 2 ? Zr C5 2.486(2) . ? Zr C5 2.486(2) 2 ? Zr C3 2.556(2) . ? Zr C3 2.556(2) 2 ? Zr C2 2.558(2) . ? Zr C2 2.558(2) 2 ? Zr C1 2.570(2) . ? Zr C1 2.570(2) 2 ? C1 C5 1.408(3) . ? C1 C2 1.420(3) . ? C1 C9 1.529(3) . ? C2 C3 1.408(3) . ? C2 H2 0.9400 . ? C3 C4 1.402(3) . ? C3 C6 1.504(3) . ? C4 C5 1.418(3) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.500(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.289(4) . ? C7 H7 0.9400 . ? C8 H8A 0.9400 . ? C8 H8B 0.9400 . ? C9 C12 1.529(4) . ? C9 C11 1.529(4) . ? C9 C10 1.540(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? 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 Cl1 Zr Cl1 92.52(3) . 2 ? Cl1 Zr C4 100.42(5) . . ? Cl1 Zr C4 137.19(6) 2 . ? Cl1 Zr C4 137.19(6) . 2 ? Cl1 Zr C4 100.42(5) 2 2 ? C4 Zr C4 97.19(10) . 2 ? Cl1 Zr C5 131.55(5) . . ? Cl1 Zr C5 114.04(6) 2 . ? C4 Zr C5 33.24(7) . . ? C4 Zr C5 79.17(7) 2 . ? Cl1 Zr C5 114.04(6) . 2 ? Cl1 Zr C5 131.55(5) 2 2 ? C4 Zr C5 79.17(7) . 2 ? C4 Zr C5 33.24(7) 2 2 ? C5 Zr C5 78.51(10) . 2 ? Cl1 Zr C3 78.55(5) . . ? Cl1 Zr C3 115.03(5) 2 . ? C4 Zr C3 32.33(7) . . ? C4 Zr C3 129.05(7) 2 . ? C5 Zr C3 53.91(7) . . ? C5 Zr C3 109.72(7) 2 . ? Cl1 Zr C3 115.03(5) . 2 ? Cl1 Zr C3 78.55(5) 2 2 ? C4 Zr C3 129.05(7) . 2 ? C4 Zr C3 32.33(7) 2 2 ? C5 Zr C3 109.72(7) . 2 ? C5 Zr C3 53.91(7) 2 2 ? C3 Zr C3 161.29(10) . 2 ? Cl1 Zr C2 91.99(5) . . ? Cl1 Zr C2 85.79(5) 2 . ? C4 Zr C2 53.41(7) . . ? C4 Zr C2 129.27(7) 2 . ? C5 Zr C2 53.33(7) . . ? C5 Zr C2 129.82(7) 2 . ? C3 Zr C2 31.96(7) . . ? C3 Zr C2 149.03(7) 2 . ? Cl1 Zr C2 85.79(5) . 2 ? Cl1 Zr C2 91.99(5) 2 2 ? C4 Zr C2 129.27(7) . 2 ? C4 Zr C2 53.41(7) 2 2 ? C5 Zr C2 129.82(7) . 2 ? C5 Zr C2 53.33(7) 2 2 ? C3 Zr C2 149.03(7) . 2 ? C3 Zr C2 31.96(7) 2 2 ? C2 Zr C2 176.80(10) . 2 ? Cl1 Zr C1 124.15(5) . . ? Cl1 Zr C1 84.89(5) 2 . ? C4 Zr C1 54.12(7) . . ? C4 Zr C1 97.72(7) 2 . ? C5 Zr C1 32.29(7) . . ? C5 Zr C1 108.46(7) 2 . ? C3 Zr C1 53.52(7) . . ? C3 Zr C1 118.92(7) 2 . ? C2 Zr C1 32.15(7) . . ? C2 Zr C1 149.96(7) 2 . ? Cl1 Zr C1 84.89(5) . 2 ? Cl1 Zr C1 124.15(5) 2 2 ? C4 Zr C1 97.72(7) . 2 ? C4 Zr C1 54.12(7) 2 2 ? C5 Zr C1 108.46(7) . 2 ? C5 Zr C1 32.29(7) 2 2 ? C3 Zr C1 118.92(7) . 2 ? C3 Zr C1 53.52(7) 2 2 ? C2 Zr C1 149.96(7) . 2 ? C2 Zr C1 32.15(7) 2 2 ? C1 Zr C1 140.07(10) . 2 ? C5 C1 C2 106.38(19) . . ? C5 C1 C9 125.0(2) . . ? C2 C1 C9 127.8(2) . . ? C5 C1 Zr 70.57(12) . . ? C2 C1 Zr 73.46(13) . . ? C9 C1 Zr 128.74(16) . . ? C3 C2 C1 109.40(19) . . ? C3 C2 Zr 73.92(13) . . ? C1 C2 Zr 74.39(13) . . ? C3 C2 H2 125.3 . . ? C1 C2 H2 125.3 . . ? Zr C2 H2 118.2 . . ? C4 C3 C2 107.20(19) . . ? C4 C3 C6 126.2(2) . . ? C2 C3 C6 126.3(2) . . ? C4 C3 Zr 70.51(12) . . ? C2 C3 Zr 74.12(12) . . ? C6 C3 Zr 125.37(15) . . ? C3 C4 C5 108.3(2) . . ? C3 C4 Zr 77.15(12) . . ? C5 C4 Zr 73.96(12) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Zr C4 H4 115.2 . . ? C1 C5 C4 108.60(19) . . ? C1 C5 Zr 77.14(12) . . ? C4 C5 Zr 72.79(12) . . ? C1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Zr C5 H5 116.4 . . ? C7 C6 C3 110.6(2) . . ? C7 C6 H6A 109.5 . . ? C3 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 125.8(3) . . ? C8 C7 H7 117.1 . . ? C6 C7 H7 117.1 . . ? C7 C8 H8A 120.0 . . ? C7 C8 H8B 120.0 . . ? H8A C8 H8B 120.0 . . ? C12 C9 C11 110.1(2) . . ? C12 C9 C1 111.4(2) . . ? C11 C9 C1 111.8(2) . . ? C12 C9 C10 108.7(2) . . ? C11 C9 C10 108.7(3) . . ? C1 C9 C10 105.9(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Zr C1 C5 115.28(12) . . . . ? Cl1 Zr C1 C5 -155.14(12) 2 . . . ? C4 Zr C1 C5 38.03(12) . . . . ? C4 Zr C1 C5 -55.29(14) 2 . . . ? C5 Zr C1 C5 -22.91(17) 2 . . . ? C3 Zr C1 C5 78.38(14) . . . . ? C3 Zr C1 C5 -81.23(14) 2 . . . ? C2 Zr C1 C5 114.63(19) . . . . ? C2 Zr C1 C5 -70.02(19) 2 . . . ? C1 Zr C1 C5 -14.69(11) 2 . . . ? Cl1 Zr C1 C2 0.65(15) . . . . ? Cl1 Zr C1 C2 90.23(12) 2 . . . ? C4 Zr C1 C2 -76.60(14) . . . . ? C4 Zr C1 C2 -169.92(13) 2 . . . ? C5 Zr C1 