# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1535 ######################################################################## ###### ### Crystallographic data associated with Chem. Commun. submission ### ######################################################################## #===================================================================== data_global #======================================================================= # SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Prof. Israel Goldberg School of Chemistry Tel-Aviv University Ramat-Aviv 69978 Tel-Aviv Israel ; _publ_contact_author_phone '972 3 6409965' _publ_contact_author_fax '972 3 6409293' _publ_contact_author_email goldberg@post.tau.ac.il _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; This CIF file contains the crystallographic data for compounds 2 & 4, the structural features of which are discussed in a manuscript submitted for a possible publication in Chemical Communications. The manuscript is entitled: "Novel zirconium complexes of amine bis(phenolate) ligands. Remarkable reactivity in polymerization of 1-hexene due to an extra donor arm" and co-authored by: E. Y. Tshuva, I. Goldberg, M. Kol, H. Weitman & Z. Goldschmidt ; #======================================================================= data_Compound-(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C48 H68 N2 O2 Zr . C5 H12' _chemical_formula_sum 'C53 H80 N2 O2 Zr' _chemical_formula_weight 868.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.4520(10) _cell_length_b 19.1310(10) _cell_length_c 28.2390(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9968.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 117 _cell_measurement_reflns_used 9375 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 25.7 _exptl_crystal_description 'plates' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 117 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi scans' _diffrn_detector_area_resol_mean '56 microns' _diffrn_reflns_number 9375 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.68 _reflns_number_total 9375 _reflns_number_gt 5867 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V' _computing_cell_refinement 'DENZO' _computing_data_reduction 'DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+73.2428P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9375 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.1028 _refine_ls_wR_factor_ref 0.2853 _refine_ls_wR_factor_gt 0.2636 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_mean 0.078 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.50635(3) 0.05735(3) 0.25897(3) 0.0337(2) Uani 1 d . . . O2 O 0.4747(3) 0.0711(2) 0.19207(19) 0.0421(12) Uani 1 d . . . O3 O 0.5471(3) 0.0779(2) 0.32286(17) 0.0375(12) Uani 1 d . . . C4 C 0.5242(4) 0.2081(3) 0.2053(3) 0.0382(17) Uani 1 d . . . H4A H 0.5467 0.2535 0.2013 0.046 Uiso 1 calc . . . H4B H 0.4766 0.2157 0.2190 0.046 Uiso 1 calc . . . C5 C 0.5682(4) 0.2108(3) 0.2848(3) 0.0396(17) Uani 1 d . . . H5A H 0.5182 0.2161 0.2947 0.048 Uiso 1 calc . . . H5B H 0.5860 0.2569 0.2765 0.048 Uiso 1 calc . . . N6 N 0.5690(3) 0.1667(3) 0.2407(2) 0.0361(13) Uani 1 d . . . C7 C 0.6440(4) 0.1589(4) 0.2232(3) 0.0441(18) Uani 1 d . . . H7A H 0.6450 0.1764 0.1903 0.050 Uiso 1 d . . . H7B H 0.6753 0.1895 0.2413 0.050 Uiso 1 d . . . C8' C 0.6795(8) 0.0966(8) 0.2395(6) 0.045(4) Uiso 0.50 d P . . C8" C 0.6586(9) 0.0933(9) 0.1990(6) 0.050(4) Uiso 0.50 d P . . N9 N 0.6372(3) 0.0321(3) 0.2301(3) 0.0454(16) Uani 1 d . . . C10 C 0.6824(9) -0.0074(9) 0.2652(6) 0.133(5) Uiso 1 d . . . C11 C 0.6394(8) -0.0145(8) 0.1895(5) 0.120(5) Uiso 1 d . . . C12 C 0.3902(4) 0.0680(4) 0.2881(3) 0.047(2) Uani 1 d . . . H12A H 0.3549 0.0532 0.2647 0.056 Uiso 1 calc . . . H12B H 0.3840 0.0400 0.3164 0.056 Uiso 1 calc . . . C13 C 0.3818(4) 0.1430(4) 0.2989(3) 0.045(2) Uani 1 d . . . C14 C 0.3586(5) 0.1919(4) 0.2661(3) 0.052(2) Uani 1 d . . . H14 H 0.3432 0.1762 0.2366 0.063 Uiso 1 calc . . . C15 C 0.3570(6) 0.2619(6) 0.2748(5) 0.076(3) Uani 1 d . . . H15 H 0.3422 0.2932 0.2516 0.091 Uiso 1 calc . . . C16 C 0.3781(7) 0.2853(5) 0.3191(6) 0.093(4) Uani 1 d . . . H16 H 0.3771 0.3331 0.3254 0.112 Uiso 1 calc . . . C17 C 0.4004(6) 0.2409(5) 0.3538(4) 0.076(3) Uani 1 d . . . H17 H 0.4143 0.2577 0.3833 0.092 Uiso 1 calc . . . C18 C 0.4019(5) 0.1687(5) 0.3437(3) 0.056(2) Uani 1 d . . . H18 H 0.4164 0.1376 0.3671 0.068 Uiso 1 calc . . . C19 C 0.5021(4) -0.0602(3) 0.2569(3) 0.0402(18) Uani 1 d . . . H19A H 0.5023 -0.0749 0.2240 0.048 Uiso 1 calc . . . H19B H 0.5459 -0.0782 0.2715 0.048 Uiso 1 calc . . . C20 C 0.4399(4) -0.0922(4) 0.2803(3) 0.0443(19) Uani 1 d . . . C21 C 0.4305(5) -0.1018(4) 0.3293(4) 0.059(2) Uani 1 d . . . H21 H 0.4683 -0.0915 0.3499 0.071 Uiso 1 calc . . . C22 C 0.3662(6) -0.1262(5) 0.3468(4) 0.071(3) Uani 1 d . . . H22 H 0.3607 -0.1310 0.3794 0.085 Uiso 1 calc . . . C23 C 0.3103(5) -0.1435(5) 0.3179(5) 0.073(3) Uani 1 d . . . H23 H 0.2672 -0.1609 0.3302 0.087 Uiso 1 calc . . . C24 C 0.3186(5) -0.1348(4) 0.2700(5) 0.070(3) Uani 1 d . . . H24 H 0.2810 -0.1465 0.2496 0.084 Uiso 1 calc . . . C25 C 0.3830(5) -0.1087(4) 0.2520(3) 0.056(2) Uani 1 d . . . H25 H 0.3873 -0.1023 0.2195 0.068 Uiso 1 calc . . . C26 C 0.4828(4) 0.1097(4) 0.1522(3) 0.0360(16) Uani 1 d . . . C27 C 0.4596(4) 0.0853(4) 0.1081(3) 0.0446(19) Uani 1 d . . . C28 C 0.4741(4) 0.1271(4) 0.0687(3) 0.0448(19) Uani 1 d . . . H28 H 0.4599 0.1111 0.0390 0.054 Uiso 1 calc . . . C29 C 0.5093(4) 0.1929(4) 0.0716(3) 0.0442(19) Uani 1 d . . . C30 C 0.5270(4) 0.2156(4) 0.1170(3) 0.0382(17) Uani 1 d . . . H30 H 0.5484 0.2593 0.1207 0.046 Uiso 1 calc . . . C31 C 0.5141(4) 0.1759(4) 0.1565(2) 0.0361(16) Uani 1 d . . . C32 C 0.4169(5) 0.0159(4) 0.1031(3) 0.058(2) Uani 1 d . . . C33 C 0.3933(7) 0.0039(5) 0.0513(4) 0.080(3) Uani 1 d . . . H33A H 0.3676 0.0442 0.0401 0.120 Uiso 1 calc R . . H33B H 0.3622 -0.0363 0.0497 0.120 Uiso 1 calc R . . H33C H 0.4353 -0.0037 0.0320 0.120 Uiso 1 calc R . . C34 C 0.3481(5) 0.0206(5) 0.1332(4) 0.067(3) Uani 1 d . . . H34A H 0.3612 0.0266 0.1659 0.101 Uiso 1 calc R . . H34B H 0.3205 -0.0217 0.1297 0.101 Uiso 1 calc R . . H34C H 0.3196 0.0597 0.1230 0.101 Uiso 1 calc R . . C35 C 0.4639(5) -0.0458(4) 0.1189(4) 0.062(3) Uani 1 d . . . H35A H 0.5078 -0.0465 0.1006 0.093 Uiso 1 calc R . . H35B H 0.4379 -0.0886 0.1141 0.093 Uiso 1 calc R . . H35C H 0.4755 -0.0408 0.1519 0.093 Uiso 1 calc R . . C36 C 0.5258(5) 0.2383(4) 0.0280(3) 0.049(2) Uani 1 d . . . C37 C 0.4972(7) 0.2084(6) -0.0175(3) 0.085(3) Uani 1 d . . . H37A H 0.5262 0.1690 -0.0267 0.128 Uiso 1 calc R . . H37B H 0.4991 0.2434 -0.0418 0.128 Uiso 1 calc R . . H37C H 0.4479 0.1937 -0.0130 0.128 Uiso 1 calc R . . C38 C 0.4938(5) 0.3101(5) 0.0349(3) 0.064(3) Uani 1 d . . . H38A H 0.4421 0.3064 0.0378 0.096 Uiso 1 calc R . . H38B H 0.5055 0.3390 0.0082 0.096 Uiso 1 calc R . . H38C H 0.5133 0.3306 0.0632 0.096 Uiso 1 calc R . . C39 C 0.6081(5) 0.2464(5) 0.0246(4) 0.071(3) Uani 1 d . . . H39A H 0.6255 0.2716 0.0517 0.107 Uiso 1 calc R . . H39B H 0.6202 0.2715 -0.0037 0.107 Uiso 1 calc R . . H39C H 0.6302 0.2010 0.0237 0.107 Uiso 1 calc R . . C40 C 0.5943(4) 0.1194(3) 0.3471(3) 0.0363(17) Uani 1 d . . . C41 C 0.6246(4) 0.0994(3) 0.3898(3) 0.0372(17) Uani 1 d . . . C42 C 0.6777(4) 0.1437(4) 0.4088(3) 0.0408(18) Uani 1 d . . . H42 H 0.6997 0.1304 0.4370 0.049 Uiso 1 calc . . . C43 C 0.6995(4) 0.2064(4) 0.3881(3) 0.0370(17) Uani 1 d . . . C44 C 0.6622(4) 0.2259(4) 0.3472(3) 0.0400(18) Uani 1 d . . . H44 H 0.6728 0.2689 0.3336 0.048 Uiso 1 calc . . . C45 C 0.6112(4) 0.1850(3) 0.3266(3) 0.0375(17) Uani 1 d . . . C46 C 0.6012(4) 0.0316(4) 0.4161(3) 0.046(2) Uani 1 d . . . C47 C 0.6213(5) -0.0320(4) 0.3862(3) 0.050(2) Uani 1 d . . . H47A H 0.6723 -0.0312 0.3796 0.076 Uiso 1 calc R . . H47B H 0.5947 -0.0310 0.3570 0.076 Uiso 1 calc R . . H47C H 0.6095 -0.0739 0.4033 0.076 Uiso 1 calc R . . C48 C 0.5182(4) 0.0331(5) 0.4238(3) 0.053(2) Uani 1 d . . . H48A H 0.5045 -0.0044 0.4445 0.080 Uiso 1 calc R . . H48B H 0.4942 0.0277 0.3939 0.080 Uiso 1 calc R . . H48C H 0.5046 0.0769 0.4377 0.080 Uiso 1 calc R . . C49 C 0.6371(5) 0.0245(5) 0.4640(3) 0.058(2) Uani 1 d . . . H49A H 0.6245 0.0640 0.4834 0.087 Uiso 1 calc R . . H49B H 0.6887 0.0228 0.4601 0.087 Uiso 1 calc R . . H49C H 0.6207 -0.0176 0.4791 0.087 Uiso 1 calc R . . C50 C 0.7598(4) 0.2524(4) 0.4079(3) 0.0383(17) Uani 1 d . . . C51 C 0.8226(4) 0.2551(5) 0.3718(3) 0.055(2) Uani 1 d . . . H51A H 0.8608 0.2840 0.3840 0.082 Uiso 1 calc R . . H51B H 0.8053 0.2743 0.3425 0.082 Uiso 1 calc R . . H51C H 0.8407 0.2087 0.3665 0.082 Uiso 1 calc R . . C52 C 0.7303(5) 0.3259(4) 0.4167(3) 0.054(2) Uani 1 d . . . H52A H 0.6881 0.3232 0.4365 0.082 Uiso 1 calc R . . H52B H 0.7175 0.3470 0.3870 0.082 Uiso 1 calc R . . H52C H 0.7666 0.3537 0.4321 0.082 Uiso 1 calc R . . C53 C 0.7906(5) 0.2245(4) 0.4546(3) 0.055(2) Uani 1 d . . . H53A H 0.8253 0.2571 0.4670 0.082 Uiso 1 calc R . . H53B H 0.8137 0.1803 0.4492 0.082 Uiso 1 calc R . . H53C H 0.7519 0.2186 0.4771 0.082 Uiso 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 0.0333(4) 0.0204(3) 0.0473(4) 0.0019(3) 0.0000(3) -0.0018(3) O2 0.044(3) 0.031(3) 0.052(3) -0.001(2) -0.001(2) -0.006(2) O3 