# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Guofu Zi' _publ_contact_author_email ZIGUOFU@HOTMAIL.COM _publ_section_title ; Synthesis and characterization of group 4 metal amides with new C2-symmetric binaphthyldiamine-based ligands and their use as catalysts for asymmetric hydroamination/cyclization ; loop_ _publ_author_name 'Guofu Zi.' 'Yue Chen.' 'Wei-Hai Fang.' 'Hai-Bin Song.' 'Li Xiang.' ; Furen Zhang ; # Attachment 'compound_7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 742595' #TrackingRef 'compound_7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 N4 O4 S2 Ti' _chemical_formula_sum 'C56 H56 N4 O4 S2 Ti' _chemical_formula_weight 961.07 _chemical_absolute_configuration rmad 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 10.8873(5) _cell_length_b 18.6323(7) _cell_length_c 24.8231(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5035.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11015 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.303 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9588 _exptl_absorpt_correction_T_max 0.9704 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35828 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 27.85 _reflns_number_total 11929 _reflns_number_gt 10454 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0478P)^2^+0.6662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 11929 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Ti1 Ti 0.62723(4) 0.39818(3) 0.412039(19) 0.02524(12) Uani 1 1 d . . . S1 S 0.44010(6) 0.31759(4) 0.46040(3) 0.02670(15) Uani 1 1 d . . . S2 S 0.62733(6) 0.53329(4) 0.32351(3) 0.02395(14) Uani 1 1 d . . . O1 O 0.57359(17) 0.30182(11) 0.45650(8) 0.0306(5) Uani 1 1 d . . . O2 O 0.3903(2) 0.32141(12) 0.51392(7) 0.0352(5) Uani 1 1 d . . . O3 O 0.68791(17) 0.52336(11) 0.27217(8) 0.0298(5) Uani 1 1 d . . . O4 O 0.69600(17) 0.56719(11) 0.36605(8) 0.0315(5) Uani 1 1 d . . . N1 N 0.4410(2) 0.38926(13) 0.42675(9) 0.0254(5) Uani 1 1 d . . . N2 N 0.57576(19) 0.45845(12) 0.34749(9) 0.0217(5) Uani 1 1 d . . . N3 N 0.6915(2) 0.45967(15) 0.46332(11) 0.0372(6) Uani 1 1 d . . . N4 N 0.7592(2) 0.34326(13) 0.38649(10) 0.0321(6) Uani 1 1 d . . . C1 C 0.3107(2) 0.43768(14) 0.35705(11) 0.0211(5) Uani 1 1 d . . . C2 C 0.3350(2) 0.42894(15) 0.41127(11) 0.0249(6) Uani 1 1 d . . . C3 C 0.2586(3) 0.46012(17) 0.45120(12) 0.0325(7) Uani 1 1 d . . . H3 H 0.2774 0.4535 0.4882 0.039 Uiso 1 1 calc R . . C4 C 0.1585(3) 0.49935(17) 0.43677(13) 0.0343(7) Uani 1 1 d . . . H4 H 0.1074 0.5194 0.4639 0.041 Uiso 1 1 calc R . . C5 C 0.1295(3) 0.51073(15) 0.38163(12) 0.0298(6) Uani 1 1 d . . . C6 C 0.2072(2) 0.48080(14) 0.34137(11) 0.0241(6) Uani 1 1 d . . . C7 C 0.1775(3) 0.49421(15) 0.28657(12) 0.0275(6) Uani 1 1 d . . . H7 H 0.2305 0.4772 0.2590 0.033 Uiso 1 1 calc R . . C8 C 0.0739(3) 0.53121(16) 0.27298(13) 0.0326(7) Uani 1 1 d . . . H8 H 0.0552 0.5385 0.2360 0.039 Uiso 1 1 calc R . . C9 C -0.0053(3) 0.55862(17) 0.31231(14) 0.0383(8) Uani 1 1 d . . . H9 H -0.0783 0.5830 0.3021 0.046 Uiso 1 1 calc R . . C10 C 0.0234(3) 0.54997(17) 0.36552(14) 0.0372(8) Uani 1 1 d . . . H10 H -0.0283 0.5705 0.3922 0.045 Uiso 1 1 calc R . . C11 C 0.3857(2) 0.39948(14) 0.31611(10) 0.0213(5) Uani 1 1 d . . . C12 C 0.5114(2) 0.41129(14) 0.31075(10) 0.0216(5) Uani 1 1 d . . . C13 C 0.5814(3) 0.37327(14) 0.27169(11) 0.0251(6) Uani 1 1 d . . . H13 H 0.6670 0.3822 0.2685 0.030 Uiso 1 1 calc R . . C14 C 0.5267(3) 0.32405(15) 0.23885(11) 0.0298(6) Uani 1 1 d . . . H14 H 0.5743 0.3000 0.2124 0.036 Uiso 1 1 calc R . . C15 C 0.4001(3) 0.30838(15) 0.24368(11) 0.0270(6) Uani 1 1 d . . . C16 C 0.3292(2) 0.34508(15) 0.28311(11) 0.0241(6) Uani 1 1 d . . . C17 C 0.2035(3) 0.32508(15) 0.28919(12) 0.0293(6) Uani 1 1 d . . . H17 H 0.1549 0.3477 0.3161 0.035 Uiso 1 1 calc R . . C18 C 0.1519(3) 0.27380(16) 0.25690(13) 0.0374(8) Uani 1 1 d . . . H18 H 0.0679 0.2616 0.2615 0.045 Uiso 1 1 calc R . . C19 C 0.2220(3) 0.23875(16) 0.21680(13) 0.0398(8) Uani 1 1 d . . . H19 H 0.1847 0.2041 0.1940 0.048 Uiso 1 1 calc R . . C20 C 0.3437(3) 0.25497(16) 0.21100(12) 0.0342(7) Uani 1 1 d . . . H20 H 0.3912 0.2303 0.1848 0.041 Uiso 1 1 calc R . . C21 C 0.3581(3) 0.25148(15) 0.42529(10) 0.0248(6) Uani 1 1 d . . . C22 C 0.4034(2) 0.22461(15) 0.37667(11) 0.0278(6) Uani 1 1 d . . . H22 H 0.4811 0.2396 0.3634 0.033 Uiso 1 1 calc R . . C23 C 0.3331(3) 0.17590(15) 0.34822(11) 0.0290(6) Uani 1 1 d . . . H23 H 0.3641 0.1566 0.3155 0.035 Uiso 1 1 calc R . . C24 C 0.2172(3) 0.15433(16) 0.36648(12) 0.0315(7) Uani 1 1 d . . . C25 C 0.1746(3) 0.18229(18) 0.41474(13) 0.0402(8) Uani 1 1 d . . . H25 H 0.0958 0.1686 0.4276 0.048 Uiso 1 1 calc R . . C26 C 0.2453(3) 0.23005(18) 0.44466(12) 0.0388(8) Uani 1 1 d . . . H26 H 0.2160 0.2478 0.4782 0.047 Uiso 1 1 calc R . . C27 C 0.1382(3) 0.10422(17) 0.33351(13) 0.0411(8) Uani 1 1 d . . . H27A H 0.0719 0.1315 0.3164 0.062 Uiso 1 1 calc R . . H27B H 0.1029 0.0674 0.3570 0.062 Uiso 1 1 calc R . . H27C H 0.1885 0.0813 0.3057 0.062 Uiso 1 1 calc R . . C28 C 0.4954(2) 0.58566(14) 0.31050(11) 0.0227(6) Uani 1 1 d . . . C29 C 0.4519(2) 0.59283(15) 0.25808(11) 0.0269(6) Uani 1 1 d . . . H29 H 0.4925 0.5694 0.2291 0.032 Uiso 1 1 calc R . . C30 C 0.3494(3) 0.63430(15) 0.24864(12) 0.0281(6) Uani 1 1 d . . . H30 H 0.3202 0.6396 0.2128 0.034 Uiso 1 1 calc R . . C31 C 0.2875(3) 0.66854(15) 0.29043(12) 0.0276(6) Uani 1 1 d . . . C32 C 0.3318(3) 0.66048(16) 0.34237(12) 0.0307(7) Uani 1 1 d . . . H32 H 0.2908 0.6838 0.3712 0.037 Uiso 1 1 calc R . . C33 C 0.4345(3) 0.61921(15) 0.35311(11) 0.0267(6) Uani 1 1 d . . . H33 H 0.4632 0.6138 0.3890 0.032 Uiso 1 1 calc R . . C34 C 0.1749(3) 0.71349(17) 0.27925(14) 0.0388(8) Uani 1 1 d . . . H34A H 0.1291 0.6926 0.2491 0.058 Uiso 1 1 calc R . . H34B H 0.2000 0.7625 0.2700 0.058 Uiso 1 1 calc R . . H34C H 0.1226 0.7145 0.3114 0.058 Uiso 1 1 calc R . . C35 C 0.8158(3) 0.4628(2) 0.48649(15) 0.0570(11) Uani 1 1 d . . . H35A H 0.8108 0.4573 0.5257 0.085 Uiso 1 1 calc R . . H35B H 0.8533 0.5092 0.4779 0.085 Uiso 1 1 calc R . . H35C H 0.8660 0.4241 0.4714 0.085 Uiso 1 1 calc R . . C36 C 0.6107(3) 0.5147(2) 0.48690(14) 0.0483(9) Uani 1 1 d . . . H36A H 0.6468 0.5623 0.4812 0.072 Uiso 1 1 calc R . . H36B H 0.6016 0.5059 0.5256 0.072 Uiso 1 1 calc R . . H36C H 0.5299 0.5126 0.4696 0.072 Uiso 1 1 calc R . . C37 C 0.8588(3) 0.38466(19) 0.36089(15) 0.0475(8) Uani 1 1 d . . . H37A H 0.8605 0.3744 0.3222 0.071 Uiso 1 1 calc R . . H37B H 0.9377 0.3711 0.3770 0.071 Uiso 1 1 calc R . . H37C H 0.8446 0.4361 0.3665 0.071 Uiso 1 1 calc R . . C38 C 0.7810(3) 0.26617(18) 0.37974(14) 0.0458(9) Uani 1 1 d . . . H38A H 0.8586 0.2531 0.3971 0.069 Uiso 1 1 calc R . . H38B H 0.7854 0.2547 0.3413 0.069 Uiso 1 1 calc R . . H38C H 0.7136 0.2392 0.3963 0.069 Uiso 1 1 calc R . . C39 C 0.1359(3) 0.91561(17) 0.31353(13) 0.0372(7) Uani 1 1 d . . . H39 H 0.1333 0.9426 0.2811 0.045 Uiso 1 1 calc R . . C40 C 0.2426(3) 0.91293(19) 0.34341(13) 0.0404(8) Uani 1 1 d . . . H40 H 0.3132 0.9384 0.3316 0.049 Uiso 1 1 calc R . . C41 C 0.2474(3) 0.8735(2) 0.39037(14) 0.0497(9) Uani 1 1 d . . . H41 H 0.3216 0.8715 0.4105 0.060 Uiso 1 1 calc R . . C42 C 0.1445(4) 0.83687(19) 0.40843(15) 0.0511(9) Uani 1 1 d . . . H42 H 0.1473 0.8098 0.4409 0.061 Uiso 1 1 calc R . . C43 C 0.0357(3) 0.8404(2) 0.37786(16) 0.0517(10) Uani 1 1 d . . . H43 H -0.0359 0.8159 0.3897 0.062 Uiso 1 1 calc R . . C44 C 0.0334(3) 0.87937(18) 0.33071(14) 0.0411(8) Uani 1 1 d . . . H44 H -0.0398 0.8812 0.3099 0.049 Uiso 1 1 calc R . . C45 C 0.7936(3) 0.00223(19) 0.37401(14) 0.0433(8) Uani 1 1 d . . . H45 H 0.8796 -0.0044 0.3702 0.052 Uiso 1 1 calc R . . C46 C 0.7127(3) -0.04923(19) 0.35471(14) 0.0428(8) Uani 1 1 d . . . H46 H 0.7434 -0.0906 0.3369 0.051 Uiso 1 1 calc R . . C47 C 0.5878(3) -0.0404(2) 0.36130(14) 0.0454(9) Uani 1 1 d . . . H47 H 0.5326 -0.0761 0.3486 0.054 Uiso 1 1 calc R . . C48 C 0.5433(3) 0.0206(2) 0.38650(14) 0.0506(9) Uani 1 1 d . . . H48 H 0.4573 0.0270 0.3908 0.061 Uiso 1 1 calc R . . C49 C 0.6237(4) 0.07206(19) 0.40545(14) 0.0507(9) Uani 1 1 d . . . H49 H 0.5932 0.1137 0.4230 0.061 Uiso 1 1 calc R . . C50 C 0.7486(4) 0.06278(18) 0.39875(13) 0.0436(8) Uani 1 1 d . . . H50 H 0.8039 0.0985 0.4113 0.052 Uiso 1 1 calc R . . C51 C 0.3193(4) 0.6684(2) 0.49605(14) 0.0527(10) Uani 1 1 d . . . H51 H 0.3299 0.6273 0.4739 0.063 Uiso 1 1 calc R . . C52 C 0.2282(4) 0.6697(3) 0.53286(16) 0.0822(16) Uani 1 1 d . . . H52 H 0.1764 0.6291 0.5375 0.099 Uiso 1 1 calc R . . C53 C 0.2113(5) 0.7300(5) 0.5634(2) 0.112(3) Uani 1 1 d . . . H53 H 0.1465 0.7313 0.5890 0.135 Uiso 1 1 calc R . . C54 C 0.2869(7) 0.7889(4) 0.5576(2) 0.109(3) Uani 1 1 d . . . H54 H 0.2749 0.8306 0.5790 0.131 Uiso 1 1 calc R . . C55 C 0.3801(6) 0.7859(3) 0.52029(19) 0.0839(16) Uani 1 1 d . . . H55 H 0.4330 0.8259 0.5154 0.101 Uiso 1 1 calc R . . C56 C 0.3964(4) 0.7255(2) 0.49038(16) 0.0610(11) Uani 1 1 d . . . H56 H 0.4621 0.7232 0.4653 0.073 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 Ti1 0.0205(2) 0.0284(3) 0.0268(2) 0.0022(2) -0.0052(2) -0.0016(2) S1 0.0280(4) 0.0312(4) 0.0210(3) 0.0038(3) -0.0023(3) -0.0030(3) S2 0.0188(3) 0.0235(3) 0.0295(3) 0.0000(3) 0.0012(3) -0.0027(3) O1 0.0242(10) 0.0371(12) 0.0306(11) 0.0102(9) -0.0075(8) -0.0011(9) O2 0.0426(13) 0.0439(13) 0.0190(9) 0.0010(9) 0.0003(9) -0.0070(11) O3 0.0256(10) 0.0317(11) 0.0320(11) 0.0010(9) 0.0103(8) 0.0013(9) O4 0.0234(10) 0.0322(11) 0.0388(12) -0.0041(9) -0.0067(9) -0.0067(9) N1 0.0218(11) 0.0292(13) 0.0253(11) 0.0034(10) -0.0024(9) -0.0019(10) N2 0.0178(11) 0.0210(12) 0.0263(11) -0.0018(9) -0.0013(9) -0.0003(9) N3 0.0347(14) 0.0431(16) 0.0337(14) 0.0004(13) -0.0097(12) -0.0096(12) N4 0.0271(13) 0.0312(14) 0.0380(14) 0.0088(11) -0.0058(11) -0.0004(11) C1 0.0150(12) 0.0206(13) 0.0276(14) -0.0003(11) -0.0016(10) -0.0014(10) C2 0.0200(13) 0.0254(14) 0.0294(14) 0.0002(12) -0.0003(11) -0.0030(11) C3 0.0291(15) 0.0396(18) 0.0288(15) -0.0025(13) 0.0051(12) -0.0040(13) C4 0.0255(16) 0.0384(18) 0.0391(17) -0.0066(14) 0.0085(13) 0.0007(13) C5 0.0198(13) 0.0269(15) 0.0429(17) -0.0021(12) 0.0036(13) -0.0027(12) C6 0.0178(13) 0.0212(14) 0.0333(15) 0.0003(11) -0.0009(11) -0.0018(11) C7 0.0215(14) 0.0219(14) 0.0392(17) 0.0031(12) -0.0057(12) -0.0004(11) C8 0.0241(14) 0.0258(15) 0.0478(18) 0.0053(14) -0.0087(13) -0.0011(12) C9 0.0202(15) 0.0315(17) 0.063(2) 0.0103(16) -0.0038(14) 0.0032(13) C10 0.0198(15) 0.0323(18) 0.059(2) -0.0033(15) 0.0088(14) 0.0043(12) C11 0.0227(13) 0.0182(12) 0.0232(12) 0.0031(10) -0.0035(10) 0.0033(11) C12 0.0201(13) 0.0234(14) 0.0214(12) 0.0005(11) -0.0013(10) 0.0014(11) C13 0.0232(14) 0.0260(15) 0.0262(14) -0.0002(12) -0.0008(11) 0.0036(11) C14 0.0354(16) 0.0242(15) 0.0297(15) -0.0037(12) 0.0010(12) 0.0082(13) C15 0.0356(16) 0.0203(14) 0.0252(14) 0.0005(11) -0.0096(11) 0.0038(12) C16 0.0265(14) 0.0215(14) 0.0245(13) 0.0018(11) -0.0067(11) -0.0007(11) C17 0.0280(15) 0.0236(15) 0.0364(16) 0.0036(12) -0.0106(12) -0.0005(12) C18 0.0337(18) 0.0285(16) 0.0502(19) 0.0010(14) -0.0185(15) -0.0065(13) C19 0.057(2) 0.0215(16) 0.0412(18) -0.0014(14) -0.0235(16) -0.0077(15) C20 0.048(2) 0.0244(15) 0.0298(15) -0.0032(12) -0.0109(14) 0.0044(14) C21 0.0283(15) 0.0251(14) 0.0211(12) 0.0039(11) -0.0023(11) -0.0017(12) C22 0.0223(14) 0.0320(16) 0.0291(14) 0.0029(12) 0.0042(11) 0.0033(12) C23 0.0341(16) 0.0252(15) 0.0276(14) -0.0009(12) 0.0025(12) 0.0069(12) C24 0.0397(17) 0.0234(15) 0.0314(15) 0.0013(12) 0.0004(13) -0.0022(13) C25 0.0364(17) 0.0454(19) 0.0388(17) -0.0086(16) 0.0112(14) -0.0183(15) C26 0.0421(19) 0.046(2) 0.0278(16) -0.0064(14) 0.0113(14) -0.0118(16) C27 0.049(2) 0.0315(17) 0.0429(18) -0.0090(14) 0.0033(15) -0.0109(16) C28 0.0214(13) 0.0192(14) 0.0275(14) -0.0004(11) 0.0022(11) -0.0040(11) C29 0.0250(14) 0.0258(15) 0.0299(14) -0.0005(12) 0.0023(11) 0.0002(12) C30 0.0270(15) 0.0273(15) 0.0300(14) 0.0021(12) -0.0049(12) 0.0001(12) C31 0.0259(14) 0.0188(14) 0.0382(16) 0.0004(12) -0.0011(12) 0.0011(11) C32 0.0321(16) 0.0247(15) 0.0354(16) -0.0027(12) 0.0069(12) 0.0012(12) C33 0.0282(15) 0.0270(15) 0.0249(13) -0.0022(12) 0.0007(11) 0.0019(12) C34 0.0310(17) 0.0308(17) 0.055(2) 0.0026(15) -0.0025(15) 0.0080(13) C35 0.039(2) 0.083(3) 0.049(2) -0.011(2) -0.0173(17) -0.020(2) C36 0.051(2) 0.052(2) 0.0420(19) -0.0124(17) -0.0027(17) -0.0093(18) C37 0.0324(18) 0.053(2) 0.057(2) 0.0078(18) -0.0036(16) -0.0003(16) C38 0.049(2) 0.043(2) 0.046(2) 0.0039(17) 0.0022(16) 0.0141(17) C39 0.0397(18) 0.0300(16) 0.0421(17) -0.0079(13) 0.0001(15) 0.0072(15) C40 0.0319(17) 0.046(2) 0.0431(19) -0.0038(16) 0.0042(14) -0.0019(15) C41 0.044(2) 0.063(3) 0.043(2) -0.0077(18) -0.0052(16) 0.0066(18) C42 0.068(3) 0.047(2) 0.0381(18) 0.0054(16) 0.0102(19) 0.0039(19) C43 0.043(2) 0.048(2) 0.065(2) -0.0145(19) 0.0232(18) -0.0118(17) C44 0.0271(16) 0.042(2) 0.054(2) -0.0127(17) 0.0021(14) 0.0028(14) C45 0.0396(19) 0.043(2) 0.047(2) -0.0002(16) -0.0060(15) -0.0029(16) C46 0.0387(19) 0.040(2) 0.050(2) -0.0110(16) 0.0008(16) 0.0003(15) C47 0.0406(19) 0.047(2) 0.048(2) -0.0064(17) -0.0034(15) 0.0000(16) C48 0.040(2) 0.065(3) 0.047(2) -0.0031(19) 0.0007(16) 0.0077(19) C49 0.072(3) 0.044(2) 0.0362(18) -0.0075(16) 0.0014(19) 0.019(2) C50 0.062(2) 0.0343(18) 0.0346(18) 0.0012(14) -0.0098(16) -0.0045(17) C51 0.068(3) 0.053(2) 0.0367(19) -0.0070(17) -0.0011(18) 0.003(2) C52 0.065(3) 0.146(5) 0.035(2) 0.000(3) -0.006(2) -0.019(3) C53 0.066(4) 0.232(9) 0.039(3) -0.041(4) -0.003(2) 0.052(4) C54 0.156(6) 0.110(5) 0.062(3) -0.047(3) -0.061(4) 0.092(5) C55 0.141(5) 0.055(3) 0.055(3) 0.002(2) -0.032(3) -0.007(3) C56 0.072(3) 0.067(3) 0.044(2) -0.008(2) 0.003(2) -0.003(2) _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 Ti1 N3 1.850(3) . ? Ti1 N4 1.874(3) . ? Ti1 N2 2.035(2) . ? Ti1 N1 2.067(2) . ? Ti1 O1 2.187(2) . ? Ti1 S1 2.8012(9) . ? S1 O2 1.436(2) . ? S1 O1 1.486(2) . ? S1 N1 1.575(2) . ? S1 C21 1.753(3) . ? S2 O4 1.440(2) . ? S2 O3 1.447(2) . ? S2 N2 1.617(2) . ? S2 C28 1.766(3) . ? N1 C2 1.424(3) . ? N2 C12 1.447(3) . ? N3 C35 1.471(4) . ? N3 C36 1.473(4) . ? N4 C38 1.465(4) . ? N4 C37 1.475(4) . ? C1 C2 1.381(4) . ? C1 C6 1.438(4) . ? C1 C11 1.485(4) . ? C2 C3 1.418(4) . ? C3 C4 1.360(4) . ? C3 H3 0.9500 . ? C4 C5 1.421(4) . ? C4 H4 0.9500 . ? C5 C6 1.423(4) . ? C5 C10 1.425(4) . ? C6 C7 1.420(4) . ? C7 C8 1.364(4) . ? C7 H7 0.9500 . ? C8 C9 1.399(4) . ? C8 H8 0.9500 . ? C9 C10 1.367(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 C16 1.441(4) . ? C12 C13 1.422(4) . ? C13 C14 1.364(4) . ? C13 H13 0.9500 . ? C14 C15 1.414(4) . ? C14 H14 0.9500 . ? C15 C16 1.422(4) . ? C15 C20 1.423(4) . ? C16 C17 1.426(4) . ? C17 C18 1.368(4) . ? C17 H17 0.9500 . ? C18 C19 1.414(5) . ? C18 H18 0.9500 . ? C19 C20 1.366(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.379(4) . ? C21 C22 1.396(4) . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.400(4) . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 C27 1.510(4) . ? C25 C26 1.391(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.391(4) . ? C28 C33 1.396(4) . ? C29 C30 1.378(4) . ? C29 H29 0.9500 . ? C30 C31 1.391(4) . ? C30 H30 0.9500 . ? C31 C32 1.385(4) . ? C31 C34 1.511(4) . ? C32 C33 1.382(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C44 1.372(4) . ? C39 C40 1.379(4) . ? C39 H39 0.9500 . ? C40 C41 1.379(5) . ? C40 H40 0.9500 . ? C41 C42 1.386(5) . ? C41 H41 0.9500 . ? C42 C43 1.408(5) . ? C42 H42 0.9500 . ? C43 C44 1.377(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.374(5) . ? C45 C46 1.387(4) . ? C45 H45 0.9500 . ? C46 C47 1.379(5) . ? C46 H46 0.9500 . ? C47 C48 1.385(5) . ? C47 H47 0.9500 . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 C50 1.381(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.349(6) . ? C51 C56 1.363(6) . ? C51 H51 0.9500 . ? C52 C53 1.368(8) . ? C52 H52 0.9500 . ? C53 C54 1.380(9) . ? C53 H53 0.9500 . ? C54 C55 1.375(8) . ? C54 H54 0.9500 . ? C55 C56 1.359(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? 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 N3 Ti1 N4 106.32(12) . . ? N3 Ti1 N2 107.71(11) . . ? N4 Ti1 N2 104.24(10) . . ? N3 Ti1 N1 107.41(11) . . ? N4 Ti1 N1 140.15(10) . . ? N2 Ti1 N1 85.03(9) . . ? N3 Ti1 O1 105.20(10) . . ? N4 Ti1 O1 85.83(9) . . ? N2 Ti1 O1 140.96(8) . . ? N1 Ti1 O1 65.34(8) . . ? N3 Ti1 S1 108.19(9) . . ? N4 Ti1 S1 114.19(8) . . ? N2 Ti1 S1 115.65(7) . . ? N1 Ti1 S1 33.66(6) . . ? O1 Ti1 S1 31.72(5) . . ? O2 S1 O1 116.03(12) . . ? O2 S1 N1 116.79(13) . . ? O1 S1 N1 97.29(12) . . ? O2 S1 C21 107.62(13) . . ? O1 S1 C21 109.06(13) . . ? N1 S1 C21 109.59(12) . . ? O2 S1 Ti1 130.09(9) . . ? O1 S1 Ti1 50.70(8) . . ? N1 S1 Ti1 46.66(8) . . ? C21 S1 Ti1 122.27(9) . . ? O4 S2 O3 117.73(12) . . ? O4 S2 N2 106.78(12) . . ? O3 S2 N2 111.86(12) . . ? O4 S2 C28 108.31(12) . . ? O3 S2 C28 106.28(12) . . ? N2 S2 C28 105.15(12) . . ? S1 O1 Ti1 97.57(10) . . ? C2 N1 S1 125.33(19) . . ? C2 N1 Ti1 134.90(18) . . ? S1 N1 Ti1 99.68(11) . . ? C12 N2 S2 117.37(18) . . ? C12 N2 Ti1 107.12(16) . . ? S2 N2 Ti1 132.07(13) . . ? C35 N3 C36 111.5(3) . . ? C35 N3 Ti1 129.9(2) . . ? C36 N3 Ti1 118.6(2) . . ? C38 N4 C37 110.1(3) . . ? C38 N4 Ti1 134.3(2) . . ? C37 N4 Ti1 115.1(2) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 C11 120.4(2) . . ? C6 C1 C11 120.9(2) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 N1 118.6(2) . . ? C3 C2 N1 120.0(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.1(3) . . ? C4 C5 C10 121.8(3) . . ? C6 C5 C10 119.1(3) . . ? C7 C6 C5 117.9(3) . . ? C7 C6 C1 122.4(3) . . ? C5 C6 C1 119.7(3) . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C5 121.1(3) . . ? C9 C10 H10 119.4 . . ? C5 C10 H10 119.4 . . ? C12 C11 C16 118.5(2) . . ? C12 C11 C1 122.0(2) . . ? C16 C11 C1 119.4(2) . . ? C11 C12 C13 120.9(2) . . ? C11 C12 N2 120.8(2) . . ? C13 C12 N2 118.2(2) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 C20 121.1(3) . . ? C16 C15 C20 119.6(3) . . ? C15 C16 C17 117.9(2) . . ? C15 C16 C11 119.8(2) . . ? C17 C16 C11 122.2(3) . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.9(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 119.7(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 120.9(3) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? C26 C21 C22 120.8(3) . . ? C26 C21 S1 118.9(2) . . ? C22 C21 S1 120.1(2) . . ? C23 C22 C21 118.8(3) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 121.5(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 118.3(3) . . ? C25 C24 C27 120.7(3) . . ? C23 C24 C27 121.0(3) . . ? C24 C25 C26 121.1(3) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C21 C26 C25 119.5(3) . . ? C21 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 120.3(3) . . ? C29 C28 S2 120.0(2) . . ? C33 C28 S2 119.7(2) . . ? C30 C29 C28 119.2(3) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 121.5(3) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 118.4(3) . . ? C32 C31 C34 120.9(3) . . ? C30 C31 C34 120.7(3) . . ? C33 C32 C31 121.4(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C28 119.1(3) . . ? C32 C33 H33 120.4 . . ? C28 C33 H33 120.4 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C44 C39 C40 120.0(3) . . ? C44 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 120.4(3) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 120.4(3) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C43 118.8(3) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C39 C44 C43 120.6(3) . . ? C39 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C50 C45 C46 119.7(3) . . ? C50 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 120.2(3) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.7(3) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 119.7(3) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C45 C50 C49 120.5(3) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C52 C51 C56 120.6(4) . . ? C52 C51 H51 119.7 . . ? C56 C51 H51 119.7 . . ? C51 C52 C53 119.3(5) . . ? C51 C52 H52 120.4 . . ? C53 C52 H52 120.4 . . ? C52 C53 C54 121.1(5) . . ? C52 C53 H53 119.5 . . ? C54 C53 H53 119.5 . . ? C55 C54 C53 118.5(5) . . ? C55 C54 H54 120.7 . . ? C53 C54 H54 120.7 . . ? C56 C55 C54 119.9(5) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C51 120.6(4) . . ? C55 C56 H56 119.7 . . ? C51 C56 H56 119.7 . . ? 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 Ti1 S1 O2 3.38(16) . . . . ? N4 Ti1 S1 O2 121.54(15) . . . . ? N2 Ti1 S1 O2 -117.47(14) . . . . ? N1 Ti1 S1 O2 -90.90(17) . . . . ? O1 Ti1 S1 O2 93.00(16) . . . . ? N3 Ti1 S1 O1 -89.61(14) . . . . ? N4 Ti1 S1 O1 28.55(13) . . . . ? N2 Ti1 S1 O1 149.53(13) . . . . ? N1 Ti1 S1 O1 176.10(16) . . . . ? N3 Ti1 S1 N1 94.28(15) . . . . ? N4 Ti1 S1 N1 -147.56(14) . . . . ? N2 Ti1 S1 N1 -26.57(13) . . . . ? O1 Ti1 S1 N1 -176.10(16) . . . . ? N3 Ti1 S1 C21 -178.61(14) . . . . ? N4 Ti1 S1 C21 -60.45(14) . . . . ? N2 Ti1 S1 C21 60.54(13) . . . . ? N1 Ti1 S1 C21 87.11(16) . . . . ? O1 Ti1 S1 C21 -88.99(15) . . . . ? O2 S1 O1 Ti1 -121.77(12) . . . . ? N1 S1 O1 Ti1 2.86(12) . . . . ? C21 S1 O1 Ti1 116.55(11) . . . . ? N3 Ti1 O1 S1 100.12(13) . . . . ? N4 Ti1 O1 S1 -154.08(12) . . . . ? N2 Ti1 O1 S1 -46.53(18) . . . . ? N1 Ti1 O1 S1 -2.38(10) . . . . ? O2 S1 N1 C2 -62.0(3) . . . . ? O1 S1 N1 C2 174.0(2) . . . . ? C21 S1 N1 C2 60.7(3) . . . . ? Ti1 S1 N1 C2 177.0(3) . . . . ? O2 S1 N1 Ti1 121.03(12) . . . . ? O1 S1 N1 Ti1 -3.04(12) . . . . ? C21 S1 N1 Ti1 -116.31(13) . . . . ? N3 Ti1 N1 C2 86.6(3) . . . . ? N4 Ti1 N1 C2 -126.8(3) . . . . ? N2 Ti1 N1 C2 -20.4(3) . . . . ? O1 Ti1 N1 C2 -174.3(3) . . . . ? S1 Ti1 N1 C2 -176.6(3) . . . . ? N3 Ti1 N1 S1 -96.86(13) . . . . ? N4 Ti1 N1 S1 49.79(19) . . . . ? N2 Ti1 N1 S1 156.12(12) . . . . ? O1 Ti1 N1 S1 2.25(9) . . . . ? O4 S2 N2 C12 -175.11(18) . . . . ? O3 S2 N2 C12 -45.0(2) . . . . ? C28 S2 N2 C12 70.0(2) . . . . ? O4 S2 N2 Ti1 -19.1(2) . . . . ? O3 S2 N2 Ti1 111.09(17) . . . . ? C28 S2 N2 Ti1 -133.98(16) . . . . ? N3 Ti1 N2 C12 -172.73(16) . . . . ? N4 Ti1 N2 C12 74.61(18) . . . . ? N1 Ti1 N2 C12 -66.02(16) . . . . ? O1 Ti1 N2 C12 -26.6(2) . . . . ? S1 Ti1 N2 C12 -51.61(17) . . . . ? N3 Ti1 N2 S2 29.4(2) . . . . ? N4 Ti1 N2 S2 -83.24(18) . . . . ? N1 Ti1 N2 S2 136.13(18) . . . . ? O1 Ti1 N2 S2 175.58(13) . . . . ? S1 Ti1 N2 S2 150.54(14) . . . . ? N4 Ti1 N3 C35 -6.8(3) . . . . ? N2 Ti1 N3 C35 -118.1(3) . . . . ? N1 Ti1 N3 C35 151.7(3) . . . . ? O1 Ti1 N3 C35 83.3(3) . . . . ? S1 Ti1 N3 C35 116.3(3) . . . . ? N4 Ti1 N3 C36 174.1(2) . . . . ? N2 Ti1 N3 C36 62.8(2) . . . . ? N1 Ti1 N3 C36 -27.4(3) . . . . ? O1 Ti1 N3 C36 -95.8(2) . . . . ? S1 Ti1 N3 C36 -62.8(2) . . . . ? N3 Ti1 N4 C38 128.6(3) . . . . ? N2 Ti1 N4 C38 -117.8(3) . . . . ? N1 Ti1 N4 C38 -18.3(4) . . . . ? O1 Ti1 N4 C38 23.9(3) . . . . ? S1 Ti1 N4 C38 9.3(3) . . . . ? N3 Ti1 N4 C37 -60.8(2) . . . . ? N2 Ti1 N4 C37 52.9(2) . . . . ? N1 Ti1 N4 C37 152.4(2) . . . . ? O1 Ti1 N4 C37 -165.4(2) . . . . ? S1 Ti1 N4 C37 -179.97(19) . . . . ? C6 C1 C2 C3 1.5(4) . . . . ? C11 C1 C2 C3 -174.8(2) . . . . ? C6 C1 C2 N1 -176.9(2) . . . . ? C11 C1 C2 N1 6.9(4) . . . . ? S1 N1 C2 C1 -118.2(3) . . . . ? Ti1 N1 C2 C1 57.7(4) . . . . ? S1 N1 C2 C3 63.4(3) . . . . ? Ti1 N1 C2 C3 -120.7(3) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? N1 C2 C3 C4 178.6(3) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C3 C4 C5 C10 178.3(3) . . . . ? C4 C5 C6 C7 -178.7(3) . . . . ? C10 C5 C6 C7 2.6(4) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? C10 C5 C6 C1 -176.5(2) . . . . ? C2 C1 C6 C7 178.3(3) . . . . ? C11 C1 C6 C7 -5.5(4) . . . . ? C2 C1 C6 C5 -2.7(4) . . . . ? C11 C1 C6 C5 173.5(2) . . . . ? C5 C6 C7 C8 -3.6(4) . . . . ? C1 C6 C7 C8 175.5(3) . . . . ? C6 C7 C8 C9 1.4(4) . . . . ? C7 C8 C9 C10 1.9(5) . . . . ? C8 C9 C10 C5 -2.9(5) . . . . ? C4 C5 C10 C9 -178.0(3) . . . . ? C6 C5 C10 C9 0.6(4) . . . . ? C2 C1 C11 C12 -62.0(3) . . . . ? C6 C1 C11 C12 121.9(3) . . . . ? C2 C1 C11 C16 113.9(3) . . . . ? C6 C1 C11 C16 -62.3(3) . . . . ? C16 C11 C12 C13 3.2(4) . . . . ? C1 C11 C12 C13 179.1(2) . . . . ? C16 C11 C12 N2 -172.0(2) . . . . ? C1 C11 C12 N2 3.9(4) . . . . ? S2 N2 C12 C11 -111.3(2) . . . . ? Ti1 N2 C12 C11 87.0(2) . . . . ? S2 N2 C12 C13 73.3(3) . . . . ? Ti1 N2 C12 C13 -88.3(2) . . . . ? C11 C12 C13 C14 -0.4(4) . . . . ? N2 C12 C13 C14 175.0(2) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C13 C14 C15 C20 -177.4(3) . . . . ? C14 C15 C16 C17 -176.3(3) . . . . ? C20 C15 C16 C17 1.6(4) . . . . ? C14 C15 C16 C11 2.4(4) . . . . ? C20 C15 C16 C11 -179.7(2) . . . . ? C12 C11 C16 C15 -4.2(4) . . . . ? C1 C11 C16 C15 179.8(2) . . . . ? C12 C11 C16 C17 174.4(3) . . . . ? C1 C11 C16 C17 -1.5(4) . . . . ? C15 C16 C17 C18 -2.0(4) . . . . ? C11 C16 C17 C18 179.3(3) . . . . ? C16 C17 C18 C19 0.5(4) . . . . ? C17 C18 C19 C20 1.6(5) . . . . ? C18 C19 C20 C15 -2.0(5) . . . . ? C14 C15 C20 C19 178.3(3) . . . . ? C16 C15 C20 C19 0.4(4) . . . . ? O2 S1 C21 C26 18.6(3) . . . . ? O1 S1 C21 C26 145.2(2) . . . . ? N1 S1 C21 C26 -109.4(2) . . . . ? Ti1 S1 C21 C26 -159.8(2) . . . . ? O2 S1 C21 C22 -165.5(2) . . . . ? O1 S1 C21 C22 -38.9(3) . . . . ? N1 S1 C21 C22 66.5(3) . . . . ? Ti1 S1 C21 C22 16.1(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? S1 C21 C22 C23 -176.0(2) . . . . ? C21 C22 C23 C24 1.4(4) . . . . ? C22 C23 C24 C25 -1.0(4) . . . . ? C22 C23 C24 C27 176.6(3) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C27 C24 C25 C26 -178.2(3) . . . . ? C22 C21 C26 C25 -1.4(5) . . . . ? S1 C21 C26 C25 174.4(3) . . . . ? C24 C25 C26 C21 1.8(5) . . . . ? O4 S2 C28 C29 143.8(2) . . . . ? O3 S2 C28 C29 16.4(3) . . . . ? N2 S2 C28 C29 -102.3(2) . . . . ? O4 S2 C28 C33 -36.7(2) . . . . ? O3 S2 C28 C33 -164.1(2) . . . . ? N2 S2 C28 C33 77.1(2) . . . . ? C33 C28 C29 C30 1.0(4) . . . . ? S2 C28 C29 C30 -179.6(2) . . . . ? C28 C29 C30 C31 -0.7(4) . . . . ? C29 C30 C31 C32 0.4(4) . . . . ? C29 C30 C31 C34 -179.7(3) . . . . ? C30 C31 C32 C33 -0.4(4) . . . . ? C34 C31 C32 C33 179.7(3) . . . . ? C31 C32 C33 C28 0.7(4) . . . . ? C29 C28 C33 C32 -1.0(4) . . . . ? S2 C28 C33 C32 179.5(2) . . . . ? C44 C39 C40 C41 0.5(5) . . . . ? C39 C40 C41 C42 -0.8(5) . . . . ? C40 C41 C42 C43 0.3(5) . . . . ? C41 C42 C43 C44 0.5(5) . . . . ? C40 C39 C44 C43 0.3(5) . . . . ? C42 C43 C44 C39 -0.8(5) . . . . ? C50 C45 C46 C47 -1.4(5) . . . . ? C45 C46 C47 C48 1.1(6) . . . . ? C46 C47 C48 C49 -0.7(6) . . . . ? C47 C48 C49 C50 0.6(5) . . . . ? C46 C45 C50 C49 1.3(5) . . . . ? C48 C49 C50 C45 -0.9(5) . . . . ? C56 C51 C52 C53 2.1(7) . . . . ? C51 C52 C53 C54 -0.9(8) . . . . ? C52 C53 C54 C55 0.1(8) . . . . ? C53 C54 C55 C56 -0.4(8) . . . . ? C54 C55 C56 C51 1.6(7) . . . . ? C52 C51 C56 C55 -2.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.235 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.057 # Attachment 'compound_8.cif' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 742596' #TrackingRef 'compound_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 N4 O4 S2 Zr' _chemical_formula_sum 'C38 H38 N4 O4 S2 Zr' _chemical_formula_weight 770.06 _chemical_absolute_configuration rmad 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' S S 0.1246 0.1234 '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 tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 20.7957(19) _cell_length_b 20.7957(19) _cell_length_c 17.2989(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7481.