Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 182 loop_ _publ_author_name 'Hagadorn, John' _publ_contact_author_name 'Prof John Hagadorn' _publ_contact_author_address ; Chemistry and Biochemistry University of Colorado 215 UCB Boulder CO 80309-0215 UNITED STATES OF AMERICA ; _publ_contact_author_email 'HAGADORN@STRIPE.COLORADO.EDU' _publ_requested_journal 'Chemical Communicatications' _publ_section_title 'New binucleating ligands to support dizirconium organometallics' data_jrh008 _database_code_CSD 170218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (iPr4DBF)Zr2Bn6(Et2O)1.5 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H91 N4 O2.50 Zr2' _chemical_formula_weight 1258.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.392(2) _cell_length_b 18.274(4) _cell_length_c 18.717(4) _cell_angle_alpha 109.66(3) _cell_angle_beta 102.65(3) _cell_angle_gamma 105.50(3) _cell_volume 3324.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 8776 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.91 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1326 _exptl_absorpt_coefficient_mu 0.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; absorption correction applied using SADABS(Sheldrick, 1996) ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer-CCD detector' _diffrn_measurement_method '0.3 deg omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32504 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 31.52 _reflns_number_total 20243 _reflns_number_gt 11705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20243 _refine_ls_number_parameters 783 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.93125(3) 0.762905(19) 0.259487(18) 0.02840(8) Uani 1 1 d . . . Zr2 Zr 0.71290(3) 0.266819(19) 0.237378(18) 0.02653(8) Uani 1 1 d . . . N1 N 1.0826(3) 0.71492(17) 0.30525(15) 0.0313(6) Uani 1 1 d . . . N2 N 0.9807(3) 0.66805(18) 0.17310(16) 0.0356(6) Uani 1 1 d . . . N3 N 0.9269(3) 0.34729(17) 0.28756(15) 0.0302(6) Uani 1 1 d . . . N4 N 0.8135(3) 0.30091(17) 0.15687(15) 0.0326(6) Uani 1 1 d . . . O1 O 1.0811(2) 0.49906(13) 0.20867(12) 0.0267(4) Uani 1 1 d . . . C1 C 1.2848(4) 0.8163(2) 0.4164(2) 0.0479(9) Uani 1 1 d . . . H1A H 1.3193 0.8304 0.3772 0.072 Uiso 1 1 calc R . . H1B H 1.3559 0.8218 0.4608 0.072 Uiso 1 1 calc R . . H1C H 1.2421 0.8544 0.4378 0.072 Uiso 1 1 calc R . . C2 C 1.1874(3) 0.7269(2) 0.37544(19) 0.0344(7) Uani 1 1 d . . . H2 H 1.2340 0.6895 0.3551 0.041 Uiso 1 1 calc R . . C3 C 1.1328(4) 0.7010(2) 0.4346(2) 0.0454(9) Uani 1 1 d . . . H3A H 1.1073 0.7450 0.4662 0.068 Uiso 1 1 calc R . . H3B H 1.1991 0.6928 0.4710 0.068 Uiso 1 1 calc R . . H3C H 1.0570 0.6487 0.4046 0.068 Uiso 1 1 calc R . . C4 C 0.9553(4) 0.6686(3) 0.0395(2) 0.0590(12) Uani 1 1 d . . . H4A H 0.8883 0.6925 0.0441 0.089 Uiso 1 1 calc R . . H4B H 0.9364 0.6329 -0.0173 0.089 Uiso 1 1 calc R . . H4C H 1.0400 0.7139 0.0602 0.089 Uiso 1 1 calc R . . C5 C 0.9568(4) 0.6172(3) 0.0876(2) 0.0467(9) Uani 1 1 d . . . H5 H 1.0288 0.5962 0.0846 0.056 Uiso 1 1 calc R . . C6 C 0.8305(6) 0.5421(3) 0.0534(3) 0.0791(17) Uani 1 1 d . . . H6A H 0.8333 0.5109 0.0869 0.119 Uiso 1 1 calc R . . H6B H 0.8189 0.5057 -0.0019 0.119 Uiso 1 1 calc R . . H6C H 0.7580 0.5613 0.0532 0.119 Uiso 1 1 calc R . . C7 C 1.0780(3) 0.67226(19) 0.23146(19) 0.0296(7) Uani 1 1 d . . . C8 C 1.1800(3) 0.6386(2) 0.21281(18) 0.0296(7) Uani 1 1 d . . . C9 C 1.2859(3) 0.6898(2) 0.2044(2) 0.0384(8) Uani 1 1 d . . . H9 H 1.2917 0.7447 0.2113 0.046 Uiso 1 1 calc R . . C10 C 1.3839(4) 0.6631(2) 0.1863(2) 0.0434(9) Uani 1 1 d . . . H10 H 1.4540 0.6995 0.1801 0.052 Uiso 1 1 calc R . . C11 C 1.3797(3) 0.5842(2) 0.1775(2) 0.0367(8) Uani 1 1 d . . . H11 H 1.4472 0.5661 0.1662 0.044 Uiso 1 1 calc R . . C12 C 1.2749(3) 0.5319(2) 0.18527(18) 0.0292(7) Uani 1 1 d . . . C13 C 1.1771(3) 0.55975(19) 0.20236(18) 0.0286(6) Uani 1 1 d . . . C14 C 1.1206(3) 0.43138(19) 0.19552(17) 0.0260(6) Uani 1 1 d . . . C15 C 1.2379(3) 0.4476(2) 0.18083(18) 0.0282(6) Uani 1 1 d . . . C16 C 1.2926(3) 0.3869(2) 0.1666(2) 0.0353(7) Uani 1 1 d . . . H16 H 1.3723 0.3970 0.1565 0.042 Uiso 1 1 calc R . . C17 C 1.2288(3) 0.3118(2) 0.1673(2) 0.0382(8) Uani 1 1 d . . . H17 H 1.2649 0.2697 0.1577 0.046 Uiso 1 1 calc R . . C18 C 1.1111(3) 0.2967(2) 0.1820(2) 0.0365(8) Uani 1 1 d . . . H18 H 1.0688 0.2443 0.1818 0.044 Uiso 1 1 calc R . . C19 C 1.0543(3) 0.35649(19) 0.19688(18) 0.0281(6) Uani 1 1 d . . . C20 C 0.9298(3) 0.33727(18) 0.21476(18) 0.0268(6) Uani 1 1 d . . . C21 C 1.0516(4) 0.3461(3) 0.4128(2) 0.0501(10) Uani 1 1 d . . . H21A H 0.9860 0.3512 0.4384 0.075 Uiso 1 1 calc R . . H21B H 1.1376 0.3718 0.4545 0.075 Uiso 1 1 calc R . . H21C H 1.0336 0.2868 0.3816 0.075 Uiso 1 1 calc R . . C22 C 1.0480(3) 0.3897(2) 0.35746(18) 0.0333(7) Uani 1 1 d . . . H22 H 1.1211 0.3879 0.3363 0.040 Uiso 1 1 calc R . . C23 C 1.0683(5) 0.4804(2) 0.4012(3) 0.0657(13) Uani 1 1 d . . . H23A H 1.0648 0.5064 0.3632 0.099 Uiso 1 1 calc R . . H23B H 1.1531 0.5095 0.4442 0.099 Uiso 1 1 calc R . . H23C H 1.0001 0.4844 0.4248 0.099 Uiso 1 1 calc R . . C24 C 0.7682(4) 0.1935(3) 0.0220(2) 0.0548(11) Uani 1 1 d . . . H24A H 0.8363 0.1758 0.0440 0.082 Uiso 1 1 calc R . . H24B H 0.7609 0.1845 -0.0337 0.082 Uiso 1 1 calc R . . H24C H 0.6855 0.1607 0.0229 0.082 Uiso 1 1 calc R . . C25 C 0.8022(3) 0.2859(2) 0.0729(2) 0.0423(9) Uani 1 1 d . . . H25 H 0.8882 0.3179 0.0727 0.051 Uiso 1 1 calc R . . C26 C 0.7023(4) 0.3172(3) 0.0372(2) 0.0525(10) Uani 1 1 d . . . H26A H 0.6152 0.2811 0.0293 0.079 Uiso 1 1 calc R . . H26B H 0.7074 0.3158 -0.0148 0.079 Uiso 1 1 calc R . . H26C H 0.7202 0.3747 0.0743 0.079 Uiso 1 1 calc R . . C27 C 0.7146(3) 0.6893(2) 0.2099(2) 0.0429(9) Uani 1 1 d . . . H27A H 0.6894 0.6312 0.1698 0.064 Uiso 1 1 calc R . . H27B H 0.6754 0.6904 0.2523 0.064 Uiso 1 1 calc R . . C28 C 0.6924(3) 0.7463(2) 0.1733(2) 0.0383(8) Uani 1 1 d . . . C29 C 0.6916(4) 0.8243(2) 0.2207(2) 0.0427(9) Uani 1 1 d . . . H29 H 0.6938 0.8365 0.2746 0.051 Uiso 1 1 calc R . . C30 C 0.6875(4) 0.8841(2) 0.1908(2) 0.0475(9) Uani 1 1 d . . . H30 H 0.6885 0.9366 0.2245 0.057 Uiso 1 1 calc R . . C31 C 0.6821(4) 0.8672(3) 0.1124(2) 0.0549(11) Uani 1 1 d . . . H31 H 0.6801 0.9080 0.0918 0.066 Uiso 1 1 calc R . . C32 C 0.6795(4) 0.7898(3) 0.0638(2) 0.0561(11) Uani 1 1 d . . . H32 H 0.6737 0.7773 0.0093 0.067 Uiso 1 1 calc R . . C33 C 0.6854(4) 0.7307(3) 0.0936(2) 0.0494(10) Uani 1 1 d . . . H33 H 0.6847 0.6785 0.0594 0.059 Uiso 1 1 calc R . . C34 C 0.9534(4) 0.8216(3) 0.3933(2) 0.0461(9) Uani 1 1 d . . . H34A H 0.9524 0.7789 0.4149 0.069 Uiso 1 1 calc R . . H34B H 1.0390 0.8678 0.4228 0.069 Uiso 1 1 calc R . . C35 C 0.8518(4) 0.8546(2) 0.4098(2) 0.0416(9) Uani 1 1 d . . . C36 C 0.7389(5) 0.8049(3) 0.4129(2) 0.0557(11) Uani 1 1 d . . . H36 H 0.7303 0.7502 0.4085 0.067 Uiso 1 1 calc R . . C37 C 0.6384(5) 0.8319(3) 0.4224(3) 0.0601(12) Uani 1 1 d . . . H37 H 0.5620 0.7955 0.4232 0.072 Uiso 1 1 calc R . . C38 C 0.6488(5) 0.9109(3) 0.4306(2) 0.0575(11) Uani 1 1 d . . . H38 H 0.5801 0.9297 0.4369 0.069 Uiso 1 1 calc R . . C39 C 0.7616(4) 0.9633(3) 0.4294(2) 0.0506(10) Uani 1 1 d . . . H39 H 0.7703 1.0185 0.4358 0.061 Uiso 1 1 calc R . . C40 C 0.8621(4) 0.9355(2) 0.4190(2) 0.0424(8) Uani 1 1 d . . . H40 H 0.9383 0.9719 0.4181 0.051 Uiso 1 1 calc R . . C41 C 1.0104(3) 0.8807(2) 0.2426(2) 0.0369(8) Uani 1 1 d . . . H41A H 0.9705 0.8694 0.1855 0.055 Uiso 1 1 calc R . . H41B H 0.9854 0.9245 0.2762 0.055 Uiso 1 1 calc R . . C42 C 1.1536(3) 0.9128(2) 0.2644(2) 0.0324(7) Uani 1 1 d . . . C43 C 1.2352(4) 0.9700(2) 0.3427(2) 0.0394(8) Uani 1 1 d . . . H43 H 1.1984 0.9894 0.3827 0.047 Uiso 1 1 calc R . . C44 C 1.3682(4) 0.9987(2) 0.3628(2) 0.0457(9) Uani 1 1 d . . . H44 H 1.4214 1.0384 0.4161 0.055 Uiso 1 1 calc R . . C45 C 1.4250(4) 0.9706(2) 0.3068(2) 0.0453(9) Uani 1 1 d . . . H45 H 1.5166 0.9902 0.3214 0.054 Uiso 1 1 calc R . . C46 C 1.3475(4) 0.9138(2) 0.2294(2) 0.0457(9) Uani 1 1 d . . . H46 H 1.3854 0.8940 0.1901 0.055 Uiso 1 1 calc R . . C47 C 1.2133(4) 0.8854(2) 0.2089(2) 0.0397(8) Uani 1 1 d . . . H47 H 1.1608 0.8460 0.1553 0.048 Uiso 1 1 calc R . . C48 C 0.5366(3) 0.2933(2) 0.1841(2) 0.0323(7) Uani 1 1 d . . . H48A H 0.5109 0.3300 0.2250 0.048 Uiso 1 1 calc R . . H48B H 0.5432 0.3130 0.1414 0.048 Uiso 1 1 calc R . . C49 C 0.4587(3) 0.2031(2) 0.15295(19) 0.0310(7) Uani 1 1 d . . . C50 C 0.4605(3) 0.1442(2) 0.0821(2) 0.0385(8) Uani 1 1 d . . . H50 H 0.5042 0.1632 0.0502 0.046 Uiso 1 1 calc R . . C51 C 0.3999(4) 0.0592(2) 0.0580(2) 0.0471(9) Uani 1 1 d . . . H51 H 0.3998 0.0209 0.0089 0.056 Uiso 1 1 calc R . . C52 C 0.3397(4) 0.0294(2) 0.1044(2) 0.0446(9) Uani 1 1 d . . . H52 H 0.3005 -0.0291 0.0882 0.053 Uiso 1 1 calc R . . C53 C 0.3369(4) 0.0855(2) 0.1748(2) 0.0411(8) Uani 1 1 d . . . H53 H 0.2952 0.0653 0.2068 0.049 Uiso 1 1 calc R . . C54 C 0.3944(3) 0.1709(2) 0.1991(2) 0.0340(7) Uani 1 1 d . . . H54 H 0.3908 0.2086 0.2473 0.041 Uiso 1 1 calc R . . C55 C 0.7223(3) 0.3293(2) 0.3677(2) 0.0399(8) Uani 1 1 d . . . H55A H 0.7787 0.3115 0.4010 0.060 Uiso 1 1 calc R . . H55B H 0.7647 0.3905 0.3868 0.060 Uiso 1 1 calc R . . C56 C 0.5972(3) 0.3121(2) 0.38272(18) 0.0339(7) Uani 1 1 d . . . C57 C 0.5258(4) 0.3630(2) 0.3792(2) 0.0398(8) Uani 1 1 d . . . H57 H 0.5617 0.4119 0.3716 0.048 Uiso 1 1 calc R . . C58 C 0.4038(4) 0.3441(2) 0.3866(2) 0.0435(9) Uani 1 1 d . . . H58 H 0.3572 0.3796 0.3835 0.052 Uiso 1 1 calc R . . C59 C 0.3502(4) 0.2738(2) 0.3986(2) 0.0457(9) Uani 1 1 d . . . H59 H 0.2664 0.2603 0.4031 0.055 Uiso 1 1 calc R . . C60 C 0.4204(4) 0.2232(2) 0.4038(2) 0.0434(9) Uani 1 1 d . . . H60 H 0.3848 0.1750 0.4126 0.052 Uiso 1 1 calc R . . C61 C 0.5422(3) 0.2425(2) 0.39641(19) 0.0377(8) Uani 1 1 d . . . H61 H 0.5891 0.2075 0.4008 0.045 Uiso 1 1 calc R . . C62 C 0.6895(4) 0.1333(2) 0.2167(2) 0.0458(9) Uani 1 1 d . . . H62A H 0.6193 0.1107 0.2356 0.069 Uiso 1 1 calc R . . H62B H 0.6625 0.0988 0.1580 0.069 Uiso 1 1 calc R . . C63 C 0.8080(3) 0.12482(19) 0.2580(2) 0.0340(7) Uani 1 1 d . . . C64 C 0.9005(4) 0.1130(2) 0.2222(3) 0.0565(11) Uani 1 1 d . . . H64 H 0.8880 0.1097 0.1691 0.068 Uiso 1 1 calc R . . C65 C 1.0146(5) 0.1058(3) 0.2653(4) 0.0790(17) Uani 1 1 d . . . H65 H 1.0780 0.0971 0.2413 0.095 Uiso 1 1 calc R . . C66 C 1.0297(5) 0.1117(3) 0.3418(4) 0.0774(17) Uani 1 1 d . . . H66 H 1.1062 0.1087 0.3712 0.093 Uiso 1 1 calc R . . C67 C 0.9418(5) 0.1215(3) 0.3768(3) 0.0690(14) Uani 1 1 d . . . H67 H 0.9540 0.1233 0.4292 0.083 Uiso 1 1 calc R . . C68 C 0.8338(4) 0.1292(2) 0.3363(2) 0.0491(10) Uani 1 1 d . . . H68 H 0.7730 0.1378 0.3626 0.059 Uiso 1 1 calc R . . O2 O 0.6134(3) 0.54858(17) 0.33461(15) 0.0491(7) Uani 1 1 d . A -1 O3 O -0.0256(10) 0.0399(7) 0.0441(5) 0.064(3) Uani 0.35 1 d P B -1 O4 O 0(32) 0(32) 0(32) 0.051(3) Uani 0.30 2 d SP B -1 C69 C 0.7627(4) 0.5173(3) 0.2691(2) 0.0541(10) Uani 1 1 d . A -1 H69A H 0.8537 0.5240 0.2782 0.081 Uiso 1 1 calc R A -1 H69B H 0.7370 0.5438 0.2339 0.081 Uiso 1 1 calc R A -1 H69C H 0.7083 0.4576 0.2435 0.081 Uiso 1 1 calc R A -1 C70 C 0.7458(4) 0.5577(3) 0.3481(2) 0.0528(10) Uani 1 1 d . A -1 H70A H 0.7716 0.5312 0.3839 0.079 Uiso 1 1 calc R A -1 H70B H 0.8018 0.6179 0.3747 0.079 Uiso 1 1 calc R A -1 C71 C 0.5904(4) 0.5842(2) 0.4080(2) 0.0483(9) Uani 1 1 d . A -1 H71A H 0.6501 0.6434 0.4388 0.072 Uiso 1 1 calc R A -1 H71B H 0.6064 0.5535 0.4414 0.072 Uiso 1 1 calc R A -1 C72 C 0.4519(4) 0.5791(3) 0.3890(2) 0.0626(12) Uani 1 1 d . A -1 H72A H 0.4358 0.6039 0.4394 0.094 Uiso 1 1 calc R A -1 H72B H 0.3932 0.5204 0.3592 0.094 Uiso 1 1 calc R A -1 H72C H 0.4367 0.6098 0.3562 0.094 Uiso 1 1 calc R A -1 C73 C 0.0213(14) 0.1134(15) -0.0314(11) 0.090(6) Uani 0.50 1 d P B -1 C74 C 0.0595(15) 0.0724(11) 0.0134(10) 