# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address H.Braunschweig ; Institut fuer Anorganische Chemie Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg, Germany ; M.Friedrich ; Institut fuer Anorganische Chemie Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg, Germany ; T.Kupfer ; Institut fuer Anorganische Chemie Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg, Germany ; K.Radacki ; Institut fuer Anorganische Chemie Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg, Germany ; _publ_contact_author_address ; Institut fuer Anorganische Chemie Universitaet Wuerzburg Am Hubland 97074 Wuerzburg, Germany ; _publ_contact_author_email H.Braunschweig@mail.uni-wuerzburg.de _publ_contact_author_fax +49-931-31-84623 _publ_contact_author_phone +49-931-31-85260 #TrackingRef '- 1.cif' # 1. Submission Details _publ_contact_author_name 'Prof. Dr. Holger Braunschweig' _publ_section_title ;Heteroleptic [1]Zirconametalloarenophanes: Potential Precursors to Metal-enriched Metallopolymers ; data_kr397 _database_code_depnum_ccdc_archive 'CCDC 804814' _publ_section_abstract ;[1]Zirconametalloarenophanes derived from heteroleptic sandwich precursors, i.e. [Cr(C5H4)ZrCp*2(C7H6)] and [Mn(C5H4)ZrCp*2(C6H5)] (Cp = C5H4tBu) have been isolated for the first time and fully characterized both in solution and in the solid state. These species represent potential precursors en route to metal-enriched metallopolymers by ROP. In addition, the missing crystal structure of the [Cr(C6H6)2] analogue has been determined. The X-ray diffraction studies substantiated the presence of zirconium-bridged ansa-complexes, and revealed a rather low degree of molecular ring strain. Details on the electronic structure were assessed by means of UV-visible spectroscopy in solution and time-dependent DFT calculations. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 Cr Zr' _chemical_formula_sum 'C30 H36 Cr Zr' _chemical_formula_weight 539.81 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' Cr Cr 0.3209 0.6236 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 16.329(3) _cell_length_b 19.239(3) _cell_length_c 7.3960(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.846(7) _cell_angle_gamma 90.00 _cell_volume 2301.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9316 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.35 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8301 _exptl_absorpt_correction_T_max 0.9633 _exptl_absorpt_process_details 'Sadabs 2008/1 (Brucker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39152 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2865 _reflns_number_gt 2721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 ver. 2008.3 (Bruker AXS)' _computing_cell_refinement 'Saint+ ver. 7.53A (Bruker AXS)' _computing_data_reduction 'Saint+ ver. 7.53A (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP ver. 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0386P)^2^+5.5929P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2865 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Cr1 Cr 0.0000 0.340483(18) 0.7500 0.00838(9) Uani 1 2 d S . . C1_1 C 0.05544(10) 0.26483(8) 0.5941(2) 0.0111(3) Uani 1 1 d . . . C2_1 C 0.11902(10) 0.30564(9) 0.6975(2) 0.0119(3) Uani 1 1 d . . . H2_1 H 0.1631 0.2821 0.7695 0.014 Uiso 1 1 calc R . . C3_1 C 0.11929(10) 0.37930(9) 0.6976(2) 0.0136(3) Uani 1 1 d . . . H3_1 H 0.1616 0.4039 0.7723 0.016 Uiso 1 1 calc R . . C4_1 C 0.05673(11) 0.41597(9) 0.5869(2) 0.0141(3) Uani 1 1 d . . . H4_1 H 0.0555 0.4653 0.5890 0.017 Uiso 1 1 calc R . . C5_1 C -0.00400(10) 0.37844(9) 0.4729(2) 0.0128(3) Uani 1 1 d . . . H5_1 H -0.0455 0.4026 0.3947 0.015 Uiso 1 1 calc R . . C6_1 C -0.00338(10) 0.30488(9) 0.4746(2) 0.0119(3) Uani 1 1 d . . . H6_1 H -0.0437 0.2809 0.3930 0.014 Uiso 1 1 calc R . . Zr1 Zr 0.0000 0.176221(10) 0.7500 0.00727(8) Uani 1 2 d S . . C1_2 C 0.14921(10) 0.12086(8) 0.8290(2) 0.0105(3) Uani 1 1 d . . . C2_2 C 0.14050(10) 0.17090(8) 0.9672(2) 0.0110(3) Uani 1 1 d . . . H2_2 H 0.1726 0.2120 0.9892 0.013 Uiso 1 1 calc R . . C3_2 C 0.07653(10) 0.14979(9) 1.0665(2) 0.0122(3) Uani 1 1 d . . . H3_2 H 0.0587 0.1738 1.1664 0.015 Uiso 1 1 calc R . . C4_2 C 0.04407(10) 0.08671(9) 0.9904(2) 0.0123(3) Uani 1 1 d . . . H4_2 H 0.0002 0.0607 1.0294 0.015 Uiso 1 1 calc R . . C5_2 C 0.08865(10) 0.06900(8) 0.8452(2) 0.0118(3) Uani 1 1 d . . . H5_2 H 0.0795 0.0288 0.7705 0.014 Uiso 1 1 calc R . . C6_2 C 0.21719(10) 0.11491(8) 0.7070(2) 0.0117(3) Uani 1 1 d . . . C7_2 C 0.26007(11) 0.04399(9) 0.7443(3) 0.0184(4) Uani 1 1 d . . . H7A_2 H 0.2822 0.0405 0.8740 0.028 Uiso 1 1 calc R . . H7B_2 H 0.3053 0.0397 0.6705 0.028 Uiso 1 1 calc R . . H7C_2 H 0.2199 0.0066 0.7122 0.028 Uiso 1 1 calc R . . C8_2 C 0.28289(11) 0.17167(9) 0.7503(3) 0.0158(3) Uani 1 1 d . . . H8A_2 H 0.3042 0.1705 0.8808 0.024 Uiso 1 1 calc R . . H8B_2 H 0.2581 0.2172 0.7189 0.024 Uiso 1 1 calc R . . H8C_2 H 0.3283 0.1635 0.6790 0.024 Uiso 1 1 calc R . . C9_2 C 0.18253(11) 0.11902(10) 0.5041(2) 0.0164(3) Uani 1 1 d . . . H9A_2 H 0.2278 0.1143 0.4305 0.025 Uiso 1 1 calc R . . H9B_2 H 0.1552 0.1640 0.4784 0.025 Uiso 1 1 calc R . . H9C_2 H 0.1425 0.0815 0.4736 0.025 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 Cr1 0.00891(18) 0.00729(17) 0.00923(18) 0.000 0.00228(13) 0.000 C1_1 0.0124(7) 0.0100(7) 0.0119(8) -0.0002(6) 0.0055(6) 0.0008(6) C2_1 0.0102(7) 0.0124(7) 0.0136(8) 0.0015(6) 0.0040(6) 0.0006(6) C3_1 0.0123(7) 0.0133(8) 0.0158(8) 0.0001(6) 0.0046(6) -0.0032(6) C4_1 0.0162(8) 0.0092(7) 0.0181(8) 0.0026(6) 0.0061(6) -0.0010(6) C5_1 0.0127(7) 0.0146(8) 0.0114(7) 0.0043(6) 0.0033(6) 0.0013(6) C6_1 0.0132(7) 0.0147(7) 0.0083(7) 0.0001(6) 0.0033(6) -0.0004(6) Zr1 0.00820(11) 0.00659(11) 0.00708(12) 0.000 0.00122(7) 0.000 C1_2 0.0099(7) 0.0100(7) 0.0112(7) 0.0010(5) -0.0003(6) 0.0015(5) C2_2 0.0112(7) 0.0111(7) 0.0103(7) 0.0007(5) -0.0006(6) 0.0008(5) C3_2 0.0142(7) 0.0135(7) 0.0090(7) 0.0022(6) 0.0014(6) 0.0025(6) C4_2 0.0127(7) 0.0113(7) 0.0127(8) 0.0048(6) 0.0009(6) 0.0017(6) C5_2 0.0116(7) 0.0095(7) 0.0139(8) 0.0004(6) 0.0002(6) 0.0011(6) C6_2 0.0104(7) 0.0117(7) 0.0131(8) -0.0006(6) 0.0020(6) 0.0007(6) C7_2 0.0192(8) 0.0147(8) 0.0225(9) 0.0022(7) 0.0069(7) 0.0053(7) C8_2 0.0126(8) 0.0167(8) 0.0187(9) -0.0039(6) 0.0038(7) -0.0020(6) C9_2 0.0136(8) 0.0246(9) 0.0112(8) -0.0016(6) 0.0026(6) 0.0013(6) _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 Cr1 C1_1 2.1336(16) . ? Cr1 C1_1 2.1337(16) 2_556 ? Cr1 C2_1 2.1409(16) 2_556 ? Cr1 C2_1 2.1409(16) . ? Cr1 C6_1 2.1423(17) 2_556 ? Cr1 C6_1 2.1423(17) . ? Cr1 C5_1 2.1679(17) 2_556 ? Cr1 C5_1 2.1680(17) . ? Cr1 C3_1 2.1699(17) 2_556 ? Cr1 C3_1 2.1699(17) . ? Cr1 C4_1 2.1742(17) 2_556 ? Cr1 C4_1 2.1742(17) . ? C1_1 C2_1 1.436(2) . ? C1_1 C6_1 1.437(2) . ? C1_1 Zr1 2.3110(16) . ? C2_1 C3_1 1.417(2) . ? C2_1 H2_1 0.9500 . ? C3_1 C4_1 1.408(2) . ? C3_1 H3_1 0.9500 . ? C4_1 C5_1 1.410(2) . ? C4_1 H4_1 0.9500 . ? C5_1 C6_1 1.415(2) . ? C5_1 H5_1 0.9500 . ? C6_1 H6_1 0.9500 . ? Zr1 C1_1 2.3109(16) 2_556 ? Zr1 C4_2 2.5093(16) . ? Zr1 C4_2 2.5093(16) 2_556 ? Zr1 C3_2 2.5500(17) . ? Zr1 C3_2 2.5500(17) 2_556 ? Zr1 C5_2 2.5627(16) . ? Zr1 C5_2 2.5628(16) 2_556 ? Zr1 C2_2 2.6169(17) 2_556 ? Zr1 C2_2 2.6169(17) . ? Zr1 C1_2 2.6501(16) 2_556 ? Zr1 C1_2 2.6502(16) . ? C1_2 C5_2 1.421(2) . ? C1_2 C2_2 1.425(2) . ? C1_2 C6_2 1.527(2) . ? C2_2 C3_2 1.416(2) . ? C2_2 H2_2 0.9500 . ? C3_2 C4_2 1.410(2) . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.419(2) . ? C4_2 H4_2 0.9500 . ? C5_2 H5_2 0.9500 . ? C6_2 C9_2 1.532(2) . ? C6_2 C8_2 1.534(2) . ? C6_2 C7_2 1.541(2) . ? C7_2 H7A_2 0.9800 . ? C7_2 H7B_2 0.9800 . ? C7_2 H7C_2 0.9800 . ? C8_2 H8A_2 0.9800 . ? C8_2 H8B_2 0.9800 . ? C8_2 H8C_2 0.9800 . ? C9_2 H9A_2 0.9800 . ? C9_2 H9B_2 0.9800 . ? C9_2 H9C_2 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_1 Cr1 C1_1 93.98(9) . 2_556 ? C1_1 Cr1 C2_1 110.31(7) . 2_556 ? C1_1 Cr1 C2_1 39.26(6) 2_556 2_556 ? C1_1 Cr1 C2_1 39.26(6) . . ? C1_1 Cr1 C2_1 110.30(7) 2_556 . ? C2_1 Cr1 C2_1 143.50(9) 2_556 . ? C1_1 Cr1 C6_1 109.75(7) . 2_556 ? C1_1 Cr1 C6_1 39.27(6) 2_556 2_556 ? C2_1 Cr1 C6_1 68.52(6) 2_556 2_556 ? C2_1 Cr1 C6_1 99.55(6) . 2_556 ? C1_1 Cr1 C6_1 39.27(6) . . ? C1_1 Cr1 C6_1 109.75(7) 2_556 . ? C2_1 Cr1 C6_1 99.56(6) 2_556 . ? C2_1 Cr1 C6_1 68.51(6) . . ? C6_1 Cr1 C6_1 142.71(9) 2_556 . ? C1_1 Cr1 C5_1 141.29(7) . 2_556 ? C1_1 Cr1 C5_1 71.28(6) 2_556 2_556 ? C2_1 Cr1 C5_1 81.08(6) 2_556 2_556 ? C2_1 Cr1 C5_1 111.46(6) . 2_556 ? C6_1 Cr1 C5_1 38.33(6) 2_556 2_556 ? C6_1 Cr1 C5_1 178.94(7) . 2_556 ? C1_1 Cr1 C5_1 71.28(6) . . ? C1_1 Cr1 C5_1 141.29(7) 2_556 . ? C2_1 Cr1 C5_1 111.47(6) 2_556 . ? C2_1 Cr1 C5_1 81.08(6) . . ? C6_1 Cr1 C5_1 178.94(7) 2_556 . ? C6_1 Cr1 C5_1 38.33(6) . . ? C5_1 Cr1 C5_1 140.64(9) 2_556 . ? C1_1 Cr1 C3_1 142.07(7) . 2_556 ? C1_1 Cr1 C3_1 71.39(6) 2_556 2_556 ? C2_1 Cr1 C3_1 38.38(6) 2_556 2_556 ? C2_1 Cr1 C3_1 178.12(7) . 2_556 ? C6_1 Cr1 C3_1 81.24(6) 2_556 2_556 ? C6_1 Cr1 C3_1 111.87(6) . 2_556 ? C5_1 Cr1 C3_1 68.12(6) 2_556 2_556 ? C5_1 Cr1 C3_1 98.10(6) . 2_556 ? C1_1 Cr1 C3_1 71.39(6) . . ? C1_1 Cr1 C3_1 142.06(7) 2_556 . ? C2_1 Cr1 C3_1 178.12(7) 2_556 . ? C2_1 Cr1 C3_1 38.38(6) . . ? C6_1 Cr1 C3_1 111.87(6) 2_556 . ? C6_1 Cr1 C3_1 81.23(6) . . ? C5_1 Cr1 C3_1 98.10(6) 2_556 . ? C5_1 Cr1 C3_1 68.12(6) . . ? C3_1 Cr1 C3_1 139.74(9) 2_556 . ? C1_1 Cr1 C4_1 178.83(6) . 2_556 ? C1_1 Cr1 C4_1 84.92(6) 2_556 2_556 ? C2_1 Cr1 C4_1 69.05(6) 2_556 2_556 ? C2_1 Cr1 C4_1 140.88(7) . 2_556 ? C6_1 Cr1 C4_1 69.13(7) 2_556 2_556 ? C6_1 Cr1 C4_1 141.57(7) . 2_556 ? C5_1 Cr1 C4_1 37.89(6) 2_556 2_556 ? C5_1 Cr1 C4_1 109.83(7) . 2_556 ? C3_1 Cr1 C4_1 37.83(6) 2_556 2_556 ? C3_1 Cr1 C4_1 109.27(7) . 