# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk7001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Zr' _chemical_formula_weight 405.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9219(3) _cell_length_b 8.0210(2) _cell_length_c 17.8888(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.216(2) _cell_angle_gamma 90.00 _cell_volume 1982.14(8) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4390 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9211 _exptl_absorpt_correction_T_max 0.9944 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12962 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3414 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The tBu group at C1 atom and one Cp group at Zr atom are disordered ower two position. Several restraints (SADI, SIMU, SAME and ISOR) were used in order to improve refinement stability. The hydrogens at C3 and C4 atoms were refined freely. ; _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^)+(0.0396P)^2^+11.0003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3414 _refine_ls_number_parameters 309 _refine_ls_number_restraints 185 _refine_ls_R_factor_all 0.0952 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.1762 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.070 _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 0.46585(5) 0.86747(8) 0.16719(4) 0.0377(2) Uani 1 1 d . . . C11 C 0.366(2) 0.745(4) 0.0323(15) 0.064(8) Uani 0.47(3) 1 d PDU A 1 H11 H 0.3749 0.7910 -0.0126 0.077 Uiso 0.47(3) 1 calc PR A 1 C12 C 0.4192(15) 0.611(4) 0.0788(19) 0.057(7) Uani 0.47(3) 1 d PDU A 1 H12 H 0.4688 0.5513 0.0703 0.068 Uiso 0.47(3) 1 calc PR A 1 C13 C 0.384(2) 0.582(3) 0.1404(14) 0.058(7) Uani 0.47(3) 1 d PDU A 1 H13 H 0.4065 0.5004 0.1809 0.070 Uiso 0.47(3) 1 calc PR A 1 C14 C 0.3095(17) 0.697(3) 0.1308(14) 0.057(6) Uani 0.47(3) 1 d PDU A 1 H14 H 0.2734 0.7044 0.1638 0.069 Uiso 0.47(3) 1 calc PR A 1 C15 C 0.2976(17) 0.799(3) 0.0635(16) 0.053(7) Uani 0.47(3) 1 d PDU A 1 H15 H 0.2527 0.8856 0.0434 0.064 Uiso 0.47(3) 1 calc PR A 1 C11A C 0.3391(16) 0.779(2) 0.0301(11) 0.049(5) Uani 0.53(3) 1 d PDU A 2 H11A H 0.3200 0.8554 -0.0131 0.058 Uiso 0.53(3) 1 calc PR A 2 C12A C 0.4158(12) 0.666(2) 0.0475(11) 0.043(4) Uani 0.53(3) 1 d PDU A 2 H12A H 0.4587 0.6551 0.0205 0.052 Uiso 0.53(3) 1 calc PR A 2 C13A C 0.4155(14) 0.571(2) 0.1137(14) 0.050(5) Uani 0.53(3) 1 d PDU A 2 H13A H 0.4576 0.4816 0.1379 0.060 Uiso 0.53(3) 1 calc PR A 2 C14A C 0.3422(18) 0.631(3) 0.1373(12) 0.063(6) Uani 0.53(3) 1 d PDU A 2 H14A H 0.3270 0.5886 0.1802 0.075 Uiso 0.53(3) 1 calc PR A 2 C15A C 0.2948(14) 0.763(3) 0.0869(16) 0.057(6) Uani 0.53(3) 1 d PDU A 2 H15A H 0.2440 0.8279 0.0902 0.069 Uiso 0.53(3) 1 calc PR A 2 C1 C 0.4805(6) 0.8073(10) 0.2972(5) 0.0504(19) Uani 1 1 d . A . C2 C 0.5653(5) 0.7917(10) 0.2975(5) 0.0469(18) Uani 1 1 d . A . C3 C 0.6317(6) 0.8185(11) 0.2619(5) 0.0453(18) Uani 1 1 d . A . H03 H 0.678(6) 0.901(11) 0.277(5) 0.06(3) Uiso 1 1 d . . . C4 C 0.6235(5) 0.7387(10) 0.1890(5) 0.0438(17) Uani 1 1 d . A . H04 H 0.601(7) 0.634(13) 0.192(6) 0.08(3) Uiso 1 1 d . . . C5 C 0.4364(6) 0.7667(11) 0.3596(5) 0.061(2) Uani 1 1 d D . . C6 C 0.3573(12) 0.888(2) 0.3553(12) 0.082(5) Uani 0.71(3) 1 d PDU A 1 H6A H 0.3310 0.8591 0.3955 0.122 Uiso 0.71(3) 1 calc PR A 1 H6B H 0.3063 0.8837 0.3020 0.122 Uiso 0.71(3) 1 calc PR A 1 H6C H 0.3838 1.0002 0.3655 0.122 Uiso 0.71(3) 1 calc PR A 1 C7 C 0.3994(15) 0.5870(16) 0.3496(11) 0.078(5) Uani 0.71(3) 1 d PDU A 1 H7A H 0.3716 0.5634 0.3895 0.117 Uiso 0.71(3) 1 calc PR A 1 H7B H 0.4527 0.5112 0.3570 0.117 Uiso 0.71(3) 1 calc PR A 1 H7C H 0.3503 0.5725 0.2959 0.117 Uiso 0.71(3) 1 calc PR A 1 C8 C 0.5188(10) 0.779(2) 0.4452(7) 0.071(5) Uani 0.71(3) 1 d PDU A 1 H8A H 0.4928 0.7543 0.4861 0.107 Uiso 0.71(3) 1 calc PR A 1 H8B H 0.5453 0.8913 0.4534 0.107 Uiso 0.71(3) 1 calc PR A 1 H8C H 0.5696 0.7001 0.4492 0.107 Uiso 0.71(3) 1 calc PR A 1 C6A C 0.3293(15) 0.819(6) 0.318(3) 0.084(12) Uani 0.29(3) 1 d PDU A 2 H6A1 H 0.2970 0.7450 0.2730 0.125 Uiso 0.29(3) 1 calc PR A 2 H6A2 H 0.3256 0.9324 0.2990 0.125 Uiso 0.29(3) 1 calc PR A 2 H6A3 H 0.2979 0.8109 0.3567 0.125 Uiso 0.29(3) 1 calc PR A 2 C7A C 0.441(4) 0.580(2) 0.376(3) 0.080(12) Uani 0.29(3) 1 d PDU A 2 H7A1 H 0.4040 0.5212 0.3262 0.119 Uiso 0.29(3) 1 calc PR A 2 H7A2 H 0.4131 0.5563 0.4159 0.119 Uiso 0.29(3) 1 calc PR A 2 H7A3 H 0.5074 0.5428 0.3958 0.119 Uiso 0.29(3) 1 calc PR A 2 C8A C 0.491(3) 0.864(6) 0.436(2) 0.101(13) Uani 0.29(3) 1 d PDU A 2 H8A1 H 0.4643 0.8400 0.4762 0.151 Uiso 0.29(3) 1 calc PR A 2 H8A2 H 0.4863 0.9819 0.4240 0.151 Uiso 0.29(3) 1 calc PR A 2 H8A3 H 0.5590 0.8307 0.4564 0.151 Uiso 0.29(3) 1 calc PR A 2 C16 C 0.3843(7) 1.1417(11) 0.1255(8) 0.073(3) Uani 1 1 d . A . H16 H 0.3163 1.1402 0.1047 0.088 Uiso 1 1 calc R . . C17 C 0.4420(8) 1.1255(11) 0.0813(6) 0.071(3) Uani 1 1 d . A . H17 H 0.4201 1.1142 0.0249 0.085 Uiso 1 1 calc R . . C18 C 0.5363(7) 1.1286(11) 0.1335(7) 0.066(3) Uani 1 1 d . A . H18 H 0.5909 1.1156 0.1200 0.079 Uiso 1 1 calc R . . C19 C 0.5367(8) 1.1544(10) 0.2105(6) 0.070(3) Uani 1 1 d . A . H19 H 0.5919 1.1657 0.2582 0.084 Uiso 1 1 calc R . . C20 C 0.4431(10) 1.1604(10) 0.2048(7) 0.077(3) Uani 1 1 d . A . H20 H 0.4225 1.1749 0.2480 0.093 Uiso 1 1 calc R . . C21 C 0.6946(5) 0.7582(9) 0.1502(4) 0.0409(16) Uani 1 1 d . . . C22 C 0.7044(5) 0.6299(10) 0.1017(4) 0.0464(17) Uani 1 1 d . A . H22 H 0.6667 0.5331 0.0950 0.056 Uiso 1 1 calc R . . C23 C 0.7694(6) 0.6421(12) 0.0625(5) 0.055(2) Uani 1 1 d . . . H23 H 0.7745 0.5552 0.0291 0.067 Uiso 1 1 calc R A . C24 C 0.8261(6) 0.7835(13) 0.0735(5) 0.059(2) Uani 1 1 d . A . H24 H 0.8711 0.7916 0.0485 0.071 Uiso 1 1 calc R . . C25 C 0.8169(6) 0.9106(11) 0.1204(5) 0.057(2) Uani 1 1 d . . . H25 H 0.8543 1.0076 0.1262 0.068 Uiso 1 1 calc R A . C26 C 0.7527(5) 0.8985(10) 0.1597(5) 0.0459(18) Uani 1 1 d . A . H26 H 0.7484 0.9862 0.1931 0.055 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 0.0383(4) 0.0294(4) 0.0419(4) 0.0009(3) 0.0113(3) -0.0003(3) C11 0.061(11) 0.063(12) 0.065(10) -0.011(8) 0.020(8) 0.000(8) C12 0.061(9) 0.051(10) 0.058(10) -0.011(8) 0.023(8) 0.000(7) C13 0.062(10) 0.044(9) 0.066(10) -0.003(7) 0.020(8) -0.006(8) C14 0.053(9) 0.052(10) 0.065(10) 0.004(8) 0.020(7) -0.006(7) C15 0.054(10) 0.043(9) 0.053(10) 0.011(8) 0.010(7) -0.005(7) C11A 0.048(9) 0.028(7) 0.057(8) -0.001(6) 0.005(6) 0.012(6) C12A 0.052(8) 0.036(8) 0.034(7) -0.003(6) 0.007(6) -0.004(6) C13A 0.053(8) 0.035(7) 0.056(9) 0.006(7) 0.015(7) -0.017(6) C14A 0.053(9) 0.060(10) 0.073(9) -0.005(7) 0.021(7) -0.013(8) C15A 0.045(8) 0.062(10) 0.060(10) 0.006(8) 0.014(7) -0.008(7) C1 0.051(5) 0.048(5) 0.052(5) 0.007(4) 0.020(4) 0.008(4) C2 0.047(4) 0.042(4) 0.045(4) 0.004(4) 0.009(3) -0.003(3) C3 0.041(4) 0.050(5) 0.044(4) 0.001(4) 0.014(3) 0.005(4) C4 0.041(4) 0.036(4) 0.055(5) 0.006(4) 0.019(4) 0.001(3) C5 0.055(5) 0.076(6) 0.066(6) 0.011(5) 0.037(5) 0.013(5) C6 0.083(8) 0.089(9) 0.086(9) 0.005(7) 0.047(7) 0.016(7) C7 0.081(9) 0.085(8) 0.073(8) 0.011(6) 0.036(7) -0.008(6) C8 0.076(7) 0.083(9) 0.067(7) 0.001(6) 0.042(6) -0.002(6) C6A 0.085(14) 0.092(15) 0.087(14) -0.002(9) 0.047(10) 0.000(9) C7A 0.080(14) 0.086(14) 0.076(14) 0.006(9) 0.034(10) 0.004(9) C8A 0.102(15) 0.107(16) 0.102(15) -0.005(10) 0.049(10) 0.001(10) C16 0.058(5) 0.038(5) 0.114(9) 0.003(6) 0.022(6) 0.013(4) C17 0.107(8) 0.036(5) 0.055(5) 0.012(4) 0.014(5) 0.006(5) C18 0.062(5) 0.041(5) 0.103(8) 0.027(5) 0.042(5) 0.008(4) C19 0.082(7) 0.032(5) 0.068(6) -0.002(4) -0.004(5) -0.010(4) C20 0.138(10) 0.028(5) 0.090(8) 0.000(5) 0.070(8) 0.011(5) C21 0.039(4) 0.039(4) 0.038(4) 0.005(3) 0.007(3) 0.004(3) C22 0.043(4) 0.047(4) 0.045(4) -0.001(4) 0.012(3) 0.006(4) C23 0.057(5) 0.064(5) 0.041(4) -0.007(4) 0.014(4) 0.016(4) C24 0.053(5) 0.081(7) 0.048(5) 0.006(5) 0.024(4) 0.008(5) C25 0.055(5) 0.058(5) 0.060(5) 0.009(4) 0.025(4) -0.002(4) C26 0.051(4) 0.039(4) 0.050(4) -0.005(4) 0.023(4) 0.003(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 2.304(8) . ? Zr1 C2 2.321(7) . ? Zr1 C3 2.446(8) . ? Zr1 C4 2.461(7) . ? Zr1 C16 2.488(9) . ? Zr1 C20 2.502(8) . ? Zr1 C11 2.51(3) . ? Zr1 C18 2.516(8) . ? Zr1 C17 2.522(9) . ? Zr1 C19 2.529(8) . ? Zr1 C12 2.53(2) . ? Zr1 C15A 2.55(2) . ? C11 C15 1.403(14) . ? C11 C12 1.407(14) . ? C11 H11 0.9400 . ? C12 C13 1.407(14) . ? C12 H12 0.9400 . ? C13 C14 1.402(14) . ? C13 H13 0.9400 . ? C14 C15 1.409(14) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C11A C12A 1.403(13) . ? C11A C15A 1.412(13) . ? C11A H11A 0.9400 . ? C12A C13A 1.410(13) . ? C12A H12A 0.9400 . ? C13A C14A 1.400(14) . ? C13A H13A 0.9400 . ? C14A C15A 1.400(14) . ? C14A H14A 0.9400 . ? C15A H15A 0.9400 . ? C1 C2 1.269(10) . ? C1 C5 1.530(11) . ? C2 C3 1.383(11) . ? C3 C4 1.415(11) . ? C3 H03 0.92(9) . ? C4 C21 1.479(10) . ? C4 H04 0.91(10) . ? C5 C6 1.510(11) . ? C5 C8A 1.515(16) . ? C5 C7A 1.524(16) . ? C5 C7 1.529(12) . ? C5 C6A 1.542(15) . ? C5 C8 1.563(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C6A H6A3 0.9700 . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C7A H7A3 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C16 C20 1.365(15) . ? C16 C17 1.378(14) . ? C16 H16 0.9400 . ? C17 C18 1.364(13) . ? C17 H17 0.9400 . ? C18 C19 1.391(14) . ? C18 H18 0.9400 . ? C19 C20 1.362(14) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.390(10) . ? C21 C26 1.392(10) . ? C22 C23 1.398(11) . ? C22 H22 0.9400 . ? C23 C24 1.384(13) . ? C23 H23 0.9400 . ? C24 C25 1.360(12) . ? C24 H24 0.9400 . ? C25 C26 1.391(10) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? 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 Zr1 C2 31.8(3) . . ? C1 Zr1 C3 65.3(3) . . ? C2 Zr1 C3 33.6(3) . . ? C1 Zr1 C4 91.8(3) . . ? C2 Zr1 C4 61.4(3) . . ? C3 Zr1 C4 33.5(3) . . ? C1 Zr1 C16 109.7(4) . . ? C2 Zr1 C16 125.9(3) . . ? C3 Zr1 C16 127.0(3) . . ? C4 Zr1 C16 138.5(3) . . ? C1 Zr1 C20 84.0(3) . . ? C2 Zr1 C20 94.4(4) . . ? C3 Zr1 C20 99.8(4) . . ? C4 Zr1 C20 124.8(4) . . ? C16 Zr1 C20 31.7(3) . . ? C1 Zr1 C11 133.2(6) . . ? C2 Zr1 C11 141.7(8) . . ? C3 Zr1 C11 132.9(8) . . ? C4 Zr1 C11 99.9(8) . . ? C16 Zr1 C11 90.8(8) . . ? C20 Zr1 C11 122.4(8) . . ? C1 Zr1 C18 121.8(3) . . ? C2 Zr1 C18 107.0(3) . . ? C3 Zr1 C18 83.9(3) . . ? C4 Zr1 C18 85.8(3) . . ? C16 Zr1 C18 52.7(3) . . ? C20 Zr1 C18 52.7(3) . . ? C11 Zr1 C18 104.3(6) . . ? C1 Zr1 C17 136.5(3) . . ? C2 Zr1 C17 135.8(3) . . ? C3 Zr1 C17 115.3(3) . . ? C4 Zr1 C17 110.3(3) . . ? C16 Zr1 C17 31.9(3) . . ? C20 Zr1 C17 52.5(3) . . ? C11 Zr1 C17 80.8(7) . . ? C18 Zr1 C17 31.4(3) . . ? C1 Zr1 C19 90.7(3) . . ? C2 Zr1 C19 84.0(3) . . ? C3 Zr1 C19 74.8(3) . . ? C4 Zr1 C19 94.0(3) . . ? C16 Zr1 C19 52.2(3) . . ? C20 Zr1 C19 31.4(3) . . ? C11 Zr1 C19 132.8(7) . . ? C18 Zr1 C19 32.0(3) . . ? C17 Zr1 C19 52.1(3) . . ? C1 Zr1 C12 111.1(9) . . ? C2 Zr1 C12 109.6(8) . . ? C3 Zr1 C12 105.6(6) . . ? C4 Zr1 C12 77.2(5) . . ? C16 Zr1 C12 123.0(8) . . ? C20 Zr1 C12 154.1(7) . . ? C11 Zr1 C12 32.4(4) . . ? C18 Zr1 C12 124.7(9) . . ? C17 Zr1 C12 110.2(9) . . ? C19 Zr1 C12 156.5(8) . . ? C1 Zr1 C15A 101.1(6) . . ? C2 Zr1 C15A 127.1(7) . . ? C3 Zr1 C15A 150.8(7) . . ? C4 Zr1 C15A 130.1(5) . . ? C16 Zr1 C15A 81.3(6) . . ? C20 Zr1 C15A 104.5(6) . . ? C11 Zr1 C15A 39.2(7) . . ? C18 Zr1 C15A 123.9(7) . . ? C17 Zr1 C15A 92.6(7) . . ? C19 Zr1 C15A 133.2(6) . . ? C12 Zr1 C15A 53.2(7) . . ? C15 C11 C12 109.5(14) . . ? C15 C11 Zr1 75.7(15) . . ? C12 C11 Zr1 74.6(14) . . ? C15 C11 H11 125.2 . . ? C12 C11 H11 125.2 . . ? Zr1 C11 H11 116.3 . . ? C11 C12 C13 107.0(14) . . ? C11 C12 Zr1 72.9(14) . . ? C13 C12 Zr1 74.9(13) . . ? C11 C12 H12 126.5 . . ? C13 C12 H12 126.5 . . ? Zr1 C12 H12 117.8 . . ? C14 C13 C12 108.1(15) . . ? C14 C13 Zr1 74.7(12) . . ? C12 C13 Zr1 73.0(12) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? Zr1 C13 H13 118.3 . . ? C13 C14 C15 108.9(15) . . ? C13 C14 Zr1 73.6(12) . . ? C15 C14 Zr1 73.5(13) . . ? C13 C14 H14 125.6 . . ? C15 C14 H14 125.6 . . ? Zr1 C14 H14 119.2 . . ? C11 C15 C14 106.5(14) . . ? C11 C15 Zr1 72.1(15) . . ? C14 C15 Zr1 74.5(13) . . ? C11 C15 H15 126.7 . . ? C14 C15 H15 126.7 . . ? Zr1 C15 H15 118.7 . . ? C12A C11A C15A 110.1(12) . . ? C12A C11A Zr1 73.9(10) . . ? C15A C11A Zr1 73.4(12) . . ? C12A C11A H11A 124.9 . . ? C15A C11A H11A 124.9 . . ? Zr1 C11A H11A 119.5 . . ? C11A C12A C13A 106.1(13) . . ? C11A C12A Zr1 74.4(10) . . ? C13A C12A Zr1 74.5(9) . . ? C11A C12A H12A 126.9 . . ? C13A C12A H12A 126.9 . . ? Zr1 C12A H12A 116.5 . . ? C14A C13A C12A 108.5(14) . . ? C14A C13A Zr1 73.8(11) . . ? C12A C13A Zr1 73.6(9) . . ? C14A C13A H13A 125.7 . . ? C12A C13A H13A 125.7 . . ? Zr1 C13A H13A 118.8 . . ? C13A C14A C15A 109.2(14) . . ? C13A C14A Zr1 74.6(10) . . ? C15A C14A Zr1 73.7(12) . . ? C13A C14A H14A 125.4 . . ? C15A C14A H14A 125.4 . . ? Zr1 C14A H14A 118.2 . . ? C14A C15A C11A 105.9(13) . . ? C14A C15A Zr1 74.5(11) . . ? C11A C15A Zr1 74.6(11) . . ? C14A C15A H15A 127.0 . . ? C11A C15A H15A 127.0 . . ? Zr1 C15A H15A 116.3 . . ? C2 C1 C5 132.8(7) . . ? C2 C1 Zr1 74.8(5) . . ? C5 C1 Zr1 151.4(6) . . ? C1 C2 C3 150.5(8) . . ? C1 C2 Zr1 73.3(5) . . ? C3 C2 Zr1 78.1(5) . . ? C2 C3 C4 121.7(8) . . ? C2 C3 Zr1 68.3(4) . . ? C4 C3 Zr1 73.8(4) . . ? C2 C3 H03 124(5) . . ? C4 C3 H03 114(5) . . ? Zr1 C3 H03 123(5) . . ? C3 C4 C21 123.8(7) . . ? C3 C4 Zr1 72.6(4) . . ? C21 C4 Zr1 133.9(5) . . ? C3 C4 H04 105(6) . . ? C21 C4 H04 118(6) . . ? Zr1 C4 H04 93(6) . . ? C6 C5 C8A 82.1(19) . . ? C6 C5 C7A 128.4(19) . . ? C8A C5 C7A 111(2) . . ? C6 C5 C7 111.2(8) . . ? C8A C5 C7 130(2) . . ? C7A C5 C7 23.4(17) . . ? C6 C5 C1 111.6(8) . . ? C8A C5 C1 108.1(19) . . ? C7A C5 C1 110.5(18) . . ? C7 C5 C1 110.6(9) . . ? C6 C5 C6A 32.2(16) . . ? C8A C5 C6A 113.9(19) . . ? C7A C5 C6A 108.5(19) . . ? C7 C5 C6A 86.3(18) . . ? C1 C5 C6A 104.3(16) . . ? C6 C5 C8 108.6(8) . . ? C8A C5 C8 29.1(19) . . ? C7A C5 C8 85.2(18) . . ? C7 C5 C8 106.9(8) . . ? C1 C5 C8 107.7(8) . . ? C6A C5 C8 137.8(18) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C6A H6A1 109.5 . . ? C5 C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5 C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5 C7A H7A1 109.5 . . ? C5 C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5 C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5 C8A H8A1 109.5 . . ? C5 C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C5 C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C20 C16 C17 108.2(9) . . ? C20 C16 Zr1 74.7(5) . . ? C17 C16 Zr1 75.4(5) . . ? C20 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Zr1 C16 H16 116.1 . . ? C18 C17 C16 108.1(9) . . ? C18 C17 Zr1 74.1(5) . . ? C16 C17 Zr1 72.7(5) . . ? C18 C17 H17 125.9 . . ? C16 C17 H17 125.9 . . ? Zr1 C17 H17 119.2 . . ? C17 C18 C19 107.4(9) . . ? C17 C18 Zr1 74.5(5) . . ? C19 C18 Zr1 74.5(5) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? Zr1 C18 H18 116.8 . . ? C20 C19 C18 108.1(9) . . ? C20 C19 Zr1 73.2(5) . . ? C18 C19 Zr1 73.5(5) . . ? C20 C19 H19 126.0 . . ? C18 C19 H19 126.0 . . ? Zr1 C19 H19 119.2 . . ? C19 C20 C16 108.2(9) . . ? C19 C20 Zr1 75.4(5) . . ? C16 C20 Zr1 73.6(5) . . ? C19 C20 H20 125.9 . . ? C16 C20 H20 125.9 . . ? Zr1 C20 H20 117.2 . . ? C22 C21 C26 117.8(7) . . ? C22 C21 C4 118.6(7) . . ? C26 C21 C4 123.5(7) . . ? C21 C22 C23 121.3(8) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 119.2(8) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 120.2(8) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.6(8) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C21 120.7(7) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? 