# ic981399j.cif _audit_creation_method ; manual editing of the .cif file created by SHELXL-97 ; # 1. SUBMISSION DETAILS _publ_contact_author_name ; Ilia A. Guzei ; _publ_contact_author_address ; Department of Chemistry Iowa State University of Science and Technology Ames, Iowa, 50011 USA ; _publ_contact_author_phone '+515-294-6419' _publ_contact_author_fax '+515-294-5717' _publ_contact_author_email iguzei@iastate.edu _publ_contact_letter ; These 5 structures will appear in one paper in Inorganic Chemistry ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, Structure, and Reactivity of Zirconium and Hafnium Imido Metalloporphyrins ; loop_ _publ_author_name _publ_author_address ; 'Joseph L. Thorman' ; Department of Chemistry Iowa State University of Science and Technology Ames, Iowa, 50011 USA ; 'Ilia A. Guzei' ; Department of Chemistry Iowa State University of Science and Technology Ames, Iowa, 50011 USA ; 'Victor G. Young' ; Department of Chemistry University of Minnesota Minneapolis MN 55455 USA ; 'L. Keith Woo' ; Department of Chemistry Iowa State University of Science and Technology Ames, Iowa, 50011 USA ; # 3. Results data_98061 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 98061 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C70.50 H69 N5 Zr' _chemical_formula_weight 1077.53 _chemical_melting_point ? _chemical_compound_source 'J. Thorman / Prof. K. Woo - ISU' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6358(2) _cell_length_b 18.7583(1) _cell_length_c 19.4375(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.970(1) _cell_angle_gamma 90.00 _cell_volume 5886.24(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_method ? _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 0.233 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29098 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10237 _reflns_number_observed 7872 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+1.8549P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10232 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0403 _refine_ls_wR_factor_all 0.1093 _refine_ls_wR_factor_obs 0.0984 _refine_ls_goodness_of_fit_all 0.977 _refine_ls_goodness_of_fit_obs 1.029 _refine_ls_restrained_S_all 0.993 _refine_ls_restrained_S_obs 1.029 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zr1 Zr -0.088226(14) 0.850698(12) 0.366714(12) 0.02126(8) Uani 1 d . . N1 N -0.05427(12) 0.89076(10) 0.27073(10) 0.0248(5) Uani 1 d . . N2 N -0.21346(12) 0.88735(10) 0.31222(10) 0.0253(5) Uani 1 d . . N3 N -0.12386(12) 0.89068(10) 0.46278(10) 0.0238(4) Uani 1 d . . N4 N 0.03461(12) 0.89471(10) 0.42093(10) 0.0241(5) Uani 1 d . . C1 C 0.0249(2) 0.90287(13) 0.26186(13) 0.0275(6) Uani 1 d . . C2 C 0.0209(2) 0.90520(15) 0.18713(14) 0.0357(6) Uani 1 d . . H2A H 0.0663(2) 0.91276(15) 0.16627(14) 0.043 Uiso 1 calc R . C3 C -0.0590(2) 0.89473(14) 0.15167(14) 0.0345(6) Uani 1 d . . H3A H -0.0796(2) 0.89293(14) 0.10166(14) 0.041 Uiso 1 calc R . C4 C -0.1069(2) 0.88683(13) 0.20378(13) 0.0264(6) Uani 1 d . . C5 C -0.1937(2) 0.87927(13) 0.18944(13) 0.0272(6) Uani 1 d . . C6 C -0.24299(15) 0.88094(13) 0.23957(13) 0.0252(5) Uani 1 d . . C7 C -0.3318(2) 0.87456(14) 0.22401(14) 0.0311(6) Uani 1 d . . H7A H -0.3678(2) 0.86969(14) 0.17820(14) 0.037 Uiso 1 calc R . C8 C -0.3549(2) 0.87672(14) 0.28604(13) 0.0306(6) Uani 1 d . . H8A H -0.4100(2) 0.87361(14) 0.29163(13) 0.037 Uiso 1 calc R . C9 C -0.28105(15) 0.88459(13) 0.34209(13) 0.0263(6) Uani 1 d . . C10 C -0.27707(15) 0.88695(13) 0.41546(13) 0.0272(6) Uani 1 d . . C11 C -0.20454(15) 0.89168(12) 0.47124(13) 0.0257(5) Uani 1 d . . C12 C -0.2018(2) 0.89672(13) 0.54540(13) 0.0302(6) Uani 1 d . . H12A H -0.2482(2) 0.89988(13) 0.56572(13) 0.036 Uiso 1 calc R . C13 C -0.1205(2) 0.89614(13) 0.58156(13) 0.0296(6) Uani 1 d . . H13A H -0.1001(2) 0.89735(13) 0.63160(13) 0.036 Uiso 1 calc R . C14 C -0.0714(2) 0.89337(12) 0.53007(13) 0.0261(6) Uani 1 d . . C15 C 0.01589(15) 0.89382(12) 0.54483(13) 0.0253(5) Uani 1 d . . C16 C 0.06418(15) 0.89928(12) 0.49382(13) 0.0255(5) Uani 1 d . . C17 C 0.15097(15) 0.91619(13) 0.50962(14) 0.0296(6) Uani 1 d . . H17A H 0.18647(15) 0.92198(13) 0.55553(14) 0.036 Uiso 1 calc R . C18 C 0.17299(15) 0.92237(13) 0.44717(13) 0.0292(6) Uani 1 d . . H18A H 0.22669(15) 0.93375(13) 0.44157(13) 0.035 Uiso 1 calc R . C19 C 0.10076(14) 0.90870(12) 0.39072(13) 0.0250(5) Uani 1 d . . C20 C 0.09688(15) 0.91151(12) 0.31760(13) 0.0264(5) Uani 1 d . . C21 C -0.23799(15) 0.86779(14) 0.11293(13) 0.0289(6) Uani 1 d . . C22 C -0.2362(2) 0.8011(2) 0.0829(2) 0.0488(8) Uani 1 d . . H22A H -0.2058(2) 0.7637(2) 0.1104(2) 0.059 Uiso 1 calc R . C23 C -0.2784(2) 0.7880(2) 0.0128(2) 0.0530(8) Uani 1 d . . H23A H -0.2768(2) 0.7416(2) -0.0063(2) 0.064 Uiso 1 calc R . C24 C -0.3223(2) 0.8405(2) -0.02917(15) 0.0445(8) Uani 1 d . . C25 C -0.3231(2) 0.9078(2) 0.0010(2) 0.0539(9) Uani 1 d . . H25A H -0.3525(2) 0.9454(2) -0.0269(2) 0.065 Uiso 1 calc R . C26 C -0.2818(2) 0.9211(2) 0.07111(15) 0.0422(7) Uani 1 d . . H26A H -0.2839(2) 0.9674(2) 0.09040(15) 0.051 Uiso 1 calc R . C27 C -0.3700(2) 0.8262(2) -0.1046(2) 0.0727(12) Uani 1 d . . H27A H -0.3981(2) 0.7800(2) -0.1069(2) 0.109 Uiso 1 d R . H27B H -0.3316(2) 0.8254(2) -0.1357(2) 0.109 Uiso 1 d R . H27C H -0.4112(2) 0.8639(2) -0.1201(2) 0.109 Uiso 1 d R . C28 C -0.3576(2) 0.88031(15) 0.43707(14) 0.0325(6) Uani 1 d . . C29 C -0.3737(2) 0.8201(2) 0.4738(2) 0.0458(7) Uani 1 d . . H29A H -0.3329(2) 0.7838(2) 0.4858(2) 0.055 Uiso 1 calc R . C30 C -0.4487(2) 0.8126(2) 0.4930(2) 0.0569(9) Uani 1 d . . H30A H -0.4582(2) 0.7713(2) 0.5183(2) 0.068 Uiso 1 calc R . C31 C -0.5095(2) 0.8641(2) 0.4761(2) 0.0549(9) Uani 1 d . . C32 C -0.4938(2) 0.9237(2) 0.4402(2) 0.0578(9) Uani 1 d . . H32A H -0.5349(2) 0.9597(2) 0.4281(2) 0.069 Uiso 1 calc R . C33 C -0.4184(2) 0.9325(2) 0.4212(2) 0.0451(7) Uani 1 d . . H33A H -0.4088(2) 0.9746(2) 0.3972(2) 0.054 Uiso 1 calc R . C34 C -0.5926(2) 0.8545(3) 0.4952(2) 0.0868(14) Uani 1 d . . H34A H -0.5867(2) 0.8192(3) 0.5333(2) 0.130 Uiso 1 d R . H34B H -0.6341(2) 0.8378(3) 0.4535(2) 0.130 Uiso 1 d R . H34C H -0.6103(2) 0.9001(3) 0.5111(2) 0.130 Uiso 1 d R . C35 C 0.06324(15) 0.88746(13) 0.62060(13) 0.0258(6) Uani 1 d . . C36 C 0.1149(2) 0.82850(14) 0.64228(14) 0.0319(6) Uani 1 d . . H36A H 0.1206(2) 0.79340(14) 0.60857(14) 0.038 Uiso 1 calc R . C37 C 0.1575(2) 0.82102(15) 0.71253(15) 0.0369(7) Uani 1 d . . H37A H 0.1918(2) 0.78038(15) 0.72613(15) 0.044 Uiso 1 calc R . C38 C 0.1517(2) 0.8712(2) 0.76362(14) 0.0362(7) Uani 1 d . . C39 C 0.1012(2) 0.93047(15) 0.74168(14) 0.0380(7) Uani 1 d . . H39A H 0.0964(2) 0.96594(15) 0.77536(14) 0.046 Uiso 1 calc R . C40 C 0.0577(2) 0.93848(13) 0.67145(13) 0.0323(6) Uani 1 d . . H40A H 0.0237(2) 0.97927(13) 0.65790(13) 0.039 Uiso 1 calc R . C41 C 0.1990(2) 0.8624(2) 0.8404(2) 0.0532(9) Uani 1 d . . H41A H 0.2133(2) 0.8120(2) 0.8499(2) 0.080 Uiso 1 d R . H41B H 0.1644(2) 0.8785(2) 0.8716(2) 0.080 Uiso 1 d R . H41C H 0.2499(2) 0.8909(2) 0.8492(2) 0.080 Uiso 1 d R . C42 C 0.1765(2) 0.92737(13) 0.29691(13) 0.0290(6) Uani 1 d . . C43 C 0.2416(2) 0.8790(2) 0.3115(2) 0.0390(7) Uani 1 d . . H43A H 0.2354(2) 0.8353(2) 0.3343(2) 0.047 Uiso 1 calc R . C44 C 0.3159(2) 0.8938(2) 0.2931(2) 0.0443(7) Uani 1 d . . H44A H 0.3600(2) 0.8603(2) 0.3043(2) 0.053 Uiso 1 calc R . C45 C 0.3264(2) 0.9566(2) 0.2588(2) 0.0453(7) Uani 1 d . . C46 C 0.2613(2) 1.0052(2) 0.2451(2) 0.0496(8) Uani 1 d . . H46A H 0.2676(2) 1.0491(2) 0.2226(2) 0.059 Uiso 1 calc R . C47 C 0.1872(2) 0.9910(2) 0.2635(2) 0.0420(7) Uani 1 d . . H47A H 0.1436(2) 1.0250(2) 0.2532(2) 0.050 Uiso 1 calc R . C48 C 0.4069(2) 0.9721(2) 0.2372(2) 0.0696(11) Uani 1 d . . H48A H 0.4016(2) 1.0174(2) 0.2114(2) 0.104 Uiso 1 d R . H48B H 0.4182(2) 0.9337(2) 0.2067(2) 0.104 Uiso 1 d R . H48C H 0.4526(2) 0.9754(2) 0.2797(2) 0.104 Uiso 1 d R . N5 N -0.08884(12) 0.75144(10) 0.36319(10) 0.0262(5) Uani 1 d . . C49 C -0.08283(14) 0.67806(13) 0.36953(13) 0.0252(5) Uani 1 d . . C50 C -0.0901(2) 0.63417(13) 0.30838(14) 0.0293(6) Uani 1 d . . C51 C -0.0809(2) 0.56045(14) 0.31730(15) 0.0365(7) Uani 1 d . . H51A H -0.0857(2) 0.53090(14) 0.27681(15) 0.044 Uiso 1 calc R . C52 C -0.0649(2) 0.52955(15) 0.3840(2) 0.0428(7) Uani 1 d . . H52A H -0.0575(2) 0.47945(15) 0.3891(2) 0.051 Uiso 1 calc R . C53 C -0.0597(2) 0.57214(14) 0.4434(2) 0.0382(7) Uani 1 d . . H53A H -0.0497(2) 0.55053(14) 0.4888(2) 0.046 Uiso 1 calc R . C54 C -0.0689(2) 0.64579(13) 0.43763(14) 0.0297(6) Uani 1 d . . C55 C -0.1070(2) 0.66805(14) 0.23524(13) 0.0324(6) Uani 1 d . . H55A H -0.1447(2) 0.70952(14) 0.23550(13) 0.039 Uiso 1 calc R . C56 C -0.1509(2) 0.6181(2) 0.1755(2) 0.0453(7) Uani 1 d . . H56A H -0.1988(2) 0.5961(2) 0.1882(2) 0.068 Uiso 1 d R . H56B H -0.1123(2) 0.5808(2) 0.1685(2) 0.068 Uiso 1 d R . H56C H -0.1695(2) 0.6454(2) 0.1316(2) 0.068 Uiso 1 d R . C57 C -0.0267(2) 0.6976(2) 0.2203(2) 0.0457(7) Uani 1 d . . H57A H -0.0010(2) 0.7310(2) 0.2579(2) 0.069 Uiso 1 d R . H57B H -0.0396(2) 0.7224(2) 0.1746(2) 0.069 Uiso 1 d R . H57C H 0.0115(2) 0.6582(2) 0.2188(2) 0.069 Uiso 1 d R . C58 C -0.0670(2) 0.69282(14) 0.50188(14) 0.0346(6) Uani 1 d . . H58A H -0.0409(2) 0.73903(14) 0.49344(14) 0.042 Uiso 1 calc R . C59 C -0.1548(2) 0.7095(2) 0.5064(2) 0.0485(8) Uani 1 d . . H59A H -0.1536(2) 0.7435(2) 0.5449(2) 0.073 Uiso 1 d R . H59B H -0.1821(2) 0.6654(2) 0.5156(2) 0.073 Uiso 1 d R . H59C H -0.1856(2) 0.7302(2) 0.4614(2) 0.073 Uiso 1 d R . C60 C -0.0158(2) 0.6631(2) 0.5713(2) 0.0494(8) Uani 1 d . . H60A H 0.0394(2) 0.6502(2) 0.5658(2) 0.074 Uiso 1 d R . H60B H -0.0431(2) 0.6207(2) 0.5843(2) 0.074 Uiso 1 d R . H60C H -0.0106(2) 0.6992(2) 0.6085(2) 0.074 Uiso 1 d R . C61 C 0.3054(3) 0.7086(2) 0.2490(2) 0.0733(11) Uani 1 d . . C62 C 0.3698(3) 0.7264(2) 0.2179(2) 0.0839(13) Uani 1 d . . H62A H 0.3576(3) 0.7397(2) 0.1693(2) 0.101 Uiso 1 calc R . C63 C 0.4493(3) 0.7250(3) 0.2557(3) 0.0925(14) Uani 1 d . . H63A H 0.4922(3) 0.7364(3) 0.2330(3) 0.111 Uiso 1 calc R . C64 C 0.4690(3) 0.7076(3) 0.3248(3) 0.109(2) Uani 1 d . . H64A H 0.5253(3) 0.7079(3) 0.3505(3) 0.131 Uiso 1 calc R . C65 C 0.4097(3) 0.6899(3) 0.3579(3) 0.099(2) Uani 1 d . . H65A H 0.4245(3) 0.6774(3) 0.4067(3) 0.118 Uiso 1 calc R . C66 C 0.3281(3) 0.6897(2) 0.3218(2) 0.0789(12) Uani 1 d . . H66A H 0.2865(3) 0.6768(2) 0.3455(2) 0.095 Uiso 1 calc R . C67 C 0.2158(3) 0.7093(3) 0.2073(3) 0.123(2) Uani 1 d . . H67A H 0.2103(3) 0.7391(3) 0.1650(3) 0.185 Uiso 1 d R . H67B H 0.1809(3) 0.7287(3) 0.2369(3) 0.185 Uiso 1 d R . H67C H 0.1982(3) 0.6606(3) 0.1931(3) 0.185 Uiso 1 d R . C68 C -0.0353(3) 1.0273(2) -0.0005(2) 0.0865(13) Uani 1 d . . H68A H -0.0389(3) 1.0362(2) 0.0488(2) 0.104 Uiso 1 calc R . H68B H -0.0208(3) 1.0729(2) -0.0201(2) 0.104 Uiso 1 calc R . C69 C -0.1193(3) 1.0033(3) -0.0436(2) 0.0927(14) Uani 1 d . . H69A H -0.1350(3) 0.9590(3) -0.0226(2) 0.111 Uiso 1 calc R 1 H69B H -0.1149(3) 0.9920(3) -0.0923(2) 0.111 Uiso 1 calc R 1 C70 C -0.1879(4) 1.0582(3) -0.0478(3) 0.116(2) Uani 0.50 d P 1 H70A H -0.2190(4) 1.0477(3) -0.0122(3) 0.174 Uiso 0.50 d PR 1 H70B H -0.2255(4) 1.0571(3) -0.0952(3) 0.174 Uiso 0.50 d PR 1 H70C H -0.1628(4) 1.1056(3) -0.0390(3) 0.174 Uiso 0.50 d PR 1 C70' C -0.1879(4) 1.0582(3) -0.0478(3) 0.116(2) Uani 0.50 d P 2 H70D H -0.2412(7) 1.0346(5) -0.0696(6) 0.140 Uiso 0.50 calc PR 2 H70E H -0.1893(7) 1.0710(5) 0.0013(6) 0.140 Uiso 0.50 calc PR 2 C71' C -0.1845(7) 1.1249(5) -0.0867(6) 0.108(3) Uani 0.50 d P 2 H71A H -0.2340(7) 1.1527(5) -0.0856(6) 0.162 Uiso 0.50 d PR 2 H71B H -0.1841(7) 1.1142(5) -0.1360(6) 0.162 Uiso 0.50 d PR 2 H71C H -0.1349(7) 1.1525(5) -0.0646(6) 0.162 Uiso 0.50 d PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02081(13) 0.02200(13) 0.01963(13) 0.00010(10) 0.00226(9) -0.00054(10) N1 0.0223(11) 0.0290(12) 0.0221(11) 0.0000(8) 0.0036(9) -0.0028(8) N2 0.0236(11) 0.0289(12) 0.0218(11) 0.0018(9) 0.0022(9) -0.0001(9) N3 0.0237(11) 0.0244(11) 0.0214(11) 0.0000(8) 0.0019(9) 0.0005(8) N4 0.0225(11) 0.0254(11) 0.0234(11) -0.0018(8) 0.0039(9) -0.0014(8) C1 0.0266(14) 0.0287(14) 0.0274(14) 0.0013(10) 0.0068(11) -0.0002(10) C2 0.032(2) 0.048(2) 0.029(2) 0.0015(12) 0.0115(13) -0.0035(12) C3 0.036(2) 0.048(2) 0.0202(14) 0.0007(11) 0.0062(12) -0.0047(12) C4 0.0287(14) 0.0277(14) 0.0219(13) 0.0014(10) 0.0041(11) -0.0020(11) C5 0.0281(14) 0.0260(13) 0.0239(14) 0.0018(10) -0.0007(11) -0.0008(11) C6 0.0256(13) 0.0223(13) 0.0249(14) 0.0033(10) 0.0006(11) -0.0001(10) C7 0.0252(14) 0.0373(15) 0.0275(15) 0.0018(11) 0.0000(11) -0.0022(11) C8 0.0204(13) 0.0376(15) 0.032(2) 0.0039(12) 0.0020(11) 0.0012(11) C9 0.0224(13) 0.0237(13) 0.0321(15) 0.0026(11) 0.0052(11) 0.0019(10) C10 0.0255(14) 0.0269(14) 0.0281(14) 0.0025(11) 0.0044(11) 0.0026(10) C11 0.0244(14) 0.0254(14) 0.0277(14) -0.0003(10) 0.0071(11) 0.0011(10) C12 0.0305(15) 0.0346(15) 0.0270(15) -0.0015(11) 0.0100(12) 0.0017(11) C13 0.033(2) 0.0342(15) 0.0213(14) -0.0007(10) 0.0060(12) 0.0010(11) C14 0.0309(15) 0.0227(13) 0.0232(14) -0.0020(10) 0.0038(11) -0.0006(10) C15 0.0270(14) 0.0229(13) 0.0232(14) -0.0005(10) 0.0007(11) -0.0007(10) C16 0.0237(13) 0.0249(13) 0.0242(14) -0.0005(10) -0.0015(11) -0.0002(10) C17 0.0254(14) 0.0304(14) 0.0291(15) -0.0003(11) -0.0013(11) -0.0020(11) C18 0.0208(13) 0.0307(14) 0.034(2) 0.0025(11) 0.0026(11) -0.0025(10) C19 0.0214(13) 0.0236(13) 0.0286(14) 0.0004(10) 0.0032(11) -0.0008(10) C20 0.0263(14) 0.0241(13) 0.0299(14) 0.0015(10) 0.0088(11) -0.0004(10) C21 0.0221(13) 0.040(2) 0.0221(13) 0.0013(11) 0.0009(11) -0.0023(11) C22 0.064(2) 0.041(2) 0.033(2) -0.0014(13) -0.0042(15) 0.0041(15) C23 0.061(2) 0.056(2) 0.038(2) -0.017(2) 0.003(2) -0.008(2) C24 0.029(2) 0.081(2) 0.024(2) -0.0064(15) 0.0054(12) -0.0040(15) C25 0.048(2) 0.078(2) 0.029(2) 0.011(2) -0.0034(15) 0.015(2) C26 0.048(2) 0.044(2) 0.029(2) 0.0007(13) -0.0018(13) 0.0074(14) C27 0.041(2) 0.143(4) 0.030(2) -0.019(2) 0.001(2) 0.001(2) C28 0.0239(14) 0.046(2) 0.0261(14) 0.0002(12) 0.0029(11) 0.0014(12) C29 0.032(2) 0.056(2) 0.049(2) 0.0123(15) 0.0103(14) 0.0004(14) C30 0.038(2) 0.084(3) 0.051(2) 0.016(2) 0.016(2) -0.010(2) C31 0.032(2) 0.100(3) 0.034(2) 0.003(2) 0.0109(14) 0.000(2) C32 0.037(2) 0.091(3) 0.047(2) 0.004(2) 0.014(2) 0.024(2) C33 0.038(2) 0.054(2) 0.045(2) 0.0074(14) 0.0141(14) 0.0120(14) C34 0.040(2) 0.166(5) 0.060(3) 0.014(3) 0.023(2) 0.000(2) C35 0.0248(13) 0.0261(14) 0.0238(14) 0.0008(10) 0.0006(11) -0.0039(10) C36 0.0316(15) 0.0309(14) 0.030(2) 0.0008(11) 0.0026(12) 0.0028(11) C37 0.033(2) 0.037(2) 0.038(2) 0.0107(13) 0.0024(13) 0.0054(12) C38 0.0276(15) 0.049(2) 0.028(2) 0.0090(13) -0.0005(12) -0.0039(12) C39 0.041(2) 0.043(2) 0.0255(15) -0.0074(12) 0.0008(13) -0.0035(13) C40 0.035(2) 0.0280(14) 0.0291(15) 0.0012(11) -0.0007(12) 0.0014(11) C41 0.040(2) 0.081(3) 0.031(2) 0.008(2) -0.0051(14) 0.004(2) C42 0.0245(14) 0.0335(15) 0.0281(14) -0.0020(11) 0.0046(11) -0.0044(11) C43 0.033(2) 0.040(2) 0.047(2) 0.0019(13) 0.0146(14) 0.0008(13) C44 0.032(2) 0.050(2) 0.053(2) -0.0013(14) 0.0136(15) 0.0063(13) C45 0.030(2) 0.059(2) 0.050(2) 0.002(2) 0.0151(14) -0.0073(14) C46 0.040(2) 0.049(2) 0.063(2) 0.016(2) 0.020(2) -0.0076(14) C47 0.036(2) 0.043(2) 0.048(2) 0.0079(14) 0.0121(14) 0.0026(13) C48 