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12312 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8478 _exptl_absorpt_correction_T_max 0.8695 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37596 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.87 _reflns_number_total 8483 _reflns_number_gt 7733 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0516P)^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 SHELXL _refine_ls_extinction_coef 0.00206(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(3) _refine_ls_number_reflns 8483 _refine_ls_number_parameters 449 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.223724(11) 0.111869(10) 0.317798(19) 0.03412(8) Uani 1 1 d . . . S1 S 0.17389(3) 0.24012(3) 0.36468(4) 0.03652(15) Uani 1 1 d . . . S2 S 0.35691(3) 0.07287(3) 0.27772(4) 0.03377(15) Uani 1 1 d . . . N1 N 0.24365(10) 0.21145(10) 0.36338(13) 0.0343(5) Uani 1 1 d . . . N2 N 0.32081(10) 0.13906(10) 0.27432(12) 0.0315(4) Uani 1 1 d . . . N3 N 0.17618(11) 0.08538(11) 0.22102(14) 0.0409(6) Uani 1 1 d . . . N4 N 0.19391(12) 0.05548(12) 0.40574(15) 0.0451(6) Uani 1 1 d . . . O1 O 0.13858(8) 0.18519(8) 0.33070(13) 0.0426(5) Uani 1 1 d . . . O2 O 0.15096(10) 0.26467(10) 0.43675(12) 0.0480(5) Uani 1 1 d . . . O3 O 0.30465(8) 0.03496(7) 0.31428(13) 0.0373(4) Uani 1 1 d . . . O4 O 0.38254(10) 0.04831(9) 0.20681(11) 0.0444(5) Uani 1 1 d . . . C1 C 0.35563(13) 0.24223(12) 0.37471(15) 0.0337(6) Uani 1 1 d . . . C2 C 0.29716(12) 0.22982(12) 0.40957(15) 0.0327(5) Uani 1 1 d . . . C3 C 0.29109(15) 0.22665(13) 0.49132(16) 0.0414(6) Uani 1 1 d . . . H3 H 0.2502 0.2193 0.5141 0.050 Uiso 1 1 calc R . . C4 C 0.34348(17) 0.23403(15) 0.53682(18) 0.0498(8) Uani 1 1 d . . . H4 H 0.3388 0.2325 0.5914 0.060 Uiso 1 1 calc R . . C5 C 0.40444(16) 0.24394(14) 0.50464(18) 0.0459(7) Uani 1 1 d . . . C6 C 0.41156(13) 0.24813(12) 0.42237(17) 0.0378(6) Uani 1 1 d . . . C7 C 0.47378(14) 0.25410(14) 0.3906(2) 0.0479(7) Uani 1 1 d . . . H7 H 0.4793 0.2567 0.3361 0.057 Uiso 1 1 calc R . . C8 C 0.52699(16) 0.25613(16) 0.4391(2) 0.0604(9) Uani 1 1 d . . . H8 H 0.5689 0.2600 0.4179 0.072 Uiso 1 1 calc R . . C9 C 0.51882(19) 0.25248(18) 0.5197(2) 0.0630(10) Uani 1 1 d . . . H9 H 0.5556 0.2537 0.5522 0.076 Uiso 1 1 calc R . . C10 C 0.46028(18) 0.24738(17) 0.5519(2) 0.0577(9) Uani 1 1 d . . . H10 H 0.4561 0.2461 0.6066 0.069 Uiso 1 1 calc R . . C11 C 0.36095(12) 0.24750(13) 0.28872(15) 0.0326(5) Uani 1 1 d . . . C12 C 0.34689(12) 0.19585(13) 0.24170(15) 0.0332(5) Uani 1 1 d . . . C13 C 0.35286(13) 0.20016(15) 0.15984(16) 0.0432(7) Uani 1 1 d . . . H13 H 0.3449 0.1634 0.1287 0.052 Uiso 1 1 calc R . . C14 C 0.36997(16) 0.25683(18) 0.12600(19) 0.0535(8) Uani 1 1 d . . . H14 H 0.3741 0.2592 0.0714 0.064 Uiso 1 1 calc R . . C15 C 0.38164(14) 0.31218(17) 0.1716(2) 0.0523(8) Uani 1 1 d . . . C16 C 0.37800(13) 0.30803(14) 0.25368(18) 0.0438(7) Uani 1 1 d . . . C17 C 0.38732(14) 0.36448(13) 0.2975(2) 0.0504(9) Uani 1 1 d . . . H17 H 0.3864 0.3623 0.3523 0.060 Uiso 1 1 calc R . . C18 C 0.39775(17) 0.42271(16) 0.2616(3) 0.0668(11) Uani 1 1 d . . . H18 H 0.4031 0.4603 0.2921 0.080 Uiso 1 1 calc R . . C19 C 0.4005(2) 0.4272(2) 0.1816(3) 0.0855(15) Uani 1 1 d . . . H19 H 0.4077 0.4678 0.1579 0.103 Uiso 1 1 calc R . . C20 C 0.39310(18) 0.3739(2) 0.1370(3) 0.0743(12) Uani 1 1 d . . . H20 H 0.3955 0.3775 0.0823 0.089 Uiso 1 1 calc R . . C21 C 0.16941(12) 0.30271(12) 0.29638(15) 0.0357(6) Uani 1 1 d . . . C22 C 0.22130(14) 0.34336(14) 0.2869(2) 0.0490(8) Uani 1 1 d . . . H22 H 0.2592 0.3368 0.3165 0.059 Uiso 1 1 calc R . . C23 C 0.21844(14) 0.39321(14) 0.2350(2) 0.0486(7) Uani 1 1 d . . . H23 H 0.2548 0.4202 0.2282 0.058 Uiso 1 1 calc R . . C24 C 0.16300(14) 0.40470(13) 0.19225(16) 0.0388(6) Uani 1 1 d . . . C25 C 0.11044(14) 0.36434(16) 0.20396(17) 0.0437(7) Uani 1 1 d . . . H25 H 0.0717 0.3720 0.1763 0.052 Uiso 1 1 calc R . . C26 C 0.11371(13) 0.31360(14) 0.25489(15) 0.0366(6) Uani 1 1 d . . . H26 H 0.0777 0.2861 0.2615 0.044 Uiso 1 1 calc R . . C27 C 0.15980(17) 0.45937(17) 0.13478(19) 0.0551(8) Uani 1 1 d . . . H27A H 0.1729 0.4438 0.0837 0.083 Uiso 1 1 calc R . . H27B H 0.1887 0.4939 0.1513 0.083 Uiso 1 1 calc R . . H27C H 0.1157 0.4758 0.1322 0.083 Uiso 1 1 calc R . . C28 C 0.42158(12) 0.07835(11) 0.34320(14) 0.0316(6) Uani 1 1 d . . . C29 C 0.40923(13) 0.08498(13) 0.42198(15) 0.0365(6) Uani 1 1 d . . . H29 H 0.3663 0.0870 0.4405 0.044 Uiso 1 1 calc R . . C30 C 0.46039(13) 0.08855(13) 0.47270(15) 0.0373(6) Uani 1 1 d . . . H30 H 0.4523 0.0917 0.5266 0.045 Uiso 1 1 calc R . . C31 C 0.52403(13) 0.08761(12) 0.44622(15) 0.0355(6) Uani 1 1 d . . . C32 C 0.53454(12) 0.08265(13) 0.36753(15) 0.0362(6) Uani 1 1 d . . . H32 H 0.5773 0.0828 0.3482 0.043 Uiso 1 1 calc R . . C33 C 0.48367(11) 0.07744(11) 0.31681(18) 0.0349(5) Uani 1 1 d . . . H33 H 0.4918 0.0732 0.2630 0.042 Uiso 1 1 calc R . . C34 C 0.57970(14) 0.09137(16) 0.50204(18) 0.0473(7) Uani 1 1 d . . . H34A H 0.5634 0.0990 0.5544 0.071 Uiso 1 1 calc R . . H34B H 0.6082 0.1267 0.4870 0.071 Uiso 1 1 calc R . . H34C H 0.6036 0.0508 0.5010 0.071 Uiso 1 1 calc R . . C35 C 0.16557(16) 0.13702(16) 0.16518(19) 0.0516(8) Uani 1 1 d . . . H35A H 0.1759 0.1215 0.1131 0.077 Uiso 1 1 calc R . . H35B H 0.1933 0.1736 0.1779 0.077 Uiso 1 1 calc R . . H35C H 0.1205 0.1505 0.1670 0.077 Uiso 1 1 calc R . . C36 C 0.13603(16) 0.02992(16) 0.2066(2) 0.0523(8) Uani 1 1 d . . . H36A H 0.0908 0.0432 0.2053 0.079 Uiso 1 1 calc R . . H36B H 0.1423 -0.0018 0.2478 0.079 Uiso 1 1 calc R . . H36C H 0.1477 0.0107 0.1568 0.079 Uiso 1 1 calc R . . C37 C 0.12332(16) 0.04987(17) 0.4118(2) 0.0559(8) Uani 1 1 d . . . H37A H 0.1109 0.0045 0.4079 0.084 Uiso 1 1 calc R . . H37B H 0.1031 0.0742 0.3698 0.084 Uiso 1 1 calc R . . H37C H 0.1091 0.0671 0.4616 0.084 Uiso 1 1 calc R . . C38 C 0.22578(18) 0.01312(19) 0.4603(2) 0.0643(10) Uani 1 1 d . . . H38A H 0.2172 0.0279 0.5131 0.096 Uiso 1 1 calc R . . H38B H 0.2722 0.0136 0.4507 0.096 Uiso 1 1 calc R . . H38C H 0.2094 -0.0308 0.4539 0.096 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 0.03200(13) 0.02694(12) 0.04342(15) -0.00124(12) -0.00349(12) 0.00423(9) S1 0.0340(3) 0.0316(3) 0.0439(4) -0.0003(3) 0.0062(3) 0.0077(3) S2 0.0370(3) 0.0301(3) 0.0342(3) -0.0060(3) -0.0042(3) 0.0094(3) N1 0.0327(11) 0.0296(10) 0.0405(12) -0.0041(9) 0.0012(9) 0.0052(9) N2 0.0314(11) 0.0292(10) 0.0339(11) -0.0023(9) -0.0023(9) 0.0065(8) N3 0.0373(12) 0.0350(12) 0.0505(15) -0.0059(10) -0.0078(11) 0.0055(10) N4 0.0441(14) 0.0383(13) 0.0529(16) 0.0003(11) -0.0011(11) 0.0025(11) O1 0.0312(9) 0.0335(9) 0.0630(14) 0.0051(9) 0.0026(9) 0.0036(7) O2 0.0480(12) 0.0488(12) 0.0472(12) 0.0030(9) 0.0167(9) 0.0165(10) O3 0.0360(9) 0.0244(8) 0.0515(10) -0.0033(9) -0.0075(10) 0.0047(7) O4 0.0542(12) 0.0441(11) 0.0349(10) -0.0140(9) -0.0046(9) 0.0172(9) C1 0.0387(14) 0.0257(12) 0.0366(14) -0.0034(10) -0.0073(11) 0.0026(10) C2 0.0395(14) 0.0251(12) 0.0336(14) -0.0021(10) -0.0003(11) 0.0061(10) C3 0.0513(17) 0.0394(15) 0.0336(15) -0.0059(12) 0.0045(12) 0.0080(13) C4 0.065(2) 0.0461(17) 0.0385(17) -0.0088(13) -0.0013(14) 0.0123(15) C5 0.0591(19) 0.0364(15) 0.0421(16) -0.0104(12) -0.0155(14) 0.0029(14) C6 0.0421(15) 0.0261(12) 0.0452(16) -0.0055(11) -0.0088(12) 0.0017(11) C7 0.0428(16) 0.0378(15) 0.063(2) -0.0039(14) -0.0132(14) -0.0002(12) C8 0.0423(18) 0.053(2) 0.086(3) -0.0104(18) -0.0138(17) -0.0069(15) C9 0.064(2) 0.059(2) 0.067(2) -0.0161(17) -0.0331(19) -0.0042(17) C10 0.066(2) 0.055(2) 0.0526(19) -0.0167(15) -0.0203(17) 0.0024(16) C11 0.0311(13) 0.0324(13) 0.0344(13) 0.0039(10) -0.0022(10) 0.0058(10) C12 0.0293(12) 0.0382(14) 0.0323(13) 0.0030(11) -0.0020(10) 0.0082(11) C13 0.0392(15) 0.0571(18) 0.0333(15) -0.0001(13) -0.0021(12) 0.0133(13) C14 0.0511(19) 0.074(2) 0.0348(16) 0.0192(16) 0.0033(14) 0.0196(17) C15 0.0410(17) 0.0545(19) 0.061(2) 0.0257(16) 0.0057(14) 0.0109(14) C16 0.0347(14) 0.0413(15) 0.0554(19) 0.0128(13) 0.0007(12) 0.0027(12) C17 0.0368(14) 0.0305(14) 0.084(3) 0.0074(14) -0.0008(14) 0.0001(11) C18 0.051(2) 0.0373(17) 0.112(4) 0.0230(19) 0.001(2) -0.0030(14) C19 0.061(2) 0.050(2) 0.145(5) 0.045(3) 0.016(3) 0.0050(19) C20 0.058(2) 0.081(3) 0.084(3) 0.051(2) 0.0139(19) 0.011(2) C21 0.0309(12) 0.0338(13) 0.0424(17) -0.0037(10) 0.0071(10) 0.0095(10) C22 0.0335(14) 0.0384(15) 0.075(2) 0.0090(14) -0.0063(13) 0.0074(12) C23 0.0342(15) 0.0390(16) 0.073(2) 0.0066(14) 0.0024(14) 0.0030(12) C24 0.0432(15) 0.0417(15) 0.0317(14) -0.0011(11) 0.0063(11) 0.0056(12) C25 0.0348(14) 0.0595(19) 0.0368(15) -0.0006(13) -0.0020(11) 0.0028(13) C26 0.0325(13) 0.0474(16) 0.0300(14) -0.0020(11) 0.0064(10) -0.0016(11) C27 0.057(2) 0.068(2) 0.0411(18) 0.0132(16) 0.0045(14) 0.0026(16) C28 0.0355(13) 0.0255(12) 0.0338(13) -0.0004(9) -0.0011(10) 0.0094(10) C29 0.0348(14) 0.0408(15) 0.0339(14) -0.0032(11) 0.0036(11) 0.0066(11) C30 0.0399(15) 0.0471(16) 0.0248(13) 0.0025(11) 0.0020(11) 0.0027(12) C31 0.0393(14) 0.0321(13) 0.0350(14) 0.0019(10) -0.0032(11) 0.0036(11) C32 0.0327(13) 0.0381(14) 0.0378(15) 0.0018(11) 0.0020(11) 0.0032(11) C33 0.0370(12) 0.0358(12) 0.0319(12) -0.0011(13) 0.0020(13) 0.0057(10) C34 0.0413(16) 0.0535(18) 0.0472(18) 0.0033(14) -0.0100(13) -0.0014(13) C35 0.0504(18) 0.0574(19) 0.0469(18) -0.0031(14) -0.0024(14) 0.0146(15) C36 0.0495(18) 0.0490(18) 0.059(2) -0.0174(15) 0.0015(15) -0.0061(14) C37 0.0527(19) 0.055(2) 0.060(2) -0.0001(16) 0.0090(16) -0.0083(15) C38 0.067(2) 0.070(2) 0.056(2) 0.0233(18) -0.0026(18) 0.0064(18) _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 N4 2.018(3) . ? Zr1 N3 2.021(2) . ? Zr1 N2 2.227(2) . ? Zr1 N1 2.254(2) . ? Zr1 O3 2.3225(16) . ? Zr1 O1 2.3473(17) . ? Zr1 S2 2.9682(7) . ? Zr1 S1 2.9741(7) . ? S1 O2 1.429(2) . ? S1 O1 1.480(2) . ? S1 N1 1.569(2) . ? S1 C21 1.760(3) . ? S2 O4 1.4316(19) . ? S2 O3 1.484(2) . ? S2 N2 1.569(2) . ? S2 C28 1.762(3) . ? N1 C2 1.422(3) . ? N2 C12 1.417(3) . ? N3 C36 1.446(4) . ? N3 C35 1.461(4) . ? N4 C38 1.451(4) . ? N4 C37 1.476(4) . ? C1 C2 1.382(4) . ? C1 C6 1.431(4) . ? C1 C11 1.496(4) . ? C2 C3 1.421(4) . ? C3 C4 1.353(4) . ? C3 H3 0.9500 . ? C4 C5 1.400(5) . ? C4 H4 0.9500 . ? C5 C10 1.422(4) . ? C5 C6 1.434(4) . ? C6 C7 1.411(4) . ? C7 C8 1.390(4) . ? C7 H7 0.9500 . ? C8 C9 1.406(6) . ? C8 H8 0.9500 . ? C9 C10 1.343(5) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.379(4) . ? C11 C16 1.441(4) . ? C12 C13 1.424(4) . ? C13 C14 1.363(5) . ? C13 H13 0.9500 . ? C14 C15 1.416(5) . ? C14 H14 0.9500 . ? C15 C16 1.425(5) . ? C15 C20 1.436(5) . ? C16 C17 1.411(4) . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(6) . ? C18 H18 0.9500 . ? C19 C20 1.360(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.380(4) . ? C21 C26 1.382(4) . ? C22 C23 1.372(4) . ? C22 H22 0.9500 . ? C23 C24 1.391(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 C27 1.512(4) . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.370(3) . ? C28 C29 1.394(4) . ? C29 C30 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.401(4) . ? C30 H30 0.9500 . ? C31 C32 1.383(4) . ? C31 C34 1.510(4) . ? C32 C33 1.379(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zr1 N3 108.40(10) . . ? N4 Zr1 N2 132.88(9) . . ? N3 Zr1 N2 103.47(9) . . ? N4 Zr1 N1 109.06(9) . . ? N3 Zr1 N1 129.06(9) . . ? N2 Zr1 N1 73.64(7) . . ? N4 Zr1 O3 80.93(9) . . ? N3 Zr1 O3 98.35(8) . . ? N2 Zr1 O3 60.61(7) . . ? N1 Zr1 O3 120.57(7) . . ? N4 Zr1 O1 94.24(9) . . ? N3 Zr1 O1 83.50(8) . . ? N2 Zr1 O1 123.43(7) . . ? N1 Zr1 O1 60.57(7) . . ? O3 Zr1 O1 175.15(8) . . ? N4 Zr1 S2 107.70(7) . . ? N3 Zr1 S2 100.87(7) . . ? N2 Zr1 S2 31.21(5) . . ? N1 Zr1 S2 99.28(5) . . ? O3 Zr1 S2 29.49(5) . . ? O1 Zr1 S2 154.64(5) . . ? N4 Zr1 S1 102.03(7) . . ? N3 Zr1 S1 107.45(7) . . ? N2 Zr1 S1 100.38(5) . . ? N1 Zr1 S1 31.23(5) . . ? O3 Zr1 S1 151.31(5) . . ? O1 Zr1 S1 29.39(5) . . ? S2 Zr1 S1 129.339(19) . . ? O2 S1 O1 117.18(12) . . ? O2 S1 N1 117.18(12) . . ? O1 S1 N1 99.20(11) . . ? O2 S1 C21 107.69(12) . . ? O1 S1 C21 106.14(12) . . ? N1 S1 C21 108.68(12) . . ? O2 S1 Zr1 132.41(9) . . ? O1 S1 Zr1 51.12(7) . . ? N1 S1 Zr1 48.16(8) . . ? C21 S1 Zr1 119.90(8) . . ? O4 S2 O3 116.63(13) . . ? O4 S2 N2 117.32(12) . . ? O3 S2 N2 97.56(10) . . ? O4 S2 C28 106.84(12) . . ? O3 S2 C28 108.61(12) . . ? N2 S2 C28 109.43(11) . . ? O4 S2 Zr1 130.17(9) . . ? O3 S2 Zr1 50.38(6) . . ? N2 S2 Zr1 47.35(8) . . ? C28 S2 Zr1 122.98(9) . . ? C2 N1 S1 127.85(17) . . ? C2 N1 Zr1 125.95(15) . . ? S1 N1 Zr1 100.61(10) . . ? C12 N2 S2 124.26(17) . . ? C12 N2 Zr1 133.88(16) . . ? S2 N2 Zr1 101.44(11) . . ? C36 N3 C35 112.6(3) . . ? C36 N3 Zr1 130.0(2) . . ? C35 N3 Zr1 114.91(19) . . ? C38 N4 C37 111.1(3) . . ? C38 N4 Zr1 134.6(2) . . ? C37 N4 Zr1 113.9(2) . . ? S1 O1 Zr1 99.49(9) . . ? S2 O3 Zr1 100.14(8) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 C11 120.8(2) . . ? C6 C1 C11 120.4(2) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 N1 119.6(2) . . ? C3 C2 N1 118.5(2) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C10 121.2(3) . . ? C4 C5 C6 119.8(3) . . ? C10 C5 C6 118.9(3) . . ? C7 C6 C1 121.9(3) . . ? C7 C6 C5 119.2(3) . . ? C1 C6 C5 118.9(3) . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 120.1(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 121.7(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C5 120.3(3) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C12 C11 C16 119.0(2) . . ? C12 C11 C1 120.9(2) . . ? C16 C11 C1 120.0(2) . . ? C11 C12 N2 119.7(2) . . ? C11 C12 C13 121.3(3) . . ? N2 C12 C13 118.8(3) . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 C20 121.5(3) . . ? C16 C15 C20 118.6(4) . . ? C17 C16 C15 118.5(3) . . ? C17 C16 C11 122.3(3) . . ? C15 C16 C11 119.0(3) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.5(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C15 120.7(4) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C22 C21 C26 119.6(3) . . ? C22 C21 S1 119.4(2) . . ? C26 C21 S1 120.9(2) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.9(3) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 118.0(3) . . ? C23 C24 C27 121.0(3) . . ? C25 C24 C27 121.0(3) . . ? C26 C25 C24 121.1(3) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C21 120.0(3) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 120.1(2) . . ? C33 C28 S2 120.3(2) . . ? C29 C28 S2 119.6(2) . . ? C30 C29 C28 119.0(2) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 121.3(2) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 118.2(2) . . ? C32 C31 C34 120.8(3) . . ? C30 C31 C34 121.0(2) . . ? C33 C32 C31 120.7(2) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C28 C33 C32 120.7(3) . . ? C28 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 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 N4 Zr1 S1 O2 16.29(15) . . . . ? N3 Zr1 S1 O2 130.20(15) . . . . ? N2 Zr1 S1 O2 -121.99(14) . . . . ? N1 Zr1 S1 O2 -90.71(17) . . . . ? O3 Zr1 S1 O2 -76.77(17) . . . . ? O1 Zr1 S1 O2 93.33(17) . . . . ? S2 Zr1 S1 O2 -108.92(13) . . . . ? N4 Zr1 S1 O1 -77.04(13) . . . . ? N3 Zr1 S1 O1 36.87(13) . . . . ? N2 Zr1 S1 O1 144.68(12) . . . . ? N1 Zr1 S1 O1 175.95(16) . . . . ? O3 Zr1 S1 O1 -170.10(16) . . . . ? S2 Zr1 S1 O1 157.75(11) . . . . ? N4 Zr1 S1 N1 107.00(14) . . . . ? N3 Zr1 S1 N1 -139.08(14) . . . . ? N2 Zr1 S1 N1 -31.27(12) . . . . ? O3 Zr1 S1 N1 13.94(17) . . . . ? O1 Zr1 S1 N1 -175.95(16) . . . . ? S2 Zr1 S1 N1 -18.20(12) . . . . ? N4 Zr1 S1 C21 -164.08(13) . . . . ? N3 Zr1 S1 C21 -50.16(13) . . . . ? N2 Zr1 S1 C21 57.65(12) . . . . ? N1 Zr1 S1 C21 88.92(15) . . . . ? O3 Zr1 S1 C21 102.86(16) . . . . ? O1 Zr1 S1 C21 -87.04(15) . . . . ? S2 Zr1 S1 C21 70.72(11) . . . . ? N4 Zr1 S2 O4 119.35(14) . . . . ? N3 Zr1 S2 O4 5.85(14) . . . . ? N2 Zr1 S2 O4 -92.25(16) . . . . ? N1 Zr1 S2 O4 -127.11(13) . . . . ? O3 Zr1 S2 O4 93.60(17) . . . . ? O1 Zr1 S2 O4 -91.96(18) . . . . ? S1 Zr1 S2 O4 -117.67(12) . . . . ? N4 Zr1 S2 O3 25.75(13) . . . . ? N3 Zr1 S2 O3 -87.75(13) . . . . ? N2 Zr1 S2 O3 174.16(16) . . . . ? N1 Zr1 S2 O3 139.29(13) . . . . ? O1 Zr1 S2 O3 174.44(17) . . . . ? S1 Zr1 S2 O3 148.73(11) . . . . ? N4 Zr1 S2 N2 -148.41(13) . . . . ? N3 Zr1 S2 N2 98.09(13) . . . . ? N1 Zr1 S2 N2 -34.87(12) . . . . ? O3 Zr1 S2 N2 -174.16(16) . . . . ? O1 Zr1 S2 N2 0.28(17) . . . . ? S1 Zr1 S2 N2 -25.42(11) . . . . ? N4 Zr1 S2 C28 -61.77(13) . . . . ? N3 Zr1 S2 C28 -175.27(12) . . . . ? N2 Zr1 S2 C28 86.64(15) . . . . ? N1 Zr1 S2 C28 51.77(12) . . . . ? O3 Zr1 S2 C28 -87.52(15) . . . . ? O1 Zr1 S2 C28 86.92(17) . . . . ? S1 Zr1 S2 C28 61.22(11) . . . . ? O2 S1 N1 C2 -30.5(3) . . . . ? O1 S1 N1 C2 -157.6(2) . . . . ? C21 S1 N1 C2 91.8(2) . . . . ? Zr1 S1 N1 C2 -154.4(3) . . . . ? O2 S1 N1 Zr1 123.92(12) . . . . ? O1 S1 N1 Zr1 -3.19(13) . . . . ? C21 S1 N1 Zr1 -113.80(12) . . . . ? N4 Zr1 N1 C2 73.4(2) . . . . ? N3 Zr1 N1 C2 -151.33(19) . . . . ? N2 Zr1 N1 C2 -57.1(2) . . . . ? O3 Zr1 N1 C2 -17.2(2) . . . . ? O1 Zr1 N1 C2 157.4(2) . . . . ? S2 Zr1 N1 C2 -39.1(2) . . . . ? S1 Zr1 N1 C2 155.1(3) . . . . ? N4 Zr1 N1 S1 -81.69(13) . . . . ? N3 Zr1 N1 S1 53.58(16) . . . . ? N2 Zr1 N1 S1 147.85(12) . . . . ? O3 Zr1 N1 S1 -172.28(9) . . . . ? O1 Zr1 N1 S1 2.28(9) . . . . ? S2 Zr1 N1 S1 165.83(9) . . . . ? O4 S2 N2 C12 -52.7(3) . . . . ? O3 S2 N2 C12 -178.0(2) . . . . ? C28 S2 N2 C12 69.2(2) . . . . ? Zr1 S2 N2 C12 -173.5(3) . . . . ? O4 S2 N2 Zr1 120.74(12) . . . . ? O3 S2 N2 Zr1 -4.54(12) . . . . ? C28 S2 N2 Zr1 -117.38(11) . . . . ? N4 Zr1 N2 C12 -144.6(2) . . . . ? N3 Zr1 N2 C12 83.7(2) . . . . ? N1 Zr1 N2 C12 -43.5(2) . . . . ? O3 Zr1 N2 C12 175.8(3) . . . . ? O1 Zr1 N2 C12 -7.4(3) . . . . ? S2 Zr1 N2 C12 172.5(3) . . . . ? S1 Zr1 N2 C12 -27.2(2) . . . . ? N4 Zr1 N2 S2 42.93(17) . . . . ? N3 Zr1 N2 S2 -88.79(11) . . . . ? N1 Zr1 N2 S2 143.98(12) . . . . ? O3 Zr1 N2 S2 3.30(9) . . . . ? O1 Zr1 N2 S2 -179.85(9) . . . . ? S1 Zr1 N2 S2 160.27(8) . . . . ? N4 Zr1 N3 C36 -10.7(3) . . . . ? N2 Zr1 N3 C36 134.1(2) . . . . ? N1 Zr1 N3 C36 -146.2(2) . . . . ? O3 Zr1 N3 C36 72.4(2) . . . . ? O1 Zr1 N3 C36 -103.1(2) . . . . ? S2 Zr1 N3 C36 102.2(2) . . . . ? S1 Zr1 N3 C36 -120.3(2) . . . . ? N4 Zr1 N3 C35 150.1(2) . . . . ? N2 Zr1 N3 C35 -65.1(2) . . . . ? N1 Zr1 N3 C35 14.6(3) . . . . ? O3 Zr1 N3 C35 -126.8(2) . . . . ? O1 Zr1 N3 C35 57.8(2) . . . . ? S2 Zr1 N3 C35 -96.9(2) . . . . ? S1 Zr1 N3 C35 40.5(2) . . . . ? N3 Zr1 N4 C38 123.7(3) . . . . ? N2 Zr1 N4 C38 -6.4(4) . . . . ? N1 Zr1 N4 C38 -91.4(3) . . . . ? O3 Zr1 N4 C38 27.9(3) . . . . ? O1 Zr1 N4 C38 -151.7(3) . . . . ? S2 Zr1 N4 C38 15.4(3) . . . . ? S1 Zr1 N4 C38 -123.1(3) . . . . ? N3 Zr1 N4 C37 -48.3(2) . . . . ? N2 Zr1 N4 C37 -178.38(18) . . . . ? N1 Zr1 N4 C37 96.6(2) . . . . ? O3 Zr1 N4 C37 -144.1(2) . . . . ? O1 Zr1 N4 C37 36.3(2) . . . . ? S2 Zr1 N4 C37 -156.6(2) . . . . ? S1 Zr1 N4 C37 64.9(2) . . . . ? O2 S1 O1 Zr1 -124.05(11) . . . . ? N1 S1 O1 Zr1 3.05(12) . . . . ? C21 S1 O1 Zr1 115.67(10) . . . . ? N4 Zr1 O1 S1 107.11(12) . . . . ? N3 Zr1 O1 S1 -144.82(12) . . . . ? N2 Zr1 O1 S1 -42.95(14) . . . . ? N1 Zr1 O1 S1 -2.41(9) . . . . ? O3 Zr1 O1 S1 102.5(8) . . . . ? S2 Zr1 O1 S1 -43.1(2) . . . . ? O4 S2 O3 Zr1 -121.44(11) . . . . ? N2 S2 O3 Zr1 4.33(12) . . . . ? C28 S2 O3 Zr1 117.83(10) . . . . ? N4 Zr1 O3 S2 -155.22(13) . . . . ? N3 Zr1 O3 S2 97.34(12) . . . . ? N2 Zr1 O3 S2 -3.47(9) . . . . ? N1 Zr1 O3 S2 -48.38(15) . . . . ? O1 Zr1 O3 S2 -150.6(7) . . . . ? S1 Zr1 O3 S2 -56.72(19) . . . . ? C6 C1 C2 C3 3.7(4) . . . . ? C11 C1 C2 C3 -178.0(2) . . . . ? C6 C1 C2 N1 -167.8(2) . . . . ? C11 C1 C2 N1 10.4(4) . . . . ? S1 N1 C2 C1 -130.5(2) . . . . ? Zr1 N1 C2 C1 81.1(3) . . . . ? S1 N1 C2 C3 57.6(3) . . . . ? Zr1 N1 C2 C3 -90.7(3) . . . . ? C1 C2 C3 C4 -1.9(4) . . . . ? N1 C2 C3 C4 169.8(3) . . . . ? C2 C3 C4 C5 -0.9(4) . . . . ? C3 C4 C5 C10 -175.7(3) . . . . ? C3 C4 C5 C6 1.7(5) . . . . ? C2 C1 C6 C7 173.3(2) . . . . ? C11 C1 C6 C7 -4.9(4) . . . . ? C2 C1 C6 C5 -2.8(4) . . . . ? C11 C1 C6 C5 178.9(3) . . . . ? C4 C5 C6 C7 -176.1(3) . . . . ? C10 C5 C6 C7 1.4(4) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C10 C5 C6 C1 177.7(3) . . . . ? C1 C6 C7 C8 -176.4(3) . . . . ? C5 C6 C7 C8 -0.3(4) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 -0.4(6) . . . . ? C8 C9 C10 C5 1.5(6) . . . . ? C4 C5 C10 C9 175.4(3) . . . . ? C6 C5 C10 C9 -2.0(5) . . . . ? C2 C1 C11 C12 -62.7(4) . . . . ? C6 C1 C11 C12 115.5(3) . . . . ? C2 C1 C11 C16 114.4(3) . . . . ? C6 C1 C11 C16 -67.4(3) . . . . ? C16 C11 C12 N2 -170.5(2) . . . . ? C1 C11 C12 N2 6.5(4) . . . . ? C16 C11 C12 C13 4.0(4) . . . . ? C1 C11 C12 C13 -178.9(2) . . . . ? S2 N2 C12 C11 -113.0(2) . . . . ? Zr1 N2 C12 C11 75.9(3) . . . . ? S2 N2 C12 C13 72.3(3) . . . . ? Zr1 N2 C12 C13 -98.8(3) . . . . ? C11 C12 C13 C14 -3.0(4) . . . . ? N2 C12 C13 C14 171.6(2) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 2.5(4) . . . . ? C13 C14 C15 C20 -173.4(3) . . . . ? C14 C15 C16 C17 -177.5(3) . . . . ? C20 C15 C16 C17 -1.5(4) . . . . ? C14 C15 C16 C11 -1.4(4) . . . . ? C20 C15 C16 C11 174.6(3) . . . . ? C12 C11 C16 C17 174.1(3) . . . . ? C1 C11 C16 C17 -3.0(4) . . . . ? C12 C11 C16 C15 -1.8(4) . . . . ? C1 C11 C16 C15 -178.9(3) . . . . ? C15 C16 C17 C18 2.0(4) . . . . ? C11 C16 C17 C18 -174.0(3) . . . . ? C16 C17 C18 C19 -1.2(5) . . . . ? C17 C18 C19 C20 -0.1(6) . . . . ? C18 C19 C20 C15 0.6(6) . . . . ? C14 C15 C20 C19 176.2(3) . . . . ? C16 C15 C20 C19 0.2(5) . . . . ? O2 S1 C21 C22 89.8(2) . . . . ? O1 S1 C21 C22 -144.0(2) . . . . ? N1 S1 C21 C22 -38.1(3) . . . . ? Zr1 S1 C21 C22 -90.0(2) . . . . ? O2 S1 C21 C26 -87.1(2) . . . . ? O1 S1 C21 C26 39.1(2) . . . . ? N1 S1 C21 C26 145.0(2) . . . . ? Zr1 S1 C21 C26 93.2(2) . . . . ? C26 C21 C22 C23 -1.9(4) . . . . ? S1 C21 C22 C23 -178.8(2) . . . . ? C21 C22 C23 C24 1.4(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C22 C23 C24 C27 -179.7(3) . . . . ? C23 C24 C25 C26 -1.6(4) . . . . ? C27 C24 C25 C26 178.4(3) . . . . ? C24 C25 C26 C21 1.1(4) . . . . ? C22 C21 C26 C25 0.6(4) . . . . ? S1 C21 C26 C25 177.5(2) . . . . ? O4 S2 C28 C33 17.6(2) . . . . ? O3 S2 C28 C33 144.24(19) . . . . ? N2 S2 C28 C33 -110.3(2) . . . . ? Zr1 S2 C28 C33 -161.47(16) . . . . ? O4 S2 C28 C29 -163.7(2) . . . . ? O3 S2 C28 C29 -37.1(2) . . . . ? N2 S2 C28 C29 68.3(2) . . . . ? Zr1 S2 C28 C29 17.2(3) . . . . ? C33 C28 C29 C30 -2.0(4) . . . . ? S2 C28 C29 C30 179.3(2) . . . . ? C28 C29 C30 C31 2.0(4) . . . . ? C29 C30 C31 C32 -0.3(4) . . . . ? C29 C30 C31 C34 -179.8(3) . . . . ? C30 C31 C32 C33 -1.3(4) . . . . ? C34 C31 C32 C33 178.2(2) . . . . ? C29 C28 C33 C32 0.4(4) . . . . ? S2 C28 C33 C32 179.03(19) . . . . ? C31 C32 C33 C28 1.3(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.029 29.4 -0.1 2 0.500 0.500 -0.006 190.3 22.0 3 0.000 0.500 0.124 14.3 0.6 4 0.500 0.000 0.124 14.3 0.6 5 0.500 0.500 0.312 18.5 -0.2 6 0.000 0.000 0.494 190.4 22.0 7 0.500 0.500 0.532 29.0 0.0 8 0.000 0.500 0.624 14.3 0.6 9 0.500 0.000 0.624 14.3 0.6 10 0.000 0.000 0.809 18.2 -0.2 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.433 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.058 # Attachment 'compound_9.cif' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 742597' #TrackingRef 'compound_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H44 N4 O2 P2 Zr' _chemical_formula_sum 'C48 H44 N4 O2 P2 Zr' _chemical_formula_weight 862.03 _chemical_absolute_configuration rmad 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.0044(4) _cell_length_b 39.4540(11) _cell_length_c 18.1111(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.427(2) _cell_angle_gamma 90.00 _cell_volume 8436.2(5) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 19159 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 0.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9347 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57397 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.88 _reflns_number_total 32663 _reflns_number_gt 29182 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0495P)^2^+0.5815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(17) _refine_ls_number_reflns 32663 _refine_ls_number_parameters 2100 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.30493(3) 0.738340(9) 0.22051(2) 0.01847(8) Uani 1 1 d . . . Zr2 Zr -0.00065(3) 0.184315(9) 0.27332(2) 0.01667(8) Uani 1 1 d . . . Zr3 Zr 0.82687(4) 0.410625(10) 0.91611(2) 0.02201(9) Uani 1 1 d . . . Zr4 Zr 0.22185(3) 0.490947(10) 0.52529(2) 0.02089(9) Uani 1 1 d . A . P1 P 0.47890(9) 0.75381(3) 0.13200(6) 0.0210(2) Uani 1 1 d . . . P2 P 0.25085(9) 0.67921(3) 0.30559(6) 0.0186(2) Uani 1 1 d . . . P3 P -0.00303(9) 0.25039(3) 0.34479(5) 0.0173(2) Uani 1 1 d . . . P4 P 0.16873(9) 0.15430(3) 0.19672(6) 0.0180(2) Uani 1 1 d . . . P5 P 0.62970(10) 0.38265(3) 0.96764(6) 0.0207(2) Uani 1 1 d . . . P6 P 0.92978(10) 0.47793(3) 0.93117(6) 0.0219(2) Uani 1 1 d . . . P7 P 0.41804(9) 0.52184(3) 0.47797(6) 0.0204(2) Uani 1 1 d . A . P8 P 0.11838(10) 0.42383(3) 0.51110(6) 0.0251(2) Uani 1 1 d . . . O1 O 0.3570(2) 0.76596(7) 0.12321(15) 0.0237(6) Uani 1 1 d . . . O2 O 0.2310(2) 0.71663(7) 0.31806(15) 0.0202(6) Uani 1 1 d . . . O3 O -0.0989(2) 0.22969(7) 0.29780(15) 0.0183(6) Uani 1 1 d . . . O4 O 0.0943(2) 0.13617(7) 0.24413(15) 0.0209(6) Uani 1 1 d . . . O5 O 0.6792(3) 0.37354(7) 0.89835(15) 0.0239(6) Uani 1 1 d . . . O6 O 0.9862(2) 0.44339(7) 0.93271(16) 0.0249(6) Uani 1 1 d . . . O7 O 0.3105(2) 0.53782(7) 0.49462(15) 0.0220(6) Uani 1 1 d . . . O8 O 0.1168(3) 0.45061(8) 0.57124(17) 0.0315(7) Uani 1 1 d . A . N1 N 0.4797(3) 0.72643(8) 0.19722(18) 0.0194(7) Uani 1 1 d . . . N2 N 0.3260(3) 0.68147(9) 0.24128(17) 0.0182(7) Uani 1 1 d . . . N3 N 0.1027(3) 0.22619(8) 0.34146(17) 0.0158(6) Uani 1 1 d . . . N4 N 0.1498(3) 0.19279(8) 0.21925(17) 0.0163(7) Uani 1 1 d . . . N5 N 0.7048(3) 0.41503(8) 0.99607(18) 0.0218(7) Uani 1 1 d . . . N6 N 0.8017(3) 0.46723(8) 0.92885(19) 0.0217(7) Uani 1 1 d . . . N7 N 0.3921(3) 0.48266(8) 0.49078(19) 0.0203(7) Uani 1 1 d . . . N8 N 0.2034(3) 0.44104(9) 0.46298(19) 0.0220(7) Uani 1 1 d . A . N9 N 0.1475(3) 0.74106(10) 0.15377(19) 0.0260(8) Uani 1 1 d . . . N10 N 0.3392(3) 0.77877(9) 0.2909(2) 0.0271(8) Uani 1 1 d . . . N11 N -0.0439(3) 0.15346(9) 0.35377(18) 0.0208(7) Uani 1 1 d . . . N12 N -0.1256(3) 0.17933(9) 0.18119(18) 0.0220(7) Uani 1 1 d . . . N13 N 0.9381(3) 0.37633(9) 0.9715(2) 0.0274(8) Uani 1 1 d . . . N14 N 0.8145(4) 0.40762(11) 0.8023(2) 0.0397(10) Uani 1 1 d . . . N15 N 0.2619(3) 0.50402(10) 0.63681(19) 0.0305(9) Uani 1 1 d . . . N16 N 0.0819(3) 0.51597(10) 0.4704(2) 0.0296(8) Uani 1 1 d . . . C1 C 0.5652(3) 0.67303(10) 0.2440(2) 0.0171(8) Uani 1 1 d . . . C2 C 0.5660(3) 0.70837(10) 0.2437(2) 0.0175(8) Uani 1 1 d . . . C3 C 0.6497(3) 0.72571(11) 0.2947(2) 0.0219(8) Uani 1 1 d . . . H3 H 0.6514 0.7498 0.2937 0.026 Uiso 1 1 calc R . . C4 C 0.7285(3) 0.70869(11) 0.3455(2) 0.0228(9) Uani 1 1 d . . . H4 H 0.7840 0.7211 0.3787 0.027 Uiso 1 1 calc R . . C5 C 0.7285(4) 0.67302(11) 0.3493(2) 0.0224(9) Uani 1 1 d . . . C6 C 0.6449(3) 0.65485(10) 0.2984(2) 0.0169(8) Uani 1 1 d . . . C7 C 0.6395(3) 0.61892(10) 0.3053(2) 0.0208(8) Uani 1 1 d . . . H7 H 0.5820 0.6064 0.2738 0.025 Uiso 1 1 calc R . . C8 C 0.7179(3) 0.60243(11) 0.3579(2) 0.0229(9) Uani 1 1 d . . . H8 H 0.7148 0.5784 0.3614 0.028 Uiso 1 1 calc R . . C9 C 0.8028(4) 0.62022(12) 0.4066(2) 0.0276(10) Uani 1 1 d . . . H9 H 0.8568 0.6083 0.4420 0.033 Uiso 1 1 calc R . . C10 C 0.8066(4) 0.65510(12) 0.4024(2) 0.0265(9) Uani 1 1 d . . . H10 H 0.8629 0.6672 0.4358 0.032 Uiso 1 1 calc R . . C11 C 0.4779(3) 0.65400(10) 0.1902(2) 0.0171(8) Uani 1 1 d . . . C12 C 0.3637(3) 0.65755(10) 0.1936(2) 0.0172(8) Uani 1 1 d . . . C13 C 0.2816(4) 0.63879(12) 0.1430(2) 0.0271(9) Uani 1 1 d . . . H13 H 0.2035 0.6413 0.1451 0.033 Uiso 1 1 calc R . . C14 C 0.3135(4) 0.61730(12) 0.0917(2) 0.0296(10) Uani 1 1 d . . . H14 H 0.2577 0.6041 0.0604 0.036 Uiso 1 1 calc R . . C15 C 0.4285(4) 0.61428(11) 0.0842(2) 0.0231(9) Uani 1 1 d . . . C16 C 0.5116(3) 0.63317(10) 0.1338(2) 0.0179(8) Uani 1 1 d . . . C17 C 0.6249(3) 0.63143(10) 0.1223(2) 0.0186(8) Uani 1 1 d . . . H17 H 0.6814 0.6444 0.1536 0.022 Uiso 1 1 calc R . . C18 C 0.6550(4) 0.61158(11) 0.0671(2) 0.0219(8) Uani 1 1 d . . . H18 H 0.7320 0.6108 0.0611 0.026 Uiso 1 1 calc R . . C19 C 0.5722(4) 0.59214(11) 0.0186(2) 0.0264(9) Uani 1 1 d . . . H19 H 0.5932 0.5782 -0.0194 0.032 Uiso 1 1 calc R . . C20 C 0.4623(4) 0.59397(11) 0.0280(2) 0.0271(9) Uani 1 1 d . . . H20 H 0.4067 0.5812 -0.0043 0.032 Uiso 1 1 calc R . . C21 C 0.5072(3) 0.73487(11) 0.0465(2) 0.0229(9) Uani 1 1 d . . . C22 C 0.5648(4) 0.75168(13) -0.0029(2) 0.0316(10) Uani 1 1 d . . . H22 H 0.5948 0.7737 0.0090 0.038 Uiso 1 1 calc R . . C23 C 0.5782(4) 0.73595(15) -0.0701(3) 0.0385(12) Uani 1 1 d . . . H23 H 0.6188 0.7471 -0.1034 0.046 Uiso 1 1 calc R . . C24 C 0.5324(4) 0.70420(14) -0.0880(3) 0.0352(11) Uani 1 1 d . . . H24 H 0.5399 0.6940 -0.1343 0.042 Uiso 1 1 calc R . . C25 C 0.4759(4) 0.68727(13) -0.0393(2) 0.0327(10) Uani 1 1 d . . . H25 H 0.4466 0.6652 -0.0509 0.039 Uiso 1 1 calc R . . C26 C 0.4624(4) 0.70326(11) 0.0276(2) 0.0265(9) Uani 1 1 d . . . H26 H 0.4214 0.6920 0.0606 0.032 Uiso 1 1 calc R . . C27 C 0.5779(4) 0.78778(11) 0.1572(2) 0.0280(10) Uani 1 1 d . . . C28 C 0.5395(5) 0.81808(12) 0.1825(3) 0.0336(11) Uani 1 1 d . . . H28 H 0.4605 0.8212 0.1800 0.040 Uiso 1 1 calc R . . C29 C 0.6131(5) 0.84388(14) 0.2113(3) 0.0480(15) Uani 1 1 d . . . H29 H 0.5859 0.8644 0.2289 0.058 Uiso 1 1 calc R . . C30 C 0.7290(5) 0.83860(15) 0.2135(3) 0.0525(16) Uani 1 1 d . . . H30 H 0.7809 0.8559 0.2335 0.063 Uiso 1 1 calc R . . C31 C 0.7694(5) 0.80957(15) 0.1878(3) 0.0468(14) Uani 1 1 d . . . H31 H 0.8483 0.8068 0.1890 0.056 Uiso 1 1 calc R . . C32 C 0.6936(4) 0.78366(13) 0.1596(3) 0.0354(11) Uani 1 1 d . . . H32 H 0.7214 0.7632 0.1421 0.043 Uiso 1 1 calc R . . C33 C 0.1173(3) 0.65771(11) 0.2807(2) 0.0207(8) Uani 1 1 d . . . C34 C 0.0204(3) 0.67765(11) 0.2581(2) 0.0242(9) Uani 1 1 d . . . H34 H 0.0268 0.7016 0.2568 0.029 Uiso 1 1 calc R . . C35 C -0.0859(4) 0.66223(12) 0.2376(2) 0.0254(9) Uani 1 1 d . . . H35 H -0.1519 0.6756 0.2225 0.030 Uiso 1 1 calc R . . C36 C -0.0935(4) 0.62710(11) 0.2394(2) 0.0263(9) Uani 1 1 d . . . H36 H -0.1655 0.6166 0.2258 0.032 Uiso 1 1 calc R . . C37 C 0.0012(4) 0.60717(11) 0.2607(2) 0.0231(9) Uani 1 1 d . . . H37 H -0.0054 0.5832 0.2618 0.028 Uiso 1 1 calc R . . C38 C 0.1057(4) 0.62252(10) 0.2804(2) 0.0222(9) Uani 1 1 d . . . H38 H 0.1712 0.6088 0.2942 0.027 Uiso 1 1 calc R . . C39 C 0.3241(3) 0.65822(10) 0.3879(2) 0.0207(8) Uani 1 1 d . . . C40 C 0.2678(4) 0.64034(11) 0.4370(2) 0.0267(9) Uani 1 1 d . . . H40 H 0.1874 0.6395 0.4282 0.032 Uiso 1 1 calc R . . C41 C 0.3311(4) 0.62370(12) 0.4995(2) 0.0324(11) Uani 1 1 d . . . H41 H 0.2935 0.6110 0.5322 0.039 Uiso 1 1 calc R . . C42 C 0.4470(4) 0.62584(12) 0.5134(2) 0.0330(11) Uani 1 1 d . . . H42 H 0.4893 0.6144 0.5554 0.040 Uiso 1 1 calc R . . C43 C 0.5031(4) 0.64453(13) 0.4666(2) 0.0340(11) Uani 1 1 d . . . H43 H 0.5833 0.6464 0.4775 0.041 Uiso 1 1 calc R . . C44 C 0.4423(4) 0.66041(12) 0.4043(2) 0.0277(10) Uani 1 1 d . . . H44 H 0.4811 0.6730 0.3721 0.033 Uiso 1 1 calc R . . C45 C 0.2913(3) 0.23957(10) 0.31330(19) 0.0163(7) Uani 1 1 d . . . C46 C 0.2199(3) 0.23148(10) 0.3646(2) 0.0182(8) Uani 1 1 d . . . C47 C 0.2674(4) 0.22556(11) 0.4406(2) 0.0233(9) Uani 1 1 d . . . H47 H 0.2184 0.2206 0.4748 0.028 Uiso 1 1 calc R . . C48 C 0.3809(4) 0.22674(11) 0.4665(2) 0.0260(9) Uani 1 1 d . . . H48 H 0.4100 0.2235 0.5184 0.031 Uiso 1 1 calc R . . C49 C 0.4557(3) 0.23290(11) 0.4157(2) 0.0223(9) Uani 1 1 d . . . C50 C 0.4108(3) 0.23922(10) 0.3389(2) 0.0190(8) Uani 1 1 d . . . C51 C 0.4901(3) 0.24353(11) 0.2895(2) 0.0228(9) Uani 1 1 d . . . H51 H 0.4626 0.2477 0.2377 0.027 Uiso 1 1 calc R . . C52 C 0.6047(4) 0.24181(12) 0.3146(2) 0.0284(10) Uani 1 1 d . . . H52 H 0.6551 0.2448 0.2802 0.034 Uiso 1 1 calc R . . C53 C 0.6481(4) 0.23570(12) 0.3907(2) 0.0287(10) Uani 1 1 d . . . H53 H 0.7277 0.2347 0.4079 0.034 Uiso 1 1 calc R . . C54 C 0.5760(4) 0.23126(12) 0.4400(2) 0.0274(10) Uani 1 1 d . . . H54 H 0.6060 0.2270 0.4913 0.033 Uiso 1 1 calc R . . C55 C 0.2403(3) 0.24807(10) 0.2334(2) 0.0160(7) Uani 1 1 d . . . C56 C 0.1732(3) 0.22466(10) 0.1890(2) 0.0166(8) Uani 1 1 d . . . C57 C 0.1176(3) 0.23309(10) 0.1156(2) 0.0203(8) Uani 1 1 d . . . H57 H 0.0665 0.2174 0.0877 0.024 Uiso 1 1 calc R . . C58 C 0.1367(4) 0.26337(11) 0.0845(2) 0.0243(9) Uani 1 1 d . . . H58 H 0.1018 0.2683 0.0343 0.029 Uiso 1 1 calc R . . C59 C 0.2082(4) 0.28763(10) 0.1266(2) 0.0201(8) Uani 1 1 d . . . C60 C 0.2576(3) 0.28040(10) 0.2023(2) 0.0178(8) Uani 1 1 d . . . C61 C 0.3252(3) 0.30649(10) 0.2433(2) 0.0197(8) Uani 1 1 d . . . H61 H 0.3567 0.3030 0.2947 0.024 Uiso 1 1 calc R . . C62 C 0.3451(4) 0.33632(11) 0.2098(2) 0.0253(9) Uani 1 1 d . . . H62 H 0.3902 0.3532 0.2382 0.030 Uiso 1 1 calc R . . C63 C 0.3000(4) 0.34243(11) 0.1341(2) 0.0273(9) Uani 1 1 d . . . H63 H 0.3168 0.3630 0.1111 0.033 Uiso 1 1 calc R . . C64 C 0.2321(4) 0.31893(11) 0.0935(2) 0.0253(9) Uani 1 1 d . . . H64 H 0.2003 0.3234 0.0425 0.030 Uiso 1 1 calc R . . C65 C -0.0344(3) 0.25633(10) 0.4376(2) 0.0199(8) Uani 1 1 d . . . C66 C -0.0730(4) 0.28696(11) 0.4616(2) 0.0249(9) Uani 1 1 d . . . H66 H -0.0751 0.3066 0.4310 0.030 Uiso 1 1 calc R . . C67 C -0.1082(4) 0.28879(12) 0.5304(2) 0.0280(10) Uani 1 1 d . . . H67 H -0.1348 0.3097 0.5465 0.034 Uiso 1 1 calc R . . C68 C -0.1051(4) 0.26058(12) 0.5755(2) 0.0287(10) Uani 1 1 d . . . H68 H -0.1293 0.2621 0.6225 0.034 Uiso 1 1 calc R . . C69 C -0.0664(4) 0.23010(11) 0.5521(2) 0.0282(10) Uani 1 1 d . . . H69 H -0.0647 0.2106 0.5831 0.034 Uiso 1 1 calc R . . C70 C -0.0301(4) 0.22766(11) 0.4837(2) 0.0245(9) Uani 1 1 d . . . H70 H -0.0026 0.2067 0.4683 0.029 Uiso 1 1 calc R . . C71 C 0.0098(3) 0.29127(10) 0.3049(2) 0.0198(8) Uani 1 1 d . . . C72 C -0.0601(4) 0.29992(11) 0.2381(2) 0.0283(10) Uani 1 1 d . . . H72 H -0.1185 0.2848 0.2163 0.034 Uiso 1 1 calc R . . C73 C -0.0461(5) 0.33016(12) 0.2027(3) 0.0360(12) Uani 1 1 d . . . H73 H -0.0940 0.3358 0.1566 0.043 Uiso 1 1 calc R . . C74 C 0.0393(4) 0.35233(11) 0.2353(3) 0.0339(11) Uani 1 1 d . . . H74 H 0.0495 0.3732 0.2115 0.041 Uiso 1 1 calc R . . C75 C 0.1082(4) 0.34408(11) 0.3015(3) 0.0292(10) Uani 1 1 d . . . H75 H 0.1658 0.3594 0.3233 0.035 Uiso 1 1 calc R . . C76 C 0.0954(4) 0.31389(11) 0.3369(2) 0.0226(9) Uani 1 1 d . . . H76 H 0.1440 0.3084 0.3828 0.027 Uiso 1 1 calc R . . C77 C 0.3155(3) 0.14201(10) 0.2174(2) 0.0180(8) Uani 1 1 d . . . C78 C 0.3859(4) 0.15644(11) 0.2796(2) 0.0242(9) Uani 1 1 d . . . H78 H 0.3550 0.1719 0.3107 0.029 Uiso 1 1 calc R . . C79 C 0.4987(4) 0.14851(12) 0.2959(3) 0.0295(10) Uani 1 1 d . . . H79 H 0.5460 0.1589 0.3375 0.035 Uiso 1 1 calc R . . C80 C 0.5443(4) 0.12525(12) 0.2519(3) 0.0299(10) Uani 1 1 d . . . H80 H 0.6223 0.1195 0.2636 0.036 Uiso 1 1 calc R . . C81 C 0.4746(4) 0.11059(13) 0.1907(3) 0.0321(10) Uani 1 1 d . . . H81 H 0.5054 0.0947 0.1606 0.039 Uiso 1 1 calc R . . C82 C 0.3613(4) 0.11887(11) 0.1733(2) 0.0264(9) Uani 1 1 d . . . H82 H 0.3145 0.1088 0.1311 0.032 Uiso 1 1 calc R . . C83 C 0.1220(4) 0.14546(10) 0.0985(2) 0.0217(8) Uani 1 1 d . . . C84 C 0.0288(4) 0.12509(14) 0.0755(3) 0.0361(11) Uani 1 1 d . . . H84 H -0.0063 0.1136 0.1113 0.043 Uiso 1 1 calc R . . C85 C -0.0133(4) 0.12153(18) -0.0010(3) 0.0536(17) Uani 1 1 d . . . H85 H -0.0755 0.1068 -0.0172 0.064 Uiso 1 1 calc R . . C86 C 0.0329(4) 0.13873(18) -0.0528(3) 0.0533(17) Uani 1 1 d . . . H86 H 0.0007 0.1367 -0.1046 0.064 Uiso 1 1 calc R . . C87 C 0.1269(4) 0.15927(14) -0.0308(2) 0.0382(12) Uani 1 1 d . . . H87 H 0.1596 0.1713 -0.0670 0.046 Uiso 1 1 calc R . . C88 C 0.1721(4) 0.16193(12) 0.0446(2) 0.0281(10) Uani 1 1 d . . . H88 H 0.2383 0.1752 0.0601 0.034 Uiso 1 1 calc R . . C89 C 0.6984(4) 0.46876(10) 1.0608(2) 0.0194(8) Uani 1 1 d . . . C90 C 0.7254(3) 0.43442(10) 1.0624(2) 0.0190(8) Uani 1 1 d . . . C91 C 0.7828(4) 0.41923(11) 1.1299(2) 0.0238(9) Uani 1 1 d . . . H91 H 0.7996 0.3957 1.1307 0.029 Uiso 1 1 calc R . . C92 C 0.8139(4) 0.43797(11) 1.1933(2) 0.0243(9) Uani 1 1 d . . . H92 H 0.8533 0.4274 1.2376 0.029 Uiso 1 1 calc R . . C93 C 0.7882(4) 0.47297(11) 1.1941(2) 0.0229(9) Uani 1 1 d . . . C94 C 0.7297(3) 0.48879(11) 