0.107(6) Uani 0.50 1 d P B -1 C75 C -0.0237(11) -0.0317(7) 0.0612(7) 0.071(3) Uani 0.50 1 d P B -1 C76 C -0.0716(17) -0.1177(14) 0.0075(15) 0.115(9) Uani 0.50 1 d P B -1 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 0.02508(16) 0.02917(17) 0.03168(17) 0.01455(14) 0.00825(13) 0.01001(13) Zr2 0.02397(16) 0.02751(16) 0.02940(16) 0.01411(13) 0.00834(13) 0.00930(13) N1 0.0286(14) 0.0343(15) 0.0311(14) 0.0143(12) 0.0059(11) 0.0145(12) N2 0.0375(16) 0.0385(16) 0.0280(14) 0.0115(12) 0.0058(12) 0.0175(13) N3 0.0274(14) 0.0336(15) 0.0258(13) 0.0119(12) 0.0062(11) 0.0089(12) N4 0.0272(14) 0.0398(16) 0.0279(14) 0.0142(12) 0.0090(11) 0.0082(12) O1 0.0242(11) 0.0269(11) 0.0337(11) 0.0148(9) 0.0132(9) 0.0111(9) C1 0.035(2) 0.042(2) 0.053(2) 0.0188(19) 0.0020(18) 0.0060(17) C2 0.0309(17) 0.0388(19) 0.0323(17) 0.0142(15) 0.0053(14) 0.0167(15) C3 0.043(2) 0.053(2) 0.045(2) 0.0288(19) 0.0092(17) 0.0183(19) C4 0.053(3) 0.071(3) 0.034(2) 0.020(2) 0.0125(19) 0.001(2) C5 0.047(2) 0.061(3) 0.0268(18) 0.0081(17) 0.0076(16) 0.029(2) C6 0.126(5) 0.039(2) 0.039(2) 0.006(2) 0.016(3) 0.002(3) C7 0.0291(16) 0.0267(16) 0.0333(17) 0.0138(14) 0.0101(14) 0.0100(13) C8 0.0306(17) 0.0316(17) 0.0297(16) 0.0149(14) 0.0120(13) 0.0122(14) C9 0.0367(19) 0.0324(18) 0.048(2) 0.0214(17) 0.0156(16) 0.0090(16) C10 0.0334(19) 0.042(2) 0.060(2) 0.0284(19) 0.0214(18) 0.0087(17) C11 0.0270(17) 0.040(2) 0.044(2) 0.0185(16) 0.0143(15) 0.0112(15) C12 0.0233(15) 0.0346(17) 0.0302(16) 0.0145(14) 0.0095(13) 0.0100(14) C13 0.0249(15) 0.0301(16) 0.0270(15) 0.0118(13) 0.0073(13) 0.0062(13) C14 0.0223(15) 0.0305(16) 0.0264(15) 0.0109(13) 0.0088(12) 0.0124(13) C15 0.0210(15) 0.0333(17) 0.0305(16) 0.0133(14) 0.0095(12) 0.0100(13) C16 0.0263(16) 0.043(2) 0.0398(19) 0.0171(16) 0.0124(14) 0.0169(15) C17 0.0334(18) 0.0343(19) 0.052(2) 0.0181(17) 0.0160(16) 0.0183(16) C18 0.0329(18) 0.0328(18) 0.047(2) 0.0183(16) 0.0156(16) 0.0142(15) C19 0.0243(15) 0.0284(16) 0.0324(16) 0.0133(13) 0.0106(13) 0.0097(13) C20 0.0244(15) 0.0212(15) 0.0354(17) 0.0125(13) 0.0116(13) 0.0077(12) C21 0.042(2) 0.051(2) 0.047(2) 0.0260(19) -0.0028(18) 0.0091(19) C22 0.0261(16) 0.0375(18) 0.0272(16) 0.0124(14) 0.0038(13) 0.0043(14) C23 0.065(3) 0.039(2) 0.056(3) 0.010(2) -0.013(2) 0.004(2) C24 0.056(3) 0.064(3) 0.034(2) 0.0079(19) 0.0160(19) 0.023(2) C25 0.0341(19) 0.057(2) 0.0291(18) 0.0177(17) 0.0118(15) 0.0069(18) C26 0.057(3) 0.059(3) 0.041(2) 0.031(2) 0.0117(19) 0.011(2) C27 0.0300(18) 0.039(2) 0.057(2) 0.0230(18) 0.0102(17) 0.0089(16) C28 0.0186(15) 0.048(2) 0.043(2) 0.0196(17) 0.0042(14) 0.0086(15) C29 0.037(2) 0.043(2) 0.039(2) 0.0174(17) 0.0042(16) 0.0072(17) C30 0.043(2) 0.042(2) 0.047(2) 0.0180(18) 0.0020(18) 0.0109(18) C31 0.050(3) 0.061(3) 0.050(2) 0.030(2) 0.005(2) 0.015(2) C32 0.054(3) 0.080(3) 0.042(2) 0.030(2) 0.015(2) 0.030(2) C33 0.042(2) 0.055(2) 0.048(2) 0.018(2) 0.0131(18) 0.021(2) C34 0.056(2) 0.065(3) 0.0353(19) 0.0264(19) 0.0195(18) 0.038(2) C35 0.052(2) 0.058(2) 0.0275(17) 0.0208(17) 0.0165(16) 0.034(2) C36 0.080(3) 0.072(3) 0.057(3) 0.046(2) 0.043(2) 0.049(3) C37 0.071(3) 0.082(3) 0.062(3) 0.045(3) 0.044(2) 0.042(3) C38 0.064(3) 0.084(3) 0.047(2) 0.031(2) 0.029(2) 0.047(3) C39 0.063(3) 0.051(2) 0.039(2) 0.0131(18) 0.0114(19) 0.035(2) C40 0.042(2) 0.047(2) 0.0322(18) 0.0101(16) 0.0075(16) 0.0200(18) C41 0.0324(18) 0.0355(18) 0.0399(19) 0.0195(16) 0.0073(15) 0.0077(15) C42 0.0294(17) 0.0284(16) 0.0405(19) 0.0204(15) 0.0087(14) 0.0071(14) C43 0.039(2) 0.0350(19) 0.046(2) 0.0192(17) 0.0143(17) 0.0134(16) C44 0.036(2) 0.040(2) 0.049(2) 0.0177(18) 0.0056(17) 0.0051(17) C45 0.0306(19) 0.049(2) 0.061(2) 0.034(2) 0.0104(18) 0.0124(17) C46 0.043(2) 0.047(2) 0.057(2) 0.030(2) 0.0240(19) 0.0158(19) C47 0.039(2) 0.0363(19) 0.042(2) 0.0181(16) 0.0136(16) 0.0093(16) C48 0.0286(17) 0.0369(18) 0.0393(18) 0.0224(15) 0.0136(14) 0.0140(15) C49 0.0231(15) 0.0373(18) 0.0325(17) 0.0163(15) 0.0043(13) 0.0133(14) C50 0.0350(19) 0.045(2) 0.0379(19) 0.0178(17) 0.0132(15) 0.0168(17) C51 0.051(2) 0.043(2) 0.038(2) 0.0078(17) 0.0126(18) 0.0190(19) C52 0.046(2) 0.0300(18) 0.049(2) 0.0112(17) 0.0127(18) 0.0111(17) C53 0.041(2) 0.036(2) 0.047(2) 0.0208(17) 0.0148(17) 0.0112(17) C54 0.0319(18) 0.0344(18) 0.0336(18) 0.0140(15) 0.0081(14) 0.0118(15) C55 0.0328(19) 0.050(2) 0.0366(19) 0.0185(17) 0.0145(15) 0.0119(17) C56 0.0318(18) 0.0389(19) 0.0236(16) 0.0091(14) 0.0082(13) 0.0081(15) C57 0.043(2) 0.0345(19) 0.0379(19) 0.0115(16) 0.0181(16) 0.0095(16) C58 0.041(2) 0.047(2) 0.043(2) 0.0111(18) 0.0203(17) 0.0215(18) C59 0.034(2) 0.052(2) 0.041(2) 0.0123(18) 0.0154(16) 0.0075(18) C60 0.046(2) 0.044(2) 0.0370(19) 0.0181(17) 0.0163(17) 0.0079(18) C61 0.0369(19) 0.046(2) 0.0322(18) 0.0185(16) 0.0112(15) 0.0161(17) C62 0.036(2) 0.036(2) 0.062(2) 0.0262(19) 0.0033(18) 0.0124(17) C63 0.0332(18) 0.0230(16) 0.0424(19) 0.0132(14) 0.0075(15) 0.0103(14) C64 0.068(3) 0.045(2) 0.085(3) 0.038(2) 0.049(3) 0.029(2) C65 0.052(3) 0.051(3) 0.154(6) 0.047(3) 0.056(3) 0.027(2) C66 0.048(3) 0.052(3) 0.129(5) 0.053(3) 0.003(3) 0.014(2) C67 0.065(3) 0.048(3) 0.078(3) 0.033(2) -0.007(3) 0.013(2) C68 0.058(3) 0.036(2) 0.053(2) 0.0215(19) 0.012(2) 0.0192(19) O2 0.0501(17) 0.0521(16) 0.0355(14) 0.0137(12) 0.0098(12) 0.0146(14) O3 0.080(7) 0.080(7) 0.048(5) 0.025(5) 0.037(5) 0.042(6) O4 0.044(8) 0.049(9) 0.036(8) 0.004(7) 0.006(6) 0.008(7) C69 0.063(3) 0.045(2) 0.057(3) 0.023(2) 0.023(2) 0.019(2) C70 0.050(3) 0.039(2) 0.055(2) 0.0131(19) 0.013(2) 0.0087(19) C71 0.054(2) 0.042(2) 0.037(2) 0.0101(17) 0.0095(18) 0.0118(19) C72 0.055(3) 0.075(3) 0.040(2) 0.011(2) 0.010(2) 0.022(2) C73 0.056(9) 0.161(17) 0.117(12) 0.109(13) 0.057(9) 0.049(10) C74 0.083(10) 0.087(11) 0.093(11) 0.042(9) -0.023(8) -0.014(9) C75 0.075(7) 0.067(7) 0.086(8) 0.041(6) 0.033(6) 0.031(6) C76 0.063(11) 0.082(11) 0.16(2) -0.002(11) 0.056(12) 0.024(10) _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 N2 2.230(3) . ? Zr1 C41 2.257(3) . ? Zr1 N1 2.267(3) . ? Zr1 C27 2.268(4) . ? Zr1 C34 2.292(3) . ? Zr1 C7 2.664(3) . ? Zr1 C28 2.721(3) . ? Zr2 N4 2.231(3) . ? Zr2 N3 2.267(3) . ? Zr2 C62 2.269(4) . ? Zr2 C55 2.282(3) . ? Zr2 C48 2.286(3) . ? Zr2 C20 2.658(3) . ? Zr2 C49 2.682(3) . ? N1 C7 1.319(4) . ? N1 C2 1.477(4) . ? N2 C7 1.340(4) . ? N2 C5 1.473(4) . ? N3 C20 1.321(4) . ? N3 C22 1.474(4) . ? N4 C20 1.337(4) . ? N4 C25 1.472(4) . ? O1 C14 1.390(3) . ? O1 C13 1.391(4) . ? C1 C2 1.518(5) . ? C2 C3 1.527(5) . ? C4 C5 1.505(6) . ? C5 C6 1.521(6) . ? C7 C8 1.505(4) . ? C8 C13 1.378(4) . ? C8 C9 1.390(4) . ? C9 C10 1.394(5) . ? C10 C11 1.382(5) . ? C11 C12 1.386(4) . ? C12 C13 1.398(4) . ? C12 C15 1.451(4) . ? C14 C19 1.387(4) . ? C14 C15 1.397(4) . ? C15 C16 1.391(4) . ? C16 C17 1.376(5) . ? C17 C18 1.402(5) . ? C18 C19 1.392(4) . ? C19 C20 1.506(4) . ? C21 C22 1.506(5) . ? C22 C23 1.507(5) . ? C24 C25 1.520(5) . ? C25 C26 1.530(5) . ? C27 C28 1.470(5) . ? C28 C33 1.401(5) . ? C28 C29 1.408(5) . ? C29 C30 1.391(5) . ? C30 C31 1.379(5) . ? C31 C32 1.390(6) . ? C32 C33 1.381(6) . ? C34 C35 1.484(5) . ? C35 C36 1.389(6) . ? C35 C40 1.398(5) . ? C36 C37 1.385(6) . ? C37 C38 1.369(6) . ? C38 C39 1.392(6) . ? C39 C40 1.396(5) . ? C41 C42 1.486(5) . ? C42 C47 1.390(5) . ? C42 C43 1.398(5) . ? C43 C44 1.381(5) . ? C44 C45 1.375(5) . ? C45 C46 1.376(5) . ? C46 C47 1.393(5) . ? C48 C49 1.480(5) . ? C49 C50 1.407(5) . ? C49 C54 1.419(4) . ? C50 C51 1.381(5) . ? C51 C52 1.379(5) . ? C52 C53 1.385(5) . ? C53 C54 1.385(5) . ? C55 C56 1.485(5) . ? C56 C61 1.393(5) . ? C56 C57 1.397(5) . ? C57 C58 1.390(5) . ? C58 C59 1.381(5) . ? C59 C60 1.387(5) . ? C60 C61 1.387(5) . ? C62 C63 1.476(5) . ? C63 C64 1.393(5) . ? C63 C68 1.400(5) . ? C64 C65 1.437(7) . ? C65 C66 1.368(8) . ? C66 C67 1.329(7) . ? C67 C68 1.364(6) . ? O2 C71 1.423(4) . ? O2 C70 1.428(5) . ? O3 O4 1(10) . ? O3 C74 1.337(17) . ? O3 C75 1.452(14) . ? O4 C74 1(10) . ? O4 C75 1(10) . ? C69 C70 1.494(5) . ? C71 C72 1.510(6) . ? C73 C74 1.37(2) . ? C75 C76 1.42(2) . ? 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 N2 Zr1 C41 104.66(12) . . ? N2 Zr1 N1 59.52(10) . . ? C41 Zr1 N1 114.81(12) . . ? N2 Zr1 C27 96.03(13) . . ? C41 Zr1 C27 119.78(13) . . ? N1 Zr1 C27 124.36(12) . . ? N2 Zr1 C34 141.23(11) . . ? C41 Zr1 C34 99.29(14) . . ? N1 Zr1 C34 82.91(12) . . ? C27 Zr1 C34 97.96(15) . . ? N2 Zr1 C7 30.15(10) . . ? C41 Zr1 C7 109.76(11) . . ? N1 Zr1 C7 29.67(9) . . ? C27 Zr1 C7 115.51(12) . . ? C34 Zr1 C7 112.52(12) . . ? N2 Zr1 C28 104.16(11) . . ? C41 Zr1 C28 87.14(12) . . ? N1 Zr1 C28 154.59(11) . . ? C27 Zr1 C28 32.70(12) . . ? C34 Zr1 C28 107.08(13) . . ? C7 Zr1 C28 133.01(11) . . ? N4 Zr2 N3 59.65(10) . . ? N4 Zr2 C62 108.40(13) . . ? N3 Zr2 C62 109.10(12) . . ? N4 Zr2 C55 136.89(12) . . ? N3 Zr2 C55 83.87(12) . . ? C62 Zr2 C55 104.58(15) . . ? N4 Zr2 C48 93.03(11) . . ? N3 Zr2 C48 130.44(11) . . ? C62 Zr2 C48 119.04(13) . . ? C55 Zr2 C48 94.55(13) . . ? N4 Zr2 C20 30.15(9) . . ? N3 Zr2 C20 29.79(9) . . ? C62 Zr2 C20 108.66(12) . . ? C55 Zr2 C20 112.20(12) . . ? C48 Zr2 C20 116.29(10) . . ? N4 Zr2 C49 105.93(10) . . ? N3 Zr2 C49 161.64(10) . . ? C62 Zr2 C49 85.59(12) . . ? C55 Zr2 C49 103.51(12) . . ? C48 Zr2 C49 33.46(11) . . ? C20 Zr2 C49 135.84(10) . . ? C7 N1 C2 120.0(3) . . ? C7 N1 Zr1 92.04(19) . . ? C2 N1 Zr1 146.0(2) . . ? C7 N2 C5 120.6(3) . . ? C7 N2 Zr1 93.1(2) . . ? C5 N2 Zr1 145.9(2) . . ? C20 N3 C22 120.2(3) . . ? C20 N3 Zr2 91.71(19) . . ? C22 N3 Zr2 147.3(2) . . ? C20 N4 C25 120.5(3) . . ? C20 N4 Zr2 92.89(18) . . ? C25 N4 Zr2 145.3(2) . . ? C14 O1 C13 105.3(2) . . ? N1 C2 C1 111.0(3) . . ? N1 C2 C3 111.1(3) . . ? C1 C2 C3 111.5(3) . . ? N2 C5 C4 111.2(3) . . ? N2 C5 C6 109.7(3) . . ? C4 C5 C6 111.3(3) . . ? N1 C7 N2 114.2(3) . . ? N1 C7 C8 123.8(3) . . ? N2 C7 C8 121.7(3) . . ? N1 C7 Zr1 58.29(16) . . ? N2 C7 Zr1 56.72(17) . . ? C8 C7 Zr1 166.1(2) . . ? C13 C8 C9 116.3(3) . . ? C13 C8 C7 125.2(3) . . ? C9 C8 C7 118.5(3) . . ? C8 C9 C10 122.2(3) . . ? C11 C10 C9 120.4(3) . . ? C10 C11 C12 118.5(3) . . ? C11 C12 C13 119.9(3) . . ? C11 C12 C15 134.3(3) . . ? C13 C12 C15 105.8(3) . . ? C8 C13 O1 125.7(3) . . ? C8 C13 C12 122.7(3) . . ? O1 C13 C12 111.5(3) . . ? C19 C14 O1 125.4(3) . . ? C19 C14 C15 123.0(3) . . ? O1 C14 C15 111.6(3) . . ? C16 C15 C14 119.7(3) . . ? C16 C15 C12 134.6(3) . . ? C14 C15 C12 105.8(3) . . ? C17 C16 C15 118.6(3) . . ? C16 C17 C18 120.8(3) . . ? C19 C18 C17 121.9(3) . . ? C14 C19 C18 116.0(3) . . ? C14 C19 C20 124.8(3) . . ? C18 C19 C20 119.2(3) . . ? N3 C20 N4 114.7(3) . . ? N3 C20 C19 122.5(3) . . ? N4 C20 C19 122.5(3) . . ? N3 C20 Zr2 58.49(16) . . ? N4 C20 Zr2 56.96(15) . . ? C19 C20 Zr2 166.1(2) . . ? N3 C22 C21 112.1(3) . . ? N3 C22 C23 110.0(3) . . ? C21 C22 C23 112.0(3) . . ? N4 C25 C24 110.5(3) . . ? N4 C25 C26 110.9(3) . . ? C24 C25 C26 111.0(3) . . ? C28 C27 Zr1 90.9(2) . . ? C33 C28 C29 116.7(3) . . ? C33 C28 C27 122.6(4) . . ? C29 C28 C27 120.3(3) . . ? C33 C28 Zr1 109.5(2) . . ? C29 C28 Zr1 98.8(2) . . ? C27 C28 Zr1 56.45(18) . . ? C30 C29 C28 121.9(4) . . ? C31 C30 C29 120.0(4) . . ? C30 C31 C32 119.2(4) . . ? C33 C32 C31 120.9(4) . . ? C32 C33 C28 121.3(4) . . ? C35 C34 Zr1 114.6(2) . . ? C36 C35 C40 116.8(4) . . ? C36 C35 C34 121.3(4) . . ? C40 C35 C34 121.8(4) . . ? C37 C36 C35 122.6(4) . . ? C38 C37 C36 120.1(4) . . ? C37 C38 C39 119.0(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C35 120.8(4) . . ? C42 C41 Zr1 113.2(2) . . ? C47 C42 C43 116.7(3) . . ? C47 C42 C41 121.7(3) . . ? C43 C42 C41 121.5(3) . . ? C44 C43 C42 121.2(3) . . ? C45 C44 C43 121.0(4) . . ? C44 C45 C46 119.3(4) . . ? C45 C46 C47 119.8(4) . . ? C42 C47 C46 122.0(4) . . ? C49 C48 Zr2 88.11(19) . . ? C50 C49 C54 116.8(3) . . ? C50 C49 C48 121.3(3) . . ? C54 C49 C48 121.3(3) . . ? C50 C49 Zr2 98.2(2) . . ? C54 C49 Zr2 106.5(2) . . ? C48 C49 Zr2 58.43(16) . . ? C51 C50 C49 121.3(3) . . ? C52 C51 C50 120.9(3) . . ? C51 C52 C53 119.4(3) . . ? C54 C53 C52 120.6(3) . . ? C53 C54 C49 121.0(3) . . ? C56 C55 Zr2 116.7(2) . . ? C61 C56 C57 116.9(3) . . ? C61 C56 C55 121.9(3) . . ? C57 C56 C55 121.1(3) . . ? C58 C57 C56 121.8(3) . . ? C59 C58 C57 120.1(4) . . ? C58 C59 C60 119.1(3) . . ? C61 C60 C59 120.5(3) . . ? C60 C61 C56 121.6(3) . . ? C63 C62 Zr2 114.0(2) . . ? C64 C63 C68 116.4(4) . . ? C64 C63 C62 122.3(4) . . ? C68 C63 C62 121.3(3) . . ? C63 C64 C65 120.1(4) . . ? C66 C65 C64 118.2(4) . . ? C67 C66 C65 122.8(5) . . ? C66 C67 C68 119.1(5) . . ? C67 C68 C63 123.4(4) . . ? C71 O2 C70 112.0(3) . . ? O4 O3 C74 60(10) . . ? O4 O3 C75 71(10) . . ? C74 O3 C75 120.6(12) . . ? O3 O4 C74 71(10) . . ? O3 O4 C75 67(10) . . ? C74 O4 C75 126(10) . . ? O2 C70 C69 109.3(3) . . ? O2 C71 C72 109.3(3) . . ? O4 C74 O3 48(10) . . ? O4 C74 C73 125(10) . . ? O3 C74 C73 116.3(14) . . ? C76 C75 O3 129.4(17) . . ? C76 C75 O4 95(10) . . ? O3 C75 O4 42(10) . . ? 