2_556 ? C1_1 Cr1 C4_1 84.92(6) . . ? C1_1 Cr1 C4_1 178.83(6) 2_556 . ? C2_1 Cr1 C4_1 140.89(7) 2_556 . ? C2_1 Cr1 C4_1 69.05(6) . . ? C6_1 Cr1 C4_1 141.56(7) 2_556 . ? C6_1 Cr1 C4_1 69.13(7) . . ? C5_1 Cr1 C4_1 109.83(7) 2_556 . ? C5_1 Cr1 C4_1 37.89(6) . . ? C3_1 Cr1 C4_1 109.27(7) 2_556 . ? C3_1 Cr1 C4_1 37.83(6) . . ? C4_1 Cr1 C4_1 96.18(9) 2_556 . ? C2_1 C1_1 C6_1 114.11(14) . . ? C2_1 C1_1 Cr1 70.64(9) . . ? C6_1 C1_1 Cr1 70.69(9) . . ? C2_1 C1_1 Zr1 116.19(12) . . ? C6_1 C1_1 Zr1 115.33(11) . . ? Cr1 C1_1 Zr1 90.54(6) . . ? C3_1 C2_1 C1_1 123.29(15) . . ? C3_1 C2_1 Cr1 71.92(9) . . ? C1_1 C2_1 Cr1 70.10(9) . . ? C3_1 C2_1 H2_1 118.4 . . ? C1_1 C2_1 H2_1 118.4 . . ? Cr1 C2_1 H2_1 133.3 . . ? C4_1 C3_1 C2_1 119.91(16) . . ? C4_1 C3_1 Cr1 71.25(10) . . ? C2_1 C3_1 Cr1 69.70(9) . . ? C4_1 C3_1 H3_1 120.0 . . ? C2_1 C3_1 H3_1 120.0 . . ? Cr1 C3_1 H3_1 131.9 . . ? C3_1 C4_1 C5_1 119.10(15) . . ? C3_1 C4_1 Cr1 70.92(10) . . ? C5_1 C4_1 Cr1 70.82(9) . . ? C3_1 C4_1 H4_1 120.5 . . ? C5_1 C4_1 H4_1 120.5 . . ? Cr1 C4_1 H4_1 130.3 . . ? C4_1 C5_1 C6_1 120.22(15) . . ? C4_1 C5_1 Cr1 71.30(10) . . ? C6_1 C5_1 Cr1 69.86(9) . . ? C4_1 C5_1 H5_1 119.9 . . ? C6_1 C5_1 H5_1 119.9 . . ? Cr1 C5_1 H5_1 131.9 . . ? C5_1 C6_1 C1_1 123.01(15) . . ? C5_1 C6_1 Cr1 71.82(9) . . ? C1_1 C6_1 Cr1 70.04(9) . . ? C5_1 C6_1 H6_1 118.5 . . ? C1_1 C6_1 H6_1 118.5 . . ? Cr1 C6_1 H6_1 133.2 . . ? C1_1 Zr1 C1_1 84.93(8) 2_556 . ? C1_1 Zr1 C4_2 104.28(6) 2_556 . ? C1_1 Zr1 C4_2 139.99(6) . . ? C1_1 Zr1 C4_2 139.99(6) 2_556 2_556 ? C1_1 Zr1 C4_2 104.28(6) . 2_556 ? C4_2 Zr1 C4_2 93.32(8) . 2_556 ? C1_1 Zr1 C3_2 82.25(6) 2_556 . ? C1_1 Zr1 C3_2 115.40(6) . . ? C4_2 Zr1 C3_2 32.36(5) . . ? C4_2 Zr1 C3_2 124.82(6) 2_556 . ? C1_1 Zr1 C3_2 115.41(6) 2_556 2_556 ? C1_1 Zr1 C3_2 82.26(6) . 2_556 ? C4_2 Zr1 C3_2 124.82(6) . 2_556 ? C4_2 Zr1 C3_2 32.36(5) 2_556 2_556 ? C3_2 Zr1 C3_2 156.99(8) . 2_556 ? C1_1 Zr1 C5_2 134.56(6) 2_556 . ? C1_1 Zr1 C5_2 119.06(6) . . ? C4_2 Zr1 C5_2 32.47(5) . . ? C4_2 Zr1 C5_2 74.86(5) 2_556 . ? C3_2 Zr1 C5_2 53.10(5) . . ? C3_2 Zr1 C5_2 106.22(5) 2_556 . ? C1_1 Zr1 C5_2 119.07(6) 2_556 2_556 ? C1_1 Zr1 C5_2 134.57(6) . 2_556 ? C4_2 Zr1 C5_2 74.86(5) . 2_556 ? C4_2 Zr1 C5_2 32.47(5) 2_556 2_556 ? C3_2 Zr1 C5_2 106.22(5) . 2_556 ? C3_2 Zr1 C5_2 53.10(5) 2_556 2_556 ? C5_2 Zr1 C5_2 72.80(7) . 2_556 ? C1_1 Zr1 C2_2 87.99(6) 2_556 2_556 ? C1_1 Zr1 C2_2 95.33(6) . 2_556 ? C4_2 Zr1 C2_2 123.42(5) . 2_556 ? C4_2 Zr1 C2_2 52.81(5) 2_556 2_556 ? C3_2 Zr1 C2_2 146.56(5) . 2_556 ? C3_2 Zr1 C2_2 31.78(5) 2_556 2_556 ? C5_2 Zr1 C2_2 123.52(5) . 2_556 ? C5_2 Zr1 C2_2 52.04(5) 2_556 2_556 ? C1_1 Zr1 C2_2 95.32(6) 2_556 . ? C1_1 Zr1 C2_2 87.99(6) . . ? C4_2 Zr1 C2_2 52.81(5) . . ? C4_2 Zr1 C2_2 123.42(5) 2_556 . ? C3_2 Zr1 C2_2 31.78(5) . . ? C3_2 Zr1 C2_2 146.56(5) 2_556 . ? C5_2 Zr1 C2_2 52.04(5) . . ? C5_2 Zr1 C2_2 123.51(5) 2_556 . ? C2_2 Zr1 C2_2 175.52(7) 2_556 . ? C1_1 Zr1 C1_2 89.74(6) 2_556 2_556 ? C1_1 Zr1 C1_2 126.68(6) . 2_556 ? C4_2 Zr1 C1_2 92.67(5) . 2_556 ? C4_2 Zr1 C1_2 53.26(5) 2_556 2_556 ? C3_2 Zr1 C1_2 116.29(5) . 2_556 ? C3_2 Zr1 C1_2 52.90(5) 2_556 2_556 ? C5_2 Zr1 C1_2 101.83(5) . 2_556 ? C5_2 Zr1 C1_2 31.59(5) 2_556 2_556 ? C2_2 Zr1 C1_2 31.39(5) 2_556 2_556 ? C2_2 Zr1 C1_2 145.31(5) . 2_556 ? C1_1 Zr1 C1_2 126.68(6) 2_556 . ? C1_1 Zr1 C1_2 89.74(6) . . ? C4_2 Zr1 C1_2 53.26(5) . . ? C4_2 Zr1 C1_2 92.67(5) 2_556 . ? C3_2 Zr1 C1_2 52.91(5) . . ? C3_2 Zr1 C1_2 116.29(5) 2_556 . ? C5_2 Zr1 C1_2 31.59(5) . . ? C5_2 Zr1 C1_2 101.82(5) 2_556 . ? C2_2 Zr1 C1_2 145.31(5) 2_556 . ? C2_2 Zr1 C1_2 31.39(5) . . ? C1_2 Zr1 C1_2 132.61(7) 2_556 . ? C5_2 C1_2 C2_2 105.96(14) . . ? C5_2 C1_2 C6_2 124.56(14) . . ? C2_2 C1_2 C6_2 128.75(15) . . ? C5_2 C1_2 Zr1 70.81(9) . . ? C2_2 C1_2 Zr1 73.02(9) . . ? C6_2 C1_2 Zr1 128.34(11) . . ? C3_2 C2_2 C1_2 109.34(14) . . ? C3_2 C2_2 Zr1 71.50(9) . . ? C1_2 C2_2 Zr1 75.59(9) . . ? C3_2 C2_2 H2_2 125.3 . . ? C1_2 C2_2 H2_2 125.3 . . ? Zr1 C2_2 H2_2 119.3 . . ? C4_2 C3_2 C2_2 107.66(15) . . ? C4_2 C3_2 Zr1 72.23(9) . . ? C2_2 C3_2 Zr1 76.72(9) . . ? C4_2 C3_2 H3_2 126.2 . . ? C2_2 C3_2 H3_2 126.2 . . ? Zr1 C3_2 H3_2 117.0 . . ? C3_2 C4_2 C5_2 107.76(14) . . ? C3_2 C4_2 Zr1 75.41(9) . . ? C5_2 C4_2 Zr1 75.84(9) . . ? C3_2 C4_2 H4_2 126.1 . . ? C5_2 C4_2 H4_2 126.1 . . ? Zr1 C4_2 H4_2 114.9 . . ? C4_2 C5_2 C1_2 109.27(14) . . ? C4_2 C5_2 Zr1 71.69(9) . . ? C1_2 C5_2 Zr1 77.60(9) . . ? C4_2 C5_2 H5_2 125.4 . . ? C1_2 C5_2 H5_2 125.4 . . ? Zr1 C5_2 H5_2 117.2 . . ? C1_2 C6_2 C9_2 111.95(13) . . ? C1_2 C6_2 C8_2 111.56(14) . . ? C9_2 C6_2 C8_2 108.80(14) . . ? C1_2 C6_2 C7_2 108.04(14) . . ? C9_2 C6_2 C7_2 108.60(14) . . ? C8_2 C6_2 C7_2 107.77(14) . . ? C6_2 C7_2 H7A_2 109.5 . . ? C6_2 C7_2 H7B_2 109.5 . . ? H7A_2 C7_2 H7B_2 109.5 . . ? C6_2 C7_2 H7C_2 109.5 . . ? H7A_2 C7_2 H7C_2 109.5 . . ? H7B_2 C7_2 H7C_2 109.5 . . ? C6_2 C8_2 H8A_2 109.5 . . ? C6_2 C8_2 H8B_2 109.5 . . ? H8A_2 C8_2 H8B_2 109.5 . . ? C6_2 C8_2 H8C_2 109.5 . . ? H8A_2 C8_2 H8C_2 109.5 . . ? H8B_2 C8_2 H8C_2 109.5 . . ? C6_2 C9_2 H9A_2 109.5 . . ? C6_2 C9_2 H9B_2 109.5 . . ? H9A_2 C9_2 H9B_2 109.5 . . ? C6_2 C9_2 H9C_2 109.5 . . ? H9A_2 C9_2 H9C_2 109.5 . . ? H9B_2 C9_2 H9C_2 109.5 . . ? 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 C1_1 Cr1 C1_1 C2_1 -117.68(11) 2_556 . . . ? C2_1 Cr1 C1_1 C2_1 -154.38(8) 2_556 . . . ? C6_1 Cr1 C1_1 C2_1 -80.76(10) 2_556 . . . ? C6_1 Cr1 C1_1 C2_1 125.58(14) . . . . ? C5_1 Cr1 C1_1 C2_1 -52.99(14) 2_556 . . . ? C5_1 Cr1 C1_1 C2_1 98.97(10) . . . . ? C3_1 Cr1 C1_1 C2_1 177.86(11) 2_556 . . . ? C3_1 Cr1 C1_1 C2_1 26.50(9) . . . . ? C1_1 Cr1 C1_1 C6_1 116.75(11) 2_556 . . . ? C2_1 Cr1 C1_1 C6_1 80.05(11) 2_556 . . . ? C2_1 Cr1 C1_1 C6_1 -125.58(14) . . . . ? C6_1 Cr1 C1_1 C6_1 153.66(8) 2_556 . . . ? C5_1 Cr1 C1_1 C6_1 -178.56(10) 2_556 . . . ? C5_1 Cr1 C1_1 C6_1 -26.61(9) . . . . ? C3_1 Cr1 C1_1 C6_1 52.28(14) 2_556 . . . ? C3_1 Cr1 C1_1 C6_1 -99.08(10) . . . . ? C4_1 Cr1 C1_1 C6_1 -62.86(10) . . . . ? C1_1 Cr1 C1_1 Zr1 0.0 2_556 . . . ? C2_1 Cr1 C1_1 Zr1 -36.70(8) 2_556 . . . ? C2_1 Cr1 C1_1 Zr1 117.68(11) . . . . ? C6_1 Cr1 C1_1 Zr1 36.92(7) 2_556 . . . ? C6_1 Cr1 C1_1 Zr1 -116.74(11) . . . . ? C5_1 Cr1 C1_1 Zr1 64.69(11) 2_556 . . . ? C5_1 Cr1 C1_1 Zr1 -143.35(7) . . . . ? C3_1 Cr1 C1_1 Zr1 -64.46(12) 2_556 . . . ? C3_1 Cr1 C1_1 Zr1 144.17(8) . . . . ? C6_1 C1_1 C2_1 C3_1 6.5(2) . . . . ? Cr1 C1_1 C2_1 C3_1 -50.75(15) . . . . ? Zr1 C1_1 C2_1 C3_1 -131.45(14) . . . . ? C6_1 C1_1 C2_1 Cr1 57.23(12) . . . . ? Zr1 C1_1 C2_1 Cr1 -80.70(9) . . . . ? C1_1 Cr1 C2_1 C3_1 137.08(15) . . . . ? C1_1 Cr1 C2_1 C3_1 -152.53(10) 2_556 . . . ? C2_1 Cr1 C2_1 C3_1 -179.93(10) 2_556 . . . ? C6_1 Cr1 C2_1 C3_1 -113.32(10) 2_556 . . . ? C6_1 Cr1 C2_1 C3_1 103.49(11) . . . . ? C5_1 Cr1 C2_1 C3_1 -75.37(11) 2_556 . . . ? C5_1 Cr1 C2_1 C3_1 65.82(10) . . . . ? C4_1 Cr1 C2_1 C3_1 -44.75(15) 2_556 . . . ? C4_1 Cr1 C2_1 C3_1 28.51(10) . . . . ? C1_1 Cr1 C2_1 C1_1 70.39(13) 2_556 . . . ? C2_1 Cr1 C2_1 C1_1 42.99(8) 2_556 . . . ? C6_1 Cr1 C2_1 C1_1 109.60(10) 2_556 . . . ? C6_1 Cr1 C2_1 C1_1 -33.59(9) . . . . ? C5_1 Cr1 C2_1 C1_1 147.55(10) 2_556 . . . ? C5_1 Cr1 C2_1 C1_1 -71.26(10) . . . . ? C4_1 Cr1 C2_1 C1_1 178.17(10) 2_556 . . . ? C4_1 Cr1 C2_1 C1_1 -108.57(11) . . . . ? C1_1 C2_1 C3_1 C4_1 -2.6(2) . . . . ? Cr1 C2_1 C3_1 C4_1 -52.55(14) . . . . ? C1_1 C2_1 C3_1 Cr1 49.99(14) . . . . ? C1_1 Cr1 C3_1 C4_1 106.34(11) . . . . ? C1_1 Cr1 C3_1 C4_1 178.11(10) 2_556 . . . ? C6_1 Cr1 C3_1 C4_1 -149.24(10) 2_556 . . . ? C6_1 Cr1 C3_1 C4_1 67.10(11) . . . . ? C5_1 Cr1 C3_1 C4_1 -112.06(11) 2_556 . . . ? C5_1 Cr1 C3_1 C4_1 29.61(10) . . . . ? C3_1 Cr1 C3_1 C4_1 -46.54(9) 2_556 . . . ? C4_1 Cr1 C3_1 C4_1 -74.68(14) 2_556 . . . ? C1_1 Cr1 C3_1 C2_1 -27.05(10) . . . . ? C1_1 Cr1 C3_1 C2_1 44.72(15) 2_556 . . . ? C6_1 Cr1 C3_1 C2_1 77.37(11) 2_556 . . . ? C6_1 Cr1 C3_1 C2_1 -66.28(10) . . . . ? C5_1 Cr1 C3_1 C2_1 114.56(10) 2_556 . . . ? C5_1 Cr1 C3_1 C2_1 -103.78(11) . . . . ? C3_1 Cr1 C3_1 C2_1 -179.93(10) 2_556 . . . ? C4_1 Cr1 C3_1 C2_1 151.93(10) 2_556 . . . ? C4_1 Cr1 C3_1 C2_1 -133.39(15) . . . . ? C2_1 C3_1 C4_1 C5_1 -2.0(2) . . . . ? Cr1 C3_1 C4_1 C5_1 -53.81(14) . . . . ? C2_1 C3_1 C4_1 Cr1 51.84(14) . . . . ? C2_1 Cr1 C4_1 C3_1 177.79(11) 2_556 . . . ? C2_1 Cr1 C4_1 C3_1 -28.89(10) . . . . ? C6_1 Cr1 C4_1 C3_1 49.78(15) 2_556 . . . ? C6_1 Cr1 C4_1 C3_1 -103.00(11) . . . . ? C5_1 Cr1 C4_1 C3_1 77.27(11) 2_556 . . . ? C5_1 Cr1 C4_1 C3_1 -131.70(15) . . . . ? C3_1 Cr1 C4_1 C3_1 150.20(9) 2_556 . . . ? C4_1 Cr1 C4_1 C3_1 113.68(11) 2_556 . . . ? C2_1 Cr1 C4_1 C5_1 -50.51(14) 2_556 . . . ? C2_1 Cr1 C4_1 C5_1 102.81(11) . . . . ? C6_1 Cr1 C4_1 C5_1 -178.52(11) 2_556 . . . ? C6_1 Cr1 C4_1 C5_1 28.70(10) . . . . ? C5_1 Cr1 C4_1 C5_1 -151.02(9) 2_556 . . . ? C3_1 Cr1 C4_1 C5_1 -78.10(11) 2_556 . . . ? C3_1 Cr1 C4_1 C5_1 131.70(15) . . . . ? C4_1 Cr1 C4_1 C5_1 -114.61(11) 2_556 . . . ? C3_1 C4_1 C5_1 C6_1 2.0(2) . . . . ? Cr1 C4_1 C5_1 C6_1 -51.83(14) . . . . ? C3_1 C4_1 C5_1 Cr1 53.85(14) . . . . ? C1_1 Cr1 C5_1 C4_1 -106.45(11) . . . . ? C1_1 Cr1 C5_1 C4_1 -178.65(10) 2_556 . . . ? C2_1 Cr1 C5_1 C4_1 148.45(10) 2_556 . . . ? C2_1 Cr1 C5_1 C4_1 -67.19(10) . . . . ? C5_1 Cr1 C5_1 C4_1 45.93(9) 2_556 . . . ? C3_1 Cr1 C5_1 C4_1 111.09(10) 2_556 . . . ? C3_1 Cr1 C5_1 C4_1 -29.57(10) . . . . ? C4_1 Cr1 C5_1 C4_1 73.91(13) 2_556 . . . ? C1_1 Cr1 C5_1 C6_1 27.21(9) . . . . ? C1_1 Cr1 C5_1 C6_1 -45.00(14) 2_556 . . . ? C2_1 Cr1 C5_1 C6_1 -77.89(10) 2_556 . . . ? C2_1 Cr1 C5_1 C6_1 66.46(10) . . . . ? C3_1 Cr1 C5_1 C6_1 -115.25(10) 2_556 . . . ? C3_1 Cr1 C5_1 C6_1 104.08(10) . . . . ? C4_1 Cr1 C5_1 C6_1 -152.43(9) 2_556 . . . ? C4_1 Cr1 C5_1 C6_1 133.65(14) . . . . ? C4_1 C5_1 C6_1 C1_1 2.4(2) . . . . ? Cr1 C5_1 C6_1 C1_1 -50.06(14) . . . . ? C4_1 C5_1 C6_1 Cr1 52.48(14) . . . . ? C2_1 C1_1 C6_1 C5_1 -6.4(2) . . . . ? Cr1 C1_1 C6_1 C5_1 50.80(14) . . . . ? Zr1 C1_1 C6_1 C5_1 131.90(14) . . . . ? C2_1 C1_1 C6_1 Cr1 -57.21(12) . . . . ? Zr1 C1_1 C6_1 Cr1 81.10(9) . . . . ? C1_1 Cr1 C6_1 C5_1 -136.84(14) . . . . ? C1_1 Cr1 C6_1 C5_1 151.98(9) 2_556 . . . ? C2_1 Cr1 C6_1 C5_1 112.67(10) 2_556 . . . ? C2_1 Cr1 C6_1 C5_1 -103.26(10) . . . . ? C6_1 Cr1 C6_1 C5_1 179.59(10) 2_556 . . . ? C3_1 Cr1 C6_1 C5_1 74.76(11) 2_556 . . . ? C3_1 Cr1 C6_1 C5_1 -65.60(10) . . . . ? C4_1 Cr1 C6_1 C5_1 44.45(14) 2_556 . . . ? C4_1 Cr1 C6_1 C5_1 -28.39(9) . . . . ? C1_1 Cr1 C6_1 C1_1 -71.18(13) 2_556 . . . ? C2_1 Cr1 C6_1 C1_1 -110.49(10) 2_556 . . . ? C2_1 Cr1 C6_1 C1_1 33.59(9) . . . . ? C6_1 Cr1 C6_1 C1_1 -43.56(8) 2_556 . . . ? C3_1 Cr1 C6_1 C1_1 -148.40(9) 2_556 . . . ? C3_1 Cr1 C6_1 C1_1 71.24(10) . . . . ? C4_1 Cr1 C6_1 C1_1 -178.71(10) 2_556 . . . ? C4_1 Cr1 C6_1 C1_1 108.45(11) . . . . ? C2_1 C1_1 Zr1 C1_1 68.61(11) . . . 