1.1276(2) 0.0215(8) Uani 1 1 d . . . C95 C 0.7058(4) 0.52373(11) 1.1303(2) 0.0238(9) Uani 1 1 d . . . H95 H 0.6672 0.5348 1.0865 0.029 Uiso 1 1 calc R . . C96 C 0.7371(4) 0.54194(11) 1.1948(2) 0.0256(9) Uani 1 1 d . . . H96 H 0.7188 0.5654 1.1955 0.031 Uiso 1 1 calc R . . C97 C 0.7958(4) 0.52654(12) 1.2598(2) 0.0297(10) Uani 1 1 d . . . H97 H 0.8181 0.5395 1.3041 0.036 Uiso 1 1 calc R . . C98 C 0.8210(4) 0.49305(12) 1.2595(2) 0.0288(10) Uani 1 1 d . . . H98 H 0.8614 0.4828 1.3038 0.035 Uiso 1 1 calc R . . C99 C 0.6435(4) 0.48529(10) 0.9886(2) 0.0201(8) Uani 1 1 d . . . C100 C 0.6998(3) 0.48558(10) 0.9274(2) 0.0211(8) Uani 1 1 d . . . C101 C 0.6489(4) 0.50190(11) 0.8599(2) 0.0245(9) Uani 1 1 d . . . H101 H 0.6894 0.5031 0.8195 0.029 Uiso 1 1 calc R . . C102 C 0.5443(4) 0.51581(11) 0.8514(2) 0.0269(9) Uani 1 1 d . . . H102 H 0.5133 0.5270 0.8059 0.032 Uiso 1 1 calc R . . C103 C 0.4810(3) 0.51386(11) 0.9096(2) 0.0225(9) Uani 1 1 d . . . C104 C 0.5315(3) 0.49875(10) 0.9795(2) 0.0206(8) Uani 1 1 d . . . C105 C 0.4652(3) 0.49558(11) 1.0362(2) 0.0235(9) Uani 1 1 d . . . H105 H 0.4973 0.4855 1.0828 0.028 Uiso 1 1 calc R . . C106 C 0.3559(4) 0.50682(12) 1.0252(3) 0.0322(11) Uani 1 1 d . . . H106 H 0.3140 0.5052 1.0648 0.039 Uiso 1 1 calc R . . C107 C 0.3043(4) 0.52086(12) 0.9552(3) 0.0305(10) Uani 1 1 d . . . H107 H 0.2269 0.5274 0.9469 0.037 Uiso 1 1 calc R . . C108 C 0.3668(4) 0.52488(12) 0.9000(3) 0.0296(10) Uani 1 1 d . . . H108 H 0.3330 0.5353 0.8541 0.036 Uiso 1 1 calc R . . C109 C 0.6424(4) 0.34770(10) 1.0320(2) 0.0215(8) Uani 1 1 d . . . C110 C 0.6066(4) 0.35003(12) 1.1013(2) 0.0299(10) Uani 1 1 d . . . H110 H 0.5748 0.3706 1.1150 0.036 Uiso 1 1 calc R . . C111 C 0.6169(4) 0.32276(12) 1.1502(3) 0.0314(10) Uani 1 1 d . . . H111 H 0.5923 0.3246 1.1970 0.038 Uiso 1 1 calc R . . C112 C 0.6633(4) 0.29276(12) 1.1301(3) 0.0322(11) Uani 1 1 d . . . H112 H 0.6702 0.2739 1.1633 0.039 Uiso 1 1 calc R . . C113 C 0.6998(4) 0.29000(12) 1.0620(3) 0.0310(10) Uani 1 1 d . . . H113 H 0.7313 0.2693 1.0486 0.037 Uiso 1 1 calc R . . C114 C 0.6903(4) 0.31752(10) 1.0133(2) 0.0242(9) Uani 1 1 d . . . H114 H 0.7167 0.3157 0.9670 0.029 Uiso 1 1 calc R . . C115 C 0.4817(4) 0.39288(11) 0.9460(2) 0.0234(9) Uani 1 1 d . . . C116 C 0.3965(4) 0.37235(12) 0.9651(2) 0.0293(10) Uani 1 1 d . . . H116 H 0.4161 0.3516 0.9906 0.035 Uiso 1 1 calc R . . C117 C 0.2839(4) 0.38181(13) 0.9475(3) 0.0328(11) Uani 1 1 d . . . H117 H 0.2270 0.3676 0.9611 0.039 Uiso 1 1 calc R . . C118 C 0.2537(4) 0.41261(13) 0.9092(3) 0.0345(11) Uani 1 1 d . . . H118 H 0.1767 0.4195 0.8979 0.041 Uiso 1 1 calc R . . C119 C 0.3373(4) 0.43249(12) 0.8884(3) 0.0373(12) Uani 1 1 d . . . H119 H 0.3175 0.4529 0.8616 0.045 Uiso 1 1 calc R . . C120 C 0.4500(4) 0.42286(12) 0.9065(3) 0.0300(10) Uani 1 1 d . . . H120 H 0.5067 0.4368 0.8918 0.036 Uiso 1 1 calc R . . C121 C 0.9560(4) 0.50136(11) 0.8506(2) 0.0258(9) Uani 1 1 d . . . C122 C 0.9552(4) 0.53615(12) 0.8459(3) 0.0343(11) Uani 1 1 d . . . H122 H 0.9464 0.5493 0.8884 0.041 Uiso 1 1 calc R . . C123 C 0.9671(5) 0.55219(13) 0.7799(3) 0.0402(12) Uani 1 1 d . . . H123 H 0.9672 0.5762 0.7775 0.048 Uiso 1 1 calc R . . C124 C 0.9788(5) 0.53354(12) 0.7180(3) 0.0400(13) Uani 1 1 d . . . H124 H 0.9817 0.5445 0.6716 0.048 Uiso 1 1 calc R . . C125 C 0.9860(6) 0.49905(14) 0.7234(3) 0.0603(19) Uani 1 1 d . . . H125 H 1.0003 0.4861 0.6818 0.072 Uiso 1 1 calc R . . C126 C 0.9726(6) 0.48279(13) 0.7891(3) 0.0508(16) Uani 1 1 d . . . H126 H 0.9748 0.4587 0.7918 0.061 Uiso 1 1 calc R . . C127 C 0.9840(3) 0.50228(11) 1.0136(2) 0.0235(9) Uani 1 1 d . . . C128 C 1.0827(4) 0.49117(12) 1.0595(2) 0.0257(9) Uani 1 1 d . . . H128 H 1.1212 0.4718 1.0455 0.031 Uiso 1 1 calc R . . C129 C 1.1256(4) 0.50824(13) 1.1260(2) 0.0317(10) Uani 1 1 d . . . H129 H 1.1931 0.5006 1.1573 0.038 Uiso 1 1 calc R . . C130 C 1.0694(4) 0.53633(13) 1.1461(3) 0.0343(11) Uani 1 1 d . . . H130 H 1.0984 0.5480 1.1914 0.041 Uiso 1 1 calc R . . C131 C 0.9699(4) 0.54786(13) 1.1001(3) 0.0338(11) Uani 1 1 d . . . H131 H 0.9317 0.5673 1.1139 0.041 Uiso 1 1 calc R . . C132 C 0.9280(4) 0.53073(12) 1.0348(3) 0.0297(10) Uani 1 1 d . . . H132 H 0.8603 0.5383 1.0038 0.036 Uiso 1 1 calc R . . C133 C 0.4303(4) 0.42723(10) 0.4412(2) 0.0213(8) Uani 1 1 d . . . C134 C 0.4624(4) 0.45364(10) 0.4917(2) 0.0218(9) Uani 1 1 d . A . C135 C 0.5587(4) 0.45009(12) 0.5490(2) 0.0283(10) Uani 1 1 d . . . H135 H 0.5791 0.4681 0.5836 0.034 Uiso 1 1 calc R A . C136 C 0.6223(4) 0.42161(12) 0.5554(2) 0.0297(10) Uani 1 1 d . A . H136 H 0.6892 0.4205 0.5925 0.036 Uiso 1 1 calc R . . C137 C 0.5908(4) 0.39334(11) 0.5077(2) 0.0270(9) Uani 1 1 d . . . C138 C 0.4934(4) 0.39600(11) 0.4503(2) 0.0223(9) Uani 1 1 d . A . C139 C 0.4626(4) 0.36710(11) 0.4048(2) 0.0245(9) Uani 1 1 d . . . H139 H 0.3975 0.3681 0.3662 0.029 Uiso 1 1 calc R A . C140 C 0.5244(4) 0.33769(12) 0.4149(3) 0.0342(11) Uani 1 1 d . A . H140 H 0.5012 0.3188 0.3834 0.041 Uiso 1 1 calc R . . C141 C 0.6219(4) 0.33513(12) 0.4714(3) 0.0337(11) Uani 1 1 d . . . H141 H 0.6649 0.3148 0.4776 0.040 Uiso 1 1 calc R A . C142 C 0.6534(4) 0.36242(12) 0.5169(3) 0.0322(11) Uani 1 1 d . A . H142 H 0.7183 0.3608 0.5554 0.039 Uiso 1 1 calc R . . C143 C 0.3340(3) 0.43108(10) 0.3779(2) 0.0201(8) Uani 1 1 d . A . C144 C 0.2245(3) 0.43599(10) 0.3897(2) 0.0207(8) Uani 1 1 d . . . C145 C 0.1328(4) 0.43930(11) 0.3275(2) 0.0252(9) Uani 1 1 d . A . H145 H 0.0583 0.4431 0.3367 0.030 Uiso 1 1 calc R . . C146 C 0.1501(4) 0.43706(11) 0.2555(2) 0.0253(9) Uani 1 1 d . . . H146 H 0.0876 0.4387 0.2151 0.030 Uiso 1 1 calc R A . C147 C 0.2622(4) 0.43226(10) 0.2402(2) 0.0222(9) Uani 1 1 d . A . C148 C 0.3537(3) 0.43015(10) 0.3014(2) 0.0194(8) Uani 1 1 d . . . C149 C 0.4654(4) 0.42811(11) 0.2841(2) 0.0249(9) Uani 1 1 d . A . H149 H 0.5288 0.4272 0.3240 0.030 Uiso 1 1 calc R . . C150 C 0.4828(4) 0.42747(11) 0.2115(2) 0.0275(10) Uani 1 1 d . . . H150 H 0.5578 0.4262 0.2017 0.033 Uiso 1 1 calc R A . C151 C 0.3916(4) 0.42875(11) 0.1518(2) 0.0260(9) Uani 1 1 d . A . H151 H 0.4044 0.4280 0.1016 0.031 Uiso 1 1 calc R . . C152 C 0.2837(4) 0.43110(10) 0.1658(2) 0.0259(9) Uani 1 1 d . . . H152 H 0.2219 0.4320 0.1248 0.031 Uiso 1 1 calc R A . C153 C 0.5389(4) 0.53924(11) 0.5386(2) 0.0225(9) Uani 1 1 d . . . C154 C 0.5415(4) 0.53825(13) 0.6162(2) 0.0335(11) Uani 1 1 d . A . H154 H 0.4844 0.5264 0.6359 0.040 Uiso 1 1 calc R . . C155 C 0.6291(4) 0.55482(13) 0.6648(3) 0.0329(11) Uani 1 1 d . . . H155 H 0.6303 0.5545 0.7173 0.039 Uiso 1 1 calc R A . C156 C 0.7130(4) 0.57142(13) 0.6370(3) 0.0320(10) Uani 1 1 d . A . H156 H 0.7719 0.5826 0.6703 0.038 Uiso 1 1 calc R . . C157 C 0.7118(4) 0.57196(15) 0.5615(3) 0.0411(13) Uani 1 1 d . . . H157 H 0.7704 0.5833 0.5425 0.049 Uiso 1 1 calc R A . C158 C 0.6251(4) 0.55591(13) 0.5122(3) 0.0361(12) Uani 1 1 d . A . H158 H 0.6252 0.5564 0.4598 0.043 Uiso 1 1 calc R . . C159 C 0.4334(3) 0.53100(11) 0.3830(2) 0.0217(8) Uani 1 1 d . . . C160 C 0.4970(4) 0.50982(11) 0.3455(2) 0.0303(10) Uani 1 1 d . A . H160 H 0.5366 0.4912 0.3712 0.036 Uiso 1 1 calc R . . C161 C 0.5030(4) 0.51569(12) 0.2703(2) 0.0339(11) Uani 1 1 d . . . H161 H 0.5452 0.5010 0.2443 0.041 Uiso 1 1 calc R A . C162 C 0.4458(4) 0.54355(12) 0.2340(2) 0.0290(10) Uani 1 1 d . A . H162 H 0.4496 0.5479 0.1829 0.035 Uiso 1 1 calc R . . C163 C 0.3843(4) 0.56468(13) 0.2712(3) 0.0335(11) Uani 1 1 d . . . H163 H 0.3466 0.5837 0.2461 0.040 Uiso 1 1 calc R A . C164 C 0.3772(4) 0.55827(12) 0.3454(2) 0.0308(10) Uani 1 1 d . A . H164 H 0.3333 0.5728 0.3707 0.037 Uiso 1 1 calc R . . C165 C -0.0215(4) 0.41526(11) 0.4597(2) 0.0255(9) Uani 1 1 d . A . C166 C -0.1088(4) 0.43818(13) 0.4590(3) 0.0405(12) Uani 1 1 d . . . H166 H -0.0960 0.4584 0.4878 0.049 Uiso 1 1 calc R A . C167 C -0.2154(5) 0.43182(15) 0.4162(4) 0.0497(14) Uani 1 1 d . A . H167 H -0.2757 0.4474 0.4169 0.060 Uiso 1 1 calc R . . C168 C -0.2331(4) 0.40282(13) 0.3729(3) 0.0377(12) Uani 1 1 d . . . H168 H -0.3052 0.3987 0.3428 0.045 Uiso 1 1 calc R A . C169 C -0.1472(4) 0.38005(12) 0.3733(2) 0.0301(10) Uani 1 1 d . A . H169 H -0.1598 0.3601 0.3437 0.036 Uiso 1 1 calc R . . C170 C -0.0422(4) 0.38602(12) 0.4168(2) 0.0297(10) Uani 1 1 d . . . H170 H 0.0167 0.3699 0.4173 0.036 Uiso 1 1 calc R A . C171 C 0.1791(11) 0.3824(2) 0.5464(7) 0.027(4) Uani 0.49(3) 1 d PG A 1 C172 C 0.1120(9) 0.3566(3) 0.5670(10) 0.045(5) Uani 0.49(3) 1 d PG A 1 H17J H 0.0331 0.3601 0.5641 0.054 Uiso 0.49(3) 1 calc PR A 1 C173 C 0.1605(12) 0.3257(3) 0.5918(9) 0.051(5) Uani 0.49(3) 1 d PG A 1 H17K H 0.1147 0.3081 0.6059 0.062 Uiso 0.49(3) 1 calc PR A 1 C174 C 0.2761(15) 0.3206(3) 0.5960(7) 0.053(5) Uani 0.49(3) 1 d PG A 1 H17L H 0.3092 0.2995 0.6129 0.064 Uiso 0.49(3) 1 calc PR A 1 C175 C 0.3431(13) 0.3464(5) 0.5753(11) 0.069(7) Uani 0.49(3) 1 d PG A 1 H17M H 0.4221 0.3429 0.5782 0.082 Uiso 0.49(3) 1 calc PR A 1 C176 C 0.2946(12) 0.3773(4) 0.5505(10) 0.060(6) Uani 0.49(3) 1 d PG A 1 H17N H 0.3405 0.3949 0.5364 0.072 Uiso 0.49(3) 1 calc PR A 1 C177 C 0.1275(4) 0.73137(16) 0.0751(3) 0.0455(14) Uani 1 1 d . . . H17A H 0.0616 0.7163 0.0647 0.068 Uiso 1 1 calc R . . H17B H 0.1943 0.7196 0.0638 0.068 Uiso 1 1 calc R . . H17C H 0.1131 0.7517 0.0438 0.068 Uiso 1 1 calc R . . C17A C 0.1614(11) 0.3836(2) 0.5486(7) 0.040(5) Uani 0.51(3) 1 d PG A 2 C17B C 0.0953(9) 0.3656(4) 0.5905(7) 0.042(4) Uani 0.51(3) 1 d PG A 2 H17O H 0.0296 0.3757 0.6035 0.051 Uiso 0.51(3) 1 calc PR A 2 C17C C 0.1252(12) 0.3327(4) 0.6135(7) 0.057(5) Uani 0.51(3) 1 d PG A 2 H17P H 0.0800 0.3203 0.6421 0.069 Uiso 0.51(3) 1 calc PR A 2 C17D C 0.2213(17) 0.3179(2) 0.5946(6) 0.050(5) Uani 0.51(3) 1 d PG A 2 H17Q H 0.2417 0.2954 0.6102 0.060 Uiso 0.51(3) 1 calc PR A 2 C17E C 0.2874(17) 0.3359(3) 0.5527(6) 0.060(5) Uani 0.51(3) 1 d PG A 2 H17R H 0.3531 0.3258 0.5397 0.072 Uiso 0.51(3) 1 calc PR A 2 C17F C 0.2575(14) 0.3688(3) 0.5297(8) 0.056(5) Uani 0.51(3) 1 d PG A 2 H17S H 0.3026 0.3812 0.5011 0.067 Uiso 0.51(3) 1 calc PR A 2 C178 C 0.0527(4) 0.75914(14) 0.1738(3) 0.0403(12) Uani 1 1 d . . . H17D H 0.0333 0.7784 0.1398 0.060 Uiso 1 1 calc R . . H17E H 0.0731 0.7674 0.2256 0.060 Uiso 1 1 calc R . . H17F H -0.0125 0.7439 0.1698 0.060 Uiso 1 1 calc R . . C179 C 0.2922(5) 0.81235(12) 0.2778(3) 0.0423(13) Uani 1 1 d . . . H17G H 0.2400 0.8167 0.3125 0.063 Uiso 1 1 calc R . . H17H H 0.2511 0.8140 0.2260 0.063 Uiso 1 1 calc R . . H17I H 0.3535 0.8291 0.2860 0.063 Uiso 1 1 calc R . . C180 C 0.4052(5) 0.77483(14) 0.3659(3) 0.0433(13) Uani 1 1 d . . . H18A H 0.4662 0.7917 0.3739 0.065 Uiso 1 1 calc R . . H18B H 0.4380 0.7520 0.3713 0.065 Uiso 1 1 calc R . . H18C H 0.3561 0.7781 0.4030 0.065 Uiso 1 1 calc R . . C181 C 0.0163(5) 0.12665(14) 0.3975(3) 0.0435(13) Uani 1 1 d . . . H18D H 0.0210 0.1316 0.4510 0.065 Uiso 1 1 calc R . . H18E H 0.0929 0.1249 0.3862 0.065 Uiso 1 1 calc R . . H18F H -0.0238 0.1052 0.3852 0.065 Uiso 1 1 calc R . . C182 C -0.1602(4) 0.15556(13) 0.3671(3) 0.0349(11) Uani 1 1 d . . . H18G H -0.1991 0.1340 0.3533 0.052 Uiso 1 1 calc R . . H18H H -0.2002 0.1738 0.3365 0.052 Uiso 1 1 calc R . . H18I H -0.1594 0.1602 0.4203 0.052 Uiso 1 1 calc R . . C183 C -0.1961(4) 0.14926(12) 0.1663(3) 0.0309(10) Uani 1 1 d . . . H18J H -0.2740 0.1548 0.1711 0.046 Uiso 1 1 calc R . . H18K H -0.1668 0.1315 0.2025 0.046 Uiso 1 1 calc R . . H18L H -0.1949 0.1412 0.1153 0.046 Uiso 1 1 calc R . . C184 C -0.1708(4) 0.20688(12) 0.1314(3) 0.0332(11) Uani 1 1 d . . . H18M H -0.1745 0.1998 0.0792 0.050 Uiso 1 1 calc R . . H18N H -0.1213 0.2267 0.1419 0.050 Uiso 1 1 calc R . . H18O H -0.2469 0.2127 0.1397 0.050 Uiso 1 1 calc R . . C185 C 1.0201(4) 0.38390(13) 1.0389(3) 0.0336(11) Uani 1 1 d . . . H18P H 1.0176 0.3661 1.0764 0.050 Uiso 1 1 calc R . . H18Q H 1.0017 0.4058 1.0593 0.050 Uiso 1 1 calc R . . H18R H 1.0962 0.3849 1.0266 0.050 Uiso 1 1 calc R . . C186 C 0.9500(4) 0.34208(12) 0.9434(3) 0.0373(12) Uani 1 1 d . . . H18S H 1.0249 0.3396 0.9297 0.056 Uiso 1 1 calc R . . H18T H 0.8913 0.3381 0.8991 0.056 Uiso 1 1 calc R . . H18U H 0.9419 0.3256 0.9826 0.056 Uiso 1 1 calc R . . C187 C 0.8952(7) 0.39255(17) 0.7605(4) 0.072(2) Uani 1 1 d . . . H8CA H 0.8613 0.3725 0.7334 0.108 Uiso 1 1 calc R . . H8CB H 0.9639 0.3859 0.7955 0.108 Uiso 1 1 calc R . . H8CC H 0.9147 0.4091 0.7246 0.108 Uiso 1 1 calc R . . C188 C 0.7081(6) 0.41799(18) 0.7559(3) 0.066(2) Uani 1 1 d . . . H8AA H 0.7224 0.4361 0.7218 0.100 Uiso 1 1 calc R . . H8AB H 0.6566 0.4263 0.7881 0.100 Uiso 1 1 calc R . . H8AC H 0.6737 0.3986 0.7266 0.100 Uiso 1 1 calc R . . C189 C 0.2867(5) 0.48016(15) 0.6994(3) 0.0498(15) Uani 1 1 d . A . H8BA H 0.3587 0.4863 0.7314 0.075 Uiso 1 1 calc R . . H8BB H 0.2922 0.4572 0.6798 0.075 Uiso 1 1 calc R . . H8BC H 0.2259 0.4810 0.7289 0.075 Uiso 1 1 calc R . . C190 C 0.2624(5) 0.53917(13) 0.6621(3) 0.0402(12) Uani 1 1 d . A . H19A H 0.2080 0.5418 0.6960 0.060 Uiso 1 1 calc R . . H19B H 0.2411 0.5541 0.6186 0.060 Uiso 1 1 calc R . . H19C H 0.3384 0.5452 0.6886 0.060 Uiso 1 1 calc R . . C191 C -0.0136(4) 0.52767(15) 0.5020(3) 0.0456(13) Uani 1 1 d . A . H19D H -0.0079 0.5522 0.5099 0.068 Uiso 1 1 calc R . . H19E H -0.0135 0.5163 0.5501 0.068 Uiso 1 1 calc R . . H19F H -0.0841 0.5224 0.4674 0.068 Uiso 1 1 calc R . . C192 C 0.0845(5) 0.5320(2) 0.3981(3) 0.076(3) Uani 1 1 d . A . H19G H 0.0118 0.5284 0.3644 0.114 Uiso 1 1 calc R . . H19H H 0.1455 0.5220 0.3758 0.114 Uiso 1 1 calc R . . H19I H 0.0979 0.5564 0.4054 0.114 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 0.0198(2) 0.01770(18) 0.01817(18) 0.00087(14) 0.00406(14) 0.00186(16) Zr2 0.01733(19) 0.01565(17) 0.01715(17) 0.00151(14) 0.00343(14) -0.00098(15) Zr3 0.0300(2) 0.01793(19) 0.01920(19) -0.00072(15) 0.00749(16) -0.00299(17) Zr4 0.0230(2) 0.0218(2) 0.01859(18) -0.00204(15) 0.00584(15) -0.00259(17) P1 0.0211(5) 0.0213(5) 0.0211(5) 0.0044(4) 0.0050(4) -0.0001(4) P2 0.0188(5) 0.0199(5) 0.0182(5) 0.0003(4) 0.0063(4) 0.0004(4) P3 0.0179(5) 0.0166(5) 0.0180(5) 0.0010(4) 0.0046(4) -0.0001(4) P4 0.0200(5) 0.0161(5) 0.0178(5) -0.0014(4) 0.0037(4) -0.0017(4) P5 0.0290(6) 0.0165(5) 0.0172(5) -0.0002(4) 0.0060(4) -0.0026(4) P6 0.0249(6) 0.0180(5) 0.0237(5) 0.0011(4) 0.0071(4) -0.0007(4) P7 0.0220(6) 0.0194(5) 0.0204(5) -0.0014(4) 0.0054(4) -0.0022(4) P8 0.0282(6) 0.0237(6) 0.0244(6) 0.0003(4) 0.0074(5) -0.0062(5) O1 0.0248(16) 0.0228(15) 0.0240(15) 0.0085(12) 0.0054(12) 0.0019(13) O2 0.0244(15) 0.0172(14) 0.0206(14) -0.0002(11) 0.0081(11) 0.0013(12) O3 0.0161(14) 0.0176(14) 0.0215(14) -0.0003(10) 0.0042(11) -0.0020(11) O4 0.0226(15) 0.0178(14) 0.0231(14) 0.0009(11) 0.0064(12) -0.0022(12) O5 0.0342(17) 0.0203(15) 0.0178(14) -0.0029(11) 0.0064(12) -0.0041(13) O6 0.0250(16) 0.0192(15) 0.0313(16) 0.0027(12) 0.0078(13) 0.0008(13) O7 0.0227(15) 0.0196(14) 0.0243(15) -0.0014(11) 0.0059(12) -0.0013(12) O8 0.0381(19) 0.0333(18) 0.0268(16) -0.0054(13) 0.0156(14) -0.0111(15) N1 0.0178(17) 0.0185(16) 0.0221(17) 0.0026(13) 0.0039(13) -0.0028(14) N2 0.0153(16) 0.0208(17) 0.0192(16) 0.0009(13) 0.0050(12) 0.0027(14) N3 0.0175(17) 0.0147(15) 0.0151(15) -0.0029(12) 0.0024(12) -0.0012(13) N4 0.0182(17) 0.0135(16) 0.0179(16) -0.0003(12) 0.0055(13) -0.0030(13) N5 0.032(2) 0.0151(16) 0.0185(16) -0.0010(13) 0.0054(14) -0.0043(15) N6 0.028(2) 0.0131(16) 0.0240(18) 0.0006(13) 0.0037(15) -0.0042(14) N7 0.0203(18) 0.0160(17) 0.0245(17) -0.0024(13) 0.0040(14) -0.0012(14) N8 0.0246(19) 0.0196(17) 0.0223(17) -0.0014(13) 0.0058(14) -0.0027(15) N9 0.0217(18) 0.034(2) 0.0223(17) 0.0030(15) 0.0038(14) 0.0030(17) N10 0.037(2) 0.0185(18) 0.0268(19) -0.0044(14) 0.0085(16) -0.0023(16) N11 0.0201(18) 0.0207(17) 0.0226(17) 0.0021(14) 0.0066(14) -0.0016(15) N12 0.0225(18) 0.0257(19) 0.0161(16) 0.0009(13) -0.0011(13) -0.0007(15) N13 0.032(2) 0.0198(18) 0.033(2) 0.0010(15) 0.0101(16) -0.0013(16) N14 0.058(3) 0.037(2) 0.027(2) -0.0042(17) 0.0136(19) -0.021(2) N15 0.044(2) 0.029(2) 0.0187(18) -0.0007(14) 0.0046(16) -0.0049(18) N16 0.028(2) 0.033(2) 0.028(2) 0.0010(16) 0.0040(16) -0.0020(17) C1 0.016(2) 0.023(2) 0.0129(17) -0.0018(14) 0.0034(14) -0.0022(16) C2 0.016(2) 0.0196(19) 0.0174(18) -0.0009(15) 0.0041(15) -0.0025(16) C3 0.024(2) 0.020(2) 0.021(2) -0.0040(15) 0.0039(16) -0.0042(17) C4 0.018(2) 0.026(2) 0.023(2) -0.0067(16) 0.0012(16) -0.0040(17) C5 0.022(2) 0.028(2) 0.0165(19) -0.0010(16) 0.0006(16) -0.0012(18) C6 0.0135(19) 0.023(2) 0.0145(17) -0.0011(15) 0.0036(14) 0.0018(16) C7 0.022(2) 0.021(2) 0.0198(19) 0.0009(15) 0.0057(16) 0.0002(17) C8 0.023(2) 0.024(2) 0.022(2) 0.0053(16) 0.0063(17) 0.0037(18) C9 0.028(2) 0.032(2) 0.020(2) 0.0044(17) -0.0004(17) 0.009(2) C10 0.026(2) 0.032(2) 0.018(2) -0.0016(17) -0.0032(17) -0.002(2) C11 0.019(2) 0.0150(18) 0.0163(18) 0.0007(14) 0.0010(15) 0.0000(16) C12 0.021(2) 0.0185(19) 0.0121(17) 0.0020(14) 0.0035(15) -0.0023(16) C13 0.013(2) 0.040(3) 0.027(2) -0.0071(19) 0.0009(17) -0.0020(19) C14 0.022(2) 0.038(3) 0.026(2) -0.0124(19) -0.0007(18) -0.007(2) C15 0.024(2) 0.024(2) 0.020(2) -0.0036(16) 0.0025(16) -0.0015(18) C16 0.018(2) 0.021(2) 0.0157(18) 0.0009(14) 0.0040(15) 0.0035(16) C17 0.020(2) 0.0156(18) 0.0209(19) 0.0006(15) 0.0051(16) 0.0021(16) C18 0.020(2) 0.025(2) 0.023(2) 0.0015(16) 0.0074(16) 0.0032(17) C19 0.040(3) 0.019(2) 0.023(2) -0.0024(16) 0.0112(19) -0.0001(19) C20 0.034(3) 0.027(2) 0.020(2) -0.0053(16) 0.0037(18) -0.003(2) C21 0.018(2) 0.027(2) 0.024(2) 0.0076(17) 0.0041(16) 0.0011(17) C22 0.027(2) 0.041(3) 0.026(2) 0.005(2) 0.0053(18) -0.006(2) C23 0.029(3) 0.060(3) 0.029(2) 0.007(2) 0.0128(19) -0.010(3) C24 0.031(3) 0.052(3) 0.023(2) 0.001(2) 0.0067(19) 0.009(2) C25 0.040(3) 0.033(3) 0.024(2) -0.0024(19) 0.0033(19) 0.006(2) C26 0.029(2) 0.029(2) 0.021(2) 0.0040(17) 0.0035(17) 0.0015(19) C27 0.034(3) 0.026(2) 0.023(2) 0.0069(17) 0.0033(18) -0.002(2) C28 0.045(3) 0.026(2) 0.029(2) 0.0037(18) 0.006(2) -0.003(2) C29 0.077(4) 0.029(3) 0.034(3) 0.006(2) -0.001(3) -0.016(3) C30 0.062(4) 0.045(3) 0.043(3) 0.007(3) -0.011(3) -0.031(3) C31 0.032(3) 0.049(4) 0.056(3) 0.016(3) -0.001(2) -0.017(3) C32 0.028(3) 0.035(3) 0.042(3) 0.006(2) 0.004(2) -0.012(2) C33 0.022(2) 0.024(2) 0.0184(19) 0.0020(15) 0.0088(16) 0.0033(17) C34 0.025(2) 0.027(2) 0.021(2) 0.0007(16) 0.0065(16) -0.0013(18) C35 0.021(2) 0.032(2) 0.023(2) 0.0020(17) 0.0027(17) -0.0016(19) C36 0.022(2) 0.031(2) 0.027(2) 0.0022(18) 0.0073(18) -0.0056(19) C37 0.029(2) 0.021(2) 0.021(2) 0.0002(16) 0.0092(17) -0.0022(18) C38 0.022(2) 0.021(2) 0.025(2) -0.0005(16) 0.0087(17) 0.0047(17) C39 0.024(2) 0.022(2) 0.0174(18) 0.0027(15) 0.0066(16) 0.0065(17) C40 0.032(2) 0.027(2) 0.023(2) 0.0016(17) 0.0088(18) 0.0032(19) C41 0.049(3) 0.028(2) 0.023(2) 0.0038(18) 0.014(2) 0.007(2) C42 0.050(3) 0.031(2) 0.017(2) -0.0027(17) 0.002(2) 0.007(2) C43 0.035(3) 0.043(3) 0.022(2) -0.0009(19) 0.0013(19) 0.003(2) C44 0.025(2) 0.036(3) 0.023(2) 0.0034(18) 0.0055(17) 0.004(2) C45 0.021(2) 0.0136(17) 0.0137(17) 0.0007(14) 0.0014(14) -0.0016(16) C46 0.019(2) 0.019(2) 0.0174(18) -0.0022(14) 0.0055(15) -0.0031(16) C47 0.027(2) 0.030(2) 0.0154(19) 0.0047(16) 0.0098(16) 0.0009(18) C48 0.024(2) 0.032(2) 0.022(2) 0.0047(17) 0.0030(17) 0.0001(19) C49 0.021(2) 0.024(2) 0.021(2) 0.0030(16) 0.0012(16) 0.0004(17) C50 0.0178(19) 0.0175(18) 0.0219(19) -0.0032(15) 0.0041(15) -0.0008(16) C51 0.022(2) 0.025(2) 0.023(2) 0.0025(16) 0.0061(16) 0.0012(17) C52 0.021(2) 0.037(3) 0.029(2) 0.0058(19) 0.0099(17) 0.000(2) C53 0.016(2) 0.039(3) 0.030(2) 0.000(2) 0.0003(17) -0.004(2) C54 0.021(2) 0.036(3) 0.024(2) 0.0013(18) 0.0012(17) -0.0034(19) C55 0.0182(19) 0.0162(18) 0.0144(17) 0.0020(14) 0.0048(14) -0.0031(15) C56 0.0145(19) 0.0176(18) 0.0190(19) 0.0003(14) 0.0065(15) 0.0011(15) C57 0.022(2) 0.020(2) 0.0179(18) -0.0037(15) 0.0024(15) -0.0049(17) C58 0.031(2) 0.021(2) 0.019(2) 0.0038(16) 0.0017(17) 0.0011(18) C59 0.027(2) 0.0171(19) 0.0169(18) 0.0023(15) 0.0055(16) -0.0009(17) C60 0.020(2) 0.0157(18) 0.0190(19) -0.0005(14) 0.0070(16) -0.0030(16) C61 0.020(2) 0.0156(19) 0.025(2) -0.0009(15) 0.0064(16) -0.0048(16) C62 0.035(3) 0.019(2) 0.025(2) -0.0054(16) 0.0128(19) -0.0078(18) C63 0.035(3) 0.020(2) 0.029(2) 0.0029(17) 0.0104(19) -0.0072(19) C64 0.033(2) 0.022(2) 0.020(2) 0.0065(16) 0.0011(17) 0.0003(19) C65 0.017(2) 0.024(2) 0.0195(19) 0.0012(15) 0.0042(15) -0.0021(16) C66 0.029(2) 0.024(2) 0.023(2) -0.0007(16) 0.0072(18) -0.0007(18) C67 0.028(2) 0.028(2) 0.031(2) -0.0070(18) 0.0129(19) 0.0012(19) C68 0.027(2) 0.040(3) 0.021(2) 0.0015(18) 0.0107(17) -0.004(2) C69 0.031(2) 0.027(2) 0.029(2) 0.0050(17) 0.0118(19) -0.0022(19) C70 0.025(2) 0.020(2) 0.028(2) 0.0028(16) 0.0060(17) 0.0000(17) C71 0.022(2) 0.0171(19) 0.022(2) -0.0019(15) 0.0093(16) 0.0004(16) C72 0.032(3) 0.024(2) 0.028(2) 0.0031(18) 0.0033(19) 0.0009(19) C73 0.057(3) 0.027(2) 0.022(2) 0.0070(18) 0.000(2) -0.004(2) C74 0.054(3) 0.018(2) 0.032(2) 0.0026(18) 0.014(2) -0.009(2) C75 0.031(3) 0.022(2) 0.037(3) -0.0061(18) 0.014(2) -0.0069(19) C76 0.025(2) 0.025(2) 0.0188(19) -0.0023(16) 0.0049(16) -0.0007(18) C77 0.020(2) 0.0152(18) 0.0188(19) 0.0003(14) 0.0038(15) -0.0023(16) C78 0.025(2) 0.023(2) 0.024(2) 0.0004(16) 0.0035(17) 0.0004(18) C79 0.025(2) 0.031(2) 0.029(2) 0.0027(18) -0.0044(18) -0.002(2) C80 0.018(2) 0.035(3) 0.037(3) 0.011(2) 0.0056(19) 0.0007(19) C81 0.033(3) 0.035(3) 0.030(2) 0.002(2) 0.012(2) 0.013(2) C82 0.028(2) 0.027(2) 0.024(2) -0.0037(17) 0.0046(18) 0.0043(19) C83 0.024(2) 0.020(2) 0.022(2) -0.0035(15) 0.0057(16) 0.0060(17) C84 0.028(3) 0.048(3) 0.033(3) -0.010(2) 0.005(2) -0.007(2) C85 0.025(3) 0.095(5) 0.040(3) -0.025(3) 0.002(2) -0.013(3) C86 0.033(3) 0.101(5) 0.025(3) -0.017(3) 0.002(2) 0.013(3) C87 0.046(3) 0.050(3) 0.020(2) 0.002(2) 0.009(2) 0.021(3) C88 0.035(3) 0.027(2) 0.024(2) -0.0037(17) 0.0105(19) -0.001(2) C89 0.025(2) 0.0135(19) 0.0192(19) -0.0015(14) 0.0019(16) -0.0044(16) C90 0.022(2) 0.0135(18) 0.0216(19) -0.0002(15) 0.0043(16) 0.0002(16) C91 0.034(2) 0.022(2) 0.0165(19) 0.0028(15) 0.0071(17) 0.0042(18) C92 0.025(2) 0.027(2) 0.020(2) 0.0029(16) -0.0003(16) 0.0037(18) C93 0.020(2) 0.027(2) 0.021(2) -0.0026(16) 0.0026(16) -0.0013(18) C94 0.022(2) 0.023(2) 0.0197(19) 0.0004(16) 0.0032(16) -0.0019(18) C95 0.026(2) 0.021(2) 0.024(2) -0.0002(16) 0.0049(17) 0.0010(18) C96 0.028(2) 0.019(2) 0.028(2) -0.0034(17) 0.0039(18) -0.0005(18) C97 0.034(3) 0.030(2) 0.023(2) -0.0092(18) -0.0031(18) 0.004(2) C98 0.027(2) 0.036(2) 0.021(2) -0.0040(18) -0.0020(17) 0.008(2) C99 0.025(2) 0.016(2) 0.0181(19) 0.0003(15) 0.0013(16) -0.0068(16) C100 0.023(2) 0.017(2) 0.022(2) 0.0026(15) 0.0015(16) -0.0055(17) C101 0.027(2) 0.025(2) 0.022(2) 0.0013(16) 0.0066(17) -0.0048(18) C102 0.028(2) 0.023(2) 0.027(2) 0.0041(17) -0.0016(18) -0.0038(19) C103 0.022(2) 0.022(2) 0.021(2) 0.0001(16) -0.0036(16) -0.0003(17) C104 0.023(2) 0.019(2) 0.0182(19) -0.0013(15) -0.0007(15) -0.0047(17) C105 0.018(2) 0.027(2) 0.025(2) -0.0003(17) 0.0038(16) -0.0022(18) C106 0.032(3) 0.030(3) 0.035(3) -0.003(2) 0.007(2) -0.004(2) C107 0.018(2) 0.031(2) 0.041(3) -0.009(2) 0.0021(19) 0.0007(19) C108 0.026(2) 0.030(2) 0.029(2) -0.0001(18) -0.0030(18) 0.000(2) C109 0.026(2) 0.0163(19) 0.023(2) 0.0028(15) 0.0054(16) -0.0025(17) C110 0.036(3) 0.028(2) 0.028(2) 0.0055(18) 0.012(2) 0.002(2) C111 0.038(3) 0.033(3) 0.026(2) 0.0115(19) 0.012(2) 0.002(2) C112 0.031(3) 0.028(2) 0.034(3) 0.0140(19) -0.001(2) 0.000(2) C113 0.035(3) 0.024(2) 0.033(2) 0.0038(18) 0.002(2) -0.001(2) C114 0.029(2) 0.020(2) 0.023(2) -0.0019(16) 0.0055(17) -0.0049(18) C115 0.027(2) 0.025(2) 0.0178(19) -0.0006(16) 0.0032(16) 0.0007(18) C116 0.036(3) 0.027(2) 0.027(2) 0.0046(17) 0.0110(19) 0.001(2) C117 0.026(3) 0.039(3) 0.035(3) 0.005(2) 0.010(2) 0.005(2) C118 0.034(3) 0.032(3) 0.036(3) -0.003(2) 0.002(2) 0.004(2) C119 0.041(3) 0.024(2) 0.042(3) 0.002(2) -0.006(2) 0.000(2) C120 0.026(2) 0.026(2) 0.036(2) 0.0029(19) 0.0001(19) -0.0075(19) C121 0.025(2) 0.026(2) 0.028(2) -0.0010(17) 0.0092(18) -0.0041(18) C122 0.053(3) 0.023(2) 0.028(2) 0.0022(18) 0.014(2) 0.004(2) C123 0.060(4) 0.029(3) 0.034(3) 0.008(2) 0.014(2) 0.003(2) C124 0.067(4) 0.029(3) 0.029(2) 0.0085(19) 0.022(2) -0.002(2) C125 0.122(6) 0.032(3) 0.036(3) -0.005(2) 0.041(3) -0.011(3) C126 0.096(5) 0.022(3) 0.044(3) -0.001(2) 0.037(3) -0.004(3) C127 0.017(2) 0.021(2) 0.032(2) 0.0011(17) 0.0034(17) -0.0022(17) C128 0.025(2) 0.026(2) 0.027(2) 0.0017(18) 0.0079(17) 0.0028(19) C129 0.028(3) 0.040(3) 0.027(2) 0.0003(19) 0.0016(18) 0.004(2) C130 0.032(3) 0.044(3) 0.026(2) -0.005(2) 0.0047(19) -0.003(2) C131 0.027(2) 0.039(3) 0.036(3) -0.011(2) 0.004(2) 0.007(2) C132 0.024(2) 0.035(3) 0.029(2) -0.0054(19) 0.0005(18) 0.006(2) C133 0.022(2) 0.020(2) 0.020(2) -0.0029(15) -0.0001(16) -0.0009(17) C134 0.024(2) 0.020(2) 0.021(2) -0.0009(15) 0.0036(17) 0.0042(17) C135 0.031(3) 0.028(2) 0.022(2) -0.0064(17) -0.0045(18) -0.004(2) C136 0.031(3) 0.029(2) 0.025(2) 0.0002(17) -0.0084(18) 0.004(2) C137 0.029(2) 0.024(2) 0.024(2) 0.0010(17) -0.0030(18) 0.0047(19) C138 0.022(2) 0.025(2) 0.0184(19) 0.0017(16) 0.0014(16) 0.0022(18) C139 0.021(2) 0.024(2) 0.025(2) -0.0026(17) -0.0030(17) -0.0012(18) C140 0.039(3) 0.021(2) 0.038(3) -0.0028(19) -0.005(2) 0.008(2) C141 0.035(3) 0.023(2) 0.040(3) 0.0028(19) 0.000(2) 0.008(2) C142 0.035(3) 0.029(2) 0.028(2) 0.0043(18) -0.0062(19) 0.011(2) C143 0.022(2) 0.0173(19) 0.0207(19) 0.0015(15) 0.0020(16) 0.0018(16) C144 0.021(2) 0.020(2) 0.0204(19) 0.0014(15) 0.0031(16) -0.0047(17) C145 0.025(2) 0.022(2) 0.028(2) 0.0032(17) 0.0025(18) -0.0004(18) C146 0.030(2) 0.022(2) 0.021(2) 0.0041(16) -0.0037(17) 0.0010(18) C147 0.029(2) 0.0172(19) 0.0192(19) 0.0012(15) 0.0004(16) -0.0044(17) C148 0.021(2) 0.0143(18) 0.022(2) 0.0008(14) 0.0029(16) -0.0006(16) C149 0.026(2) 0.025(2) 0.023(2) -0.0025(17) 0.0046(17) 0.0041(18) C150 0.038(3) 0.021(2) 0.026(2) 0.0005(16) 0.0115(19) -0.0031(19) C151 0.035(3) 0.022(2) 0.023(2) 0.0005(16) 0.0092(18) 0.0001(19) C152 0.037(3) 0.019(2) 0.020(2) 0.0039(16) 0.0002(18) 0.0018(19) C153 0.025(2) 0.020(2) 0.023(2) -0.0032(16) 0.0060(17) -0.0028(17) C154 0.031(3) 0.046(3) 0.026(2) -0.004(2) 0.0100(19) -0.014(2) C155 0.036(3) 0.041(3) 0.021(2) -0.0051(19) 0.0023(19) 0.000(2) C156 0.020(2) 0.037(3) 0.034(3) -0.002(2) -0.0047(19) -0.006(2) C157 0.027(3) 0.062(4) 0.033(3) -0.001(2) 0.002(2) -0.024(3) C158 0.032(3) 0.048(3) 0.027(2) 0.002(2) 0.0013(19) -0.018(2) C159 0.021(2) 0.023(2) 0.020(2) -0.0005(16) 0.0021(16) -0.0043(17) C160 0.042(3) 0.025(2) 0.027(2) 0.0004(18) 0.013(2) 0.000(2) C161 0.051(3) 0.028(2) 0.027(2) -0.0014(18) 0.020(2) -0.002(2) C162 0.035(3) 0.033(2) 0.019(2) -0.0016(17) 0.0042(18) -0.009(2) C163 0.037(3) 0.034(3) 0.029(2) 0.0094(19) 0.004(2) 0.004(2) C164 0.032(3) 0.032(2) 0.028(2) -0.0014(18) 0.0058(19) 0.010(2) C165 0.026(2) 0.024(2) 0.029(2) 0.0009(17) 0.0138(18) -0.0018(18) C166 0.042(3) 0.029(3) 0.053(3) -0.009(2) 0.018(3) -0.001(2) C167 0.040(3) 0.037(3) 0.075(4) -0.002(3) 0.018(3) 0.010(3) C168 0.024(2) 0.040(3) 0.049(3) 0.007(2) 0.004(2) 0.001(2) C169 0.028(2) 0.031(2) 0.030(2) 0.0018(19) 0.0008(19) -0.001(2) C170 0.032(3) 0.028(2) 0.028(2) 0.0030(18) 0.0057(19) 0.009(2) C171 0.035(8) 0.025(9) 0.015(7) 0.015(6) -0.007(5) -0.004(6) C172 0.032(7) 0.036(8) 0.059(11) 0.008(7) -0.014(7) -0.015(6) C173 0.019(8) 0.044(9) 0.085(13) 0.035(8) -0.007(8) 0.000(6) C174 0.039(11) 0.046(9) 0.067(9) 0.030(7) -0.010(8) -0.006(7) C175 0.036(9) 0.106(15) 0.067(11) 0.053(11) 0.018(8) 0.044(10) C176 0.059(11) 0.041(9) 0.082(12) 0.050(9) 0.017(9) 0.015(8) C177 0.035(3) 0.072(4) 0.027(2) -0.001(2) -0.003(2) -0.010(3) C17A 0.033(8) 0.041(11) 0.048(11) -0.011(8) 0.016(7) -0.008(7) C17B 0.050(8) 0.044(8) 0.027(7) 0.011(6) -0.010(5) -0.025(6) C17C 0.064(10) 0.044(8) 0.051(9) 0.024(7) -0.027(8) -0.036(8) C17D 0.041(12) 0.022(6) 0.075(9) 0.013(6) -0.025(9) -0.012(7) C17E 0.041(10) 0.057(9) 0.078(10) 0.025(8) -0.002(8) 0.023(7) C17F 0.033(9) 0.056(9) 0.087(12) 0.039(8) 0.034(8) 0.015(7) C178 0.029(3) 0.040(3) 0.053(3) 0.014(2) 0.010(2) 0.011(2) C179 0.054(3) 0.022(2) 0.053(3) -0.001(2) 0.018(3) 0.007(2) C180 0.052(3) 0.044(3) 0.030(3) -0.007(2) 0.000(2) -0.007(3) C181 0.052(3) 0.045(3) 0.035(3) 0.017(2) 0.010(2) 0.015(3) C182 0.030(3) 0.040(3) 0.036(3) 0.007(2) 0.012(2) -0.008(2) C183 0.025(2) 0.033(3) 0.032(2) 0.0017(19) -0.0020(19) -0.008(2) C184 0.038(3) 0.032(3) 0.026(2) 0.0107(19) -0.002(2) -0.003(2) C185 0.036(3) 0.037(3) 0.030(2) 0.006(2) 0.011(2) 0.010(2) C186 0.037(3) 0.022(2) 0.055(3) -0.004(2) 0.014(2) 0.001(2) C187 0.121(6) 0.052(4) 0.059(4) -0.025(3) 0.058(4) -0.040(4) C188 0.095(5) 0.073(5) 0.023(3) 0.015(3) -0.011(3) -0.023(4) C189 0.069(4) 0.048(3) 0.027(3) 0.004(2) -0.005(3) -0.011(3) C190 0.050(3) 0.040(3) 0.033(3) -0.016(2) 0.014(2) -0.005(3) C191 0.032(3) 0.044(3) 0.061(4) -0.008(3) 0.007(2) 0.008(2) C192 0.035(3) 0.137(7) 0.048(4) 0.048(4) -0.014(3) -0.021(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 N10 2.037(4) . ? Zr1 N9 2.054(3) . ? Zr1 O1 2.254(3) . ? Zr1 N1 2.263(3) . ? Zr1 N2 2.281(3) . ? Zr1 O2 2.283(3) . ? Zr1 P1 2.9181(11) . ? Zr1 P2 2.9327(11) . ? Zr2 N11 2.037(3) . ? Zr2 N12 2.042(3) . ? Zr2 N4 2.230(3) . ? Zr2 O3 2.232(3) . ? Zr2 N3 2.288(3) . ? Zr2 O4 2.325(3) . ? Zr2 P4 2.9126(11) . ? Zr2 P3 2.9129(11) . ? Zr3 N13 2.033(4) . ? Zr3 N14 2.044(4) . ? Zr3 N5 2.246(3) . ? Zr3 N6 2.271(3) . ? Zr3 O5 2.276(3) . ? Zr3 O6 2.283(3) . ? Zr3 P5 2.9138(12) . ? Zr3 P6 2.9205(12) . ? Zr4 N16 2.045(4) . ? Zr4 N15 2.056(4) . ? Zr4 O7 2.253(3) . ? Zr4 N8 2.260(3) . ? Zr4 N7 2.267(3) . ? Zr4 O8 2.279(3) . ? Zr4 P7 2.9149(11) . ? Zr4 P8 2.9162(12) . ? P1 O1 1.521(3) . ? P1 N1 1.599(3) . ? P1 C27 1.795(5) . ? P1 C21 1.806(4) . ? P2 O2 1.519(3) . ? P2 N2 1.600(3) . ? P2 C39 1.791(4) . ? P2 C33 1.798(4) . ? P3 O3 1.536(3) . ? P3 N3 1.598(3) . ? P3 C71 1.786(4) . ? P3 C65 1.804(4) . ? P4 O4 1.525(3) . ? P4 N4 1.599(3) . ? P4 C83 1.800(4) . ? P4 C77 1.800(4) . ? P5 O5 1.525(3) . ? P5 N5 1.594(3) . ? P5 C109 1.794(4) . ? P5 C115 1.795(4) . ? P6 O6 1.520(3) . ? P6 N6 1.588(4) . ? P6 C127 1.796(4) . ? P6 C121 1.803(4) . ? P7 O7 1.515(3) . ? P7 N7 1.602(3) . ? P7 C153 1.791(4) . ? P7 C159 1.799(4) . ? P8 O8 1.520(3) . ? P8 N8 1.608(3) . ? P8 C17A 1.766(9) . ? P8 C165 1.799(5) . ? P8 C171 1.855(8) . ? N1 C2 1.404(5) . ? N2 C12 1.408(5) . ? N3 C46 1.409(5) . ? N4 C56 1.420(5) . ? N5 C90 1.407(5) . ? N6 C100 1.417(5) . ? N7 C134 1.421(5) . ? N8 C144 1.409(5) . ? N9 C178 1.444(6) . ? N9 C177 1.452(6) . ? N10 C179 1.443(6) . ? N10 C180 1.452(6) . ? N11 C181 1.436(6) . ? N11 C182 1.461(5) . ? N12 C184 1.453(5) . ? N12 C183 1.453(5) . ? N13 C185 1.454(6) . ? N13 C186 1.460(6) . ? N14 C188 1.454(8) . ? N14 C187 1.460(7) . ? N15 C190 1.460(6) . ? N15 C189 1.462(6) . ? N16 C191 1.447(6) . ? N16 C192 1.459(6) . ? C1 C2 1.394(5) . ? C1 C6 1.435(5) . ? C1 C11 1.497(5) . ? C2 C3 1.412(5) . ? C3 C4 1.371(6) . ? C3 H3 0.9500 . ? C4 C5 1.409(6) . ? C4 H4 0.9500 . ? C5 C10 1.406(6) . ? C5 C6 1.427(5) . ? C6 C7 1.426(5) . ? C7 C8 1.375(6) . ? C7 H7 0.9500 . ? C8 C9 1.408(6) . ? C8 H8 0.9500 . ? C9 C10 1.380(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.391(5) . ? C11 C16 1.425(5) . ? C12 C13 1.425(5) . ? C13 C14 1.364(6) . ? C13 H13 0.9500 . ? C14 C15 1.416(6) . ? C14 H14 0.9500 . ? C15 C20 1.411(6) . ? C15 C16 1.426(6) . ? C16 C17 1.414(5) . ? C17 C18 1.369(5) . ? C17 H17 0.9500 . ? C18 C19 1.426(6) . ? C18 H18 0.9500 . ? C19 C20 1.362(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.377(6) . ? C21 C22 1.394(6) . ? C22 C23 1.401(7) . ? C22 H22 0.9500 . ? C23 C24 1.383(7) . ? C23 H23 0.9500 . ? C24 C25 1.378(7) . ? C24 H24 0.9500 . ? C25 C26 1.401(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.388(6) . ? C27 C32 1.391(7) . ? C28 C29 1.386(7) . ? C28 H28 0.9500 . ? C29 C30 1.400(9) . ? C29 H29 0.9500 . ? C30 C31 1.358(9) . ? C30 H30 0.9500 . ? C31 C32 1.402(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.395(6) . ? C33 C34 1.402(6) . ? C34 C35 1.402(6) . ? C34 H34 0.9500 . ? C35 C36 1.390(6) . ? C35 H35 0.9500 . ? C36 C37 1.379(6) . ? C36 H36 0.9500 . ? C37 C38 1.380(6) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.398(6) . ? C39 C40 1.401(6) . ? C40 C41 1.407(6) . ? C40 H40 0.9500 . ? C41 C42 1.371(7) . ? C41 H41 0.9500 . ? C42 C43 1.386(7) . ? C42 H42 0.9500 . ? C43 C44 1.379(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.409(5) . ? C45 C50 1.426(5) . ? C45 C55 1.503(5) . ? C46 C47 1.411(5) . ? C47 C48 1.359(6) . ? C47 H47 0.9500 . ? C48 C49 1.418(6) . ? C48 H48 0.9500 . ? C49 C50 1.420(5) . ? C49 C54 1.433(6) . ? C50 C51 1.430(5) . ? C51 C52 1.370(6) . ? C51 H51 0.9500 . ? C52 C53 1.404(6) . ? C52 H52 0.9500 . ? C53 C54 1.362(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.384(5) . ? C55 C60 1.425(5) . ? C56 C57 1.416(5) . ? C57 C58 1.357(6) . ? C57 H57 0.9500 . ? C58 C59 1.413(6) . ? C58 H58 0.9500 . ? C59 C60 1.421(5) . ? C59 C64 1.425(5) . ? C60 C61 1.431(5) . ? C61 C62 1.364(5) . ? C61 H61 0.9500 . ? C62 C63 1.401(6) . ? C62 H62 0.9500 . ? C63 C64 1.358(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.391(6) . ? C65 C70 1.401(5) . ? C66 C67 1.388(6) . ? C66 H66 0.9500 . ? C67 C68 1.377(6) . ? C67 H67 0.9500 . ? C68 C69 1.383(6) . ? C68 H68 0.9500 . ? C69 C70 1.387(6) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.385(6) . ? C71 C76 1.404(6) . ? C72 C73 1.379(6) . ? C72 H72 0.9500 . ? C73 C74 1.395(7) . ? C73 H73 0.9500 . ? C74 C75 1.366(7) . ? C74 H74 0.9500 . ? C75 C76 1.375(6) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C82 1.390(5) . ? C77 C78 1.401(5) . ? C78 C79 1.369(6) . ? C78 H78 0.9500 . ? C79 C80 1.391(6) . ? C79 H79 0.9500 . ? C80 C81 1.388(7) . ? C80 H80 0.9500 . ? C81 C82 1.380(6) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.379(6) . ? C83 C88 1.397(6) . ? C84 C85 1.393(7) . ? C84 H84 0.9500 . ? C85 C86 1.355(8) . ? C85 H85 0.9500 . ? C86 C87 1.388(8) . ? C86 H86 0.9500 . ? C87 C88 1.379(6) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.392(5) . ? C89 C94 1.436(5) . ? C89 C99 1.503(5) . ? C90 C91 1.423(5) . ? C91 C92 1.360(6) . ? C91 H91 0.9500 . ? C92 C93 1.415(6) . ? C92 H92 0.9500 . ? C93 C98 1.420(6) . ? C93 C94 1.424(6) . ? C94 C95 1.411(6) . ? C95 C96 1.365(6) . ? C95 H95 0.9500 . ? C96 C97 1.396(6) . ? C96 H96 0.9500 . ? C97 C98 1.356(6) . ? C97 H97 0.9500 . ? C98 H98 0.9500 . ? C99 C100 1.399(5) . ? C99 C104 1.427(6) . ? C100 C101 1.418(6) . ? C101 C102 1.353(6) . ? C101 H101 0.9500 . ? C102 C103 1.408(6) . ? C102 H102 0.9500 . ? C103 C108 1.419(6) . ? C103 C104 1.430(5) . ? C104 C105 1.415(5) . ? C105 C106 1.365(6) . ? C105 H105 0.9500 . ? C106 C107 1.419(7) . ? C106 H106 0.9500 . ? C107 C108 1.364(6) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C114 1.391(6) . ? C109 C110 1.402(6) . ? C110 C111 1.384(6) . ? C110 H110 0.9500 . ? C111 C112 1.384(7) . ? C111 H111 0.9500 . ? C112 C113 1.386(6) . ? C112 H112 0.9500 . ? C113 C114 1.391(6) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C115 C116 1.396(6) . ? C115 C120 1.399(6) . ? C116 C117 1.382(6) . ? C116 H116 0.9500 . ? C117 C118 1.414(7) . ? C117 H117 0.9500 . ? C118 C119 1.378(7) . ? C118 H118 0.9500 . ? C119 C120 1.387(7) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C122 1.375(6) . ? C121 C126 1.377(6) . ? C122 C123 1.383(6) . ? C122 H122 0.9500 . ? C123 C124 1.370(7) . ? C123 H123 0.9500 . ? C124 C125 1.366(7) . ? C124 H124 0.9500 . ? C125 C126 1.388(7) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 C128 1.390(6) . ? C127 C132 1.397(6) . ? C128 C129 1.395(6) . ? C128 H128 0.9500 . ? C129 C130 1.380(7) . ? C129 H129 0.9500 . ? C130 C131 1.403(7) . ? C130 H130 0.9500 . ? C131 C132 1.375(6) . ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? C133 C134 1.394(5) . ? C133 C138 1.440(6) . ? C133 C143 1.481(5) . ? C134 C135 1.413(6) . ? C135 C136 1.352(6) . ? C135 H135 0.9500 . ? C136 C137 1.420(6) . ? C136 H136 0.9500 . ? C137 C138 1.421(6) . ? C137 C142 1.427(6) . ? C138 C139 1.417(6) . ? C139 C140 1.371(6) . ? C139 H139 0.9500 . ? C140 C141 1.412(6) . ? C140 H140 0.9500 . ? C141 C142 1.367(6) . ? C141 H141 0.9500 . ? C142 H142 0.9500 . ? C143 C144 1.384(6) . ? C143 C148 1.447(5) . ? C144 C145 1.432(6) . ? C145 C146 1.360(6) . ? C145 H145 0.9500 . ? C146 C147 1.435(6) . ? C146 H146 0.9500 . ? C147 C148 1.415(5) . ? C147 C152 1.419(6) . ? C148 C149 1.434(6) . ? C149 C150 1.369(6) . ? C149 H149 0.9500 . ? C150 C151 1.394(6) . ? C150 H150 0.9500 . ? C151 C152 1.367(6) . ? C151 H151 0.9500 . ? C152 H152 0.9500 . ? C153 C158 1.382(6) . ? C153 C154 1.401(6) . ? C154 C155 1.404(6) . ? C154 H154 0.9500 . ? C155 C156 1.370(7) . ? C155 H155 0.9500 . ? C156 C157 1.364(6) . ? C156 H156 0.9500 . ? C157 C158 1.395(6) . ? C157 H157 0.9500 . ? C158 H158 0.9500 . ? C159 C164 1.382(6) . ? C159 C160 1.389(6) . ? C160 C161 1.396(6) . ? C160 H160 0.9500 . ? C161 C162 1.396(7) . ? C161 H161 0.9500 . ? C162 C163 1.369(6) . ? C162 H162 0.9500 . ? C163 C164 1.385(6) . ? C163 H163 0.9500 . ? C164 H164 0.9500 . ? C165 C166 1.382(6) . ? C165 C170 1.389(6) . ? C166 C167 1.394(8) . ? C166 H166 0.9500 . ? C167 C168 1.382(8) . ? C167 H167 0.9500 . ? C168 C169 1.367(6) . ? C168 H168 0.9500 . ? C169 C170 1.380(6) . ? C169 H169 0.9500 . ? C170 H170 0.9500 . ? C171 C172 1.3900 . ? C171 C176 1.3900 . ? C172 C173 1.3900 . ? C172 H17J 0.9500 . ? C173 C174 1.3900 . ? C173 H17K 0.9500 . ? C174 C175 1.3900 . ? C174 H17L 0.9500 . ? C175 C176 1.3900 . ? C175 H17M 0.9500 . ? C176 H17N 0.9500 . ? C177 H17A 0.9800 . ? C177 H17B 0.9800 . ? C177 H17C 0.9800 . ? C17A C17B 1.3900 . ? C17A C17F 1.3900 . ? C17B C17C 1.3900 . ? C17B H17O 0.9500 . ? C17C C17D 1.3900 . ? C17C H17P 0.9500 . ? C17D C17E 1.3900 . ? C17D H17Q 0.9500 . ? C17E C17F 1.3900 . ? C17E H17R 0.9500 . ? C17F H17S 0.9500 . ? C178 H17D 0.9800 . ? C178 H17E 0.9800 . ? C178 H17F 0.9800 . ? C179 H17G 0.9800 . ? C179 H17H 0.9800 . ? C179 H17I 0.9800 . ? C180 H18A 0.9800 . ? C180 H18B 0.9800 . ? C180 H18C 0.9800 . ? C181 H18D 0.9800 . ? C181 H18E 0.9800 . ? C181 H18F 0.9800 . ? C182 H18G 0.9800 . ? C182 H18H 0.9800 . ? C182 H18I 0.9800 . ? C183 H18J 0.9800 . ? C183 H18K 0.9800 . ? C183 H18L 0.9800 . ? C184 H18M 0.9800 . ? C184 H18N 0.9800 . ? C184 H18O 0.9800 . ? C185 H18P 0.9800 . ? C185 H18Q 0.9800 . ? C185 H18R 0.9800 . ? C186 H18S 0.9800 . ? C186 H18T 0.9800 . ? C186 H18U 0.9800 . ? C187 H8CA 0.9800 . ? C187 H8CB 0.9800 . ? C187 H8CC 0.9800 . ? C188 H8AA 0.9800 . ? C188 H8AB 0.9800 . ? C188 H8AC 0.9800 . ? C189 H8BA 0.9800 . ? C189 H8BB 0.9800 . ? C189 H8BC 0.9800 . ? C190 H19A 0.9800 . ? C190 H19B 0.9800 . ? C190 H19C 0.9800 . ? C191 H19D 0.9800 . ? C191 H19E 0.9800 . ? C191 H19F 0.9800 . ? C192 H19G 0.9800 . ? C192 H19H 0.9800 . ? C192 H19I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Zr1 N9 112.80(16) . . ? N10 Zr1 O1 93.29(13) . . ? N9 Zr1 O1 82.55(12) . . ? N10 Zr1 N1 100.97(14) . . ? N9 Zr1 N1 133.37(13) . . ? O1 Zr1 N1 63.72(11) . . ? N10 Zr1 N2 131.55(13) . . ? N9 Zr1 N2 102.19(14) . . ? O1 Zr1 N2 124.47(11) . . ? N1 Zr1 N2 75.37(11) . . ? N10 Zr1 O2 82.67(12) . . ? N9 Zr1 O2 91.70(12) . . ? O1 Zr1 O2 171.12(10) . . ? N1 Zr1 O2 124.74(11) . . ? N2 Zr1 O2 63.29(10) . . ? N10 Zr1 P1 95.53(11) . . ? N9 Zr1 P1 109.85(10) . . ? O1 Zr1 P1 30.94(7) . . ? N1 Zr1 P1 32.99(8) . . ? N2 Zr1 P1 103.13(8) . . ? O2 Zr1 P1 157.06(8) . . ? N10 Zr1 P2 109.46(10) . . ? N9 Zr1 P2 94.77(11) . . ? O1 Zr1 P2 156.11(8) . . ? N1 Zr1 P2 103.51(9) . . ? N2 Zr1 P2 32.82(8) . . ? O2 Zr1 P2 30.77(7) . . ? P1 Zr1 P2 134.71(3) . . ? N11 Zr2 N12 106.40(14) . . ? N11 Zr2 N4 137.34(13) . . ? N12 Zr2 N4 100.91(13) . . ? N11 Zr2 O3 97.19(12) . . ? N12 Zr2 O3 84.44(12) . . ? N4 Zr2 O3 117.77(10) . . ? N11 Zr2 N3 103.25(12) . . ? N12 Zr2 N3 139.18(13) . . ? N4 Zr2 N3 74.07(11) . . ? O3 Zr2 N3 64.41(10) . . ? N11 Zr2 O4 82.72(12) . . ? N12 Zr2 O4 93.07(12) . . ? N4 Zr2 O4 63.46(10) . . ? O3 Zr2 O4 177.38(10) . . ? N3 Zr2 O4 118.18(11) . . ? N11 Zr2 P4 112.83(10) . . ? N12 Zr2 P4 92.56(10) . . ? N4 Zr2 P4 32.97(8) . . ? O3 Zr2 P4 149.34(7) . . ? N3 Zr2 P4 101.15(8) . . ? O4 Zr2 P4 31.36(7) . . ? N11 Zr2 P3 101.12(10) . . ? N12 Zr2 P3 112.61(10) . . ? N4 Zr2 P3 97.75(8) . . ? O3 Zr2 P3 31.33(7) . . ? N3 Zr2 P3 33.10(8) . . ? O4 Zr2 P3 151.26(7) . . ? P4 Zr2 P3 129.75(3) . . ? N13 Zr3 N14 112.37(17) . . ? N13 Zr3 N5 100.39(14) . . ? N14 Zr3 N5 135.90(16) . . ? N13 Zr3 N6 133.77(14) . . ? N14 Zr3 N6 99.95(15) . . ? N5 Zr3 N6 75.16(12) . . ? N13 Zr3 O5 93.85(13) . . ? N14 Zr3 O5 84.69(13) . . ? N5 Zr3 O5 63.79(11) . . ? N6 Zr3 O5 122.14(12) . . ? N13 Zr3 O6 81.49(13) . . ? N14 Zr3 O6 94.13(14) . . ? N5 Zr3 O6 120.02(11) . . ? N6 Zr3 O6 63.48(12) . . ? O5 Zr3 O6 174.37(11) . . ? N13 Zr3 P5 95.10(11) . . ? N14 Zr3 P5 112.71(12) . . ? N5 Zr3 P5 32.87(9) . . ? N6 Zr3 P5 102.08(9) . . ? O5 Zr3 P5 31.21(7) . . ? O6 Zr3 P5 151.89(8) . . ? N13 Zr3 P6 109.27(11) . . ? N14 Zr3 P6 95.69(12) . . ? N5 Zr3 P6 100.59(9) . . ? N6 Zr3 P6 32.67(9) . . ? O5 Zr3 P6 154.58(8) . . ? O6 Zr3 P6 30.99(7) . . ? P5 Zr3 P6 131.98(3) . . ? N16 Zr4 N15 112.48(15) . . ? N16 Zr4 O7 82.35(13) . . ? N15 Zr4 O7 89.97(13) . . ? N16 Zr4 N8 100.37(14) . . ? N15 Zr4 N8 133.91(14) . . ? O7 Zr4 N8 126.86(11) . . ? N16 Zr4 N7 129.63(14) . . ? N15 Zr4 N7 104.18(14) . . ? O7 Zr4 N7 63.93(11) . . ? N8 Zr4 N7 75.43(12) . . ? N16 Zr4 O8 93.14(14) . . ? N15 Zr4 O8 82.12(13) . . ? O7 Zr4 O8 168.65(11) . . ? N8 Zr4 O8 64.12(11) . . ? N7 Zr4 O8 125.88(12) . . ? N16 Zr4 P7 106.93(11) . . ? N15 Zr4 P7 97.26(11) . . ? O7 Zr4 P7 30.83(7) . . ? N8 Zr4 P7 103.23(9) . . ? N7 Zr4 P7 33.12(9) . . ? O8 Zr4 P7 158.30(9) . . ? N16 Zr4 P8 95.52(11) . . ? N15 Zr4 P8 109.55(11) . . ? O7 Zr4 P8 159.44(7) . . ? N8 Zr4 P8 33.21(9) . . ? N7 Zr4 P8 103.63(9) . . ? O8 Zr4 P8 31.05(8) . . ? P7 Zr4 P8 135.04(3) . . ? O1 P1 N1 99.64(17) . . ? O1 P1 C27 111.83(19) . . ? N1 P1 C27 113.67(19) . . ? O1 P1 C21 111.55(18) . . ? N1 P1 C21 112.13(19) . . ? C27 P1 C21 108.0(2) . . ? O1 P1 Zr1 49.65(10) . . ? N1 P1 Zr1 50.40(12) . . ? C27 P1 Zr1 121.58(15) . . ? C21 P1 Zr1 130.44(14) . . ? O2 P2 N2 100.29(17) . . ? O2 P2 C39 113.09(18) . . ? N2 P2 C39 112.05(18) . . ? O2 P2 C33 109.81(18) . . ? N2 P2 C33 116.01(18) . . ? C39 P2 C33 105.78(19) . . ? O2 P2 Zr1 50.26(10) . . ? N2 P2 Zr1 50.61(12) . . ? C39 P2 Zr1 133.10(14) . . ? C33 P2 Zr1 121.04(13) . . ? O3 P3 N3 100.47(16) . . ? O3 P3 C71 111.52(18) . . ? N3 P3 C71 113.39(18) . . ? O3 P3 C65 108.88(17) . . ? N3 P3 C65 114.47(18) . . ? C71 P3 C65 107.93(18) . . ? O3 P3 Zr2 49.06(10) . . ? N3 P3 Zr2 51.45(11) . . ? C71 P3 Zr2 128.31(13) . . ? C65 P3 Zr2 123.44(14) . . ? O4 P4 N4 100.19(16) . . ? O4 P4 C83 110.85(18) . . ? N4 P4 C83 113.75(18) . . ? O4 P4 C77 114.04(17) . . ? N4 P4 C77 112.43(18) . . ? C83 P4 C77 105.81(18) . . ? O4 P4 Zr2 52.53(11) . . ? N4 P4 Zr2 49.36(11) . . ? C83 P4 Zr2 115.45(13) . . ? C77 P4 Zr2 138.72(13) . . ? O5 P5 N5 99.97(17) . . ? O5 P5 C109 110.69(18) . . ? N5 P5 C109 115.44(19) . . ? O5 P5 C115 113.03(18) . . ? N5 P5 C115 111.69(19) . . ? C109 P5 C115 106.2(2) . . ? O5 P5 Zr3 50.65(11) . . ? N5 P5 Zr3 49.87(12) . . ? C109 P5 Zr3 121.39(14) . . ? C115 P5 Zr3 132.41(14) . . ? O6 P6 N6 100.86(17) . . ? O6 P6 C127 111.80(19) . . ? N6 P6 C127 111.57(19) . . ? O6 P6 C121 109.40(19) . . ? N6 P6 C121 115.2(2) . . ? C127 P6 C121 108.0(2) . . ? O6 P6 Zr3 50.66(11) . . ? N6 P6 Zr3 50.54(12) . . ? C127 P6 Zr3 130.36(14) . . ? C121 P6 Zr3 121.57(15) . . ? O7 P7 N7 100.26(17) . . ? O7 P7 C153 110.08(18) . . ? N7 P7 C153 115.99(19) . . ? O7 P7 C159 110.18(18) . . ? N7 P7 C159 112.87(18) . . ? C153 P7 C159 107.29(19) . . ? O7 P7 Zr4 49.68(11) . . ? N7 P7 Zr4 50.62(12) . . ? C153 P7 Zr4 126.02(14) . . ? C159 P7 Zr4 126.38(14) . . ? O8 P8 N8 100.75(18) . . ? O8 P8 C17A 112.9(5) . . ? N8 P8 C17A 114.7(5) . . ? O8 P8 C165 111.7(2) . . ? N8 P8 C165 115.10(19) . . ? C17A P8 C165 102.2(5) . . ? O8 P8 C171 114.9(4) . . ? N8 P8 C171 108.1(5) . . ? C17A P8 C171 6.7(7) . . ? C165 P8 C171 106.5(4) . . ? O8 P8 Zr4 50.66(12) . . ? N8 P8 Zr4 50.38(12) . . ? C17A P8 Zr4 133.8(4) . . ? C165 P8 Zr4 124.01(15) . . ? C171 P8 Zr4 129.4(4) . . ? P1 O1 Zr1 99.41(14) . . ? P2 O2 Zr1 98.97(13) . . ? P3 O3 Zr2 99.60(13) . . ? P4 O4 Zr2 96.11(14) . . ? P5 O5 Zr3 98.14(14) . . ? P6 O6 Zr3 98.35(14) . . ? P7 O7 Zr4 99.49(14) . . ? P8 O8 Zr4 98.29(15) . . ? C2 N1 P1 133.7(3) . . ? C2 N1 Zr1 127.0(2) . . ? P1 N1 Zr1 96.62(16) . . ? C12 N2 P2 134.0(3) . . ? C12 N2 Zr1 126.6(2) . . ? P2 N2 Zr1 96.58(15) . . ? C46 N3 P3 131.1(3) . . ? C46 N3 Zr2 133.0(2) . . ? P3 N3 Zr2 95.45(15) . . ? C56 N4 P4 134.1(3) . . ? C56 N4 Zr2 122.3(2) . . ? P4 N4 Zr2 97.67(15) . . ? C90 N5 P5 135.5(3) . . ? C90 N5 Zr3 123.9(3) . . ? P5 N5 Zr3 97.26(16) . . ? C100 N6 P6 133.9(3) . . ? C100 N6 Zr3 129.1(3) . . ? P6 N6 Zr3 96.78(17) . . ? C134 N7 P7 130.5(3) . . ? C134 N7 Zr4 132.6(3) . . ? P7 N7 Zr4 96.27(16) . . ? C144 N8 P8 133.7(3) . . ? C144 N8 Zr4 125.1(3) . . ? P8 N8 Zr4 96.41(16) . . ? C178 N9 C177 112.3(4) . . ? C178 N9 Zr1 124.1(3) . . ? C177 N9 Zr1 122.3(3) . . ? C179 N10 C180 112.5(4) . . ? C179 N10 Zr1 126.0(3) . . ? C180 N10 Zr1 121.1(3) . . ? C181 N11 C182 110.6(4) . . ? C181 N11 Zr2 131.8(3) . . ? C182 N11 Zr2 117.3(3) . . ? C184 N12 C183 110.9(3) . . ? C184 N12 Zr2 124.8(3) . . ? C183 N12 Zr2 123.1(3) . . ? C185 N13 C186 112.8(4) . . ? C185 N13 Zr3 124.2(3) . . ? C186 N13 Zr3 122.8(3) . . ? C188 N14 C187 114.3(5) . . ? C188 N14 Zr3 117.5(4) . . ? C187 N14 Zr3 127.8(4) . . ? C190 N15 C189 112.3(4) . . ? C190 N15 Zr4 122.2(3) . . ? C189 N15 Zr4 125.4(3) . . ? C191 N16 C192 111.3(5) . . ? C191 N16 Zr4 127.0(3) . . ? C192 N16 Zr4 119.8(4) . . ? C2 C1 C6 119.9(4) . . ? C2 C1 C11 120.2(4) . . ? C6 C1 C11 119.8(3) . . ? C1 C2 N1 120.3(4) . . ? C1 C2 C3 119.1(4) . . ? N1 C2 C3 120.4(4) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 121.1(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C10 C5 C4 122.0(4) . . ? C10 C5 C6 119.6(4) . . ? C4 C5 C6 118.4(4) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 C1 121.5(4) . . ? C5 C6 C1 119.8(4) . . ? C8 C7 C6 119.7(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 121.6(4) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C5 121.0(4) . . ? C9 C10 H10 119.5 . . ? C5 C10 H10 119.5 . . ? C12 C11 C16 120.0(3) . . ? C12 C11 C1 120.0(3) . . ? C16 C11 C1 120.0(3) . . ? C11 C12 N2 121.5(3) . . ? C11 C12 C13 119.5(4) . . ? N2 C12 C13 118.8(3) . . ? C14 C13 C12 120.9(4) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 121.1(4) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C20 C15 C14 122.0(4) . . ? C20 C15 C16 119.5(4) . . ? C14 C15 C16 118.6(4) . . ? C17 C16 C11 122.6(4) . . ? C17 C16 C15 117.6(3) . . ? C11 C16 C15 119.8(4) . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 120.7(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 118.5(4) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C15 122.1(4) . . ? C19 C20 H20 118.9 . . ? C15 C20 H20 118.9 . . ? C26 C21 C22 119.2(4) . . ? C26 C21 P1 117.6(3) . . ? C22 C21 P1 123.0(4) . . ? C21 C22 C23 119.7(5) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 118.9(5) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C21 C26 C25 121.5(4) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C32 118.6(5) . . ? C28 C27 P1 118.8(4) . . ? C32 C27 P1 122.2(4) . . ? C29 C28 C27 122.0(5) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 117.6(5) . . ? C28 C29 H29 121.2 . . ? C30 C29 H29 121.2 . . ? C31 C30 C29 122.0(5) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 119.4(5) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C27 C32 C31 120.3(5) . . ? C27 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C38 C33 C34 118.7(4) . . ? C38 C33 P2 123.7(3) . . ? C34 C33 P2 117.6(3) . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 119.1(4) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C37 C36 C35 121.4(4) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 119.1(4) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C37 C38 C33 121.5(4) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? C44 C39 C40 119.0(4) . . ? C44 C39 P2 118.3(3) . . ? C40 C39 P2 122.7(3) . . ? C39 C40 C41 119.6(4) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C42 C41 C40 120.0(4) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.7(4) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 119.9(5) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C39 120.8(4) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C46 C45 C50 118.7(3) . . ? C46 C45 C55 119.6(3) . . ? C50 C45 C55 121.7(3) . . ? C45 C46 N3 122.1(3) . . ? C45 C46 C47 119.6(4) . . ? N3 C46 C47 118.1(3) . . ? C48 C47 C46 122.3(4) . . ? C48 C47 H47 118.9 . . ? C46 C47 H47 118.9 . . ? C47 C48 C49 119.7(4) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C48 C49 C50 119.6(4) . . ? C48 C49 C54 121.0(4) . . ? C50 C49 C54 119.4(4) . . ? C49 C50 C45 120.1(3) . . ? C49 C50 C51 117.2(4) . . ? C45 C50 C51 122.7(3) . . ? C52 C51 C50 121.9(4) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C51 C52 C53 120.4(4) . . ? C51 C52 H52 119.8 . . ? C53 C52 H52 119.8 . . ? C54 C53 C52 119.9(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C49 121.2(4) . . ? C53 C54 H54 119.4 . . ? C49 C54 H54 119.4 . . ? C56 C55 C60 118.6(3) . . ? C56 C55 C45 120.2(3) . . ? C60 C55 C45 121.1(3) . . ? C55 C56 C57 121.0(4) . . ? C55 C56 N4 120.1(3) . . ? C57 C56 N4 118.6(3) . . ? C58 C57 C56 120.7(4) . . ? C58 C57 H57 119.7 . . ? C56 C57 H57 119.7 . . ? C57 C58 C59 120.3(4) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C60 119.5(4) . . ? C58 C59 C64 120.6(4) . . ? C60 C59 C64 119.9(4) . . ? C59 C60 C55 119.7(3) . . ? C59 C60 C61 117.0(4) . . ? C55 C60 C61 123.3(4) . . ? C62 C61 C60 121.2(4) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C61 C62 C63 121.0(4) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C64 C63 C62 120.0(4) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C59 120.7(4) . . ? C63 C64 H64 119.6 . . ? C59 C64 H64 119.6 . . ? C66 C65 C70 119.6(4) . . ? C66 C65 P3 122.8(3) . . ? C70 C65 P3 117.3(3) . . ? C67 C66 C65 119.9(4) . . ? C67 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C68 C67 C66 120.7(4) . . ? C68 C67 H67 119.7 . . ? C66 C67 H67 119.7 . . ? C67 C68 C69 119.7(4) . . ? C67 C68 H68 120.2 . . ? C69 C68 H68 120.2 . . ? C68 C69 C70 120.7(4) . . ? C68 C69 H69 119.6 . . ? C70 C69 H69 119.6 . . ? C69 C70 C65 119.5(4) . . ? C69 C70 H70 120.3 . . ? C65 C70 H70 120.3 . . ? C72 C71 C76 119.1(4) . . ? C72 C71 P3 119.5(3) . . ? C76 C71 P3 121.2(3) . . ? C73 C72 C71 120.9(4) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 119.2(4) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C75 C74 C73 120.3(4) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 C76 121.0(4) . . ? C74 C75 H75 119.5 . . ? C76 C75 H75 119.5 . . ? C75 C76 C71 119.5(4) . . ? C75 C76 H76 120.2 . . ? C71 C76 H76 120.2 . . ? C82 C77 C78 119.0(4) . . ? C82 C77 P4 122.1(3) . . ? C78 C77 P4 118.9(3) . . ? C79 C78 C77 120.7(4) . . ? C79 C78 H78 119.7 . . ? C77 C78 H78 119.7 . . ? C78 C79 C80 120.2(4) . . ? C78 C79 H79 119.9 . . ? C80 C79 H79 119.9 . . ? C81 C80 C79 119.3(4) . . ? C81 C80 H80 120.3 . . ? C79 C80 H80 120.3 . . ? C82 C81 C80 120.7(4) . . ? C82 C81 H81 119.6 . . ? C80 C81 H81 119.6 . . ? C81 C82 C77 120.0(4) . . ? C81 C82 H82 120.0 . . ? C77 C82 H82 120.0 . . ? C84 C83 C88 119.2(4) . . ? C84 C83 P4 120.2(3) . . ? C88 C83 P4 120.3(3) . . ? C83 C84 C85 119.2(5) . . ? C83 C84 H84 120.4 . . ? C85 C84 H84 120.4 . . ? C86 C85 C84 121.2(5) . . ? C86 C85 H85 119.4 . . ? C84 C85 H85 119.4 . . ? C85 C86 C87 120.5(5) . . ? C85 C86 H86 119.8 . . ? C87 C86 H86 119.8 . . ? C88 C87 C86 118.9(5) . . ? C88 C87 H87 120.6 . . ? C86 C87 H87 120.6 . . ? C87 C88 C83 121.0(4) . . ? C87 C88 H88 119.5 . . ? C83 C88 H88 119.5 . . ? C90 C89 C94 119.6(4) . . ? C90 C89 C99 120.2(3) . . ? C94 C89 C99 120.0(4) . . ? C89 C90 N5 120.5(4) . . ? C89 C90 C91 120.1(4) . . ? N5 C90 C91 119.2(4) . . ? C92 C91 C90 120.9(4) . . ? C92 C91 H91 119.6 . . ? C90 C91 H91 119.6 . . ? C91 C92 C93 120.7(4) . . ? C91 C92 H92 119.6 . . ? C93 C92 H92 119.6 . . ? C92 C93 C98 121.6(4) . . ? C92 C93 C94 119.7(4) . . ? C98 C93 C94 118.7(4) . . ? C95 C94 C93 118.1(4) . . ? C95 C94 C89 122.9(4) . . ? C93 C94 C89 119.0(4) . . ? C96 C95 C94 121.2(4) . . ? C96 C95 H95 119.4 . . ? C94 C95 H95 119.4 . . ? C95 C96 C97 120.7(4) . . ? C95 C96 H96 119.6 . . ? C97 C96 H96 119.6 . . ? C98 C97 C96 120.0(4) . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C97 C98 C93 121.2(4) . . ? C97 C98 H98 119.4 . . ? C93 C98 H98 119.4 . . ? C100 C99 C104 119.0(4) . . ? C100 C99 C89 119.6(4) . . ? C104 C99 C89 121.2(4) . . ? C99 C100 N6 121.4(3) . . ? C99 C100 C101 119.4(4) . . ? N6 C100 C101 118.9(4) . . ? C102 C101 C100 121.9(4) . . ? C102 C101 H101 119.1 . . ? C100 C101 H101 119.1 . . ? C101 C102 C103 120.5(4) . . ? C101 C102 H102 119.7 . . ? C103 C102 H102 119.7 . . ? C102 C103 C108 122.1(4) . . ? C102 C103 C104 119.0(4) . . ? C108 C103 C104 118.8(4) . . ? C105 C104 C99 121.7(4) . . ? C105 C104 C103 118.4(4) . . ? C99 C104 C103 119.8(4) . . ? C106 C105 C104 121.2(4) . . ? C106 C105 H105 119.4 . . ? C104 C105 H105 119.4 . . ? C105 C106 C107 120.6(4) . . ? C105 C106 H106 119.7 . . ? C107 C106 H106 119.7 . . ? C108 C107 C106 119.5(4) . . ? C108 C107 H107 120.3 . . ? C106 C107 H107 120.3 . . ? C107 C108 C103 121.4(4) . . ? C107 C108 H108 119.3 . . ? C103 C108 H108 119.3 . . ? C114 C109 C110 118.8(4) . . ? C114 C109 P5 119.3(3) . . ? C110 C109 P5 121.9(3) . . ? C111 C110 C109 121.0(4) . . ? C111 C110 H110 119.5 . . ? C109 C110 H110 119.5 . . ? C110 C111 C112 119.4(4) . . ? C110 C111 H111 120.3 . . ? C112 C111 H111 120.3 . . ? C111 C112 C113 120.5(4) . . ? C111 C112 H112 119.7 . . ? C113 C112 H112 119.7 . . ? C112 C113 C114 120.0(4) . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C109 C114 C113 120.2(4) . . ? C109 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C116 C115 C120 118.3(4) . . ? C116 C115 P5 123.8(3) . . ? C120 C115 P5 117.9(3) . . ? C117 C116 C115 121.0(4) . . ? C117 C116 H116 119.5 . . ? C115 C116 H116 119.5 . . ? C116 C117 C118 119.9(5) . . ? C116 C117 H117 120.0 . . ? C118 C117 H117 120.0 . . ? C119 C118 C117 119.2(5) . . ? C119 C118 H118 120.4 . . ? C117 C118 H118 120.4 . . ? C118 C119 C120 120.5(4) . . ? C118 C119 H119 119.8 . . ? C120 C119 H119 119.8 . . ? C119 C120 C115 121.0(4) . . ? C119 C120 H120 119.5 . . ? C115 C120 H120 119.5 . . ? C122 C121 C126 118.8(4) . . ? C122 C121 P6 124.2(3) . . ? C126 C121 P6 117.0(3) . . ? C121 C122 C123 120.6(4) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 120.3(5) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 119.4(4) . . ? C125 C124 H124 120.3 . . ? C123 C124 H124 120.3 . . ? C124 C125 C126 120.4(5) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C121 C126 C125 120.3(5) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? C128 C127 C132 119.3(4) . . ? C128 C127 P6 118.0(3) . . ? C132 C127 P6 122.6(3) . . ? C127 C128 C129 120.4(4) . . ? C127 C128 H128 119.8 . . ? C129 C128 H128 119.8 . . ? C130 C129 C128 119.5(4) . . ? C130 C129 H129 120.2 . . ? C128 C129 H129 120.2 . . ? C129 C130 C131 120.6(4) . . ? C129 C130 H130 119.7 . . ? C131 C130 H130 119.7 . . ? C132 C131 C130 119.4(4) . . ? C132 C131 H131 120.3 . . ? C130 C131 H131 120.3 . . ? C131 C132 C127 120.8(4) . . ? C131 C132 H132 119.6 . . ? C127 C132 H132 119.6 . . ? C134 C133 C138 119.2(4) . . ? C134 C133 C143 121.0(4) . . ? C138 C133 C143 119.8(3) . . ? C133 C134 C135 120.0(4) . . ? C133 C134 N7 120.1(4) . . ? C135 C134 N7 119.6(4) . . ? C136 C135 C134 121.3(4) . . ? C136 C135 H135 119.3 . . ? C134 C135 H135 119.3 . . ? C135 C136 C137 121.1(4) . . ? C135 C136 H136 119.5 . . ? C137 C136 H136 119.5 . . ? C136 C137 C138 118.7(4) . . ? C136 C137 C142 121.6(4) . . ? C138 C137 C142 119.6(4) . . ? C139 C138 C137 117.4(4) . . ? C139 C138 C133 123.1(4) . . ? C137 C138 C133 119.5(4) . . ? C140 C139 C138 121.7(4) . . ? C140 C139 H139 119.2 . . ? C138 C139 H139 119.2 . . ? C139 C140 C141 121.0(4) . . ? C139 C140 H140 119.5 . . ? C141 C140 H140 119.5 . . ? C142 C141 C140 118.9(4) . . ? C142 C141 H141 120.6 . . ? C140 C141 H141 120.6 . . ? C141 C142 C137 121.4(4) . . ? C141 C142 H142 119.3 . . ? C137 C142 H142 119.3 . . ? C144 C143 C148 118.4(4) . . ? C144 C143 C133 121.7(4) . . ? C148 C143 C133 119.9(4) . . ? C143 C144 N8 120.2(4) . . ? C143 C144 C145 120.5(4) . . ? N8 C144 C145 119.0(4) . . ? C146 C145 C144 121.3(4) . . ? C146 C145 H145 119.3 . . ? C144 C145 H145 119.3 . . ? C145 C146 C147 120.3(4) . . ? C145 C146 H146 119.9 . . ? C147 C146 H146 119.9 . . ? C148 C147 C152 119.6(4) . . ? C148 C147 C146 118.7(4) . . ? C152 C147 C146 121.7(4) . . ? C147 C148 C149 117.2(4) . . ? C147 C148 C143 120.7(4) . . ? C149 C148 C143 122.1(4) . . ? C150 C149 C148 121.5(4) . . ? C150 C149 H149 119.3 . . ? C148 C149 H149 119.3 . . ? C149 C150 C151 120.6(4) . . ? C149 C150 H150 119.7 . . ? C151 C150 H150 119.7 . . ? C152 C151 C150 119.8(4) . . ? C152 C151 H151 120.1 . . ? C150 C151 H151 120.1 . . ? C151 C152 C147 121.3(4) . . ? C151 C152 H152 119.3 . . ? C147 C152 H152 119.3 . . ? C158 C153 C154 118.6(4) . . ? C158 C153 P7 123.0(3) . . ? C154 C153 P7 118.2(3) . . ? C153 C154 C155 119.5(4) . . ? C153 C154 H154 120.2 . . ? C155 C154 H154 120.2 . . ? C156 C155 C154 120.6(4) . . ? C156 C155 H155 119.7 . . ? C154 C155 H155 119.7 . . ? C157 C156 C155 120.0(4) . . ? C157 C156 H156 120.0 . . ? C155 C156 H156 120.0 . . ? C156 C157 C158 120.3(4) . . ? C156 C157 H157 119.8 . . ? C158 C157 H157 119.8 . . ? C153 C158 C157 120.9(4) . . ? C153 C158 H158 119.6 . . ? C157 C158 H158 119.6 . . ? C164 C159 C160 119.3(4) . . ? C164 C159 P7 120.2(3) . . ? C160 C159 P7 120.5(3) . . ? C159 C160 C161 120.5(4) . . ? C159 C160 H160 119.8 . . ? C161 C160 H160 119.8 . . ? C162 C161 C160 118.8(4) . . ? C162 C161 H161 120.6 . . ? C160 C161 H161 120.6 . . ? C163 C162 C161 120.7(4) . . ? C163 C162 H162 119.6 . . ? C161 C162 H162 119.6 . . ? C162 C163 C164 120.0(4) . . ? C162 C163 H163 120.0 . . ? C164 C163 H163 120.0 . . ? C159 C164 C163 120.7(4) . . ? C159 C164 H164 119.7 . . ? C163 C164 H164 119.7 . . ? C166 C165 C170 118.7(4) . . ? C166 C165 P8 121.1(4) . . ? C170 C165 P8 120.1(3) . . ? C165 C166 C167 120.4(5) . . ? C165 C166 H166 119.8 . . ? C167 C166 H166 119.8 . . ? C168 C167 C166 119.7(5) . . ? C168 C167 H167 120.1 . . ? C166 C167 H167 120.1 . . ? C169 C168 C167 120.2(5) . . ? C169 C168 H168 119.9 . . ? C167 C168 H168 119.9 . . ? C168 C169 C170 120.1(5) . . ? C168 C169 H169 120.0 . . ? C170 C169 H169 120.0 . . ? C169 C170 C165 120.9(4) . . ? C169 C170 H170 119.6 . . ? C165 C170 H170 119.6 . . ? C172 C171 C176 120.0 . . ? C172 C171 P8 121.8(7) . . ? C176 C171 P8 118.2(7) . . ? C171 C172 C173 120.0 . . ? C171 C172 H17J 120.0 . . ? C173 C172 H17J 120.0 . . ? C174 C173 C172 120.0 . . ? C174 C173 H17K 120.0 . . ? C172 C173 H17K 120.0 . . ? C175 C174 C173 120.0 . . ? C175 C174 H17L 120.0 . . ? C173 C174 H17L 120.0 . . ? C174 C175 C176 120.0 . . ? C174 C175 H17M 120.0 . . ? C176 C175 H17M 120.0 . . ? C175 C176 C171 120.0 . . ? C175 C176 H17N 120.0 . . ? C171 C176 H17N 120.0 . . ? N9 C177 H17A 109.5 . . ? N9 C177 H17B 109.5 . . ? H17A C177 H17B 109.5 . . ? N9 C177 H17C 109.5 . . ? H17A C177 H17C 109.5 . . ? H17B C177 H17C 109.5 . . ? C17B C17A C17F 120.0 . . ? C17B C17A P8 121.0(7) . . ? C17F C17A P8 118.7(7) . . ? C17C C17B C17A 120.0 . . ? C17C C17B H17O 120.0 . . ? C17A C17B H17O 120.0 . . ? C17B C17C C17D 120.0 . . ? C17B C17C H17P 120.0 . . ? C17D C17C H17P 120.0 . . ? C17C C17D C17E 120.0 . . ? C17C C17D H17Q 120.0 . . ? C17E C17D H17Q 120.0 . . ? C17F C17E C17D 120.0 . . ? C17F C17E H17R 120.0 . . ? C17D C17E H17R 120.0 . . ? C17E C17F C17A 120.0 . . ? C17E C17F H17S 120.0 . . ? C17A C17F H17S 120.0 . . ? N9 C178 H17D 109.5 . . ? N9 C178 H17E 109.5 . . ? H17D C178 H17E 109.5 . . ? N9 C178 H17F 109.5 . . ? H17D C178 H17F 109.5 . . ? H17E C178 H17F 109.5 . . ? N10 C179 H17G 109.5 . . ? N10 C179 H17H 109.5 . . ? H17G C179 H17H 109.5 . . ? N10 C179 H17I 109.5 . . ? H17G C179 H17I 109.5 . . ? H17H C179 H17I 109.5 . . ? N10 C180 H18A 109.5 . . ? N10 C180 H18B 109.5 . . ? H18A C180 H18B 109.5 . . ? N10 C180 H18C 109.5 . . ? H18A C180 H18C 109.5 . . ? H18B C180 H18C 109.5 . . ? N11 C181 H18D 109.5 . . ? N11 C181 H18E 109.5 . . ? H18D C181 H18E 109.5 . . ? N11 C181 H18F 109.5 . . ? H18D C181 H18F 109.5 . . ? H18E C181 H18F 109.5 . . ? N11 C182 H18G 109.5 . . ? N11 C182 H18H 109.5 . . ? H18G C182 H18H 109.5 . . ? N11 C182 H18I 109.5 . . ? H18G C182 H18I 109.5 . . ? H18H C182 H18I 109.5 . . ? N12 C183 H18J 109.5 . . ? N12 C183 H18K 109.5 . . ? H18J C183 H18K 109.5 . . ? N12 C183 H18L 109.5 . . ? H18J C183 H18L 109.5 . . ? H18K C183 H18L 109.5 . . ? N12 C184 H18M 109.5 . . ? N12 C184 H18N 109.5 . . ? H18M C184 H18N 109.5 . . ? N12 C184 H18O 109.5 . . ? H18M C184 H18O 109.5 . . ? H18N C184 H18O 109.5 . . ? N13 C185 H18P 109.5 . . ? N13 C185 H18Q 109.5 . . ? H18P C185 H18Q 109.5 . . ? N13 C185 H18R 109.5 . . ? H18P C185 H18R 109.5 . . ? H18Q C185 H18R 109.5 . . ? N13 C186 H18S 109.5 . . ? N13 C186 H18T 109.5 . . ? H18S C186 H18T 109.5 . . ? N13 C186 H18U 109.5 . . ? H18S C186 H18U 109.5 . . ? H18T C186 H18U 109.5 . . ? N14 C187 H8CA 109.5 . . ? N14 C187 H8CB 109.5 . . ? H8CA C187 H8CB 109.5 . . ? N14 C187 H8CC 109.5 . . ? H8CA C187 H8CC 109.5 . . ? H8CB C187 H8CC 109.5 . . ? N14 C188 H8AA 109.5 . . ? N14 C188 H8AB 109.5 . . ? H8AA C188 H8AB 109.5 . . ? N14 C188 H8AC 109.5 . . ? H8AA C188 H8AC 109.5 . . ? H8AB C188 H8AC 109.5 . . ? N15 C189 H8BA 109.5 . . ? N15 C189 H8BB 109.5 . . ? H8BA C189 H8BB 109.5 . . ? N15 C189 H8BC 109.5 . . ? H8BA C189 H8BC 109.5 . . ? H8BB C189 H8BC 109.5 . . ? N15 C190 H19A 109.5 . . ? N15 C190 H19B 109.5 . . ? H19A C190 H19B 109.5 . . ? N15 C190 H19C 109.5 . . ? H19A C190 H19C 109.5 . . ? H19B C190 H19C 109.5 . . ? N16 C191 H19D 109.5 . . ? N16 C191 H19E 109.5 . . ? H19D C191 H19E 109.5 . . ? N16 C191 H19F 109.5 . . ? H19D C191 H19F 109.5 . . ? H19E C191 H19F 109.5 . . ? N16 C192 H19G 109.5 . . ? N16 C192 H19H 109.5 . . ? H19G C192 H19H 109.5 . . ? N16 C192 H19I 109.5 . . ? H19G C192 H19I 109.5 . . ? H19H C192 H19I 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 N10 Zr1 P1 O1 -87.17(19) . . . . ? N9 Zr1 P1 O1 29.51(19) . . . . ? N1 Zr1 P1 O1 171.2(2) . . . . ? N2 Zr1 P1 O1 137.85(17) . . . . ? O2 Zr1 P1 O1 -171.4(2) . . . . ? P2 Zr1 P1 O1 148.30(15) . . . . ? N10 Zr1 P1 N1 101.64(19) . . . . ? N9 Zr1 P1 N1 -141.7(2) . . . . ? O1 Zr1 P1 N1 -171.2(2) . . . . ? N2 Zr1 P1 N1 -33.33(18) . . . . ? O2 Zr1 P1 N1 17.4(3) . . . . ? P2 Zr1 P1 N1 -22.89(17) . . . . ? N10 Zr1 P1 C27 5.7(2) . . . . ? N9 Zr1 P1 C27 122.4(2) . . . . ? O1 Zr1 P1 C27 92.9(2) . . . . ? N1 Zr1 P1 C27 -95.9(2) . . . . ? N2 Zr1 P1 C27 -129.25(19) . . . . ? O2 Zr1 P1 C27 -78.5(3) . . . . ? P2 Zr1 P1 C27 -118.80(17) . . . . ? N10 Zr1 P1 C21 -172.0(2) . . . . ? N9 Zr1 P1 C21 -55.3(2) . . . . ? O1 Zr1 P1 C21 -84.8(2) . . . . ? N1 Zr1 P1 C21 86.4(2) . . . . ? N2 Zr1 P1 C21 53.1(2) . . . . ? O2 Zr1 P1 C21 103.8(3) . . . . ? P2 Zr1 P1 C21 63.52(19) . . . . ? N10 Zr1 P2 O2 30.92(18) . . . . ? N9 Zr1 P2 O2 -85.31(18) . . . . ? O1 Zr1 P2 O2 -167.7(2) . . . . ? N1 Zr1 P2 O2 137.92(17) . . . . ? N2 Zr1 P2 O2 169.5(2) . . . . ? P1 Zr1 P2 O2 150.50(14) . . . . ? N10 Zr1 P2 N2 -138.60(19) . . . . ? N9 Zr1 P2 N2 105.18(18) . . . . ? O1 Zr1 P2 N2 22.8(2) . . . . ? N1 Zr1 P2 N2 -31.60(17) . . . . ? O2 Zr1 P2 N2 -169.5(2) . . . . ? P1 Zr1 P2 N2 -19.02(16) . . . . ? N10 Zr1 P2 C39 -54.5(2) . . . . ? N9 Zr1 P2 C39 -170.7(2) . . . . ? O1 Zr1 P2 C39 106.9(3) . . . . ? N1 Zr1 P2 C39 52.5(2) . . . . ? N2 Zr1 P2 C39 84.1(2) . . . . ? O2 Zr1 P2 C39 -85.4(2) . . . . ? P1 