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 Zr1 C11 C15 59(2) . . . . ? C2 Zr1 C11 C15 105(2) . . . . ? C3 Zr1 C11 C15 154.3(14) . . . . ? C4 Zr1 C11 C15 161.2(15) . . . . ? C16 Zr1 C11 C15 -59.2(16) . . . . ? C20 Zr1 C11 C15 -56.0(17) . . . . ? C18 Zr1 C11 C15 -110.7(15) . . . . ? C17 Zr1 C11 C15 -89.6(17) . . . . ? C19 Zr1 C11 C15 -93.8(14) . . . . ? C12 Zr1 C11 C15 115.3(16) . . . . ? C15A Zr1 C11 C15 16.1(10) . . . . ? C1 Zr1 C11 C12 -56(2) . . . . ? C2 Zr1 C11 C12 -10(2) . . . . ? C3 Zr1 C11 C12 39.0(17) . . . . ? C4 Zr1 C11 C12 45.9(16) . . . . ? C16 Zr1 C11 C12 -174.4(16) . . . . ? C20 Zr1 C11 C12 -171.3(15) . . . . ? C18 Zr1 C11 C12 134.0(15) . . . . ? C17 Zr1 C11 C12 155.1(17) . . . . ? C19 Zr1 C11 C12 150.9(12) . . . . ? C15A Zr1 C11 C12 -99.2(14) . . . . ? C15 C11 C12 C13 -1(3) . . . . ? Zr1 C11 C12 C13 67.7(17) . . . . ? C15 C11 C12 Zr1 -68(2) . . . . ? C1 Zr1 C12 C11 139.5(16) . . . . ? C2 Zr1 C12 C11 173.5(14) . . . . ? C3 Zr1 C12 C11 -151.4(14) . . . . ? C4 Zr1 C12 C11 -133.5(17) . . . . ? C16 Zr1 C12 C11 7(2) . . . . ? C20 Zr1 C12 C11 17(3) . . . . ? C18 Zr1 C12 C11 -57.9(15) . . . . ? C17 Zr1 C12 C11 -26.3(17) . . . . ? C19 Zr1 C12 C11 -63.7(18) . . . . ? C15A Zr1 C12 C11 51.3(11) . . . . ? C1 Zr1 C12 C13 26.0(17) . . . . ? C2 Zr1 C12 C13 59.9(15) . . . . ? C3 Zr1 C12 C13 95.0(15) . . . . ? C4 Zr1 C12 C13 112.9(17) . . . . ? C16 Zr1 C12 C13 -107.0(19) . . . . ? C20 Zr1 C12 C13 -97(3) . . . . ? C11 Zr1 C12 C13 -113.6(16) . . . . ? C18 Zr1 C12 C13 -171.5(14) . . . . ? C17 Zr1 C12 C13 -139.9(16) . . . . ? C19 Zr1 C12 C13 -177.3(11) . . . . ? C15A Zr1 C12 C13 -62.3(11) . . . . ? C11 C12 C13 C14 1(3) . . . . ? Zr1 C12 C13 C14 67.0(17) . . . . ? C11 C12 C13 Zr1 -66.4(18) . . . . ? C1 Zr1 C13 C14 89.5(16) . . . . ? C2 Zr1 C13 C14 119.8(15) . . . . ? C3 Zr1 C13 C14 150.9(13) . . . . ? C4 Zr1 C13 C14 -178.7(15) . . . . ? C16 Zr1 C13 C14 -19(2) . . . . ? C20 Zr1 C13 C14 20(2) . . . . ? C11 Zr1 C13 C14 -76.9(11) . . . . ? C18 Zr1 C13 C14 -97(3) . . . . ? C17 Zr1 C13 C14 -60(2) . . . . ? C19 Zr1 C13 C14 58(4) . . . . ? C12 Zr1 C13 C14 -114.8(16) . . . . ? C15A Zr1 C13 C14 -25.2(10) . . . . ? C1 Zr1 C13 C12 -155.6(17) . . . . ? C2 Zr1 C13 C12 -125.3(16) . . . . ? C3 Zr1 C13 C12 -94.3(15) . . . . ? C4 Zr1 C13 C12 -63.9(16) . . . . ? C16 Zr1 C13 C12 96(2) . . . . ? C20 Zr1 C13 C12 135.2(18) . . . . ? C11 Zr1 C13 C12 37.9(9) . . . . ? C18 Zr1 C13 C12 17(3) . . . . ? C17 Zr1 C13 C12 55(2) . . . . ? C19 Zr1 C13 C12 173(3) . . . . ? C15A Zr1 C13 C12 89.7(13) . . . . ? C12 C13 C14 C15 0(3) . . . . ? Zr1 C13 C14 C15 65.6(17) . . . . ? C12 C13 C14 Zr1 -65.9(17) . . . . ? C1 Zr1 C14 C13 -86.1(16) . . . . ? C2 Zr1 C14 C13 -64.9(15) . . . . ? C3 Zr1 C14 C13 -39.4(17) . . . . ? C4 Zr1 C14 C13 1.5(18) . . . . ? C16 Zr1 C14 C13 164.8(15) . . . . ? C20 Zr1 C14 C13 -166.7(14) . . . . ? C11 Zr1 C14 C13 78.2(11) . . . . ? C18 Zr1 C14 C13 137.5(17) . . . . ? C17 Zr1 C14 C13 136.4(16) . . . . ? C19 Zr1 C14 C13 -167.6(12) . . . . ? C12 Zr1 C14 C13 37.2(9) . . . . ? C15A Zr1 C14 C13 120(2) . . . . ? C1 Zr1 C14 C15 157.9(16) . . . . ? C2 Zr1 C14 C15 179.0(14) . . . . ? C3 Zr1 C14 C15 -155.4(13) . . . . ? C4 Zr1 C14 C15 -114.6(16) . . . . ? C16 Zr1 C14 C15 48.7(15) . . . . ? C20 Zr1 C14 C15 77.2(15) . . . . ? C11 Zr1 C14 C15 -37.8(9) . . . . ? C18 Zr1 C14 C15 21(2) . . . . ? C17 Zr1 C14 C15 20.3(17) . . . . ? C19 Zr1 C14 C15 76.3(15) . . . . ? C12 Zr1 C14 C15 -78.9(11) . . . . ? C15A Zr1 C14 C15 3.9(17) . . . . ? C12 C11 C15 C14 1(3) . . . . ? Zr1 C11 C15 C14 -67.2(17) . . . . ? C12 C11 C15 Zr1 67.7(19) . . . . ? C13 C14 C15 C11 0(3) . . . . ? Zr1 C14 C15 C11 65.5(19) . . . . ? C13 C14 C15 Zr1 -65.6(16) . . . . ? C1 Zr1 C15 C11 -137.4(17) . . . . ? C2 Zr1 C15 C11 -115.0(19) . . . . ? C3 Zr1 C15 C11 -58(3) . . . . ? C4 Zr1 C15 C11 -24(2) . . . . ? C16 Zr1 C15 C11 117.2(18) . . . . ? C20 Zr1 C15 C11 134.4(16) . . . . ? C18 Zr1 C15 C11 80.1(16) . . . . ? C17 Zr1 C15 C11 85.4(17) . . . . ? C19 Zr1 C15 C11 113.6(14) . . . . ? C12 Zr1 C15 C11 -37.0(10) . . . . ? C15A Zr1 C15 C11 -120(4) . . . . ? C1 Zr1 C15 C14 -23.8(16) . . . . ? C2 Zr1 C15 C14 -1(2) . . . . ? C3 Zr1 C15 C14 55(3) . . . . ? C4 Zr1 C15 C14 89.1(19) . . . . ? C16 Zr1 C15 C14 -129.2(17) . . . . ? C20 Zr1 C15 C14 -112.1(15) . . . . ? C11 Zr1 C15 C14 113.5(16) . . . . ? C18 Zr1 C15 C14 -166.3(14) . . . . ? C17 Zr1 C15 C14 -161.0(16) . . . . ? C19 Zr1 C15 C14 -132.8(12) . . . . ? C12 Zr1 C15 C14 76.5(11) . . . . ? C15A Zr1 C15 C14 -7(3) . . . . ? C1 Zr1 C11A C12A -95.2(15) . . . . ? C2 Zr1 C11A C12A -52(2) . . . . ? C3 Zr1 C11A C12A 9.8(17) . . . . ? C4 Zr1 C11A C12A 16.9(14) . . . . ? C16 Zr1 C11A C12A 155.8(13) . . . . ? C20 Zr1 C11A C12A 161.9(11) . . . . ? C11 Zr1 C11A C12A 9(3) . . . . ? C18 Zr1 C11A C12A 107.2(12) . . . . ? C17 Zr1 C11A C12A 123.7(14) . . . . ? C19 Zr1 C11A C12A 129.6(10) . . . . ? C12 Zr1 C11A C12A -21.3(8) . . . . ? C15A Zr1 C11A C12A -117.4(13) . . . . ? C1 Zr1 C11A C15A 22.2(17) . . . . ? C2 Zr1 C11A C15A 66(2) . . . . ? C3 Zr1 C11A C15A 127.2(16) . . . . ? C4 Zr1 C11A C15A 134.3(14) . . . . ? C16 Zr1 C11A C15A -86.8(14) . . . . ? C20 Zr1 C11A C15A -80.7(13) . . . . ? C11 Zr1 C11A C15A 126(4) . . . . ? C18 Zr1 C11A C15A -135.4(13) . . . . ? C17 Zr1 C11A C15A -118.9(15) . . . . ? C19 Zr1 C11A C15A -113.0(12) . . . . ? C12 Zr1 C11A C15A 96.0(12) . . . . ? C15A C11A C12A C13A 3(2) . . . . ? Zr1 C11A C12A C13A 68.3(11) . . . . ? C15A C11A C12A Zr1 -65.0(15) . . . . ? C1 Zr1 C12A C11A 111.3(14) . . . . ? C2 Zr1 C12A C11A 150.2(12) . . . . ? C3 Zr1 C12A C11A -173.8(11) . . . . ? C4 Zr1 C12A C11A -164.0(13) . . . . ? C16 Zr1 C12A C11A -25.7(14) . . . . ? C20 Zr1 C12A C11A -27.9(16) . . . . ? C11 Zr1 C12A C11A -4.5(17) . . . . ? C18 Zr1 C12A C11A -82.2(12) . . . . ? C17 Zr1 C12A C11A -54.1(13) . . . . ? C19 Zr1 C12A C11A -80.3(12) . . . . ? C12 Zr1 C12A C11A 118(2) . . . . ? C15A Zr1 C12A C11A 35.8(8) . . . . ? C1 Zr1 C12A C13A -0.9(14) . . . . ? C2 Zr1 C12A C13A 38.0(13) . . . . ? C3 Zr1 C12A C13A 74.1(12) . . . . ? C4 Zr1 C12A C13A 83.9(13) . . . . ? C16 Zr1 C12A C13A -137.9(12) . . . . ? C20 Zr1 C12A C13A -140.0(13) . . . . ? C11 Zr1 C12A C13A -117(2) . . . . ? C18 Zr1 C12A C13A 165.6(11) . . . . ? C17 Zr1 C12A C13A -166.2(12) . . . . ? C19 Zr1 C12A C13A 167.5(9) . . . . ? C12 Zr1 C12A C13A 6(2) . . . . ? C15A Zr1 C12A C13A -76.4(9) . . . . ? C11A C12A C13A C14A -2(2) . . . . ? Zr1 C12A C13A C14A 66.1(13) . . . . ? C11A C12A C13A Zr1 -68.2(12) . . . . ? C1 Zr1 C13A C14A 63.8(14) . . . . ? C2 Zr1 C13A C14A 95.8(13) . . . . ? C3 Zr1 C13A C14A 129.5(13) . . . . ? C4 Zr1 C13A C14A 154.7(15) . . . . ? C16 Zr1 C13A C14A -58.2(18) . . . . ? C20 Zr1 C13A C14A -22(3) . . . . ? C11 Zr1 C13A C14A -88.3(12) . . . . ? C18 Zr1 C13A C14A -137.0(15) . . . . ? C17 Zr1 C13A C14A -98.6(16) . . . . ? C19 Zr1 C13A C14A -170(2) . . . . ? C12 Zr1 C13A C14A -121(3) . . . . ? C15A Zr1 C13A C14A -36.5(8) . . . . ? C1 Zr1 C13A C12A 179.3(12) . . . . ? C2 Zr1 C13A C12A -148.7(11) . . . . ? C3 Zr1 C13A C12A -115.0(11) . . . . ? C4 Zr1 C13A C12A -89.8(12) . . . . ? C16 Zr1 C13A C12A 57.3(17) . . . . ? C20 Zr1 C13A C12A 93(2) . . . . ? C11 Zr1 C13A C12A 27.2(10) . . . . ? C18 Zr1 C13A C12A -21.5(15) . . . . ? C17 Zr1 C13A C12A 16.9(15) . . . . ? C19 Zr1 C13A C12A -55(3) . . . . ? C12 Zr1 C13A C12A -6(2) . . . . ? C15A Zr1 C13A C12A 79.0(9) . . . . ? C12A C13A C14A C15A 0(2) . . . . ? Zr1 C13A C14A C15A 66.1(15) . . . . ? C12A C13A C14A Zr1 -65.9(12) . . . . ? C1 Zr1 C14A C13A -115.1(14) . . . . ? C2 Zr1 C14A C13A -88.6(13) . . . . ? C3 Zr1 C14A C13A -60.1(13) . . . . ? C4 Zr1 C14A C13A -26.0(14) . . . . ? C16 Zr1 C14A C13A 137.2(13) . . . . ? C20 Zr1 C14A C13A 169.3(11) . . . . ? C11 Zr1 C14A C13A 63.5(11) . . . . ? C18 Zr1 C14A C13A 91(2) . . . . ? C17 Zr1 C14A C13A 104.0(16) . . . . ? C19 Zr1 C14A C13A 175.8(10) . . . . ? C12 Zr1 C14A C13A 20.9(10) . . . . ? C15A Zr1 C14A C13A 115.9(15) . . . . ? C1 Zr1 C14A C15A 129.0(14) . . . . ? C2 Zr1 C14A C15A 155.5(13) . . . . ? C3 Zr1 C14A C15A -176.0(11) . . . . ? C4 Zr1 C14A C15A -141.9(13) . . . . ? C16 Zr1 C14A C15A 21.4(14) . . . . ? C20 Zr1 C14A C15A 53.5(14) . . . . ? C11 Zr1 C14A C15A -52.3(11) . . . . ? C18 Zr1 C14A C15A -25(3) . . . . ? C17 Zr1 C14A C15A -11.9(17) . . . . ? C19 Zr1 C14A C15A 60.0(17) . . . . ? C12 Zr1 C14A C15A -94.9(14) . . . . ? C13A C14A C15A C11A 2(2) . . . . ? Zr1 C14A C15A C11A 68.5(15) . . . . ? C13A C14A C15A Zr1 -66.7(14) . . . . ? C12A C11A C15A C14A -3(2) . . . . ? Zr1 C11A C15A C14A -68.5(15) . . . . ? C12A C11A C15A Zr1 65.3(14) . . . . ? C1 Zr1 C15A C14A -51.4(13) . . . . ? C2 Zr1 C15A C14A -30.9(15) . . . . ? C3 Zr1 C15A C14A 7(2) . . . . ? C4 Zr1 C15A C14A 50.6(18) . . . . ? C16 Zr1 C15A C14A -159.9(14) . . . . ? C20 Zr1 C15A C14A -138.0(12) . . . . ? C11 Zr1 C15A C14A 98.1(15) . . . . ? C18 Zr1 C15A C14A 167.4(12) . . . . ? C17 Zr1 C15A C14A 170.1(13) . . . . ? C19 Zr1 C15A C14A -153.0(11) . . . . ? C12 Zr1 C15A C14A 56.7(11) . . . . ? C1 Zr1 C15A C11A -163.2(12) . . . . ? C2 Zr1 C15A C11A -142.7(12) . . . . ? C3 Zr1 C15A C11A -104.7(18) . . . . ? C4 Zr1 C15A C11A -61.2(17) . . . . ? C16 Zr1 C15A C11A 88.3(14) . . . . ? C20 Zr1 C15A C11A 110.1(12) . . . . ? C11 Zr1 C15A C11A -13.7(11) . . . . ? C18 Zr1 C15A C11A 55.6(14) . . . . ? C17 Zr1 C15A C11A 58.3(13) . . . . ? C19 Zr1 C15A C11A 95.2(11) . . . . ? C12 Zr1 C15A C11A -55.1(10) . . . . ? C3 Zr1 C1 C2 -4.6(5) . . . . ? C4 Zr1 C1 C2 16.5(5) . . . . ? C16 Zr1 C1 C2 -127.3(5) . . . . ? C20 Zr1 C1 C2 -108.3(6) . . . . ? C11 Zr1 C1 C2 121.9(12) . . . . ? C18 Zr1 C1 C2 -69.7(6) . . . . ? C17 Zr1 C1 C2 -106.0(6) . . . . ? C19 Zr1 C1 C2 -77.5(6) . . . . ? C12 Zr1 C1 C2 93.5(7) . . . . ? C15A Zr1 C1 C2 148.1(7) . . . . ? C2 Zr1 C1 C5 -167.1(16) . . . . ? C3 Zr1 C1 C5 -171.7(13) . . . . ? C4 Zr1 C1 C5 -150.6(12) . . . . ? C16 Zr1 C1 C5 65.6(13) . . . . ? C20 Zr1 C1 C5 84.6(13) . . . . ? C11 Zr1 C1 C5 -45.2(17) . . . . ? C18 Zr1 C1 C5 123.2(12) . . . . ? C17 Zr1 C1 C5 86.9(13) . . . . ? C19 Zr1 C1 C5 115.4(13) . . . . ? C12 Zr1 C1 C5 -73.6(13) . . . . ? C15A Zr1 C1 C5 -19.0(14) . . . . ? C5 C1 C2 C3 -173.1(13) . . . . ? Zr1 C1 C2 C3 15.3(16) . . . . ? C5 C1 C2 Zr1 171.6(10) . . . . ? C3 Zr1 C2 C1 172.4(8) . . . . ? C4 Zr1 C2 C1 -161.1(6) . . . . ? C16 Zr1 C2 C1 67.8(6) . . . . ? C20 Zr1 C2 C1 71.3(6) . . . . ? C11 Zr1 C2 C1 -93.1(11) . . . . ? C18 Zr1 C2 C1 123.6(5) . . . . ? C17 Zr1 C2 C1 108.5(6) . . . . ? C19 Zr1 C2 C1 101.0(6) . . . . ? C12 Zr1 C2 C1 -98.6(8) . . . . ? C15A Zr1 C2 C1 -40.6(8) . . . . ? C1 Zr1 C2 C3 -172.4(8) . . . . ? C4 Zr1 C2 C3 26.5(5) . . . . ? C16 Zr1 C2 C3 -104.6(6) . . . . ? C20 Zr1 C2 C3 -101.1(5) . . . . ? C11 Zr1 C2 C3 94.5(11) . . . . ? C18 Zr1 C2 C3 -48.8(6) . . . . ? C17 Zr1 C2 C3 -63.9(7) . . . . ? C19 Zr1 C2 C3 -71.4(6) . . . . ? C12 Zr1 C2 C3 89.0(8) . . . . ? C15A Zr1 C2 C3 147.0(7) . . . . ? C1 C2 C3 C4 -68(2) . . . . ? Zr1 C2 C3 C4 -53.2(7) . . . . ? C1 C2 C3 Zr1 -14.9(16) . . . . ? C1 Zr1 C3 C2 4.4(5) . . . . ? C4 Zr1 C3 C2 -134.8(8) . . . . ? C16 Zr1 C3 C2 101.2(6) . . . . ? C20 Zr1 C3 C2 83.2(5) . . . . ? C11 Zr1 C3 C2 -122.5(9) . . . . ? C18 Zr1 C3 C2 133.6(5) . . . . ? C17 Zr1 C3 C2 136.1(5) . . . . ? C19 Zr1 C3 C2 102.4(6) . . . . ? C12 Zr1 C3 C2 -102.0(10) . . . . ? C15A Zr1 C3 C2 -62.8(12) . . . . ? C1 Zr1 C3 C4 139.2(6) . . . . ? C2 Zr1 C3 C4 134.8(8) . . . . ? C16 Zr1 C3 C4 -124.0(5) . . . . ? C20 Zr1 C3 C4 -142.0(5) . . . . ? C11 Zr1 C3 C4 12.4(9) . . . . ? C18 Zr1 C3 C4 -91.5(5) . . . . ? C17 Zr1 C3 C4 -89.0(5) . . . . ? C19 Zr1 C3 C4 -122.8(5) . . . . ? C12 Zr1 C3 C4 32.9(10) . . . . ? C15A Zr1 C3 C4 72.1(12) . . . . ? C2 C3 C4 C21 -177.6(7) . . . . ? Zr1 C3 C4 C21 131.7(7) . . . . ? C2 C3 C4 Zr1 50.7(7) . . . . ? C1 Zr1 C4 C3 -36.4(5) . . . . ? C2 Zr1 C4 C3 -26.6(5) . . . . ? C16 Zr1 C4 C3 86.6(7) . . . . ? C20 Zr1 C4 C3 47.6(6) . . . . ? C11 Zr1 C4 C3 -170.8(7) . . . . ? C18 Zr1 C4 C3 85.4(5) . . . . ? C17 Zr1 C4 C3 105.4(5) . . . . ? C19 Zr1 C4 C3 54.4(5) . . . . ? C12 Zr1 C4 C3 -147.6(10) . . . . ? C15A Zr1 C4 C3 -142.6(9) . . . . ? C1 Zr1 C4 C21 -156.9(8) . . . . ? C2 Zr1 C4 C21 -147.1(9) . . . . ? C3 Zr1 C4 C21 -120.5(10) . . . . ? C16 Zr1 C4 C21 -34.0(10) . . . . ? C20 Zr1 C4 C21 -72.9(8) . . . . ? C11 Zr1 C4 C21 68.6(10) . . . . ? C18 Zr1 C4 C21 -35.1(8) . . . . ? C17 Zr1 C4 C21 -15.2(8) . . . . ? C19 Zr1 C4 C21 -66.1(8) . . . . ? C12 Zr1 C4 C21 91.9(12) . . . . ? C15A Zr1 C4 C21 96.9(11) . . . . ? C2 C1 C5 C6 146.9(13) . . . . ? Zr1 C1 C5 C6 -50.1(17) . . . . ? C2 C1 C5 C8A 58(3) . . . . ? Zr1 C1 C5 C8A -139(3) . . . . ? C2 C1 C5 C7A -64(2) . . . . ? Zr1 C1 C5 C7A 99(2) . . . . ? C2 C1 C5 C7 -88.7(14) . . . . ? Zr1 C1 C5 C7 74.2(15) . . . . ? C2 C1 C5 C6A 180(2) . . . . ? Zr1 C1 C5 C6A -17(3) . . . . ? C2 C1 C5 C8 27.8(15) . . . . ? Zr1 C1 C5 C8 -169.2(12) . . . . ? C1 Zr1 C16 C20 38.0(7) . . . . ? C2 Zr1 C16 C20 6.7(8) . . . . ? C3 Zr1 C16 C20 -35.4(8) . . . . ? C4 Zr1 C16 C20 -79.0(9) . . . . ? C11 Zr1 C16 C20 175.0(8) . . . . ? C18 Zr1 C16 C20 -77.6(7) . . . . ? C17 Zr1 C16 C20 -113.9(9) . . . . ? C19 Zr1 C16 C20 -36.9(6) . . . . ? C12 Zr1 C16 C20 171.4(10) . . . . ? C15A Zr1 C16 C20 136.7(9) . . . . ? C1 Zr1 C16 C17 151.9(6) . . . . ? C2 Zr1 C16 C17 120.6(6) . . . . ? C3 Zr1 C16 C17 78.5(7) . . . . ? C4 Zr1 C16 C17 34.9(9) . . . . ? C20 Zr1 C16 C17 113.9(9) . . . . ? C11 Zr1 C16 C17 -71.1(8) . . . . ? C18 Zr1 C16 C17 36.3(6) . . . . ? C19 Zr1 C16 C17 77.0(7) . . . . ? C12 Zr1 C16 C17 -74.7(10) . . . . ? C15A Zr1 C16 C17 -109.4(8) . . . . ? C20 C16 C17 C18 2.0(11) . . . . ? Zr1 C16 C17 C18 -66.1(7) . . . . ? C20 C16 C17 Zr1 68.1(7) . . . . ? C1 Zr1 C17 C18 75.2(8) . . . . ? C2 Zr1 C17 C18 28.6(9) . . . . ? C3 Zr1 C17 C18 -4.7(7) . . . . ? C4 Zr1 C17 C18 -40.8(7) . . . . ? C16 Zr1 C17 C18 115.3(9) . . . . ? C20 Zr1 C17 C18 78.0(7) . . . . ? C11 Zr1 C17 C18 -138.1(9) . . . . ? C19 Zr1 C17 C18 38.0(6) . . . . ? C12 Zr1 C17 C18 -124.2(8) . . . . ? C15A Zr1 C17 C18 -175.6(7) . . . . ? C1 Zr1 C17 C16 -40.1(8) . . . . ? C2 Zr1 C17 C16 -86.7(8) . . . . ? C3 Zr1 C17 C16 -120.1(6) . . . . ? C4 Zr1 C17 C16 -156.2(6) . . . . ? C20 Zr1 C17 C16 -37.3(6) . . . . ? C11 Zr1 C17 C16 106.6(9) . . . . ? C18 Zr1 C17 C16 -115.3(9) . . . . ? C19 Zr1 C17 C16 -77.3(7) . . . . ? C12 Zr1 C17 C16 120.5(8) . . . . ? C15A Zr1 C17 C16 69.0(8) . . . . ? C16 C17 C18 C19 -2.6(10) . . . . ? Zr1 C17 C18 C19 -67.8(6) . . . . ? C16 C17 C18 Zr1 65.2(7) . . . . ? C1 Zr1 C18 C17 -128.4(6) . . . . ? C2 Zr1 C18 C17 -159.6(6) . . . . ? C3 Zr1 C18 C17 175.7(7) . . . . ? C4 Zr1 C18 C17 142.1(7) . . . . ? C16 Zr1 C18 C17 -36.9(6) . . . . ? C20 Zr1 C18 C17 -77.2(7) . . . . ? C11 Zr1 C18 C17 42.9(10) . . . . ? C19 Zr1 C18 C17 -113.5(9) . . . . ? C12 Zr1 C18 C17 70.8(9) . . . . ? C15A Zr1 C18 C17 5.3(9) . . . . ? C1 Zr1 C18 C19 -14.9(7) . . . . ? C2 Zr1 C18 C19 -46.1(6) . . . . ? C3 Zr1 C18 C19 -70.8(6) . . . . ? C4 Zr1 C18 C19 -104.4(6) . . . . ? C16 Zr1 C18 C19 76.5(6) . . . . ? C20 Zr1 C18 C19 36.3(6) . . . . ? C11 Zr1 C18 C19 156.4(9) . . . . ? C17 Zr1 C18 C19 113.5(9) . . . . ? C12 Zr1 C18 C19 -175.7(8) . . . . ? C15A Zr1 C18 C19 118.7(8) . . . . ? C17 C18 C19 C20 2.3(10) . . . . ? Zr1 C18 C19 C20 -65.6(6) . . . . ? C17 C18 C19 Zr1 67.8(6) . . . . ? C1 Zr1 C19 C20 -77.3(6) . . . . ? C2 Zr1 C19 C20 -108.5(7) . . . . ? C3 Zr1 C19 C20 -141.5(7) . . . . ? C4 Zr1 C19 C20 -169.2(6) . . . . ? C16 Zr1 C19 C20 37.3(6) . . . . ? C11 Zr1 C19 C20 83.3(12) . . . . ? C18 Zr1 C19 C20 115.3(9) . . . . ? C17 Zr1 C19 C20 78.0(7) . . . . ? C12 Zr1 C19 C20 124.3(16) . . . . ? C15A Zr1 C19 C20 28.7(11) . . . . ? C1 Zr1 C19 C18 167.4(6) . . . . ? C2 Zr1 C19 C18 136.2(6) . . . . ? C3 Zr1 C19 C18 103.2(6) . . . . ? C4 Zr1 C19 C18 75.5(6) . . . . ? C16 Zr1 C19 C18 -78.0(6) . . . . ? C20 Zr1 C19 C18 -115.3(9) . . . . ? C11 Zr1 C19 C18 -32.0(12) . . . . ? C17 Zr1 C19 C18 -37.3(5) . . . . ? C12 Zr1 C19 C18 9.0(17) . . . . ? C15A Zr1 C19 C18 -86.6(10) . . . . ? C18 C19 C20 C16 -1.0(10) . . . . ? Zr1 C19 C20 C16 -66.8(6) . . . . ? C18 C19 C20 Zr1 65.8(6) . . . . ? C17 C16 C20 C19 -0.6(11) . . . . ? Zr1 C16 C20 C19 68.0(6) . . . . ? C17 C16 C20 Zr1 -68.6(7) . . . . ? C1 Zr1 C20 C19 101.2(6) . . . . ? C2 Zr1 C20 C19 71.0(6) . . . . ? C3 Zr1 C20 C19 37.6(7) . . . . ? C4 Zr1 C20 C19 13.1(8) . . . . ? C16 Zr1 C20 C19 -114.4(9) . . . . ? C11 Zr1 C20 C19 -120.4(9) . . . . ? C18 Zr1 C20 C19 -37.0(6) . . . . ? C17 Zr1 C20 C19 -76.9(6) . . . . ? C12 Zr1 C20 C19 -131.1(18) . . . . ? C15A Zr1 C20 C19 -158.8(9) . . . . ? C1 Zr1 C20 C16 -144.4(7) . . . . ? C2 Zr1 C20 C16 -174.5(7) . . . . ? C3 Zr1 C20 C16 152.0(7) . . . . ? C4 Zr1 C20 C16 127.6(7) . . . . ? C11 Zr1 C20 C16 -5.9(10) . . . . ? C18 Zr1 C20 C16 77.4(7) . . . . ? C17 Zr1 C20 C16 37.6(6) . . . . ? C19 Zr1 C20 C16 114.4(9) . . . . ? C12 Zr1 C20 C16 -17(2) . . . . ? C15A Zr1 C20 C16 -44.4(9) . . . . ? C3 C4 C21 C22 153.2(7) . . . . ? Zr1 C4 C21 C22 -108.4(8) . . . . ? C3 C4 C21 C26 -26.8(11) . . . . ? Zr1 C4 C21 C26 71.6(10) . . . . ? C26 C21 C22 C23 -1.0(11) . . . . ? C4 C21 C22 C23 179.1(7) . . . . ? C21 C22 C23 C24 1.1(11) . . . . ? C22 C23 C24 C25 -1.6(13) . . . . ? C23 C24 C25 C26 1.9(13) . . . . ? C24 C25 C26 C21 -1.8(12) . . . . ? C22 C21 C26 C25 1.3(11) . . . . ? C4 C21 C26 C25 -178.