# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Frank Schaper ' _publ_contact_author_email Frank.Schaper@umontreal.ca _publ_author_name 'Frank Schaper' data_todd15 _database_code_depnum_ccdc_archive 'CCDC 894423' #TrackingRef '- Zoghbi-2012.cif' _vrf_PLAT331_todd15 ; RESPONSE Cocrystallized solvent shows some disorder. ; _vrf_PLAT154_todd15 ; RESPONSE Coincidental. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H42 Cl2 N4 Zr, C6 H6' _chemical_formula_sum 'C38 H48 Cl2 N4 Zr' _chemical_formula_weight 722.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7217(4) _cell_length_b 11.9708(5) _cell_length_c 16.5433(7) _cell_angle_alpha 100.423(2) _cell_angle_beta 104.614(2) _cell_angle_gamma 96.408(2) _cell_volume 1807.04(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 6871 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 68.30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 4.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios multi-layers optics' _diffrn_measurement_device_type 'Bruker SMART 6000 / Nonius FR591' _diffrn_detector_area_resol_mean 5.5 _diffrn_measurement_method '\w scan' _diffrn_reflns_number 25219 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 69.62 _reflns_number_total 6640 _reflns_number_gt 5226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6640 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.13074(2) 0.29037(2) 0.236105(15) 0.02210(7) Uani 1 1 d . . . Cl1 Cl -0.04838(7) 0.11741(6) 0.17629(4) 0.03191(17) Uani 1 1 d . . . Cl2 Cl 0.37237(7) 0.40224(6) 0.29707(4) 0.03259(17) Uani 1 1 d . . . N1 N 0.0428(2) 0.42133(19) 0.17173(14) 0.0283(5) Uani 1 1 d . . . N3 N -0.0034(2) 0.37459(19) 0.31048(14) 0.0274(5) Uani 1 1 d . . . N4 N 0.1848(2) 0.21956(19) 0.35709(13) 0.0248(5) Uani 1 1 d . . . C1 C 0.0688(4) 0.7314(3) 0.3027(2) 0.0491(9) Uani 1 1 d . . . H1A H 0.1719 0.7410 0.3283 0.059 Uiso 1 1 calc R . . H1B H 0.0459 0.8046 0.2906 0.059 Uiso 1 1 calc R . . C2 C 0.0258(3) 0.6389(3) 0.2174(2) 0.0391(7) Uani 1 1 d . . . H2A H -0.0750 0.6347 0.1878 0.047 Uiso 1 1 calc R . . H2B H 0.0834 0.6587 0.1804 0.047 Uiso 1 1 calc R . . C3 C 0.0522(3) 0.5241(2) 0.23950(18) 0.0343(7) Uani 1 1 d . . . H3 H 0.1530 0.5389 0.2741 0.041 Uiso 1 1 calc R . . C4 C -0.1611(3) 0.4645(3) 0.0619(2) 0.0401(8) Uani 1 1 d . . . H4A H -0.1196 0.5335 0.0491 0.060 Uiso 1 1 calc R . . H4B H -0.2073 0.4844 0.1061 0.060 Uiso 1 1 calc R . . H4C H -0.2309 0.4190 0.0114 0.060 Uiso 1 1 calc R . . C5 C -0.0444(3) 0.3965(2) 0.09164(18) 0.0282(6) Uani 1 1 d . . . C6 C -0.0262(3) 0.3086(2) 0.02947(18) 0.0298(6) Uani 1 1 d . . . H6 H -0.1008 0.2858 -0.0210 0.036 Uiso 1 1 calc R . . C7 C 0.0920(3) 0.2508(2) 0.03445(17) 0.0264(6) Uani 1 1 d . . . C8 C 0.1183(3) 0.1979(3) -0.04925(18) 0.0361(7) Uani 1 1 d . . . H8A H 0.1943 0.2470 -0.0595 0.054 Uiso 1 1 calc R . . H8B H 0.0318 0.1894 -0.0950 0.054 Uiso 1 1 calc R . . H8C H 0.1456 0.1238 -0.0465 0.054 Uiso 1 1 calc R . . N2 N 0.1831(2) 0.24663(19) 0.10808(14) 0.0246(5) Uani 1 1 d . . . C9 C 0.3173(3) 0.2083(3) 0.10418(17) 0.0292(6) Uani 1 1 d . . . C10 C 0.4358(3) 0.2897(3) 0.10832(19) 0.0360(7) Uani 1 1 d . . . C11 C 0.5659(4) 0.2525(3) 0.1100(2) 0.0546(10) Uani 1 1 d . . . H12 H 0.6464 0.3059 0.1150 0.066 Uiso 1 1 calc R . . C12 C 0.5790(4) 0.1383(4) 0.1045(3) 0.0673(12) Uani 1 1 d . . . H13 H 0.6678 0.1151 0.1063 0.081 Uiso 1 1 calc R . . C13 C 0.4607(4) 0.0589(3) 0.0963(2) 0.0561(10) Uani 1 1 d . . . H14 H 0.4699 -0.0183 0.0916 0.067 Uiso 1 1 calc R . . C14 C 0.3277(3) 0.0909(3) 0.09483(19) 0.0363(7) Uani 1 1 d . . . C15 C 0.1999(3) -0.0024(2) 0.0771(2) 0.0387(7) Uani 1 1 d . . . H16A H 0.2266 -0.0597 0.1092 0.058 Uiso 1 1 calc R . . H16B H 0.1686 -0.0373 0.0171 0.058 Uiso 1 1 calc R . . H16C H 0.1228 0.0303 0.0938 0.058 Uiso 1 1 calc R . . C17 C 0.4229(4) 0.4129(3) 0.1067(2) 0.0456(8) Uani 1 1 d . . . H17A H 0.4131 0.4244 0.0497 0.068 Uiso 1 1 calc R . . H17B H 0.5077 0.4620 0.1451 0.068 Uiso 1 1 calc R . . H17C H 0.3397 0.4311 0.1243 0.068 Uiso 1 1 calc R . . C21 C -0.0077(4) 0.6985(3) 0.3641(2) 0.0472(9) Uani 1 1 d . . . H21A H -0.1095 0.7007 0.3419 0.057 Uiso 1 1 calc R . . H21B H 0.0282 0.7550 0.4178 0.057 Uiso 1 1 calc R . . C22 C 0.0095(3) 0.5799(3) 0.3814(2) 0.0396(8) Uani 1 1 d . . . H22A H -0.0513 0.5605 0.4168 0.048 Uiso 1 1 calc R . . H22B H 0.1088 0.5806 0.4124 0.048 Uiso 1 1 calc R . . C23 C -0.0311(3) 0.4892(2) 0.29830(18) 0.0326(7) Uani 1 1 d . . . H23 H -0.1341 0.4839 0.2705 0.039 Uiso 1 1 calc R . . C24 C -0.2339(3) 0.3459(3) 0.3495(2) 0.0434(8) Uani 1 1 d . . . H24A H -0.2850 0.2879 0.3692 0.065 Uiso 1 1 calc R . . H24B H -0.2898 0.3520 0.2941 0.065 Uiso 1 1 calc R . . H24C H -0.2179 0.4185 0.3890 0.065 Uiso 1 1 calc R . . C25 C -0.0905(3) 0.3130(3) 0.34334(17) 0.0307(7) Uani 1 1 d . . . C26 C -0.0534(3) 0.2165(3) 0.37379(18) 0.0306(7) Uani 1 1 d . . . H26 H -0.1268 0.1696 0.3844 0.037 Uiso 1 1 calc R . . C27 C 0.0813(3) 0.1819(2) 0.39020(17) 0.0283(6) Uani 1 1 d . . . C28 C 0.1088(3) 0.1005(3) 0.4502(2) 0.0400(8) Uani 1 1 d . . . H28A H 0.1702 0.1420 0.5049 0.060 Uiso 1 1 calc R . . H28B H 0.1546 0.0405 0.4269 0.060 Uiso 1 1 calc R . . H28C H 0.0188 0.0672 0.4568 0.060 Uiso 1 1 calc R . . C29 C 0.3297(3) 0.2090(2) 0.40191(17) 0.0266(6) Uani 1 1 d . . . C30 C 0.4030(3) 0.2946(2) 0.47512(18) 0.0299(6) Uani 1 1 d . . . C31 C 0.5422(3) 0.2854(3) 0.51808(19) 0.0355(7) Uani 1 1 d . . . H31 H 0.5934 0.3422 0.5658 0.043 Uiso 1 1 calc R . . C32 C 0.6064(3) 0.1937(3) 0.4915(2) 0.0404(8) Uani 1 1 d . . . H32 H 0.6993 0.1884 0.5217 0.048 Uiso 1 1 calc R . . C33 C 0.5325(3) 0.1099(3) 0.4202(2) 0.0388(7) Uani 1 1 d . . . H33 H 0.5760 0.0480 0.4027 0.047 Uiso 1 1 calc R . . C34 C 0.3936(3) 0.1164(3) 0.37375(19) 0.0324(7) Uani 1 1 d . . . C35 C 0.3164(4) 0.0235(3) 0.2966(2) 0.0493(9) Uani 1 1 d . . . H35A H 0.2159 0.0296 0.2803 0.074 Uiso 1 1 calc R . . H35B H 0.3271 -0.0504 0.3098 0.074 Uiso 1 1 calc R . . H35C H 0.3566 0.0320 0.2502 0.074 Uiso 1 1 calc R . . C36 C 0.3325(3) 0.3925(3) 0.50678(19) 0.0364(7) Uani 1 1 d . . . H36A H 0.2587 0.3643 0.5306 0.055 Uiso 1 1 calc R . . H36B H 0.2903 0.4263 0.4600 0.055 Uiso 1 1 calc R . . H36C H 0.4033 0.4496 0.5500 0.055 Uiso 1 1 calc R . . C100 C 0.6023(4) 0.7992(3) 0.3151(2) 0.0494(9) Uani 1 1 d . . . H100 H 0.6117 0.8021 0.3729 0.059 Uiso 1 1 calc R . . C101 C 0.4977(4) 0.7217(3) 0.2551(3) 0.0637(11) Uani 1 1 d . . . H101 H 0.4360 0.6708 0.2716 0.076 Uiso 1 1 calc R . . C102 C 0.4825(5) 0.7180(3) 0.1700(3) 0.0730(13) Uani 1 1 d . . . H102 H 0.4092 0.6659 0.1287 0.088 Uiso 1 1 calc R . . C103 C 0.5759(5) 0.7917(4) 0.1456(3) 0.0692(12) Uani 1 1 d . . . H103 H 0.5675 0.7884 0.0879 0.083 Uiso 1 1 calc R . . C104 C 0.6808(5) 0.8694(3) 0.2071(3) 0.0623(11) Uani 1 1 d . . . H104 H 0.7437 0.9202 0.1914 0.075 Uiso 1 1 calc R . . C105 C 0.6935(4) 0.8725(3) 0.2916(2) 0.0504(9) Uani 1 1 d . . . H105 H 0.7654 0.9255 0.3333 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02155(12) 0.02542(13) 0.02060(12) 0.00561(9) 0.00787(9) 0.00351(9) Cl1 0.0284(4) 0.0348(4) 0.0294(4) 0.0027(3) 0.0094(3) -0.0041(3) Cl2 0.0260(3) 0.0407(4) 0.0284(4) 0.0088(3) 0.0057(3) -0.0034(3) N1 0.0369(13) 0.0288(13) 0.0244(13) 0.0091(10) 0.0129(11) 0.0116(11) N3 0.0335(13) 0.0306(13) 0.0241(12) 0.0073(10) 0.0156(10) 0.0101(10) N4 0.0266(12) 0.0291(13) 0.0211(12) 0.0093(10) 0.0079(10) 0.0053(10) C1 0.062(2) 0.0304(18) 0.056(2) 0.0062(16) 0.0185(18) 0.0116(16) C2 0.0450(19) 0.0314(17) 0.0423(19) 0.0136(15) 0.0106(15) 0.0062(14) C3 0.0460(18) 0.0305(17) 0.0277(16) 0.0058(13) 0.0117(14) 0.0095(14) C4 0.0368(18) 0.046(2) 0.0409(19) 0.0165(15) 0.0098(14) 0.0134(15) C5 0.0263(15) 0.0342(16) 0.0288(16) 0.0136(13) 0.0113(12) 0.0053(12) C6 0.0285(15) 0.0343(16) 0.0249(15) 0.0100(13) 0.0037(12) 0.0014(13) C7 0.0299(15) 0.0267(15) 0.0216(15) 0.0053(12) 0.0081(12) -0.0015(12) C8 0.0467(18) 0.0382(18) 0.0248(16) 0.0072(13) 0.0124(14) 0.0064(14) N2 0.0249(12) 0.0267(13) 0.0222(12) 0.0029(10) 0.0091(10) 0.0024(10) C9 0.0238(15) 0.0380(17) 0.0260(15) 0.0034(13) 0.0093(12) 0.0064(13) C10 0.0287(16) 0.047(2) 0.0337(17) 0.0034(14) 0.0153(13) 0.0042(14) C11 0.0321(19) 0.064(3) 0.063(2) -0.0014(19) 0.0211(17) -0.0055(17) C12 0.034(2) 0.076(3) 0.088(3) -0.001(2) 0.018(2) 0.020(2) C13 0.043(2) 0.049(2) 0.074(3) 0.0019(19) 0.0147(18) 0.0198(18) C14 0.0345(17) 0.0382(18) 0.0341(18) 0.0012(14) 0.0089(13) 0.0102(14) C15 0.0457(19) 0.0276(16) 0.0403(19) 0.0021(14) 0.0102(15) 0.0079(14) C17 0.047(2) 0.046(2) 0.046(2) 0.0086(16) 0.0225(16) -0.0069(16) C21 0.051(2) 0.039(2) 0.046(2) -0.0023(16) 0.0079(16) 0.0169(16) C22 0.0425(18) 0.0409(19) 0.0375(18) 0.0009(15) 0.0192(15) 0.0096(15) C23 0.0417(17) 0.0318(17) 0.0292(16) 0.0077(13) 0.0139(13) 0.0149(14) C24 0.0381(18) 0.056(2) 0.049(2) 0.0187(17) 0.0268(16) 0.0156(16) C25 0.0298(15) 0.0409(18) 0.0226(15) 0.0050(13) 0.0117(12) 0.0037(13) C26 0.0304(16) 0.0370(17) 0.0280(16) 0.0099(13) 0.0146(13) 0.0006(13) C27 0.0353(16) 0.0264(15) 0.0233(15) 0.0053(12) 0.0100(12) 0.0009(12) C28 0.0408(18) 0.045(2) 0.0405(19) 0.0217(16) 0.0154(15) 0.0048(15) C29 0.0286(15) 0.0309(16) 0.0240(15) 0.0133(12) 0.0085(12) 0.0048(12) C30 0.0328(16) 0.0343(17) 0.0251(15) 0.0095(13) 0.0113(12) 0.0035(13) C31 0.0329(16) 0.0461(19) 0.0260(16) 0.0078(14) 0.0075(13) 0.0023(14) C32 0.0285(16) 0.057(2) 0.0363(19) 0.0147(16) 0.0056(14) 0.0091(15) C33 0.0396(18) 0.0426(19) 0.0402(19) 0.0128(15) 0.0143(15) 0.0181(15) C34 0.0367(17) 0.0334(17) 0.0300(17) 0.0100(13) 0.0107(13) 0.0091(13) C35 0.057(2) 0.039(2) 0.046(2) 0.0002(16) 0.0074(17) 0.0146(17) C36 0.0365(17) 0.0408(18) 0.0275(16) 0.0025(13) 0.0058(13) 0.0036(14) C100 0.055(2) 0.060(2) 0.039(2) 0.0212(18) 0.0155(17) 0.0126(19) C101 0.068(3) 0.055(3) 0.069(3) 0.026(2) 0.017(2) -0.001(2) C102 0.093(3) 0.048(2) 0.057(3) -0.001(2) -0.005(2) 0.004(2) C103 0.117(4) 0.065(3) 0.038(2) 0.017(2) 0.029(2) 0.037(3) C104 0.081(3) 0.055(3) 0.071(3) 0.025(2) 0.048(2) 0.015(2) C105 0.045(2) 0.050(2) 0.055(2) 0.0079(18) 0.0147(18) 0.0078(17) _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 N1 2.183(2) . ? Zr1 N3 2.211(2) . ? Zr1 N4 2.277(2) . ? Zr1 N2 2.285(2) . ? Zr1 Cl1 2.4255(7) . ? Zr1 Cl2 2.4377(7) . ? N1 C5 1.341(3) . ? N1 C3 1.484(3) . ? N3 C25 1.339(3) . ? N3 C23 1.466(4) . ? N4 C27 1.335(3) . ? N4 C29 1.448(3) . ? C1 C21 1.484(5) . ? C1 C2 1.557(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.517(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C23 1.499(4) . ? C3 H3 0.9800 . ? C4 C5 1.504(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.392(4) . ? C6 C7 1.398(4) . ? C6 H6 0.9300 . ? C7 N2 1.326(3) . ? C7 C8 1.511(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N2 C9 1.443(3) . ? C9 C10 1.402(4) . ? C9 C14 1.403(4) . ? C10 C11 1.382(4) . ? C10 C17 1.498(4) . ? C11 C12 1.376(5) . ? C11 H12 0.9300 . ? C12 C13 1.369(5) . ? C12 H13 0.9300 . ? C13 C14 1.384(4) . ? C13 H14 0.9300 . ? C14 C15 1.506(4) . ? C15 H16A 0.9600 . ? C15 H16B 0.9600 . ? C15 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C21 C22 1.517(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.521(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23 0.9800 . ? C24 C25 1.512(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.390(4) . ? C26 C27 1.394(4) . ? C26 H26 0.9300 . ? C27 C28 1.509(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.394(4) . ? C29 C30 1.406(4) . ? C30 C31 1.388(4) . ? C30 C36 1.503(4) . ? C31 C32 1.380(4) . ? C31 H31 0.9300 . ? C32 C33 1.378(4) . ? C32 H32 0.9300 . ? C33 C34 1.393(4) . ? C33 H33 0.9300 . ? C34 C35 1.499(4) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C100 C101 1.353(5) . ? C100 C105 1.354(5) . ? C100 H100 0.9300 . ? C101 C102 1.370(6) . ? C101 H101 0.9300 . ? C102 C103 1.378(6) . ? C102 H102 0.9300 . ? C103 C104 1.365(6) . ? C103 H103 0.9300 . ? C104 C105 1.366(5) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? 