Zr1 P2 C39 65.06(19) . . . . ? N10 Zr1 P2 C33 121.73(19) . . . . ? N9 Zr1 P2 C33 5.50(18) . . . . ? O1 Zr1 P2 C33 -76.9(2) . . . . ? N1 Zr1 P2 C33 -131.28(17) . . . . ? N2 Zr1 P2 C33 -99.7(2) . . . . ? O2 Zr1 P2 C33 90.8(2) . . . . ? P1 Zr1 P2 C33 -118.70(15) . . . . ? N11 Zr2 P3 O3 -85.56(16) . . . . ? N12 Zr2 P3 O3 27.61(17) . . . . ? N4 Zr2 P3 O3 132.90(16) . . . . ? N3 Zr2 P3 O3 177.2(2) . . . . ? O4 Zr2 P3 O3 179.28(19) . . . . ? P4 Zr2 P3 O3 141.78(13) . . . . ? N11 Zr2 P3 N3 97.26(17) . . . . ? N12 Zr2 P3 N3 -149.57(18) . . . . ? N4 Zr2 P3 N3 -44.28(17) . . . . ? O3 Zr2 P3 N3 -177.2(2) . . . . ? O4 Zr2 P3 N3 2.1(2) . . . . ? P4 Zr2 P3 N3 -35.40(15) . . . . ? N11 Zr2 P3 C71 -171.8(2) . . . . ? N12 Zr2 P3 C71 -58.6(2) . . . . ? N4 Zr2 P3 C71 46.7(2) . . . . ? O3 Zr2 P3 C71 -86.2(2) . . . . ? N3 Zr2 P3 C71 91.0(2) . . . . ? O4 Zr2 P3 C71 93.1(2) . . . . ? P4 Zr2 P3 C71 55.58(19) . . . . ? N11 Zr2 P3 C65 1.03(19) . . . . ? N12 Zr2 P3 C65 114.20(19) . . . . ? N4 Zr2 P3 C65 -140.51(18) . . . . ? O3 Zr2 P3 C65 86.6(2) . . . . ? N3 Zr2 P3 C65 -96.2(2) . . . . ? O4 Zr2 P3 C65 -94.1(2) . . . . ? P4 Zr2 P3 C65 -131.63(16) . . . . ? N11 Zr2 P4 O4 17.30(17) . . . . ? N12 Zr2 P4 O4 -91.69(17) . . . . ? N4 Zr2 P4 O4 162.1(2) . . . . ? O3 Zr2 P4 O4 -175.10(19) . . . . ? N3 Zr2 P4 O4 126.96(16) . . . . ? P3 Zr2 P4 O4 145.77(14) . . . . ? N11 Zr2 P4 N4 -144.80(18) . . . . ? N12 Zr2 P4 N4 106.21(18) . . . . ? O3 Zr2 P4 N4 22.8(2) . . . . ? N3 Zr2 P4 N4 -35.13(17) . . . . ? O4 Zr2 P4 N4 -162.1(2) . . . . ? P3 Zr2 P4 N4 -16.32(16) . . . . ? N11 Zr2 P4 C83 114.87(19) . . . . ? N12 Zr2 P4 C83 5.88(18) . . . . ? N4 Zr2 P4 C83 -100.3(2) . . . . ? O3 Zr2 P4 C83 -77.5(2) . . . . ? N3 Zr2 P4 C83 -135.46(17) . . . . ? O4 Zr2 P4 C83 97.6(2) . . . . ? P3 Zr2 P4 C83 -116.65(16) . . . . ? N11 Zr2 P4 C77 -67.2(2) . . . . ? N12 Zr2 P4 C77 -176.2(2) . . . . ? N4 Zr2 P4 C77 77.6(2) . . . . ? O3 Zr2 P4 C77 100.4(2) . . . . ? N3 Zr2 P4 C77 42.4(2) . . . . ? O4 Zr2 P4 C77 -84.5(2) . . . . ? P3 Zr2 P4 C77 61.2(2) . . . . ? N13 Zr3 P5 O5 -89.01(18) . . . . ? N14 Zr3 P5 O5 27.8(2) . . . . ? N5 Zr3 P5 O5 169.7(2) . . . . ? N6 Zr3 P5 O5 134.16(17) . . . . ? O6 Zr3 P5 O5 -170.5(2) . . . . ? P6 Zr3 P5 O5 149.26(15) . . . . ? N13 Zr3 P5 N5 101.27(19) . . . . ? N14 Zr3 P5 N5 -141.9(2) . . . . ? N6 Zr3 P5 N5 -35.56(19) . . . . ? O5 Zr3 P5 N5 -169.7(2) . . . . ? O6 Zr3 P5 N5 19.8(2) . . . . ? P6 Zr3 P5 N5 -20.46(17) . . . . ? N13 Zr3 P5 C109 3.00(19) . . . . ? N14 Zr3 P5 C109 119.8(2) . . . . ? N5 Zr3 P5 C109 -98.3(2) . . . . ? N6 Zr3 P5 C109 -133.83(18) . . . . ? O5 Zr3 P5 C109 92.0(2) . . . . ? O6 Zr3 P5 C109 -78.5(2) . . . . ? P6 Zr3 P5 C109 -118.73(16) . . . . ? N13 Zr3 P5 C115 -175.3(2) . . . . ? N14 Zr3 P5 C115 -58.5(2) . . . . ? N5 Zr3 P5 C115 83.4(2) . . . . ? N6 Zr3 P5 C115 47.8(2) . . . . ? O5 Zr3 P5 C115 -86.3(2) . . . . ? O6 Zr3 P5 C115 103.2(2) . . . . ? P6 Zr3 P5 C115 62.93(19) . . . . ? N13 Zr3 P6 O6 27.57(18) . . . . ? N14 Zr3 P6 O6 -88.5(2) . . . . ? N5 Zr3 P6 O6 132.63(17) . . . . ? N6 Zr3 P6 O6 171.9(2) . . . . ? O5 Zr3 P6 O6 -178.2(2) . . . . ? P5 Zr3 P6 O6 143.75(15) . . . . ? N13 Zr3 P6 N6 -144.3(2) . . . . ? N14 Zr3 P6 N6 99.6(2) . . . . ? N5 Zr3 P6 N6 -39.28(18) . . . . ? O5 Zr3 P6 N6 9.9(2) . . . . ? O6 Zr3 P6 N6 -171.9(2) . . . . ? P5 Zr3 P6 N6 -28.15(17) . . . . ? N13 Zr3 P6 C127 -58.6(2) . . . . ? N14 Zr3 P6 C127 -174.7(2) . . . . ? N5 Zr3 P6 C127 46.4(2) . . . . ? N6 Zr3 P6 C127 85.7(2) . . . . ? O5 Zr3 P6 C127 95.7(2) . . . . ? O6 Zr3 P6 C127 -86.2(2) . . . . ? P5 Zr3 P6 C127 57.57(19) . . . . ? N13 Zr3 P6 C121 117.6(2) . . . . ? N14 Zr3 P6 C121 1.5(2) . . . . ? N5 Zr3 P6 C121 -137.35(19) . . . . ? N6 Zr3 P6 C121 -98.1(2) . . . . ? O5 Zr3 P6 C121 -88.1(2) . . . . ? O6 Zr3 P6 C121 90.0(2) . . . . ? P5 Zr3 P6 C121 -126.23(17) . . . . ? N16 Zr4 P7 O7 38.60(18) . . . . ? N15 Zr4 P7 O7 -77.62(18) . . . . ? N8 Zr4 P7 O7 143.95(17) . . . . ? N7 Zr4 P7 O7 177.5(2) . . . . ? O8 Zr4 P7 O7 -164.5(3) . . . . ? P8 Zr4 P7 O7 155.17(14) . . . . ? N16 Zr4 P7 N7 -138.90(19) . . . . ? N15 Zr4 P7 N7 104.9(2) . . . . ? O7 Zr4 P7 N7 -177.5(2) . . . . ? N8 Zr4 P7 N7 -33.54(18) . . . . ? O8 Zr4 P7 N7 18.0(3) . . . . ? P8 Zr4 P7 N7 -22.33(17) . . . . ? N16 Zr4 P7 C153 125.1(2) . . . . ? N15 Zr4 P7 C153 8.9(2) . . . . ? O7 Zr4 P7 C153 86.5(2) . . . . ? N8 Zr4 P7 C153 -129.5(2) . . . . ? N7 Zr4 P7 C153 -96.0(2) . . . . ? O8 Zr4 P7 C153 -78.0(3) . . . . ? P8 Zr4 P7 C153 -118.30(18) . . . . ? N16 Zr4 P7 C159 -47.8(2) . . . . ? N15 Zr4 P7 C159 -164.0(2) . . . . ? O7 Zr4 P7 C159 -86.4(2) . . . . ? N8 Zr4 P7 C159 57.6(2) . . . . ? N7 Zr4 P7 C159 91.1(2) . . . . ? O8 Zr4 P7 C159 109.1(3) . . . . ? P8 Zr4 P7 C159 68.79(19) . . . . ? N16 Zr4 P8 O8 -86.9(2) . . . . ? N15 Zr4 P8 O8 29.3(2) . . . . ? O7 Zr4 P8 O8 -169.8(3) . . . . ? N8 Zr4 P8 O8 172.6(2) . . . . ? N7 Zr4 P8 O8 140.04(19) . . . . ? P7 Zr4 P8 O8 152.37(17) . . . . ? N16 Zr4 P8 N8 100.5(2) . . . . ? N15 Zr4 P8 N8 -143.3(2) . . . . ? O7 Zr4 P8 N8 17.6(3) . . . . ? N7 Zr4 P8 N8 -32.55(19) . . . . ? O8 Zr4 P8 N8 -172.6(2) . . . . ? P7 Zr4 P8 N8 -20.22(17) . . . . ? N16 Zr4 P8 C17A -171.9(6) . . . . ? N15 Zr4 P8 C17A -55.6(6) . . . . ? O7 Zr4 P8 C17A 105.2(7) . . . . ? N8 Zr4 P8 C17A 87.6(6) . . . . ? N7 Zr4 P8 C17A 55.1(6) . . . . ? O8 Zr4 P8 C17A -84.9(6) . . . . ? P7 Zr4 P8 C17A 67.4(6) . . . . ? N16 Zr4 P8 C165 4.4(2) . . . . ? N15 Zr4 P8 C165 120.7(2) . . . . ? O7 Zr4 P8 C165 -78.5(3) . . . . ? N8 Zr4 P8 C165 -96.1(2) . . . . ? N7 Zr4 P8 C165 -128.62(19) . . . . ? O8 Zr4 P8 C165 91.3(2) . . . . ? P7 Zr4 P8 C165 -116.28(17) . . . . ? N16 Zr4 P8 C171 -178.6(6) . . . . ? N15 Zr4 P8 C171 -62.4(6) . . . . ? O7 Zr4 P8 C171 98.4(6) . . . . ? N8 Zr4 P8 C171 80.8(6) . . . . ? N7 Zr4 P8 C171 48.3(6) . . . . ? O8 Zr4 P8 C171 -91.7(6) . . . . ? P7 Zr4 P8 C171 60.6(6) . . . . ? N1 P1 O1 Zr1 6.88(18) . . . . ? C27 P1 O1 Zr1 -113.57(17) . . . . ? C21 P1 O1 Zr1 125.42(17) . . . . ? N10 Zr1 O1 P1 95.27(17) . . . . ? N9 Zr1 O1 P1 -152.15(18) . . . . ? N1 Zr1 O1 P1 -5.34(14) . . . . ? N2 Zr1 O1 P1 -52.44(19) . . . . ? O2 Zr1 O1 P1 157.9(6) . . . . ? P2 Zr1 O1 P1 -67.2(3) . . . . ? N2 P2 O2 Zr1 8.22(17) . . . . ? C39 P2 O2 Zr1 127.70(16) . . . . ? C33 P2 O2 Zr1 -114.41(16) . . . . ? N10 Zr1 O2 P2 -150.76(17) . . . . ? N9 Zr1 O2 P2 96.47(17) . . . . ? O1 Zr1 O2 P2 145.9(6) . . . . ? N1 Zr1 O2 P2 -52.47(19) . . . . ? N2 Zr1 O2 P2 -6.34(13) . . . . ? P1 Zr1 O2 P2 -63.9(3) . . . . ? N3 P3 O3 Zr2 2.24(16) . . . . ? C71 P3 O3 Zr2 122.69(15) . . . . ? C65 P3 O3 Zr2 -118.32(16) . . . . ? N11 Zr2 O3 P3 99.58(15) . . . . ? N12 Zr2 O3 P3 -154.54(16) . . . . ? N4 Zr2 O3 P3 -55.12(17) . . . . ? N3 Zr2 O3 P3 -1.71(12) . . . . ? O4 Zr2 O3 P3 -172(2) . . . . ? P4 Zr2 O3 P3 -68.9(2) . . . . ? N4 P4 O4 Zr2 13.71(16) . . . . ? C83 P4 O4 Zr2 -106.70(16) . . . . ? C77 P4 O4 Zr2 134.02(15) . . . . ? N11 Zr2 O4 P4 -163.96(16) . . . . ? N12 Zr2 O4 P4 89.89(15) . . . . ? N4 Zr2 O4 P4 -10.78(12) . . . . ? O3 Zr2 O4 P4 108(2) . . . . ? N3 Zr2 O4 P4 -62.79(16) . . . . ? P3 Zr2 O4 P4 -64.1(2) . . . . ? N5 P5 O5 Zr3 7.96(17) . . . . ? C109 P5 O5 Zr3 -114.22(17) . . . . ? C115 P5 O5 Zr3 126.81(18) . . . . ? N13 Zr3 O5 P5 93.50(17) . . . . ? N14 Zr3 O5 P5 -154.37(19) . . . . ? N5 Zr3 O5 P5 -6.20(14) . . . . ? N6 Zr3 O5 P5 -55.94(19) . . . . ? O6 Zr3 O5 P5 127.5(10) . . . . ? P6 Zr3 O5 P5 -62.3(2) . . . . ? N6 P6 O6 Zr3 6.35(17) . . . . ? C127 P6 O6 Zr3 125.03(17) . . . . ? C121 P6 O6 Zr3 -115.41(17) . . . . ? N13 Zr3 O6 P6 -153.78(17) . . . . ? N14 Zr3 O6 P6 94.19(19) . . . . ? N5 Zr3 O6 P6 -56.65(18) . . . . ? N6 Zr3 O6 P6 -4.87(13) . . . . ? O5 Zr3 O6 P6 171.9(10) . . . . ? P5 Zr3 O6 P6 -68.9(2) . . . . ? N7 P7 O7 Zr4 1.96(17) . . . . ? C153 P7 O7 Zr4 -120.74(17) . . . . ? C159 P7 O7 Zr4 121.13(16) . . . . ? N16 Zr4 O7 P7 -142.98(17) . . . . ? N15 Zr4 O7 P7 104.32(17) . . . . ? N8 Zr4 O7 P7 -45.7(2) . . . . ? N7 Zr4 O7 P7 -1.52(13) . . . . ? O8 Zr4 O7 P7 149.9(5) . . . . ? P8 Zr4 O7 P7 -57.7(3) . . . . ? N8 P8 O8 Zr4 5.81(19) . . . . ? C17A P8 O8 Zr4 128.6(5) . . . . ? C165 P8 O8 Zr4 -116.89(18) . . . . ? C171 P8 O8 Zr4 121.7(5) . . . . ? N16 Zr4 O8 P8 95.50(18) . . . . ? N15 Zr4 O8 P8 -152.2(2) . . . . ? O7 Zr4 O8 P8 161.6(5) . . . . ? N8 Zr4 O8 P8 -4.51(15) . . . . ? N7 Zr4 O8 P8 -50.4(2) . . . . ? P7 Zr4 O8 P8 -62.4(3) . . . . ? O1 P1 N1 C2 -168.3(4) . . . . ? C27 P1 N1 C2 -49.2(4) . . . . ? C21 P1 N1 C2 73.6(4) . . . . ? Zr1 P1 N1 C2 -161.5(5) . . . . ? O1 P1 N1 Zr1 -6.80(17) . . . . ? C27 P1 N1 Zr1 112.30(19) . . . . ? C21 P1 N1 Zr1 -124.91(17) . . . . ? N10 Zr1 N1 C2 80.0(3) . . . . ? N9 Zr1 N1 C2 -143.4(3) . . . . ? O1 Zr1 N1 C2 168.3(4) . . . . ? N2 Zr1 N1 C2 -50.3(3) . . . . ? O2 Zr1 N1 C2 -8.6(4) . . . . ? P1 Zr1 N1 C2 163.3(4) . . . . ? P2 Zr1 N1 C2 -33.2(3) . . . . ? N10 Zr1 N1 P1 -83.22(18) . . . . ? N9 Zr1 N1 P1 53.3(2) . . . . ? O1 Zr1 N1 P1 5.04(13) . . . . ? N2 Zr1 N1 P1 146.42(17) . . . . ? O2 Zr1 N1 P1 -171.85(12) . . . . ? P2 Zr1 N1 P1 163.49(12) . . . . ? O2 P2 N2 C12 -169.4(4) . . . . ? C39 P2 N2 C12 70.4(4) . . . . ? C33 P2 N2 C12 -51.2(4) . . . . ? Zr1 P2 N2 C12 -161.2(4) . . . . ? O2 P2 N2 Zr1 -8.17(16) . . . . ? C39 P2 N2 Zr1 -128.41(17) . . . . ? C33 P2 N2 Zr1 109.98(18) . . . . ? N10 Zr1 N2 C12 -140.3(3) . . . . ? N9 Zr1 N2 C12 83.5(3) . . . . ? O1 Zr1 N2 C12 -5.8(4) . . . . ? N1 Zr1 N2 C12 -48.5(3) . . . . ? O2 Zr1 N2 C12 169.2(3) . . . . ? P1 Zr1 N2 C12 -30.5(3) . . . . ? P2 Zr1 N2 C12 163.2(4) . . . . ? N10 Zr1 N2 P2 56.4(2) . . . . ? N9 Zr1 N2 P2 -79.73(16) . . . . ? O1 Zr1 N2 P2 -169.02(12) . . . . ? N1 Zr1 N2 P2 148.23(17) . . . . ? O2 Zr1 N2 P2 5.98(12) . . . . ? P1 Zr1 N2 P2 166.24(11) . . . . ? O3 P3 N3 C46 170.7(3) . . . . ? C71 P3 N3 C46 51.6(4) . . . . ? C65 P3 N3 C46 -72.9(4) . . . . ? Zr2 P3 N3 C46 172.8(4) . . . . ? O3 P3 N3 Zr2 -2.17(15) . . . . ? C71 P3 N3 Zr2 -121.27(17) . . . . ? C65 P3 N3 Zr2 114.30(17) . . . . ? N11 Zr2 N3 C46 97.3(3) . . . . ? N12 Zr2 N3 C46 -127.0(3) . . . . ? N4 Zr2 N3 C46 -38.6(3) . . . . ? O3 Zr2 N3 C46 -171.0(4) . . . . ? O4 Zr2 N3 C46 8.5(4) . . . . ? P4 Zr2 N3 C46 -19.6(3) . . . . ? P3 Zr2 N3 C46 -172.6(4) . . . . ? N11 Zr2 N3 P3 -90.08(16) . . . . ? N12 Zr2 N3 P3 45.7(2) . . . . ? N4 Zr2 N3 P3 133.99(16) . . . . ? O3 Zr2 N3 P3 1.63(12) . . . . ? O4 Zr2 N3 P3 -178.85(11) . . . . ? P4 Zr2 N3 P3 153.00(11) . . . . ? O4 P4 N4 C56 -166.1(4) . . . . ? C83 P4 N4 C56 -47.8(4) . . . . ? C77 P4 N4 C56 72.4(4) . . . . ? Zr2 P4 N4 C56 -151.8(4) . . . . ? O4 P4 N4 Zr2 -14.36(16) . . . . ? C83 P4 N4 Zr2 103.94(18) . . . . ? C77 P4 N4 Zr2 -135.82(15) . . . . ? N11 Zr2 N4 C56 -152.1(3) . . . . ? N12 Zr2 N4 C56 78.6(3) . . . . ? O3 Zr2 N4 C56 -10.8(3) . . . . ? N3 Zr2 N4 C56 -59.7(3) . . . . ? O4 Zr2 N4 C56 166.6(3) . . . . ? P4 Zr2 N4 C56 156.3(4) . . . . ? P3 Zr2 N4 C56 -36.3(3) . . . . ? N11 Zr2 N4 P4 51.6(2) . . . . ? N12 Zr2 N4 P4 -77.67(17) . . . . ? O3 Zr2 N4 P4 -167.09(12) . . . . ? N3 Zr2 N4 P4 144.05(17) . . . . ? O4 Zr2 N4 P4 10.30(12) . . . . ? P3 Zr2 N4 P4 167.41(12) . . . . ? O5 P5 N5 C90 -166.7(4) . . . . ? C109 P5 N5 C90 -48.0(5) . . . . ? C115 P5 N5 C90 73.5(4) . . . . ? Zr3 P5 N5 C90 -158.7(5) . . . . ? O5 P5 N5 Zr3 -8.05(18) . . . . ? C109 P5 N5 Zr3 110.69(18) . . . . ? C115 P5 N5 Zr3 -127.88(17) . . . . ? N13 Zr3 N5 C90 78.8(3) . . . . ? N14 Zr3 N5 C90 -143.0(3) . . . . ? N6 Zr3 N5 C90 -53.9(3) . . . . ? O5 Zr3 N5 C90 168.0(3) . . . . ? O6 Zr3 N5 C90 -7.3(4) . . . . ? P5 Zr3 N5 C90 162.1(4) . . . . ? P6 Zr3 N5 C90 -33.2(3) . . . . ? N13 Zr3 N5 P5 -83.27(18) . . . . ? N14 Zr3 N5 P5 54.9(3) . . . . ? N6 Zr3 N5 P5 143.97(18) . . . . ? O5 Zr3 N5 P5 5.92(13) . . . . ? O6 Zr3 N5 P5 -169.38(13) . . . . ? P6 Zr3 N5 P5 164.67(13) . . . . ? O6 P6 N6 C100 179.2(4) . . . . ? C127 P6 N6 C100 60.4(4) . . . . ? C121 P6 N6 C100 -63.1(4) . . . . ? Zr3 P6 N6 C100 -174.4(5) . . . . ? O6 P6 N6 Zr3 -6.36(17) . . . . ? C127 P6 N6 Zr3 -125.20(18) . . . . ? C121 P6 N6 Zr3 111.26(19) . . . . ? N13 Zr3 N6 C100 -135.5(3) . . . . ? N14 Zr3 N6 C100 89.8(3) . . . . ? N5 Zr3 N6 C100 -45.3(3) . . . . ? O5 Zr3 N6 C100 -0.2(4) . . . . ? O6 Zr3 N6 C100 179.4(4) . . . . ? P5 Zr3 N6 C100 -26.2(3) . . . . ? P6 Zr3 N6 C100 174.8(4) . . . . ? N13 Zr3 N6 P6 49.7(2) . . . . ? N14 Zr3 N6 P6 -85.02(19) . . . . ? N5 Zr3 N6 P6 139.92(18) . . . . ? O5 Zr3 N6 P6 -174.98(12) . . . . ? O6 Zr3 N6 P6 4.65(13) . . . . ? P5 Zr3 N6 P6 158.98(12) . . . . ? O7 P7 N7 C134 -173.0(3) . . . . ? C153 P7 N7 C134 -54.6(4) . . . . ? C159 P7 N7 C134 69.8(4) . . . . ? Zr4 P7 N7 C134 -171.1(4) . . . . ? O7 P7 N7 Zr4 -1.94(17) . . . . ? C153 P7 N7 Zr4 116.51(18) . . . . ? C159 P7 N7 Zr4 -119.13(18) . . . . ? N16 Zr4 N7 C134 -134.5(3) . . . . ? N15 Zr4 N7 C134 89.4(4) . . . . ? O7 Zr4 N7 C134 172.2(4) . . . . ? N8 Zr4 N7 C134 -43.0(3) . . . . ? O8 Zr4 N7 C134 -1.1(4) . . . . ? P7 Zr4 N7 C134 170.8(4) . . . . ? P8 Zr4 N7 C134 -25.2(4) . . . . ? N16 Zr4 N7 P7 54.7(2) . . . . ? N15 Zr4 N7 P7 -81.43(18) . . . . ? O7 Zr4 N7 P7 1.43(12) . . . . ? N8 Zr4 N7 P7 146.23(18) . . . . ? O8 Zr4 N7 P7 -171.90(12) . . . . ? P8 Zr4 N7 P7 163.96(12) . . . . ? O8 P8 N8 C144 -161.0(4) . . . . ? C17A P8 N8 C144 77.4(6) . . . . ? C165 P8 N8 C144 -40.7(5) . . . . ? C171 P8 N8 C144 78.2(6) . . . . ? Zr4 P8 N8 C144 -155.2(5) . . . . ? O8 P8 N8 Zr4 -5.83(19) . . . . ? C17A P8 N8 Zr4 -127.4(5) . . . . ? C165 P8 N8 Zr4 114.46(19) . . . . ? C171 P8 N8 Zr4 -126.7(4) . . . . ? N16 Zr4 N8 C144 74.0(3) . . . . ? N15 Zr4 N8 C144 -150.3(3) . . . . ? O7 Zr4 N8 C144 -14.2(4) . . . . ? N7 Zr4 N8 C144 -54.5(3) . . . . ? O8 Zr4 N8 C144 162.5(4) . . . . ? P7 Zr4 N8 C144 -36.3(3) . . . . ? P8 Zr4 N8 C144 158.2(4) . . . . ? N16 Zr4 N8 P8 -84.21(18) . . . . ? N15 Zr4 N8 P8 51.5(3) . . . . ? O7 Zr4 N8 P8 -172.38(12) . . . . ? N7 Zr4 N8 P8 147.30(18) . . . . ? O8 Zr4 N8 P8 4.24(14) . . . . ? P7 Zr4 N8 P8 165.47(12) . . . . ? N10 Zr1 N9 C178 -26.6(4) . . . . ? O1 Zr1 N9 C178 -117.0(4) . . . . ? N1 Zr1 N9 C178 -159.5(3) . . . . ? N2 Zr1 N9 C178 119.2(4) . . . . ? O2 Zr1 N9 C178 56.2(4) . . . . ? P1 Zr1 N9 C178 -131.8(3) . . . . ? P2 Zr1 N9 C178 86.9(4) . . . . ? N10 Zr1 N9 C177 139.4(4) . . . . ? O1 Zr1 N9 C177 48.9(4) . . . . ? N1 Zr1 N9 C177 6.5(5) . . . . ? N2 Zr1 N9 C177 -74.8(4) . . . . ? O2 Zr1 N9 C177 -137.8(4) . . . . ? P1 Zr1 N9 C177 34.2(4) . . . . ? P2 Zr1 N9 C177 -107.2(4) . . . . ? N9 Zr1 N10 C179 -27.2(4) . . . . ? O1 Zr1 N10 C179 56.1(4) . . . . ? N1 Zr1 N10 C179 120.0(4) . . . . ? N2 Zr1 N10 C179 -159.9(3) . . . . ? O2 Zr1 N10 C179 -116.0(4) . . . . ? P1 Zr1 N10 C179 87.1(4) . . . . ? P2 Zr1 N10 C179 -131.3(4) . . . . ? N9 Zr1 N10 C180 144.7(4) . . . . ? O1 Zr1 N10 C180 -132.0(4) . . . . ? N1 Zr1 N10 C180 -68.1(4) . . . . ? N2 Zr1 N10 C180 12.0(4) . . . . ? O2 Zr1 N10 C180 56.0(4) . . . . ? P1 Zr1 N10 C180 -101.0(4) . . . . ? P2 Zr1 N10 C180 40.6(4) . . . . ? N12 Zr2 N11 C181 125.4(4) . . . . ? N4 Zr2 N11 C181 -2.2(5) . . . . ? O3 Zr2 N11 C181 -148.3(4) . . . . ? N3 Zr2 N11 C181 -83.0(4) . . . . ? O4 Zr2 N11 C181 34.3(4) . . . . ? P4 Zr2 N11 C181 25.4(4) . . . . ? P3 Zr2 N11 C181 -116.8(4) . . . . ? N12 Zr2 N11 C182 -47.8(3) . . . . ? N4 Zr2 N11 C182 -175.5(3) . . . . ? O3 Zr2 N11 C182 38.4(3) . . . . ? N3 Zr2 N11 C182 103.8(3) . . . . ? O4 Zr2 N11 C182 -138.9(3) . . . . ? P4 Zr2 N11 C182 -147.9(3) . . . . ? P3 Zr2 N11 C182 69.9(3) . . . . ? N11 Zr2 N12 C184 141.3(3) . . . . ? N4 Zr2 N12 C184 -71.8(4) . . . . ? O3 Zr2 N12 C184 45.5(3) . . . . ? N3 Zr2 N12 C184 6.4(4) . . . . ? O4 Zr2 N12 C184 -135.3(3) . . . . ? P4 Zr2 N12 C184 -103.9(3) . . . . ? P3 Zr2 N12 C184 31.4(4) . . . . ? N11 Zr2 N12 C183 -25.5(4) . . . . ? N4 Zr2 N12 C183 121.3(3) . . . . ? O3 Zr2 N12 C183 -121.4(3) . . . . ? N3 Zr2 N12 C183 -160.4(3) . . . . ? O4 Zr2 N12 C183 57.8(3) . . . . ? P4 Zr2 N12 C183 89.2(3) . . . . ? P3 Zr2 N12 C183 -135.4(3) . . . . ? N14 Zr3 N13 C185 137.1(3) . . . . ? N5 Zr3 N13 C185 -73.0(3) . . . . ? N6 Zr3 N13 C185 6.3(4) . . . . ? O5 Zr3 N13 C185 -137.1(3) . . . . ? O6 Zr3 N13 C185 46.1(3) . . . . ? P5 Zr3 N13 C185 -105.8(3) . . . . ? P6 Zr3 N13 C185 32.1(4) . . . . ? N14 Zr3 N13 C186 -37.5(4) . . . . ? N5 Zr3 N13 C186 112.4(3) . . . . ? N6 Zr3 N13 C186 -168.2(3) . . . . ? O5 Zr3 N13 C186 48.4(3) . . . . ? O6 Zr3 N13 C186 -128.4(3) . . . . ? P5 Zr3 N13 C186 79.7(3) . . . . ? P6 Zr3 N13 C186 -142.4(3) . . . . ? N13 Zr3 N14 C188 152.2(4) . . . . ? N5 Zr3 N14 C188 17.4(5) . . . . ? N6 Zr3 N14 C188 -61.5(4) . . . . ? O5 Zr3 N14 C188 60.3(4) . . . . ? O6 Zr3 N14 C188 -125.3(4) . . . . ? P5 Zr3 N14 C188 46.2(4) . . . . ? P6 Zr3 N14 C188 -94.2(4) . . . . ? N13 Zr3 N14 C187 -20.0(5) . . . . ? N5 Zr3 N14 C187 -154.8(4) . . . . ? N6 Zr3 N14 C187 126.3(4) . . . . ? O5 Zr3 N14 C187 -112.0(4) . . . . ? O6 Zr3 N14 C187 62.5(4) . . . . ? P5 Zr3 N14 C187 -126.1(4) . . . . ? P6 Zr3 N14 C187 93.5(4) . . . . ? N16 Zr4 N15 C190 -44.9(4) . . . . ? O7 Zr4 N15 C190 36.8(4) . . . . ? N8 Zr4 N15 C190 -176.9(3) . . . . ? N7 Zr4 N15 C190 99.8(4) . . . . ? O8 Zr4 N15 C190 -135.0(4) . . . . ? P7 Zr4 N15 C190 66.8(4) . . . . ? P8 Zr4 N15 C190 -149.8(3) . . . . ? N16 Zr4 N15 C189 131.7(4) . . . . ? O7 Zr4 N15 C189 -146.6(4) . . . . ? N8 Zr4 N15 C189 -0.3(5) . . . . ? N7 Zr4 N15 C189 -83.6(4) . . . . ? O8 Zr4 N15 C189 41.6(4) . . . . ? P7 Zr4 N15 C189 -116.6(4) . . . . ? P8 Zr4 N15 C189 26.8(4) . . . . ? N15 Zr4 N16 C191 -30.2(4) . . . . ? O7 Zr4 N16 C191 -117.0(4) . . . . ? N8 Zr4 N16 C191 116.8(4) . . . . ? N7 Zr4 N16 C191 -163.6(4) . . . . ? O8 Zr4 N16 C191 52.5(4) . . . . ? P7 Zr4 N16 C191 -135.8(4) . . . . ? P8 Zr4 N16 C191 83.6(4) . . . . ? N15 Zr4 N16 C192 132.7(5) . . . . ? O7 Zr4 N16 C192 45.9(5) . . . . ? N8 Zr4 N16 C192 -80.3(5) . . . . ? N7 Zr4 N16 C192 -0.7(5) . . . . ? O8 Zr4 N16 C192 -144.6(5) . . . . ? P7 Zr4 N16 C192 27.1(5) . . . . ? P8 Zr4 N16 C192 -113.5(5) . . . . ? C6 C1 C2 N1 -171.9(3) . . . . ? C11 C1 C2 N1 5.1(6) . . . . ? C6 C1 C2 C3 3.4(6) . . . . ? C11 C1 C2 C3 -179.6(3) . . . . ? P1 N1 C2 C1 -122.0(4) . . . . ? Zr1 N1 C2 C1 81.3(4) . . . . ? P1 N1 C2 C3 62.8(5) . . . . ? Zr1 N1 C2 C3 -93.9(4) . . . . ? C1 C2 C3 C4 -1.5(6) . . . . ? N1 C2 C3 C4 173.8(4) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 C10 -178.2(4) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C10 C5 C6 C7 3.0(6) . . . . ? C4 C5 C6 C7 -175.7(4) . . . . ? C10 C5 C6 C1 -179.8(4) . . . . ? C4 C5 C6 C1 1.4(6) . . . . ? C2 C1 C6 C7 173.7(4) . . . . ? C11 C1 C6 C7 -3.4(5) . . . . ? C2 C1 C6 C5 -3.4(6) . . . . ? C11 C1 C6 C5 179.6(3) . . . . ? C5 C6 C7 C8 -3.3(6) . . . . ? C1 C6 C7 C8 179.6(3) . . . . ? C6 C7 C8 C9 1.4(6) . . . . ? C7 C8 C9 C10 0.9(6) . . . . ? C8 C9 C10 C5 -1.2(7) . . . . ? C4 C5 C10 C9 177.9(4) . . . . ? C6 C5 C10 C9 -0.8(6) . . . . ? C2 C1 C11 C12 -62.5(5) . . . . ? C6 C1 C11 C12 114.5(4) . . . . ? C2 C1 C11 C16 115.3(4) . . . . ? C6 C1 C11 C16 -67.7(5) . . . . ? C16 C11 C12 N2 -170.9(3) . . . . ? C1 C11 C12 N2 6.9(5) . . . . ? C16 C11 C12 C13 3.4(6) . . . . ? C1 C11 C12 C13 -178.8(4) . . . . ? P2 N2 C12 C11 -125.2(4) . . . . ? Zr1 N2 C12 C11 78.3(4) . . . . ? P2 N2 C12 C13 60.4(5) . . . . ? Zr1 N2 C12 C13 -96.1(4) . . . . ? C11 C12 C13 C14 0.3(7) . . . . ? N2 C12 C13 C14 174.8(4) . . . . ? C12 C13 C14 C15 -3.4(7) . . . . ? C13 C14 C15 C20 -175.6(5) . . . . ? C13 C14 C15 C16 2.7(7) . . . . ? C12 C11 C16 C17 172.9(4) . . . . ? C1 C11 C16 C17 -4.9(6) . . . . ? C12 C11 C16 C15 -4.1(6) . . . . ? C1 C11 C16 C15 178.1(4) . . . . ? C20 C15 C16 C17 2.2(6) . . . . ? C14 C15 C16 C17 -176.1(4) . . . . ? C20 C15 C16 C11 179.4(4) . . . . ? C14 C15 C16 C11 1.1(6) . . . . ? C11 C16 C17 C18 -179.1(4) . . . . ? C15 C16 C17 C18 -2.0(6) . . . . ? C16 C17 C18 C19 0.7(6) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C18 C19 C20 C15 -0.3(7) . . . . ? C14 C15 C20 C19 177.1(4) . . . . ? C16 C15 C20 C19 -1.1(7) . . . . ? O1 P1 C21 C26 -73.4(4) . . . . ? N1 P1 C21 C26 37.4(4) . . . . ? C27 P1 C21 C26 163.4(3) . . . . ? Zr1 P1 C21 C26 -18.7(4) . . . . ? O1 P1 C21 C22 102.1(4) . . . . ? N1 P1 C21 C22 -147.2(4) . . . . ? C27 P1 C21 C22 -21.2(4) . . . . ? Zr1 P1 C21 C22 156.7(3) . . . . ? C26 C21 C22 C23 -1.2(7) . . . . ? P1 C21 C22 C23 -176.6(4) . . . . ? C21 C22 C23 C24 1.4(7) . . . . ? C22 C23 C24 C25 -1.8(7) . . . . ? C23 C24 C25 C26 2.1(7) . . . . ? C22 C21 C26 C25 1.6(7) . . . . ? P1 C21 C26 C25 177.2(3) . . . . ? C24 C25 C26 C21 -2.0(7) . . . . ? O1 P1 C27 C28 14.6(4) . . . . ? N1 P1 C27 C28 -97.3(4) . . . . ? C21 P1 C27 C28 137.6(3) . . . . ? Zr1 P1 C27 C28 -40.5(4) . . . . ? O1 P1 C27 C32 -172.2(4) . . . . ? N1 P1 C27 C32 75.9(4) . . . . ? C21 P1 C27 C32 -49.2(4) . . . . ? Zr1 P1 C27 C32 132.7(3) . . . . ? C32 C27 C28 C29 -1.3(7) . . . . ? P1 C27 C28 C29 172.2(4) . . . . ? C27 C28 C29 C30 0.6(7) . . . . ? C28 C29 C30 C31 0.7(8) . . . . ? C29 C30 C31 C32 -1.3(8) . . . . ? C28 C27 C32 C31 0.6(7) . . . . ? P1 C27 C32 C31 -172.6(4) . . . . ? C30 C31 C32 C27 0.6(8) . . . . ? O2 P2 C33 C38 -166.5(3) . . . . ? N2 P2 C33 C38 80.7(4) . . . . ? C39 P2 C33 C38 -44.2(4) . . . . ? Zr1 P2 C33 C38 138.7(3) . . . . ? O2 P2 C33 C34 15.5(4) . . . . ? N2 P2 C33 C34 -97.3(3) . . . . ? C39 P2 C33 C34 137.8(3) . . . . ? Zr1 P2 C33 C34 -39.3(4) . . . . ? C38 C33 C34 C35 1.4(6) . . . . ? P2 C33 C34 C35 179.6(3) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C34 C35 C36 C37 -0.3(6) . . . . ? C35 C36 C37 C38 -0.1(6) . . . . ? C36 C37 C38 C33 1.2(6) . . . . ? C34 C33 C38 C37 -1.9(6) . . . . ? P2 C33 C38 C37 -179.9(3) . . . . ? O2 P2 C39 C44 -83.1(4) . . . . ? N2 P2 C39 C44 29.3(4) . . . . ? C33 P2 C39 C44 156.6(3) . . . . ? Zr1 P2 C39 C44 -26.7(4) . . . . ? O2 P2 C39 C40 95.6(4) . . . . ? N2 P2 C39 C40 -151.9(3) . . . . ? C33 P2 C39 C40 -24.6(4) . . . . ? Zr1 P2 C39 C40 152.1(3) . . . . ? C44 C39 C40 C41 -3.0(6) . . . . ? P2 C39 C40 C41 178.3(3) . . . . ? C39 C40 C41 C42 1.9(7) . . . . ? C40 C41 C42 C43 0.5(7) . . . . ? C41 C42 C43 C44 -1.8(7) . . . . ? C42 C43 C44 C39 0.7(7) . . . . ? C40 C39 C44 C43 1.7(7) . . . . ? P2 C39 C44 C43 -179.5(4) . . . . ? C50 C45 C46 N3 -170.1(4) . . . . ? C55 C45 C46 N3 9.5(6) . . . . ? C50 C45 C46 C47 4.3(6) . . . . ? C55 C45 C46 C47 -176.1(4) . . . . ? P3 N3 C46 C45 -101.0(4) . . . . ? Zr2 N3 C46 C45 69.3(5) . . . . ? P3 N3 C46 C47 84.5(5) . . . . ? Zr2 N3 C46 C47 -105.3(4) . . . . ? C45 C46 C47 C48 -1.3(6) . . . . ? N3 C46 C47 C48 173.4(4) . . . . ? C46 C47 C48 C49 -2.3(7) . . . . ? C47 C48 C49 C50 2.7(6) . . . . ? C47 C48 C49 C54 -174.3(4) . . . . ? C48 C49 C50 C45 0.4(6) . . . . ? C54 C49 C50 C45 177.5(4) . . . . ? C48 C49 C50 C51 -176.9(4) . . . . ? C54 C49 C50 C51 0.2(6) . . . . ? C46 C45 C50 C49 -3.9(6) . . . . ? C55 C45 C50 C49 176.5(4) . . . . ? C46 C45 C50 C51 173.2(4) . . . . ? C55 C45 C50 C51 -6.3(6) . . . . ? C49 C50 C51 C52 -0.2(6) . . . . ? C45 C50 C51 C52 -177.4(4) . . . . ? C50 C51 C52 C53 0.0(7) . . . . ? C51 C52 C53 C54 0.4(7) . . . . ? C52 C53 C54 C49 -0.4(7) . . . . ? C48 C49 C54 C53 177.1(4) . . . . ? C50 C49 C54 C53 0.1(7) . . . . ? C46 C45 C55 C56 -59.9(5) . . . . ? C50 C45 C55 C56 119.7(4) . . . . ? C46 C45 C55 C60 118.7(4) . . . . ? C50 C45 C55 C60 -61.7(5) . . . . ? C60 C55 C56 C57 -3.4(6) . . . . ? C45 C55 C56 C57 175.3(3) . . . . ? C60 C55 C56 N4 -177.1(3) . . . . ? C45 C55 C56 N4 1.5(5) . . . . ? P4 N4 C56 C55 -123.0(4) . . . . ? Zr2 N4 C56 C55 90.7(4) . . . . ? P4 N4 C56 C57 63.2(5) . . . . ? Zr2 N4 C56 C57 -83.1(4) . . . . ? C55 C56 C57 C58 5.7(6) . . . . ? N4 C56 C57 C58 179.5(4) . . . . ? C56 C57 C58 C59 -3.1(6) . . . . ? C57 C58 C59 C60 -1.6(6) . . . . ? C57 C58 C59 C64 177.5(4) . . . . ? C58 C59 C60 C55 3.8(6) . . . . ? C64 C59 C60 C55 -175.3(4) . . . . ? C58 C59 C60 C61 -177.3(4) . . . . ? C64 C59 C60 C61 3.6(6) . . . . ? C56 C55 C60 C59 -1.3(6) . . . . ? C45 C55 C60 C59 -180.0(4) . . . . ? C56 C55 C60 C61 179.8(4) . . . . ? C45 C55 C60 C61 1.2(6) . . . . ? C59 C60 C61 C62 -2.9(6) . . . . ? C55 C60 C61 C62 176.0(4) . . . . ? C60 C61 C62 C63 0.0(6) . . . . ? C61 C62 C63 C64 2.2(7) . . . . ? C62 C63 C64 C59 -1.5(7) . . . . ? C58 C59 C64 C63 179.4(4) . . . . ? C60 C59 C64 C63 -1.5(6) . . . . ? O3 P3 C65 C66 -104.7(4) . . . . ? N3 P3 C65 C66 143.8(3) . . . . ? C71 P3 C65 C66 16.5(4) . . . . ? Zr2 P3 C65 C66 -157.5(3) . . . . ? O3 P3 C65 C70 68.8(4) . . . . ? N3 P3 C65 C70 -42.7(4) . . . . ? C71 P3 C65 C70 -170.0(3) . . . . ? Zr2 P3 C65 C70 15.9(4) . . . . ? C70 C65 C66 C67 -0.9(6) . . . . ? P3 C65 C66 C67 172.4(3) . . . . ? C65 C66 C67 C68 0.3(7) . . . . ? C66 C67 C68 C69 0.0(7) . . . . ? C67 C68 C69 C70 0.4(7) . . . . ? C68 C69 C70 C65 -1.0(7) . . . . ? C66 C65 C70 C69 1.2(6) . . . . ? P3 C65 C70 C69 -172.5(3) . . . . ? O3 P3 C71 C72 -2.1(4) . . . . ? N3 P3 C71 C72 110.4(3) . . . . ? C65 P3 C71 C72 -121.7(3) . . . . ? Zr2 P3 C71 C72 52.0(4) . . . . ? O3 P3 C71 C76 -177.2(3) . . . . ? N3 P3 C71 C76 -64.7(4) . . . . ? C65 P3 C71 C76 63.2(4) . . . . ? Zr2 P3 C71 C76 -123.1(3) . . . . ? C76 C71 C72 C73 0.5(6) . . . . ? P3 C71 C72 C73 -174.7(4) . . . . ? C71 C72 C73 C74 -0.5(7) . . . . ? C72 C73 C74 C75 0.1(7) . . . . ? C73 C74 C75 C76 0.3(7) . . . . ? C74 C75 C76 C71 -0.3(6) . . . . ? C72 C71 C76 C75 -0.1(6) . . . . ? P3 C71 C76 C75 175.0(3) . . . . ? O4 P4 C77 C82 99.9(4) . . . . ? N4 P4 C77 C82 -147.0(3) . . . . ? C83 P4 C77 C82 -22.2(4) . . . . ? Zr2 P4 C77 C82 159.8(3) . . . . ? O4 P4 C77 C78 -80.7(4) . . . . ? N4 P4 C77 C78 32.5(4) . . . . ? C83 P4 C77 C78 157.2(3) . . . . ? Zr2 P4 C77 C78 -20.8(4) . . . . ? C82 C77 C78 C79 1.4(6) . . . . ? P4 C77 C78 C79 -178.1(3) . . . . ? C77 C78 C79 C80 -1.7(7) . . . . ? C78 C79 C80 C81 0.9(7) . . . . ? C79 C80 C81 C82 0.1(7) . . . . ? C80 C81 C82 C77 -0.4(7) . . . . ? C78 C77 C82 C81 -0.4(6) . . . . ? P4 C77 C82 C81 179.1(3) . . . . ? O4 P4 C83 C84 1.0(4) . . . . ? N4 P4 C83 C84 -111.0(4) . . . . ? C77 P4 C83 C84 125.1(4) . . . . ? Zr2 P4 C83 C84 -56.3(4) . . . . ? O4 P4 C83 C88 174.3(3) . . . . ? N4 P4 C83 C88 62.3(4) . . . . ? C77 P4 C83 C88 -61.6(4) . . . . ? Zr2 P4 C83 C88 117.0(3) . . . . ? C88 C83 C84 C85 -0.2(7) . . . . ? P4 C83 C84 C85 173.1(4) . . . . ? C83 C84 C85 C86 -2.6(9) . . . . ? C84 C85 C86 C87 2.8(9) . . . . ? C85 C86 C87 C88 -0.2(8) . . . . ? C86 C87 C88 C83 -2.6(7) . . . . ? C84 C83 C88 C87 2.8(7) . . . . ? P4 C83 C88 C87 -170.5(4) . . . . ? C94 C89 C90 N5 -174.2(4) . . . . ? C99 C89 C90 N5 1.9(6) . . . . ? C94 C89 C90 C91 0.5(6) . . . . ? C99 C89 C90 C91 176.6(4) . . . . ? P5 N5 C90 C89 -119.3(4) . . . . ? Zr3 N5 C90 C89 86.5(4) . . . . ? P5 N5 C90 C91 65.9(6) . . . . ? Zr3 N5 C90 C91 -88.3(4) . . . . ? C89 C90 C91 C92 -1.2(6) . . . . ? N5 C90 C91 C92 173.6(4) . . . . ? C90 C91 C92 C93 1.0(7) . . . . ? C91 C92 C93 C98 -179.3(4) . . . . ? C91 C92 C93 C94 -0.3(6) . . . . ? C92 C93 C94 C95 -179.8(4) . . . . ? C98 C93 C94 C95 -0.8(6) . . . . ? C92 C93 C94 C89 -0.3(6) . . . . ? C98 C93 C94 C89 178.7(4) . . . . ? C90 C89 C94 C95 179.7(4) . . . . ? C99 C89 C94 C95 3.6(6) . . . . ? C90 C89 C94 C93 0.2(6) . . . . ? C99 C89 C94 C93 -175.9(4) . . . . ? C93 C94 C95 C96 -0.4(6) . . . . ? C89 C94 C95 C96 -179.8(4) . . . . ? C94 C95 C96 C97 1.2(7) . . . . ? C95 C96 C97 C98 -0.8(7) . . . . ? C96 C97 C98 C93 -0.4(7) . . . . ? C92 C93 C98 C97 -179.8(4) . . . . ? C94 C93 C98 C97 1.2(7) . . . . ? C90 C89 C99 C100 -60.6(5) . . . . ? C94 C89 C99 C100 115.5(4) . . . . ? C90 C89 C99 C104 115.2(5) . . . . ? C94 C89 C99 C104 -68.7(5) . . . . ? C104 C99 C100 N6 -168.4(4) . . . . ? C89 C99 C100 N6 7.5(6) . . . . ? C104 C99 C100 C101 5.6(6) . . . . ? C89 C99 C100 C101 -178.5(4) . . . . ? P6 N6 C100 C99 -111.5(4) . . . . ? Zr3 N6 C100 C99 75.7(5) . . . . ? P6 N6 C100 C101 74.5(5) . . . . ? Zr3 N6 C100 C101 -98.3(4) . . . . ? C99 C100 C101 C102 -3.4(6) . . . . ? N6 C100 C101 C102 170.7(4) . . . . ? C100 C101 C102 C103 -1.3(7) . . . . ? C101 C102 C103 C108 -173.1(4) . . . . ? C101 C102 C103 C104 3.7(6) . . . . ? C100 C99 C104 C105 172.4(4) . . . . ? C89 C99 C104 C105 -3.4(6) . . . . ? C100 C99 C104 C103 -3.2(6) . . . . ? C89 C99 C104 C103 -179.0(4) . . . . ? C102 C103 C104 C105 -177.2(4) . . . . ? C108 C103 C104 C105 -0.3(6) . . . . ? C102 C103 C104 C99 -1.4(6) . . . . ? C108 C103 C104 C99 175.5(4) . . . . ? C99 C104 C105 C106 -176.2(4) . . . . ? C103 C104 C105 C106 -0.5(6) . . . . ? C104 C105 C106 C107 2.5(7) . . . . ? C105 C106 C107 C108 -3.7(7) . . . . ? C106 C107 C108 C103 3.0(7) . . . . ? C102 C103 C108 C107 175.8(4) . . . . ? C104 C103 C108 C107 -1.1(7) . . . . ? O5 P5 C109 C114 -1.3(4) . . . . ? N5 P5 C109 C114 -114.0(4) . . . . ? C115 P5 C109 C114 121.7(3) . . . . ? Zr3 P5 C109 C114 -57.0(4) . . . . ? O5 P5 C109 C110 177.8(4) . . . . ? N5 P5 C109 C110 65.2(4) . . . . ? C115 P5 C109 C110 -59.1(4) . . . . ? Zr3 P5 C109 C110 122.1(3) . . . . ? C114 C109 C110 C111 -0.9(7) . . . . ? P5 C109 C110 C111 179.9(4) . . . . ? C109 C110 C111 C112 0.0(7) . . . . ? C110 C111 C112 C113 0.3(7) . . . . ? C111 C112 C113 C114 0.2(7) . . . . ? C110 C109 C114 C113 1.5(6) . . . . ? P5 C109 C114 C113 -179.3(3) . . . . ? C112 C113 C114 C109 -1.2(7) . . . . ? O5 P5 C115 C116 109.9(4) . . . . ? N5 P5 C115 C116 -138.2(4) . . . . ? C109 P5 C115 C116 -11.6(4) . . . . ? Zr3 P5 C115 C116 166.9(3) . . . . ? O5 P5 C115 C120 -68.8(4) . . . . ? N5 P5 C115 C120 43.1(4) . . . . ? C109 P5 C115 C120 169.7(3) . . . . ? Zr3 P5 C115 C120 -11.8(4) . . . . ? C120 C115 C116 C117 -1.9(6) . . . . ? P5 C115 C116 C117 179.4(4) . . . . ? C115 C116 C117 C118 0.4(7) . . . . ? C116 C117 C118 C119 1.4(7) . . . . ? C117 C118 C119 C120 -1.6(7) . . . . ? C118 C119 C120 C115 0.0(7) . . . . ? C116 C115 C120 C119 1.8(7) . . . . ? P5 C115 C120 C119 -179.4(4) . . . . ? O6 P6 C121 C122 -155.0(4) . . . . ? N6 P6 C121 C122 92.2(5) . . . . ? C127 P6 C121 C122 -33.2(5) . . . . ? Zr3 P6 C121 C122 149.9(4) . . . . ? O6 P6 C121 C126 28.0(5) . . . . ? N6 P6 C121 C126 -84.7(5) . . . . ? C127 P6 C121 C126 149.9(4) . . . . ? Zr3 P6 C121 C126 -27.1(5) . . . . ? C126 C121 C122 C123 2.1(8) . . . . ? P6 C121 C122 C123 -174.8(4) . . . . ? C121 C122 C123 C124 0.6(8) . . . . ? C122 C123 C124 C125 -4.3(9) . . . . ? C123 C124 C125 C126 5.2(10) . . . . ? C122 C121 C126 C125 -1.2(9) . . . . ? P6 C121 C126 C125 175.9(5) . . . . ? C124 C125 C126 C121 -2.4(11) . . . . ? O6 P6 C127 C128 13.4(4) . . . . ? N6 P6 C127 C128 125.5(3) . . . . ? C121 P6 C127 C128 -107.0(4) . . . . ? Zr3 P6 C127 C128 69.6(4) . . . . ? O6 P6 C127 C132 -163.5(4) . . . . ? N6 P6 C127 C132 -51.4(4) . . . . ? C121 P6 C127 C132 76.1(4) . . . . ? Zr3 P6 C127 C132 -107.3(4) . . . . ? C132 C127 C128 C129 0.0(6) . . . . ? P6 C127 C128 C129 -177.0(3) . . . . ? C127 C128 C129 C130 -0.1(7) . . . . ? C128 C129 C130 C131 -0.1(7) . . . . ? C129 C130 C131 C132 0.4(8) . . . . ? C130 C131 C132 C127 -0.6(7) . . . . ? C128 C127 C132 C131 0.3(7) . . . . ? P6 C127 C132 C131 177.2(4) . . . . ? C138 C133 C134 C135 2.7(6) . . . . ? C143 C133 C134 C135 -176.2(4) . . . . ? C138 C133 C134 N7 -170.7(4) . . . . ? C143 C133 C134 N7 10.4(6) . . . . ? P7 N7 C134 C133 -121.0(4) . . . . ? Zr4 N7 C134 C133 71.1(5) . . . . ? P7 N7 C134 C135 65.6(5) . . . . ? Zr4 N7 C134 C135 -102.3(4) . . . . ? C133 C134 C135 C136 1.1(7) . . . . ? N7 C134 C135 C136 174.5(4) . . . . ? C134 C135 C136 C137 -3.9(7) . . . . ? C135 C136 C137 C138 2.9(7) . . . . ? C135 C136 C137 C142 -176.2(5) . . . . ? C136 C137 C138 C139 -178.6(4) . . . . ? C142 C137 C138 C139 0.5(6) . . . . ? C136 C137 C138 C133 0.9(6) . . . . ? C142 C137 C138 C133 180.0(4) . . . . ? C134 C133 C138 C139 175.8(4) . . . . ? C143 C133 C138 C139 -5.3(6) . . . . ? C134 C133 C138 C137 -3.6(6) . . . . ? C143 C133 C138 C137 175.3(4) . . . . ? C137 C138 C139 C140 -0.5(6) . . . . ? C133 C138 C139 C140 -179.9(4) . . . . ? C138 C139 C140 C141 -0.2(7) . . . . ? C139 C140 C141 C142 0.9(7) . . . . ? C140 C141 C142 C137 -0.9(8) . . . . ? C136 C137 C142 C141 179.2(5) . . . . ? C138 C137 C142 C141 0.2(7) . . . . ? C134 C133 C143 C144 -64.1(6) . . . . ? C138 C133 C143 C144 117.1(5) . . . . ? C134 C133 C143 C148 115.2(5) . . . . ? C138 C133 C143 C148 -63.7(5) . . . . ? C148 C143 C144 N8 -172.5(4) . . . . ? C133 C143 C144 N8 6.7(6) . . . . ? C148 C143 C144 C145 1.4(6) . . . . ? C133 C143 C144 C145 -179.4(4) . . . . ? P8 N8 C144 C143 -128.8(4) . . . . ? Zr4 N8 C144 C143 81.8(5) . . . . ? P8 N8 C144 C145 57.2(6) . . . . ? Zr4 N8 C144 C145 -92.1(4) . . . . ? C143 C144 C145 C146 1.3(6) . . . . ? N8 C144 C145 C146 175.3(4) . . . . ? C144 C145 C146 C147 -1.8(6) . . . . ? C145 C146 C147 C148 -0.4(6) . . . . ? C145 C146 C147 C152 -177.6(4) . . . . ? C152 C147 C148 C149 2.1(6) . . . . ? C146 C147 C148 C149 -175.1(4) . . . . ? C152 C147 C148 C143 -179.6(4) . . . . ? C146 C147 C148 C143 3.1(6) . . . . ? C144 C143 C148 C147 -3.6(6) . . . . ? C133 C143 C148 C147 177.1(4) . . . . ? C144 C143 C148 C149 174.5(4) . . . . ? C133 C143 C148 C149 -4.7(6) . . . . ? C147 C148 C149 C150 -1.4(6) . . . . ? C143 C148 C149 C150 -179.6(4) . . . . ? C148 C149 C150 C151 -0.1(6) . . . . ? C149 C150 C151 C152 0.9(6) . . . . ? C150 C151 C152 C147 -0.1(6) . . . . ? C148 C147 C152 C151 -1.5(6) . . . . ? C146 C147 C152 C151 175.7(4) . . . . ? O7 P7 C153 C158 -120.7(4) . . . . ? N7 P7 C153 C158 126.4(4) . . . . ? C159 P7 C153 C158 -0.7(5) . . . . ? Zr4 P7 C153 C158 -174.8(3) . . . . ? O7 P7 C153 C154 54.1(4) . . . . ? N7 P7 C153 C154 -58.8(4) . . . . ? C159 P7 C153 C154 174.0(4) . . . . ? Zr4 P7 C153 C154 0.0(4) . . . . ? C158 C153 C154 C155 1.6(7) . . . . ? P7 C153 C154 C155 -173.3(4) . . . . ? C153 C154 C155 C156 -1.1(8) . . . . ? C154 C155 C156 C157 0.0(8) . . . . ? C155 C156 C157 C158 0.5(8) . . . . ? C154 C153 C158 C157 -1.1(8) . . . . ? P7 C153 C158 C157 173.6(4) . . . . ? C156 C157 C158 C153 0.0(9) . . . . ? O7 P7 C159 C164 21.2(4) . . . . ? N7 P7 C159 C164 132.4(4) . . . . ? C153 P7 C159 C164 -98.6(4) . . . . ? Zr4 P7 C159 C164 75.4(4) . . . . ? O7 P7 C159 C160 -155.4(3) . . . . ? N7 P7 C159 C160 -44.3(4) . . . . ? C153 P7 C159 C160 84.7(4) . . . . ? Zr4 P7 C159 C160 -101.3(4) . . . . ? C164 C159 C160 C161 -0.8(7) . . . . ? P7 C159 C160 C161 175.9(4) . . . . ? C159 C160 C161 C162 1.2(7) . . . . ? C160 C161 C162 C163 -0.4(7) . . . . ? C161 C162 C163 C164 -0.8(7) . . . . ? C160 C159 C164 C163 -0.4(7) . . . . ? P7 C159 C164 C163 -177.1(4) . . . . ? C162 C163 C164 C159 1.2(7) . . . . ? O8 P8 C165 C166 20.1(4) . . . . ? N8 P8 C165 C166 -94.0(4) . . . . ? C17A P8 C165 C166 141.1(6) . . . . ? C171 P8 C165 C166 146.3(6) . . . . ? Zr4 P8 C165 C166 -36.2(4) . . . . ? O8 P8 C165 C170 -163.2(3) . . . . ? N8 P8 C165 C170 82.7(4) . . . . ? C17A P8 C165 C170 -42.3(6) . . . . ? C171 P8 C165 C170 -37.0(6) . . . . ? Zr4 P8 C165 C170 140.5(3) . . . . ? C170 C165 C166 C167 0.4(7) . . . . ? P8 C165 C166 C167 177.1(4) . . . . ? C165 C166 C167 C168 -1.6(8) . . . . ? C166 C167 C168 C169 1.5(8) . . . . ? C167 C168 C169 C170 -0.3(7) . . . . ? C168 C169 C170 C165 -0.8(7) . . . . ? C166 C165 C170 C169 0.8(7) . . . . ? P8 C165 C170 C169 -176.0(3) . . . . ? O8 P8 C171 C172 90.9(10) . . . . ? N8 P8 C171 C172 -157.6(9) . . . . ? C17A P8 C171 C172 17(6) . . . . ? C165 P8 C171 C172 -33.4(10) . . . . ? Zr4 P8 C171 C172 149.3(9) . . . . ? O8 P8 C171 C176 -90.3(11) . . . . ? N8 P8 C171 C176 21.2(10) . . . . ? C17A P8 C171 C176 -165(7) . . . . ? C165 P8 C171 C176 145.4(9) . . . . ? Zr4 P8 C171 C176 -31.9(12) . . . . ? C176 C171 C172 C173 0.0 . . . . ? P8 C171 C172 C173 178.8(9) . . . . ? C171 C172 C173 C174 0.0 . . . . ? C172 C173 C174 C175 0.0 . . . . ? C173 C174 C175 C176 0.0 . . . . ? C174 C175 C176 C171 0.0 . . . . ? C172 C171 C176 C175 0.0 . . . . ? P8 C171 C176 C175 -178.8(9) . . . . ? O8 P8 C17A C17B 66.3(9) . . . . ? N8 P8 C17A C17B -179.0(7) . . . . ? C165 P8 C17A C17B -53.8(9) . . . . ? C171 P8 C17A C17B 175(7) . . . . ? Zr4 P8 C17A C17B 123.1(8) . . . . ? O8 P8 C17A C17F -119.7(8) . . . . ? N8 P8 C17A C17F -5.1(9) . . . . ? C165 P8 C17A C17F 120.2(7) . . . . ? C171 P8 C17A C17F -11(6) . . . . ? Zr4 P8 C17A C17F -63.0(10) . . . . ? C17F C17A C17B C17C 0.0 . . . . ? P8 C17A C17B C17C 173.9(10) . . . . ? C17A C17B C17C C17D 0.0 . . . . ? C17B C17C C17D C17E 0.0 . . . . ? C17C C17D C17E C17F 0.0 . . . . ? C17D C17E C17F C17A 0.0 . . . . ? C17B C17A C17F C17E 0.0 . . . . ? P8 C17A C17F C17E -174.