0.041(3) 0.025(2) 0.047(3) 0.003(2) -0.001(2) -0.003(2) C4 0.048(4) 0.018(3) 0.049(4) 0.004(3) 0.002(3) -0.001(3) C5 0.059(5) 0.016(3) 0.044(4) -0.002(3) -0.005(4) -0.005(3) N6 0.034(3) 0.027(3) 0.047(4) 0.005(3) 0.004(3) 0.002(2) C7 0.044(4) 0.034(4) 0.055(5) 0.004(3) 0.006(4) -0.008(3) N9 0.037(3) 0.027(3) 0.072(5) 0.001(3) 0.003(3) 0.002(3) C12 0.033(4) 0.031(4) 0.077(6) -0.002(4) 0.004(4) 0.000(3) C13 0.029(4) 0.032(4) 0.073(6) 0.012(4) 0.008(4) 0.006(3) C14 0.045(5) 0.047(5) 0.064(6) 0.007(4) 0.000(4) 0.007(4) C15 0.065(6) 0.059(6) 0.104(9) 0.016(6) 0.017(6) 0.020(5) C16 0.087(8) 0.034(5) 0.159(13) -0.008(7) 0.035(8) 0.007(5) C17 0.084(7) 0.052(6) 0.093(8) -0.020(6) 0.024(6) 0.011(5) C18 0.067(6) 0.053(5) 0.050(5) -0.002(4) 0.007(4) 0.013(5) C19 0.050(4) 0.008(3) 0.062(5) -0.011(3) 0.027(4) -0.013(3) C20 0.040(4) 0.023(4) 0.070(6) 0.000(4) 0.002(4) 0.001(3) C21 0.063(6) 0.028(4) 0.086(7) 0.009(4) 0.009(5) 0.011(4) C22 0.067(7) 0.045(5) 0.100(8) 0.005(5) 0.011(6) 0.012(5) C23 0.055(6) 0.040(5) 0.123(10) 0.002(6) 0.020(6) 0.008(4) C24 0.047(5) 0.032(5) 0.130(10) -0.013(5) 0.002(6) 0.008(4) C25 0.057(5) 0.027(4) 0.085(7) -0.006(4) -0.005(5) 0.003(4) C26 0.043(4) 0.029(4) 0.036(4) 0.002(3) 0.000(3) -0.007(3) C27 0.051(5) 0.027(4) 0.055(5) 0.001(4) -0.004(4) -0.003(3) C28 0.046(4) 0.052(5) 0.037(4) -0.004(4) -0.005(3) 0.002(4) C29 0.045(4) 0.037(4) 0.051(5) 0.003(3) 0.005(4) -0.002(3) C30 0.041(4) 0.035(4) 0.039(4) -0.004(3) -0.001(3) -0.003(3) C31 0.039(4) 0.035(4) 0.034(4) 0.000(3) -0.002(3) 0.004(3) C32 0.079(6) 0.032(4) 0.061(6) 0.000(4) -0.019(5) -0.027(4) C33 0.120(9) 0.050(5) 0.071(7) 0.005(5) -0.025(6) -0.018(6) C34 0.066(6) 0.046(5) 0.090(7) 0.010(5) -0.021(5) -0.021(5) C35 0.079(6) 0.026(4) 0.083(7) -0.003(4) -0.020(5) -0.007(4) C36 0.070(5) 0.046(5) 0.031(4) -0.002(3) 0.007(4) -0.007(4) C37 0.125(10) 0.085(8) 0.045(6) -0.008(5) 0.010(6) -0.022(7) C38 0.076(6) 0.061(6) 0.055(6) 0.022(4) 0.013(5) -0.010(5) C39 0.060(6) 0.086(7) 0.068(6) 0.017(5) 0.028(5) -0.006(5) C40 0.041(4) 0.023(3) 0.045(4) 0.000(3) 0.005(3) -0.004(3) C41 0.042(4) 0.023(3) 0.047(5) 0.006(3) -0.004(3) 0.004(3) C42 0.043(4) 0.034(4) 0.046(5) 0.002(3) -0.001(3) 0.009(3) C43 0.044(4) 0.030(4) 0.037(4) -0.003(3) 0.005(3) -0.005(3) C44 0.045(4) 0.026(4) 0.049(5) 0.001(3) 0.005(4) -0.006(3) C45 0.043(4) 0.023(3) 0.047(5) 0.003(3) -0.001(3) -0.002(3) C46 0.055(5) 0.037(4) 0.046(5) 0.015(4) -0.003(4) -0.010(4) C47 0.056(5) 0.023(4) 0.072(6) 0.012(4) -0.006(4) -0.005(4) C48 0.055(5) 0.052(5) 0.052(5) 0.014(4) -0.006(4) -0.010(4) C49 0.074(6) 0.056(5) 0.044(5) 0.019(4) -0.012(4) -0.011(5) C50 0.036(4) 0.043(4) 0.036(4) 0.000(3) 0.000(3) -0.006(3) C51 0.044(5) 0.056(5) 0.064(6) -0.009(4) 0.003(4) -0.010(4) C52 0.061(5) 0.044(5) 0.059(6) 0.002(4) -0.002(4) -0.020(4) C53 0.050(5) 0.047(5) 0.067(6) 0.002(4) -0.007(4) -0.002(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 O3 1.994(5) . ? Zr1 O2 1.995(5) . ? Zr1 C19 2.250(6) . ? Zr1 C12 2.305(7) . ? Zr1 N6 2.446(6) . ? Zr1 N9 2.594(6) . ? O2 C26 1.356(8) . ? O3 C40 1.364(8) . ? C4 N6 1.519(9) . ? C4 C31 1.520(10) . ? C5 N6 1.503(9) . ? C5 C45 1.505(10) . ? N6 C7 1.477(9) . ? C7 C8" 1.454(18) . ? C7 C8' 1.435(17) . ? C8' C8" 1.21(2) . ? C8' N9 1.483(17) . ? C8" N9 1.515(18) . ? N9 C11 1.451(16) . ? N9 C10 1.501(18) . ? C12 C13 1.475(10) . ? C13 C14 1.385(11) . ? C13 C18 1.407(12) . ? C14 C15 1.360(13) . ? C15 C16 1.386(17) . ? C16 C17 1.359(17) . ? C17 C18 1.410(13) . ? C19 C20 1.459(10) . ? C20 C25 1.356(12) . ? C20 C21 1.406(12) . ? C21 C22 1.367(13) . ? C22 C23 1.359(15) . ? C23 C24 1.369(15) . ? C24 C25 1.385(13) . ? C26 C27 1.396(10) . ? C26 C31 1.397(10) . ? C27 C28 1.397(11) . ? C27 C32 1.550(10) . ? C28 C29 1.419(11) . ? C29 C30 1.391(11) . ? C29 C36 1.538(11) . ? C30 C31 1.372(10) . ? C32 C35 1.531(12) . ? C32 C34 1.530(14) . ? C32 C33 1.544(13) . ? C36 C39 1.528(12) . ? C36 C37 1.502(12) . ? C36 C38 1.508(12) . ? C40 C41 1.383(10) . ? C40 C45 1.417(9) . ? C41 C42 1.401(10) . ? C41 C46 1.555(10) . ? C42 C43 1.394(10) . ? C43 C44 1.394(10) . ? C43 C50 1.525(10) . ? C44 C45 1.355(10) . ? C46 C49 1.513(11) . ? C46 C47 1.528(11) . ? C46 C48 1.546(11) . ? C50 C53 1.532(11) . ? C50 C52 1.528(11) . ? C50 C51 1.545(11) . ? 