0.039(2) 0.096(3) 0.081(3) 0.015(2) 0.029(2) -0.004(2) N5 0.0274(11) 0.0259(11) 0.0240(11) -0.0003(9) 0.0036(9) 0.0017(9) C49 0.0195(13) 0.0239(12) 0.0301(14) 0.0006(11) 0.0018(10) 0.0010(10) C50 0.0260(14) 0.0289(14) 0.0319(15) -0.0031(11) 0.0048(11) 0.0018(10) C51 0.040(2) 0.0282(15) 0.040(2) -0.0069(12) 0.0069(13) 0.0017(12) C52 0.053(2) 0.0226(14) 0.049(2) -0.0001(13) 0.0042(15) 0.0029(13) C53 0.046(2) 0.0291(15) 0.037(2) 0.0052(12) 0.0039(13) 0.0022(12) C54 0.0301(14) 0.0277(14) 0.0287(14) 0.0024(11) 0.0021(11) 0.0027(11) C55 0.035(2) 0.0340(15) 0.0269(14) -0.0025(11) 0.0057(12) 0.0069(11) C56 0.051(2) 0.046(2) 0.034(2) -0.0077(13) 0.0014(14) 0.0072(14) C57 0.052(2) 0.049(2) 0.040(2) 0.0034(14) 0.0174(15) 0.0032(14) C58 0.045(2) 0.0292(15) 0.0271(15) 0.0048(11) 0.0028(12) 0.0039(12) C59 0.058(2) 0.047(2) 0.041(2) -0.0080(14) 0.012(2) 0.0028(15) C60 0.061(2) 0.050(2) 0.032(2) -0.0027(13) 0.0002(15) 0.006(2) C61 0.071(3) 0.068(3) 0.077(3) -0.026(2) 0.011(2) 0.001(2) C62 0.108(4) 0.091(3) 0.058(3) -0.008(2) 0.032(3) 0.015(3) C63 0.081(4) 0.108(4) 0.099(4) -0.015(3) 0.044(3) 0.006(3) C64 0.074(3) 0.145(5) 0.108(5) -0.021(4) 0.021(3) 0.029(3) C65 0.087(4) 0.119(4) 0.086(4) 0.012(3) 0.010(3) 0.008(3) C66 0.086(3) 0.076(3) 0.083(3) 0.000(2) 0.038(3) -0.011(2) C67 0.101(4) 0.129(5) 0.116(4) -0.039(3) -0.019(3) 0.006(3) C68 0.111(4) 0.092(3) 0.065(3) 0.016(2) 0.039(3) 0.007(3) C69 0.100(4) 0.113(4) 0.068(3) 0.021(3) 0.024(3) 0.002(3) C70 0.141(5) 0.131(5) 0.090(4) 0.016(3) 0.052(4) 0.045(4) C70' 0.141(5) 0.131(5) 0.090(4) 0.016(3) 0.052(4) 0.045(4) C71' 0.121(9) 0.110(8) 0.116(8) 0.016(6) 0.075(7) 0.025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N5 1.863(2) . ? Zr1 N2 2.207(2) . ? Zr1 N1 2.208(2) . ? Zr1 N4 2.220(2) . ? Zr1 N3 2.221(2) . ? N1 C4 1.384(3) . ? N1 C1 1.388(3) . ? N2 C6 1.384(3) . ? N2 C9 1.385(3) . ? N3 C14 1.387(3) . ? N3 C11 1.391(3) . ? N4 C16 1.386(3) . ? N4 C19 1.392(3) . ? C1 C20 1.416(3) . ? C1 C2 1.439(3) . ? C2 C3 1.356(4) . ? C3 C4 1.440(3) . ? C4 C5 1.411(3) . ? C5 C6 1.417(3) . ? C5 C21 1.507(3) . ? C6 C7 1.439(3) . ? C7 C8 1.352(3) . ? C8 C9 1.439(3) . ? C9 C10 1.412(3) . ? C10 C11 1.417(3) . ? C10 C28 1.502(3) . ? C11 C12 1.434(3) . ? C12 C13 1.365(4) . ? C13 C14 1.437(3) . ? C14 C15 1.411(3) . ? C15 C16 1.422(3) . ? C15 C35 1.498(3) . ? C16 C17 1.437(3) . ? C17 C18 1.355(3) . ? C18 C19 1.441(3) . ? C19 C20 1.408(3) . ? C20 C42 1.504(3) . ? C21 C26 1.380(4) . ? C21 C22 1.384(4) . ? C22 C23 1.397(4) . ? C23 C24 1.372(4) . ? C24 C25 1.392(4) . ? C24 C27 1.514(4) . ? C25 C26 1.393(4) . ? C28 C33 1.388(4) . ? C28 C29 1.395(4) . ? C29 C30 1.395(4) . ? C30 C31 1.379(5) . ? C31 C32 1.377(5) . ? C31 C34 1.526(4) . ? C32 C33 1.399(4) . ? C35 C40 1.395(3) . ? C35 C36 1.401(4) . ? C36 C37 1.386(4) . ? C37 C38 1.388(4) . ? C38 C39 1.398(4) . ? C38 C41 1.518(4) . ? C39 C40 1.390(4) . ? C42 C43 1.388(4) . ? C42 C47 1.390(4) . ? C43 C44 1.396(4) . ? C44 C45 1.386(4) . ? C45 C46 1.392(4) . ? C45 C48 1.524(4) . ? C46 C47 1.390(4) . ? N5 C49 1.383(3) . ? C49 C54 1.423(3) . ? C49 C50 1.427(3) . ? C50 C51 1.397(3) . ? C50 C55 1.520(4) . ? C51 C52 1.386(4) . ? C52 C53 1.388(4) . ? C53 C54 1.391(4) . ? C54 C58 1.523(4) . ? C55 C56 1.533(4) . ? C55 C57 1.537(4) . ? C58 C60 1.517(4) . ? C58 C59 1.518(4) . ? C61 C62 1.392(6) . ? C61 C66 1.418(6) . ? C61 C67 1.515(6) . ? C62 C63 1.349(6) . ? C63 C64 1.344(7) . ? C64 C65 1.344(6) . ? C65 C66 1.370(6) . ? C68 C69 1.514(6) . ? C68 C68 1.553(8) 3_575 ? C69 C70' 1.525(6) . ? C69 C70 1.525(6) . ? C70' C71' 1.470(10) . ? 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 N5 Zr1 N2 107.31(8) . . ? N5 Zr1 N1 108.02(8) . . ? N2 Zr1 N1 83.85(7) . . ? N5 Zr1 N4 112.67(8) . . ? N2 Zr1 N4 140.01(7) . . ? N1 Zr1 N4 83.14(7) . . ? N5 Zr1 N3 111.60(8) . . ? N2 Zr1 N3 83.44(7) . . ? N1 Zr1 N3 140.36(7) . . ? N4 Zr1 N3 82.95(7) . . ? C4 N1 C1 107.2(2) . . ? C4 N1 Zr1 122.94(15) . . ? C1 N1 Zr1 127.2(2) . . ? C6 N2 C9 107.5(2) . . ? C6 N2 Zr1 121.6(2) . . ? C9 N2 Zr1 123.7(2) . . ? C14 N3 C11 107.0(2) . . ? C14 N3 Zr1 124.8(2) . . ? C11 N3 Zr1 124.4(2) . . ? C16 N4 C19 107.3(2) . . ? C16 N4 Zr1 124.6(2) . . ? C19 N4 Zr1 126.9(2) . . ? N1 C1 C20 125.2(2) . . ? N1 C1 C2 108.4(2) . . ? C20 C1 C2 126.4(2) . . ? C3 C2 C1 108.1(2) . . ? C2 C3 C4 107.4(2) . . ? N1 C4 C5 125.2(2) . . ? N1 C4 C3 108.9(2) . . ? C5 C4 C3 125.9(2) . . ? C4 C5 C6 126.6(2) . . ? C4 C5 C21 116.3(2) . . ? C6 C5 C21 117.1(2) . . ? N2 C6 C5 125.6(2) . . ? N2 C6 C7 108.4(2) . . ? C5 C6 C7 126.0(2) . . ? C8 C7 C6 108.0(2) . . ? C7 C8 C9 107.7(2) . . ? N2 C9 C10 125.2(2) . . ? N2 C9 C8 108.5(2) . . ? C10 C9 C8 126.2(2) . . ? C9 C10 C11 126.7(2) . . ? C9 C10 C28 116.9(2) . . ? C11 C10 C28 116.3(2) . . ? N3 C11 C10 125.2(2) . . ? N3 C11 C12 108.8(2) . . ? C10 C11 C12 126.0(2) . . ? C13 C12 C11 107.7(2) . . ? C12 C13 C14 107.5(2) . . ? N3 C14 C15 125.0(2) . . ? N3 C14 C13 108.9(2) . . ? C15 C14 C13 126.0(2) . . ? C14 C15 C16 125.8(2) . . ? C14 C15 C35 118.1(2) . . ? C16 C15 C35 116.1(2) . . ? N4 C16 C15 126.0(2) . . ? N4 C16 C17 108.8(2) . . ? C15 C16 C17 125.1(2) . . ? C18 C17 C16 107.6(2) . . ? C17 C18 C19 108.1(2) . . ? N4 C19 C20 125.8(2) . . ? N4 C19 C18 108.1(2) . . ? C20 C19 C18 126.0(2) . . ? C19 C20 C1 126.3(2) . . ? C19 C20 C42 116.7(2) . . ? C1 C20 C42 117.0(2) . . ? C26 C21 C22 117.9(3) . . ? C26 C21 C5 122.7(2) . . ? C22 C21 C5 119.3(2) . . ? C21 C22 C23 120.9(3) . . ? C24 C23 C22 121.6(3) . . ? C23 C24 C25 117.3(3) . . ? C23 C24 C27 121.8(3) . . ? C25 C24 C27 120.9(3) . . ? C24 C25 C26 121.5(3) . . ? C21 C26 C25 120.8(3) . . ? C33 C28 C29 117.7(2) . . ? C33 C28 C10 122.1(2) . . ? C29 C28 C10 120.3(2) . . ? C28 C29 C30 120.9(3) . . ? C31 C30 C29 121.1(3) . . ? C32 C31 C30 118.2(3) . . ? C32 C31 C34 120.9(3) . . ? C30 C31 C34 121.0(3) . . ? C31 C32 C33 121.4(3) . . ? C28 C33 C32 120.7(3) . . ? C40 C35 C36 118.0(2) . . ? C40 C35 C15 122.2(2) . . ? C36 C35 C15 119.8(2) . . ? C37 C36 C35 120.5(3) . . ? C36 C37 C38 121.9(3) . . ? C37 C38 C39 117.5(2) . . ? C37 C38 C41 121.3(3) . . ? C39 C38 C41 121.2(3) . . ? C40 C39 C38 121.2(3) . . ? C39 C40 C35 120.9(2) . . ? C43 C42 C47 118.3(2) . . ? C43 C42 C20 120.6(2) . . ? C47 C42 C20 121.0(2) . . ? C42 C43 C44 120.9(3) . . ? C45 C44 C43 121.0(3) . . ? C44 C45 C46 117.8(3) . . ? C44 C45 C48 121.1(3) . . ? C46 C45 C48 121.1(3) . . ? C47 C46 C45 121.6(3) . . ? C46 C47 C42 120.4(3) . . ? C49 N5 Zr1 172.5(2) . . ? N5 C49 C54 119.9(2) . . ? N5 C49 C50 120.7(2) . . ? C54 C49 C50 119.4(2) . . ? C51 C50 C49 118.9(2) . . ? C51 C50 C55 121.3(2) . . ? C49 C50 C55 119.8(2) . . ? C52 C51 C50 121.3(2) . . ? C51 C52 C53 119.7(3) . . ? C52 C53 C54 121.4(3) . . ? C53 C54 C49 119.1(2) . . ? C53 C54 C58 122.0(2) . . ? C49 C54 C58 118.9(2) . . ? C50 C55 C56 113.6(2) . . ? C50 C55 C57 110.8(2) . . ? C56 C55 C57 110.7(2) . . ? C60 C58 C59 111.5(2) . . ? C60 C58 C54 114.4(2) . . ? C59 C58 C54 109.7(2) . . ? C62 C61 C66 116.5(4) . . ? C62 C61 C67 121.7(5) . . ? C66 C61 C67 121.8(4) . . ? C63 C62 C61 121.0(4) . . ? C64 C63 C62 121.2(5) . . ? C63 C64 C65 120.7(5) . . ? C64 C65 C66 120.4(5) . . ? C65 C66 C61 120.2(4) . . ? C69 C68 C68 114.0(5) . 3_575 ? C68 C69 C70' 114.1(4) . . ? C68 C69 C70 114.1(4) . . ? C71' C70' C69 118.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C4 71.6(2) . . . . ? N2 Zr1 N1 C4 -34.7(2) . . . . ? N4 Zr1 N1 C4 -176.8(2) . . . . ? N3 Zr1 N1 C4 -106.6(2) . . . . ? N5 Zr1 N1 C1 -87.6(2) . . . . ? N2 Zr1 N1 C1 166.1(2) . . . . ? N4 Zr1 N1 C1 24.0(2) . . . . ? N3 Zr1 N1 C1 94.2(2) . . . . ? N5 Zr1 N2 C6 -70.0(2) . . . . ? N1 Zr1 N2 C6 37.0(2) . . . . ? N4 Zr1 N2 C6 108.6(2) . . . . ? N3 Zr1 N2 C6 179.4(2) . . . . ? N5 Zr1 N2 C9 76.5(2) . . . . ? N1 Zr1 N2 C9 -176.5(2) . . . . ? N4 Zr1 N2 C9 -104.8(2) . . . . ? N3 Zr1 N2 C9 -34.1(2) . . . . ? N5 Zr1 N3 C14 79.3(2) . . . . ? N2 Zr1 N3 C14 -174.7(2) . . . . ? N1 Zr1 N3 C14 -102.6(2) . . . . ? N4 Zr1 N3 C14 -32.4(2) . . . . ? N5 Zr1 N3 C11 -75.9(2) . . . . ? N2 Zr1 N3 C11 30.2(2) . . . . ? N1 Zr1 N3 C11 102.2(2) . . . . ? N4 Zr1 N3 C11 172.5(2) . . . . ? N5 Zr1 N4 C16 -80.8(2) . . . . ? N2 Zr1 N4 C16 100.6(2) . . . . ? N1 Zr1 N4 C16 172.5(2) . . . . ? N3 Zr1 N4 C16 29.7(2) . . . . ? N5 Zr1 N4 C19 85.3(2) . . . . ? N2 Zr1 N4 C19 -93.3(2) . . . . ? N1 Zr1 N4 C19 -21.4(2) . . . . ? N3 Zr1 N4 C19 -164.2(2) . . . . ? C4 N1 C1 C20 178.9(2) . . . . ? Zr1 N1 C1 C20 -19.3(3) . . . . ? C4 N1 C1 C2 -1.0(3) . . . . ? Zr1 N1 C1 C2 160.8(2) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? C20 C1 C2 C3 -179.9(2) . . . . ? C1 C2 C3 C4 1.0(3) . . . . ? C1 N1 C4 C5 -176.0(2) . . . . ? Zr1 N1 C4 C5 21.2(3) . . . . ? C1 N1 C4 C3 1.6(3) . . . . ? Zr1 N1 C4 C3 -161.2(2) . . . . ? C2 C3 C4 N1 -1.6(3) . . . . ? C2 C3 C4 C5 176.0(3) . . . . ? N1 C4 C5 C6 6.2(4) . . . . ? C3 C4 C5 C6 -171.0(2) . . . . ? N1 C4 C5 C21 -173.3(2) . . . . ? C3 C4 C5 C21 9.5(4) . . . . ? C9 N2 C6 C5 -178.2(2) . . . . ? Zr1 N2 C6 C5 -26.9(3) . . . . ? C9 N2 C6 C7 0.4(3) . . . . ? Zr1 N2 C6 C7 151.7(2) . . . . ? C4 C5 C6 N2 -2.9(4) . . . . ? C21 C5 C6 N2 176.6(2) . . . . ? C4 C5 C6 C7 178.7(2) . . . . ? C21 C5 C6 C7 -1.7(4) . . . . ? N2 C6 C7 C8 -0.3(3) . . . . ? C5 C6 C7 C8 178.3(2) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C6 N2 C9 C10 177.8(2) . . . . ? Zr1 N2 C9 C10 27.3(3) . . . . ? C6 N2 C9 C8 -0.4(3) . . . . ? Zr1 N2 C9 C8 -150.9(2) . . . . ? C7 C8 C9 N2 0.2(3) . . . . ? C7 C8 C9 C10 -178.0(2) . . . . ? N2 C9 C10 C11 -0.8(4) . . . . ? C8 C9 C10 C11 177.2(2) . . . . ? N2 C9 C10 C28 -177.6(2) . . . . ? C8 C9 C10 C28 0.3(4) . . . . ? C14 N3 C11 C10 -177.5(2) . . . . ? Zr1 N3 C11 C10 -18.6(3) . . . . ? C14 N3 C11 C12 1.3(3) . . . . ? Zr1 N3 C11 C12 160.2(2) . . . . ? C9 C10 C11 N3 -3.9(4) . . . . ? C28 C10 C11 N3 173.0(2) . . . . ? C9 C10 C11 C12 177.5(2) . . . . ? C28 C10 C11 C12 -5.6(4) . . . . ? N3 C11 C12 C13 -2.2(3) . . . . ? C10 C11 C12 C13 176.6(2) . . . . ? C11 C12 C13 C14 2.1(3) . . . . ? C11 N3 C14 C15 -179.6(2) . . . . ? Zr1 N3 C14 C15 21.6(3) . . . . ? C11 N3 C14 C13 0.0(2) . . . . ? Zr1 N3 C14 C13 -158.8(2) . . . . ? C12 C13 C14 N3 -1.3(3) . . . . ? C12 C13 C14 C15 178.3(2) . . . . ? N3 C14 C15 C16 7.2(4) . . . . ? C13 C14 C15 C16 -172.3(2) . . . . ? N3 C14 C15 C35 -172.3(2) . . . . ? C13 C14 C15 C35 8.2(4) . . . . ? C19 N4 C16 C15 175.2(2) . . . . ? Zr1 N4 C16 C15 -16.5(3) . . . . ? C19 N4 C16 C17 -0.3(3) . . . . ? Zr1 N4 C16 C17 168.1(2) . . . . ? C14 C15 C16 N4 -10.0(4) . . . . ? C35 C15 C16 N4 169.5(2) . . . . ? C14 C15 C16 C17 164.7(2) . . . . ? C35 C15 C16 C17 -15.7(3) . . . . ? N4 C16 C17 C18 0.6(3) . . . . ? C15 C16 C17 C18 -174.9(2) . . . . ? C16 C17 C18 C19 -0.6(3) . . . . ? C16 N4 C19 C20 -178.0(2) . . . . ? Zr1 N4 C19 C20 14.0(3) . . . . ? C16 N4 C19 C18 -0.1(2) . . . . ? Zr1 N4 C19 C18 -168.1(2) . . . . ? C17 C18 C19 N4 0.5(3) . . . . ? C17 C18 C19 C20 178.4(2) . . . . ? N4 C19 C20 C1 2.1(4) . . . . ? C18 C19 C20 C1 -175.4(2) . . . . ? N4 C19 C20 C42 -179.8(2) . . . . ? C18 C19 C20 C42 2.6(4) . . . . ? N1 C1 C20 C19 0.6(4) . . . . ? C2 C1 C20 C19 -179.5(2) . . . . ? N1 C1 C20 C42 -177.4(2) . . . . ? C2 C1 C20 C42 2.4(4) . . . . ? C4 C5 C21 C26 -103.4(3) . . . . ? C6 C5 C21 C26 77.0(3) . . . . ? C4 C5 C21 C22 77.6(3) . . . . ? C6 C5 C21 C22 -102.0(3) . . . . ? C26 C21 C22 C23 -0.9(4) . . . . ? C5 C21 C22 C23 178.2(3) . . . . ? C21 C22 C23 C24 0.8(5) . . . . ? C22 C23 C24 C25 0.0(5) . . . . ? C22 C23 C24 C27 -178.4(3) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C27 C24 C25 C26 177.8(3) . . . . ? C22 C21 C26 C25 0.2(4) . . . . ? C5 C21 C26 C25 -178.8(3) . . . . ? C24 C25 C26 C21 0.5(5) . . . . ? C9 C10 C28 C33 -67.0(3) . . . . ? C11 C10 C28 C33 115.8(3) . . . . ? C9 C10 C28 C29 112.5(3) . . . . ? C11 C10 C28 C29 -64.7(3) . . . . ? C33 C28 C29 C30 0.7(4) . . . . ? C10 C28 C29 C30 -178.8(3) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C29 C30 C31 C32 -0.7(5) . . . . ? C29 C30 C31 C34 178.0(3) . . . . ? C30 C31 C32 C33 0.0(5) . . . . ? C34 C31 C32 C33 -178.7(3) . . . . ? C29 C28 C33 C32 -1.4(4) . . . . ? C10 C28 C33 C32 178.1(3) . . . . ? C31 C32 C33 C28 1.1(5) . . . . ? C14 C15 C35 C40 -62.6(3) . . . . ? C16 C15 C35 C40 117.9(3) . . . . ? C14 C15 C35 C36 117.1(3) . . . . ? C16 C15 C35 C36 -62.5(3) . . . . ? C40 C35 C36 C37 1.2(4) . . . . ? C15 C35 C36 C37 -178.5(2) . . . . ? C35 C36 C37 C38 -0.6(4) . . . . ? C36 C37 C38 C39 -0.3(4) . . . . ? C36 C37 C38 C41 -179.9(3) . . . . ? C37 C38 C39 C40 0.6(4) . . . . ? C41 C38 C39 C40 -179.8(3) . . . . ? C38 C39 C40 C35 0.0(4) . . . . ? C36 C35 C40 C39 -0.9(4) . . . . ? C15 C35 C40 C39 178.8(2) . . . . ? C19 C20 C42 C43 66.8(3) . . . . ? C1 C20 C42 C43 -114.9(3) . . . . ? C19 C20 C42 C47 -112.5(3) . . . . ? C1 C20 C42 C47 65.8(3) . . . . ? C47 C42 C43 C44 0.0(4) . . . . ? C20 C42 C43 C44 -179.3(2) . . . . ? C42 C43 C44 C45 -1.1(5) . . . . ? C43 C44 C45 C46 1.8(5) . . . . ? C43 C44 C45 C48 -178.7(3) . . . . ? C44 C45 C46 C47 -1.5(5) . . . . ? C48 C45 C46 C47 178.9(3) . . . . ? C45 C46 C47 C42 0.5(5) . . . . ? C43 C42 C47 C46 0.3(4) . . . . ? C20 C42 C47 C46 179.6(3) . . . . ? N2 Zr1 N5 C49 -141.2(13) . . . . ? N1 Zr1 N5 C49 129.8(13) . . . . ? N4 Zr1 N5 C49 39.8(13) . . . . ? N3 Zr1 N5 C49 -51.5(13) . . . . ? Zr1 N5 C49 C54 26.8(14) . . . . ? Zr1 N5 C49 C50 -152.9(12) . . . . ? N5 C49 C50 C51 177.9(2) . . . . ? C54 C49 C50 C51 -1.9(3) . . . . ? N5 C49 C50 C55 -1.7(3) . . . . ? C54 C49 C50 C55 178.6(2) . . . . ? C49 C50 C51 C52 0.0(4) . . . . ? C55 C50 C51 C52 179.5(3) . . . . ? C50 C51 C52 C53 1.5(4) . . . . ? C51 C52 C53 C54 -1.1(4) . . . . ? C52 C53 C54 C49 -0.8(4) . . . . ? C52 C53 C54 C58 177.4(3) . . . . ? N5 C49 C54 C53 -177.5(2) . . . . ? C50 C49 C54 C53 2.2(4) . . . . ? N5 C49 C54 C58 4.3(3) . . . . ? C50 C49 C54 C58 -176.0(2) . . . . ? C51 C50 C55 C56 26.5(3) . . . . ? C49 C50 C55 C56 -153.9(2) . . . . ? C51 C50 C55 C57 -98.7(3) . . . . ? C49 C50 C55 C57 80.8(3) . . . . ? C53 C54 C58 C60 28.2(4) . . . . ? C49 C54 C58 C60 -153.7(3) . . . . ? C53 C54 C58 C59 -97.9(3) . . . . ? C49 C54 C58 C59 80.2(3) . . . . ? C66 C61 C62 C63 0.4(6) . . . . ? C67 C61 C62 C63 -179.6(4) . . . . ? C61 C62 C63 C64 -1.2(7) . . . . ? C62 C63 C64 C65 1.2(8) . . . . ? C63 C64 C65 C66 -0.4(8) . . . . ? C64 C65 C66 C61 -0.3(8) . . . . ? C62 C61 C66 C65 0.3(6) . . . . ? C67 C61 C66 C65 -179.7(4) . . . . ? C68 C68 C69 C70' -177.1(4) 3_575 . . . ? C68 C68 C69 C70 -177.1(4) 3_575 . . . ? C68 C69 C70' C71' 67.2(8) . . . . ? C70 C69 C70' C71' 0.0(1000) . . . . ? _refine_diff_density_max 0.305 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.055 data_98063 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 98063 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C70.50 H69 Hf N5' _chemical_formula_weight 1164.80 _chemical_melting_point ? _chemical_compound_source 'J. Thorman / Prof. K. Woo - ISU' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hf' 'Hf' -0.5830 6.1852 '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-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.6081(2) _cell_length_b 18.6360(3) _cell_length_c 19.3910(1) _cell_angle_alpha 90.00 _cell_angle_beta 104.029(1) _cell_angle_gamma 90.00 _cell_volume 5822.67(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method ? _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 1.838 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1996) _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32323 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.06 _reflns_number_total 10215 _reflns_number_observed 9002 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+6.0854P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10215 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_obs 0.0263 _refine_ls_wR_factor_all 0.0602 _refine_ls_wR_factor_obs 0.0573 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.076 _refine_ls_shift/esd_max -0.011 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hf1 Hf -0.087843(7) 0.852927(6) 0.366437(6) 0.01930(4) Uani 1 d . . N1 N -0.05394(14) 0.89105(12) 0.27095(12) 0.0225(5) Uani 1 d . . N2 N -0.21251(14) 0.88714(12) 0.31219(12) 0.0220(5) Uani 1 d . . N3 N -0.12337(14) 0.89067(12) 0.46204(12) 0.0223(5) Uani 1 d . . N4 N 0.03442(14) 0.89506(12) 0.42062(12) 0.0219(5) Uani 1 d . . C1 C 0.0252(2) 0.9030(2) 0.2622(2) 0.0255(6) Uani 1 d . . C2 C 0.0209(2) 0.9055(2) 0.1872(2) 0.0324(7) Uani 1 d . . H2A H 0.0662(2) 0.9129(2) 0.1662(2) 0.039 Uiso 1 calc R . C3 C -0.0589(2) 0.8953(2) 0.1522(2) 0.0317(7) Uani 1 d . . H3A H -0.0796(2) 0.8939(2) 0.1020(2) 0.038 Uiso 1 calc R . C4 C -0.1068(2) 0.8870(2) 0.20389(15) 0.0254(6) Uani 1 d . . C5 C -0.1935(2) 0.8796(2) 0.18916(15) 0.0254(6) Uani 1 d . . C6 C -0.2423(2) 0.88091(15) 0.23918(15) 0.0234(6) Uani 1 d . . C7 C -0.3309(2) 0.8750(2) 0.2235(2) 0.0285(7) Uani 1 d . . H7A H -0.3669(2) 0.8707(2) 0.1775(2) 0.034 Uiso 1 calc R . C8 C -0.3544(2) 0.8767(2) 0.2856(2) 0.0293(7) Uani 1 d . . H8A H -0.4095(2) 0.8732(2) 0.2911(2) 0.035 Uiso 1 calc R . C9 C -0.2801(2) 0.88477(15) 0.3420(2) 0.0237(6) Uani 1 d . . C10 C -0.2768(2) 0.8870(2) 0.4152(2) 0.0253(6) Uani 1 d . . C11 C -0.2040(2) 0.8919(2) 0.4706(2) 0.0244(6) Uani 1 d . . C12 C -0.2011(2) 0.8966(2) 0.5448(2) 0.0281(7) Uani 1 d . . H12A H -0.2476(2) 0.8994(2) 0.5653(2) 0.034 Uiso 1 calc R . C13 C -0.1204(2) 0.8962(2) 0.5806(2) 0.0268(7) Uani 1 d . . H13A H -0.0999(2) 0.8978(2) 0.6307(2) 0.032 Uiso 1 calc R . C14 C -0.0710(2) 0.89306(14) 0.52940(15) 0.0226(6) Uani 1 d . . C15 C 0.0166(2) 0.89329(14) 0.54436(15) 0.0240(6) Uani 1 d . . C16 C 0.0642(2) 0.89888(14) 0.49349(15) 0.0231(6) Uani 1 d . . C17 C 0.1513(2) 0.9152(2) 0.5093(2) 0.0278(7) Uani 1 d . . H17A H 0.1870(2) 0.9203(2) 0.5554(2) 0.033 Uiso 1 calc R . C18 C 0.1734(2) 0.9218(2) 0.4470(2) 0.0273(7) Uani 1 d . . H18A H 0.2272(2) 0.9331(2) 0.4413(2) 0.033 Uiso 1 calc R . C19 C 0.1004(2) 0.90850(15) 0.39064(15) 0.0233(6) Uani 1 d . . C20 C 0.0969(2) 0.91180(15) 0.3176(2) 0.0243(6) Uani 1 d . . C21 C -0.2378(2) 0.8682(2) 0.11271(15) 0.0275(7) Uani 1 d . . C22 C -0.2348(2) 0.8019(2) 0.0820(2) 0.0449(9) Uani 1 d . . H22A H -0.2036(2) 0.7644(2) 0.1093(2) 0.054 Uiso 1 calc R . C23 C -0.2764(2) 0.7890(2) 0.0120(2) 0.0514(10) Uani 1 d . . H23A H -0.2733(2) 0.7427(2) -0.0077(2) 0.062 Uiso 1 calc R . C24 C -0.3220(2) 0.8416(2) -0.0294(2) 0.0431(9) Uani 1 d . . C25 C -0.3241(2) 0.9083(2) 0.0013(2) 0.0493(10) Uani 1 d . . H25A H -0.3546(2) 0.9459(2) -0.0265(2) 0.059 Uiso 1 calc R . C26 C -0.2828(2) 0.9223(2) 0.0715(2) 0.0402(8) Uani 1 d . . H26A H -0.2855(2) 0.9687(2) 0.0912(2) 0.048 Uiso 1 calc R . C27 C -0.3696(2) 0.8273(3) -0.1046(2) 0.0710(14) Uani 1 d . . H27A H -0.3977(2) 0.7811(3) -0.1069(2) 0.106 Uiso 1 d R . H27B H -0.3312(2) 0.8265(3) -0.1357(2) 0.106 Uiso 1 d R . H27C H -0.4108(2) 0.8650(3) -0.1201(2) 0.106 Uiso 1 d R . C28 C -0.3567(2) 0.8806(2) 0.4367(2) 0.0300(7) Uani 1 d . . C29 C -0.3727(2) 0.8203(2) 0.4737(2) 0.0425(8) Uani 1 d . . H29A H -0.3318(2) 0.7838(2) 0.4862(2) 0.051 Uiso 1 calc R . C30 C -0.4478(2) 0.8131(2) 0.4926(2) 0.0518(10) Uani 1 d . . H30A H -0.4575(2) 0.7716(2) 0.5178(2) 0.062 Uiso 1 calc R . C31 C -0.5084(2) 0.8648(3) 0.4755(2) 0.0519(11) Uani 1 d . . C32 C -0.4924(2) 0.9245(2) 0.4397(2) 0.0509(10) Uani 1 d . . H32A H -0.5334(2) 0.9610(2) 0.4278(2) 0.061 Uiso 1 calc R . C33 C -0.4178(2) 0.9330(2) 0.4204(2) 0.0421(8) Uani 1 d . . H33A H -0.4084(2) 0.9751(2) 0.3957(2) 0.050 Uiso 1 calc R . C34 C -0.5913(2) 0.8553(3) 0.4949(2) 0.081(2) Uani 1 d . . H34A H -0.5854(2) 0.8201(3) 0.5330(2) 0.121 Uiso 1 d R . H34B H -0.6329(2) 0.8387(3) 0.4532(2) 0.121 Uiso 1 d R . H34C H -0.6090(2) 0.9010(3) 0.5108(2) 0.121 Uiso 1 d R . C35 C 0.0636(2) 0.8870(2) 0.62033(15) 0.0252(6) Uani 1 d . . C36 C 0.1159(2) 0.8281(2) 0.6417(2) 0.0288(7) Uani 1 d . . H36A H 0.1219(2) 0.7932(2) 0.6076(2) 0.035 Uiso 1 calc R . C37 C 0.1588(2) 0.8202(2) 0.7118(2) 0.0339(7) Uani 1 d . . H37A H 0.1932(2) 0.7794(2) 0.7252(2) 0.041 Uiso 1 calc R . C38 C 0.1528(2) 0.8705(2) 0.7630(2) 0.0329(7) Uani 1 d . . C39 C 0.1017(2) 0.9296(2) 0.7415(2) 0.0352(7) Uani 1 d . . H39A H 0.0968(2) 0.9649(2) 0.7756(2) 0.042 Uiso 1 calc R . C40 C 0.0578(2) 0.9379(2) 0.6713(2) 0.0292(7) Uani 1 d . . H40A H 0.0235(2) 0.9789(2) 0.6580(2) 0.035 Uiso 1 calc R . C41 C 0.2001(2) 0.8615(2) 0.8399(2) 0.0497(10) Uani 1 d . . H41A H 0.2143(2) 0.8111(2) 0.8494(2) 0.075 Uiso 1 d R . H41B H 0.1655(2) 0.8776(2) 0.8712(2) 0.075 Uiso 1 d R . H41C H 0.2509(2) 0.8900(2) 0.8488(2) 0.075 Uiso 1 d R . C42 C 0.1766(2) 0.9273(2) 0.2970(2) 0.0264(6) Uani 1 d . . C43 C 0.2417(2) 0.8789(2) 0.3113(2) 0.0353(7) Uani 1 d . . H43A H 0.2356(2) 0.8349(2) 0.3342(2) 0.042 Uiso 1 calc R . C44 C 0.3157(2) 0.8934(2) 0.2928(2) 0.0399(8) Uani 1 d . . H44A H 0.3596(2) 0.8594(2) 0.3037(2) 0.048 Uiso 1 calc R . C45 C 0.3265(2) 0.9563(2) 0.2589(2) 0.0422(8) Uani 1 d . . C46 C 0.2614(2) 1.0055(2) 0.2449(2) 0.0450(9) Uani 1 d . . H46A H 0.2678(2) 1.0495(2) 0.2220(2) 0.054 Uiso 1 calc R . C47 C 0.1875(2) 0.9915(2) 0.2636(2) 0.0380(8) Uani 1 d . . H47A H 0.1440(2) 1.0259(2) 0.2536(2) 0.046 Uiso 1 calc R . C48 C 0.4070(2) 0.9713(3) 0.2373(2) 0.0649(12) Uani 1 d . . H48A H 0.4017(2) 1.0165(3) 0.2114(2) 0.097 Uiso 1 d R . H48B H 0.4183(2) 0.9328(3) 0.2068(2) 0.097 Uiso 1 d R . H48C H 0.4526(2) 0.9745(3) 0.2798(2) 0.097 Uiso 1 d R . N5 N -0.08781(14) 0.75321(12) 0.36357(12) 0.0240(5) Uani 1 d . . C49 C -0.0823(2) 0.67981(15) 0.36943(15) 0.0224(6) Uani 1 d . . C50 C -0.0890(2) 0.6357(2) 0.3082(2) 0.0262(6) Uani 1 d . . C51 C -0.0794(2) 0.5620(2) 0.3169(2) 0.0319(7) Uani 1 d . . H51A H -0.0840(2) 0.5324(2) 0.2762(2) 0.038 Uiso 1 calc R . C52 C -0.0634(2) 0.5305(2) 0.3839(2) 0.0384(8) Uani 1 d . . H52A H -0.0556(2) 0.4801(2) 0.3889(2) 0.046 Uiso 1 calc R . C53 C -0.0589(2) 0.5730(2) 0.4431(2) 0.0338(7) Uani 1 d . . H53A H -0.0494(2) 0.5512(2) 0.4887(2) 0.041 Uiso 1 calc R . C54 C -0.0680(2) 0.6472(2) 0.4373(2) 0.0272(6) Uani 1 d . . C55 C -0.1054(2) 0.6699(2) 0.2354(2) 0.0307(7) Uani 1 d . . H55A H -0.1432(2) 0.7117(2) 0.2355(2) 0.037 Uiso 1 calc R . C56 C -0.1493(2) 0.6192(2) 0.1756(2) 0.0422(8) Uani 1 d . . H56A H -0.1972(2) 0.5972(2) 0.1883(2) 0.063 Uiso 1 d R . H56B H -0.1107(2) 0.5819(2) 0.1686(2) 0.063 Uiso 1 d R . H56C H -0.1680(2) 0.6465(2) 0.1317(2) 0.063 Uiso 1 d R . C57 C -0.0250(2) 0.6992(2) 0.2207(2) 0.0435(8) Uani 1 d . . H57A H 0.0007(2) 0.7326(2) 0.2584(2) 0.065 Uiso 1 d R . H57B H -0.0379(2) 0.7240(2) 0.1750(2) 0.065 Uiso 1 d R . H57C H 0.0132(2) 0.6598(2) 0.2193(2) 0.065 Uiso 1 d R . C58 C -0.0670(2) 0.6937(2) 0.5015(2) 0.0296(7) Uani 1 d . . H58A H -0.0414(2) 0.7405(2) 0.4934(2) 0.035 Uiso 1 calc R . C59 C -0.1551(2) 0.7095(2) 0.5060(2) 0.0447(9) Uani 1 d . . H59A H -0.1538(2) 0.7435(2) 0.5445(2) 0.067 Uiso 1 d R . H59B H -0.1824(2) 0.6654(2) 0.5153(2) 0.067 Uiso 1 d R . H59C H -0.1859(2) 0.7302(2) 0.4611(2) 0.067 Uiso 1 d R . C60 C -0.0160(2) 0.6641(2) 0.5714(2) 0.0455(9) Uani 1 d . . H60A H 0.0392(2) 0.6512(2) 0.5659(2) 0.068 Uiso 1 d R . H60B H -0.0434(2) 0.6217(2) 0.5844(2) 0.068 Uiso 1 d R . H60C H -0.0108(2) 0.7002(2) 0.6086(2) 0.068 Uiso 1 d R . C61 C 0.3061(3) 0.7084(2) 0.2487(3) 0.0677(13) Uani 1 d . . C62 C 0.3707(3) 0.7262(3) 0.2178(3) 0.0740(14) Uani 1 d . . H62A H 0.3585(3) 0.7397(3) 0.1691(3) 0.089 Uiso 1 calc R . C63 C 0.4509(3) 0.7246(3) 0.2559(3) 0.085(2) Uani 1 d . . H63A H 0.4940(3) 0.7358(3) 0.2332(3) 0.102 Uiso 1 calc R . C64 C 0.4702(3) 0.7074(3) 0.3249(3) 0.096(2) Uani 1 d . . H64A H 0.5266(3) 0.7077(3) 0.3509(3) 0.115 Uiso 1 calc R . C65 C 0.4101(3) 0.6895(3) 0.3581(3) 0.088(2) Uani 1 d . . H65A H 0.4242(3) 0.6770(3) 0.4070(3) 0.106 Uiso 1 calc R . C66 C 0.3290(3) 0.6895(3) 0.3208(3) 0.0728(13) Uani 1 d . . H66A H 0.2871(3) 0.6764(3) 0.3442(3) 0.087 Uiso 1 calc R . C67 C 0.2172(4) 0.7097(4) 0.2071(3) 0.114(2) Uani 1 d . . H67A H 0.2117(4) 0.7394(4) 0.1647(3) 0.171 Uiso 1 d R . H67B H 0.1823(4) 0.7291(4) 0.2366(3) 0.171 Uiso 1 d R . H67C H 0.1996(4) 0.6609(4) 0.1928(3) 0.171 Uiso 1 d R . C68 C -0.0346(3) 1.0276(3) -0.0006(3) 0.0801(15) Uani 1 d . . H68A H -0.0380(3) 1.0374(3) 0.0488(3) 0.096 Uiso 1 calc R . H68B H -0.0200(3) 1.0731(3) -0.0209(3) 0.096 Uiso 1 calc R . C69 C -0.1189(3) 1.0030(3) -0.0434(3) 0.085(2) Uani 1 d . . H69A H -0.1342(3) 0.9583(3) -0.0220(3) 0.102 Uiso 1 calc R 1 H69B H -0.1148(3) 0.9915(3) -0.0923(3) 0.102 Uiso 1 calc R 1 C70 C -0.1876(4) 1.0581(4) -0.0474(3) 0.107(2) Uani 0.50 d P 1 H70A H -0.2187(4) 1.0476(4) -0.0117(3) 0.161 Uiso 0.50 d PR 1 H70B H -0.2252(4) 1.0569(4) -0.0947(3) 0.161 Uiso 0.50 d PR 1 H70C H -0.1625(4) 1.1055(4) -0.0385(3) 0.161 Uiso 0.50 d PR 1 C70' C -0.1876(4) 1.0581(4) -0.0474(3) 0.107(2) Uani 0.50 d P 2 H70D H -0.2411(7) 1.0339(6) -0.0680(6) 0.129 Uiso 0.50 calc PR 2 H70E H -0.1878(7) 1.0716(6) 0.0020(6) 0.129 Uiso 0.50 calc PR 2 C71' C -0.1859(7) 1.1241(6) -0.0872(6) 0.091(3) Uani 0.50 d P 2 H71A H -0.2354(7) 1.1519(6) -0.0862(6) 0.137 Uiso 0.50 d PR 2 H71B H -0.1855(7) 1.1134(6) -0.1365(6) 0.137 Uiso 0.50 d PR 2 H71C H -0.1363(7) 1.1517(6) -0.0652(6) 0.137 Uiso 0.50 d PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hf1 0.01875(6) 0.01997(7) 0.01785(7) -0.00009(5) 0.00186(4) -0.00046(5) N1 0.0204(12) 0.0253(13) 0.0205(12) 0.0021(10) 0.0025(10) -0.0029(10) N2 0.0198(12) 0.0256(12) 0.0196(12) 0.0009(10) 0.0026(9) 0.0007(10) N3 0.0211(12) 0.0227(12) 0.0211(12) -0.0019(10) 0.0009(10) 0.0004(10) N4 0.0209(12) 0.0239(13) 0.0198(12) -0.0005(10) 0.0031(10) -0.0009(10) C1 0.0245(15) 0.026(2) 0.026(2) 0.0018(12) 0.0063(12) 0.0004(12) C2 0.029(2) 0.044(2) 0.025(2) 0.0006(14) 0.0092(13) -0.0054(14) C3 0.034(2) 0.042(2) 0.018(2) 0.0019(13) 0.0045(13) -0.0043(14) C4 0.029(2) 0.0245(15) 0.0208(15) 0.0007(12) 0.0032(12) -0.0006(12) C5 0.0256(15) 0.0244(15) 0.023(2) 0.0028(12) -0.0015(12) -0.0007(12) C6 0.0232(14) 0.0217(14) 0.022(2) 0.0024(12) -0.0001(12) 0.0007(12) C7 0.0242(15) 0.033(2) 0.025(2) 0.0045(13) -0.0012(12) 0.0014(13) C8 0.0188(14) 0.037(2) 0.030(2) 0.0018(14) 0.0011(12) -0.0006(13) C9 0.0213(14) 0.0220(14) 0.026(2) 0.0023(12) 0.0025(12) 0.0019(12) C10 0.027(2) 0.0226(15) 0.025(2) 0.0016(12) 0.0042(12) 0.0029(12) C11 0.0242(15) 0.025(2) 0.025(2) -0.0009(12) 0.0065(12) 0.0007(12) C12 0.028(2) 0.030(2) 0.027(2) -0.0038(13) 0.0097(13) -0.0009(13) C13 0.029(2) 0.031(2) 0.021(2) 0.0003(12) 0.0049(12) 0.0009(13) C14 0.0262(15) 0.0199(14) 0.0205(15) -0.0023(11) 0.0034(12) 0.0000(12) C15 0.028(2) 0.0195(14) 0.023(2) -0.0022(12) 0.0015(12) 0.0005(12) C16 0.0235(14) 0.0204(14) 0.0227(15) -0.0019(12) 0.0005(12) 0.0002(11) C17 0.0229(15) 0.032(2) 0.024(2) 0.0014(13) -0.0026(12) -0.0004(13) C18 0.0203(14) 0.029(2) 0.029(2) 0.0010(13) -0.0006(12) -0.0006(12) C19 0.0203(14) 0.0208(14) 0.027(2) 0.0000(12) 0.0019(12) 0.0005(11) C20 0.0204(14) 0.0232(14) 0.030(2) -0.0007(12) 0.0063(12) -0.0006(12) C21 0.0234(15) 0.038(2) 0.0196(15) 0.0013(13) 0.0026(12) -0.0037(13) C22 0.058(2) 0.039(2) 0.030(2) -0.002(2) -0.003(2) 0.003(2) C23 0.057(2) 0.055(2) 0.036(2) -0.015(2) 0.001(2) -0.006(2) C24 0.023(2) 0.082(3) 0.024(2) -0.008(2) 0.0044(13) -0.004(2) C25 0.041(2) 0.076(3) 0.028(2) 0.012(2) 0.001(2) 0.014(2) C26 0.041(2) 0.044(2) 0.032(2) 0.002(2) 0.0000(15) 0.008(2) C27 0.033(2) 0.147(5) 0.028(2) -0.021(2) 0.000(2) 0.002(2) C28 0.0234(15) 0.043(2) 0.023(2) 0.0004(14) 0.0042(12) 0.0000(13) C29 0.032(2) 0.050(2) 0.046(2) 0.011(2) 0.010(2) 0.001(2) C30 0.036(2) 0.073(3) 0.050(2) 0.015(2) 0.016(2) -0.009(2) C31 0.027(2) 0.100(3) 0.031(2) 0.000(2) 0.0099(15) -0.001(2) C32 0.031(2) 0.080(3) 0.043(2) 0.004(2) 0.012(2) 0.019(2) C33 0.034(2) 0.050(2) 0.043(2) 0.007(2) 0.011(2) 0.012(2) C34 0.037(2) 0.155(5) 0.057(3) 0.009(3) 0.023(2) 0.000(3) C35 0.0246(15) 0.026(2) 0.022(2) 0.0004(12) 0.0009(12) -0.0023(12) C36 0.0261(15) 0.029(2) 0.030(2) -0.0004(13) 0.0053(13) 0.0008(13) C37 0.027(2) 0.036(2) 0.035(2) 0.0099(15) 0.0009(13) 0.0068(14) C38 0.027(2) 0.044(2) 0.024(2) 0.0049(14) -0.0004(13) -0.0031(14) C39 0.039(2) 0.038(2) 0.026(2) -0.0051(14) 0.0023(14) -0.0027(15) C40 0.033(2) 0.025(2) 0.026(2) 0.0027(13) -0.0002(13) 0.0024(13) C41 0.041(2) 0.074(3) 0.028(2) 0.009(2) -0.0044(15) 0.004(2) C42 0.0247(15) 0.028(2) 0.025(2) -0.0029(13) 0.0036(12) -0.0030(12) C43 0.033(2) 0.033(2) 0.041(2) 0.0004(15) 0.0105(15) 0.0001(14) C44 0.027(2) 0.047(2) 0.047(2) -0.001(2) 0.0108(15) 0.0052(15) C45 0.030(2) 0.053(2) 0.045(2) 0.001(2) 0.0122(15) -0.007(2) C46 0.038(2) 0.043(2) 0.056(2) 0.012(2) 0.015(2) -0.008(2) C47 0.031(2) 0.037(2) 0.047(2) 0.007(2) 0.0105(15) 0.0014(14) C48 0.039(2) 0.088(3) 0.075(3) 0.012(3) 0.028(2) -0.004(2) N5 0.0251(12) 0.0252(13) 0.0203(12) 0.0002(10) 0.0030(10) 0.0004(10) C49 0.0199(13) 0.0205(14) 0.0251(15) 0.0010(12) 0.0024(11) 0.0000(12) C50 0.0242(14) 0.026(2) 0.027(2) -0.0028(13) 0.0029(12) 0.0027(12) C51 0.034(2) 0.027(2) 0.033(2) -0.0085(14) 0.0063(14) 0.0015(13) C52 0.047(2) 0.021(2) 0.045(2) 0.0013(15) 0.006(2) 0.0040(14) C53 0.043(2) 0.026(2) 0.030(2) 0.0048(14) 0.0051(14) 0.0014(14) C54 0.0272(15) 0.025(2) 0.027(2) 0.0010(13) 0.0021(12) 0.0016(13) C55 0.034(2) 0.029(2) 0.027(2) -0.0047(13) 0.0044(13) 0.0055(13) C56 0.053(2) 0.042(2) 0.028(2) -0.008(2) 0.003(2) 0.007(2) C57 0.048(2) 0.051(2) 0.035(2) 0.002(2) 0.016(2) 0.002(2) C58 0.041(2) 0.023(2) 0.022(2) 0.0025(12) 0.0022(13) 0.0016(13) C59 0.048(2) 0.045(2) 0.040(2) -0.006(2) 0.008(2) 0.002(2) C60 0.055(2) 0.045(2) 0.030(2) 0.000(2) -0.001(2) 0.009(2) C61 0.064(3) 0.060(3) 0.076(3) -0.025(2) 0.010(2) 0.002(2) C62 0.099(4) 0.075(3) 0.053(3) -0.013(2) 0.030(3) 0.010(3) C63 0.075(4) 0.104(4) 0.085(4) -0.015(3) 0.038(3) 0.010(3) C64 0.065(3) 0.125(5) 0.097(5) -0.018(4) 0.016(3) 0.025(3) C65 0.080(4) 0.104(4) 0.076(4) 0.011(3) 0.009(3) 0.012(3) C66 0.083(4) 0.066(3) 0.079(4) -0.004(3) 0.038(3) -0.011(3) C67 0.088(4) 0.122(5) 0.112(5) -0.038(4) -0.015(4) 0.007(4) C68 0.103(4) 0.088(4) 0.058(3) 0.018(3) 0.036(3) 0.009(3) C69 0.095(4) 0.101(4) 0.061(3) 0.025(3) 0.025(3) 0.005(3) C70 0.122(5) 0.126(5) 0.082(4) 0.017(4) 0.042(4) 0.035(4) C70' 0.122(5) 0.126(5) 0.082(4) 0.017(4) 0.042(4) 0.035(4) C71' 0.104(9) 0.103(9) 0.082(8) 0.005(7) 0.052(7) 0.018(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 Hf1 N5 1.859(2) . ? Hf1 N2 2.178(2) . ? Hf1 N1 2.181(2) . ? Hf1 N4 2.193(2) . ? Hf1 N3 2.193(2) . ? N1 C4 1.384(3) . ? N1 C1 1.383(4) . ? N2 C9 1.382(4) . ? N2 C6 1.387(3) . ? N3 C14 1.383(3) . ? N3 C11 1.388(4) . ? N4 C16 1.381(3) . ? N4 C19 1.382(4) . ? C1 C20 1.407(4) . ? C1 C2 1.439(4) . ? C2 C3 1.348(4) . ? C3 C4 1.432(4) . ? C4 C5 1.405(4) . ? C5 C6 1.406(4) . ? C5 C21 1.502(4) . ? C6 C7 1.432(4) . ? C7 C8 1.353(4) . ? C8 C9 1.444(4) . ? C9 C10 1.407(4) . ? C10 C11 1.413(4) . ? C10 C28 1.489(4) . ? C11 C12 1.431(4) . ? C12 C13 1.353(4) . ? C13 C14 1.433(4) . ? C14 C15 1.413(4) . ? C15 C16 1.409(4) . ? C15 C35 1.495(4) . ? C16 C17 1.437(4) . ? C17 C18 1.351(4) . ? C18 C19 1.444(4) . ? C19 C20 1.404(4) . ? C20 C42 1.499(4) . ? C21 C22 1.377(4) . ? C21 C26 1.387(4) . ? C22 C23 1.388(5) . ? C23 C24 1.372(5) . ? C24 C25 1.383(5) . ? C24 C27 1.504(5) . ? C25 C26 1.393(5) . ? C28 C33 1.388(4) . ? C28 C29 1.393(5) . ? C29 C30 1.389(5) . ? C30 C31 1.374(5) . ? C31 C32 1.372(6) . ? C31 C34 1.523(5) . ? C32 C33 1.388(5) . ? C35 C40 1.390(4) . ? C35 C36 1.398(4) . ? C36 C37 1.381(4) . ? C37 C38 1.385(5) . ? C38 C39 1.391(4) . ? C38 C41 1.518(4) . ? C39 C40 1.389(4) . ? C42 C43 1.384(4) . ? C42 C47 1.393(4) . ? C43 C44 1.388(4) . ? C44 C45 1.377(5) . ? C45 C46 1.392(5) . ? C45 C48 1.522(5) . ? C46 C47 1.388(5) . ? N5 C49 1.374(4) . ? C49 C54 1.416(4) . ? C49 C50 1.426(4) . ? C50 C51 1.388(4) . ? C50 C55 1.513(4) . ? C51 C52 1.391(4) . ? C52 C53 1.382(4) . ? C53 C54 1.393(4) . ? C54 C58 1.514(4) . ? C55 C57 1.532(5) . ? C55 C56 1.537(4) . ? C58 C60 1.516(4) . ? C58 C59 1.517(5) . ? C61 C62 1.389(7) . ? C61 C66 1.402(7) . ? C61 C67 1.501(7) . ? C62 C63 1.358(7) . ? C63 C64 1.337(7) . ? C64 C65 1.354(7) . ? C65 C66 1.366(7) . ? C68 C69 1.515(7) . ? C68 C68 1.539(9) 3_575 ? C69 C70' 1.523(7) . ? C69 C70 1.523(7) . ? C70' C71' 1.458(12) . ? 