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.493 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.079 # Attachment 'compound_11.cif' data_compound11 _database_code_depnum_ccdc_archive 'CCDC 742598' #TrackingRef 'compound_11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 N6 Ti' _chemical_formula_sum 'C34 H40 N6 Ti' _chemical_formula_weight 580.62 _chemical_absolute_configuration rmad 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' '-x, y, -z' 'x, -y, -z+1/2' 'y, x, -z+1/4' '-y, -x, -z+3/4' _cell_length_a 9.4541(13) _cell_length_b 9.4541(13) _cell_length_c 34.487(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3082.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5858 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9462 _exptl_absorpt_correction_T_max 0.9756 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23249 _diffrn_reflns_av_R_equivalents 0.1604 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2722 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.1002P)^2^+0.2966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 2722 _refine_ls_number_parameters 195 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1649 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.105 _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 Ti1 Ti 0.64541(6) 0.64541(6) 0.1250 0.0274(3) Uani 1 2 d S . . N1 N 0.4187(3) 0.5976(3) 0.10659(7) 0.0259(6) Uani 1 1 d . . . N2 N 0.5112(3) 0.7678(3) 0.16202(7) 0.0297(6) Uani 1 1 d . . . N3 N 0.6733(3) 0.7913(3) 0.08779(8) 0.0364(7) Uani 1 1 d . . . C1 C 0.3448(3) 0.3498(3) 0.10302(8) 0.0250(7) Uani 1 1 d . . . C2 C 0.3755(3) 0.4775(3) 0.08430(8) 0.0253(6) Uani 1 1 d . . . C3 C 0.3704(3) 0.4868(3) 0.04366(8) 0.0288(7) Uani 1 1 d . . . H3 H 0.3903 0.5740 0.0311 0.035 Uiso 1 1 calc R . . C4 C 0.3364(3) 0.3692(4) 0.02196(9) 0.0320(7) Uani 1 1 d . . . H4 H 0.3303 0.3771 -0.0054 0.038 Uiso 1 1 calc R . . C5 C 0.3110(4) 0.2408(4) 0.03922(10) 0.0358(8) Uani 1 1 d . A . C6 C 0.3156(4) 0.2292(4) 0.08030(10) 0.0332(8) Uani 1 1 d . A . C7 C 0.2973(6) 0.0844(4) 0.09770(12) 0.0656(15) Uani 1 1 d D . . H7A H 0.2635 0.0935 0.1236 0.079 Uiso 0.746(14) 1 d PR A 1 H7B H 0.3884 0.0412 0.0988 0.079 Uiso 0.746(14) 1 d PR A 1 H7C H 0.2220 0.0877 0.1161 0.079 Uiso 0.254(14) 1 d PR A 2 H7D H 0.3818 0.0635 0.1117 0.079 Uiso 0.254(14) 1 d PR A 2 C8 C 0.1975(10) -0.0124(7) 0.07666(13) 0.0486(18) Uani 0.746(14) 1 d PDU A 1 H8A H 0.1078 -0.0162 0.0914 0.058 Uiso 0.746(14) 1 calc PR A 1 H8B H 0.2385 -0.1087 0.0768 0.058 Uiso 0.746(14) 1 calc PR A 1 C9 C 0.1632(7) 0.0260(8) 0.03529(13) 0.0427(15) Uani 0.746(14) 1 d PDU A 1 H9A H 0.1481 -0.0621 0.0204 0.051 Uiso 0.746(14) 1 calc PR A 1 H9B H 0.0735 0.0800 0.0349 0.051 Uiso 0.746(14) 1 calc PR A 1 C8' C 0.267(3) -0.0447(11) 0.0740(3) 0.0486(18) Uani 0.254(14) 1 d PDU A 2 H8'1 H 0.2030 -0.1073 0.0888 0.058 Uiso 0.254(14) 1 calc PR A 2 H8'2 H 0.3569 -0.0967 0.0698 0.058 Uiso 0.254(14) 1 calc PR A 2 C9' C 0.201(2) -0.0126(15) 0.0352(3) 0.0427(15) Uani 0.254(14) 1 d PDU A 2 H9'1 H 0.1000 0.0098 0.0388 0.051 Uiso 0.254(14) 1 calc PR A 2 H9'2 H 0.2083 -0.0971 0.0183 0.051 Uiso 0.254(14) 1 calc PR A 2 C10 C 0.2748(5) 0.1112(4) 0.01568(10) 0.0492(10) Uani 1 1 d D . . H10A H 0.3591 0.0574 0.0119 0.059 Uiso 0.746(14) 1 d PR A 1 H10B H 0.2411 0.1411 -0.0091 0.059 Uiso 0.746(14) 1 d PR A 1 H10C H 0.3624 0.0709 0.0075 0.059 Uiso 0.254(14) 1 d PR A 2 H10D H 0.2257 0.1420 -0.0070 0.059 Uiso 0.254(14) 1 d PR A 2 C11 C 0.3234(3) 0.6612(3) 0.12733(8) 0.0266(7) Uani 1 1 d . . . H11 H 0.2260 0.6401 0.1237 0.032 Uiso 1 1 calc R . . C12 C 0.3654(3) 0.7620(3) 0.15533(9) 0.0276(7) Uani 1 1 d . . . C13 C 0.2976(4) 0.8675(4) 0.17655(9) 0.0340(7) Uani 1 1 d . . . H13 H 0.1988 0.8855 0.1773 0.041 Uiso 1 1 calc R . . C14 C 0.4020(4) 0.9413(4) 0.19650(10) 0.0350(8) Uani 1 1 d . . . H14 H 0.3884 1.0196 0.2134 0.042 Uiso 1 1 calc R . . C15 C 0.5300(4) 0.8782(4) 0.18697(10) 0.0363(8) Uani 1 1 d . . . H15 H 0.6193 0.9080 0.1966 0.044 Uiso 1 1 calc R . . C16 C 0.7205(5) 0.9335(4) 0.09700(14) 0.0587(12) Uani 1 1 d . . . H16A H 0.7478 0.9381 0.1244 0.088 Uiso 1 1 calc R . . H16B H 0.6435 1.0005 0.0921 0.088 Uiso 1 1 calc R . . H16C H 0.8020 0.9578 0.0808 0.088 Uiso 1 1 calc R . . C17 C 0.6414(5) 0.7790(4) 0.04597(11) 0.0463(9) Uani 1 1 d . . . H17A H 0.6167 0.6808 0.0399 0.070 Uiso 1 1 calc R . . H17B H 0.7246 0.8070 0.0309 0.070 Uiso 1 1 calc R . . H17C H 0.5618 0.8409 0.0395 0.070 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 Ti1 0.0281(3) 0.0281(3) 0.0259(5) -0.0043(2) 0.0043(2) -0.0022(3) N1 0.0327(14) 0.0271(13) 0.0180(12) -0.0018(10) 0.0003(11) 0.0006(10) N2 0.0311(14) 0.0315(14) 0.0265(13) -0.0079(11) 0.0009(12) 0.0001(11) N3 0.0399(16) 0.0312(14) 0.0381(17) -0.0071(13) 0.0110(13) -0.0008(12) C1 0.0272(15) 0.0316(16) 0.0163(16) 0.0002(12) 0.0007(12) -0.0037(13) C2 0.0281(15) 0.0316(16) 0.0161(14) -0.0007(12) 0.0010(12) 0.0011(12) C3 0.0348(17) 0.0343(16) 0.0172(14) 0.0041(13) -0.0016(13) -0.0052(14) C4 0.0344(17) 0.0485(19) 0.0132(14) 0.0008(14) 0.0004(12) 0.0010(15) C5 0.047(2) 0.0383(18) 0.0217(16) -0.0042(14) -0.0085(14) -0.0004(15) C6 0.046(2) 0.0324(17) 0.0209(15) 0.0023(13) -0.0076(14) -0.0043(14) C7 0.110(4) 0.036(2) 0.050(3) 0.0138(19) -0.037(3) -0.025(2) C8 0.075(4) 0.036(3) 0.035(2) 0.004(2) -0.010(3) -0.015(3) C9 0.048(3) 0.037(3) 0.043(2) -0.020(2) -0.003(2) 0.004(2) C8' 0.075(4) 0.036(3) 0.035(2) 0.004(2) -0.010(3) -0.015(3) C9' 0.048(3) 0.037(3) 0.043(2) -0.020(2) -0.003(2) 0.004(2) C10 0.077(3) 0.045(2) 0.0258(18) -0.0054(16) -0.0062(18) -0.0043(19) C11 0.0287(14) 0.0304(15) 0.0207(14) 0.0062(13) -0.0008(12) -0.0009(11) C12 0.0333(16) 0.0297(15) 0.0198(14) -0.0003(12) 0.0014(13) -0.0004(13) C13 0.0385(17) 0.0387(18) 0.0248(16) 0.0044(15) 0.0037(14) 0.0092(15) C14 0.054(2) 0.0297(16) 0.0217(15) -0.0067(13) 0.0052(14) 0.0053(15) C15 0.0451(19) 0.0333(18) 0.0304(17) -0.0089(15) -0.0009(15) -0.0021(15) C16 0.068(3) 0.035(2) 0.073(3) 0.001(2) 0.012(3) -0.005(2) C17 0.063(2) 0.043(2) 0.0327(18) 0.0098(16) 0.0136(19) 0.003(2) _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 Ti1 N3 1.902(3) 7 ? Ti1 N3 1.902(3) . ? Ti1 N2 2.140(3) . ? Ti1 N2 2.140(3) 7 ? Ti1 N1 2.281(3) 7 ? Ti1 N1 2.281(3) . ? N1 C11 1.298(4) . ? N1 C2 1.431(4) . ? N2 C15 1.364(4) . ? N2 C12 1.399(4) . ? N3 C16 1.451(5) . ? N3 C17 1.478(5) . ? C1 C2 1.399(4) . ? C1 C6 1.411(4) . ? C1 C1 1.517(6) 7 ? C2 C3 1.405(4) . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.373(5) . ? C4 H4 0.9500 . ? C5 C6 1.422(4) . ? C5 C10 1.509(5) . ? C6 C7 1.504(5) . ? C7 C8' 1.496(9) . ? C7 C8 1.501(6) . ? C7 H7A 0.9534 . ? C7 H7B 0.9543 . ? C7 H7C 0.9539 . ? C7 H7D 0.9541 . ? C8 C9 1.507(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.490(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' C9' 1.507(9) . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9' C10 1.518(10) . ? C9' H9'1 0.9900 . ? C9' H9'2 0.9900 . ? C10 H10A 0.9543 . ? C10 H10B 0.9538 . ? C10 H10C 0.9542 . ? C10 H10D 0.9539 . ? C11 C12 1.413(4) . ? C11 H11 0.9500 . ? C12 C13 1.394(5) . ? C13 C14 1.391(5) . ? C13 H13 0.9500 . ? C14 C15 1.389(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ti1 N3 104.71(18) 7 . ? N3 Ti1 N2 87.27(11) 7 . ? N3 Ti1 N2 95.32(11) . . ? N3 Ti1 N2 95.32(11) 7 7 ? N3 Ti1 N2 87.27(11) . 7 ? N2 Ti1 N2 175.76(15) . 7 ? N3 Ti1 N1 94.95(10) 7 7 ? N3 Ti1 N1 153.73(11) . 7 ? N2 Ti1 N1 102.97(10) . 7 ? N2 Ti1 N1 73.50(10) 7 7 ? N3 Ti1 N1 153.73(11) 7 . ? N3 Ti1 N1 94.95(10) . . ? N2 Ti1 N1 73.50(10) . . ? N2 Ti1 N1 102.97(10) 7 . ? N1 Ti1 N1 72.84(12) 7 . ? C11 N1 C2 117.7(3) . . ? C11 N1 Ti1 114.0(2) . . ? C2 N1 Ti1 125.11(19) . . ? C15 N2 C12 105.2(3) . . ? C15 N2 Ti1 135.5(2) . . ? C12 N2 Ti1 117.7(2) . . ? C16 N3 C17 110.4(3) . . ? C16 N3 Ti1 124.5(3) . . ? C17 N3 Ti1 125.0(2) . . ? C2 C1 C6 118.8(3) . . ? C2 C1 C1 118.8(2) . 7 ? C6 C1 C1 122.4(2) . 7 ? C1 C2 C3 120.4(3) . . ? C1 C2 N1 119.7(2) . . ? C3 C2 N1 119.8(3) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 121.2(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 C10 121.6(3) . . ? C6 C5 C10 118.7(3) . . ? C1 C6 C5 119.8(3) . . ? C1 C6 C7 122.4(3) . . ? C5 C6 C7 117.6(3) . . ? C8' C7 C8 28.3(9) . . ? C8' C7 C6 123.1(4) . . ? C8 C7 C6 115.7(3) . . ? C8' C7 H7A 121.5 . . ? C8 C7 H7A 107.3 . . ? C6 C7 H7A 109.3 . . ? C8' C7 H7B 81.0 . . ? C8 C7 H7B 109.0 . . ? C6 C7 H7B 107.6 . . ? H7A C7 H7B 107.6 . . ? C8' C7 H7C 104.4 . . ? C8 C7 H7C 82.7 . . ? C6 C7 H7C 108.8 . . ? H7A C7 H7C 28.8 . . ? H7B C7 H7C 131.3 . . ? C8' C7 H7D 105.4 . . ? C8 C7 H7D 130.1 . . ? C6 C7 H7D 107.1 . . ? H7A C7 H7D 79.9 . . ? H7B C7 H7D 30.1 . . ? H7C C7 H7D 107.2 . . ? C7 C8 C9 116.5(4) . . ? C7 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? C7 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C8 114.1(4) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C7 C8' C9' 113.5(8) . . ? C7 C8' H8'1 108.9 . . ? C9' C8' H8'1 108.9 . . ? C7 C8' H8'2 108.9 . . ? C9' C8' H8'2 108.9 . . ? H8'1 C8' H8'2 107.7 . . ? C8' C9' C10 111.1(8) . . ? C8' C9' H9'1 109.4 . . ? C10 C9' H9'1 109.4 . . ? C8' C9' H9'2 109.4 . . ? C10 C9' H9'2 109.4 . . ? H9'1 C9' H9'2 108.0 . . ? C9 C10 C5 110.8(3) . . ? C9 C10 C9' 19.6(7) . . ? C5 C10 C9' 119.4(5) . . ? C9 C10 H10A 111.4 . . ? C5 C10 H10A 108.4 . . ? C9' C10 H10A 91.8 . . ? C9 C10 H10B 109.3 . . ? C5 C10 H10B 108.5 . . ? C9' C10 H10B 118.2 . . ? H10A C10 H10B 108.4 . . ? C9 C10 H10C 122.1 . . ? C5 C10 H10C 106.6 . . ? C9' C10 H10C 102.6 . . ? H10A C10 H10C 12.0 . . ? H10B C10 H10C 98.3 . . ? C9 C10 H10D 101.1 . . ? C5 C10 H10D 107.7 . . ? C9' C10 H10D 112.1 . . ? H10A C10 H10D 117.2 . . ? H10B C10 H10D 9.8 . . ? H10C C10 H10D 107.6 . . ? N1 C11 C12 119.6(3) . . ? N1 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 N2 109.8(3) . . ? C13 C12 C11 135.4(3) . . ? N2 C12 C11 114.6(3) . . ? C14 C13 C12 107.0(3) . . ? C14 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? C15 C14 C13 106.6(3) . . ? C15 C14 H14 126.7 . . ? C13 C14 H14 126.7 . . ? N2 C15 C14 111.4(3) . . ? N2 C15 H15 124.3 . . ? C14 C15 H15 124.3 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 N3 Ti1 N1 C11 42.6(4) 7 . . . ? N3 Ti1 N1 C11 -96.1(2) . . . . ? N2 Ti1 N1 C11 -2.0(2) . . . . ? N2 Ti1 N1 C11 175.5(2) 7 . . . ? N1 Ti1 N1 C11 107.6(2) 7 . . . ? N3 Ti1 N1 C2 -116.9(3) 7 . . . ? N3 Ti1 N1 C2 104.4(2) . . . . ? N2 Ti1 N1 C2 -161.5(2) . . . . ? N2 Ti1 N1 C2 16.1(2) 7 . . . ? N1 Ti1 N1 C2 -51.82(19) 7 . . . ? N3 Ti1 N2 C15 32.3(3) 7 . . . ? N3 Ti1 N2 C15 -72.2(3) . . . . ? N2 Ti1 N2 C15 160.2(3) 7 . . . ? N1 Ti1 N2 C15 126.7(3) 7 . . . ? N1 Ti1 N2 C15 -165.8(3) . . . . ? N3 Ti1 N2 C12 -164.8(2) 7 . . . ? N3 Ti1 N2 C12 90.7(2) . . . . ? N2 Ti1 N2 C12 -36.9(2) 7 . . . ? N1 Ti1 N2 C12 -70.3(2) 7 . . . ? N1 Ti1 N2 C12 -2.9(2) . . . . ? N3 Ti1 N3 C16 -36.3(3) 7 . . . ? N2 Ti1 N3 C16 52.3(3) . . . . ? N2 Ti1 N3 C16 -131.1(3) 7 . . . ? N1 Ti1 N3 C16 -173.4(3) 7 . . . ? N1 Ti1 N3 C16 126.1(3) . . . . ? N3 Ti1 N3 C17 147.9(3) 7 . . . ? N2 Ti1 N3 C17 -123.5(3) . . . . ? N2 Ti1 N3 C17 53.1(3) 7 . . . ? N1 Ti1 N3 C17 10.8(5) 7 . . . ? N1 Ti1 N3 C17 -49.7(3) . . . . ? C6 C1 C2 C3 3.2(5) . . . . ? C1 C1 C2 C3 -179.3(3) 7 . . . ? C6 C1 C2 N1 -174.0(3) . . . . ? C1 C1 C2 N1 3.6(5) 7 . . . ? C11 N1 C2 C1 -72.6(4) . . . . ? Ti1 N1 C2 C1 86.2(3) . . . . ? C11 N1 C2 C3 110.2(3) . . . . ? Ti1 N1 C2 C3 -91.0(3) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? N1 C2 C3 C4 176.4(3) . . . . ? C2 C3 C4 C5 -1.9(5) . . . . ? C3 C4 C5 C6 1.9(5) . . . . ? C3 C4 C5 C10 -179.5(3) . . . . ? C2 C1 C6 C5 -3.1(5) . . . . ? C1 C1 C6 C5 179.4(3) 7 . . . ? C2 C1 C6 C7 173.1(4) . . . . ? C1 C1 C6 C7 -4.3(6) 7 . . . ? C4 C5 C6 C1 0.6(5) . . . . ? C10 C5 C6 C1 -178.0(3) . . . . ? C4 C5 C6 C7 -175.8(4) . . . . ? C10 C5 C6 C7 5.6(6) . . . . ? C1 C6 C7 C8' -179.6(14) . . . . ? C5 C6 C7 C8' -3.2(14) . . . . ? C1 C6 C7 C8 148.9(5) . . . . ? C5 C6 C7 C8 -34.8(7) . . . . ? C8' C7 C8 C9 -94.2(10) . . . . ? C6 C7 C8 C9 18.4(8) . . . . ? C7 C8 C9 C10 25.6(7) . . . . ? C8 C7 C8' C9' 60.4(12) . . . . ? C6 C7 C8' C9' -23(2) . . . . ? C7 C8' C9' C10 43.8(19) . . . . ? C8 C9 C10 C5 -53.5(6) . . . . ? C8 C9 C10 C9' 66.4(13) . . . . ? C4 C5 C10 C9 -140.3(4) . . . . ? C6 C5 C10 C9 38.3(6) . . . . ? C4 C5 C10 C9' -159.8(10) . . . . ? C6 C5 C10 C9' 18.7(11) . . . . ? C8' C9' C10 C9 -112.4(19) . . . . ? C8' C9' C10 C5 -43.9(15) . . . . ? C2 N1 C11 C12 167.8(3) . . . . ? Ti1 N1 C11 C12 6.8(3) . . . . ? C15 N2 C12 C13 -0.6(4) . . . . ? Ti1 N2 C12 C13 -168.3(2) . . . . ? C15 N2 C12 C11 174.9(3) . . . . ? Ti1 N2 C12 C11 7.2(3) . . . . ? N1 C11 C12 C13 164.7(3) . . . . ? N1 C11 C12 N2 -9.3(4) . . . . ? N2 C12 C13 C14 0.6(4) . . . . ? C11 C12 C13 C14 -173.6(3) . . . . ? C12 C13 C14 C15 -0.3(4) . . . . ? C12 N2 C15 C14 0.5(4) . . . . ? Ti1 N2 C15 C14 164.9(2) . . . . ? C13 C14 C15 N2 -0.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.593 _refine_diff_density_min -0.988 _refine_diff_density_rms 0.076 # Attachment 'compound_12.cif' data_compound12 _database_code_depnum_ccdc_archive 'CCDC 742599' #TrackingRef 'compound_12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 N6 Zr' _chemical_formula_sum 'C34 H40 N6 Zr' _chemical_formula_weight 623.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 43 2 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+3/4' '-x, -y, z+1/2' 'y, -x, z+1/4' '-x, y, -z' 'y, x, -z+1/4' 'x, -y, -z+1/2' '-y, -x, -z+3/4' _cell_length_a 9.5106(4) _cell_length_b 9.5106(4) _cell_length_c 34.7237(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3140.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8235 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9071 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _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 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29467 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3705 _reflns_number_gt 3654 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0348P)^2^+1.4241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 3705 _refine_ls_number_parameters 195 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.135 _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 0.645768(19) 0.645768(19) 0.1250 0.02209(8) Uani 1 2 d S . . N1 N 0.40966(18) 0.59995(18) 0.10941(5) 0.0215(3) Uani 1 1 d . . . N2 N 0.50208(19) 0.7842(2) 0.16103(5) 0.0262(3) Uani 1 1 d . . . N3 N 0.6795(2) 0.7883(2) 0.08199(6) 0.0318(4) Uani 1 1 d . . . C1 C 0.3438(2) 0.3534(2) 0.10334(5) 0.0220(3) Uani 1 1 d . . . C2 C 0.3678(2) 0.4835(2) 0.08600(6) 0.0219(4) Uani 1 1 d . . . C3 C 0.3621(2) 0.4985(2) 0.04618(6) 0.0262(4) Uani 1 1 d . . . H3 H 0.3781 0.5877 0.0347 0.031 Uiso 1 1 calc R . . C4 C 0.3332(2) 0.3827(2) 0.02345(6) 0.0292(5) Uani 1 1 d . . . H4 H 0.3272 0.3935 -0.0037 0.035 Uiso 1 1 calc R . . C5 C 0.3130(2) 0.2519(2) 0.03961(6) 0.0300(5) Uani 1 1 d . A . C6 C 0.3194(2) 0.2358(2) 0.08005(6) 0.0287(5) Uani 1 1 d . A . C7 C 0.3043(4) 0.0906(3) 0.09653(8) 0.0530(8) Uani 1 1 d D . . H7A H 0.2705 0.0996 0.1225 0.064 Uiso 0.568(7) 1 d PR A 1 H7B H 0.3954 0.0473 0.0977 0.064 Uiso 0.568(7) 1 d PR A 1 H7C H 0.2290 0.0939 0.1149 0.064 Uiso 0.432(7) 1 d PR A 2 H7D H 0.3888 0.0697 0.1105 0.064 Uiso 0.432(7) 1 d PR A 2 C8 C 0.2048(7) -0.0054(5) 0.07525(13) 0.0404(10) Uani 0.568(7) 1 d PDU A 1 H8A H 0.2450 -0.1014 0.0752 0.048 Uiso 0.568(7) 1 calc PR A 1 H8B H 0.1149 -0.0093 0.0896 0.048 Uiso 0.568(7) 1 calc PR A 1 C9 C 0.1740(10) 0.0368(11) 0.03428(19) 0.0415(18) Uani 0.568(7) 1 d PDU A 1 H9A H 0.1613 -0.0498 0.0188 0.050 Uiso 0.568(7) 1 calc PR A 1 H9B H 0.0835 0.0883 0.0339 0.050 Uiso 0.568(7) 1 calc PR A 1 C8' C 0.2760(10) -0.0266(6) 0.07074(17) 0.0404(10) Uani 0.432(7) 1 d PDU A 2 H8'1 H 0.2224 -0.0991 0.0850 0.048 Uiso 0.432(7) 1 calc PR A 2 H8'2 H 0.3667 -0.0691 0.0629 0.048 Uiso 0.432(7) 1 calc PR A 2 C9' C 0.1936(15) 0.0134(15) 0.0345(3) 0.0415(18) Uani 0.432(7) 1 d PDU A 2 H9'1 H 0.1817 -0.0691 0.0174 0.050 Uiso 0.432(7) 1 calc PR A 2 H9'2 H 0.0997 0.0507 0.0413 0.050 Uiso 0.432(7) 1 calc PR A 2 C10 C 0.2818(3) 0.1254(3) 0.01507(7) 0.0448(6) Uani 1 1 d D . . H10A H 0.3661 0.0716 0.0113 0.054 Uiso 0.568(7) 1 d PR A 1 H10B H 0.2482 0.1553 -0.0097 0.054 Uiso 0.568(7) 1 d PR A 1 H10C H 0.3694 0.0850 0.0069 0.054 Uiso 0.432(7) 1 d PR A 2 H10D H 0.2328 0.1561 -0.0076 0.054 Uiso 0.432(7) 1 d PR A 2 C11 C 0.3144(2) 0.6682(2) 0.12888(6) 0.0241(4) Uani 1 1 d . . . H11 H 0.2174 0.6483 0.1253 0.029 Uiso 1 1 calc R . . C12 C 0.3582(2) 0.7722(2) 0.15539(6) 0.0236(4) Uani 1 1 d . . . C13 C 0.2877(2) 0.8742(2) 0.17671(6) 0.0300(5) Uani 1 1 d . . . H13 H 0.1889 0.8880 0.1780 0.036 Uiso 1 1 calc R . . C14 C 0.3893(2) 0.9513(2) 0.19568(7) 0.0324(5) Uani 1 1 d . . . H14 H 0.3739 1.0286 0.2125 0.039 Uiso 1 1 calc R . . C15 C 0.5180(3) 0.8941(2) 0.18550(7) 0.0314(5) Uani 1 1 d . . . H15 H 0.6061 0.9277 0.1945 0.038 Uiso 1 1 calc R . . C16 C 0.7309(3) 0.9289(3) 0.08970(9) 0.0453(7) Uani 1 1 d . . . H16A H 0.7421 0.9417 0.1175 0.068 Uiso 1 1 calc R . . H16B H 0.6635 0.9980 0.0798 0.068 Uiso 1 1 calc R . . H16C H 0.8219 0.9422 0.0770 0.068 Uiso 1 1 calc R . . C17 C 0.6584(3) 0.7656(3) 0.04089(7) 0.0435(6) Uani 1 1 d . . . H17A H 0.6290 0.6682 0.0365 0.065 Uiso 1 1 calc R . . H17B H 0.7465 0.7837 0.0271 0.065 Uiso 1 1 calc R . . H17C H 0.5854 0.8297 0.0314 0.065 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 0.02050(9) 0.02050(9) 0.02528(14) -0.00418(8) 0.00418(8) -0.00314(10) N1 0.0244(8) 0.0202(8) 0.0198(8) -0.0004(6) 0.0006(6) -0.0024(6) N2 0.0262(9) 0.0254(9) 0.0269(9) -0.0077(7) 0.0008(7) -0.0009(7) N3 0.0349(11) 0.0254(9) 0.0351(11) -0.0002(8) 0.0081(8) -0.0038(8) C1 0.0219(9) 0.0273(9) 0.0168(9) 0.0006(8) 0.0001(7) -0.0060(8) C2 0.0207(9) 0.0256(9) 0.0193(9) -0.0015(7) 0.0005(8) -0.0028(8) C3 0.0283(10) 0.0296(10) 0.0208(10) 0.0037(8) 0.0008(9) -0.0027(9) C4 0.0308(11) 0.0418(12) 0.0150(9) -0.0003(8) 0.0015(7) -0.0037(9) C5 0.0356(12) 0.0336(11) 0.0208(11) -0.0066(8) -0.0010(8) -0.0054(9) C6 0.0349(12) 0.0285(11) 0.0227(11) 0.0000(8) -0.0026(8) -0.0081(8) C7 0.083(2) 0.0330(13) 0.0427(15) 0.0086(11) -0.0292(15) -0.0241(14) C8 0.056(3) 0.0242(17) 0.0409(18) -0.0051(14) -0.010(2) -0.004(2) C9 0.049(3) 0.034(3) 0.0419(15) -0.0192(15) -0.0001(14) -0.001(3) C8' 0.056(3) 0.0242(17) 0.0409(18) -0.0051(14) -0.010(2) -0.004(2) C9' 0.049(3) 0.034(3) 0.0419(15) -0.0192(15) -0.0001(14) -0.001(3) C10 0.0658(17) 0.0426(15) 0.0259(12) -0.0152(11) 0.0000(12) -0.0075(13) C11 0.0222(8) 0.0278(10) 0.0223(9) 0.0043(8) 0.0008(7) 0.0004(7) C12 0.0238(9) 0.0231(9) 0.0239(9) -0.0005(7) 0.0031(8) 0.0018(8) C13 0.0312(11) 0.0285(11) 0.0301(11) -0.0020(9) 0.0034(9) 0.0090(9) C14 0.0425(13) 0.0267(10) 0.0280(11) -0.0077(8) 0.0043(9) 0.0062(9) C15 0.0362(12) 0.0278(11) 0.0301(12) -0.0082(9) -0.0012(9) -0.0016(8) C16 0.0496(16) 0.0251(12) 0.0613(18) -0.0005(12) 0.0038(13) -0.0047(11) C17 0.0589(17) 0.0383(13) 0.0332(13) 0.0073(10) 0.0111(13) 0.0013(13) _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 N3 2.043(2) 6 ? Zr1 N3 2.043(2) . ? Zr1 N2 2.2729(17) 6 ? Zr1 N2 2.2729(17) . ? Zr1 N1 2.3506(18) . ? Zr1 N1 2.3506(18) 6 ? N1 C11 1.303(3) . ? N1 C2 1.430(2) . ? N2 C15 1.356(3) . ? N2 C12 1.387(3) . ? N3 C16 1.448(3) . ? N3 C17 1.457(3) . ? C1 C2 1.395(3) . ? C1 C6 1.400(3) . ? C1 C1 1.509(3) 6 ? C2 C3 1.391(3) . ? C3 C4 1.382(3) . ? C3 H3 0.9500 . ? C4 C5 1.379(3) . ? C4 H4 0.9500 . ? C5 C6 1.414(3) . ? C5 C10 1.504(3) . ? C6 C7 1.502(3) . ? C7 C8' 1.455(6) . ? C7 C8 1.508(5) . ? C7 H7A 0.9599 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7D 0.9601 . ? C8 C9 1.507(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.486(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C8' C9' 1.531(8) . ? C8' H8'1 0.9900 . ? C8' H8'2 0.9900 . ? C9' C10 1.514(9) . ? C9' H9'1 0.9900 . ? C9' H9'2 0.9900 . ? C10 H10A 0.9600 . ? C10 H10B 0.9602 . ? C10 H10C 0.9600 . ? C10 H10D 0.9601 . ? C11 C12 1.414(3) . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zr1 N3 109.03(11) 6 . ? N3 Zr1 N2 96.45(7) 6 6 ? N3 Zr1 N2 84.58(7) . 6 ? N3 Zr1 N2 84.58(7) 6 . ? N3 Zr1 N2 96.45(7) . . ? N2 Zr1 N2 178.22(9) 6 . ? N3 Zr1 N1 146.27(7) 6 . ? N3 Zr1 N1 96.01(7) . . ? N2 Zr1 N1 108.37(6) 6 . ? N2 Zr1 N1 70.11(6) . . ? N3 Zr1 N1 96.01(7) 6 6 ? N3 Zr1 N1 146.27(7) . 6 ? N2 Zr1 N1 70.11(6) 6 6 ? N2 Zr1 N1 108.37(6) . 6 ? N1 Zr1 N1 72.47(8) . 6 ? C11 N1 C2 119.12(18) . . ? C11 N1 Zr1 116.90(14) . . ? C2 N1 Zr1 122.70(13) . . ? C15 N2 C12 105.17(18) . . ? C15 N2 Zr1 136.45(16) . . ? C12 N2 Zr1 117.90(13) . . ? C16 N3 C17 111.4(2) . . ? C16 N3 Zr1 122.04(18) . . ? C17 N3 Zr1 126.58(16) . . ? C2 C1 C6 119.11(16) . . ? C2 C1 C1 118.27(15) . 6 ? C6 C1 C1 122.53(17) . 6 ? C3 C2 C1 120.90(18) . . ? C3 C2 N1 119.76(18) . . ? C1 C2 N1 119.15(16) . . ? C4 C3 C2 119.60(19) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.94(19) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.8(2) . . ? C4 C5 C10 121.3(2) . . ? C6 C5 C10 119.0(2) . . ? C1 C6 C5 119.63(19) . . ? C1 C6 C7 122.03(19) . . ? C5 C6 C7 118.3(2) . . ? C8' C7 C6 119.2(3) . . ? C8' C7 C8 28.2(3) . . ? C6 C7 C8 115.4(3) . . ? C8' C7 H7A 125.7 . . ? C6 C7 H7A 107.9 . . ? C8 C7 H7A 107.7 . . ? C8' C7 H7B 82.2 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.6 . . ? C8' C7 H7C 107.2 . . ? C6 C7 H7C 107.1 . . ? C8 C7 H7C 83.0 . . ? H7A C7 H7C 28.8 . . ? H7B C7 H7C 131.3 . . ? C8' C7 H7D 107.9 . . ? C6 C7 H7D 107.7 . . ? C8 C7 H7D 130.4 . . ? H7A C7 H7D 79.9 . . ? H7B C7 H7D 30.1 . . ? H7C C7 H7D 107.1 . . ? C9 C8 C7 115.0(4) . . ? C9 C8 H8A 108.5 . . ? C7 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 116.1(5) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C7 C8' C9' 114.2(7) . . ? C7 C8' H8'1 108.7 . . ? C9' C8' H8'1 108.7 . . ? C7 C8' H8'2 108.7 . . ? C9' C8' H8'2 108.7 . . ? H8'1 C8' H8'2 107.6 . . ? C10 C9' C8' 104.9(6) . . ? C10 C9' H9'1 110.8 . . ? C8' C9' H9'1 110.8 . . ? C10 C9' H9'2 110.8 . . ? C8' C9' H9'2 110.8 . . ? H9'1 C9' H9'2 108.8 . . ? C9 C10 C5 109.6(4) . . ? C9 C10 C9' 11.1(12) . . ? C5 C10 C9' 114.8(5) . . ? C9 C10 H10A 109.6 . . ? C5 C10 H10A 109.8 . . ? C9' C10 H10A 98.5 . . ? C9 C10 H10B 109.9 . . ? C5 C10 H10B 109.6 . . ? C9' C10 H10B 115.0 . . ? H10A C10 H10B 108.4 . . ? C9 C10 H10C 120.3 . . ? C5 C10 H10C 108.4 . . ? C9' C10 H10C 109.3 . . ? H10A C10 H10C 12.0 . . ? H10B C10 H10C 98.3 . . ? C9 C10 H10D 101.8 . . ? C5 C10 H10D 108.4 . . ? C9' C10 H10D 108.1 . . ? H10A C10 H10D 117.2 . . ? H10B C10 H10D 9.8 . . ? H10C C10 H10D 107.6 . . ? N1 C11 C12 118.77(19) . . ? N1 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N2 C12 C13 110.05(19) . . ? N2 C12 C11 116.09(18) . . ? C13 C12 C11 133.8(2) . . ? C14 C13 C12 106.7(2) . . ? C14 C13 H13 126.7 . . ? C12 C13 H13 126.7 . . ? C13 C14 C15 106.76(19) . . ? C13 C14 H14 126.6 . . ? C15 C14 H14 126.6 . . ? N2 C15 C14 111.4(2) . . ? N2 C15 H15 124.3 . . ? C14 C15 H15 124.3 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 N3 Zr1 N1 C11 41.3(2) 6 . . . ? N3 Zr1 N1 C11 -97.16(15) . . . . ? N2 Zr1 N1 C11 176.56(14) 6 . . . ? N2 Zr1 N1 C11 -2.46(14) . . . . ? N1 Zr1 N1 C11 115.30(16) 6 . . . ? N3 Zr1 N1 C2 -125.69(16) 6 . . . ? N3 Zr1 N1 C2 95.87(15) . . . . ? N2 Zr1 N1 C2 9.60(16) 6 . . . ? N2 Zr1 N1 C2 -169.42(16) . . . . ? N1 Zr1 N1 C2 -51.66(12) 6 . . . ? N3 Zr1 N2 C15 31.5(2) 6 . . . ? N3 Zr1 N2 C15 -77.1(2) . . . . ? N2 Zr1 N2 C15 157.3(2) 6 . . . ? N1 Zr1 N2 C15 -171.2(2) . . . . ? N1 Zr1 N2 C15 126.0(2) 6 . . . ? N3 Zr1 N2 C12 -157.90(17) 6 . . . ? N3 Zr1 N2 C12 93.50(16) . . . . ? N2 Zr1 N2 C12 -32.12(15) 6 . . . ? N1 Zr1 N2 C12 -0.58(14) . . . . ? N1 Zr1 N2 C12 -63.35(16) 6 . . . ? N3 Zr1 N3 C16 -32.32(17) 6 . . . ? N2 Zr1 N3 C16 -127.29(19) 6 . . . ? N2 Zr1 N3 C16 54.16(19) . . . . ? N1 Zr1 N3 C16 124.75(19) . . . . ? N1 Zr1 N3 C16 -168.06(16) 6 . . . ? N3 Zr1 N3 C17 147.0(2) 6 . . . ? N2 Zr1 N3 C17 52.0(2) 6 . . . ? N2 Zr1 N3 C17 -126.5(2) . . . . ? N1 Zr1 N3 C17 -55.9(2) . . . . ? N1 Zr1 N3 C17 11.2(3) 6 . . . ? C6 C1 C2 C3 2.6(3) . . . . ? C1 C1 C2 C3 179.2(2) 6 . . . ? C6 C1 C2 N1 -172.44(19) . . . . ? C1 C1 C2 N1 4.2(3) 6 . . . ? C11 N1 C2 C3 105.0(2) . . . . ? Zr1 N1 C2 C3 -88.3(2) . . . . ? C11 N1 C2 C1 -80.0(2) . . . . ? Zr1 N1 C2 C1 86.7(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? N1 C2 C3 C4 174.57(19) . . . . ? C2 C3 C4 C5 -1.5(3) . . . . ? C3 C4 C5 C6 1.1(3) . . . . ? C3 C4 C5 C10 -179.8(2) . . . . ? C2 C1 C6 C5 -2.9(3) . . . . ? C1 C1 C6 C5 -179.4(2) 6 . . . ? C2 C1 C6 C7 175.0(2) . . . . ? C1 C1 C6 C7 -1.5(4) 6 . . . ? C4 C5 C6 C1 1.1(3) . . . . ? C10 C5 C6 C1 -178.0(2) . . . . ? C4 C5 C6 C7 -176.9(2) . . . . ? C10 C5 C6 C7 4.1(4) . . . . ? C1 C6 C7 C8' 178.7(5) . . . . ? C5 C6 C7 C8' -3.4(6) . . . . ? C1 C6 C7 C8 147.1(4) . . . . ? C5 C6 C7 C8 -35.0(5) . . . . ? C8' C7 C8 C9 -84.6(10) . . . . ? C6 C7 C8 C9 20.2(8) . . . . ? C7 C8 C9 C10 24.0(12) . . . . ? C6 C7 C8' C9' -29.4(9) . . . . ? C8 C7 C8' C9' 60.5(8) . . . . ? C7 C8' C9' C10 57.5(12) . . . . ? C8 C9 C10 C5 -53.1(10) . . . . ? C8 C9 C10 C9' 67(2) . . . . ? C4 C5 C10 C9 -140.0(5) . . . . ? C6 C5 C10 C9 39.0(5) . . . . ? C4 C5 C10 C9' -150.6(7) . . . . ? C6 C5 C10 C9' 28.5(7) . . . . ? C8' C9' C10 C9 -121(3) . . . . ? C8' C9' C10 C5 -57.1(12) . . . . ? C2 N1 C11 C12 172.64(17) . . . . ? Zr1 N1 C11 C12 5.2(2) . . . . ? C15 N2 C12 C13 -0.5(2) . . . . ? Zr1 N2 C12 C13 -173.79(14) . . . . ? C15 N2 C12 C11 176.64(18) . . . . ? Zr1 N2 C12 C11 3.3(2) . . . . ? N1 C11 C12 N2 -5.7(3) . . . . ? N1 C11 C12 C13 170.6(2) . . . . ? N2 C12 C13 C14 0.4(3) . . . . ? C11 C12 C13 C14 -176.0(2) . . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C12 N2 C15 C14 0.4(3) . . . . ? Zr1 N2 C15 C14 171.81(16) . . . . ? C13 C14 C15 N2 -0.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.512 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.051 # Attachment 'compound_13.cif' data_compound13 _database_code_depnum_ccdc_archive 'CCDC 742600' #TrackingRef 'compound_13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H54 N4 O2 Ti' _chemical_formula_sum 'C44 H54 N4 O2 Ti' _chemical_formula_weight 718.81 _chemical_absolute_configuration rmad 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9926(12) _cell_length_b 9.9667(8) _cell_length_c 17.5936(18) _cell_angle_alpha 90.00 _cell_angle_beta 109.007(8) _cell_angle_gamma 90.00 _cell_volume 1988.