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 N1 Zr1 N3 72.26(8) . . ? N1 Zr1 N4 148.55(8) . . ? N3 Zr1 N4 77.85(8) . . ? N1 Zr1 N2 77.97(8) . . ? N3 Zr1 N2 148.00(8) . . ? N4 Zr1 N2 133.18(8) . . ? N1 Zr1 Cl1 105.28(6) . . ? N3 Zr1 Cl1 93.02(6) . . ? N4 Zr1 Cl1 85.59(6) . . ? N2 Zr1 Cl1 83.59(6) . . ? N1 Zr1 Cl2 94.80(6) . . ? N3 Zr1 Cl2 105.30(6) . . ? N4 Zr1 Cl2 83.67(6) . . ? N2 Zr1 Cl2 88.41(6) . . ? Cl1 Zr1 Cl2 156.24(3) . . ? C5 N1 C3 126.5(2) . . ? C5 N1 Zr1 123.01(19) . . ? C3 N1 Zr1 106.92(17) . . ? C25 N3 C23 119.0(2) . . ? C25 N3 Zr1 121.01(18) . . ? C23 N3 Zr1 116.87(16) . . ? C27 N4 C29 115.5(2) . . ? C27 N4 Zr1 120.96(18) . . ? C29 N4 Zr1 123.56(15) . . ? C21 C1 C2 111.6(3) . . ? C21 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? C21 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C3 C2 C1 107.7(3) . . ? C3 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? C3 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N1 C3 C23 108.2(2) . . ? N1 C3 C2 121.1(2) . . ? C23 C3 C2 113.1(2) . . ? N1 C3 H3 104.2 . . ? C23 C3 H3 104.2 . . ? C2 C3 H3 104.2 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 121.1(3) . . ? N1 C5 C4 122.9(3) . . ? C6 C5 C4 115.9(3) . . ? C5 C6 C7 127.2(3) . . ? C5 C6 H6 116.4 . . ? C7 C6 H6 116.4 . . ? N2 C7 C6 123.0(2) . . ? N2 C7 C8 120.1(3) . . ? C6 C7 C8 116.8(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 N2 C9 116.9(2) . . ? C7 N2 Zr1 122.65(17) . . ? C9 N2 Zr1 120.36(17) . . ? C10 C9 C14 120.7(3) . . ? C10 C9 N2 119.0(3) . . ? C14 C9 N2 120.2(2) . . ? C11 C10 C9 118.2(3) . . ? C11 C10 C17 119.8(3) . . ? C9 C10 C17 121.9(3) . . ? C12 C11 C10 121.6(3) . . ? C12 C11 H12 119.2 . . ? C10 C11 H12 119.2 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H13 120.2 . . ? C11 C12 H13 120.2 . . ? C12 C13 C14 121.6(3) . . ? C12 C13 H14 119.2 . . ? C14 C13 H14 119.2 . . ? C13 C14 C9 118.2(3) . . ? C13 C14 C15 118.4(3) . . ? C9 C14 C15 123.3(3) . . ? C14 C15 H16A 109.5 . . ? C14 C15 H16B 109.5 . . ? H16A C15 H16B 109.5 . . ? C14 C15 H16C 109.5 . . ? H16A C15 H16C 109.5 . . ? H16B C15 H16C 109.5 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C1 C21 C22 113.7(3) . . ? C1 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C1 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 111.1(3) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? N3 C23 C3 107.8(2) . . ? N3 C23 C22 113.5(2) . . ? C3 C23 C22 109.9(2) . . ? N3 C23 H23 108.5 . . ? C3 C23 H23 108.5 . . ? C22 C23 H23 108.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 121.7(3) . . ? N3 C25 C24 121.4(3) . . ? C26 C25 C24 116.8(2) . . ? C25 C26 C27 127.4(3) . . ? C25 C26 H26 116.3 . . ? C27 C26 H26 116.3 . . ? N4 C27 C26 122.9(3) . . ? N4 C27 C28 120.1(3) . . ? C26 C27 C28 117.0(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 121.3(3) . . ? C34 C29 N4 121.0(3) . . ? C30 C29 N4 117.7(2) . . ? C31 C30 C29 118.0(3) . . ? C31 C30 C36 120.8(3) . . ? C29 C30 C36 121.2(3) . . ? C32 C31 C30 121.4(3) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C33 C32 C31 119.8(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 121.0(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C29 118.5(3) . . ? C33 C34 C35 119.5(3) . . ? C29 C34 C35 122.0(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C101 C100 C105 120.3(4) . . ? C101 C100 H100 119.8 . . ? C105 C100 H100 119.8 . . ? C100 C101 C102 120.0(4) . . ? C100 C101 H101 120.0 . . ? C102 C101 H101 120.0 . . ? C101 C102 C103 120.0(4) . . ? C101 C102 H102 120.0 . . ? C103 C102 H102 120.0 . . ? C104 C103 C102 119.2(4) . . ? C104 C103 H103 120.4 . . ? C102 C103 H103 120.4 . . ? C103 C104 C105 120.0(4) . . ? C103 C104 H104 120.0 . . ? C105 C104 H104 120.0 . . ? C100 C105 C104 120.5(4) . . ? C100 C105 H105 119.8 . . ? C104 C105 H105 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zr1 N1 C5 -118.5(2) . . . . ? N4 Zr1 N1 C5 -137.31(19) . . . . ? N2 Zr1 N1 C5 49.6(2) . . . . ? Cl1 Zr1 N1 C5 -30.2(2) . . . . ? Cl2 Zr1 N1 C5 136.97(19) . . . . ? N3 Zr1 N1 C3 41.45(17) . . . . ? N4 Zr1 N1 C3 22.6(3) . . . . ? N2 Zr1 N1 C3 -150.44(18) . . . . ? Cl1 Zr1 N1 C3 129.73(16) . . . . ? Cl2 Zr1 N1 C3 -63.09(17) . . . . ? N1 Zr1 N3 C25 138.9(2) . . . . ? N4 Zr1 N3 C25 -51.0(2) . . . . ? N2 Zr1 N3 C25 116.5(2) . . . . ? Cl1 Zr1 N3 C25 33.8(2) . . . . ? Cl2 Zr1 N3 C25 -130.9(2) . . . . ? N1 Zr1 N3 C23 -21.06(19) . . . . ? N4 Zr1 N3 C23 149.0(2) . . . . ? N2 Zr1 N3 C23 -43.4(3) . . . . ? Cl1 Zr1 N3 C23 -126.15(19) . . . . ? Cl2 Zr1 N3 C23 69.1(2) . . . . ? N1 Zr1 N4 C27 63.2(3) . . . . ? N3 Zr1 N4 C27 44.9(2) . . . . ? N2 Zr1 N4 C27 -126.1(2) . . . . ? Cl1 Zr1 N4 C27 -49.2(2) . . . . ? Cl2 Zr1 N4 C27 152.1(2) . . . . ? N1 Zr1 N4 C29 -118.5(2) . . . . ? N3 Zr1 N4 C29 -136.9(2) . . . . ? N2 Zr1 N4 C29 52.1(2) . . . . ? Cl1 Zr1 N4 C29 129.1(2) . . . . ? Cl2 Zr1 N4 C29 -29.68(19) . . . . ? C21 C1 C2 C3 -54.7(4) . . . . ? C5 N1 C3 C23 100.6(3) . . . . ? Zr1 N1 C3 C23 -58.4(3) . . . . ? C5 N1 C3 C2 -32.2(4) . . . . ? Zr1 N1 C3 C2 168.8(2) . . . . ? C1 C2 C3 N1 -170.7(3) . . . . ? C1 C2 C3 C23 58.6(3) . . . . ? C3 N1 C5 C6 168.6(3) . . . . ? Zr1 N1 C5 C6 -35.5(3) . . . . ? C3 N1 C5 C4 -7.9(4) . . . . ? Zr1 N1 C5 C4 148.0(2) . . . . ? N1 C5 C6 C7 -12.4(4) . . . . ? C4 C5 C6 C7 164.4(3) . . . . ? C5 C6 C7 N2 21.5(4) . . . . ? C5 C6 C7 C8 -154.7(3) . . . . ? C6 C7 N2 C9 -165.8(2) . . . . ? C8 C7 N2 C9 10.3(4) . . . . ? C6 C7 N2 Zr1 16.6(4) . . . . ? C8 C7 N2 Zr1 -167.26(19) . . . . ? N1 Zr1 N2 C7 -40.2(2) . . . . ? N3 Zr1 N2 C7 -18.4(3) . . . . ? N4 Zr1 N2 C7 144.78(19) . . . . ? Cl1 Zr1 N2 C7 67.0(2) . . . . ? Cl2 Zr1 N2 C7 -135.4(2) . . . . ? N1 Zr1 N2 C9 142.3(2) . . . . ? N3 Zr1 N2 C9 164.05(18) . . . . ? N4 Zr1 N2 C9 -32.7(2) . . . . ? Cl1 Zr1 N2 C9 -110.52(19) . . . . ? Cl2 Zr1 N2 C9 47.06(19) . . . . ? C7 N2 C9 C10 88.9(3) . . . . ? Zr1 N2 C9 C10 -93.4(3) . . . . ? C7 N2 C9 C14 -89.9(3) . . . . ? Zr1 N2 C9 C14 87.7(3) . . . . ? C14 C9 C10 C11 -5.2(4) . . . . ? N2 C9 C10 C11 175.9(3) . . . . ? C14 C9 C10 C17 171.8(3) . . . . ? N2 C9 C10 C17 -7.0(4) . . . . ? C9 C10 C11 C12 2.5(5) . . . . ? C17 C10 C11 C12 -174.6(4) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C14 -1.1(6) . . . . ? C12 C13 C14 C9 -1.6(5) . . . . ? C12 C13 C14 C15 174.2(3) . . . . ? C10 C9 C14 C13 4.8(5) . . . . ? N2 C9 C14 C13 -176.4(3) . . . . ? C10 C9 C14 C15 -170.8(3) . . . . ? N2 C9 C14 C15 8.1(4) . . . . ? C2 C1 C21 C22 53.7(4) . . . . ? C1 C21 C22 C23 -52.8(4) . . . . ? C25 N3 C23 C3 -164.3(3) . . . . ? Zr1 N3 C23 C3 -4.0(3) . . . . ? C25 N3 C23 C22 73.7(3) . . . . ? Zr1 N3 C23 C22 -125.9(2) . . . . ? N1 C3 C23 N3 39.7(3) . . . . ? C2 C3 C23 N3 176.6(2) . . . . ? N1 C3 C23 C22 163.9(2) . . . . ? C2 C3 C23 C22 -59.2(3) . . . . ? C21 C22 C23 N3 174.5(2) . . . . ? C21 C22 C23 C3 53.7(3) . . . . ? C23 N3 C25 C26 -165.7(3) . . . . ? Zr1 N3 C25 C26 34.8(4) . . . . ? C23 N3 C25 C24 14.0(4) . . . . ? Zr1 N3 C25 C24 -145.5(2) . . . . ? N3 C25 C26 C27 12.9(5) . . . . ? C24 C25 C26 C27 -166.8(3) . . . . ? C29 N4 C27 C26 159.3(3) . . . . ? Zr1 N4 C27 C26 -22.3(4) . . . . ? C29 N4 C27 C28 -19.0(4) . . . . ? Zr1 N4 C27 C28 159.4(2) . . . . ? C25 C26 C27 N4 -19.1(5) . . . . ? C25 C26 C27 C28 159.3(3) . . . . ? C27 N4 C29 C34 97.7(3) . . . . ? Zr1 N4 C29 C34 -80.6(3) . . . . ? C27 N4 C29 C30 -81.7(3) . . . . ? Zr1 N4 C29 C30 99.9(2) . . . . ? C34 C29 C30 C31 0.9(4) . . . . ? N4 C29 C30 C31 -179.6(2) . . . . ? C34 C29 C30 C36 -178.3(3) . . . . ? N4 C29 C30 C36 1.1(4) . . . . ? C29 C30 C31 C32 -1.6(4) . . . . ? C36 C30 C31 C32 177.6(3) . . . . ? C30 C31 C32 C33 1.0(5) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C32 C33 C34 C29 -1.0(4) . . . . ? C32 C33 C34 C35 -179.8(3) . . . . ? C30 C29 C34 C33 0.3(4) . . . . ? N4 C29 C34 C33 -179.1(2) . . . . ? C30 C29 C34 C35 179.1(3) . . . . ? N4 C29 C34 C35 -0.3(4) . . . . ? C105 C100 C101 C102 -0.8(6) . . . . ? C100 C101 C102 C103 1.4(7) . . . . ? C101 C102 C103 C104 -1.4(7) . . . . ? C102 C103 C104 C105 0.8(6) . . . . ? C101 C100 C105 C104 0.2(6) . . . . ? C103 C104 C105 C100 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 69.62 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.585 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.064 data_todd16 _database_code_depnum_ccdc_archive 'CCDC 894424' #TrackingRef '- Zoghbi-2012.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 N6 Zr' _chemical_formula_sum 'C36 H54 N6 Zr' _chemical_formula_weight 662.07 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.5065(3) _cell_length_b 11.7278(2) _cell_length_c 17.2506(4) _cell_angle_alpha 90 _cell_angle_beta 112.8420(10) _cell_angle_gamma 90 _cell_volume 3450.46(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 9335 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 72.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 2.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.542796 _exptl_absorpt_correction_T_max 0.701245 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 4K Charged-Coupled Device (CCD) Area Detector using the program APEX2 and a Nonius FR591 rotating anode equiped with a Montel 200 optics The crystal-to-detector distance was 5.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over four different parts of the reciprocal space (132 frames total). One complete sphere of data was collected, to better than 0.80\%A resolution. ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios multi-layers optics' _diffrn_measurement_device_type 'Bruker SMART 6000 / Nonius FR591' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 22047 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 72.56 _reflns_number_total 3393 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0491P)^2^+1.9476P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00245(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3393 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.5000 0.385688(13) 0.2500 0.02301(10) Uani 1 2 d S . . N1 N 0.46516(8) 0.23023(12) 0.30399(9) 0.0307(3) Uani 1 1 d . . . N2 N 0.37055(7) 0.42176(11) 0.24029(8) 0.0264(3) Uani 1 1 d . . . N5 N 0.54053(8) 0.46723(12) 0.36537(8) 0.0314(3) Uani 1 1 d . . . C1 C 0.49543(11) 0.11893(12) 0.29231(13) 0.0346(4) Uani 1 1 d . . . H1 H 0.5474 0.1085 0.3371 0.041 Uiso 1 1 calc R . . C3 C 0.44485(12) 0.01488(17) 0.29221(16) 0.0515(5) Uani 1 1 d . . . H3A H 0.3951 0.0191 0.2445 0.062 Uiso 1 1 calc R . . H3B H 0.4345 0.0144 0.3432 0.062 Uiso 1 1 calc R . . C4 C 0.48817(16) -0.09510(17) 0.28709(17) 0.0644(8) Uani 1 1 d . . . H4A H 0.5346 -0.1033 0.3384 0.077 Uiso 1 1 calc R . . H4B H 0.4544 -0.1601 0.2829 0.077 Uiso 1 1 calc R . . C11 C 0.44515(10) 0.24645(15) 0.37058(11) 0.0363(4) Uani 1 1 d . . . C12 C 0.39632(10) 0.33475(16) 0.37383(11) 0.0370(4) Uani 1 1 d . . . H12 H 0.3935 0.3496 0.4256 0.044 Uiso 1 1 calc R . . C13 C 0.35093(10) 0.40331(15) 0.30584(11) 0.0309(3) Uani 1 1 d . . . C14 C 0.27601(11) 0.45193(17) 0.30810(13) 0.0412(4) Uani 1 1 d . . . H14A H 0.2694 0.5290 0.2878 0.062 Uiso 1 1 calc R . . H14B H 0.2789 0.4509 0.3649 0.062 Uiso 1 1 calc R . . H14C H 0.2323 0.4067 0.2731 0.062 Uiso 1 1 calc R . . C15 C 0.47460(12) 0.1697(2) 0.44766(14) 0.0507(5) Uani 1 1 d . . . H15A H 0.5197 0.1281 0.4489 0.076 Uiso 1 1 calc R . . H15B H 0.4340 0.1171 0.4452 0.076 Uiso 1 1 calc R . . H15C H 0.4886 0.2154 0.4975 0.076 Uiso 1 1 calc R . . C30 C 0.30741(9) 0.45736(14) 0.16404(10) 0.0292(3) Uani 1 1 d . . . C31 C 0.25773(11) 0.37235(15) 0.11394(13) 0.0370(4) Uani 1 1 d . . . C32 C 0.19916(12) 0.4032(2) 0.03682(14) 0.0488(5) Uani 1 1 d . . . H32 H 0.1662 0.3474 0.0029 0.059 Uiso 1 1 calc R . . C33 C 0.18966(12) 0.5151(2) 0.01057(14) 0.0557(6) Uani 1 1 d . . . H33 H 0.1516 0.5342 -0.0416 0.067 Uiso 1 1 calc R . . C34 C 0.23657(14) 0.59863(19) 0.06159(15) 0.0497(5) Uani 1 1 d . . . H34 H 0.2287 0.6743 0.0442 0.060 Uiso 1 1 calc R . . C35 C 0.29595(10) 0.57155(16) 0.13922(11) 0.0363(4) Uani 1 1 d . . . C36 C 0.26734(13) 0.24933(17) 0.14096(14) 0.0490(5) Uani 1 1 d . . . H36A H 0.3204 0.2257 0.1534 0.074 Uiso 1 1 calc R . . H36B H 0.2321 0.2030 0.0964 0.074 Uiso 1 1 calc R . . H36C H 0.2557 0.2408 0.1902 0.074 Uiso 1 1 calc R . . C37 C 0.34523(13) 0.66480(16) 0.19412(14) 0.0476(5) Uani 1 1 d . . . H37A H 0.3260 0.7375 0.1689 0.071 Uiso 1 1 calc R . . H37B H 0.3987 0.6555 0.2001 0.071 Uiso 1 1 calc R . . H37C H 0.3425 0.6610 0.2485 0.071 Uiso 1 1 calc R . . C50 C 0.51765(13) 0.57804(19) 0.38416(14) 0.0499(5) Uani 1 1 d . . . H50A H 0.4881 0.6171 0.3326 0.075 Uiso 1 1 calc R . . H50B H 0.5636 0.6215 0.4158 0.075 Uiso 1 1 calc R . . H50C H 0.4860 0.5693 0.4166 0.075 Uiso 1 1 calc R . . C51 C 0.59225(12) 0.4111(2) 0.44171(12) 0.0452(4) Uani 1 1 d . . . H51A H 0.6077 0.3383 0.4279 0.068 Uiso 1 1 calc R . . H51B H 0.5653 0.4007 0.4789 0.068 Uiso 1 1 calc R . . H51C H 0.6380 0.4573 0.4689 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02175(12) 0.02208(13) 0.02611(13) 0.000 0.01029(8) 0.000 N1 0.0277(6) 0.0251(7) 0.0409(7) 0.0071(5) 0.0152(6) 0.0008(5) N2 0.0225(6) 0.0258(6) 0.0317(7) -0.0005(5) 0.0114(5) 0.0009(5) N5 0.0284(7) 0.0388(8) 0.0281(6) -0.0047(5) 0.0120(5) -0.0023(5) C1 0.0261(8) 0.0240(8) 0.0469(11) 0.0052(6) 0.0068(8) -0.0008(5) C3 0.0424(10) 0.0328(10) 0.0663(13) 0.0126(9) 0.0070(9) -0.0110(8) C4 0.0598(14) 0.0255(9) 0.0742(16) 0.0108(9) -0.0108(12) -0.0077(9) C11 0.0301(8) 0.0395(9) 0.0407(9) 0.0112(7) 0.0151(7) -0.0030(7) C12 0.0358(9) 0.0454(10) 0.0357(8) 0.0053(7) 0.0204(7) -0.0006(7) C13 0.0273(8) 0.0322(8) 0.0366(9) -0.0038(6) 0.0160(7) -0.0019(6) C14 0.0377(9) 0.0434(10) 0.0518(10) -0.0015(8) 0.0274(8) 0.0044(8) C15 0.0444(11) 0.0584(13) 0.0524(11) 0.0232(10) 0.0221(9) 0.0055(9) C30 0.0229(7) 0.0320(8) 0.0330(8) -0.0016(6) 0.0112(6) 0.0033(6) C31 0.0280(9) 0.0407(10) 0.0418(10) -0.0063(7) 0.0129(8) -0.0024(7) C32 0.0289(9) 0.0616(13) 0.0465(11) -0.0114(9) 0.0043(9) -0.0032(8) C33 0.0352(10) 0.0742(15) 0.0443(11) 0.0025(10) 0.0008(8) 0.0121(10) C34 0.0438(11) 0.0481(11) 0.0522(12) 0.0120(9) 0.0132(10) 0.0178(9) C35 0.0336(8) 0.0334(9) 0.0410(9) 0.0005(7) 0.0136(7) 0.0065(7) C36 0.0503(11) 0.0375(10) 0.0585(12) -0.0112(9) 0.0202(10) -0.0140(8) C37 0.0564(12) 0.0280(9) 0.0561(11) -0.0014(8) 0.0193(10) 0.0011(8) C50 0.0481(11) 0.0499(12) 0.0518(11) -0.0190(10) 0.0193(9) -0.0022(9) C51 0.0332(9) 0.0674(12) 0.0322(9) 0.0074(9) 0.0097(8) -0.0029(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N5 2.0685(13) 2_655 ? Zr1 N5 2.0685(13) . ? Zr1 N1 2.2524(13) 2_655 ? Zr1 N1 2.2524(13) . ? Zr1 N2 2.3737(12) . ? Zr1 N2 2.3737(12) 2_655 ? N1 C11 1.350(2) . ? N1 C1 1.465(2) . ? N2 C13 1.333(2) . ? N2 C30 1.441(2) . ? N5 C50 1.442(2) . ? N5 C51 1.451(2) . ? C1 C1 1.533(4) 2_655 ? C1 C3 1.537(2) . ? C1 H1 0.9800 . ? C3 C4 1.539(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C4 1.505(7) 2_655 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C11 C12 1.390(3) . ? C11 C15 1.521(2) . ? C12 C13 1.401(3) . ? C12 H12 0.9300 . ? C13 C14 1.514(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C30 C35 1.397(2) . ? C30 C31 1.403(2) . ? C31 C32 1.398(3) . ? C31 C36 1.505(3) . ? C32 C33 1.377(3) . ? C32 H32 0.9300 . ? C33 C34 1.377(3) . ? C33 H33 0.9300 . ? C34 C35 1.400(3) . ? C34 H34 0.9300 . ? C35 C37 1.501(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? 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 N5 124.93(8) 2_655 . ? N5 Zr1 N1 91.80(5) 2_655 2_655 ? N5 Zr1 N1 135.80(5) . 2_655 ? N5 Zr1 N1 135.80(5) 2_655 . ? N5 Zr1 N1 91.80(5) . . ? N1 Zr1 N1 71.92(7) 2_655 . ? N5 Zr1 N2 82.57(5) 2_655 . ? N5 Zr1 N2 87.97(5) . . ? N1 Zr1 N2 123.93(5) 2_655 . ? N1 Zr1 N2 74.36(5) . . ? N5 Zr1 N2 87.97(5) 2_655 2_655 ? N5 Zr1 N2 82.57(5) . 2_655 ? N1 Zr1 N2 74.36(5) 2_655 2_655 ? N1 Zr1 N2 123.93(5) . 2_655 ? N2 Zr1 N2 159.47(7) . 2_655 ? C11 N1 C1 119.23(14) . . ? C11 N1 Zr1 117.06(11) . . ? C1 N1 Zr1 118.57(11) . . ? C13 N2 C30 115.47(13) . . ? C13 N2 Zr1 120.74(11) . . ? C30 N2 Zr1 123.68(10) . . ? C50 N5 C51 110.64(16) . . ? C50 N5 Zr1 127.19(12) . . ? C51 N5 Zr1 121.92(13) . . ? N1 C1 C1 108.68(11) . 2_655 ? N1 C1 C3 116.25(17) . . ? C1 C1 C3 106.92(15) 2_655 . ? N1 C1 H1 108.3 . . ? C1 C1 H1 108.3 2_655 . ? C3 C1 H1 108.3 . . ? C1 C3 C4 109.55(18) . . ? C1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C4 C4 C3 112.26(16) 2_655 . ? C4 C4 H4A 109.2 2_655 . ? C3 C4 H4A 109.2 . . ? C4 C4 H4B 109.2 2_655 . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C11 C12 122.46(15) . . ? N1 C11 C15 122.47(17) . . ? C12 C11 C15 115.07(17) . . ? C11 C12 C13 125.57(16) . . ? C11 C12 H12 117.2 . . ? C13 C12 H12 117.2 . . ? N2 C13 C12 122.09(15) . . ? N2 C13 C14 120.98(16) . . ? C12 C13 C14 116.88(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C35 C30 C31 120.47(16) . . ? C35 C30 N2 122.03(15) . . ? C31 C30 N2 117.48(15) . . ? C32 C31 C30 118.86(18) . . ? C32 C31 C36 119.81(18) . . ? C30 C31 C36 121.32(17) . . ? C33 C32 C31 120.79(19) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.99(19) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.1(2) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C30 C35 C34 118.70(18) . . ? C30 C35 C37 121.48(16) . . ? C34 C35 C37 119.82(18) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C50 H50A 109.5 . . ? N5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C11 -120.01(12) 2_655 . . . ? N5 Zr1 N1 C11 28.65(12) . . . . ? N1 Zr1 N1 C11 166.74(15) 2_655 . . . ? N2 Zr1 N1 C11 -58.74(12) . . . . ? N2 Zr1 N1 C11 110.90(12) 2_655 . . . ? N5 Zr1 N1 C1 85.50(14) 2_655 . . . ? N5 Zr1 N1 C1 -125.84(13) . . . . ? N1 Zr1 N1 C1 12.25(9) 2_655 . . . ? N2 Zr1 N1 C1 146.77(13) . . . . ? N2 Zr1 N1 C1 -43.59(14) 2_655 . . . ? N5 Zr1 N2 C13 -170.68(13) 2_655 . . . ? N5 Zr1 N2 C13 -45.06(13) . . . . ? N1 Zr1 N2 C13 102.16(13) 2_655 . . . ? N1 Zr1 N2 C13 47.38(12) . . . . ? N2 Zr1 N2 C13 -107.44(12) 2_655 . . . ? N5 Zr1 N2 C30 13.27(12) 2_655 . . . ? N5 Zr1 N2 C30 138.89(12) . . . . ? N1 Zr1 N2 C30 -73.89(13) 2_655 . . . ? N1 Zr1 N2 C30 -128.67(13) . . . . ? N2 Zr1 N2 C30 76.51(12) 2_655 . . . ? N5 Zr1 N5 C50 28.35(14) 2_655 . . . ? N1 Zr1 N5 C50 169.00(14) 2_655 . . . ? N1 Zr1 N5 C50 -125.40(15) . . . . ? N2 Zr1 N5 C50 -51.12(15) . . . . ? N2 Zr1 N5 C50 110.61(16) 2_655 . . . ? N5 Zr1 N5 C51 -158.02(14) 2_655 . . . ? N1 Zr1 N5 C51 -17.38(17) 2_655 . . . ? N1 Zr1 N5 C51 48.23(14) . . . . ? N2 Zr1 N5 C51 122.50(14) . . . . ? N2 Zr1 N5 C51 -75.76(13) 2_655 . . . ? C11 N1 C1 C1 173.61(17) . . . 2_655 ? Zr1 N1 C1 C1 -32.5(2) . . . 2_655 ? C11 N1 C1 C3 53.0(2) . . . . ? Zr1 N1 C1 C3 -153.08(14) . . . . ? N1 C1 C3 C4 -175.10(18) . . . . ? C1 C1 C3 C4 63.3(2) 2_655 . . . ? C1 C3 C4 C4 -54.7(3) . . . 2_655 ? C1 N1 C11 C12 -161.14(17) . . . . ? Zr1 N1 C11 C12 44.5(2) . . . . ? C1 N1 C11 C15 19.1(2) . . . . ? Zr1 N1 C11 C15 -135.24(15) . . . . ? N1 C11 C12 C13 12.4(3) . . . . ? C15 C11 C12 C13 -167.80(18) . . . . ? C30 N2 C13 C12 158.61(16) . . . . ? Zr1 N2 C13 C12 -17.8(2) . . . . ? C30 N2 C13 C14 -18.7(2) . . . . ? Zr1 N2 C13 C14 164.98(13) . . . . ? C11 C12 C13 N2 -26.3(3) . . . . ? C11 C12 C13 C14 151.11(18) . . . . ? C13 N2 C30 C35 99.67(19) . . . . ? Zr1 N2 C30 C35 -84.09(17) . . . . ? C13 N2 C30 C31 -81.35(19) . . . . ? Zr1 N2 C30 C31 94.89(16) . . . . ? C35 C30 C31 C32 3.2(3) . . . . ? N2 C30 C31 C32 -175.78(17) . . . . ? C35 C30 C31 C36 -177.88(18) . . . . ? N2 C30 C31 C36 3.1(3) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C36 C31 C32 C33 -179.5(2) . . . . ? C31 C32 C33 C34 -2.0(4) . . . . ? C32 C33 C34 C35 2.0(4) . . . . ? C31 C30 C35 C34 -3.2(3) . . . . ? N2 C30 C35 C34 175.78(17) . . . . ? C31 C30 C35 C37 176.29(18) . . . . ? N2 C30 C35 C37 -4.8(3) . . . . ? C33 C34 C35 C30 0.5(3) . . . . ? C33 C34 C35 C37 -178.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 72.56 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.356 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.079 data_todd12 _database_code_depnum_ccdc_archive 'CCDC 894425' #TrackingRef '- Zoghbi-2012.cif' _vrf_PLAT230_todd12 ; RESPONSE No restraints were applied to this atom. A slightly shorter than expected O-C distance indicates a slight disorder of the second OEt group, which was not resolved. ; _vrf_PLAT041_todd12 ; RESPONSE Probable bug. There is no difference in the calculated and reported sum formula. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H52 N4 O2 Zr' _chemical_formula_sum 'C36 H52 N4 O2 Zr' _chemical_formula_weight 664.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9326(11) _cell_length_b 11.2187(12) _cell_length_c 16.3787(16) _cell_angle_alpha 82.459(5) _cell_angle_beta 71.522(5) _cell_angle_gamma 65.213(5) _cell_volume 1729.