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 N5 Hf1 N2 106.57(9) . . ? N5 Hf1 N1 107.35(9) . . ? N2 Hf1 N1 84.58(8) . . ? N5 Hf1 N4 111.42(9) . . ? N2 Hf1 N4 142.00(8) . . ? N1 Hf1 N4 83.71(8) . . ? N5 Hf1 N3 110.36(9) . . ? N2 Hf1 N3 83.99(8) . . ? N1 Hf1 N3 142.27(8) . . ? N4 Hf1 N3 83.56(8) . . ? C4 N1 C1 107.4(2) . . ? C4 N1 Hf1 123.0(2) . . ? C1 N1 Hf1 127.2(2) . . ? C9 N2 C6 107.4(2) . . ? C9 N2 Hf1 124.2(2) . . ? C6 N2 Hf1 122.0(2) . . ? C14 N3 C11 106.9(2) . . ? C14 N3 Hf1 124.9(2) . . ? C11 N3 Hf1 124.8(2) . . ? C16 N4 C19 107.3(2) . . ? C16 N4 Hf1 124.7(2) . . ? C19 N4 Hf1 126.8(2) . . ? N1 C1 C20 125.3(3) . . ? N1 C1 C2 108.2(2) . . ? C20 C1 C2 126.4(3) . . ? C3 C2 C1 107.9(3) . . ? C2 C3 C4 107.9(3) . . ? N1 C4 C5 125.6(3) . . ? N1 C4 C3 108.5(2) . . ? C5 C4 C3 125.8(3) . . ? C4 C5 C6 126.2(3) . . ? C4 C5 C21 116.6(3) . . ? C6 C5 C21 117.2(2) . . ? N2 C6 C5 125.7(2) . . ? N2 C6 C7 108.5(2) . . ? C5 C6 C7 125.9(3) . . ? C8 C7 C6 108.2(3) . . ? C7 C8 C9 107.4(3) . . ? N2 C9 C10 125.7(2) . . ? N2 C9 C8 108.5(2) . . ? C10 C9 C8 125.7(3) . . ? C9 C10 C11 125.9(3) . . ? C9 C10 C28 117.4(2) . . ? C11 C10 C28 116.6(3) . . ? N3 C11 C10 125.4(3) . . ? N3 C11 C12 108.9(2) . . ? C10 C11 C12 125.6(3) . . ? C13 C12 C11 107.6(3) . . ? C12 C13 C14 107.9(3) . . ? N3 C14 C15 125.1(3) . . ? N3 C14 C13 108.7(2) . . ? C15 C14 C13 126.2(3) . . ? C16 C15 C14 125.5(3) . . ? C16 C15 C35 116.6(2) . . ? C14 C15 C35 117.9(3) . . ? N4 C16 C15 126.2(3) . . ? N4 C16 C17 108.8(2) . . ? C15 C16 C17 124.9(3) . . ? C18 C17 C16 107.8(3) . . ? C17 C18 C19 107.5(3) . . ? N4 C19 C20 126.1(2) . . ? N4 C19 C18 108.6(2) . . ? C20 C19 C18 125.3(3) . . ? C19 C20 C1 125.8(3) . . ? C19 C20 C42 117.0(2) . . ? C1 C20 C42 117.2(3) . . ? C22 C21 C26 118.4(3) . . ? C22 C21 C5 119.5(3) . . ? C26 C21 C5 122.1(3) . . ? C21 C22 C23 121.1(3) . . ? C24 C23 C22 121.5(4) . . ? C23 C24 C25 117.3(3) . . ? C23 C24 C27 121.8(4) . . ? C25 C24 C27 120.9(4) . . ? C24 C25 C26 122.1(3) . . ? C21 C26 C25 119.7(3) . . ? C33 C28 C29 117.7(3) . . ? C33 C28 C10 122.1(3) . . ? C29 C28 C10 120.2(3) . . ? C30 C29 C28 120.6(3) . . ? C31 C30 C29 121.4(4) . . ? C32 C31 C30 118.0(3) . . ? C32 C31 C34 121.1(4) . . ? C30 C31 C34 120.8(4) . . ? C31 C32 C33 121.6(3) . . ? C28 C33 C32 120.6(3) . . ? C40 C35 C36 118.0(3) . . ? C40 C35 C15 122.5(3) . . ? C36 C35 C15 119.4(3) . . ? C37 C36 C35 120.7(3) . . ? C36 C37 C38 121.6(3) . . ? C37 C38 C39 117.8(3) . . ? C37 C38 C41 121.3(3) . . ? C39 C38 C41 120.9(3) . . ? C40 C39 C38 121.2(3) . . ? C39 C40 C35 120.7(3) . . ? C43 C42 C47 118.0(3) . . ? C43 C42 C20 121.3(3) . . ? C47 C42 C20 120.8(3) . . ? C42 C43 C44 121.3(3) . . ? C45 C44 C43 121.0(3) . . ? C44 C45 C46 118.0(3) . . ? C44 C45 C48 120.8(3) . . ? C46 C45 C48 121.2(3) . . ? C47 C46 C45 121.2(3) . . ? C46 C47 C42 120.5(3) . . ? C49 N5 Hf1 173.4(2) . . ? N5 C49 C54 119.8(3) . . ? N5 C49 C50 121.0(3) . . ? C54 C49 C50 119.2(3) . . ? C51 C50 C49 119.1(3) . . ? C51 C50 C55 121.3(3) . . ? C49 C50 C55 119.6(3) . . ? C50 C51 C52 121.4(3) . . ? C53 C52 C51 119.6(3) . . ? C52 C53 C54 121.2(3) . . ? C53 C54 C49 119.5(3) . . ? C53 C54 C58 121.4(3) . . ? C49 C54 C58 119.0(3) . . ? C50 C55 C57 110.8(3) . . ? C50 C55 C56 113.0(3) . . ? C57 C55 C56 110.7(3) . . ? C54 C58 C60 114.9(3) . . ? C54 C58 C59 109.8(3) . . ? C60 C58 C59 110.9(3) . . ? C62 C61 C66 116.0(4) . . ? C62 C61 C67 121.7(5) . . ? C66 C61 C67 122.3(5) . . ? C63 C62 C61 121.2(5) . . ? C64 C63 C62 121.0(5) . . ? C63 C64 C65 120.6(5) . . ? C64 C65 C66 119.6(5) . . ? C65 C66 C61 121.5(5) . . ? C69 C68 C68 113.1(6) . 3_575 ? C68 C69 C70' 113.9(5) . . ? C68 C69 C70 113.9(5) . . ? C71' C70' C69 119.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Hf1 N1 C4 72.6(2) . . . . ? N2 Hf1 N1 C4 -33.1(2) . . . . ? N4 Hf1 N1 C4 -176.9(2) . . . . ? N3 Hf1 N1 C4 -106.0(2) . . . . ? N5 Hf1 N1 C1 -87.7(2) . . . . ? N2 Hf1 N1 C1 166.6(2) . . . . ? N4 Hf1 N1 C1 22.8(2) . . . . ? N3 Hf1 N1 C1 93.7(3) . . . . ? N5 Hf1 N2 C9 77.4(2) . . . . ? N1 Hf1 N2 C9 -176.1(2) . . . . ? N4 Hf1 N2 C9 -103.6(2) . . . . ? N3 Hf1 N2 C9 -32.1(2) . . . . ? N5 Hf1 N2 C6 -71.1(2) . . . . ? N1 Hf1 N2 C6 35.4(2) . . . . ? N4 Hf1 N2 C6 107.9(2) . . . . ? N3 Hf1 N2 C6 179.4(2) . . . . ? N5 Hf1 N3 C14 79.3(2) . . . . ? N2 Hf1 N3 C14 -175.3(2) . . . . ? N1 Hf1 N3 C14 -102.2(2) . . . . ? N4 Hf1 N3 C14 -31.2(2) . . . . ? N5 Hf1 N3 C11 -77.1(2) . . . . ? N2 Hf1 N3 C11 28.3(2) . . . . ? N1 Hf1 N3 C11 101.4(2) . . . . ? N4 Hf1 N3 C11 172.4(2) . . . . ? N5 Hf1 N4 C16 -80.4(2) . . . . ? N2 Hf1 N4 C16 100.6(2) . . . . ? N1 Hf1 N4 C16 173.4(2) . . . . ? N3 Hf1 N4 C16 29.0(2) . . . . ? N5 Hf1 N4 C19 85.7(2) . . . . ? N2 Hf1 N4 C19 -93.4(2) . . . . ? N1 Hf1 N4 C19 -20.6(2) . . . . ? N3 Hf1 N4 C19 -165.0(2) . . . . ? C4 N1 C1 C20 178.7(3) . . . . ? Hf1 N1 C1 C20 -18.6(4) . . . . ? C4 N1 C1 C2 -0.8(3) . . . . ? Hf1 N1 C1 C2 162.0(2) . . . . ? N1 C1 C2 C3 0.1(4) . . . . ? C20 C1 C2 C3 -179.4(3) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C1 N1 C4 C5 -176.0(3) . . . . ? Hf1 N1 C4 C5 20.4(4) . . . . ? C1 N1 C4 C3 1.1(3) . . . . ? Hf1 N1 C4 C3 -162.5(2) . . . . ? C2 C3 C4 N1 -1.1(4) . . . . ? C2 C3 C4 C5 176.0(3) . . . . ? N1 C4 C5 C6 5.7(5) . . . . ? C3 C4 C5 C6 -171.0(3) . . . . ? N1 C4 C5 C21 -173.5(3) . . . . ? C3 C4 C5 C21 9.8(4) . . . . ? C9 N2 C6 C5 -178.8(3) . . . . ? Hf1 N2 C6 C5 -25.7(4) . . . . ? C9 N2 C6 C7 0.4(3) . . . . ? Hf1 N2 C6 C7 153.4(2) . . . . ? C4 C5 C6 N2 -2.6(5) . . . . ? C21 C5 C6 N2 176.5(3) . . . . ? C4 C5 C6 C7 178.4(3) . . . . ? C21 C5 C6 C7 -2.4(4) . . . . ? N2 C6 C7 C8 -0.7(3) . . . . ? C5 C6 C7 C8 178.4(3) . . . . ? C6 C7 C8 C9 0.8(3) . . . . ? C6 N2 C9 C10 177.8(3) . . . . ? Hf1 N2 C9 C10 25.5(4) . . . . ? C6 N2 C9 C8 0.1(3) . . . . ? Hf1 N2 C9 C8 -152.2(2) . . . . ? C7 C8 C9 N2 -0.6(3) . . . . ? C7 C8 C9 C10 -178.3(3) . . . . ? N2 C9 C10 C11 -0.2(5) . . . . ? C8 C9 C10 C11 177.2(3) . . . . ? N2 C9 C10 C28 -177.4(3) . . . . ? C8 C9 C10 C28 -0.1(4) . . . . ? C14 N3 C11 C10 -177.0(3) . . . . ? Hf1 N3 C11 C10 -17.1(4) . . . . ? C14 N3 C11 C12 1.1(3) . . . . ? Hf1 N3 C11 C12 161.1(2) . . . . ? C9 C10 C11 N3 -4.4(5) . . . . ? C28 C10 C11 N3 172.9(3) . . . . ? C9 C10 C11 C12 177.8(3) . . . . ? C28 C10 C11 C12 -4.9(4) . . . . ? N3 C11 C12 C13 -1.6(3) . . . . ? C10 C11 C12 C13 176.5(3) . . . . ? C11 C12 C13 C14 1.4(3) . . . . ? C11 N3 C14 C15 -179.5(3) . . . . ? Hf1 N3 C14 C15 20.6(4) . . . . ? C11 N3 C14 C13 -0.3(3) . . . . ? Hf1 N3 C14 C13 -160.2(2) . . . . ? C12 C13 C14 N3 -0.7(3) . . . . ? C12 C13 C14 C15 178.5(3) . . . . ? N3 C14 C15 C16 7.2(4) . . . . ? C13 C14 C15 C16 -171.9(3) . . . . ? N3 C14 C15 C35 -172.7(3) . . . . ? C13 C14 C15 C35 8.2(4) . . . . ? C19 N4 C16 C15 175.5(3) . . . . ? Hf1 N4 C16 C15 -16.2(4) . . . . ? C19 N4 C16 C17 0.0(3) . . . . ? Hf1 N4 C16 C17 168.3(2) . . . . ? C14 C15 C16 N4 -9.6(5) . . . . ? C35 C15 C16 N4 170.3(3) . . . . ? C14 C15 C16 C17 165.3(3) . . . . ? C35 C15 C16 C17 -14.8(4) . . . . ? N4 C16 C17 C18 0.7(3) . . . . ? C15 C16 C17 C18 -175.0(3) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C16 N4 C19 C20 -178.1(3) . . . . ? Hf1 N4 C19 C20 13.9(4) . . . . ? C16 N4 C19 C18 -0.6(3) . . . . ? Hf1 N4 C19 C18 -168.5(2) . . . . ? C17 C18 C19 N4 1.0(3) . . . . ? C17 C18 C19 C20 178.5(3) . . . . ? N4 C19 C20 C1 1.0(5) . . . . ? C18 C19 C20 C1 -176.1(3) . . . . ? N4 C19 C20 C42 179.9(3) . . . . ? C18 C19 C20 C42 2.8(4) . . . . ? N1 C1 C20 C19 1.4(5) . . . . ? C2 C1 C20 C19 -179.3(3) . . . . ? N1 C1 C20 C42 -177.6(3) . . . . ? C2 C1 C20 C42 1.8(4) . . . . ? C4 C5 C21 C22 76.1(4) . . . . ? C6 C5 C21 C22 -103.2(4) . . . . ? C4 C5 C21 C26 -104.5(4) . . . . ? C6 C5 C21 C26 76.3(4) . . . . ? C26 C21 C22 C23 -0.9(5) . . . . ? C5 C21 C22 C23 178.6(3) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C25 0.7(6) . . . . ? C22 C23 C24 C27 -178.0(4) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C27 C24 C25 C26 177.9(4) . . . . ? C22 C21 C26 C25 0.7(5) . . . . ? C5 C21 C26 C25 -178.7(3) . . . . ? C24 C25 C26 C21 0.2(6) . . . . ? C9 C10 C28 C33 -66.4(4) . . . . ? C11 C10 C28 C33 116.1(3) . . . . ? C9 C10 C28 C29 112.9(3) . . . . ? C11 C10 C28 C29 -64.6(4) . . . . ? C33 C28 C29 C30 0.8(5) . . . . ? C10 C28 C29 C30 -178.5(3) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 C32 -0.7(6) . . . . ? C29 C30 C31 C34 178.4(4) . . . . ? C30 C31 C32 C33 0.5(6) . . . . ? C34 C31 C32 C33 -178.5(4) . . . . ? C29 C28 C33 C32 -0.9(5) . . . . ? C10 C28 C33 C32 178.4(3) . . . . ? C31 C32 C33 C28 0.3(6) . . . . ? C16 C15 C35 C40 118.0(3) . . . . ? C14 C15 C35 C40 -62.1(4) . . . . ? C16 C15 C35 C36 -61.8(4) . . . . ? C14 C15 C35 C36 118.1(3) . . . . ? C40 C35 C36 C37 1.4(5) . . . . ? C15 C35 C36 C37 -178.7(3) . . . . ? C35 C36 C37 C38 -1.0(5) . . . . ? C36 C37 C38 C39 0.1(5) . . . . ? C36 C37 C38 C41 180.0(3) . . . . ? C37 C38 C39 C40 0.3(5) . . . . ? C41 C38 C39 C40 -179.5(3) . . . . ? C38 C39 C40 C35 0.2(5) . . . . ? C36 C35 C40 C39 -1.0(5) . . . . ? C15 C35 C40 C39 179.1(3) . . . . ? C19 C20 C42 C43 66.4(4) . . . . ? C1 C20 C42 C43 -114.5(3) . . . . ? C19 C20 C42 C47 -112.7(3) . . . . ? C1 C20 C42 C47 66.3(4) . . . . ? C47 C42 C43 C44 -0.3(5) . . . . ? C20 C42 C43 C44 -179.5(3) . . . . ? C42 C43 C44 C45 -0.6(5) . . . . ? C43 C44 C45 C46 1.0(5) . . . . ? C43 C44 C45 C48 -178.6(3) . . . . ? C44 C45 C46 C47 -0.6(6) . . . . ? C48 C45 C46 C47 179.0(4) . . . . ? C45 C46 C47 C42 -0.2(5) . . . . ? C43 C42 C47 C46 0.7(5) . . . . ? C20 C42 C47 C46 179.9(3) . . . . ? N2 Hf1 N5 C49 -139.3(18) . . . . ? N1 Hf1 N5 C49 131.3(18) . . . . ? N4 Hf1 N5 C49 41.3(18) . . . . ? N3 Hf1 N5 C49 -49.7(18) . . . . ? Hf1 N5 C49 C54 24.6(20) . . . . ? Hf1 N5 C49 C50 -153.9(17) . . . . ? N5 C49 C50 C51 177.2(3) . . . . ? C54 C49 C50 C51 -1.4(4) . . . . ? N5 C49 C50 C55 -2.2(4) . . . . ? C54 C49 C50 C55 179.2(3) . . . . ? C49 C50 C51 C52 -0.1(5) . . . . ? C55 C50 C51 C52 179.3(3) . . . . ? C50 C51 C52 C53 1.7(5) . . . . ? C51 C52 C53 C54 -1.7(5) . . . . ? C52 C53 C54 C49 0.1(5) . . . . ? C52 C53 C54 C58 177.3(3) . . . . ? N5 C49 C54 C53 -177.2(3) . . . . ? C50 C49 C54 C53 1.4(4) . . . . ? N5 C49 C54 C58 5.6(4) . . . . ? C50 C49 C54 C58 -175.8(3) . . . . ? C51 C50 C55 C57 -98.0(3) . . . . ? C49 C50 C55 C57 81.4(3) . . . . ? C51 C50 C55 C56 26.9(4) . . . . ? C49 C50 C55 C56 -153.7(3) . . . . ? C53 C54 C58 C60 28.7(4) . . . . ? C49 C54 C58 C60 -154.1(3) . . . . ? C53 C54 C58 C59 -97.1(3) . . . . ? C49 C54 C58 C59 80.1(3) . . . . ? C66 C61 C62 C63 0.4(7) . . . . ? C67 C61 C62 C63 -179.7(5) . . . . ? C61 C62 C63 C64 -1.5(8) . . . . ? C62 C63 C64 C65 1.6(9) . . . . ? C63 C64 C65 C66 -0.5(10) . . . . ? C64 C65 C66 C61 -0.7(9) . . . . ? C62 C61 C66 C65 0.7(7) . . . . ? C67 C61 C66 C65 -179.2(5) . . . . ? C68 C68 C69 C70' -178.0(5) 3_575 . . . ? C68 C68 C69 C70 -178.0(5) 3_575 . . . ? C68 C69 C70' C71' 68.3(8) . . . . ? C70 C69 C70' C71' 0.0(1000) . . . . ? _refine_diff_density_max 0.444 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.098 data_woo04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H74 N6 O Zr ' _chemical_formula_weight 1226.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5421(10) _cell_length_b 15.4623(11) _cell_length_c 16.7239(12) _cell_angle_alpha 98.0192(14) _cell_angle_beta 100.8337(14) _cell_angle_gamma 113.9894(11) _cell_volume 3050.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Dark red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker CCD-1000' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19079 _diffrn_reflns_av_R_equivalents 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.86 _reflns_number_total 13540 _reflns_number_gt 11508 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.0566P)^2^+0.6977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13540 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Zr Zr 0.750876(12) 0.153179(11) 0.212653(9) 0.02549(5) Uani 1 1 d . . . O O 0.87371(10) 0.26270(10) 0.31186(7) 0.0388(3) Uani 1 1 d . . . N1 N 0.64559(11) 0.16712(10) 0.10128(8) 0.0299(3) Uani 1 1 d . . . N2 N 0.71611(11) 0.01443(10) 0.12600(8) 0.0293(3) Uani 1 1 d . . . N3 N 0.71352(11) 0.05081(10) 0.29602(8) 0.0285(3) Uani 1 1 d . . . N4 N 0.64287(11) 0.20280(10) 0.27182(8) 0.0292(3) Uani 1 1 d . . . N5 N 1.05331(12) 0.36135(11) 0.29736(10) 0.0377(3) Uani 1 1 d . . . N6 N 0.90881(11) 0.22905(10) 0.19102(8) 0.0305(3) Uani 1 1 d . . . C1 C 0.59213(14) 0.22685(13) 0.09714(10) 0.0325(3) Uani 1 1 d . . . C2 C 0.55564(15) 0.22831(14) 0.01094(10) 0.0356(4) Uani 1 1 d . . . H2A H 0.5154 0.2624 -0.0093 0.043 Uiso 1 1 calc R . . C3 C 0.58881(15) 0.17256(14) -0.03585(11) 0.0367(4) Uani 1 1 d . . . H3A H 0.5776 0.1614 -0.0949 0.044 Uiso 1 1 calc R . . C4 C 0.64416(14) 0.13310(13) 0.01957(10) 0.0310(3) Uani 1 1 d . . . C5 C 0.68294(14) 0.06574(13) -0.00654(10) 0.0315(3) Uani 1 1 d . . . C6 C 0.70982(14) 0.00713(13) 0.04154(10) 0.0314(3) Uani 1 1 d . . . C7 C 0.72278(15) -0.07682(14) 0.00798(11) 0.0365(4) Uani 1 1 d . . . H7A H 0.7238 -0.0970 -0.0480 0.044 Uiso 1 1 calc R . . C8 C 0.73331(15) -0.12219(14) 0.07040(11) 0.0362(4) Uani 1 1 d . . . H8A H 0.7411 -0.1809 0.0660 0.043 Uiso 1 1 calc R . . C9 C 0.73055(14) -0.06491(12) 0.14437(10) 0.0309(3) Uani 1 1 d . . . C10 C 0.73888(14) -0.08669(12) 0.22345(10) 0.0312(3) Uani 1 1 d . . . C11 C 0.73105(13) -0.03154(12) 0.29411(10) 0.0302(3) Uani 1 1 d . . . C12 C 0.73988(15) -0.05185(13) 0.37565(10) 0.0342(4) Uani 1 1 d . . . H12A H 0.7527 -0.1039 0.3913 0.041 Uiso 1 1 calc R . . C13 C 0.72659(15) 0.01667(13) 0.42602(10) 0.0343(4) Uani 1 1 d . . . H13A H 0.7288 0.0216 0.4837 0.041 Uiso 1 1 calc R . . C14 C 0.70856(13) 0.08044(12) 