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 N2 Zr1 N1 C7 6.34(18) . . . . ? C41 Zr1 N1 C7 -86.6(2) . . . . ? C27 Zr1 N1 C7 81.6(2) . . . . ? C34 Zr1 N1 C7 176.4(2) . . . . ? C28 Zr1 N1 C7 61.1(3) . . . . ? N2 Zr1 N1 C2 167.6(4) . . . . ? C41 Zr1 N1 C2 74.7(4) . . . . ? C27 Zr1 N1 C2 -117.1(4) . . . . ? C34 Zr1 N1 C2 -22.3(4) . . . . ? C7 Zr1 N1 C2 161.3(5) . . . . ? C28 Zr1 N1 C2 -137.6(4) . . . . ? C41 Zr1 N2 C7 104.2(2) . . . . ? N1 Zr1 N2 C7 -6.25(18) . . . . ? C27 Zr1 N2 C7 -132.9(2) . . . . ? C34 Zr1 N2 C7 -22.1(3) . . . . ? C28 Zr1 N2 C7 -165.07(19) . . . . ? C41 Zr1 N2 C5 -67.4(5) . . . . ? N1 Zr1 N2 C5 -177.8(5) . . . . ? C27 Zr1 N2 C5 55.6(5) . . . . ? C34 Zr1 N2 C5 166.3(4) . . . . ? C7 Zr1 N2 C5 -171.6(6) . . . . ? C28 Zr1 N2 C5 23.3(5) . . . . ? N4 Zr2 N3 C20 -6.23(17) . . . . ? C62 Zr2 N3 C20 94.4(2) . . . . ? C55 Zr2 N3 C20 -162.3(2) . . . . ? C48 Zr2 N3 C20 -71.5(2) . . . . ? C49 Zr2 N3 C20 -47.3(4) . . . . ? N4 Zr2 N3 C22 -174.4(4) . . . . ? C62 Zr2 N3 C22 -73.8(4) . . . . ? C55 Zr2 N3 C22 29.5(4) . . . . ? C48 Zr2 N3 C22 120.3(4) . . . . ? C20 Zr2 N3 C22 -168.2(5) . . . . ? C49 Zr2 N3 C22 144.5(4) . . . . ? N3 Zr2 N4 C20 6.17(17) . . . . ? C62 Zr2 N4 C20 -95.6(2) . . . . ? C55 Zr2 N4 C20 42.4(3) . . . . ? C48 Zr2 N4 C20 142.4(2) . . . . ? C49 Zr2 N4 C20 173.75(18) . . . . ? N3 Zr2 N4 C25 170.8(4) . . . . ? C62 Zr2 N4 C25 69.0(4) . . . . ? C55 Zr2 N4 C25 -153.0(4) . . . . ? C48 Zr2 N4 C25 -53.0(4) . . . . ? C20 Zr2 N4 C25 164.6(5) . . . . ? C49 Zr2 N4 C25 -21.6(4) . . . . ? C7 N1 C2 C1 107.0(4) . . . . ? Zr1 N1 C2 C1 -51.3(5) . . . . ? C7 N1 C2 C3 -128.2(3) . . . . ? Zr1 N1 C2 C3 73.5(5) . . . . ? C7 N2 C5 C4 -125.3(4) . . . . ? Zr1 N2 C5 C4 44.9(6) . . . . ? C7 N2 C5 C6 111.0(4) . . . . ? Zr1 N2 C5 C6 -78.7(5) . . . . ? C2 N1 C7 N2 -178.1(3) . . . . ? Zr1 N1 C7 N2 -10.0(3) . . . . ? C2 N1 C7 C8 -4.4(5) . . . . ? Zr1 N1 C7 C8 163.7(3) . . . . ? C2 N1 C7 Zr1 -168.1(3) . . . . ? C5 N2 C7 N1 -175.3(3) . . . . ? Zr1 N2 C7 N1 10.2(3) . . . . ? C5 N2 C7 C8 10.9(5) . . . . ? Zr1 N2 C7 C8 -163.6(3) . . . . ? C5 N2 C7 Zr1 174.5(4) . . . . ? N2 Zr1 C7 N1 -169.1(3) . . . . ? C41 Zr1 C7 N1 105.7(2) . . . . ? C27 Zr1 C7 N1 -115.2(2) . . . . ? C34 Zr1 C7 N1 -3.9(2) . . . . ? C28 Zr1 C7 N1 -149.10(19) . . . . ? C41 Zr1 C7 N2 -85.2(2) . . . . ? N1 Zr1 C7 N2 169.1(3) . . . . ? C27 Zr1 C7 N2 53.9(2) . . . . ? C34 Zr1 C7 N2 165.2(2) . . . . ? C28 Zr1 C7 N2 20.0(3) . . . . ? N2 Zr1 C7 C8 87.8(9) . . . . ? C41 Zr1 C7 C8 2.6(9) . . . . ? N1 Zr1 C7 C8 -103.1(10) . . . . ? C27 Zr1 C7 C8 141.7(9) . . . . ? C34 Zr1 C7 C8 -107.0(9) . . . . ? C28 Zr1 C7 C8 107.8(9) . . . . ? N1 C7 C8 C13 92.4(4) . . . . ? N2 C7 C8 C13 -94.3(4) . . . . ? Zr1 C7 C8 C13 -173.4(7) . . . . ? N1 C7 C8 C9 -88.2(4) . . . . ? N2 C7 C8 C9 85.0(4) . . . . ? Zr1 C7 C8 C9 6.0(11) . . . . ? C13 C8 C9 C10 0.1(5) . . . . ? C7 C8 C9 C10 -179.3(3) . . . . ? C8 C9 C10 C11 -1.2(6) . . . . ? C9 C10 C11 C12 1.3(5) . . . . ? C10 C11 C12 C13 -0.4(5) . . . . ? C10 C11 C12 C15 -179.4(3) . . . . ? C9 C8 C13 O1 179.4(3) . . . . ? C7 C8 C13 O1 -1.2(5) . . . . ? C9 C8 C13 C12 0.8(5) . . . . ? C7 C8 C13 C12 -179.8(3) . . . . ? C14 O1 C13 C8 -178.5(3) . . . . ? C14 O1 C13 C12 0.3(3) . . . . ? C11 C12 C13 C8 -0.6(5) . . . . ? C15 C12 C13 C8 178.6(3) . . . . ? C11 C12 C13 O1 -179.4(3) . . . . ? C15 C12 C13 O1 -0.2(3) . . . . ? C13 O1 C14 C19 179.4(3) . . . . ? C13 O1 C14 C15 -0.3(3) . . . . ? C19 C14 C15 C16 0.1(5) . . . . ? O1 C14 C15 C16 179.8(3) . . . . ? C19 C14 C15 C12 -179.5(3) . . . . ? O1 C14 C15 C12 0.1(3) . . . . ? C11 C12 C15 C16 -0.5(6) . . . . ? C13 C12 C15 C16 -179.6(3) . . . . ? C11 C12 C15 C14 179.1(4) . . . . ? C13 C12 C15 C14 0.0(3) . . . . ? C14 C15 C16 C17 0.1(5) . . . . ? C12 C15 C16 C17 179.6(3) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? O1 C14 C19 C18 179.9(3) . . . . ? C15 C14 C19 C18 -0.4(5) . . . . ? O1 C14 C19 C20 -1.4(5) . . . . ? C15 C14 C19 C20 178.2(3) . . . . ? C17 C18 C19 C14 0.5(5) . . . . ? C17 C18 C19 C20 -178.2(3) . . . . ? C22 N3 C20 N4 -177.4(3) . . . . ? Zr2 N3 C20 N4 9.9(3) . . . . ? C22 N3 C20 C19 9.0(4) . . . . ? Zr2 N3 C20 C19 -163.6(2) . . . . ? C22 N3 C20 Zr2 172.6(3) . . . . ? C25 N4 C20 N3 -180.0(3) . . . . ? Zr2 N4 C20 N3 -10.1(3) . . . . ? C25 N4 C20 C19 -6.4(5) . . . . ? Zr2 N4 C20 C19 163.5(2) . . . . ? C25 N4 C20 Zr2 -169.9(3) . . . . ? C14 C19 C20 N3 -95.6(4) . . . . ? C18 C19 C20 N3 83.0(4) . . . . ? C14 C19 C20 N4 91.4(4) . . . . ? C18 C19 C20 N4 -90.0(4) . . . . ? C14 C19 C20 Zr2 174.6(7) . . . . ? C18 C19 C20 Zr2 -6.8(11) . . . . ? N4 Zr2 C20 N3 169.2(3) . . . . ? C62 Zr2 C20 N3 -96.0(2) . . . . ? C55 Zr2 C20 N3 19.1(2) . . . . ? C48 Zr2 C20 N3 126.38(19) . . . . ? C49 Zr2 C20 N3 160.60(18) . . . . ? N3 Zr2 C20 N4 -169.2(3) . . . . ? C62 Zr2 C20 N4 94.7(2) . . . . ? C55 Zr2 C20 N4 -150.2(2) . . . . ? C48 Zr2 C20 N4 -42.9(2) . . . . ? C49 Zr2 C20 N4 -8.6(2) . . . . ? N4 Zr2 C20 C19 -92.2(9) . . . . ? N3 Zr2 C20 C19 98.5(9) . . . . ? C62 Zr2 C20 C19 2.5(9) . . . . ? C55 Zr2 C20 C19 117.6(9) . . . . ? C48 Zr2 C20 C19 -135.1(9) . . . . ? C49 Zr2 C20 C19 -100.9(9) . . . . ? C20 N3 C22 C21 -137.6(3) . . . . ? Zr2 N3 C22 C21 28.7(5) . . . . ? C20 N3 C22 C23 97.1(4) . . . . ? Zr2 N3 C22 C23 -96.6(4) . . . . ? C20 N4 C25 C24 105.7(4) . . . . ? Zr2 N4 C25 C24 -56.5(5) . . . . ? C20 N4 C25 C26 -130.8(3) . . . . ? Zr2 N4 C25 C26 67.0(5) . . . . ? N2 Zr1 C27 C28 -106.9(2) . . . . ? C41 Zr1 C27 C28 3.8(3) . . . . ? N1 Zr1 C27 C28 -163.83(19) . . . . ? C34 Zr1 C27 C28 109.3(2) . . . . ? C7 Zr1 C27 C28 -131.0(2) . . . . ? Zr1 C27 C28 C33 92.9(3) . . . . ? Zr1 C27 C28 C29 -80.0(3) . . . . ? N2 Zr1 C28 C33 -37.9(3) . . . . ? C41 Zr1 C28 C33 66.5(3) . . . . ? N1 Zr1 C28 C33 -84.5(4) . . . . ? C27 Zr1 C28 C33 -116.8(4) . . . . ? C34 Zr1 C28 C33 165.3(3) . . . . ? C7 Zr1 C28 C33 -48.1(3) . . . . ? N2 Zr1 C28 C29 -160.4(2) . . . . ? C41 Zr1 C28 C29 -56.0(2) . . . . ? N1 Zr1 C28 C29 153.1(2) . . . . ? C27 Zr1 C28 C29 120.7(3) . . . . ? C34 Zr1 C28 C29 42.8(3) . . . . ? C7 Zr1 C28 C29 -170.6(2) . . . . ? N2 Zr1 C28 C27 78.9(2) . . . . ? C41 Zr1 C28 C27 -176.7(2) . . . . ? N1 Zr1 C28 C27 32.4(4) . . . . ? C34 Zr1 C28 C27 -77.8(3) . . . . ? C7 Zr1 C28 C27 68.7(3) . . . . ? C33 C28 C29 C30 -1.7(5) . . . . ? C27 C28 C29 C30 171.6(3) . . . . ? Zr1 C28 C29 C30 115.5(3) . . . . ? C28 C29 C30 C31 1.0(6) . . . . ? C29 C30 C31 C32 0.6(6) . . . . ? C30 C31 C32 C33 -1.5(7) . . . . ? C31 C32 C33 C28 0.9(7) . . . . ? C29 C28 C33 C32 0.7(6) . . . . ? C27 C28 C33 C32 -172.4(4) . . . . ? Zr1 C28 C33 C32 -110.4(4) . . . . ? N2 Zr1 C34 C35 -153.7(2) . . . . ? C41 Zr1 C34 C35 78.4(3) . . . . ? N1 Zr1 C34 C35 -167.5(3) . . . . ? C27 Zr1 C34 C35 -43.6(3) . . . . ? C7 Zr1 C34 C35 -165.6(3) . . . . ? C28 Zr1 C34 C35 -11.4(3) . . . . ? Zr1 C34 C35 C36 90.9(4) . . . . ? Zr1 C34 C35 C40 -86.0(4) . . . . ? C40 C35 C36 C37 1.8(6) . . . . ? C34 C35 C36 C37 -175.2(4) . . . . ? C35 C36 C37 C38 -1.2(6) . . . . ? C36 C37 C38 C39 -0.2(6) . . . . ? C37 C38 C39 C40 0.9(6) . . . . ? C38 C39 C40 C35 -0.3(5) . . . . ? C36 C35 C40 C39 -1.0(5) . . . . ? C34 C35 C40 C39 176.0(3) . . . . ? N2 Zr1 C41 C42 -63.2(3) . . . . ? N1 Zr1 C41 C42 -0.4(3) . . . . ? C27 Zr1 C41 C42 -169.2(2) . . . . ? C34 Zr1 C41 C42 86.0(3) . . . . ? C7 Zr1 C41 C42 -32.1(3) . . . . ? C28 Zr1 C41 C42 -167.1(3) . . . . ? Zr1 C41 C42 C47 87.5(3) . . . . ? Zr1 C41 C42 C43 -90.3(3) . . . . ? C47 C42 C43 C44 1.3(5) . . . . ? C41 C42 C43 C44 179.2(3) . . . . ? C42 C43 C44 C45 -1.4(6) . . . . ? C43 C44 C45 C46 0.8(6) . . . . ? C44 C45 C46 C47 -0.2(5) . . . . ? C43 C42 C47 C46 -0.7(5) . . . . ? C41 C42 C47 C46 -178.6(3) . . . . ? C45 C46 C47 C42 0.2(5) . . . . ? N4 Zr2 C48 C49 114.72(19) . . . . ? N3 Zr2 C48 C49 166.44(16) . . . . ? C62 Zr2 C48 C49 1.7(2) . . . . ? C55 Zr2 C48 C49 -107.7(2) . . . . ? C20 Zr2 C48 C49 134.73(18) . . . . ? Zr2 C48 C49 C50 -79.8(3) . . . . ? Zr2 C48 C49 C54 90.9(3) . . . . ? N4 Zr2 C49 C50 51.2(2) . . . . ? N3 Zr2 C49 C50 87.3(4) . . . . ? C62 Zr2 C49 C50 -56.7(2) . . . . ? C55 Zr2 C49 C50 -160.6(2) . . . . ? C48 Zr2 C49 C50 121.8(3) . . . . ? C20 Zr2 C49 C50 55.7(3) . . . . ? N4 Zr2 C49 C54 172.4(2) . . . . ? N3 Zr2 C49 C54 -151.5(3) . . . . ? C62 Zr2 C49 C54 64.5(2) . . . . ? C55 Zr2 C49 C54 -39.4(2) . . . . ? C48 Zr2 C49 C54 -117.0(3) . . . . ? C20 Zr2 C49 C54 176.90(19) . . . . ? N4 Zr2 C49 C48 -70.6(2) . . . . ? N3 Zr2 C49 C48 -34.5(4) . . . . ? C62 Zr2 C49 C48 -178.5(2) . . . . ? C55 Zr2 C49 C48 77.5(2) . . . . ? C20 Zr2 C49 C48 -66.1(2) . . . . ? C54 C49 C50 C51 1.4(5) . . . . ? C48 C49 C50 C51 172.4(3) . . . . ? Zr2 C49 C50 C51 114.6(3) . . . . ? C49 C50 C51 C52 -2.4(6) . . . . ? C50 C51 C52 C53 1.8(6) . . . . ? C51 C52 C53 C54 -0.3(6) . . . . ? C52 C53 C54 C49 -0.7(5) . . . . ? C50 C49 C54 C53 0.1(5) . . . . ? C48 C49 C54 C53 -170.9(3) . . . . ? Zr2 C49 C54 C53 -108.3(3) . . . . ? N4 Zr2 C55 C56 141.9(2) . . . . ? N3 Zr2 C55 C56 172.7(3) . . . . ? C62 Zr2 C55 C56 -79.1(3) . . . . ? C48 Zr2 C55 C56 42.5(3) . . . . ? C20 Zr2 C55 C56 163.3(2) . . . . ? C49 Zr2 C55 C56 9.8(3) . . . . ? Zr2 C55 C56 C61 86.5(4) . . . . ? Zr2 C55 C56 C57 -89.9(4) . . . . ? C61 C56 C57 C58 -1.9(5) . . . . ? C55 C56 C57 C58 174.7(3) . . . . ? C56 C57 C58 C59 0.6(5) . . . . ? C57 C58 C59 C60 0.6(5) . . . . ? C58 C59 C60 C61 -0.6(5) . . . . ? C59 C60 C61 C56 -0.7(5) . . . . ? C57 C56 C61 C60 1.9(5) . . . . ? C55 C56 C61 C60 -174.6(3) . . . . ? N4 Zr2 C62 C63 79.0(3) . . . . ? N3 Zr2 C62 C63 15.7(3) . . . . ? C55 Zr2 C62 C63 -72.8(3) . . . . ? C48 Zr2 C62 C63 -176.6(2) . . . . ? C20 Zr2 C62 C63 47.2(3) . . . . ? C49 Zr2 C62 C63 -175.6(3) . . . . ? Zr2 C62 C63 C64 -89.1(4) . . . . ? Zr2 C62 C63 C68 90.3(4) . . . . ? C68 C63 C64 C65 0.1(5) . . . . ? C62 C63 C64 C65 179.5(4) . . . . ? C63 C64 C65 C66 -0.7(6) . . . . ? C64 C65 C66 C67 1.9(7) . . . . ? C65 C66 C67 C68 -2.5(7) . . . . ? C66 C67 C68 C63 1.9(7) . . . . ? C64 C63 C68 C67 -0.7(6) . . . . ? C62 C63 C68 C67 179.9(4) . . . . ? C75 O3 O4 C74 -145(100) . . . . ? C74 O3 O4 C75 145(100) . . . . ? C71 O2 C70 C69 178.6(3) . . . . ? C70 O2 C71 C72 175.1(3) . . . . ? C75 O4 C74 O3 -41(100) . . . . ? O3 O4 C74 C73 -96(100) . . . . ? C75 O4 C74 C73 -137(100) . . . . ? C75 O3 C74 O4 39(100) . . . . ? O4 O3 C74 C73 114(100) . . . . ? C75 O3 C74 C73 153.5(18) . . . . ? O4 O3 C75 C76 -43(100) . . . . ? C74 O3 C75 C76 -77.9(17) . . . . ? C74 O3 C75 O4 -35(100) . . . . ? O3 O4 C75 C76 148(100) . . . . ? C74 O4 C75 C76 -169(100) . . . . ? C74 O4 C75 O3 42(100) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 31.52 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.575 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.086 #===END data_jrh013 _database_code_CSD 170219 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (iPr4Xan)Zr2Bn6(Et2O) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H92 N4 O2 Zr2' _chemical_formula_weight 1263.