2_556 ? C6_1 C1_1 Zr1 C1_1 -68.82(11) . . . 2_556 ? Cr1 C1_1 Zr1 C1_1 0.0 . . . 2_556 ? C2_1 C1_1 Zr1 C4_2 -37.62(16) . . . . ? C6_1 C1_1 Zr1 C4_2 -175.04(10) . . . . ? Cr1 C1_1 Zr1 C4_2 -106.23(8) . . . . ? C2_1 C1_1 Zr1 C4_2 -150.96(12) . . . 2_556 ? C6_1 C1_1 Zr1 C4_2 71.62(13) . . . 2_556 ? Cr1 C1_1 Zr1 C4_2 140.43(6) . . . 2_556 ? C2_1 C1_1 Zr1 C3_2 -10.33(14) . . . . ? C6_1 C1_1 Zr1 C3_2 -147.75(11) . . . . ? Cr1 C1_1 Zr1 C3_2 -78.94(7) . . . . ? C2_1 C1_1 Zr1 C3_2 -174.86(13) . . . 2_556 ? C6_1 C1_1 Zr1 C3_2 47.72(12) . . . 2_556 ? Cr1 C1_1 Zr1 C3_2 116.53(6) . . . 2_556 ? C2_1 C1_1 Zr1 C5_2 -70.56(13) . . . . ? C6_1 C1_1 Zr1 C5_2 152.01(11) . . . . ? Cr1 C1_1 Zr1 C5_2 -139.17(5) . . . . ? C2_1 C1_1 Zr1 C5_2 -164.72(10) . . . 2_556 ? C6_1 C1_1 Zr1 C5_2 57.86(15) . . . 2_556 ? Cr1 C1_1 Zr1 C5_2 126.67(7) . . . 2_556 ? C2_1 C1_1 Zr1 C2_2 156.10(12) . . . 2_556 ? C6_1 C1_1 Zr1 C2_2 18.68(12) . . . 2_556 ? Cr1 C1_1 Zr1 C2_2 87.49(6) . . . 2_556 ? C2_1 C1_1 Zr1 C2_2 -26.92(12) . . . . ? C6_1 C1_1 Zr1 C2_2 -164.34(12) . . . . ? Cr1 C1_1 Zr1 C2_2 -95.53(6) . . . . ? C2_1 C1_1 Zr1 C1_2 154.49(11) . . . 2_556 ? C6_1 C1_1 Zr1 C1_2 17.07(15) . . . 2_556 ? Cr1 C1_1 Zr1 C1_2 85.89(7) . . . 2_556 ? C2_1 C1_1 Zr1 C1_2 -58.27(12) . . . . ? C6_1 C1_1 Zr1 C1_2 164.30(12) . . . . ? Cr1 C1_1 Zr1 C1_2 -126.88(6) . . . . ? C1_1 Zr1 C1_2 C5_2 117.33(10) 2_556 . . . ? C1_1 Zr1 C1_2 C5_2 -159.19(10) . . . . ? C4_2 Zr1 C1_2 C5_2 37.24(9) . . . . ? C4_2 Zr1 C1_2 C5_2 -54.91(10) 2_556 . . . ? C3_2 Zr1 C1_2 C5_2 78.04(10) . . . . ? C3_2 Zr1 C1_2 C5_2 -77.97(11) 2_556 . . . ? C5_2 Zr1 C1_2 C5_2 -23.47(13) 2_556 . . . ? C2_2 Zr1 C1_2 C5_2 -60.19(13) 2_556 . . . ? C2_2 Zr1 C1_2 C5_2 114.25(14) . . . . ? C1_2 Zr1 C1_2 C5_2 -15.33(8) 2_556 . . . ? C1_1 Zr1 C1_2 C2_2 3.08(12) 2_556 . . . ? C1_1 Zr1 C1_2 C2_2 86.56(10) . . . . ? C4_2 Zr1 C1_2 C2_2 -77.01(10) . . . . ? C4_2 Zr1 C1_2 C2_2 -169.16(10) 2_556 . . . ? C3_2 Zr1 C1_2 C2_2 -36.21(9) . . . . ? C3_2 Zr1 C1_2 C2_2 167.78(9) 2_556 . . . ? C5_2 Zr1 C1_2 C2_2 -114.25(14) . . . . ? C5_2 Zr1 C1_2 C2_2 -137.72(10) 2_556 . . . ? C2_2 Zr1 C1_2 C2_2 -174.44(9) 2_556 . . . ? C1_2 Zr1 C1_2 C2_2 -129.58(10) 2_556 . . . ? C1_1 Zr1 C1_2 C6_2 -123.29(13) 2_556 . . . ? C1_1 Zr1 C1_2 C6_2 -39.81(14) . . . . ? C4_2 Zr1 C1_2 C6_2 156.63(16) . . . . ? C4_2 Zr1 C1_2 C6_2 64.47(14) 2_556 . . . ? C3_2 Zr1 C1_2 C6_2 -162.58(16) . . . . ? C3_2 Zr1 C1_2 C6_2 41.42(15) 2_556 . . . ? C5_2 Zr1 C1_2 C6_2 119.38(18) . . . . ? C5_2 Zr1 C1_2 C6_2 95.91(13) 2_556 . . . ? C2_2 Zr1 C1_2 C6_2 59.19(17) 2_556 . . . ? C2_2 Zr1 C1_2 C6_2 -126.37(18) . . . . ? C1_2 Zr1 C1_2 C6_2 104.05(13) 2_556 . . . ? C5_2 C1_2 C2_2 C3_2 0.47(18) . . . . ? C6_2 C1_2 C2_2 C3_2 -170.01(15) . . . . ? Zr1 C1_2 C2_2 C3_2 64.07(12) . . . . ? C5_2 C1_2 C2_2 Zr1 -63.59(11) . . . . ? C6_2 C1_2 C2_2 Zr1 125.92(16) . . . . ? C1_1 Zr1 C2_2 C3_2 65.95(10) 2_556 . . . ? C1_1 Zr1 C2_2 C3_2 150.67(10) . . . . ? C4_2 Zr1 C2_2 C3_2 -37.95(9) . . . . ? C4_2 Zr1 C2_2 C3_2 -103.52(10) 2_556 . . . ? C3_2 Zr1 C2_2 C3_2 -136.67(15) 2_556 . . . ? C5_2 Zr1 C2_2 C3_2 -79.24(10) . . . . ? C5_2 Zr1 C2_2 C3_2 -64.36(11) 2_556 . . . ? C1_2 Zr1 C2_2 C3_2 -31.33(14) 2_556 . . . ? C1_2 Zr1 C2_2 C3_2 -116.52(14) . . . . ? C1_1 Zr1 C2_2 C1_2 -177.52(10) 2_556 . . . ? C1_1 Zr1 C2_2 C1_2 -92.81(10) . . . . ? C4_2 Zr1 C2_2 C1_2 78.58(10) . . . . ? C4_2 Zr1 C2_2 C1_2 13.01(12) 2_556 . . . ? C3_2 Zr1 C2_2 C1_2 116.52(14) . . . . ? C3_2 Zr1 C2_2 C1_2 -20.14(15) 2_556 . . . ? C5_2 Zr1 C2_2 C1_2 37.28(9) . . . . ? C5_2 Zr1 C2_2 C1_2 52.16(11) 2_556 . . . ? C1_2 Zr1 C2_2 C1_2 85.20(15) 2_556 . . . ? C1_2 C2_2 C3_2 C4_2 -0.54(19) . . . . ? Zr1 C2_2 C3_2 C4_2 66.16(11) . . . . ? C1_2 C2_2 C3_2 Zr1 -66.70(12) . . . . ? C1_1 Zr1 C3_2 C4_2 132.82(10) 2_556 . . . ? C1_1 Zr1 C3_2 C4_2 -146.58(10) . . . . ? C4_2 Zr1 C3_2 C4_2 -15.06(15) 2_556 . . . ? C3_2 Zr1 C3_2 C4_2 -9.13(9) 2_556 . . . ? C5_2 Zr1 C3_2 C4_2 -38.16(9) . . . . ? C5_2 Zr1 C3_2 C4_2 14.72(11) 2_556 . . . ? C2_2 Zr1 C3_2 C4_2 58.50(14) 2_556 . . . ? C2_2 Zr1 C3_2 C4_2 -113.77(14) . . . . ? C1_2 Zr1 C3_2 C4_2 46.96(11) 2_556 . . . ? C1_2 Zr1 C3_2 C4_2 -78.01(10) . . . . ? C1_1 Zr1 C3_2 C2_2 -113.42(10) 2_556 . . . ? C1_1 Zr1 C3_2 C2_2 -32.82(11) . . . . ? C4_2 Zr1 C3_2 C2_2 113.77(14) . . . . ? C4_2 Zr1 C3_2 C2_2 98.70(10) 2_556 . . . ? C3_2 Zr1 C3_2 C2_2 104.64(9) 2_556 . . . ? C5_2 Zr1 C3_2 C2_2 75.60(10) . . . . ? C5_2 Zr1 C3_2 C2_2 128.48(10) 2_556 . . . ? C2_2 Zr1 C3_2 C2_2 172.27(12) 2_556 . . . ? C1_2 Zr1 C3_2 C2_2 160.73(9) 2_556 . . . ? C1_2 Zr1 C3_2 C2_2 35.75(9) . . . . ? C2_2 C3_2 C4_2 C5_2 0.39(18) . . . . ? Zr1 C3_2 C4_2 C5_2 69.58(11) . . . . ? C2_2 C3_2 C4_2 Zr1 -69.19(11) . . . . ? C1_1 Zr1 C4_2 C3_2 -48.59(11) 2_556 . . . ? C1_1 Zr1 C4_2 C3_2 50.70(13) . . . . ? C4_2 Zr1 C4_2 C3_2 167.66(12) 2_556 . . . ? C3_2 Zr1 C4_2 C3_2 175.67(4) 2_556 . . . ? C5_2 Zr1 C4_2 C3_2 113.00(14) . . . . ? C5_2 Zr1 C4_2 C3_2 -165.36(11) 2_556 . . . ? C2_2 Zr1 C4_2 C3_2 -145.74(9) 2_556 . . . ? C2_2 Zr1 C4_2 C3_2 37.23(9) . . . . ? C1_2 Zr1 C4_2 C3_2 -139.00(10) 2_556 . . . ? C1_2 Zr1 C4_2 C3_2 76.81(10) . . . . ? C1_1 Zr1 C4_2 C5_2 -161.59(10) 2_556 . . . ? C1_1 Zr1 C4_2 C5_2 -62.31(13) . . . . ? C4_2 Zr1 C4_2 C5_2 54.66(9) 2_556 . . . ? C3_2 Zr1 C4_2 C5_2 -113.00(14) . . . . ? C3_2 Zr1 C4_2 C5_2 62.66(11) 2_556 . . . ? C5_2 Zr1 C4_2 C5_2 81.63(11) 2_556 . . . ? C2_2 Zr1 C4_2 C5_2 101.25(10) 2_556 . . . ? C2_2 Zr1 C4_2 C5_2 -75.77(10) . . . . ? C1_2 Zr1 C4_2 C5_2 107.99(10) 2_556 . . . ? C1_2 Zr1 C4_2 C5_2 -36.19(9) . . . . ? C3_2 C4_2 C5_2 C1_2 -0.10(19) . . . . ? Zr1 C4_2 C5_2 C1_2 69.19(11) . . . . ? C3_2 C4_2 C5_2 Zr1 -69.29(11) . . . . ? C2_2 C1_2 C5_2 C4_2 -0.23(18) . . . . ? C6_2 C1_2 C5_2 C4_2 170.77(15) . . . . ? Zr1 C1_2 C5_2 C4_2 -65.32(11) . . . . ? C2_2 C1_2 C5_2 Zr1 65.09(11) . . . . ? C6_2 C1_2 C5_2 Zr1 -123.91(15) . . . . ? C1_1 Zr1 C5_2 C4_2 25.44(13) 2_556 . . . ? C1_1 Zr1 C5_2 C4_2 139.36(10) . . . . ? C4_2 Zr1 C5_2 C4_2 -122.48(10) 2_556 . . . ? C3_2 Zr1 C5_2 C4_2 38.03(9) . . . . ? C3_2 Zr1 C5_2 C4_2 -130.58(10) 2_556 . . . ? C5_2 Zr1 C5_2 C4_2 -88.70(11) 2_556 . . . ? C2_2 Zr1 C5_2 C4_2 -100.94(10) 2_556 . . . ? C2_2 Zr1 C5_2 C4_2 78.34(10) . . . . ? C1_2 Zr1 C5_2 C4_2 -76.09(10) 2_556 . . . ? C1_2 Zr1 C5_2 C4_2 115.38(14) . . . . ? C1_1 Zr1 C5_2 C1_2 -89.95(11) 2_556 . . . ? C1_1 Zr1 C5_2 C1_2 23.98(12) . . . . ? C4_2 Zr1 C5_2 C1_2 -115.38(14) . . . . ? C4_2 Zr1 C5_2 C1_2 122.14(10) 2_556 . . . ? C3_2 Zr1 C5_2 C1_2 -77.35(10) . . . . ? C3_2 Zr1 C5_2 C1_2 114.04(10) 2_556 . . . ? C5_2 Zr1 C5_2 C1_2 155.92(13) 2_556 . . . ? C2_2 Zr1 C5_2 C1_2 143.68(9) 2_556 . . . ? C2_2 Zr1 C5_2 C1_2 -37.04(9) . . . . ? C1_2 Zr1 C5_2 C1_2 168.53(7) 2_556 . . . ? C5_2 C1_2 C6_2 C9_2 70.0(2) . . . . ? C2_2 C1_2 C6_2 C9_2 -121.15(18) . . . . ? Zr1 C1_2 C6_2 C9_2 -22.09(19) . . . . ? C5_2 C1_2 C6_2 C8_2 -167.84(15) . . . . ? C2_2 C1_2 C6_2 C8_2 1.0(2) . . . . ? Zr1 C1_2 C6_2 C8_2 100.10(15) . . . . ? C5_2 C1_2 C6_2 C7_2 -49.6(2) . . . . ? C2_2 C1_2 C6_2 C7_2 119.32(18) . . . . ? Zr1 C1_2 C6_2 C7_2 -141.63(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.565 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.086 # Attachment '- 2.cif' data_kr395 _database_code_depnum_ccdc_archive 'CCDC 804815' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 Cr Zr' _chemical_formula_sum 'C30 H36 Cr Zr' _chemical_formula_weight 539.81 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' Cr Cr 0.3209 0.6236 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 16.780(5) _cell_length_b 19.128(5) _cell_length_c 7.402(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.303(14) _cell_angle_gamma 90.00 _cell_volume 2361.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9185 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 28.38 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8160 _exptl_absorpt_correction_T_max 0.9642 _exptl_absorpt_process_details 'Sadabs 2008/1 (Brucker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39926 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.38 _reflns_number_total 2931 _reflns_number_gt 2795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 ver. 2008.3 (Bruker AXS)' _computing_cell_refinement 'Saint+ ver. 7.53A (Bruker AXS)' _computing_data_reduction 'Saint+ ver. 7.53A (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP ver. 