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 9792 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 69.44 _exptl_crystal_description block _exptl_crystal_colour colorless-yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios multi-layers optics' _diffrn_measurement_device_type 'Bruker SMART 6000 / Nonius FR591' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 5.5 _diffrn_reflns_number 66389 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 69.75 _reflns_number_total 6426 _reflns_number_gt 6000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0692P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6426 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.420589(17) 0.756182(16) 0.252032(11) 0.02546(9) Uani 1 1 d . A . N4 N 0.21977(19) 0.94909(18) 0.30055(13) 0.0293(4) Uani 1 1 d . . . N3 N 0.31563(19) 0.71247(18) 0.38580(12) 0.0282(4) Uani 1 1 d . . . N1 N 0.41951(19) 0.55569(17) 0.25128(12) 0.0281(4) Uani 1 1 d . . . N2 N 0.64515(19) 0.63148(18) 0.16952(12) 0.0275(4) Uani 1 1 d . . . O1 O 0.52156(18) 0.83340(18) 0.29046(12) 0.0383(4) Uani 1 1 d . . . O2 O 0.37355(18) 0.80923(16) 0.14443(11) 0.0366(4) Uani 1 1 d . . . C1 C 0.2568(3) 0.3491(3) 0.42263(19) 0.0481(7) Uani 1 1 d . . . H1A H 0.1708 0.3759 0.4067 0.058 Uiso 1 1 calc R . . H1B H 0.2877 0.2564 0.4366 0.058 Uiso 1 1 calc R . . C2 C 0.3702(3) 0.3699(2) 0.34566(17) 0.0380(5) Uani 1 1 d . . . H2A H 0.3806 0.3255 0.2954 0.046 Uiso 1 1 calc R . . H2B H 0.4598 0.3331 0.3583 0.046 Uiso 1 1 calc R . . C3 C 0.3274(2) 0.5183(2) 0.32722(15) 0.0293(5) Uani 1 1 d . . . H3 H 0.2323 0.5549 0.3208 0.035 Uiso 1 1 calc R . . C4 C 0.3782(3) 0.4281(3) 0.15544(18) 0.0399(6) Uani 1 1 d . . . H4A H 0.4320 0.3352 0.1573 0.060 Uiso 1 1 calc R . . H4B H 0.3657 0.4520 0.0993 0.060 Uiso 1 1 calc R . . H4C H 0.2879 0.4510 0.1977 0.060 Uiso 1 1 calc R . . C5 C 0.4562(2) 0.5011(2) 0.17458(15) 0.0295(5) Uani 1 1 d . . . C6 C 0.5684(2) 0.5059(2) 0.10592(16) 0.0321(5) Uani 1 1 d . . . H6 H 0.5774 0.4765 0.0529 0.038 Uiso 1 1 calc R . . C7 C 0.6698(2) 0.5506(2) 0.10862(14) 0.0282(5) Uani 1 1 d . . . C8 C 0.8098(3) 0.4999(2) 0.04008(16) 0.0364(5) Uani 1 1 d . . . H8A H 0.8287 0.5727 0.0101 0.055 Uiso 1 1 calc R . . H8B H 0.8071 0.4463 0.0002 0.055 Uiso 1 1 calc R . . H8C H 0.8828 0.4486 0.0664 0.055 Uiso 1 1 calc R . . C9 C 0.7660(2) 0.6485(2) 0.17516(15) 0.0286(5) Uani 1 1 d . . . C10 C 0.8448(2) 0.5623(2) 0.22752(16) 0.0336(5) Uani 1 1 d . . . C11 C 0.9628(3) 0.5777(3) 0.23162(18) 0.0428(6) Uani 1 1 d . . . H11 H 1.0165 0.5214 0.2660 0.051 Uiso 1 1 calc R . . C12 C 1.0015(3) 0.6751(3) 0.18553(19) 0.0458(6) Uani 1 1 d . . . H12 H 1.0824 0.6820 0.1874 0.055 Uiso 1 1 calc R . . C13 C 0.9199(3) 0.7621(3) 0.13673(18) 0.0428(6) Uani 1 1 d . . . H13 H 0.9447 0.8292 0.1074 0.051 Uiso 1 1 calc R . . C14 C 0.8005(2) 0.7506(2) 0.13085(16) 0.0347(5) Uani 1 1 d . . . C15 C 0.7093(3) 0.8486(3) 0.08018(19) 0.0445(6) Uani 1 1 d . . . H15A H 0.6214 0.9030 0.1190 0.067 Uiso 1 1 calc R . . H15B H 0.6919 0.8031 0.0423 0.067 Uiso 1 1 calc R . . H15C H 0.7563 0.9025 0.0469 0.067 Uiso 1 1 calc R . . C16 C 0.8016(3) 0.4583(3) 0.27834(18) 0.0436(6) Uani 1 1 d . . . H16A H 0.7129 0.4987 0.3212 0.065 Uiso 1 1 calc R . . H16B H 0.8716 0.4033 0.3059 0.065 Uiso 1 1 calc R . . H16C H 0.7924 0.4060 0.2405 0.065 Uiso 1 1 calc R . . C21 C 0.2258(3) 0.4259(3) 0.50195(19) 0.0475(6) Uani 1 1 d . . . H21A H 0.3053 0.3872 0.5253 0.057 Uiso 1 1 calc R . . H21B H 0.1443 0.4202 0.5456 0.057 Uiso 1 1 calc R . . C22 C 0.1975(3) 0.5704(2) 0.48064(17) 0.0385(5) Uani 1 1 d . . . H22A H 0.1856 0.6154 0.5311 0.046 Uiso 1 1 calc R . . H22B H 0.1115 0.6124 0.4638 0.046 Uiso 1 1 calc R . . C23 C 0.3214(2) 0.5795(2) 0.40705(15) 0.0302(5) Uani 1 1 d . . . H23 H 0.4084 0.5271 0.4226 0.036 Uiso 1 1 calc R . . C24 C 0.3401(3) 0.7331(3) 0.52966(17) 0.0391(5) Uani 1 1 d . . . H24A H 0.2562 0.7466 0.5766 0.059 Uiso 1 1 calc R . . H24B H 0.3918 0.7761 0.5421 0.059 Uiso 1 1 calc R . . H24C H 0.3974 0.6407 0.5221 0.059 Uiso 1 1 calc R . . C25 C 0.3002(2) 0.7897(2) 0.44787(15) 0.0299(5) Uani 1 1 d . . . C26 C 0.2495(2) 0.9254(2) 0.44076(16) 0.0322(5) Uani 1 1 d . . . H26 H 0.2569 0.9710 0.4812 0.039 Uiso 1 1 calc R . . C27 C 0.1876(2) 0.9994(2) 0.37716(16) 0.0304(5) Uani 1 1 d . . . C28 C 0.0786(3) 1.1363(2) 0.40169(18) 0.0379(5) Uani 1 1 d . . . H28A H 0.0868 1.1935 0.3531 0.057 Uiso 1 1 calc R . . H28B H 0.0930 1.1670 0.4484 0.057 Uiso 1 1 calc R . . H28C H -0.0137 1.1356 0.4191 0.057 Uiso 1 1 calc R . . C29 C 0.1263(2) 1.0202(2) 0.24924(16) 0.0306(5) Uani 1 1 d . . . C30 C 0.0062(2) 0.9954(2) 0.26193(17) 0.0347(5) Uani 1 1 d . . . C31 C -0.0837(3) 1.0620(3) 0.2115(2) 0.0450(6) Uani 1 1 d . . . H31 H -0.1635 1.0460 0.2192 0.054 Uiso 1 1 calc R . . C32 C -0.0556(3) 1.1513(3) 0.1502(2) 0.0478(7) Uani 1 1 d . . . H32 H -0.1161 1.1952 0.1168 0.057 Uiso 1 1 calc R . . C33 C 0.0630(3) 1.1754(3) 0.13855(19) 0.0434(6) Uani 1 1 d . . . H33 H 0.0809 1.2363 0.0975 0.052 Uiso 1 1 calc R . . C34 C 0.1563(3) 1.1101(2) 0.18700(16) 0.0346(5) Uani 1 1 d . . . C35 C 0.2844(3) 1.1380(3) 0.17411(19) 0.0432(6) Uani 1 1 d . . . H35A H 0.2762 1.1772 0.2253 0.065 Uiso 1 1 calc R . . H35B H 0.2916 1.1972 0.1266 0.065 Uiso 1 1 calc R . . H35C H 0.3671 1.0574 0.1622 0.065 Uiso 1 1 calc R . . C36 C -0.0257(3) 0.8995(3) 0.33007(18) 0.0430(6) Uani 1 1 d . . . H36A H -0.1070 0.8890 0.3272 0.065 Uiso 1 1 calc R . . H36B H -0.0439 0.9323 0.3859 0.065 Uiso 1 1 calc R . . H36C H 0.0535 0.8162 0.3205 0.065 Uiso 1 1 calc R . . C51 C 0.3846(3) 0.8319(3) 0.05681(18) 0.0435(6) Uani 1 1 d . A . H51A H 0.4728 0.7675 0.0230 0.052 Uiso 1 1 calc R . . H51B H 0.3851 0.9183 0.0416 0.052 Uiso 1 1 calc R . . C52 C 0.2643(3) 0.8235(3) 0.0361(2) 0.0520(7) Uani 1 1 d . . . H52A H 0.2655 0.7372 0.0495 0.078 Uiso 1 1 calc R A . H52B H 0.2733 0.8407 -0.0241 0.078 Uiso 1 1 calc R . . H52C H 0.1770 0.8873 0.0695 0.078 Uiso 1 1 calc R . . C41A C 0.5925(4) 0.8679(5) 0.3353(3) 0.0373(12) Uani 0.731(10) 1 d P A 1 H41A H 0.6934 0.8198 0.3124 0.045 Uiso 0.731(10) 1 calc PR A 1 H41B H 0.5645 0.8463 0.3958 0.045 Uiso 0.731(10) 1 calc PR A 1 C42A C 0.5549(4) 1.0129(5) 0.3249(4) 0.0589(16) Uani 0.731(10) 1 d P A 1 H42A H 0.5780 1.0340 0.2647 0.088 Uiso 0.731(10) 1 calc PR A 1 H42B H 0.6068 1.0376 0.3520 0.088 Uiso 0.731(10) 1 calc PR A 1 H42C H 0.4558 1.0598 0.3512 0.088 Uiso 0.731(10) 1 calc PR A 1 C41B C 0.5462(15) 0.9434(15) 0.3082(9) 0.049(4) Uani 0.269(10) 1 d P A 2 H41C H 0.4589 1.0212 0.3229 0.059 Uiso 0.269(10) 1 calc PR A 2 H41D H 0.6124 0.9627 0.2587 0.059 Uiso 0.269(10) 1 calc PR A 2 C42B C 0.6048(14) 0.9000(15) 0.3818(11) 0.068(5) Uani 0.269(10) 1 d P A 2 H42D H 0.5383 0.8801 0.4296 0.102 Uiso 0.269(10) 1 calc PR A 2 H42E H 0.6234 0.9687 0.3977 0.102 Uiso 0.269(10) 1 calc PR A 2 H42F H 0.6909 0.8230 0.3658 0.102 Uiso 0.269(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02222(12) 0.02501(12) 0.02713(14) -0.00259(8) -0.00422(9) -0.00898(8) N4 0.0254(9) 0.0269(9) 0.0322(11) -0.0024(8) -0.0039(8) -0.0098(8) N3 0.0265(9) 0.0272(9) 0.0289(10) -0.0002(7) -0.0060(8) -0.0103(7) N1 0.0252(9) 0.0272(9) 0.0329(10) -0.0015(7) -0.0077(8) -0.0113(7) N2 0.0247(9) 0.0276(9) 0.0303(10) 0.0000(8) -0.0077(8) -0.0109(7) O1 0.0302(8) 0.0428(9) 0.0408(10) -0.0137(8) 0.0007(7) -0.0177(7) O2 0.0378(9) 0.0337(8) 0.0277(9) -0.0038(7) -0.0082(7) -0.0044(7) C1 0.0551(17) 0.0389(14) 0.0525(17) 0.0053(12) -0.0079(14) -0.0280(13) C2 0.0432(14) 0.0308(12) 0.0403(14) 0.0001(10) -0.0106(12) -0.0163(11) C3 0.0266(11) 0.0274(11) 0.0339(13) 0.0003(9) -0.0074(9) -0.0119(9) C4 0.0420(14) 0.0468(14) 0.0410(15) -0.0040(11) -0.0141(12) -0.0246(12) C5 0.0293(11) 0.0280(11) 0.0324(12) -0.0039(9) -0.0109(10) -0.0101(9) C6 0.0331(12) 0.0334(12) 0.0305(13) -0.0043(9) -0.0103(10) -0.0121(10) C7 0.0268(11) 0.0283(11) 0.0245(11) -0.0020(9) -0.0053(9) -0.0072(9) C8 0.0311(12) 0.0393(13) 0.0344(13) -0.0054(10) -0.0054(10) -0.0114(10) C9 0.0215(10) 0.0324(11) 0.0287(12) -0.0051(9) -0.0028(9) -0.0096(9) C10 0.0275(11) 0.0384(12) 0.0287(12) -0.0064(10) -0.0033(10) -0.0089(10) C11 0.0308(12) 0.0571(16) 0.0394(15) -0.0053(12) -0.0131(11) -0.0130(12) C12 0.0295(12) 0.0649(17) 0.0463(16) -0.0156(13) -0.0033(11) -0.0230(12) C13 0.0356(13) 0.0461(14) 0.0459(16) -0.0093(12) 0.0019(12) -0.0229(12) C14 0.0278(11) 0.0371(12) 0.0343(13) -0.0048(10) -0.0008(10) -0.0131(10) C15 0.0395(14) 0.0402(14) 0.0457(16) 0.0080(12) -0.0046(12) -0.0162(11) C16 0.0412(14) 0.0427(14) 0.0432(16) 0.0078(12) -0.0151(12) -0.0136(12) C21 0.0540(16) 0.0413(14) 0.0423(16) 0.0037(12) -0.0010(13) -0.0250(13) C22 0.0377(13) 0.0367(13) 0.0361(14) 0.0004(10) -0.0025(11) -0.0165(11) C23 0.0265(11) 0.0268(11) 0.0352(13) 0.0014(9) -0.0074(9) -0.0101(9) C24 0.0373(13) 0.0465(14) 0.0319(13) -0.0032(11) -0.0089(11) -0.0152(11) C25 0.0226(10) 0.0363(12) 0.0281(12) -0.0045(9) -0.0024(9) -0.0118(9) C26 0.0279(11) 0.0359(12) 0.0328(13) -0.0065(9) -0.0035(10) -0.0147(10) C27 0.0250(11) 0.0298(11) 0.0352(13) -0.0057(9) -0.0021(10) -0.0131(9) C28 0.0329(12) 0.0320(12) 0.0430(15) -0.0108(10) -0.0031(11) -0.0102(10) C29 0.0268(11) 0.0258(10) 0.0341(13) -0.0044(9) -0.0060(10) -0.0064(9) C30 0.0282(11) 0.0341(12) 0.0375(14) -0.0079(10) -0.0047(10) -0.0097(10) C31 0.0308(13) 0.0461(14) 0.0577(18) -0.0088(13) -0.0135(12) -0.0119(11) C32 0.0394(14) 0.0428(14) 0.0559(18) -0.0018(13) -0.0221(13) -0.0050(12) C33 0.0425(14) 0.0330(12) 0.0476(16) 0.0040(11) -0.0143(12) -0.0087(11) C34 0.0318(12) 0.0289(11) 0.0374(14) -0.0038(10) -0.0061(10) -0.0085(10) C35 0.0412(14) 0.0364(13) 0.0518(17) 0.0062(11) -0.0114(12) -0.0189(11) C36 0.0373(13) 0.0486(15) 0.0470(16) -0.0028(12) -0.0067(12) -0.0241(12) C51 0.0429(14) 0.0425(14) 0.0431(15) 0.0057(12) -0.0156(12) -0.0146(12) C52 0.0569(18) 0.0536(17) 0.0495(18) -0.0057(13) -0.0183(15) -0.0221(14) C41A 0.0298(18) 0.037(2) 0.047(2) -0.0141(19) -0.0088(17) -0.0137(17) C42A 0.043(2) 0.046(3) 0.091(4) -0.021(2) -0.009(2) -0.0226(19) C41B 0.053(7) 0.040(7) 0.056(7) -0.022(6) 0.012(6) -0.034(6) C42B 0.050(7) 0.080(10) 0.085(12) -0.022(8) -0.012(7) -0.037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O1 1.9366(17) . ? Zr1 O2 1.9410(16) . ? Zr1 N3 2.2257(19) . ? Zr1 N1 2.2559(18) . ? Zr1 N2 2.3074(19) . ? Zr1 N4 2.3445(19) . ? N4 C27 1.326(3) . ? N4 C29 1.439(3) . ? N3 C25 1.346(3) . ? N3 C23 1.466(3) . ? N1 C5 1.338(3) . ? N1 C3 1.470(3) . ? N2 C7 1.324(3) . ? N2 C9 1.444(3) . ? O1 C41A 1.406(4) . ? O1 C41B 1.450(12) . ? O2 C51 1.400(3) . ? C1 C21 1.521(4) . ? C1 C2 1.534(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.544(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C23 1.527(3) . ? C3 H3 0.9800 . ? C4 C5 1.523(3) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.392(3) . ? C6 C7 1.409(3) . ? C6 H6 0.9300 . ? C7 C8 1.508(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C14 1.397(3) . ? C9 C10 1.402(3) . ? C10 C11 1.394(3) . ? C10 C16 1.496(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C13 C14 1.398(3) . ? C13 H13 0.9300 . ? C14 C15 1.503(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 C22 1.530(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.532(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23 0.9800 . ? C24 C25 1.517(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.388(3) . ? C26 C27 1.407(3) . ? C26 H26 0.9300 . ? C27 C28 1.505(3) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.400(3) . ? C29 C34 1.400(3) . ? C30 C31 1.395(4) . ? C30 C36 1.509(4) . ? C31 C32 1.381(4) . ? C31 H31 0.9300 . ? C32 C33 1.383(4) . ? C32 H32 0.9300 . ? C33 C34 1.392(4) . ? C33 H33 0.9300 . ? C34 C35 1.506(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C51 C52 1.500(4) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C41A C42A 1.503(7) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A H42A 0.9600 . ? C42A H42B 0.9600 . ? C42A H42C 0.9600 . ? C41B C42B 1.47(2) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B H42D 0.9600 . ? C42B H42E 0.9600 . ? C42B H42F 0.9600 . ? 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 O1 Zr1 O2 121.13(8) . . ? O1 Zr1 N3 92.79(7) . . ? O2 Zr1 N3 137.31(7) . . ? O1 Zr1 N1 137.25(7) . . ? O2 Zr1 N1 93.94(7) . . ? N3 Zr1 N1 72.32(7) . . ? O1 Zr1 N2 81.77(7) . . ? O2 Zr1 N2 86.57(7) . . ? N3 Zr1 N2 126.33(7) . . ? N1 Zr1 N2 76.41(7) . . ? O1 Zr1 N4 86.66(7) . . ? O2 Zr1 N4 81.65(7) . . ? N3 Zr1 N4 74.82(7) . . ? N1 Zr1 N4 124.88(6) . . ? N2 Zr1 N4 156.14(7) . . ? C27 N4 C29 116.40(19) . . ? C27 N4 Zr1 121.11(15) . . ? C29 N4 Zr1 122.48(14) . . ? C25 N3 C23 119.72(19) . . ? C25 N3 Zr1 115.94(14) . . ? C23 N3 Zr1 119.21(14) . . ? C5 N1 C3 120.33(18) . . ? C5 N1 Zr1 117.36(14) . . ? C3 N1 Zr1 117.39(14) . . ? C7 N2 C9 115.94(19) . . ? C7 N2 Zr1 122.47(14) . . ? C9 N2 Zr1 121.25(14) . . ? C41A O1 Zr1 165.9(2) . . ? C41B O1 Zr1 153.3(7) . . ? C51 O2 Zr1 162.39(16) . . ? C21 C1 C2 112.7(2) . . ? C21 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? C21 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C1 C2 C3 109.5(2) . . ? C1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C23 108.77(17) . . ? N1 C3 C2 116.81(19) . . ? C23 C3 C2 106.50(18) . . ? N1 C3 H3 108.2 . . ? C23 C3 H3 108.2 . . ? C2 C3 H3 108.2 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C5 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C6 123.1(2) . . ? N1 C5 C4 122.5(2) . . ? C6 C5 C4 114.4(2) . . ? C5 C6 C7 126.5(2) . . ? C5 C6 H6 116.7 . . ? C7 C6 H6 116.7 . . ? N2 C7 C6 121.8(2) . . ? N2 C7 C8 121.1(2) . . ? C6 C7 C8 117.1(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 121.3(2) . . ? C14 C9 N2 120.3(2) . . ? C10 C9 N2 118.3(2) . . ? C11 C10 C9 118.2(2) . . ? C11 C10 C16 121.3(2) . . ? C9 C10 C16 120.6(2) . . ? C12 C11 C10 121.2(2) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 118.5(2) . . ? C9 C14 C15 121.0(2) . . ? C13 C14 C15 120.5(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C21 C22 111.5(2) . . ? C1 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C1 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 109.5(2) . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N3 C23 C3 108.78(18) . . ? N3 C23 C22 115.46(19) . . ? C3 C23 C22 107.70(19) . . ? N3 C23 H23 108.2 . . ? C3 C23 H23 108.2 . . ? C22 C23 H23 108.2 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C26 122.5(2) . . ? N3 C25 C24 121.8(2) . . ? C26 C25 C24 115.7(2) . . ? C25 C26 C27 125.1(2) . . ? C25 C26 H26 117.4 . . ? C27 C26 H26 117.4 . . ? N4 C27 C26 121.6(2) . . ? N4 C27 C28 121.6(2) . . ? C26 C27 C28 116.8(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C34 120.9(2) . . ? C30 C29 N4 118.4(2) . . ? C34 C29 N4 120.7(2) . . ? C31 C30 C29 118.9(2) . . ? C31 C30 C36 120.8(2) . . ? C29 C30 C36 120.3(2) . . ? C32 C31 C30 120.7(2) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 121.3(2) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C29 118.4(2) . . ? C33 C34 C35 120.8(2) . . ? C29 C34 C35 120.9(2) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 C51 C52 111.0(2) . . ? O2 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? O2 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O1 C41A C42A 108.1(4) . . ? O1 C41A H41A 110.1 . . ? C42A C41A H41A 110.1 . . ? O1 C41A H41B 110.1 . . ? C42A C41A H41B 110.1 . . ? H41A C41A H41B 108.4 . . ? O1 C41B C42B 104.5(12) . . ? O1 C41B H41C 110.8 . . ? C42B C41B H41C 110.8 . . ? O1 C41B H41D 110.8 . . ? C42B C41B H41D 110.8 . . ? H41C C41B H41D 108.9 . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zr1 N4 C27 -46.66(17) . . . . ? O2 Zr1 N4 C27 -168.79(17) . . . . ? N3 Zr1 N4 C27 47.15(16) . . . . ? N1 Zr1 N4 C27 102.21(17) . . . . ? N2 Zr1 N4 C27 -107.6(2) . . . . ? O1 Zr1 N4 C29 132.42(17) . . . . ? O2 Zr1 N4 C29 10.28(16) . . . . ? N3 Zr1 N4 C29 -133.77(17) . . . . ? N1 Zr1 N4 C29 -78.71(18) . . . . ? N2 Zr1 N4 C29 71.5(2) . . . . ? O1 Zr1 N3 C25 25.78(16) . . . . ? O2 Zr1 N3 C25 -118.92(16) . . . . ? N1 Zr1 N3 C25 164.91(17) . . . . ? N2 Zr1 N3 C25 107.62(16) . . . . ? N4 Zr1 N3 C25 -59.99(16) . . . . ? O1 Zr1 N3 C23 -128.84(16) . . . . ? O2 Zr1 N3 C23 86.45(17) . . . . ? N1 Zr1 N3 C23 10.28(14) . . . . ? N2 Zr1 N3 C23 -47.00(18) . . . . ? N4 Zr1 N3 C23 145.39(16) . . . . ? O1 Zr1 N1 C5 -116.37(16) . . . . ? O2 Zr1 N1 C5 30.56(16) . . . . ? N3 Zr1 N1 C5 169.26(17) . . . . ? N2 Zr1 N1 C5 -54.95(15) . . . . ? N4 Zr1 N1 C5 113.13(16) . . . . ? O1 Zr1 N1 C3 88.32(17) . . . . ? O2 Zr1 N1 C3 -124.75(15) . . . . ? N3 Zr1 N1 C3 13.96(14) . . . . ? N2 Zr1 N1 C3 149.75(15) . . . . ? N4 Zr1 N1 C3 -42.18(17) . . . . ? O1 Zr1 N2 C7 -171.70(18) . . . . ? O2 Zr1 N2 C7 -49.56(17) . . . . ? N3 Zr1 N2 C7 100.89(17) . . . . ? N1 Zr1 N2 C7 45.33(17) . . . . ? N4 Zr1 N2 C7 -109.9(2) . . . . ? O1 Zr1 N2 C9 1.28(16) . . . . ? O2 Zr1 N2 C9 123.42(16) . . . . ? N3 Zr1 N2 C9 -86.13(17) . . . . ? N1 Zr1 N2 C9 -141.69(17) . . . . ? N4 Zr1 N2 C9 63.1(2) . . . . ? O2 Zr1 O1 C41A -178.3(8) . . . . ? N3 Zr1 O1 C41A 28.9(8) . . . . ? N1 Zr1 O1 C41A -37.8(9) . . . . ? N2 Zr1 O1 C41A -97.4(8) . . . . ? N4 Zr1 O1 C41A 103.5(8) . . . . ? O2 Zr1 O1 C41B 48.0(10) . . . . ? N3 Zr1 O1 C41B -104.8(10) . . . . ? N1 Zr1 O1 C41B -171.5(10) . . . . ? N2 Zr1 O1 C41B 128.9(10) . . . . ? N4 Zr1 O1 C41B -30.2(10) . . . . ? O1 Zr1 O2 C51 62.2(6) . . . . ? N3 Zr1 O2 C51 -160.2(5) . . . . ? N1 Zr1 O2 C51 -92.2(5) . . . . ? N2 Zr1 O2 C51 -16.1(5) . . . . ? N4 Zr1 O2 C51 143.1(5) . . . . ? C21 C1 C2 C3 -54.5(3) . . . . ? C5 N1 C3 C23 171.60(19) . . . . ? Zr1 N1 C3 C23 -33.9(2) . . . . ? C5 N1 C3 C2 51.1(3) . . . . ? Zr1 N1 C3 C2 -154.37(16) . . . . ? C1 C2 C3 N1 -175.7(2) . . . . ? C1 C2 C3 C23 62.6(2) . . . . ? C3 N1 C5 C6 -163.4(2) . . . . ? Zr1 N1 C5 C6 42.1(3) . . . . ? C3 N1 C5 C4 16.5(3) . . . . ? Zr1 N1 C5 C4 -138.09(18) . . . . ? N1 C5 C6 C7 9.1(4) . . . . ? C4 C5 C6 C7 -170.8(2) . . . . ? C9 N2 C7 C6 167.9(2) . . . . ? Zr1 N2 C7 C6 -18.8(3) . . . . ? C9 N2 C7 C8 -10.6(3) . . . . ? Zr1 N2 C7 C8 162.69(16) . . . . ? C5 C6 C7 N2 -22.2(4) . . . . ? C5 C6 C7 C8 156.4(2) . . . . ? C7 N2 C9 C14 92.6(3) . . . . ? Zr1 N2 C9 C14 -80.9(2) . . . . ? C7 N2 C9 C10 -88.9(3) . . . . ? Zr1 N2 C9 C10 97.7(2) . . . . ? C14 C9 C10 C11 -2.6(4) . . . . ? N2 C9 C10 C11 178.9(2) . . . . ? C14 C9 C10 C16 176.6(2) . . . . ? N2 C9 C10 C16 -2.0(3) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C16 C10 C11 C12 -179.1(3) . . . . ? C10 C11 C12 C13 2.3(4) . . . . ? C11 C12 C13 C14 -2.1(4) . . . . ? C10 C9 C14 C13 2.7(4) . . . . ? N2 C9 C14 C13 -178.8(2) . . . . ? C10 C9 C14 C15 -175.4(2) . . . . ? N2 C9 C14 C15 3.1(4) . . . . ? C12 C13 C14 C9 -0.3(4) . . . . ? C12 C13 C14 C15 177.8(3) . . . . ? C2 C1 C21 C22 50.4(3) . . . . ? C1 C21 C22 C23 -54.8(3) . . . . ? C25 N3 C23 C3 175.56(19) . . . . ? Zr1 N3 C23 C3 -30.8(2) . . . . ? C25 N3 C23 C22 54.4(3) . . . . ? Zr1 N3 C23 C22 -151.95(16) . . . . ? N1 C3 C23 N3 39.6(2) . . . . ? C2 C3 C23 N3 166.28(18) . . . . ? N1 C3 C23 C22 165.40(18) . . . . ? C2 C3 C23 C22 -67.9(2) . . . . ? C21 C22 C23 N3 -173.8(2) . . . . ? C21 C22 C23 C3 64.4(3) . . . . ? C23 N3 C25 C26 -158.8(2) . . . . ? Zr1 N3 C25 C26 46.7(3) . . . . ? C23 N3 C25 C24 22.4(3) . . . . ? Zr1 N3 C25 C24 -132.10(18) . . . . ? N3 C25 C26 C27 10.9(4) . . . . ? C24 C25 C26 C27 -170.2(2) . . . . ? C29 N4 C27 C26 164.8(2) . . . . ? Zr1 N4 C27 C26 -16.0(3) . . . . ? C29 N4 C27 C28 -12.3(3) . . . . ? Zr1 N4 C27 C28 166.78(16) . . . . ? C25 C26 C27 N4 -27.1(3) . . . . ? C25 C26 C27 C28 150.2(2) . . . . ? C27 N4 C29 C30 -85.6(3) . . . . ? Zr1 N4 C29 C30 95.3(2) . . . . ? C27 N4 C29 C34 95.6(3) . . . . ? Zr1 N4 C29 C34 -83.5(2) . . . . ? C34 C29 C30 C31 0.0(4) . . . . ? N4 C29 C30 C31 -178.8(2) . . . . ? C34 C29 C30 C36 -179.2(2) . . . . ? N4 C29 C30 C36 2.0(3) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C36 C30 C31 C32 178.9(3) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? C31 C32 C33 C34 0.6(4) . . . . ? C32 C33 C34 C29 -0.9(4) . . . . ? C32 C33 C34 C35 -179.5(3) . . . . ? C30 C29 C34 C33 0.6(4) . . . . ? N4 C29 C34 C33 179.4(2) . . . . ? C30 C29 C34 C35 179.2(2) . . . . ? N4 C29 C34 C35 -2.0(4) . . . . ? Zr1 O2 C51 C52 148.8(4) . . . . ? Zr1 O1 C41A C42A -144.2(7) . . . . ? Zr1 O1 C41B C42B 148.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 69.75 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.966 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.076 data_todd34 _database_code_depnum_ccdc_archive 'CCDC 894426' #TrackingRef '- Zoghbi-2012.cif' _vrf_PLAT201_todd34 ; RESPONSE The cyclohexane bridge is disordered and present as the R,R- as well as the S,S-enantiomer. The disorder affects the whole diketiminate ligand, but in particular N1,C5,C4 and N3,C25,C24. The disorder was refined using appropriate restraints (SIMU and SADI). Anisotropic refinement of N1,C5,C4 and N3,C25,C24 led to inacceptable thermal ellipsoids, even if EADP or strong SIMU restraints were applied. These atoms were thus refined isotropic. Occupation factors refined to 60:40. No indications for the presence of a superstructure could be found. ; _vrf_PLAT413_todd34 ; RESPONSE H24F and H4A2 is part of the disorder described above. Hydrogen positions are likely affected with high errors. ; _vrf_PLAT094_todd34 ; RESPONSE Electron densities above 0.5 e-/A^3 are associated with the described disorder. ; _vrf_PLAT366_todd34 ; RESPONSE Distance expected for delocalized aromatic bond. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H48 N4 Zr' _chemical_formula_sum 'C34 H48 N4 Zr' _chemical_formula_weight 603.98 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_hall '-P 2yn' 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 11.4759(9) _cell_length_b 14.9142(12) _cell_length_c 18.6288(14) _cell_angle_alpha 90 _cell_angle_beta 91.042(3) _cell_angle_gamma 90 _cell_volume 3187.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 55149 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 69.31 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 3.021 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.5469 _exptl_absorpt_correction_T_max 0.7393 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker microstar diffractometer equiped with a Platinum 135 CCD Detector, a Helios optics and a Kappa goniometer. The crystal-to-detector distance was 4.0 cm, and the data collection was carried out in 512 x 512 pixel mode. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 10.0 degree scan in 33 frames over three different parts of the reciprocal space (99 frames total). ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Helios optics' _diffrn_measurement_device_type 'Bruker Microstar' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 116139 _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 69.81 _reflns_number_total 5989 _reflns_number_gt 5599 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT V7.68A(Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A(Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'UdMX (Maris, 2004)' _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^)+(0.0483P)^2^+5.7398P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5989 _refine_ls_number_parameters 407 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.230 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.38132(2) 0.797022(18) 0.244497(14) 0.02605(11) Uani 1 1 d . . . N2 N 0.2842(2) 0.7871(2) 0.13477(15) 0.0316(6) Uani 1 1 d . C . N4 N 0.5738(2) 0.79992(19) 0.28881(15) 0.0284(6) Uani 1 1 d . C . C6 C 0.1396(4) 0.6880(3) 0.1807(2) 0.0561(12) Uani 1 1 d D . . H6 H 0.1005 0.6352 0.1688 0.067 Uiso 1 1 calc R A 1 C7 C 0.2022(3) 0.7241(3) 0.1247(2) 0.0416(9) Uani 1 1 d D C . C8 C 0.1716(5) 0.6918(3) 0.0500(3) 0.0613(13) Uani 1 1 d . . . H8A H 0.2415 0.6850 0.0231 0.092 Uiso 1 1 calc R C . H8B H 0.1215 0.7348 0.0267 0.092 Uiso 1 1 calc R . . H8C H 0.1323 0.6351 0.0528 0.092 Uiso 1 1 calc R . . C9 C 0.3049(3) 0.8443(2) 0.07408(18) 0.0323(7) Uani 1 1 d . . . C10 C 0.2228(3) 0.9105(3) 0.0574(2) 0.0417(9) Uani 1 1 d . C . C11 C 0.2432(4) 0.9678(3) -0.0004(2) 0.0527(11) Uani 1 1 d . . . H11A H 0.1876 1.0108 -0.0128 0.063 Uiso 1 1 calc R C . C12 C 0.3435(4) 0.9622(3) -0.0393(2) 0.0510(11) Uani 1 1 d . C . H12A H 0.3562 1.0014 -0.0771 0.061 Uiso 1 1 calc R . . C13 C 0.4238(4) 0.8985(3) -0.0218(2) 0.0456(10) Uani 1 1 d . . . H13A H 0.4922 0.8953 -0.0477 0.055 Uiso 1 1 calc R C . C14 C 0.4063(3) 0.8378(3) 0.03423(19) 0.0398(9) Uani 1 1 d . C . C15 C 0.4963(5) 0.7694(4) 0.0521(3) 0.0673(14) Uani 1 1 d . . . H15A H 0.4610 0.7111 0.0526 0.101 Uiso 1 1 calc R