C2 -114.63(19) . . . . ? C5 Zr C1 C2 -137.54(13) 2 . . . ? C3 Zr C1 C2 -36.25(12) . . . . ? C3 Zr C1 C2 164.14(12) 2 . . . ? C2 Zr C1 C2 175.35(15) 2 . . . ? C1 Zr C1 C2 -129.32(13) 2 . . . ? Cl1 Zr C1 C9 -124.93(19) . . . . ? Cl1 Zr C1 C9 -35.3(2) 2 . . . ? C4 Zr C1 C9 157.8(2) . . . . ? C4 Zr C1 C9 64.5(2) 2 . . . ? C5 Zr C1 C9 119.8(3) . . . . ? C5 Zr C1 C9 96.9(2) 2 . . . ? C3 Zr C1 C9 -161.8(2) . . . . ? C3 Zr C1 C9 38.6(2) 2 . . . ? C2 Zr C1 C9 -125.6(3) . . . . ? C2 Zr C1 C9 49.8(3) 2 . . . ? C1 Zr C1 C9 105.1(2) 2 . . . ? C5 C1 C2 C3 2.9(3) . . . . ? C9 C1 C2 C3 -167.2(2) . . . . ? Zr C1 C2 C3 66.22(16) . . . . ? C5 C1 C2 Zr -63.32(15) . . . . ? C9 C1 C2 Zr 126.6(2) . . . . ? Cl1 Zr C2 C3 64.47(12) . . . . ? Cl1 Zr C2 C3 156.85(12) 2 . . . ? C4 Zr C2 C3 -37.04(12) . . . . ? C4 Zr C2 C3 -103.11(14) 2 . . . ? C5 Zr C2 C3 -78.81(14) . . . . ? C5 Zr C2 C3 -59.57(16) 2 . . . ? C3 Zr C2 C3 -143.76(19) 2 . . . ? C2 Zr C2 C3 110.60(12) 2 . . . ? C1 Zr C2 C3 -116.06(19) . . . . ? C1 Zr C2 C3 -18.8(2) 2 . . . ? Cl1 Zr C2 C1 -179.46(12) . . . . ? Cl1 Zr C2 C1 -87.08(12) 2 . . . ? C4 Zr C2 C1 79.02(14) . . . . ? C4 Zr C2 C1 12.95(17) 2 . . . ? C5 Zr C2 C1 37.26(13) . . . . ? C5 Zr C2 C1 56.49(16) 2 . . . ? C3 Zr C2 C1 116.06(19) . . . . ? C3 Zr C2 C1 -27.7(2) 2 . . . ? C2 Zr C2 C1 -133.33(12) 2 . . . ? C1 Zr C2 C1 97.3(2) 2 . . . ? C1 C2 C3 C4 -3.3(3) . . . . ? Zr C2 C3 C4 63.19(15) . . . . ? C1 C2 C3 C6 171.0(2) . . . . ? Zr C2 C3 C6 -122.5(2) . . . . ? C1 C2 C3 Zr -66.52(16) . . . . ? Cl1 Zr C3 C4 131.69(14) . . . . ? Cl1 Zr C3 C4 -140.90(12) 2 . . . ? C4 Zr C3 C4 -11.4(2) 2 . . . ? C5 Zr C3 C4 -38.42(13) . . . . ? C5 Zr C3 C4 20.03(15) 2 . . . ? C3 Zr C3 C4 -6.75(12) 2 . . . ? C2 Zr C3 C4 -115.26(19) . . . . ? C2 Zr C3 C4 70.56(19) 2 . . . ? C1 Zr C3 C4 -78.78(14) . . . . ? C1 Zr C3 C4 54.15(15) 2 . . . ? Cl1 Zr C3 C2 -113.05(13) . . . . ? Cl1 Zr C3 C2 -25.64(14) 2 . . . ? C4 Zr C3 C2 115.26(19) . . . . ? C4 Zr C3 C2 103.86(14) 2 . . . ? C5 Zr C3 C2 76.83(14) . . . . ? C5 Zr C3 C2 135.29(13) 2 . . . ? C3 Zr C3 C2 108.50(12) 2 . . . ? C2 Zr C3 C2 -174.18(18) 2 . . . ? C1 Zr C3 C2 36.48(12) . . . . ? C1 Zr C3 C2 169.40(12) 2 . . . ? Cl1 Zr C3 C6 10.49(19) . . . . ? Cl1 Zr C3 C6 97.91(19) 2 . . . ? C4 Zr C3 C6 -121.2(3) . . . . ? C4 Zr C3 C6 -132.59(19) 2 . . . ? C5 Zr C3 C6 -159.6(2) . . . . ? C5 Zr C3 C6 -101.2(2) 2 . . . ? C3 Zr C3 C6 -127.9(2) 2 . . . ? C2 Zr C3 C6 123.5(3) . . . . ? C2 Zr C3 C6 -50.6(3) 2 . . . ? C1 Zr C3 C6 160.0(2) . . . . ? C1 Zr C3 C6 -67.0(2) 2 . . . ? C2 C3 C4 C5 2.5(2) . . . . ? C6 C3 C4 C5 -171.8(2) . . . . ? Zr C3 C4 C5 68.04(14) . . . . ? C2 C3 C4 Zr -65.58(16) . . . . ? C6 C3 C4 Zr 120.1(2) . . . . ? Cl1 Zr C4 C3 -48.09(13) . . . . ? Cl1 Zr C4 C3 57.23(16) 2 . . . ? C4 Zr C4 C3 171.10(16) 2 . . . ? C5 Zr C4 C3 113.64(19) . . . . ? C5 Zr C4 C3 -160.83(15) 2 . . . ? C3 Zr C4 C3 177.22(5) 2 . . . ? C2 Zr C4 C3 36.60(13) . . . . ? C2 Zr C4 C3 -141.19(13) 2 . . . ? C1 Zr C4 C3 76.75(14) . . . . ? C1 Zr C4 C3 -134.28(14) 2 . . . ? Cl1 Zr C4 C5 -161.73(12) . . . . ? Cl1 Zr C4 C5 -56.41(15) 2 . . . ? C4 Zr C4 C5 57.46(11) 2 . . . ? C5 Zr C4 C5 85.52(15) 2 . . . ? C3 Zr C4 C5 -113.64(19) . . . . ? C3 Zr C4 C5 63.57(16) 2 . . . ? C2 Zr C4 C5 -77.04(14) . . . . ? C2 Zr C4 C5 105.17(14) 2 . . . ? C1 Zr C4 C5 -36.89(12) . . . . ? C1 Zr C4 C5 112.08(13) 2 . . . ? C2 C1 C5 C4 -1.3(2) . . . . ? C9 C1 C5 C4 169.1(2) . . . . ? Zr C1 C5 C4 -66.61(15) . . . . ? C2 C1 C5 Zr 65.27(15) . . . . ? C9 C1 C5 Zr -124.3(2) . . . . ? C3 C4 C5 C1 -0.7(2) . . . . ? Zr C4 C5 C1 69.51(15) . . . . ? C3 C4 C5 Zr -70.19(15) . . . . ? Cl1 Zr C5 C1 -90.08(13) . . . . ? Cl1 Zr C5 C1 27.29(14) 2 . . . ? C4 Zr C5 C1 -114.41(18) . . . . ? C4 Zr C5 C1 123.97(14) 2 . . . ? C5 Zr C5 C1 157.87(17) 2 . . . ? C3 Zr C5 C1 -77.08(14) . . . . ? C3 Zr C5 C1 113.22(13) 2 . . . ? C2 Zr C5 C1 -37.10(12) . . . . ? C2 Zr C5 C1 142.22(12) 2 . . . ? C1 Zr C5 C1 