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 O3 Zr1 O2 160.31(19) . . ? O3 Zr1 C19 103.5(2) . . ? O2 Zr1 C19 95.5(3) . . ? O3 Zr1 C12 90.6(3) . . ? O2 Zr1 C12 93.1(3) . . ? C19 Zr1 C12 93.7(2) . . ? O3 Zr1 N6 81.01(19) . . ? O2 Zr1 N6 80.00(19) . . ? C19 Zr1 N6 150.0(2) . . ? C12 Zr1 N6 116.1(2) . . ? O3 Zr1 N9 88.3(2) . . ? O2 Zr1 N9 89.9(2) . . ? C19 Zr1 N9 80.7(2) . . ? C12 Zr1 N9 173.9(2) . . ? N6 Zr1 N9 69.68(19) . . ? C26 O2 Zr1 145.7(4) . . ? C40 O3 Zr1 144.2(4) . . ? N6 C4 C31 116.9(6) . . ? N6 C5 C45 117.4(6) . . ? C7 N6 C5 110.1(6) . . ? C7 N6 C4 110.0(6) . . ? C5 N6 C4 104.3(5) . . ? C7 N6 Zr1 115.2(4) . . ? C5 N6 Zr1 107.5(4) . . ? C4 N6 Zr1 109.1(4) . . ? C8" C7 C8' 49.4(9) . . ? C8" C7 N6 114.8(8) . . ? C8' C7 N6 113.9(8) . . ? C8" C8' C7 66.1(11) . . ? C8" C8' N9 67.6(11) . . ? C7 C8' N9 113.1(11) . . ? C8' C8" N9 64.9(11) . . ? C8' C8" C7 64.5(11) . . ? N9 C8" C7 110.2(11) . . ? C8" N9 C11 90.6(10) . . ? C8" N9 C8' 47.5(8) . . ? C11 N9 C8' 129.6(10) . . ? C8" N9 C10 128.8(10) . . ? C11 N9 C10 101.3(9) . . ? C8' N9 C10 90.5(10) . . ? C8" N9 Zr1 106.3(7) . . ? C11 N9 Zr1 112.9(7) . . ? C8' N9 Zr1 106.1(7) . . ? C10 N9 Zr1 113.7(7) . . ? C13 C12 Zr1 104.9(5) . . ? C14 C13 C18 116.5(7) . . ? C14 C13 C12 123.5(8) . . ? C18 C13 C12 119.9(7) . . ? C15 C14 C13 123.4(9) . . ? C14 C15 C16 118.4(10) . . ? C17 C16 C15 122.1(9) . . ? C16 C17 C18 118.3(10) . . ? C17 C18 C13 121.2(9) . . ? C20 C19 Zr1 115.8(5) . . ? C25 C20 C21 117.0(8) . . ? C25 C20 C19 116.1(8) . . ? C21 C20 C19 126.7(8) . . ? C22 C21 C20 120.6(9) . . ? C23 C22 C21 121.6(11) . . ? C24 C23 C22 118.6(10) . . ? C23 C24 C25 120.2(10) . . ? C20 C25 C24 122.0(10) . . ? O2 C26 C27 121.7(6) . . ? O2 C26 C31 117.8(6) . . ? C27 C26 C31 120.5(7) . . ? C26 C27 C28 117.4(7) . . ? C26 C27 C32 121.5(7) . . ? C28 C27 C32 121.0(7) . . ? C27 C28 C29 123.3(7) . . ? C30 C29 C28 116.0(7) . . ? C30 C29 C36 121.0(7) . . ? C28 C29 C36 123.0(7) . . ? C31 C30 C29 122.4(7) . . ? C30 C31 C26 120.1(7) . . ? C30 C31 C4 119.4(6) . . ? C26 C31 C4 119.9(6) . . ? C35 C32 C34 110.7(8) . . ? C35 C32 C33 108.7(8) . . ? C34 C32 C33 107.5(8) . . ? C35 C32 C27 110.2(7) . . ? C34 C32 C27 108.7(7) . . ? C33 C32 C27 110.9(7) . . ? C39 C36 C37 109.6(8) . . ? C39 C36 C38 107.8(7) . . ? C37 C36 C38 108.6(8) . . ? C39 C36 C29 107.7(7) . . ? C37 C36 C29 113.6(7) . . ? C38 C36 C29 109.4(6) . . ? C41 C40 O3 122.3(6) . . ? C41 C40 C45 120.9(6) . . ? O3 C40 C45 116.8(6) . . ? C40 C41 C42 116.7(6) . . ? C40 C41 C46 122.3(6) . . ? C42 C41 C46 121.0(6) . . ? C43 C42 C41 124.1(7) . . ? C42 C43 C44 115.8(6) . . ? C42 C43 C50 123.5(7) . . ? C44 C43 C50 120.7(6) . . ? C45 C44 C43 123.0(6) . . ? C44 C45 C40 119.1(7) . . ? C44 C45 C5 121.0(6) . . ? C40 C45 C5 119.7(6) . . ? C49 C46 C47 108.5(7) . . ? C49 C46 C48 108.0(7) . . ? C47 C46 C48 109.4(7) . . ? C49 C46 C41 112.4(6) . . ? C47 C46 C41 109.5(6) . . ? C48 C46 C41 109.1(6) . . ? C53 C50 C52 108.3(7) . . ? C53 C50 C43 112.7(6) . . ? C52 C50 C43 109.3(6) . . ? C53 C50 C51 107.6(6) . . ? C52 C50 C51 110.1(6) . . ? C43 C50 C51 108.8(6) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 1.326 _refine_diff_density_min -1.537 _refine_diff_density_rms 0.114 #==== END #=================================================================== data_Compound-(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '(C47 H65 N O2 Zr).(C7 H16)' _chemical_formula_sum 'C54 H81 N O2 Zr' _chemical_formula_weight 867.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.48400(10) _cell_length_b 19.2970(4) _cell_length_c 24.5940(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.0480(10) _cell_angle_gamma 90.00 _cell_volume 4974.77(15) _cell_formula_units_Z 4 _cell_measurement_temperature 116 _cell_measurement_reflns_used 12508 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 28.74 _exptl_crystal_description 'parallelpiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.259 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 116 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. Phi & Omega scans - 187 frames' _diffrn_detector_area_resol_mean '56 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12508 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.74 _reflns_number_total 12508 _reflns_number_gt 10397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement 'Denzo' _computing_data_reduction 'Denzo' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+6.9977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12508 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.393 _refine_ls_shift/su_mean 0.063 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.212339(19) 0.163659(11) -0.099186(9) 0.02006(7) Uani 1 d . . . O2 O 0.26261(14) 0.07047(8) -0.12739(7) 0.0236(3) Uani 1 d . . . C3 C 0.3587(2) 0.03307(12) -0.14914(9) 0.0216(4) Uani 1 d . . . C4 C 0.3390(2) -0.02725(12) -0.18037(9) 0.0228(4) Uani 1 d . . . C5 C 0.4465(2) -0.05791(12) -0.20339(9) 0.0229(4) Uani 1 d . . . H5 H 0.4346 -0.0974 -0.2245 0.028 Uiso 1 calc R . . C6 C 0.5702(2) -0.03261(12) -0.19639(9) 0.0218(4) Uani 1 d . . . C7 C 0.5865(2) 0.02514(12) -0.16287(9) 0.0219(4) Uani 1 d . . . H7 H 0.6682 0.0423 -0.1563 0.026 Uiso 1 calc R . . C8 C 0.4831(2) 0.05747(11) -0.13922(9) 0.0206(4) Uani 1 d . . . C9 C 0.5040(2) 0.11602(12) -0.10036(9) 0.0223(4) Uani 1 d . . . H9A H 0.5945 0.1263 -0.0984 0.027 Uiso 1 calc R . . H9B H 0.4786 0.1011 -0.0645 0.027 Uiso 1 calc R . . N10 N 0.43322(17) 0.18146(10) -0.11450(8) 0.0208(4) Uani 1 d . . . C11 C 0.4871(2) 0.23583(12) -0.07732(10) 0.0250(5) Uani 1 d . . . H11A H 0.5790 0.2363 -0.0809 0.030 Uiso 1 calc R . . H11B H 0.4691 0.2227 -0.0402 0.030 Uiso 1 calc R . . C12 C 0.4380(2) 0.30814(12) -0.08673(9) 0.0241(5) Uani 1 d . . . C13 C 0.5237(2) 0.36245(13) -0.09186(10) 0.0272(5) Uani 1 d . . . H13 H 0.6105 0.3528 -0.0928 0.033 Uiso 1 calc R . . C14 C 0.4830(2) 0.43073(12) -0.09559(10) 0.0251(5) Uani 1 d . . . C15 C 0.3519(2) 0.44258(12) -0.09270(9) 0.0250(5) Uani 1 d . . . H15 H 0.3232 0.4882 -0.0941 0.030 Uiso 1 calc R . . C16 C 0.2612(2) 0.38981(12) -0.08780(9) 0.0229(4) Uani 1 d . . . C17 C 0.3063(2) 0.32107(12) -0.08623(9) 0.0217(4) Uani 1 d . . . O18 O 0.22803(14) 0.26520(8) -0.08423(7) 0.0229(3) Uani 1 d . . . C19 C 0.2056(2) -0.05907(12) -0.18839(10) 0.0266(5) Uani 1 d . . . C20 C 0.1214(2) -0.00862(14) -0.22137(11) 0.0308(5) Uani 1 d . . . H20A H 0.0380 -0.0283 -0.2267 0.046 Uiso 1 calc . . . H20B H 0.1590 -0.0004 -0.2561 0.046 Uiso 1 calc . . . H20C H 0.1145 0.0344 -0.2020 0.046 Uiso 1 calc . . . C21 C 0.1486(2) -0.07406(13) -0.13219(11) 0.0318(5) Uani 1 d . . . H21A H 0.0649 -0.0936 -0.1369 0.048 Uiso 1 calc . . . H21B H 0.1430 -0.0317 -0.1119 0.048 Uiso 1 calc . . . H21C H 0.2024 -0.1062 -0.1128 0.048 Uiso 1 calc . . . C22 C 0.2079(2) -0.12799(14) -0.21949(13) 0.0366(6) Uani 1 d . . . H22A H 0.1223 -0.1449 -0.2244 0.055 Uiso 1 calc . . . H22B H 0.2573 -0.1613 -0.1992 0.055 Uiso 1 calc . . . H22C H 0.2454 -0.1210 -0.2544 0.055 Uiso 1 calc . . . C23 C 0.6864(2) -0.06549(12) -0.22305(10) 0.0244(5) Uani 1 d . . . C24 C 0.6509(2) -0.12729(14) -0.25928(11) 0.0323(5) Uani 1 d . . . H24A H 0.5919 -0.1126 -0.2873 0.049 Uiso 1 calc . . . H24B H 0.6121 -0.1627 -0.2377 0.049 Uiso 1 calc . . . H24C H 0.7264 -0.1454 -0.2756 0.049 Uiso 1 calc . . . C25 C 0.7798(2) -0.09073(13) -0.17837(11) 0.0290(5) Uani 1 d . . . H25A H 0.8039 -0.0525 -0.1555 0.043 Uiso 1 calc . . . H25B H 0.8544 -0.1098 -0.1948 0.043 Uiso 1 calc . . . H25C H 0.7393 -0.1257 -0.1569 0.043 Uiso 1 calc . . . C26 C 0.7518(3) -0.01045(14) -0.25791(11) 0.0342(6) Uani 1 d . . . H26A H 0.7742 0.0287 -0.2356 0.051 Uiso 1 calc . . . H26B H 0.6946 0.0040 -0.2866 0.051 Uiso 1 calc . . . H26C H 0.8275 -0.0297 -0.2733 0.051 Uiso 1 calc . . . C27 C 0.4487(2) 0.20014(12) -0.17272(9) 0.0234(4) Uani 1 d . . . H27A H 0.3979 0.2412 -0.1803 0.028 Uiso 1 calc R . . H27B H 0.4139 0.1628 -0.1949 0.028 Uiso 1 calc R . . C28 C 0.5855(3) 0.21417(14) -0.19062(12) 0.0346(6) Uani 1 d . . . H28A H 0.6099 0.2609 -0.1802 0.042 Uiso 1 calc R . . H28B H 0.6431 0.1822 -0.1722 0.042 Uiso 1 calc R . . C29 C 0.5975(3) 0.20593(17) -0.25183(13) 0.0493(8) Uani 1 d . . . H29A H 0.6841 0.2145 -0.2619 0.074 Uiso 1 calc . . . H29B H 0.5421 0.2384 -0.2701 0.074 Uiso 1 calc . . . H29C H 0.5738 0.1596 -0.2622 0.074 Uiso 1 calc . . . C30 C 0.1182(2) 0.40624(13) -0.08280(10) 0.0270(5) Uani 1 d . . . C31 C 0.0428(2) 0.37570(13) -0.13116(11) 0.0308(5) Uani 1 d . . . H31A H -0.0461 0.3863 -0.1275 0.046 Uiso 1 calc . . . H31B H 0.0542 0.3263 -0.1319 0.046 Uiso 1 calc . . . H31C H 0.0731 0.3954 -0.1644 0.046 Uiso 1 calc . . . C32 C 0.0695(3) 0.37565(15) -0.02926(11) 0.0350(6) Uani 1 d . . . H32A H -0.0196 0.3860 -0.0259 0.052 Uiso 1 calc . . . H32B H 0.1163 0.3955 0.0008 0.052 Uiso 1 calc . . . H32C H 0.0814 0.3263 -0.0293 0.052 Uiso 1 calc . . . C33 C 0.0922(2) 0.48459(14) -0.08149(13) 0.0385(6) Uani 1 d . . . H33A H 0.0023 0.4925 -0.0781 0.058 Uiso 1 calc . . . H33B H 0.1212 0.5053 -0.1145 0.058 Uiso 1 calc . . . H33C H 0.1369 0.5049 -0.0510 0.058 Uiso 1 calc . . . C34 C 0.5801(2) 0.48997(14) -0.10241(10) 0.0312(5) Uani 1 d . . . C38 C 0.1661(2) 0.12984(15) -0.01330(10) 0.0322(5) Uani 1 d . . . H38A H 0.0930 0.1554 -0.0004 0.039 Uiso 1 calc R . . H38B H 0.1453 0.0809 -0.0129 0.039 Uiso 1 calc R . . C39 C 0.2789(2) 0.14336(14) 0.02266(10) 0.0282(5) Uani 1 d . . . C40 C 0.3014(3) 0.20864(15) 0.04553(11) 0.0381(6) Uani 1 d . . . H40 H 0.2429 0.2441 0.0393 0.046 Uiso 1 calc R . . C41 C 0.4092(4) 0.22143(18) 0.07725(12) 0.0493(8) Uani 1 d . . . H41 H 0.4223 0.2653 0.0920 0.059 Uiso 1 