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.971 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.110 _database_code_depnum_ccdc_archive 'CCDC 938715' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk6964 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Zr2' _chemical_formula_weight 627.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2886(2) _cell_length_b 13.2145(3) _cell_length_c 15.2253(4) _cell_angle_alpha 67.3370(10) _cell_angle_beta 85.1820(10) _cell_angle_gamma 83.6090(10) _cell_volume 1527.76(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3738 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9461 _exptl_absorpt_correction_T_max 0.9793 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14047 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 28.23 _reflns_number_total 7350 _reflns_number_gt 5792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogens at C3 and C4 atoms were refined freely. An unidentified disordered solvent molecule was found in the asymmetrical unit and could not be satisfactorily refined. The program SQUEEZE (A. L. Spek J. Appl. Cryst., 2003, 36, 7-13) was therefore used to remove mathematically the effect of the solvent. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.021 0.000 0.000 205 21 ' ' _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^)+(0.0106P)^2^+5.5161P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7350 _refine_ls_number_parameters 336 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.052 _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 0.18295(4) 0.39271(3) 0.33636(3) 0.02871(10) Uani 1 1 d . . . Zr2 Zr 0.33185(4) 0.15106(3) 0.30250(3) 0.02808(10) Uani 1 1 d . . . C1 C 0.2447(5) 0.2933(4) 0.1586(3) 0.0374(9) Uani 1 1 d . . . C2 C 0.2143(5) 0.3351(3) 0.2192(3) 0.0326(9) Uani 1 1 d . . . C3 C 0.3226(5) 0.2495(3) 0.4839(3) 0.0337(9) Uani 1 1 d . . . H3 H 0.427(5) 0.280(3) 0.461(3) 0.025(10) Uiso 1 1 d . . . C4 C 0.2680(5) 0.1941(3) 0.4318(3) 0.0309(8) Uani 1 1 d . . . H4 H 0.169(5) 0.163(3) 0.464(3) 0.031(11) Uiso 1 1 d . . . C5 C 0.2310(7) 0.3209(5) 0.0525(4) 0.0573(14) Uani 1 1 d . . . C6 C 0.3129(14) 0.2285(9) 0.0210(6) 0.141(4) Uani 1 1 d . . . H6A H 0.2699 0.1592 0.0606 0.211 Uiso 1 1 calc R . . H6B H 0.4293 0.2225 0.0277 0.211 Uiso 1 1 calc R . . H6C H 0.2909 0.2460 -0.0451 0.211 Uiso 1 1 calc R . . C7 C 0.3047(10) 0.4304(7) -0.0022(5) 0.098(3) Uani 1 1 d U . . H7A H 0.2930 0.4515 -0.0699 0.147 Uiso 1 1 calc R . . H7B H 0.4190 0.4224 0.0107 0.147 Uiso 1 1 calc R . . H7C H 0.2486 0.4868 0.0181 0.147 Uiso 1 1 calc R . . C8 C 0.0510(9) 0.3346(7) 0.0321(5) 0.094(3) Uani 1 1 d . . . H8A H 0.0039 0.2651 0.0658 0.141 Uiso 1 1 calc R . . H8B H 0.0392 0.3569 -0.0358 0.141 Uiso 1 1 calc R . . H8C H -0.0046 0.3903 0.0533 0.141 Uiso 1 1 calc R . . C10 C 0.4607(6) 0.4661(4) 0.3241(5) 0.0633(17) Uani 1 1 d . . . H10 H 0.5502 0.4159 0.3498 0.076 Uiso 1 1 calc R . . C11 C 0.4117(8) 0.5017(5) 0.2321(5) 0.0658(18) Uani 1 1 d . . . H11 H 0.4614 0.4799 0.1836 0.079 Uiso 1 1 calc R . . C12 C 0.2763(8) 0.5753(5) 0.2236(5) 0.0692(18) Uani 1 1 d . . . H12 H 0.2164 0.6115 0.1687 0.083 Uiso 1 1 calc R . . C13 C 0.2450(7) 0.5862(4) 0.3089(6) 0.0680(19) Uani 1 1 d . . . H13 H 0.1616 0.6332 0.3222 0.082 Uiso 1 1 calc R . . C14 C 0.3542(8) 0.5178(5) 0.3717(4) 0.0621(16) Uani 1 1 d . . . H14 H 0.3568 0.5074 0.4362 0.075 Uiso 1 1 calc R . . C15 C -0.1025(5) 0.3710(5) 0.3043(5) 0.0568(15) Uani 1 1 d . . . H15 H -0.1164 0.3440 0.2569 0.068 Uiso 1 1 calc R . . C16 C -0.0961(6) 0.4817(4) 0.2901(4) 0.0533(13) Uani 1 1 d . . . H16 H -0.1029 0.5418 0.2315 0.064 Uiso 1 1 calc R . . C17 C -0.0779(6) 0.4870(4) 0.3776(4) 0.0507(13) Uani 1 1 d . . . H17 H -0.0726 0.5513 0.3894 0.061 Uiso 1 1 calc R . . C18 C -0.0687(6) 0.3800(5) 0.4451(4) 0.0539(13) Uani 1 1 d . . . H18 H -0.0540 0.3591 0.5105 0.065 Uiso 1 1 calc R . . C19 C -0.0853(5) 0.3089(4) 0.3991(5) 0.0554(15) Uani 1 1 d . . . H19 H -0.0846 0.2319 0.4280 0.066 Uiso 1 1 calc R . . C20 C 0.1115(8) 0.0648(5) 0.2524(5) 0.071(2) Uani 1 1 d . . . H20 H 0.0638 0.1054 0.1938 0.086 Uiso 1 1 calc R . . C21 C 0.2505(7) -0.0109(5) 0.2688(5) 0.0633(17) Uani 1 1 d . . . H21 H 0.3138 -0.0299 0.2224 0.076 Uiso 1 1 calc R . . C22 C 0.2773(7) -0.0519(4) 0.3644(4) 0.0540(13) Uani 1 1 d . . . H22 H 0.3618 -0.1046 0.3944 0.065 Uiso 1 1 calc R . . C23 C 0.1632(6) -0.0048(4) 0.4086(4) 0.0503(12) Uani 1 1 d . . . H23 H 0.1565 -0.0190 0.4742 0.060 Uiso 1 1 calc R . . C24 C 0.0585(6) 0.0670(4) 0.3431(5) 0.0553(15) Uani 1 1 d . . . H24 H -0.0319 0.1098 0.3558 0.066 Uiso 1 1 calc R . . C25 C 0.6090(6) 0.1695(8) 0.3495(6) 0.079(2) Uani 1 1 d . . . H25 H 0.6133 0.1951 0.3989 0.095 Uiso 1 1 calc R . . C26 C 0.6028(7) 0.2321(5) 0.2566(8) 0.088(3) Uani 1 1 d . . . H26 H 0.6013 0.3092 0.2300 0.106 Uiso 1 1 calc R . . C27 C 0.5989(7) 0.1668(9) 0.2071(5) 0.085(3) Uani 1 1 d . . . H27 H 0.5941 0.1900 0.1407 0.102 Uiso 1 1 calc R . . C28 C 0.6033(6) 0.0611(6) 0.2716(7) 0.076(2) Uani 1 1 d . . . H28 H 0.6030 -0.0021 0.2575 0.091 Uiso 1 1 calc R . . C29 C 0.6082(6) 0.0630(6) 0.3602(5) 0.0668(18) Uani 1 1 d . . . H29 H 0.6106 0.0017 0.4181 0.080 Uiso 1 1 calc R . . C31 C 0.2746(5) 0.2395(3) 0.5823(3) 0.0307(8) Uani 1 1 d . . . C32 C 0.1387(5) 0.1880(4) 0.6333(3) 0.0375(9) Uani 1 1 d . . . H32 H 0.0690 0.1610 0.6034 0.045 Uiso 1 1 calc R . . C33 C 0.1056(6) 0.1763(4) 0.7261(4) 0.0446(11) Uani 1 1 d . . . H33 H 0.0132 0.1417 0.7591 0.054 Uiso 1 1 calc R . . C34 C 0.2078(7) 0.2153(4) 0.7727(4) 0.0524(13) Uani 1 1 d . . . H34 H 0.1846 0.2069 0.8365 0.063 Uiso 1 1 calc R . . C35 C 0.3420(7) 0.2660(4) 0.7239(4) 0.0498(12) Uani 1 1 d . . . H35 H 0.4118 0.2921 0.7545 0.060 Uiso 1 1 calc R . . C36 C 0.3746(6) 0.2785(4) 0.6302(3) 0.0391(10) Uani 1 1 d . . . H36 H 0.4663 0.3141 0.5974 0.047 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 0.02566(19) 0.02578(19) 0.0363(2) -0.01318(16) -0.00128(15) -0.00363(14) Zr2 0.02477(19) 0.0290(2) 0.0337(2) -0.01515(16) -0.00201(15) -0.00296(14) C1 0.039(2) 0.037(2) 0.036(2) -0.0128(18) -0.0060(18) -0.0032(18) C2 0.0284(19) 0.030(2) 0.038(2) -0.0102(17) -0.0068(16) -0.0014(16) C3 0.029(2) 0.033(2) 0.040(2) -0.0132(18) -0.0040(17) -0.0050(16) C4 0.033(2) 0.0288(19) 0.032(2) -0.0126(16) -0.0009(16) -0.0021(16) C5 0.068(4) 0.068(4) 0.038(3) -0.020(3) -0.013(3) -0.005(3) C6 0.185(10) 0.192(11) 0.077(6) -0.099(7) -0.034(6) 0.053(8) C7 0.112(5) 0.127(6) 0.046(3) -0.011(4) 0.002(4) -0.055(5) C8 0.089(5) 0.123(6) 0.052(4) -0.001(4) -0.036(4) -0.032(5) C10 0.032(2) 0.042(3) 0.103(5) -0.010(3) -0.002(3) -0.015(2) C11 0.077(4) 0.062(4) 0.072(4) -0.039(3) 0.044(3) -0.046(3) C12 0.068(4) 0.046(3) 0.073(4) 0.009(3) -0.015(3) -0.027(3) C13 0.052(3) 0.035(3) 0.121(6) -0.036(3) 0.020(4) -0.014(2) C14 0.077(4) 0.066(4) 0.058(3) -0.032(3) 0.010(3) -0.047(3) C15 0.023(2) 0.080(4) 0.091(5) -0.058(4) 0.001(2) -0.007(2) C16 0.030(2) 0.054(3) 0.066(4) -0.012(3) -0.008(2) 0.004(2) C17 0.033(2) 0.050(3) 0.080(4) -0.037(3) -0.007(2) 0.000(2) C18 0.029(2) 0.085(4) 0.044(3) -0.023(3) 0.005(2) 0.001(2) C19 0.024(2) 0.041(3) 0.094(5) -0.019(3) 0.010(2) -0.0056(19) C20 0.088(5) 0.053(3) 0.068(4) -0.001(3) -0.039(4) -0.039(3) C21 0.069(4) 0.065(4) 0.084(4) -0.059(4) 0.023(3) -0.033(3) C22 0.056(3) 0.032(2) 0.073(4) -0.016(2) -0.007(3) -0.011(2) C23 0.050(3) 0.048(3) 0.061(3) -0.027(3) 0.012(2) -0.022(2) C24 0.028(2) 0.049(3) 0.102(5) -0.043(3) 0.003(3) -0.011(2) C25 0.028(3) 0.140(7) 0.114(6) -0.100(6) -0.005(3) 0.001(3) C26 0.027(3) 0.045(3) 0.173(9) -0.019(4) -0.006(4) -0.008(2) C27 0.033(3) 0.150(8) 0.051(4) -0.017(4) 0.005(3) -0.001(4) C28 0.030(3) 0.084(5) 0.150(7) -0.088(5) -0.002(3) 0.006(3) C29 0.029(3) 0.076(4) 0.067(4) 0.005(3) -0.009(2) -0.003(3) C31 0.035(2) 0.0256(18) 0.033(2) -0.0133(16) -0.0049(17) 0.0007(16) C32 0.040(2) 0.037(2) 0.040(2) -0.0189(19) -0.0040(19) -0.0067(18) C33 0.049(3) 0.042(3) 0.043(3) -0.017(2) 0.006(2) -0.007(2) C34 0.074(4) 0.053(3) 0.037(3) -0.024(2) -0.005(2) -0.003(3) C35 0.062(3) 0.049(3) 0.050(3) -0.030(2) -0.012(2) -0.004(2) C36 0.040(2) 0.034(2) 0.049(3) -0.020(2) -0.010(2) -0.0040(18) _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 C2 2.181(4) . ? Zr1 C16 2.501(5) . ? Zr1 C4 2.514(4) . ? Zr1 C14 2.524(5) . ? Zr1 C12 2.524(5) . ? Zr1 C15 2.524(5) . ? Zr1 C17 2.529(5) . ? Zr1 C18 2.531(5) . ? Zr1 C13 2.531(5) . ? Zr1 C19 2.541(5) . ? Zr1 C11 2.555(5) . ? Zr1 C10 2.562(5) . ? Zr2 C4 2.258(4) . ? Zr2 C1 2.376(4) . ? Zr2 C2 2.403(4) . ? Zr2 C29 2.516(5) . ? Zr2 C28 2.521(5) . ? Zr2 C26 2.524(6) . ? Zr2 C27 2.526(6) . ? Zr2 C25 2.527(5) . ? Zr2 C23 2.550(5) . ? Zr2 C21 2.554(5) . ? Zr2 C22 2.557(5) . ? Zr2 C24 2.559(5) . ? C1 C2 1.242(6) . ? C1 C5 1.523(7) . ? C3 C4 1.396(6) . ? C3 C31 1.477(6) . ? C3 H3 0.98(4) . ? C4 H4 0.97(4) . ? C5 C8 1.527(8) . ? C5 C7 1.530(9) . ? C5 C6 1.547(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C10 C11 1.376(9) . ? C10 C14 1.382(8) . ? C10 H10 0.9400 . ? C11 C12 1.380(9) . ? C11 H11 0.9400 . ? C12 C13 1.361(9) . ? C12 H12 0.9400 . ? C13 C14 1.359(9) . ? C13 H13 0.9400 . ? C14 H14 0.9400 . ? C15 C19 1.368(8) . ? C15 C16 1.400(7) . ? C15 H15 0.9400 . ? C16 C17 1.382(8) . ? C16 H16 0.9400 . ? C17 C18 1.390(8) . ? C17 H17 0.9400 . ? C18 C19 1.395(8) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C21 1.411(9) . ? C20 C24 1.424(9) . ? C20 H20 0.9400 . ? C21 C22 1.372(8) . ? C21 H21 0.9400 . ? C22 C23 1.349(7) . ? C22 H22 0.9400 . ? C23 C24 1.372(8) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 C26 1.337(11) . ? C25 C29 1.354(10) . ? C25 H25 0.9400 . ? C26 C27 1.350(11) . ? C26 H26 0.9400 . ? C27 C28 1.361(10) . ? C27 H27 0.9400 . ? C28 C29 1.364(9) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C31 C32 1.397(6) . ? C31 C36 1.403(6) . ? C32 C33 1.368(6) . ? C32 H32 0.9400 . ? C33 C34 1.402(7) . ? C33 H33 0.9400 . ? C34 C35 1.371(8) . ? C34 H34 0.9400 . ? C35 C36 1.379(7) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? 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 C2 Zr1 C16 92.95(17) . . ? C2 Zr1 C4 82.07(14) . . ? C16 Zr1 C4 128.65(16) . . ? C2 Zr1 C14 128.37(18) . . ? C16 Zr1 C14 111.8(2) . . ? C4 Zr1 C14 110.80(19) . . ? C2 Zr1 C12 88.7(2) . . ? C16 Zr1 C12 84.6(2) . . ? C4 Zr1 C12 145.67(19) . . ? C14 Zr1 C12 52.0(2) . . ? C2 Zr1 C15 75.80(16) . . ? C16 Zr1 C15 32.36(17) . . ? C4 Zr1 C15 98.54(17) . . ? C14 Zr1 C15 143.3(2) . . ? C12 Zr1 C15 111.2(2) . . ? C2 Zr1 C17 124.39(16) . . ? C16 Zr1 C17 31.89(18) . . ? C4 Zr1 C17 121.45(16) . . ? C14 Zr1 C17 92.13(19) . . ? C12 Zr1 C17 91.0(2) . . ? C15 Zr1 C17 52.87(16) . . ? C2 Zr1 C18 125.67(17) . . ? C16 Zr1 C18 52.79(18) . . ? C4 Zr1 C18 89.57(17) . . ? C14 Zr1 C18 104.8(2) . . ? C12 Zr1 C18 121.9(2) . . ? C15 Zr1 C18 52.46(18) . . ? C17 Zr1 C18 31.88(17) . . ? C2 Zr1 C13 120.0(2) . . ? C16 Zr1 C13 83.8(2) . . ? C4 Zr1 C13 142.0(2) . . ? C14 Zr1 C13 31.2(2) . . ? C12 Zr1 C13 31.2(2) . . ? C15 Zr1 C13 116.1(2) . . ? C17 Zr1 C13 73.79(18) . . ? C18 Zr1 C13 98.9(2) . . ? C2 Zr1 C19 94.62(18) . . ? C16 Zr1 C19 52.84(18) . . ? C4 Zr1 C19 76.53(15) . . ? C14 Zr1 C19 136.7(2) . . ? C12 Zr1 C19 137.4(2) . . ? C15 Zr1 C19 31.34(19) . . ? C17 Zr1 C19 52.81(16) . . ? C18 Zr1 C19 31.92(18) . . ? C13 Zr1 C19 126.56(18) . . ? C2 Zr1 C11 76.87(17) . . ? C16 Zr1 C11 114.1(2) . . ? C4 Zr1 C11 114.30(19) . . ? C14 Zr1 C11 51.92(19) . . ? C12 Zr1 C11 31.5(2) . . ? C15 Zr1 C11 133.3(2) . . ? C17 Zr1 C11 121.84(19) . . ? C18 Zr1 C11 150.56(19) . . ? C13 Zr1 C11 51.65(19) . . ? C19 Zr1 C11 164.6(2) . . ? C2 Zr1 C10 99.6(2) . . ? C16 Zr1 C10 133.96(18) . . ? C4 Zr1 C10 97.03(16) . . ? C14 Zr1 C10 31.52(19) . . ? C12 Zr1 C10 51.93(19) . . ? C15 Zr1 C10 163.0(2) . . ? C17 Zr1 C10 122.70(18) . . ? C18 Zr1 C10 134.7(2) . . ? C13 Zr1 C10 51.64(19) . . ? C19 Zr1 C10 163.4(2) . . ? C11 Zr1 C10 31.2(2) . . ? C4 Zr2 C1 113.00(15) . . ? C4 Zr2 C2 83.05(14) . . ? C1 Zr2 C2 30.12(14) . . ? C4 Zr2 C29 92.8(2) . . ? C1 Zr2 C29 132.64(18) . . ? C2 Zr2 C29 136.06(18) . . ? C4 Zr2 C28 124.1(2) . . ? C1 Zr2 C28 109.3(2) . . ? C2 Zr2 C28 129.0(2) . . ? C29 Zr2 C28 31.4(2) . . ? C4 Zr2 C26 98.2(3) . . ? C1 Zr2 C26 85.0(2) . . ? C2 Zr2 C26 85.91(18) . . ? C29 Zr2 C26 51.3(2) . . ? C28 Zr2 C26 51.2(2) . . ? C4 Zr2 C27 128.0(2) . . ? C1 Zr2 C27 81.6(2) . . ? C2 Zr2 C27 97.7(2) . . ? C29 Zr2 C27 51.9(2) . . ? C28 Zr2 C27 31.3(2) . . ? C26 Zr2 C27 31.0(3) . . ? C4 Zr2 C25 78.32(18) . . ? C1 Zr2 C25 114.2(3) . . ? C2 Zr2 C25 106.4(2) . . ? C29 Zr2 C25 31.1(2) . . ? C28 Zr2 C25 51.44(19) . . ? C26 Zr2 C25 30.7(2) . . ? C27 Zr2 C25 51.4(2) . . ? C4 Zr2 C23 77.26(16) . . ? C1 Zr2 C23 124.83(17) . . ? C2 Zr2 C23 122.74(16) . . ? C29 Zr2 C23 98.46(19) . . ? C28 Zr2 C23 106.2(2) . . ? C26 Zr2 C23 149.5(2) . . ? C27 Zr2 C23 136.3(3) . . ? C25 Zr2 C23 120.9(3) . . ? C4 Zr2 C21 128.77(17) . . ? C1 Zr2 C21 97.5(2) . . ? C2 Zr2 C21 121.08(19) . . ? C29 Zr2 C21 95.4(2) . . ? C28 Zr2 C21 77.66(19) . . ? C26 Zr2 C21 125.6(3) . . ? C27 Zr2 C21 95.3(3) . . ? C25 Zr2 C21 125.9(2) . . ? C23 Zr2 C21 51.52(18) . . ? C4 Zr2 C22 102.45(17) . . ? C1 Zr2 C22 127.35(17) . . ? C2 Zr2 C22 143.57(16) . . ? C29 Zr2 C22 80.1(2) . . ? C28 Zr2 C22 77.8(2) . . ? C26 Zr2 C22 127.78(19) . . ? C27 Zr2 C22 106.1(3) . . ? C25 Zr2 C22 110.0(3) . . ? C23 Zr2 C22 30.62(17) . . ? C21 Zr2 C22 31.13(19) . . ? C4 Zr2 C24 84.07(17) . . ? C1 Zr2 C24 94.02(18) . . ? C2 Zr2 C24 94.27(16) . . ? C29 Zr2 C24 128.95(19) . . ? C28 Zr2 C24 127.46(18) . . ? C26 Zr2 C24 177.7(3) . . ? C27 Zr2 C24 146.8(3) . . ? C25 Zr2 C24 150.8(3) . . ? C23 Zr2 C24 31.15(18) . . ? C21 Zr2 C24 52.45(17) . . ? C22 Zr2 C24 51.48(17) . . ? C2 C1 C5 140.8(5) . . ? C2 C1 Zr2 76.1(3) . . ? C5 C1 Zr2 143.1(3) . . ? C1 C2 Zr1 172.8(4) . . ? C1 C2 Zr2 73.7(3) . . ? Zr1 C2 Zr2 