# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Moshe Kol' _publ_contact_author_email MOSHEKOL@POST.TAU.AC.IL _publ_section_title ; Construction of C1-Symmetric Zirconium Complexes by Designing of New Salan Ligands. Coordination Chemistry and Preliminary Polymerisation Catalysis Studies ; loop_ _publ_author_name 'Moshe Kol' 'Ad Cohen' 'I Goldberg' 'Jacob Kopilov' 'Adi Yeori' data_mk179 _database_code_depnum_ccdc_archive 'CCDC 673841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H60 Cl2 N2 O4 Zr' _chemical_formula_sum 'C38 H60 Cl2 N2 O4 Zr' _chemical_formula_weight 771.00 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 19.6465(4) _cell_length_b 10.6398(2) _cell_length_c 20.5229(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.2014(8) _cell_angle_gamma 90.00 _cell_volume 4026.10(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9418 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.21 _exptl_crystal_description needles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '0.5 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36196 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.21 _reflns_number_total 9543 _reflns_number_gt 5678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. Some of the t-butyl fragments are rotationally disordered. This disorder imparts to the crystals relatively large mosaicity. The ADP parameters of this disordered fragments are considerably higher than those of the remaining atoms in the molecular framework. ; _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^)+(0.0551P)^2^+2.8548P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9543 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _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 0.21633(2) 0.11033(3) 0.33699(2) 0.02263(11) Uani 1 1 d . . . O2 O 0.29945(14) -0.0100(2) 0.38356(14) 0.0261(6) Uani 1 1 d . . . O3 O 0.12737(14) 0.1977(2) 0.26410(14) 0.0256(6) Uani 1 1 d . . . O4 O 0.27275(15) 0.2615(2) 0.34498(15) 0.0295(7) Uani 1 1 d . . . O5 O 0.17795(14) 0.1099(2) 0.41185(14) 0.0282(6) Uani 1 1 d . . . N6 N 0.24731(17) 0.0328(3) 0.23770(17) 0.0249(7) Uani 1 1 d . . . N7 N 0.13539(17) -0.0684(3) 0.28113(17) 0.0230(7) Uani 1 1 d . . . C8 C 0.3539(2) -0.0777(3) 0.3745(2) 0.0239(9) Uani 1 1 d . . . C9 C 0.3969(2) -0.1616(3) 0.4262(2) 0.0224(8) Uani 1 1 d . . . C10 C 0.4474(2) -0.2346(3) 0.4085(2) 0.0277(9) Uani 1 1 d . . . H10 H 0.4757 -0.2932 0.4418 0.033 Uiso 1 1 calc R . . C11 C 0.4590(2) -0.2270(3) 0.3454(2) 0.0261(9) Uani 1 1 d . . . C12 C 0.4181(2) -0.1390(3) 0.2980(2) 0.0260(9) Uani 1 1 d . . . H12 H 0.4250 -0.1300 0.2546 0.031 Uiso 1 1 calc R . . C13 C 0.3673(2) -0.0639(3) 0.3126(2) 0.0239(9) Uani 1 1 d . . . C14 C 0.0669(2) 0.1729(3) 0.2124(2) 0.0262(9) Uani 1 1 d . . . C15 C 0.0400(2) 0.2526(3) 0.1552(2) 0.0275(9) Uani 1 1 d . . . C16 C -0.0220(2) 0.2263(4) 0.0997(2) 0.0325(10) Uani 1 1 d . . . H16 H -0.0385 0.2819 0.0612 0.039 Uiso 1 1 calc R . . C17 C -0.0597(2) 0.1168(4) 0.1012(2) 0.0338(9) Uani 1 1 d . . . C18 C -0.0352(2) 0.0354(4) 0.1565(2) 0.0320(10) Uani 1 1 d . . . H18 H -0.0619 -0.0388 0.1568 0.038 Uiso 1 1 calc R . . C19 C 0.0278(2) 0.0598(3) 0.2117(2) 0.0253(9) Uani 1 1 d . . . C20 C 0.2206(2) -0.1005(3) 0.2177(2) 0.0277(9) Uani 1 1 d . . . H20 H 0.2500 -0.1570 0.2561 0.033 Uiso 1 1 calc R . . C21 C 0.2310(2) -0.1455(4) 0.1509(2) 0.0305(9) Uani 1 1 d . . . H21A H 0.2074 -0.0852 0.1131 0.037 Uiso 1 1 calc R . . H21B H 0.2834 -0.1470 0.1580 0.037 Uiso 1 1 calc R . . C22 C 0.1993(3) -0.2757(4) 0.1294(3) 0.0419(12) Uani 1 1 d . . . H22A H 0.2262 -0.3380 0.1647 0.050 Uiso 1 1 calc R . . H22B H 0.2045 -0.2991 0.0847 0.050 Uiso 1 1 calc R . . C23 C 0.1195(2) -0.2776(4) 0.1219(2) 0.0378(11) Uani 1 1 d . . . H23A H 0.0993 -0.3626 0.1078 0.045 Uiso 1 1 calc R . . H23B H 0.0922 -0.2174 0.0854 0.045 Uiso 1 1 calc R . . C24 C 0.1112(2) -0.2419(3) 0.1906(2) 0.0309(10) Uani 1 1 d . . . H24A H 0.1368 -0.3043 0.2265 0.037 Uiso 1 1 calc R . . H24B H 0.0592 -0.2433 0.1855 0.037 Uiso 1 1 calc R . . C25 C 0.1422(2) -0.1111(3) 0.2137(2) 0.0267(8) Uani 1 1 d . . . H25 H 0.1136 -0.0509 0.1771 0.032 Uiso 1 1 calc R . . C26 C 0.2206(2) 0.1232(4) 0.1796(2) 0.0311(9) Uani 1 1 d . . . H26A H 0.2332 0.2088 0.1972 0.047 Uiso 1 1 calc R . . H26B H 0.1677 0.1159 0.1584 0.047 Uiso 1 1 calc R . . H26C H 0.2430 0.1048 0.1448 0.047 Uiso 1 1 calc R . . C27 C 0.1553(2) -0.1696(3) 0.3347(2) 0.0290(9) Uani 1 1 d . . . H27A H 0.1559 -0.1352 0.3792 0.043 Uiso 1 1 calc R . . H27B H 0.2035 -0.2023 0.3399 0.043 Uiso 1 1 calc R . . H27C H 0.1197 -0.2377 0.3204 0.043 Uiso 1 1 calc R . . C28 C 0.3906(2) -0.1674(4) 0.4985(2) 0.0292(9) Uani 1 1 d . . . C29 C 0.3155(2) -0.2127(4) 0.4944(2) 0.0363(10) Uani 1 1 d . . . H29A H 0.2789 -0.1519 0.4681 0.054 Uiso 1 1 calc R . . H29B H 0.3138 -0.2209 0.5414 0.054 Uiso 1 1 calc R . . H29C H 0.3056 -0.2946 0.4711 0.054 Uiso 1 1 calc R . . C30 C 0.4054(3) -0.0359(4) 0.5326(2) 0.0385(11) Uani 1 1 d . . . H30A H 0.4559 -0.0123 0.5411 0.058 Uiso 1 1 calc R . . H30B H 0.3965 -0.0379 0.5767 0.058 Uiso 1 1 calc R . . H30C H 0.3731 0.0257 0.5015 0.058 Uiso 1 1 calc R . . C31 C 0.4474(3) -0.2567(4) 0.5476(2) 0.0408(11) Uani 1 1 d . . . H31A H 0.4415 -0.3411 0.5273 0.061 Uiso 1 1 calc R . . H31B H 0.4405 -0.2601 0.5926 0.061 Uiso 1 1 calc R . . H31C H 0.4963 -0.2256 0.5540 0.061 Uiso 1 1 calc R . . C32 C 0.5163(2) -0.3061(3) 0.3284(2) 0.0278(9) Uani 1 1 d . . . C33 C 0.5824(3) -0.2250(5) 0.3390(4) 0.075(2) Uani 1 1 d . . . H33A H 0.6187 -0.2726 0.3263 0.113 Uiso 1 1 calc R . . H33B H 0.6029 -0.1998 0.3879 0.113 Uiso 1 1 calc R . . H33C H 0.5685 -0.1499 0.3097 0.113 Uiso 1 1 calc R . . C34 C 0.5384(3) -0.4222(5) 0.3742(3) 0.0674(19) Uani 1 1 d . . . H34A H 0.5700 -0.4751 0.3578 0.101 Uiso 1 1 calc R . . H34B H 0.4949 -0.4696 0.3720 0.101 Uiso 1 1 calc R . . H34C H 0.5644 -0.3964 0.4222 0.101 Uiso 1 1 calc R . . C35 C 0.4864(3) -0.3510(5) 0.2535(3) 0.0554(15) Uani 1 1 d . . . H35A H 0.4786 -0.2786 0.2222 0.083 Uiso 1 1 calc R . . H35B H 0.4402 -0.3944 0.2453 0.083 Uiso 1 1 calc R . . H35C H 0.5210 -0.4089 0.2446 0.083 Uiso 1 1 calc R . . C36 C 0.2975(2) 0.3882(4) 0.3532(2) 0.0375(10) Uani 1 1 d . . . C37 C 0.2329(3) 0.4736(4) 0.3384(3) 0.0678(18) Uani 1 1 d . . . H37A H 0.1978 0.4547 0.2923 0.102 Uiso 1 1 calc R . . H37B H 0.2486 0.5613 0.3399 0.102 Uiso 1 1 calc R . . H37C H 0.2101 0.4605 0.3735 0.102 Uiso 1 1 calc R . . C38 C 0.3474(3) 0.4061(5) 0.4265(3) 0.077(2) Uani 1 1 d . . . H38A H 0.3202 0.3948 0.4582 0.115 Uiso 1 1 calc R . . H38B H 0.3679 0.4910 0.4320 0.115 Uiso 1 1 calc R . . H38C H 0.3867 0.3442 0.4374 0.115 Uiso 1 1 calc R . . C39 C 0.3352(5) 0.4114(6) 0.3013(5) 0.080(4) Uani 1 1 d . . . H39A H 0.3769 0.3548 0.3111 0.120 Uiso 1 1 calc R . . H39B H 0.3519 0.4988 0.3049 0.120 Uiso 1 1 calc R . . H39C H 0.3013 0.3955 0.2543 0.120 Uiso 1 1 calc R . . C40 C 0.1569(2) 0.1327(4) 0.4706(2) 0.0300(9) Uani 1 1 d . . . C41 C 0.1139(5) 0.0202(5) 0.4807(4) 0.079(3) Uani 1 1 d . . . H41A H 0.0714 0.0076 0.4387 0.119 Uiso 1 1 calc R . . H41B H 0.0981 0.0353 0.5203 0.119 Uiso 1 1 calc R . . H41C H 0.1445 -0.0551 0.4894 0.119 Uiso 1 1 calc R . . C42 C 0.1066(5) 0.2409(7) 0.4566(4) 0.085(3) Uani 1 1 d . . . H42A H 0.1313 0.3161 0.4484 0.127 Uiso 1 1 calc R . . H42B H 0.0913 0.2549 0.4967 0.127 Uiso 1 1 calc R . . H42C H 0.0640 0.2234 0.4155 0.127 Uiso 1 1 calc R . . C43 C 0.2214(4) 0.1488(10) 0.5328(4) 0.078(4) Uani 1 1 d . . . H43A H 0.2540 0.0771 0.5374 0.119 Uiso 1 1 calc R . . H43B H 0.2068 0.1538 0.5738 0.119 Uiso 1 1 calc R . . H43C H 0.2465 0.2264 0.5287 0.119 Uiso 1 1 calc R . . Cl44 Cl 0.08684(6) 0.39151(9) 0.15477(6) 0.0358(3) Uani 1 1 d . . . Cl45 Cl -0.14103(7) 0.09012(11) 0.03350(7) 0.0523(3) Uani 1 1 d . . . C46 C 0.3287(2) 0.0368(3) 0.2613(2) 0.0244(8) Uani 1 1 d . . . H46A H 0.3452 0.1199 0.2826 0.029 Uiso 1 1 calc R . . H46B H 0.3435 0.0295 0.2200 0.029 Uiso 1 1 calc R . . C47 C 0.0582(2) -0.0310(3) 0.2703(2) 0.0253(9) Uani 1 1 d . . . H47A H 0.0275 -0.1074 0.2608 0.030 Uiso 1 1 calc R . . H47B H 0.0562 0.0075 0.3135 0.030 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 0.0237(2) 0.01755(17) 0.0277(2) 0.00094(16) 0.01013(16) 0.00134(15) O2 0.0267(15) 0.0235(13) 0.0291(16) 0.0033(11) 0.0110(13) 0.0046(11) O3 0.0209(15) 0.0223(13) 0.0323(17) 0.0017(11) 0.0075(13) 0.0008(10) O4 0.0274(16) 0.0195(13) 0.0411(19) 0.0004(12) 0.0110(14) 0.0004(11) O5 0.0319(16) 0.0273(13) 0.0288(16) -0.0011(12) 0.0149(13) 0.0021(12) N6 0.0266(19) 0.0238(16) 0.026(2) 0.0054(13) 0.0116(16) 0.0019(13) N7 0.0244(18) 0.0218(15) 0.0252(19) 0.0019(13) 0.0115(15) 0.0028(12) C8 0.021(2) 0.0168(18) 0.033(2) -0.0002(15) 0.0094(18) 0.0018(14) C9 0.022(2) 0.0171(17) 