C . H15B H 0.5300 0.7822 0.0985 0.101 Uiso 1 1 calc R . . H15C H 0.5560 0.7709 0.0167 0.101 Uiso 1 1 calc R . . C16 C 0.1145(4) 0.9217(4) 0.1014(3) 0.0597(13) Uani 1 1 d . . . H16A H 0.0706 0.9722 0.0838 0.090 Uiso 1 1 calc R C . H16B H 0.1365 0.9316 0.1507 0.090 Uiso 1 1 calc R . . H16C H 0.0677 0.8685 0.0976 0.090 Uiso 1 1 calc R . . C26 C 0.5255(3) 0.7136(3) 0.3916(2) 0.0426(9) Uani 1 1 d D . . H26 H 0.5432 0.6603 0.4153 0.051 Uiso 1 1 calc R B 1 C27 C 0.6055(3) 0.7495(2) 0.34443(19) 0.0336(8) Uani 1 1 d D C . C28 C 0.7327(3) 0.7323(3) 0.3614(2) 0.0474(10) Uani 1 1 d . . . H28A H 0.7690 0.7062 0.3204 0.071 Uiso 1 1 calc R C . H28B H 0.7395 0.6920 0.4014 0.071 Uiso 1 1 calc R . . H28C H 0.7705 0.7880 0.3733 0.071 Uiso 1 1 calc R . . C29 C 0.6644(3) 0.8551(2) 0.25882(19) 0.0324(7) Uani 1 1 d . . . C30 C 0.6865(3) 0.9387(3) 0.2904(2) 0.0446(9) Uani 1 1 d . C . C31 C 0.7716(4) 0.9938(3) 0.2598(3) 0.0569(12) Uani 1 1 d . . . H31A H 0.7869 1.0497 0.2800 0.068 Uiso 1 1 calc R C . C32 C 0.8326(4) 0.9671(3) 0.2012(3) 0.0554(12) Uani 1 1 d . C . H32A H 0.8867 1.0055 0.1809 0.066 Uiso 1 1 calc R . . C33 C 0.8137(3) 0.8837(3) 0.1725(2) 0.0473(10) Uani 1 1 d . . . H33A H 0.8572 0.8652 0.1336 0.057 Uiso 1 1 calc R C . C34 C 0.7302(3) 0.8261(3) 0.2007(2) 0.0351(8) Uani 1 1 d . C . C35 C 0.7230(4) 0.7319(3) 0.1721(2) 0.0452(9) Uani 1 1 d . . . H35A H 0.6509 0.7051 0.1864 0.068 Uiso 1 1 calc R C . H35B H 0.7871 0.6974 0.1911 0.068 Uiso 1 1 calc R . . H35C H 0.7263 0.7331 0.1207 0.068 Uiso 1 1 calc R . . C36 C 0.6239(4) 0.9670(3) 0.3571(3) 0.0599(12) Uani 1 1 d . . . H36A H 0.5417 0.9573 0.3504 0.090 Uiso 1 1 calc R C . H36B H 0.6381 1.0295 0.3661 0.090 Uiso 1 1 calc R . . H36C H 0.6518 0.9323 0.3972 0.090 Uiso 1 1 calc R . . C37 C 0.4282(3) 0.6509(2) 0.2227(2) 0.0346(8) Uani 1 1 d . C . H37A H 0.3623 0.6209 0.2013 0.052 Uiso 1 1 calc R . . H37B H 0.4495 0.6220 0.2670 0.052 Uiso 1 1 calc R . . H37C H 0.4926 0.6485 0.1905 0.052 Uiso 1 1 calc R . . C38 C 0.4274(3) 0.9344(3) 0.20167(19) 0.0361(8) Uani 1 1 d . C . H38A H 0.3612 0.9591 0.1763 0.054 Uiso 1 1 calc R . . H38B H 0.4916 0.9292 0.1696 0.054 Uiso 1 1 calc R . . H38C H 0.4487 0.9731 0.2409 0.054 Uiso 1 1 calc R . . C4A C 0.0252(6) 0.6724(5) 0.2889(4) 0.0464(17) Uiso 0.592(6) 1 d PDU C 1 H4A1 H 0.0238 0.6947 0.3372 0.070 Uiso 0.592(6) 1 calc PR C 1 H4A2 H 0.0353 0.6086 0.2897 0.070 Uiso 0.592(6) 1 calc PR C 1 H4A3 H -0.0470 0.6869 0.2647 0.070 Uiso 0.592(6) 1 calc PR C 1 C5A C 0.1242(6) 0.7149(6) 0.2499(3) 0.0401(19) Uiso 0.592(6) 1 d PDU C 1 N1A N 0.1949(4) 0.7800(4) 0.2724(3) 0.0311(14) Uiso 0.592(6) 1 d PDU C 1 C3A C 0.1556(5) 0.8241(4) 0.3392(3) 0.0317(14) Uani 0.592(6) 1 d PDU C 1 H3AA H 0.1314 0.7781 0.3734 0.038 Uiso 0.592(6) 1 calc PR C 1 C2A C 0.0545(6) 0.8915(5) 0.3269(4) 0.0382(17) Uani 0.592(6) 1 d PDU C 1 H2AA H 0.0757 0.9350 0.2907 0.046 Uiso 0.592(6) 1 calc PR C 1 H2AB H -0.0147 0.8600 0.3101 0.046 Uiso 0.592(6) 1 calc PR C 1 C1A C 0.0294(6) 0.9395(5) 0.3976(4) 0.0446(17) Uani 0.592(6) 1 d PDU C 1 H1AA H -0.0292 0.9852 0.3888 0.054 Uiso 0.592(6) 1 calc PR C 1 H1AB H -0.0026 0.8965 0.4311 0.054 Uiso 0.592(6) 1 calc PR C 1 C21A C 0.1368(11) 0.9832(8) 0.4322(7) 0.044(3) Uani 0.592(6) 1 d PDU C 1 H21A H 0.1624 1.0324 0.4023 0.053 Uiso 0.592(6) 1 calc PR C 1 H21B H 0.1168 1.0073 0.4787 0.053 Uiso 0.592(6) 1 calc PR C 1 C22A C 0.2352(8) 0.9161(6) 0.4414(4) 0.0407(19) Uani 0.592(6) 1 d PDU C 1 H22A H 0.2134 0.8703 0.4756 0.049 Uiso 0.592(6) 1 calc PR C 1 H22B H 0.3044 0.9463 0.4599 0.049 Uiso 0.592(6) 1 calc PR C 1 C23A C 0.2611(5) 0.8729(4) 0.3692(3) 0.0306(13) Uani 0.592(6) 1 d PDU C 1 H23A H 0.2717 0.9236 0.3366 0.037 Uiso 0.592(6) 1 calc PR C 1 N3A N 0.3661(4) 0.8178(4) 0.3603(3) 0.0316(15) Uiso 0.592(6) 1 d PDU C 1 C25A C 0.4174(4) 0.7564(5) 0.4043(3) 0.0353(18) Uiso 0.592(6) 1 d PDU C 1 C24A C 0.3547(6) 0.7339(5) 0.4734(3) 0.0440(17) Uiso 0.592(6) 1 d PDU C 1 H24A H 0.2838 0.7678 0.4756 0.066 Uiso 0.592(6) 1 calc PR C 1 H24B H 0.4039 0.7486 0.5139 0.066 Uiso 0.592(6) 1 calc PR C 1 H24C H 0.3368 0.6710 0.4742 0.066 Uiso 0.592(6) 1 calc PR C 1 C5B C 0.1290(9) 0.7398(8) 0.2447(5) 0.055(4) Uiso 0.408(6) 1 d PDU C 2 C4B C 0.0262(10) 0.7267(10) 0.2940(6) 0.065(3) Uiso 0.408(6) 1 d PDU C 2 H4B1 H 0.0330 0.7672 0.3339 0.098 Uiso 0.408(6) 1 calc PR C 2 H4B2 H 0.0257 0.6661 0.3113 0.098 Uiso 0.408(6) 1 calc PR C 2 H4B3 H -0.0451 0.7385 0.2679 0.098 Uiso 0.408(6) 1 calc PR C 2 N1B N 0.1921(6) 0.8095(6) 0.2723(4) 0.032(2) Uiso 0.408(6) 1 d PDU C 2 C3B C 0.1923(8) 0.8734(6) 0.3342(4) 0.0341(19) Uani 0.408(6) 1 d PDU C 2 H3BA H 0.2397 0.9243 0.3187 0.041 Uiso 0.408(6) 1 calc PR C 2 C2B C 0.0770(8) 0.9150(8) 0.3588(6) 0.042(2) Uani 0.408(6) 1 d PDU C 2 H2BA H 0.0363 0.9425 0.3183 0.051 Uiso 0.408(6) 1 calc PR C 2 H2BB H 0.0272 0.8690 0.3786 0.051 Uiso 0.408(6) 1 calc PR C 2 C1B C 0.1062(18) 0.9857(11) 0.4160(9) 0.045(4) Uani 0.408(6) 1 d PDU C 2 H1BA H 0.1507 1.0336 0.3943 0.053 Uiso 0.408(6) 1 calc PR C 2 H1BB H 0.0343 1.0113 0.4334 0.053 Uiso 0.408(6) 1 calc PR C 2 C21B C 0.1759(9) 0.9471(7) 0.4794(5) 0.045(3) Uani 0.408(6) 1 d PD C 2 H21C H 0.1954 0.9948 0.5129 0.054 Uiso 0.408(6) 1 calc PR C 2 H21D H 0.1286 0.9035 0.5043 0.054 Uiso 0.408(6) 1 calc PR C 2 C22B C 0.2869(10) 0.9026(8) 0.4547(5) 0.039(2) Uani 0.408(6) 1 d PDU C 2 H22C H 0.3257 0.8737 0.4952 0.046 Uiso 0.408(6) 1 calc PR C 2 H22D H 0.3390 0.9476 0.4358 0.046 Uiso 0.408(6) 1 calc PR C 2 C23B C 0.2594(7) 0.8325(6) 0.3963(4) 0.031(2) Uani 0.408(6) 1 d PDU C 2 H23B H 0.2120 0.7848 0.4172 0.038 Uiso 0.408(6) 1 calc PR C 2 N3B N 0.3619(6) 0.7915(6) 0.3631(4) 0.025(2) Uiso 0.408(6) 1 d PDU C 2 C25B C 0.4104(5) 0.7296(8) 0.4058(4) 0.036(3) Uiso 0.408(6) 1 d PDU C 2 C24B C 0.3649(9) 0.6844(8) 0.4720(5) 0.046(2) Uiso 0.408(6) 1 d PDU C 2 H24D H 0.2847 0.7003 0.4781 0.068 Uiso 0.408(6) 1 calc PR C 2 H24E H 0.4098 0.7035 0.5133 0.068 Uiso 0.408(6) 1 calc PR C 2 H24F H 0.3714 0.6205 0.4668 0.068 Uiso 0.408(6) 1 calc PR C 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 0.02264(16) 0.03122(17) 0.02429(17) 0.00123(10) 0.00008(11) 0.00239(10) N2 0.0276(14) 0.0413(17) 0.0259(14) 0.0014(12) -0.0032(11) -0.0001(12) N4 0.0237(13) 0.0346(15) 0.0269(14) 0.0012(11) 0.0004(11) 0.0032(11) C6 0.036(2) 0.068(3) 0.064(3) 0.024(2) -0.013(2) -0.017(2) C7 0.035(2) 0.047(2) 0.042(2) 0.0068(17) -0.0113(16) -0.0042(16) C8 0.068(3) 0.062(3) 0.053(3) 0.003(2) -0.024(2) -0.022(2) C9 0.0316(17) 0.0405(19) 0.0248(16) -0.0018(14) -0.0051(13) -0.0037(14) C10 0.037(2) 0.048(2) 0.040(2) 0.0076(17) -0.0032(16) 0.0001(17) C11 0.053(3) 0.054(3) 0.051(3) 0.016(2) -0.006(2) -0.001(2) C12 0.057(3) 0.057(3) 0.039(2) 0.0104(19) -0.0048(19) -0.020(2) C13 0.042(2) 0.066(3) 0.0281(18) -0.0064(18) 0.0027(16) -0.018(2) C14 0.037(2) 0.055(2) 0.0268(17) -0.0076(16) 0.0001(15) -0.0040(17) C15 0.056(3) 0.090(4) 0.057(3) 0.003(3) 0.020(2) 0.023(3) C16 0.042(2) 0.076(3) 0.061(3) 0.023(2) 0.006(2) 0.020(2) C26 0.044(2) 0.052(2) 0.0315(19) 0.0092(17) -0.0072(16) -0.0050(17) C27 0.0322(18) 0.039(2) 0.0298(18) -0.0006(15) -0.0029(14) 0.0050(15) C28 0.037(2) 0.065(3) 0.040(2) 0.010(2) -0.0043(17) 0.0124(19) C29 0.0256(16) 0.0346(18) 0.0366(18) 0.0040(15) -0.0055(14) 0.0009(14) C30 0.035(2) 0.042(2) 0.056(2) -0.0049(18) -0.0081(18) -0.0019(16) C31 0.047(2) 0.040(2) 0.083(3) -0.003(2) -0.013(2) -0.0085(19) C32 0.039(2) 0.059(3) 0.069(3) 0.015(2) 0.003(2) -0.012(2) C33 0.034(2) 0.061(3) 0.047(2) 0.011(2) 0.0015(17) -0.0052(18) C34 0.0263(17) 0.045(2) 0.0335(18) 0.0071(16) -0.0021(14) -0.0019(15) C35 0.037(2) 0.054(2) 0.045(2) -0.0076(19) 0.0088(17) 0.0003(18) C36 0.061(3) 0.051(3) 0.067(3) -0.023(2) -0.009(2) 0.001(2) C37 0.0307(17) 0.0344(18) 0.0386(19) -0.0071(15) -0.0044(15) 0.0046(14) C38 0.0355(19) 0.041(2) 0.0319(18) -0.0008(15) -0.0030(15) 0.0039(15) C3A 0.028(3) 0.033(3) 0.034(3) 0.006(3) 0.007(2) 0.005(3) C2A 0.030(3) 0.046(4) 0.039(4) 0.005(3) 0.001(3) 0.007(3) C1A 0.040(4) 0.052(4) 0.043(4) 0.006(3) 0.011(3) 0.013(3) C21A 0.051(8) 0.050(4) 0.031(6) -0.003(4) 0.010(5) 0.013(4) C22A 0.043(5) 0.051(4) 0.028(4) 0.001(3) 0.002(4) 0.004(4) C23A 0.030(3) 0.037(3) 0.025(3) 0.005(3) 0.003(2) 0.007(3) C3B 0.033(4) 0.039(5) 0.031(4) 0.006(4) 0.007(4) 0.005(4) C2B 0.028(5) 0.059(6) 0.040(6) 0.014(5) 0.003(4) 0.013(4) C1B 0.046(9) 0.052(6) 0.036(9) 0.007(5) 0.009(7) 0.023(6) C21B 0.050(6) 0.052(6) 0.034(5) 0.003(5) 0.014(5) 0.013(5) C22B 0.043(7) 0.045(5) 0.028(5) 0.001(4) -0.001(4) 0.004(5) C23B 0.028(4) 0.037(5) 0.030(5) 0.005(4) 0.004(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N3A 2.190(5) . Y Zr1 N1B 2.250(7) . Y Zr1 N1A 2.226(5) . Y Zr1 C38 2.265(4) . Y Zr1 N3B 2.226(7) . Y Zr1 C37 2.283(3) . Y Zr1 N2 2.315(3) . Y Zr1 N4 2.344(3) . Y N2 C7 1.340(5) . Y N2 C9 1.440(4) . Y N4 C27 1.326(4) . Y N4 C29 1.447(4) . Y C6 C5A 1.366(5) . Y C6 C7 1.386(6) . Y C6 C5B 1.428(6) . Y C6 H6 0.9300 . Y C7 C8 1.507(6) . Y C8 H8A 0.9600 . Y C8 H8B 0.9600 . Y C8 H8C 0.9600 . Y C9 C14 1.395(5) . Y C9 C10 1.396(5) . Y C10 C11 1.397(6) . Y C10 C16 1.510(6) . Y C11 C12 1.374(7) . Y C11 H11A 0.9300 . Y C12 C13 1.359(6) . Y C12 H12A 0.9300 . Y C13 C14 1.399(6) . Y C13 H13A 0.9300 . Y C14 C15 1.484(6) . Y C15 H15A 0.9600 . Y C15 H15B 0.9600 . Y C15 H15C 0.9600 . Y C16 H16A 0.9600 . Y C16 H16B 0.9600 . Y C16 H16C 0.9600 . Y C26 C25B 1.373(6) . Y C26 C27 1.390(5) . Y C26 C25A 1.419(5) . Y C26 H26 0.9300 . Y C27 C28 1.509(5) . Y C28 H28A 0.9600 . Y C28 H28B 0.9600 . Y C28 H28C 0.9600 . Y C29 C34 1.399(5) . Y C29 C30 1.400(5) . Y C30 C31 1.404(6) . Y C30 C36 1.507(6) . Y C31 C32 1.366(7) . Y C31 H31A 0.9300 . Y C32 C33 1.369(7) . Y C32 H32A 0.9300 . Y C33 C34 1.398(5) . Y C33 H33A 0.9300 . Y C34 C35 1.505(6) . Y C35 H35A 0.9600 . Y C35 H35B 0.9600 . Y C35 H35C 0.9600 . Y C36 H36A 0.9600 . Y C36 H36B 0.9600 . Y C36 H36C 0.9600 . Y C37 H37A 0.9600 . Y C37 H37B 0.9600 . Y C37 H37C 0.9600 . Y C38 H38A 0.9600 . Y C38 H38B 0.9600 . Y C38 H38C 0.9600 . Y C4A C5A 1.500(8) . Y C4A H4A1 0.9600 . Y C4A H4A2 0.9600 . Y C4A H4A3 0.9600 . Y C5A N1A 1.329(6) . Y N1A C3A 1.484(7) . Y C3A C23A 1.512(8) . Y C3A C2A 1.549(7) . Y C3A H3AA 0.9800 . Y C2A C1A 1.531(10) . Y C2A H2AA 0.9700 . Y C2A H2AB 0.9700 . Y C1A C21A 1.527(12) . Y C1A H1AA 0.9700 . Y C1A H1AB 0.9700 . Y C21A C22A 1.515(12) . Y C21A H21A 0.9700 . Y C21A H21B 0.9700 . Y C22A C23A 1.524(8) . Y C22A H22A 0.9700 . Y C22A H22B 0.9700 . Y C23A N3A 1.470(7) . Y C23A H23A 0.9800 . Y N3A C25A 1.356(6) . Y C25A C24A 1.524(7) . Y C24A H24A 0.9600 . Y C24A H24B 0.9600 . Y C24A H24C 0.9600 . Y C5B C4B 1.521(9) . Y C5B N1B 1.362(7) . Y C4B H4B1 0.9600 . Y C4B H4B2 0.9600 . Y C4B H4B3 0.9600 . Y N1B C3B 1.496(9) . Y C3B C23B 1.507(9) . Y C3B C2B 1.538(9) . Y C3B H3BA 0.9800 . Y C2B C1B 1.533(14) . Y C2B H2BA 0.9700 . Y C2B H2BB 0.9700 . Y C1B C21B 1.527(13) . Y C1B H1BA 0.9700 . Y C1B H1BB 0.9700 . Y C21B C22B 1.515(12) . Y C21B H21C 0.9700 . Y C21B H21D 0.9700 . Y C22B C23B 1.537(9) . Y C22B H22C 0.9700 . Y C22B H22D 0.9700 . Y C23B N3B 1.472(8) . Y C23B H23B 0.9800 . Y N3B C25B 1.334(7) . Y C25B C24B 1.508(8) . Y C24B H24D 0.9600 . Y C24B H24E 0.9600 . Y C24B H24F 0.9600 . Y 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 N3A Zr1 N1A 72.04(18) . . Y N3A Zr1 C38 104.0(2) . . Y N1B Zr1 C38 103.8(3) . . Y N1A Zr1 C38 114.63(19) . . Y N1B Zr1 N3B 70.1(2) . . Y C38 Zr1 N3B 114.3(2) . . Y N3A Zr1 C37 109.50(19) . . Y N1B Zr1 C37 110.6(2) . . Y N1A