0.37696(10) 0.0298(3) Uani 1 1 d . . . C15 C 0.68478(13) 0.15703(12) 0.40596(10) 0.0297(3) Uani 1 1 d . . . C16 C 0.65354(14) 0.21334(12) 0.35713(10) 0.0303(3) Uani 1 1 d . . . C17 C 0.62170(16) 0.28680(14) 0.38723(11) 0.0371(4) Uani 1 1 d . . . H17A H 0.6225 0.3085 0.4435 0.045 Uiso 1 1 calc R . . C18 C 0.59019(17) 0.31963(14) 0.32036(11) 0.0401(4) Uani 1 1 d . . . H18A H 0.5647 0.3685 0.3211 0.048 Uiso 1 1 calc R . . C19 C 0.60250(14) 0.26691(13) 0.24858(10) 0.0335(3) Uani 1 1 d . . . C20 C 0.57502(15) 0.27664(13) 0.16560(10) 0.0343(4) Uani 1 1 d . . . C21 C 0.69426(14) 0.05283(13) -0.09447(10) 0.0320(3) Uani 1 1 d . . . C22 C 0.60916(17) -0.01494(17) -0.16163(12) 0.0504(5) Uani 1 1 d . . . H22A H 0.5383 -0.0540 -0.1536 0.061 Uiso 1 1 calc R . . C23 C 0.62574(18) -0.02687(17) -0.24111(12) 0.0531(5) Uani 1 1 d . . . H23A H 0.5660 -0.0746 -0.2865 0.064 Uiso 1 1 calc R . . C24 C 0.72605(16) 0.02846(15) -0.25558(11) 0.0385(4) Uani 1 1 d . . . C25 C 0.81041(18) 0.09766(18) -0.18859(13) 0.0543(6) Uani 1 1 d . . . H25A H 0.8803 0.1381 -0.1972 0.065 Uiso 1 1 calc R . . C26 C 0.79532(17) 0.10948(18) -0.10873(12) 0.0522(5) Uani 1 1 d . . . H26A H 0.8552 0.1571 -0.0634 0.063 Uiso 1 1 calc R . . C27 C 0.7442(2) 0.01428(18) -0.34206(12) 0.0533(5) Uani 1 1 d . . . H27A H 0.6756 -0.0380 -0.3814 0.080 Uiso 1 1 calc R . . H27B H 0.8062 -0.0034 -0.3401 0.080 Uiso 1 1 calc R . . H27C H 0.7624 0.0750 -0.3606 0.080 Uiso 1 1 calc R . . C28 C 0.75694(15) -0.17434(13) 0.23332(10) 0.0348(4) Uani 1 1 d . . . C29 C 0.85191(17) -0.18192(16) 0.22122(13) 0.0451(4) Uani 1 1 d . . . H29A H 0.9048 -0.1321 0.2027 0.054 Uiso 1 1 calc R . . C30 C 0.87144(19) -0.26048(17) 0.23552(14) 0.0521(5) Uani 1 1 d . . . H30A H 0.9369 -0.2639 0.2261 0.063 Uiso 1 1 calc R . . C31 C 0.79686(19) -0.33444(16) 0.26348(13) 0.0479(5) Uani 1 1 d . . . C32 C 0.69985(19) -0.32924(15) 0.27250(13) 0.0495(5) Uani 1 1 d . . . H32A H 0.6459 -0.3803 0.2892 0.059 Uiso 1 1 calc R . . C33 C 0.67955(17) -0.25091(14) 0.25770(12) 0.0424(4) Uani 1 1 d . . . H33A H 0.6120 -0.2494 0.2643 0.051 Uiso 1 1 calc R . . C34 C 0.8219(3) -0.4167(2) 0.28412(17) 0.0681(7) Uani 1 1 d . . . H34A H 0.8942 -0.4076 0.2742 0.102 Uiso 1 1 calc R . . H34B H 0.7625 -0.4790 0.2484 0.102 Uiso 1 1 calc R . . H34C H 0.8254 -0.4168 0.3432 0.102 Uiso 1 1 calc R . . C35 C 0.68475(15) 0.17738(13) 0.49649(10) 0.0327(3) Uani 1 1 d . . . C36 C 0.78206(18) 0.23963(14) 0.55837(11) 0.0449(4) Uani 1 1 d . . . H36A H 0.8513 0.2673 0.5444 0.054 Uiso 1 1 calc R . . C37 C 0.7789(2) 0.26196(16) 0.64119(12) 0.0549(6) Uani 1 1 d . . . H37A H 0.8463 0.3056 0.6828 0.066 Uiso 1 1 calc R . . C38 C 0.6808(2) 0.22252(17) 0.66404(12) 0.0521(5) Uani 1 1 d . . . C39 C 0.5851(2) 0.1586(2) 0.60265(14) 0.0673(7) Uani 1 1 d . . . H39A H 0.5165 0.1289 0.6172 0.081 Uiso 1 1 calc R . . C40 C 0.58674(18) 0.1367(2) 0.51990(13) 0.0572(6) Uani 1 1 d . . . H40A H 0.5191 0.0928 0.4786 0.069 Uiso 1 1 calc R . . C41 C 0.6781(3) 0.2497(2) 0.75434(15) 0.0819(9) Uani 1 1 d . . . H41A H 0.6015 0.2146 0.7588 0.123 Uiso 1 1 calc R . . H41B H 0.7027 0.3201 0.7714 0.123 Uiso 1 1 calc R . . H41C H 0.7286 0.2319 0.7910 0.123 Uiso 1 1 calc R . . C42 C 0.52015(17) 0.34172(14) 0.15002(11) 0.0397(4) Uani 1 1 d . . . C43 C 0.5702(2) 0.42211(16) 0.11737(13) 0.0497(5) Uani 1 1 d . . . H43A H 0.6389 0.4353 0.1035 0.060 Uiso 1 1 calc R . . C44 C 0.5187(2) 0.48308(18) 0.10519(14) 0.0603(6) Uani 1 1 d . . . H44A H 0.5539 0.5382 0.0837 0.072 Uiso 1 1 calc R . . C45 C 0.4190(2) 0.46569(18) 0.12331(14) 0.0608(6) Uani 1 1 d . . . C46 C 0.3688(2) 0.38583(19) 0.15544(15) 0.0598(6) Uani 1 1 d . . . H46A H 0.2996 0.3727 0.1686 0.072 Uiso 1 1 calc R . . C47 C 0.41952(19) 0.32440(17) 0.16866(13) 0.0492(5) Uani 1 1 d . . . H47A H 0.3843 0.2699 0.1908 0.059 Uiso 1 1 calc R . . C48 C 0.3650(3) 0.5338(2) 0.1101(2) 0.0907(10) Uani 1 1 d . . . H48A H 0.2946 0.5102 0.1266 0.136 Uiso 1 1 calc R . . H48B H 0.3493 0.5353 0.0508 0.136 Uiso 1 1 calc R . . H48C H 0.4162 0.5996 0.1445 0.136 Uiso 1 1 calc R . . C49 C 0.95489(14) 0.29162(12) 0.27140(10) 0.0310(3) Uani 1 1 d . . . C50 C 1.09235(18) 0.42700(15) 0.38120(13) 0.0492(5) Uani 1 1 d . . . C51 C 1.0903(2) 0.3726(2) 0.45149(15) 0.0733(8) Uani 1 1 d . . . H51A H 1.0127 0.3263 0.4463 0.110 Uiso 1 1 calc R . . H51B H 1.1212 0.4196 0.5061 0.110 Uiso 1 1 calc R . . H51C H 1.1355 0.3372 0.4469 0.110 Uiso 1 1 calc R . . C52 C 1.0208(2) 0.48229(17) 0.38827(15) 0.0576(6) Uani 1 1 d . . . H52A H 1.0220 0.5170 0.3434 0.086 Uiso 1 1 calc R . . H52B H 1.0515 0.5293 0.4429 0.086 Uiso 1 1 calc R . . H52C H 0.9433 0.4358 0.3830 0.086 Uiso 1 1 calc R . . C53 C 1.2136(2) 0.49981(18) 0.38987(17) 0.0699(7) Uani 1 1 d . . . H53A H 1.2150 0.5352 0.3455 0.105 Uiso 1 1 calc R . . H53B H 1.2590 0.4646 0.3849 0.105 Uiso 1 1 calc R . . H53C H 1.2442 0.5462 0.4448 0.105 Uiso 1 1 calc R . . C54 C 0.97207(14) 0.24721(13) 0.13097(11) 0.0341(4) Uani 1 1 d . . . C55 C 0.97783(16) 0.32034(15) 0.08819(12) 0.0428(4) Uani 1 1 d . . . C56 C 1.03733(17) 0.33321(17) 0.02741(13) 0.0498(5) Uani 1 1 d . . . H56A H 1.0417 0.3824 -0.0019 0.060 Uiso 1 1 calc R . . C57 C 1.08930(18) 0.27638(17) 0.00943(14) 0.0549(6) Uani 1 1 d . . . H57A H 1.1278 0.2851 -0.0330 0.066 Uiso 1 1 calc R . . C58 C 1.0857(2) 0.20640(17) 0.05306(17) 0.0612(6) Uani 1 1 d . . . H58A H 1.1232 0.1679 0.0409 0.073 Uiso 1 1 calc R . . C59 C 1.02842(18) 0.19089(15) 0.11461(15) 0.0486(5) Uani 1 1 d . . . C60 C 0.9290(2) 0.3908(2) 0.11141(17) 0.0637(7) Uani 1 1 d . . . H60A H 0.8837 0.3663 0.1513 0.076 Uiso 1 1 calc R . . C61 C 0.8511(2) 0.3947(2) 0.0346(2) 0.0907(11) Uani 1 1 d . . . H61A H 0.8216 0.4406 0.0516 0.136 Uiso 1 1 calc R . . H61B H 0.7886 0.3297 0.0093 0.136 Uiso 1 1 calc R . . H61C H 0.8929 0.4163 -0.0064 0.136 Uiso 1 1 calc R . . C62 C 1.0228(3) 0.4927(2) 0.15601(17) 0.0732(8) Uani 1 1 d . . . H62A H 1.0724 0.4886 0.2046 0.110 Uiso 1 1 calc R . . H62B H 0.9900 0.5352 0.1748 0.110 Uiso 1 1 calc R . . H62C H 1.0662 0.5197 0.1172 0.110 Uiso 1 1 calc R . . C63 C 1.0357(3) 0.1211(2) 0.1686(2) 0.0872(11) Uani 1 1 d . . . H63A H 0.9679 0.0994 0.1905 0.105 Uiso 1 1 calc R . . C64 C 1.0350(3) 0.0291(2) 0.1186(3) 0.1279(18) Uani 1 1 d . . . H64A H 0.9673 -0.0040 0.0714 0.192 Uiso 1 1 calc R . . H64B H 1.0356 -0.0150 0.1553 0.192 Uiso 1 1 calc R . . H64C H 1.1017 0.0478 0.0974 0.192 Uiso 1 1 calc R . . C65 C 1.1373(4) 0.1734(3) 0.2431(2) 0.1141(15) Uani 1 1 d . . . H65A H 1.1351 0.2311 0.2738 0.171 Uiso 1 1 calc R . . H65B H 1.2055 0.1936 0.2237 0.171 Uiso 1 1 calc R . . H65C H 1.1375 0.1296 0.2801 0.171 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.02786(8) 0.03122(9) 0.01930(8) 0.00841(6) 0.00946(5) 0.01292(6) O 0.0357(6) 0.0469(7) 0.0250(6) 0.0052(5) 0.0116(5) 0.0095(6) N1 0.0332(7) 0.0394(8) 0.0213(6) 0.0099(6) 0.0114(5) 0.0176(6) N2 0.0333(7) 0.0355(7) 0.0205(6) 0.0081(5) 0.0104(5) 0.0148(6) N3 0.0330(7) 0.0346(7) 0.0213(6) 0.0076(5) 0.0109(5) 0.0165(6) N4 0.0324(7) 0.0361(7) 0.0218(6) 0.0087(5) 0.0092(5) 0.0163(6) N5 0.0354(8) 0.0367(8) 0.0373(8) 0.0100(6) 0.0081(6) 0.0129(6) N6 0.0331(7) 0.0318(7) 0.0280(7) 0.0089(6) 0.0128(6) 0.0133(6) C1 0.0354(8) 0.0396(9) 0.0251(8) 0.0113(7) 0.0093(6) 0.0176(7) C2 0.0389(9) 0.0460(10) 0.0269(8) 0.0150(7) 0.0094(7) 0.0214(8) C3 0.0408(9) 0.0487(11) 0.0227(8) 0.0128(7) 0.0097(7) 0.0199(8) C4 0.0319(8) 0.0395(9) 0.0207(7) 0.0095(6) 0.0090(6) 0.0135(7) C5 0.0317(8) 0.0398(9) 0.0208(7) 0.0079(6) 0.0096(6) 0.0124(7) C6 0.0327(8) 0.0385(9) 0.0228(8) 0.0065(6) 0.0111(6) 0.0145(7) C7 0.0424(9) 0.0456(10) 0.0255(8) 0.0073(7) 0.0145(7) 0.0215(8) C8 0.0431(9) 0.0407(10) 0.0284(8) 0.0062(7) 0.0125(7) 0.0216(8) C9 0.0332(8) 0.0345(9) 0.0262(8) 0.0076(6) 0.0109(6) 0.0148(7) C10 0.0337(8) 0.0356(9) 0.0273(8) 0.0095(7) 0.0112(6) 0.0163(7) C11 0.0316(8) 0.0355(9) 0.0253(8) 0.0103(6) 0.0107(6) 0.0145(7) C12 0.0426(9) 0.0403(9) 0.0270(8) 0.0141(7) 0.0129(7) 0.0219(8) C13 0.0409(9) 0.0436(10) 0.0231(8) 0.0127(7) 0.0116(7) 0.0204(8) C14 0.0322(8) 0.0376(9) 0.0207(7) 0.0087(6) 0.0098(6) 0.0151(7) C15 0.0315(8) 0.0376(9) 0.0208(7) 0.0081(6) 0.0107(6) 0.0142(7) C16 0.0328(8) 0.0368(9) 0.0226(7) 0.0067(6) 0.0102(6) 0.0159(7) C17 0.0470(10) 0.0436(10) 0.0260(8) 0.0065(7) 0.0131(7) 0.0245(8) C18 0.0544(11) 0.0463(11) 0.0297(9) 0.0093(8) 0.0136(8) 0.0313(9) C19 0.0370(9) 0.0384(9) 0.0282(8) 0.0095(7) 0.0105(7) 0.0186(7) C20 0.0393(9) 0.0416(10) 0.0277(8) 0.0114(7) 0.0110(7) 0.0217(8) C21 0.0370(9) 0.0411(9) 0.0215(7) 0.0097(7) 0.0118(6) 0.0184(7) C22 0.0413(10) 0.0631(13) 0.0275(9) 0.0068(9) 0.0137(8) 0.0040(9) C23 0.0530(12) 0.0620(13) 0.0230(9) 0.0018(8) 0.0098(8) 0.0080(10) C24 0.0507(10) 0.0529(11) 0.0249(8) 0.0153(8) 0.0166(7) 0.0308(9) C25 0.0426(11) 0.0802(16) 0.0340(10) 0.0171(10) 0.0198(8) 0.0164(11) C26 0.0378(10) 0.0728(15) 0.0276(9) 0.0078(9) 0.0109(8) 0.0074(10) C27 0.0748(15) 0.0738(15) 0.0289(10) 0.0188(10) 0.0256(10) 0.0429(13) C28 0.0442(9) 0.0401(9) 0.0259(8) 0.0100(7) 0.0130(7) 0.0219(8) C29 0.0495(11) 0.0518(12) 0.0469(11) 0.0209(9) 0.0229(9) 0.0277(10) C30 0.0584(13) 0.0625(14) 0.0552(13) 0.0210(11) 0.0236(10) 0.0401(11) C31 0.0671(13) 0.0479(12) 0.0395(10) 0.0121(9) 0.0137(9) 0.0356(11) C32 0.0664(13) 0.0395(11) 0.0504(12) 0.0173(9) 0.0259(10) 0.0246(10) C33 0.0483(11) 0.0420(10) 0.0439(10) 0.0125(8) 0.0197(9) 0.0230(9) C34 0.097(2) 0.0646(16) 0.0671(16) 0.0268(13) 0.0228(14) 0.0554(15) C35 0.0429(9) 0.0404(9) 0.0221(8) 0.0095(7) 0.0128(7) 0.0233(8) C36 0.0546(12) 0.0420(10) 0.0276(9) 0.0069(8) 0.0129(8) 0.0111(9) C37 0.0812(16) 0.0452(12) 0.0242(9) 0.0009(8) 0.0080(9) 0.0194(11) C38 0.0916(17) 0.0621(13) 0.0276(9) 0.0157(9) 0.0259(10) 0.0523(13) C39 0.0629(14) 0.120(2) 0.0397(12) 0.0292(13) 0.0318(11) 0.0490(16) C40 0.0430(11) 0.0973(18) 0.0300(10) 0.0166(11) 0.0144(8) 0.0277(12) C41 0.149(3) 0.104(2) 0.0363(12) 0.0222(13) 0.0455(15) 0.088(2) C42 0.0515(11) 0.0457(10) 0.0279(9) 0.0090(7) 0.0070(8) 0.0288(9) C43 0.0688(14) 0.0502(12) 0.0380(10) 0.0155(9) 0.0147(10) 0.0324(11) C44 0.0944(19) 0.0509(13) 0.0436(12) 0.0158(10) 0.0099(12) 0.0422(13) C45 0.0834(17) 0.0605(14) 0.0460(12) 0.0058(10) -0.0018(11) 0.0498(14) C46 0.0598(14) 0.0723(16) 0.0563(14) 0.0085(12) 0.0060(11) 0.0444(13) C47 0.0560(12) 0.0555(13) 0.0458(11) 0.0139(9) 0.0120(9) 0.0344(11) C48 0.118(3) 0.088(2) 0.089(2) 0.0164(17) 0.0055(19) 0.079(2) C49 0.0329(8) 0.0342(9) 0.0286(8) 0.0111(7) 0.0100(6) 0.0157(7) C50 0.0492(11) 0.0434(11) 0.0373(10) 0.0051(8) -0.0007(8) 0.0104(9) C51 0.0869(19) 0.0657(16) 0.0384(12) 0.0126(11) -0.0092(12) 0.0174(14) C52 0.0697(15) 0.0470(12) 0.0476(12) 0.0006(10) 0.0186(11) 0.0202(11) C53 0.0510(13) 0.0530(14) 0.0714(17) 0.0016(12) -0.0053(11) 0.0039(11) C54 0.0320(8) 0.0351(9) 0.0327(9) 0.0083(7) 0.0144(7) 0.0101(7) C55 0.0411(10) 0.0504(11) 0.0410(10) 0.0208(9) 0.0199(8) 0.0175(9) C56 0.0446(11) 0.0600(13) 0.0415(11) 0.0234(10) 0.0202(9) 0.0129(10) C57 0.0512(12) 0.0577(13) 0.0456(12) 0.0066(10) 0.0325(10) 0.0080(10) C58 0.0645(14) 0.0499(13) 0.0810(17) 0.0142(12) 0.0521(13) 0.0232(11) C59 0.0490(11) 0.0421(11) 0.0661(14) 0.0188(10) 0.0377(10) 0.0197(9) C60 0.0722(15) 0.0797(17) 0.0832(17) 0.0595(15) 0.0542(14) 0.0492(14) C61 0.0547(15) 0.089(2) 0.146(3) 0.080(2) 0.0298(17) 0.0311(15) C62 0.121(2) 0.0654(16) 0.0648(16) 0.0316(13) 0.0462(16) 0.0574(17) C63 0.098(2) 0.085(2) 0.161(3) 0.086(2) 0.106(2) 0.0719(19) C64 0.111(3) 0.0649(19) 0.276(6) 0.078(3) 0.134(3) 0.058(2) C65 0.166(4) 0.168(4) 0.115(3) 0.099(3) 0.085(3) 0.135(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr O 2.0677(12) . ? Zr N6 2.1096(13) . ? Zr N1 2.2163(13) . ? Zr N3 2.2216(13) . ? Zr N4 2.2254(13) . ? Zr N2 2.2314(14) . ? Zr C49 2.6008(17) . ? O C49 1.3530(19) . ? N1 C1 1.387(2) . ? N1 C4 1.388(2) . ? N2 C9 1.384(2) . ? N2 C6 1.3848(19) . ? N3 C11 1.384(2) . ? N3 C14 1.3902(19) . ? N4 C19 1.379(2) . ? N4 C16 1.3861(19) . ? N5 C49 1.269(2) . ? N5 C50 1.471(3) . ? N6 C49 1.401(2) . ? N6 C54 1.424(2) . ? C1 C20 1.399(2) . ? C1 C2 1.440(2) . ? C2 C3 1.348(3) . ? C3 C4 1.436(2) . ? C4 C5 1.398(2) . ? C5 C6 1.401(2) . ? C5 C21 1.501(2) . ? C6 C7 1.432(2) . ? C7 C8 1.353(2) . ? C8 C9 1.434(2) . ? C9 C10 1.405(2) . ? C10 C11 1.405(2) . ? C10 C28 1.497(2) . ? C11 C12 1.436(2) . ? C12 C13 1.352(2) . ? C13 C14 1.432(2) . ? C14 C15 1.396(2) . ? C15 C16 1.404(2) . ? C15 C35 1.503(2) . ? C16 C17 1.432(2) . ? C17 C18 1.359(2) . ? C18 C19 1.430(2) . ? C19 C20 1.413(2) . ? C20 C42 1.497(2) . ? C21 C22 1.375(3) . ? C21 C26 1.380(3) . ? C22 C23 1.389(3) . ? C23 C24 1.368(3) . ? C24 C25 1.377(3) . ? C24 C27 1.513(2) . ? C25 C26 1.387(3) . ? C28 C29 1.387(3) . ? C28 C33 1.397(3) . ? C29 C30 1.386(3) . ? C30 C31 1.391(3) . ? C31 C32 1.383(3) . ? C31 C34 1.511(3) . ? C32 C33 1.390(3) . ? C35 C40 1.377(3) . ? C35 C36 1.383(3) . ? C36 C37 1.393(3) . ? C37 C38 1.371(3) . ? C38 C39 1.373(4) . ? C38 C41 1.521(3) . ? C39 C40 1.385(3) . ? C42 C47 1.383(3) . ? C42 C43 1.395(3) . ? C43 C44 1.397(3) . ? C44 C45 1.367(4) . ? C45 C46 1.384(4) . ? C45 C48 1.524(3) . ? C46 C47 1.398(3) . ? C50 C53 1.532(3) . ? C50 C51 1.536(3) . ? C50 C52 1.541(3) . ? C54 C59 1.403(3) . ? C54 C55 1.404(3) . ? C55 C56 1.399(3) . ? C55 C60 1.529(3) . ? C56 C57 1.366(3) . ? C57 C58 1.377(3) . ? C58 C59 1.392(3) . ? C59 C63 1.522(3) . ? C60 C61 1.527(4) . ? C60 C62 1.531(4) . ? C63 C65 1.506(5) . ? C63 C64 1.541(4) . ? 