0.026(2) -0.0003(15) 0.0058(18) 0.0004(14) C10 0.029(2) 0.0196(18) 0.032(3) 0.0013(16) 0.008(2) 0.0039(15) C11 0.025(2) 0.0226(19) 0.031(2) -0.0038(16) 0.0103(19) 0.0017(15) C12 0.028(2) 0.027(2) 0.026(2) 0.0023(15) 0.0129(19) 0.0021(15) C13 0.024(2) 0.0186(17) 0.029(2) 0.0027(15) 0.0086(18) 0.0015(14) C14 0.026(2) 0.0256(19) 0.031(2) -0.0007(17) 0.015(2) 0.0055(16) C15 0.033(2) 0.0238(19) 0.031(3) 0.0056(16) 0.017(2) 0.0040(16) C16 0.040(3) 0.031(2) 0.026(3) 0.0061(17) 0.011(2) 0.0077(18) C17 0.029(2) 0.043(2) 0.025(2) -0.0017(19) 0.0025(19) 0.0048(19) C18 0.032(2) 0.030(2) 0.032(3) -0.0035(17) 0.008(2) -0.0028(17) C19 0.028(2) 0.0249(18) 0.026(2) -0.0018(16) 0.0133(19) 0.0024(15) C20 0.034(2) 0.0238(19) 0.026(2) -0.0023(16) 0.0121(19) -0.0013(16) C21 0.033(2) 0.032(2) 0.030(3) -0.0038(17) 0.016(2) 0.0000(16) C22 0.053(3) 0.035(2) 0.042(3) -0.009(2) 0.022(3) 0.002(2) C23 0.044(3) 0.031(2) 0.042(3) -0.0079(19) 0.020(2) -0.0064(19) C24 0.038(3) 0.023(2) 0.035(3) -0.0026(17) 0.017(2) -0.0052(17) C25 0.033(2) 0.0214(18) 0.028(2) -0.0031(17) 0.0144(19) -0.0020(16) C26 0.027(2) 0.031(2) 0.038(3) 0.0101(18) 0.015(2) 0.0044(17) C27 0.034(2) 0.0192(18) 0.035(3) 0.0028(17) 0.014(2) -0.0026(16) C28 0.032(2) 0.028(2) 0.027(2) 0.0046(17) 0.011(2) 0.0113(17) C29 0.046(3) 0.039(2) 0.027(3) 0.0082(18) 0.016(2) 0.0039(19) C30 0.046(3) 0.038(2) 0.032(3) -0.0081(19) 0.014(2) 0.003(2) C31 0.047(3) 0.046(3) 0.027(3) 0.007(2) 0.011(2) 0.019(2) C32 0.030(2) 0.025(2) 0.031(2) 0.0006(16) 0.013(2) 0.0073(16) C33 0.037(3) 0.050(3) 0.153(7) -0.040(4) 0.051(4) -0.007(2) C34 0.090(5) 0.059(3) 0.072(4) 0.030(3) 0.052(4) 0.054(3) C35 0.053(3) 0.068(3) 0.039(3) -0.012(2) 0.009(3) 0.028(3) C36 0.042(3) 0.0205(19) 0.052(3) -0.0045(19) 0.019(2) -0.0058(18) C37 0.069(4) 0.023(2) 0.086(5) -0.012(2) -0.006(3) 0.015(2) C38 0.058(4) 0.037(3) 0.097(5) -0.021(3) -0.022(3) -0.003(2) C39 0.093(10) 0.062(4) 0.086(9) -0.032(5) 0.042(9) -0.036(5) C40 0.036(2) 0.031(2) 0.025(2) -0.0034(16) 0.013(2) 0.0033(17) C41 0.096(9) 0.059(4) 0.081(5) -0.017(3) 0.059(6) -0.036(4) C42 0.082(7) 0.090(6) 0.084(6) 0.039(5) 0.040(5) 0.043(5) C43 0.053(4) 0.121(11) 0.060(5) -0.028(6) 0.018(4) -0.003(6) Cl44 0.0367(6) 0.0272(5) 0.0439(7) 0.0114(5) 0.0146(5) 0.0025(4) Cl45 0.0470(8) 0.0545(7) 0.0390(7) 0.0016(6) -0.0060(6) -0.0054(6) C46 0.025(2) 0.0229(19) 0.028(2) 0.0034(16) 0.0116(18) -0.0003(15) C47 0.025(2) 0.0256(19) 0.031(2) -0.0025(16) 0.0157(19) -0.0043(15) _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 O4 1.928(2) . ? Zr1 O5 1.931(3) . ? Zr1 O2 2.035(2) . ? Zr1 O3 2.086(3) . ? Zr1 N6 2.462(3) . ? Zr1 N7 2.490(3) . ? O2 C8 1.355(4) . ? O3 C14 1.317(5) . ? O4 C36 1.423(4) . ? O5 C40 1.425(5) . ? N6 C26 1.480(5) . ? N6 C46 1.503(5) . ? N6 C20 1.518(5) . ? N7 C27 1.492(5) . ? N7 C25 1.506(5) . ? N7 C47 1.508(5) . ? C8 C13 1.392(5) . ? C8 C9 1.420(5) . ? C9 C10 1.402(5) . ? C9 C28 1.534(6) . ? C10 C11 1.391(6) . ? C10 H10 0.9500 . ? C11 C12 1.389(5) . ? C11 C32 1.541(5) . ? C12 C13 1.390(5) . ? C12 H12 0.9500 . ? C13 C46 1.509(5) . ? C14 C15 1.397(5) . ? C14 C19 1.424(5) . ? C15 C16 1.379(6) . ? C15 Cl44 1.743(4) . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.377(6) . ? C17 Cl45 1.740(4) . ? C18 C19 1.383(6) . ? C18 H18 0.9500 . ? C19 C47 1.497(5) . ? C20 C25 1.517(5) . ? C20 C21 1.531(5) . ? C20 H20 1.0000 . ? C21 C22 1.521(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.522(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.523(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.528(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.527(6) . ? C28 C31 1.545(5) . ? C28 C30 1.545(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.510(6) . ? C32 C35 1.521(6) . ? C32 C34 1.522(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C38 1.497(7) . ? C36 C37 1.506(6) . ? C36 C39 1.512(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C43 1.465(8) . ? C40 C42 1.478(7) . ? C40 C41 1.519(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? 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 O4 Zr1 O5 107.76(11) . . ? O4 Zr1 O2 98.07(11) . . ? O5 Zr1 O2 95.48(11) . . ? O4 Zr1 O3 90.21(10) . . ? O5 Zr1 O3 96.36(11) . . ? O2 Zr1 O3 162.75(10) . . ? O4 Zr1 N6 92.92(11) . . ? O5 Zr1 N6 159.05(10) . . ? O2 Zr1 N6 77.89(10) . . ? O3 Zr1 N6 86.63(10) . . ? O4 Zr1 N7 158.96(11) . . ? O5 Zr1 N7 90.11(11) . . ? O2 Zr1 N7 90.98(10) . . ? O3 Zr1 N7 76.50(10) . . ? N6 Zr1 N7 70.37(10) . . ? C8 O2 Zr1 144.5(2) . . ? C14 O3 Zr1 141.9(2) . . ? C36 O4 Zr1 164.4(3) . . ? C40 O5 Zr1 168.7(2) . . ? C26 N6 C46 106.5(3) . . ? C26 N6 C20 113.4(3) . . ? C46 N6 C20 110.1(3) . . ? C26 N6 Zr1 109.2(2) . . ? C46 N6 Zr1 105.3(2) . . ? C20 N6 Zr1 112.0(2) . . ? C27 N7 C25 112.1(3) . . ? C27 N7 C47 107.1(3) . . ? C25 N7 C47 110.4(3) . . ? C27 N7 Zr1 104.4(2) . . ? C25 N7 Zr1 114.1(2) . . ? C47 N7 Zr1 108.4(2) . . ? O2 C8 C13 118.4(3) . . ? O2 C8 C9 121.8(3) . . ? C13 C8 C9 119.8(3) . . ? C10 C9 C8 116.5(4) . . ? C10 C9 C28 122.0(3) . . ? C8 C9 C28 121.4(3) . . ? C11 C10 C9 124.5(4) . . ? C11 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? C12 C11 C10 116.8(3) . . ? C12 C11 C32 120.0(4) . . ? C10 C11 C32 123.1(3) . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 120.8(3) . . ? C12 C13 C46 118.9(4) . . ? C8 C13 C46 120.3(3) . . ? O3 C14 C15 122.0(3) . . ? O3 C14 C19 120.7(3) . . ? C15 C14 C19 117.2(4) . . ? C16 C15 C14 122.8(4) . . ? C16 C15 Cl44 119.1(3) . . ? C14 C15 Cl44 118.1(3) . . ? C15 C16 C17 118.6(4) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? C18 C17 C16 120.6(4) . . ? C18 C17 Cl45 121.3(3) . . ? C16 C17 Cl45 118.0(3) . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C14 119.6(4) . . ? C18 C19 C47 122.1(3) . . ? C14 C19 C47 118.2(4) . . ? C25 C20 N6 109.5(3) . . ? C25 C20 C21 112.0(3) . . ? N6 C20 C21 113.1(3) . . ? C25 C20 H20 107.3 . . ? N6 C20 H20 107.3 . . ? C21 C20 H20 107.3 . . ? C22 C21 C20 112.2(3) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 110.2(3) . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 109.8(4) . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 110.8(3) . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N7 C25 C20 109.8(3) . . ? N7 C25 C24 114.0(3) . . ? C20 C25 C24 112.0(3) . . ? N7 C25 H25 106.9 . . ? C20 C25 H25 106.9 . . ? C24 C25 H25 106.9 . . ? N6 C26 H26A 109.5 . . ? N6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 H27A 109.5 . . ? N7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C9 111.0(3) . . ? C29 C28 C31 108.0(3) . . ? C9 C28 C31 111.9(3) . . ? C29 C28 C30 109.8(3) . . ? C9 C28 C30 109.7(3) . . ? C31 C28 C30 106.4(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C35 109.8(4) . . ? C33 C32 C34 109.1(4) . . ? C35 C32 C34 107.3(4) . . ? C33 C32 C11 108.3(3) . . ? C35 C32 C11 110.1(3) . . ? C34 C32 C11 112.1(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O4 C36 C38 108.6(4) . . ? O4 C36 C37 108.5(4) . . ? C38 C36 C37 109.8(4) . . ? O4 C36 C39 107.5(4) . . ? C38 C36 C39 112.2(5) . . ? C37 C36 C39 110.1(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O5 C40 C43 109.9(4) . . ? O5 C40 C42 109.7(4) . . ? C43 C40 C42 113.4(6) . . ? O5 C40 C41 108.6(3) . . ? C43 C40 C41 109.2(6) . . ? C42 C40 C41 106.0(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C46 C13 115.2(3) . . ? N6 C46 H46A 108.5 . . ? C13 C46 H46A 108.5 . . ? N6 C46 H46B 108.5 . . ? C13 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C19 C47 N7 113.0(3) . . ? C19 C47 H47A 109.0 . . ? N7 C47 H47A 109.0 . . ? C19 C47 H47B 109.0 . . ? N7 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.195 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.092 #=========================================================== data_mk180 _database_code_depnum_ccdc_archive 'CCDC 673842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Cl2 N2 O4 Zr, C5 H12' _chemical_formula_sum 'C39 H66 Cl2 N2 O4 Zr' _chemical_formula_weight 789.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/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 15.1736(2) _cell_length_b 15.2555(2) _cell_length_c 36.9388(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.8897(6) _cell_angle_gamma 90.00 _cell_volume 8519.