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.940(4) _cell_length_b 18.075(4) _cell_length_c 21.577(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.70(3) _cell_angle_gamma 90.00 _cell_volume 6736(2) _cell_formula_units_Z 4 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 5447 _cell_measurement_theta_min 2.262 _cell_measurement_theta_max 1.000 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; absorption correction applied using SADABS(Sheldrick, 1996) ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART with CCD detector' _diffrn_measurement_method '0.3 deg omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63367 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_sigmaI/netI 0.1527 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 31.53 _reflns_number_total 21557 _reflns_number_gt 10074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21557 _refine_ls_number_parameters 752 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1721 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 1.968 _refine_ls_shift/su_mean 0.004 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 0.108132(17) 0.199356(18) 0.590254(14) 0.02744(9) Uani 1 1 d . . . Zr2 Zr -0.043081(19) 0.373613(19) 0.789631(15) 0.03078(9) Uani 1 1 d . A . N1 N 0.04265(15) 0.27819(15) 0.51343(12) 0.0298(6) Uani 1 1 d . . . N2 N -0.02036(14) 0.20872(15) 0.56796(12) 0.0295(6) Uani 1 1 d . . . N3 N -0.03589(15) 0.41130(15) 0.69178(12) 0.0292(6) Uani 1 1 d . . . N4 N -0.14441(16) 0.36145(17) 0.70352(13) 0.0399(7) Uani 1 1 d . . . O1 O -0.13499(12) 0.35675(12) 0.53765(10) 0.0272(5) Uani 1 1 d . . . C1 C 0.0712(2) 0.4071(2) 0.48990(18) 0.0473(10) Uani 1 1 d . . . H1A H 0.0323 0.4257 0.5104 0.071 Uiso 1 1 calc R . . H1B H 0.0747 0.4406 0.4552 0.071 Uiso 1 1 calc R . . H1C H 0.1216 0.4042 0.5219 0.071 Uiso 1 1 calc R . . C2 C 0.0478(2) 0.33105(19) 0.46254(16) 0.0340(8) Uani 1 1 d . . . H2 H -0.0055 0.3357 0.4328 0.041 Uiso 1 1 calc R . . C3 C 0.0997(2) 0.3029(2) 0.42271(17) 0.0428(9) Uani 1 1 d . . . H3A H 0.1534 0.3012 0.4494 0.064 Uiso 1 1 calc R . . H3B H 0.0960 0.3361 0.3861 0.064 Uiso 1 1 calc R . . H3C H 0.0832 0.2531 0.4068 0.064 Uiso 1 1 calc R . . C4 C -0.0891(2) 0.1785(2) 0.64873(17) 0.0471(10) Uani 1 1 d . . . H4A H -0.0439 0.1526 0.6757 0.071 Uiso 1 1 calc R . . H4B H -0.1365 0.1563 0.6548 0.071 Uiso 1 1 calc R . . H4C H -0.0868 0.2308 0.6611 0.071 Uiso 1 1 calc R . . C5 C -0.08932(19) 0.17212(19) 0.57805(16) 0.0329(8) Uani 1 1 d . . . H5 H -0.1359 0.1991 0.5518 0.040 Uiso 1 1 calc R . . C6 C -0.0957(2) 0.0927(2) 0.5560(2) 0.0544(11) Uani 1 1 d . . . H6A H -0.0997 0.0907 0.5099 0.082 Uiso 1 1 calc R . . H6B H -0.1419 0.0703 0.5641 0.082 Uiso 1 1 calc R . . H6C H -0.0496 0.0654 0.5798 0.082 Uiso 1 1 calc R . . C7 C -0.02514(18) 0.25365(17) 0.51821(14) 0.0259(7) Uani 1 1 d . . . C8 C -0.10025(17) 0.27106(18) 0.46856(15) 0.0276(7) Uani 1 1 d . . . C9 C -0.1158(2) 0.2345(2) 0.41002(16) 0.0373(8) Uani 1 1 d . . . H9 H -0.0812 0.1974 0.4035 0.045 Uiso 1 1 calc R . . C10 C -0.1811(2) 0.2515(2) 0.36075(17) 0.0426(9) Uani 1 1 d . . . H10 H -0.1926 0.2247 0.3214 0.051 Uiso 1 1 calc R . . C11 C -0.2287(2) 0.3075(2) 0.36955(16) 0.0374(8) Uani 1 1 d . . . H11 H -0.2728 0.3197 0.3354 0.045 Uiso 1 1 calc R . . C12 C -0.21455(18) 0.34706(18) 0.42694(15) 0.0295(7) Uani 1 1 d . . . C13 C -0.15118(18) 0.32613(18) 0.47667(14) 0.0262(7) Uani 1 1 d . . . C14 C -0.26741(18) 0.41100(19) 0.43315(15) 0.0319(8) Uani 1 1 d . . . C15 C -0.2710(2) 0.4676(2) 0.37902(18) 0.0512(11) Uani 1 1 d . . . H15A H -0.3069 0.5075 0.3819 0.077 Uiso 1 1 calc R . . H15B H -0.2890 0.4430 0.3372 0.077 Uiso 1 1 calc R . . H15C H -0.2193 0.4883 0.3836 0.077 Uiso 1 1 calc R . . C16 C -0.3498(2) 0.3818(2) 0.4276(2) 0.0487(10) Uani 1 1 d . . . H16A H -0.3479 0.3453 0.4616 0.073 Uiso 1 1 calc R . . H16B H -0.3705 0.3586 0.3854 0.073 Uiso 1 1 calc R . . H16C H -0.3833 0.4231 0.4323 0.073 Uiso 1 1 calc R . . C17 C -0.17835(18) 0.41758(18) 0.54725(15) 0.0285(7) Uani 1 1 d . A . C18 C -0.23733(19) 0.44757(19) 0.49843(16) 0.0335(8) Uani 1 1 d . . . C19 C -0.2734(2) 0.5115(2) 0.51296(18) 0.0471(10) Uani 1 1 d . . . H19 H -0.3138 0.5336 0.4804 0.057 Uiso 1 1 calc R . . C20 C -0.2518(2) 0.5429(2) 0.5729(2) 0.0591(12) Uani 1 1 d . . . H20 H -0.2752 0.5878 0.5809 0.071 Uiso 1 1 calc R . . C21 C -0.1960(2) 0.5092(2) 0.62178(18) 0.0470(10) Uani 1 1 d . A . H21 H -0.1823 0.5302 0.6637 0.056 Uiso 1 1 calc R . . C22 C -0.15985(18) 0.44471(19) 0.60963(16) 0.0327(8) Uani 1 1 d . . . C23 C -0.11166(18) 0.40381(19) 0.66752(15) 0.0295(7) Uani 1 1 d . A . C24 C 0.0842(2) 0.4106(2) 0.65851(18) 0.0478(10) Uani 1 1 d . . . H24A H 0.1169 0.4107 0.7030 0.072 Uiso 1 1 calc R . . H24B H 0.1117 0.4348 0.6305 0.072 Uiso 1 1 calc R . . H24C H 0.0719 0.3595 0.6442 0.072 Uiso 1 1 calc R . . C25 C 0.00956(19) 0.4523(2) 0.65517(16) 0.0353(8) Uani 1 1 d . . . H25 H -0.0215 0.4529 0.6091 0.042 Uiso 1 1 calc R . . C26 C 0.0241(2) 0.5321(2) 0.67658(19) 0.0476(10) Uani 1 1 d . . . H26A H -0.0255 0.5569 0.6728 0.071 Uiso 1 1 calc R . . H26B H 0.0518 0.5574 0.6493 0.071 Uiso 1 1 calc R . . H26C H 0.0554 0.5336 0.7215 0.071 Uiso 1 1 calc R . . C27 C -0.2631(2) 0.3452(2) 0.73678(19) 0.0507(12) Uiso 0.755(7) 1 d P A 2 H27A H -0.2363 0.3040 0.7631 0.076 Uiso 0.755(7) 1 calc PR A 2 H27B H -0.3186 0.3342 0.7217 0.076 Uiso 0.755(7) 1 calc PR A 2 H27C H -0.2554 0.3906 0.7627 0.076 Uiso 0.755(7) 1 calc PR A 2 C28 C -0.2319(3) 0.3555(3) 0.6816(2) 0.0327(12) Uiso 0.755(7) 1 d P A 2 H28 H -0.2528 0.4031 0.6602 0.039 Uiso 0.755(7) 1 calc PR A 2 C29 C -0.2554(2) 0.2936(2) 0.63187(19) 0.0485(11) Uiso 0.755(7) 1 d P A 2 H29A H -0.2373 0.2460 0.6522 0.073 Uiso 0.755(7) 1 calc PR A 2 H29B H -0.2321 0.3025 0.5964 0.073 Uiso 0.755(7) 1 calc PR A 2 H29C H -0.3120 0.2926 0.6151 0.073 Uiso 0.755(7) 1 calc PR A 2 C271 C -0.2631(2) 0.3452(2) 0.73678(19) 0.0507(12) Uiso 0.25 1 d P A 3 H27D H -0.2901 0.3891 0.7150 0.076 Uiso 0.245(7) 1 calc PR A 3 H27E H -0.2298 0.3594 0.7791 0.076 Uiso 0.245(7) 1 calc PR A 3 H27F H -0.3012 0.3087 0.7422 0.076 Uiso 0.245(7) 1 calc PR A 3 C281 C -0.2128(8) 0.3113(9) 0.6955(6) 0.031(4) Uiso 0.245(7) 1 d P A 3 H28A H -0.1922 0.2634 0.7166 0.037 Uiso 0.245(7) 1 calc PR A 3 C291 C -0.2554(2) 0.2936(2) 0.63187(19) 0.0485(11) Uiso 0.25 1 d P A 3 H29D H -0.2734 0.3393 0.6081 0.073 Uiso 0.245(7) 1 calc PR A 3 H29E H -0.3001 0.2630 0.6330 0.073 Uiso 0.245(7) 1 calc PR A 3 H29F H -0.2223 0.2663 0.6104 0.073 Uiso 0.245(7) 1 calc PR A 3 C30 C 0.1375(2) 0.2178(2) 0.69888(16) 0.0399(9) Uani 1 1 d . . . H30A H 0.1788 0.2547 0.7155 0.048 Uiso 1 1 calc R . . H30B H 0.0920 0.2271 0.7154 0.048 Uiso 1 1 calc R . . C31 C 0.16416(19) 0.1411(2) 0.70498(15) 0.0352(8) Uani 1 1 d . . . C32 C 0.2423(2) 0.1230(2) 0.71105(17) 0.0432(9) Uani 1 1 d . . . H32 H 0.2798 0.1614 0.7186 0.052 Uiso 1 1 calc R . . C33 C 0.2655(2) 0.0514(3) 0.7064(2) 0.0577(12) Uani 1 1 d . . . H33 H 0.3187 0.0412 0.7109 0.069 Uiso 1 1 calc R . . C34 C 0.2136(3) -0.0057(3) 0.6952(2) 0.0648(13) Uani 1 1 d . . . H34 H 0.2302 -0.0550 0.6916 0.078 Uiso 1 1 calc R . . C35 C 0.1375(3) 0.0096(3) 0.6894(2) 0.0614(13) Uani 1 1 d . . . H35 H 0.1011 -0.0298 0.6827 0.074 Uiso 1 1 calc R . . C36 C 0.1124(2) 0.0815(2) 0.69325(19) 0.0502(11) Uani 1 1 d . . . H36 H 0.0588 0.0906 0.6878 0.060 Uiso 1 1 calc R . . C37 C 0.21334(19) 0.2612(2) 0.57463(17) 0.0405(9) Uani 1 1 d . . . H37A H 0.2222 0.2417 0.5344 0.049 Uiso 1 1 calc R . . H37B H 0.1977 0.3136 0.5663 0.049 Uiso 1 1 calc R . . C38 C 0.28933(19) 0.2614(2) 0.62341(17) 0.0370(8) Uani 1 1 d . . . C39 C 0.3092(2) 0.3169(2) 0.66963(19) 0.0484(10) Uani 1 1 d . . . H39 H 0.2736 0.3560 0.6689 0.058 Uiso 1 1 calc R . . C40 C 0.3784(3) 0.3167(3) 0.7161(2) 0.0680(14) Uani 1 1 d . . . H40 H 0.3895 0.3552 0.7472 0.082 Uiso 1 1 calc R . . C41 C 0.4320(3) 0.2617(3) 0.7185(2) 0.0848(18) Uani 1 1 d . . . H41 H 0.4800 0.2618 0.7507 0.102 Uiso 1 1 calc R . . C42 C 0.4140(2) 0.2060(3) 0.6725(2) 0.0741(16) Uani 1 1 d . . . H42 H 0.4504 0.1676 0.6730 0.089 Uiso 1 1 calc R . . C43 C 0.3439(2) 0.2059(2) 0.62620(19) 0.0506(11) Uani 1 1 d . . . H43 H 0.3325 0.1670 0.5954 0.061 Uiso 1 1 calc R . . C44 C 0.1237(2) 0.0880(2) 0.54753(17) 0.0379(9) Uani 1 1 d . . . H44A H 0.1737 0.0662 0.5718 0.045 Uiso 1 1 calc R . . H44B H 0.0818 0.0542 0.5516 0.045 Uiso 1 1 calc R . . C45 C 0.12218(19) 0.09506(19) 0.47872(17) 0.0334(8) Uani 1 1 d . . . C46 C 0.1895(2) 0.1002(2) 0.45859(19) 0.0474(10) Uani 1 1 d . . . H46 H 0.2382 0.0976 0.4899 0.057 Uiso 1 1 calc R . . C47 C 0.1878(2) 0.1091(3) 0.3949(2) 0.0572(12) Uani 1 1 d . . . H47 H 0.2349 0.1132 0.3830 0.069 Uiso 1 1 calc R . . C48 C 0.1183(2) 0.1119(2) 0.3485(2) 0.0533(11) Uani 1 1 d . . . H48 H 0.1169 0.1177 0.3044 0.064 Uiso 1 1 calc R . . C49 C 0.0508(2) 0.1062(2) 0.36660(19) 0.0448(10) Uani 1 1 d . . . H49 H 0.0024 0.1082 0.3348 0.054 Uiso 1 1 calc R . . C50 C 0.0526(2) 0.0978(2) 0.43033(17) 0.0369(8) Uani 1 1 d . . . H50 H 0.0052 0.0936 0.4417 0.044 Uiso 1 1 calc R . . C51 C -0.0024(2) 0.2581(2) 0.81981(17) 0.0439(9) Uani 1 1 d . . . H51A H -0.0222 0.2205 0.7861 0.053 Uiso 1 1 calc R A . H51B H 0.0544 0.2540 0.8374 0.053 Uiso 1 1 calc R . . C52 C -0.0443(2) 0.2602(2) 0.86924(17) 0.0396(9) Uani 1 1 d . A . C53 C -0.1219(2) 0.2368(2) 0.8557(2) 0.0482(10) Uani 1 1 d . . . H53 H -0.1451 0.2135 0.8156 0.058 Uiso 1 1 calc R A . C54 C -0.1651(3) 0.2467(3) 0.8988(2) 0.0609(12) Uani 1 1 d . A . H54 H -0.2173 0.2302 0.8882 0.073 Uiso 1 1 calc R . . C55 C -0.1337(3) 0.2801(3) 0.9569(2) 0.0620(12) Uani 1 1 d . . . H55 H -0.1637 0.2865 0.9866 0.074 Uiso 1 1 calc R A . C56 C -0.0582(3) 0.3044(3) 0.9720(2) 0.0578(11) Uani 1 1 d . A . H56 H -0.0363 0.3277 1.0122 0.069 Uiso 1 1 calc R . . C57 C -0.0133(2) 0.2951(2) 0.92872(18) 0.0476(10) Uani 1 1 d . . . H57 H 0.0385 0.3127 0.9397 0.057 Uiso 1 1 calc R A . C58 C 0.0759(2) 0.4310(2) 0.82325(17) 0.0490(10) Uani 1 1 d . . . H58A H 0.1094 0.4124 0.7970 0.059 Uiso 1 1 calc R A . H58B H 0.0687 0.4848 0.8152 0.059 Uiso 1 1 calc R . . C59 C 0.1164(2) 0.4193(2) 0.89265(17) 0.0400(9) Uani 1 1 d . A . C60 C 0.1043(2) 0.4645(2) 0.94084(19) 0.0525(11) Uani 1 1 d . . . H60 H 0.0720 0.5068 0.9297 0.063 Uiso 1 1 calc R A . C61 C 0.1391(3) 0.4487(3) 1.0056(2) 0.0636(13) Uani 1 1 d . A . H61 H 0.1302 0.4803 1.0380 0.076 Uiso 1 1 calc R . . C62 C 0.1857(3) 0.3879(3) 1.0228(2) 0.0683(14) Uani 1 1 d . . . H62 H 0.2078 0.3762 1.0669 0.082 Uiso 1 1 calc R A . C63 C 0.2000(2) 0.3446(3) 0.9760(2) 0.0665(14) Uani 1 1 d . A . H63 H 0.2338 0.3034 0.9875 0.080 Uiso 1 1 calc R . . C64 C 0.1661(2) 0.3596(2) 0.9120(2) 0.0511(11) Uani 1 1 d . . . H64 H 0.1769 0.3283 0.8801 0.061 Uiso 1 1 calc R A . C65 C -0.0998(2) 0.4449(2) 0.85097(16) 0.0388(9) Uani 1 1 d . . . H65A H -0.1413 0.4161 0.8621 0.047 Uiso 1 1 calc R A . H65B H -0.0608 0.4576 0.8916 0.047 Uiso 1 1 calc R . . C66 C -0.1334(2) 0.5144(2) 0.81810(17) 0.0382(9) Uani 1 1 d . A . C67 C -0.0866(2) 0.5686(2) 0.8024(2) 0.0590(12) Uani 1 1 d . . . H67 H -0.0321 0.5619 0.8150 0.071 Uiso 1 1 calc R A . C68 C -0.1170(3) 0.6320(2) 0.7688(3) 0.0701(14) Uani 1 1 d . A . H68 H -0.0832 0.6679 0.7589 0.084 Uiso 1 1 calc R . . C69 C -0.1951(3) 0.6431(2) 0.7499(2) 0.0600(12) Uani 1 1 d . . . H69 H -0.2161 0.6862 0.7264 0.072 Uiso 1 1 calc R A . C70 C -0.2427(2) 0.5918(3) 0.7653(2) 0.0555(11) Uani 1 1 d . A . H70 H -0.2971 0.5994 0.7527 