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 O Zr N6 63.62(5) . . ? O Zr N1 128.36(5) . . ? N6 Zr N1 98.15(5) . . ? O Zr N3 90.39(5) . . ? N6 Zr N3 125.61(5) . . ? N1 Zr N3 132.82(5) . . ? O Zr N4 80.85(5) . . ? N6 Zr N4 132.57(5) . . ? N1 Zr N4 79.44(5) . . ? N3 Zr N4 82.23(5) . . ? O Zr N2 141.42(5) . . ? N6 Zr N2 92.80(5) . . ? N1 Zr N2 82.58(5) . . ? N3 Zr N2 78.93(5) . . ? N4 Zr N2 132.90(5) . . ? O Zr C49 31.11(5) . . ? N6 Zr C49 32.53(5) . . ? N1 Zr C49 116.28(5) . . ? N3 Zr C49 110.55(5) . . ? N4 Zr C49 106.66(5) . . ? N2 Zr C49 120.33(5) . . ? C49 O Zr 96.76(10) . . ? C1 N1 C4 106.28(13) . . ? C1 N1 Zr 128.87(11) . . ? C4 N1 Zr 123.28(11) . . ? C9 N2 C6 105.92(13) . . ? C9 N2 Zr 129.27(10) . . ? C6 N2 Zr 122.05(11) . . ? C11 N3 C14 106.30(13) . . ? C11 N3 Zr 128.57(10) . . ? C14 N3 Zr 121.27(11) . . ? C19 N4 C16 105.96(13) . . ? C19 N4 Zr 126.74(10) . . ? C16 N4 Zr 120.54(10) . . ? C49 N5 C50 120.92(16) . . ? C49 N6 C54 119.01(14) . . ? C49 N6 Zr 93.40(9) . . ? C54 N6 Zr 146.76(12) . . ? N1 C1 C20 125.46(14) . . ? N1 C1 C2 109.12(14) . . ? C20 C1 C2 125.41(16) . . ? C3 C2 C1 107.62(15) . . ? C2 C3 C4 107.70(15) . . ? N1 C4 C5 126.02(14) . . ? N1 C4 C3 109.25(15) . . ? C5 C4 C3 124.59(15) . . ? C4 C5 C6 125.73(14) . . ? C4 C5 C21 117.52(14) . . ? C6 C5 C21 116.73(15) . . ? N2 C6 C5 125.83(15) . . ? N2 C6 C7 109.46(14) . . ? C5 C6 C7 124.38(15) . . ? C8 C7 C6 107.72(15) . . ? C7 C8 C9 107.05(16) . . ? N2 C9 C10 124.82(15) . . ? N2 C9 C8 109.81(14) . . ? C10 C9 C8 125.36(16) . . ? C9 C10 C11 124.20(15) . . ? C9 C10 C28 118.12(15) . . ? C11 C10 C28 117.68(14) . . ? N3 C11 C10 125.36(14) . . ? N3 C11 C12 109.32(14) . . ? C10 C11 C12 125.32(15) . . ? C13 C12 C11 107.47(15) . . ? C12 C13 C14 107.78(14) . . ? N3 C14 C15 126.20(14) . . ? N3 C14 C13 109.11(14) . . ? C15 C14 C13 124.63(14) . . ? C14 C15 C16 126.05(14) . . ? C14 C15 C35 117.49(14) . . ? C16 C15 C35 116.32(14) . . ? N4 C16 C15 125.37(15) . . ? N4 C16 C17 109.65(14) . . ? C15 C16 C17 124.90(15) . . ? C18 C17 C16 107.19(15) . . ? C17 C18 C19 107.31(16) . . ? N4 C19 C20 124.59(15) . . ? N4 C19 C18 109.88(14) . . ? C20 C19 C18 125.52(16) . . ? C1 C20 C19 124.22(16) . . ? C1 C20 C42 118.28(15) . . ? C19 C20 C42 117.46(15) . . ? C22 C21 C26 118.12(16) . . ? C22 C21 C5 122.98(15) . . ? C26 C21 C5 118.88(16) . . ? C21 C22 C23 120.63(18) . . ? C24 C23 C22 121.56(18) . . ? C23 C24 C25 117.72(16) . . ? C23 C24 C27 121.35(19) . . ? C25 C24 C27 120.93(18) . . ? C24 C25 C26 121.25(18) . . ? C21 C26 C25 120.69(19) . . ? C29 C28 C33 117.26(17) . . ? C29 C28 C10 121.82(16) . . ? C33 C28 C10 120.89(16) . . ? C28 C29 C30 121.49(19) . . ? C29 C30 C31 121.16(19) . . ? C32 C31 C30 117.59(18) . . ? C32 C31 C34 121.4(2) . . ? C30 C31 C34 121.0(2) . . ? C31 C32 C33 121.38(19) . . ? C32 C33 C28 121.00(18) . . ? C40 C35 C36 117.99(17) . . ? C40 C35 C15 120.76(16) . . ? C36 C35 C15 121.22(15) . . ? C35 C36 C37 120.24(19) . . ? C38 C37 C36 121.6(2) . . ? C39 C38 C37 117.81(18) . . ? C39 C38 C41 121.2(2) . . ? C37 C38 C41 120.9(2) . . ? C38 C39 C40 121.2(2) . . ? C35 C40 C39 121.1(2) . . ? C47 C42 C43 118.43(18) . . ? C47 C42 C20 120.86(17) . . ? C43 C42 C20 120.71(18) . . ? C42 C43 C44 119.7(2) . . ? C45 C44 C43 121.9(2) . . ? C44 C45 C46 118.7(2) . . ? C44 C45 C48 120.9(3) . . ? C46 C45 C48 120.4(3) . . ? C45 C46 C47 120.3(2) . . ? C42 C47 C46 121.1(2) . . ? N5 C49 O 129.14(16) . . ? N5 C49 N6 124.69(15) . . ? O C49 N6 106.16(14) . . ? N5 C49 Zr 177.14(13) . . ? O C49 Zr 52.14(8) . . ? N6 C49 Zr 54.07(8) . . ? N5 C50 C53 105.63(19) . . ? N5 C50 C51 112.40(18) . . ? C53 C50 C51 109.3(2) . . ? N5 C50 C52 110.60(17) . . ? C53 C50 C52 109.42(19) . . ? C51 C50 C52 109.4(2) . . ? C59 C54 C55 120.17(16) . . ? C59 C54 N6 119.28(16) . . ? C55 C54 N6 120.55(16) . . ? C56 C55 C54 118.66(19) . . ? C56 C55 C60 119.57(18) . . ? C54 C55 C60 121.59(16) . . ? C57 C56 C55 121.3(2) . . ? C56 C57 C58 119.79(18) . . ? C57 C58 C59 121.3(2) . . ? C58 C59 C54 118.68(19) . . ? C58 C59 C63 120.61(19) . . ? C54 C59 C63 120.46(17) . . ? C61 C60 C55 111.6(2) . . ? C61 C60 C62 110.7(2) . . ? C55 C60 C62 110.8(2) . . ? C65 C63 C59 110.1(2) . . ? C65 C63 C64 111.4(3) . . ? C59 C63 C64 112.6(3) . . ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 28.86 _diffrn_measured_fraction_theta_full 0.846 _refine_diff_density_max 0.491 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.046 data_woo01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H77 N6 O Zr' _chemical_formula_weight 1229.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9237(8) _cell_length_b 16.3912(10) _cell_length_c 16.6590(10) _cell_angle_alpha 97.1370(10) _cell_angle_beta 105.1960(10) _cell_angle_gamma 100.5320(10) _cell_volume 3292.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1294 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Vruker CCD-1000' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15220 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 23.35 _reflns_number_total 9395 _reflns_number_gt 6933 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9395 _refine_ls_number_parameters 729 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.11872(3) -0.15361(2) 0.14463(2) 0.02244(15) Uani 1 1 d . . . O O 0.2275(2) -0.17096(16) 0.07614(16) 0.0272(7) Uani 1 1 d . . . N1 N 0.1686(3) -0.0729(2) 0.2716(2) 0.0268(8) Uani 1 1 d . . . N2 N -0.0271(3) -0.2054(2) 0.18682(19) 0.0237(8) Uani 1 1 d . . . N3 N -0.0153(3) -0.1672(2) 0.02688(19) 0.0226(8) Uani 1 1 d . . . N4 N 0.1687(3) -0.0265(2) 0.11174(19) 0.0234(8) Uani 1 1 d . . . N5 N 0.1780(3) -0.2670(2) 0.1484(2) 0.0282(8) Uani 1 1 d . . . N6 N 0.2807(3) -0.2977(2) 0.0521(2) 0.0281(8) Uani 1 1 d . . . C1 C 0.2533(4) -0.0009(3) 0.3010(3) 0.0286(10) Uani 1 1 d . . . C2 C 0.2841(4) 0.0170(3) 0.3911(3) 0.0348(11) Uani 1 1 d . . . H2 H 0.3416 0.0616 0.4269 0.042 Uiso 1 1 calc R . . C3 C 0.2167(4) -0.0407(3) 0.4162(3) 0.0358(11) Uani 1 1 d . . . H3 H 0.2181 -0.0439 0.4730 0.043 Uiso 1 1 calc R . . C4 C 0.1431(4) -0.0961(3) 0.3428(2) 0.0288(10) Uani 1 1 d . . . C5 C 0.0528(4) -0.1578(3) 0.3420(3) 0.0296(10) Uani 1 1 d . . . C6 C -0.0283(3) -0.2061(3) 0.2692(2) 0.0264(10) Uani 1 1 d . . . C7 C -0.1249(4) -0.2646(3) 0.2702(3) 0.0347(11) Uani 1 1 d . . . H7 H -0.1444 -0.2771 0.3192 0.042 Uiso 1 1 calc R . . C8 C -0.1831(4) -0.2987(3) 0.1893(3) 0.0320(10) Uani 1 1 d . . . H8 H -0.2511 -0.3392 0.1707 0.038 Uiso 1 1 calc R . . C9 C -0.1222(3) -0.2618(3) 0.1370(2) 0.0262(10) Uani 1 1 d . . . C10 C -0.1582(3) -0.2780(2) 0.0476(2) 0.0255(9) Uani 1 1 d . . . C11 C -0.1080(3) -0.2326(3) -0.0028(2) 0.0255(9) Uani 1 1 d . . . C12 C -0.1441(4) -0.2462(3) -0.0936(3) 0.0291(10) Uani 1 1 d . . . H12 H -0.2057 -0.2874 -0.1295 0.035 Uiso 1 1 calc R . . C13 C -0.0747(4) -0.1899(3) -0.1185(3) 0.0288(10) Uani 1 1 d . . . H13 H -0.0788 -0.1845 -0.1753 0.035 Uiso 1 1 calc R . . C14 C 0.0055(3) -0.1401(3) -0.0449(2) 0.0242(9) Uani 1 1 d . . . C15 C 0.0913(3) -0.0731(2) -0.0433(2) 0.0243(9) Uani 1 1 d . . . C16 C 0.1607(3) -0.0175(2) 0.0290(2) 0.0236(9) Uani 1 1 d . . . C17 C 0.2386(4) 0.0569(3) 0.0282(3) 0.0301(10) Uani 1 1 d . . . H17 H 0.2490 0.0777 -0.0206 0.036 Uiso 1 1 calc R . . C18 C 0.2942(4) 0.0917(3) 0.1089(3) 0.0291(10) Uani 1 1 d . . . H18 H 0.3506 0.1419 0.1277 0.035 Uiso 1 1 calc R . . C19 C 0.2531(3) 0.0393(2) 0.1617(2) 0.0240(9) Uani 1 1 d . . . C20 C 0.2949(3) 0.0506(3) 0.2499(3) 0.0271(10) Uani 1 1 d . . . C21 C 0.0339(4) -0.1721(3) 0.4253(3) 0.0343(11) Uani 1 1 d . . . C22 C -0.0289(5) -0.1279(4) 0.4601(3) 0.0590(16) Uani 1 1 d . . . H22 H -0.0561 -0.0850 0.4333 0.071 Uiso 1 1 calc R . . C23 C -0.0537(5) -0.1440(5) 0.5331(3) 0.0684(18) Uani 1 1 d . . . H23 H -0.0979 -0.1124 0.5552 0.082 Uiso 1 1 calc R . . C24 C -0.0157(5) -0.2047(4) 0.5740(3) 0.0590(16) Uani 1 1 d . . . C25 C 0.0489(6) -0.2484(4) 0.5412(3) 0.076(2) Uani 1 1 d . . . H25 H 0.0772 -0.2903 0.5690 0.091 Uiso 1 1 calc R . . C26 C 0.0741(5) -0.2321(4) 0.4668(3) 0.0590(16) Uani 1 1 d . . . H26 H 0.1194 -0.2629 0.4450 0.071 Uiso 1 1 calc R . . C27 C -0.0422(6) -0.2245(5) 0.6546(4) 0.095(3) Uani 1 1 d . . . H27A H -0.0701 -0.2854 0.6482 0.114 Uiso 1 1 calc R . . H27B H -0.0982 -0.1948 0.6647 0.114 Uiso 1 1 calc R . . H27C H 0.0246 -0.2059 0.7027 0.114 Uiso 1 1 calc R . . C28 C -0.2571(3) -0.3473(2) 0.0044(2) 0.0249(9) Uani 1 1 d . . . C29 C -0.3559(4) -0.3315(3) -0.0401(3) 0.0321(10) Uani 1 1 d . . . H29 H -0.3627 -0.2749 -0.0415 0.039 Uiso 1 1 calc R . . C30 C -0.4449(4) -0.3974(3) -0.0824(3) 0.0355(11) Uani 1 1 d . . . H30 H -0.5124 -0.3851 -0.1113 0.043 Uiso 1 1 calc R . . C31 C -0.4379(4) -0.4808(3) -0.0837(3) 0.0319(10) Uani 1 1 d . . . C32 C -0.3397(4) -0.4966(3) -0.0379(3) 0.0339(11) Uani 1 1 d . . . H32 H -0.3335 -0.5533 -0.0360 0.041 Uiso 1 1 calc R . . C33 C -0.2503(4) -0.4311(3) 0.0053(3) 0.0319(10) Uani 1 1 d . . . H33A H -0.1836 -0.4435 0.0358 0.038 Uiso 1 1 calc R . . C34 C -0.5328(4) -0.5528(3) -0.1308(3) 0.0438(12) Uani 1 1 d . . . H34A H -0.5908 -0.5313 -0.1668 0.053 Uiso 1 1 calc R . . H34B H -0.5617 -0.5814 -0.0903 0.053 Uiso 1 1 calc R . . H34C H -0.5079 -0.5929 -0.1660 0.053 Uiso 1 1 calc R . . C35 C 0.1168(3) -0.0619(2) -0.1243(2) 0.0250(9) Uani 1 1 d . . . C36 C 0.0636(4) -0.0180(3) -0.1809(3) 0.0462(14) Uani 1 1 d . . . H36 H 0.0036 0.0036 -0.1713 0.055 Uiso 1 1 calc R . . C37 C 0.0967(5) -0.0049(3) -0.2520(3) 0.0507(15) Uani 1 1 d . . . H37 H 0.0591 0.0260 -0.2900 0.061 Uiso 1 1 calc R . . C38 C 0.1818(4) -0.0352(3) -0.2685(3) 0.0327(11) Uani 1 1 d . . . C39 C 0.2323(4) -0.0818(3) -0.2130(3) 0.0369(11) Uani 1 1 d . . . H39 H 0.2897 -0.1058 -0.2243 0.044 Uiso 1 1 calc R . . C40 C 0.2015(4) -0.0943(3) -0.1418(3) 0.0364(11) Uani 1 1 d . . . H40 H 0.2390 -0.1256 -0.1041 0.044 Uiso 1 1 calc R . . C41 C 0.2194(4) -0.0203(3) -0.3455(3) 0.0461(13) Uani 1 1 d . . . H41A H 0.2006 -0.0736 -0.3856 0.055 Uiso 1 1 calc R . . H41B H 0.2993 0.0018 -0.3280 0.055 Uiso 1 1 calc R . . H41C H 0.1827 0.0207 -0.3727 0.055 Uiso 1 1 calc R . . C42 C 0.3898(4) 0.1237(3) 0.2920(3) 0.0319(10) Uani 1 1 d . . . C43 C 0.3784(4) 0.2061(3) 0.2917(3) 0.0408(12) Uani 1 1 d . . . H43 H 0.3081 0.2166 0.2669 0.049 Uiso 1 1 calc R . . C44 C 0.4679(5) 0.2734(3) 0.3268(3) 0.0555(15) Uani 1 1 d . . . H44 H 0.4577 0.3293 0.3261 0.067 Uiso 1 1 calc R . . C45 C 0.5714(5) 0.2611(4) 0.3629(3) 0.0583(15) Uani 1 1 d . . . C46 C 0.5829(5) 0.1794(4) 0.3628(4) 0.0584(15) Uani 1 1 d . . . H46 H 0.6536 0.1693 0.3868 0.070 Uiso 1 1 calc R . . C47 C 0.4943(4) 0.1115(3) 0.3286(3) 0.0430(12) Uani 1 1 d . . . H47 H 0.5049 0.0558 0.3302 0.052 Uiso 1 1 calc R . . C48 C 0.6691(6) 0.3364(4) 0.4009(5) 0.094(2) Uani 1 1 d . . . H48A H 0.6505 0.3866 0.3795 0.113 Uiso 1 1 calc R . . H48B H 0.7332 0.3243 0.3848 0.113 Uiso 1 1 calc R . . H48C H 0.6861 0.3466 0.4626 0.113 Uiso 1 1 calc R . . C49 C 0.2339(3) -0.2496(3) 0.0898(3) 0.0258(10) Uani 1 1 d . . . C50 C 0.1740(4) -0.3481(3) 0.1798(3) 0.0389(12) Uani 1 1 d . . . C51 C 0.1174(5) -0.3453(3) 0.2490(4) 0.0577(16) Uani 1 1 d . . . H51A H 0.1551 -0.2953 0.2927 0.069 Uiso 1 1 calc R . . H51B H 0.1200 -0.3962 0.2741 0.069 Uiso 1 1 calc R . . H51C H 0.0406 -0.3428 0.2247 0.069 Uiso 1 1 calc R . . C52 C 0.2909(5) -0.3593(4) 0.2180(4) 0.0595(16) Uani 1 1 d . . . H52A H 0.3269 -0.3656 0.1734 0.071 Uiso 1 1 calc R . . H52B H 0.2876 -0.4097 0.2441 0.071 Uiso 1 1 calc R . . H52C H 0.3330 -0.3096 0.2610 0.071 Uiso 1 1 calc R . . C53 C 0.1087(5) -0.4215(3) 0.1082(4) 0.0556(15) Uani 1 1 d . . . H53A H 0.0345 -0.4129 0.0845 0.067 Uiso 1 1 calc R . . H53B H 0.1039 -0.4743 0.1302 0.067 Uiso 1 1 calc R . . H53C H 0.1458 -0.4243 0.0640 0.067 Uiso 1 1 calc R . . C54 C 0.3281(4) -0.2665(3) -0.0096(3) 0.0287(10) Uani 1 1 d . . . C55 C 0.4219(4) -0.2002(3) 0.0120(3) 0.0322(11) Uani 1 1 d . . . C56 C 0.4638(4) -0.1749(3) -0.0519(3) 0.0365(11) Uani 1 1 d . . . H56 H 0.5260 -0.1291 -0.0379 0.044 Uiso 1 1 calc R . . C57 C 0.4176(4) -0.2145(3) -0.1349(3) 0.0383(12) Uani 1 1 d . . . H57 H 0.4478 -0.1962 -0.1775 0.046 Uiso 1 1 calc R . . C58 C 0.3272(4) -0.2807(3) -0.1557(3) 0.0378(11) Uani 1 1 d . . . H58 H 0.2954 -0.3079 -0.2131 0.045 Uiso 1 1 calc R . . C59 C 0.2812(4) -0.3087(3) -0.0941(3) 0.0306(10) Uani 1 1 d . . . C60 C 0.4804(4) -0.1566(3) 0.1032(3) 0.0365(11) Uani 1 1 d . . . H60 H 0.4379 -0.1816 0.1399 0.044 Uiso 1 1 calc R . . C61 C 0.5968(4) -0.1721(3) 0.1317(3) 0.0464(13) Uani 1 1 d . . . H61A H 0.5928 -0.2329 0.1256 0.056 Uiso 1 1 calc R . . H61B H 0.6319 -0.1453 0.1910 0.056 Uiso 1 1 calc R . . H61C H 0.6401 -0.1479 0.0966 0.056 Uiso 1 1 calc R . . C62 C 0.4831(5) -0.0618(3) 0.1142(4) 0.0538(14) Uani 1 1 d . . . H62A H 0.5279 -0.0352 0.0813 0.065 Uiso 1 1 calc R . . H62B H 0.5151 -0.0361 0.1742 0.065 Uiso 1 1 calc R . . H62C H 0.4080 -0.0535 0.0944 0.065 Uiso 1 1 calc R . . C63 C 0.1785(4) -0.3792(3) -0.1168(3) 0.0358(11) Uani 1 1 d . . . H63 H 0.1837 -0.4090 -0.0675 0.043 Uiso 1 1 calc R . . C64 C 0.0767(4) -0.3420(3) -0.1279(4) 0.0534(14) Uani 1 1 d . . . H64A H 0.0862 -0.3003 -0.0774 0.064 Uiso 1 1 calc R . . H64B H 0.0118 -0.3871 -0.1358 0.064 Uiso 1 1 calc R . . H64C H 0.0669 -0.3145 -0.1775 0.064 Uiso 1 1 calc R . . C65 C 0.1664(5) -0.4451(3) -0.1939(3) 0.0606(15) Uani 1 1 d . . . H65A H 0.1591 -0.4183 -0.2440 0.073 Uiso 1 1 calc R . . H65B H 0.1007 -0.4898 -0.2028 0.073 Uiso 1 1 calc R . . H65C H 0.2315 -0.4693 -0.1845 0.073 Uiso 1 1 calc R . . C100 C -0.2680(8) -0.4124(8) -0.3834(9) 0.398(15) Uiso 1 1 d D . . H10A H -0.2157 -0.3852 -0.4079 0.478 Uiso 1 1 calc R . . C101 C -0.3643(9) -0.4645(7) -0.4392(14) 0.407(16) Uiso 1 1 d D . . H10B H -0.3712 -0.4694 -0.4979 0.488 Uiso 1 1 calc R . . C102 C -0.4513(15) -0.5101(9) -0.4166(8) 0.252(8) Uiso 1 1 d D . . H10C H -0.5175 -0.5459 -0.4532 0.302 Uiso 1 1 calc R . . C103 C -0.4199(9) -0.4916(6) -0.3283(7) 0.164(4) Uiso 1 1 d D . . H10D H -0.4724 -0.5189 -0.3039 0.197 Uiso 1 1 calc R . . C104 C -0.3256(8) -0.4404(6) -0.2692(7) 0.141(4) Uiso 1 1 d D . . H10E H -0.3190 -0.4357 -0.2106 0.170 Uiso 1 1 calc R . . C105 C -0.2408(11) -0.3962(7) -0.2952(9) 0.194(5) Uiso 1 1 d D . . H10F H -0.1747 -0.3604 -0.2584 0.232 Uiso 1 1 calc R . . C200 C 0.5445(7) 0.1508(5) -0.3742(5) 0.137(3) Uiso 1 1 d D . . H20A H 0.6004 0.1208 -0.3571 0.165 Uiso 1 1 calc R . . C201 C 0.5431(8) 0.1936(4) -0.4382(5) 0.148(4) Uiso 1 1 d D . . H20B H 0.5984 0.1935 -0.4662 0.177 Uiso 1 1 calc R . . C202 C 0.4645(7) 0.2364(5) -0.4632(6) 0.127(3) Uiso 1 1 d D . . H20C H 0.4651 0.2662 -0.5086 0.152 Uiso 1 1 calc R . . C203 C 0.3850(8) 0.2378(6) -0.4250(5) 0.149(4) Uiso 1 1 d D . . H20D H 0.3291 0.2678 -0.4420 0.178 Uiso 1 1 calc R . . C204 C 0.3891(8) 0.1944(5) -0.3612(5) 0.146(4) Uiso 1 1 d D . . H20E H 0.3338 0.1945 -0.3332 0.176 Uiso 1 1 calc R . . C205 C 0.4663(6) 0.1508(5) -0.3344(6) 0.131(3) Uiso 1 1 d D . . H20F H 0.4656 0.1211 -0.2890 0.157 Uiso 1 1 calc R . . C300 C 0.1029(19) -0.5219(12) 0.5263(14) 0.273(9) Uiso 1 1 d D . . H30B H 0.1716 -0.5371 0.5449 0.327 Uiso 1 1 calc R . . C301 C 0.0701(14) -0.4930(9) 0.4538(10) 0.200(6) Uiso 1 1 d D . . H30C H 0.1175 -0.4867 0.4189 0.240 Uiso 1 1 calc R . . C302 C -0.0284(12) -0.4728(8) 0.4300(8) 0.165(4) Uiso 1 1 d D . . H30D H -0.0470 -0.4532 0.3779 0.198 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.0257(3) 0.0230(2) 0.0212(2) 0.00462(16) 0.01036(18) 0.00621(17) O 0.0349(18) 0.0240(16) 0.0308(15) 0.0085(13) 0.0176(14) 0.0124(13) N1 0.030(2) 0.028(2) 0.0270(19) 0.0076(16) 0.0122(17) 0.0078(17) N2 0.029(2) 0.0244(19) 0.0200(17) 0.0066(15) 0.0107(16) 0.0062(16) N3 0.025(2) 0.0222(18) 0.0222(17) 0.0048(15) 0.0102(16) 0.0041(15) N4 0.025(2) 0.0258(19) 0.0218(18) 0.0018(15) 0.0113(16) 0.0077(16) N5 0.034(2) 0.027(2) 0.0287(19) 0.0102(16) 0.0147(17) 0.0078(17) N6 0.029(2) 0.0253(19) 0.034(2) 0.0055(16) 0.0142(18) 0.0084(16) C1 0.029(3) 0.029(2) 0.027(2) 0.0017(19) 0.009(2) 0.006(2) C2 0.035(3) 0.041(3) 0.022(2) -0.001(2) 0.006(2) 0.000(2) C3 0.038(3) 0.044(3) 0.019(2) 0.003(2) 0.005(2) -0.001(2) C4 0.036(3) 0.034(3) 0.019(2) 0.0063(19) 0.012(2) 0.008(2) C5 0.037(3) 0.031(2) 0.025(2) 0.009(2) 0.014(2) 0.009(2) C6 0.031(3) 0.028(2) 0.024(2) 0.0055(19) 0.013(2) 0.006(2) C7 0.040(3) 0.043(3) 0.026(2) 0.013(2) 0.018(2) 0.007(2) C8 0.029(3) 0.034(3) 0.032(2) 0.007(2) 0.011(2) 0.002(2) C9 0.027(2) 0.028(2) 0.025(2) 0.0065(19) 0.008(2) 0.006(2) C10 0.025(2) 0.026(2) 0.027(2) 0.0027(18) 0.010(2) 0.0082(19) C11 0.025(2) 0.030(2) 0.023(2) 0.0049(19) 0.0075(19) 0.010(2) C12 0.027(2) 0.034(3) 0.024(2) 0.0029(19) 0.007(2) 0.005(2) C13 0.032(3) 0.037(3) 0.020(2) 0.0058(19) 0.011(2) 0.011(2) C14 0.025(2) 0.028(2) 0.024(2) 0.0084(19) 0.012(2) 0.0093(19) C15 0.026(2) 0.027(2) 0.025(2) 0.0085(19) 0.011(2) 0.0117(19) C16 0.030(2) 0.022(2) 0.027(2) 0.0073(18) 0.016(2) 0.0112(19) C17 0.041(3) 0.025(2) 0.031(2) 0.008(2) 0.019(2) 0.009(2) C18 0.033(3) 0.024(2) 0.034(2) 0.005(2) 0.018(2) 0.004(2) C19 0.022(2) 0.025(2) 0.027(2) 0.0015(19) 0.0118(19) 0.0069(19) C20 0.027(2) 0.025(2) 0.031(2) 0.0011(19) 0.013(2) 0.0074(19) C21 0.039(3) 0.043(3) 0.020(2) 0.005(2) 0.013(2) 0.000(2) C22 0.063(4) 