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0066P)^2^+19.6779P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2931 _refine_ls_number_parameters 185 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.0000 0.32232(2) 0.2500 0.01677(12) Uani 1 2 d S . . Cr1 Cr 0.0000 0.15800(4) 0.2500 0.0382(3) Uani 1 2 d SD . . C1_1 C 0.14504(19) 0.37636(17) 0.3214(4) 0.0201(6) Uani 1 1 d . . . C2_1 C 0.1357(2) 0.3264(2) 0.4587(4) 0.0248(7) Uani 1 1 d . A . H2_1 H 0.1661 0.2846 0.4787 0.030 Uiso 1 1 calc R . . C3_1 C 0.0743(2) 0.3483(2) 0.5608(5) 0.0275(8) Uani 1 1 d . A . H3_1 H 0.0566 0.3245 0.6617 0.033 Uiso 1 1 calc R . . C4_1 C 0.0440(2) 0.41149(19) 0.4875(5) 0.0264(7) Uani 1 1 d . A . H4_1 H 0.0019 0.4381 0.5293 0.032 Uiso 1 1 calc R . . C5_1 C 0.0871(2) 0.42864(17) 0.3399(5) 0.0227(7) Uani 1 1 d . A . H5_1 H 0.0785 0.4689 0.2650 0.027 Uiso 1 1 calc R . . C6_1 C 0.2118(2) 0.38168(18) 0.1980(5) 0.0222(7) Uani 1 1 d . A . C7_1 C 0.2547(3) 0.4516(2) 0.2356(6) 0.0374(9) Uani 1 1 d . . . H7A_1 H 0.2166 0.4900 0.2074 0.056 Uiso 1 1 calc R A . H7B_1 H 0.2987 0.4556 0.1596 0.056 Uiso 1 1 calc R . . H7C_1 H 0.2761 0.4540 0.3641 0.056 Uiso 1 1 calc R . . C8_1 C 0.1793(2) 0.3787(2) -0.0035(5) 0.0294(8) Uani 1 1 d . . . H8A_1 H 0.1518 0.3340 -0.0296 0.044 Uiso 1 1 calc R A . H8B_1 H 0.2238 0.3830 -0.0781 0.044 Uiso 1 1 calc R . . H8C_1 H 0.1414 0.4172 -0.0319 0.044 Uiso 1 1 calc R . . C9_1 C 0.2738(2) 0.3234(2) 0.2370(6) 0.0401(10) Uani 1 1 d . . . H9A_1 H 0.2933 0.3234 0.3667 0.060 Uiso 1 1 calc R A . H9B_1 H 0.3188 0.3314 0.1657 0.060 Uiso 1 1 calc R . . H9C_1 H 0.2489 0.2782 0.2035 0.060 Uiso 1 1 calc R . . C1_2 C 0.0518(5) 0.2362(4) 0.0951(11) 0.0238(10) Uani 0.50 1 d PDU A 1 C2_2 C -0.0044(5) 0.1946(4) -0.0220(8) 0.0359(9) Uani 0.50 1 d PDU A 1 H2_2 H -0.0511 0.2116 -0.0924 0.043 Uiso 0.50 1 calc PR A 1 C3_2 C 0.0220(4) 0.1243(4) -0.0141(8) 0.047(2) Uani 0.50 1 d PDU A 1 H3_2 H -0.0041 0.0863 -0.0785 0.056 Uiso 0.50 1 calc PR A 1 C4_2 C 0.0939(4) 0.1198(4) 0.1056(10) 0.045(2) Uani 0.50 1 d PDU A 1 H4_2 H 0.1238 0.0784 0.1349 0.054 Uiso 0.50 1 calc PR A 1 C5_2 C 0.1136(4) 0.1885(4) 0.1748(12) 0.0346(11) Uani 0.50 1 d PDU A 1 H5_2 H 0.1587 0.2006 0.2577 0.042 Uiso 0.50 1 calc PR A 1 C1_3 C -0.0554(5) 0.2299(4) 0.4321(10) 0.0238(10) Uani 0.50 1 d PDU A 2 C2_3 C 0.0080(5) 0.1944(4) 0.5300(8) 0.0359(9) Uani 0.50 1 d PDU A 2 H2_3 H 0.0434 0.2228 0.6076 0.043 Uiso 0.50 1 calc PR A 2 C3_3 C 0.0273(5) 0.1233(4) 0.5310(9) 0.051(2) Uani 0.50 1 d PDU A 2 H3_3 H 0.0731 0.1105 0.6112 0.062 Uiso 0.50 1 calc PR A 2 C4_3 C -0.0105(5) 0.0685(4) 0.4322(10) 0.061(3) Uani 0.50 1 d PDU A 2 H4_3 H 0.0138 0.0238 0.4505 0.073 Uiso 0.50 1 calc PR A 2 C5_3 C -0.0791(4) 0.0712(4) 0.3103(12) 0.054(2) Uani 0.50 1 d PDU A 2 H5_3 H -0.0959 0.0281 0.2547 0.065 Uiso 0.50 1 calc PR A 2 C6_3 C -0.1265(4) 0.1286(4) 0.2591(12) 0.043(2) Uani 0.50 1 d PDU A 2 H6_3 H -0.1724 0.1197 0.1753 0.052 Uiso 0.50 1 calc PR A 2 C7_3 C -0.1155(4) 0.1976(5) 0.3147(13) 0.0346(11) Uani 0.50 1 d PDU A 2 H7_3 H -0.1561 0.2286 0.2637 0.042 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0169(2) 0.0132(2) 0.0191(2) 0.000 -0.00256(15) 0.000 Cr1 0.0303(5) 0.0145(4) 0.0722(7) 0.000 0.0162(5) 0.000 C1_1 0.0187(15) 0.0228(16) 0.0176(14) -0.0029(12) -0.0030(12) -0.0038(12) C2_1 0.0212(16) 0.0315(18) 0.0203(15) 0.0037(14) -0.0045(12) -0.0031(14) C3_1 0.0260(17) 0.039(2) 0.0165(15) -0.0003(14) -0.0017(13) -0.0096(15) C4_1 0.0249(17) 0.0288(18) 0.0264(17) -0.0124(14) 0.0064(14) -0.0074(14) C5_1 0.0232(16) 0.0186(15) 0.0262(17) -0.0050(13) 0.0013(13) -0.0051(13) C6_1 0.0181(15) 0.0263(17) 0.0218(16) 0.0010(13) 0.0008(12) -0.0007(13) C7_1 0.036(2) 0.039(2) 0.039(2) -0.0065(18) 0.0126(17) -0.0141(18) C8_1 0.0228(17) 0.044(2) 0.0219(17) 0.0008(15) 0.0027(13) -0.0002(16) C9_1 0.0266(19) 0.047(2) 0.048(2) 0.017(2) 0.0103(17) 0.0112(18) C1_2 0.0206(16) 0.0220(17) 0.029(2) -0.009(2) 0.0055(15) 0.002(3) C2_2 0.0300(18) 0.0314(18) 0.047(2) 0.002(4) 0.0059(16) 0.001(4) C3_2 0.038(4) 0.038(4) 0.065(4) -0.022(3) 0.011(3) -0.007(3) C4_2 0.039(4) 0.032(3) 0.066(4) -0.009(3) 0.020(3) -0.002(3) C5_2 0.0284(17) 0.031(2) 0.046(2) -0.004(3) 0.0131(16) 0.001(3) C1_3 0.0206(16) 0.0220(17) 0.029(2) -0.009(2) 0.0055(15) 0.002(3) C2_3 0.0300(18) 0.0314(18) 0.047(2) 0.002(4) 0.0059(16) 0.001(4) C3_3 0.044(4) 0.039(4) 0.069(5) 0.020(4) -0.003(4) -0.001(3) C4_3 0.055(4) 0.043(4) 0.085(5) 0.007(4) 0.011(4) -0.003(4) C5_3 0.050(4) 0.039(4) 0.075(5) -0.003(4) 0.017(4) -0.010(3) C6_3 0.035(4) 0.042(4) 0.054(4) -0.012(3) 0.011(3) -0.011(3) C7_3 0.0284(17) 0.031(2) 0.046(2) -0.004(3) 0.0131(16) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C1_2 2.237(8) . ? Zr1 C1_2 2.237(8) 2 ? Zr1 C1_3 2.466(9) . ? Zr1 C1_3 2.466(9) 2 ? Zr1 C4_1 2.502(3) 2 ? Zr1 C4_1 2.502(3) . ? Zr1 C3_1 2.543(3) . ? Zr1 C3_1 2.543(3) 2 ? Zr1 C5_1 2.550(3) . ? Zr1 C5_1 2.550(3) 2 ? Zr1 C2_1 2.609(3) . ? Zr1 C2_1 2.609(3) 2 ? Cr1 C5_2 2.124(5) . ? Cr1 C5_2 2.124(5) 2 ? Cr1 C2_2 2.125(5) 2 ? Cr1 C2_2 2.125(5) . ? Cr1 C1_2 2.127(5) . ? Cr1 C1_2 2.127(5) 2 ? Cr1 C4_2 2.127(5) 2 ? Cr1 C4_2 2.127(5) . ? Cr1 C3_2 2.129(5) 2 ? Cr1 C3_2 2.129(5) . ? Cr1 C2_3 2.176(6) . ? Cr1 C2_3 2.176(6) 2 ? C1_1 C5_1 1.412(5) . ? C1_1 C2_1 1.417(5) . ? C1_1 C6_1 1.525(5) . ? C2_1 C3_1 1.407(5) . ? C2_1 H2_1 0.9500 . ? C3_1 C4_1 1.397(5) . ? C3_1 H3_1 0.9500 . ? C4_1 C5_1 1.414(5) . ? C4_1 H4_1 0.9500 . ? C5_1 H5_1 0.9500 . ? C6_1 C9_1 1.530(5) . ? C6_1 C7_1 1.530(5) . ? C6_1 C8_1 1.532(5) . ? C7_1 H7A_1 0.9800 . ? C7_1 H7B_1 0.9800 . ? C7_1 H7C_1 0.9800 . ? C8_1 H8A_1 0.9800 . ? C8_1 H8B_1 0.9800 . ? C8_1 H8C_1 0.9800 . ? C9_1 H9A_1 0.9800 . ? C9_1 H9B_1 0.9800 . ? C9_1 H9C_1 0.9800 . ? C1_2 C2_2 1.446(8) . ? C1_2 C5_2 1.457(8) . ? C2_2 C3_2 1.415(8) . ? C2_2 H2_2 0.9500 . ? C3_2 C4_2 1.418(8) . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.435(8) . ? C4_2 H4_2 0.9500 . ? C5_2 H5_2 0.9500 . ? C1_3 C2_3 1.396(7) . ? C1_3 C7_3 1.400(7) . ? C2_3 C3_3 1.398(7) . ? C2_3 H2_3 0.9500 . ? C3_3 C4_3 1.390(7) . ? C3_3 H3_3 0.9500 . ? C4_3 C5_3 1.384(7) . ? C4_3 H4_3 0.9500 . ? C5_3 C6_3 1.385(7) . ? C5_3 H5_3 0.9500 . ? C6_3 C7_3 1.389(7) . ? C6_3 H6_3 0.9500 . ? C7_3 H7_3 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_2 Zr1 C1_2 85.1(3) . 2 ? C1_2 Zr1 C1_3 86.72(13) . . ? C1_2 Zr1 C1_3 2.3(3) 2 . ? C1_2 Zr1 C1_3 2.3(3) . 2 ? C1_2 Zr1 C1_3 86.72(13) 2 2 ? C1_3 Zr1 C1_3 88.4(3) . 2 ? C1_2 Zr1 C4_1 104.1(2) . 2 ? C1_2 Zr1 C4_1 139.6(2) 2 2 ? C1_3 Zr1 C4_1 140.6(2) . 2 ? C1_3 Zr1 C4_1 101.81(19) 2 2 ? C1_2 Zr1 C4_1 139.6(2) . . ? C1_2 Zr1 C4_1 104.1(2) 2 . ? C1_3 Zr1 C4_1 101.81(19) . . ? C1_3 Zr1 C4_1 140.6(2) 2 . ? C4_1 Zr1 C4_1 94.03(18) 2 . ? C1_2 Zr1 C3_1 115.4(3) . . ? C1_2 Zr1 C3_1 81.9(2) 2 . ? C1_3 Zr1 C3_1 79.8(2) . . ? C1_3 Zr1 C3_1 117.3(2) 2 . ? C4_1 Zr1 C3_1 125.44(13) 2 . ? C4_1 Zr1 C3_1 32.15(13) . . ? C1_2 Zr1 C3_1 81.9(2) . 2 ? C1_2 Zr1 C3_1 115.4(3) 2 2 ? C1_3 Zr1 C3_1 117.3(2) . 2 ? C1_3 Zr1 C3_1 79.8(2) 2 2 ? C4_1 Zr1 C3_1 32.14(13) 2 2 ? C4_1 Zr1 C3_1 125.43(13) . 2 ? C3_1 Zr1 C3_1 157.42(18) . 2 ? C1_2 Zr1 C5_1 118.5(2) . . ? C1_2 Zr1 C5_1 134.2(2) 2 . ? C1_3 Zr1 C5_1 132.0(2) . . ? C1_3 Zr1 C5_1 118.34(19) 2 . ? C4_1 Zr1 C5_1 75.87(12) 2 . ? C4_1 Zr1 C5_1 32.49(11) . . ? C3_1 Zr1 C5_1 52.97(12) . . ? C3_1 Zr1 C5_1 106.86(12) 2 . ? C1_2 Zr1 C5_1 134.2(2) . 2 ? C1_2 Zr1 C5_1 118.5(2) 2 2 ? C1_3 Zr1 C5_1 118.34(19) . 2 ? C1_3 Zr1 C5_1 132.0(2) 2 2 ? C4_1 Zr1 C5_1 32.49(11) 2 2 ? C4_1 Zr1 C5_1 75.87(12) . 2 ? C3_1 Zr1 C5_1 106.86(12) . 2 ? C3_1 Zr1 C5_1 52.97(12) 2 2 ? C5_1 Zr1 C5_1 74.19(16) . 2 ? C1_2 Zr1 C2_1 87.9(3) . . ? C1_2 Zr1 C2_1 94.7(3) 2 . ? C1_3 Zr1 C2_1 93.1(2) . . ? C1_3 Zr1 C2_1 89.3(2) 2 . ? C4_1 Zr1 C2_1 124.53(12) 2 . ? C4_1 Zr1 C2_1 52.60(12) . . ? C3_1 Zr1 C2_1 31.67(11) . . ? C3_1 Zr1 C2_1 147.09(11) 2 . ? C5_1 Zr1 C2_1 51.96(12) . . ? C5_1 Zr1 C2_1 124.68(12) 2 . ? C1_2 Zr1 C2_1 94.6(3) . 2 ? C1_2 Zr1 C2_1 87.9(3) 2 2 ? C1_3 Zr1 C2_1 89.3(2) . 2 ? C1_3 Zr1 C2_1 93.1(2) 2 2 ? C4_1 Zr1 C2_1 52.61(12) 2 2 ? C4_1 Zr1 C2_1 124.54(12) . 2 ? C3_1 Zr1 C2_1 147.09(11) . 2 ? C3_1 Zr1 C2_1 31.67(11) 2 2 ? C5_1 Zr1 C2_1 124.68(12) . 2 ? C5_1 Zr1 C2_1 51.96(12) 2 2 ? C2_1 Zr1 C2_1 176.61(17) . 2 ? C5_2 Cr1 C5_2 148.1(5) . 2 ? C5_2 Cr1 C2_2 102.7(3) . 2 ? C5_2 Cr1 C2_2 66.4(3) 2 2 ? C5_2 Cr1 C2_2 66.4(3) . . ? C5_2 Cr1 C2_2 102.7(3) 2 . ? C2_2 Cr1 C2_2 141.6(5) 2 . ? C5_2 Cr1 C1_2 40.1(2) . . ? C5_2 Cr1 C1_2 112.3(4) 2 . ? C2_2 Cr1 C1_2 107.8(4) 2 . ? C2_2 Cr1 C1_2 39.8(2) . . ? C5_2 Cr1 C1_2 112.3(4) . 2 ? C5_2 Cr1 C1_2 40.1(2) 2 2 ? C2_2 Cr1 C1_2 39.8(2) 2 2 ? C2_2 Cr1 C1_2 107.8(4) . 2 ? C1_2 Cr1 C1_2 90.7(5) . 2 ? C5_2 Cr1 C4_2 163.8(3) . 2 ? C5_2 Cr1 C4_2 39.5(2) 2 2 ? C2_2 Cr1 C4_2 65.6(3) 2 2 ? C2_2 Cr1 C4_2 129.7(3) . 2 ? C1_2 Cr1 C4_2 151.8(3) . 2 ? C1_2 Cr1 C4_2 66.5(3) 2 2 ? C5_2 Cr1 C4_2 39.5(2) . . ? C5_2 Cr1 C4_2 163.8(3) 2 . ? C2_2 Cr1 C4_2 129.7(3) 2 . ? C2_2 Cr1 C4_2 65.6(3) . . ? C1_2 Cr1 C4_2 66.5(3) . . ? C1_2 Cr1 C4_2 151.8(3) 2 . ? C4_2 Cr1 C4_2 139.8(4) 2 . ? C5_2 Cr1 C3_2 125.1(3) . 2 ? C5_2 Cr1 C3_2 65.9(3) 2 2 ? C2_2 Cr1 C3_2 38.9(2) 2 2 ? C2_2 Cr1 C3_2 168.0(2) . 2 ? C1_2 Cr1 C3_2 146.1(4) . 2 ? C1_2 Cr1 C3_2 66.2(3) 2 2 ? C4_2 Cr1 C3_2 38.9(2) 2 2 ? C4_2 Cr1 C3_2 124.8(3) . 2 ? C5_2 Cr1 C3_2 65.9(3) . . ? C5_2 Cr1 C3_2 125.1(3) 2 . ? C2_2 Cr1 C3_2 168.0(2) 2 . ? C2_2 Cr1 C3_2 38.9(2) . . ? C1_2 Cr1 C3_2 66.2(3) . . ? C1_2 Cr1 C3_2 146.1(4) 2 . ? C4_2 Cr1 C3_2 124.8(3) 2 . ? C4_2 Cr1 C3_2 38.9(2) . . ? C3_2 Cr1 C3_2 144.7(4) 2 . ? C5_2 Cr1 C2_3 101.4(3) . . ? C5_2 Cr1 C2_3 68.1(4) 2 . ? C2_2 Cr1 C2_3 1.7(4) 2 . ? C2_2 Cr1 C2_3 142.1(2) . . ? C1_2 Cr1 C2_3 107.6(2) . . ? C1_2 Cr1 C2_3 41.2(4) 2 . ? C4_2 Cr1 C2_3 66.6(3) 2 . ? C4_2 Cr1 C2_3 128.1(3) . . ? C3_2 Cr1 C2_3 38.9(3) 2 . ? C3_2 Cr1 C2_3 166.5(3) . . ? C5_2 Cr1 C2_3 68.1(4) . 2 ? C5_2 Cr1 C2_3 101.4(3) 2 2 ? C2_2 Cr1 C2_3 142.1(2) 2 2 ? C2_2 Cr1 C2_3 1.7(4) . 2 ? C1_2 Cr1 C2_3 41.2(4) . 2 ? C1_2 Cr1 C2_3 107.6(2) 2 2 ? C4_2 Cr1 C2_3 128.1(3) 2 2 ? C4_2 Cr1 C2_3 66.6(3) . 2 ? C3_2 Cr1 C2_3 166.5(3) 2 2 ? C3_2 Cr1 C2_3 38.9(3) . 2 ? C2_3 Cr1 C2_3 142.7(4) . 