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 15694 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.18 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45312 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.18 _reflns_number_total 20076 _reflns_number_gt 11535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. One of the t-Bu groups shows rotational disorder, which could not be resolved by discrete atoms. The same applies to one of the pentane solvent molecules. ; _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^)+(0.0845P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20076 _refine_ls_number_parameters 897 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 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 0.84475(2) 0.14071(2) 0.084518(9) 0.02408(10) Uani 1 1 d . . . O2 O 0.86170(15) 0.27103(14) 0.07862(6) 0.0273(5) Uani 1 1 d . . . O3 O 0.86344(14) 0.00891(15) 0.07652(6) 0.0283(6) Uani 1 1 d . . . O4 O 0.72141(15) 0.13668(15) 0.06814(6) 0.0304(6) Uani 1 1 d . . . O5 O 0.85465(15) 0.13925(14) 0.13730(6) 0.0284(5) Uani 1 1 d . . . N6 N 0.89183(19) 0.15315(17) 0.02257(8) 0.0270(7) Uani 1 1 d . . . N7 N 1.00874(18) 0.12415(18) 0.08880(8) 0.0259(6) Uani 1 1 d . . . C8 C 0.8550(2) 0.3365(2) 0.05407(9) 0.0249(8) Uani 1 1 d . . . C9 C 0.8521(2) 0.4252(2) 0.06549(9) 0.0272(8) Uani 1 1 d . . . C10 C 0.8470(2) 0.4902(2) 0.03859(10) 0.0279(8) Uani 1 1 d . . . H10 H 0.8454 0.5497 0.0460 0.033 Uiso 1 1 calc R . . C11 C 0.8442(2) 0.4724(2) 0.00162(10) 0.0283(8) Uani 1 1 d . . . C12 C 0.8461(2) 0.3843(2) -0.00845(10) 0.0293(8) Uani 1 1 d . . . H12 H 0.8448 0.3702 -0.0335 0.035 Uiso 1 1 calc R . . C13 C 0.8499(2) 0.3161(2) 0.01677(9) 0.0267(8) Uani 1 1 d . . . C14 C 0.8394(2) 0.2245(2) 0.00284(9) 0.0295(8) Uani 1 1 d . . . H14A H 0.8545 0.2243 -0.0227 0.035 Uiso 1 1 calc R . . H14B H 0.7760 0.2089 0.0026 0.035 Uiso 1 1 calc R . . C15 C 0.8735(2) 0.0726(2) 0.00070(10) 0.0343(9) Uani 1 1 d . . . H15A H 0.8862 0.0835 -0.0245 0.051 Uiso 1 1 calc R . . H15B H 0.8112 0.0563 0.0013 0.051 Uiso 1 1 calc R . . H15C H 0.9111 0.0247 0.0108 0.051 Uiso 1 1 calc R . . C16 C 0.9869(2) 0.1747(2) 0.02457(10) 0.0312(8) Uani 1 1 d . . . H16A H 0.9957 0.2366 0.0321 0.037 Uiso 1 1 calc R . . H16B H 1.0089 0.1678 0.0003 0.037 Uiso 1 1 calc R . . C17 C 1.0398(2) 0.1148(2) 0.05180(10) 0.0303(8) Uani 1 1 d . . . H17A H 1.0329 0.0531 0.0437 0.036 Uiso 1 1 calc R . . H17B H 1.1034 0.1300 0.0526 0.036 Uiso 1 1 calc R . . C18 C 1.0498(2) 0.2028(2) 0.10692(10) 0.0331(9) Uani 1 1 d . . . H18A H 1.0307 0.2077 0.1315 0.050 Uiso 1 1 calc R . . H18B H 1.0315 0.2553 0.0930 0.050 Uiso 1 1 calc R . . H18C H 1.1144 0.1973 0.1083 0.050 Uiso 1 1 calc R . . C19 C 1.0368(2) 0.0476(2) 0.11217(10) 0.0290(8) Uani 1 1 d . . . H19A H 1.0130 0.0554 0.1361 0.035 Uiso 1 1 calc R . . H19B H 1.1022 0.0482 0.1163 0.035 Uiso 1 1 calc R . . C20 C 1.0084(2) -0.0419(2) 0.09740(9) 0.0280(8) Uani 1 1 d . . . C21 C 0.9234(2) -0.0558(2) 0.08033(9) 0.0275(8) Uani 1 1 d . . . C22 C 0.9029(2) -0.1392(2) 0.06667(9) 0.0300(8) Uani 1 1 d . . . C23 C 0.9592(2) -0.2096(2) 0.07224(9) 0.0330(9) Uani 1 1 d . . . H23 H 0.9425 -0.2663 0.0634 0.040 Uiso 1 1 calc R . . C24 C 1.0405(2) -0.1955(2) 0.09097(10) 0.0333(9) Uani 1 1 d . . . C25 C 1.0661(2) -0.1120(2) 0.10272(10) 0.0306(8) Uani 1 1 d . . . H25 H 1.1235 -0.1029 0.1145 0.037 Uiso 1 1 calc R . . C26 C 0.8505(2) 0.4488(2) 0.10579(10) 0.0280(8) Uani 1 1 d . . . C27 C 0.7676(2) 0.4099(3) 0.12042(10) 0.0375(9) Uani 1 1 d . . . H27A H 0.7149 0.4344 0.1070 0.056 Uiso 1 1 calc R . . H27B H 0.7670 0.4243 0.1463 0.056 Uiso 1 1 calc R . . H27C H 0.7679 0.3461 0.1174 0.056 Uiso 1 1 calc R . . C28 C 0.9326(2) 0.4133(3) 0.12848(10) 0.0389(10) Uani 1 1 d . . . H28A H 0.9340 0.3492 0.1266 0.058 Uiso 1 1 calc R . . H28B H 0.9301 0.4302 0.1540 0.058 Uiso 1 1 calc R . . H28C H 0.9861 0.4378 0.1193 0.058 Uiso 1 1 calc R . . C29 C 0.8497(3) 0.5481(2) 0.11156(11) 0.0486(11) Uani 1 1 d . . . H29A H 0.9042 0.5735 0.1037 0.073 Uiso 1 1 calc R . . H29B H 0.8457 0.5608 0.1374 0.073 Uiso 1 1 calc R . . H29C H 0.7986 0.5736 0.0973 0.073 Uiso 1 1 calc R . . C30 C 0.8382(2) 0.5441(2) -0.02752(10) 0.0315(8) Uani 1 1 d . . . C31 C 0.8497(3) 0.6358(2) -0.01061(11) 0.0483(11) Uani 1 1 d . . . H31A H 0.8034 0.6460 0.0058 0.072 Uiso 1 1 calc R . . H31B H 0.8453 0.6801 -0.0299 0.072 Uiso 1 1 calc R . . H31C H 0.9079 0.6399 0.0030 0.072 Uiso 1 1 calc R . . C32 C 0.9109(3) 0.5320(3) -0.05347(11) 0.0492(11) Uani 1 1 d . . . H32A H 0.9689 0.5318 -0.0395 0.074 Uiso 1 1 calc R . . H32B H 0.9084 0.5804 -0.0710 0.074 Uiso 1 1 calc R . . H32C H 0.9020 0.4763 -0.0664 0.074 Uiso 1 1 calc R . . C33 C 0.7470(2) 0.5395(3) -0.04914(11) 0.0462(11) Uani 1 1 d . . . H33A H 0.7384 0.4810 -0.0598 0.069 Uiso 1 1 calc R . . H33B H 0.7440 0.5834 -0.0686 0.069 Uiso 1 1 calc R . . H33C H 0.7007 0.5512 -0.0329 0.069 Uiso 1 1 calc R . . C34 C 0.6292(2) 0.1355(3) 0.05834(11) 0.0363(9) Uani 1 1 d . . . C35 C 0.5992(3) 0.2291(3) 0.04930(14) 0.0638(14) Uani 1 1 d . . . H35A H 0.6087 0.2657 0.0711 0.096 Uiso 1 1 calc R . . H35B H 0.5363 0.2291 0.0408 0.096 Uiso 1 1 calc R . . H35C H 0.6336 0.2527 0.0302 0.096 Uiso 1 1 calc R . . C36 C 0.6122(3) 0.0761(3) 0.02556(12) 0.0565(13) Uani 1 1 d . . . H36A H 0.6352 0.1038 0.0043 0.085 Uiso 1 1 calc R . . H36B H 0.5485 0.0663 0.0208 0.085 Uiso 1 1 calc R . . H36C H 0.6421 0.0198 0.0304 0.085 Uiso 1 1 calc R . . C37 C 0.5835(3) 0.0999(3) 0.09044(12) 0.0606(14) Uani 1 1 d . . . H37A H 0.6095 0.0432 0.0979 0.091 Uiso 1 1 calc R . . H37B H 0.5202 0.0924 0.0833 0.091 Uiso 1 1 calc R . . H37C H 0.5914 0.1412 0.1108 0.091 Uiso 1 1 calc R . . C38 C 0.8363(2) 0.1212(2) 0.17330(10) 0.0310(9) Uani 1 1 d . . . C39 C 0.7532(2) 0.1701(3) 0.18115(10) 0.0425(10) Uani 1 1 d . . . H39A H 0.7625 0.2332 0.1783 0.064 Uiso 1 1 calc R . . H39B H 0.7395 0.1579 0.2061 0.064 Uiso 1 1 calc R . . H39C H 0.7038 0.1510 0.1642 0.064 Uiso 1 1 calc R . . C40 C 0.9145(2) 0.1529(3) 0.19923(11) 0.0449(11) Uani 1 1 d . . . H40A H 0.9682 0.1210 0.1941 0.067 Uiso 1 1 calc R . . H40B H 0.9018 0.1420 0.2244 0.067 Uiso 1 1 calc R . . H40C H 0.9235 0.2158 0.1957 0.067 Uiso 1 1 calc R . . C41 C 0.8241(3) 0.0225(3) 0.17686(12) 0.0538(12) Uani 1 1 d . . . H41A H 0.7770 0.0027 0.1589 0.081 Uiso 1 1 calc R . . H41B H 0.8081 0.0087 0.2014 0.081 Uiso 1 1 calc R . . H41C H 0.8795 -0.0073 0.1726 0.081 Uiso 1 1 calc R . . Cl42 Cl 1.11200(7) -0.28401(6) 0.10002(3) 0.0448(3) Uani 1 1 d . . . Cl43 Cl 0.80020(7) -0.15562(6) 0.04266(3) 0.0456(3) Uani 1 1 d . . . Zr44 Zr 0.63794(2) 0.40986(2) 0.292167(9) 0.02710(10) Uani 1 1 d . . . O45 O 0.55610(15) 0.39954(15) 0.24552(6) 0.0309(6) Uani 1 1 d . . . O46 O 0.68698(15) 0.44022(15) 0.34511(6) 0.0310(6) Uani 1 1 d . . . O47 O 0.64956(15) 0.28713(15) 0.30154(7) 0.0311(6) Uani 1 1 d . . . O48 O 0.74051(14) 0.44784(15) 0.26885(6) 0.0314(6) Uani 1 1 d . . . N49 N 0.48909(18) 0.4187(2) 0.31355(8) 0.0324(7) Uani 1 1 d . . . N50 N 0.5977(2) 0.56695(19) 0.29840(8) 0.0336(7) Uani 1 1 d . . . C51 C 0.4725(2) 0.3858(2) 0.23151(10) 0.0295(8) Uani 1 1 d . . . C52 C 0.4478(2) 0.3932(2) 0.19378(10) 0.0269(8) Uani 1 1 d . . . C53 C 0.3575(2) 0.3862(2) 0.18251(10) 0.0297(8) Uani 1 1 d . . . H53 H 0.3402 0.3923 0.1573 0.036 Uiso 1 1 calc R . . C54 C 0.2915(2) 0.3708(2) 0.20561(10) 0.0287(8) Uani 1 1 d . . . C55 C 0.3191(2) 0.3587(2) 0.24228(10) 0.0305(8) Uani 1 1 d . . . H55 H 0.2762 0.3459 0.2588 0.037 Uiso 1 1 calc R . . C56 C 0.4077(2) 0.3649(2) 0.25535(10) 0.0304(8) Uani 1 1 d . . . C57 C 0.4340(2) 0.3482(2) 0.29475(10) 0.0358(9) Uani 1 1 d . . . H57A H 0.3796 0.3406 0.3075 0.043 Uiso 1 1 calc R . . H57B H 0.4673 0.2924 0.2970 0.043 Uiso 1 1 calc R . . C58 C 0.4909(2) 0.4008(3) 0.35307(10) 0.0414(10) Uani 1 1 d . . . H58A H 0.4302 0.3974 0.3602 0.062 Uiso 1 1 calc R . . H58B H 0.5226 0.4481 0.3666 0.062 Uiso 1 1 calc R . . H58C H 0.5212 0.3450 0.3586 0.062 Uiso 1 1 calc R . . C59 C 0.4489(2) 0.5059(2) 0.30523(11) 0.0385(10) Uani 1 1 d . . . H59A H 0.3953 0.5127 0.3185 0.046 Uiso 1 1 calc R . . H59B H 0.4309 0.5099 0.2789 0.046 Uiso 1 1 calc R . . C60 C 0.5137(2) 0.5789(2) 0.31608(11) 0.0375(9) Uani 1 1 d . . . H60A H 0.4869 0.6361 0.3088 0.045 Uiso 1 1 calc R . . H60B H 0.5265 0.5791 0.3428 0.045 Uiso 1 1 calc R . . C61 C 0.5894(3) 0.6050(2) 0.26143(10) 0.0410(10) Uani 1 1 d . . . H61A H 0.5423 0.5746 0.2465 0.062 Uiso 1 1 calc R . . H61B H 0.6454 0.5982 0.2504 0.062 Uiso 1 1 calc R . . H61C H 0.5748 0.6674 0.2629 0.062 Uiso 1 1 calc R . . C62 C 0.6713(2) 0.6161(2) 0.31977(10) 0.0353(9) Uani 1 1 d . . . H62A H 0.7278 0.6032 0.3093 0.042 Uiso 1 1 calc R . . H62B H 0.6601 0.6798 0.3172 0.042 Uiso 1 1 calc R . . C63 C 0.6801(2) 0.5928(2) 0.35942(10) 0.0316(9) Uani 1 1 d . . . C64 C 0.6777(2) 0.6576(2) 0.38573(11) 0.0362(9) Uani 1 1 d . . . H64 H 0.6720 0.7173 0.3786 0.043 Uiso 1 1 calc R . . C65 C 0.6836(2) 0.6358(2) 0.42229(11) 0.0374(10) Uani 1 1 d . . . C66 C 0.6918(2) 0.5494(2) 0.43339(11) 0.0349(9) Uani 1 1 d . . . H66 H 0.6956 0.5344 0.4584 0.042 Uiso 1 1 calc R . . C67 C 0.6944(2) 0.4847(2) 0.40679(10) 0.0290(8) Uani 1 1 d . . . C68 C 0.6884(2) 0.5035(2) 0.36973(10) 0.0304(8) Uani 1 1 d . . . C69 C 0.5171(2) 0.4055(2) 