0.096(5) 0.036(3) 0.024(3) 0.025(3) 0.040(4) C23 0.061(4) 0.123(6) 0.035(3) 0.016(3) 0.031(3) 0.030(4) C24 0.066(4) 0.072(4) 0.025(3) -0.001(3) 0.019(3) -0.022(3) C25 0.133(6) 0.060(4) 0.037(3) 0.027(3) 0.026(4) 0.012(4) C26 0.095(5) 0.061(4) 0.039(3) 0.022(3) 0.033(3) 0.032(3) C27 0.114(6) 0.113(6) 0.038(3) 0.007(4) 0.036(4) -0.040(5) C28 0.025(2) 0.026(2) 0.025(2) 0.0023(18) 0.0094(19) 0.0044(19) C29 0.031(3) 0.029(2) 0.037(2) 0.006(2) 0.008(2) 0.011(2) C30 0.023(3) 0.040(3) 0.040(3) 0.004(2) 0.003(2) 0.009(2) C31 0.030(3) 0.033(3) 0.031(2) 0.002(2) 0.012(2) 0.002(2) C32 0.036(3) 0.029(3) 0.038(3) 0.004(2) 0.014(2) 0.009(2) C33 0.027(3) 0.030(3) 0.038(2) 0.005(2) 0.006(2) 0.010(2) C34 0.034(3) 0.046(3) 0.041(3) -0.004(2) 0.005(2) -0.002(2) C35 0.027(2) 0.025(2) 0.023(2) 0.0029(18) 0.0100(19) 0.0040(19) C36 0.059(4) 0.060(3) 0.045(3) 0.029(3) 0.031(3) 0.040(3) C37 0.069(4) 0.068(4) 0.041(3) 0.032(3) 0.032(3) 0.042(3) C38 0.037(3) 0.040(3) 0.027(2) 0.008(2) 0.017(2) 0.009(2) C39 0.038(3) 0.049(3) 0.033(3) 0.009(2) 0.019(2) 0.018(2) C40 0.042(3) 0.046(3) 0.032(2) 0.016(2) 0.017(2) 0.022(2) C41 0.050(3) 0.065(4) 0.034(3) 0.018(3) 0.024(3) 0.018(3) C42 0.035(3) 0.034(3) 0.025(2) -0.0002(19) 0.014(2) 0.001(2) C43 0.045(3) 0.034(3) 0.039(3) 0.000(2) 0.012(2) 0.002(2) C44 0.070(4) 0.034(3) 0.054(3) -0.006(3) 0.022(3) -0.005(3) C45 0.047(4) 0.059(4) 0.053(3) -0.014(3) 0.015(3) -0.012(3) C46 0.035(3) 0.063(4) 0.065(4) -0.013(3) 0.013(3) -0.001(3) C47 0.035(3) 0.043(3) 0.046(3) -0.003(2) 0.010(2) 0.006(2) C48 0.069(5) 0.076(5) 0.103(6) -0.023(4) 0.014(4) -0.028(4) C49 0.026(2) 0.023(2) 0.029(2) 0.0059(19) 0.007(2) 0.0071(19) C50 0.048(3) 0.034(3) 0.052(3) 0.024(2) 0.029(3) 0.018(2) C51 0.084(4) 0.050(3) 0.074(4) 0.042(3) 0.055(4) 0.036(3) C52 0.068(4) 0.074(4) 0.063(4) 0.044(3) 0.035(3) 0.037(3) C53 0.063(4) 0.033(3) 0.086(4) 0.017(3) 0.044(3) 0.008(3) C54 0.028(3) 0.028(2) 0.037(3) 0.009(2) 0.014(2) 0.014(2) C55 0.034(3) 0.029(2) 0.044(3) 0.009(2) 0.021(2) 0.015(2) C56 0.034(3) 0.038(3) 0.048(3) 0.016(2) 0.023(2) 0.016(2) C57 0.038(3) 0.050(3) 0.040(3) 0.018(2) 0.024(2) 0.019(3) C58 0.039(3) 0.048(3) 0.035(3) 0.009(2) 0.017(2) 0.022(3) C59 0.032(3) 0.034(3) 0.033(2) 0.008(2) 0.013(2) 0.018(2) C60 0.034(3) 0.036(3) 0.040(3) 0.003(2) 0.016(2) 0.005(2) C61 0.040(3) 0.054(3) 0.048(3) 0.008(3) 0.014(3) 0.016(3) C62 0.051(3) 0.045(3) 0.065(4) 0.000(3) 0.018(3) 0.012(3) C63 0.040(3) 0.033(3) 0.034(2) 0.004(2) 0.008(2) 0.012(2) C64 0.032(3) 0.054(3) 0.074(4) 0.016(3) 0.013(3) 0.010(3) C65 0.066(4) 0.052(3) 0.052(3) -0.011(3) 0.014(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr O 2.066(3) . ? Zr N5 2.137(3) . ? Zr N3 2.206(3) . ? Zr N1 2.217(3) . ? Zr N2 2.241(3) . ? Zr N4 2.244(3) . ? Zr C49 2.596(4) . ? O C49 1.349(5) . ? N1 C4 1.390(5) . ? N1 C1 1.391(5) . ? N2 C6 1.377(5) . ? N2 C9 1.384(5) . ? N3 C11 1.385(5) . ? N3 C14 1.399(5) . ? N4 C16 1.384(5) . ? N4 C19 1.384(5) . ? N5 C49 1.387(5) . ? N5 C50 1.485(5) . ? N6 C49 1.277(5) . ? N6 C54 1.428(5) . ? C1 C20 1.406(6) . ? C1 C2 1.425(6) . ? C2 C3 1.349(6) . ? C3 C4 1.422(6) . ? C4 C5 1.394(6) . ? C5 C6 1.410(6) . ? C5 C21 1.510(5) . ? C6 C7 1.434(6) . ? C7 C8 1.350(6) . ? C8 C9 1.436(6) . ? C9 C10 1.413(6) . ? C10 C11 1.394(6) . ? C10 C28 1.493(6) . ? C11 C12 1.436(5) . ? C12 C13 1.347(6) . ? C13 C14 1.422(6) . ? C14 C15 1.402(6) . ? C15 C16 1.395(6) . ? C15 C35 1.495(5) . ? C16 C17 1.437(6) . ? C17 C18 1.343(6) . ? C18 C19 1.434(5) . ? C19 C20 1.403(6) . ? C20 C42 1.494(6) . ? C21 C26 1.371(7) . ? C21 C22 1.371(7) . ? C22 C23 1.379(7) . ? C23 C24 1.366(8) . ? C24 C25 1.368(9) . ? C24 C27 1.528(7) . ? C25 C26 1.405(7) . ? C28 C29 1.385(6) . ? C28 C33 1.394(6) . ? C29 C30 1.386(6) . ? C30 C31 1.384(6) . ? C31 C32 1.387(6) . ? C31 C34 1.500(6) . ? C32 C33 1.387(6) . ? C35 C36 1.376(6) . ? C35 C40 1.381(6) . ? C36 C37 1.388(6) . ? C37 C38 1.364(6) . ? C38 C39 1.380(6) . ? C38 C41 1.517(6) . ? C39 C40 1.374(6) . ? C42 C43 1.386(6) . ? C42 C47 1.391(6) . ? C43 C44 1.384(7) . ? C44 C45 1.378(8) . ? C45 C46 1.375(8) . ? C45 C48 1.528(8) . ? C46 C47 1.381(7) . ? C50 C51 1.519(6) . ? C50 C53 1.525(7) . ? C50 C52 1.532(7) . ? C54 C55 1.404(6) . ? C54 C59 1.409(6) . ? C55 C56 1.389(6) . ? C55 C60 1.524(6) . ? C56 C57 1.375(7) . ? C57 C58 1.376(7) . ? C58 C59 1.398(6) . ? C59 C63 1.519(6) . ? C60 C61 1.533(6) . ? C60 C62 1.535(6) . ? C63 C64 1.527(6) . ? C63 C65 1.527(6) . ? C100 C101 1.397(5) . ? C100 C105 1.397(5) . ? C101 C102 1.397(5) . ? C102 C103 1.397(5) . ? C103 C104 1.396(5) . ? C104 C105 1.396(5) . ? C200 C201 1.345(4) . ? C200 C205 1.346(4) . ? C201 C202 1.345(4) . ? C202 C203 1.345(4) . ? C203 C204 1.346(4) . ? C204 C205 1.345(4) . ? C300 C301 1.346(11) . ? C300 C302 1.35(2) 2_546 ? C301 C302 1.345(11) . ? C302 C300 1.35(2) 2_546 ? 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 O Zr N5 63.13(11) . . ? O Zr N3 90.79(11) . . ? N5 Zr N3 110.13(12) . . ? O Zr N1 123.28(12) . . ? N5 Zr N1 111.73(12) . . ? N3 Zr N1 134.72(11) . . ? O Zr N2 149.98(11) . . ? N5 Zr N2 93.40(12) . . ? N3 Zr N2 79.62(11) . . ? N1 Zr N2 81.47(12) . . ? O Zr N4 76.15(10) . . ? N5 Zr N4 137.36(12) . . ? N3 Zr N4 81.23(12) . . ? N1 Zr N4 79.70(11) . . ? N2 Zr N4 129.24(11) . . ? O Zr C49 31.08(11) . . ? N5 Zr C49 32.26(12) . . ? N3 Zr C49 99.36(12) . . ? N1 Zr C49 125.42(12) . . ? N2 Zr C49 122.30(12) . . ? N4 Zr C49 106.95(12) . . ? C49 O Zr 96.7(2) . . ? C4 N1 C1 105.9(3) . . ? C4 N1 Zr 125.8(3) . . ? C1 N1 Zr 126.2(3) . . ? C6 N2 C9 105.8(3) . . ? C6 N2 Zr 126.2(3) . . ? C9 N2 Zr 125.9(2) . . ? C11 N3 C14 105.9(3) . . ? C11 N3 Zr 125.6(2) . . ? C14 N3 Zr 121.3(3) . . ? C16 N4 C19 105.8(3) . . ? C16 N4 Zr 121.1(3) . . ? C19 N4 Zr 126.0(2) . . ? C49 N5 C50 120.4(3) . . ? C49 N5 Zr 92.4(2) . . ? C50 N5 Zr 147.0(3) . . ? C49 N6 C54 117.7(3) . . ? N1 C1 C20 125.4(4) . . ? N1 C1 C2 109.2(4) . . ? C20 C1 C2 125.1(4) . . ? C3 C2 C1 107.5(4) . . ? C2 C3 C4 108.1(4) . . ? N1 C4 C5 125.3(4) . . ? N1 C4 C3 109.1(4) . . ? C5 C4 C3 125.2(4) . . ? C4 C5 C6 125.8(4) . . ? C4 C5 C21 118.5(4) . . ? C6 C5 C21 115.5(4) . . ? N2 C6 C5 125.9(4) . . ? N2 C6 C7 109.6(4) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 108.0(4) . . ? C7 C8 C9 106.6(4) . . ? N2 C9 C10 125.5(4) . . ? N2 C9 C8 110.1(3) . . ? C10 C9 C8 124.4(4) . . ? C11 C10 C9 124.2(4) . . ? C11 C10 C28 117.9(3) . . ? C9 C10 C28 117.9(4) . . ? N3 C11 C10 125.3(3) . . ? N3 C11 C12 109.2(3) . . ? C10 C11 C12 125.5(4) . . ? C13 C12 C11 107.6(4) . . ? C12 C13 C14 108.0(4) . . ? N3 C14 C15 124.7(4) . . ? N3 C14 C13 109.2(3) . . ? C15 C14 C13 126.1(4) . . ? C16 C15 C14 125.6(4) . . ? C16 C15 C35 115.8(4) . . ? C14 C15 C35 118.4(4) . . ? N4 C16 C15 126.0(4) . . ? N4 C16 C17 109.5(4) . . ? C15 C16 C17 124.5(4) . . ? C18 C17 C16 107.5(4) . . ? C17 C18 C19 107.6(4) . . ? N4 C19 C20 125.0(4) . . ? N4 C19 C18 109.5(3) . . ? C20 C19 C18 125.4(4) . . ? C19 C20 C1 124.8(4) . . ? C19 C20 C42 116.9(4) . . ? C1 C20 C42 118.3(4) . . ? C26 C21 C22 117.7(4) . . ? C26 C21 C5 121.7(4) . . ? C22 C21 C5 120.6(4) . . ? C21 C22 C23 121.6(5) . . ? C24 C23 C22 121.2(5) . . ? C23 C24 C25 118.0(5) . . ? C23 C24 C27 122.4(6) . . ? C25 C24 C27 119.5(6) . . ? C24 C25 C26 120.8(6) . . ? C21 C26 C25 120.7(5) . . ? C29 C28 C33 118.1(4) . . ? C29 C28 C10 122.0(4) . . ? C33 C28 C10 119.9(4) . . ? C28 C29 C30 120.6(4) . . ? C31 C30 C29 121.7(4) . . ? C30 C31 C32 117.7(4) . . ? C30 C31 C34 122.2(4) . . ? C32 C31 C34 120.0(4) . . ? C31 C32 C33 121.1(4) . . ? C32 C33 C28 120.8(4) . . ? C36 C35 C40 117.9(4) . . ? C36 C35 C15 123.6(4) . . ? C40 C35 C15 118.4(4) . . ? C35 C36 C37 120.6(4) . . ? C38 C37 C36 121.7(4) . . ? C37 C38 C39 117.4(4) . . ? C37 C38 C41 122.0(4) . . ? C39 C38 C41 120.6(4) . . ? C40 C39 C38 121.6(4) . . ? C39 C40 C35 120.8(4) . . ? C43 C42 C47 117.5(4) . . ? C43 C42 C20 121.3(4) . . ? C47 C42 C20 121.2(4) . . ? C44 C43 C42 121.0(5) . . ? C45 C44 C43 121.4(5) . . ? C46 C45 C44 117.6(5) . . ? C46 C45 C48 121.9(6) . . ? C44 C45 C48 120.5(6) . . ? C45 C46 C47 121.8(5) . . ? C46 C47 C42 120.8(5) . . ? N6 C49 O 124.6(4) . . ? N6 C49 N5 128.3(4) . . ? O C49 N5 107.1(3) . . ? N6 C49 Zr 171.6(3) . . ? O C49 Zr 52.23(17) . . ? N5 C49 Zr 55.35(18) . . ? N5 C50 C51 108.2(3) . . ? N5 C50 C53 110.2(4) . . ? C51 C50 C53 109.1(4) . . ? N5 C50 C52 110.2(4) . . ? C51 C50 C52 108.2(4) . . ? C53 C50 C52 110.8(4) . . ? C55 C54 C59 120.1(4) . . ? C55 C54 N6 122.5(4) . . ? C59 C54 N6 117.2(4) . . ? C56 C55 C54 118.8(4) . . ? C56 C55 C60 119.0(4) . . ? C54 C55 C60 122.2(4) . . ? C57 C56 C55 121.7(5) . . ? C56 C57 C58 119.5(4) . . ? C57 C58 C59 121.3(4) . . ? C58 C59 C54 118.6(4) . . ? C58 C59 C63 121.8(4) . . ? C54 C59 C63 119.5(4) . . ? C55 C60 C61 110.8(4) . . ? C55 C60 C62 111.0(4) . . ? C61 C60 C62 111.0(4) . . ? C59 C63 C64 109.9(4) . . ? C59 C63 C65 114.2(4) . . ? C64 C63 C65 111.0(4) . . ? C101 C100 C105 126.6(17) . . ? C102 C101 C100 126(2) . . ? C101 C102 C103 105.0(18) . . ? C104 C103 C102 131.9(14) . . ? C105 C104 C103 120.9(12) . . ? C104 C105 C100 109.7(13) . . ? C201 C200 C205 119.7(10) . . ? C202 C201 C200 120.9(10) . . ? C203 C202 C201 121.0(10) . . ? C202 C203 C204 116.4(11) . . ? C205 C204 C203 124.3(11) . . ? C204 C205 C200 117.7(10) . . ? C301 C300 C302 113.3(18) . 2_546 ? C302 C301 C300 121.2(18) . . ? C301 C302 C300 125.6(14) . 2_546 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.032 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.081 data_woo02 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H75 Hf N7' _chemical_formula_weight 1333.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hf' 'Hf' -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8756(8) _cell_length_b 16.7514(9) _cell_length_c 26.1874(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.7960(10) _cell_angle_gamma 90.00 _cell_volume 6522.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark red _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 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker CCD-1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40118 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.34 _reflns_number_total 15118 _reflns_number_gt 12709 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15118 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf 0.299339(7) 0.510053(6) 0.344802(4) 0.02214(4) Uani 1 1 d . . . N1 N 0.21411(14) 0.41057(12) 0.37489(8) 0.0244(4) Uani 1 1 d . . . N2 N 0.17738(14) 0.57789(11) 0.35927(8) 0.0260(4) Uani 1 1 d . . . N3 N 0.35951(15) 0.61412(12) 0.38713(8) 0.0266(4) Uani 1 1 d . . . N4 N 0.40004(15) 0.44717(12) 0.39364(8) 0.0273(4) Uani 1 1 d . . . N5 N 0.27209(15) 0.46095(12) 0.27000(8) 0.0261(4) Uani 1 1 d . . . N6 N 0.37376(15) 0.55585(12) 0.28525(8) 0.0270(4) Uani 1 1 d . . . N7 N 0.37841(19) 0.50044(13) 0.20303(9) 0.0350(5) Uani 1 1 d . . . C1 C 0.24180(18) 0.33517(14) 0.39032(9) 0.0272(5) Uani 1 1 d . . . C2 C 0.1654(2) 0.28301(15) 0.39177(10) 0.0332(6) Uani 1 1 d . . . H2A H 0.1662 0.2285 0.4017 0.040 Uiso 1 1 calc R . . C3 C 0.0922(2) 0.32526(15) 0.37650(11) 0.0329(6) Uani 1 1 d . . . H3A H 0.0322 0.3060 0.3733 0.039 Uiso 1 1 calc R . . C4 C 0.12234(18) 0.40531(15) 0.36594(10) 0.0276(5) Uani 1 1 d . . . C5 C 0.06524(18) 0.46825(16) 0.35134(10) 0.0291(5) Uani 1 1 d . . . C6 C 0.09023(18) 0.54909(15) 0.35008(10) 0.0283(5) Uani 1 1 d . . . C7 C 0.03050(19) 0.61470(16) 0.34190(12) 0.0353(6) Uani 1 1 d . . . H7A H -0.0322 0.6112 0.3342 0.042 Uiso 1 1 calc R . . C8 C 0.07869(19) 0.68260(16) 0.34705(11) 0.0355(6) Uani 1 1 d . . . H8A H 0.0561 0.7354 0.3435 0.043 Uiso 1 1 calc R . . C9 C 0.16975(18) 0.66076(14) 0.35874(10) 0.0284(5) Uani 1 1 d . . . C10 C 0.23966(18) 0.71375(14) 0.37125(10) 0.0269(5) Uani 1 1 d . . . C11 C 0.32704(18) 0.69134(14) 0.38651(10) 0.0285(5) Uani 1 1 d . . . C12 C 0.3946(2) 0.74512(16) 0.40651(12) 0.0368(6) Uani 1 1 d . . . H12A H 0.3883 0.8011 0.4107 0.044 Uiso 1 1 calc R . . C13 C 0.4685(2) 0.70167(16) 0.41823(12) 0.0383(7) Uani 1 1 d . . . H13A H 0.5237 0.7212 0.4324 0.046 Uiso 1 1 calc R . . C14 C 0.44807(18) 0.61979(15) 0.40520(10) 0.0292(5) Uani 1 1 d . . . C15 C 0.50861(18) 0.55700(15) 0.41083(10) 0.0297(5) Uani 1 1 d . . . C16 C 0.48581(18) 0.47593(15) 0.40615(10) 0.0292(5) Uani 1 1 d . . . C17 C 0.5442(2) 0.41089(16) 0.41995(11) 0.0356(6) Uani 1 1 d . . . H17A H 0.6066 0.4145 0.4284 0.043 Uiso 1 1 calc R . . C18 C 0.49436(19) 0.34379(16) 0.41877(11) 0.0355(6) Uani 1 1 d . . . H18A H 0.5152 0.2917 0.4272 0.043 Uiso 1 1 calc R . . C19 C 0.40421(19) 0.36477(15) 0.40262(10) 0.0291(5) Uani 1 1 d . . . C20 C 0.33112(19) 0.31317(14) 0.40142(10) 0.0288(5) Uani 1 1 d . . . C21 C -0.03094(18) 0.44751(15) 0.33916(10) 0.0304(6) Uani 1 1 d . . . C22 C -0.0522(2) 0.39946(17) 0.29705(11) 0.0365(6) Uani 1 1 d . . . H22A H -0.0060 0.3829 0.2752 0.044 Uiso 1 1 calc R . . C23 C -0.1401(2) 0.37570(18) 0.28677(12) 0.0410(7) Uani 1 1 d . . . H23A H -0.1530 0.3420 0.2583 0.049 Uiso 1 1 calc R . . C24 C -0.2098(2) 0.40021(18) 0.31727(12) 0.0397(7) Uani 1 1 d . . . C25 C -0.1884(2) 0.4489(2) 0.35883(13) 0.0457(8) Uani 1 1 d . . . H25A H -0.2348 0.4667 0.3801 0.055 Uiso 1 1 calc R . . C26 C -0.1001(2) 0.47194(18) 0.36978(12) 0.0405(7) Uani 1 1 d . . . H26A H -0.0870 0.5048 0.3986 0.049 Uiso 1 1 calc R . . C27 C -0.3054(2) 0.3732(2) 0.30667(15) 0.0569(9) Uani 1 1 d . . . H27A H -0.3079 0.3398 0.2759 0.085 Uiso 1 1 calc R . . H27B H -0.3442 0.4199 0.3014 0.085 Uiso 1 1 calc R . . H27C H -0.3262 0.3423 0.3358 0.085 Uiso 1 1 calc R . . C28 C 0.21972(18) 0.80143(14) 0.37113(10) 0.0277(5) Uani 1 1 d . . . C29 C 0.1611(2) 0.83431(16) 0.40496(12) 0.0390(7) Uani 1 1 d . . . H29A H 0.1322 0.8008 0.4287 0.047 Uiso 1 1 calc R . . C30 C 0.1439(2) 0.91586(16) 0.40488(13) 0.0421(7) Uani 1 1 d . . . H30A H 0.1032 0.9374 0.4285 0.051 Uiso 1 1 calc R . . C31 C 0.1849(2) 0.96590(16) 0.37101(12) 0.0377(7) Uani 1 1 d . . . C32 C 0.2443(2) 0.93353(17) 0.33780(11) 0.0405(7) Uani 1 1 d . . . H32A H 0.2737 0.9674 0.3145 0.049 Uiso 1 1 calc R . . C33 C 0.2624(2) 0.85223(16) 0.33751(10) 0.0362(6) Uani 1 1 d . . . H33A H 0.3041 0.8312 0.3143 0.043 Uiso 1 1 calc R . . C34 C 0.1654(2) 1.05500(17) 0.37109(16) 0.0551(9) Uani 1 1 d . . . H34A H 0.2008 1.0813 0.3450 0.083 Uiso 1 1 calc R . . H34B H 0.1817 1.0773 0.4047 0.083 Uiso 1 1 calc R . . H34C H 0.1012 1.0639 0.3636 0.083 Uiso 1 1 calc R . . C35 C 0.60387(19) 0.57956(15) 0.42460(11) 0.0321(6) Uani 1 1 d . . . C36 C 0.6522(2) 0.62469(18) 0.39052(12) 0.0420(7) Uani 1 1 d . . . H36A H 0.6257 0.6376 0.3581 0.050 Uiso 1 1 calc R . . C37 C 0.7383(2) 0.6513(2) 0.40287(14) 0.0517(8) Uani 1 1 d . . . H37A H 0.7701 0.6820 0.3788 0.062 Uiso 1 1 calc R . . C38 C 0.7788(2) 0.6335(2) 0.45019(14) 0.0474(8) Uani 1 1 d . . . C39 C 0.7302(2) 0.58781(19) 0.48397(12) 0.0445(8) Uani 1 1 d . . . H39A H 0.7566 0.5745 0.5164 0.053 Uiso 1 1 calc R . . C40 C 0.6448(2) 0.56142(17) 0.47163(11) 0.0369(6) Uani 1 1 d . . . H40A H 0.6133 0.5303 0.4956 0.044 Uiso 1 1 calc R . . C41 C 0.8719(2) 0.6639(3) 0.46363(17) 0.0747(13) Uani 1 1 d . . . H41A H 0.8897 0.6461 0.4981 0.112 Uiso 1 1 calc R . . H41B H 0.8720 0.7223 0.4624 0.112 Uiso 1 1 calc R . . H41C H 0.9144 0.6429 0.4391 0.112 Uiso 1 1 calc R . . C42 C 