2 ? C5_1 C1_1 C2_1 106.1(3) . . ? C5_1 C1_1 C6_1 124.7(3) . . ? C2_1 C1_1 C6_1 128.4(3) . . ? C5_1 C1_1 Zr1 70.59(18) . . ? C2_1 C1_1 Zr1 72.99(18) . . ? C6_1 C1_1 Zr1 128.8(2) . . ? C3_1 C2_1 C1_1 109.2(3) . . ? C3_1 C2_1 Zr1 71.59(19) . . ? C1_1 C2_1 Zr1 75.72(18) . . ? C3_1 C2_1 H2_1 125.4 . . ? C1_1 C2_1 H2_1 125.4 . . ? Zr1 C2_1 H2_1 119.0 . . ? C4_1 C3_1 C2_1 107.8(3) . . ? C4_1 C3_1 Zr1 72.31(19) . . ? C2_1 C3_1 Zr1 76.74(19) . . ? C4_1 C3_1 H3_1 126.1 . . ? C2_1 C3_1 H3_1 126.1 . . ? Zr1 C3_1 H3_1 116.9 . . ? C3_1 C4_1 C5_1 107.8(3) . . ? C3_1 C4_1 Zr1 75.5(2) . . ? C5_1 C4_1 Zr1 75.62(19) . . ? C3_1 C4_1 H4_1 126.1 . . ? C5_1 C4_1 H4_1 126.1 . . ? Zr1 C4_1 H4_1 115.0 . . ? C1_1 C5_1 C4_1 109.1(3) . . ? C1_1 C5_1 Zr1 77.93(19) . . ? C4_1 C5_1 Zr1 71.90(19) . . ? C1_1 C5_1 H5_1 125.5 . . ? C4_1 C5_1 H5_1 125.5 . . ? Zr1 C5_1 H5_1 116.6 . . ? C1_1 C6_1 C9_1 111.5(3) . . ? C1_1 C6_1 C7_1 108.1(3) . . ? C9_1 C6_1 C7_1 107.8(3) . . ? C1_1 C6_1 C8_1 112.0(3) . . ? C9_1 C6_1 C8_1 108.6(3) . . ? C7_1 C6_1 C8_1 108.7(3) . . ? C6_1 C7_1 H7A_1 109.5 . . ? C6_1 C7_1 H7B_1 109.5 . . ? H7A_1 C7_1 H7B_1 109.5 . . ? C6_1 C7_1 H7C_1 109.5 . . ? H7A_1 C7_1 H7C_1 109.5 . . ? H7B_1 C7_1 H7C_1 109.5 . . ? C6_1 C8_1 H8A_1 109.5 . . ? C6_1 C8_1 H8B_1 109.5 . . ? H8A_1 C8_1 H8B_1 109.5 . . ? C6_1 C8_1 H8C_1 109.5 . . ? H8A_1 C8_1 H8C_1 109.5 . . ? H8B_1 C8_1 H8C_1 109.5 . . ? C6_1 C9_1 H9A_1 109.5 . . ? C6_1 C9_1 H9B_1 109.5 . . ? H9A_1 C9_1 H9B_1 109.5 . . ? C6_1 C9_1 H9C_1 109.5 . . ? H9A_1 C9_1 H9C_1 109.5 . . ? H9B_1 C9_1 H9C_1 109.5 . . ? C2_2 C1_2 C5_2 106.6(3) . . ? C2_2 C1_2 Cr1 70.06(13) . . ? C5_2 C1_2 Cr1 69.88(13) . . ? C2_2 C1_2 Zr1 116.7(4) . . ? C5_2 C1_2 Zr1 123.6(4) . . ? Cr1 C1_2 Zr1 92.1(3) . . ? C3_2 C2_2 C1_2 108.5(3) . . ? C3_2 C2_2 Cr1 70.72(14) . . ? C1_2 C2_2 Cr1 70.17(14) . . ? C3_2 C2_2 H2_2 125.7 . . ? C1_2 C2_2 H2_2 125.7 . . ? Cr1 C2_2 H2_2 125.0 . . ? C2_2 C3_2 C4_2 108.9(3) . . ? C2_2 C3_2 Cr1 70.43(14) . . ? C4_2 C3_2 Cr1 70.48(14) . . ? C2_2 C3_2 H3_2 125.6 . . ? C4_2 C3_2 H3_2 125.6 . . ? Cr1 C3_2 H3_2 125.1 . . ? C3_2 C4_2 C5_2 108.3(3) . . ? C3_2 C4_2 Cr1 70.61(14) . . ? C5_2 C4_2 Cr1 70.16(14) . . ? C3_2 C4_2 H4_2 125.8 . . ? C5_2 C4_2 H4_2 125.8 . . ? Cr1 C4_2 H4_2 125.0 . . ? C4_2 C5_2 C1_2 107.6(3) . . ? C4_2 C5_2 Cr1 70.38(14) . . ? C1_2 C5_2 Cr1 70.05(14) . . ? C4_2 C5_2 H5_2 126.2 . . ? C1_2 C5_2 H5_2 126.2 . . ? Cr1 C5_2 H5_2 125.0 . . ? C2_3 C1_3 C7_3 124.3(5) . . ? C2_3 C1_3 Cr1 70.4(2) . . ? C7_3 C1_3 Cr1 70.6(2) . . ? C2_3 C1_3 Zr1 108.7(4) . . ? C7_3 C1_3 Zr1 105.4(4) . . ? Cr1 C1_3 Zr1 84.5(2) . . ? C1_3 C2_3 C3_3 129.7(5) . . ? C1_3 C2_3 Cr1 72.4(3) . . ? C3_3 C2_3 Cr1 71.6(3) . . ? C1_3 C2_3 H2_3 115.1 . . ? C3_3 C2_3 H2_3 115.1 . . ? Cr1 C2_3 H2_3 136.7 . . ? C4_3 C3_3 C2_3 129.7(6) . . ? C4_3 C3_3 Cr1 72.1(3) . . ? C2_3 C3_3 Cr1 71.0(3) . . ? C4_3 C3_3 H3_3 115.2 . . ? C2_3 C3_3 H3_3 115.2 . . ? Cr1 C3_3 H3_3 138.1 . . ? C5_3 C4_3 C3_3 127.9(6) . . ? C5_3 C4_3 Cr1 71.9(3) . . ? C3_3 C4_3 Cr1 70.9(3) . . ? C5_3 C4_3 H4_3 116.0 . . ? C3_3 C4_3 H4_3 116.0 . . ? Cr1 C4_3 H4_3 136.6 . . ? C4_3 C5_3 C6_3 128.2(6) . . ? C4_3 C5_3 Cr1 71.5(3) . . ? C6_3 C5_3 Cr1 71.7(3) . . ? C4_3 C5_3 H5_3 115.9 . . ? C6_3 C5_3 H5_3 115.9 . . ? Cr1 C5_3 H5_3 136.3 . . ? C5_3 C6_3 C7_3 128.3(6) . . ? C5_3 C6_3 Cr1 71.6(3) . . ? C7_3 C6_3 Cr1 70.7(3) . . ? C5_3 C6_3 H6_3 115.9 . . ? C7_3 C6_3 H6_3 115.9 . . ? Cr1 C6_3 H6_3 137.8 . . ? C6_3 C7_3 C1_3 131.8(6) . . ? C6_3 C7_3 Cr1 72.4(3) . . ? C1_3 C7_3 Cr1 72.1(3) . . ? C6_3 C7_3 H7_3 114.1 . . ? C1_3 C7_3 H7_3 114.1 . . ? Cr1 C7_3 H7_3 138.2 . . ? 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 C1_2 Zr1 C1_1 C5_1 158.6(3) . . . . ? C1_2 Zr1 C1_1 C5_1 -117.9(2) 2 . . . ? C1_3 Zr1 C1_1 C5_1 -115.7(2) . . . . ? C1_3 Zr1 C1_1 C5_1 156.4(2) 2 . . . ? C4_1 Zr1 C1_1 C5_1 54.6(2) 2 . . . ? C4_1 Zr1 C1_1 C5_1 -37.6(2) . . . . ? C3_1 Zr1 C1_1 C5_1 -78.2(2) . . . . ? C3_1 Zr1 C1_1 C5_1 78.0(2) 2 . . . ? C5_1 Zr1 C1_1 C5_1 23.0(3) 2 . . . ? C2_1 Zr1 C1_1 C5_1 -114.5(3) . . . . ? C2_1 Zr1 C1_1 C5_1 61.1(3) 2 . . . ? C1_2 Zr1 C1_1 C2_1 -86.8(3) . . . . ? C1_2 Zr1 C1_1 C2_1 -3.3(3) 2 . . . ? C1_3 Zr1 C1_1 C2_1 -1.2(3) . . . . ? C1_3 Zr1 C1_1 C2_1 -89.1(3) 2 . . . ? C4_1 Zr1 C1_1 C2_1 169.1(2) 2 . . . ? C4_1 Zr1 C1_1 C2_1 77.0(2) . . . . ? C3_1 Zr1 C1_1 C2_1 36.3(2) . . . . ? C3_1 Zr1 C1_1 C2_1 -167.5(2) 2 . . . ? C5_1 Zr1 C1_1 C2_1 114.5(3) . . . . ? C5_1 Zr1 C1_1 C2_1 137.6(2) 2 . . . ? C2_1 Zr1 C1_1 C2_1 175.7(2) 2 . . . ? C1_2 Zr1 C1_1 C6_1 39.2(3) . . . . ? C1_2 Zr1 C1_1 C6_1 122.7(3) 2 . . . ? C1_3 Zr1 C1_1 C6_1 124.8(3) . . . . ? C1_3 Zr1 C1_1 C6_1 36.9(3) 2 . . . ? C4_1 Zr1 C1_1 C6_1 -64.9(3) 2 . . . ? C4_1 Zr1 C1_1 C6_1 -157.0(3) . . . . ? C3_1 Zr1 C1_1 C6_1 162.3(3) . . . . ? C3_1 Zr1 C1_1 C6_1 -41.5(3) 2 . . . ? C5_1 Zr1 C1_1 C6_1 -119.4(4) . . . . ? C5_1 Zr1 C1_1 C6_1 -96.4(3) 2 . . . ? C2_1 Zr1 C1_1 C6_1 126.0(4) . . . . ? C2_1 Zr1 C1_1 C6_1 -58.3(4) 2 . . . ? C5_1 C1_1 C2_1 C3_1 -1.0(4) . . . . ? C6_1 C1_1 C2_1 C3_1 169.2(3) . . . . ? Zr1 C1_1 C2_1 C3_1 -64.3(2) . . . . ? C5_1 C1_1 C2_1 Zr1 63.3(2) . . . . ? C6_1 C1_1 C2_1 Zr1 -126.5(3) . . . . ? C1_2 Zr1 C2_1 C3_1 -151.3(3) . . . . ? C1_2 Zr1 C2_1 C3_1 -66.4(3) 2 . . . ? C1_3 Zr1 C2_1 C3_1 -64.7(3) . . . . ? C1_3 Zr1 C2_1 C3_1 -153.1(3) 2 . . . ? C4_1 Zr1 C2_1 C3_1 103.0(2) 2 . . . ? C4_1 Zr1 C2_1 C3_1 37.7(2) . . . . ? C3_1 Zr1 C2_1 C3_1 137.1(3) 2 . . . ? C5_1 Zr1 C2_1 C3_1 79.2(2) . . . . ? C5_1 Zr1 C2_1 C3_1 63.3(3) 2 . . . ? C1_1 C2_1 C3_1 C4_1 0.8(4) . . . . ? Zr1 C2_1 C3_1 C4_1 -66.2(2) . . . . ? C1_1 C2_1 C3_1 Zr1 67.0(2) . . . . ? C1_2 Zr1 C3_1 C4_1 146.0(2) . . . . ? C1_2 Zr1 C3_1 C4_1 -133.4(3) 2 . . . ? C1_3 Zr1 C3_1 C4_1 -132.6(3) . . . . ? C1_3 Zr1 C3_1 C4_1 144.5(2) 2 . . . ? C4_1 Zr1 C3_1 C4_1 14.0(3) 2 . . . ? C3_1 Zr1 C3_1 C4_1 8.51(19) 2 . . . ? C5_1 Zr1 C3_1 C4_1 38.2(2) . . . . ? C5_1 Zr1 C3_1 C4_1 -15.9(2) 2 . . . ? C2_1 Zr1 C3_1 C4_1 113.9(3) . . . . ? C2_1 Zr1 C3_1 C4_1 -60.2(3) 2 . . . ? C1_2 Zr1 C3_1 C2_1 32.0(3) . . . . ? C1_2 Zr1 C3_1 C2_1 112.7(3) 2 . . . ? C1_3 Zr1 C3_1 C2_1 113.4(3) . . . . ? C1_3 Zr1 C3_1 C2_1 30.6(3) 2 . . . ? C4_1 Zr1 C3_1 C2_1 -99.9(2) 2 . . . ? C4_1 Zr1 C3_1 C2_1 -113.9(3) . . . . ? C3_1 Zr1 C3_1 C2_1 -105.4(2) 2 . . . ? C5_1 Zr1 C3_1 C2_1 -75.7(2) . . . . ? C5_1 Zr1 C3_1 C2_1 -129.9(2) 2 . . . ? C2_1 Zr1 C3_1 C2_1 -174.1(3) 2 . . . ? C2_1 C3_1 C4_1 C5_1 -0.2(4) . . . . ? Zr1 C3_1 C4_1 C5_1 -69.4(2) . . . . ? C2_1 C3_1 C4_1 Zr1 69.2(2) . . . . ? C1_2 Zr1 C4_1 C3_1 -51.2(3) . . . . ? C1_2 Zr1 C4_1 C3_1 47.9(3) 2 . . . ? C1_3 Zr1 C4_1 C3_1 47.7(3) . . . . ? C1_3 Zr1 C4_1 C3_1 -54.4(3) 2 . . . ? C4_1 Zr1 C4_1 C3_1 -168.6(3) 2 . . . ? C3_1 Zr1 C4_1 C3_1 -176.00(10) 2 . . . ? C5_1 Zr1 C4_1 C3_1 -113.1(3) . . . . ? C5_1 Zr1 C4_1 C3_1 164.3(2) 2 . . . ? C2_1 Zr1 C4_1 C3_1 -37.2(2) . . . . ? C2_1 Zr1 C4_1 C3_1 145.1(2) 2 . . . ? C1_2 Zr1 C4_1 C5_1 61.8(3) . . . . ? C1_2 Zr1 C4_1 C5_1 160.9(3) 2 . . . ? C1_3 Zr1 C4_1 C5_1 160.8(3) . . . . ? C1_3 Zr1 C4_1 C5_1 58.6(3) 2 . . . ? C4_1 Zr1 C4_1 C5_1 -55.51(19) 2 . . . ? C3_1 Zr1 C4_1 C5_1 113.1(3) . . . . ? C3_1 Zr1 C4_1 C5_1 -62.9(3) 2 . . . ? C5_1 Zr1 C4_1 C5_1 -82.7(2) 2 . . . ? C2_1 Zr1 C4_1 C5_1 75.9(2) . . . . ? C2_1 Zr1 C4_1 C5_1 -101.8(2) 2 . . . ? C2_1 C1_1 C5_1 C4_1 0.9(4) . . . . ? C6_1 C1_1 C5_1 C4_1 -169.8(3) . . . . ? Zr1 C1_1 C5_1 C4_1 65.8(2) . . . . ? C2_1 C1_1 C5_1 Zr1 -64.9(2) . . . . ? C6_1 C1_1 C5_1 Zr1 124.4(3) . . . . ? C3_1 C4_1 C5_1 C1_1 -0.4(4) . . . . ? Zr1 C4_1 C5_1 C1_1 -69.8(2) . . . . ? C3_1 C4_1 C5_1 Zr1 69.3(2) . . . . ? C1_2 Zr1 C5_1 C1_1 -24.5(3) . . . . ? C1_2 Zr1 C5_1 C1_1 88.7(3) 2 . . . ? C1_3 Zr1 C5_1 C1_1 89.2(3) . . . . ? C1_3 Zr1 C5_1 C1_1 -27.1(3) 2 . . . ? C4_1 Zr1 C5_1 C1_1 -123.1(2) 2 . . . ? C4_1 Zr1 C5_1 C1_1 114.9(3) . . . . ? C3_1 Zr1 C5_1 C1_1 77.1(2) . . . . ? C3_1 Zr1 C5_1 C1_1 -114.4(2) 2 . . . ? C5_1 Zr1 C5_1 C1_1 -156.7(3) 2 . . . ? C2_1 Zr1 C5_1 C1_1 36.86(19) . . . . ? C2_1 Zr1 C5_1 C1_1 -143.73(19) 2 . . . ? C1_2 Zr1 C5_1 C4_1 -139.4(3) . . . . ? C1_2 Zr1 C5_1 C4_1 -26.2(4) 2 . . . ? C1_3 Zr1 C5_1 C4_1 -25.7(3) . . . . ? C1_3 Zr1 C5_1 C4_1 -142.0(3) 2 . . . ? C4_1 Zr1 C5_1 C4_1 122.0(2) 2 . . . ? C3_1 Zr1 C5_1 C4_1 -37.8(2) . . . . ? C3_1 Zr1 C5_1 C4_1 130.7(2) 2 . . . ? C5_1 Zr1 C5_1 C4_1 88.4(2) 2 . . . ? C2_1 Zr1 C5_1 C4_1 -78.1(2) . . . . ? C2_1 Zr1 C5_1 C4_1 101.4(2) 2 . . . ? C5_1 C1_1 C6_1 C9_1 168.7(3) . . . . ? C2_1 C1_1 C6_1 C9_1 0.0(5) . . . . ? Zr1 C1_1 C6_1 C9_1 -99.1(3) . . . . ? C5_1 C1_1 C6_1 C7_1 50.3(4) . . . . ? C2_1 C1_1 C6_1 C7_1 -118.3(4) . . . . ? Zr1 C1_1 C6_1 C7_1 142.5(3) . . . . ? C5_1 C1_1 C6_1 C8_1 -69.4(4) . . . . ? C2_1 C1_1 C6_1 C8_1 122.0(4) . . . . ? Zr1 C1_1 C6_1 C8_1 22.8(4) . . . . ? C5_2 Cr1 C1_2 C2_2 117.2(3) . . . . ? C5_2 Cr1 C1_2 C2_2 -83.0(3) 2 . . . ? C2_2 Cr1 C1_2 C2_2 -154.2(4) 2 . . . ? C1_2 Cr1 C1_2 C2_2 -117.6(5) 2 . . . ? C4_2 Cr1 C1_2 C2_2 -82.7(5) 2 . . . ? C4_2 Cr1 C1_2 C2_2 79.5(3) . . . . ? C3_2 Cr1 C1_2 C2_2 -162.5(4) 2 . . . ? C3_2 Cr1 C1_2 C2_2 36.9(2) . . . . ? C2_3 Cr1 C1_2 C2_2 -155.9(4) . . . . ? C2_3 Cr1 C1_2 C2_2 -1.2(6) 2 . . . ? C5_2 Cr1 C1_2 C5_2 159.8(3) 2 . . . ? C2_2 Cr1 C1_2 C5_2 88.6(4) 2 . . . ? C2_2 Cr1 C1_2 C5_2 -117.2(3) . . . . ? C1_2 Cr1 C1_2 C5_2 125.2(5) 2 . . . ? C4_2 Cr1 C1_2 C5_2 160.1(5) 2 . . . ? C4_2 Cr1 C1_2 C5_2 -37.7(2) . . . . ? C3_2 Cr1 C1_2 C5_2 80.3(4) 2 . . . ? C3_2 Cr1 C1_2 C5_2 -80.3(3) . . . . ? C2_3 Cr1 C1_2 C5_2 86.9(4) . . . . ? C2_3 Cr1 C1_2 C5_2 -118.4(6) 2 . . . ? C5_2 Cr1 C1_2 Zr1 -125.2(5) . . . . ? C5_2 Cr1 C1_2 Zr1 34.7(3) 2 . . . ? C2_2 Cr1 C1_2 Zr1 -36.5(2) 2 . . . ? C2_2 Cr1 C1_2 Zr1 117.6(5) . . . . ? C1_2 Cr1 C1_2 Zr1 0.0 2 . . . ? C4_2 Cr1 C1_2 Zr1 34.9(7) 2 . . . ? C4_2 Cr1 C1_2 Zr1 -162.8(4) . . . . ? C3_2 Cr1 C1_2 Zr1 -44.9(6) 2 . . . ? C3_2 Cr1 C1_2 Zr1 154.5(4) . . . . ? C2_3 Cr1 C1_2 Zr1 -38.2(5) . . . . ? C2_3 Cr1 C1_2 Zr1 116.5(7) 2 . . . ? C1_2 Zr1 C1_2 C2_2 68.70(17) 2 . . . ? C1_3 Zr1 C1_2 C2_2 70.3(5) . . . . ? C1_3 Zr1 C1_2 C2_2 -67(9) 2 . . . ? C4_1 Zr1 C1_2 C2_2 -71.3(3) 2 . . . ? C4_1 Zr1 C1_2 C2_2 174.7(3) . . . . ? C3_1 