0.16605(10) 0.0298(8) Uani 1 1 d . . . C70 C 0.5800(2) 0.3268(2) 0.16885(11) 0.0409(10) Uani 1 1 d . . . H70A H 0.6089 0.3232 0.1936 0.061 Uiso 1 1 calc R . . H70B H 0.6249 0.3339 0.1515 0.061 Uiso 1 1 calc R . . H70C H 0.5465 0.2729 0.1633 0.061 Uiso 1 1 calc R . . C71 C 0.4757(2) 0.4088(3) 0.12663(10) 0.0380(9) Uani 1 1 d . . . H71A H 0.4439 0.3540 0.1208 0.057 Uiso 1 1 calc R . . H71B H 0.5225 0.4162 0.1102 0.057 Uiso 1 1 calc R . . H71C H 0.4345 0.4582 0.1237 0.057 Uiso 1 1 calc R . . C72 C 0.5698(2) 0.4914(2) 0.17353(10) 0.0357(9) Uani 1 1 d . . . H72A H 0.5291 0.5413 0.1718 0.054 Uiso 1 1 calc R . . H72B H 0.6132 0.4980 0.1555 0.054 Uiso 1 1 calc R . . H72C H 0.6006 0.4892 0.1979 0.054 Uiso 1 1 calc R . . C73 C 0.1925(2) 0.3686(2) 0.19295(10) 0.0319(9) Uani 1 1 d . . . C74 C 0.1532(2) 0.2786(3) 0.20105(12) 0.0463(11) Uani 1 1 d . . . H74A H 0.1830 0.2331 0.1879 0.069 Uiso 1 1 calc R . . H74B H 0.0898 0.2784 0.1932 0.069 Uiso 1 1 calc R . . H74C H 0.1617 0.2670 0.2272 0.069 Uiso 1 1 calc R . . C75 C 0.1761(3) 0.3858(3) 0.15206(11) 0.0509(12) Uani 1 1 d . . . H75A H 0.1969 0.4447 0.1466 0.076 Uiso 1 1 calc R . . H75B H 0.1127 0.3812 0.1447 0.076 Uiso 1 1 calc R . . H75C H 0.2084 0.3424 0.1387 0.076 Uiso 1 1 calc R . . C76 C 0.1443(2) 0.4382(3) 0.21357(12) 0.0454(11) Uani 1 1 d . . . H76A H 0.1510 0.4251 0.2396 0.068 Uiso 1 1 calc R . . H76B H 0.0814 0.4382 0.2050 0.068 Uiso 1 1 calc R . . H76C H 0.1696 0.4960 0.2093 0.068 Uiso 1 1 calc R . . C77 C 0.8282(2) 0.4576(2) 0.25840(10) 0.0324(9) Uani 1 1 d . . . C78 C 0.8902(2) 0.4631(3) 0.29304(12) 0.0560(13) Uani 1 1 d . . . H78A H 0.8744 0.5140 0.3073 0.084 Uiso 1 1 calc R . . H78B H 0.9513 0.4692 0.2867 0.084 Uiso 1 1 calc R . . H78C H 0.8847 0.4096 0.3074 0.084 Uiso 1 1 calc R . . C79 C 0.8324(3) 0.5406(3) 0.23581(12) 0.0554(12) Uani 1 1 d . . . H79A H 0.7891 0.5369 0.2146 0.083 Uiso 1 1 calc R . . H79B H 0.8919 0.5471 0.2277 0.083 Uiso 1 1 calc R . . H79C H 0.8187 0.5915 0.2506 0.083 Uiso 1 1 calc R . . C80 C 0.8498(3) 0.3781(3) 0.23618(12) 0.0467(11) Uani 1 1 d . . . H80A H 0.8458 0.3250 0.2509 0.070 Uiso 1 1 calc R . . H80B H 0.9099 0.3837 0.2286 0.070 Uiso 1 1 calc R . . H80C H 0.8076 0.3741 0.2146 0.070 Uiso 1 1 calc R . . C81 C 0.6789(3) 0.2002(2) 0.31157(10) 0.0356(9) Uani 1 1 d . . . C82 C 0.6317(3) 0.1369(3) 0.28514(12) 0.0549(13) Uani 1 1 d . . . H82A H 0.5676 0.1429 0.2861 0.082 Uiso 1 1 calc R . . H82B H 0.6496 0.0768 0.2916 0.082 Uiso 1 1 calc R . . H82C H 0.6472 0.1499 0.2605 0.082 Uiso 1 1 calc R . . C83 C 0.7788(3) 0.1971(3) 0.30903(12) 0.0481(11) Uani 1 1 d . . . H83A H 0.7913 0.1997 0.2835 0.072 Uiso 1 1 calc R . . H83B H 0.8025 0.1424 0.3198 0.072 Uiso 1 1 calc R . . H83C H 0.8066 0.2470 0.3222 0.072 Uiso 1 1 calc R . . C84 C 0.6565(3) 0.1823(3) 0.34989(11) 0.0496(11) Uani 1 1 d . . . H84A H 0.6881 0.2238 0.3665 0.074 Uiso 1 1 calc R . . H84B H 0.6741 0.1223 0.3567 0.074 Uiso 1 1 calc R . . H84C H 0.5926 0.1890 0.3513 0.074 Uiso 1 1 calc R . . Cl85 Cl 0.70130(6) 0.37565(6) 0.42069(3) 0.0369(2) Uani 1 1 d . . . Cl86 Cl 0.67587(8) 0.71775(7) 0.45477(3) 0.0542(3) Uani 1 1 d . . . C87 C 0.5904(3) 0.5094(4) 0.03870(15) 0.0792(17) Uani 1 1 d . . . H87A H 0.5837 0.5120 0.0121 0.119 Uiso 1 1 calc R . . H87B H 0.5693 0.4526 0.0468 0.119 Uiso 1 1 calc R . . H87C H 0.6529 0.5167 0.0473 0.119 Uiso 1 1 calc R . . C88 C 0.5353(4) 0.5840(3) 0.05445(15) 0.0791(17) Uani 1 1 d . . . H88A H 0.4725 0.5769 0.0452 0.095 Uiso 1 1 calc R . . H88B H 0.5388 0.5781 0.0812 0.095 Uiso 1 1 calc R . . C89 C 0.5649(3) 0.6734(4) 0.04521(14) 0.0667(14) Uani 1 1 d . . . H89A H 0.5643 0.6782 0.0185 0.080 Uiso 1 1 calc R . . H89B H 0.6268 0.6813 0.0555 0.080 Uiso 1 1 calc R . . C90 C 0.5097(3) 0.7463(4) 0.05875(14) 0.0682(14) Uani 1 1 d . . . H90A H 0.5046 0.7379 0.0851 0.082 Uiso 1 1 calc R . . H90B H 0.4495 0.7428 0.0462 0.082 Uiso 1 1 calc R . . C91 C 0.5476(3) 0.8378(4) 0.05265(15) 0.0759(16) Uani 1 1 d . . . H91A H 0.6068 0.8423 0.0654 0.114 Uiso 1 1 calc R . . H91B H 0.5089 0.8822 0.0620 0.114 Uiso 1 1 calc R . . H91C H 0.5515 0.8473 0.0266 0.114 Uiso 1 1 calc R . . C92 C 0.0257(4) 0.2326(4) 0.30328(18) 0.109(2) Uani 1 1 d . . . H92A H 0.0166 0.1791 0.3171 0.163 Uiso 1 1 calc R . . H92B H 0.0207 0.2191 0.2772 0.163 Uiso 1 1 calc R . . H92C H -0.0191 0.2762 0.3084 0.163 Uiso 1 1 calc R . . C93 C 0.1132(6) 0.2676(5) 0.3138(2) 0.167(4) Uani 1 1 d . . . H93A H 0.1536 0.2340 0.2993 0.200 Uiso 1 1 calc R . . H93B H 0.1122 0.3280 0.3040 0.200 Uiso 1 1 calc R . . C94 C 0.1555(5) 0.2740(4) 0.34659(17) 0.101(2) Uani 1 1 d . . . H94A H 0.1382 0.2207 0.3595 0.121 Uiso 1 1 calc R . . H94B H 0.1265 0.3235 0.3582 0.121 Uiso 1 1 calc R . . C95 C 0.2466(5) 0.2845(5) 0.3572(2) 0.125(3) Uani 1 1 d . . . H95A H 0.2515 0.3016 0.3832 0.150 Uiso 1 1 calc R . . H95B H 0.2672 0.3352 0.3435 0.150 Uiso 1 1 calc R . . C96 C 0.3142(4) 0.2089(4) 0.35324(18) 0.097(2) Uani 1 1 d . . . H96A H 0.3074 0.1646 0.3720 0.146 Uiso 1 1 calc R . . H96B H 0.3745 0.2326 0.3560 0.146 Uiso 1 1 calc R . . H96C H 0.3033 0.1821 0.3292 0.146 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 0.02392(18) 0.02542(19) 0.02278(19) 0.00018(14) 0.00120(14) 0.00159(14) O2 0.0342(14) 0.0255(13) 0.0222(13) 0.0027(10) 0.0035(10) 0.0037(10) O3 0.0287(13) 0.0264(13) 0.0291(14) 0.0015(10) -0.0019(11) -0.0021(10) O4 0.0229(13) 0.0359(14) 0.0318(15) -0.0003(11) -0.0004(11) 0.0019(11) O5 0.0315(13) 0.0313(14) 0.0224(13) 0.0023(10) 0.0030(10) 0.0009(11) N6 0.0319(17) 0.0236(16) 0.0255(16) -0.0005(12) 0.0015(13) 0.0019(13) N7 0.0261(16) 0.0279(16) 0.0239(16) -0.0024(12) 0.0036(12) -0.0015(12) C8 0.0186(17) 0.0291(19) 0.0263(19) -0.0015(15) -0.0014(15) -0.0007(14) C9 0.0235(18) 0.031(2) 0.027(2) -0.0009(15) 0.0016(15) -0.0019(15) C10 0.0282(19) 0.0245(19) 0.031(2) -0.0011(15) 0.0007(16) 0.0024(15) C11 0.0255(18) 0.029(2) 0.030(2) 0.0026(16) -0.0003(16) -0.0002(15) C12 0.030(2) 0.034(2) 0.0233(19) -0.0017(15) 0.0024(16) -0.0011(16) C13 0.0273(19) 0.0285(19) 0.0240(19) -0.0009(15) 0.0008(15) 0.0030(15) C14 0.038(2) 0.0270(19) 0.0229(19) -0.0001(15) -0.0021(16) 0.0001(16) C15 0.046(2) 0.027(2) 0.030(2) -0.0031(16) 0.0037(18) 0.0035(17) C16 0.035(2) 0.031(2) 0.029(2) 0.0001(16) 0.0093(16) 0.0013(16) C17 0.029(2) 0.034(2) 0.029(2) -0.0010(16) 0.0092(16) 0.0039(16) C18 0.027(2) 0.029(2) 0.043(2) -0.0069(17) 0.0013(17) -0.0045(16) C19 0.0263(19) 0.029(2) 0.031(2) 0.0016(16) -0.0041(16) 0.0061(15) C20 0.029(2) 0.030(2) 0.025(2) 0.0009(15) 0.0028(16) 0.0063(16) C21 0.034(2) 0.0275(19) 0.0209(19) 0.0037(15) 0.0023(16) 0.0041(16) C22 0.036(2) 0.0280(19) 0.0248(19) -0.0034(16) -0.0032(16) 0.0018(16) C23 0.046(2) 0.028(2) 0.026(2) -0.0028(16) 0.0050(18) 0.0038(17) C24 0.046(2) 0.028(2) 0.026(2) 0.0047(16) 0.0044(18) 0.0096(17) C25 0.035(2) 0.033(2) 0.024(2) 0.0022(16) 0.0029(16) 0.0060(16) C26 0.0285(19) 0.0270(19) 0.029(2) -0.0010(15) 0.0032(16) 0.0009(15) C27 0.035(2) 0.046(2) 0.032(2) -0.0034(18) 0.0087(17) 0.0039(18) C28 0.035(2) 0.052(3) 0.030(2) -0.0057(18) 0.0022(17) 0.0011(19) C29 0.078(3) 0.033(2) 0.036(2) -0.0047(19) 0.008(2) 0.009(2) C30 0.029(2) 0.033(2) 0.033(2) 0.0028(17) 0.0013(16) 0.0013(16) C31 0.066(3) 0.033(2) 0.045(3) 0.0096(19) -0.003(2) -0.007(2) C32 0.055(3) 0.046(3) 0.049(3) 0.022(2) 0.021(2) 0.013(2) C33 0.046(3) 0.044(2) 0.048(3) 0.015(2) -0.007(2) -0.002(2) C34 0.0235(19) 0.049(2) 0.035(2) -0.0034(19) -0.0058(17) 0.0003(17) C35 0.044(3) 0.067(3) 0.078(4) -0.004(3) -0.008(3) 0.023(2) C36 0.047(3) 0.072(3) 0.048(3) -0.014(2) -0.007(2) -0.013(2) C37 0.032(2) 0.108(4) 0.042(3) 0.007(3) 0.001(2) -0.013(2) C38 0.037(2) 0.033(2) 0.022(2) 0.0023(15) -0.0026(16) -0.0029(16) C39 0.033(2) 0.063(3) 0.032(2) -0.008(2) 0.0042(18) 0.009(2) C40 0.034(2) 0.062(3) 0.037(2) -0.007(2) -0.0059(18) 0.011(2) C41 0.066(3) 0.044(3) 0.053(3) 0.016(2) 0.013(2) -0.004(2) Cl42 0.0596(7) 0.0366(5) 0.0374(6) 0.0040(4) 0.0004(5) 0.0202(5) Cl43 0.0436(6) 0.0340(5) 0.0565(7) -0.0075(5) -0.0118(5) -0.0020(4) Zr44 0.02239(18) 0.0301(2) 0.0284(2) 0.00241(15) 0.00017(14) -0.00002(14) O45 0.0212(13) 0.0411(15) 0.0300(14) 0.0033(11) -0.0001(11) -0.0028(11) O46 0.0335(14) 0.0299(14) 0.0291(14) 0.0002(11) -0.0010(11) 0.0020(11) O47 0.0271(13) 0.0279(13) 0.0378(15) -0.0011(11) -0.0003(11) -0.0020(10) O48 0.0229(13) 0.0359(14) 0.0353(15) 0.0022(11) 0.0011(11) -0.0033(11) N49 0.0256(16) 0.047(2) 0.0240(17) 0.0031(14) -0.0005(13) 0.0031(14) N50 0.0332(17) 0.0353(18) 0.0313(18) 0.0037(14) -0.0024(14) 0.0037(14) C51 0.0232(19) 0.034(2) 0.031(2) -0.0009(16) 0.0006(16) 0.0012(15) C52 0.0255(19) 0.0270(19) 0.028(2) -0.0005(15) 0.0006(16) 0.0021(15) C53 0.030(2) 0.0296(19) 0.029(2) -0.0054(16) -0.0005(16) -0.0017(15) C54 0.0227(18) 0.034(2) 0.029(2) 