99.54(16) . . ? C4 C3 C31 128.6(4) . . ? C4 C3 Zr1 71.6(2) . . ? C31 C3 Zr1 123.3(3) . . ? C4 C3 H3 115(2) . . ? C31 C3 H3 114(2) . . ? Zr1 C3 H3 91(2) . . ? C3 C4 Zr2 142.2(3) . . ? C3 C4 Zr1 76.6(2) . . ? Zr2 C4 Zr1 94.30(15) . . ? C3 C4 H4 107(3) . . ? Zr2 C4 H4 111(3) . . ? Zr1 C4 H4 105(2) . . ? C1 C5 C8 108.1(5) . . ? C1 C5 C7 107.9(5) . . ? C8 C5 C7 109.0(6) . . ? C1 C5 C6 112.4(5) . . ? C8 C5 C6 107.5(6) . . ? C7 C5 C6 111.7(7) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C10 C14 107.4(5) . . ? C11 C10 Zr1 74.2(3) . . ? C14 C10 Zr1 72.7(3) . . ? C11 C10 H10 126.3 . . ? C14 C10 H10 126.3 . . ? Zr1 C10 H10 118.8 . . ? C10 C11 C12 107.7(5) . . ? C10 C11 Zr1 74.6(3) . . ? C12 C11 Zr1 73.0(3) . . ? C10 C11 H11 126.1 . . ? C12 C11 H11 126.1 . . ? Zr1 C11 H11 118.2 . . ? C13 C12 C11 107.9(6) . . ? C13 C12 Zr1 74.7(3) . . ? C11 C12 Zr1 75.5(3) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Zr1 C12 H12 115.9 . . ? C14 C13 C12 108.8(5) . . ? C14 C13 Zr1 74.1(3) . . ? C12 C13 Zr1 74.1(3) . . ? C14 C13 H13 125.6 . . ? C12 C13 H13 125.6 . . ? Zr1 C13 H13 118.1 . . ? C13 C14 C10 108.1(6) . . ? C13 C14 Zr1 74.7(3) . . ? C10 C14 Zr1 75.8(3) . . ? C13 C14 H14 126.0 . . ? C10 C14 H14 126.0 . . ? Zr1 C14 H14 115.7 . . ? C19 C15 C16 108.3(5) . . ? C19 C15 Zr1 75.0(3) . . ? C16 C15 Zr1 72.9(3) . . ? C19 C15 H15 125.9 . . ? C16 C15 H15 125.9 . . ? Zr1 C15 H15 118.1 . . ? C17 C16 C15 107.9(5) . . ? C17 C16 Zr1 75.2(3) . . ? C15 C16 Zr1 74.7(3) . . ? C17 C16 H16 126.0 . . ? C15 C16 H16 126.0 . . ? Zr1 C16 H16 116.2 . . ? C16 C17 C18 107.7(5) . . ? C16 C17 Zr1 73.0(3) . . ? C18 C17 Zr1 74.1(3) . . ? C16 C17 H17 126.2 . . ? C18 C17 H17 126.2 . . ? Zr1 C17 H17 118.7 . . ? C17 C18 C19 108.2(5) . . ? C17 C18 Zr1 74.0(3) . . ? C19 C18 Zr1 74.4(3) . . ? C17 C18 H18 125.9 . . ? C19 C18 H18 125.9 . . ? Zr1 C18 H18 117.6 . . ? C15 C19 C18 108.0(5) . . ? C15 C19 Zr1 73.7(3) . . ? C18 C19 Zr1 73.7(3) . . ? C15 C19 H19 126.0 . . ? C18 C19 H19 126.0 . . ? Zr1 C19 H19 118.6 . . ? C21 C20 C24 105.7(5) . . ? C21 C20 Zr2 73.5(3) . . ? C24 C20 Zr2 73.6(3) . . ? C21 C20 H20 127.2 . . ? C24 C20 H20 127.2 . . ? Zr2 C20 H20 117.9 . . ? C22 C21 C20 108.0(5) . . ? C22 C21 Zr2 74.6(3) . . ? C20 C21 Zr2 74.5(3) . . ? C22 C21 H21 126.0 . . ? C20 C21 H21 126.0 . . ? Zr2 C21 H21 117.0 . . ? C23 C22 C21 109.3(5) . . ? C23 C22 Zr2 74.4(3) . . ? C21 C22 Zr2 74.3(3) . . ? C23 C22 H22 125.4 . . ? C21 C22 H22 125.4 . . ? Zr2 C22 H22 117.8 . . ? C22 C23 C24 109.5(5) . . ? C22 C23 Zr2 75.0(3) . . ? C24 C23 Zr2 74.8(3) . . ? C22 C23 H23 125.2 . . ? C24 C23 H23 125.2 . . ? Zr2 C23 H23 116.9 . . ? C23 C24 C20 107.5(5) . . ? C23 C24 Zr2 74.1(3) . . ? C20 C24 Zr2 74.1(3) . . ? C23 C24 H24 126.3 . . ? C20 C24 H24 126.3 . . ? Zr2 C24 H24 117.6 . . ? C26 C25 C29 108.2(6) . . ? C26 C25 Zr2 74.5(4) . . ? C29 C25 Zr2 74.0(3) . . ? C26 C25 H25 125.9 . . ? C29 C25 H25 125.9 . . ? Zr2 C25 H25 117.6 . . ? C25 C26 C27 109.2(6) . . ? C25 C26 Zr2 74.8(4) . . ? C27 C26 Zr2 74.6(4) . . ? C25 C26 H26 125.4 . . ? C27 C26 H26 125.4 . . ? Zr2 C26 H26 117.2 . . ? C26 C27 C28 107.1(7) . . ? C26 C27 Zr2 74.4(4) . . ? C28 C27 Zr2 74.1(3) . . ? C26 C27 H27 126.5 . . ? C28 C27 H27 126.5 . . ? Zr2 C27 H27 117.1 . . ? C27 C28 C29 108.0(6) . . ? C27 C28 Zr2 74.6(3) . . ? C29 C28 Zr2 74.1(3) . . ? C27 C28 H28 126.0 . . ? C29 C28 H28 126.0 . . ? Zr2 C28 H28 117.4 . . ? C25 C29 C28 107.5(6) . . ? C25 C29 Zr2 74.9(3) . . ? C28 C29 Zr2 74.5(3) . . ? C25 C29 H29 126.3 . . ? C28 C29 H29 126.3 . . ? Zr2 C29 H29 116.5 . . ? C32 C31 C36 117.3(4) . . ? C32 C31 C3 123.8(4) . . ? C36 C31 C3 118.8(4) . . ? C33 C32 C31 121.0(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 120.8(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 119.2(5) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 121.8(4) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? 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 C4 Zr2 C1 C2 6.3(3) . . . . ? C29 Zr2 C1 C2 -111.3(4) . . . . ? C28 Zr2 C1 C2 -136.3(3) . . . . ? C26 Zr2 C1 C2 -90.5(4) . . . . ? C27 Zr2 C1 C2 -121.5(4) . . . . ? C25 Zr2 C1 C2 -80.8(3) . . . . ? C23 Zr2 C1 C2 96.5(3) . . . . ? C21 Zr2 C1 C2 144.2(3) . . . . ? C22 Zr2 C1 C2 134.5(3) . . . . ? C24 Zr2 C1 C2 91.6(3) . . . . ? C4 Zr2 C1 C5 -173.5(5) . . . . ? C2 Zr2 C1 C5 -179.8(7) . . . . ? C29 Zr2 C1 C5 68.9(6) . . . . ? C28 Zr2 C1 C5 43.9(6) . . . . ? C26 Zr2 C1 C5 89.7(6) . . . . ? C27 Zr2 C1 C5 58.7(6) . . . . ? C25 Zr2 C1 C5 99.4(6) . . . . ? C23 Zr2 C1 C5 -83.3(6) . . . . ? C21 Zr2 C1 C5 -35.6(6) . . . . ? C22 Zr2 C1 C5 -45.2(6) . . . . ? C24 Zr2 C1 C5 -88.2(6) . . . . ? C5 C1 C2 Zr1 -160(3) . . . . ? Zr2 C1 C2 Zr1 21(3) . . . . ? C5 C1 C2 Zr2 179.8(7) . . . . ? C16 Zr1 C2 C1 -156(3) . . . . ? C4 Zr1 C2 C1 -28(3) . . . . ? C14 Zr1 C2 C1 83(3) . . . . ? C12 Zr1 C2 C1 119(3) . . . . ? C15 Zr1 C2 C1 -128(3) . . . . ? C17 Zr1 C2 C1 -150(3) . . . . ? C18 Zr1 C2 C1 -111(3) . . . . ? C13 Zr1 C2 C1 119(3) . . . . ? C19 Zr1 C2 C1 -103(3) . . . . ? C11 Zr1 C2 C1 90(3) . . . . ? C10 Zr1 C2 C1 68(3) . . . . ? C16 Zr1 C2 Zr2 -136.18(17) . . . . ? C4 Zr1 C2 Zr2 -7.56(14) . . . . ? C14 Zr1 C2 Zr2 102.8(2) . . . . ? C12 Zr1 C2 Zr2 139.27(19) . . . . ? C15 Zr1 C2 Zr2 -108.5(2) . . . . ? C17 Zr1 C2 Zr2 -130.44(18) . . . . ? C18 Zr1 C2 Zr2 -91.3(2) . . . . ? C13 Zr1 C2 Zr2 139.33(19) . . . . ? C19 Zr1 C2 Zr2 -83.24(17) . . . . ? C11 Zr1 C2 Zr2 109.8(2) . . . . ? C10 Zr1 C2 Zr2 88.28(18) . . . . ? C4 Zr2 C2 C1 -174.1(3) . . . . ? C29 Zr2 C2 C1 99.0(4) . . . . ? C28 Zr2 C2 C1 57.0(4) . . . . ? C26 Zr2 C2 C1 87.1(4) . . . . ? C27 Zr2 C2 C1 58.3(3) . . . . ? C25 Zr2 C2 C1 110.2(3) . . . . ? C23 Zr2 C2 C1 -104.2(3) . . . . ? C21 Zr2 C2 C1 -42.6(3) . . . . ? C22 Zr2 C2 C1 -72.6(4) . . . . ? C24 Zr2 C2 C1 -90.7(3) . . . . ? C4 Zr2 C2 Zr1 8.40(15) . . . . ? C1 Zr2 C2 Zr1 -177.5(4) . . . . ? C29 Zr2 C2 Zr1 -78.4(3) . . . . ? C28 Zr2 C2 Zr1 -120.5(2) . . . . ? C26 Zr2 C2 Zr1 -90.4(3) . . . . ? C27 Zr2 C2 Zr1 -119.2(2) . . . . ? C25 Zr2 C2 Zr1 -67.2(2) . . . . ? C23 Zr2 C2 Zr1 78.4(2) . . . . ? C21 Zr2 C2 Zr1 139.92(17) . . . . ? C22 Zr2 C2 Zr1 110.0(3) . . . . ? C24 Zr2 C2 Zr1 91.88(19) . . . . ? C2 Zr1 C3 C4 -30.9(3) . . . . ? C16 Zr1 C3 C4 88.2(3) . . . . ? C14 Zr1 C3 C4 -158.6(3) . . . . ? C12 Zr1 C3 C4 -135.8(3) . . . . ? C15 Zr1 C3 C4 53.6(3) . . . . ? C17 Zr1 C3 C4 112.8(3) . . . . ? C18 Zr1 C3 C4 95.7(3) . . . . ? C13 Zr1 C3 C4 -166.3(3) . . . . ? C19 Zr1 C3 C4 64.0(3) . . . . ? C11 Zr1 C3 C4 -112.1(3) . . . . ? C10 Zr1 C3 C4 -126.8(3) . . . . ? C2 Zr1 C3 C31 -155.5(3) . . . . ? C16 Zr1 C3 C31 -36.3(4) . . . . ? C4 Zr1 C3 C31 -124.6(4) . . . . ? C14 Zr1 C3 C31 76.8(3) . . . . ? C12 Zr1 C3 C31 99.6(4) . . . . ? C15 Zr1 C3 C31 -71.0(4) . . . . ? C17 Zr1 C3 C31 -11.8(4) . . . . ? C18 Zr1 C3 C31 -28.9(3) . . . . ? C13 Zr1 C3 C31 69.1(4) . . . . ? C19 Zr1 C3 C31 -60.6(3) . . . . ? C11 Zr1 C3 C31 123.3(3) . . . . ? C10 Zr1 C3 C31 108.7(4) . . . . ? C31 C3 C4 Zr2 -162.2(4) . . . . ? Zr1 C3 C4 Zr2 79.5(4) . . . . ? C31 C3 C4 Zr1 118.3(4) . . . . ? C1 Zr2 C4 C3 -83.9(5) . . . . ? C2 Zr2 C4 C3 -80.7(5) . . . . ? C29 Zr2 C4 C3 55.3(5) . . . . ? C28 Zr2 C4 C3 52.3(6) . . . . ? C26 Zr2 C4 C3 4.1(5) . . . . ? C27 Zr2 C4 C3 13.6(6) . . . . ? C25 Zr2 C4 C3 27.6(5) . . . . ? C23 Zr2 C4 C3 153.4(5) . . . . ? C21 Zr2 C4 C3 154.6(5) . . . . ? C22 Zr2 C4 C3 135.8(5) . . . . ? C24 Zr2 C4 C3 -175.8(5) . . . . ? C1 Zr2 C4 Zr1 -10.39(19) . . . . ? C2 Zr2 C4 Zr1 -7.20(13) . . . . ? C29 Zr2 C4 Zr1 128.88(18) . . . . ? C28 Zr2 C4 Zr1 125.8(2) . . . . ? C26 Zr2 C4 Zr1 77.63(19) . . . . ? C27 Zr2 C4 Zr1 87.1(3) . . . . ? C25 Zr2 C4 Zr1 101.2(3) . . . . ? C23 Zr2 C4 Zr1 -133.08(18) . . . . ? C21 Zr2 C4 Zr1 -131.9(2) . . . . ? C22 Zr2 C4 Zr1 -150.63(15) . . . . ? C24 Zr2 C4 Zr1 -102.25(17) . . . . ? C2 Zr1 C4 C3 150.8(3) . . . . ? C16 Zr1 C4 C3 -121.8(3) . . . . ? C14 Zr1 C4 C3 22.7(3) . . . . ? C12 Zr1 C4 C3 74.9(4) . . . . ? C15 Zr1 C4 C3 -135.0(3) . . . . ? C17 Zr1 C4 C3 -83.5(3) . . . . ? C18 Zr1 C4 C3 -83.1(3) . . . . ? C13 Zr1 C4 C3 21.0(4) . . . . ? C19 Zr1 C4 C3 -112.5(3) . . . . ? C11 Zr1 C4 C3 79.1(3) . . . . ? C10 Zr1 C4 C3 52.0(3) . . . . ? C2 Zr1 C4 Zr2 7.95(15) . . . . ? C16 Zr1 C4 Zr2 95.4(2) . . . . ? C14 Zr1 C4 Zr2 -120.18(18) . . . . ? C12 Zr1 C4 Zr2 -67.9(4) . . . . ? C15 Zr1 C4 Zr2 82.21(18) . . . . ? C17 Zr1 C4 Zr2 133.63(16) . . . . ? C18 Zr1 C4 Zr2 134.10(17) . . . . ? C13 Zr1 C4 Zr2 -121.9(3) . . . . ? C19 Zr1 C4 Zr2 104.7(2) . . . . ? C11 Zr1 C4 Zr2 -63.7(2) . . . . ? C10 Zr1 C4 Zr2 -90.9(2) . . . . ? C2 C1 C5 C8 -67.4(9) . . . . ? Zr2 C1 C5 C8 112.3(6) . . . . ? C2 C1 C5 C7 50.4(9) . . . . ? Zr2 C1 C5 C7 -129.9(6) . . . . ? C2 C1 C5 C6 174.0(8) . . . . ? Zr2 C1 C5 C6 -6.3(9) . . . . ? C2 Zr1 C10 C11 43.5(4) . . . . ? C16 Zr1 C10 C11 -60.2(5) . . . . ? C4 Zr1 C10 C11 126.6(4) . . . . ? C14 Zr1 C10 C11 -114.5(5) . . . . ? C12 Zr1 C10 C11 -37.2(4) . . . . ? C15 Zr1 C10 C11 -29.3(9) . . . . ? C17 Zr1 C10 C11 -98.6(4) . . . . ? C18 Zr1 C10 C11 -137.0(4) . . . . ? C13 Zr1 C10 C11 -77.3(4) . . . . ? C19 Zr1 C10 C11 -167.5(5) . . . . ? C2 Zr1 C10 C14 158.0(4) . . . . ? C16 Zr1 C10 C14 54.3(5) . . . . ? C4 Zr1 C10 C14 -118.9(4) . . . . ? C12 Zr1 C10 C14 77.3(4) . . . . ? C15 Zr1 C10 C14 85.1(8) . . . . ? C17 Zr1 C10 C14 15.8(5) . . . . ? C18 Zr1 C10 C14 -22.5(5) . . . . ? C13 Zr1 C10 C14 37.2(4) . . . . ? C19 Zr1 C10 C14 -53.0(8) . . . . ? C11 Zr1 C10 C14 114.5(5) . . . . ? C14 C10 C11 C12 0.4(6) . . . . ? Zr1 C10 C11 C12 66.0(4) . . . . ? C14 C10 C11 Zr1 -65.6(3) . . . . ? C2 Zr1 C11 C10 -135.8(4) . . . . ? C16 Zr1 C11 C10 136.8(4) . . . . ? C4 Zr1 C11 C10 -60.9(4) . . . . ? C14 Zr1 C11 C10 37.2(3) . . . . ? C12 Zr1 C11 C10 114.5(5) . . . . ? C15 Zr1 C11 C10 168.6(3) . . . . ? C17 Zr1 C11 C10 101.7(4) . . . . ? C18 Zr1 C11 C10 80.6(6) . . . . ? C13 Zr1 C11 C10 77.2(4) . . . . ? C19 Zr1 C11 C10 166.5(6) . . . . ? C2 Zr1 C11 C12 109.7(4) . . . . ? C16 Zr1 C11 C12 22.3(5) . . . . ? C4 Zr1 C11 C12 -175.4(4) . . . . ? C14 Zr1 C11 C12 -77.3(4) . . . . ? C15 Zr1 C11 C12 54.1(5) . . . . ? C17 Zr1 C11 C12 -12.8(5) . . . . ? C18 Zr1 C11 C12 -33.9(7) . . . . ? C13 Zr1 C11 C12 -37.3(4) . . . . ? C19 Zr1 C11 C12 52.0(8) . . . . ? C10 Zr1 C11 C12 -114.5(5) . . . . ? C10 C11 C12 C13 1.2(6) . . . . ? Zr1 C11 C12 C13 68.3(4) . . . . ? C10 C11 C12 Zr1 -67.1(4) . . . . ? C2 Zr1 C12 C13 179.9(4) . . . . ? C16 Zr1 C12 C13 86.8(4) . . . . ? C4 Zr1 C12 C13 -106.2(5) . . . . ? C14 Zr1 C12 C13 -36.4(4) . . . . ? C15 Zr1 C12 C13 105.7(4) . . . . ? C17 Zr1 C12 C13 55.5(4) . . . . ? C18 Zr1 C12 C13 47.6(5) . . . . ? C19 Zr1 C12 C13 84.4(5) . . . . ? C11 Zr1 C12 C13 -113.6(6) . . . . ? C10 Zr1 C12 C13 -76.8(4) . . . . ? C2 Zr1 C12 C11 -66.5(4) . . . . ? C16 Zr1 C12 C11 -159.6(4) . . . . ? C4 Zr1 C12 C11 7.4(6) . . . . ? C14 Zr1 C12 C11 77.2(4) . . . . ? C15 Zr1 C12 C11 -140.7(4) . . . . ? C17 Zr1 C12 C11 169.1(4) . . . . ? C18 Zr1 C12 C11 161.2(4) . . . . ? C13 Zr1 C12 C11 113.6(6) . . . . ? C19 Zr1 C12 C11 -162.0(4) . . . . ? C10 Zr1 C12 C11 36.8(4) . . . . ? C11 C12 C13 C14 -2.3(6) . . . . ? Zr1 C12 C13 C14 66.5(4) . . . . ? C11 C12 C13 Zr1 -68.8(4) . . . . ? C2 Zr1 C13 C14 -115.5(4) . . . . ? C16 Zr1 C13 C14 154.7(4) . . . . ? C4 Zr1 C13 C14 3.0(6) . . . . ? C12 Zr1 C13 C14 -115.4(5) . . . . ? C15 Zr1 C13 C14 156.4(4) . . . . ? C17 Zr1 C13 C14 123.7(4) . . . . ? C18 Zr1 C13 C14 103.9(4) . . . . ? C19 Zr1 C13 C14 121.6(4) . . . . ? C11 Zr1 C13 C14 -77.8(4) . . . . ? C10 Zr1 C13 C14 -37.6(4) . . . . ? C2 Zr1 C13 C12 -0.1(5) . . . . ? C16 Zr1 C13 C12 -89.9(4) . . . . ? C4 Zr1 C13 C12 118.5(5) . . . . ? C14 Zr1 C13 C12 115.4(5) . . . . ? C15 Zr1 C13 C12 -88.2(4) . . . . ? C17 Zr1 C13 C12 -120.9(4) . . . . ? C18 Zr1 C13 C12 -140.6(4) . . . . ? C19 Zr1 C13 C12 -123.0(4) . . . . ? C11 Zr1 C13 C12 37.7(4) . . . . ? C10 Zr1 C13 C12 77.8(4) . . . . ? C12 C13 C14 C10 2.5(6) . . . . ? Zr1 C13 C14 C10 69.0(4) . . . . ? C12 C13 C14 Zr1 -66.5(4) . . . . ? C11 C10 C14 C13 -1.8(6) . . . . ? Zr1 C10 C14 C13 -68.3(4) . . . . ? C11 C10 C14 Zr1 66.6(4) . . . . ? C2 Zr1 C14 C13 85.5(5) . . . . ? C16 Zr1 C14 C13 -27.3(4) . . . . ? C4 Zr1 C14 C13 -178.0(4) . . . . ? C12 Zr1 C14 C13 36.5(4) . . . . ? C15 Zr1 C14 C13 -37.1(6) . . . . ? C17 Zr1 C14 C13 -53.1(4) . . . . ? C18 Zr1 C14 C13 -82.7(4) . . . . ? C19 Zr1 C14 C13 -85.7(4) . . . . ? C11 Zr1 C14 C13 76.8(4) . . . . ? C10 Zr1 C14 C13 113.7(6) . . . . ? C2 Zr1 C14 C10 -28.1(5) . . . . ? C16 Zr1 C14 C10 -141.0(4) . . . . ? C4 Zr1 C14 C10 68.3(4) . . . . ? C12 Zr1 C14 C10 -77.2(4) . . . . ? C15 Zr1 C14 C10 -150.7(4) . . . . ? C17 Zr1 C14 C10 -166.7(4) . . . . ? C18 Zr1 C14 C10 163.6(4) . . . . ? C13 Zr1 C14 C10 -113.7(6) . . . . ? C19 Zr1 C14 C10 160.6(4) . . . . ? C11 Zr1 C14 C10 -36.8(4) . . . . ? C2 Zr1 C15 C19 125.1(3) . . . . ? C16 Zr1 C15 C19 -115.0(5) . . . . ? C4 Zr1 C15 C19 45.6(3) . . . . ? C14 Zr1 C15 C19 -97.8(4) . . . . ? C12 Zr1 C15 C19 -151.9(4) . . . . ? C17 Zr1 C15 C19 -77.6(4) . . . . ? C18 Zr1 C15 C19 -37.2(3) . . . . ? C13 Zr1 C15 C19 -118.1(4) . . . . ? C11 Zr1 C15 C19 -178.9(3) . . . . ? C10 Zr1 C15 C19 -158.5(6) . . . . ? C2 Zr1 C15 C16 -119.9(4) . . . . ? C4 Zr1 C15 C16 160.6(3) . . . . ? C14 Zr1 C15 C16 17.2(6) . . . . ? C12 Zr1 C15 C16 -36.9(4) . . . . ? C17 Zr1 C15 C16 37.3(3) . . . . ? C18 Zr1 C15 C16 77.7(4) . . . . ? C13 Zr1 C15 C16 -3.2(4) . . . . ? C19 Zr1 C15 C16 115.0(5) . . . . ? C11 Zr1 C15 C16 -64.0(4) . . . . ? C10 Zr1 C15 C16 -43.6(8) . . . . ? C19 C15 C16 C17 -1.2(5) . . . . ? Zr1 C15 C16 C17 -68.5(3) . . . . ? C19 C15 C16 Zr1 67.3(3) . . . . ? C2 Zr1 C16 C17 171.0(3) . . . . ? C4 Zr1 C16 C17 88.8(4) . . . . ? C14 Zr1 C16 C17 -55.3(4) . . . . ? C12 Zr1 C16 C17 -100.5(4) . . . . ? C15 Zr1 C16 C17 113.7(5) . . . . ? C18 Zr1 C16 C17 37.1(3) . . . . ? C13 Zr1 C16 C17 -69.2(4) . . . . ? C19 Zr1 C16 C17 77.4(4) . . . . ? C11 Zr1 C16 C17 -112.1(3) . . . . ? C10 Zr1 C16 C17 -82.6(4) . . . . ? C2 Zr1 C16 C15 57.3(4) . . . . ? C4 Zr1 C16 C15 -24.9(4) . . . . ? C14 Zr1 C16 C15 -169.1(3) . . . . ? C12 Zr1 C16 C15 145.7(4) . . . . ? C17 Zr1 C16 C15 -113.7(5) . . . . ? C18 Zr1 C16 C15 -76.7(4) . . . . ? C13 Zr1 C16 C15 177.1(4) . . . . ? C19 Zr1 C16 C15 -36.3(3) . . . . ? C11 Zr1 C16 C15 134.2(4) . . . . ? C10 Zr1 C16 C15 163.7(4) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? Zr1 C16 C17 C18 -66.6(3) . . . . ? C15 C16 C17 Zr1 68.2(3) . . . . ? C2 Zr1 C17 C16 -10.9(4) . . . . ? C4 Zr1 C17 C16 -113.8(3) . . . . ? C14 Zr1 C17 C16 130.2(3) . . . . ? C12 Zr1 C17 C16 78.2(4) . . . . ? C15 Zr1 C17 C16 -37.9(3) . . . . ? C18 Zr1 C17 C16 -114.6(5) . . . . ? C13 Zr1 C17 C16 104.6(4) . . . . ? C19 Zr1 C17 C16 -77.5(4) . . . . ? C11 Zr1 C17 C16 84.9(4) . . . . ? C10 Zr1 C17 C16 122.0(3) . . . . ? C2 Zr1 C17 C18 103.7(3) . . . . ? C16 Zr1 C17 C18 114.6(5) . . . . ? C4 Zr1 C17 C18 0.9(4) . . . . ? C14 Zr1 C17 C18 -115.2(3) . . . . ? C12 Zr1 C17 C18 -167.1(3) . . . . ? C15 Zr1 C17 C18 76.7(4) . . . . ? C13 Zr1 C17 C18 -140.7(4) . . . . ? C19 Zr1 C17 C18 37.1(3) . . . . ? C11 Zr1 C17 C18 -160.5(3) . . . . ? C10 Zr1 C17 C18 -123.4(3) . . . . ? C16 C17 C18 C19 -1.4(5) . . . . ? Zr1 C17 C18 C19 -67.2(3) . . . . ? C16 C17 C18 Zr1 65.8(3) . . . . ? C2 Zr1 C18 C17 -99.3(3) . . . . ? C16 Zr1 C18 C17 -37.1(3) . . . . ? C4 Zr1 C18 C17 -179.2(3) . . . . ? C14 Zr1 C18 C17 69.3(4) . . . . ? C12 Zr1 C18 C17 15.2(4) . . . . ? C15 Zr1 C18 C17 -78.1(3) . . . . ? C13 Zr1 C18 C17 38.0(4) . . . . ? C19 Zr1 C18 C17 -114.6(5) . . . . ? C11 Zr1 C18 C17 35.3(6) . . . . ? C10 Zr1 C18 C17 81.3(4) . . . . ? C2 Zr1 C18 C19 