Zr1 C1_2 C2_2 147.4(3) . . . . ? C3_1 Zr1 C1_2 C2_2 -47.8(3) 2 . . . ? C5_1 Zr1 C1_2 C2_2 -152.7(3) . . . . ? C5_1 Zr1 C1_2 C2_2 -57.1(3) 2 . . . ? C2_1 Zr1 C1_2 C2_2 163.6(3) . . . . ? C2_1 Zr1 C1_2 C2_2 -18.7(3) 2 . . . ? C1_2 Zr1 C1_2 C5_2 -67.1(2) 2 . . . ? C1_3 Zr1 C1_2 C5_2 -65.5(5) . . . . ? C1_3 Zr1 C1_2 C5_2 157(9) 2 . . . ? C4_1 Zr1 C1_2 C5_2 152.9(3) 2 . . . ? C4_1 Zr1 C1_2 C5_2 38.9(4) . . . . ? C3_1 Zr1 C1_2 C5_2 11.5(4) . . . . ? C3_1 Zr1 C1_2 C5_2 176.3(4) 2 . . . ? C5_1 Zr1 C1_2 C5_2 71.5(3) . . . . ? C5_1 Zr1 C1_2 C5_2 167.0(3) 2 . . . ? C2_1 Zr1 C1_2 C5_2 27.7(4) . . . . ? C2_1 Zr1 C1_2 C5_2 -154.6(4) 2 . . . ? C1_2 Zr1 C1_2 Cr1 -0.001(2) 2 . . . ? C1_3 Zr1 C1_2 Cr1 1.6(4) . . . . ? C1_3 Zr1 C1_2 Cr1 -136(9) 2 . . . ? C4_1 Zr1 C1_2 Cr1 -140.0(2) 2 . . . ? C4_1 Zr1 C1_2 Cr1 106.0(3) . . . . ? C3_1 Zr1 C1_2 Cr1 78.7(3) . . . . ? C3_1 Zr1 C1_2 Cr1 -116.5(3) 2 . . . ? C5_1 Zr1 C1_2 Cr1 138.62(19) . . . . ? C5_1 Zr1 C1_2 Cr1 -125.8(2) 2 . . . ? C2_1 Zr1 C1_2 Cr1 94.9(3) . . . . ? C2_1 Zr1 C1_2 Cr1 -87.4(3) 2 . . . ? C5_2 C1_2 C2_2 C3_2 0.05(5) . . . . ? Cr1 C1_2 C2_2 C3_2 -60.59(14) . . . . ? Zr1 C1_2 C2_2 C3_2 -142.7(3) . . . . ? C5_2 C1_2 C2_2 Cr1 60.64(15) . . . . ? Zr1 C1_2 C2_2 Cr1 -82.1(3) . . . . ? C5_2 Cr1 C2_2 C3_2 80.3(3) . . . . ? C5_2 Cr1 C2_2 C3_2 -131.3(4) 2 . . . ? C2_2 Cr1 C2_2 C3_2 160.8(3) 2 . . . ? C1_2 Cr1 C2_2 C3_2 118.9(3) . . . . ? C1_2 Cr1 C2_2 C3_2 -172.6(4) 2 . . . ? C4_2 Cr1 C2_2 C3_2 -98.7(5) 2 . . . ? C4_2 Cr1 C2_2 C3_2 36.9(2) . . . . ? C3_2 Cr1 C2_2 C3_2 -114.8(18) 2 . . . ? C2_3 Cr1 C2_2 C3_2 158.3(6) . . . . ? C2_3 Cr1 C2_2 C3_2 -89(15) 2 . . . ? C5_2 Cr1 C2_2 C1_2 -38.7(2) . . . . ? C5_2 Cr1 C2_2 C1_2 109.7(4) 2 . . . ? C2_2 Cr1 C2_2 C1_2 41.8(3) 2 . . . ? C1_2 Cr1 C2_2 C1_2 68.5(5) 2 . . . ? C4_2 Cr1 C2_2 C1_2 142.4(4) 2 . . . ? C4_2 Cr1 C2_2 C1_2 -82.0(3) . . . . ? C3_2 Cr1 C2_2 C1_2 126.2(18) 2 . . . ? C3_2 Cr1 C2_2 C1_2 -118.9(3) . . . . ? C2_3 Cr1 C2_2 C1_2 39.3(6) . . . . ? C2_3 Cr1 C2_2 C1_2 152(15) 2 . . . ? C1_2 C2_2 C3_2 C4_2 0.02(5) . . . . ? Cr1 C2_2 C3_2 C4_2 -60.23(14) . . . . ? C1_2 C2_2 C3_2 Cr1 60.25(14) . . . . ? C5_2 Cr1 C3_2 C2_2 -81.8(3) . . . . ? C5_2 Cr1 C3_2 C2_2 63.6(5) 2 . . . ? C2_2 Cr1 C3_2 C2_2 -99(2) 2 . . . ? C1_2 Cr1 C3_2 C2_2 -37.7(2) . . . . ? C1_2 Cr1 C3_2 C2_2 12.8(7) 2 . . . ? C4_2 Cr1 C3_2 C2_2 112.2(4) 2 . . . ? C4_2 Cr1 C3_2 C2_2 -119.4(3) . . . . ? C3_2 Cr1 C3_2 C2_2 161.0(4) 2 . . . ? C2_3 Cr1 C3_2 C2_2 -102.5(11) . . . . ? C2_3 Cr1 C3_2 C2_2 2.6(7) 2 . . . ? C5_2 Cr1 C3_2 C4_2 37.6(2) . . . . ? C5_2 Cr1 C3_2 C4_2 -177.0(5) 2 . . . ? C2_2 Cr1 C3_2 C4_2 20(2) 2 . . . ? C2_2 Cr1 C3_2 C4_2 119.4(3) . . . . ? C1_2 Cr1 C3_2 C4_2 81.6(3) . . . . ? C1_2 Cr1 C3_2 C4_2 132.1(6) 2 . . . ? C4_2 Cr1 C3_2 C4_2 -128.4(5) 2 . . . ? C3_2 Cr1 C3_2 C4_2 -79.6(3) 2 . . . ? C2_3 Cr1 C3_2 C4_2 16.9(12) . . . . ? C2_3 Cr1 C3_2 C4_2 122.0(7) 2 . . . ? C2_2 C3_2 C4_2 C5_2 -0.08(9) . . . . ? Cr1 C3_2 C4_2 C5_2 -60.28(15) . . . . ? C2_2 C3_2 C4_2 Cr1 60.20(14) . . . . ? C5_2 Cr1 C4_2 C3_2 -118.8(3) . . . . ? C5_2 Cr1 C4_2 C3_2 8.8(13) 2 . . . ? C2_2 Cr1 C4_2 C3_2 -174.7(5) 2 . . . ? C2_2 Cr1 C4_2 C3_2 -36.9(2) . . . . ? C1_2 Cr1 C4_2 C3_2 -80.6(3) . . . . ? C1_2 Cr1 C4_2 C3_2 -119.2(8) 2 . . . ? C4_2 Cr1 C4_2 C3_2 86.5(3) 2 . . . ? C3_2 Cr1 C4_2 C3_2 136.3(5) 2 . . . ? C2_3 Cr1 C4_2 C3_2 -175.1(4) . . . . ? C2_3 Cr1 C4_2 C3_2 -35.4(5) 2 . . . ? C5_2 Cr1 C4_2 C5_2 127.6(13) 2 . . . ? C2_2 Cr1 C4_2 C5_2 -55.9(5) 2 . . . ? C2_2 Cr1 C4_2 C5_2 81.9(3) . . . . ? C1_2 Cr1 C4_2 C5_2 38.2(2) . . . . ? C1_2 Cr1 C4_2 C5_2 -0.4(8) 2 . . . ? C4_2 Cr1 C4_2 C5_2 -154.7(4) 2 . . . ? C3_2 Cr1 C4_2 C5_2 -104.9(4) 2 . . . ? C3_2 Cr1 C4_2 C5_2 118.8(3) . . . . ? C2_3 Cr1 C4_2 C5_2 -56.3(4) . . . . ? C2_3 Cr1 C4_2 C5_2 83.4(5) 2 . . . ? C3_2 C4_2 C5_2 C1_2 0.11(11) . . . . ? Cr1 C4_2 C5_2 C1_2 -60.45(15) . . . . ? C3_2 C4_2 C5_2 Cr1 60.56(15) . . . . ? C2_2 C1_2 C5_2 C4_2 -0.10(9) . . . . ? Cr1 C1_2 C5_2 C4_2 60.66(15) . . . . ? Zr1 C1_2 C5_2 C4_2 139.4(3) . . . . ? C2_2 C1_2 C5_2 Cr1 -60.76(15) . . . . ? Zr1 C1_2 C5_2 Cr1 78.7(4) . . . . ? C5_2 Cr1 C5_2 C4_2 -155.3(3) 2 . . . ? C2_2 Cr1 C5_2 C4_2 139.2(5) 2 . . . ? C2_2 Cr1 C5_2 C4_2 -79.7(3) . . . . ? C1_2 Cr1 C5_2 C4_2 -118.1(3) . . . . ? C1_2 Cr1 C5_2 C4_2 179.8(4) 2 . . . ? C4_2 Cr1 C5_2 C4_2 97.3(12) 2 . . . ? C3_2 Cr1 C5_2 C4_2 104.1(5) 2 . . . ? C3_2 Cr1 C5_2 C4_2 -37.1(2) . . . . ? C2_3 Cr1 C5_2 C4_2 138.1(3) . . . . ? C2_3 Cr1 C5_2 C4_2 -79.4(4) 2 . . . ? C5_2 Cr1 C5_2 C1_2 -37.2(3) 2 . . . ? C2_2 Cr1 C5_2 C1_2 -102.7(5) 2 . . . ? C2_2 Cr1 C5_2 C1_2 38.4(2) . . . . ? C1_2 Cr1 C5_2 C1_2 -62.1(5) 2 . . . ? C4_2 Cr1 C5_2 C1_2 -144.6(11) 2 . . . ? C4_2 Cr1 C5_2 C1_2 118.1(3) . . . . ? C3_2 Cr1 C5_2 C1_2 -137.8(4) 2 . . . ? C3_2 Cr1 C5_2 C1_2 81.0(3) . . . . ? C2_3 Cr1 C5_2 C1_2 -103.8(3) . . . . ? C2_3 Cr1 C5_2 C1_2 38.7(4) 2 . . . ? C5_2 Cr1 C1_3 C2_3 -73.7(4) . . . . ? C5_2 Cr1 C1_3 C2_3 131.7(6) 2 . . . ? C2_2 Cr1 C1_3 C2_3 1.0(7) 2 . . . ? C2_2 Cr1 C1_3 C2_3 -147.9(4) . . . . ? C1_2 Cr1 C1_3 C2_3 -110.5(3) . . . . ? C1_2 Cr1 C1_3 C2_3 -127(4) 2 . . . ? C4_2 Cr1 C1_3 C2_3 88.3(4) 2 . . . ? C4_2 Cr1 C1_3 C2_3 -65.2(8) . . . . ? C3_2 Cr1 C1_3 C2_3 43.4(4) 2 . . . ? C3_2 Cr1 C1_3 C2_3 -160.8(7) . . . . ? C2_3 Cr1 C1_3 C2_3 -149.7(4) 2 . . . ? C5_2 Cr1 C1_3 C7_3 146.9(5) . . . . ? C5_2 Cr1 C1_3 C7_3 -7.7(7) 2 . . . ? C2_2 Cr1 C1_3 C7_3 -138.4(8) 2 . . . ? C2_2 Cr1 C1_3 C7_3 72.7(5) . . . . ? C1_2 Cr1 C1_3 C7_3 110.1(4) . . . . ? C1_2 Cr1 C1_3 C7_3 93(4) 2 . . . ? C4_2 Cr1 C1_3 C7_3 -51.1(5) 2 . . . ? C4_2 Cr1 C1_3 C7_3 155.5(8) . . . . ? C3_2 Cr1 C1_3 C7_3 -95.9(5) 2 . . . ? C3_2 Cr1 C1_3 C7_3 59.8(8) . . . . ? C2_3 Cr1 C1_3 C7_3 -139.4(5) . . . . ? C2_3 Cr1 C1_3 C7_3 70.9(5) 2 . . . ? C5_2 Cr1 C1_3 Zr1 38.4(5) . . . . ? C5_2 Cr1 C1_3 Zr1 -116.2(6) 2 . . . ? C2_2 Cr1 C1_3 Zr1 113.1(7) 2 . . . ? C2_2 Cr1 C1_3 Zr1 -35.8(5) . . . . ? C1_2 Cr1 C1_3 Zr1 1.6(4) . . . . ? C1_2 Cr1 C1_3 Zr1 -15(4) 2 . . . ? C4_2 Cr1 C1_3 Zr1 -159.6(4) 2 . . . ? C4_2 Cr1 C1_3 Zr1 47.0(9) . . . . ? C3_2 Cr1 C1_3 Zr1 155.6(4) 2 . . . ? C3_2 Cr1 C1_3 Zr1 -48.7(8) . . . . ? C2_3 Cr1 C1_3 Zr1 112.1(4) . . . . ? C2_3 Cr1 C1_3 Zr1 -37.6(2) 2 . . . ? C1_2 Zr1 C1_3 C2_3 65.6(5) . . . . ? C1_2 Zr1 C1_3 C2_3 110(9) 2 . . . ? C1_3 Zr1 C1_3 C2_3 67.1(3) 2 . . . ? C4_1 Zr1 C1_3 C2_3 173.9(3) 2 . . . ? C4_1 Zr1 C1_3 C2_3 -74.5(4) . . . . ? C3_1 Zr1 C1_3 C2_3 -50.9(4) . . . . ? C3_1 Zr1 C1_3 C2_3 144.8(4) 2 . . . ? C5_1 Zr1 C1_3 C2_3 -60.7(4) . . . . ? C5_1 Zr1 C1_3 C2_3 -154.7(3) 2 . . . ? C2_1 Zr1 C1_3 C2_3 -22.1(4) . . . . ? C2_1 Zr1 C1_3 C2_3 160.3(4) 2 . . . ? C1_2 Zr1 C1_3 C7_3 -69.7(5) . . . . ? C1_2 Zr1 C1_3 C7_3 -25(8) 2 . . . ? C1_3 Zr1 C1_3 C7_3 -68.1(3) 2 . . . ? C4_1 Zr1 C1_3 C7_3 38.6(4) 2 . . . ? C4_1 Zr1 C1_3 C7_3 150.2(3) . . . . ? C3_1 Zr1 C1_3 C7_3 173.8(4) . . . . ? C3_1 Zr1 C1_3 C7_3 9.5(4) 2 . . . ? C5_1 Zr1 C1_3 C7_3 164.0(3) . . . . ? C5_1 Zr1 C1_3 C7_3 70.0(3) 2 . . . ? C2_1 Zr1 C1_3 C7_3 -157.4(4) . . . . ? C2_1 Zr1 C1_3 C7_3 25.0(4) 2 . . . ? C1_2 Zr1 C1_3 Cr1 -1.6(4) . . . . ? C1_2 Zr1 C1_3 Cr1 43(8) 2 . . . ? C1_3 Zr1 C1_3 Cr1 0.0 2 . . . ? C4_1 Zr1 C1_3 Cr1 106.8(3) 2 . . . ? C4_1 Zr1 C1_3 Cr1 -141.6(2) . . . . ? C3_1 Zr1 C1_3 Cr1 -118.1(3) . . . . ? C3_1 Zr1 C1_3 Cr1 77.6(3) 2 . . . ? C5_1 Zr1 C1_3 Cr1 -127.86(17) . . . . ? C5_1 Zr1 C1_3 Cr1 138.18(17) 2 . . . ? C2_1 Zr1 C1_3 Cr1 -89.2(2) . . . . ? C2_1 Zr1 C1_3 Cr1 93.1(2) 2 . . . ? C7_3 C1_3 C2_3 C3_3 2.0(3) . . . . ? Cr1 C1_3 C2_3 C3_3 -46.01(16) . . . . ? Zr1 C1_3 C2_3 C3_3 -122.8(3) . . . . ? C7_3 C1_3 C2_3 Cr1 48.0(3) . . . . ? Zr1 C1_3 C2_3 Cr1 -76.8(3) . . . . ? C5_2 Cr1 C2_3 C1_3 118.4(3) . . . . ? C5_2 Cr1 C2_3 C1_3 -30.1(4) 2 . . . ? C2_2 Cr1 C2_3 C1_3 -20(15) 2 . . . ? C2_2 Cr1 C2_3 C1_3 52.3(6) . . . . ? C1_2 Cr1 C2_3 C1_3 77.5(3) . . . . ? C1_2 Cr1 C2_3 C1_3 7.6(7) 2 . . . ? C4_2 Cr1 C2_3 C1_3 -73.0(4) 2 . . . ? C4_2 Cr1 C2_3 C1_3 151.1(4) . . . . ? C3_2 Cr1 C2_3 C1_3 -108.4(5) 2 . . . ? C3_2 Cr1 C2_3 C1_3 137.7(10) . . . . ? C2_3 Cr1 C2_3 C1_3 49.8(3) 2 . . . ? C5_2 Cr1 C2_3 C3_3 -97.2(4) . . . . ? C5_2 Cr1 C2_3 C3_3 114.2(5) 2 . . . ? C2_2 Cr1 C2_3 C3_3 125(15) 2 . . . ? C2_2 Cr1 C2_3 C3_3 -163.4(6) . . . . ? C1_2 Cr1 C2_3 C3_3 -138.2(3) . . . . ? C1_2 Cr1 C2_3 C3_3 151.9(7) 2 . . . ? C4_2 Cr1 C2_3 C3_3 71.3(4) 2 . . . ? C4_2 Cr1 C2_3 C3_3 -64.6(4) . . . . ? C3_2 Cr1 C2_3 C3_3 35.9(5) 2 . . . ? C3_2 Cr1 C2_3 C3_3 -78.0(11) . . . . ? C2_3 Cr1 C2_3 C3_3 -165.9(4) 2 . . . ? C1_3 C2_3 C3_3 C4_3 1.4(3) . . . . ? Cr1 C2_3 C3_3 C4_3 -44.9(4) . . . . ? C1_3 C2_3 C3_3 Cr1 46.28(17) . . . . ? C5_2 Cr1 C3_3 C4_3 -123.5(4) . . . . ? C5_2 Cr1 C3_3 C4_3 87.2(5) 2 . . . ? C2_2 Cr1 C3_3 C4_3 143.0(7) 2 . . . ? C2_2 Cr1 C3_3 C4_3 -121.1(15) . . . . ? C1_2 Cr1 C3_3 C4_3 -155.8(5) . . . . ? C1_2 Cr1 C3_3 C4_3 126.5(5) 2 . . . ? C4_2 Cr1 C3_3 C4_3 55.7(4) 2 . . . ? C4_2 Cr1 C3_3 C4_3 -82.7(4) . . . . ? C3_2 Cr1 C3_3 C4_3 65.8(8) 2 . . . ? C3_2 Cr1 C3_3 C4_3 -54.8(6) . . . . ? C1_2 Cr1 C3_3 C2_3 59.0(4) . . . . ? C1_2 Cr1 C3_3 C2_3 -18.7(5) 2 . . . ? C4_2 Cr1 C3_3 C2_3 -89.5(4) 2 . . . ? C4_2 Cr1 C3_3 C2_3 132.1(4) . . . . ? C3_2 Cr1 C3_3 C2_3 -79.4(8) 2 . . . ? C3_2 Cr1 C3_3 C2_3 160.1(5) . . . . ? C2_3 C3_3 C4_3 C5_3 -2.1(8) . . . . ? Cr1 C3_3 C4_3 C5_3 -46.6(5) . . . . ? C2_3 C3_3 C4_3 Cr1 44.6(3) . . . . ? C5_2 Cr1 C4_3 C5_3 -146.7(5) . . . . ? C5_2 Cr1 C4_3 C5_3 52.9(5) 2 . . . ? C2_2 Cr1 C4_3 C5_3 119.6(5) 2 . . . ? C2_2 Cr1 C4_3 C5_3 -53.3(8) . . . . ? C1_2 Cr1 C4_3 C5_3 -151.1(9) . . . . ? C1_2 Cr1 C4_3 C5_3 90.8(5) 2 . . . ? C4_2 Cr1 C4_3 C5_3 45.4(5) 2 . . . ? C4_2 Cr1 C4_3 C5_3 -111.4(5) . . . . ? C3_2 Cr1 C4_3 C5_3 104.8(7) 2 . . . ? C3_2 Cr1 C4_3 C5_3 -73.0(5) . . . . ? C2_3 Cr1 C4_3 C5_3 121.3(5) . . . . ? C2_3 Cr1 C4_3 C5_3 -50.7(7) 2 . . . ? C5_2 Cr1 C4_3 C3_3 70.4(5) . . . . ? C5_2 Cr1 C4_3 