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5900 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9226 _exptl_absorpt_correction_T_max 0.9506 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24538 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.87 _reflns_number_total 9422 _reflns_number_gt 7418 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0613P)^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 SHELXL _refine_ls_extinction_coef 0.042(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(19) _refine_ls_number_reflns 9422 _refine_ls_number_parameters 555 _refine_ls_number_restraints 149 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.79134(3) 0.30103(5) 0.05899(2) 0.04629(12) Uani 1 1 d . C . O1 O 0.67061(13) 0.17294(19) 0.08263(9) 0.0563(4) Uani 1 1 d . C . O2 O 0.94797(14) 0.40658(17) 0.08467(8) 0.0522(4) Uani 1 1 d . C . N1 N 0.85422(15) 0.1106(2) 0.12435(10) 0.0455(4) Uani 1 1 d . C . N2 N 0.88696(15) 0.36321(19) 0.18572(9) 0.0448(4) Uani 1 1 d . C . N3 N 0.66740(19) 0.4267(2) 0.02080(12) 0.0618(5) Uani 1 1 d . . . N4 N 0.79860(19) 0.2275(2) -0.03846(11) 0.0565(5) Uani 1 1 d . . . C1 C 1.00822(17) 0.1118(2) 0.25544(12) 0.0456(5) Uani 1 1 d . . . C2 C 0.96253(18) 0.0631(2) 0.17628(12) 0.0445(5) Uani 1 1 d . . . C3 C 1.0327(2) -0.0169(3) 0.14539(15) 0.0535(6) Uani 1 1 d . . . H3A H 1.0033 -0.0482 0.0928 0.064 Uiso 1 1 calc R . . C4 C 1.1458(2) -0.0499(3) 0.19246(16) 0.0617(6) Uani 1 1 d . . . H4A H 1.1907 -0.1064 0.1719 0.074 Uiso 1 1 calc R . . C5 C 1.1940(2) 0.0000(3) 0.27046(16) 0.0629(7) Uani 1 1 d . A . C6 C 1.1271(2) 0.0846(3) 0.30166(14) 0.0559(6) Uani 1 1 d . A . C7 C 1.1831(2) 0.1543(4) 0.38115(14) 0.0678(7) Uani 1 1 d D . . H7A H 1.1297 0.1498 0.4116 0.081 Uiso 0.507(12) 1 d PR A 1 H7B H 1.1934 0.2473 0.3708 0.081 Uiso 0.507(12) 1 d PR A 1 H7C H 1.1511 0.1182 0.4202 0.081 Uiso 0.493(12) 1 d PR A 2 H7D H 1.1634 0.2480 0.3748 0.081 Uiso 0.493(12) 1 d PR A 2 C8 C 1.2991(7) 0.0926(14) 0.4329(5) 0.085(3) Uani 0.507(12) 1 d PDU A 1 H8A H 1.2840 0.0076 0.4547 0.101 Uiso 0.507(12) 1 calc PR A 1 H8B H 1.3374 0.1519 0.4775 0.101 Uiso 0.507(12) 1 calc PR A 1 C9 C 1.3792(6) 0.0704(12) 0.3821(5) 0.098(3) Uani 0.507(12) 1 d PDU A 1 H9A H 1.4558 0.0385 0.4158 0.118 Uiso 0.507(12) 1 calc PR A 1 H9B H 1.3903 0.1541 0.3574 0.118 Uiso 0.507(12) 1 calc PR A 1 C8' C 1.3165(7) 0.1380(10) 0.4154(9) 0.095(4) Uani 0.493(12) 1 d PDU A 2 H8'A H 1.3435 0.1617 0.4719 0.114 Uiso 0.493(12) 1 calc PR A 2 H8'B H 1.3541 0.1979 0.3877 0.114 Uiso 0.493(12) 1 calc PR A 2 C9' C 1.3512(9) -0.0081(11) 0.4052(4) 0.104(4) Uani 0.493(12) 1 d PDU A 2 H9'A H 1.4349 -0.0212 0.4323 0.124 Uiso 0.493(12) 1 calc PR A 2 H9'B H 1.3081 -0.0694 0.4282 0.124 Uiso 0.493(12) 1 calc PR A 2 C10 C 1.3214(2) -0.0340(4) 0.3168(2) 0.0902(10) Uani 1 1 d D . . H10A H 1.3647 -0.0396 0.2796 0.108 Uiso 0.507(12) 1 d PR A 1 H10B H 1.3250 -0.1201 0.3420 0.108 Uiso 0.507(12) 1 d PR A 1 H10C H 1.3722 0.0171 0.2954 0.108 Uiso 0.493(12) 1 d PR A 2 H10D H 1.3344 -0.1274 0.3094 0.108 Uiso 0.493(12) 1 d PR A 2 C11 C 0.93381(18) 0.1920(2) 0.29246(11) 0.0463(5) Uani 1 1 d . . . C12 C 0.88956(16) 0.3191(3) 0.26355(11) 0.0447(5) Uani 1 1 d . . . C13 C 0.8309(2) 0.3942(3) 0.30505(13) 0.0568(6) Uani 1 1 d . . . H13A H 0.8018 0.4785 0.2860 0.068 Uiso 1 1 calc R . . C14 C 0.8153(3) 0.3451(3) 0.37442(15) 0.0671(7) Uani 1 1 d . . . H14A H 0.7807 0.3993 0.4036 0.081 Uiso 1 1 calc R . . C15 C 0.8508(2) 0.2154(3) 0.40101(14) 0.0608(7) Uani 1 1 d . B . C16 C 0.9070(2) 0.1373(3) 0.35932(12) 0.0513(6) Uani 1 1 d . B . C17 C 0.9331(3) -0.0091(3) 0.38067(16) 0.0643(7) Uani 1 1 d D . . H17A H 1.0168 -0.0205 0.4042 0.077 Uiso 0.579(10) 1 d PR B 1 H17B H 0.9079 -0.0601 0.3317 0.077 Uiso 0.579(10) 1 d PR B 1 H17C H 1.0122 -0.0293 0.3825 0.077 Uiso 0.421(10) 1 d PR B 2 H17D H 0.8801 -0.0634 0.3395 0.077 Uiso 0.421(10) 1 d PR B 2 C18 C 0.8733(8) -0.0678(9) 0.4370(4) 0.077(2) Uani 0.579(10) 1 d PDU B 1 H18A H 0.9080 -0.1540 0.4573 0.092 Uiso 0.579(10) 1 calc PR B 1 H18B H 0.7899 -0.0810 0.4087 0.092 Uiso 0.579(10) 1 calc PR B 1 C19 C 0.8907(8) 0.0326(7) 0.5077(4) 0.092(3) Uani 0.579(10) 1 d PDU B 1 H19A H 0.8614 -0.0061 0.5482 0.111 Uiso 0.579(10) 1 calc PR B 1 H19B H 0.9738 0.0528 0.5326 0.111 Uiso 0.579(10) 1 calc PR B 1 C18' C 0.9189(9) -0.0457(15) 0.4604(6) 0.078(3) Uani 0.421(10) 1 d PDU B 2 H18C H 0.9858 -0.0111 0.5035 0.093 Uiso 0.421(10) 1 calc PR B 2 H18D H 0.9195 -0.1426 0.4653 0.093 Uiso 0.421(10) 1 calc PR B 2 C19' C 0.8043(10) 0.0093(8) 0.4707(6) 0.094(3) Uani 0.421(10) 1 d PDU B 2 H19C H 0.7360 -0.0166 0.4258 0.112 Uiso 0.421(10) 1 calc PR B 2 H19D H 0.7946 -0.0231 0.5202 0.112 Uiso 0.421(10) 1 calc PR B 2 C20 C 0.8219(3) 0.1613(4) 0.47324(17) 0.0877(10) Uani 1 1 d D . . H20A H 0.7389 0.1423 0.4571 0.105 Uiso 0.579(10) 1 d PR B 1 H20B H 0.8389 0.2291 0.5142 0.105 Uiso 0.579(10) 1 d PR B 1 H20C H 0.7505 0.2034 0.4746 0.105 Uiso 0.421(10) 1 d PR B 2 H20D H 0.8837 0.1849 0.5218 0.105 Uiso 0.421(10) 1 d PR B 2 C21 C 0.74723(18) 0.0867(2) 0.12443(12) 0.0488(5) Uani 1 1 d D . . C22 C 0.6954(15) -0.0117(11) 0.1649(11) 0.0436(15) Uani 0.406(12) 1 d PG C 1 C23 C 0.6383(15) 0.0193(9) 0.2199(11) 0.0568(13) Uani 0.406(12) 1 d PGD C 1 C24 C 0.6042(14) -0.0827(12) 0.2615(9) 0.0677(19) Uani 0.406(12) 1 d PG C 1 H24A H 0.5660 -0.0619 0.2983 0.081 Uiso 0.406(12) 1 calc PR C 1 C25 C 0.6271(14) -0.2157(11) 0.2481(7) 0.073(2) Uani 0.406(12) 1 d PGD C 1 C26 C 0.6842(16) -0.2468(9) 0.1931(9) 0.0671(18) Uani 0.406(12) 1 d PG C 1 H26A H 0.6995 -0.3358 0.1841 0.081 Uiso 0.406(12) 1 calc PR C 1 C27 C 0.7184(16) -0.1448(13) 0.1515(9) 0.0550(13) Uani 0.406(12) 1 d PGD C 1 C28 C 0.6018(18) 0.1640(12) 0.2264(11) 0.063(3) Uani 0.406(12) 1 d PDU C 1 H28A H 0.5235 0.1783 0.1900 0.094 Uiso 0.406(12) 1 calc PR C 1 H28B H 0.6556 0.2234 0.2130 0.094 Uiso 0.406(12) 1 calc PR C 1 H28C H 0.6034 0.1815 0.2804 0.094 Uiso 0.406(12) 1 calc PR C 1 C29 C 0.5923(13) -0.3195(15) 0.3000(10) 0.116(5) Uani 0.406(12) 1 d PDU C 1 H29A H 0.5618 -0.2746 0.3373 0.174 Uiso 0.406(12) 1 calc PR C 1 H29B H 0.6603 -0.3713 0.3290 0.174 Uiso 0.406(12) 1 calc PR C 1 H29C H 0.5329 -0.3778 0.2663 0.174 Uiso 0.406(12) 1 calc PR C 1 C30 C 0.7768(19) -0.197(2) 0.0924(11) 0.075(4) Uani 0.406(12) 1 d PDU C 1 H30A H 0.7767 -0.2929 0.0927 0.113 Uiso 0.406(12) 1 calc PR C 1 H30B H 0.8566 -0.1646 0.1078 0.113 Uiso 0.406(12) 1 calc PR C 1 H30C H 0.7340 -0.1649 0.0394 0.113 Uiso 0.406(12) 1 calc PR C 1 C22' C 0.7108(10) -0.0379(7) 0.1604(7) 0.0436(15) Uani 0.594(12) 1 d PGD C 2 C23' C 0.6461(9) -0.0160(7) 0.2119(7) 0.0568(13) Uani 0.594(12) 1 d PGD C 2 C24' C 0.6019(8) -0.1243(9) 0.2429(6) 0.0677(19) Uani 0.594(12) 1 d PG C 2 H24B H 0.5585 -0.1097 0.2774 0.081 Uiso 0.594(12) 1 calc PR C 2 C25' C 0.6224(9) -0.2545(7) 0.2224(6) 0.073(2) Uani 0.594(12) 1 d PGD C 2 C26' C 0.6872(10) -0.2763(6) 0.1708(6) 0.0671(18) Uani 0.594(12) 1 d PG C 2 H26B H 0.7009 -0.3634 0.1571 0.081 Uiso 0.594(12) 1 calc PR C 2 C27' C 0.7314(10) -0.1681(8) 0.1398(6) 0.0550(13) Uani 0.594(12) 1 d PGD C 2 C28' C 0.6092(11) 0.1198(10) 0.2334(8) 0.070(2) Uani 0.594(12) 1 d PDU C 2 H28D H 0.6778 0.1749 0.2558 0.106 Uiso 0.594(12) 1 calc PR C 2 H28E H 0.5690 0.1091 0.2721 0.106 Uiso 0.594(12) 1 calc PR C 2 H28F H 0.5573 0.1619 0.1859 0.106 Uiso 0.594(12) 1 calc PR C 2 C29' C 0.5781(6) -0.3743(9) 0.2584(6) 0.096(3) Uani 0.594(12) 1 d PDU C 2 H29D H 0.5775 -0.4528 0.2266 0.144 Uiso 0.594(12) 1 calc PR C 2 H29E H 0.4997 -0.3566 0.2588 0.144 Uiso 0.594(12) 1 calc PR C 2 H29F H 0.6294 -0.3891 0.3124 0.144 Uiso 0.594(12) 1 calc PR C 2 C30' C 0.7829(13) -0.1889(14) 0.0737(7) 0.072(3) Uani 0.594(12) 1 d PDU C 2 H30D H 0.7339 -0.2495 0.0345 0.108 Uiso 0.594(12) 1 calc PR C 2 H30E H 0.8607 -0.2260 0.0957 0.108 Uiso 0.594(12) 1 calc PR C 2 H30F H 0.7872 -0.1044 0.0486 0.108 Uiso 0.594(12) 1 calc PR C 2 C31 C 0.97307(18) 0.4057(2) 0.16232(12) 0.0454(5) Uani 1 1 d D . . C32 C 1.0963(8) 0.4373(16) 0.2196(8) 0.0486(12) Uani 0.341(12) 1 d PGD C 1 C33 C 1.1168(7) 0.5310(12) 0.2811(7) 0.0467(11) Uani 0.341(12) 1 d PGD C 1 C34 C 1.2313(9) 0.5557(13) 0.3311(6) 0.0610(16) Uani 0.341(12) 1 d PG C 1 H34A H 1.2450 0.6184 0.3723 0.073 Uiso 0.341(12) 1 calc PR C 1 C35 C 1.3252(6) 0.4868(15) 0.3196(6) 0.068(2) Uani 0.341(12) 1 d PGD C 1 C36 C 1.3047(10) 0.3931(16) 0.2580(8) 0.0638(15) Uani 0.341(12) 1 d PG C 1 H36A H 1.3676 0.3470 0.2503 0.077 Uiso 0.341(12) 1 calc PR C 1 C37 C 1.1903(12) 0.3684(19) 0.2080(9) 0.0553(10) Uani 0.341(12) 1 d PGD C 1 C38 C 1.0165(16) 0.626(2) 0.2765(15) 0.077(5) Uani 0.341(12) 1 d PDU C 1 H38A H 0.9428 0.5799 0.2557 0.115 Uiso 0.341(12) 1 calc PR C 1 H38B H 1.0181 0.7000 0.2417 0.115 Uiso 0.341(12) 1 calc PR C 1 H38C H 1.0251 0.6600 0.3293 0.115 Uiso 0.341(12) 1 calc PR C 1 C39 C 1.4394(11) 0.4862(15) 0.3926(7) 0.080(4) Uani 0.341(12) 1 d PDU C 1 H39A H 1.4523 0.5738 0.4164 0.120 Uiso 0.341(12) 1 calc PR C 1 H39B H 1.5049 0.4622 0.3753 0.120 Uiso 0.341(12) 1 calc PR C 1 H39C H 1.4321 0.4221 0.4314 0.120 Uiso 0.341(12) 1 calc PR C 1 C40 C 1.192(2) 0.269(3) 0.1434(15) 0.083(6) Uani 0.341(12) 1 d PDU C 1 H40A H 1.1170 0.2259 0.1229 0.124 Uiso 0.341(12) 1 calc PR C 1 H40B H 1.2523 0.2033 0.1657 0.124 Uiso 0.341(12) 1 calc PR C 1 H40C H 1.2089 0.3159 0.1005 0.124 Uiso 0.341(12) 1 calc PR C 1 C32' C 1.0909(4) 0.4606(8) 0.2126(4) 0.0486(12) Uani 0.659(12) 1 d PGD C 2 C33' C 1.0931(4) 0.5630(7) 0.2667(3) 0.0467(11) Uani 0.659(12) 1 d PGD C 2 C34' C 1.1987(6) 0.5982(7) 0.3250(3) 0.0610(16) Uani 0.659(12) 1 d PG C 2 H34B H 1.2002 0.6667 0.3612 0.073 Uiso 0.659(12) 1 calc PR C 2 C35' C 1.3021(4) 0.5310(8) 0.3291(3) 0.068(2) Uani 0.659(12) 1 d PGD C 2 C36' C 1.2999(4) 0.4287(8) 0.2749(4) 0.0638(15) Uani 0.659(12) 1 d PG C 2 H36B H 1.3690 0.3837 0.2777 0.077 Uiso 0.659(12) 1 calc PR C 2 C37' C 1.1943(6) 0.3934(9) 0.2167(4) 0.0553(10) Uani 0.659(12) 1 d PGD C 2 C38' C 0.9888(8) 0.6516(11) 0.2652(7) 0.0648(18) Uani 0.659(12) 1 d PDU C 2 H38D H 1.0096 0.7441 0.2626 0.097 Uiso 0.659(12) 1 calc PR C 2 H38E H 0.9688 0.6367 0.3131 0.097 Uiso 0.659(12) 1 calc PR C 2 H38F H 0.9224 0.6299 0.2190 0.097 Uiso 0.659(12) 1 calc PR C 2 C39' C 1.4166(6) 0.5607(12) 0.3971(4) 0.094(2) Uani 0.659(12) 1 d PDU C 2 H39D H 1.4275 0.6560 0.4030 0.140 Uiso 0.659(12) 1 calc PR C 2 H39E H 1.4817 0.5216 0.3847 0.140 Uiso 0.659(12) 1 calc PR C 2 H39F H 1.4123 0.5232 0.4463 0.140 Uiso 0.659(12) 1 calc PR C 2 C40' C 1.1942(9) 0.2951(12) 0.1512(7) 0.0663(19) Uani 0.659(12) 1 d PDU C 2 H40D H 1.1425 0.2216 0.1513 0.099 Uiso 0.659(12) 1 calc PR C 2 H40E H 1.2727 0.2618 0.1608 0.099 Uiso 0.659(12) 1 calc PR C 2 H40F H 1.1674 0.3394 0.1000 0.099 Uiso 0.659(12) 1 calc PR C 2 C41 C 0.6590(3) 0.5078(4) -0.04974(18) 0.0909(10) Uani 1 1 d . . . H41A H 0.6297 0.5954 -0.0435 0.136 Uiso 1 1 calc R . . H41B H 0.6062 0.4656 -0.0967 0.136 Uiso 1 1 calc R . . H41C H 0.7357 0.5160 -0.0554 0.136 Uiso 1 1 calc R . . C42 C 0.5604(3) 0.4366(4) 0.0422(3) 0.1066(12) Uani 1 1 d . . . H42A H 0.5446 0.5291 0.0500 0.160 Uiso 1 1 calc R . . H42B H 0.5704 0.3877 0.0910 0.160 Uiso 1 1 calc R . . H42C H 0.4955 0.3995 -0.0002 0.160 Uiso 1 1 calc R . . C43 C 0.6937(3) 0.1819(4) -0.10174(16) 0.0761(8) Uani 1 1 d . . . H43A H 0.7016 0.2013 -0.1532 0.114 Uiso 1 1 calc R . . H43B H 0.6257 0.2273 -0.0970 0.114 Uiso 1 1 calc R . . H43C H 0.6848 0.0869 -0.0968 0.114 Uiso 1 1 calc R . . C44 C 0.9060(3) 0.1668(3) -0.04610(16) 0.0720(8) Uani 1 1 d . . . H44A H 0.9120 0.1885 -0.0978 0.108 Uiso 1 1 calc R . . H44B H 0.9025 0.0711 -0.0409 0.108 Uiso 1 1 calc R . . H44C H 0.9736 0.2011 -0.0046 0.108 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 Ti1 0.04211(19) 0.0575(2) 0.03580(18) -0.00071(18) 0.00789(14) -0.00010(19) O1 0.0401(8) 0.0712(11) 0.0521(9) 0.0055(8) 0.0076(7) 0.0000(8) O2 0.0535(9) 0.0661(10) 0.0356(7) 0.0026(7) 0.0127(7) -0.0087(8) N1 0.0395(9) 0.0564(11) 0.0391(9) -0.0009(8) 0.0107(7) 0.0002(8) N2 0.0421(9) 0.0558(11) 0.0334(8) 0.0002(8) 0.0082(7) -0.0025(8) N3 0.0556(12) 0.0718(14) 0.0478(11) 0.0001(10) 0.0028(9) 0.0082(10) N4 0.0637(12) 0.0625(12) 0.0429(10) -0.0001(9) 0.0169(9) -0.0022(10) C1 0.0365(10) 0.0593(13) 0.0419(11) 0.0060(10) 0.0142(8) 0.0037(9) C2 0.0401(10) 0.0519(12) 0.0428(11) 0.0050(10) 0.0151(9) -0.0016(9) C3 0.0527(13) 0.0580(14) 0.0546(13) -0.0034(11) 0.0239(11) 0.0032(11) C4 0.0555(14) 0.0631(16) 0.0719(16) 0.0021(13) 0.0282(13) 0.0099(12) C5 0.0416(12) 0.0758(17) 0.0726(17) 0.0124(14) 0.0204(12) 0.0105(12) C6 0.0422(11) 0.0733(17) 0.0496(13) 0.0136(12) 0.0112(10) 0.0067(11) C7 0.0470(13) 0.101(2) 0.0474(13) 0.0062(14) 0.0040(10) 0.0024(14) C8 0.054(4) 0.117(7) 0.065(4) 0.009(4) -0.004(3) 0.013(4) C9 0.051(3) 0.141(7) 0.094(5) 0.016(5) 0.011(3) 0.016(4) C8' 0.073(5) 0.106(7) 0.086(6) 0.007(5) -0.004(4) -0.009(4) C9' 0.069(5) 0.118(7) 0.091(5) 0.018(5) -0.018(4) 0.027(5) C10 0.0453(14) 0.115(3) 0.106(3) 0.014(2) 0.0178(16) 0.0223(17) C11 0.0400(10) 0.0638(14) 0.0327(10) -0.0003(9) 0.0086(8) 0.0020(10) C12 0.0392(9) 0.0599(14) 0.0342(9) 0.0009(10) 0.0107(7) -0.0013(10) C13 0.0619(14) 0.0647(15) 0.0478(12) 0.0021(11) 0.0236(11) 0.0068(12) C14 0.0816(18) 0.0793(19) 0.0501(13) -0.0040(13) 0.0348(13) 0.0095(15) C15 0.0672(16) 0.0777(19) 0.0430(12) 0.0021(12) 0.0254(11) 0.0062(14) C16 0.0493(12) 0.0694(16) 0.0355(10) 0.0087(10) 0.0141(9) 0.0035(11) C17 0.0687(16) 0.0709(17) 0.0564(14) 0.0181(13) 0.0246(12) 0.0128(13) C18 0.087(5) 0.084(4) 0.065(4) 0.015(3) 0.032(3) -0.001(4) C19 0.121(6) 0.105(5) 0.066(4) 0.025(3) 0.050(4) 0.018(4) C18' 0.089(6) 0.080(6) 0.072(6) 0.021(5) 0.037(5) 0.002(5) C19' 0.113(7) 0.119(6) 0.075(5) 0.015(4) 0.067(5) -0.005(5) C20 0.124(3) 0.099(2) 0.0601(16) 0.0126(17) 0.0573(19) 0.019(2) C21 0.0404(11) 0.0655(15) 0.0386(11) -0.0048(10) 0.0103(9) -0.0057(10) C22 0.030(3) 0.054(3) 0.0468(17) 0.004(3) 0.0126(14) 0.008(3) C23 0.0331(17) 0.084(4) 0.054(3) 0.002(3) 0.0147(13) 0.003(3) C24 0.0456(15) 0.106(6) 0.058(5) 0.011(4) 0.027(3) 0.006(4) C25 0.0441(16) 0.102(5) 0.077(5) 0.033(4) 0.023(4) 0.004(3) C26 0.0544(17) 0.063(3) 0.088(6) 0.015(3) 0.029(3) 0.002(3) C27 0.042(3) 0.064(3) 0.062(3) 0.007(3) 0.0218(15) 0.003(2) C28 0.058(5) 0.076(6) 0.061(5) 0.004(5) 0.028(4) 0.011(5) C29 0.125(8) 0.106(8) 0.136(8) 0.035(6) 0.069(7) -0.006(6) C30 0.089(7) 0.071(6) 0.068(7) 0.010(6) 0.030(5) -0.017(5) C22' 0.030(3) 0.054(3) 0.0468(17) 0.004(3) 0.0126(14) 0.008(3) C23' 0.0331(17) 0.084(4) 0.054(3) 0.002(3) 0.0147(13) 0.003(3) C24' 0.0456(15) 0.106(6) 0.058(5) 0.011(4) 0.027(3) 0.006(4) C25' 0.0441(16) 0.102(5) 0.077(5) 0.033(4) 0.023(4) 0.004(3) C26' 0.0544(17) 0.063(3) 0.088(6) 0.015(3) 0.029(3) 0.002(3) C27' 0.042(3) 0.064(3) 0.062(3) 0.007(3) 0.0218(15) 0.003(2) C28' 0.050(4) 0.089(6) 0.081(5) -0.009(5) 0.032(3) -0.004(4) C29' 0.065(3) 0.110(5) 0.116(5) 0.059(4) 0.035(4) 0.002(3) C30' 0.090(4) 0.062(5) 0.077(6) -0.019(4) 0.046(4) -0.012(4) C31 0.0448(11) 0.0519(12) 0.0371(10) -0.0007(10) 0.0100(9) -0.0017(10) C32 0.0471(13) 0.058(3) 0.0370(16) 0.0095(19) 0.0087(10) -0.0097(15) C33 0.051(2) 0.059(3) 0.024(2) 0.0162(19) 0.0040(17) -0.002(2) C34 0.053(3) 0.090(4) 0.0380(15) -0.005(2) 0.0122(19) -0.019(3) C35 0.042(2) 0.123(6) 0.0407(18) -0.003(2) 0.0154(16) -0.018(3) C36 0.0466(15) 0.100(5) 0.044(3) 0.004(3) 0.0124(16) -0.013(2) C37 0.0487(14) 0.065(4) 0.051(2) 0.0082(15) 0.0148(13) -0.0118(18) C38 0.094(9) 0.059(8) 0.070(7) -0.014(6) 0.016(7) -0.012(6) C39 0.075(6) 0.084(7) 0.063(5) 0.012(5) -0.003(4) -0.022(5) C40 0.091(9) 0.080(10) 0.083(8) -0.012(6) 0.037(6) -0.005(6) C32' 0.0471(13) 0.058(3) 0.0370(16) 0.0095(19) 0.0087(10) -0.0097(15) C33' 0.051(2) 0.059(3) 0.024(2) 0.0162(19) 0.0040(17) -0.002(2) C34' 0.053(3) 0.090(4) 0.0380(15) -0.005(2) 0.0122(19) -0.019(3) C35' 0.042(2) 0.123(6) 0.0407(18) -0.003(2) 0.0154(16) -0.018(3) C36' 0.0466(15) 0.100(5) 0.044(3) 0.004(3) 0.0124(16) -0.013(2) C37' 0.0487(14) 0.065(4) 0.051(2) 0.0082(15) 0.0148(13) -0.0118(18) C38' 0.066(3) 0.060(4) 0.072(4) -0.008(3) 0.028(3) -0.002(3) C39' 0.067(3) 0.141(6) 0.061(3) -0.005(4) 0.004(2) -0.024(4) C40' 0.049(3) 0.066(4) 0.093(5) 0.008(3) 0.034(3) 0.004(3) C41 0.113(3) 0.081(2) 0.0612(17) 0.0072(16) 0.0038(17) 0.021(2) C42 0.075(2) 0.104(3) 0.146(3) 0.014(2) 0.043(2) 0.030(2) C43 0.0836(19) 0.085(2) 0.0552(14) -0.0147(15) 0.0157(13) -0.0192(17) C44 0.0857(19) 0.0800(19) 0.0583(14) -0.0023(14) 0.0345(14) 0.0117(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 Ti1 N3 1.892(2) . ? Ti1 N4 1.893(2) . ? Ti1 O2 2.0703(16) . ? Ti1 O1 2.0716(17) . ? Ti1 N1 2.2203(19) . ? Ti1 N2 2.2371(17) . ? Ti1 C31 2.562(2) . ? Ti1 C21 2.562(2) . ? O1 C21 1.297(3) . ? O2 C31 1.300(2) . ? N1 C21 1.305(3) . ? N1 C2 1.404(3) . ? N2 C31 1.301(3) . ? N2 C12 1.429(2) . ? N3 C42 1.454(4) . ? N3 C41 1.457(4) . ? N4 C43 1.454(4) . ? N4 C44 1.468(3) . ? C1 C2 1.406(3) . ? C1 C6 1.418(3) . ? C1 C11 1.496(3) . ? C2 C3 1.392(3) . ? C3 C4 1.379(3) . ? C3 H3A 0.9300 . ? C4 C5 1.396(4) . ? C4 H4A 0.9300 . ? C5 C6 1.394(4) . ? C5 C10 1.518(4) . ? C6 C7 1.509(4) . ? C7 C8 1.522(7) . ? C7 C8' 1.523(8) . ? C7 H7A 0.9599 . ? C7 H7B 0.9599 . ? C7 H7C 0.9600 . ? C7 H7D 0.9600 . ? C8 C9 1.526(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.538(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8' C9' 1.541(9) . ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? C9' C10 1.501(7) . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C9' H10B 1.5339 . ? C10 H10A 0.9599 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H10D 0.9600 . ? C11 C12 1.404(3) . ? C11 C16 1.425(3) . ? C12 C13 1.386(3) . ? C13 C14 1.383(3) . ? C13 H13A 0.9300 . ? C14 C15 1.394(4) . ? C14 H14A 0.9300 . ? C15 C16 1.386(3) . ? C15 C20 1.520(4) . ? C16 C17 1.513(4) . ? C17 C18' 1.512(8) . ? C17 C18 1.517(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9601 . ? C17 H17C 0.9600 . ? C17 H17D 0.9600 . ? C18 C19 1.557(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.540(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H20D 1.5453 . ? C18' C19' 1.544(9) . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19' C20 1.529(8) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C19' H20A 1.5193 . ? C20 H20A 0.9600 . ? C20 H20B 0.9601 . ? C20 H20C 0.9600 . ? C20 H20D 0.9601 . ? C21 C22 1.464(9) . ? C21 C22' 1.521(5) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.522(9) . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 C29 1.525(8) . ? C26 C27 1.3900 . ? C26 H26A 0.9300 . ? C27 C30 1.521(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C22' C23' 1.3900 . ? C22' C27' 1.3900 . ? C23' C24' 1.3900 . ? C23' C28' 1.510(7) . ? C24' C25' 1.3900 . ? C24' H24B 0.9300 . ? C25' C26' 1.3900 . ? C25' C29' 1.526(6) . ? C26' C27' 1.3900 . ? C26' H26B 0.9300 . ? C27' C30' 1.499(7) . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? C31 C32' 1.505(4) . ? C31 C32 1.526(6) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C33 C38 1.515(9) . ? C34 C35 1.3900 . ? C34 H34A 0.9300 . ? C35 C36 1.3900 . ? C35 C39 1.542(8) . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C40 1.512(10) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C32' C33' 1.3900 . ? C32' C37' 1.3900 . ? C33' C34' 1.3900 . ? C33' C38' 1.525(7) . ? C34' C35' 1.3900 . ? C34' H34B 0.9300 . ? C35' C36' 1.3900 . ? C35' C39' 1.528(5) . ? C36' C37' 1.3900 . ? C36' H36B 0.9300 . ? C37' C40' 1.512(7) . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? C40' H40D 0.9600 . ? C40' H40E 0.9600 . ? C40' H40F 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 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 N3 Ti1 N4 101.38(9) . . ? N3 Ti1 O2 107.05(9) . . ? N4 Ti1 O2 95.07(8) . . ? N3 Ti1 O1 87.69(9) . . ? N4 Ti1 O1 100.63(8) . . ? O2 Ti1 O1 155.94(6) . . ? N3 Ti1 N1 147.67(8) . . ? N4 Ti1 N1 91.71(8) . . ? O2 Ti1 N1 100.98(7) . . ? O1 Ti1 N1 60.71(6) . . ? N3 Ti1 N2 105.01(8) . . ? N4 Ti1 N2 148.25(8) . . ? O2 Ti1 N2 60.50(6) . . ? O1 Ti1 N2 97.79(6) . . ? N1 Ti1 N2 75.13(7) . . ? N3 Ti1 C31 111.78(8) . . ? N4 Ti1 C31 121.41(8) . . ? O2 Ti1 C31 30.29(6) . . ? O1 Ti1 C31 126.67(7) . . ? N1 Ti1 C31 85.04(7) . . ? N2 Ti1 C31 30.51(6) . . ? N3 Ti1 C21 117.27(9) . . ? N4 Ti1 C21 99.28(8) . . ? O2 Ti1 C21 129.13(7) . . ? O1 Ti1 C21 30.22(6) . . ? N1 Ti1 C21 30.63(6) . . ? N2 Ti1 C21 84.08(7) . . ? C31 Ti1 C21 105.84(7) . . ? C21 O1 Ti1 96.30(12) . . ? C31 O2 Ti1 96.25(12) . . ? C21 N1 C2 129.73(19) . . ? C21 N1 Ti1 89.31(14) . . ? C2 N1 Ti1 135.32(14) . . ? C31 N2 C12 129.17(17) . . ? C31 N2 Ti1 88.67(12) . . ? C12 N2 Ti1 135.57(14) . . ? C42 N3 C41 111.2(3) . . ? C42 N3 Ti1 127.6(2) . . ? C41 N3 Ti1 119.88(19) . . ? C43 N4 C44 111.5(2) . . ? C43 N4 Ti1 122.08(18) . . ? C44 N4 Ti1 122.89(17) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 C11 121.34(18) . . ? C6 C1 C11 118.88(19) . . ? C3 C2 N1 119.2(2) . . ? C3 C2 C1 119.6(2) . . ? N1 C2 C1 120.5(2) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 121.1(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 119.7(2) . . ? C6 C5 C10 122.1(3) . . ? C4 C5 C10 118.0(2) . . ? C5 C6 C1 119.3(2) . . ? C5 C6 C7 120.3(2) . . ? C1 C6 C7 120.3(2) . . ? C6 C7 C8 114.4(5) . . ? C6 C7 C8' 114.2(6) . . ? C8 C7 C8' 23.6(5) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 107.0 . . ? C8' C7 H7A 125.4 . . ? C6 C7 H7B 108.3 . . ? C8 C7 H7B 110.8 . . ? C8' C7 H7B 89.7 . . ? H7A C7 H7B 107.6 . . ? C6 C7 H7C 109.3 . . ? C8 C7 H7C 85.4 . . ? C8' C7 H7C 106.9 . . ? H7A C7 H7C 24.3 . . ? H7B C7 H7C 127.2 . . ? C6 C7 H7D 108.8 . . ? C8 C7 H7D 127.2 . . ? C8' C7 H7D 109.7 . . ? H7A C7 H7D 85.8 . . ? H7B C7 H7D 23.4 . . ? H7C C7 H7D 107.9 . . ? C7 C8 C9 109.6(6) . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 108.6(8) . . ? C8 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? C8 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C7 C8' C9' 110.1(7) . . ? C7 C8' H8'A 109.6 . . ? C9' C8' H8'A 109.6 . . ? C7 C8' H8'B 109.6 . . ? C9' C8' H8'B 109.6 . . ? H8'A C8' H8'B 108.2 . . ? C10 C9' C8' 107.5(9) . . ? C10 C9' H9'A 110.2 . . ? C8' C9' H9'A 110.2 . . ? C10 C9' H9'B 110.2 . . ? C8' C9' H9'B 110.2 . . ? H9'A C9' H9'B 108.5 . . ? C10 C9' H10B 36.9 . . ? C8' C9' H10B 140.6 . . ? H9'A C9' H10B 101.2 . . ? H9'B C9' H10B 80.4 . . ? C9' C10 C5 112.1(4) . . ? C9' C10 C9 38.0(4) . . ? C5 C10 C9 112.3(4) . . ? C9' C10 H10A 135.8 . . ? C5 C10 H10A 108.7 . . ? C9 C10 H10A 109.7 . . ? C9' C10 H10B 73.5 . . ? C5 C10 H10B 109.5 . . ? C9 C10 H10B 108.5 . . ? H10A C10 H10B 108.1 . . ? C9' C10 H10C 110.4 . . ? C5 C10 H10C 109.1 . . ? C9 C10 H10C 75.3 . . ? H10A C10 H10C 37.8 . . ? H10B C10 H10C 135.8 . . ? C9' C10 H10D 108.3 . . ? C5 C10 H10D 108.9 . . ? C9 C10 H10D 134.8 . . ? H10A C10 H10D 72.8 . . ? H10B C10 H10D 37.9 . . ? H10C C10 H10D 108.0 . . ? C12 C11 C16 118.9(2) . . ? C12 C11 C1 122.24(18) . . ? C16 C11 C1 118.8(2) . . ? C13 C12 C11 119.55(19) . . ? C13 C12 N2 118.8(2) . . ? C11 C12 N2 120.82(19) . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.6(2) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 119.5(2) . . ? C16 C15 C20 121.7(3) . . ? C14 C15 C20 118.8(2) . . ? C15 C16 C11 120.1(2) . . ? C15 C16 C17 120.5(2) . . ? C11 C16 C17 119.3(2) . . ? C18' C17 C16 112.7(6) . . ? C18' C17 C18 23.2(5) . . ? C16 C17 C18 115.5(4) . . ? C18' C17 H17A 89.4 . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 108.8 . . ? C18' C17 H17B 127.3 . . ? C16 C17 H17B 108.0 . . ? C18 C17 H17B 107.7 . . ? H17A C17 H17B 107.6 . . ? C18' C17 H17C 109.1 . . ? C16 C17 H17C 109.4 . . ? C18 C17 H17C 124.7 . . ? H17A C17 H17C 22.7 . . ? H17B C17 H17C 86.4 . . ? C18' C17 H17D 108.5 . . ? C16 C17 H17D 108.9 . . ? C18 C17 H17D 86.4 . . ? H17A C17 H17D 126.9 . . ? H17B C17 H17D 24.1 . . ? H17C C17 H17D 108.1 . . ? C17 C18 C19 107.7(6) . . ? C17 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? C17 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C20 C19 C18 107.8(6) . . ? C20 C19 H19A 110.2 . . ? C18 C19 H19A 110.2 . . ? C20 C19 H19B 110.2 . . ? C18 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C20 C19 H20D 36.3 . . ? C18 C19 H20D 139.4 . . ? H19A C19 H20D 102.8 . . ? H19B C19 H20D 79.9 . . ? C17 C18' C19' 113.4(7) . . ? C17 C18' H18C 108.9 . . ? C19' C18' H18C 108.9 . . ? C17 C18' H18D 108.9 . . ? C19' C18' H18D 108.9 . . ? H18C C18' H18D 107.7 . . ? C20 C19' C18' 103.7(9) . . ? C20 C19' H19C 111.0 . . ? C18' C19' H19C 111.0 . . ? C20 C19' H19D 111.0 . . ? C18' C19' H19D 111.0 . . ? H19C C19' H19D 109.0 . . ? C20 C19' H20A 36.7 . . ? C18' C19' H20A 136.4 . . ? H19C C19' H20A 81.2 . . ? H19D C19' H20A 103.0 . . ? C15 C20 C19' 113.2(4) . . ? C15 C20 C19 112.7(3) . . ? C19' C20 C19 40.2(4) . . ? C15 C20 H20A 108.6 . . ? C19' C20 H20A 71.1 . . ? C19 C20 H20A 108.8 . . ? C15 C20 H20B 109.1 . . ? C19' C20 H20B 135.5 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 107.9 . . ? C15 C20 H20C 108.3 . . ? C19' C20 H20C 108.6 . . ? C19 C20 H20C 136.2 . . ? H20A C20 H20C 41.2 . . ? H20B C20 H20C 69.4 . . ? C15 C20 H20D 109.7 . . ? C19' C20 H20D 109.1 . . ? C19 C20 H20D 72.2 . . ? H20A C20 H20D 137.5 . . ? H20B C20 H20D 41.0 . . ? H20C C20 H20D 107.9 . . ? O1 C21 N1 113.2(2) . . ? O1 C21 C22 112.7(7) . . ? N1 C21 C22 134.0(7) . . ? O1 C21 C22' 122.0(5) . . ? N1 C21 C22' 124.4(5) . . ? C22 C21 C22' 13.0(8) . . ? O1 C21 Ti1 53.48(11) . . ? N1 C21 Ti1 60.06(12) . . ? C22 C21 Ti1 163.7(5) . . ? C22' C21 Ti1 175.5(5) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 124.9(9) . . ? C27 C22 C21 114.7(9) . . ? C24 C23 C22 120.0 . . ? C24 C23 C28 120.8(11) . . ? C22 C23 C28 118.8(11) . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 C29 115.9(9) . . ? C26 C25 C29 124.0(9) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 C30 113.1(12) . . ? C22 C27 C30 126.9(12) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23' C22' C27' 120.0 . . ? C23' C22' C21 116.1(5) . . ? C27' C22' C21 123.7(5) . . ? C24' C23' C22' 120.0 . . ? C24' C23' C28' 114.7(7) . . ? C22' C23' C28' 125.1(7) . . ? C23' C24' C25' 120.0 . . ? C23' C24' H24B 120.0 . . ? C25' C24' H24B 120.0 . . ? C26' C25' C24' 120.0 . . ? C26' C25' C29' 119.5(6) . . ? C24' C25' C29' 120.5(6) . . ? C25' C26' C27' 120.0 . . ? C25' C26' H26B 120.0 . . ? C27' C26' H26B 120.0 . . ? C26' C27' C22' 120.0 . . ? C26' C27' C30' 120.2(7) . . ? C22' C27' C30' 118.9(7) . . ? C23' C28' H28D 109.5 . . ? C23' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C23' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C25' C29' H29D 109.5 . . ? C25' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C25' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C27' C30' H30D 109.5 . . ? C27' C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C27' C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? O2 C31 N2 113.52(18) . . ? O2 C31 C32' 117.8(4) . . ? N2 C31 C32' 128.5(4) . . ? O2 C31 C32 122.4(7) . . ? N2 C31 C32 123.8(7) . . ? C32' C31 C32 9.8(9) . . ? O2 C31 Ti1 53.46(10) . . ? N2 C31 Ti1 60.82(11) . . ? C32' C31 Ti1 169.8(3) . . ? C32 C31 Ti1 165.9(6) . . ? C33 C32 C37 120.0 . . ? C33 C32 C31 122.7(9) . . ? C37 C32 C31 117.3(9) . . ? C34 C33 C32 120.0 . . ? C34 C33 C38 121.7(11) . . ? C32 C33 C38 116.4(11) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C39 122.0(9) . . ? C34 C35 C39 115.0(9) . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 C40 109.7(14) . . ? C32 C37 C40 130.2(14) . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C33' C32' C37' 120.0 . . ? C33' C32' C31 118.4(4) . . ? C37' C32' C31 120.4(4) . . ? C32' C33' C34' 120.0 . . ? C32' C33' C38' 125.5(6) . . ? C34' C33' C38' 114.3(6) . . ? C35' C34' C33' 120.0 . . ? C35' C34' H34B 120.0 . . ? C33' C34' H34B 120.0 . . ? C36' C35' C34' 120.0 . . ? C36' C35' C39' 119.4(4) . . ? C34' C35' C39' 120.4(4) . . ? C37' C36' C35' 120.0 . . ? C37' C36' H36B 120.0 . . ? C35' C36' H36B 120.0 . . ? C36' C37' C32' 120.0 . . ? C36' C37' C40' 119.9(6) . . ? C32' C37' C40' 119.6(6) . . ? C33' C38' H38D 109.5 . . ? C33' C38' H38E 109.5 . . ? H38D C38' H38E 109.5 . . ? C33' C38' H38F 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? C35' C39' H39D 109.5 . . ? C35' C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C35' C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C37' C40' H40D 109.5 . . ? C37' C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C37' C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 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 N3 Ti1 O1 C21 -168.64(14) . . . . ? N4 Ti1 O1 C21 90.22(14) . . . . ? O2 Ti1 O1 C21 -39.6(2) . . . . ? N1 Ti1 O1 C21 4.26(12) . . . . ? N2 Ti1 O1 C21 -63.79(14) . . . . ? C31 Ti1 O1 C21 -52.98(16) . . . . ? N3 Ti1 O2 C31 104.16(14) . . . . ? N4 Ti1 O2 C31 -152.29(14) . . . . ? O1 Ti1 O2 C31 -21.5(2) . . . . ? N1 Ti1 O2 C31 -59.55(14) . . . . ? N2 Ti1 O2 C31 6.23(13) . . . . ? C21 Ti1 O2 C31 -45.98(16) . . . . ? N3 Ti1 N1 C21 9.2(2) . . . . ? N4 Ti1 N1 C21 -105.44(14) . . . . ? O2 Ti1 N1 C21 159.06(13) . . . . ? O1 Ti1 N1 C21 -4.20(12) . . . . ? N2 Ti1 N1 C21 103.84(13) . . . . ? C31 Ti1 N1 C21 133.18(13) . . . . ? N3 Ti1 N1 C2 -144.6(2) . . . . ? N4 Ti1 N1 C2 100.8(2) . . . . ? O2 Ti1 N1 C2 5.3(2) . . . . ? O1 Ti1 N1 C2 -157.9(2) . . . . ? N2 Ti1 N1 C2 -49.90(19) . . . . ? C31 Ti1 N1 C2 -20.6(2) . . . . ? C21 Ti1 N1 C2 -153.7(3) . . . . ? N3 Ti1 N2 C31 -107.56(15) . . . . ? N4 Ti1 N2 C31 37.7(2) . . . . ? O2 Ti1 N2 C31 -6.19(13) . . . . ? O1 Ti1 N2 C31 162.76(14) . . . . ? N1 Ti1 N2 C31 105.93(14) . . . . ? C21 Ti1 N2 C31 135.76(14) . . . . ? N3 Ti1 N2 C12 100.9(2) . . . . ? N4 Ti1 N2 C12 -113.8(2) . . . . ? O2 Ti1 N2 C12 -157.7(2) . . . . ? O1 Ti1 N2 C12 11.3(2) . . . . ? N1 Ti1 N2 C12 -45.6(2) . . . . ? C31 Ti1 N2 C12 -151.5(3) . . . . ? C21 Ti1 N2 C12 -15.7(2) . . . . ? N4 Ti1 N3 C42 125.0(3) . . . . ? O2 Ti1 N3 C42 -136.0(3) . . . . ? O1 Ti1 N3 C42 24.6(3) . . . . ? N1 Ti1 N3 C42 13.0(4) . . . . ? N2 Ti1 N3 C42 -72.8(3) . . . . ? C31 Ti1 N3 C42 -104.2(3) . . . . ? C21 Ti1 N3 C42 18.2(3) . . . . ? N4 Ti1 N3 C41 -40.7(2) . . . . ? O2 Ti1 N3 C41 58.2(2) . . . . ? O1 Ti1 N3 C41 -141.1(2) . . . . ? N1 Ti1 N3 C41 -152.8(2) . . . . ? N2 Ti1 N3 C41 121.4(2) . . . . ? C31 Ti1 N3 C41 90.0(2) . . . . ? C21 Ti1 N3 C41 -147.5(2) . . . . ? N3 Ti1 N4 C43 -48.2(2) . . . . ? O2 Ti1 N4 C43 -156.8(2) . . . . ? O1 Ti1 N4 C43 41.5(2) . . . . ? N1 Ti1 N4 C43 102.0(2) . . . . ? N2 Ti1 N4 C43 165.9(2) . . . . ? C31 Ti1 N4 C43 -172.7(2) . . . . ? C21 Ti1 N4 C43 72.2(2) . . . . ? N3 Ti1 N4 C44 154.7(2) . . . . ? O2 Ti1 N4 C44 46.2(2) . . . . ? O1 Ti1 N4 C44 -115.5(2) . . . . ? N1 Ti1 N4 C44 -55.0(2) . . . . ? N2 Ti1 N4 C44 8.9(3) . . . . ? C31 Ti1 N4 C44 30.2(2) . . . . ? C21 Ti1 N4 C44 -84.9(2) . . . . ? C21 N1 C2 C3 116.9(3) . . . . ? Ti1 N1 C2 C3 -98.2(3) . . . . ? C21 N1 C2 C1 -72.8(3) . . . . ? Ti1 N1 C2 C1 72.1(3) . . . . ? C6 C1 C2 C3 3.2(3) . . . . ? C11 C1 C2 C3 -176.7(2) . . . . ? C6 C1 C2 N1 -167.1(2) . . . . ? C11 C1 C2 N1 13.0(3) . . . . ? N1 C2 C3 C4 171.3(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C2 C3 C4 C5 -2.6(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C3 C4 C5 C10 -176.4(3) . . . . ? C4 C5 C6 C1 4.1(4) . . . . ? C10 C5 C6 C1 -179.7(3) . . . . ? C4 C5 C6 C7 -171.6(3) . . . . ? C10 C5 C6 C7 4.7(4) . . . . ? C2 C1 C6 C5 -5.7(4) . . . . ? C11 C1 C6 C5 174.2(2) . . . . ? C2 C1 C6 C7 170.0(2) . . . . ? C11 C1 C6 C7 -10.1(4) . . . . ? C5 C6 C7 C8 -18.2(6) . . . . ? C1 C6 C7 C8 166.2(5) . . . . ? C5 C6 C7 C8' 7.7(6) . . . . ? C1 C6 C7 C8' -167.9(5) . . . . ? C6 C7 C8 C9 48.2(12) . . . . ? C8' C7 C8 C9 -46.9(15) . . . . ? C7 C8 C9 C10 -64.7(13) . . . . ? C6 C7 C8' C9' -42.8(12) . . . . ? C8 C7 C8' C9' 52.9(15) . . . . ? C7 C8' C9' C10 66.3(14) . . . . ? C8' C9' C10 C5 -53.6(11) . . . . ? C8' C9' C10 C9 44.8(7) . . . . ? C6 C5 C10 C9' 19.6(7) . . . . ? C4 C5 C10 C9' -164.0(6) . . . . ? C6 C5 C10 C9 -21.5(6) . . . . ? C4 C5 C10 C9 154.8(5) . . . . ? C8 C9 C10 C9' -47.1(7) . . . . ? C8 C9 C10 C5 50.7(10) . . . . ? C2 C1 C11 C12 -65.1(3) . . . . ? C6 C1 C11 C12 115.0(2) . . . . ? C2 C1 C11 C16 114.9(2) . . . . ? C6 C1 C11 C16 -65.0(3) . . . . ? C16 C11 C12 C13 6.3(3) . . . . ? C1 C11 C12 C13 -173.7(2) . . . . ? C16 C11 C12 N2 -163.47(19) . . . . ? C1 C11 C12 N2 16.5(3) . . . . ? C31 N2 C12 C13 114.1(3) . . . . ? Ti1 N2 C12 C13 -103.8(3) . . . . ? C31 N2 C12 C11 -76.0(3) . . . . ? Ti1 N2 C12 C11 66.0(3) . . . . ? C11 C12 C13 C14 -0.2(4) . . . . ? N2 C12 C13 C14 169.8(2) . . . . ? C12 C13 C14 C15 -4.5(4) . . . . ? C13 C14 C15 C16 2.9(4) . . . . ? C13 C14 C15 C20 -174.6(3) . . . . ? C14 C15 C16 C11 3.4(4) . . . . ? C20 C15 C16 C11 -179.3(3) . . . . ? C14 C15 C16 C17 -172.5(3) . . . . ? C20 C15 C16 C17 4.8(4) . . . . ? C12 C11 C16 C15 -7.9(3) . . . . ? C1 C11 C16 C15 172.1(2) . . . . ? C12 C11 C16 C17 168.0(2) . . . . ? C1 C11 C16 C17 -12.0(3) . . . . ? C15 C16 C17 C18' -13.6(6) . . . . ? C11 C16 C17 C18' 170.4(5) . . . . ? C15 C16 C17 C18 11.6(5) . . . . ? C11 C16 C17 C18 -164.3(4) . . . . ? C18' C17 C18 C19 41.7(15) . . . . ? C16 C17 C18 C19 -46.7(8) . . . . ? C17 