Zr1 C37 99.43(19) . . Y C38 Zr1 C37 138.04(14) . . Y N3B Zr1 C37 99.8(2) . . Y N3A Zr1 N2 146.44(14) . . Y N1B Zr1 N2 75.94(18) . . Y N1A Zr1 N2 75.50(15) . . Y C38 Zr1 N2 81.88(12) . . Y N3B Zr1 N2 144.95(19) . . Y C37 Zr1 N2 83.85(12) . . Y N3A Zr1 N4 75.04(14) . . Y N1B Zr1 N4 145.58(18) . . Y N1A Zr1 N4 145.42(15) . . Y C38 Zr1 N4 83.28(12) . . Y N3B Zr1 N4 76.22(18) . . Y C37 Zr1 N4 81.76(11) . . Y N2 Zr1 N4 138.38(10) . . Y C7 N2 C9 115.6(3) . . Y C7 N2 Zr1 119.6(2) . . Y C9 N2 Zr1 124.8(2) . . Y C27 N4 C29 115.8(3) . . Y C27 N4 Zr1 120.5(2) . . Y C29 N4 Zr1 123.6(2) . . Y C5A C6 C7 132.4(5) . . Y C5A C6 C5B 15.8(6) . . Y C7 C6 C5B 118.1(6) . . Y C5A C6 H6 113.8 . . Y C7 C6 H6 113.8 . . Y C5B C6 H6 127.5 . . Y N2 C7 C6 122.6(4) . . Y N2 C7 C8 120.3(4) . . Y C6 C7 C8 117.0(4) . . Y C7 C8 H8A 109.5 . . Y C7 C8 H8B 109.5 . . Y H8A C8 H8B 109.5 . . Y C7 C8 H8C 109.5 . . Y H8A C8 H8C 109.5 . . Y H8B C8 H8C 109.5 . . Y C14 C9 C10 119.8(3) . . Y C14 C9 N2 121.9(3) . . Y C10 C9 N2 118.3(3) . . Y C9 C10 C11 118.9(4) . . Y C9 C10 C16 121.0(4) . . Y C11 C10 C16 120.1(4) . . Y C12 C11 C10 121.5(4) . . Y C12 C11 H11A 119.3 . . Y C10 C11 H11A 119.3 . . Y C13 C12 C11 119.2(4) . . Y C13 C12 H12A 120.4 . . Y C11 C12 H12A 120.4 . . Y C12 C13 C14 121.7(4) . . Y C12 C13 H13A 119.2 . . Y C14 C13 H13A 119.2 . . Y C9 C14 C13 119.0(4) . . Y C9 C14 C15 120.8(4) . . Y C13 C14 C15 120.2(4) . . Y C14 C15 H15A 109.5 . . Y C14 C15 H15B 109.5 . . Y H15A C15 H15B 109.5 . . Y C14 C15 H15C 109.5 . . Y H15A C15 H15C 109.5 . . Y H15B C15 H15C 109.5 . . Y C10 C16 H16A 109.5 . . Y C10 C16 H16B 109.5 . . Y H16A C16 H16B 109.5 . . Y C10 C16 H16C 109.5 . . Y H16A C16 H16C 109.5 . . Y H16B C16 H16C 109.5 . . Y C25B C26 C27 134.8(5) . . Y C25B C26 C25A 16.8(5) . . Y C27 C26 C25A 121.5(4) . . Y C25B C26 H26 105.0 . . Y C27 C26 H26 119.3 . . Y C25A C26 H26 119.3 . . Y N4 C27 C26 122.5(3) . . Y N4 C27 C28 120.7(3) . . Y C26 C27 C28 116.7(3) . . Y C27 C28 H28A 109.5 . . Y C27 C28 H28B 109.5 . . Y H28A C28 H28B 109.5 . . Y C27 C28 H28C 109.5 . . Y H28A C28 H28C 109.5 . . Y H28B C28 H28C 109.5 . . Y C34 C29 C30 120.3(3) . . Y C34 C29 N4 121.6(3) . . Y C30 C29 N4 118.1(3) . . Y C29 C30 C31 118.2(4) . . Y C29 C30 C36 120.7(4) . . Y C31 C30 C36 121.1(4) . . Y C32 C31 C30 121.6(4) . . Y C32 C31 H31A 119.2 . . Y C30 C31 H31A 119.2 . . Y C31 C32 C33 119.8(4) . . Y C31 C32 H32A 120.1 . . Y C33 C32 H32A 120.1 . . Y C32 C33 C34 121.0(4) . . Y C32 C33 H33A 119.5 . . Y C34 C33 H33A 119.5 . . Y C33 C34 C29 119.0(4) . . Y C33 C34 C35 118.3(4) . . Y C29 C34 C35 122.4(3) . . Y C34 C35 H35A 109.5 . . Y C34 C35 H35B 109.5 . . Y H35A C35 H35B 109.5 . . Y C34 C35 H35C 109.5 . . Y H35A C35 H35C 109.5 . . Y H35B C35 H35C 109.5 . . Y C30 C36 H36A 109.5 . . Y C30 C36 H36B 109.5 . . Y H36A C36 H36B 109.5 . . Y C30 C36 H36C 109.5 . . Y H36A C36 H36C 109.5 . . Y H36B C36 H36C 109.5 . . Y Zr1 C37 H37A 109.5 . . Y Zr1 C37 H37B 109.5 . . Y H37A C37 H37B 109.5 . . Y Zr1 C37 H37C 109.5 . . Y H37A C37 H37C 109.5 . . Y H37B C37 H37C 109.5 . . Y Zr1 C38 H38A 109.5 . . Y Zr1 C38 H38B 109.5 . . Y H38A C38 H38B 109.5 . . Y Zr1 C38 H38C 109.5 . . Y H38A C38 H38C 109.5 . . Y H38B C38 H38C 109.5 . . Y C5A C4A H4A1 109.5 . . Y C5A C4A H4A2 109.5 . . Y H4A1 C4A H4A2 109.5 . . Y C5A C4A H4A3 109.5 . . Y H4A1 C4A H4A3 109.5 . . Y H4A2 C4A H4A3 109.5 . . Y N1A C5A C6 115.1(5) . . Y N1A C5A C4A 128.3(5) . . Y C6 C5A C4A 116.4(5) . . Y C5A N1A C3A 113.3(5) . . Y C5A N1A Zr1 126.4(4) . . Y C3A N1A Zr1 117.0(4) . . Y N1A C3A C23A 105.7(4) . . Y N1A C3A C2A 113.7(5) . . Y C23A C3A C2A 109.6(6) . . Y N1A C3A H3AA 109.3 . . Y C23A C3A H3AA 109.3 . . Y C2A C3A H3AA 109.3 . . Y C1A C2A C3A 109.2(6) . . Y C1A C2A H2AA 109.8 . . Y C3A C2A H2AA 109.8 . . Y C1A C2A H2AB 109.8 . . Y C3A C2A H2AB 109.8 . . Y H2AA C2A H2AB 108.3 . . Y C21A C1A C2A 113.5(7) . . Y C21A C1A H1AA 108.9 . . Y C2A C1A H1AA 108.9 . . Y C21A C1A H1AB 108.9 . . Y C2A C1A H1AB 108.9 . . Y H1AA C1A H1AB 107.7 . . Y C22A C21A C1A 111.1(8) . . Y C22A C21A H21A 109.4 . . Y C1A C21A H21A 109.4 . . Y C22A C21A H21B 109.4 . . Y C1A C21A H21B 109.4 . . Y H21A C21A H21B 108.0 . . Y C21A C22A C23A 109.6(7) . . Y C21A C22A H22A 109.7 . . Y C23A C22A H22A 109.7 . . Y C21A C22A H22B 109.7 . . Y C23A C22A H22B 109.7 . . Y H22A C22A H22B 108.2 . . Y N3A C23A C3A 110.0(5) . . Y N3A C23A C22A 120.6(6) . . Y C3A C23A C22A 111.2(5) . . Y N3A C23A H23A 104.4 . . Y C3A C23A H23A 104.4 . . Y C22A C23A H23A 104.4 . . Y C25A N3A C23A 131.0(5) . . Y C25A N3A Zr1 117.3(4) . . Y C23A N3A Zr1 105.7(4) . . Y C26 C25A N3A 125.0(5) . . Y C26 C25A C24A 118.0(5) . . Y N3A C25A C24A 116.9(5) . . Y C25A C24A H24A 109.5 . . Y C25A C24A H24B 109.5 . . Y H24A C24A H24B 109.5 . . Y C25A C24A H24C 109.5 . . Y H24A C24A H24C 109.5 . . Y H24B C24A H24C 109.5 . . Y C6 C5B C4B 120.9(8) . . Y C6 C5B N1B 132.5(7) . . Y C4B C5B N1B 106.4(7) . . Y C5B C4B H4B1 109.5 . . Y C5B C4B H4B2 109.5 . . Y H4B1 C4B H4B2 109.5 . . Y C5B C4B H4B3 109.5 . . Y H4B1 C4B H4B3 109.5 . . Y H4B2 C4B H4B3 109.5 . . Y C3B N1B C5B 140.4(7) . . Y C3B N1B Zr1 104.0(5) . . Y C5B N1B Zr1 111.0(6) . . Y N1B C3B C23B 109.1(6) . . Y N1B C3B C2B 119.8(8) . . Y C23B C3B C2B 111.4(7) . . Y N1B C3B H3BA 105.1 . . Y C23B C3B H3BA 105.1 . . Y C2B C3B H3BA 105.1 . . Y C1B C2B C3B 107.8(10) . . Y C1B C2B H2BA 110.1 . . Y C3B C2B H2BA 110.1 . . Y C1B C2B H2BB 110.1 . . Y C3B C2B H2BB 110.1 . . Y H2BA C2B H2BB 108.5 . . Y C21B C1B C2B 112.5(11) . . Y C21B C1B H1BA 109.1 . . Y C2B C1B H1BA 109.1 . . Y C21B C1B H1BB 109.1 . . Y C2B C1B H1BB 109.1 . . Y H1BA C1B H1BB 107.8 . . Y C22B C21B C1B 111.2(10) . . Y C22B C21B H21C 109.4 . . Y C1B C21B H21C 109.4 . . Y C22B C21B H21D 109.4 . . Y C1B C21B H21D 109.4 . . Y H21C C21B H21D 108.0 . . Y C21B C22B C23B 110.5(8) . . Y C21B C22B H22C 109.5 . . Y C23B C22B H22C 109.5 . . Y C21B C22B H22D 109.5 . . Y C23B C22B H22D 109.5 . . Y H22C C22B H22D 108.1 . . Y N3B C23B C3B 104.3(6) . . Y N3B C23B C22B 115.1(7) . . Y C3B C23B C22B 111.3(8) . . Y N3B C23B H23B 108.7 . . Y C3B C23B H23B 108.7 . . Y C22B C23B H23B 108.7 . . Y C25B N3B C23B 111.4(6) . . Y C25B N3B Zr1 124.7(5) . . Y C23B N3B Zr1 119.8(5) . . Y N3B C25B C26 113.4(6) . . Y N3B C25B C24B 130.6(6) . . Y C26 C25B C24B 115.4(6) . . Y C25B C24B H24D 109.5 . . Y C25B C24B H24E 109.5 . . Y H24D C24B H24E 109.5 . . Y C25B C24B H24F 109.5 . . Y H24D C24B H24F 109.5 . . Y H24E C24B H24F 109.5 . . Y 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 N3A Zr1 N2 C7 -59.7(5) . . . . Y N1B Zr1 N2 C7 -56.3(4) . . . . Y N1A Zr1 N2 C7 -44.7(3) . . . . Y C38 Zr1 N2 C7 -162.8(3) . . . . Y N3B Zr1 N2 C7 -41.5(5) . . . . Y C37 Zr1 N2 C7 56.7(3) . . . . Y N4 Zr1 N2 C7 126.9(3) . . . . Y N3A Zr1 N2 C9 120.6(4) . . . . Y N1B Zr1 N2 C9 123.9(4) . . . . Y N1A Zr1 N2 C9 135.6(3) . . . . Y C38 Zr1 N2 C9 17.4(3) . . . . Y N3B Zr1 N2 C9 138.7(4) . . . . Y C37 Zr1 N2 C9 -123.0(3) . . . . Y N4 Zr1 N2 C9 -52.8(3) . . . . Y N3A Zr1 N4 C27 50.2(3) . . . . Y N1B Zr1 N4 C27 52.0(5) . . . . Y N1A Zr1 N4 C27 32.0(4) . . . . Y C38 Zr1 N4 C27 156.7(3) . . . . Y N3B Zr1 N4 C27 39.6(3) . . . . Y C37 Zr1 N4 C27 -62.6(3) . . . . Y N2 Zr1 N4 C27 -133.6(3) . . . . Y N3A Zr1 N4 C29 -129.7(3) . . . . Y N1B Zr1 N4 C29 -127.8(5) . . . . Y N1A Zr1 N4 C29 -147.8(4) . . . . Y C38 Zr1 N4 C29 -23.2(3) . . . . Y N3B Zr1 N4 C29 -140.2(3) . . . . Y C37 Zr1 N4 C29 117.5(3) . . . . Y N2 Zr1 N4 C29 46.5(3) . . . . Y C9 N2 C7 C6 -154.2(4) . . . . Y Zr1 N2 C7 C6 26.1(5) . . . . Y C9 N2 C7 C8 23.6(5) . . . . Y Zr1 N2 C7 C8 -156.1(3) . . . . Y C5A C6 C7 N2 15.4(9) . . . . Y C5B C6 C7 N2 23.7(9) . . . . Y C5A C6 C7 C8 -162.4(6) . . . . Y C5B C6 C7 C8 -154.2(7) . . . . Y C7 N2 C9 C14 -108.2(4) . . . . Y Zr1 N2 C9 C14 71.6(4) . . . . Y C7 N2 C9 C10 74.7(4) . . . . Y Zr1 N2 C9 C10 -105.5(3) . . . . Y C14 C9 C10 C11 1.4(6) . . . . Y N2 C9 C10 C11 178.6(4) . . . . Y C14 C9 C10 C16 -177.5(4) . . . . Y N2 C9 C10 C16 -0.3(6) . . . . Y C9 C10 C11 C12 -2.1(7) . . . . Y C16 C10 C11 C12 176.8(4) . . . . Y C10 C11 C12 C13 0.9(7) . . . . Y C11 C12 C13 C14 0.9(6) . . . . Y C10 C9 C14 C13 0.4(5) . . . . Y N2 C9 C14 C13 -176.7(3) . . . . Y C10 C9 C14 C15 178.5(4) . . . . Y N2 C9 C14 C15 1.5(6) . . . . Y C12 C13 C14 C9 -1.5(6) . . . . Y C12 C13 C14 C15 -179.7(4) . . . . Y C29 N4 C27 C26 160.9(4) . . . . Y Zr1 N4 C27 C26 -19.0(5) . . . . Y C29 N4 C27 C28 -16.0(5) . . . . Y Zr1 N4 C27 C28 164.2(3) . . . . Y C25B C26 C27 N4 -15.2(10) . . . . Y C25A C26 C27 N4 -28.2(7) . . . . Y C25B C26 C27 C28 161.7(8) . . . . Y C25A C26 C27 C28 148.7(5) . . . . Y C27 N4 C29 C34 94.2(4) . . . . Y Zr1 N4 C29 C34 -86.0(4) . . . . Y C27 N4 C29 C30 -84.7(4) . . . . Y Zr1 N4 C29 C30 95.2(3) . . . . Y C34 C29 C30 C31 3.3(6) . . . . Y N4 C29 C30 C31 -177.8(4) . . . . Y C34 C29 C30 C36 -174.4(4) . . . . Y N4 C29 C30 C36 4.5(5) . . . . Y C29 C30 C31 C32 -0.5(7) . . . . Y C36 C30 C31 C32 177.1(4) . . . . Y C30 C31 C32 C33 -2.1(7) . . . . Y C31 C32 C33 C34 2.1(7) . . . . Y C32 C33 C34 C29 0.7(6) . . . . Y C32 C33 C34 C35 -173.3(4) . . . . Y C30 C29 C34 C33 -3.4(5) . . . . Y N4 C29 C34 C33 177.8(3) . . . . Y C30 C29 C34 C35 170.3(4) . . . . Y N4 C29 C34 C35 -8.5(5) . . . . Y C7 C6 C5A N1A -11.7(11) . . . . Y C5B C6 C5A N1A -39(2) . . . . Y C7 C6 C5A C4A 164.0(6) . . . . Y C5B C6 C5A C4A 136(3) . . . . Y C6 C5A N1A C3A 164.3(6) . . . . Y C4A C5A N1A C3A -10.9(11) . . . . Y C6 C5A N1A Zr1 -37.2(10) . . . . Y C4A C5A N1A Zr1 147.7(6) . . . . Y N3A Zr1 N1A C5A -134.7(6) . . . . Y N1B Zr1 N1A C5A 144.7(16) . . . . Y C38 Zr1 N1A C5A 127.8(6) . . . . Y N3B Zr1 N1A C5A -124.1(6) . . . . Y C37 Zr1 N1A C5A -27.1(6) . . . . Y N2 Zr1 N1A C5A 54.0(6) . . . . Y N4 Zr1 N1A C5A -116.2(6) . . . . Y N3A Zr1 N1A C3A 23.2(4) . . . . Y N1B Zr1 N1A C3A -57.4(12) . . . . Y C38 Zr1 N1A C3A -74.4(5) . . . . Y N3B Zr1 N1A C3A 33.8(5) . . . . Y C37 Zr1 N1A C3A 130.7(4) . . . . Y N2 Zr1 N1A C3A -148.2(5) . . . . Y N4 Zr1 N1A C3A 41.6(6) . . . . Y C5A N1A C3A C23A 162.3(6) . . . . Y Zr1 N1A C3A C23A 1.6(6) . . . . Y C5A N1A C3A C2A -77.5(8) . . . . Y Zr1 N1A C3A C2A 121.8(5) . . . . Y N1A C3A C2A C1A -174.4(6) . . . . Y C23A C3A C2A C1A -56.5(7) . . . . Y C3A C2A C1A C21A 53.6(9) . . . . Y C2A C1A C21A C22A -53.7(12) . . . . Y C1A C21A C22A C23A 55.0(12) . . . . Y N1A C3A C23A N3A -39.7(7) . . . . Y C2A C3A C23A N3A -162.5(5) . . . . Y N1A C3A C23A C22A -175.9(6) . . . . Y C2A C3A C23A C22A 61.2(7) . . . . Y C21A C22A C23A N3A 168.8(8) . . . . Y C21A C22A C23A C3A -60.2(10) . . . . Y C3A C23A N3A C25A -90.8(8) . . . . Y C22A C23A N3A C25A 40.7(11) . . . . Y C3A C23A N3A Zr1 60.3(6) . . . . Y C22A C23A N3A Zr1 -168.1(6) . . . . Y N1B Zr1 N3A C25A 124.9(6) . . . . Y N1A Zr1 N3A C25A 113.1(5) . . . . Y C38 Zr1 N3A C25A -135.1(5) . . . . Y N3B Zr1 N3A C25A 39.1(12) . . . . Y C37 Zr1 N3A C25A 19.2(5) . . . . Y N2 Zr1 N3A C25A 128.4(4) . . . . Y N4 Zr1 N3A C25A -56.2(5) . . . . Y N1B Zr1 N3A C23A -30.9(4) . . . . Y N1A Zr1 N3A C23A -42.7(4) . . . . Y C38 Zr1 N3A C23A 69.0(4) . . . . Y N3B Zr1 N3A C23A -116.7(14) . . . . Y C37 Zr1 N3A C23A -136.6(4) . . . . Y N2 Zr1 N3A C23A -27.4(6) . . . . Y N4 Zr1 N3A C23A 148.0(4) . . . . Y C25B C26 C25A N3A -126(2) . . . . Y C27 C26 C25A N3A 19.8(10) . . . . Y C25B C26 C25A C24A 55.0(16) . . . . Y C27 C26 C25A C24A -158.7(6) . . . . Y C23A N3A C25A C26 -174.0(6) . . . . Y Zr1 N3A C25A C26 37.5(9) . . . . Y C23A N3A C25A C24A 