0.0017(16) -0.0037(16) -0.0005(15) C55 0.0230(19) 0.036(2) 0.033(2) 0.0014(17) 0.0052(16) -0.0039(16) C56 0.0220(19) 0.039(2) 0.029(2) 0.0015(16) -0.0019(16) -0.0025(16) C57 0.030(2) 0.047(2) 0.030(2) 0.0085(18) 0.0024(17) -0.0086(17) C58 0.026(2) 0.070(3) 0.029(2) 0.003(2) 0.0007(17) -0.0043(19) C59 0.027(2) 0.050(3) 0.038(2) -0.0030(19) -0.0005(18) 0.0063(18) C60 0.034(2) 0.042(2) 0.035(2) -0.0053(18) -0.0039(18) 0.0081(18) C61 0.045(2) 0.039(2) 0.039(2) 0.0077(19) -0.0018(19) 0.0094(19) C62 0.035(2) 0.029(2) 0.041(2) 0.0040(17) 0.0032(18) -0.0014(16) C63 0.0229(19) 0.032(2) 0.039(2) -0.0019(17) 0.0003(16) -0.0024(16) C64 0.030(2) 0.032(2) 0.046(3) -0.0020(18) -0.0050(18) -0.0031(16) C65 0.026(2) 0.039(2) 0.046(3) -0.0197(19) -0.0035(18) -0.0051(17) C66 0.030(2) 0.039(2) 0.034(2) -0.0015(18) -0.0047(17) -0.0035(17) C67 0.0222(18) 0.030(2) 0.034(2) 0.0023(16) 0.0006(16) -0.0028(15) C68 0.0189(18) 0.037(2) 0.035(2) -0.0019(17) 0.0009(16) 0.0002(16) C69 0.0276(19) 0.030(2) 0.032(2) 0.0015(16) 0.0045(16) 0.0012(16) C70 0.039(2) 0.038(2) 0.049(3) -0.0017(19) 0.0193(19) 0.0032(18) C71 0.036(2) 0.052(3) 0.027(2) 0.0006(18) 0.0077(17) -0.0031(18) C72 0.037(2) 0.035(2) 0.036(2) 0.0026(17) 0.0083(18) -0.0016(17) C73 0.0223(19) 0.040(2) 0.032(2) -0.0015(17) -0.0009(16) -0.0005(16) C74 0.029(2) 0.050(3) 0.059(3) -0.002(2) -0.001(2) -0.0088(19) C75 0.029(2) 0.088(3) 0.034(2) 0.004(2) -0.0069(19) 0.000(2) C76 0.030(2) 0.049(3) 0.056(3) -0.007(2) -0.005(2) 0.0043(19) C77 0.0254(19) 0.040(2) 0.032(2) -0.0032(17) 0.0067(16) -0.0062(16) C78 0.023(2) 0.078(3) 0.065(3) -0.015(3) -0.005(2) -0.010(2) C79 0.065(3) 0.043(3) 0.062(3) 0.007(2) 0.033(2) -0.008(2) C80 0.044(2) 0.050(3) 0.048(3) -0.009(2) 0.015(2) -0.004(2) C81 0.046(2) 0.028(2) 0.031(2) -0.0004(16) -0.0028(18) -0.0060(17) C82 0.073(3) 0.042(3) 0.047(3) -0.003(2) -0.010(2) -0.020(2) C83 0.050(3) 0.040(2) 0.052(3) 0.003(2) -0.005(2) 0.012(2) C84 0.072(3) 0.037(2) 0.040(3) 0.003(2) 0.002(2) -0.006(2) Cl85 0.0406(6) 0.0381(5) 0.0309(5) 0.0030(4) -0.0031(4) -0.0011(4) Cl86 0.0622(7) 0.0469(6) 0.0510(7) -0.0198(5) -0.0093(6) -0.0026(5) C87 0.071(4) 0.103(5) 0.063(4) 0.017(3) 0.005(3) 0.010(3) C88 0.117(5) 0.067(4) 0.056(4) -0.006(3) 0.019(3) -0.019(3) C89 0.056(3) 0.092(4) 0.051(3) 0.014(3) -0.001(2) 0.002(3) C90 0.063(3) 0.086(4) 0.055(3) -0.003(3) 0.000(3) 0.008(3) C91 0.066(4) 0.099(5) 0.062(4) -0.001(3) 0.001(3) -0.006(3) C92 0.074(4) 0.117(6) 0.135(6) -0.040(5) 0.002(4) 0.015(4) C93 0.208(9) 0.162(8) 0.115(7) 0.054(6) -0.078(7) -0.110(7) C94 0.135(6) 0.071(4) 0.094(5) 0.024(4) -0.003(5) -0.023(4) C95 0.098(6) 0.175(9) 0.107(6) 0.018(5) 0.042(5) -0.025(6) C96 0.090(5) 0.073(4) 0.131(6) 0.035(4) 0.023(4) -0.012(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 O4 1.918(2) . ? Zr1 O5 1.943(2) . ? Zr1 O2 2.019(2) . ? Zr1 O3 2.055(2) . ? Zr1 N6 2.462(3) . ? Zr1 N7 2.493(3) . ? O2 C8 1.347(4) . ? O3 C21 1.342(4) . ? O4 C34 1.415(4) . ? O5 C38 1.409(4) . ? N6 C16 1.476(4) . ? N6 C15 1.484(4) . ? N6 C14 1.500(4) . ? N7 C18 1.485(4) . ? N7 C17 1.490(4) . ? N7 C19 1.493(4) . ? C8 C13 1.408(5) . ? C8 C9 1.418(5) . ? C9 C10 1.401(5) . ? C9 C26 1.534(5) . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.396(5) . ? C11 C30 1.531(5) . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 C14 1.493(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.534(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.519(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.384(5) . ? C20 C21 1.403(5) . ? C21 C22 1.395(5) . ? C22 C23 1.377(5) . ? C22 Cl43 1.743(4) . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.391(5) . ? C24 Cl42 1.746(3) . ? C25 H25 0.9500 . ? C26 C27 1.530(5) . ? C26 C29 1.530(5) . ? C26 C28 1.540(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.533(5) . ? C30 C31 1.536(5) . ? C30 C33 1.539(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C36 1.517(5) . ? C34 C37 1.524(6) . ? C34 C35 1.528(5) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.515(5) . ? C38 C41 1.523(5) . ? C38 C40 1.539(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? Zr44 O47 1.909(2) . ? Zr44 O48 1.931(2) . ? Zr44 O45 2.042(2) . ? Zr44 O46 2.085(2) . ? Zr44 N49 2.459(3) . ? Zr44 N50 2.488(3) . ? O45 C51 1.345(4) . ? O46 C68 1.325(4) . ? O47 C81 1.437(4) . ? O48 C77 1.425(4) . ? N49 C58 1.483(4) . ? N49 C59 1.484(4) . ? N49 C57 1.497(4) . ? N50 C61 1.480(5) . ? N50 C60 1.493(5) . ? N50 C62 1.510(4) . ? C51 C56 1.411(5) . ? C51 C52 1.417(5) . ? C52 C53 1.401(5) . ? C52 C69 1.540(5) . ? C53 C54 1.390(5) . ? C53 H53 0.9500 . ? C54 C55 1.396(5) . ? C54 C73 1.535(5) . ? C55 C56 1.392(4) . ? C55 H55 0.9500 . ? C56 C57 1.498(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.517(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.502(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.389(5) . ? C63 C68 1.417(5) . ? C64 C65 1.386(5) . ? C64 H64 0.9500 . ? C65 C66 1.384(5) . ? C65 Cl86 1.743(4) . ? C66 C67 1.395(5) . ? C66 H66 0.9500 . ? C67 C68 1.394(5) . ? C67 Cl85 1.741(4) . ? C69 C70 1.532(5) . ? C69 C71 1.537(5) . ? C69 C72 1.548(5) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C76 1.529(5) . ? C73 C75 1.532(5) . ? C73 C74 1.536(5) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C80 1.516(5) . ? C77 C79 1.522(5) . ? C77 C78 1.524(5) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C84 1.509(5) . ? C81 C82 1.510(5) . ? C81 C83 1.527(5) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C87 C88 1.554(7) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 C89 1.484(7) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.503(7) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.533(7) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 C93 1.452(8) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 C94 1.324(8) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.413(8) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.559(8) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zr1 O5 107.83(10) . . ? O4 Zr1 O2 97.32(9) . . ? O5 Zr1 O2 96.89(9) . . ? O4 Zr1 O3 93.80(9) . . ? O5 Zr1 O3 97.66(9) . . ? O2 Zr1 O3 158.03(10) . . ? O4 Zr1 N6 93.55(10) . . ? O5 Zr1 N6 158.42(9) . . ? O2 Zr1 N6 76.94(9) . . ? O3 Zr1 N6 83.53(9) . . ? O4 Zr1 N7 163.46(10) . . ? O5 Zr1 N7 86.77(9) . . ? O2 Zr1 N7 88.34(9) . . ? O3 Zr1 N7 76.16(9) . . ? N6 Zr1 N7 72.52(9) . . ? C8 O2 Zr1 143.1(2) . . ? C21 O3 Zr1 143.6(2) . . ? C34 O4 Zr1 176.3(2) . . ? C38 O5 Zr1 160.9(2) . . ? C16 N6 C15 110.4(3) . . ? C16 N6 C14 109.8(3) . . ? C15 N6 C14 105.7(3) . . ? C16 N6 Zr1 109.3(2) . . ? C15 N6 Zr1 112.7(2) . . ? C14 N6 Zr1 108.9(2) . . ? C18 N7 C17 109.7(3) . . ? C18 N7 C19 106.5(3) . . ? C17 N7 C19 111.0(3) . . ? C18 N7 Zr1 109.0(2) . . ? C17 N7 Zr1 110.08(19) . . ? C19 N7 Zr1 110.5(2) . . ? O2 C8 C13 119.3(3) . . ? O2 C8 C9 120.6(3) . . ? C13 C8 C9 120.1(3) . . ? C10 C9 C8 117.7(3) . . ? C10 C9 C26 121.2(3) . . ? C8 C9 C26 121.1(3) . . ? C11 C10 C9 123.7(3) . . ? C11 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? C10 C11 C12 116.7(3) . . ? C10 C11 C30 123.2(3) . . ? C12 C11 C30 120.1(3) . . ? C13 C12 C11 122.8(3) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C8 119.0(3) . . ? C12 C13 C14 118.1(3) . . ? C8 C13 C14 122.6(3) . . ? C13 C14 N6 118.4(3) . . ? C13 C14 H14A 107.7 . . ? N6 C14 H14A 107.7 . . ? C13 C14 H14B 107.7 . . ? N6 C14 H14B 107.7 . . ? H14A C14 H14B 107.1 . . ? N6 C15 H15A 109.5 . . ? N6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N6 C16 C17 110.7(3) . . ? N6 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N7 C17 C16 110.8(3) . . ? N7 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? N7 C18 H18A 109.5 . . ? N7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N7 C19 C20 115.9(3) . . ? N7 C19 H19A 108.3 . . ? C20 C19 H19A 108.3 . . ? N7 C19 H19B 108.3 . . ? C20 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? C25 C20 C21 119.6(3) . . ? C25 C20 C19 119.1(3) . . ? C21 C20 C19 121.3(3) . . ? O3 C21 C22 120.3(3) . . ? O3 C21 C20 121.7(3) . . ? C22 C21 C20 118.0(3) . . ? C23 C22 C21 122.7(3) . . ? C23 C22 Cl43 118.7(3) . . ? C21 C22 Cl43 118.5(3) . . ? C22 C23 C24 118.1(3) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C23 C24 C25 120.9(3) . . ? C23 C24 Cl42 119.3(3) . . ? C25 C24 Cl42 119.8(3) . . ? C20 C25 C24 120.5(3) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C27 C26 C29 108.6(3) . . ? C27 C26 C9 109.5(3) . . ? C29 C26 C9 111.6(3) . . ? C27 C26 C28 108.8(3) . . ? C29 C26 C28 106.8(3) . . ? C9 C26 C28 111.5(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C11 C30 C32 110.5(3) . . ? C11 C30 C31 111.5(3) . . ? C32 C30 C31 107.5(3) . . ? C11 C30 C33 109.3(3) . . ? C32 C30 C33 109.5(3) . . ? C31 