15.3(4) . . . . ? C16 Zr1 C18 C19 77.6(4) . . . . ? C4 Zr1 C18 C19 -64.6(3) . . . . ? C14 Zr1 C18 C19 -176.1(4) . . . . ? C12 Zr1 C18 C19 129.8(4) . . . . ? C15 Zr1 C18 C19 36.5(3) . . . . ? C17 Zr1 C18 C19 114.6(5) . . . . ? C13 Zr1 C18 C19 152.6(4) . . . . ? C11 Zr1 C18 C19 149.9(5) . . . . ? C10 Zr1 C18 C19 -164.1(3) . . . . ? C16 C15 C19 C18 0.3(5) . . . . ? Zr1 C15 C19 C18 66.2(3) . . . . ? C16 C15 C19 Zr1 -65.9(3) . . . . ? C17 C18 C19 C15 0.6(5) . . . . ? Zr1 C18 C19 C15 -66.2(3) . . . . ? C17 C18 C19 Zr1 66.9(3) . . . . ? C2 Zr1 C19 C15 -52.7(3) . . . . ? C16 Zr1 C19 C15 37.5(3) . . . . ? C4 Zr1 C19 C15 -133.4(3) . . . . ? C14 Zr1 C19 C15 120.5(4) . . . . ? C12 Zr1 C19 C15 40.5(5) . . . . ? C17 Zr1 C19 C15 77.8(3) . . . . ? C18 Zr1 C19 C15 114.9(5) . . . . ? C13 Zr1 C19 C15 80.4(4) . . . . ? C11 Zr1 C19 C15 2.9(8) . . . . ? C10 Zr1 C19 C15 157.9(6) . . . . ? C2 Zr1 C19 C18 -167.6(3) . . . . ? C16 Zr1 C19 C18 -77.4(4) . . . . ? C4 Zr1 C19 C18 111.7(4) . . . . ? C14 Zr1 C19 C18 5.6(5) . . . . ? C12 Zr1 C19 C18 -74.4(5) . . . . ? C15 Zr1 C19 C18 -114.9(5) . . . . ? C17 Zr1 C19 C18 -37.1(3) . . . . ? C13 Zr1 C19 C18 -34.5(5) . . . . ? C11 Zr1 C19 C18 -112.0(7) . . . . ? C10 Zr1 C19 C18 43.0(7) . . . . ? C4 Zr2 C20 C21 -122.4(4) . . . . ? C1 Zr2 C20 C21 128.0(4) . . . . ? C2 Zr2 C20 C21 154.0(4) . . . . ? C29 Zr2 C20 C21 -6.4(5) . . . . ? C28 Zr2 C20 C21 21.5(5) . . . . ? C26 Zr2 C20 C21 67.2(5) . . . . ? C27 Zr2 C20 C21 54.0(4) . . . . ? C25 Zr2 C20 C21 4.1(9) . . . . ? C23 Zr2 C20 C21 -75.7(4) . . . . ? C22 Zr2 C20 C21 -36.7(3) . . . . ? C24 Zr2 C20 C21 -112.4(5) . . . . ? C4 Zr2 C20 C24 -10.0(4) . . . . ? C1 Zr2 C20 C24 -119.6(4) . . . . ? C2 Zr2 C20 C24 -93.6(3) . . . . ? C29 Zr2 C20 C24 105.9(4) . . . . ? C28 Zr2 C20 C24 133.9(4) . . . . ? C26 Zr2 C20 C24 179.6(3) . . . . ? C27 Zr2 C20 C24 166.4(4) . . . . ? C25 Zr2 C20 C24 116.5(7) . . . . ? C23 Zr2 C20 C24 36.7(3) . . . . ? C21 Zr2 C20 C24 112.4(5) . . . . ? C22 Zr2 C20 C24 75.7(4) . . . . ? C24 C20 C21 C22 0.5(6) . . . . ? Zr2 C20 C21 C22 67.6(3) . . . . ? C24 C20 C21 Zr2 -67.1(3) . . . . ? C4 Zr2 C21 C22 -37.4(5) . . . . ? C1 Zr2 C21 C22 -165.0(4) . . . . ? C2 Zr2 C21 C22 -145.0(3) . . . . ? C29 Zr2 C21 C22 60.6(4) . . . . ? C28 Zr2 C21 C22 86.7(4) . . . . ? C26 Zr2 C21 C22 105.8(4) . . . . ? C27 Zr2 C21 C22 112.7(4) . . . . ? C25 Zr2 C21 C22 67.7(4) . . . . ? C23 Zr2 C21 C22 -35.9(3) . . . . ? C24 Zr2 C21 C22 -75.7(4) . . . . ? C4 Zr2 C21 C20 76.8(5) . . . . ? C1 Zr2 C21 C20 -50.8(4) . . . . ? C2 Zr2 C21 C20 -30.8(4) . . . . ? C29 Zr2 C21 C20 174.9(4) . . . . ? C28 Zr2 C21 C20 -159.1(5) . . . . ? C26 Zr2 C21 C20 -140.0(4) . . . . ? C27 Zr2 C21 C20 -133.0(4) . . . . ? C25 Zr2 C21 C20 -178.1(4) . . . . ? C23 Zr2 C21 C20 78.3(4) . . . . ? C22 Zr2 C21 C20 114.2(5) . . . . ? C24 Zr2 C21 C20 38.5(3) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? Zr2 C21 C22 C23 66.8(4) . . . . ? C20 C21 C22 Zr2 -67.5(3) . . . . ? C4 Zr2 C22 C23 35.3(4) . . . . ? C1 Zr2 C22 C23 -97.0(4) . . . . ? C2 Zr2 C22 C23 -59.9(5) . . . . ? C29 Zr2 C22 C23 126.0(4) . . . . ? C28 Zr2 C22 C23 157.9(4) . . . . ? C26 Zr2 C22 C23 146.1(5) . . . . ? C27 Zr2 C22 C23 171.3(4) . . . . ? C25 Zr2 C22 C23 117.2(4) . . . . ? C21 Zr2 C22 C23 -115.7(5) . . . . ? C24 Zr2 C22 C23 -36.6(3) . . . . ? C4 Zr2 C22 C21 151.0(4) . . . . ? C1 Zr2 C22 C21 18.8(4) . . . . ? C2 Zr2 C22 C21 55.8(5) . . . . ? C29 Zr2 C22 C21 -118.3(4) . . . . ? C28 Zr2 C22 C21 -86.3(4) . . . . ? C26 Zr2 C22 C21 -98.1(5) . . . . ? C27 Zr2 C22 C21 -72.9(4) . . . . ? C25 Zr2 C22 C21 -127.1(4) . . . . ? C23 Zr2 C22 C21 115.7(5) . . . . ? C24 Zr2 C22 C21 79.1(4) . . . . ? C21 C22 C23 C24 0.7(6) . . . . ? Zr2 C22 C23 C24 67.4(3) . . . . ? C21 C22 C23 Zr2 -66.7(4) . . . . ? C4 Zr2 C23 C22 -144.7(4) . . . . ? C1 Zr2 C23 C22 106.0(4) . . . . ? C2 Zr2 C23 C22 142.3(3) . . . . ? C29 Zr2 C23 C22 -53.7(4) . . . . ? C28 Zr2 C23 C22 -22.5(4) . . . . ? C26 Zr2 C23 C22 -60.2(7) . . . . ? C27 Zr2 C23 C22 -12.1(5) . . . . ? C25 Zr2 C23 C22 -76.8(4) . . . . ? C21 Zr2 C23 C22 36.5(3) . . . . ? C24 Zr2 C23 C22 115.6(5) . . . . ? C4 Zr2 C23 C24 99.7(3) . . . . ? C1 Zr2 C23 C24 -9.6(4) . . . . ? C2 Zr2 C23 C24 26.8(4) . . . . ? C29 Zr2 C23 C24 -169.3(4) . . . . ? C28 Zr2 C23 C24 -138.0(4) . . . . ? C26 Zr2 C23 C24 -175.7(5) . . . . ? C27 Zr2 C23 C24 -127.6(4) . . . . ? C25 Zr2 C23 C24 167.6(3) . . . . ? C21 Zr2 C23 C24 -79.1(4) . . . . ? C22 Zr2 C23 C24 -115.6(5) . . . . ? C22 C23 C24 C20 -0.4(6) . . . . ? Zr2 C23 C24 C20 67.2(3) . . . . ? C22 C23 C24 Zr2 -67.6(4) . . . . ? C21 C20 C24 C23 -0.1(5) . . . . ? Zr2 C20 C24 C23 -67.1(3) . . . . ? C21 C20 C24 Zr2 67.1(3) . . . . ? C4 Zr2 C24 C23 -75.1(3) . . . . ? C1 Zr2 C24 C23 172.1(3) . . . . ? C2 Zr2 C24 C23 -157.7(3) . . . . ? C29 Zr2 C24 C23 13.7(5) . . . . ? C28 Zr2 C24 C23 54.0(5) . . . . ? C26 Zr2 C24 C23 108(5) . . . . ? C27 Zr2 C24 C23 91.3(5) . . . . ? C25 Zr2 C24 C23 -22.2(6) . . . . ? C21 Zr2 C24 C23 75.8(4) . . . . ? C22 Zr2 C24 C23 36.0(3) . . . . ? C4 Zr2 C24 C20 170.9(4) . . . . ? C1 Zr2 C24 C20 58.2(4) . . . . ? C2 Zr2 C24 C20 88.4(4) . . . . ? C29 Zr2 C24 C20 -100.2(4) . . . . ? C28 Zr2 C24 C20 -60.0(5) . . . . ? C26 Zr2 C24 C20 -6(5) . . . . ? C27 Zr2 C24 C20 -22.6(6) . . . . ? C25 Zr2 C24 C20 -136.2(5) . . . . ? C23 Zr2 C24 C20 -113.9(5) . . . . ? C21 Zr2 C24 C20 -38.2(3) . . . . ? C22 Zr2 C24 C20 -78.0(4) . . . . ? C4 Zr2 C25 C26 -129.3(5) . . . . ? C1 Zr2 C25 C26 -19.2(5) . . . . ? C2 Zr2 C25 C26 -50.2(5) . . . . ? C29 Zr2 C25 C26 114.6(6) . . . . ? C28 Zr2 C25 C26 76.9(5) . . . . ? C27 Zr2 C25 C26 36.6(4) . . . . ? C23 Zr2 C25 C26 163.4(5) . . . . ? C21 Zr2 C25 C26 100.9(6) . . . . ? C22 Zr2 C25 C26 131.5(5) . . . . ? C24 Zr2 C25 C26 176.6(4) . . . . ? C4 Zr2 C25 C29 116.0(5) . . . . ? C1 Zr2 C25 C29 -133.8(4) . . . . ? C2 Zr2 C25 C29 -164.9(4) . . . . ? C28 Zr2 C25 C29 -37.7(4) . . . . ? C26 Zr2 C25 C29 -114.6(6) . . . . ? C27 Zr2 C25 C29 -78.1(5) . . . . ? C23 Zr2 C25 C29 48.8(5) . . . . ? C21 Zr2 C25 C29 -13.7(6) . . . . ? C22 Zr2 C25 C29 16.9(5) . . . . ? C24 Zr2 C25 C29 61.9(6) . . . . ? C29 C25 C26 C27 -0.4(7) . . . . ? Zr2 C25 C26 C27 -67.2(4) . . . . ? C29 C25 C26 Zr2 66.9(4) . . . . ? C4 Zr2 C26 C25 50.0(5) . . . . ? C1 Zr2 C26 C25 162.5(5) . . . . ? C2 Zr2 C26 C25 132.3(5) . . . . ? C29 Zr2 C26 C25 -37.1(4) . . . . ? C28 Zr2 C26 C25 -77.7(5) . . . . ? C27 Zr2 C26 C25 -115.4(6) . . . . ? C23 Zr2 C26 C25 -28.9(9) . . . . ? C21 Zr2 C26 C25 -101.9(6) . . . . ? C22 Zr2 C26 C25 -62.8(7) . . . . ? C24 Zr2 C26 C25 -133(5) . . . . ? C4 Zr2 C26 C27 165.4(5) . . . . ? C1 Zr2 C26 C27 -82.1(5) . . . . ? C2 Zr2 C26 C27 -112.3(5) . . . . ? C29 Zr2 C26 C27 78.3(5) . . . . ? C28 Zr2 C26 C27 37.7(4) . . . . ? C25 Zr2 C26 C27 115.4(6) . . . . ? C23 Zr2 C26 C27 86.5(8) . . . . ? C21 Zr2 C26 C27 13.5(7) . . . . ? C22 Zr2 C26 C27 52.6(7) . . . . ? C24 Zr2 C26 C27 -18(5) . . . . ? C25 C26 C27 C28 -0.1(7) . . . . ? Zr2 C26 C27 C28 -67.5(4) . . . . ? C25 C26 C27 Zr2 67.4(4) . . . . ? C4 Zr2 C27 C26 -18.5(6) . . . . ? C1 Zr2 C27 C26 94.2(5) . . . . ? C2 Zr2 C27 C26 68.6(5) . . . . ? C29 Zr2 C27 C26 -76.2(5) . . . . ? C28 Zr2 C27 C26 -113.3(6) . . . . ? C25 Zr2 C27 C26 -36.2(4) . . . . ? C23 Zr2 C27 C26 -132.8(5) . . . . ? C21 Zr2 C27 C26 -169.0(5) . . . . ? C22 Zr2 C27 C26 -139.2(5) . . . . ? C24 Zr2 C27 C26 178.7(4) . . . . ? C4 Zr2 C27 C28 94.8(6) . . . . ? C1 Zr2 C27 C28 -152.4(5) . . . . ? C2 Zr2 C27 C28 -178.0(5) . . . . ? C29 Zr2 C27 C28 37.1(4) . . . . ? C26 Zr2 C27 C28 113.3(6) . . . . ? C25 Zr2 C27 C28 77.2(5) . . . . ? C23 Zr2 C27 C28 -19.5(6) . . . . ? C21 Zr2 C27 C28 -55.6(5) . . . . ? C22 Zr2 C27 C28 -25.9(5) . . . . ? C24 Zr2 C27 C28 -67.9(6) . . . . ? C26 C27 C28 C29 0.6(7) . . . . ? Zr2 C27 C28 C29 -67.1(4) . . . . ? C26 C27 C28 Zr2 67.7(4) . . . . ? C4 Zr2 C28 C27 -108.5(5) . . . . ? C1 Zr2 C28 C27 29.0(5) . . . . ? C2 Zr2 C28 C27 2.5(6) . . . . ? C29 Zr2 C28 C27 -114.4(6) . . . . ? C26 Zr2 C28 C27 -37.4(5) . . . . ? C25 Zr2 C28 C27 -77.0(5) . . . . ? C23 Zr2 C28 C27 166.1(5) . . . . ? C21 Zr2 C28 C27 122.7(5) . . . . ? C22 Zr2 C28 C27 154.6(5) . . . . ? C24 Zr2 C28 C27 140.3(5) . . . . ? C4 Zr2 C28 C29 5.8(5) . . . . ? C1 Zr2 C28 C29 143.4(4) . . . . ? C2 Zr2 C28 C29 116.9(5) . . . . ? C26 Zr2 C28 C29 77.0(5) . . . . ? C27 Zr2 C28 C29 114.4(6) . . . . ? C25 Zr2 C28 C29 37.4(4) . . . . ? C23 Zr2 C28 C29 -79.5(4) . . . . ? C21 Zr2 C28 C29 -122.9(5) . . . . ? C22 Zr2 C28 C29 -91.0(5) . . . . ? C24 Zr2 C28 C29 -105.4(4) . . . . ? C26 C25 C29 C28 0.7(6) . . . . ? Zr2 C25 C29 C28 68.0(4) . . . . ? C26 C25 C29 Zr2 -67.2(4) . . . . ? C27 C28 C29 C25 -0.8(6) . . . . ? Zr2 C28 C29 C25 -68.2(4) . . . . ? C27 C28 C29 Zr2 67.4(4) . . . . ? C4 Zr2 C29 C25 -61.8(5) . . . . ? C1 Zr2 C29 C25 63.5(6) . . . . ? C2 Zr2 C29 C25 21.1(6) . . . . ? C28 Zr2 C29 C25 113.4(6) . . . . ? C26 Zr2 C29 C25 36.5(4) . . . . ? C27 Zr2 C29 C25 76.4(5) . . . . ? C23 Zr2 C29 C25 -139.3(5) . . . . ? C21 Zr2 C29 C25 168.9(5) . . . . ? C22 Zr2 C29 C25 -163.9(5) . . . . ? C24 Zr2 C29 C25 -146.4(4) . . . . ? C4 Zr2 C29 C28 -175.2(4) . . . . ? C1 Zr2 C29 C28 -49.9(5) . . . . ? C2 Zr2 C29 C28 -92.3(5) . . . . ? C26 Zr2 C29 C28 -76.9(5) . . . . ? C27 Zr2 C29 C28 -37.0(4) . . . . ? C25 Zr2 C29 C28 -113.4(6) . . . . ? C23 Zr2 C29 C28 107.3(4) . . . . ? C21 Zr2 C29 C28 55.5(4) . . . . ? C22 Zr2 C29 C28 82.7(4) . . . . ? C24 Zr2 C29 C28 100.2(4) . . . . ? C4 C3 C31 C32 -14.2(7) . . . . ? Zr1 C3 C31 C32 78.1(5) . . . . ? C4 C3 C31 C36 162.4(4) . . . . ? Zr1 C3 C31 C36 -105.2(4) . . . . ? C36 C31 C32 C33 -0.1(6) . . . . ? C3 C31 C32 C33 176.6(4) . . . . ? C31 C32 C33 C34 -0.3(7) . . . . ? C32 C33 C34 C35 0.2(8) . . . . ? C33 C34 C35 C36 0.4(8) . . . . ? C34 C35 C36 C31 -0.8(7) . . . . ? C32 C31 C36 C35 0.6(6) . . . . ? C3 C31 C36 C35 -176.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.455 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.101 _database_code_depnum_ccdc_archive 'CCDC 938716' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_erk7052 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H62 Cl4 N2 Zr2' _chemical_formula_weight 1063.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7664(2) _cell_length_b 15.5494(3) _cell_length_c 18.6857(6) _cell_angle_alpha 96.1130(10) _cell_angle_beta 93.6850(10) _cell_angle_gamma 99.5410(10) _cell_volume 2488.84(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6368 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9359 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_measurement_device_type 'Nonius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23389 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8603 _reflns_number_gt 6393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (BrukerAXS, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Two disordered over two positions dichloromethane molecules were found in the asymmetrical unit. Several restraints (SADI, SAME, ISOR and SIMU) were used in order to improve refinement stability. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+15.2444P] 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 8603 _refine_ls_number_parameters 602 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.099 _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 0.93077(7) 0.02946(4) 0.09128(3) 0.03151(17) Uani 1 1 d . . . N1A N 1.0697(6) 0.0831(3) 0.0040(3) 0.0337(12) Uani 1 1 d . . . C1A C 1.1434(8) 0.2170(4) 0.0867(4) 0.0421(16) Uani 1 1 d . . . C2A C 1.0307(8) 0.1826(5) 0.1263(4) 0.0418(16) Uani 1 1 d . . . C3A C 0.9778(8) 0.2264(5) 0.1914(4) 0.0429(17) Uani 1 1 d . . . H3A H 1.0005 0.2055 0.2356 0.052 Uiso 1 1 calc R . . C4A C 0.9001(8) 0.2935(5) 0.1928(4) 0.0457(17) Uani 1 1 d . . . H4A H 0.8884 0.3176 0.1491 0.055 Uiso 1 1 calc R . . C5A C 1.2757(9) 0.2963(5) 0.1122(4) 0.056(2) Uani 1 1 d . . . C6A C 1.2969(11) 0.3169(7) 0.1951(5) 0.084(3) Uani 1 1 d . . . H6A1 H 1.3118 0.2643 0.2163 0.126 Uiso 1 1 calc R . . H6A2 H 1.2052 0.3369 0.2124 0.126 Uiso 1 1 calc R . . H6A3 H 1.3869 0.3625 0.2088 0.126 Uiso 1 1 calc R . . C7A C 1.2516(14) 0.3804(6) 0.0824(7) 0.104(4) Uani 1 1 d . . . H7A1 H 1.1578 0.3980 0.0993 0.157 Uiso 1 1 calc R . . H7A2 H 1.2417 0.3706 0.0300 0.157 Uiso 1 1 calc R . . H7A3 H 1.3398 0.4263 0.0986 0.157 Uiso 1 1 calc R . . C8A C 1.4319(11) 0.2716(8) 0.0935(6) 0.100(4) Uani 1 1 d . . . H8A1 H 1.5153 0.3190 0.1133 0.150 Uiso 1 1 calc R . . H8A2 H 1.4338 0.2619 0.0415 0.150 Uiso 1 1 calc R . . H8A3 H 1.4454 0.2184 0.1141 0.150 Uiso 1 1 calc R . . C9A C 1.1405(7) 0.1632(4) 0.0150(4) 0.0373(15) Uani 1 1 d . . . C10A C 1.2102(9) 0.2083(5) -0.0468(4) 0.0507(19) Uani 1 1 d . . . H10A H 1.1735 0.1724 -0.0923 0.076 Uiso 1 1 calc R . . H10B H 1.3225 0.2158 -0.0403 0.076 Uiso 1 1 calc R . . H10C H 1.1789 0.2652 -0.0471 0.076 Uiso 1 1 calc R . . C11A C 0.9951(8) 0.0174(5) 0.2251(4) 0.0445(17) Uani 1 1 d . . . H11A H 0.9345 0.0419 0.2588 0.053 Uiso 1 1 calc R . . C12A C 1.1324(8) 0.0595(5) 0.2012(3) 0.0427(17) Uani 1 1 d . . . H12A H 1.1797 0.1180 0.2166 0.051 Uiso 1 1 calc R . . C13A C 1.1891(8) 0.0020(5) 0.1512(3) 0.0428(17) Uani 1 1 d . . . H13A H 1.2791 0.0144 0.1267 0.051 Uiso 1 1 calc R . . C14A C 1.0846(9) -0.0783(5) 0.1446(4) 0.0453(17) Uani 1 1 d . . . H14A H 1.0941 -0.1296 0.1150 0.054 Uiso 1 1 calc R . . C15A C 0.9642(8) -0.0693(5) 0.1893(4) 0.0448(17) Uani 1 1 d . . . H15A H 0.8788 -0.1128 0.1945 0.054 Uiso 1 1 calc R . . C16A C 0.6848(7) 0.0687(5) 0.1415(4) 0.0444(17) Uani 1 1 d . . . H16A H 0.6893 0.0895 0.1909 0.053 Uiso 1 1 calc R . . C17A C 0.6473(8) -0.0190(5) 0.1111(4) 0.0500(19) Uani 1 1 d . . . H17A H 0.6222 -0.0678 0.1365 0.060 Uiso 1 1 calc R . . C18A C 0.6533(7) -0.0220(5) 0.0369(4) 0.0412(17) Uani 1 1 d . . . H18A H 0.6321 -0.0728 0.0033 0.049 Uiso 1 1 calc R . . C19A C 0.6970(7) 0.0649(5) 0.0209(4) 0.0392(16) Uani 1 1 d . . . H19A H 0.7117 0.0823 -0.0252 0.047 Uiso 1 1 calc R . . C20A C 0.7143(7) 0.1195(5) 0.0853(4) 0.0428(17) Uani 1 1 d . . . H20A H 0.7416 0.1811 0.0903 0.051 Uiso 1 1 calc R . . C21A C 0.8311(8) 0.3338(5) 0.2541(4) 0.0459(17) Uani 1 1 d . . . C22A C 0.8330(10) 0.3036(5) 0.3218(4) 0.057(2) Uani 1 1 d . . . H22A H 0.8761 0.2533 0.3287 0.068 Uiso 1 1 calc R . . C23A C 0.7723(11) 0.3467(6) 0.3787(5) 0.068(2) Uani 1 1 d . . . H23A H 0.7770 0.3262 0.4242 0.082 Uiso 1 1 calc R . . C24A C 0.7052(10) 0.4188(6) 0.3701(5) 0.065(2) Uani 1 1 d . . . H24A H 0.6630 0.4472 0.4090 0.078 Uiso 1 1 calc R . . C25A C 0.7005(9) 0.4492(5) 0.3030(5) 0.059(2) Uani 1 1 d . . . H25A H 0.6543 0.4984 0.2961 0.071 Uiso 1 1 calc R . . C26A C 0.7635(9) 0.4071(5) 0.2465(4) 0.0509(18) Uani 1 1 d . . . H26A H 0.7606 0.4287 0.2015 0.061 Uiso 1 1 calc R . . Zr2 Zr 0.47224(7) 0.92972(4) 0.41079(3) 0.03378(18) Uani 1 1 d . . . N1B N 0.5888(6) 0.9456(3) 0.5233(3) 0.0353(12) Uani 1 1 d . . . C1B C 0.6703(8) 0.8062(4) 0.4903(4) 0.0383(15) Uani 1 1 d . . . C2B C 0.6189(7) 0.8136(4) 0.4215(4) 0.0397(16) Uani 1 1 d . . . C3B C 0.6335(9) 0.7548(4) 0.3572(4) 0.0431(17) Uani 1 1 d . . . H3B H 0.5415 0.7198 0.3349 0.052 Uiso 1 1 calc R . . C4B C 0.7652(3) 0.74548(18) 0.32631(15) 0.0474(18) Uani 1 1 d . . . H4B H 0.8586 0.7760 0.3509 0.057 Uiso 1 1 calc R . . C5B C 0.7145(3) 0.72185(18) 0.51863(15) 0.0433(16) Uani 1 1 d R . . C6B C 0.6644(3) 0.71142(18) 0.59539(15) 0.077(3) Uani 1 1 d R . . H6B1 H 0.6847 0.6557 0.6091 0.116 Uiso 1 1 calc R . . H6B2 H 0.5543 0.7130 0.5961 0.116 Uiso 1 1 calc R . . H6B3 H 0.7226 0.7590 0.6292 0.116 Uiso 1 1 calc R . . C7B C 0.6246(3) 0.63944(18) 0.47165(15) 0.086(3) Uani 1 1 d R . . H7B1 