0.067 Uiso 1 1 calc R . . C71 C -0.2128(2) 0.5288(2) 0.79882(19) 0.0486(10) Uani 1 1 d . . . H71 H -0.2473 0.4941 0.8092 0.058 Uiso 1 1 calc R A . O2 O 0.0081(3) -0.0444(2) 0.89680(19) 0.1077(14) Uani 1 1 d . B 1 C72 C 0.0287(4) -0.1067(4) 0.9957(4) 0.127(3) Uani 1 1 d . B 1 H72A H 0.0805 -0.1246 0.9964 0.191 Uiso 1 1 calc R B 1 H72B H 0.0048 -0.1407 1.0201 0.191 Uiso 1 1 calc R B 1 H72C H 0.0327 -0.0574 1.0152 0.191 Uiso 1 1 calc R B 1 C73 C -0.0165(6) -0.1029(4) 0.9328(3) 0.184(5) Uani 1 1 d . B 1 H73A H -0.0710 -0.0944 0.9326 0.221 Uiso 1 1 calc R B 1 H73B H -0.0138 -0.1509 0.9113 0.221 Uiso 1 1 calc R B 1 C74 C -0.0388(4) -0.0357(4) 0.8369(3) 0.134(3) Uani 1 1 d . B 1 H74A H -0.0926 -0.0310 0.8401 0.161 Uiso 1 1 calc R B 1 H74B H -0.0362 -0.0815 0.8123 0.161 Uiso 1 1 calc R B 1 C75 C -0.0234(3) 0.0246(4) 0.8014(3) 0.0970(19) Uani 1 1 d . B 1 H75A H -0.0255 0.0706 0.8249 0.145 Uiso 1 1 calc R B 1 H75B H -0.0621 0.0264 0.7595 0.145 Uiso 1 1 calc R B 1 H75C H 0.0283 0.0191 0.7948 0.145 Uiso 1 1 calc R B 1 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 0.02584(16) 0.03029(18) 0.02530(16) 0.00230(14) 0.00540(12) 0.00466(14) Zr2 0.03159(18) 0.0345(2) 0.02618(16) 0.00069(14) 0.00763(13) -0.00257(15) N1 0.0288(15) 0.0317(16) 0.0304(14) 0.0067(12) 0.0108(12) 0.0009(12) N2 0.0250(14) 0.0339(17) 0.0294(14) 0.0062(12) 0.0071(11) 0.0040(12) N3 0.0242(14) 0.0307(16) 0.0309(14) 0.0019(12) 0.0048(11) -0.0016(12) N4 0.0342(16) 0.055(2) 0.0326(15) -0.0102(15) 0.0133(13) -0.0178(14) O1 0.0249(11) 0.0306(13) 0.0235(11) -0.0011(9) 0.0022(9) 0.0066(9) C1 0.064(3) 0.039(2) 0.041(2) 0.0084(18) 0.019(2) 0.0057(19) C2 0.0362(19) 0.035(2) 0.0313(18) 0.0103(15) 0.0096(15) 0.0053(15) C3 0.059(2) 0.037(2) 0.0358(19) 0.0049(17) 0.0194(18) 0.0004(18) C4 0.039(2) 0.062(3) 0.045(2) 0.016(2) 0.0184(18) 0.0068(19) C5 0.0269(17) 0.0314(19) 0.0407(19) 0.0085(16) 0.0095(15) 0.0030(14) C6 0.048(2) 0.036(2) 0.084(3) -0.006(2) 0.025(2) -0.0034(19) C7 0.0291(17) 0.0258(18) 0.0226(15) -0.0018(13) 0.0066(13) 0.0064(13) C8 0.0251(16) 0.0300(18) 0.0271(16) 0.0028(14) 0.0062(13) 0.0021(14) C9 0.043(2) 0.034(2) 0.0336(18) -0.0037(16) 0.0083(16) 0.0091(16) C10 0.049(2) 0.045(2) 0.0299(18) -0.0067(17) 0.0031(17) 0.0090(18) C11 0.0353(19) 0.045(2) 0.0265(17) -0.0020(16) -0.0010(14) 0.0086(16) C12 0.0276(17) 0.0292(19) 0.0294(17) -0.0001(14) 0.0040(14) 0.0024(14) C13 0.0271(16) 0.0257(17) 0.0236(15) -0.0026(13) 0.0030(13) -0.0008(13) C14 0.0306(18) 0.032(2) 0.0289(17) -0.0006(15) 0.0006(14) 0.0067(14) C15 0.064(3) 0.047(3) 0.041(2) 0.0116(19) 0.011(2) 0.018(2) C16 0.030(2) 0.052(3) 0.059(3) -0.014(2) 0.0041(18) 0.0016(18) C17 0.0242(16) 0.0301(19) 0.0302(17) 0.0015(14) 0.0058(13) 0.0040(14) C18 0.0303(18) 0.036(2) 0.0308(17) -0.0019(15) 0.0023(14) 0.0037(15) C19 0.038(2) 0.051(3) 0.044(2) -0.0094(19) -0.0029(17) 0.0181(18) C20 0.052(3) 0.056(3) 0.059(3) -0.019(2) -0.002(2) 0.023(2) C21 0.042(2) 0.053(3) 0.039(2) -0.0186(19) -0.0016(17) 0.0146(19) C22 0.0241(17) 0.037(2) 0.0342(18) -0.0031(15) 0.0031(14) 0.0036(15) C23 0.0268(17) 0.036(2) 0.0255(16) -0.0076(14) 0.0076(13) 0.0005(14) C24 0.031(2) 0.075(3) 0.039(2) 0.003(2) 0.0117(17) 0.0028(19) C25 0.0326(19) 0.045(2) 0.0277(17) 0.0073(16) 0.0066(14) -0.0080(16) C26 0.051(2) 0.038(2) 0.048(2) 0.0113(18) 0.0047(19) -0.0091(18) C30 0.037(2) 0.052(3) 0.0276(17) 0.0017(17) 0.0046(15) 0.0112(17) C31 0.0313(18) 0.050(2) 0.0225(16) 0.0089(15) 0.0043(14) 0.0075(16) C32 0.038(2) 0.046(2) 0.043(2) 0.0045(18) 0.0056(17) 0.0041(18) C33 0.042(2) 0.055(3) 0.067(3) 0.004(2) 0.000(2) 0.013(2) C34 0.068(3) 0.045(3) 0.067(3) 0.012(2) -0.006(2) 0.016(2) C35 0.060(3) 0.050(3) 0.063(3) 0.019(2) -0.001(2) -0.011(2) C36 0.034(2) 0.065(3) 0.047(2) 0.018(2) 0.0040(18) -0.004(2) C37 0.0322(19) 0.049(2) 0.038(2) 0.0064(17) 0.0046(16) 0.0033(17) C38 0.0313(19) 0.042(2) 0.038(2) 0.0020(17) 0.0084(15) -0.0021(16) C39 0.036(2) 0.048(3) 0.057(3) -0.006(2) 0.0057(18) 0.0009(18) C40 0.048(3) 0.079(4) 0.069(3) -0.028(3) 0.004(2) -0.001(2) C41 0.043(3) 0.125(5) 0.070(3) -0.032(3) -0.013(2) 0.015(3) C42 0.040(2) 0.097(4) 0.074(3) -0.021(3) -0.004(2) 0.029(3) C43 0.037(2) 0.063(3) 0.046(2) -0.012(2) 0.0015(17) 0.005(2) C44 0.036(2) 0.037(2) 0.040(2) 0.0000(17) 0.0079(16) 0.0097(16) C45 0.0321(19) 0.0275(19) 0.041(2) -0.0055(15) 0.0095(15) 0.0054(14) C46 0.033(2) 0.061(3) 0.048(2) -0.023(2) 0.0097(17) -0.0027(18) C47 0.040(2) 0.085(3) 0.053(3) -0.026(2) 0.025(2) -0.010(2) C48 0.061(3) 0.063(3) 0.039(2) -0.015(2) 0.021(2) -0.018(2) C49 0.043(2) 0.046(2) 0.041(2) -0.0004(18) 0.0043(18) 0.0004(18) C50 0.0333(19) 0.035(2) 0.044(2) 0.0016(17) 0.0131(16) 0.0029(16) C51 0.047(2) 0.049(3) 0.035(2) -0.0019(18) 0.0109(17) 0.0063(18) C52 0.044(2) 0.035(2) 0.038(2) 0.0104(17) 0.0069(17) 0.0019(17) C53 0.044(2) 0.049(3) 0.048(2) 0.0027(19) 0.0066(19) 0.0007(19) C54 0.052(3) 0.063(3) 0.069(3) 0.014(2) 0.020(2) -0.007(2) C55 0.060(3) 0.077(3) 0.058(3) 0.014(3) 0.031(2) 0.013(2) C56 0.069(3) 0.068(3) 0.039(2) 0.003(2) 0.019(2) 0.006(2) C57 0.052(2) 0.051(3) 0.038(2) 0.0032(19) 0.0104(18) 0.000(2) C58 0.041(2) 0.071(3) 0.0315(19) 0.0030(19) 0.0037(17) -0.013(2) C59 0.0286(19) 0.052(3) 0.0353(19) -0.0020(18) 0.0023(15) -0.0085(17) C60 0.042(2) 0.056(3) 0.051(2) -0.011(2) -0.0026(19) -0.0016(19) C61 0.055(3) 0.089(4) 0.043(2) -0.029(2) 0.005(2) -0.010(3) C62 0.053(3) 0.097(4) 0.041(2) 0.005(3) -0.012(2) 0.000(3) C63 0.046(3) 0.072(3) 0.064(3) -0.004(3) -0.015(2) 0.006(2) C64 0.035(2) 0.065(3) 0.048(2) -0.016(2) 0.0035(18) 0.001(2) C65 0.037(2) 0.045(2) 0.0334(19) -0.0019(17) 0.0075(15) -0.0023(17) C66 0.038(2) 0.039(2) 0.0372(19) -0.0109(17) 0.0094(16) -0.0030(17) C67 0.042(2) 0.045(3) 0.078(3) 0.005(2) -0.004(2) -0.005(2) C68 0.055(3) 0.041(3) 0.103(4) 0.015(3) 0.002(3) -0.007(2) C69 0.057(3) 0.042(3) 0.073(3) -0.003(2) 0.004(2) 0.013(2) C70 0.043(2) 0.059(3) 0.063(3) -0.009(2) 0.012(2) 0.013(2) C71 0.043(2) 0.047(3) 0.058(3) -0.005(2) 0.017(2) 0.0038(19) O2 0.155(4) 0.075(3) 0.073(3) 0.013(2) -0.003(3) -0.037(3) C72 0.144(7) 0.092(5) 0.157(7) 0.053(5) 0.062(6) 0.014(4) C73 0.293(12) 0.122(7) 0.088(5) 0.038(5) -0.035(6) -0.111(7) C74 0.172(7) 0.144(7) 0.062(4) 0.003(4) -0.009(4) -0.074(6) C75 0.107(5) 0.110(5) 0.067(4) 0.009(3) 0.012(3) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N2 2.230(3) . ? Zr1 N1 2.259(3) . ? Zr1 C44 2.263(3) . ? Zr1 C30 2.283(3) . ? Zr1 C37 2.296(4) . ? Zr1 C31 2.627(3) . ? Zr1 C7 2.662(3) . ? Zr2 N4 2.231(3) . ? Zr2 C51 2.249(4) . ? Zr2 N3 2.255(3) . ? Zr2 C65 2.276(4) . ? Zr2 C58 2.307(4) . ? Zr2 C23 2.646(3) . ? Zr2 C52 2.678(4) . ? N1 C7 1.325(4) . ? N1 C2 1.477(4) . ? N2 C7 1.330(4) . ? N2 C5 1.470(4) . ? N3 C23 1.325(4) . ? N3 C25 1.479(4) . ? N4 C23 1.335(4) . ? N4 C281 1.498(13) . ? N4 C28 1.516(5) . ? O1 C13 1.384(3) . ? O1 C17 1.394(4) . ? C1 C2 1.509(5) . ? C2 C3 1.516(5) . ? C4 C5 1.529(5) . ? C5 C6 1.507(5) . ? C7 C8 1.510(4) . ? C8 C9 1.385(4) . ? C8 C13 1.394(4) . ? C9 C10 1.386(5) . ? C10 C11 1.370(5) . ? C11 C12 1.393(4) . ? C12 C13 1.388(4) . ? C12 C14 1.524(4) . ? C14 C18 1.517(4) . ? C14 C15 1.541(5) . ? C14 C16 1.543(5) . ? C17 C18 1.385(4) . ? C17 C22 1.386(4) . ? C18 C19 1.401(5) . ? C19 C20 1.368(5) . ? C20 C21 1.384(5) . ? C21 C22 1.393(5) . ? C22 C23 1.507(4) . ? C24 C25 1.521(5) . ? C25 C26 1.515(5) . ? C27 C28 1.458(6) . ? C28 C29 1.528(6) . ? C30 C31 1.461(5) . ? C31 C36 1.399(5) . ? C31 C32 1.410(5) . ? C32 C33 1.372(5) . ? C33 C34 1.366(6) . ? C34 C35 1.365(6) . ? C35 C36 1.385(6) . ? C37 C38 1.480(5) . ? C38 C39 1.390(5) . ? C38 C43 1.392(5) . ? C39 C40 1.369(5) . ? C40 C41 1.374(6) . ? C41 C42 1.389(6) . ? C42 C43 1.379(5) . ? C44 C45 1.483(5) . ? C45 C46 1.393(5) . ? C45 C50 1.395(5) . ? C46 C47 1.376(6) . ? C47 C48 1.373(5) . ? C48 C49 1.373(5) . ? C49 C50 1.375(5) . ? C51 C52 1.461(5) . ? C52 C57 1.403(5) . ? C52 C53 1.409(5) . ? C53 C54 1.375(6) . ? C54 C55 1.367(6) . ? C55 C56 1.377(6) . ? C56 C57 1.397(6) . ? C58 C59 1.492(5) . ? C59 C60 1.385(5) . ? C59 C64 1.390(5) . ? C60 C61 1.397(6) . ? C61 C62 1.371(6) . ? C62 C63 1.355(6) . ? C63 C64 1.378(6) . ? C65 C66 1.486(5) . ? C66 C67 1.391(5) . ? C66 C71 1.395(5) . ? C67 C68 1.387(6) . ? C68 C69 1.365(6) . ? C69 C70 1.361(6) . ? C70 C71 1.377(6) . ? O2 C74 1.346(6) . ? O2 C73 1.450(7) . ? C72 C73 1.381(8) . ? C74 C75 1.404(8) . ? 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 N2 Zr1 N1 59.47(10) . . ? N2 Zr1 C44 102.36(12) . . ? N1 Zr1 C44 111.05(11) . . ? N2 Zr1 C30 98.51(12) . . ? N1 Zr1 C30 126.22(12) . . ? C44 Zr1 C30 121.89(13) . . ? N2 Zr1 C37 140.72(11) . . ? N1 Zr1 C37 82.52(11) . . ? C44 Zr1 C37 100.18(14) . . ? C30 Zr1 C37 96.28(14) . . ? N2 Zr1 C31 110.08(10) . . ? N1 Zr1 C31 159.18(11) . . ? C44 Zr1 C31 88.23(12) . . ? C30 Zr1 C31 33.70(12) . . ? C37 Zr1 C31 102.33(12) . . ? N2 Zr1 C7 29.93(9) . . ? N1 Zr1 C7 29.82(9) . . ? C44 Zr1 C7 106.29(11) . . ? C30 Zr1 C7 117.83(11) . . ? C37 Zr1 C7 112.26(11) . . ? C31 Zr1 C7 138.80(10) . . ? N4 Zr2 C51 106.09(13) . . ? N4 Zr2 N3 59.34(10) . . ? C51 Zr2 N3 117.08(12) . . ? N4 Zr2 C65 98.53(12) . . ? C51 Zr2 C65 121.24(13) . . ? N3 Zr2 C65 121.41(11) . . ? N4 Zr2 C58 141.47(12) . . ? C51 Zr2 C58 97.26(15) . . ? N3 Zr2 C58 82.88(11) . . ? C65 Zr2 C58 94.81(14) . . ? N4 Zr2 C23 30.27(10) . . ? C51 Zr2 C23 120.46(12) . . ? N3 Zr2 C23 30.03(9) . . ? C65 Zr2 C23 107.56(11) . . ? C58 Zr2 C23 111.21(12) . . ? N4 Zr2 C52 108.23(11) . . ? C51 Zr2 C52 33.07(12) . . ? N3 Zr2 C52 147.57(11) . . ? C65 Zr2 C52 88.75(13) . . ? C58 Zr2 C52 108.05(13) . . ? C23 Zr2 C52 135.60(11) . . ? C7 N1 C2 121.2(3) . . ? C7 N1 Zr1 92.17(19) . . ? C2 N1 Zr1 146.0(2) . . ? C7 N2 C5 121.4(3) . . ? C7 N2 Zr1 93.31(19) . . ? C5 N2 Zr1 142.8(2) . . ? C23 N3 C25 119.7(3) . . ? C23 N3 Zr2 91.5(2) . . ? C25 N3 Zr2 146.2(2) . . ? C23 N4 C281 139.1(6) . . ? C23 N4 C28 116.2(3) . . ? C281 N4 C28 34.3(5) . . ? C23 N4 Zr2 92.32(19) . . ? C281 N4 Zr2 127.8(6) . . ? C28 N4 Zr2 144.0(2) . . ? C13 O1 C17 118.3(2) . . ? N1 C2 C1 111.4(3) . . ? N1 C2 C3 112.1(3) . . ? C1 C2 C3 112.3(3) . . ? N2 C5 C6 112.2(3) . . ? N2 C5 C4 109.8(3) . . ? C6 C5 C4 111.5(3) . . ? N1 C7 N2 114.0(3) . . ? N1 C7 C8 122.5(3) . . ? N2 C7 C8 123.4(3) . . ? N1 C7 Zr1 58.01(16) . . ? N2 C7 Zr1 56.77(15) . . ? C8 C7 Zr1 168.3(2) . . ? C9 C8 C13 118.6(3) . . ? C9 C8 C7 117.9(3) . . ? C13 C8 C7 123.3(3) . . ? C8 C9 C10 120.9(3) . . ? C11 C10 C9 119.1(3) . . ? C10 C11 C12 122.2(3) . . ? C13 C12 C11 117.4(3) . . ? C13 C12 C14 122.5(3) . . ? C11 C12 C14 120.0(3) . . ? O1 C13 C12 122.9(3) . . ? O1 C13 C8 115.4(3) . . ? C12 C13 C8 121.7(3) . . ? C18 C14 C12 109.8(3) . . ? C18 C14 C15 110.2(3) . . ? C12 C14 C15 109.6(3) . . ? C18 C14 C16 108.3(3) . . ? C12 C14 C16 109.9(3) . . ? C15 C14 C16 109.0(3) . . ? C18 C17 C22 122.2(3) . . ? C18 C17 O1 122.5(3) . . ? C22 C17 O1 115.3(3) . . ? C17 C18 C19 117.2(3) . . ? C17 C18 C14 122.8(3) . . ? C19 C18 C14 119.8(3) . . ? C20 C19 C18 121.6(3) . . ? C19 C20 C21 120.0(4) . . ? C20 C21 C22 120.1(3) . . ? C17 C22 C21 118.5(3) . . ? C17 C22 C23 124.4(3) . . ? C21 C22 C23 116.5(3) . . ? N3 C23 N4 113.3(3) . . ? N3 C23 C22 125.1(3) . . ? N4 C23 C22 121.3(3) . . ? N3 C23 Zr2 58.44(17) . . ? N4 C23 Zr2 57.41(17) . . ? C22 C23 Zr2 159.2(2) . . ? N3 C25 C26 112.9(3) . . ? N3 C25 C24 109.4(3) . . ? C26 C25 C24 112.4(3) . . ? C27 C28 N4 110.3(3) . . ? C27 C28 C29 112.8(4) . . ? N4 C28 C29 109.7(4) . . ? C31 C30 Zr1 86.2(2) . . ? C36 C31 C32 115.7(4) . . ? C36 C31 C30 121.9(3) . . ? C32 C31 C30 121.4(3) . . ? C36 C31 Zr1 94.1(2) . . ? C32 C31 Zr1 107.3(2) . . ? C30 C31 Zr1 60.14(17) . . ? C33 C32 C31 121.6(4) . . ? C34 C33 C32 121.3(4) . . ? C33 C34 C35 118.8(4) . . ? C34 C35 C36 121.1(4) . . ? C35 C36 C31 121.5(4) . . ? C38 C37 Zr1 122.2(2) . . ? C39 C38 C43 116.6(3) . . ? C39 C38 C37 121.3(3) . . ? C43 C38 C37 122.1(3) . . ? C40 C39 C38 122.0(4) . . ? C39 C40 C41 121.0(4) . . ? C40 C41 C42 118.3(4) . . ? C43 C42 C41 120.5(4) . . ? C42 C43 C38 121.6(4) . . ? C45 C44 Zr1 111.1(2) . . ? C46 C45 C50 116.1(3) . . ? C46 C45 C44 122.4(3) . . ? C50 C45 C44 121.5(3) . . ? C47 C46 C45 122.2(4) . . ? C48 C47 C46 120.2(4) . . ? C47 C48 C49 119.2(4) . . ? C48 C49 C50 120.6(4) . . ? C49 C50 C45 121.7(3) . . ? C52 C51 Zr2 89.8(2) . . ? C57 C52 C53 116.7(4) . . ? C57 C52 C51 121.7(4) . . ? C53 C52 C51 121.0(3) . . ? C57 C52 Zr2 99.9(2) . . ? C53 C52 Zr2 106.0(2) . . ? C51 C52 Zr2 57.10(19) . . ? C54 C53 C52 121.8(4) . . ? C55 C54 C53 120.6(4) . . ? C54 C55 C56 119.5(4) . . ? C55 C56 C57 120.8(4) . . ? C56 C57 C52 120.5(4) . . ? C59 C58 Zr2 114.2(2) . . ? C60 C59 C64 116.8(3) . . ? C60 C59 C58 122.5(4) . . ? C64 C59 C58 120.6(4) . . ? C59 C60 C61 120.8(4) . . ? C62 C61 C60 120.7(4) . . ? C63 C62 C61 119.0(4) . . ? C62 C63 C64 120.8(4) . . ? C63 C64 C59 121.8(4) . . ? C66 C65 Zr2 112.8(2) . . ? C67 C66 C71 115.5(4) . . ? C67 C66 C65 121.2(3) . . ? C71 C66 C65 123.3(4) . . ? C68 C67 C66 122.2(4) . . ? C69 C68 C67 120.2(4) . . ? C70 C69 C68 119.3(4) . . ? C69 C70 C71 120.7(4) . . ? C70 C71 C66 122.2(4) . . ? C74 O2 C73 113.4(5) . . ? C72 C73 O2 112.3(6) . . ? O2 C74 C75 116.