C30 C33 108.6(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O4 C34 C36 108.0(3) . . ? O4 C34 C37 108.1(3) . . ? C36 C34 C37 110.6(4) . . ? O4 C34 C35 108.2(3) . . ? C36 C34 C35 110.9(3) . . ? C37 C34 C35 110.9(4) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 C39 108.6(3) . . ? O5 C38 C41 108.1(3) . . ? C39 C38 C41 111.2(3) . . ? O5 C38 C40 108.8(3) . . ? C39 C38 C40 109.7(3) . . ? C41 C38 C40 110.4(3) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O47 Zr44 O48 108.04(10) . . ? O47 Zr44 O45 96.75(9) . . ? O48 Zr44 O45 95.86(10) . . ? O47 Zr44 O46 91.59(10) . . ? O48 Zr44 O46 96.60(10) . . ? O45 Zr44 O46 162.07(9) . . ? O47 Zr44 N49 93.93(10) . . ? O48 Zr44 N49 157.54(10) . . ? O45 Zr44 N49 76.48(9) . . ? O46 Zr44 N49 87.17(9) . . ? O47 Zr44 N50 161.28(11) . . ? O48 Zr44 N50 88.03(10) . . ? O45 Zr44 N50 90.92(9) . . ? O46 Zr44 N50 76.70(9) . . ? N49 Zr44 N50 71.24(10) . . ? C51 O45 Zr44 145.3(2) . . ? C68 O46 Zr44 142.1(2) . . ? C81 O47 Zr44 166.7(2) . . ? C77 O48 Zr44 163.6(2) . . ? C58 N49 C59 110.0(3) . . ? C58 N49 C57 106.7(3) . . ? C59 N49 C57 110.1(3) . . ? C58 N49 Zr44 111.4(2) . . ? C59 N49 Zr44 110.8(2) . . ? C57 N49 Zr44 107.7(2) . . ? C61 N50 C60 110.3(3) . . ? C61 N50 C62 106.8(3) . . ? C60 N50 C62 109.4(3) . . ? C61 N50 Zr44 107.2(2) . . ? C60 N50 Zr44 112.6(2) . . ? C62 N50 Zr44 110.5(2) . . ? O45 C51 C56 118.7(3) . . ? O45 C51 C52 121.9(3) . . ? C56 C51 C52 119.5(3) . . ? C53 C52 C51 117.1(3) . . ? C53 C52 C69 121.1(3) . . ? C51 C52 C69 121.7(3) . . ? C54 C53 C52 124.6(3) . . ? C54 C53 H53 117.7 . . ? C52 C53 H53 117.7 . . ? C53 C54 C55 116.4(3) . . ? C53 C54 C73 123.7(3) . . ? C55 C54 C73 119.9(3) . . ? C56 C55 C54 122.0(3) . . ? C56 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? C55 C56 C51 120.1(3) . . ? C55 C56 C57 119.7(3) . . ? C51 C56 C57 120.2(3) . . ? N49 C57 C56 114.9(3) . . ? N49 C57 H57A 108.6 . . ? C56 C57 H57A 108.6 . . ? N49 C57 H57B 108.6 . . ? C56 C57 H57B 108.6 . . ? H57A C57 H57B 107.5 . . ? N49 C58 H58A 109.5 . . ? N49 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? N49 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N49 C59 C60 111.0(3) . . ? N49 C59 H59A 109.4 . . ? C60 C59 H59A 109.4 . . ? N49 C59 H59B 109.4 . . ? C60 C59 H59B 109.4 . . ? H59A C59 H59B 108.0 . . ? N50 C60 C59 110.7(3) . . ? N50 C60 H60A 109.5 . . ? C59 C60 H60A 109.5 . . ? N50 C60 H60B 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? N50 C61 H61A 109.5 . . ? N50 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N50 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 N50 113.1(3) . . ? C63 C62 H62A 109.0 . . ? N50 C62 H62A 109.0 . . ? C63 C62 H62B 109.0 . . ? N50 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C64 C63 C68 120.2(4) . . ? C64 C63 C62 120.6(3) . . ? C68 C63 C62 119.2(3) . . ? C65 C64 C63 120.5(4) . . ? C65 C64 H64 119.7 . . ? C63 C64 H64 119.7 . . ? C66 C65 C64 120.9(3) . . ? C66 C65 Cl86 119.3(3) . . ? C64 C65 Cl86 119.8(3) . . ? C65 C66 C67 118.2(4) . . ? C65 C66 H66 120.9 . . ? C67 C66 H66 120.9 . . ? C68 C67 C66 122.8(3) . . ? C68 C67 Cl85 118.9(3) . . ? C66 C67 Cl85 118.2(3) . . ? O46 C68 C67 121.3(3) . . ? O46 C68 C63 121.3(3) . . ? C67 C68 C63 117.3(3) . . ? C70 C69 C71 106.9(3) . . ? C70 C69 C52 108.5(3) . . ? C71 C69 C52 112.8(3) . . ? C70 C69 C72 109.9(3) . . ? C71 C69 C72 107.7(3) . . ? C52 C69 C72 110.9(3) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C76 C73 C75 109.1(3) . . ? C76 C73 C54 109.3(3) . . ? C75 C73 C54 111.6(3) . . ? C76 C73 C74 108.3(3) . . ? C75 C73 C74 108.2(3) . . ? C54 C73 C74 110.2(3) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O48 C77 C80 108.3(3) . . ? O48 C77 C79 108.6(3) . . ? C80 C77 C79 110.4(3) . . ? O48 C77 C78 107.6(3) . . ? C80 C77 C78 110.6(3) . . ? C79 C77 C78 111.3(3) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O47 C81 C84 108.6(3) . . ? O47 C81 C82 107.7(3) . . ? C84 C81 C82 111.0(3) . . ? O47 C81 C83 107.5(3) . . ? C84 C81 C83 110.9(3) . . ? C82 C81 C83 111.0(4) . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C88 C87 H87A 109.5 . . ? C88 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C88 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C89 C88 C87 113.8(5) . . ? C89 C88 H88A 108.8 . . ? C87 C88 H88A 108.8 . . ? C89 C88 H88B 108.8 . . ? C87 C88 H88B 108.8 . . ? H88A C88 H88B 107.7 . . ? C88 C89 C90 114.5(5) . . ? C88 C89 H89A 108.6 . . ? C90 C89 H89A 108.6 . . ? C88 C89 H89B 108.6 . . ? C90 C89 H89B 108.6 . . ? H89A C89 H89B 107.6 . . ? C89 C90 C91 113.5(5) . . ? C89 C90 H90A 108.9 . . ? C91 C90 H90A 108.9 . . ? C89 C90 H90B 108.9 . . ? C91 C90 H90B 108.9 . . ? H90A C90 H90B 107.7 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C93 C92 H92A 109.5 . . ? C93 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C93 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C94 C93 C92 129.3(8) . . ? C94 C93 H93A 104.9 . . ? C92 C93 H93A 105.0 . . ? C94 C93 H93B 105.0 . . ? C92 C93 H93B 105.0 . . ? H93A C93 H93B 105.8 . . ? C93 C94 C95 130.5(8) . . ? C93 C94 H94A 104.7 . . ? C95 C94 H94A 104.7 . . ? C93 C94 H94B 104.6 . . ? C95 C94 H94B 104.7 . . ? H94A C94 H94B 105.7 . . ? C94 C95 C96 121.7(7) . . ? C94 C95 H95A 106.9 . . ? C96 C95 H95A 106.9 . . ? C94 C95 H95B 106.9 . . ? C96 C95 H95B 106.9 . . ? H95A C95 H95B 106.7 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.208 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.091 # Attachment 'mk182j.cif' data_mk182j _database_code_depnum_ccdc_archive 'CCDC 673843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C40 H50 Cl2 N2 O2 Zr), 5(C4 H10 O)' _chemical_formula_sum 'C180 H250 Cl8 N8 O13 Zr4' _chemical_formula_weight 3382.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M 'I ba2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 28.4938(6) _cell_length_b 17.8978(3) _cell_length_c 17.8233(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9089.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5528 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3572 _exptl_absorpt_coefficient_mu 0.398 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29291 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.87 _reflns_number_total 9894 _reflns_number_gt 7350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. One of the t-Bu groups is severely disordered. The diethyl ether solvent is disordered as well. SIMU retraints were applied to the ADP's of this disordered t-Bu group. DFIX restraints were applied to the two unique bonds of the diethyl ether solvent located on the twofold axis. 75 restraints in total. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.3115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 9894 _refine_ls_number_parameters 533 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.740490(11) 0.725199(17) 0.79490(5) 0.03085(9) Uani 1 1 d . . . N2 N 0.77340(11) 0.84560(17) 0.83843(18) 0.0330(7) Uani 1 1 d . A . N3 N 0.70229(12) 0.76085(17) 0.91504(18) 0.0321(7) Uani 1 1 d . . . O4 O 0.80073(9) 0.69350(15) 0.84219(15) 0.0351(6) Uani 1 1 d . . . O5 O 0.68039(10) 0.77437(15) 0.76336(16) 0.0368(6) Uani 1 1 d . . . C6 C 0.77242(17) 0.7597(2) 0.6808(2) 0.0423(10) Uani 1 1 d . . . H6A H 0.7551 0.8004 0.6554 0.051 Uiso 1 1 calc R . . H6B H 0.8064 0.7708 0.6831 0.051 Uiso 1 1 calc R . . C7 C 0.71003(14) 0.6049(2) 0.8067(2) 0.0379(9) Uani 1 1 d . . . H7A H 0.7188 0.5783 0.7600 0.046 Uiso 1 1 calc R . . H7B H 0.7280 0.5809 0.8476 0.046 Uiso 1 1 calc R . . C8 C 0.83965(14) 0.7149(2) 0.8821(2) 0.0325(8) Uani 1 1 d . . . C9 C 0.86677(14) 0.6630(2) 0.9221(2) 0.0341(8) Uani 1 1 d . . . C10 C 0.85650(14) 0.5785(2) 0.9206(2) 0.0362(9) Uani 1 1 d . . . C11 C 0.89390(17) 0.5330(2) 0.9628(3) 0.0461(11) Uani 1 1 d . . . H11A H 0.8922 0.5444 1.0165 0.069 Uiso 1 1 calc R . . H11B H 0.9251 0.5461 0.9438 0.069 Uiso 1 1 calc R . . H11C H 0.8882 0.4796 0.9550 0.069 Uiso 1 1 calc R . . C12 C 0.85639(17) 0.5497(2) 0.8391(2) 0.0449(10) Uani 1 1 d . . . H12A H 0.8861 0.5629 0.8148 0.067 Uiso 1 1 calc R . . H12B H 0.8303 0.5726 0.8116 0.067 Uiso 1 1 calc R . . H12C H 0.8527 0.4952 0.8391 0.067 Uiso 1 1 calc R . . C13 C 0.80892(17) 0.5627(3) 0.9579(3) 0.0443(10) Uani 1 1 d . . . H13A H 0.7841 0.5887 0.9303 0.066 Uiso 1 1 calc R . . H13B H 0.8095 0.5805 1.0099 0.066 Uiso 1 1 calc R . . H13C H 0.8028 0.5088 0.9573 0.066 Uiso 1 1 calc R . . C14 C 0.90402(14) 0.6925(2) 0.9650(2) 0.0382(9) Uani 1 1 d . . . H14 H 0.9228 0.6587 0.9931 0.046 Uiso 1 1 calc R . . C15 C 0.91467(15) 0.7676(2) 0.9686(2) 0.0388(9) Uani 1 1 d . A . C16 C 0.95511(16) 0.7974(3) 1.0191(3) 0.0458(11) Uani 1 1 d U . . C17 C 0.9903(3) 0.8394(5) 0.9655(5) 0.065(2) Uani 0.65 1 d PU A 1 H17A H 1.0152 0.8627 0.9954 0.097 