calc R . . C42 C 0.4976(3) 0.16965(18) 0.08713(13) 0.0492(8) Uani 1 d . . . H42 H 0.5697 0.1785 0.1086 0.059 Uiso 1 calc R . . C43 C 0.4782(3) 0.10500(17) 0.06505(12) 0.0419(7) Uani 1 d . . . H43 H 0.5375 0.0700 0.0715 0.050 Uiso 1 calc R . . C44 C 0.3700(2) 0.09177(14) 0.03303(10) 0.0315(5) Uani 1 d . . . H44 H 0.3580 0.0478 0.0183 0.038 Uiso 1 calc R . . C45 C 0.0450(2) 0.17644(13) -0.15963(10) 0.0263(5) Uani 1 d . . . H45A H 0.0306 0.2240 -0.1710 0.032 Uiso 1 calc R . . H45B H 0.0490 0.1457 -0.1908 0.032 Uiso 1 calc R . . C46 C -0.0430(2) 0.15253(13) -0.11726(10) 0.0253(5) Uani 1 d . . . C47 C -0.0571(2) 0.08138(13) -0.10686(10) 0.0284(5) Uani 1 d . . . H47 H -0.0196 0.0497 -0.1301 0.034 Uiso 1 calc R . . C48 C -0.1252(2) 0.05680(16) -0.06293(11) 0.0356(6) Uani 1 d . . . H48 H -0.1331 0.0094 -0.0572 0.043 Uiso 1 calc R . . C49 C -0.1813(3) 0.10315(18) -0.02762(11) 0.0399(7) Uani 1 d . . . H49 H -0.2264 0.0871 0.0020 0.048 Uiso 1 calc R . . C50 C -0.1696(3) 0.17321(17) -0.03683(12) 0.0401(7) Uani 1 d . . . H50 H -0.2077 0.2043 -0.0133 0.048 Uiso 1 calc R . . C51 C -0.1017(2) 0.19827(15) -0.08077(11) 0.0334(6) Uani 1 d . . . H51 H -0.0950 0.2458 -0.0861 0.040 Uiso 1 calc R . . C35A C 0.6565(4) 0.4740(2) -0.15363(18) 0.0341(9) Uiso 0.60 d P . . C36A C 0.5222(5) 0.5585(3) -0.1032(2) 0.0383(10) Uiso 0.60 d P . . C37A C 0.6784(5) 0.4845(3) -0.05243(19) 0.0375(10) Uiso 0.60 d P . . C35B C 0.5826(8) 0.5384(4) -0.0522(3) 0.0457(17) Uiso 0.40 d P . . C36B C 0.5303(8) 0.5447(4) -0.1520(3) 0.0459(18) Uiso 0.40 d P . . C37B C 0.7124(8) 0.4724(5) -0.1190(4) 0.0495(19) Uiso 0.40 d P . . C52A C 0.2705(6) 0.8341(3) 0.4530(3) 0.0435(13) Uiso 0.50 d P . . C53A C 0.2623(6) 0.7958(4) 0.3995(3) 0.0474(14) Uiso 0.50 d P . . C54A C 0.1514(6) 0.8192(3) 0.3660(3) 0.0459(14) Uiso 0.50 d P . . C55' C 0.0186(9) 0.7792(5) 0.3893(4) 0.037(2) Uiso 0.30 d P . . C55A C 0.0193(14) 0.8199(8) 0.3973(6) 0.038(3) Uiso 0.20 d P . . C56A C -0.0965(15) 0.8454(8) 0.3587(6) 0.128(5) Uiso 0.50 d P . . C57A C -0.1032(14) 0.7861(8) 0.3246(6) 0.128(4) Uiso 0.50 d P . . C58A C -0.2327(11) 0.8114(6) 0.2883(5) 0.091(3) Uiso 0.50 d P . . C52B C 0.2777(11) 0.8419(6) 0.4753(5) 0.088(3) Uiso 0.50 d P . . C53B C 0.2554(11) 0.8164(6) 0.4224(5) 0.097(3) Uiso 0.50 d P . . C54B C 0.1059(10) 0.8126(6) 0.4080(5) 0.087(3) Uiso 0.50 d P . . C55B C 0.1031(12) 0.7931(7) 0.3509(5) 0.104(4) Uiso 0.50 d P . . C56B C -0.0614(12) 0.7746(7) 0.3400(5) 0.096(4) Uiso 0.50 d P . . C57B C -0.1305(6) 0.8472(3) 0.3244(2) 0.0393(12) Uiso 0.50 d P . . C58B C -0.2534(7) 0.8418(4) 0.2910(3) 0.0559(17) Uiso 0.50 d P . . 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 0.01650(11) 0.02202(11) 0.02173(11) 0.00128(8) 0.00233(7) 0.00090(8) O2 0.0173(7) 0.0227(8) 0.0310(8) -0.0006(7) 0.0036(6) 0.0010(6) C3 0.0182(10) 0.0227(10) 0.0240(10) 0.0034(9) 0.0022(8) 0.0028(8) C4 0.0180(10) 0.0235(10) 0.0268(11) 0.0016(9) -0.0017(8) -0.0005(8) C5 0.0212(10) 0.0230(10) 0.0245(11) 0.0001(9) -0.0027(8) 0.0005(8) C6 0.0203(10) 0.0226(10) 0.0226(10) 0.0011(8) 0.0012(8) 0.0019(8) C7 0.0173(10) 0.0236(10) 0.0248(10) 0.0030(9) -0.0007(8) 0.0009(8) C8 0.0197(10) 0.0197(10) 0.0224(10) 0.0009(8) -0.0022(8) 0.0010(8) C9 0.0193(10) 0.0229(10) 0.0245(10) -0.0009(9) -0.0022(8) 0.0037(8) N10 0.0194(9) 0.0215(9) 0.0213(9) -0.0012(7) -0.0005(7) 0.0018(7) C11 0.0192(10) 0.0269(11) 0.0286(11) -0.0086(9) -0.0051(9) 0.0031(9) C12 0.0207(10) 0.0265(11) 0.0250(11) -0.0082(9) -0.0006(8) 0.0019(9) C13 0.0189(10) 0.0315(12) 0.0312(12) -0.0111(10) 0.0007(9) -0.0012(9) C14 0.0221(11) 0.0277(11) 0.0254(11) -0.0092(9) 0.0014(9) -0.0035(9) C15 0.0246(11) 0.0249(11) 0.0256(11) -0.0047(9) 0.0029(9) 0.0009(9) C16 0.0203(10) 0.0260(11) 0.0224(10) -0.0032(9) 0.0029(8) 0.0011(8) C17 0.0211(10) 0.0233(10) 0.0206(10) -0.0028(8) 0.0020(8) -0.0006(8) O18 0.0192(7) 0.0229(8) 0.0267(8) -0.0006(6) 0.0034(6) -0.0001(6) C19 0.0191(10) 0.0246(11) 0.0359(13) -0.0028(10) -0.0016(9) -0.0030(9) C20 0.0207(11) 0.0364(13) 0.0350(13) -0.0027(11) -0.0026(9) -0.0003(10) C21 0.0231(11) 0.0294(12) 0.0429(14) 0.0026(11) 0.0010(10) -0.0040(9) C22 0.0248(12) 0.0312(13) 0.0537(17) -0.0116(12) -0.0023(11) -0.0042(10) C23 0.0201(10) 0.0258(11) 0.0273(11) -0.0024(9) 0.0023(9) 0.0004(8) C24 0.0253(12) 0.0338(13) 0.0380(14) -0.0121(11) 0.0031(10) -0.0002(10) C25 0.0227(11) 0.0299(12) 0.0343(13) -0.0024(10) 0.0001(9) 0.0054(9) C26 0.0336(13) 0.0350(13) 0.0345(13) 0.0003(11) 0.0107(10) 0.0020(11) C27 0.0254(11) 0.0221(10) 0.0227(10) -0.0013(9) 0.0021(8) -0.0009(8) C28 0.0318(13) 0.0310(13) 0.0416(15) -0.0013(11) 0.0139(11) -0.0051(10) C29 0.058(2) 0.0451(17) 