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zr1 N1 C7 -6.10(18) . . . . ? C44 Zr1 N1 C7 86.1(2) . . . . ? C30 Zr1 N1 C7 -83.5(2) . . . . ? C37 Zr1 N1 C7 -175.8(2) . . . . ? C31 Zr1 N1 C7 -70.7(4) . . . . ? N2 Zr1 N1 C2 -175.1(4) . . . . ? C44 Zr1 N1 C2 -82.9(4) . . . . ? C30 Zr1 N1 C2 107.5(4) . . . . ? C37 Zr1 N1 C2 15.2(4) . . . . ? C31 Zr1 N1 C2 120.3(4) . . . . ? C7 Zr1 N1 C2 -169.0(5) . . . . ? N1 Zr1 N2 C7 6.08(18) . . . . ? C44 Zr1 N2 C7 -101.2(2) . . . . ? C30 Zr1 N2 C7 133.3(2) . . . . ? C37 Zr1 N2 C7 22.4(3) . . . . ? C31 Zr1 N2 C7 166.09(19) . . . . ? N1 Zr1 N2 C5 165.8(4) . . . . ? C44 Zr1 N2 C5 58.5(4) . . . . ? C30 Zr1 N2 C5 -66.9(4) . . . . ? C37 Zr1 N2 C5 -177.9(3) . . . . ? C31 Zr1 N2 C5 -34.1(4) . . . . ? C7 Zr1 N2 C5 159.8(5) . . . . ? N4 Zr2 N3 C23 11.29(19) . . . . ? C51 Zr2 N3 C23 104.7(2) . . . . ? C65 Zr2 N3 C23 -69.5(2) . . . . ? C58 Zr2 N3 C23 -160.8(2) . . . . ? C52 Zr2 N3 C23 86.5(3) . . . . ? N4 Zr2 N3 C25 169.8(4) . . . . ? C51 Zr2 N3 C25 -96.9(4) . . . . ? C65 Zr2 N3 C25 89.0(4) . . . . ? C58 Zr2 N3 C25 -2.3(4) . . . . ? C23 Zr2 N3 C25 158.5(5) . . . . ? C52 Zr2 N3 C25 -115.0(4) . . . . ? C51 Zr2 N4 C23 -123.5(2) . . . . ? N3 Zr2 N4 C23 -11.21(19) . . . . ? C65 Zr2 N4 C23 110.4(2) . . . . ? C58 Zr2 N4 C23 1.4(3) . . . . ? C52 Zr2 N4 C23 -158.1(2) . . . . ? C51 Zr2 N4 C281 48.1(8) . . . . ? N3 Zr2 N4 C281 160.4(8) . . . . ? C65 Zr2 N4 C281 -78.0(8) . . . . ? C58 Zr2 N4 C281 173.0(7) . . . . ? C23 Zr2 N4 C281 171.6(8) . . . . ? C52 Zr2 N4 C281 13.5(8) . . . . ? C51 Zr2 N4 C28 92.8(5) . . . . ? N3 Zr2 N4 C28 -154.9(5) . . . . ? C65 Zr2 N4 C28 -33.3(5) . . . . ? C58 Zr2 N4 C28 -142.2(5) . . . . ? C23 Zr2 N4 C28 -143.7(6) . . . . ? C52 Zr2 N4 C28 58.2(5) . . . . ? C7 N1 C2 C1 108.2(4) . . . . ? Zr1 N1 C2 C1 -84.6(5) . . . . ? C7 N1 C2 C3 -125.0(3) . . . . ? Zr1 N1 C2 C3 42.2(5) . . . . ? C7 N2 C5 C6 100.8(4) . . . . ? Zr1 N2 C5 C6 -55.4(5) . . . . ? C7 N2 C5 C4 -134.7(3) . . . . ? Zr1 N2 C5 C4 69.2(4) . . . . ? C2 N1 C7 N2 -177.5(3) . . . . ? Zr1 N1 C7 N2 9.7(3) . . . . ? C2 N1 C7 C8 6.7(5) . . . . ? Zr1 N1 C7 C8 -166.1(3) . . . . ? C2 N1 C7 Zr1 172.9(3) . . . . ? C5 N2 C7 N1 -175.6(3) . . . . ? Zr1 N2 C7 N1 -9.8(3) . . . . ? C5 N2 C7 C8 0.1(5) . . . . ? Zr1 N2 C7 C8 165.9(3) . . . . ? C5 N2 C7 Zr1 -165.8(3) . . . . ? N2 Zr1 C7 N1 169.4(3) . . . . ? C44 Zr1 C7 N1 -104.1(2) . . . . ? C30 Zr1 C7 N1 115.0(2) . . . . ? C37 Zr1 C7 N1 4.5(2) . . . . ? C31 Zr1 C7 N1 149.4(2) . . . . ? N1 Zr1 C7 N2 -169.4(3) . . . . ? C44 Zr1 C7 N2 86.5(2) . . . . ? C30 Zr1 C7 N2 -54.4(2) . . . . ? C37 Zr1 C7 N2 -164.9(2) . . . . ? C31 Zr1 C7 N2 -20.0(3) . . . . ? N2 Zr1 C7 C8 -94.5(12) . . . . ? N1 Zr1 C7 C8 96.0(12) . . . . ? C44 Zr1 C7 C8 -8.0(12) . . . . ? C30 Zr1 C7 C8 -149.0(11) . . . . ? C37 Zr1 C7 C8 100.6(11) . . . . ? C31 Zr1 C7 C8 -114.6(11) . . . . ? N1 C7 C8 C9 74.4(4) . . . . ? N2 C7 C8 C9 -101.0(4) . . . . ? Zr1 C7 C8 C9 -14.2(13) . . . . ? N1 C7 C8 C13 -100.0(4) . . . . ? N2 C7 C8 C13 84.6(4) . . . . ? Zr1 C7 C8 C13 171.4(10) . . . . ? C13 C8 C9 C10 -0.9(5) . . . . ? C7 C8 C9 C10 -175.6(3) . . . . ? C8 C9 C10 C11 2.9(6) . . . . ? C9 C10 C11 C12 -1.3(6) . . . . ? C10 C11 C12 C13 -2.2(5) . . . . ? C10 C11 C12 C14 177.3(3) . . . . ? C17 O1 C13 C12 -8.4(5) . . . . ? C17 O1 C13 C8 173.0(3) . . . . ? C11 C12 C13 O1 -174.2(3) . . . . ? C14 C12 C13 O1 6.2(5) . . . . ? C11 C12 C13 C8 4.3(5) . . . . ? C14 C12 C13 C8 -175.2(3) . . . . ? C9 C8 C13 O1 175.8(3) . . . . ? C7 C8 C13 O1 -9.8(5) . . . . ? C9 C8 C13 C12 -2.8(5) . . . . ? C7 C8 C13 C12 171.6(3) . . . . ? C13 C12 C14 C18 2.7(5) . . . . ? C11 C12 C14 C18 -176.8(3) . . . . ? C13 C12 C14 C15 124.0(4) . . . . ? C11 C12 C14 C15 -55.6(4) . . . . ? C13 C12 C14 C16 -116.3(4) . . . . ? C11 C12 C14 C16 64.2(4) . . . . ? C13 O1 C17 C18 0.9(5) . . . . ? C13 O1 C17 C22 179.1(3) . . . . ? C22 C17 C18 C19 5.9(5) . . . . ? O1 C17 C18 C19 -176.0(3) . . . . ? C22 C17 C18 C14 -169.3(3) . . . . ? O1 C17 C18 C14 8.7(5) . . . . ? C12 C14 C18 C17 -9.9(5) . . . . ? C15 C14 C18 C17 -130.8(4) . . . . ? C16 C14 C18 C17 110.1(4) . . . . ? C12 C14 C18 C19 175.0(3) . . . . ? C15 C14 C18 C19 54.1(5) . . . . ? C16 C14 C18 C19 -65.1(4) . . . . ? C17 C18 C19 C20 -0.5(6) . . . . ? C14 C18 C19 C20 174.9(4) . . . . ? C18 C19 C20 C21 -3.4(7) . . . . ? C19 C20 C21 C22 2.1(7) . . . . ? C18 C17 C22 C21 -7.3(5) . . . . ? O1 C17 C22 C21 174.5(3) . . . . ? C18 C17 C22 C23 163.7(3) . . . . ? O1 C17 C22 C23 -14.5(5) . . . . ? C20 C21 C22 C17 3.2(6) . . . . ? C20 C21 C22 C23 -168.5(4) . . . . ? C25 N3 C23 N4 175.8(3) . . . . ? Zr2 N3 C23 N4 -17.8(3) . . . . ? C25 N3 C23 C22 -11.0(5) . . . . ? Zr2 N3 C23 C22 155.4(3) . . . . ? C25 N3 C23 Zr2 -166.4(3) . . . . ? C281 N4 C23 N3 -151.8(10) . . . . ? C28 N4 C23 N3 175.2(3) . . . . ? Zr2 N4 C23 N3 18.1(3) . . . . ? C281 N4 C23 C22 34.7(11) . . . . ? C28 N4 C23 C22 1.7(5) . . . . ? Zr2 N4 C23 C22 -155.5(3) . . . . ? C281 N4 C23 Zr2 -169.8(10) . . . . ? C28 N4 C23 Zr2 157.2(3) . . . . ? C17 C22 C23 N3 93.9(4) . . . . ? C21 C22 C23 N3 -95.0(4) . . . . ? C17 C22 C23 N4 -93.4(4) . . . . ? C21 C22 C23 N4 77.8(4) . . . . ? C17 C22 C23 Zr2 -173.4(5) . . . . ? C21 C22 C23 Zr2 -2.2(8) . . . . ? N4 Zr2 C23 N3 -160.5(3) . . . . ? C51 Zr2 C23 N3 -92.2(2) . . . . ? C65 Zr2 C23 N3 123.0(2) . . . . ? C58 Zr2 C23 N3 20.5(2) . . . . ? C52 Zr2 C23 N3 -130.1(2) . . . . ? C51 Zr2 C23 N4 68.3(2) . . . . ? N3 Zr2 C23 N4 160.5(3) . . . . ? C65 Zr2 C23 N4 -76.5(2) . . . . ? C58 Zr2 C23 N4 -179.0(2) . . . . ? C52 Zr2 C23 N4 30.4(3) . . . . ? N4 Zr2 C23 C22 93.1(7) . . . . ? C51 Zr2 C23 C22 161.4(6) . . . . ? N3 Zr2 C23 C22 -106.4(7) . . . . ? C65 Zr2 C23 C22 16.6(7) . . . . ? C58 Zr2 C23 C22 -85.9(7) . . . . ? C52 Zr2 C23 C22 123.5(6) . . . . ? C23 N3 C25 C26 97.1(4) . . . . ? Zr2 N3 C25 C26 -57.9(5) . . . . ? C23 N3 C25 C24 -137.0(3) . . . . ? Zr2 N3 C25 C24 68.0(5) . . . . ? C23 N4 C28 C27 -149.0(4) . . . . ? C281 N4 C28 C27 70.2(10) . . . . ? Zr2 N4 C28 C27 -10.2(7) . . . . ? C23 N4 C28 C29 86.2(4) . . . . ? C281 N4 C28 C29 -54.6(10) . . . . ? Zr2 N4 C28 C29 -135.0(4) . . . . ? N2 Zr1 C30 C31 113.6(2) . . . . ? N1 Zr1 C30 C31 171.84(18) . . . . ? C44 Zr1 C30 C31 3.3(3) . . . . ? C37 Zr1 C30 C31 -102.8(2) . . . . ? C7 Zr1 C30 C31 137.88(19) . . . . ? Zr1 C30 C31 C36 -75.0(3) . . . . ? Zr1 C30 C31 C32 92.9(3) . . . . ? N2 Zr1 C31 C36 50.0(3) . . . . ? N1 Zr1 C31 C36 105.9(4) . . . . ? C44 Zr1 C31 C36 -52.5(3) . . . . ? C30 Zr1 C31 C36 124.7(4) . . . . ? C37 Zr1 C31 C36 -152.5(3) . . . . ? C7 Zr1 C31 C36 60.5(3) . . . . ? N2 Zr1 C31 C32 168.5(2) . . . . ? N1 Zr1 C31 C32 -135.6(3) . . . . ? C44 Zr1 C31 C32 66.0(3) . . . . ? C30 Zr1 C31 C32 -116.8(4) . . . . ? C37 Zr1 C31 C32 -34.0(3) . . . . ? C7 Zr1 C31 C32 179.0(2) . . . . ? N2 Zr1 C31 C30 -74.7(2) . . . . ? N1 Zr1 C31 C30 -18.8(4) . . . . ? C44 Zr1 C31 C30 -177.2(2) . . . . ? C37 Zr1 C31 C30 82.8(2) . . . . ? C7 Zr1 C31 C30 -64.2(3) . . . . ? C36 C31 C32 C33 -0.7(5) . . . . ? C30 C31 C32 C33 -169.3(4) . . . . ? Zr1 C31 C32 C33 -104.2(4) . . . . ? C31 C32 C33 C34 0.3(7) . . . . ? C32 C33 C34 C35 -0.7(7) . . . . ? C33 C34 C35 C36 1.4(7) . . . . ? C34 C35 C36 C31 -1.8(7) . . . . ? C32 C31 C36 C35 1.4(5) . . . . ? C30 C31 C36 C35 170.0(4) . . . . ? Zr1 C31 C36 C35 112.9(4) . . . . ? N2 Zr1 C37 C38 145.3(3) . . . . ? N1 Zr1 C37 C38 159.4(3) . . . . ? C44 Zr1 C37 C38 -90.4(3) . . . . ? C30 Zr1 C37 C38 33.6(3) . . . . ? C31 Zr1 C37 C38 0.0(3) . . . . ? C7 Zr1 C37 C38 157.2(3) . . . . ? Zr1 C37 C38 C39 -92.4(4) . . . . ? Zr1 C37 C38 C43 86.5(4) . . . . ? C43 C38 C39 C40 -0.7(6) . . . . ? C37 C38 C39 C40 178.2(4) . . . . ? C38 C39 C40 C41 0.9(8) . . . . ? C39 C40 C41 C42 -0.2(9) . . . . ? C40 C41 C42 C43 -0.5(9) . . . . ? C41 C42 C43 C38 0.6(8) . . . . ? C39 C38 C43 C42 0.0(6) . . . . ? C37 C38 C43 C42 -178.9(4) . . . . ? N2 Zr1 C44 C45 87.6(2) . . . . ? N1 Zr1 C44 C45 25.9(3) . . . . ? C30 Zr1 C44 C45 -164.0(2) . . . . ? C37 Zr1 C44 C45 -60.0(3) . . . . ? C31 Zr1 C44 C45 -162.2(2) . . . . ? C7 Zr1 C44 C45 57.0(3) . . . . ? Zr1 C44 C45 C46 96.4(3) . . . . ? Zr1 C44 C45 C50 -82.9(4) . . . . ? C50 C45 C46 C47 1.3(6) . . . . ? C44 C45 C46 C47 -178.0(4) . . . . ? C45 C46 C47 C48 -1.1(7) . . . . ? C46 C47 C48 C49 0.4(7) . . . . ? C47 C48 C49 C50 0.0(6) . . . . ? C48 C49 C50 C45 0.4(6) . . . . ? C46 C45 C50 C49 -1.0(5) . . . . ? C44 C45 C50 C49 178.3(3) . . . . ? N4 Zr2 C51 C52 -98.8(2) . . . . ? N3 Zr2 C51 C52 -162.19(19) . . . . ? C65 Zr2 C51 C52 12.0(3) . . . . ? C58 Zr2 C51 C52 112.1(2) . . . . ? C23 Zr2 C51 C52 -128.0(2) . . . . ? Zr2 C51 C52 C57 -80.9(3) . . . . ? Zr2 C51 C52 C53 89.7(3) . . . . ? N4 Zr2 C52 C57 -146.9(2) . . . . ? C51 Zr2 C52 C57 121.4(4) . . . . ? N3 Zr2 C52 C57 152.0(2) . . . . ? C65 Zr2 C52 C57 -48.3(3) . . . . ? C58 Zr2 C52 C57 46.3(3) . . . . ? C23 Zr2 C52 C57 -162.5(2) . . . . ? N4 Zr2 C52 C53 -25.2(3) . . . . ? C51 Zr2 C52 C53 -116.9(4) . . . . ? N3 Zr2 C52 C53 -86.4(3) . . . . ? C65 Zr2 C52 C53 73.3(3) . . . . ? C58 Zr2 C52 C53 168.0(3) . . . . ? C23 Zr2 C52 C53 -40.8(3) . . . . ? N4 Zr2 C52 C51 91.7(2) . . . . ? N3 Zr2 C52 C51 30.5(3) . . . . ? C65 Zr2 C52 C51 -169.8(2) . . . . ? C58 Zr2 C52 C51 -75.1(3) . . . . ? C23 Zr2 C52 C51 76.1(3) . . . . ? C57 C52 C53 C54 -0.8(6) . . . . ? C51 C52 C53 C54 -171.9(4) . . . . ? Zr2 C52 C53 C54 -111.0(4) . . . . ? C52 C53 C54 C55 0.1(7) . . . . ? C53 C54 C55 C56 0.4(7) . . . . ? C54 C55 C56 C57 -0.1(7) . . . . ? C55 C56 C57 C52 -0.6(6) . . . . ? C53 C52 C57 C56 1.1(6) . . . . ? C51 C52 C57 C56 172.1(4) . . . . ? Zr2 C52 C57 C56 114.8(4) . . . . ? N4 Zr2 C58 C59 176.5(2) . . . . ? C51 Zr2 C58 C59 -56.0(3) . . . . ? N3 Zr2 C58 C59 -172.6(3) . . . . ? C65 Zr2 C58 C59 66.3(3) . . . . ? C23 Zr2 C58 C59 177.3(3) . . . . ? C52 Zr2 C58 C59 -23.9(3) . . . . ? Zr2 C58 C59 C60 -87.1(4) . . . . ? Zr2 C58 C59 C64 90.0(4) . . . . ? C64 C59 C60 C61 -1.8(6) . . . . ? C58 C59 C60 C61 175.4(4) . . . . ? C59 C60 C61 C62 -0.2(7) . . . . ? C60 C61 C62 C63 2.3(7) . . . . ? C61 C62 C63 C64 -2.3(8) . . . . ? C62 C63 C64 C59 0.2(7) . . . . ? C60 C59 C64 C63 1.8(6) . . . . ? C58 C59 C64 C63 -175.4(4) . . . . ? N4 Zr2 C65 C66 -56.3(3) . . . . ? C51 Zr2 C65 C66 -171.1(2) . . . . ? N3 Zr2 C65 C66 2.9(3) . . . . ? C58 Zr2 C65 C66 87.4(3) . . . . ? C23 Zr2 C65 C66 -26.6(3) . . . . ? C52 Zr2 C65 C66 -164.5(3) . . . . ? Zr2 C65 C66 C67 -64.6(4) . . . . ? Zr2 C65 C66 C71 112.9(3) . . . . ? C71 C66 C67 C68 -1.1(6) . . . . ? C65 C66 C67 C68 176.6(4) . . . . ? C66 C67 C68 C69 0.0(8) . . . . ? C67 C68 C69 C70 0.9(8) . . . . ? C68 C69 C70 C71 -0.7(7) . . . . ? C69 C70 C71 C66 -0.5(7) . . . . ? C67 C66 C71 C70 1.3(6) . . . . ? C65 C66 C71 C70 -176.3(4) . . . . ? C74 O2 C73 C72 -175.0(8) . . . . ? C73 O2 C74 C75 173.