4.5(11) . . . . Y Zr1 N3A C25A C24A -143.9(5) . . . . Y C5A C6 C5B C4B -48.9(18) . . . . Y C7 C6 C5B C4B 154.1(10) . . . . Y C5A C6 C5B N1B 137(4) . . . . Y C7 C6 C5B N1B -20.3(19) . . . . Y C6 C5B N1B C3B 176.3(10) . . . . Y C4B C5B N1B C3B 1(2) . . . . Y C6 C5B N1B Zr1 -33.1(18) . . . . Y C4B C5B N1B Zr1 151.9(8) . . . . Y N3A Zr1 N1B C3B 32.7(5) . . . . Y N1A Zr1 N1B C3B 128.3(15) . . . . Y C38 Zr1 N1B C3B -67.6(5) . . . . Y N3B Zr1 N1B C3B 43.6(5) . . . . Y C37 Zr1 N1B C3B 136.9(5) . . . . Y N2 Zr1 N1B C3B -145.4(6) . . . . Y N4 Zr1 N1B C3B 30.8(8) . . . . Y N3A Zr1 N1B C5B -128.5(8) . . . . Y N1A Zr1 N1B C5B -32.9(11) . . . . Y C38 Zr1 N1B C5B 131.2(7) . . . . Y N3B Zr1 N1B C5B -117.6(8) . . . . Y C37 Zr1 N1B C5B -24.3(8) . . . . Y N2 Zr1 N1B C5B 53.5(7) . . . . Y N4 Zr1 N1B C5B -130.4(7) . . . . Y C5B N1B C3B C23B 88.9(15) . . . . Y Zr1 N1B C3B C23B -62.9(8) . . . . Y C5B N1B C3B C2B -41.1(18) . . . . Y Zr1 N1B C3B C2B 167.1(7) . . . . Y N1B C3B C2B C1B -172.9(11) . . . . Y C23B C3B C2B C1B 58.0(13) . . . . Y C3B C2B C1B C21B -56.9(17) . . . . Y C2B C1B C21B C22B 56.3(18) . . . . Y C1B C21B C22B C23B -53.9(13) . . . . Y N1B C3B C23B N3B 42.2(9) . . . . Y C2B C3B C23B N3B 176.6(8) . . . . Y N1B C3B C23B C22B 166.8(8) . . . . Y C2B C3B C23B C22B -58.7(11) . . . . Y C21B C22B C23B N3B 174.0(8) . . . . Y C21B C22B C23B C3B 55.7(11) . . . . Y C3B C23B N3B C25B -160.4(9) . . . . Y C22B C23B N3B C25B 77.4(11) . . . . Y C3B C23B N3B Zr1 -2.1(9) . . . . Y C22B C23B N3B Zr1 -124.3(8) . . . . Y N3A Zr1 N3B C25B -138.5(18) . . . . Y N1B Zr1 N3B C25B 131.0(8) . . . . Y N1A Zr1 N3B C25B 119.0(8) . . . . Y C38 Zr1 N3B C25B -132.3(7) . . . . Y C37 Zr1 N3B C25B 22.5(8) . . . . Y N2 Zr1 N3B C25B 115.7(7) . . . . Y N4 Zr1 N3B C25B -56.4(7) . . . . Y N3A Zr1 N3B C23B 66.3(12) . . . . Y N1B Zr1 N3B C23B -24.2(6) . . . . Y N1A Zr1 N3B C23B -36.2(6) . . . . Y C38 Zr1 N3B C23B 72.5(7) . . . . Y C37 Zr1 N3B C23B -132.7(6) . . . . Y N2 Zr1 N3B C23B -39.4(9) . . . . Y N4 Zr1 N3B C23B 148.4(7) . . . . Y C23B N3B C25B C26 -157.2(8) . . . . Y Zr1 N3B C25B C26 45.8(12) . . . . Y C23B N3B C25B C24B 13.7(16) . . . . Y Zr1 N3B C25B C24B -143.3(10) . . . . Y C27 C26 C25B N3B 3.0(14) . . . . Y C25A C26 C25B N3B 44.9(13) . . . . Y C27 C26 C25B C24B -169.4(7) . . . . Y C25A C26 C25B C24B -127(2) . . . . Y _iucr_refine_instructions_details ; CELL 1.54178 11.4759 14.9142 18.6288 90.000 91.042 90.000 ZERR 4.00 0.0009 0.0012 0.0014 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Zr UNIT 136 192 16 4 SIZE 0.1 0.1 0.1 TEMP 223 L.S. 10 BOND $H ACTA CONF FMAP 2 PLAN 5 SIMU 0.01 0.02 1 rem SIMU 0.02 0.04 2 C4a > C24b rem simu 0.01 0.02 1.7 c24a c24b c25a c25b n3a n3b n1a n1b c4a c4b c5a c5b defs 0.01 SADI 0.005 c25a c26 c25b c26 c5a c6 c5b c6 SADI 0.02 c25a c27 c25b c27 c5a c7 c5b c7 SADI 0.005 C24A C25A C24b C25b SADI 0.005 C4a C5a C4b C5b SADI 0.02 C4a C6 C4b C6 SADI 0.02 C24a C26 C24b C26 SADi 0.005 N1A C5A N1B C5b N3A C25A N3B C25B WGHT 0.048300 5.739800 FVAR 0.29913 0.59243 ZR1 4 0.381315 0.797022 0.244497 11.00000 0.02264 0.03122 = 0.02429 0.00123 0.00008 0.00239 N2 3 0.284155 0.787063 0.134768 11.00000 0.02758 0.04129 = 0.02588 0.00135 -0.00324 -0.00012 N4 3 0.573796 0.799919 0.288806 11.00000 0.02371 0.03458 = 0.02692 0.00121 0.00042 0.00319 C6 1 0.139595 0.687951 0.180665 11.00000 0.03563 0.06836 = 0.06389 0.02440 -0.01331 -0.01670 AFIX 43 H6 2 0.100499 0.635239 0.168760 11.00000 -1.20000 AFIX 0 C7 1 0.202247 0.724074 0.124685 11.00000 0.03501 0.04732 = 0.04202 0.00675 -0.01133 -0.00416 C8 1 0.171592 0.691812 0.050039 11.00000 0.06824 0.06191 = 0.05274 0.00339 -0.02416 -0.02186 AFIX 137 H8A 2 0.241533 0.684991 0.023072 11.00000 -1.50000 H8B 2 0.121453 0.734753 0.026671 11.00000 -1.50000 H8C 2 0.132263 0.635142 0.052823 11.00000 -1.50000 AFIX 0 C9 1 0.304922 0.844324 0.074085 11.00000 0.03156 0.04046 = 0.02479 -0.00184 -0.00509 -0.00375 C10 1 0.222790 0.910507 0.057350 11.00000 0.03716 0.04808 = 0.03962 0.00756 -0.00320 0.00008 C11 1 0.243174 0.967821 -0.000372 11.00000 0.05343 0.05384 = 0.05059 0.01572 -0.00569 -0.00125 AFIX 43 H11A 2 0.187598 1.010771 -0.012751 11.00000 -1.20000 AFIX 0 C12 1 0.343465 0.962182 -0.039273 11.00000 0.05653 0.05729 = 0.03897 0.01037 -0.00483 -0.01978 AFIX 43 H12A 2 0.356199 1.001428 -0.077124 11.00000 -1.20000 AFIX 0 C13 1 0.423844 0.898548 -0.021764 11.00000 0.04244 0.06640 = 0.02813 -0.00641 0.00269 -0.01837 AFIX 43 H13A 2 0.492230 0.895295 -0.047669 11.00000 -1.20000 AFIX 0 C14 1 0.406317 0.837824 0.034233 11.00000 0.03749 0.05518 = 0.02677 -0.00756 0.00015 -0.00403 C15 1 0.496254 0.769447 0.052074 11.00000 0.05612 0.08987 = 0.05668 0.00339 0.02022 0.02274 AFIX 137 H15A 2 0.460969 0.711094 0.052578 11.00000 -1.50000 H15B 2 0.529973 0.782155 0.098504 11.00000 -1.50000 H15C 2 0.555989 0.770868 0.016677 11.00000 -1.50000 AFIX 0 C16 1 0.114540 0.921728 0.101380 11.00000 0.04212 0.07646 = 0.06076 0.02253 0.00598 0.01997 AFIX 137 H16A 2 0.070614 0.972171 0.083779 11.00000 -1.50000 H16B 2 0.136453 0.931624 0.150725 11.00000 -1.50000 H16C 2 0.067747 0.868520 0.097622 11.00000 -1.50000 AFIX 0 C26 1 0.525500 0.713605 0.391585 11.00000 0.04366 0.05227 = 0.03153 0.00920 -0.00723 -0.00503 AFIX 43 H26 2 0.543163 0.660329 0.415333 11.00000 -1.20000 AFIX 0 C27 1 0.605539 0.749463 0.344430 11.00000 0.03222 0.03851 = 0.02983 -0.00058 -0.00290 0.00502 C28 1 0.732704 0.732343 0.361428 11.00000 0.03727 0.06465 = 0.04013 0.01050 -0.00427 0.01237 AFIX 137 H28A 2 0.768983 0.706180 0.320391 11.00000 -1.50000 H28B 2 0.739485 0.691997 0.401441 11.00000 -1.50000 H28C 2 0.770522 0.787962 0.373265 11.00000 -1.50000 AFIX 0 C29 1 0.664392 0.855147 0.258821 11.00000 0.02565 0.03463 = 0.03660 0.00397 -0.00547 0.00087 C30 1 0.686550 0.938742 0.290409 11.00000 0.03549 0.04206 = 0.05603 -0.00491 -0.00814 -0.00188 C31 1 0.771642 0.993752 0.259847 11.00000 0.04716 0.03994 = 0.08302 -0.00286 -0.01310 -0.00849 AFIX 43 H31A 2 0.786896 1.049689 0.279978 11.00000 -1.20000 AFIX 0 C32 1 0.832588 0.967095 0.201241 11.00000 0.03877 0.05895 = 0.06850 0.01489 0.00274 -0.01194 AFIX 43 H32A 2 0.886710 1.005459 0.180927 11.00000 -1.20000 AFIX 0 C33 1 0.813744 0.883734 0.172510 11.00000 0.03356 0.06142 = 0.04686 0.01121 0.00148 -0.00522 AFIX 43 H33A 2 0.857248 0.865154 0.133589 11.00000 -1.20000 AFIX 0 C34 1 0.730169 0.826130 0.200748 11.00000 0.02628 0.04529 = 0.03351 0.00713 -0.00213 -0.00189 C35 1 0.722976 0.731887 0.172139 11.00000 0.03722 0.05390 = 0.04477 -0.00756 0.00878 0.00029 AFIX 137 H35A 2 0.650935 0.705071 0.186360 11.00000 -1.50000 H35B 2 0.787097 0.697394 0.191115 11.00000 -1.50000 H35C 2 0.726309 0.733077 0.120693 11.00000 -1.50000 AFIX 0 C36 1 0.623851 0.967027 0.357070 11.00000 0.06125 0.05131 = 0.06677 -0.02338 -0.00854 0.00099 AFIX 137 H36A 2 0.541678 0.957296 0.350378 11.00000 -1.50000 H36B 2 0.638112 1.029482 0.366082 11.00000 -1.50000 H36C 2 0.651815 0.932324 0.397222 11.00000 -1.50000 AFIX 0 C37 1 0.428209 0.650932 0.222676 11.00000 0.03071 0.03439 = 0.03862 -0.00707 -0.00443 0.00460 AFIX 33 H37A 2 0.362268 0.620853 0.201292 11.00000 -1.50000 H37B 2 0.449506 0.621973 0.267029 11.00000 -1.50000 H37C 2 0.492575 0.648527 0.190530 11.00000 -1.50000 AFIX 0 C38 1 0.427352 0.934397 0.201672 11.00000 0.03548 0.04084 = 0.03190 -0.00084 -0.00302 0.00391 AFIX 33 H38A 2 0.361249 0.959098 0.176295 11.00000 -1.50000 H38B 2 0.491586 0.929247 0.169630 11.00000 -1.50000 H38C 2 0.448734 0.973082 0.240938 11.00000 -1.50000 AFIX 0 PART 1 C4A 1 0.025184 0.672442 0.288886 21.00000 0.04640 AFIX 33 H4A1 2 0.023797 0.694725 0.337209 21.00000 -1.50000 H4A2 2 0.035334 0.608555 0.289673 21.00000 -1.50000 H4A3 2 -0.046985 0.686889 0.264710 21.00000 -1.50000 AFIX 0 C5A 1 0.124225 0.714863 0.249935 21.00000 0.04011 SAME n1B > n3B N1A 3 0.194881 0.780043 0.272446 21.00000 0.03111 C3A 1 0.155580 0.824092 0.339194 21.00000 0.02833 0.03343 = 0.03366 0.00611 0.00656 0.00481 AFIX 13 H3AA 2 0.131417 0.778131 0.373449 21.00000 -1.20000 AFIX 0 C2A 1 0.054493 0.891490 0.326938 21.00000 0.02979 0.04627 = 0.03860 0.00462 0.00101 0.00711 AFIX 23 H2AA 2 0.075731 0.934969 0.290728 21.00000 -1.20000 H2AB 2 -0.014680 0.859954 0.310082 21.00000 -1.20000 AFIX 0 C1A 1 0.029386 0.939462 0.397626 21.00000 0.04005 0.05151 = 0.04259 0.00576 0.01085 0.01349 AFIX 23 H1AA 2 -0.029194 0.985224 0.388774 21.00000 -1.20000 H1AB 2 -0.002613 0.896541 0.431062 21.00000 -1.20000 AFIX 0 C21A 1 0.136845 0.983154 0.432170 21.00000 0.05084 0.05010 = 0.03082 -0.00305 0.00981 0.01286 AFIX 23 H21A 2 0.162400 1.032436 0.402343 21.00000 -1.20000 H21B 2 0.116803 1.007316 0.478687 21.00000 -1.20000 AFIX 0 C22A 1 0.235232 0.916122 0.441373 21.00000 0.04348 0.05092 = 0.02761 0.00062 0.00152 0.00432 AFIX 23 H22A 2 0.213379 0.870327 0.475565 21.00000 -1.20000 H22B 2 0.304405 0.946252 0.459874 21.00000 -1.20000 AFIX 0 C23A 1 0.261113 0.872889 0.369243 21.00000 0.02998 0.03707 = 0.02484 0.00482 0.00273 0.00674 AFIX 13 H23A 2 0.271736 0.923611 0.336564 21.00000 -1.20000 AFIX 0 N3A 3 0.366142 0.817815 0.360319 21.00000 0.03164 C25A 1 0.417426 0.756437 0.404324 21.00000 0.03534 C24A 1 0.354679 0.733877 0.473423 21.00000 0.04397 AFIX 33 H24A 2 0.283775 0.767844 0.475617 21.00000 -1.50000 H24B 2 0.403920 0.748570 0.513943 21.00000 -1.50000 H24C 2 0.336815 0.671006 0.474238 21.00000 -1.50000 AFIX 0 PART 2 C5B 1 0.128999 0.739812 0.244673 -21.00000 0.05486 C4B 1 0.026161 0.726717 0.293977 -21.00000 0.06518 AFIX 33 H4B1 2 0.032982 0.767244 0.333869 -21.00000 -1.50000 H4B2 2 0.025677 0.666105 0.311315 -21.00000 -1.50000 H4B3 2 -0.045076 0.738539 0.267864 -21.00000 -1.50000 AFIX 0 N1B 3 0.192063 0.809509 0.272282 -21.00000 0.03242 C3B 1 0.192287 0.873389 0.334172 -21.00000 0.03268 0.03888 = 0.03098 0.00571 0.00656 0.00523 AFIX 13 H3BA 2 0.239701 0.924273 0.318733 -21.00000 -1.20000 AFIX 0 C2B 1 0.077000 0.914976 0.358751 -21.00000 0.02815 0.05872 = 0.03956 0.01364 0.00333 0.01343 AFIX 23 H2BA 2 0.036316 0.942540 0.318340 -21.00000 -1.20000 H2BB 2 0.027195 0.869006 0.378583 -21.00000 -1.20000 AFIX 0 C1B 1 0.106194 0.985733 0.416016 -21.00000 0.04571 0.05209 = 0.03613 0.00698 0.00923 0.02334 AFIX 23 H1BA 2 0.150683 1.033607 0.394349 -21.00000 -1.20000 H1BB 2 0.034323 1.011345 0.433411 -21.00000 -1.20000 AFIX 0 C21B 1 0.175923 0.947098 0.479395 -21.00000 0.05002 0.05196 = 0.03431 0.00264 0.01384 0.01256 AFIX 23 H21C 2 0.195423 0.994817 0.512892 -21.00000 -1.20000 H21D 2 0.128618 0.903509 0.504253 -21.00000 -1.20000 AFIX 0 C22B 1 0.286854 0.902563 0.454653 -21.00000 0.04267 0.04527 = 0.02768 0.00139 -0.00056 0.00380 AFIX 23 H22C 2 0.325715 0.873750 0.495166 -21.00000 -1.20000 H22D 2 0.339039 0.947590 0.435778 -21.00000 -1.20000 AFIX 0 C23B 1 0.259397 0.832461 0.396288 -21.00000 0.02751 0.03697 = 0.03001 0.00496 0.00427 0.00296 AFIX 13 H23B 2 0.212026 0.784811 0.417226 -21.00000 -1.20000 AFIX 0 N3B 3 0.361922 0.791510 0.363087 -21.00000 0.02504 C25B 1 0.410410 0.729609 0.405801 -21.00000 0.03606 C24B 1 0.364945 0.684359 0.472023 -21.00000 0.04558 AFIX 33 H24D 2 0.284687 0.700294 0.478138 -21.00000 -1.50000 H24E 2 0.409806 0.703451 0.513251 -21.00000 -1.50000 H24F 2 0.371393 0.620518 0.466847 -21.00000 -1.50000 PART 0 HKLF 4 ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 69.81 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.391 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.077 #=== END OF THE CIF FILE