170.12(8) 2 . . . ? Cl1 Zr C5 C4 24.32(15) . . . . ? Cl1 Zr C5 C4 141.69(11) 2 . . . ? C4 Zr C5 C4 -121.62(13) 2 . . . ? C5 Zr C5 C4 -87.73(14) 2 . . . ? C3 Zr C5 C4 37.32(12) . . . . ? C3 Zr C5 C4 -132.37(13) 2 . . . ? C2 Zr C5 C4 77.31(14) . . . . ? C2 Zr C5 C4 -103.37(14) 2 . . . ? C1 Zr C5 C4 114.41(18) . . . . ? C1 Zr C5 C4 -75.48(14) 2 . . . ? C4 C3 C6 C7 84.5(3) . . . . ? C2 C3 C6 C7 -88.7(3) . . . . ? Zr C3 C6 C7 175.25(18) . . . . ? C3 C6 C7 C8 -129.2(3) . . . . ? C5 C1 C9 C12 50.5(3) . . . . ? C2 C1 C9 C12 -141.1(3) . . . . ? Zr C1 C9 C12 -41.9(3) . . . . ? C5 C1 C9 C11 174.3(2) . . . . ? C2 C1 C9 C11 -17.3(4) . . . . ? Zr C1 C9 C11 81.9(3) . . . . ? C5 C1 C9 C10 -67.5(3) . . . . ? C2 C1 C9 C10 100.9(3) . . . . ? Zr C1 C9 C10 -159.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.337 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.062 # Attachment 'erk5063.cif' data_erk5063 _database_code_depnum_ccdc_archive 'CCDC 735246' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 Cl2 Zr' _chemical_formula_weight 456.58 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 monoclinic _symmetry_space_group_name_H-M P21/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 10.9542(2) _cell_length_b 7.4462(2) _cell_length_c 26.3865(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.954(1) _cell_angle_gamma 90.00 _cell_volume 2151.97(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3191 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8324 _exptl_absorpt_correction_T_max 0.9277 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14440 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.30 _reflns_number_total 4310 _reflns_number_gt 3519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Several crystals were tried, all of them are twinned. Remaining electron density is located close to Zr and Cl. ; _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^)+(0.0909P)^2^+16.1892P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4310 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.2017 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.24889(6) 0.82538(8) 0.39785(2) 0.0282(2) Uani 1 1 d . . . Cl1 Cl 0.24805(18) 1.1146(2) 0.44370(8) 0.0469(5) Uani 1 1 d . . . Cl2 Cl 0.25739(18) 0.9316(3) 0.31107(7) 0.0484(5) Uani 1 1 d . . . C1 C 0.0133(6) 0.8128(10) 0.3788(3) 0.0402(16) Uani 1 1 d . . . C2 C 0.0305(6) 0.8519(9) 0.4308(3) 0.0366(15) Uani 1 1 d . . . H2 H 0.0065 0.9592 0.4466 0.044 Uiso 1 1 calc R . . C3 C 0.0889(6) 0.7069(9) 0.4558(3) 0.0317(14) Uani 1 1 d . . . C4 C 0.1094(6) 0.5747(9) 0.4185(3) 0.0326(14) Uani 1 1 d . . . H4 H 0.1466 0.4625 0.4241 0.039 Uiso 1 1 calc R . . C5 C 0.0647(6) 0.6396(10) 0.3713(3) 0.0374(15) Uani 1 1 d . . . H5 H 0.0684 0.5784 0.3402 0.045 Uiso 1 1 calc R . . C6 C 0.1090(7) 0.6964(10) 0.5124(3) 0.0392(16) Uani 1 1 d . . . H6A H 0.0296 0.6862 0.5287 0.047 Uiso 1 1 calc R . . H6B H 0.1470 0.8086 0.5241 0.047 Uiso 1 1 calc R . . C7 C 0.1885(7) 0.5407(10) 0.5293(2) 0.0389(16) Uani 1 1 d . . . H7 H 0.1494 0.4342 0.5392 0.047 Uiso 1 1 calc R . . C8 C -0.0656(7) 0.9230(14) 0.3418(4) 0.059(2) Uani 1 1 d . . . C9A C -0.0330(9) 1.1232(13) 0.3437(4) 0.070(3) Uani 1 1 d . . . H9AA H 0.0461 1.1416 0.3285 0.104 Uiso 1 1 calc R . . H9AB H -0.0300 1.1633 0.3786 0.104 Uiso 1 1 calc R . . H9AC H -0.0944 1.1913 0.3250 0.104 Uiso 1 1 calc R . . C9B C -0.0565(10) 0.8544(17) 0.2876(4) 0.079(3) Uani 1 1 d . . . H9BA H 0.0270 0.8661 0.2764 0.119 Uiso 1 1 calc R . . H9BB H -0.1100 0.9243 0.2656 0.119 Uiso 1 1 calc R . . H9BC H -0.0806 0.7291 0.2863 0.119 Uiso 1 1 calc R . . C9C C -0.1993(9) 0.9003(19) 0.3603(5) 0.086(4) Uani 1 1 d . . . H9CA H -0.2537 0.9732 0.3394 0.129 Uiso 1 1 calc R . . H9CB H -0.2042 0.9384 0.3953 0.129 Uiso 1 1 calc R . . H9CC H -0.2231 0.7751 0.3575 0.129 Uiso 1 1 calc R . . C11 C 0.4307(6) 0.6227(9) 0.3754(3) 0.0346(14) Uani 1 1 d . . . C12 C 0.3852(5) 0.5704(8) 0.4230(2) 