H 0.6357 0.6458 0.4211 0.129 Uiso 1 1 calc R . . H7B2 H 0.5156 0.6324 0.4804 0.129 Uiso 1 1 calc R . . H7B3 H 0.6658 0.5882 0.4838 0.129 Uiso 1 1 calc R . . C8B C 0.8880(3) 0.72073(18) 0.51801(15) 0.080(3) Uani 1 1 d R . . H8B1 H 0.9077 0.6624 0.5247 0.120 Uiso 1 1 calc R . . H8B2 H 0.9439 0.7628 0.5568 0.120 Uiso 1 1 calc R . . H8B3 H 0.9229 0.7362 0.4721 0.120 Uiso 1 1 calc R . . C9B C 0.6718(3) 0.88871(18) 0.54034(15) 0.0378(15) Uani 1 1 d R . . C10B C 0.7831(3) 0.90583(18) 0.60656(15) 0.062(2) Uani 1 1 d R . . H10D H 0.8355 0.9665 0.6121 0.093 Uiso 1 1 calc R . . H10E H 0.8592 0.8673 0.6019 0.093 Uiso 1 1 calc R . . H10F H 0.7268 0.8948 0.6486 0.093 Uiso 1 1 calc R . . C11B C 0.5717(3) 1.06417(18) 0.34568(15) 0.060(2) Uani 1 1 d R . . H11B H 0.5377 1.1175 0.3586 0.072 Uiso 1 1 calc R . . C12B C 0.5006(11) 0.9961(6) 0.2925(4) 0.063(2) Uani 1 1 d . . . H12B H 0.4099 0.9966 0.2629 0.075 Uiso 1 1 calc R . . C13B C 0.5856(10) 0.9278(5) 0.2905(4) 0.055(2) Uani 1 1 d . . . H13B H 0.5606 0.8740 0.2606 0.067 Uiso 1 1 calc R . . C14B C 0.7130(9) 0.9529(5) 0.3403(4) 0.0511(19) Uani 1 1 d . . . H14B H 0.7918 0.9202 0.3491 0.061 Uiso 1 1 calc R . . C15B C 0.7038(9) 1.0366(5) 0.3756(4) 0.052(2) Uani 1 1 d . . . H15B H 0.7743 1.0685 0.4129 0.062 Uiso 1 1 calc R . . C16B C 0.2735(9) 0.8089(5) 0.3375(4) 0.0531(19) Uani 1 1 d . . . H16B H 0.2991 0.7878 0.2915 0.064 Uiso 1 1 calc R . . C17B C 0.3049(8) 0.7751(5) 0.4022(4) 0.0480(18) Uani 1 1 d . . . H17B H 0.3523 0.7258 0.4070 0.058 Uiso 1 1 calc R . . C18B C 0.2545(8) 0.8264(5) 0.4580(4) 0.0504(19) Uani 1 1 d . . . H18B H 0.2663 0.8197 0.5074 0.060 Uiso 1 1 calc R . . C19B C 0.1824(8) 0.8904(5) 0.4280(4) 0.0514(19) Uani 1 1 d . . . H19B H 0.1337 0.9323 0.4533 0.062 Uiso 1 1 calc R . . C20B C 0.1968(9) 0.8799(6) 0.3537(4) 0.058(2) Uani 1 1 d . . . H20B H 0.1612 0.9147 0.3202 0.069 Uiso 1 1 calc R . . C21B C 0.7767(10) 0.6926(5) 0.2585(4) 0.0502(19) Uani 1 1 d . . . C22B C 0.6510(11) 0.6579(6) 0.2097(4) 0.065(2) Uani 1 1 d . . . H22B H 0.5523 0.6702 0.2192 0.078 Uiso 1 1 calc R . . C23B C 0.6677(15) 0.6047(7) 0.1462(5) 0.084(3) Uani 1 1 d . . . H23B H 0.5812 0.5816 0.1133 0.100 Uiso 1 1 calc R . . C24B C 0.8118(17) 0.5867(6) 0.1327(5) 0.083(3) Uani 1 1 d . . . H24B H 0.8240 0.5503 0.0907 0.100 Uiso 1 1 calc R . . C25B C 0.9350(14) 0.6207(7) 0.1790(6) 0.080(3) Uani 1 1 d . . . H25B H 1.0332 0.6080 0.1692 0.096 Uiso 1 1 calc R . . C26B C 0.9198(11) 0.6740(6) 0.2411(5) 0.071(3) Uani 1 1 d . . . H26B H 1.0085 0.6983 0.2722 0.085 Uiso 1 1 calc R . . C30 C 0.694(8) 0.343(3) -0.070(4) 0.18(4) Uani 0.189(18) 1 d PDU A 1 H30A H 0.7212 0.3814 -0.1073 0.210 Uiso 0.189(18) 1 calc PR A 1 H30B H 0.6029 0.3610 -0.0481 0.210 Uiso 0.189(18) 1 calc PR A 1 Cl1 Cl 0.647(3) 0.2367(17) -0.1083(14) 0.059(5) Uani 0.189(18) 1 d PDU A 1 Cl2 Cl 0.845(4) 0.358(3) -0.0051(15) 0.155(12) Uani 0.189(18) 1 d PDU A 1 C30A C 0.805(2) 0.2954(8) -0.0412(8) 0.112(6) Uani 0.811(18) 1 d PDU A 2 H30C H 0.7928 0.2639 0.0013 0.134 Uiso 0.811(18) 1 calc PR A 2 H30D H 0.9055 0.2889 -0.0591 0.134 Uiso 0.811(18) 1 calc PR A 2 Cl1A Cl 0.6598(12) 0.2492(6) -0.1069(6) 0.137(4) Uani 0.811(18) 1 d PDU A 2 Cl2A Cl 0.8024(9) 0.4034(5) -0.0170(4) 0.167(3) Uani 0.811(18) 1 d PDU A 2 C31 C 0.122(2) 0.5191(14) 0.3389(8) 0.110(6) Uani 0.82(2) 1 d PDU B 1 H31A H 0.0458 0.5530 0.3216 0.132 Uiso 0.82(2) 1 calc PR B 1 H31B H 0.0812 0.4566 0.3246 0.132 Uiso 0.82(2) 1 calc PR B 1 Cl3 Cl 0.1504(10) 0.5387(4) 0.4319(3) 0.108(2) Uani 0.82(2) 1 d PDU B 1 Cl4 Cl 0.2936(10) 0.5475(6) 0.2991(6) 0.119(3) Uani 0.82(2) 1 d PDU B 1 C31A C 0.154(13) 0.495(3) 0.339(4) 0.107(12) Uani 0.18(2) 1 d PDU B 2 H31C H 0.0631 0.4545 0.3144 0.128 Uiso 0.18(2) 1 calc PR B 2 H31D H 0.2255 0.4593 0.3584 0.128 Uiso 0.18(2) 1 calc PR B 2 Cl3A Cl 0.095(4) 0.559(2) 0.409(2) 0.122(10) Uani 0.18(2) 1 d PDU B 2 Cl4A Cl 0.244(4) 0.556(2) 0.2766(18) 0.099(9) Uani 0.18(2) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0252(3) 0.0421(4) 0.0278(3) 0.0073(3) 0.0002(2) 0.0062(3) N1A 0.028(3) 0.044(3) 0.030(3) 0.007(2) 0.002(2) 0.007(2) C1A 0.046(4) 0.040(4) 0.040(4) 0.006(3) 0.000(3) 0.007(3) C2A 0.036(4) 0.048(4) 0.039(4) 0.002(3) -0.008(3) 0.007(3) C3A 0.045(4) 0.045(4) 0.034(4) -0.006(3) -0.002(3) 0.003(3) C4A 0.048(4) 0.044(4) 0.046(4) 0.006(3) 0.000(3) 0.011(3) C5A 0.052(5) 0.053(5) 0.057(5) -0.007(4) 0.006(4) -0.005(4) C6A 0.061(6) 0.104(8) 0.063(6) -0.024(5) -0.003(5) -0.030(5) C7A 0.117(10) 0.053(6) 0.131(10) 0.015(6) -0.025(8) -0.012(6) C8A 0.049(6) 0.119(9) 0.107(8) -0.049(7) 0.010(5) -0.018(6) C9A 0.029(3) 0.042(4) 0.041(4) 0.009(3) 0.007(3) 0.004(3) C10A 0.052(5) 0.051(4) 0.044(4) 0.007(3) 0.003(3) -0.008(4) C11A 0.036(4) 0.064(5) 0.035(4) 0.016(3) -0.002(3) 0.012(3) C12A 0.038(4) 0.060(5) 0.030(4) 0.008(3) -0.012(3) 0.010(3) C13A 0.029(3) 0.071(5) 0.031(4) 0.009(3) -0.008(3) 0.018(3) C14A 0.051(4) 0.054(5) 0.035(4) 0.012(3) -0.005(3) 0.022(4) C15A 0.043(4) 0.056(5) 0.037(4) 0.015(3) 0.000(3) 0.009(3) C16A 0.024(3) 0.071(5) 0.040(4) 0.007(4) 0.002(3) 0.012(3) C17A 0.033(4) 0.063(5) 0.057(5) 0.016(4) 0.015(3) 0.007(4) C18A 0.015(3) 0.062(5) 0.042(4) -0.003(3) -0.008(3) 0.005(3) C19A 0.019(3) 0.057(4) 0.044(4) 0.010(3) 0.000(3) 0.012(3) C20A 0.026(3) 0.055(4) 0.051(4) 0.003(3) 0.001(3) 0.017(3) C21A 0.046(4) 0.037(4) 0.052(4) -0.002(3) 0.008(3) 0.003(3) C22A 0.069(6) 0.051(5) 0.053(5) 0.005(4) 0.012(4) 0.018(4) C23A 0.081(6) 0.065(6) 0.063(6) 0.003(4) 0.028(5) 0.022(5) C24A 0.055(5) 0.054(5) 0.084(7) -0.013(5) 0.025(5) 0.012(4) C25A 0.046(5) 0.041(4) 0.090(7) 0.000(4) 0.003(4) 0.013(4) C26A 0.046(4) 0.048(5) 0.057(5) 0.007(4) -0.001(4) 0.008(4) Zr2 0.0326(4) 0.0391(4) 0.0280(3) 0.0051(3) -0.0005(3) 0.0019(3) N1B 0.034(3) 0.039(3) 0.031(3) 0.007(2) -0.001(2) -0.001(2) C1B 0.035(4) 0.042(4) 0.040(4) 0.011(3) 0.003(3) 0.008(3) C2B 0.027(3) 0.042(4) 0.048(4) 0.010(3) -0.002(3) -0.001(3) C3B 0.049(4) 0.036(4) 0.040(4) 0.002(3) 0.000(3) 0.000(3) C4B 0.046(4) 0.041(4) 0.052(4) 0.000(3) 0.006(4) 0.000(3) C5B 0.037(4) 0.048(4) 0.046(4) 0.011(3) 0.006(3) 0.006(3) C6B 0.099(8) 0.059(6) 0.084(7) 0.032(5) 0.036(6) 0.018(5) C7B 0.122(9) 0.045(5) 0.087(7) 0.019(5) -0.018(6) 0.009(5) C8B 0.052(5) 0.077(7) 0.122(9) 0.036(6) 0.018(5) 0.024(5) C9B 0.037(4) 0.042(4) 0.035(4) 0.011(3) 0.002(3) 0.005(3) C10B 0.075(6) 0.059(5) 0.051(5) 0.000(4) -0.029(4) 0.026(4) C11B 0.076(6) 0.056(5) 0.057(5) 0.028(4) 0.030(5) 0.018(4) C12B 0.074(6) 0.080(6) 0.039(4) 0.024(4) 0.002(4) 0.020(5) C13B 0.074(6) 0.057(5) 0.039(4) 0.010(4) 0.015(4) 0.017(4) C14B 0.057(5) 0.054(5) 0.045(4) 0.015(4) 0.021(4) 0.007(4) C15B 0.056(5) 0.054(5) 0.043(4) 0.007(3) 0.020(4) -0.006(4) C16B 0.046(4) 0.057(5) 0.050(5) -0.007(4) -0.003(4) 0.001(4) C17B 0.035(4) 0.040(4) 0.064(5) 0.005(4) -0.005(4) -0.003(3) C18B 0.039(4) 0.054(5) 0.053(5) 0.004(4) 0.008(4) -0.007(4) C19B 0.026(4) 0.054(5) 0.069(5) -0.003(4) -0.001(3) -0.001(3) C20B 0.047(5) 0.066(5) 0.053(5) 0.003(4) -0.016(4) -0.003(4) C21B 0.066(5) 0.043(4) 0.041(4) 0.002(3) 0.013(4) 0.005(4) C22B 0.081(6) 0.065(6) 0.047(5) 0.004(4) 0.008(4) 0.006(5) C23B 0.127(10) 0.076(7) 0.041(5) 0.000(4) 0.005(6) 0.004(6) C24B 0.140(11) 0.060(6) 0.056(6) 0.007(5) 0.028(7) 0.028(7) C25B 0.097(8) 0.073(7) 0.077(7) 0.005(5) 0.030(6) 0.032(6) C26B 0.074(6) 0.064(6) 0.078(6) 0.004(5) 0.031(5) 0.012(5) C30 0.17(4) 0.18(4) 0.18(4) 0.020(11) 0.014(11) 0.033(13) Cl1 0.040(7) 0.052(8) 0.090(9) 0.017(6) 0.000(6) 0.017(6) Cl2 0.163(14) 0.165(15) 0.137(13) 0.023(9) 0.008(9) 0.023(9) C30A 0.130(10) 0.089(9) 0.118(9) 0.024(7) 0.006(8) 0.018(7) Cl1A 0.122(6) 0.113(6) 0.172(6) 0.003(4) -0.004(4) 0.023(4) Cl2A 0.208(6) 0.099(4) 0.186(6) -0.040(4) 0.044(5) 0.029(4) C31 0.091(9) 0.118(9) 0.112(8) 0.015(7) -0.003(7) 0.000(7) Cl3 0.125(4) 0.088(3) 0.104(3) 0.024(2) -0.012(3) -0.006(2) Cl4 0.095(4) 0.105(4) 0.141(5) -0.037(4) 0.022(4) 0.000(3) C31A 0.102(14) 0.106(14) 0.110(14) 0.011(9) 0.005(9) 0.012(9) Cl3A 0.116(12) 0.118(12) 0.127(13) 0.014(8) 0.009(9) 0.011(8) Cl4A 0.107(12) 0.088(10) 0.100(11) 0.003(8) 0.004(8) 0.017(8) _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 N1A 2.247(5) . ? Zr1 N1A 2.359(5) 2_755 ? Zr1 C2A 2.402(7) . ? Zr1 C19A 2.532(6) . ? Zr1 C17A 2.537(7) . ? Zr1 C18A 2.540(6) . ? Zr1 C20A 2.542(6) . ? Zr1 C15A 2.545(7) . ? Zr1 C16A 2.545(6) . ? Zr1 C14A 2.559(7) . ? Zr1 C11A 2.562(6) . ? Zr1 C12A 2.573(6) . ? N1A C9A 1.286(8) . ? N1A Zr1 2.359(5) 2_755 ? C1A C2A 1.347(9) . ? C1A C9A 1.498(9) . ? C1A C5A 1.557(10) . ? C2A C3A 1.468(9) . ? C3A C4A 1.337(10) . ? C3A H3A 0.9400 . ? C4A C21A 1.461(10) . ? C4A H4A 0.9400 . ? C5A C7A 1.515(12) . ? C5A C8A 1.533(12) . ? C5A C6A 1.541(11) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C6A H6A3 0.9700 . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C7A H7A3 0.9700 . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C8A H8A3 0.9700 . ? C9A C10A 1.522(9) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C10A H10C 0.9700 . ? C11A C12A 1.396(9) . ? C11A C15A 1.414(10) . ? C11A H11A 0.9400 . ? C12A C13A 1.396(10) . ? C12A H12A 0.9400 . ? C13A C14A 1.410(10) . ? C13A H13A 0.9400 . ? C14A C15A 1.403(10) . ? C14A H14A 0.9400 . ? C15A H15A 0.9400 . ? C16A C20A 1.394(10) . ? C16A C17A 1.398(10) . ? C16A H16A 0.9400 . ? C17A C18A 1.386(9) . ? C17A H17A 0.9400 . ? C18A C19A 1.410(10) . ? C18A H18A 0.9400 . ? C19A C20A 1.382(9) . ? C19A H19A 0.9400 . ? C20A H20A 0.9400 . ? C21A C26A 1.384(10) . ? C21A C22A 1.396(10) . ? C22A C23A 1.379(10) . ? C22A H22A 0.9400 . ? C23A C24A 1.368(12) . ? C23A H23A 0.9400 . ? C24A C25A 1.386(12) . ? C24A H24A 0.9400 . ? C25A C26A 1.377(11) . ? C25A H25A 0.9400 . ? C26A H26A 0.9400 . ? Zr2 N1B 2.248(5) . ? Zr2 N1B 2.342(5) 2_676 ? Zr2 C2B 2.401(7) . ? Zr2 C13B 2.514(7) . ? Zr2 C20B 2.538(8) . ? Zr2 C12B 2.547(7) . ? Zr2 C16B 2.550(7) . ? Zr2 C18B 2.551(7) . ? Zr2 C14B 2.555(7) . ? Zr2 C19B 2.562(7) . ? Zr2 C15B 2.569(7) . ? Zr2 C17B 2.584(7) . ? N1B C9B 1.287(6) . ? N1B Zr2 2.342(5) 2_676 ? C1B C2B 1.358(9) . ? C1B C9B 1.503(7) . ? C1B C5B 1.562(7) . ? C2B C3B 1.456(9) . ? C3B C4B 1.345(8) . ? C3B H3B 0.9400 . ? C4B C21B 1.454(8) . ? C4B H4B 0.9400 . ? C5B C8B 1.5253 . ? C5B C7B 1.5395 . ? C5B C6B 1.5439 . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C6B H6B3 0.9700 . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C7B H7B3 0.9700 . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C8B H8B3 0.9700 . ? C9B C10B 1.4977 . ? C10B H10D 0.9700 . ? C10B H10E 0.9700 . ? C10B H10F 0.9700 . ? C11B C15B 1.403(9) . ? C11B C12B 1.405(9) . ? C11B H11B 0.9400 . ? C12B C13B 1.394(11) . ? C12B H12B 0.9400 . ? C13B C14B 1.382(11) . ? C13B H13B 0.9400 . ? C14B C15B 1.412(10) . ? C14B H14B 0.9400 . ? C15B H15B 0.9400 . ? C16B C17B 1.397(10) . ? C16B C20B 1.402(11) . ? C16B H16B 0.9400 . ? C17B C18B 1.386(10) . ? C17B H17B 0.9400 . ? C18B C19B 1.409(11) . ? C18B H18B 0.9400 . ? C19B C20B 1.397(11) . ? C19B H19B 0.9400 . ? C20B H20B 0.9400 . ? C21B C22B 1.380(11) . ? C21B C26B 1.384(11) . ? C22B C23B 1.403(12) . ? C22B H22B 0.9400 . ? C23B C24B 1.371(15) . ? C23B H23B 0.9400 . ? C24B C25B 1.337(14) . ? C24B H24B 0.9400 . ? C25B C26B 1.379(12) . ? C25B H25B 0.9400 . ? C26B H26B 0.9400 . ? C30 Cl2 1.708(19) . ? C30 Cl1 1.709(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30A Cl2A 1.697(13) . ? C30A Cl1A 1.716(13) . ? C30A H30C 0.9800 . ? C30A H30D 0.9800 . ? C31 Cl3 1.726(14) . ? C31 Cl4 1.731(13) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31A Cl3A 1.73(2) . ? C31A Cl4A 1.73(2) . ? C31A H31C 0.9800 . ? C31A H31D 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 N1A Zr1 N1A 70.3(2) . 2_755 ? N1A Zr1 C2A 70.8(2) . . ? N1A Zr1 C2A 141.1(2) 2_755 . ? N1A Zr1 C19A 86.2(2) . . ? N1A Zr1 C19A 86.0(2) 2_755 . ? C2A Zr1 C19A 91.5(2) . . ? N1A Zr1 C17A 137.7(2) . . ? N1A Zr1 C17A 93.9(2) 2_755 . ? C2A Zr1 C17A 115.2(2) . . ? C19A Zr1 C17A 52.9(2) . . ? N1A Zr1 C18A 107.3(2) . . ? N1A Zr1 C18A 71.6(2) 2_755 . ? C2A Zr1 C18A 121.1(2) . . ? C19A Zr1 C18A 32.3(2) . . ? C17A Zr1 C18A 31.7(2) . . ? N1A Zr1 C20A 99.3(2) . . ? N1A Zr1 C20A 117.5(2) 2_755 . ? C2A Zr1 C20A 69.3(2) . . ? C19A Zr1 C20A 31.6(2) . . ? C17A Zr1 C20A 52.6(2) . . ? C18A Zr1 C20A 52.6(2) . . ? N1A Zr1 C15A 137.0(2) . . ? N1A Zr1 C15A 93.9(2) 2_755 . ? C2A Zr1 C15A 114.8(2) . . ? C19A Zr1 C15A 133.8(2) . . ? C17A Zr1 C15A 81.1(2) . . ? C18A Zr1 C15A 104.6(2) . . ? C20A Zr1 C15A 123.1(2) . . ? N1A Zr1 C16A 131.0(2) . . ? N1A Zr1 C16A 123.5(2) 2_755 . ? C2A Zr1 C16A 83.4(2) . . ? C19A Zr1 C16A 52.8(2) . . ? C17A Zr1 C16A 31.9(2) . . ? C18A Zr1 C16A 52.7(2) . . ? C20A Zr1 C16A 31.8(2) . . ? C15A Zr1 C16A 91.4(2) . . ? N1A Zr1 C14A 105.6(2) . . ? N1A Zr1 C14A 75.0(2) 2_755 . ? C2A Zr1 C14A 116.0(2) . . ? C19A Zr1 C14A 152.2(2) . . ? C17A Zr1 C14A 107.7(2) . . ? C18A Zr1 C14A 120.5(2) . . ? C20A Zr1 C14A 155.0(2) . . ? C15A Zr1 C14A 31.9(2) . . ? C16A Zr1 C14A 123.2(2) . . ? N1A Zr1 C11A 133.8(2) . . ? N1A Zr1 C11A 125.0(2) 2_755 . ? C2A Zr1 C11A 83.4(2) . . ? C19A Zr1 C11A 133.4(2) . . ? C17A Zr1 C11A 87.8(2) . . ? C18A Zr1 C11A 118.9(2) . . ? C20A Zr1 C11A 106.7(2) . . ? C15A Zr1 C11A 32.2(2) . . ? C16A Zr1 C11A 80.6(2) . . ? C14A Zr1 C11A 52.6(2) . . ? N1A Zr1 C12A 102.2(2) . . ? N1A Zr1 C12A 122.9(2) 2_755 . ? C2A Zr1 C12A 66.2(2) . . ? C19A Zr1 C12A 151.1(2) . . ? C17A Zr1 C12A 118.8(2) . . ? C18A Zr1 C12A 150.3(2) . . ? C20A Zr1 C12A 119.6(2) . . ? C15A Zr1 C12A 52.5(2) . . ? C16A Zr1 C12A 104.2(2) . . ? C14A Zr1 C12A 51.9(2) . . ? C11A Zr1 C12A 31.5(2) . . ? C9A N1A Zr1 118.3(4) . . ? C9A N1A Zr1 131.8(4) . 2_755 ? Zr1 N1A Zr1 109.7(2) . 2_755 ? C2A C1A C9A 112.0(6) . . ? C2A C1A C5A 126.3(6) . . ? C9A C1A C5A 121.4(6) . . ? C1A C2A C3A 126.7(6) . . ? C1A C2A Zr1 114.4(5) . . ? C3A C2A Zr1 118.6(5) . . ? C4A C3A C2A 125.2(7) . . ? C4A C3A H3A 117.4 . . ? C2A C3A H3A 117.4 . . ? C3A C4A C21A 127.7(7) . . ? C3A C4A H4A 116.2 . . ? C21A C4A H4A 116.2 . . ? C7A C5A C8A 111.1(9) . . ? C7A C5A C6A 107.0(8) . . ? C8A C5A C6A 102.9(8) . . ? C7A C5A C1A 113.7(7) . . ? C8A C5A C1A 109.3(7) . . ? C6A C5A C1A 112.3(6) . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C5A C7A H7A1 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C5A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5A C8A H8A1 109.5 . . ? C5A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C5A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? N1A C9A C1A 121.0(6) . . ? N1A C9A C10A 120.5(6) . . ? C1A C9A C10A 118.3(6) . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C12A C11A C15A 107.3(7) . . ? C12A C11A Zr1 74.7(4) . . ? C15A C11A Zr1 73.2(4) . . ? C12A C11A H11A 126.4 . . ? C15A C11A H11A 126.4 . . ? Zr1 C11A H11A 117.8 . . ? C11A C12A C13A 109.9(7) . . ? C11A C12A Zr1 73.8(4) . . ? C13A C12A Zr1 74.6(4) . . ? C11A C12A H12A 125.1 . . ? C13A C12A H12A 125.1 . . ? Zr1 C12A H12A 118.3 . . ? C12A C13A C14A 106.5(6) . . ? C12A C13A Zr1 74.0(4) . . ? C14A C13A Zr1 73.3(4) . . ? C12A C13A H13A 126.8 . . ? C14A C13A H13A 126.8 . . ? Zr1 C13A H13A 118.1 . . ? C15A C14A C13A 109.0(7) . . ? C15A C14A Zr1 73.5(4) . . ? C13A C14A Zr1 74.9(4) . . ? C15A C14A H14A 125.5 . . ? C13A C14A H14A 125.5 . . ? Zr1 C14A H14A 118.0 . . ? C14A C15A C11A 107.4(7) . . ? C14A C15A Zr1 74.6(4) . . ? C11A C15A Zr1 74.6(4) . . ? C14A C15A H15A 126.3 . . ? C11A C15A H15A 126.3 . . ? Zr1 C15A H15A 116.6 . . ? C20A C16A C17A 107.3(7) . . ? C20A C16A Zr1 74.0(4) . . ? C17A C16A Zr1 73.7(4) . . ? C20A C16A H16A 126.3 . . ? C17A C16A H16A 126.3 . . ? Zr1 C16A H16A 118.0 . . ? C18A C17A C16A 108.4(7) . . ? C18A C17A Zr1 74.3(4) . . ? C16A C17A Zr1 74.3(4) . . ? C18A C17A H17A 125.8 . . ? C16A C17A H17A 125.8 . . ? Zr1 C17A H17A 117.6 . . ? C17A C18A C19A 107.8(6) . . ? C17A C18A Zr1 74.1(4) . . ? C19A C18A Zr1 73.6(3) . . ? C17A C18A H18A 126.1 . . ? C19A C18A H18A 126.1 . . ? Zr1 C18A H18A 118.2 . . ? C20A C19A C18A 107.5(6) . . ? C20A C19A Zr1 74.6(4) . . ? C18A C19A Zr1 74.1(4) . . ? C20A C19A H19A 126.3 . . ? C18A C19A H19A 126.3 . . ? Zr1 C19A H19A 117.1 . . ? C19A C20A C16A 108.9(7) . . ? C19A C20A Zr1 73.8(4) . . ? C16A C20A Zr1 74.2(4) . . ? C19A C20A H20A 125.5 . . ? C16A C20A H20A 125.5 . . ? Zr1 C20A H20A 118.3 . . ? C26A C21A C22A 117.3(7) . . ? C26A C21A C4A 119.4(7) . . ? C22A C21A C4A 123.2(7) . . ? C23A C22A C21A 120.7(8) . . ? C23A C22A H22A 119.7 . . ? C21A C22A H22A 119.7 . . ? C24A C23A C22A 121.1(9) . . ? C24A C23A H23A 119.4 . . ? C22A C23A H23A 119.4 . . ? C23A C24A C25A 119.1(8) . . ? C23A C24A H24A 120.5 . . ? C25A C24A H24A 120.5 . . ? C26A C25A C24A 119.8(8) . . ? C26A C25A H25A 120.1 . . ? C24A C25A H25A 120.1 . . ? C25A C26A C21A 122.0(8) . . ? C25A C26A H26A 119.0 . . ? C21A C26A H26A 119.0 . . ? N1B Zr2 N1B 70.7(2) . 2_676 ? N1B Zr2 C2B 71.0(2) . . ? N1B Zr2 C2B 141.7(2) 2_676 . ? N1B Zr2 C13B 130.5(2) . . ? N1B Zr2 C13B 124.9(2) 2_676 . ? C2B Zr2 C13B 81.2(2) . . ? N1B Zr2 C20B 135.6(2) . . ? N1B Zr2 C20B 93.3(2) 2_676 . ? C2B Zr2 C20B 114.7(3) . . ? C13B Zr2 C20B 93.0(3) . . ? N1B Zr2 C12B 140.0(3) . . ? N1B Zr2 C12B 95.9(2) 2_676 . ? C2B Zr2 C12B 113.1(3) . . ? C13B Zr2 C12B 32.0(3) . . ? C20B Zr2 C12B 81.0(3) . . ? N1B Zr2 C16B 133.6(2) . . ? N1B Zr2 C16B 124.5(2) 2_676 . ? C2B Zr2 C16B 83.7(2) . . ? C13B Zr2 C16B 80.2(3) . . ? C20B Zr2 C16B 32.0(3) . . ? C12B Zr2 C16B 85.5(3) . . ? N1B Zr2 C18B 86.0(2) . . ? N1B Zr2 C18B 93.1(2) 2_676 . ? C2B Zr2 C18B 84.9(2) . . ? C13B Zr2 C18B 132.0(3) . . ? C20B Zr2 C18B 52.7(3) . . ? C12B Zr2 C18B 133.3(3) . . ? C16B Zr2 C18B 52.6(3) . . ? N1B Zr2 C14B 99.2(2) . . ? N1B Zr2 C14B 116.7(2) 2_676 . ? C2B Zr2 C14B 69.2(2) . . ? C13B Zr2 C14B 31.6(2) . . ? C20B Zr2 C14B 124.6(3) . . ? C12B Zr2 C14B 52.2(3) . . ? C16B Zr2 C14B 107.5(3) . . ? C18B Zr2 C14B 149.9(3) . . ? N1B Zr2 C19B 104.2(2) . . ? N1B Zr2 C19B 75.0(2) 2_676 . ? C2B Zr2 C19B 115.5(2) . . ? C13B Zr2 C19B 124.8(3) . . ? C20B Zr2 C19B 31.8(2) . . ? C12B Zr2 C19B 108.4(3) . . ? C16B Zr2 C19B 52.8(3) . . ? C18B Zr2 C19B 32.0(2) . . ? C14B Zr2 C19B 156.4(3) . . ? N1B Zr2 C15B 88.5(2) . . ? N1B Zr2 C15B 84.7(2) 2_676 . ? C2B Zr2 C15B 93.7(2) . . ? C13B Zr2 C15B 52.7(3) . . ? C20B Zr2 C15B 132.3(3) . . ? C12B Zr2 C15B 52.1(3) . . ? C16B Zr2 C15B 132.5(2) . . ? C18B Zr2 C15B 174.5(3) . . ? C14B Zr2 C15B 32.0(2) . . ? C19B Zr2 C15B 150.5(3) . . ? N1B Zr2 C17B 102.0(2) . . ? N1B Zr2 C17B 123.7(2) 2_676 . ? C2B Zr2 C17B 65.8(2) . . ? C13B Zr2 C17B 102.5(3) . . ? C20B Zr2 C17B 52.3(3) . . ? C12B Zr2 C17B 116.1(3) . . ? C16B Zr2 C17B 31.6(2) . . ? C18B Zr2 C17B 31.3(2) . . ? C14B Zr2 C17B 119.6(2) . . ? C19B Zr2 C17B 52.2(2) . . ? C15B Zr2 C17B 151.5(2) . . ? C9B N1B Zr2 118.6(3) . . ? C9B N1B Zr2 132.1(3) . 2_676 ? Zr2 N1B Zr2 109.3(2) . 2_676 ? C2B C1B C9B 112.2(5) . . ? C2B C1B C5B 126.2(6) . . ? C9B C1B C5B 121.5(5) . . ? C1B C2B C3B 126.5(6) . . ? C1B C2B Zr2 114.3(5) . . ? C3B C2B Zr2 119.0(5) . . ? C4B C3B C2B 126.7(6) . . ? C4B C3B H3B 116.6 . . ? C2B C3B H3B 116.6 . . ? C3B C4B C21B 126.2(5) . . ? C3B C4B H4B 116.9 . . ? C21B C4B H4B 116.9 . . ? C8B C5B C7B 109.0 . . ? C8B C5B C6B 109.4 . . ? C7B C5B C6B 104.4 . . ? C8B C5B C1B 111.8(3) . . ? C7B C5B C1B 109.9(3) . . ? C6B C5B C1B 112.1(3) . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C5B C7B H7B1 109.5 . . ? C5B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C5B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C5B C8B H8B1 109.5 . . ? C5B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C5B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? N1B C9B C10B 121.6(3) . . ? N1B C9B C1B 120.4(4) . . ? C10B C9B C1B 117.8(3) . . ? C9B C10B H10D 109.5 . . ? C9B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C9B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C15B C11B C12B 106.2(5) . . ? C15B C11B Zr2 73.6(3) . . ? C12B C11B Zr2 72.6(3) . . ? C15B C11B H11B 126.9 . . ? C12B C11B H11B 126.9 . . ? Zr2 C11B H11B 119.0 . . ? C13B C12B C11B 109.3(7) . . ? C13B C12B Zr2 72.7(4) . . ? C11B C12B Zr2 75.6(3) . . ? C13B C12B H12B 125.4 . . ? C11B C12B H12B 125.4 . . ? Zr2 C12B H12B 118.1 . . ? C14B C13B C12B 108.0(8) . . ? C14B C13B Zr2 75.8(4) . . ? C12B C13B Zr2 75.3(4) . . ? C14B C13B H13B 126.0 . . ? C12B C13B H13B 126.0 . . ? Zr2 C13B H13B 115.1 . . ? C13B C14B C15B 107.8(7) . . ? C13B C14B Zr2 72.6(4) . . ? C15B C14B Zr2 74.6(4) . . ? C13B C14B H14B 126.1 . . ? C15B C14B H14B 126.1 . . ? Zr2 C14B H14B 118.7 . . ? C11B C15B C14B 108.6(7) . . ? C11B C15B Zr2 74.9(3) . . ? C14B C15B Zr2 73.4(4) . . ? C11B C15B H15B 125.7 . . ? C14B C15B H15B 125.7 . . ? Zr2 C15B H15B 117.9 . . ? C17B C16B C20B 107.4(7) . . ? C17B C16B Zr2 75.5(4) . . ? C20B C16B Zr2 73.5(4) . . ? C17B C16B H16B 126.3 . . ? C20B C16B H16B 126.3 . . ? Zr2 C16B H16B 116.8 . . ? C18B C17B C16B 108.6(7) . . ? C18B C17B Zr2 73.0(4) . . ? C16B C17B Zr2 72.9(4) . . ? C18B C17B H17B 125.7 . . ? C16B C17B H17B 125.7 . . ? Zr2 C17B H17B 120.2 . . ? C17B C18B C19B 108.1(7) . . ? C17B C18B Zr2 75.7(4) . . ? C19B C18B Zr2 74.5(4) . . ? C17B C18B H18B 125.9 . . ? C19B C18B H18B 125.9 . . ? Zr2 C18B H18B 116.1 . . ? C20B C19B C18B 107.3(7) . . ? C20B C19B Zr2 73.1(4) . . ? C18B C19B Zr2 73.6(4) . . ? C20B C19B H19B 126.3 . . ? C18B C19B H19B 126.3 . . ? Zr2 C19B H19B 118.9 . . ? C19B C20B C16B 108.4(7) . . ? C19B C20B Zr2 75.1(4) . . ? C16B C20B Zr2 74.5(4) . . ? C19B C20B H20B 125.8 . . ? C16B C20B H20B 125.8 . . ? Zr2 C20B H20B 116.7 . . ? C22B C21B C26B 117.0(8) . . ? C22B C21B C4B 123.6(7) . . ? C26B C21B C4B 119.4(7) . . ? C21B C22B C23B 121.3(10) . . ? C21B C22B H22B 119.4 . . ? C23B C22B H22B 119.4 . . ? C24B C23B C22B 119.1(10) . . ? C24B C23B H23B 120.4 . . ? C22B C23B H23B 120.4 . . ? C25B C24B C23B 120.3(10) . . ? C25B C24B H24B 119.8 . . ? C23B C24B H24B 119.8 . . ? C24B C25B C26B 120.9(10) . . ? C24B C25B H25B 119.6 . . ? C26B C25B H25B 119.6 . . ? C25B C26B C21B 121.4(10) . . ? C25B C26B H26B 119.3 . . ? C21B C26B H26B 119.3 . . ? Cl2 C30 Cl1 112(2) . . ? Cl2 C30 H30A 109.3 . . ? Cl1 C30 H30A 109.3 . . ? Cl2 C30 H30B 109.3 . . ? Cl1 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? Cl2A C30A Cl1A 112.1(10) . . ? Cl2A C30A H30C 109.2 . . ? Cl1A C30A H30C 109.2 . . ? Cl2A C30A H30D 109.2 . . ? Cl1A C30A H30D 109.2 . . ? H30C C30A H30D 107.9 . . ? Cl3 C31 Cl4 111.6(12) . . ? Cl3 C31 H31A 109.3 . . ? Cl4 C31 H31A 109.3 . . ? Cl3 C31 H31B 109.3 . . ? Cl4 C31 H31B 109.3 . . ? H31A C31 H31B 108.0 . . ? Cl3A C31A Cl4A 113(2) . . ? Cl3A C31A H31C 109.1 . . ? Cl4A C31A H31C 109.1 . . ? Cl3A C31A H31D 109.1 . . ? Cl4A C31A H31D 109.1 . . ? H31C C31A H31D 107.8 . . ? 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 N1A Zr1 N1A C9A -175.8(6) 2_755 . . . ? C2A Zr1 N1A C9A 4.1(5) . . . . ? C19A Zr1 N1A C9A 97.1(5) . . . . ? C17A Zr1 N1A C9A 110.8(5) . . . . ? C18A Zr1 N1A C9A 121.8(5) . . . . ? C20A Zr1 N1A C9A 68.2(5) . . . . ? C15A Zr1 N1A C9A -102.0(5) . . . . ? C16A Zr1 N1A C9A 66.5(6) . . . . ? C14A Zr1 N1A C9A -108.5(5) . . . . ? C11A Zr1 N1A C9A -55.8(6) . . . . ? C12A Zr1 N1A C9A -55.0(5) . . . . ? N1A Zr1 N1A Zr1 0.0 2_755 . . 2_755 ? C2A Zr1 N1A Zr1 179.9(3) . . . 2_755 ? C19A Zr1 N1A Zr1 -87.1(2) . . . 2_755 ? C17A Zr1 N1A Zr1 -73.4(4) . . . 2_755 ? C18A Zr1 N1A Zr1 -62.4(3) . . . 2_755 ? C20A Zr1 N1A Zr1 -116.0(2) . . . 2_755 ? C15A Zr1 N1A Zr1 73.8(4) . . . 2_755 ? C16A Zr1 N1A Zr1 -117.7(3) . . . 2_755 ? C14A Zr1 N1A Zr1 67.3(3) . . . 2_755 ? C11A Zr1 N1A Zr1 120.0(3) . . . 2_755 ? C12A Zr1 N1A Zr1 120.8(2) . . . 2_755 ? C9A C1A C2A C3A -166.0(6) . . . . ? C5A C1A C2A C3A 20.7(12) . . . . ? C9A C1A C2A Zr1 20.9(7) . . . . ? C5A C1A C2A Zr1 -152.4(6) . . . . ? N1A Zr1 C2A C1A -14.3(5) . . . . ? N1A Zr1 C2A C1A -14.2(7) 2_755 . . . ? C19A Zr1 C2A C1A -99.7(5) . . . . ? C17A Zr1 C2A C1A -148.8(5) . . . . ? C18A Zr1 C2A C1A -113.4(5) . . . . ? C20A Zr1 C2A C1A -122.6(6) . . . . ? C15A Zr1 C2A C1A 119.5(5) . . . . ? C16A Zr1 C2A C1A -152.0(5) . . . . ? C14A Zr1 C2A C1A 84.1(5) . . . . ? C11A Zr1 C2A C1A 126.8(5) . . . . ? C12A Zr1 C2A C1A 99.3(5) . . . . ? N1A Zr1 C2A C3A 172.0(6) . . . . ? N1A Zr1 C2A C3A 172.1(4) 2_755 . . . ? C19A Zr1 C2A C3A 86.6(5) . . . . ? C17A Zr1 C2A C3A 37.5(6) . . . . ? C18A Zr1 C2A C3A 72.9(6) . . . . ? C20A Zr1 C2A C3A 63.7(5) . . . . ? C15A Zr1 C2A C3A -54.2(6) . . . . ? C16A Zr1 C2A C3A 34.3(5) . . . . ? C14A Zr1 C2A C3A -89.6(5) . . . . ? C11A Zr1 C2A C3A -46.9(5) . . . . ? C12A Zr1 C2A C3A -74.4(5) . . . . ? C1A C2A C3A C4A 69.1(11) . . . . ? Zr1 C2A C3A C4A -118.1(7) . . . . ? C2A C3A C4A C21A 173.3(7) . . . . ? C2A C1A C5A C7A -104.7(10) . . . . ? C9A C1A C5A C7A 82.6(10) . . . . ? C2A C1A C5A C8A 130.5(9) . . . . ? C9A C1A C5A C8A -42.2(10) . . . . ? C2A C1A C5A C6A 16.9(12) . . . . ? C9A C1A C5A C6A -155.8(7) . . . . ? Zr1 N1A C9A C1A 5.8(8) . . . . ? Zr1 N1A C9A C1A -168.9(4) 2_755 . . . ? Zr1 N1A C9A C10A -168.3(5) . . . . ? Zr1 N1A C9A C10A 17.0(10) 2_755 . . . ? C2A C1A C9A N1A -18.7(9) . . . . ? C5A C1A C9A N1A 155.0(7) . . . . ? C2A C1A C9A C10A 155.6(6) . . . . ? C5A C1A C9A C10A -30.8(10) . . . . ? N1A Zr1 C11A C12A 1.5(6) . . . . ? N1A Zr1 C11A C12A 97.3(5) 2_755 . . . ? C2A Zr1 C11A C12A -53.8(5) . . . . ? C19A Zr1 C11A C12A -139.7(4) . . . . ? C17A Zr1 C11A C12A -169.5(5) . . . . ? C18A Zr1 C11A C12A -175.8(4) . . . . ? C20A Zr1 C11A C12A -119.8(5) . . . . ? C15A Zr1 C11A C12A 113.8(6) . . . . ? C16A Zr1 C11A C12A -138.2(5) . . . . ? C14A Zr1 C11A C12A 76.2(5) . . . . ? N1A Zr1 C11A C15A -112.3(4) . . . . ? N1A Zr1 C11A C15A -16.6(5) 2_755 . . . ? C2A Zr1 C11A C15A -167.6(4) . . . . ? C19A Zr1 C11A C15A 106.5(5) . . . . ? C17A Zr1 C11A C15A 76.7(4) . . . . ? C18A Zr1 C11A C15A 70.4(5) . . . . ? C20A Zr1 C11A C15A 126.4(4) . . . . ? C16A Zr1 C11A C15A 108.0(4) . . . . ? C14A Zr1 C11A C15A -37.6(4) . . . . ? C12A Zr1 C11A C15A -113.8(6) . . . . ? C15A C11A C12A C13A 0.1(7) . . . . ? Zr1 C11A C12A C13A -66.4(5) . . . . ? C15A C11A C12A Zr1 66.5(5) . . . . ? N1A Zr1 C12A C11A -178.9(4) . . . . ? N1A Zr1 C12A C11A -104.6(5) 2_755 . . . ? C2A Zr1 C12A C11A 118.8(5) . . . . ? C19A Zr1 C12A C11A 76.6(6) . . . . ? C17A Zr1 C12A C11A 12.0(5) . . . . ? C18A Zr1 C12A C11A 7.4(7) . . . . ? C20A Zr1 C12A C11A 72.9(5) . . . . ? C15A Zr1 C12A C11A -37.9(4) . . . . ? C16A Zr1 C12A C11A 42.7(5) . . . . ? C14A Zr1 C12A C11A -78.6(5) . . . . ? N1A Zr1 C12A C13A -62.3(5) . . . . ? N1A Zr1 C12A C13A 12.0(5) 2_755 . . . ? C2A Zr1 C12A C13A -124.6(5) . . . . ? C19A Zr1 C12A C13A -166.8(5) . . . . ? C17A Zr1 C12A C13A 128.6(4) . . . . ? C18A Zr1 C12A C13A 124.0(5) . . . . ? C20A Zr1 C12A C13A -170.5(4) . . . . ? C15A Zr1 C12A C13A 78.7(5) . . . . ? C16A Zr1 C12A C13A 159.3(4) . . . . ? C14A Zr1 C12A C13A 38.0(4) . . . . ? C11A Zr1 C12A C13A 116.6(7) . . . . ? C11A C12A C13A C14A -0.7(7) . . . . ? Zr1 C12A C13A C14A -66.6(4) . . . . ? C11A C12A C13A Zr1 65.9(5) . . . . ? N1A Zr1 C13A C12A 119.9(4) . . . . ? N1A Zr1 C13A C12A -170.0(4) 2_755 . . . ? C2A Zr1 C13A C12A 49.0(4) . . . . ? C19A Zr1 C13A C12A 116.8(18) . . . . ? C17A Zr1 C13A C12A -72.6(5) . . . . ? C18A Zr1 C13A C12A -117.8(5) . . . . ? C20A Zr1 C13A C12A 16.9(7) . . . . ? C15A Zr1 C13A C12A -76.6(5) . . . . ? C16A Zr1 C13A C12A -28.0(6) . . . . ? C14A Zr1 C13A C12A -113.2(6) . . . . ? C11A Zr1 C13A C12A -36.0(4) . . . . ? N1A Zr1 C13A C14A -126.9(4) . . . . ? N1A Zr1 C13A C14A -56.8(4) 2_755 . . . ? C2A Zr1 C13A C14A 162.2(4) . . . . ? C19A Zr1 C13A C14A -130.0(18) . . . . ? C17A Zr1 C13A C14A 40.6(5) . . . . ? C18A Zr1 C13A C14A -4.6(7) . . . . ? C20A Zr1 C13A C14A 130.1(5) . . . . ? C15A Zr1 C13A C14A 36.6(4) . . . . ? C16A Zr1 C13A C14A 85.2(5) . . . . ? C11A Zr1 C13A C14A 77.2(4) . . . . ? C12A Zr1 C13A C14A 113.2(6) . . . . ? C12A C13A C14A C15A 1.0(7) . . . . ? Zr1 C13A C14A C15A -66.1(5) . . . . ? C12A C13A C14A Zr1 67.1(4) . . . . ? N1A Zr1 C14A C15A 171.6(4) . . . . ? N1A Zr1 C14A C15A -124.3(5) 2_755 . . . ? C2A Zr1 C14A C15A 95.8(5) . . . . ? C19A Zr1 C14A C15A -76.1(6) . . . . ? C17A Zr1 C14A C15A -35.0(5) . . . . ? C18A Zr1 C14A C15A -66.9(5) . . . . ? C20A Zr1 C14A C15A -0.7(8) . . . . ? C16A Zr1 C14A C15A -3.9(5) . . . . ? C11A Zr1 C14A C15A 37.9(4) . . . . ? C12A Zr1 C14A C15A 78.1(5) . . . . ? N1A Zr1 C14A C13A 56.0(4) . . . . ? N1A Zr1 C14A C13A 120.1(4) 2_755 . . . ? C2A Zr1 C14A C13A -19.8(5) . . . . ? C19A Zr1 C14A C13A 168.3(4) . . . . ? C17A Zr1 C14A C13A -150.6(4) . . . . ? C18A Zr1 C14A C13A 177.5(4) . . . . ? C20A Zr1 C14A C13A -116.3(6) . . . . ? C15A Zr1 C14A C13A -115.6(6) . . . . ? C16A Zr1 C14A C13A -119.5(4) . . . . ? C11A Zr1 C14A C13A -77.7(4) . . . . ? C12A Zr1 C14A C13A -37.5(4) . . . . ? C13A C14A C15A C11A -0.9(7) . . . . ? Zr1 C14A C15A C11A -68.0(5) . . . . ? C13A C14A C15A Zr1 67.1(5) . . . . ? C12A C11A C15A C14A 0.5(7) . . . . ? Zr1 C11A C15A C14A 68.0(5) . . . . ? C12A C11A C15A Zr1 -67.5(4) . . . . ? N1A Zr1 C15A C14A -11.9(6) . . . . ? N1A Zr1 C15A C14A 53.1(4) 2_755 . . . ? C2A Zr1 C15A C14A -99.8(5) . . . . ? C19A Zr1 C15A C14A 141.2(4) . . . . ? C17A Zr1 C15A C14A 146.4(5) . . . . ? C18A Zr1 C15A C14A 125.0(4) . . . . ? C20A Zr1 C15A C14A 179.6(4) . . . . ? C16A Zr1 C15A C14A 176.7(5) . . . . ? C11A Zr1 C15A C14A -113.4(6) . . . . ? C12A Zr1 C15A C14A -76.3(5) . . . . ? N1A Zr1 C15A C11A 101.5(5) . . . . ? N1A Zr1 C15A C11A 166.5(4) 2_755 . . . ? C2A Zr1 C15A C11A 13.6(5) . . . . ? C19A Zr1 C15A C11A -105.4(5) . . . . ? C17A Zr1 C15A C11A -100.2(4) . . . . ? C18A Zr1 C15A C11A -121.5(4) . . . . ? C20A Zr1 C15A C11A -67.0(5) . . . . ? C16A Zr1 C15A C11A -69.8(4) . . . . ? C14A Zr1 C15A C11A 113.4(6) . . . . ? C12A Zr1 C15A C11A 37.1(4) . . . . ? N1A Zr1 C16A C20A 3.2(6) . . . . ? N1A Zr1 C16A C20A -89.0(5) 2_755 . . . ? C2A Zr1 C16A C20A 60.6(4) . . . . ? C19A Zr1 C16A C20A -36.4(4) . . . . ? C17A Zr1 C16A C20A -114.0(6) . . . . ? C18A Zr1 C16A C20A -77.2(5) . . . . ? C15A Zr1 C16A C20A 175.4(5) . . . . ? C14A Zr1 C16A C20A 177.5(4) . . . . ? C11A Zr1 C16A C20A 145.0(5) . . . . ? C12A Zr1 C16A C20A 123.9(4) . . . . ? N1A Zr1 C16A C17A 117.2(4) . . . . ? N1A Zr1 C16A C17A 25.0(5) 2_755 . . . ? C2A Zr1 C16A C17A 174.6(5) . . . . ? C19A Zr1 C16A C17A 77.7(5) . . . . ? C18A Zr1 C16A C17A 36.8(4) . . . . ? C20A Zr1 C16A C17A 114.0(6) . . . . ? C15A Zr1 C16A C17A -70.6(5) . . . . ? C14A Zr1 C16A C17A -68.5(5) . . . . ? C11A Zr1 C16A C17A -101.0(5) . . . . ? C12A Zr1 C16A C17A -122.1(4) . . . . ? C20A C16A C17A C18A -0.1(8) . . . . ? Zr1 C16A C17A C18A -67.0(5) . . . . ? C20A C16A C17A Zr1 66.9(5) . . . . ? N1A Zr1 C17A C18A 20.2(6) . . . . ? N1A Zr1 C17A C18A -44.5(5) 2_755 . . . ? C2A Zr1 C17A C18A 108.9(5) . . . . ? C19A Zr1 C17A C18A 37.5(4) . . . . ? C20A Zr1 C17A C18A 77.5(5) . . . . ? C15A Zr1 C17A C18A -137.8(5) . . . . ? C16A Zr1 C17A C18A 114.8(7) . . . . ? C14A Zr1 C17A C18A -119.9(5) . . . . ? C11A Zr1 C17A C18A -169.4(5) . . . . ? C12A Zr1 C17A C18A -175.7(4) . . . . ? N1A Zr1 C17A C16A -94.6(5) . . . . ? N1A Zr1 C17A C16A -159.3(4) 2_755 . . . ? C2A Zr1 C17A C16A -5.9(5) . . . . ? C19A Zr1 C17A C16A -77.3(5) . . . . ? C18A Zr1 C17A C16A -114.8(7) . . . . ? C20A Zr1 C17A C16A -37.3(4) . . . . ? C15A Zr1 C17A