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.698 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.083 #===END data_jrh010 _database_code_CSD 170220 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (iPr4Xan)ZrBn2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H54 N4 O Zr' _chemical_formula_weight 734.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.887(2) _cell_length_b 16.325(3) _cell_length_c 21.427(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.47(3) _cell_angle_gamma 90.00 _cell_volume 3784.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 135(2) _cell_measurement_reflns_used 6399 _cell_measurement_theta_min 0.872 _cell_measurement_theta_max 1.000 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.329 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; absorption correction applied using SADABS(Sheldrick, 1996) ; _diffrn_ambient_temperature 135(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART with CCD detector' _diffrn_measurement_method '0.3 deg omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35224 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 31.53 _reflns_number_total 12039 _reflns_number_gt 8425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12039 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.003 _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 0.262806(16) 0.845074(11) 0.134310(9) 0.02165(6) Uani 1 1 d . . . O1 O 0.29021(11) 0.95285(8) 0.26462(6) 0.0266(3) Uani 1 1 d . . . N1 N 0.09756(15) 0.84251(9) 0.19006(8) 0.0250(3) Uani 1 1 d . . . N2 N 0.13655(14) 0.95356(9) 0.13720(8) 0.0250(3) Uani 1 1 d . . . N3 N 0.40837(14) 0.80101(10) 0.21245(8) 0.0242(3) Uani 1 1 d . . . N4 N 0.45023(14) 0.91116(9) 0.15582(7) 0.0231(3) Uani 1 1 d . . . C1 C -0.10271(19) 0.79805(14) 0.22025(12) 0.0380(5) Uani 1 1 d . . . H1A H -0.1288 0.8532 0.2310 0.057 Uiso 1 1 calc R . . H1B H -0.1425 0.7576 0.2452 0.057 Uiso 1 1 calc R . . H1C H -0.1268 0.7879 0.1755 0.057 Uiso 1 1 calc R . . C2 C 0.03752(17) 0.79092(12) 0.23445(10) 0.0279(4) Uani 1 1 d . . . H2 H 0.0583 0.7330 0.2245 0.034 Uiso 1 1 calc R . . C3 C 0.0784(2) 0.80207(14) 0.30428(11) 0.0364(5) Uani 1 1 d . . . H3A H 0.1686 0.8069 0.3111 0.055 Uiso 1 1 calc R . . H3B H 0.0520 0.7546 0.3274 0.055 Uiso 1 1 calc R . . H3C H 0.0408 0.8519 0.3192 0.055 Uiso 1 1 calc R . . C4 C -0.0042(2) 1.06273(15) 0.09576(13) 0.0427(6) Uani 1 1 d . . . H4A H -0.0404 1.0227 0.0649 0.064 Uiso 1 1 calc R . . H4B H -0.0074 1.1174 0.0767 0.064 Uiso 1 1 calc R . . H4C H -0.0510 1.0628 0.1322 0.064 Uiso 1 1 calc R . . C5 C 0.12983(18) 1.03980(12) 0.11660(10) 0.0294(4) Uani 1 1 d . . . H5 H 0.1739 1.0427 0.0782 0.035 Uiso 1 1 calc R . . C6 C 0.1910(2) 1.10361(13) 0.16231(11) 0.0367(5) Uani 1 1 d . . . H6A H 0.1383 1.1137 0.1957 0.055 Uiso 1 1 calc R . . H6B H 0.2022 1.1548 0.1397 0.055 Uiso 1 1 calc R . . H6C H 0.2717 1.0832 0.1808 0.055 Uiso 1 1 calc R . . C7 C 0.09553(16) 0.92415(11) 0.18912(9) 0.0235(4) Uani 1 1 d . . . C8 C 0.07859(17) 0.97540(11) 0.24546(9) 0.0244(4) Uani 1 1 d . . . C9 C -0.03005(17) 1.00857(12) 0.26223(10) 0.0285(4) Uani 1 1 d . . . H9 H -0.1056 1.0004 0.2362 0.034 Uiso 1 1 calc R . . C10 C -0.02825(19) 1.05393(13) 0.31728(11) 0.0328(5) Uani 1 1 d . . . H10 H -0.1033 1.0752 0.3294 0.039 Uiso 1 1 calc R . . C11 C 0.08185(19) 1.06840(13) 0.35454(10) 0.0315(4) Uani 1 1 d . . . H11 H 0.0813 1.1004 0.3915 0.038 Uiso 1 1 calc R . . C12 C 0.19447(18) 1.03689(12) 0.33892(10) 0.0269(4) Uani 1 1 d . . . C13 C 0.18835(17) 0.98991(11) 0.28523(9) 0.0246(4) Uani 1 1 d . . . C14 C 0.3139(2) 1.03443(14) 0.44669(10) 0.0350(5) Uani 1 1 d . . . H14A H 0.2999 0.9754 0.4498 0.053 Uiso 1 1 calc R . . H14B H 0.2468 1.0641 0.4636 0.053 Uiso 1 1 calc R . . H14C H 0.3929 1.0488 0.4708 0.053 Uiso 1 1 calc R . . C15 C 0.31732(18) 1.05814(12) 0.37719(9) 0.0270(4) Uani 1 1 d . . . C16 C 0.3374(2) 1.15138(12) 0.37236(12) 0.0347(5) Uani 1 1 d . . . H16A H 0.4186 1.1659 0.3940 0.052 Uiso 1 1 calc R . . H16B H 0.2729 1.1804 0.3919 0.052 Uiso 1 1 calc R . . H16C H 0.3336 1.1671 0.3281 0.052 Uiso 1 1 calc R . . C17 C 0.40519(16) 0.96460(11) 0.29783(9) 0.0228(4) Uani 1 1 d . . . C18 C 0.42320(17) 1.01336(12) 0.35103(9) 0.0249(4) Uani 1 1 d . . . C19 C 0.54593(18) 1.02028(13) 0.37886(10) 0.0289(4) Uani 1 1 d . . . H19 H 0.5633 1.0534 0.4152 0.035 Uiso 1 1 calc R . . C20 C 0.64243(18) 0.98011(13) 0.35476(10) 0.0312(4) Uani 1 1 d . . . H20 H 0.7244 0.9858 0.3747 0.037 Uiso 1 1 calc R . . C21 C 0.61967(18) 0.93151(13) 0.30148(10) 0.0285(4) Uani 1 1 d . . . H21 H 0.6862 0.9041 0.2852 0.034 Uiso 1 1 calc R . . C22 C 0.49993(17) 0.92272(12) 0.27182(9) 0.0237(4) Uani 1 1 d . . . C23 C 0.45962(16) 0.87548(12) 0.21237(9) 0.0228(4) Uani 1 1 d . . . C24 C 0.46654(19) 1.03577(13) 0.09117(10) 0.0320(4) Uani 1 1 d . . . H24A H 0.4736 1.0034 0.0532 0.048 Uiso 1 1 calc R . . H24B H 0.5127 1.0870 0.0890 0.048 Uiso 1 1 calc R . . H24C H 0.3793 1.0481 0.0942 0.048 Uiso 1 1 calc R . . C25 C 0.51891(17) 0.98755(12) 0.14840(10) 0.0261(4) Uani 1 1 d . . . H25 H 0.5158 1.0222 0.1867 0.031 Uiso 1 1 calc R . . C26 C 0.65428(18) 0.96634(14) 0.14171(11) 0.0367(5) Uani 1 1 d . . . H26A H 0.6893 0.9349 0.1784 0.055 Uiso 1 1 calc R . . H26B H 0.7017 1.0170 0.1388 0.055 Uiso 1 1 calc R . . H26C H 0.6583 0.9336 0.1036 0.055 Uiso 1 1 calc R . . C27 C 0.54575(19) 0.72406(14) 0.29112(11) 0.0372(5) Uani 1 1 d . . . H27A H 0.5682 0.6835 0.2607 0.056 Uiso 1 1 calc R . . H27B H 0.5501 0.6989 0.3328 0.056 Uiso 1 1 calc R . . H27C H 0.6032 0.7704 0.2924 0.056 Uiso 1 1 calc R . . C28 C 0.41443(18) 0.75433(12) 0.27161(10) 0.0265(4) Uani 1 1 d . . . H28 H 0.3885 0.7906 0.3054 0.032 Uiso 1 1 calc R . . C29 C 0.3293(2) 0.68044(13) 0.26435(11) 0.0336(5) Uani 1 1 d . . . H29A H 0.2443 0.6987 0.2520 0.050 Uiso 1 1 calc R . . H29B H 0.3333 0.6510 0.3044 0.050 Uiso 1 1 calc R . . H29C H 0.3553 0.6439 0.2320 0.050 Uiso 1 1 calc R . . C30 C 0.26687(18) 0.87585(13) 0.03079(9) 0.0271(4) Uani 1 1 d . . . H30A H 0.1813 0.8770 0.0095 0.033 Uiso 1 1 calc R . . H30B H 0.3032 0.9310 0.0270 0.033 Uiso 1 1 calc R . . C31 C 0.34042(18) 0.81482(12) -0.00047(9) 0.0261(4) Uani 1 1 d . . . C32 C 0.46865(19) 0.80746(13) 0.01473(10) 0.0313(4) Uani 1 1 d . . . H32 H 0.5104 0.8441 0.0443 0.038 Uiso 1 1 calc R . . C33 C 0.5356(2) 0.74774(15) -0.01256(11) 0.0370(5) Uani 1 1 d . . . H33 H 0.6226 0.7447 -0.0020 0.044 Uiso 1 1 calc R . . C34 C 0.4774(2) 0.69241(15) -0.05505(11) 0.0405(5) Uani 1 1 d . . . H34 H 0.5234 0.6512 -0.0735 0.049 Uiso 1 1 calc R . . C35 C 0.3512(2) 0.69847(14) -0.07006(11) 0.0375(5) Uani 1 1 d . . . H35 H 0.3098 0.6605 -0.0987 0.045 Uiso 1 1 calc R . . C36 C 0.28388(19) 0.75883(13) -0.04417(10) 0.0308(4) Uani 1 1 d . . . H36 H 0.1974 0.7624 -0.0563 0.037 Uiso 1 1 calc R . . C37 C 0.20722(19) 0.71423(12) 0.10589(10) 0.0298(4) Uani 1 1 d . . . H37A H 0.2805 0.6874 0.0914 0.036 Uiso 1 1 calc R . . H37B H 0.1893 0.6851 0.1444 0.036 Uiso 1 1 calc R . . C38 C 0.1006(2) 0.69959(13) 0.05688(10) 0.0324(5) Uani 1 1 d . . . C39 C 0.0980(3) 0.63165(15) 0.01671(12) 0.0436(6) Uani 1 1 d . . . H39 H 0.1646 0.5937 0.0213 0.052 Uiso 1 1 calc R . . C40 C 0.0009(3) 0.61866(19) -0.02940(13) 0.0583(8) Uani 1 1 d . . . H40 H 0.0012 0.5718 -0.0556 0.070 Uiso 1 1 calc R . . C41 C -0.0965(3) 0.6729(2) -0.03784(13) 0.0598(8) Uani 1 1 d . . . H41 H -0.1626 0.6640 -0.0700 0.072 Uiso 1 1 calc R . . C42 C -0.0969(2) 0.74033(18) 0.00109(13) 0.0489(6) Uani 1 1 d . . . H42 H -0.1635 0.7782 -0.0044 0.059 Uiso 1 1 calc R . . C43 C 0.0000(2) 0.75302(15) 0.04835(11) 0.0367(5) Uani 1 1 d . . . H43 H -0.0024 0.7990 0.0754 0.044 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 0.02168(9) 0.02100(9) 0.02234(10) -0.00088(7) 0.00285(6) 0.00037(7) O1 0.0195(6) 0.0317(7) 0.0280(7) -0.0084(6) -0.0001(5) 0.0040(5) N1 0.0246(8) 0.0234(8) 0.0272(9) -0.0010(7) 0.0036(6) -0.0013(6) N2 0.0254(8) 0.0214(8) 0.0279(9) -0.0005(7) 0.0014(6) 0.0000(6) N3 0.0259(8) 0.0243(8) 0.0228(8) 0.0009(6) 0.0045(6) 0.0020(6) N4 0.0236(8) 0.0237(8) 0.0221(8) 0.0003(6) 0.0028(6) -0.0017(6) C1 0.0270(10) 0.0382(12) 0.0499(15) 0.0033(11) 0.0089(10) -0.0030(9) C2 0.0251(9) 0.0257(9) 0.0336(11) 0.0026(8) 0.0060(8) 0.0007(7) C3 0.0401(12) 0.0391(12) 0.0309(12) 0.0034(10) 0.0078(9) 0.0019(9) C4 0.0312(11) 0.0375(12) 0.0569(16) 0.0126(11) -0.0058(10) 0.0053(9) C5 0.0278(9) 0.0242(9) 0.0353(12) 0.0026(9) 0.0002(8) 0.0004(7) C6 0.0413(12) 0.0243(10) 0.0447(14) -0.0005(9) 0.0054(10) -0.0048(9) C7 0.0171(8) 0.0270(9) 0.0259(10) -0.0026(8) -0.0003(7) 0.0013(7) C8 0.0234(9) 0.0233(9) 0.0267(10) -0.0031(7) 0.0041(7) 0.0015(7) C9 0.0233(9) 0.0255(10) 0.0370(12) -0.0034(8) 0.0047(8) 0.0018(7) C10 0.0271(10) 0.0308(11) 0.0424(13) -0.0043(9) 0.0120(9) 0.0038(8) C11 0.0348(11) 0.0290(10) 0.0319(11) -0.0067(9) 0.0094(9) 0.0020(8) C12 0.0282(9) 0.0248(9) 0.0282(10) -0.0020(8) 0.0058(8) 0.0003(7) C13 0.0223(9) 0.0241(9) 0.0281(10) -0.0016(8) 0.0063(7) 0.0028(7) C14 0.0406(12) 0.0403(12) 0.0248(11) -0.0006(9) 0.0065(9) 0.0019(9) C15 0.0311(10) 0.0263(10) 0.0236(10) -0.0030(8) 0.0041(8) -0.0017(8) C16 0.0404(12) 0.0270(10) 0.0365(12) -0.0054(9) 0.0038(9) -0.0016(9) C17 0.0210(8) 0.0252(9) 0.0218(9) 0.0011(7) 0.0008(7) -0.0014(7) C18 0.0287(9) 0.0251(9) 0.0209(9) 0.0001(7) 0.0027(7) -0.0025(7) C19 0.0323(10) 0.0325(11) 0.0212(10) -0.0015(8) -0.0003(8) -0.0067(8) C20 0.0255(9) 0.0393(12) 0.0272(11) 0.0031(9) -0.0032(8) -0.0047(8) C21 0.0237(9) 0.0351(11) 0.0265(10) 0.0007(8) 0.0021(8) 0.0010(8) C22 0.0239(9) 0.0255(9) 0.0214(9) 0.0018(7) 0.0007(7) 0.0009(7) C23 0.0183(8) 0.0261(9) 0.0246(10) 0.0017(8) 0.0044(7) 0.0055(7) C24 0.0336(11) 0.0319(11) 0.0308(11) 0.0058(9) 0.0055(9) -0.0056(8) C25 0.0274(9) 0.0251(9) 0.0263(10) 0.0011(8) 0.0049(8) -0.0048(7) C26 0.0259(10) 0.0432(13) 0.0419(13) 0.0010(10) 0.0074(9) -0.0061(9) C27 0.0315(11) 0.0378(12) 0.0417(13) 0.0122(10) 0.0017(9) 0.0097(9) C28 0.0294(9) 0.0259(9) 0.0247(10) 0.0043(8) 0.0056(8) 0.0062(7) C29 0.0365(11) 0.0283(10) 0.0361(12) 0.0096(9) 0.0043(9) 0.0024(8) C30 0.0270(9) 0.0288(10) 0.0252(10) 0.0000(8) 0.0010(8) 0.0010(8) C31 0.0320(10) 0.0286(9) 0.0182(9) 0.0032(8) 0.0048(8) 0.0001(8) C32 0.0310(10) 0.0343(11) 0.0284(11) 0.0045(9) 0.0029(8) -0.0007(8) C33 0.0330(11) 0.0442(13) 0.0345(12) 0.0083(10) 0.0073(9) 0.0071(9) C34 0.0538(14) 0.0385(13) 0.0310(12) 0.0030(10) 0.0127(11) 0.0124(11) C35 0.0520(14) 0.0359(12) 0.0250(11) -0.0004(9) 0.0065(10) 0.0010(10) C36 0.0337(10) 0.0356(11) 0.0236(10) 0.0010(8) 0.0049(8) -0.0035(8) C37 0.0350(11) 0.0234(10) 0.0320(11) -0.0020(8) 0.0085(9) -0.0013(8) C38 0.0396(12) 0.0304(11) 0.0295(11) -0.0046(9) 0.0142(9) -0.0137(9) C39 0.0574(15) 0.0378(12) 0.0391(14) -0.0113(11) 0.0204(12) -0.0164(11) C40 0.079(2) 0.0593(18) 0.0395(15) -0.0157(14) 0.0190(14) -0.0341(16) C41 0.0625(18) 0.082(2) 0.0334(14) -0.0003(14) 0.0002(13) -0.0414(17) C42 0.0371(12) 0.0641(17) 0.0450(15) 0.0073(13) 0.0019(11) -0.0174(12) C43 0.0349(11) 0.0433(13) 0.0326(12) -0.0018(10) 0.0071(9) -0.0105(9) _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 N2 2.2471(16) . ? Zr1 N1 2.2694(18) . ? Zr1 C30 2.280(2) . ? Zr1 C37 2.284(2) . ? Zr1 N3 2.2879(17) . ? Zr1 N4 2.3083(16) . ? Zr1 C23 2.613(2) . ? Zr1 C7 2.6163(19) . ? O1 C13 1.379(2) . ? O1 C17 1.382(2) . ? N1 C7 1.333(2) . ? N1 C2 1.477(3) . ? N2 C7 1.334(2) . ? N2 C5 1.475(2) . ? N3 C23 1.338(3) . ? N3 C28 1.474(2) . ? N4 C23 1.338(2) . ? N4 C25 1.472(2) . ? C1 C2 1.527(3) . ? C2 C3 1.523(3) . ? C4 C5 1.524(3) . ? C5 C6 1.530(3) . ? C7 C8 1.497(3) . ? C8 C9 1.385(3) . ? C8 C13 1.407(3) . ? C9 C10 1.391(3) . ? C10 C11 1.384(3) . ? C11 C12 1.404(3) . ? C12 C13 1.378(3) . ? C12 C15 1.528(3) . ? C14 C15 1.543(3) . ? C15 C18 1.524(3) . ? C15 C16 1.543(3) . ? C17 C18 1.386(3) . ? C17 C22 1.404(3) . ? C18 C19 1.405(3) . ? C19 C20 1.387(3) . ? C20 C21 1.389(3) . ? C21 C22 1.392(3) . ? C22 C23 1.511(3) . ? C24 C25 1.514(3) . ? C25 C26 1.536(3) . ? C27 C28 1.526(3) . ? C28 C29 1.519(3) . ? C30 C31 1.484(3) . ? C31 C36 1.400(3) . ? C31 C32 1.402(3) . ? C32 C33 1.386(3) . ? C33 C34 1.384(3) . ? C34 C35 1.379(3) . ? C35 C36 1.381(3) . ? C37 C38 1.494(3) . ? C38 C43 1.396(3) . ? C38 C39 1.402(3) . ? C39 C40 1.380(4) . ? C40 C41 1.378(5) . ? C41 C42 1.382(4) . ? C42 C43 1.393(3) . ? 