0.0274(13) Uani 1 1 d . . . H12 H 0.3473 0.4599 0.4299 0.033 Uiso 1 1 calc R . . C13 C 0.4052(6) 0.7093(9) 0.4586(2) 0.0315(14) Uani 1 1 d . . . C14 C 0.4634(6) 0.8501(9) 0.4326(3) 0.0343(14) Uani 1 1 d . . . H14 H 0.4892 0.9593 0.4471 0.041 Uiso 1 1 calc R . . C15 C 0.4767(6) 0.8003(9) 0.3813(3) 0.0358(15) Uani 1 1 d . . . H15 H 0.5100 0.8718 0.3556 0.043 Uiso 1 1 calc R . . C16 C 0.3833(6) 0.7026(9) 0.5153(2) 0.0349(15) Uani 1 1 d . . . H16A H 0.4623 0.6983 0.5333 0.042 Uiso 1 1 calc R . . H16B H 0.3418 0.8131 0.5256 0.042 Uiso 1 1 calc R . . C17 C 0.3081(7) 0.5441(9) 0.5311(2) 0.0358(15) Uani 1 1 d . . . H17 H 0.3493 0.4413 0.5430 0.043 Uiso 1 1 calc R . . C18 C 0.4431(7) 0.4990(11) 0.3302(3) 0.0439(17) Uani 1 1 d . . . C19A C 0.5264(9) 0.3410(13) 0.3463(4) 0.064(3) Uani 1 1 d . . . H19A H 0.4904 0.2781 0.3745 0.096 Uiso 1 1 calc R . . H19B H 0.6061 0.3867 0.3564 0.096 Uiso 1 1 calc R . . H19C H 0.5351 0.2590 0.3180 0.096 Uiso 1 1 calc R . . C19B C 0.5038(9) 0.5988(14) 0.2871(4) 0.065(3) Uani 1 1 d . . . H19D H 0.4535 0.7003 0.2769 0.098 Uiso 1 1 calc R . . H19E H 0.5131 0.5184 0.2585 0.098 Uiso 1 1 calc R . . H19F H 0.5834 0.6415 0.2983 0.098 Uiso 1 1 calc R . . C19C C 0.3195(8) 0.4223(12) 0.3121(3) 0.055(2) Uani 1 1 d . . . H19G H 0.2790 0.3656 0.3403 0.082 Uiso 1 1 calc R . . H19H H 0.3327 0.3341 0.2857 0.082 Uiso 1 1 calc R . . H19I H 0.2687 0.5187 0.2988 0.082 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 0.0329(4) 0.0212(3) 0.0305(3) 0.0014(2) 0.0043(2) -0.0005(2) Cl1 0.0558(12) 0.0225(8) 0.0625(12) -0.0077(7) 0.0062(9) -0.0001(7) Cl2 0.0536(11) 0.0534(11) 0.0383(9) 0.0153(8) 0.0064(8) 0.0043(9) C1 0.028(3) 0.044(4) 0.048(4) 0.002(3) 0.000(3) -0.004(3) C2 0.033(4) 0.030(3) 0.047(4) 0.002(3) 0.006(3) 0.002(3) C3 0.026(3) 0.033(3) 0.037(3) 0.005(3) 0.010(3) -0.002(3) C4 0.029(3) 0.025(3) 0.043(4) 0.000(3) 0.006(3) -0.001(3) C5 0.029(3) 0.037(4) 0.047(4) -0.008(3) 0.002(3) -0.004(3) C6 0.041(4) 0.039(4) 0.037(4) 0.004(3) 0.007(3) 0.004(3) C7 0.050(4) 0.036(4) 0.031(3) 0.009(3) 0.005(3) 0.000(3) C8 0.033(4) 0.077(6) 0.066(6) 0.013(5) -0.002(4) 0.010(4) C9A 0.065(6) 0.065(6) 0.079(7) 0.026(5) -0.003(5) 0.021(5) C9B 0.073(7) 0.106(9) 0.057(6) 0.002(6) -0.020(5) 0.015(6) C9C 0.040(5) 0.117(10) 0.102(9) 0.028(8) -0.010(5) 0.009(6) C11 0.032(3) 0.035(4) 0.037(4) -0.002(3) 0.006(3) 0.002(3) C12 0.022(3) 0.024(3) 0.036(3) 0.003(2) 0.002(2) -0.001(2) C13 0.032(3) 0.029(3) 0.034(3) -0.001(3) 0.000(3) 0.002(3) C14 0.033(4) 0.029(3) 0.041(4) -0.006(3) 0.002(3) -0.007(3) C15 0.034(4) 0.033(4) 0.040(4) 0.001(3) 0.007(3) -0.004(3) C16 0.038(4) 0.035(4) 0.031(3) -0.001(3) 0.000(3) -0.001(3) C17 0.047(4) 0.034(4) 0.027(3) 0.003(3) -0.001(3) 0.003(3) C18 0.036(4) 0.048(4) 0.047(4) -0.001(3) 0.006(3) 0.006(3) C19A 0.071(6) 0.063(6) 0.058(5) -0.012(4) -0.002(4) 0.030(5) C19B 0.073(6) 0.069(6) 0.055(5) -0.001(5) 0.024(5) 0.001(5) C19C 0.056(5) 0.054(5) 0.055(5) -0.018(4) 0.002(4) 0.001(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 Cl2 2.4259(18) . ? Zr Cl1 2.4705(18) . ? Zr C4 2.478(6) . ? Zr C13 2.481(6) . ? Zr C12 2.498(6) . ? Zr C3 2.506(6) . ? Zr C14 2.515(7) . ? Zr C5 2.535(7) . ? Zr C15 2.547(7) . ? Zr C2 2.567(7) . ? Zr C11 2.575(7) . ? Zr C1 2.623(7) . ? C1 C2 1.414(10) . ? C1 C5 1.423(10) . ? C1 C8 1.530(11) . ? C2 C3 1.413(9) . ? C2 H2 0.9400 . ? C3 C4 1.413(9) . ? C3 C6 1.507(10) . ? C4 C5 1.416(10) . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 C7 1.513(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C17 1.311(10) . ? C7 H7 0.9400 . ? C8 C9B 1.524(14) . ? C8 C9A 1.533(14) . ? C8 C9C 1.560(13) . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C9A H9AC 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C9B H9BC 0.9700 . ? C9C H9CA 0.9700 . ? C9C H9CB 0.9700 . ? C9C H9CC 0.9700 . ? C11 C12 1.413(9) . ? C11 C15 1.423(9) . ? C11 C18 1.516(10) . ? C12 C13 1.411(9) . ? C12 H12 0.9400 . ? C13 C14 1.411(9) . ? C13 C16 1.522(9) . ? C14 C15 1.413(10) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 C17 1.502(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 H17 0.9400 . ? C18 C19B 1.521(12) . ? C18 C19C 1.539(11) . ? C18 C19A 1.544(11) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19A H19C 0.9700 . ? C19B H19D 0.9700 . ? C19B H19E 0.9700 . ? C19B H19F 0.9700 . ? C19C H19G 0.9700 . ? C19C H19H 0.9700 . ? C19C H19I 0.9700 . ? 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 Cl2 Zr Cl1 100.29(7) . . ? Cl2 Zr C4 119.10(17) . . ? Cl1 Zr C4 122.80(16) . . ? Cl2 Zr C13 133.35(16) . . ? Cl1 Zr C13 89.75(16) . . ? C4 Zr C13 91.0(2) . . ? Cl2 Zr C12 117.81(15) . . ? Cl1 Zr C12 122.65(15) . . ? C4 Zr C12 74.7(2) . . ? C13 Zr C12 32.9(2) . . ? Cl2 Zr C3 136.82(17) . . ? Cl1 Zr C3 89.98(16) . . ? C4 Zr C3 32.9(2) . . ? C13 Zr C3 88.0(2) . . ? C12 Zr C3 89.5(2) . . ? Cl2 Zr C14 105.66(17) . . ? Cl1 Zr C14 76.62(16) . . ? C4 Zr C14 123.4(2) . . ? C13 Zr C14 32.8(2) . . ? C12 Zr C14 53.7(2) . . ? C3 Zr C14 117.5(2) . . ? Cl2 Zr C5 87.69(18) . . ? Cl1 Zr C5 126.99(17) . . ? C4 Zr C5 32.8(2) . . ? C13 Zr C5 121.7(2) . . ? C12 Zr C5 97.4(2) . . ? C3 Zr C5 54.2(2) . . ? C14 Zr C5 151.1(2) . . ? Cl2 Zr C15 78.99(17) . . ? Cl1 Zr C15 99.17(16) . . ? C4 Zr C15 126.3(2) . . ? C13 Zr C15 54.4(2) . . ? C12 Zr C15 53.6(2) . . ? C3 Zr C15 140.9(2) . . ? C14 Zr C15 32.4(2) . . ? C5 Zr C15 133.6(2) . . ? Cl2 Zr C2 110.22(17) . . ? Cl1 Zr C2 75.86(17) . . ? C4 Zr C2 53.3(2) . . ? C13 Zr C2 116.4(2) . . ? C12 Zr C2 121.6(2) . . ? C3 Zr C2 32.3(2) . . ? C14 Zr C2 137.8(2) . . ? C5 Zr C2 52.7(2) . . ? C15 Zr C2 170.0(2) . . ? Cl2 Zr C11 86.12(16) . . ? Cl1 Zr C11 129.24(17) . . ? C4 Zr C11 95.2(2) . . ? C13 Zr C11 54.3(2) . . ? C12 Zr C11 32.3(2) . . ? C3 Zr C11 119.0(2) . . ? C14 Zr C11 53.5(2) . . ? C5 Zr C11 103.4(2) . . ? C15 Zr C11 32.3(2) . . ? C2 Zr C11 148.4(2) . . ? Cl2 Zr C1 83.31(17) . . ? Cl1 Zr C1 96.52(18) . . ? C4 Zr C1 53.6(2) . . ? C13 Zr C1 141.1(2) . . ? C12 Zr C1 127.3(2) . . ? C3 Zr C1 53.7(2) . . ? C14 Zr C1 169.4(2) . . ? C5 Zr C1 32.0(2) . . ? C15 Zr C1 158.1(2) . . ? C2 Zr C1 31.6(2) . . ? C11 Zr C1 134.2(2) . . ? C2 C1 C5 106.0(6) . . ? C2 C1 C8 125.0(7) . . ? C5 C1 C8 128.2(7) . . ? C2 C1 Zr 72.0(4) . . ? C5 C1 Zr 70.6(4) . . ? C8 C1 Zr 130.2(5) . . ? C3 C2 C1 110.4(6) . . ? C3 C2 Zr 71.5(4) . . ? C1 C2 Zr 76.4(4) . . ? C3 C2 H2 124.8 . . ? C1 C2 H2 124.8 . . ? Zr C2 H2 119.0 . . ? C2 C3 C4 106.5(6) . . ? C2 C3 C6 124.0(6) . . ? C4 C3 C6 129.2(6) . . ? C2 C3 Zr 76.2(4) . . ? C4 C3 Zr 72.5(4) . . ? C6 C3 Zr 122.0(5) . . ? C3 C4 C5 108.6(6) . . ? C3 C4 Zr 74.6(4) . . ? C5 C4 Zr 75.8(4) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Zr C4 H4 115.9 . . ? C4 C5 C1 108.6(6) . . ? C4 C5 Zr 71.4(4) . . ? C1 C5 Zr 77.4(4) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Zr C5 H5 117.4 . . ? C3 C6 C7 113.9(6) . . ? C3 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? C3 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C17 C7 C6 124.5(7) . . ? C17 C7 H7 117.8 . . ? C6 C7 H7 117.8 . . ? C9B C8 C1 111.9(8) . . ? C9B C8 C9A 109.7(9) . . ? C1 C8 C9A 111.9(8) . . ? C9B C8 C9C 109.4(9) . . ? C1 C8 C9C 105.4(7) . . ? C9A C8 C9C 108.3(9) . . ? C8 C9A H9AA 109.5 . . ? C8 C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C8 C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C8 C9B H9BA 109.5 . . ? C8 C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C8 C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C8 C9C H9CA 109.5 . . ? C8 C9C H9CB 109.5 . . ? H9CA C9C H9CB 109.5 . . ? C8 C9C H9CC 109.5 . . ? H9CA C9C H9CC 109.5 . . ? H9CB C9C H9CC 109.5 . . ? C12 C11 C15 106.8(6) . . ? C12 C11 C18 124.8(6) . . ? C15 C11 C18 127.9(6) . . ? C12 C11 Zr 70.9(4) . . ? C15 C11 Zr 72.8(4) . . ? C18 C11 Zr 128.1(5) . . ? C13 C12 C11 109.6(6) . . ? C13 C12 Zr 72.8(4) . . ? C11 C12 Zr 76.8(4) . . ? C13 C12 H12 125.2 . . ? C11 C12 H12 125.2 . . ? Zr C12 H12 116.9 . . ? C14 C13 C12 106.8(6) . . ? C14 C13 C16 125.6(6) . . ? C12 C13 C16 127.2(6) . . ? C14 C13 Zr 74.9(4) . . ? C12 C13 Zr 74.2(4) . . ? C16 C13 Zr 122.0(4) . . ? C13 C14 C15 109.0(6) . . ? C13 C14 Zr 72.3(4) . . ? C15 C14 Zr 75.1(4) . . ? C13 C14 H14 125.5 . . ? C15 C14 H14 125.5 . . ? Zr C14 H14 119.0 . . ? C14 C15 C11 107.8(6) . . ? C14 C15 Zr 72.5(4) . . ? C11 C15 Zr 75.0(4) . . ? C14 C15 H15 126.1 . . ? C11 C15 H15 126.1 . . ? Zr C15 H15 118.4 . . ? C17 C16 C13 113.3(6) . . ? C17 C16 H16A 108.9 . . ? C13 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C13 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C7 C17 C16 123.9(6) . . ? C7 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C11 C18 C19B 109.8(7) . . ? C11 C18 C19C 112.3(6) . . ? C19B C18 C19C 110.0(7) . . ? C11 C18 C19A 107.9(6) . . ? C19B C18 C19A 108.3(7) . . ? C19C C18 C19A 108.4(7) . . ? C18 C19A H19A 109.5 . . ? C18 C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18 C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18 C19B H19D 109.5 . . ? C18 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C18 C19C H19G 109.5 . . ? C18 C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? C18 C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Zr C1 C2 -148.7(4) . . . . ? Cl1 Zr C1 C2 -49.1(4) . . . . ? C4 Zr C1 C2 77.3(4) . . . . ? C13 Zr C1 C2 48.6(6) . . . . ? C12 Zr C1 C2 91.2(5) . . . . ? C3 Zr C1 C2 36.1(4) . . . . ? C14 Zr C1 C2 -0.1(15) . . . . ? C5 Zr C1 C2 114.9(6) . . . . ? C15 Zr C1 C2 175.2(5) . . . . ? C11 Zr C1 C2 133.3(4) . . . . ? Cl2 Zr C1 C5 96.4(4) . . . . ? Cl1 Zr C1 C5 -164.0(4) . . . . ? C4 Zr C1 C5 -37.6(4) . . . . ? C13 Zr C1 C5 -66.2(6) . . . . ? C12 Zr C1 C5 -23.7(5) . . . . ? C3 Zr C1 C5 -78.8(5) . . . . ? C14 Zr C1 C5 -115.0(12) . . . . ? C15 Zr C1 C5 60.3(8) . . . . ? C2 Zr C1 C5 -114.9(6) . . . . ? C11 Zr C1 C5 18.4(6) . . . . ? Cl2 Zr C1 C8 -27.8(7) . . . . ? Cl1 Zr C1 C8 71.9(7) . . . . ? C4 Zr C1 C8 -161.7(8) . . . . ? C13 Zr C1 C8 169.6(7) . . . . ? C12 Zr C1 C8 -147.8(7) . . . . ? C3 Zr C1 C8 157.1(8) . . . . ? C14 Zr C1 C8 120.8(12) . . . . ? C5 Zr C1 C8 -124.1(9) . . . . ? C15 Zr C1 C8 -63.8(10) . . . . ? C2 Zr C1 C8 121.0(9) . . . . ? C11 Zr C1 C8 -105.7(8) . . . . ? C5 C1 C2 C3 -1.1(8) . . . . ? C8 C1 C2 C3 169.0(7) . . . . ? Zr C1 C2 C3 -64.0(5) . . . . ? C5 C1 C2 Zr 62.9(5) . . . . ? C8 C1 C2 Zr -127.0(7) . . . . ? Cl2 Zr C2 C3 150.6(4) . . . . ? Cl1 Zr C2 C3 -113.4(4) . . . . ? C4 Zr C2 C3 38.8(4) . . . . ? C13 Zr C2 C3 -30.9(5) . . . . ? C12 Zr C2 C3 6.5(5) . . . . ? C14 Zr C2 C3 -62.7(5) . . . . ? C5 Zr C2 C3 80.2(4) . . . . ? C15 Zr C2 C3 -52.4(14) . . . . ? C11 Zr C2 C3 33.2(6) . . . . ? C1 Zr C2 C3 117.3(6) . . . . ? Cl2 Zr C2 C1 33.3(4) . . . . ? Cl1 Zr C2 C1 129.3(4) . . . . ? C4 Zr C2 C1 -78.5(5) . . . . ? C13 Zr C2 C1 -148.2(4) . . . . ? C12 Zr C2 C1 -110.8(4) . . . . ? C3 Zr C2 C1 -117.3(6) . . . . ? C14 Zr C2 C1 180.0(4) . . . . ? C5 Zr C2 C1 -37.1(4) . . . . ? C15 Zr C2 C1 -169.7(11) . . . . ? C11 Zr C2 C1 -84.1(6) . . . . ? C1 C2 C3 C4 0.4(8) . . . . ? Zr C2 C3 C4 -66.7(4) . . . . ? C1 C2 C3 C6 -173.3(6) . . . . ? Zr C2 C3 C6 119.6(6) . . . . ? C1 C2 C3 Zr 67.1(5) . . . . ? Cl2 Zr C3 C2 -42.3(5) . . . . ? Cl1 Zr C3 C2 62.8(4) . . . . ? C4 Zr C3 C2 -112.5(6) . . . . ? C13 Zr C3 C2 152.6(4) . . . . ? C12 Zr C3 C2 -174.5(4) . . . . ? C14 Zr C3 C2 137.7(4) . . . . ? C5 Zr C3 C2 -75.1(4) . . . . ? C15 Zr C3 C2 167.5(4) . . . . ? C11 Zr C3 C2 -160.8(4) . . . . ? C1 Zr C3 C2 -35.3(4) . . . . ? Cl2 Zr C3 C4 70.3(4) . . . . ? Cl1 Zr C3 C4 175.4(4) . . . . ? C13 Zr C3 C4 -94.9(4) . . . . ? C12 Zr C3 C4 -62.0(4) . . . . ? C14 Zr C3 C4 -109.8(4) . . . . ? C5 Zr C3 C4 37.5(4) . . . . ? C15 Zr C3 C4 -80.0(5) . . . . ? C2 Zr C3 C4 112.5(6) . . . . ? C11 Zr C3 C4 -48.3(5) . . . . ? C1 Zr C3 C4 77.3(4) . . . . ? Cl2 Zr C3 C6 -164.0(4) . . . . ? Cl1 Zr C3 C6 -58.9(5) . . . . ? C4 Zr C3 C6 