Uiso 0.65 1 calc PR A 1 H17B H 0.9735 0.8781 0.9374 0.097 Uiso 0.65 1 calc PR A 1 H17C H 1.0043 0.8036 0.9303 0.097 Uiso 0.65 1 calc PR A 1 C18 C 0.9342(3) 0.8497(5) 1.0758(5) 0.069(2) Uani 0.65 1 d PU A 1 H18A H 0.9113 0.8227 1.1067 0.103 Uiso 0.65 1 calc PR A 1 H18B H 0.9185 0.8910 1.0499 0.103 Uiso 0.65 1 calc PR A 1 H18C H 0.9591 0.8697 1.1080 0.103 Uiso 0.65 1 calc PR A 1 C19 C 0.9833(3) 0.7349(4) 1.0560(5) 0.056(2) Uani 0.65 1 d PU A 1 H19A H 0.9626 0.7052 1.0882 0.084 Uiso 0.65 1 calc PR A 1 H19B H 1.0085 0.7567 1.0864 0.084 Uiso 0.65 1 calc PR A 1 H19C H 0.9970 0.7028 1.0172 0.084 Uiso 0.65 1 calc PR A 1 C20 C 0.9450(5) 0.7717(7) 1.1063(7) 0.054(3) Uani 0.35 1 d PU A 2 H20A H 0.9157 0.7944 1.1237 0.081 Uiso 0.35 1 calc PR A 2 H20B H 0.9709 0.7882 1.1383 0.081 Uiso 0.35 1 calc PR A 2 H20C H 0.9423 0.7171 1.1087 0.081 Uiso 0.35 1 calc PR A 2 C21 C 1.0011(5) 0.7665(7) 0.9972(10) 0.057(4) Uani 0.35 1 d PU A 2 H21A H 1.0248 0.7816 1.0340 0.086 Uiso 0.35 1 calc PR A 2 H21B H 1.0098 0.7856 0.9476 0.086 Uiso 0.35 1 calc PR A 2 H21C H 0.9992 0.7119 0.9955 0.086 Uiso 0.35 1 calc PR A 2 C22 C 0.9570(5) 0.8856(7) 1.0276(8) 0.054(3) Uani 0.35 1 d PU A 2 H22A H 0.9809 0.8990 1.0649 0.081 Uiso 0.35 1 calc PR A 2 H22B H 0.9264 0.9041 1.0441 0.081 Uiso 0.35 1 calc PR A 2 H22C H 0.9651 0.9081 0.9792 0.081 Uiso 0.35 1 calc PR A 2 C23 C 0.88795(14) 0.8160(2) 0.9261(2) 0.0379(9) Uani 1 1 d . . . H23 H 0.8949 0.8679 0.9274 0.045 Uiso 1 1 calc R A . C24 C 0.85143(14) 0.7913(2) 0.8817(2) 0.0336(9) Uani 1 1 d . A . C25 C 0.82599(14) 0.8456(2) 0.8307(2) 0.0375(9) Uani 1 1 d . . . H25A H 0.8377 0.8966 0.8411 0.045 Uiso 1 1 calc R A . H25B H 0.8340 0.8335 0.7780 0.045 Uiso 1 1 calc R . . C26 C 0.75559(14) 0.90620(19) 0.7898(3) 0.0410(9) Uani 1 1 d . . . H26A H 0.7671 0.9544 0.8083 0.061 Uiso 1 1 calc R A . H26B H 0.7212 0.9060 0.7904 0.061 Uiso 1 1 calc R . . H26C H 0.7667 0.8984 0.7383 0.061 Uiso 1 1 calc R . . C27 C 0.76135(14) 0.8608(2) 0.9182(2) 0.0369(9) Uani 1 1 d . . . H27A H 0.7667 0.9144 0.9294 0.044 Uiso 1 1 calc R A . H27B H 0.7820 0.8310 0.9513 0.044 Uiso 1 1 calc R . . C28 C 0.71122(15) 0.8415(2) 0.9333(2) 0.0374(9) Uani 1 1 d . A . H28A H 0.6905 0.8736 0.9025 0.045 Uiso 1 1 calc R . . H28B H 0.7039 0.8509 0.9868 0.045 Uiso 1 1 calc R . . C29 C 0.72187(18) 0.7129(3) 0.9757(2) 0.0426(10) Uani 1 1 d . . . H29A H 0.7134 0.6606 0.9662 0.064 Uiso 1 1 calc R . . H29B H 0.7090 0.7286 1.0241 0.064 Uiso 1 1 calc R . . H29C H 0.7561 0.7178 0.9766 0.064 Uiso 1 1 calc R . . C30 C 0.65097(15) 0.7479(2) 0.9147(2) 0.0372(9) Uani 1 1 d . . . H30A H 0.6387 0.7576 0.9658 0.045 Uiso 1 1 calc R . . H30B H 0.6452 0.6945 0.9032 0.045 Uiso 1 1 calc R . . C31 C 0.62348(15) 0.7950(2) 0.8595(2) 0.0354(9) Uani 1 1 d . . . C32 C 0.58076(15) 0.8267(2) 0.8803(3) 0.0438(10) Uani 1 1 d . . . H32 H 0.5697 0.8202 0.9301 0.053 Uiso 1 1 calc R . . C33 C 0.55448(15) 0.8668(3) 0.8307(3) 0.0464(11) Uani 1 1 d . . . Cl34 Cl 0.50045(5) 0.90215(9) 0.85889(10) 0.0723(4) Uani 1 1 d . . . C35 C 0.57058(17) 0.8800(3) 0.7577(3) 0.0511(12) Uani 1 1 d . . . H35 H 0.5528 0.9093 0.7235 0.061 Uiso 1 1 calc R . . C36 C 0.61326(15) 0.8492(2) 0.7368(2) 0.0421(10) Uani 1 1 d . . . Cl37 Cl 0.63472(4) 0.86458(8) 0.64737(8) 0.0587(3) Uani 1 1 d . . . C38 C 0.63967(13) 0.8052(2) 0.7866(3) 0.0366(9) Uani 1 1 d . . . C39 C 0.65979(18) 0.5858(2) 0.8208(3) 0.0514(12) Uani 1 1 d . . . C40 C 0.6449(2) 0.5505(3) 0.8860(3) 0.0642(15) Uani 1 1 d . . . H40 H 0.6671 0.5342 0.9222 0.077 Uiso 1 1 calc R . . C41 C 0.5954(3) 0.5389(3) 0.8983(5) 0.087(2) Uani 1 1 d . . . H41 H 0.5845 0.5172 0.9437 0.104 Uiso 1 1 calc R . . C42 C 0.5640(2) 0.5599(4) 0.8427(6) 0.094(2) Uani 1 1 d . . . H42 H 0.5315 0.5506 0.8492 0.113 Uiso 1 1 calc R . . C43 C 0.5789(2) 0.5928(4) 0.7809(5) 0.089(2) Uani 1 1 d . . . H43 H 0.5568 0.6069 0.7437 0.106 Uiso 1 1 calc R . . C44 C 0.62455(18) 0.6068(3) 0.7694(3) 0.0664(16) Uani 1 1 d . . . H44 H 0.6335 0.6319 0.7246 0.080 Uiso 1 1 calc R . . C45 C 0.76173(16) 0.6851(3) 0.6511(2) 0.0419(10) Uani 1 1 d . . . C46 C 0.79392(17) 0.6258(3) 0.6600(2) 0.0458(11) Uani 1 1 d . . . H46 H 0.8241 0.6362 0.6800 0.055 Uiso 1 1 calc R . . C47 C 0.7829(2) 0.5531(3) 0.6405(3) 0.0545(12) Uani 1 1 d . . . H47 H 0.8052 0.5143 0.6476 0.065 Uiso 1 1 calc R . . C48 C 0.73919(18) 0.5373(3) 0.6105(3) 0.0528(12) Uani 1 1 d . . . H48 H 0.7313 0.4874 0.5971 0.063 Uiso 1 1 calc R . . C49 C 0.70654(18) 0.5949(3) 0.6000(2) 0.0492(11) Uani 1 1 d . . . H49 H 0.6768 0.5841 0.5784 0.059 Uiso 1 1 calc R . . C50 C 0.71726(17) 0.6673(3) 0.6208(2) 0.0448(10) Uani 1 1 d . . . H50 H 0.6945 0.7056 0.6146 0.054 Uiso 1 1 calc R . . C51 C 0.8698(3) 0.9063(5) 0.5910(5) 0.106(2) Uani 1 1 d . . . H51A H 0.8394 0.8890 0.6096 0.159 Uiso 1 1 calc R . . H51B H 0.8831 0.8687 0.5571 0.159 Uiso 1 1 calc R . . H51C H 0.8657 0.9534 0.5638 0.159 Uiso 1 1 calc R . . C52 C 0.9012(2) 0.9177(4) 0.6531(4) 0.0825(18) Uani 1 1 d . . . H52A H 0.8857 0.9479 0.6924 0.099 Uiso 1 1 calc R . . H52B H 0.9298 0.9442 0.6363 0.099 Uiso 1 1 calc R . . O53 O 0.91346(17) 0.8429(3) 0.6827(3) 0.0859(13) Uani 1 1 d . . . C54 C 0.9459(2) 0.8469(5) 0.7401(4) 0.091(2) Uani 1 1 d . . . H54A H 0.9326 0.8745 0.7833 0.110 Uiso 1 1 calc R . . H54B H 0.9745 0.8732 0.7229 0.110 Uiso 1 1 calc R . . C55 C 0.9579(3) 0.7669(5) 0.7631(4) 0.116(3) Uani 1 1 d . . . H55A H 0.9628 0.7364 0.7180 0.174 Uiso 1 1 calc R . . H55B H 0.9319 0.7459 0.7925 0.174 Uiso 1 1 calc R . . H55C H 0.9865 0.7669 0.7934 0.174 Uiso 1 1 calc R . . C56 C 1.0684(4) 0.4207(7) 0.6458(7) 0.097(7) Uani 0.50 1 d PD . . H56A H 1.0752 0.3717 0.6237 0.171 Uiso 0.50 1 calc PR . . H56B H 1.0591 0.4143 0.6984 0.171 Uiso 0.50 1 calc PR . . H56C H 1.0965 0.4521 0.6431 0.171 Uiso 0.50 1 calc PR . . C57 C 1.0306(3) 0.4560(5) 0.6047(5) 0.058(8) Uani 0.50 1 d PD . . H57A H 1.0449 0.4865 0.5644 0.142 Uiso 0.50 1 calc PR . . H57B H 1.0123 0.4160 0.5800 0.142 Uiso 0.50 1 calc PR . . O58 O 1.0000 0.5000 0.6420(6) 0.075(3) Uani 0.50 2 d SPD . . 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 0.03466(17) 0.02760(15) 0.03028(16) -0.00161(19) 0.0019(2) 0.00147(14) N2 0.0369(18) 0.0267(16) 0.0354(18) -0.0022(13) -0.0007(14) -0.0011(13) N3 0.0370(18) 0.0278(17) 0.0317(17) -0.0035(13) 0.0027(14) 0.0038(14) O4 0.0357(15) 0.0331(14) 0.0365(15) -0.0015(11) 0.0009(12) -0.0006(12) O5 0.0389(16) 0.0382(15) 0.0334(13) -0.0021(11) 0.0013(11) 0.0046(13) C6 0.047(3) 0.043(2) 0.037(2) 0.0002(18) 0.0052(18) -0.0012(19) C7 0.041(2) 0.038(2) 0.035(2) -0.0022(17) 0.0040(17) -0.0015(16) C8 0.030(2) 0.034(2) 0.033(2) 0.0000(16) 0.0066(16) -0.0038(16) C9 0.037(2) 0.034(2) 0.032(2) 0.0004(16) 0.0068(16) 0.0011(17) C10 0.041(2) 0.031(2) 0.036(2) 0.0003(16) 0.0037(17) 0.0018(17) C11 0.050(3) 0.035(2) 0.053(3) 0.0027(18) -0.001(2) 0.011(2) C12 0.055(3) 0.034(2) 0.046(3) -0.0033(19) 0.005(2) 0.002(2) C13 0.043(3) 0.040(2) 0.050(3) 0.0026(19) 0.002(2) -0.004(2) C14 0.030(2) 0.043(2) 0.041(2) 0.0065(17) 0.0022(17) 0.0024(18) C15 0.034(2) 0.042(2) 0.040(2) -0.0001(17) 0.0071(17) -0.0006(19) C16 0.038(3) 0.050(3) 0.049(3) 0.000(2) -0.008(2) -0.003(2) C17 0.044(5) 0.067(5) 0.083(6) 0.012(4) -0.013(4) -0.022(4) C18 0.054(5) 0.078(6) 0.074(6) -0.035(5) -0.011(4) -0.003(4) C19 0.047(5) 0.055(5) 0.065(5) 0.012(4) -0.006(4) -0.009(3) C20 0.055(8) 0.054(8) 0.053(8) -0.018(6) -0.014(6) -0.008(6) C21 0.029(6) 0.046(7) 0.097(11) 0.007(7) -0.015(7) 0.008(6) C22 0.057(8) 0.032(6) 0.073(9) 0.009(6) -0.020(7) -0.009(6) C23 0.036(2) 0.034(2) 0.044(2) -0.0001(17) 0.0040(18) -0.0071(18) C24 0.033(2) 0.030(2) 0.038(2) 0.0018(16) 0.0063(17) -0.0018(16) C25 0.043(2) 0.030(2) 0.039(2) 0.0062(17) -0.0032(18) -0.0022(18) C26 0.053(2) 0.0282(16) 0.041(2) 0.013(2) -0.007(2) 0.0013(16) C27 0.045(2) 0.029(2) 0.037(2) -0.0075(16) -0.0010(18) 0.0054(18) C28 0.049(3) 0.030(2) 0.033(2) -0.0083(16) 0.0024(17) 0.0019(18) C29 0.052(3) 0.043(3) 0.033(2) -0.0001(18) 0.0003(19) -0.003(2) C30 0.043(2) 0.033(2) 0.036(2) 0.0008(17) 0.0095(18) 0.0019(18) C31 0.037(2) 0.025(2) 0.044(2) -0.0076(16) 0.0010(18) -0.0023(16) C32 0.036(2) 0.046(2) 0.049(2) -0.011(2) 0.0013(19) -0.001(2) C33 0.030(2) 0.049(3) 0.060(3) -0.008(2) -0.002(2) 0.006(2) Cl34 0.0415(6) 0.0872(10) 0.0882(10) -0.0122(8) 0.0023(6) 0.0220(7) C35 0.042(3) 0.046(3) 0.065(3) -0.001(2) -0.014(2) 0.004(2) C36 0.037(2) 0.046(3) 0.043(2) -0.0057(19) -0.0044(19) -0.002(2) Cl37 0.0549(7) 0.0761(8) 0.0451(6) 0.0142(6) -0.0049(5) 0.0124(6) C38 0.035(2) 0.0289(17) 0.046(3) -0.004(2) -0.001(2) -0.0007(14) C39 0.055(3) 0.038(2) 0.061(3) -0.0129(19) 0.013(2) -0.008(2) C40 0.080(4) 0.032(2) 0.080(4) -0.004(2) 0.033(3) -0.006(2) C41 0.102(5) 0.038(3) 0.119(6) -0.012(3) 0.055(5) -0.023(3) C42 0.057(4) 