C3_3 -90.0(5) 2 . . . ? C2_2 Cr1 C4_3 C3_3 -23.3(5) 2 . . . ? C2_2 Cr1 C4_3 C3_3 163.8(6) . . . . ? C1_2 Cr1 C4_3 C3_3 66.0(10) . . . . ? C1_2 Cr1 C4_3 C3_3 -52.1(5) 2 . . . ? C4_2 Cr1 C4_3 C3_3 -97.5(5) 2 . . . ? C4_2 Cr1 C4_3 C3_3 105.8(4) . . . . ? C3_2 Cr1 C4_3 C3_3 -38.1(5) 2 . . . ? C3_2 Cr1 C4_3 C3_3 144.1(4) . . . . ? C2_3 Cr1 C4_3 C3_3 -21.6(3) . . . . ? C2_3 Cr1 C4_3 C3_3 166.4(4) 2 . . . ? C3_3 C4_3 C5_3 C6_3 -0.5(10) . . . . ? Cr1 C4_3 C5_3 C6_3 -46.8(6) . . . . ? C3_3 C4_3 C5_3 Cr1 46.3(5) . . . . ? C5_2 Cr1 C5_3 C4_3 59.9(8) . . . . ? C5_2 Cr1 C5_3 C4_3 -118.6(6) 2 . . . ? C2_2 Cr1 C5_3 C4_3 -55.3(5) 2 . . . ? C2_2 Cr1 C5_3 C4_3 150.3(5) . . . . ? C1_2 Cr1 C5_3 C4_3 154.1(8) . . . . ? C1_2 Cr1 C5_3 C4_3 -94.6(5) 2 . . . ? C4_2 Cr1 C5_3 C4_3 -89.6(7) 2 . . . ? C4_2 Cr1 C5_3 C4_3 77.9(5) . . . . ? C3_2 Cr1 C5_3 C4_3 -41.2(5) 2 . . . ? C3_2 Cr1 C5_3 C4_3 116.0(5) . . . . ? C2_3 Cr1 C5_3 C4_3 -53.7(5) . . . . ? C2_3 Cr1 C5_3 C4_3 151.1(5) 2 . . . ? C5_2 Cr1 C5_3 C6_3 -157.2(6) . . . . ? C5_2 Cr1 C5_3 C6_3 24.3(5) 2 . . . ? C2_2 Cr1 C5_3 C6_3 87.7(5) 2 . . . ? C2_2 Cr1 C5_3 C6_3 -66.7(5) . . . . ? C1_2 Cr1 C5_3 C6_3 -63.0(10) . . . . ? C1_2 Cr1 C5_3 C6_3 48.3(5) 2 . . . ? C4_2 Cr1 C5_3 C6_3 53.3(6) 2 . . . ? C4_2 Cr1 C5_3 C6_3 -139.1(5) . . . . ? C3_2 Cr1 C5_3 C6_3 101.7(5) 2 . . . ? C3_2 Cr1 C5_3 C6_3 -101.1(5) . . . . ? C2_3 Cr1 C5_3 C6_3 89.3(4) . . . . ? C2_3 Cr1 C5_3 C6_3 -65.9(5) 2 . . . ? C4_3 C5_3 C6_3 C7_3 1.6(10) . . . . ? Cr1 C5_3 C6_3 C7_3 -45.1(6) . . . . ? C4_3 C5_3 C6_3 Cr1 46.7(6) . . . . ? C5_2 Cr1 C6_3 C5_3 114.5(11) . . . . ? C5_2 Cr1 C6_3 C5_3 -137.6(8) 2 . . . ? C2_2 Cr1 C6_3 C5_3 -92.4(5) 2 . . . ? C2_2 Cr1 C6_3 C5_3 125.1(5) . . . . ? C1_2 Cr1 C6_3 C5_3 154.6(5) . . . . ? C1_2 Cr1 C6_3 C5_3 -129.3(5) 2 . . . ? C4_2 Cr1 C6_3 C5_3 -57.5(6) 2 . . . ? C4_2 Cr1 C6_3 C5_3 59.1(6) . . . . ? C3_2 Cr1 C6_3 C5_3 -58.9(5) 2 . . . ? C3_2 Cr1 C6_3 C5_3 85.4(5) . . . . ? C2_3 Cr1 C6_3 C5_3 -91.4(5) . . . . ? C2_3 Cr1 C6_3 C5_3 124.8(5) 2 . . . ? C5_2 Cr1 C6_3 C7_3 -101.6(11) . . . . ? C5_2 Cr1 C6_3 C7_3 6.3(8) 2 . . . ? C2_2 Cr1 C6_3 C7_3 51.5(6) 2 . . . ? C2_2 Cr1 C6_3 C7_3 -91.0(5) . . . . ? C1_2 Cr1 C6_3 C7_3 -61.5(5) . . . . ? C1_2 Cr1 C6_3 C7_3 14.6(6) 2 . . . ? C4_2 Cr1 C6_3 C7_3 86.5(7) 2 . . . ? C4_2 Cr1 C6_3 C7_3 -157.0(6) . . . . ? C3_2 Cr1 C6_3 C7_3 85.1(5) 2 . . . ? C3_2 Cr1 C6_3 C7_3 -130.6(5) . . . . ? C2_3 Cr1 C6_3 C7_3 52.5(5) . . . . ? C2_3 Cr1 C6_3 C7_3 -91.3(6) 2 . . . ? C5_3 C6_3 C7_3 C1_3 1.0(10) . . . . ? Cr1 C6_3 C7_3 C1_3 -44.4(6) . . . . ? C5_3 C6_3 C7_3 Cr1 45.4(6) . . . . ? C2_3 C1_3 C7_3 C6_3 -3.5(8) . . . . ? Cr1 C1_3 C7_3 C6_3 44.4(6) . . . . ? Zr1 C1_3 C7_3 C6_3 122.7(7) . . . . ? C2_3 C1_3 C7_3 Cr1 -47.9(3) . . . . ? Zr1 C1_3 C7_3 Cr1 78.3(3) . . . . ? C5_2 Cr1 C7_3 C6_3 157.4(6) . . . . ? C5_2 Cr1 C7_3 C6_3 -45(5) 2 . . . ? C2_2 Cr1 C7_3 C6_3 -122.0(6) 2 . . . ? C2_2 Cr1 C7_3 C6_3 95.5(5) . . . . ? C1_2 Cr1 C7_3 C6_3 135.4(4) . . . . ? C1_2 Cr1 C7_3 C6_3 -157.0(9) 2 . . . ? C4_2 Cr1 C7_3 C6_3 -44.4(5) 2 . . . ? C4_2 Cr1 C7_3 C6_3 68.6(11) . . . . ? C3_2 Cr1 C7_3 C6_3 -80.3(5) 2 . . . ? C3_2 Cr1 C7_3 C6_3 62.9(6) . . . . ? C2_3 Cr1 C7_3 C6_3 -121.9(5) . . . . ? C2_3 Cr1 C7_3 C6_3 94.3(5) 2 . . . ? C5_2 Cr1 C7_3 C1_3 -55.8(8) . . . . ? C5_2 Cr1 C7_3 C1_3 101(5) 2 . . . ? C2_2 Cr1 C7_3 C1_3 24.7(5) 2 . . . ? C2_2 Cr1 C7_3 C1_3 -117.8(4) . . . . ? C1_2 Cr1 C7_3 C1_3 -77.8(4) . . . . ? C1_2 Cr1 C7_3 C1_3 -10.2(7) 2 . . . ? C4_2 Cr1 C7_3 C1_3 102.3(6) 2 . . . ? C4_2 Cr1 C7_3 C1_3 -144.6(8) . . . . ? C3_2 Cr1 C7_3 C1_3 66.5(5) 2 . . . ? C3_2 Cr1 C7_3 C1_3 -150.3(4) . . . . ? C2_3 Cr1 C7_3 C1_3 24.9(3) . . . . ? C2_3 Cr1 C7_3 C1_3 -118.9(5) 2 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.159 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.104 # Attachment '- 3.cif' data_cu112 _database_code_depnum_ccdc_archive 'CCDC 804816' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 Mn Zr' _chemical_formula_sum 'C29 H35 Mn Zr' _chemical_formula_weight 529.73 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' Mn Mn 0.3368 0.7283 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 16.367(7) _cell_length_b 19.183(8) _cell_length_c 7.386(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.165(11) _cell_angle_gamma 90.00 _cell_volume 2300.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3158 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 25.79 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7175 _exptl_absorpt_correction_T_max 0.9605 _exptl_absorpt_process_details 'Sadabs 2008/1 (Brucker 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5075 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.91 _reflns_number_total 2201 _reflns_number_gt 2008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 ver. 2008.3 (Bruker AXS)' _computing_cell_refinement 'Saint+ ver. 7.53A (Bruker AXS)' _computing_data_reduction 'Saint+ ver. 7.53A (Bruker AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP ver. 5.1 (Bruker AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1048P)^2^+11.5254P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2201 _refine_ls_number_parameters 173 _refine_ls_number_restraints 171 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.107 _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 1.0000 0.17675(3) 0.2500 0.0115(2) Uani 1 2 d SU . . Mn1 Mn 1.0000 0.33654(5) 0.2500 0.0166(3) Uani 1 2 d SDU . . C1 C 1.0575(2) 0.26624(17) 0.0897(4) 0.0168(9) Uani 0.50 1 d PDU A 1 C2 C 1.1161(3) 0.3137(3) 0.1778(8) 0.0164(10) Uani 0.50 1 d PDU A 1 H2 H 1.1628 0.3013 0.2612 0.020 Uiso 0.50 1 calc PR A 1 C3 C 1.0940(4) 0.3819(3) 0.1220(9) 0.0199(18) Uani 0.50 1 d PDU A 1 H3 H 1.1232 0.4231 0.1609 0.024 Uiso 0.50 1 calc PR A 1 C4 C 1.0214(5) 0.3787(4) -0.0015(7) 0.021(2) Uani 0.50 1 d PDU A 1 H4 H 0.9921 0.4170 -0.0595 0.025 Uiso 0.50 1 calc PR A 1 C5 C 1.0003(4) 0.3079(4) -0.0224(5) 0.0175(9) Uani 0.50 1 d PDU A 1 H5 H 0.9544 0.2905 -0.1005 0.021 Uiso 0.50 1 calc PR A 1 C11 C 1.0575(2) 0.26624(17) 0.0897(4) 0.0168(9) Uani 0.50 1 d PDU A 2 C12 C 1.1174(2) 0.3041(3) 0.2044(7) 0.0164(10) Uani 0.50 1 d PDU A 2 H12 H 1.1594 0.2796 0.2789 0.020 Uiso 0.50 1 calc PR A 2 C13 C 1.1159(3) 0.3770(3) 0.2101(9) 0.0197(18) Uani 0.50 1 d PDU A 2 H13 H 1.1573 0.4011 0.2872 0.024 Uiso 0.50 1 calc PR A 2 C14 C 1.0548(4) 0.4146(3) 0.1049(9) 0.0253(19) Uani 0.50 1 d PDU A 2 H14 H 1.0534 0.4640 0.1124 0.030 Uiso 0.50 1 calc PR A 2 C15 C 0.9952(5) 0.3787(4) -0.0124(6) 0.022(2) Uani 0.50 1 d PDU A 2 H15 H 0.9535 0.4039 -0.0861 0.026 Uiso 0.50 1 calc PR A 2 C16 C 0.9970(4) 0.3054(4) -0.0212(5) 0.0175(9) Uani 0.50 1 d PDU A 2 H16 H 0.9569 0.2817 -0.1030 0.021 Uiso 0.50 1 calc PR A 2 C21 C 0.8511(3) 0.1218(2) 0.1733(5) 0.0146(9) Uani 1 1 d . . . C22 C 0.9110(3) 0.0697(2) 0.1545(6) 0.0157(9) Uani 1 1 d . A . H22 H 0.9200 0.0291 0.2277 0.019 Uiso 1 1 calc R . . C23 C 0.9551(3) 0.0884(2) 0.0086(6) 0.0180(9) Uani 1 1 d . A . H23 H 0.9984 0.0623 -0.0330 0.022 Uiso 1 1 calc R . . C24 C 0.9237(3) 0.1522(3) -0.0644(6) 0.0176(9) Uani 1 1 d . A . H24 H 0.9419 0.1768 -0.1636 0.021 Uiso 1 1 calc R . . C25 C 0.8604(3) 0.1728(2) 0.0370(6) 0.0172(10) Uani 1 1 d . A . H25 H 0.8288 0.2142 0.0175 0.021 Uiso 1 1 calc R . . C26 C 0.7825(3) 0.1157(2) 0.2961(5) 0.0154(9) Uani 1 1 d . A . C27 C 0.7389(3) 0.0451(3) 0.2567(7) 0.0252(11) Uani 1 1 d . . . H27A H 0.7178 0.0422 0.1268 0.038 Uiso 1 1 calc R A . H27B H 0.6931 0.0411 0.3297 0.038 Uiso 1 1 calc R . . H27C H 0.7782 0.0071 0.2885 0.038 Uiso 1 1 calc R . . C28 C 0.8173(3) 0.1188(3) 0.5000(6) 0.0209(10) Uani 1 1 d . . . H28A H 0.8549 0.0795 0.5295 0.031 Uiso 1 1 calc R A . H28B H 0.7719 0.1161 0.5746 0.031 Uiso 1 1 calc R . . H28C H 0.8472 0.1627 0.5253 0.031 Uiso 1 1 calc R . . C29 C 0.7185(3) 0.1741(3) 0.2564(7) 0.0242(11) Uani 1 1 d . . . H29A H 0.7439 0.2191 0.2930 0.036 Uiso 1 1 calc R A . H29B H 0.6721 0.1656 0.3255 0.036 Uiso 1 1 calc R . . H29C H 0.6987 0.1750 0.1257 0.036 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 0.0068(4) 0.0175(4) 0.0092(4) 0.000 -0.0036(2) 0.000 Mn1 0.0157(6) 0.0177(5) 0.0167(6) 0.000 0.0025(4) 0.000 C1 0.010(2) 0.024(2) 0.016(2) -0.0010(16) 0.0015(16) 0.0013(16) C2 0.016(2) 0.024(2) 0.011(2) 0.0049(19) 0.0058(16) -0.0042(19) C3 0.020(4) 0.024(3) 0.018(5) 0.003(4) 0.008(3) 0.001(3) C4 0.017(5) 0.025(3) 0.020(5) 0.004(4) 0.007(3) -0.002(4) C5 0.013(2) 0.024(2) 0.016(2) 0.0031(17) 0.0038(15) 0.0007(17) C11 0.010(2) 0.024(2) 0.016(2) -0.0010(16) 0.0015(16) 0.0013(16) C12 0.016(2) 0.024(2) 0.011(2) 0.0049(19) 0.0058(16) -0.0042(19) C13 0.020(4) 0.027(3) 0.014(4) 0.000(3) 0.011(3) -0.007(3) C14 0.024(5) 0.027(4) 0.026(5) 0.004(4) 0.008(4) -0.004(3) C15 0.012(5) 0.025(3) 0.029(5) 0.005(4) 0.003(3) 0.004(4) C16 0.013(2) 0.024(2) 0.016(2) 0.0031(17) 0.0038(15) 0.0007(17) C21 0.006(2) 0.027(2) 0.0097(19) -0.0017(17) -0.0041(15) -0.0003(18) C22 0.008(2) 0.018(2) 0.019(2) -0.0034(17) -0.0059(16) -0.0032(17) C23 0.012(2) 0.024(2) 0.017(2) -0.0073(18) -0.0017(16) -0.0018(18) C24 0.014(2) 0.028(2) 0.010(2) -0.0018(17) -0.0045(16) -0.0051(19) C25 0.012(2) 0.026(2) 0.013(2) -0.0004(17) -0.0025(17) -0.0010(18) C26 0.009(2) 0.027(2) 0.010(2) -0.0004(17) -0.0007(15) -0.0012(18) C27 0.018(2) 0.034(3) 0.023(2) -0.004(2) 0.0037(19) -0.010(2) C28 0.013(2) 0.037(3) 0.012(2) 0.0033(18) -0.0003(16) 0.000(2) C29 0.013(2) 0.036(3) 0.024(3) 0.008(2) 0.0033(19) 0.006(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 C11 2.348(4) 2_755 ? Zr1 C1 2.348(4) 2_755 ? Zr1 C1 2.348(4) . ? Zr1 C23 2.503(4) . ? Zr1 C23 2.503(4) 2_755 ? Zr1 C24 2.540(4) . ? Zr1 C24 2.540(4) 2_755 ? Zr1 C22 2.565(4) . ? Zr1 C22 2.565(4) 2_755 ? Zr1 C25 2.609(5) 2_755 ? Zr1 C25 2.609(5) . ? C1 C5 1.416(5) . ? C1 C2 1.420(5) . ? C2 C3 1.405(5) . ? C2 H2 0.9500 . ? C3 C4 1.407(5) . ? C3 H3 0.9500 . ? C4 C5 1.404(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C12 C13 1.399(5) . ? C12 H12 0.9500 . ? C13 C14 1.390(5) . ? C13 H13 0.9500 . ? C14 C15 1.402(5) . ? C14 H14 0.9500 . ? C15 C16 1.408(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C22 1.419(6) . ? C21 C25 1.425(6) . ? C21 C26 1.532(6) . ? C22 C23 1.416(6) . ? C22 H22 0.9500 . ? C23 C24 1.409(7) . ? C23 H23 0.9500 . ? C24 C25 1.409(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C29 1.537(6) . ? C26 C27 1.542(7) . ? C26 C28 1.543(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Zr1 C1 0.00(15) 2_755 2_755 ? C11 Zr1 C1 86.01(14) 2_755 . ? C1 Zr1 C1 86.01(14) 2_755 . ? C11 Zr1 C23 138.93(13) 2_755 . ? C1 Zr1 C23 138.93(13) 2_755 . ? C1 Zr1 C23 103.68(13) . . ? C11 Zr1 C23 103.68(13) 2_755 2_755 ? C1 Zr1 C23 103.68(13) 2_755 2_755 ? C1 Zr1 C23 138.93(13) . 