125.7(7) . . . . ? C13 Zr C3 C6 30.9(5) . . . . ? C12 Zr C3 C6 63.8(5) . . . . ? C14 Zr C3 C6 16.0(6) . . . . ? C5 Zr C3 C6 163.2(6) . . . . ? C15 Zr C3 C6 45.7(7) . . . . ? C2 Zr C3 C6 -121.7(7) . . . . ? C11 Zr C3 C6 77.4(6) . . . . ? C1 Zr C3 C6 -157.0(6) . . . . ? C2 C3 C4 C5 0.4(7) . . . . ? C6 C3 C4 C5 173.8(7) . . . . ? Zr C3 C4 C5 -68.9(5) . . . . ? C2 C3 C4 Zr 69.3(4) . . . . ? C6 C3 C4 Zr -117.4(7) . . . . ? Cl2 Zr C4 C3 -132.5(4) . . . . ? Cl1 Zr C4 C3 -5.5(5) . . . . ? C13 Zr C4 C3 84.8(4) . . . . ? C12 Zr C4 C3 113.8(4) . . . . ? C14 Zr C4 C3 90.0(4) . . . . ? C5 Zr C4 C3 -114.2(6) . . . . ? C15 Zr C4 C3 129.6(4) . . . . ? C2 Zr C4 C3 -38.0(4) . . . . ? C11 Zr C4 C3 139.0(4) . . . . ? C1 Zr C4 C3 -77.6(4) . . . . ? Cl2 Zr C4 C5 -18.3(4) . . . . ? Cl1 Zr C4 C5 108.7(4) . . . . ? C13 Zr C4 C5 -160.9(4) . . . . ? C12 Zr C4 C5 -131.9(4) . . . . ? C3 Zr C4 C5 114.2(6) . . . . ? C14 Zr C4 C5 -155.8(4) . . . . ? C15 Zr C4 C5 -116.2(4) . . . . ? C2 Zr C4 C5 76.2(4) . . . . ? C11 Zr C4 C5 -106.7(4) . . . . ? C1 Zr C4 C5 36.6(4) . . . . ? C3 C4 C5 C1 -1.1(8) . . . . ? Zr C4 C5 C1 -69.2(5) . . . . ? C3 C4 C5 Zr 68.0(4) . . . . ? C2 C1 C5 C4 1.3(8) . . . . ? C8 C1 C5 C4 -168.3(7) . . . . ? Zr C1 C5 C4 65.2(5) . . . . ? C2 C1 C5 Zr -63.8(5) . . . . ? C8 C1 C5 Zr 126.5(8) . . . . ? Cl2 Zr C5 C4 164.1(4) . . . . ? Cl1 Zr C5 C4 -94.8(4) . . . . ? C13 Zr C5 C4 22.6(5) . . . . ? C12 Zr C5 C4 46.3(4) . . . . ? C3 Zr C5 C4 -37.7(4) . . . . ? C14 Zr C5 C4 45.1(7) . . . . ? C15 Zr C5 C4 91.7(5) . . . . ? C2 Zr C5 C4 -78.2(4) . . . . ? C11 Zr C5 C4 78.6(4) . . . . ? C1 Zr C5 C4 -114.8(6) . . . . ? Cl2 Zr C5 C1 -81.1(4) . . . . ? Cl1 Zr C5 C1 20.1(5) . . . . ? C4 Zr C5 C1 114.8(6) . . . . ? C13 Zr C5 C1 137.4(4) . . . . ? C12 Zr C5 C1 161.2(4) . . . . ? C3 Zr C5 C1 77.2(5) . . . . ? C14 Zr C5 C1 159.9(5) . . . . ? C15 Zr C5 C1 -153.5(4) . . . . ? C2 Zr C5 C1 36.7(4) . . . . ? C11 Zr C5 C1 -166.5(4) . . . . ? C2 C3 C6 C7 -172.1(6) . . . . ? C4 C3 C6 C7 15.6(10) . . . . ? Zr C3 C6 C7 -77.3(7) . . . . ? C3 C6 C7 C17 85.1(9) . . . . ? C2 C1 C8 C9B 175.2(8) . . . . ? C5 C1 C8 C9B -16.9(12) . . . . ? Zr C1 C8 C9B 79.6(10) . . . . ? C2 C1 C8 C9A 51.6(11) . . . . ? C5 C1 C8 C9A -140.5(9) . . . . ? Zr C1 C8 C9A -44.0(11) . . . . ? C2 C1 C8 C9C -65.9(11) . . . . ? C5 C1 C8 C9C 102.0(10) . . . . ? Zr C1 C8 C9C -161.6(7) . . . . ? Cl2 Zr C11 C12 -169.2(4) . . . . ? Cl1 Zr C11 C12 90.7(4) . . . . ? C4 Zr C11 C12 -50.3(4) . . . . ? C13 Zr C11 C12 37.1(4) . . . . ? C3 Zr C11 C12 -26.2(5) . . . . ? C14 Zr C11 C12 78.0(4) . . . . ? C5 Zr C11 C12 -82.5(4) . . . . ? C15 Zr C11 C12 115.3(6) . . . . ? C2 Zr C11 C12 -45.8(6) . . . . ? C1 Zr C11 C12 -92.4(5) . . . . ? Cl2 Zr C11 C15 75.5(4) . . . . ? Cl1 Zr C11 C15 -24.7(5) . . . . ? C4 Zr C11 C15 -165.6(4) . . . . ? C13 Zr C11 C15 -78.2(4) . . . . ? C12 Zr C11 C15 -115.3(6) . . . . ? C3 Zr C11 C15 -141.6(4) . . . . ? C14 Zr C11 C15 -37.3(4) . . . . ? C5 Zr C11 C15 162.1(4) . . . . ? C2 Zr C11 C15 -161.1(4) . . . . ? C1 Zr C11 C15 152.2(4) . . . . ? Cl2 Zr C11 C18 -49.6(6) . . . . ? Cl1 Zr C11 C18 -149.7(5) . . . . ? C4 Zr C11 C18 69.3(6) . . . . ? C13 Zr C11 C18 156.8(7) . . . . ? C12 Zr C11 C18 119.6(8) . . . . ? C3 Zr C11 C18 93.4(6) . . . . ? C14 Zr C11 C18 -162.3(7) . . . . ? C5 Zr C11 C18 37.1(7) . . . . ? C15 Zr C11 C18 -125.0(8) . . . . ? C2 Zr C11 C18 73.8(8) . . . . ? C1 Zr C11 C18 27.2(8) . . . . ? C15 C11 C12 C13 -1.7(7) . . . . ? C18 C11 C12 C13 170.2(6) . . . . ? Zr C11 C12 C13 -66.1(4) . . . . ? C15 C11 C12 Zr 64.4(5) . . . . ? C18 C11 C12 Zr -123.6(7) . . . . ? Cl2 Zr C12 C13 127.8(3) . . . . ? Cl1 Zr C12 C13 2.5(4) . . . . ? C4 Zr C12 C13 -117.0(4) . . . . ? C3 Zr C12 C13 -87.1(4) . . . . ? C14 Zr C12 C13 38.3(4) . . . . ? C5 Zr C12 C13 -140.9(4) . . . . ? C15 Zr C12 C13 78.8(4) . . . . ? C2 Zr C12 C13 -90.6(4) . . . . ? C11 Zr C12 C13 115.6(5) . . . . ? C1 Zr C12 C13 -128.5(4) . . . . ? Cl2 Zr C12 C11 