0.0456(17) 0.0022(14) 0.0301(15) 0.0020(14) C30 0.0191(11) 0.0252(11) 0.0370(13) -0.0018(10) 0.0064(9) 0.0016(9) C31 0.0217(11) 0.0295(12) 0.0411(14) 0.0029(11) -0.0008(10) 0.0007(9) C32 0.0304(13) 0.0375(14) 0.0375(14) -0.0019(12) 0.0130(11) 0.0026(11) C33 0.0234(12) 0.0280(13) 0.0642(19) -0.0043(13) 0.0092(12) 0.0034(10) C34 0.0256(12) 0.0356(13) 0.0325(13) -0.0103(11) 0.0043(10) -0.0095(10) C38 0.0248(12) 0.0448(15) 0.0270(12) 0.0084(11) 0.0010(9) -0.0012(11) C39 0.0286(12) 0.0356(13) 0.0205(11) 0.0072(10) 0.0032(9) 0.0000(10) C40 0.0492(17) 0.0383(15) 0.0268(12) 0.0022(11) 0.0001(11) 0.0062(12) C41 0.071(2) 0.0454(17) 0.0311(15) -0.0004(13) -0.0063(14) -0.0113(16) C42 0.0500(18) 0.061(2) 0.0359(15) 0.0137(15) -0.0171(13) -0.0162(15) C43 0.0340(14) 0.0526(18) 0.0389(15) 0.0226(14) -0.0030(12) 0.0027(12) C44 0.0343(13) 0.0317(13) 0.0287(12) 0.0089(10) 0.0034(10) -0.0014(10) C45 0.0216(11) 0.0263(11) 0.0309(12) 0.0014(9) -0.0010(9) 0.0010(9) C46 0.0160(10) 0.0299(12) 0.0298(12) -0.0031(9) -0.0047(9) 0.0002(8) C47 0.0246(11) 0.0308(12) 0.0297(12) -0.0029(10) 0.0007(9) -0.0011(9) C48 0.0295(13) 0.0423(15) 0.0349(14) 0.0024(12) 0.0008(10) -0.0077(11) C49 0.0267(13) 0.0620(19) 0.0311(13) -0.0023(13) 0.0027(10) -0.0072(12) C50 0.0252(13) 0.0564(18) 0.0386(15) -0.0156(13) 0.0019(11) 0.0040(12) C51 0.0235(12) 0.0349(14) 0.0416(14) -0.0091(12) -0.0014(10) 0.0032(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O18 1.9999(16) . ? Zr1 O2 2.0015(16) . ? Zr1 C38 2.272(2) . ? Zr1 C45 2.292(2) . ? Zr1 N10 2.3779(19) . ? Zr1 C46 2.714(2) . ? O2 C3 1.357(3) . ? C3 C4 1.408(3) . ? C3 C8 1.404(3) . ? C4 C5 1.401(3) . ? C4 C19 1.537(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9300 . ? C6 C7 1.395(3) . ? C6 C23 1.532(3) . ? C7 C8 1.387(3) . ? C7 H7 0.9300 . ? C8 C9 1.493(3) . ? C9 N10 1.502(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? N10 C27 1.488(3) . ? N10 C11 1.496(3) . ? C11 C12 1.504(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.388(3) . ? C12 C17 1.403(3) . ? C13 C14 1.387(3) . ? C13 H13 0.9300 . ? C14 C15 1.396(3) . ? C14 C34 1.541(3) . ? C15 C16 1.400(3) . ? C15 H15 0.9300 . ? C16 C17 1.408(3) . ? C16 C30 1.539(3) . ? C17 O18 1.356(3) . ? C19 C20 1.536(4) . ? C19 C22 1.535(4) . ? C19 C21 1.543(4) . ? C20 H20A 0.9597 . ? C20 H20B 0.9604 . ? C20 H20C 0.9599 . ? C21 H21A 0.9602 . ? C21 H21B 0.9602 . ? C21 H21C 0.9599 . ? C22 H22A 0.9599 . ? C22 H22B 0.9594 . ? C22 H22C 0.9611 . ? C23 C24 1.531(3) . ? C23 C26 1.534(4) . ? C23 C25 1.537(3) . ? C24 H24A 0.9598 . ? C24 H24B 0.9605 . ? C24 H24C 0.9599 . ? C25 H25A 0.9603 . ? C25 H25B 0.9599 . ? C25 H25C 0.9601 . ? C26 H26A 0.9597 . ? C26 H26B 0.9605 . ? C26 H26C 0.9598 . ? C27 C28 1.532(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.521(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9598 . ? C29 H29B 0.9600 . ? C29 H29C 0.9604 . ? C30 C31 1.534(4) . ? C30 C33 1.537(4) . ? C30 C32 1.539(4) . ? C31 H31A 0.9601 . ? C31 H31B 0.9599 . ? C31 H31C 0.9599 . ? C32 H32A 0.9599 . ? C32 H32B 0.9598 . ? C32 H32C 0.9603 . ? C33 H33A 0.9600 . ? C33 H33B 0.9603 . ? C33 H33C 0.9601 . ? C34 C36A 1.455(5) . ? C34 C37B 1.493(9) . ? C34 C35A 1.537(5) . ? C34 C35B 1.548(9) . ? C34 C37A 1.593(5) . ? C34 C36B 1.689(8) . ? C38 C39 1.487(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.398(4) . ? C39 C44 1.400(4) . ? C40 C41 1.384(4) . ? C40 H40 0.9300 . ? C41 C42 1.381(5) . ? C41 H41 0.9300 . ? C42 C43 1.374(5) . ? C42 H42 0.9300 . ? C43 C44 1.393(4) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.479(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.405(3) . ? C46 C51 1.408(3) . ? C47 C48 1.389(4) . ? C47 H47 0.9300 . ? C48 C49 1.385(4) . ? C48 H48 0.9300 . ? C49 C50 1.377(4) . ? C49 H49 0.9300 . ? C50 C51 1.392(4) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52A C53A 1.511(9) . ? C53A C54A 1.483(9) . ? C54A C55A 1.597(16) . ? C55A C56A 1.61(2) . ? C56A C57A 1.420(19) . ? C57A C58A 1.683(18) . ? C52B C53B 1.407(15) . ? C53B C54B 1.601(16) . ? C54B C55B 1.456(16) . ? C55B C56B 1.777(18) . ? C56B C57B 1.620(15) . ? C57B C58B 1.519(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O18 Zr1 O2 157.33(6) . . ? O18 Zr1 C38 97.39(9) . . ? O2 Zr1 C38 97.25(9) . . ? O18 Zr1 C45 94.20(8) . . ? O2 Zr1 C45 94.31(8) . . ? C38 Zr1 C45 117.39(9) . . ? O18 Zr1 N10 79.08(6) . . ? O2 Zr1 N10 79.14(6) . . ? C38 Zr1 N10 114.45(8) . . ? C45 Zr1 N10 128.15(8) . . ? O18 Zr1 C46 100.67(7) . . ? O2 Zr1 C46 97.89(7) . . ? C38 Zr1 C46 84.42(8) . . ? C45 Zr1 C46 33.00(8) . . ? N10 Zr1 C46 161.08(7) . . ? C3 O2 Zr1 144.74(14) . . ? O2 C3 C4 123.5(2) . . ? O2 