0.34968(19) 0.22733(15) 0.41563(10) 0.0307(6) Uani 1 1 d . . . C43 C 0.3208(2) 0.19647(17) 0.46160(11) 0.0435(8) Uani 1 1 d . . . H43A H 0.2891 0.2296 0.4844 0.052 Uiso 1 1 calc R . . C44 C 0.3382(3) 0.11740(18) 0.47427(12) 0.0486(8) Uani 1 1 d . . . H44A H 0.3179 0.0972 0.5058 0.058 Uiso 1 1 calc R . . C45 C 0.3840(2) 0.06734(16) 0.44253(12) 0.0402(7) Uani 1 1 d . . . C46 C 0.4137(2) 0.09848(16) 0.39709(11) 0.0400(7) Uani 1 1 d . . . H46A H 0.4463 0.0655 0.3747 0.048 Uiso 1 1 calc R . . C47 C 0.3964(2) 0.17774(16) 0.38395(11) 0.0360(6) Uani 1 1 d . . . H47A H 0.4173 0.1980 0.3526 0.043 Uiso 1 1 calc R . . C48 C 0.3981(3) -0.02002(17) 0.45632(15) 0.0529(9) Uani 1 1 d . . . H48A H 0.4310 -0.0466 0.4293 0.079 Uiso 1 1 calc R . . H48B H 0.3396 -0.0460 0.4599 0.079 Uiso 1 1 calc R . . H48C H 0.4329 -0.0238 0.4886 0.079 Uiso 1 1 calc R . . C49 C 0.34307(19) 0.50410(14) 0.24699(10) 0.0261(5) Uani 1 1 d . . . C50 C 0.20090(18) 0.43113(15) 0.23723(9) 0.0286(5) Uani 1 1 d . . . C51 C 0.18750(19) 0.34757(16) 0.23203(10) 0.0314(6) Uani 1 1 d . . . C52 C 0.1243(2) 0.32024(18) 0.19574(11) 0.0406(7) Uani 1 1 d . . . H52A H 0.1153 0.2644 0.1918 0.049 Uiso 1 1 calc R . . C53 C 0.0747(2) 0.3724(2) 0.16545(12) 0.0479(8) Uani 1 1 d . . . H53A H 0.0347 0.3525 0.1395 0.058 Uiso 1 1 calc R . . C54 C 0.0833(2) 0.45362(19) 0.17305(11) 0.0436(7) Uani 1 1 d . . . H54A H 0.0469 0.4892 0.1532 0.052 Uiso 1 1 calc R . . C55 C 0.1449(2) 0.48458(17) 0.20952(11) 0.0360(6) Uani 1 1 d . . . C56 C 0.2425(2) 0.28867(16) 0.26421(11) 0.0360(6) Uani 1 1 d . . . H56A H 0.2477 0.3113 0.2995 0.043 Uiso 1 1 calc R . . C57 C 0.3372(2) 0.2780(2) 0.24588(14) 0.0555(9) Uani 1 1 d . . . H57A H 0.3662 0.3303 0.2431 0.083 Uiso 1 1 calc R . . H57B H 0.3351 0.2520 0.2123 0.083 Uiso 1 1 calc R . . H57C H 0.3716 0.2447 0.2703 0.083 Uiso 1 1 calc R . . C58 C 0.1980(3) 0.20692(19) 0.26857(14) 0.0583(10) Uani 1 1 d . . . H58A H 0.1369 0.2134 0.2810 0.087 Uiso 1 1 calc R . . H58B H 0.2333 0.1736 0.2926 0.087 Uiso 1 1 calc R . . H58C H 0.1951 0.1812 0.2349 0.087 Uiso 1 1 calc R . . C59 C 0.1457(2) 0.57502(17) 0.21760(12) 0.0433(7) Uani 1 1 d . . . H59A H 0.1748 0.5858 0.2518 0.052 Uiso 1 1 calc R . . C60 C 0.1977(3) 0.6209(2) 0.17820(15) 0.0572(10) Uani 1 1 d . . . H60A H 0.2594 0.6007 0.1776 0.086 Uiso 1 1 calc R . . H60B H 0.1985 0.6777 0.1871 0.086 Uiso 1 1 calc R . . H60C H 0.1686 0.6139 0.1444 0.086 Uiso 1 1 calc R . . C61 C 0.0497(3) 0.6087(2) 0.21807(14) 0.0570(9) Uani 1 1 d . . . H61A H 0.0522 0.6666 0.2232 0.086 Uiso 1 1 calc R . . H61B H 0.0171 0.5840 0.2459 0.086 Uiso 1 1 calc R . . H61C H 0.0186 0.5969 0.1854 0.086 Uiso 1 1 calc R . . C62 C 0.45023(19) 0.60932(16) 0.27687(10) 0.0326(6) Uani 1 1 d . . . H62A H 0.4614 0.6391 0.3095 0.039 Uiso 1 1 calc R . . C63 C 0.5372(2) 0.5644(2) 0.26602(13) 0.0453(7) Uani 1 1 d . . . H63A H 0.5492 0.5250 0.2930 0.068 Uiso 1 1 calc R . . H63B H 0.5873 0.6023 0.2651 0.068 Uiso 1 1 calc R . . H63C H 0.5308 0.5371 0.2330 0.068 Uiso 1 1 calc R . . C64 C 0.4272(2) 0.67212(18) 0.23571(12) 0.0461(8) Uani 1 1 d . . . H64A H 0.3713 0.6994 0.2441 0.069 Uiso 1 1 calc R . . H64B H 0.4196 0.6458 0.2024 0.069 Uiso 1 1 calc R . . H64C H 0.4761 0.7112 0.2343 0.069 Uiso 1 1 calc R . . C65 C 0.3613(2) 0.4365(2) 0.16573(12) 0.0472(8) Uani 1 1 d . . . H65A H 0.3159 0.3985 0.1791 0.057 Uiso 1 1 calc R . . C66 C 0.3271(4) 0.4711(3) 0.11546(14) 0.0813(14) Uani 1 1 d . . . H66A H 0.2697 0.4983 0.1204 0.122 Uiso 1 1 calc R . . H66B H 0.3183 0.4280 0.0905 0.122 Uiso 1 1 calc R . . H66C H 0.3710 0.5094 0.1029 0.122 Uiso 1 1 calc R . . C67 C 0.4512(3) 0.3929(2) 0.15926(17) 0.0727(13) Uani 1 1 d . . . H67A H 0.4718 0.3706 0.1922 0.109 Uiso 1 1 calc R . . H67B H 0.4962 0.4307 0.1472 0.109 Uiso 1 1 calc R . . H67C H 0.4430 0.3497 0.1343 0.109 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 Hf 0.02450(6) 0.02003(6) 0.02194(6) 0.00015(3) 0.00144(4) 0.00136(4) N1 0.0258(11) 0.0237(10) 0.0239(10) 0.0014(8) 0.0036(9) 0.0014(8) N2 0.0270(12) 0.0215(10) 0.0296(11) 0.0001(8) 0.0002(9) 0.0016(8) N3 0.0286(12) 0.0247(10) 0.0266(11) -0.0005(8) 0.0010(9) 0.0034(8) N4 0.0339(12) 0.0212(10) 0.0269(10) 0.0003(8) 0.0040(9) 0.0015(8) N5 0.0304(12) 0.0262(10) 0.0219(10) -0.0019(8) 0.0026(9) -0.0020(9) N6 0.0296(12) 0.0252(10) 0.0264(10) 0.0023(8) 0.0022(9) -0.0016(8) N7 0.0426(15) 0.0351(12) 0.0277(12) -0.0021(9) 0.0067(11) -0.0044(10) C1 0.0347(15) 0.0245(12) 0.0228(12) 0.0016(9) 0.0060(11) 0.0008(10) C2 0.0407(17) 0.0264(13) 0.0329(14) 0.0039(11) 0.0055(12) -0.0030(11) C3 0.0335(15) 0.0284(13) 0.0371(15) 0.0019(11) 0.0052(12) -0.0047(11) C4 0.0283(14) 0.0275(12) 0.0274(12) 0.0005(10) 0.0072(11) -0.0017(10) C5 0.0281(14) 0.0287(12) 0.0309(13) -0.0009(10) 0.0050(11) 0.0008(10) C6 0.0294(14) 0.0275(13) 0.0280(12) -0.0010(10) 0.0020(11) 0.0023(10) C7 0.0268(15) 0.0309(13) 0.0481(17) -0.0009(12) 0.0013(12) 0.0033(11) C8 0.0335(16) 0.0280(13) 0.0450(16) -0.0011(11) 0.0017(13) 0.0073(11) C9 0.0325(15) 0.0229(12) 0.0300(13) -0.0004(10) 0.0045(11) 0.0036(10) C10 0.0303(14) 0.0234(12) 0.0272(12) -0.0011(9) 0.0037(11) 0.0027(10) C11 0.0308(14) 0.0241(12) 0.0304(13) -0.0012(10) -0.0003(11) 0.0009(10) C12 0.0368(16) 0.0257(13) 0.0475(17) -0.0057(12) -0.0056(13) -0.0005(11) C13 0.0360(17) 0.0299(14) 0.0484(17) -0.0044(12) -0.0081(14) -0.0017(11) C14 0.0304(14) 0.0275(12) 0.0296(13) -0.0019(10) -0.0024(11) -0.0008(10) C15 0.0307(14) 0.0304(13) 0.0278(13) -0.0012(10) -0.0007(11) 0.0011(10) C16 0.0290(14) 0.0300(13) 0.0288(13) 0.0030(10) 0.0026(11) 0.0038(10) C17 0.0314(15) 0.0331(14) 0.0420(16) 0.0011(12) -0.0042(12) 0.0062(11) C18 0.0340(16) 0.0305(13) 0.0420(16) 0.0037(12) 0.0001(12) 0.0073(11) C19 0.0344(15) 0.0264(12) 0.0267(13) 0.0025(10) 0.0031(11) 0.0062(10) C20 0.0372(15) 0.0237(12) 0.0256(12) 0.0029(10) 0.0031(11) 0.0037(10) C21 0.0285(14) 0.0269(13) 0.0357(14) 0.0010(10) 0.0016(11) 0.0001(10) C22 0.0320(15) 0.0390(15) 0.0389(15) -0.0057(12) 0.0063(12) 0.0019(11) C23 0.0374(17) 0.0432(16) 0.0424(17) -0.0082(13) -0.0010(13) -0.0030(13) C24 0.0317(16) 0.0408(16) 0.0468(17) -0.0034(13) 0.0037(13) -0.0028(12) C25 0.0319(17) 0.0521(19) 0.0539(19) -0.0147(15) 0.0128(14) -0.0040(13) C26 0.0379(17) 0.0401(15) 0.0439(16) -0.0130(13) 0.0101(13) -0.0062(13) C27 0.0352(19) 0.072(2) 0.063(2) -0.0153(19) 0.0043(16) -0.0119(16) C28 0.0321(14) 0.0217(11) 0.0290(13) 0.0000(9) -0.0015(11) 0.0013(10) C29 0.0489(18) 0.0244(13) 0.0446(16) 0.0013(11) 0.0142(14) 0.0006(12) C30 0.0461(19) 0.0292(14) 0.0517(18) -0.0058(13) 0.0120(15) 0.0057(12) C31 0.0423(17) 0.0226(12) 0.0478(16) 0.0017(12) -0.0083(14) 0.0019(11) C32 0.053(2) 0.0306(14) 0.0385(16) 0.0098(12) 0.0051(14) -0.0034(13) C33 0.0461(18) 0.0331(14) 0.0299(14) 0.0019(11) 0.0077(12) 0.0006(12) C34 0.059(2) 0.0234(14) 0.082(3) 0.0025(15) -0.0078(19) 0.0059(13) C35 0.0295(15) 0.0303(13) 0.0362(14) -0.0022(11) -0.0014(12) 0.0037(10) C36 0.0395(18) 0.0462(17) 0.0403(16) 0.0012(13) 0.0020(14) -0.0092(13) C37 0.043(2) 0.056(2) 0.057(2) -0.0094(16) 0.0091(16) -0.0139(15) C38 0.0269(16) 0.0567(19) 0.058(2) -0.0274(16) -0.0023(14) 0.0019(13) C39 0.0397(18) 0.0514(18) 0.0417(17) -0.0188(14) -0.0114(14) 0.0127(14) C40 0.0353(16) 0.0425(15) 0.0329(14) -0.0089(12) -0.0004(12) 0.0063(12) C41 0.041(2) 0.093(3) 0.090(3) -0.048(3) -0.004(2) -0.009(2) C42 0.0361(16) 0.0236(12) 0.0324(14) 0.0040(10) 0.0001(12) 0.0028(10) C43 0.069(2) 0.0324(15) 0.0297(14) 0.0026(11) 0.0091(15) 0.0126(14) C44 0.076(3) 0.0381(16) 0.0320(15) 0.0136(12) 0.0095(16) 0.0073(15) C45 0.0512(19) 0.0252(13) 0.0437(17) 0.0044(12) -0.0061(14) 0.0042(12) C46 0.0525(19) 0.0289(14) 0.0391(16) 0.0009(12) 0.0074(14) 0.0091(12) C47 0.0429(17) 0.0308(14) 0.0347(14) 0.0036(11) 0.0073(13) 0.0065(12) C48 0.075(3) 0.0273(15) 0.056(2) 0.0095(14) -0.0036(19) 0.0076(15) C49 0.0294(14) 0.0248(12) 0.0242(12) 0.0030(9) 0.0018(10) 0.0000(9) C50 0.0319(14) 0.0314(13) 0.0227(12) -0.0020(10) 0.0018(11) -0.0037(10) C51 0.0369(16) 0.0311(13) 0.0263(13) -0.0026(10) 0.0035(11) -0.0053(11) C52 0.0496(19) 0.0361(15) 0.0360(15) -0.0038(12) 0.0016(14) -0.0121(13) C53 0.050(2) 0.0540(19) 0.0392(17) -0.0021(14) -0.0126(15) -0.0156(15) C54 0.050(2) 0.0465(17) 0.0338(15) 0.0038(13) -0.0134(14) -0.0045(14) C55 0.0422(17) 0.0357(14) 0.0297(14) 0.0014(11) -0.0027(12) -0.0044(12) C56 0.0491(18) 0.0272(13) 0.0317(14) -0.0025(11) 0.0015(13) -0.0020(12) C57 0.057(2) 0.0509(19) 0.059(2) 0.0036(16) 0.0101(18) 0.0193(16) C58 0.086(3) 0.0338(16) 0.055(2) 0.0073(15) -0.006(2) -0.0125(17) C59 0.057(2) 0.0360(15) 0.0358(15) 0.0018(12) -0.0168(15) 0.0046(13) C60 0.066(2) 0.0375(17) 0.067(2) 0.0150(16) -0.0180(19) -0.0049(15) C61 0.066(3) 0.055(2) 0.049(2) 0.0012(16) -0.0090(18) 0.0167(17) C62 0.0324(15) 0.0338(14) 0.0317(14) 0.0027(11) 0.0022(11) -0.0074(11) C63 0.0291(16) 0.0539(19) 0.0532(19) -0.0025(15) 0.0044(14) -0.0020(13) C64 0.051(2) 0.0388(16) 0.0481(18) 0.0134(14) 0.0021(15) -0.0129(14) C65 0.060(2) 0.0493(18) 0.0330(15) -0.0133(13) 0.0197(15) -0.0149(15) C66 0.105(4) 0.112(4) 0.0266(17) -0.011(2) 0.008(2) -0.030(3) C67 0.077(3) 0.054(2) 0.090(3) -0.024(2) 0.053(2) -0.0123(19) _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 Hf N6 2.087(2) . ? Hf N5 2.151(2) . ? Hf N2 2.184(2) . ? Hf N4 2.207(2) . ? Hf N3 2.238(2) . ? Hf N1 2.251(2) . ? Hf C49 2.664(3) . ? N1 C4 1.381(3) . ? N1 C1 1.385(3) . ? N2 C9 1.393(3) . ? N2 C6 1.397(3) . ? N3 C11 1.381(3) . ? N3 C14 1.389(3) . ? N4 C16 1.393(3) . ? N4 C19 1.401(3) . ? N5 C49 1.428(3) . ? N5 C50 1.432(3) . ? N6 C49 1.391(3) . ? N6 C62 1.470(3) . ? N7 C49 1.282(4) . ? N7 C65 1.466(4) . ? C1 C20 1.400(4) . ? C1 C2 1.435(4) . ? C2 C3 1.349(4) . ? C3 C4 1.444(3) . ? C4 C5 1.400(4) . ? C5 C6 1.405(4) . ? C5 C21 1.497(4) . ? C6 C7 1.425(3) . ? C7 C8 1.349(4) . ? C8 C9 1.427(4) . ? C9 C10 1.398(4) . ? C10 C11 1.399(4) . ? C10 C28 1.498(3) . ? C11 C12 1.436(4) . ? C12 C13 1.345(4) . ? C13 C14 1.443(4) . ? C14 C15 1.390(4) . ? C15 C16 1.404(4) . ? C15 C35 1.500(4) . ? C16 C17 1.432(4) . ? C17 C18 1.346(4) . ? C18 C19 1.437(4) . ? C19 C20 1.389(4) . ? C20 C42 1.509(3) . ? C21 C26 1.386(4) . ? C21 C22 1.393(4) . ? C22 C23 1.384(4) . ? C23 C24 1.391(4) . ? C24 C25 1.389(4) . ? C24 C27 1.510(4) . ? C25 C26 1.389(4) . ? C28 C29 1.377(4) . ? C28 C33 1.392(4) . ? C29 C30 1.390(4) . ? C30 C31 1.377(4) . ? C31 C32 1.371(4) . ? C31 C34 1.520(4) . ? C32 C33 1.388(4) . ? C35 C36 1.387(4) . ? C35 C40 1.390(4) . ? C36 C37 1.385(4) . ? C37 C38 1.393(5) . ? C38 C39 1.390(5) . ? C38 C41 1.505(4) . ? C39 C40 1.374(4) . ? C42 C47 1.378(4) . ? C42 C43 1.391(4) . ? C43 C44 1.388(4) . ? C44 C45 1.376(4) . ? C45 C46 1.385(4) . ? C45 C48 1.520(4) . ? C46 C47 1.394(4) . ? C50 C55 1.409(4) . ? C50 C51 1.420(4) . ? C51 C52 1.393(4) . ? C51 C56 1.519(4) . ? C52 C53 1.379(4) . ? C53 C54 1.381(4) . ? C54 C55 1.402(4) . ? C55 C59 1.530(4) . ? C56 C57 1.513(4) . ? C56 C58 1.527(4) . ? C59 C60 1.517(5) . ? C59 C61 1.535(5) . ? C62 C63 1.531(4) . ? C62 C64 1.537(4) . ? C65 C66 1.512(5) . ? C65 C67 1.538(5) . ? 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 N6 Hf N5 63.21(8) . . ? N6 Hf N2 113.66(8) . . ? N5 Hf N2 102.89(8) . . ? N6 Hf N4 104.02(8) . . ? N5 Hf N4 116.76(8) . . ? N2 Hf N4 134.46(8) . . ? N6 Hf N3 82.56(8) . . ? N5 Hf N3 144.09(8) . . ? N2 Hf N3 80.23(8) . . ? N4 Hf N3 80.27(7) . . ? N6 Hf N1 148.38(8) . . ? N5 Hf N1 86.77(8) . . ? N2 Hf N1 81.05(8) . . ? N4 Hf N1 79.82(8) . . ? N3 Hf N1 128.63(7) . . ? N6 Hf C49 31.13(8) . . ? N5 Hf C49 32.33(8) . . ? N2 Hf C49 114.55(8) . . ? N4 Hf C49 110.95(8) . . ? N3 Hf C49 113.54(8) . . ? N1 Hf C49 117.77(7) . . ? C4 N1 C1 106.0(2) . . ? C4 N1 Hf 123.54(16) . . ? C1 N1 Hf 127.71(17) . . ? C9 N2 C6 105.5(2) . . ? C9 N2 Hf 125.79(17) . . ? C6 N2 Hf 124.19(16) . . ? C11 N3 C14 105.5(2) . . ? C11 N3 Hf 126.14(17) . . ? C14 N3 Hf 125.62(16) . . ? C16 N4 C19 105.4(2) . . ? C16 N4 Hf 124.84(16) . . ? C19 N4 Hf 126.38(17) . . ? C49 N5 C50 117.8(2) . . ? C49 N5 Hf 94.01(15) . . ? C50 N5 Hf 142.54(17) . . ? C49 N6 C62 120.7(2) . . ? C49 N6 Hf 98.01(15) . . ? C62 N6 Hf 140.07(17) . . ? C49 N7 C65 124.5(2) . . ? N1 C1 C20 124.9(2) . . ? N1 C1 C2 109.5(2) . . ? C20 C1 C2 125.5(2) . . ? C3 C2 C1 107.8(2) . . ? C2 C3 C4 106.9(2) . . ? N1 C4 C5 125.9(2) . . ? N1 C4 C3 109.8(2) . . ? C5 C4 C3 124.2(3) . . ? C4 C5 C6 125.0(2) . . ? C4 C5 C21 116.8(2) . . ? C6 C5 C21 118.1(2) . . ? N2 C6 C5 125.0(2) . . ? N2 C6 C7 109.3(2) . . ? C5 C6 C7 125.6(2) . . ? C8 C7 C6 108.0(3) . . ? C7 C8 C9 107.7(2) . . ? N2 C9 C10 124.8(2) . . ? N2 C9 C8 109.5(2) . . ? C10 C9 C8 125.6(2) . . ? C9 C10 C11 125.0(2) . . ? C9 C10 C28 118.4(2) . . ? C11 C10 C28 116.5(2) . . ? N3 C11 C10 125.2(2) . . ? N3 C11 C12 110.0(2) . . ? C10 C11 C12 124.7(2) . . ? C13 C12 C11 107.5(2) . . ? C12 C13 C14 107.2(2) . . ? N3 C14 C15 126.1(2) . . ? N3 C14 C13 109.6(2) . . ? C15 C14 C13 124.3(3) . . ? C14 C15 C16 124.7(2) . . ? C14 C15 C35 116.1(2) . . ? C16 C15 C35 119.3(2) . . ? N4 C16 C15 124.9(2) . . ? N4 C16 C17 109.8(2) . . ? C15 C16 C17 124.8(3) . . ? C18 C17 C16 107.5(3) . . ? C17 C18 C19 108.1(2) . . ? C20 C19 N4 125.4(2) . . ? C20 C19 C18 125.3(2) . . ? N4 C19 C18 109.0(2) . . ? C19 C20 C1 125.3(2) . . ? C19 C20 C42 116.8(2) . . ? C1 C20 C42 117.8(2) . . ? C26 C21 C22 118.3(3) . . ? C26 C21 C5 122.0(2) . . ? C22 C21 C5 119.6(2) . . ? C23 C22 C21 120.6(3) . . ? C22 C23 C24 121.3(3) . . ? C25 C24 C23 117.8(3) . . ? C25 C24 C27 120.8(3) . . ? C23 C24 C27 121.4(3) . . ? C24 C25 C26 121.1(3) . . ? C21 C26 C25 120.8(3) . . ? C29 C28 C33 118.2(2) . . ? C29 C28 C10 121.3(2) . . ? C33 C28 C10 120.4(2) . . ? C28 C29 C30 120.9(3) . . ? C31 C30 C29 120.9(3) . . ? C32 C31 C30 118.4(3) . . ? C32 C31 C34 121.1(3) . . ? C30 C31 C34 120.5(3) . . ? C31 C32 C33 121.4(3) . . ? C32 C33 C28 120.3(3) . . ? C36 C35 C40 117.9(3) . . ? C36 C35 C15 119.2(3) . . ? C40 C35 C15 122.8(3) . . ? C37 C36 C35 121.3(3) . . ? C36 C37 C38 120.6(3) . . ? C39 C38 C37 117.7(3) . . ? C39 C38 C41 122.0(3) . . ? C37 C38 C41 120.3(4) . . ? C40 C39 C38 121.6(3) . . ? C39 C40 C35 120.9(3) . . ? C47 C42 C43 118.2(2) . . ? C47 C42 C20 121.2(2) . . ? C43 C42 C20 120.6(2) . . ? C44 C43 C42 120.1(3) . . ? C45 C44 C43 122.0(3) . . ? C44 C45 C46 117.9(3) . . ? C44 C45 C48 120.7(3) . . ? C46 C45 C48 121.4(3) . . ? C45 C46 C47 120.6(3) . . ? C42 C47 C46 121.2(3) . . ? N7 C49 N6 122.8(2) . . ? N7 C49 N5 133.2(2) . . ? N6 C49 N5 104.0(2) . . ? N7 C49 Hf 169.9(2) . . ? N6 C49 Hf 50.86(12) . . ? N5 C49 Hf 53.66(12) . . ? C55 C50 C51 119.9(2) . . ? C55 C50 N5 120.1(2) . . ? C51 C50 N5 120.0(2) . . ? C52 C51 C50 118.6(3) . . ? C52 C51 C56 120.3(2) . . ? C50 C51 C56 121.0(2) . . ? C53 C52 C51 121.5(3) . . ? C52 C53 C54 119.7(3) . . ? C53 C54 C55 121.3(3) . . ? C54 C55 C50 118.6(3) . . ? C54 C55 C59 117.5(3) . . ? C50 C55 C59 123.8(3) . . ? C57 C56 C51 113.0(2) . . ? C57 C56 C58 109.1(3) . . ? C51 C56 C58 113.4(3) . . ? C60 C59 C55 114.1(3) . . ? C60 C59 C61 108.3(3) . . ? C55 C59 C61 111.2(3) . . ? N6 C62 C63 113.0(2) . . ? N6 C62 C64 111.4(2) . . ? C63 C62 C64 112.2(3) . . ? N7 C65 C66 110.3(3) . . ? N7 C65 C67 106.7(3) . . ? C66 C65 C67 110.9(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.414 _refine_diff_density_min -1.744 _refine_diff_density_rms 0.086