12.2(4) . . . . ? Cl1 Zr C12 C11 -113.1(4) . . . . ? C4 Zr C12 C11 127.4(4) . . . . ? C13 Zr C12 C11 -115.6(5) . . . . ? C3 Zr C12 C11 157.2(4) . . . . ? C14 Zr C12 C11 -77.3(4) . . . . ? C5 Zr C12 C11 103.5(4) . . . . ? C15 Zr C12 C11 -36.8(4) . . . . ? C2 Zr C12 C11 153.8(4) . . . . ? C1 Zr C12 C11 115.8(4) . . . . ? C11 C12 C13 C14 0.3(7) . . . . ? Zr C12 C13 C14 -68.5(5) . . . . ? C11 C12 C13 C16 -172.8(6) . . . . ? Zr C12 C13 C16 118.4(7) . . . . ? C11 C12 C13 Zr 68.7(5) . . . . ? Cl2 Zr C13 C14 38.8(5) . . . . ? Cl1 Zr C13 C14 -65.2(4) . . . . ? C4 Zr C13 C14 172.0(4) . . . . ? C12 Zr C13 C14 112.7(5) . . . . ? C3 Zr C13 C14 -155.1(4) . . . . ? C5 Zr C13 C14 160.0(4) . . . . ? C15 Zr C13 C14 36.3(4) . . . . ? C2 Zr C13 C14 -139.2(4) . . . . ? C11 Zr C13 C14 76.3(4) . . . . ? C1 Zr C13 C14 -165.2(4) . . . . ? Cl2 Zr C13 C12 -73.9(4) . . . . ? Cl1 Zr C13 C12 -177.9(4) . . . . ? C4 Zr C13 C12 59.3(4) . . . . ? C3 Zr C13 C12 92.1(4) . . . . ? C14 Zr C13 C12 -112.7(5) . . . . ? C5 Zr C13 C12 47.3(4) . . . . ? C15 Zr C13 C12 -76.4(4) . . . . ? C2 Zr C13 C12 108.1(4) . . . . ? C11 Zr C13 C12 -36.4(4) . . . . ? C1 Zr C13 C12 82.0(5) . . . . ? Cl2 Zr C13 C16 161.7(4) . . . . ? Cl1 Zr C13 C16 57.7(5) . . . . ? C4 Zr C13 C16 -65.1(5) . . . . ? C12 Zr C13 C16 -124.4(7) . . . . ? C3 Zr C13 C16 -32.3(5) . . . . ? C14 Zr C13 C16 122.9(7) . . . . ? C5 Zr C13 C16 -77.1(6) . . . . ? C15 Zr C13 C16 159.2(6) . . . . ? C2 Zr C13 C16 -16.3(6) . . . . ? C11 Zr C13 C16 -160.8(6) . . . . ? C1 Zr C13 C16 -42.4(7) . . . . ? C12 C13 C14 C15 1.3(8) . . . . ? C16 C13 C14 C15 174.6(6) . . . . ? Zr C13 C14 C15 -66.7(5) . . . . ? C12 C13 C14 Zr 68.0(4) . . . . ? C16 C13 C14 Zr -118.8(7) . . . . ? Cl2 Zr C14 C13 -151.7(3) . . . . ? Cl1 Zr C14 C13 111.1(4) . . . . ? C4 Zr C14 C13 -9.5(5) . . . . ? C12 Zr C14 C13 -38.5(4) . . . . ? C3 Zr C14 C13 28.3(4) . . . . ? C5 Zr C14 C13 -36.9(6) . . . . ? C15 Zr C14 C13 -116.0(6) . . . . ? C2 Zr C14 C13 60.7(5) . . . . ? C11 Zr C14 C13 -78.9(4) . . . . ? C1 Zr C14 C13 60.8(13) . . . . ? Cl2 Zr C14 C15 -35.7(4) . . . . ? Cl1 Zr C14 C15 -132.9(4) . . . . ? C4 Zr C14 C15 106.5(4) . . . . ? C13 Zr C14 C15 116.0(6) . . . . ? C12 Zr C14 C15 77.5(4) . . . . ? C3 Zr C14 C15 144.3(4) . . . . ? C5 Zr C14 C15 79.1(6) . . . . ? C2 Zr C14 C15 176.7(4) . . . . ? C11 Zr C14 C15 37.1(4) . . . . ? C1 Zr C14 C15 176.8(11) . . . . ? C13 C14 C15 C11 -2.4(8) . . . . ? Zr C14 C15 C11 -67.2(5) . . . . ? C13 C14 C15 Zr 64.8(5) . . . . ? C12 C11 C15 C14 2.5(8) . . . . ? C18 C11 C15 C14 -169.1(7) . . . . ? Zr C11 C15 C14 65.6(5) . . . . ? C12 C11 C15 Zr -63.1(4) . . . . ? C18 C11 C15 Zr 125.3(7) . . . . ? Cl2 Zr C15 C14 145.0(4) . . . . ? Cl1 Zr C15 C14 46.2(4) . . . . ? C4 Zr C15 C14 -96.8(4) . . . . ? C13 Zr C15 C14 -36.8(4) . . . . ? C12 Zr C15 C14 -77.8(4) . . . . ? C3 Zr C15 C14 -55.2(5) . . . . ? C5 Zr C15 C14 -139.0(4) . . . . ? C2 Zr C15 C14 -13.0(15) . . . . ? C11 Zr C15 C14 -114.6(6) . . . . ? C1 Zr C15 C14 -178.4(5) . . . . ? Cl2 Zr C15 C11 -100.3(4) . . . . ? Cl1 Zr C15 C11 160.9(4) . . . . ? C4 Zr C15 C11 17.8(5) . . . . ? C13 Zr C15 C11 77.8(4) . . . . ? C12 Zr C15 C11 36.8(4) . . . . ? C3 Zr C15 C11 59.5(5) . . . . ? C14 Zr C15 C11 114.6(6) . . . . ? C5 Zr C15 C11 -24.3(6) . . . . ? C2 Zr C15 C11 101.6(13) . . . . ? C1 Zr C15 C11 -63.8(8) . . . . ? C14 C13 C16 C17 174.3(6) . . . . ? C12 C13 C16 C17 -13.8(10) . . . . ? Zr C13 C16 C17 80.3(7) . . . . ? C6 C7 C17 C16 -1.6(11) . . . . ? C13 C16 C17 C7 -83.8(8) . . . . ? C12 C11 C18 C19B -175.9(7) . . . . ? C15 C11 C18 C19B -5.7(11) . . . . ? Zr C11 C18 C19B 92.0(7) . . . . ? C12 C11 C18 C19C 61.3(9) . . . . ? C15 C11 C18 C19C -128.5(8) . . . . ? Zr C11 C18 C19C -30.8(9) . . . . ? C12 C11 C18 C19A -58.1(9) . . . . ? C15 C11 C18 C19A 112.2(9) . . . . ? Zr C11 C18 C19A -150.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.144 _refine_diff_density_min -0.904 _refine_diff_density_rms 0.147