C3 C8 116.6(2) . . ? C4 C3 C8 119.9(2) . . ? C5 C4 C3 117.3(2) . . ? C5 C4 C19 121.1(2) . . ? C3 C4 C19 121.6(2) . . ? C6 C5 C4 123.8(2) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C5 C6 C7 117.2(2) . . ? C5 C6 C23 123.2(2) . . ? C7 C6 C23 119.6(2) . . ? C8 C7 C6 121.3(2) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C3 120.4(2) . . ? C7 C8 C9 120.2(2) . . ? C3 C8 C9 119.3(2) . . ? C8 C9 N10 114.95(18) . . ? C8 C9 H9A 108.5 . . ? N10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? N10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C27 N10 C11 111.83(18) . . ? C27 N10 C9 111.37(17) . . ? C11 N10 C9 105.59(17) . . ? C27 N10 Zr1 108.11(13) . . ? C11 N10 Zr1 111.24(13) . . ? C9 N10 Zr1 108.68(13) . . ? N10 C11 C12 115.62(18) . . ? N10 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? N10 C11 H11B 108.4 . . ? C12 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C17 120.4(2) . . ? C13 C12 C11 119.6(2) . . ? C17 C12 C11 119.9(2) . . ? C14 C13 C12 121.6(2) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.0(2) . . ? C13 C14 C34 120.6(2) . . ? C15 C14 C34 122.4(2) . . ? C14 C15 C16 123.8(2) . . ? C14 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C15 C16 C17 117.3(2) . . ? C15 C16 C30 121.4(2) . . ? C17 C16 C30 121.2(2) . . ? O18 C17 C12 117.1(2) . . ? O18 C17 C16 123.2(2) . . ? C12 C17 C16 119.8(2) . . ? C17 O18 Zr1 145.08(14) . . ? C20 C19 C22 107.5(2) . . ? C20 C19 C4 109.11(19) . . ? C22 C19 C4 112.8(2) . . ? C20 C19 C21 111.3(2) . . ? C22 C19 C21 107.1(2) . . ? C4 C19 C21 109.0(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.4 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.4 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.4 . . ? H22B C22 H22C 109.4 . . ? C24 C23 C6 112.64(19) . . ? C24 C23 C26 108.7(2) . . ? C6 C23 C26 108.63(19) . . ? C24 C23 C25 108.3(2) . . ? C6 C23 C25 109.05(19) . . ? C26 C23 C25 109.5(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.4 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.4 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.4 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.4 . . ? N10 C27 C28 116.0(2) . . ? N10 C27 H27A 108.3 . . ? C28 C27 H27A 108.3 . . ? N10 C27 H27B 108.3 . . ? C28 C27 H27B 108.3 . . ? H27A C27 H27B 107.4 . . ? C29 C28 C27 111.1(2) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.4 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.4 . . ? C31 C30 C33 107.8(2) . . ? C31 C30 C16 110.36(19) . . ? C33 C30 C16 112.2(2) . . ? C31 C30 C32 110.0(2) . . ? C33 C30 C32 107.3(2) . . ? C16 C30 C32 109.2(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.4 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.4 . . ? C36A C34 C35A 113.3(3) . . ? C36A C34 C14 113.55(19) . . ? C37B C34 C14 118.6(3) . . ? C35A C34 C14 107.17(17) . . ? C37B C34 C35B 110.6(5) . . ? C14 C34 C35B 111.3(3) . . ? C36A C34 C37A 109.6(3) . . ? C35A C34 C37A 106.2(2) . . ? C14 C34 C37A 106.59(19) . . ? C37B C34 C36B 102.8(4) . . ? C14 C34 C36B 110.3(3) . . ? C35B C34 C36B 101.4(4) . . ? C39 C38 Zr1 108.75(16) . . ? C39 C38 H38A 109.9 . . ? Zr1 C38 H38A 109.9 . . ? C39 C38 H38B 109.9 . . ? Zr1 C38 H38B 109.9 . . ? H38A C38 H38B 108.3 . . ? C40 C39 C44 117.3(2) . . ? C40 C39 C38 121.6(2) . . ? C44 C39 C38 121.1(2) . . ? C41 C40 C39 121.2(3) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 121.2(3) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? C46 C45 Zr1 89.40(14) . . ? C46 C45 H45A 113.8 . . ? Zr1 C45 H45A 113.7 . . ? C46 C45 H45B 113.7 . . ? Zr1 C45 H45B 113.7 . . ? H45A C45 H45B 111.0 . . ? C47 C46 C51 116.6(2) . . ? C47 C46 C45 120.2(2) . . ? C51 C46 C45 122.6(2) . . ? C47 C46 Zr1 98.86(15) . . ? C51 C46 Zr1 106.69(15) . . ? C45 C46 Zr1 57.59(12) . . ? C48 C47 C46 122.2(2) . . ? C48 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C49 C48 C47 119.8(3) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C50 C49 C48 119.4(3) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 121.2(3) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C50 C51 C46 120.8(3) . . ? C50 C51 H51 119.6 . . ? C46 C51 H51 119.6 . . ? C54A C53A C62A 111.5(6) . . ? C53A C54A C55A 114.4(7) . . ? C56A C55A C54A 111.7(11) . . ? C57A C56A C55A 97.6(12) . . ? C56A C57A C58A 96.3(11) . . ? C52B C53B C54B 111.4(10) . . ? C55B C54B C53B 103.1(9) . . ? C54B C55B C56B 101.6(10) . . ? C57B C56B C55B 106.9(9) . . ? C58B C57B C56B 116.0(7) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.785 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.075 #=== END #====================================================================