C16A 107.4(5) . . . . ? C14A Zr1 C17A C16A 125.2(4) . . . . ? C11A Zr1 C17A C16A 75.7(4) . . . . ? C12A Zr1 C17A C16A 69.5(5) . . . . ? C16A C17A C18A C19A 0.7(7) . . . . ? Zr1 C17A C18A C19A -66.4(4) . . . . ? C16A C17A C18A Zr1 67.1(5) . . . . ? N1A Zr1 C18A C17A -165.9(4) . . . . ? N1A Zr1 C18A C17A 132.5(5) 2_755 . . . ? C2A Zr1 C18A C17A -88.3(5) . . . . ? C19A Zr1 C18A C17A -114.6(6) . . . . ? C20A Zr1 C18A C17A -77.4(5) . . . . ? C15A Zr1 C18A C17A 43.3(5) . . . . ? C16A Zr1 C18A C17A -37.1(4) . . . . ? C14A Zr1 C18A C17A 73.4(5) . . . . ? C11A Zr1 C18A C17A 12.1(5) . . . . ? C12A Zr1 C18A C17A 7.7(7) . . . . ? N1A Zr1 C18A C19A -51.3(4) . . . . ? N1A Zr1 C18A C19A -112.9(4) 2_755 . . . ? C2A Zr1 C18A C19A 26.3(5) . . . . ? C17A Zr1 C18A C19A 114.6(6) . . . . ? C20A Zr1 C18A C19A 37.2(4) . . . . ? C15A Zr1 C18A C19A 157.9(4) . . . . ? C16A Zr1 C18A C19A 77.5(4) . . . . ? C14A Zr1 C18A C19A -172.0(4) . . . . ? C11A Zr1 C18A C19A 126.7(4) . . . . ? C12A Zr1 C18A C19A 122.3(5) . . . . ? C17A C18A C19A C20A -1.0(7) . . . . ? Zr1 C18A C19A C20A -67.7(4) . . . . ? C17A C18A C19A Zr1 66.7(5) . . . . ? N1A Zr1 C19A C20A -114.6(4) . . . . ? N1A Zr1 C19A C20A 174.9(4) 2_755 . . . ? C2A Zr1 C19A C20A -44.0(4) . . . . ? C17A Zr1 C19A C20A 76.9(5) . . . . ? C18A Zr1 C19A C20A 113.7(6) . . . . ? C15A Zr1 C19A C20A 83.4(5) . . . . ? C16A Zr1 C19A C20A 36.6(4) . . . . ? C14A Zr1 C19A C20A 128.7(5) . . . . ? C11A Zr1 C19A C20A 38.4(5) . . . . ? C12A Zr1 C19A C20A -6.1(7) . . . . ? N1A Zr1 C19A C18A 131.7(4) . . . . ? N1A Zr1 C19A C18A 61.2(4) 2_755 . . . ? C2A Zr1 C19A C18A -157.7(4) . . . . ? C17A Zr1 C19A C18A -36.8(4) . . . . ? C20A Zr1 C19A C18A -113.7(6) . . . . ? C15A Zr1 C19A C18A -30.3(5) . . . . ? C16A Zr1 C19A C18A -77.1(4) . . . . ? C14A Zr1 C19A C18A 15.0(7) . . . . ? C11A Zr1 C19A C18A -75.3(5) . . . . ? C12A Zr1 C19A C18A -119.8(5) . . . . ? C18A C19A C20A C16A 0.9(7) . . . . ? Zr1 C19A C20A C16A -66.5(5) . . . . ? C18A C19A C20A Zr1 67.4(4) . . . . ? C17A C16A C20A C19A -0.5(7) . . . . ? Zr1 C16A C20A C19A 66.2(5) . . . . ? C17A C16A C20A Zr1 -66.7(5) . . . . ? N1A Zr1 C20A C19A 66.8(4) . . . . ? N1A Zr1 C20A C19A -5.7(5) 2_755 . . . ? C2A Zr1 C20A C19A 132.0(5) . . . . ? C17A Zr1 C20A C19A -78.2(5) . . . . ? C18A Zr1 C20A C19A -38.0(4) . . . . ? C15A Zr1 C20A C19A -121.2(4) . . . . ? C16A Zr1 C20A C19A -115.7(6) . . . . ? C14A Zr1 C20A C19A -120.7(6) . . . . ? C11A Zr1 C20A C19A -151.9(4) . . . . ? C12A Zr1 C20A C19A 176.6(4) . . . . ? N1A Zr1 C20A C16A -177.5(4) . . . . ? N1A Zr1 C20A C16A 110.0(4) 2_755 . . . ? C2A Zr1 C20A C16A -112.3(5) . . . . ? C19A Zr1 C20A C16A 115.7(6) . . . . ? C17A Zr1 C20A C16A 37.5(4) . . . . ? C18A Zr1 C20A C16A 77.7(5) . . . . ? C15A Zr1 C20A C16A -5.5(5) . . . . ? C14A Zr1 C20A C16A -5.0(8) . . . . ? C11A Zr1 C20A C16A -36.2(5) . . . . ? C12A Zr1 C20A C16A -67.7(5) . . . . ? C3A C4A C21A C26A 175.7(7) . . . . ? C3A C4A C21A C22A -2.6(12) . . . . ? C26A C21A C22A C23A -1.3(12) . . . . ? C4A C21A C22A C23A 177.0(8) . . . . ? C21A C22A C23A C24A 1.6(14) . . . . ? C22A C23A C24A C25A -0.8(14) . . . . ? C23A C24A C25A C26A -0.3(13) . . . . ? C24A C25A C26A C21A 0.7(12) . . . . ? C22A C21A C26A C25A 0.1(11) . . . . ? C4A C21A C26A C25A -178.2(7) . . . . ? N1B Zr2 N1B C9B 179.7(5) 2_676 . . . ? C2B Zr2 N1B C9B -1.0(4) . . . . ? C13B Zr2 N1B C9B -60.4(5) . . . . ? C20B Zr2 N1B C9B 105.4(5) . . . . ? C12B Zr2 N1B C9B -104.6(5) . . . . ? C16B Zr2 N1B C9B 59.9(5) . . . . ? C18B Zr2 N1B C9B 85.0(4) . . . . ? C14B Zr2 N1B C9B -65.2(4) . . . . ? C19B Zr2 N1B C9B 111.5(4) . . . . ? C15B Zr2 N1B C9B -95.4(4) . . . . ? C17B Zr2 N1B C9B 57.9(4) . . . . ? N1B Zr2 N1B Zr2 0.0 2_676 . . 2_676 ? C2B Zr2 N1B Zr2 179.4(3) . . . 2_676 ? C13B Zr2 N1B Zr2 119.9(3) . . . 2_676 ? C20B Zr2 N1B Zr2 -74.3(4) . . . 2_676 ? C12B Zr2 N1B Zr2 75.7(4) . . . 2_676 ? C16B Zr2 N1B Zr2 -119.7(3) . . . 2_676 ? C18B Zr2 N1B Zr2 -94.7(3) . . . 2_676 ? C14B Zr2 N1B Zr2 115.2(2) . . . 2_676 ? C19B Zr2 N1B Zr2 -68.1(3) . . . 2_676 ? C15B Zr2 N1B Zr2 84.9(3) . . . 2_676 ? C17B Zr2 N1B Zr2 -121.8(2) . . . 2_676 ? C9B C1B C2B C3B 165.9(6) . . . . ? C5B C1B C2B C3B -17.8(10) . . . . ? C9B C1B C2B Zr2 -19.5(6) . . . . ? C5B C1B C2B Zr2 156.8(4) . . . . ? N1B Zr2 C2B C1B 11.9(5) . . . . ? N1B Zr2 C2B C1B 12.9(7) 2_676 . . . ? C13B Zr2 C2B C1B 150.4(5) . . . . ? C20B Zr2 C2B C1B -120.4(5) . . . . ? C12B Zr2 C2B C1B 149.1(5) . . . . ? C16B Zr2 C2B C1B -128.5(5) . . . . ? C18B Zr2 C2B C1B -75.6(5) . . . . ? C14B Zr2 C2B C1B 120.0(5) . . . . ? C19B Zr2 C2B C1B -85.2(5) . . . . ? C15B Zr2 C2B C1B 99.1(5) . . . . ? C17B Zr2 C2B C1B -101.5(5) . . . . ? N1B Zr2 C2B C3B -173.0(5) . . . . ? N1B Zr2 C2B C3B -172.1(4) 2_676 . . . ? C13B Zr2 C2B C3B -34.5(5) . . . . ? C20B Zr2 C2B C3B 54.7(6) . . . . ? C12B Zr2 C2B C3B -35.8(6) . . . . ? C16B Zr2 C2B C3B 46.5(5) . . . . ? C18B Zr2 C2B C3B 99.4(5) . . . . ? C14B Zr2 C2B C3B -64.9(5) . . . . ? C19B Zr2 C2B C3B 89.9(5) . . . . ? C15B Zr2 C2B C3B -85.9(5) . . . . ? C17B Zr2 C2B C3B 73.6(5) . . . . ? C1B C2B C3B C4B -69.5(10) . . . . ? Zr2 C2B C3B C4B 116.1(6) . . . . ? C2B C3B C4B C21B -174.0(6) . . . . ? C2B C1B C5B C8B 94.6(6) . . . . ? C9B C1B C5B C8B -89.4(5) . . . . ? C2B C1B C5B C7B -26.5(7) . . . . ? C9B C1B C5B C7B 149.5(4) . . . . ? C2B C1B C5B C6B -142.1(6) . . . . ? C9B C1B C5B C6B 33.9(6) . . . . ? Zr2 N1B C9B C10B 164.76(14) . . . . ? Zr2 N1B C9B C10B -15.7(5) 2_676 . . . ? Zr2 N1B C9B C1B -9.6(6) . . . . ? Zr2 N1B C9B C1B 170.0(4) 2_676 . . . ? C2B C1B C9B N1B 20.1(7) . . . . ? C5B C1B C9B N1B -156.4(4) . . . . ? C2B C1B C9B C10B -154.4(4) . . . . ? C5B C1B C9B C10B 29.1(6) . . . . ? N1B Zr2 C11B C15B 49.2(4) . . . . ? N1B Zr2 C11B C15B 109.9(4) 2_676 . . . ? C2B Zr2 C11B C15B -30.6(4) . . . . ? C13B Zr2 C11B C15B -76.9(4) . . . . ? C20B Zr2 C11B C15B -160.9(4) . . . . ? C12B Zr2 C11B C15B -113.5(5) . . . . ? C16B Zr2 C11B C15B -129.8(4) . . . . ? C18B Zr2 C11B C15B 171.2(5) . . . . ? C14B Zr2 C11B C15B -37.0(4) . . . . ? C19B Zr2 C11B C15B 170.0(4) . . . . ? C17B Zr2 C11B C15B -124.8(5) . . . . ? N1B Zr2 C11B C12B 162.6(4) . . . . ? N1B Zr2 C11B C12B -136.7(4) 2_676 . . . ? C2B Zr2 C11B C12B 82.9(5) . . . . ? C13B Zr2 C11B C12B 36.5(5) . . . . ? C20B Zr2 C11B C12B -47.4(5) . . . . ? C16B Zr2 C11B C12B -16.3(5) . . . . ? C18B Zr2 C11B C12B -75.3(6) . . . . ? C14B Zr2 C11B C12B 76.5(5) . . . . ? C19B Zr2 C11B C12B -76.6(5) . . . . ? C15B Zr2 C11B C12B 113.5(5) . . . . ? C17B Zr2 C11B C12B -11.3(5) . . . . ? C15B C11B C12B C13B 0.9(7) . . . . ? Zr2 C11B C12B C13B -65.5(5) . . . . ? C15B C11B C12B Zr2 66.4(4) . . . . ? N1B Zr2 C12B C13B 90.0(6) . . . . ? N1B Zr2 C12B C13B 156.9(5) 2_676 . . . ? C2B Zr2 C12B C13B 2.4(6) . . . . ? C20B Zr2 C12B C13B -110.7(6) . . . . ? C16B Zr2 C12B C13B -78.8(6) . . . . ? C18B Zr2 C12B C13B -103.1(6) . . . . ? C14B Zr2 C12B C13B 37.5(5) . . . . ? C19B Zr2 C12B C13B -127.0(5) . . . . ? C15B Zr2 C12B C13B 78.4(6) . . . . ? C17B Zr2 C12B C13B -70.9(6) . . . . ? N1B Zr2 C12B C11B -25.8(6) . . . . ? N1B Zr2 C12B C11B 41.0(4) 2_676 . . . ? C2B Zr2 C12B C11B -113.5(4) . . . . ? C13B Zr2 C12B C11B -115.9(7) . . . . ? C20B Zr2 C12B C11B 133.4(4) . . . . ? C16B Zr2 C12B C11B 165.3(4) . . . . ? C18B Zr2 C12B C11B 141.0(4) . . . . ? C14B Zr2 C12B C11B -78.3(4) . . . . ? C19B Zr2 C12B C11B 117.1(4) . . . . ? C15B Zr2 C12B C11B -37.5(3) . . . . ? C17B Zr2 C12B C11B 173.3(3) . . . . ? C11B C12B C13B C14B -2.0(8) . . . . ? Zr2 C12B C13B C14B -69.4(5) . . . . ? C11B C12B C13B Zr2 67.4(5) . . . . ? N1B Zr2 C13B C14B -8.9(6) . . . . ? N1B Zr2 C13B C14B 84.9(5) 2_676 . . . ? C2B Zr2 C13B C14B -64.5(5) . . . . ? C20B Zr2 C13B C14B -179.0(5) . . . . ? C12B Zr2 C13B C14B 113.3(7) . . . . ? C16B Zr2 C13B C14B -149.5(5) . . . . ? C18B Zr2 C13B C14B -139.3(5) . . . . ? C19B Zr2 C13B C14B -179.4(4) . . . . ? C15B Zr2 C13B C14B 37.2(5) . . . . ? C17B Zr2 C13B C14B -127.0(5) . . . . ? N1B Zr2 C13B C12B -122.2(5) . . . . ? N1B Zr2 C13B C12B -28.4(6) 2_676 . . . ? C2B Zr2 C13B C12B -177.8(6) . . . . ? C20B Zr2 C13B C12B 67.7(6) . . . . ? C16B Zr2 C13B C12B 97.1(6) . . . . ? C18B Zr2 C13B C12B 107.4(6) . . . . ? C14B Zr2 C13B C12B -113.3(7) . . . . ? C19B Zr2 C13B C12B 67.3(6) . . . . ? C15B Zr2 C13B C12B -76.2(6) . . . . ? C17B Zr2 C13B C12B 119.6(5) . . . . ? C12B C13B C14B C15B 2.3(8) . . . . ? Zr2 C13B C14B C15B -66.8(5) . . . . ? C12B C13B C14B Zr2 69.1(5) . . . . ? N1B Zr2 C14B C13B 173.2(5) . . . . ? N1B Zr2 C14B C13B -113.9(5) 2_676 . . . ? C2B Zr2 C14B C13B 107.6(5) . . . . ? C20B Zr2 C14B C13B 1.2(6) . . . . ? C12B Zr2 C14B C13B -38.0(5) . . . . ? C16B Zr2 C14B C13B 31.6(5) . . . . ? C18B Zr2 C14B C13B 75.1(7) . . . . ? C19B Zr2 C14B C13B 1.2(9) . . . . ? C15B Zr2 C14B C13B -114.8(7) . . . . ? C17B Zr2 C14B C13B 63.6(5) . . . . ? N1B Zr2 C14B C15B -72.0(5) . . . . ? N1B Zr2 C14B C15B 0.9(5) 2_676 . . . ? C2B Zr2 C14B C15B -137.6(5) . . . . ? C13B Zr2 C14B C15B 114.8(7) . . . . ? C20B Zr2 C14B C15B 116.0(5) . . . . ? C12B Zr2 C14B C15B 76.8(5) . . . . ? C16B Zr2 C14B C15B 146.4(5) . . . . ? C18B Zr2 C14B C15B -170.0(5) . . . . ? C19B Zr2 C14B C15B 116.0(7) . . . . ? C17B Zr2 C14B C15B 178.4(4) . . . . ? C12B C11B C15B C14B 0.5(6) . . . . ? Zr2 C11B C15B C14B 66.3(4) . . . . ? C12B C11B C15B Zr2 -65.7(4) . . . . ? C13B C14B C15B C11B -1.7(7) . . . . ? Zr2 C14B C15B C11B -67.2(4) . . . . ? C13B C14B C15B Zr2 65.5(5) . . . . ? N1B Zr2 C15B C11B -134.8(3) . . . . ? N1B Zr2 C15B C11B -64.0(3) 2_676 . . . ? C2B Zr2 C15B C11B 154.3(3) . . . . ? C13B Zr2 C15B C11B 78.4(4) . . . . ? C20B Zr2 C15B C11B 25.6(5) . . . . ? C12B Zr2 C15B C11B 37.7(3) . . . . ? C16B Zr2 C15B C11B 69.4(5) . . . . ? C18B Zr2 C15B C11B -131(3) . . . . ? C14B Zr2 C15B C11B 115.2(6) . . . . ? C19B Zr2 C15B C11B -17.9(7) . . . . ? C17B Zr2 C15B C11B 112.3(5) . . . . ? N1B Zr2 C15B C14B 110.0(5) . . . . ? N1B Zr2 C15B C14B -179.2(5) 2_676 . . . ? C2B Zr2 C15B C14B 39.2(5) . . . . ? C13B Zr2 C15B C14B -36.7(4) . . . . ? C20B Zr2 C15B C14B -89.6(6) . . . . ? C12B Zr2 C15B C14B -77.4(5) . . . . ? C16B Zr2 C15B C14B -45.7(6) . . . . ? C18B Zr2 C15B C14B 114(3) . . . . ? C19B Zr2 C15B C14B -133.1(6) . . . . ? C17B Zr2 C15B C14B -2.9(8) . . . . ? N1B Zr2 C16B C17B -3.8(6) . . . . ? N1B Zr2 C16B C17B -99.6(5) 2_676 . . . ? C2B Zr2 C16B C17B 52.4(5) . . . . ? C13B Zr2 C16B C17B 134.5(5) . . . . ? C20B Zr2 C16B C17B -113.5(7) . . . . ? C12B Zr2 C16B C17B 166.3(5) . . . . ? C18B Zr2 C16B C17B -35.9(4) . . . . ? C14B Zr2 C16B C17B 118.3(5) . . . . ? C19B Zr2 C16B C17B -76.4(5) . . . . ? C15B Zr2 C16B C17B 141.8(5) . . . . ? N1B Zr2 C16B C20B 109.7(5) . . . . ? N1B Zr2 C16B C20B 13.9(6) 2_676 . . . ? C2B Zr2 C16B C20B 165.9(5) . . . . ? C13B Zr2 C16B C20B -112.0(5) . . . . ? C12B Zr2 C16B C20B -80.2(5) . . . . ? C18B Zr2 C16B C20B 77.6(5) . . . . ? C14B Zr2 C16B C20B -128.2(5) . . . . ? C19B Zr2 C16B C20B 37.1(5) . . . . ? C15B Zr2 C16B C20B -104.7(5) . . . . ? C17B Zr2 C16B C20B 113.5(7) . . . . ? C20B C16B C17B C18B -2.4(8) . . . . ? Zr2 C16B C17B C18B 64.8(5) . . . . ? C20B C16B C17B Zr2 -67.2(5) . . . . ? N1B Zr2 C17B C18B 60.9(5) . . . . ? N1B Zr2 C17B C18B -13.8(5) 2_676 . . . ? C2B Zr2 C17B C18B 123.5(5) . . . . ? C13B Zr2 C17B C18B -162.4(5) . . . . ? C20B Zr2 C17B C18B -78.4(5) . . . . ? C12B Zr2 C17B C18B -131.5(5) . . . . ? C16B Zr2 C17B C18B -116.3(7) . . . . ? C14B Zr2 C17B C18B 168.9(5) . . . . ? C19B Zr2 C17B C18B -37.8(5) . . . . ? C15B Zr2 C17B C18B 170.6(5) . . . . ? N1B Zr2 C17B C16B 177.2(5) . . . . ? N1B Zr2 C17B C16B 102.5(5) 2_676 . . . ? C2B Zr2 C17B C16B -120.2(5) . . . . ? C13B Zr2 C17B C16B -46.1(5) . . . . ? C20B Zr2 C17B C16B 37.9(5) . . . . ? C12B Zr2 C17B C16B -15.2(6) . . . . ? C18B Zr2 C17B C16B 116.3(7) . . . . ? C14B Zr2 C17B C16B -74.8(5) . . . . ? C19B Zr2 C17B C16B 78.5(5) . . . . ? C15B Zr2 C17B C16B -73.1(7) . . . . ? C16B C17B C18B C19B 3.3(8) . . . . ? Zr2 C17B C18B C19B 68.0(5) . . . . ? C16B C17B C18B Zr2 -64.7(5) . . . . ? N1B Zr2 C18B C17B -121.1(5) . . . . ? N1B Zr2 C18B C17B 168.5(5) 2_676 . . . ? C2B Zr2 C18B C17B -49.8(5) . . . . ? C13B Zr2 C18B C17B 23.4(6) . . . . ? C20B Zr2 C18B C17B 76.8(5) . . . . ? C12B Zr2 C18B C17B 67.4(6) . . . . ? C16B Zr2 C18B C17B 36.2(4) . . . . ? C14B Zr2 C18B C17B -19.6(8) . . . . ? C19B Zr2 C18B C17B 113.8(7) . . . . ? C15B Zr2 C18B C17B -125(3) . . . . ? N1B Zr2 C18B C19B 125.1(5) . . . . ? N1B Zr2 C18B C19B 54.7(5) 2_676 . . . ? C2B Zr2 C18B C19B -163.6(5) . . . . ? C13B Zr2 C18B C19B -90.4(5) . . . . ? C20B Zr2 C18B C19B -37.1(4) . . . . ? C12B Zr2 C18B C19B -46.5(6) . . . . ? C16B Zr2 C18B C19B -77.6(5) . . . . ? C14B Zr2 C18B C19B -133.4(6) . . . . ? C15B Zr2 C18B C19B 121(3) . . . . ? C17B Zr2 C18B C19B -113.8(7) . . . . ? C17B C18B C19B C20B -2.9(8) . . . . ? Zr2 C18B C19B C20B 65.9(5) . . . . ? C17B C18B C19B Zr2 -68.8(5) . . . . ? N1B Zr2 C19B C20B -171.8(5) . . . . ? N1B Zr2 C19B C20B 123.1(5) 2_676 . . . ? C2B Zr2 C19B C20B -96.3(5) . . . . ? C13B Zr2 C19B C20B 0.8(6) . . . . ? C12B Zr2 C19B C20B 31.8(6) . . . . ? C16B Zr2 C19B C20B -37.3(5) . . . . ? C18B Zr2 C19B C20B -114.4(7) . . . . ? C14B Zr2 C19B C20B 0.0(9) . . . . ? C15B Zr2 C19B C20B 75.1(7) . . . . ? C17B Zr2 C19B C20B -77.4(5) . . . . ? N1B Zr2 C19B C18B -57.4(5) . . . . ? N1B Zr2 C19B C18B -122.5(5) 2_676 . . . ? C2B Zr2 C19B C18B 18.1(5) . . . . ? C13B Zr2 C19B C18B 115.2(5) . . . . ? C20B Zr2 C19B C18B 114.4(7) . . . . ? C12B Zr2 C19B C18B 146.2(5) . . . . ? C16B Zr2 C19B C18B 77.1(5) . . . . ? C14B Zr2 C19B C18B 114.5(7) . . . . ? C15B Zr2 C19B C18B -170.5(5) . . . . ? C17B Zr2 C19B C18B 37.0(4) . . . . ? C18B C19B C20B C16B 1.5(8) . . . . ? Zr2 C19B C20B C16B 67.6(5) . . . . ? C18B C19B C20B Zr2 -66.2(5) . . . . ? C17B C16B C20B C19B 0.5(8) . . . . ? Zr2 C16B C20B C19B -68.0(5) . . . . ? C17B C16B C20B Zr2 68.5(5) . . . . ? N1B Zr2 C20B C19B 11.4(7) . . . . ? N1B Zr2 C20B C19B -54.1(5) 2_676 . . . ? C2B Zr2 C20B C19B 99.0(5) . . . . ? C13B Zr2 C20B C19B -179.4(5) . . . . ? C12B Zr2 C20B C19B -149.6(5) . . . . ? C16B Zr2 C20B C19B 114.4(7) . . . . ? C18B Zr2 C20B C19B 37.3(4) . . . . ? C14B Zr2 C20B C19B -180.0(4) . . . . ? C15B Zr2 C20B C19B -139.9(5) . . . . ? C17B Zr2 C20B C19B 77.1(5) . . . . ? N1B Zr2 C20B C16B -103.0(5) . . . . ? N1B Zr2 C20B C16B -168.6(5) 2_676 . . . ? C2B Zr2 C20B C16B -15.4(6) . . . . ? C13B Zr2 C20B C16B 66.2(5) . . . . ? C12B Zr2 C20B C16B 95.9(5) . . . . ? C18B Zr2 C20B C16B -77.1(5) . . . . ? C14B Zr2 C20B C16B 65.6(6) . . . . ? C19B Zr2 C20B C16B -114.4(7) . . . . ? C15B Zr2 C20B C16B 105.6(5) . . . . ? C17B Zr2 C20B C16B -37.4(5) . . . . ? C3B C4B C21B C22B 12.9(10) . . . . ? C3B C4B C21B C26B -166.2(6) . . . . ? C26B C21B C22B C23B 1.4(12) . . . . ? C4B C21B C22B C23B -177.7(7) . . . . ? C21B C22B C23B C24B 0.2(14) . . . . ? C22B C23B C24B C25B -1.0(15) . . . . ? C23B C24B C25B C26B 0.2(16) . . . . ? C24B C25B C26B C21B 1.5(15) . . . . ? C22B C21B C26B C25B -2.3(13) . . . . ? C4B C21B C26B C25B 176.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.502 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.100 #============================================================================= # end of cif data for "erk7052" (compound 8) #============================================================================= #============================================================================= # end of cif file #============================================================================= _database_code_depnum_ccdc_archive 'CCDC 938717'