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 N2 Zr1 N1 58.42(6) . . ? N2 Zr1 C30 86.11(7) . . ? N1 Zr1 C30 128.30(7) . . ? N2 Zr1 C37 126.86(7) . . ? N1 Zr1 C37 85.48(7) . . ? C30 Zr1 C37 88.87(8) . . ? N2 Zr1 N3 127.09(6) . . ? N1 Zr1 N3 97.69(6) . . ? C30 Zr1 N3 133.91(7) . . ? C37 Zr1 N3 92.41(7) . . ? N2 Zr1 N4 98.97(6) . . ? N1 Zr1 N4 129.71(6) . . ? C30 Zr1 N4 88.72(7) . . ? C37 Zr1 N4 133.79(7) . . ? N3 Zr1 N4 58.46(6) . . ? N2 Zr1 C23 107.02(6) . . ? N1 Zr1 C23 107.95(6) . . ? C30 Zr1 C23 118.46(7) . . ? C37 Zr1 C23 121.46(7) . . ? N3 Zr1 C23 30.77(6) . . ? N4 Zr1 C23 30.76(6) . . ? N2 Zr1 C7 30.66(6) . . ? N1 Zr1 C7 30.63(6) . . ? C30 Zr1 C7 114.77(7) . . ? C37 Zr1 C7 113.84(7) . . ? N3 Zr1 C7 106.64(6) . . ? N4 Zr1 C7 108.92(6) . . ? C23 Zr1 C7 100.43(6) . . ? C13 O1 C17 119.25(15) . . ? C7 N1 C2 124.89(17) . . ? C7 N1 Zr1 89.22(12) . . ? C2 N1 Zr1 141.65(12) . . ? C7 N2 C5 125.68(17) . . ? C7 N2 Zr1 90.15(11) . . ? C5 N2 Zr1 138.94(13) . . ? C23 N3 C28 119.52(16) . . ? C23 N3 Zr1 88.16(11) . . ? C28 N3 Zr1 138.76(12) . . ? C23 N4 C25 118.61(16) . . ? C23 N4 Zr1 87.30(11) . . ? C25 N4 Zr1 145.38(12) . . ? N1 C2 C3 117.58(17) . . ? N1 C2 C1 109.47(17) . . ? C3 C2 C1 111.19(18) . . ? N2 C5 C4 109.62(16) . . ? N2 C5 C6 117.07(17) . . ? C4 C5 C6 110.72(18) . . ? N1 C7 N2 111.46(17) . . ? N1 C7 C8 123.36(18) . . ? N2 C7 C8 123.68(17) . . ? N1 C7 Zr1 60.15(10) . . ? N2 C7 Zr1 59.19(10) . . ? C8 C7 Zr1 142.46(12) . . ? C9 C8 C13 117.96(18) . . ? C9 C8 C7 127.90(17) . . ? C13 C8 C7 114.14(16) . . ? C8 C9 C10 119.83(18) . . ? C11 C10 C9 120.58(19) . . ? C10 C11 C12 121.53(19) . . ? C13 C12 C11 116.19(18) . . ? C13 C12 C15 122.11(17) . . ? C11 C12 C15 121.60(18) . . ? C12 C13 O1 123.14(17) . . ? C12 C13 C8 123.85(17) . . ? O1 C13 C8 113.00(17) . . ? C18 C15 C12 110.26(16) . . ? C18 C15 C14 109.63(17) . . ? C12 C15 C14 110.27(17) . . ? C18 C15 C16 109.23(17) . . ? C12 C15 C16 108.08(17) . . ? C14 C15 C16 109.34(17) . . ? O1 C17 C18 122.63(17) . . ? O1 C17 C22 113.04(16) . . ? C18 C17 C22 124.32(17) . . ? C17 C18 C19 115.78(18) . . ? C17 C18 C15 122.35(17) . . ? C19 C18 C15 121.86(17) . . ? C20 C19 C18 121.87(19) . . ? C19 C20 C21 120.24(18) . . ? C20 C21 C22 120.35(19) . . ? C21 C22 C17 117.43(18) . . ? C21 C22 C23 127.27(18) . . ? C17 C22 C23 115.24(16) . . ? N3 C23 N4 114.06(17) . . ? N3 C23 C22 122.96(17) . . ? N4 C23 C22 121.77(17) . . ? N3 C23 Zr1 61.06(9) . . ? N4 C23 Zr1 61.94(10) . . ? C22 C23 Zr1 140.87(12) . . ? N4 C25 C24 112.24(16) . . ? N4 C25 C26 108.88(16) . . ? C24 C25 C26 108.63(17) . . ? N3 C28 C29 110.78(17) . . ? N3 C28 C27 110.65(17) . . ? C29 C28 C27 108.26(17) . . ? C31 C30 Zr1 111.21(13) . . ? C36 C31 C32 116.76(19) . . ? C36 C31 C30 121.40(18) . . ? C32 C31 C30 121.75(18) . . ? C33 C32 C31 121.3(2) . . ? C34 C33 C32 120.8(2) . . ? C35 C34 C33 118.5(2) . . ? C34 C35 C36 121.2(2) . . ? C35 C36 C31 121.4(2) . . ? C38 C37 Zr1 119.91(14) . . ? C43 C38 C39 116.9(2) . . ? C43 C38 C37 121.87(19) . . ? C39 C38 C37 121.2(2) . . ? C40 C39 C38 121.5(3) . . ? C41 C40 C39 120.8(3) . . ? C40 C41 C42 119.2(3) . . ? C41 C42 C43 120.2(3) . . ? C42 C43 C38 121.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zr1 N1 C7 -19.32(11) . . . . ? C30 Zr1 N1 C7 -73.38(14) . . . . ? C37 Zr1 N1 C7 -158.35(12) . . . . ? N3 Zr1 N1 C7 109.83(11) . . . . ? N4 Zr1 N1 C7 54.85(14) . . . . ? C23 Zr1 N1 C7 80.01(12) . . . . ? N2 Zr1 N1 C2 -174.1(2) . . . . ? C30 Zr1 N1 C2 131.8(2) . . . . ? C37 Zr1 N1 C2 46.9(2) . . . . ? N3 Zr1 N1 C2 -45.0(2) . . . . ? N4 Zr1 N1 C2 -99.9(2) . . . . ? C23 Zr1 N1 C2 -74.8(2) . . . . ? C7 Zr1 N1 C2 -154.8(3) . . . . ? N1 Zr1 N2 C7 19.30(10) . . . . ? C30 Zr1 N2 C7 159.74(12) . . . . ? C37 Zr1 N2 C7 74.09(13) . . . . ? N3 Zr1 N2 C7 -55.16(13) . . . . ? N4 Zr1 N2 C7 -112.17(11) . . . . ? C23 Zr1 N2 C7 -81.66(11) . . . . ? N1 Zr1 N2 C5 172.3(2) . . . . ? C30 Zr1 N2 C5 -47.27(19) . . . . ? C37 Zr1 N2 C5 -132.92(19) . . . . ? N3 Zr1 N2 C5 97.8(2) . . . . ? N4 Zr1 N2 C5 40.8(2) . . . . ? C23 Zr1 N2 C5 71.3(2) . . . . ? C7 Zr1 N2 C5 153.0(3) . . . . ? N2 Zr1 N3 C23 -56.48(13) . . . . ? N1 Zr1 N3 C23 -112.39(11) . . . . ? C30 Zr1 N3 C23 71.10(14) . . . . ? C37 Zr1 N3 C23 161.85(12) . . . . ? N4 Zr1 N3 C23 19.95(10) . . . . ? C7 Zr1 N3 C23 -82.38(11) . . . . ? N2 Zr1 N3 C28 78.9(2) . . . . ? N1 Zr1 N3 C28 22.95(19) . . . . ? C30 Zr1 N3 C28 -153.55(18) . . . . ? C37 Zr1 N3 C28 -62.80(19) . . . . ? N4 Zr1 N3 C28 155.3(2) . . . . ? C23 Zr1 N3 C28 135.3(2) . . . . ? C7 Zr1 N3 C28 53.0(2) . . . . ? N2 Zr1 N4 C23 108.32(11) . . . . ? N1 Zr1 N4 C23 52.25(13) . . . . ? C30 Zr1 N4 C23 -165.82(12) . . . . ? C37 Zr1 N4 C23 -78.62(14) . . . . ? N3 Zr1 N4 C23 -19.96(10) . . . . ? C7 Zr1 N4 C23 78.37(12) . . . . ? N2 Zr1 N4 C25 -32.5(2) . . . . ? N1 Zr1 N4 C25 -88.6(2) . . . . ? C30 Zr1 N4 C25 53.3(2) . . . . ? C37 Zr1 N4 C25 140.5(2) . . . . ? N3 Zr1 N4 C25 -160.8(2) . . . . ? C23 Zr1 N4 C25 -140.8(3) . . . . ? C7 Zr1 N4 C25 -62.5(2) . . . . ? C7 N1 C2 C3 -59.7(3) . . . . ? Zr1 N1 C2 C3 89.0(2) . . . . ? C7 N1 C2 C1 68.4(2) . . . . ? Zr1 N1 C2 C1 -142.86(18) . . . . ? C7 N2 C5 C4 -69.9(2) . . . . ? Zr1 N2 C5 C4 144.06(18) . . . . ? C7 N2 C5 C6 57.2(3) . . . . ? Zr1 N2 C5 C6 -88.8(2) . . . . ? C2 N1 C7 N2 -168.13(16) . . . . ? Zr1 N1 C7 N2 30.67(15) . . . . ? C2 N1 C7 C8 25.4(3) . . . . ? Zr1 N1 C7 C8 -135.79(16) . . . . ? C2 N1 C7 Zr1 161.2(2) . . . . ? C5 N2 C7 N1 170.54(16) . . . . ? Zr1 N2 C7 N1 -31.00(15) . . . . ? C5 N2 C7 C8 -23.0(3) . . . . ? Zr1 N2 C7 C8 135.40(15) . . . . ? C5 N2 C7 Zr1 -158.45(19) . . . . ? N2 Zr1 C7 N1 146.45(17) . . . . ? C30 Zr1 C7 N1 124.09(12) . . . . ? C37 Zr1 C7 N1 23.71(14) . . . . ? N3 Zr1 C7 N1 -76.66(12) . . . . ? N4 Zr1 C7 N1 -138.32(11) . . . . ? C23 Zr1 C7 N1 -107.70(12) . . . . ? N1 Zr1 C7 N2 -146.45(17) . . . . ? C30 Zr1 C7 N2 -22.36(13) . . . . ? C37 Zr1 C7 N2 -122.74(12) . . . . ? N3 Zr1 C7 N2 136.89(11) . . . . ? N4 Zr1 C7 N2 75.23(11) . . . . ? C23 Zr1 C7 N2 105.85(11) . . . . ? N2 Zr1 C7 C8 -106.5(3) . . . . ? N1 Zr1 C7 C8 107.1(3) . . . . ? C30 Zr1 C7 C8 -128.8(2) . . . . ? C37 Zr1 C7 C8 130.8(2) . . . . ? N3 Zr1 C7 C8 30.4(2) . . . . ? N4 Zr1 C7 C8 -31.2(2) . . . . ? C23 Zr1 C7 C8 -0.6(2) . . . . ? N1 C7 C8 C9 -95.4(3) . . . . ? N2 C7 C8 C9 99.7(2) . . . . ? Zr1 C7 C8 C9 -178.48(16) . . . . ? N1 C7 C8 C13 84.2(2) . . . . ? N2 C7 C8 C13 -80.6(2) . . . . ? Zr1 C7 C8 C13 1.1(3) . . . . ? C13 C8 C9 C10 -0.6(3) . . . . ? C7 C8 C9 C10 179.0(2) . . . . ? C8 C9 C10 C11 2.0(3) . . . . ? C9 C10 C11 C12 -1.2(3) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? C10 C11 C12 C15 175.3(2) . . . . ? C11 C12 C13 O1 -178.16(18) . . . . ? C15 C12 C13 O1 5.5(3) . . . . ? C11 C12 C13 C8 2.5(3) . . . . ? C15 C12 C13 C8 -173.75(18) . . . . ? C17 O1 C13 C12 -1.9(3) . . . . ? C17 O1 C13 C8 177.47(16) . . . . ? C9 C8 C13 C12 -1.8(3) . . . . ? C7 C8 C13 C12 178.58(18) . . . . ? C9 C8 C13 O1 178.88(17) . . . . ? C7 C8 C13 O1 -0.8(2) . . . . ? C13 C12 C15 C18 -5.8(3) . . . . ? C11 C12 C15 C18 178.14(18) . . . . ? C13 C12 C15 C14 -127.0(2) . . . . ? C11 C12 C15 C14 56.9(2) . . . . ? C13 C12 C15 C16 113.6(2) . . . . ? C11 C12 C15 C16 -62.5(3) . . . . ? C13 O1 C17 C18 -0.9(3) . . . . ? C13 O1 C17 C22 179.46(16) . . . . ? O1 C17 C18 C19 -178.93(17) . . . . ? C22 C17 C18 C19 0.7(3) . . . . ? O1 C17 C18 C15 -0.1(3) . . . . ? C22 C17 C18 C15 179.54(18) . . . . ? C12 C15 C18 C17 3.2(3) . . . . ? C14 C15 C18 C17 124.7(2) . . . . ? C16 C15 C18 C17 -115.5(2) . . . . ? C12 C15 C18 C19 -178.06(18) . . . . ? C14 C15 C18 C19 -56.5(2) . . . . ? C16 C15 C18 C19 63.3(2) . . . . ? C17 C18 C19 C20 -0.6(3) . . . . ? C15 C18 C19 C20 -179.44(19) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C20 C21 C22 C17 0.1(3) . . . . ? C20 C21 C22 C23 177.26(19) . . . . ? O1 C17 C22 C21 179.21(17) . . . . ? C18 C17 C22 C21 -0.4(3) . . . . ? O1 C17 C22 C23 1.7(2) . . . . ? C18 C17 C22 C23 -177.98(18) . . . . ? C28 N3 C23 N4 178.84(15) . . . . ? Zr1 N3 C23 N4 -33.33(15) . . . . ? C28 N3 C23 C22 -13.6(3) . . . . ? Zr1 N3 C23 C22 134.26(16) . . . . ? C28 N3 C23 Zr1 -147.83(17) . . . . ? C25 N4 C23 N3 -171.10(16) . . . . ? Zr1 N4 C23 N3 33.02(15) . . . . ? C25 N4 C23 C22 21.1(2) . . . . ? Zr1 N4 C23 C22 -134.74(16) . . . . ? C25 N4 C23 Zr1 155.88(17) . . . . ? C21 C22 C23 N3 101.5(2) . . . . ? C17 C22 C23 N3 -81.3(2) . . . . ? C21 C22 C23 N4 -91.9(2) . . . . ? C17 C22 C23 N4 85.4(2) . . . . ? C21 C22 C23 Zr1 -175.21(16) . . . . ? C17 C22 C23 Zr1 2.0(3) . . . . ? N2 Zr1 C23 N3 135.93(11) . . . . ? N1 Zr1 C23 N3 74.39(11) . . . . ? C30 Zr1 C23 N3 -129.18(11) . . . . ? C37 Zr1 C23 N3 -21.40(14) . . . . ? N4 Zr1 C23 N3 -145.35(17) . . . . ? C7 Zr1 C23 N3 105.07(11) . . . . ? N2 Zr1 C23 N4 -78.72(12) . . . . ? N1 Zr1 C23 N4 -140.26(10) . . . . ? C30 Zr1 C23 N4 16.17(13) . . . . ? C37 Zr1 C23 N4 123.95(12) . . . . ? N3 Zr1 C23 N4 145.35(17) . . . . ? C7 Zr1 C23 N4 -109.58(11) . . . . ? N2 Zr1 C23 C22 28.1(2) . . . . ? N1 Zr1 C23 C22 -33.4(2) . . . . ? C30 Zr1 C23 C22 123.0(2) . . . . ? C37 Zr1 C23 C22 -129.2(2) . . . . ? N3 Zr1 C23 C22 -107.8(2) . . . . ? N4 Zr1 C23 C22 106.9(2) . . . . ? C7 Zr1 C23 C22 -2.7(2) . . . . ? C23 N4 C25 C24 -159.73(17) . . . . ? Zr1 N4 C25 C24 -25.7(3) . . . . ? C23 N4 C25 C26 80.0(2) . . . . ? Zr1 N4 C25 C26 -145.96(18) . . . . ? C23 N3 C28 C29 168.34(17) . . . . ? Zr1 N3 C28 C29 42.2(3) . . . . ? C23 N3 C28 C27 -71.6(2) . . . . ? Zr1 N3 C28 C27 162.25(15) . . . . ? N2 Zr1 C30 C31 -176.95(14) . . . . ? N1 Zr1 C30 C31 -133.21(13) . . . . ? C37 Zr1 C30 C31 -49.88(14) . . . . ? N3 Zr1 C30 C31 42.37(18) . . . . ? N4 Zr1 C30 C31 83.97(14) . . . . ? C23 Zr1 C30 C31 75.78(15) . . . . ? C7 Zr1 C30 C31 -165.73(12) . . . . ? Zr1 C30 C31 C36 109.30(18) . . . . ? Zr1 C30 C31 C32 -67.2(2) . . . . ? C36 C31 C32 C33 0.3(3) . . . . ? C30 C31 C32 C33 176.9(2) . . . . ? C31 C32 C33 C34 -1.1(3) . . . . ? C32 C33 C34 C35 0.5(3) . . . . ? C33 C34 C35 C36 0.9(3) . . . . ? C34 C35 C36 C31 -1.7(3) . . . . ? C32 C31 C36 C35 1.1(3) . . . . ? C30 C31 C36 C35 -175.5(2) . . . . ? N2 Zr1 C37 C38 32.83(19) . . . . ? N1 Zr1 C37 C38 77.12(16) . . . . ? C30 Zr1 C37 C38 -51.45(16) . . . . ? N3 Zr1 C37 C38 174.64(16) . . . . ? N4 Zr1 C37 C38 -138.58(14) . . . . ? C23 Zr1 C37 C38 -174.59(14) . . . . ? C7 Zr1 C37 C38 65.25(17) . . . . ? Zr1 C37 C38 C43 -30.8(3) . . . . ? Zr1 C37 C38 C39 148.40(17) . . . . ? C43 C38 C39 C40 0.5(3) . . . . ? C37 C38 C39 C40 -178.8(2) . . . . ? C38 C39 C40 C41 0.7(4) . . . . ? C39 C40 C41 C42 -0.8(4) . . . . ? C40 C41 C42 C43 -0.2(4) . . . . ? C41 C42 C43 C38 1.4(4) . . . . ? C39 C38 C43 C42 -1.5(3) . . . . ? C37 C38 C43 C42 177.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.480 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.073