2_755 ? C23 Zr1 C23 94.7(2) . 2_755 ? C11 Zr1 C24 114.48(14) 2_755 . ? C1 Zr1 C24 114.48(14) 2_755 . ? C1 Zr1 C24 81.75(14) . . ? C23 Zr1 C24 32.44(15) . . ? C23 Zr1 C24 126.37(16) 2_755 . ? C11 Zr1 C24 81.75(14) 2_755 2_755 ? C1 Zr1 C24 81.75(14) 2_755 2_755 ? C1 Zr1 C24 114.48(14) . 2_755 ? C23 Zr1 C24 126.37(16) . 2_755 ? C23 Zr1 C24 32.44(15) 2_755 2_755 ? C24 Zr1 C24 158.6(2) . 2_755 ? C11 Zr1 C22 118.32(13) 2_755 . ? C1 Zr1 C22 118.32(13) 2_755 . ? C1 Zr1 C22 134.12(13) . . ? C23 Zr1 C22 32.41(14) . . ? C23 Zr1 C22 76.13(15) 2_755 . ? C24 Zr1 C22 53.32(14) . . ? C24 Zr1 C22 107.51(15) 2_755 . ? C11 Zr1 C22 134.12(13) 2_755 2_755 ? C1 Zr1 C22 134.12(13) 2_755 2_755 ? C1 Zr1 C22 118.32(13) . 2_755 ? C23 Zr1 C22 76.13(15) . 2_755 ? C23 Zr1 C22 32.41(14) 2_755 2_755 ? C24 Zr1 C22 107.51(15) . 2_755 ? C24 Zr1 C22 53.31(14) 2_755 2_755 ? C22 Zr1 C22 73.7(2) . 2_755 ? C11 Zr1 C25 95.35(13) 2_755 2_755 ? C1 Zr1 C25 95.35(13) 2_755 2_755 ? C1 Zr1 C25 87.11(13) . 2_755 ? C23 Zr1 C25 124.54(15) . 2_755 ? C23 Zr1 C25 52.65(15) 2_755 2_755 ? C24 Zr1 C25 147.11(14) . 2_755 ? C24 Zr1 C25 31.73(14) 2_755 2_755 ? C22 Zr1 C25 124.56(14) . 2_755 ? C22 Zr1 C25 52.11(14) 2_755 2_755 ? C11 Zr1 C25 87.11(13) 2_755 . ? C1 Zr1 C25 87.11(13) 2_755 . ? C1 Zr1 C25 95.35(13) . . ? C23 Zr1 C25 52.65(15) . . ? C23 Zr1 C25 124.54(15) 2_755 . ? C24 Zr1 C25 31.73(14) . . ? C24 Zr1 C25 147.11(14) 2_755 . ? C22 Zr1 C25 52.11(14) . . ? C22 Zr1 C25 124.56(14) 2_755 . ? C25 Zr1 C25 176.6(2) 2_755 . ? C5 C1 C2 105.4(4) . . ? C5 C1 Zr1 115.5(4) . . ? C2 C1 Zr1 121.9(3) . . ? C3 C2 C1 109.1(4) . . ? C3 C2 H2 125.4 . . ? C1 C2 H2 125.4 . . ? C2 C3 C4 108.4(5) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? C5 C4 C3 106.8(6) . . ? C5 C4 H4 126.6 . . ? C3 C4 H4 126.6 . . ? C4 C5 C1 110.3(5) . . ? C4 C5 H5 124.9 . . ? C1 C5 H5 124.9 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.2(5) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 120.1(6) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 119.4 . . ? C22 C21 C25 106.1(4) . . ? C22 C21 C26 124.8(4) . . ? C25 C21 C26 128.4(4) . . ? C22 C21 Zr1 70.9(2) . . ? C25 C21 Zr1 72.7(3) . . ? C26 C21 Zr1 128.7(3) . . ? C23 C22 C21 108.7(4) . . ? C23 C22 Zr1 71.4(2) . . ? C21 C22 Zr1 77.6(3) . . ? C23 C22 H22 125.6 . . ? C21 C22 H22 125.6 . . ? Zr1 C22 H22 117.2 . . ? C24 C23 C22 108.3(4) . . ? C24 C23 Zr1 75.2(3) . . ? C22 C23 Zr1 76.2(2) . . ? C24 C23 H23 125.8 . . ? C22 C23 H23 125.8 . . ? Zr1 C23 H23 115.0 . . ? C25 C24 C23 107.3(4) . . ? C25 C24 Zr1 76.8(3) . . ? C23 C24 Zr1 72.4(2) . . ? C25 C24 H24 126.4 . . ? C23 C24 H24 126.4 . . ? Zr1 C24 H24 116.6 . . ? C24 C25 C21 109.6(4) . . ? C24 C25 Zr1 71.4(3) . . ? C21 C25 Zr1 75.9(3) . . ? C24 C25 H25 125.2 . . ? C21 C25 H25 125.2 . . ? Zr1 C25 H25 119.1 . . ? C21 C26 C29 111.3(4) . . ? C21 C26 C27 108.1(4) . . ? C29 C26 C27 108.4(4) . . ? C21 C26 C28 111.5(3) . . ? C29 C26 C28 108.5(4) . . ? C27 C26 C28 108.8(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 C11 Zr1 C1 C5 -66.1(2) 2_755 . . . ? C1 Zr1 C1 C5 -66.1(2) 2_755 . . . ? C23 Zr1 C1 C5 73.4(3) . . . . ? C23 Zr1 C1 C5 -172.4(3) 2_755 . . . ? C24 Zr1 C1 C5 49.4(3) . . . . ? C24 Zr1 C1 C5 -145.2(3) 2_755 . . . ? C22 Zr1 C1 C5 60.4(3) . . . . ? C22 Zr1 C1 C5 154.9(3) 2_755 . . . ? C25 Zr1 C1 C5 -161.7(3) 2_755 . . . ? C25 Zr1 C1 C5 20.6(3) . . . . ? C11 Zr1 C1 C2 63.9(2) 2_755 . . . ? C1 Zr1 C1 C2 63.9(2) 2_755 . . . ? C23 Zr1 C1 C2 -156.6(3) . . . . ? C23 Zr1 C1 C2 -42.4(3) 2_755 . . . ? C24 Zr1 C1 C2 179.4(3) . . . . ? C24 Zr1 C1 C2 -15.2(3) 2_755 . . . ? C22 Zr1 C1 C2 -169.6(3) . . . . ? C22 Zr1 C1 C2 -75.1(3) 2_755 . . . ? C25 Zr1 C1 C2 -31.7(3) 2_755 . . . ? C25 Zr1 C1 C2 150.6(3) . . . . ? C5 C1 C2 C3 0.8(2) . . . . ? Zr1 C1 C2 C3 -133.4(3) . . . . ? C1 C2 C3 C4 0.1(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C1 1.5(5) . . . . ? C2 C1 C5 C4 -1.4(4) . . . . ? Zr1 C1 C5 C4 136.1(4) . . . . ? C12 C13 C14 C15 -1.8(5) . . . . ? C13 C14 C15 C16 0.7(7) . . . . ? C11 Zr1 C21 C22 -159.4(2) 2_755 . . . ? C1 Zr1 C21 C22 -159.4(2) 2_755 . . . ? C1 Zr1 C21 C22 116.4(2) . . . . ? C23 Zr1 C21 C22 37.5(2) . . . . ? C23 Zr1 C21 C22 -55.7(3) 2_755 . . . ? C24 Zr1 C21 C22 78.5(3) . . . . ? C24 Zr1 C21 C22 -79.1(3) 2_755 . . . ? C22 Zr1 C21 C22 -24.2(3) 2_755 . . . ? C25 Zr1 C21 C22 -61.2(3) 2_755 . . . ? C25 Zr1 C21 C22 114.6(4) . . . . ? C11 Zr1 C21 C25 86.1(3) 2_755 . . . ? C1 Zr1 C21 C25 86.1(3) 2_755 . . . ? C1 Zr1 C21 C25 1.8(3) . . . . ? C23 Zr1 C21 C25 -77.1(3) . . . . ? C23 Zr1 C21 C25 -170.3(3) 2_755 . . . ? C24 Zr1 C21 C25 -36.1(3) . . . . ? C24 Zr1 C21 C25 166.3(3) 2_755 . . . ? C22 Zr1 C21 C25 -114.6(4) . . . . ? C22 Zr1 C21 C25 -138.7(3) 2_755 . . . ? C25 Zr1 C21 C25 -175.8(3) 2_755 . . . ? C11 Zr1 C21 C26 -39.7(4) 2_755 . . . ? C1 Zr1 C21 C26 -39.7(4) 2_755 . . . ? C1 Zr1 C21 C26 -123.9(3) . . . . ? C23 Zr1 C21 C26 157.2(4) . . . . ? C23 Zr1 C21 C26 64.0(4) 2_755 . . . ? C24 Zr1 C21 C26 -161.8(4) . . . . ? C24 Zr1 C21 C26 40.5(4) 2_755 . . . ? C22 Zr1 C21 C26 119.7(5) . . . . ? C22 Zr1 C21 C26 95.5(4) 2_755 . . . ? C25 Zr1 C21 C26 58.5(5) 2_755 . . . ? C25 Zr1 C21 C26 -125.7(5) . . . . ? C25 C21 C22 C23 -0.6(5) . . . . ? C26 C21 C22 C23 170.4(4) . . . . ? Zr1 C21 C22 C23 -65.2(3) . . . . ? C25 C21 C22 Zr1 64.6(3) . . . . ? C26 C21 C22 Zr1 -124.4(4) . . . . ? C11 Zr1 C22 C23 138.5(2) 2_755 . . . ? C1 Zr1 C22 C23 138.5(2) 2_755 . . . ? C1 Zr1 C22 C23 24.1(3) . . . . ? C23 Zr1 C22 C23 -123.2(3) 2_755 . . . ? C24 Zr1 C22 C23 37.8(3) . . . . ? C24 Zr1 C22 C23 -131.6(3) 2_755 . . . ? C22 Zr1 C22 C23 -89.7(3) 2_755 . . . ? C25 Zr1 C22 C23 -101.5(3) 2_755 . . . ? C25 Zr1 C22 C23 78.0(3) . . . . ? C11 Zr1 C22 C21 23.6(3) 2_755 . . . ? C1 Zr1 C22 C21 23.6(3) 2_755 . . . ? C1 Zr1 C22 C21 -90.8(3) . . . . ? C23 Zr1 C22 C21 -114.9(4) . . . . ? C23 Zr1 C22 C21 121.9(3) 2_755 . . . ? C24 Zr1 C22 C21 -77.1(3) . . . . ? C24 Zr1 C22 C21 113.6(2) 2_755 . . . ? C22 Zr1 C22 C21 155.4(3) 2_755 . . . ? C25 Zr1 C22 C21 143.6(2) 2_755 . . . ? C25 Zr1 C22 C21 -36.9(2) . . . . ? C21 C22 C23 C24 0.3(5) . . . . ? Zr1 C22 C23 C24 -69.0(3) . . . . ? C21 C22 C23 Zr1 69.3(3) . . . . ? C11 Zr1 C23 C24 51.0(3) 2_755 . . . ? C1 Zr1 C23 C24 51.0(3) 2_755 . . . ? C1 Zr1 C23 C24 -48.8(3) . . . . ? C23 Zr1 C23 C24 168.2(3) 2_755 . . . ? C24 Zr1 C23 C24 176.02(12) 2_755 . . . ? C22 Zr1 C23 C24 113.6(4) . . . . ? C22 Zr1 C23 C24 -165.1(3) 2_755 . . . ? C25 Zr1 C23 C24 -144.8(3) 2_755 . . . ? C25 Zr1 C23 C24 37.4(3) . . . . ? C11 Zr1 C23 C22 -62.6(3) 2_755 . . . ? C1 Zr1 C23 C22 -62.6(3) 2_755 . . . ? C1 Zr1 C23 C22 -162.4(2) . . . . ? C23 Zr1 C23 C22 54.6(2) 2_755 . . . ? C24 Zr1 C23 C22 -113.6(4) . . . . ? C24 Zr1 C23 C22 62.4(3) 2_755 . . . ? C22 Zr1 C23 C22 81.3(3) 2_755 . . . ? C25 Zr1 C23 C22 101.6(3) 2_755 . . . ? C25 Zr1 C23 C22 -76.1(3) . . . . ? C22 C23 C24 C25 0.1(5) . . . . ? Zr1 C23 C24 C25 -69.6(3) . . . . ? C22 C23 C24 Zr1 69.6(3) . . . . ? C11 Zr1 C24 C25 -32.7(3) 2_755 . . . ? C1 Zr1 C24 C25 -32.7(3) 2_755 . . . ? C1 Zr1 C24 C25 -114.4(3) . . . . ? C23 Zr1 C24 C25 113.2(4) . . . . ? C23 Zr1 C24 C25 98.5(3) 2_755 . . . ? C24 Zr1 C24 C25 104.4(3) 2_755 . . . ? C22 Zr1 C24 C25 75.4(3) . . . . ? C22 Zr1 C24 C25 128.4(3) 2_755 . . . ? C25 Zr1 C24 C25 174.1(4) 2_755 . . . ? C11 Zr1 C24 C23 -145.9(2) 2_755 . . . ? C1 Zr1 C24 C23 -145.9(2) 2_755 . . . ? C1 Zr1 C24 C23 132.4(3) . . . . ? C23 Zr1 C24 C23 -14.7(4) 2_755 . . . ? C24 Zr1 C24 C23 -8.8(2) 2_755 . . . ? C22 Zr1 C24 C23 -37.8(3) . . . . ? C22 Zr1 C24 C23 15.2(3) 2_755 . . . ? C25 Zr1 C24 C23 60.9(4) 2_755 . . . ? C25 Zr1 C24 C23 -113.2(4) . . . . ? C23 C24 C25 C21 -0.4(5) . . . . ? Zr1 C24 C25 C21 -66.9(3) . . . . ? C23 C24 C25 Zr1 66.5(3) . . . . ? C22 C21 C25 C24 0.6(5) . . . . ? C26 C21 C25 C24 -169.9(4) . . . . ? Zr1 C21 C25 C24 64.1(3) . . . . ? C22 C21 C25 Zr1 -63.4(3) . . . . ? C26 C21 C25 Zr1 126.1(4) . . . . ? C11 Zr1 C25 C24 150.5(3) 2_755 . . . ? C1 Zr1 C25 C24 150.5(3) 2_755 . . . ? C1 Zr1 C25 C24 64.8(3) . . . . ? C23 Zr1 C25 C24 -38.3(3) . . . . ? C23 Zr1 C25 C24 -104.8(3) 2_755 . . . ? C24 Zr1 C25 C24 -139.5(4) 2_755 . . . ? C22 Zr1 C25 C24 -79.6(3) . . . . ? C22 Zr1 C25 C24 -65.2(3) 2_755 . . . ? C11 Zr1 C25 C21 -92.8(3) 2_755 . . . ? C1 Zr1 C25 C21 -92.8(3) 2_755 . . . ? C1 Zr1 C25 C21 -178.5(2) . . . . ? C23 Zr1 C25 C21 78.3(3) . . . . ? C23 Zr1 C25 C21 11.8(3) 2_755 . . . ? C24 Zr1 C25 C21 116.6(4) . . . . ? C24 Zr1 C25 C21 -22.9(4) 2_755 . . . ? C22 Zr1 C25 C21 37.1(2) . . . . ? C22 Zr1 C25 C21 51.4(3) 2_755 . . . ? C22 C21 C26 C29 -168.7(4) . . . . ? C25 C21 C26 C29 0.2(6) . . . . ? Zr1 C21 C26 C29 98.7(4) . . . . ? C22 C21 C26 C27 -49.6(5) . . . . ? C25 C21 C26 C27 119.2(5) . . . . ? Zr1 C21 C26 C27 -142.2(3) . . . . ? C22 C21 C26 C28 70.0(5) . . . . ? C25 C21 C26 C28 -121.1(5) . . . . ? Zr1 C21 C26 C28 -22.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.790 _refine_diff_density_min -2.372 _refine_diff_density_rms 0.173