0.091(5) 0.134(7) -0.014(5) 0.020(4) -0.016(4) C43 0.046(3) 0.106(5) 0.113(6) -0.005(4) 0.009(4) -0.007(3) C44 0.041(3) 0.075(4) 0.084(4) -0.017(3) -0.002(2) -0.004(3) C45 0.050(3) 0.043(3) 0.032(2) 0.0015(18) 0.0086(19) 0.005(2) C46 0.050(3) 0.051(3) 0.037(2) 0.0000(19) 0.0058(19) 0.009(2) C47 0.066(3) 0.054(3) 0.043(3) -0.001(2) 0.008(3) 0.013(3) C48 0.073(3) 0.042(3) 0.043(3) -0.006(2) 0.012(2) 0.002(2) C49 0.060(3) 0.050(3) 0.038(2) -0.0020(19) 0.002(2) 0.001(2) C50 0.049(3) 0.050(3) 0.035(2) 0.006(2) 0.0066(19) 0.000(2) C51 0.103(6) 0.107(6) 0.108(6) 0.016(5) -0.014(5) -0.018(5) C52 0.082(4) 0.069(4) 0.096(5) -0.006(4) 0.016(4) -0.005(3) O53 0.087(3) 0.086(3) 0.085(3) -0.001(2) 0.003(2) 0.008(3) C54 0.050(4) 0.159(7) 0.065(4) 0.021(4) 0.000(3) -0.005(4) C55 0.098(6) 0.170(8) 0.079(5) 0.031(5) 0.025(4) 0.058(6) C56 0.123(19) 0.086(7) 0.083(9) -0.009(7) 0.062(12) -0.036(10) C57 0.072(8) 0.15(2) 0.051(6) -0.020(9) 0.022(6) -0.019(12) O58 0.120(10) 0.071(7) 0.033(5) 0.000 0.000 -0.033(7) _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 O4 1.995(3) . ? Zr1 O5 2.006(3) . ? Zr1 C6 2.312(4) . ? Zr1 C7 2.331(4) . ? Zr1 N2 2.475(3) . ? Zr1 N3 2.485(3) . ? Zr1 C45 2.730(4) . ? N2 C26 1.479(5) . ? N2 C27 1.487(5) . ? N2 C25 1.505(5) . ? N3 C30 1.481(5) . ? N3 C29 1.489(5) . ? N3 C28 1.502(5) . ? O4 C8 1.372(5) . ? O5 C38 1.350(5) . ? C6 C45 1.468(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C39 1.493(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.403(6) . ? C8 C24 1.409(5) . ? C9 C14 1.410(6) . ? C9 C10 1.541(5) . ? C10 C13 1.536(6) . ? C10 C11 1.538(6) . ? C10 C12 1.542(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.379(6) . ? C14 H14 0.9500 . ? C15 C23 1.380(6) . ? C15 C16 1.556(6) . ? C16 C21 1.474(13) . ? C16 C18 1.502(9) . ? C16 C19 1.526(9) . ? C16 C17 1.577(10) . ? C16 C22 1.587(12) . ? C16 C20 1.646(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 C25 1.514(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.494(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.514(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C38 1.392(7) . ? C31 C32 1.393(6) . ? C32 C33 1.363(7) . ? C32 H32 0.9500 . ? C33 C35 1.399(7) . ? C33 Cl34 1.739(5) . ? C35 C36 1.387(7) . ? C35 H35 0.9500 . ? C36 C38 1.404(6) . ? C36 Cl37 1.729(5) . ? C39 C40 1.389(7) . ? C39 C44 1.411(8) . ? C40 C41 1.440(8) . ? C40 H40 0.9500 . ? C41 C42 1.387(11) . ? C41 H41 0.9500 . ? C42 C43 1.318(11) . ? C42 H42 0.9500 . ? C43 C44 1.340(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.411(6) . ? C45 C50 1.413(7) . ? C46 C47 1.383(7) . ? C46 H46 0.9500 . ? C47 C48 1.385(8) . ? C47 H47 0.9500 . ? C48 C49 1.401(7) . ? C48 H48 0.9500 . ? C49 C50 1.383(7) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.436(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O53 1.480(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? O53 C54 1.381(7) . ? C54 C55 1.528(11) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.4482(10) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O58 1.3493(10) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O58 C57 1.3493(10) 2_765 ? 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 O4 Zr1 O5 167.94(11) . . ? O4 Zr1 C6 96.26(15) . . ? O5 Zr1 C6 88.42(15) . . ? O4 Zr1 C7 91.12(13) . . ? O5 Zr1 C7 96.47(13) . . ? C6 Zr1 C7 118.18(15) . . ? O4 Zr1 N2 77.82(11) . . ? O5 Zr1 N2 91.68(11) . . ? C6 Zr1 N2 83.94(13) . . ? C7 Zr1 N2 156.50(13) . . ? O4 Zr1 N3 94.92(11) . . ? O5 Zr1 N3 75.81(11) . . ? C6 Zr1 N3 149.53(13) . . ? C7 Zr1 N3 89.79(13) . . ? N2 Zr1 N3 70.87(11) . . ? O4 Zr1 C45 97.54(12) . . ? O5 Zr1 C45 92.39(12) . . ? C6 Zr1 C45 32.53(15) . . ? C7 Zr1 C45 85.65(14) . . ? N2 Zr1 C45 116.07(12) . . ? N3 Zr1 C45 166.81(13) . . ? C26 N2 C27 110.3(3) . . ? C26 N2 C25 106.8(3) . . ? C27 N2 C25 108.5(3) . . ? C26 N2 Zr1 109.0(2) . . ? C27 N2 Zr1 111.8(2) . . ? C25 N2 Zr1 110.4(2) . . ? C30 N3 C29 106.4(3) . . ? C30 N3 C28 108.6(3) . . ? C29 N3 C28 109.5(3) . . ? C30 N3 Zr1 112.9(2) . . ? C29 N3 Zr1 108.3(2) . . ? C28 N3 Zr1 111.1(2) . . ? C8 O4 Zr1 146.6(2) . . ? C38 O5 Zr1 145.8(3) . . ? C45 C6 Zr1 89.6(3) . . ? C45 C6 H6A 113.7 . . ? Zr1 C6 H6A 113.7 . . ? C45 C6 H6B 113.7 . . ? Zr1 C6 H6B 113.7 . . ? H6A C6 H6B 111.0 . . ? C39 C7 Zr1 125.7(3) . . ? C39 C7 H7A 105.9 . . ? Zr1 C7 H7A 105.9 . . ? C39 C7 H7B 105.9 . . ? Zr1 C7 H7B 105.9 . . ? H7A C7 H7B 106.2 . . ? O4 C8 C9 121.6(3) . . ? O4 C8 C24 117.5(4) . . ? C9 C8 C24 120.9(4) . . ? C8 C9 C14 116.3(4) . . ? C8 C9 C10 122.4(4) . . ? C14 C9 C10 121.3(4) . . ? C13 C10 C11 107.6(4) . . ? C13 C10 C9 109.9(3) . . ? C11 C10 C9 112.3(4) . . ? C13 C10 C12 110.1(4) . . ? C11 C10 C12 106.6(3) . . ? C9 C10 C12 110.2(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C9 123.7(4) . . ? C15 C14 H14 118.1 . . ? C9 C14 H14 118.1 . . ? C14 C15 C23 117.7(4) . . ? C14 C15 C16 121.5(4) . . ? C23 C15 C16 120.7(4) . . ? C21 C16 C18 139.9(6) . . ? C21 C16 C19 51.1(6) . . ? C18 C16 C19 112.1(6) . . ? C21 C16 C15 112.1(6) . . ? C18 C16 C15 108.0(5) . . ? C19 C16 C15 112.9(5) . . ? C21 C16 C17 56.8(6) . . ? C18 C16 C17 111.3(6) . . ? C19 C16 C17 106.0(5) . . ? C15 C16 C17 106.5(4) . . ? C21 C16 C22 111.5(7) . . ? C18 C16 C22 47.8(6) . . ? C19 C16 C22 132.0(5) . . ? C15 C16 C22 114.9(5) . . ? C17 C16 C22 64.0(6) . . ? C21 C16 C20 107.5(8) . . ? C18 C16 C20 57.9(5) . . ? C19 C16 C20 58.7(5) . . ? C15 C16 C20 108.7(5) . . ? C17 C16 C20 144.8(5) . . ? C22 C16 C20 101.2(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.4 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.4 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C15 122.0(4) . . ? C24 C23 H23 119.0 . . ? C15 C23 H23 119.0 . . ? C23 C24 C8 119.2(4) . . ? C23 C24 C25 120.0(4) . . ? C8 C24 C25 120.8(4) . . ? N2 C25 C24 115.0(3) . . ? N2 C25 H25A 108.5 . . ? C24 C25 H25A 108.5 . . ? N2 C25 H25B 108.5 . . ? C24 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C27 C28 110.6(3) . . ? N2 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N2 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 N3 110.2(3) . . ? C27 C28 H28A 109.6 . . ? N3 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? N3 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? N3 C29 H29A 109.5 . . ? N3 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N3 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 115.2(3) . . ? N3 C30 H30A 108.5 . . ? C31 C30 H30A 108.5 . . ? N3 C30 H30B 108.5 . . ? C31 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C38 C31 C32 119.0(4) . . ? C38 C31 C30 120.6(4) . . ? C32 C31 C30 120.4(4) . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C35 120.8(5) . . ? C32 C33 Cl34 119.4(4) . . ? C35 C33 Cl34 119.9(4) . . ? C36 C35 C33 118.1(5) . . ? C36 C35 H35 121.0 . . ? C33 C35 H35 121.0 . . ? C35 C36 C38 121.5(4) . . ? C35 C36 Cl37 119.7(4) . . ? C38 C36 Cl37 118.8(3) . . ? O5 C38 C31 121.2(4) . . ? O5 C38 C36 119.7(4) . . ? C31 C38 C36 119.1(4) . . ? C40 C39 C44 116.5(5) . . ? C40 C39 C7 122.6(5) . . ? C44 C39 C7 120.8(5) . . ? C39 C40 C41 119.5(6) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 118.8(6) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C41 120.7(7) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 121.6(7) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C43 C44 C39 122.7(6) . . ? C43 C44 H44 118.6 . . ? C39 C44 H44 118.6 . . ? C46 C45 C50 117.2(4) . . ? C46 C45 C6 120.5(4) . . ? C50 C45 C6 121.9(4) . . ? C46 C45 Zr1 103.7(3) . . ? C50 C45 Zr1 102.7(3) . . ? C6 C45 Zr1 57.9(2) . . ? C47 C46 C45 122.1(5) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C46 C47 C48 119.5(5) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C47 C48 C49 119.9(5) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.5(5) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C45 120.7(5) . . ? C49 C50 H50 119.6 . . ? C45 C50 H50 119.6 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C51 C52 O53 107.1(6) . . ? C51 C52 H52A 110.3 . . ? O53 C52 H52A 110.3 . . ? C51 C52 H52B 110.3 . . ? O53 C52 H52B 110.3 . . ? H52A C52 H52B 108.5 . . ? C54 O53 C52 112.2(6) . . ? O53 C54 C55 107.4(7) . . ? O53 C54 H54A 110.2 . . ? C55 C54 H54A 110.2 . . ? O53 C54 H54B 110.2 . . ? C55 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 H56A 109.5 . . ? C57 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C57 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O58 C57 C56 119.1(9) . . ? O58 C57 H57A 107.5 . . ? C56 C57 H57A 107.5 . . ? O58 C57 H57B 107.5 . . ? C56 C57 H57B 107.5 . . ? H57A C57 H57B 107.0 . . ? C57 O58 C57 121.0(14) . 2_765 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.593 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.070