C18 C19 C20 66.2(9) . . . . ? C16 C17 C18' C19' 46.2(12) . . . . ? C18 C17 C18' C19' -55.8(14) . . . . ? C17 C18' C19' C20 -66.0(13) . . . . ? C16 C15 C20 C19' -27.6(6) . . . . ? C14 C15 C20 C19' 149.8(6) . . . . ? C16 C15 C20 C19 16.3(6) . . . . ? C14 C15 C20 C19 -166.4(4) . . . . ? C18' C19' C20 C15 54.5(9) . . . . ? C18' C19' C20 C19 -43.8(6) . . . . ? C18 C19 C20 C15 -51.2(8) . . . . ? C18 C19 C20 C19' 48.3(6) . . . . ? Ti1 O1 C21 N1 -6.9(2) . . . . ? Ti1 O1 C21 C22 170.0(8) . . . . ? Ti1 O1 C21 C22' -179.8(5) . . . . ? C2 N1 C21 O1 162.5(2) . . . . ? Ti1 N1 C21 O1 6.38(18) . . . . ? C2 N1 C21 C22 -13.5(10) . . . . ? Ti1 N1 C21 C22 -169.6(10) . . . . ? C2 N1 C21 C22' -24.8(6) . . . . ? Ti1 N1 C21 C22' 179.1(6) . . . . ? C2 N1 C21 Ti1 156.1(3) . . . . ? N3 Ti1 C21 O1 12.80(16) . . . . ? N4 Ti1 C21 O1 -95.21(14) . . . . ? O2 Ti1 C21 O1 160.41(12) . . . . ? N1 Ti1 C21 O1 -172.7(2) . . . . ? N2 Ti1 C21 O1 116.66(13) . . . . ? C31 Ti1 C21 O1 138.26(13) . . . . ? N3 Ti1 C21 N1 -174.50(13) . . . . ? N4 Ti1 C21 N1 77.49(14) . . . . ? O2 Ti1 C21 N1 -26.89(16) . . . . ? O1 Ti1 C21 N1 172.7(2) . . . . ? N2 Ti1 C21 N1 -70.64(13) . . . . ? C31 Ti1 C21 N1 -49.04(14) . . . . ? N3 Ti1 C21 C22 -22(3) . . . . ? N4 Ti1 C21 C22 -130(3) . . . . ? O2 Ti1 C21 C22 126(3) . . . . ? O1 Ti1 C21 C22 -35(3) . . . . ? N1 Ti1 C21 C22 153(3) . . . . ? N2 Ti1 C21 C22 82(3) . . . . ? C31 Ti1 C21 C22 104(3) . . . . ? N3 Ti1 C21 C22' 15(5) . . . . ? N4 Ti1 C21 C22' -93(5) . . . . ? O2 Ti1 C21 C22' 163(5) . . . . ? O1 Ti1 C21 C22' 2(5) . . . . ? N1 Ti1 C21 C22' -170(6) . . . . ? N2 Ti1 C21 C22' 119(5) . . . . ? C31 Ti1 C21 C22' 141(5) . . . . ? O1 C21 C22 C23 -58.8(13) . . . . ? N1 C21 C22 C23 117.2(10) . . . . ? C22' C21 C22 C23 163(7) . . . . ? Ti1 C21 C22 C23 -29(4) . . . . ? O1 C21 C22 C27 128.1(8) . . . . ? N1 C21 C22 C27 -55.9(14) . . . . ? C22' C21 C22 C27 -10(5) . . . . ? Ti1 C21 C22 C27 158(2) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 -172.8(16) . . . . ? C27 C22 C23 C28 -173.1(17) . . . . ? C21 C22 C23 C28 14.2(17) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C28 C23 C24 C25 172.9(17) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C29 176.7(13) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C29 C25 C26 C27 -176.5(14) . . . . ? C25 C26 C27 C22 0.0 . . . . ? C25 C26 C27 C30 -178.6(17) . . . . ? C23 C22 C27 C26 0.0 . . . . ? C21 C22 C27 C26 173.5(14) . . . . ? C23 C22 C27 C30 178.3(19) . . . . ? C21 C22 C27 C30 -8.2(17) . . . . ? O1 C21 C22' C23' -57.4(8) . . . . ? N1 C21 C22' C23' 130.6(5) . . . . ? C22 C21 C22' C23' -11(5) . . . . ? Ti1 C21 C22' C23' -60(6) . . . . ? O1 C21 C22' C27' 117.8(6) . . . . ? N1 C21 C22' C27' -54.3(9) . . . . ? C22 C21 C22' C27' 164(6) . . . . ? Ti1 C21 C22' C27' 116(5) . . . . ? C27' C22' C23' C24' 0.0 . . . . ? C21 C22' C23' C24' 175.4(9) . . . . ? C27' C22' C23' C28' -174.7(12) . . . . ? C21 C22' C23' C28' 0.7(11) . . . . ? C22' C23' C24' C25' 0.0 . . . . ? C28' C23' C24' C25' 175.2(11) . . . . ? C23' C24' C25' C26' 0.0 . . . . ? C23' C24' C25' C29' 177.8(9) . . . . ? C24' C25' C26' C27' 0.0 . . . . ? C29' C25' C26' C27' -177.8(8) . . . . ? C25' C26' C27' C22' 0.0 . . . . ? C25' C26' C27' C30' -169.5(11) . . . . ? C23' C22' C27' C26' 0.0 . . . . ? C21 C22' C27' C26' -175.0(10) . . . . ? C23' C22' C27' C30' 169.6(11) . . . . ? C21 C22' C27' C30' -5.4(11) . . . . ? Ti1 O2 C31 N2 -10.2(2) . . . . ? Ti1 O2 C31 C32' 173.7(4) . . . . ? Ti1 O2 C31 C32 163.6(7) . . . . ? C12 N2 C31 O2 163.9(2) . . . . ? Ti1 N2 C31 O2 9.39(19) . . . . ? C12 N2 C31 C32' -20.6(5) . . . . ? Ti1 N2 C31 C32' -175.1(4) . . . . ? C12 N2 C31 C32 -9.9(8) . . . . ? Ti1 N2 C31 C32 -164.4(7) . . . . ? C12 N2 C31 Ti1 154.5(3) . . . . ? N3 Ti1 C31 O2 -86.66(15) . . . . ? N4 Ti1 C31 O2 32.87(17) . . . . ? O1 Ti1 C31 O2 169.25(12) . . . . ? N1 Ti1 C31 O2 121.85(14) . . . . ? N2 Ti1 C31 O2 -169.3(2) . . . . ? C21 Ti1 C31 O2 144.56(13) . . . . ? N3 Ti1 C31 N2 82.61(15) . . . . ? N4 Ti1 C31 N2 -157.86(14) . . . . ? O2 Ti1 C31 N2 169.3(2) . . . . ? O1 Ti1 C31 N2 -21.48(17) . . . . ? N1 Ti1 C31 N2 -68.88(14) . . . . ? C21 Ti1 C31 N2 -46.17(14) . . . . ? N3 Ti1 C31 C32' -120(2) . . . . ? N4 Ti1 C31 C32' 0(2) . . . . ? O2 Ti1 C31 C32' -33(2) . . . . ? O1 Ti1 C31 C32' 136(2) . . . . ? N1 Ti1 C31 C32' 89(2) . . . . ? N2 Ti1 C31 C32' 158(2) . . . . ? C21 Ti1 C31 C32' 112(2) . . . . ? N3 Ti1 C31 C32 -164(3) . . . . ? N4 Ti1 C31 C32 -45(3) . . . . ? O2 Ti1 C31 C32 -78(3) . . . . ? O1 Ti1 C31 C32 92(3) . . . . ? N1 Ti1 C31 C32 44(3) . . . . ? N2 Ti1 C31 C32 113(3) . . . . ? C21 Ti1 C31 C32 67(3) . . . . ? O2 C31 C32 C33 128.9(10) . . . . ? N2 C31 C32 C33 -57.9(15) . . . . ? C32' C31 C32 C33 64(5) . . . . ? Ti1 C31 C32 C33 -162.8(18) . . . . ? O2 C31 C32 C37 -50.8(8) . . . . ? N2 C31 C32 C37 122.4(6) . . . . ? C32' C31 C32 C37 -116(5) . . . . ? Ti1 C31 C32 C37 17(3) . . . . ? C37 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C34 -179.8(14) . . . . ? C37 C32 C33 C38 164.5(14) . . . . ? C31 C32 C33 C38 -15.2(18) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C38 C33 C34 C35 -163.7(15) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C39 -160.7(12) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C39 C35 C36 C37 159.4(13) . . . . ? C35 C36 C37 C32 0.0 . . . . ? C35 C36 C37 C40 177(2) . . . . ? C33 C32 C37 C36 0.0 . . . . ? C31 C32 C37 C36 179.8(13) . . . . ? C33 C32 C37 C40 -176(3) . . . . ? C31 C32 C37 C40 4(2) . . . . ? O2 C31 C32' C33' 124.4(5) . . . . ? N2 C31 C32' C33' -51.0(7) . . . . ? C32 C31 C32' C33' -116(5) . . . . ? Ti1 C31 C32' C33' 154.1(16) . . . . ? O2 C31 C32' C37' -68.4(4) . . . . ? N2 C31 C32' C37' 116.3(4) . . . . ? C32 C31 C32' C37' 51(5) . . . . ? Ti1 C31 C32' C37' -39(2) . . . . ? C37' C32' C33' C34' 0.0 . . . . ? C31 C32' C33' C34' 167.3(6) . . . . ? C37' C32' C33' C38' 175.1(7) . . . . ? C31 C32' C33' C38' -17.6(9) . . . . ? C32' C33' C34' C35' 0.0 . . . . ? C38' C33' C34' C35' -175.6(6) . . . . ? C33' C34' C35' C36' 0.0 . . . . ? C33' C34' C35' C39' -174.8(7) . . . . ? C34' C35' C36' C37' 0.0 . . . . ? C39' C35' C36' C37' 174.9(7) . . . . ? C35' C36' C37' C32' 0.0 . . . . ? C35' C36' C37' C40' 172.0(10) . . . . ? C33' C32' C37' C36' 0.0 . . . . ? C31 C32' C37' C36' -167.0(7) . . . . ? C33' C32' C37' C40' -172.1(10) . . . . ? C31 C32' C37' C40' 20.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.296 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.034 # Attachment 'compound_15.cif' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 742601' #TrackingRef 'compound_15.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 N4 O4 S2 Ti' _chemical_formula_sum 'C42 H54 N4 O4 S2 Ti' _chemical_formula_weight 790.91 _chemical_absolute_configuration rmad 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 11.4515(4) _cell_length_b 11.4515(4) _cell_length_c 26.7751(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3040.8(2) _cell_formula_units_Z 3 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6863 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.9 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9122 _exptl_absorpt_correction_T_max 0.9649 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area dector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20696 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.85 _reflns_number_total 4816 _reflns_number_gt 4342 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0749P)^2^+2.3821P] 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 0.0067(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(6) _refine_ls_number_reflns 4816 _refine_ls_number_parameters 303 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1641 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.007 _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 O2 O 0.755(4) 0.4208(7) 0.4246(5) 0.034(3) Uani 0.50 1 d P A -1 C1 C 0.3603(5) 0.3027(8) 0.5114(3) 0.0264(9) Uani 0.50 1 d PGD A -1 C2 C 0.4849(5) 0.3336(7) 0.4918(2) 0.0257(9) Uani 0.50 1 d PGD A -1 C3 C 0.5452(5) 0.2595(8) 0.5062(2) 0.0366(11) Uani 0.50 1 d PG A -1 H3A H 0.6303 0.2806 0.4928 0.044 Uiso 0.50 1 calc PR A -1 C4 C 0.4809(6) 0.1545(8) 0.5402(3) 0.0393(12) Uani 0.50 1 d PG A -1 H4A H 0.5221 0.1038 0.5501 0.047 Uiso 0.50 1 calc PR A -1 C5 C 0.3563(6) 0.1236(8) 0.5598(3) 0.0368(12) Uani 0.50 1 d PGD A -1 C6 C 0.2960(5) 0.1977(10) 0.5454(4) 0.0330(13) Uani 0.50 1 d PGD A -1 C7 C 0.1694(8) 0.1702(8) 0.5727(3) 0.0356(19) Uani 0.50 1 d PD A -1 H7A H 0.0926 0.1312 0.5491 0.043 Uiso 0.50 1 calc PR A -1 H7B H 0.1801 0.2562 0.5853 0.043 Uiso 0.50 1 calc PR A -1 C8 C 0.1381(9) 0.0731(9) 0.6164(3) 0.061(2) Uani 0.50 1 d PD A -1 H8A H 0.0442 0.0394 0.6276 0.073 Uiso 0.50 1 calc PR A -1 H8B H 0.1987 0.1223 0.6446 0.073 Uiso 0.50 1 calc PR A -1 C9 C 0.1557(8) -0.0474(8) 0.6022(3) 0.077(3) Uani 0.50 1 d PD A -1 H9A H 0.1175 -0.0828 0.5688 0.092 Uiso 0.50 1 calc PR A -1 H9B H 0.1122 -0.1209 0.6270 0.092 Uiso 0.50 1 calc PR A -1 C10 C 0.3149(9) 0.0163(10) 0.6024(4) 0.0570(19) Uani 0.50 1 d PD A -1 H10A H 0.3547 0.0589 0.6349 0.068 Uiso 0.50 1 calc PR A -1 H10B H 0.3412 -0.0519 0.5944 0.068 Uiso 0.50 1 calc PR A -1 C11 C 0.2976(8) 0.3818(5) 0.4896(4) 0.0264(9) Uani 0.50 1 d PGD A -1 C12 C 0.3437(7) 0.5151(5) 0.5031(3) 0.0257(9) Uani 0.50 1 d PGD A -1 C13 C 0.2800(8) 0.5824(4) 0.4847(2) 0.0366(11) Uani 0.50 1 d PG A -1 H13A H 0.3115 0.6734 0.4940 0.044 Uiso 0.50 1 calc PR A -1 C14 C 0.1701(8) 0.5164(6) 0.4529(3) 0.0393(12) Uani 0.50 1 d PG A -1 H14A H 0.1266 0.5624 0.4403 0.047 Uiso 0.50 1 calc PR A -1 C15 C 0.1240(9) 0.3832(6) 0.4394(3) 0.0368(12) Uani 0.50 1 d PGD A -1 C16 C 0.1877(10) 0.3159(4) 0.4577(4) 0.0330(13) Uani 0.50 1 d PGD A -1 C17 C 0.1549(8) 0.1763(8) 0.4403(3) 0.0356(19) Uani 0.50 1 d PD A -1 H17A H 0.2392 0.1828 0.4276 0.043 Uiso 0.50 1 calc PR A -1 H17B H 0.1266 0.1162 0.4698 0.043 Uiso 0.50 1 calc PR A -1 C19 C -0.0108(12) 0.1863(8) 0.3805(4) 0.077(3) Uani 0.50 1 d PD A -1 H19A H 0.0286 0.2185 0.3470 0.092 Uiso 0.50 1 calc PR A -1 H19B H -0.1083 0.1228 0.3757 0.092 Uiso 0.50 1 calc PR A -1 C18 C 0.0485(10) 0.1094(8) 0.4008(3) 0.061(2) Uani 0.50 1 d PD A -1 H18A H 0.0881 0.0847 0.3727 0.073 Uiso 0.50 1 calc PR A -1 H18B H -0.0253 0.0245 0.4149 0.073 Uiso 0.50 1 calc PR A -1 C20 C 0.0021(11) 0.3020(9) 0.4079(4) 0.0570(19) Uani 0.50 1 d PD A -1 H20A H -0.0778 0.2692 0.4299 0.068 Uiso 0.50 1 calc PR A -1 H20B H -0.0030 0.3639 0.3833 0.068 Uiso 0.50 1 calc PR A -1 Ti1 Ti 0.65087(11) 0.61898(12) 0.52528(4) 0.0297(3) Uani 0.50 1 d P A -1 N3 N 0.8094(13) 0.6324(12) 0.5560(3) 0.043(3) Uani 0.50 1 d PD A -1 C39 C 0.9042(8) 0.6151(11) 0.5236(3) 0.053(2) Uani 0.50 1 d PD A -1 H39A H 0.9970 0.6784 0.5339 0.080 Uiso 0.50 1 calc PR A -1 H39B H 0.8914 0.6329 0.4888 0.080 Uiso 0.50 1 calc PR A -1 H39C H 0.8871 0.5226 0.5266 0.080 Uiso 0.50 1 calc PR A -1 C40 C 0.8346(8) 0.6283(13) 0.6101(3) 0.065(3) Uani 0.50 1 d PD A -1 H40A H 0.9264 0.6998 0.6182 0.097 Uiso 0.50 1 calc PR A -1 H40B H 0.8245 0.5405 0.6186 0.097 Uiso 0.50 1 calc PR A -1 H40C H 0.7697 0.6420 0.6294 0.097 Uiso 0.50 1 calc PR A -1 N4 N 0.7219(5) 0.7780(6) 0.4883(2) 0.0403(14) Uani 0.50 1 d PD A -1 C41 C 0.8654(6) 0.8786(8) 0.4813(3) 0.051(2) Uani 0.50 1 d PD A -1 H41A H 0.8826 0.9666 0.4934 0.076 Uiso 0.50 1 calc PR A -1 H41B H 0.8882 0.8850 0.4458 0.076 Uiso 0.50 1 calc PR A -1 H41C H 0.9210 0.8510 0.5002 0.076 Uiso 0.50 1 calc PR A -1 C42 C 0.6242(13) 0.8043(19) 0.4591(6) 0.057(4) Uani 0.50 1 d PD A -1 H42A H 0.6376 0.8932 0.4679 0.086 Uiso 0.50 1 calc PR A -1 H42B H 0.5315 0.7349 0.4671 0.086 Uiso 0.50 1 calc PR A -1 H42C H 0.6401 0.8017 0.4232 0.086 Uiso 0.50 1 calc PR A -1 O4 O 0.4449(7) 0.754(4) 0.5758(6) 0.034(3) Uani 0.50 1 d P A -1 N2 N 0.4751(7) 0.5910(6) 0.5281(2) 0.0252(8) Uani 0.50 1 d PD A -1 N1 N 0.5537(6) 0.4509(7) 0.4606(2) 0.0252(8) Uani 0.50 1 d PD A -1 S2 S 0.4801(7) 0.6673(4) 0.5792(2) 0.0281(3) Uani 0.50 1 d PD A -1 S1 S 0.6416(4) 0.4631(7) 0.4126(2) 0.0281(3) Uani 0.50 1 d PD A -1 C30 C 0.3684(5) 0.5394(4) 0.62220(16) 0.0280(10) Uani 0.50 1 d PGD A -1 C31 C 0.4156(4) 0.4627(5) 0.64561(17) 0.0295(10) Uani 0.50 1 d PGD A -1 C32 C 0.3464(5) 0.3820(4) 0.68622(16) 0.0353(14) Uani 0.50 1 d PGD A -1 H32A H 0.3787 0.3296 0.7022 0.042 Uiso 0.50 1 calc PR A -1 C33 C 0.2299(5) 0.3780(4) 0.70341(15) 0.052(2) Uani 0.50 1 d PGD A -1 C34 C 0.1827(4) 0.4547(5) 0.68000(17) 0.0418(15) Uani 0.50 1 d PGD A -1 H34A H 0.1031 0.4520 0.6918 0.050 Uiso 0.50 1 calc PR A -1 C35 C 0.2519(5) 0.5354(4) 0.63939(17) 0.0342(13) Uani 0.50 1 d PGD A -1 C36 C 0.5395(7) 0.4591(7) 0.6281(3) 0.0368(13) Uani 0.50 1 d PD A -1 H36A H 0.5461 0.3881 0.6461 0.055 Uiso 0.50 1 calc PR A -1 H36B H 0.6201 0.5464 0.6347 0.055 Uiso 0.50 1 calc PR A -1 H36C H 0.5323 0.4403 0.5922 0.055 Uiso 0.50 1 calc PR A -1 C37 C 0.1538(9) 0.2924(8) 0.7479(3) 0.072(3) Uani 0.50 1 d PD A -1 H37A H 0.1828 0.2266 0.7545 0.107 Uiso 0.50 1 calc PR A -1 H37B H 0.0569 0.2449 0.7409 0.107 Uiso 0.50 1 calc PR A -1 H37C H 0.1724 0.3504 0.7773 0.107 Uiso 0.50 1 calc PR A -1 C38 C 0.1882(10) 0.6115(8) 0.6163(3) 0.0413(15) Uani 0.50 1 d PD A -1 H38A H 0.1021 0.5847 0.6329 0.062 Uiso 0.50 1 calc PR A -1 H38B H 0.1727 0.5901 0.5806 0.062 Uiso 0.50 1 calc PR A -1 H38C H 0.2488 0.7086 0.6205 0.062 Uiso 0.50 1 calc PR A -1 C21 C 0.5344(4) 0.3533(5) 0.36457(15) 0.0280(10) Uani 0.50 1 d PGD A -1 C22 C 0.4464(5) 0.3843(4) 0.34005(17) 0.0295(10) Uani 0.50 1 d PGD A -1 C23 C 0.3799(4) 0.3141(5) 0.29718(16) 0.0353(14) Uani 0.50 1 d PGD A -1 H23A H 0.3197 0.3353 0.2804 0.042 Uiso 0.50 1 calc PR A -1 C24 C 0.4014(5) 0.2129(4) 0.27883(15) 0.052(2) Uani 0.50 1 d PGD A -1 C25 C 0.4894(5) 0.1818(4) 0.30335(18) 0.0418(15) Uani 0.50 1 d PGD A -1 H25A H 0.5041 0.1126 0.2908 0.050 Uiso 0.50 1 calc PR A -1 C26 C 0.5559(4) 0.2520(5) 0.34622(17) 0.0342(13) Uani 0.50 1 d PGD A -1 C27 C 0.4144(7) 0.4914(7) 0.3576(3) 0.0368(13) Uani 0.50 1 d PD A -1 H27A H 0.4268 0.5024 0.3939 0.055 Uiso 0.50 1 calc PR A -1 H27B H 0.3208 0.4637 0.3493 0.055 Uiso 0.50 1 calc PR A -1 H27C H 0.4750 0.5772 0.3411 0.055 Uiso 0.50 1 calc PR A -1 C28 C 0.3309(9) 0.1387(9) 0.2323(3) 0.072(3) Uani 0.50 1 d PD A -1 H28A H 0.2924 0.0416 0.2375 0.107 Uiso 0.50 1 calc PR A -1 H28B H 0.3955 0.1682 0.2046 0.107 Uiso 0.50 1 calc PR A -1 H28C H 0.2585 0.1577 0.2242 0.107 Uiso 0.50 1 calc PR A -1 C29 C 0.6456(7) 0.2052(9) 0.3701(3) 0.0413(15) Uani 0.50 1 d PD A -1 H29A H 0.6368 0.1271 0.3517 0.062 Uiso 0.50 1 calc PR A -1 H29B H 0.6182 0.1798 0.4049 0.062 Uiso 0.50 1 calc PR A -1 H29C H 0.7396 0.2784 0.3690 0.062 Uiso 0.50 1 calc PR A -1 O1 O 0.6824(6) 0.6046(13) 0.4004(2) 0.0354(9) Uani 0.50 1 d P A -1 O3 O 0.6169(14) 0.7298(6) 0.5973(2) 0.0354(9) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.026(2) 0.030(2) 0.0446(14) -0.003(3) 0.005(3) 0.014(6) C1 0.024(2) 0.024(3) 0.0274(15) -0.001(3) -0.008(3) 0.0093(17) C2 0.034(3) 0.022(2) 0.0213(17) 0.007(2) 0.000(2) 0.013(2) C3 0.040(3) 0.040(3) 0.035(3) 0.004(2) -0.002(2) 0.024(3) C4 0.049(4) 0.035(3) 0.038(2) -0.002(2) -0.020(3) 0.024(3) C5 0.034(3) 0.033(3) 0.0340(17) 0.005(3) -0.011(3) 0.010(2) C6 0.036(3) 0.022(2) 0.0293(19) 0.011(3) -0.002(3) 0.0054(18) C7 0.031(3) 0.042(3) 0.009(4) -0.001(2) -0.007(2) -0.0009(18) C8 0.054(4) 0.057(4) 0.040(5) -0.017(3) -0.030(3) 0.004(3) C9 0.084(6) 0.037(3) 0.066(5) 0.007(3) -0.057(4) -0.002(4) C10 0.074(6) 0.043(4) 0.028(4) 0.014(3) -0.015(3) 0.010(3) C11 0.024(2) 0.024(3) 0.0274(15) -0.001(3) -0.008(3) 0.0093(17) C12 0.034(3) 0.022(2) 0.0213(17) 0.007(2) 0.000(2) 0.013(2) C13 0.040(3) 0.040(3) 0.035(3) 0.004(2) -0.002(2) 0.024(3) C14 0.049(4) 0.035(3) 0.038(2) -0.002(2) -0.020(3) 0.024(3) C15 0.034(3) 0.033(3) 0.0340(17) 0.005(3) -0.011(3) 0.010(2) C16 0.036(3) 0.022(2) 0.0293(19) 0.011(3) -0.002(3) 0.0054(18) C17 0.031(3) 0.042(3) 0.009(4) -0.001(2) -0.007(2) -0.0009(18) C19 0.084(6) 0.037(3) 0.066(5) 0.007(3) -0.057(4) -0.002(4) C18 0.054(4) 0.057(4) 0.040(5) -0.017(3) -0.030(3) 0.004(3) C20 0.074(6) 0.043(4) 0.028(4) 0.014(3) -0.015(3) 0.010(3) Ti1 0.0233(6) 0.0310(6) 0.0283(6) -0.0004(5) -0.0012(4) 0.0087(5) N3 0.027(5) 0.052(6) 0.043(6) -0.020(4) -0.015(4) 0.014(4) C39 0.032(4) 0.080(6) 0.047(4) -0.019(4) -0.004(3) 0.029(4) C40 0.036(4) 0.114(9) 0.044(5) -0.013(5) -0.018(4) 0.037(5) N4 0.027(3) 0.024(3) 0.045(3) -0.005(2) 0.004(2) -0.007(2) C41 0.028(4) 0.033(4) 0.064(5) 0.002(3) 0.010(3) -0.006(3) C42 0.053(7) 0.047(7) 0.070(10) 0.042(7) 0.033(7) 0.024(5) O4 0.026(2) 0.030(2) 0.0446(14) -0.003(3) 0.005(3) 0.014(6) N2 0.028(3) 0.022(2) 0.021(2) 0.0027(14) -0.0006(15) 0.009(2) N1 0.028(3) 0.022(2) 0.021(2) 0.0027(14) -0.0006(15) 0.009(2) S2 0.0279(14) 0.0278(14) 0.0238(15) 0.0015(6) 0.0021(6) 0.0105(14) S1 0.0279(14) 0.0278(14) 0.0238(15) 0.0015(6) 0.0021(6) 0.0105(14) C30 0.024(3) 0.031(3) 0.024(3) 0.008(2) 0.0087(18) 0.0101(15) C31 0.030(3) 0.032(3) 0.021(3) -0.0005(18) -0.0040(18) 0.012(2) C32 0.042(3) 0.035(3) 0.028(4) -0.004(2) -0.006(2) 0.018(2) C33 0.058(4) 0.038(3) 0.036(4) 0.003(2) -0.008(3) 0.006(3) C34 0.036(3) 0.037(3) 0.044(4) -0.004(2) 0.001(2) 0.012(2) C35 0.031(3) 0.029(3) 0.036(4) -0.004(2) 0.003(2) 0.0107(18) C36 0.044(4) 0.040(4) 0.029(3) 0.005(2) -0.003(2) 0.023(4) C37 0.074(5) 0.073(5) 0.042(5) -0.006(3) -0.006(3) 0.017(4) C38 0.036(3) 0.030(3) 0.054(5) -0.009(2) -0.004(3) 0.014(3) C21 0.024(3) 0.031(3) 0.024(3) 0.008(2) 0.0087(18) 0.0101(15) C22 0.030(3) 0.032(3) 0.021(3) -0.0005(18) -0.0040(18) 0.012(2) C23 0.042(3) 0.035(3) 0.028(4) -0.004(2) -0.006(2) 0.018(2) C24 0.058(4) 0.038(3) 0.036(4) 0.003(2) -0.008(3) 0.006(3) C25 0.036(3) 0.037(3) 0.044(4) -0.004(2) 0.001(2) 0.012(2) C26 0.031(3) 0.029(3) 0.036(4) -0.004(2) 0.003(2) 0.0107(18) C27 0.044(4) 0.040(4) 0.029(3) 0.005(2) -0.003(2) 0.023(4) C28 0.074(5) 0.073(5) 0.042(5) -0.006(3) -0.006(3) 0.017(4) C29 0.036(3) 0.030(3) 0.054(5) -0.009(2) -0.004(3) 0.014(3) O1 0.031(3) 0.027(3) 0.0339(14) 0.0019(16) -0.0011(16) 0.004(4) O3 0.031(3) 0.027(3) 0.0339(14) 0.0019(16) -0.0011(16) 0.004(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 O2 S1 1.63(4) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C11 1.524(3) . ? C2 C3 1.3900 . ? C2 N1 1.436(7) . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 C10 1.566(8) . ? C6 C7 1.509(8) . ? C7 C8 1.528(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.539(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.589(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 N2 1.469(8) . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 C16 1.3900 . ? C15 C20 1.491(9) . ? C16 C17 1.521(8) . ? C17 C18 1.502(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 C20 1.455(8) . ? C19 C18 1.459(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Ti1 N4 1.864(6) . ? Ti1 N2 1.874(8) . ? Ti1 N3 1.928(11) . ? Ti1 N1 2.407(6) . ? Ti1 O3 2.444(7) . ? Ti1 S2 2.701(3) . ? N3 C39 1.479(10) . ? N3 C40 1.484(9) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N4 C41 1.473(7) . ? N4 C42 1.515(9) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O4 S2 1.24(4) . ? N2 S2 1.609(6) . ? N1 S1 1.595(6) . ? S2 O3 1.442(16) . ? S2 C30 1.799(4) . ? S1 O1 1.481(15) . ? S1 C21 1.789(4) . ? C30 C31 1.3900 . ? C30 C35 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.513(6) . ? C32 C33 1.3900 . ? C32 H32A 0.9500 . ? C33 C34 1.3900 . ? C33 C37 1.512(6) . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C38 1.519(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.519(5) . ? C23 C24 1.3900 . ? C23 H23A 0.9500 . ? C24 C25 1.3900 . ? C24 C28 1.497(6) . ? C25 C26 1.3900 . ? C25 H25A 0.9500 . ? C26 C29 1.516(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 C2 C1 C6 120.0 . . ? C2 C1 C11 115.6(5) . . ? C6 C1 C11 124.1(5) . . ? C1 C2 C3 120.0 . . ? C1 C2 N1 118.1(5) . . ? C3 C2 N1 121.6(5) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C10 110.1(6) . . ? C6 C5 C10 129.3(6) . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 117.2(6) . . ? C1 C6 C7 122.4(6) . . ? C6 C7 C8 112.0(7) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.0(6) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 102.9(6) . . ? C8 C9 H9A 111.2 . . ? C10 C9 H9A 111.2 . . ? C8 C9 H9B 111.2 . . ? C10 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? C5 C10 C9 100.7(6) . . ? C5 C10 H10A 111.6 . . ? C9 C10 H10A 111.6 . . ? C5 C10 H10B 111.6 . . ? C9 C10 H10B 111.6 . . ? H10A C10 H10B 109.4 . . ? C12 C11 C16 120.0 . . ? C12 C11 C1 121.3(5) . . ? C16 C11 C1 118.6(5) . . ? C11 C12 C13 120.0 . . ? C11 C12 N2 118.9(5) . . ? C13 C12 N2 119.9(4) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 C20 116.2(5) . . ? C14 C15 C20 123.7(6) . . ? C15 C16 C11 120.0 . . ? C15 C16 C17 123.5(6) . . ? C11 C16 C17 116.1(6) . . ? C18 C17 C16 117.6(7) . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? C16 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C20 C19 C18 119.7(6) . . ? C20 C19 H19A 107.4 . . ? C18 C19 H19A 107.4 . . ? C20 C19 H19B 107.4 . . ? C18 C19 H19B 107.4 . . ? H19A C19 H19B 106.9 . . ? C19 C18 C17 117.3(6) . . ? C19 C18 H18A 108.0 . . ? C17 C18 H18A 108.0 . . ? C19 C18 H18B 108.0 . . ? C17 C18 H18B 108.0 . . ? H18A C18 H18B 107.2 . . ? C19 C20 C15 119.3(8) . . ? C19 C20 H20A 107.5 . . ? C15 C20 H20A 107.5 . . ? C19 C20 H20B 107.5 . . ? C15 C20 H20B 107.5 . . ? H20A C20 H20B 107.0 . . ? N4 Ti1 N2 95.5(2) . . ? N4 Ti1 N3 102.4(4) . . ? N2 Ti1 N3 152.2(4) . . ? N4 Ti1 N1 101.6(3) . . ? N2 Ti1 N1 82.2(2) . . ? N3 Ti1 N1 114.3(3) . . ? N4 Ti1 O3 90.9(2) . . ? N2 Ti1 O3 67.7(4) . . ? N3 Ti1 O3 90.6(4) . . ? N1 Ti1 O3 148.4(4) . . ? N4 Ti1 S2 95.2(2) . . ? N2 Ti1 S2 35.7(2) . . ? N3 Ti1 S2 120.4(3) . . ? N1 Ti1 S2 117.06(19) . . ? O3 Ti1 S2 32.1(4) . . ? C39 N3 C40 113.7(8) . . ? C39 N3 Ti1 117.7(6) . . ? C40 N3 Ti1 127.2(7) . . ? C41 N4 C42 115.2(7) . . ? C41 N4 Ti1 127.1(5) . . ? C42 N4 Ti1 117.6(7) . . ? C12 N2 S2 117.1(6) . . ? C12 N2 Ti1 141.0(5) . . ? S2 N2 Ti1 101.4(4) . . ? C2 N1 S1 125.2(6) . . ? C2 N1 Ti1 98.5(4) . . ? S1 N1 Ti1 119.3(3) . . ? O4 S2 O3 109.4(9) . . ? O4 S2 N2 115.6(9) . . ? O3 S2 N2 106.9(4) . . ? O4 S2 C30 108.3(7) . . ? O3 S2 C30 110.0(4) . . ? N2 S2 C30 106.5(4) . . ? O4 S2 Ti1 132.8(7) . . ? O3 S2 Ti1 64.1(3) . . ? N2 S2 Ti1 42.9(3) . . ? C30 S2 Ti1 117.9(2) . . ? O1 S1 N1 96.6(4) . . ? O1 S1 O2 120.4(7) . . ? N1 S1 O2 112.2(7) . . ? O1 S1 C21 109.9(4) . . ? N1 S1 C21 109.7(4) . . ? O2 S1 C21 107.5(5) . . ? C31 C30 C35 120.0 . . ? C31 C30 S2 117.4(3) . . ? C35 C30 S2 121.2(3) . . ? C32 C31 C30 120.0 . . ? C32 C31 C36 117.1(4) . . ? C30 C31 C36 122.9(4) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 C37 119.0(5) . . ? C32 C33 C37 121.0(4) . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C30 120.0 . . ? C34 C35 C38 114.9(4) . . ? C30 C35 C38 125.0(4) . . ? C22 C21 C26 120.0 . . ? C22 C21 S1 119.4(3) . . ? C26 C21 S1 119.7(3) . . ? C23 C22 C21 120.0 . . ? C23 C22 C27 116.1(3) . . ? C21 C22 C27 123.9(3) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 C28 119.8(5) . . ? C25 C24 C28 120.2(5) . . ? C26 C25 C24 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C29 114.5(4) . . ? C21 C26 C29 125.5(4) . . ? S2 O3 Ti1 83.8(3) . . ? 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 C6 C1 C2 C3 0.0 . . . . ? C11 C1 C2 C3 -174.8(6) . . . . ? C6 C1 C2 N1 -174.0(6) . . . . ? C11 C1 C2 N1 11.3(7) . . . . ? C1 C2 C3 C4 0.0 . . . . ? N1 C2 C3 C4 173.7(7) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C10 -172.1(8) . . . . ? C4 C5 C6 C1 0.0 . . . . ? C10 C5 C6 C1 170.4(9) . . . . ? C4 C5 C6 C7 -172.8(8) . . . . ? C10 C5 C6 C7 -2.4(9) . . . . ? C2 C1 C6 C5 0.0 . . . . ? C11 C1 C6 C5 174.3(6) . . . . ? C2 C1 C6 C7 172.4(9) . . . . ? C11 C1 C6 C7 -13.3(7) . . . . ? C5 C6 C7 C8 6.3(9) . . . . ? C1 C6 C7 C8 -166.3(5) . . . . ? C6 C7 C8 C9 -44.3(9) . . . . ? C7 C8 C9 C10 76.4(8) . . . . ? C4 C5 C10 C9 -156.8(6) . . . . ? C6 C5 C10 C9 32.1(10) . . . . ? C8 C9 C10 C5 -62.6(9) . . . . ? C2 C1 C11 C12 -76.2(3) . . . . ? C6 C1 C11 C12 109.3(6) . . . . ? C2 C1 C11 C16 107.2(5) . . . . ? C6 C1 C11 C16 -67.3(3) . . . . ? C16 C11 C12 C13 0.0 . . . . ? C1 C11 C12 C13 -176.6(6) . . . . ? C16 C11 C12 N2 -167.5(6) . . . . ? C1 C11 C12 N2 15.9(7) . . . . ? C11 C12 C13 C14 0.0 . . . . ? N2 C12 C13 C14 167.4(7) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C13 C14 C15 C20 176.2(9) . . . . ? C14 C15 C16 C11 0.0 . . . . ? C20 C15 C16 C11 -176.4(9) . . . . ? C14 C15 C16 C17 -172.5(9) . . . . ? C20 C15 C16 C17 11.0(9) . . . . ? C12 C11 C16 C15 0.0 . . . . ? C1 C11 C16 C15 176.7(6) . . . . ? C12 C11 C16 C17 173.1(8) . . . . ? C1 C11 C16 C17 -10.3(7) . . . . ? C15 C16 C17 C18 0.5(11) . . . . ? C11 C16 C17 C18 -172.4(7) . . . . ? C20 C19 C18 C17 -18.3(16) . . . . ? C16 C17 C18 C19 2.8(14) . . . . ? C18 C19 C20 C15 31.0(16) . . . . ? C16 C15 C20 C19 -26.6(12) . . . . ? C14 C15 C20 C19 157.1(8) . . . . ? N4 Ti1 N3 C39 -71.7(9) . . . . ? N2 Ti1 N3 C39 159.6(7) . . . . ? N1 Ti1 N3 C39 37.3(10) . . . . ? O3 Ti1 N3 C39 -162.8(9) . . . . ? S2 Ti1 N3 C39 -175.3(7) . . . . ? N4 Ti1 N3 C40 122.9(10) . . . . ? N2 Ti1 N3 C40 -5.8(17) . . . . ? N1 Ti1 N3 C40 -128.2(10) . . . . ? O3 Ti1 N3 C40 31.8(11) . . . . ? S2 Ti1 N3 C40 19.2(12) . . . . ? N2 Ti1 N4 C41 164.2(6) . . . . ? N3 Ti1 N4 C41 5.7(7) . . . . ? N1 Ti1 N4 C41 -112.7(6) . . . . ? O3 Ti1 N4 C41 96.5(7) . . . . ? S2 Ti1 N4 C41 128.3(6) . . . . ? N2 Ti1 N4 C42 -20.5(9) . . . . ? N3 Ti1 N4 C42 -179.0(10) . . . . ? N1 Ti1 N4 C42 62.7(9) . . . . ? O3 Ti1 N4 C42 -88.2(10) . . . . ? S2 Ti1 N4 C42 -56.4(9) . . . . ? C11 C12 N2 S2 -128.8(5) . . . . ? C13 C12 N2 S2 63.7(6) . . . . ? C11 C12 N2 Ti1 41.6(8) . . . . ? C13 C12 N2 Ti1 -125.9(6) . . . . ? N4 Ti1 N2 C12 97.4(6) . . . . ? N3 Ti1 N2 C12 -132.6(9) . . . . ? N1 Ti1 N2 C12 -3.6(6) . . . . ? O3 Ti1 N2 C12 -173.8(7) . . . . ? S2 Ti1 N2 C12 -171.3(8) . . . . ? N4 Ti1 N2 S2 -91.3(3) . . . . ? N3 Ti1 N2 S2 38.7(9) . . . . ? N1 Ti1 N2 S2 167.7(3) . . . . ? O3 Ti1 N2 S2 -2.5(2) . . . . ? C1 C2 N1 S1 -143.3(5) . . . . ? C3 C2 N1 S1 42.8(8) . . . . ? C1 C2 N1 Ti1 81.3(4) . . . . ? C3 C2 N1 Ti1 -92.6(5) . . . . ? N4 Ti1 N1 C2 -172.1(4) . . . . ? N2 Ti1 N1 C2 -78.1(4) . . . . ? N3 Ti1 N1 C2 78.5(6) . . . . ? O3 Ti1 N1 C2 -60.6(6) . . . . ? S2 Ti1 N1 C2 -70.0(4) . . . . ? N4 Ti1 N1 S1 49.1(5) . . . . ? N2 Ti1 N1 S1 143.1(5) . . . . ? N3 Ti1 N1 S1 -60.4(6) . . . . ? O3 Ti1 N1 S1 160.5(4) . . . . ? S2 Ti1 N1 S1 151.1(4) . . . . ? C12 N2 S2 O4 -59.9(10) . . . . ? Ti1 N2 S2 O4 126.2(9) . . . . ? C12 N2 S2 O3 178.0(4) . . . . ? Ti1 N2 S2 O3 4.1(4) . . . . ? C12 N2 S2 C30 60.4(6) . . . . ? Ti1 N2 S2 C30 -113.4(4) . . . . ? C12 N2 S2 Ti1 173.9(6) . . . . ? N4 Ti1 S2 O4 9.7(13) . . . . ? N2 Ti1 S2 O4 -82.5(13) . . . . ? N3 Ti1 S2 O4 117.3(13) . . . . ? N1 Ti1 S2 O4 -96.2(12) . . . . ? O3 Ti1 S2 O4 93.1(12) . . . . ? N4 Ti1 S2 O3 -83.4(3) . . . . ? N2 Ti1 S2 O3 -175.6(4) . . . . ? N3 Ti1 S2 O3 24.2(5) . . . . ? N1 Ti1 S2 O3 170.7(3) . . . . ? N4 Ti1 S2 N2 92.2(3) . . . . ? N3 Ti1 S2 N2 -160.2(5) . . . . ? N1 Ti1 S2 N2 -13.7(4) . . . . ? O3 Ti1 S2 N2 175.6(4) . . . . ? N4 Ti1 S2 C30 176.6(5) . . . . ? N2 Ti1 S2 C30 84.4(5) . . . . ? N3 Ti1 S2 C30 -75.8(6) . . . . ? N1 Ti1 S2 C30 70.7(5) . . . . ? O3 Ti1 S2 C30 -100.0(5) . . . . ? C2 N1 S1 O1 -178.8(5) . . . . ? Ti1 N1 S1 O1 -51.6(4) . . . . ? C2 N1 S1 O2 -52.1(8) . . . . ? Ti1 N1 S1 O2 75.1(7) . . . . ? C2 N1 S1 C21 67.3(7) . . . . ? Ti1 N1 S1 C21 -165.5(4) . . . . ? O4 S2 C30 C31 -156.7(9) . . . . ? O3 S2 C30 C31 -37.1(5) . . . . ? N2 S2 C30 C31 78.3(5) . . . . ? Ti1 S2 C30 C31 33.4(5) . . . . ? O4 S2 C30 C35 10.2(10) . . . . ? O3 S2 C30 C35 129.8(4) . . . . ? N2 S2 C30 C35 -114.8(4) . . . . ? Ti1 S2 C30 C35 -159.7(3) . . . . ? C35 C30 C31 C32 0.0 . . . . ? S2 C30 C31 C32 167.0(4) . . . . ? C35 C30 C31 C36 178.3(3) . . . . ? S2 C30 C31 C36 -14.7(4) . . . . ? C30 C31 C32 C33 0.0 . . . . ? C36 C31 C32 C33 -178.4(3) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C37 -179.2(3) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C37 C33 C34 C35 179.2(3) . . . . ? C33 C34 C35 C30 0.0 . . . . ? C33 C34 C35 C38 178.5(2) . . . . ? C31 C30 C35 C34 0.0 . . . . ? S2 C30 C35 C34 -166.5(4) . . . . ? C31 C30 C35 C38 -178.4(3) . . . . ? S2 C30 C35 C38 15.1(5) . . . . ? O1 S1 C21 C22 -34.1(5) . . . . ? N1 S1 C21 C22 70.9(5) . . . . ? O2 S1 C21 C22 -166.9(7) . . . . ? O1 S1 C21 C26 134.7(3) . . . . ? N1 S1 C21 C26 -120.2(4) . . . . ? O2 S1 C21 C26 2.0(9) . . . . ? C26 C21 C22 C23 0.0 . . . . ? S1 C21 C22 C23 168.8(4) . . . . ? C26 C21 C22 C27 178.9(3) . . . . ? S1 C21 C22 C27 -12.3(5) . . . . ? C21 C22 C23 C24 0.0 . . . . ? C27 C22 C23 C24 -179.0(3) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C22 C23 C24 C28 -179.2(3) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C28 C24 C25 C26 179.2(3) . . . . ? C24 C25 C26 C21 0.0 . . . . ? C24 C25 C26 C29 178.2(2) . . . . ? C22 C21 C26 C25 0.0 . . . . ? S1 C21 C26 C25 -168.8(4) . . . . ? C22 C21 C26 C29 -178.0(3) . . . . ? S1 C21 C26 C29 13.2(5) . . . . ? O4 S2 O3 Ti1 -129.0(7) . . . . ? N2 S2 O3 Ti1 -3.1(3) . . . . ? C30 S2 O3 Ti1 112.1(3) . . . . ? N4 Ti1 O3 S2 98.3(3) . . . . ? N2 Ti1 O3 S2 2.8(3) . . . . ? N3 Ti1 O3 S2 -159.3(4) . . . . ? N1 Ti1 O3 S2 -15.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.560 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.062 # Attachment 'compound_16.cif' data_compound16 _database_code_depnum_ccdc_archive 'CCDC 742602' #TrackingRef 'compound_16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H62 N4 O4 S2 Zr' _chemical_formula_sum 'C49 H62 N4 O4 S2 Zr' _chemical_formula_weight 926.37 _chemical_absolute_configuration rmad 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' S S 0.1246 0.1234 '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 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.611(3) _cell_length_b 23.611(6) _cell_length_c 43.195(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13882(6) _cell_formula_units_Z 12 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16385 _cell_measurement_theta_min 11.2 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5856 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9021 _exptl_absorpt_correction_T_max 0.9153 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 51199 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 27.43 _reflns_number_total 28327 _reflns_number_gt 23885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0714P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 28327 _refine_ls_number_parameters 1741 _refine_ls_number_restraints 276 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _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 0.40643(3) 0.353334(18) 0.785268(9) 0.02651(10) Uani 1 1 d . . . Zr2 Zr -0.09087(3) 0.18125(2) 0.883688(10) 0.03248(10) Uani 1 1 d . D . Zr3 Zr 0.14160(3) 0.68483(2) 0.941416(10) 0.03165(11) Uani 1 1 d . . . S1 S 0.38448(8) 0.47353(5) 0.80507(2) 0.0276(2) Uani 1 1 d . . . S2 S 0.53308(8) 0.29738(5) 0.73774(3) 0.0303(2) Uani 1 1 d . . . S3 S -0.11632(9) 0.06282(5) 0.86145(3) 0.0347(3) Uani 1 1 d . D . S4 S 0.02844(11) 0.23073(6) 0.93512(3) 0.0460(3) Uani 1 1 d D . . S5 S 0.14682(9) 0.56668(5) 0.96564(3) 0.0327(2) Uani 1 1 d . . . S6 S 0.02912(9) 0.74035(5) 0.89039(3) 0.0335(3) Uani 1 1 d . . . N1 N 0.4667(2) 0.44217(15) 0.78535(8) 0.0249(7) Uani 1 1 d . . . N2 N 0.4870(3) 0.35836(16) 0.73994(8) 0.0264(8) Uani 1 1 d . . . N3 N 0.4302(3) 0.31967(18) 0.82805(8) 0.0363(9) Uani 1 1 d . . . N4 N 0.2778(3) 0.31939(18) 0.77151(9) 0.0346(9) Uani 1 1 d . . . N5 N -0.0334(3) 0.09214(16) 0.88118(8) 0.0323(9) Uani 1 1 d . . . N6 N -0.0167(3) 0.17004(17) 0.92955(8) 0.0335(9) Uani 1 1 d . D . N7 N 0.0690(3) 0.60018(17) 0.94622(8) 0.0307(9) Uani 1 1 d . . . N8 N 0.0555(3) 0.67655(16) 0.89785(8) 0.0301(8) Uani 1 1 d . . . N9 N -0.0506(3) 0.21588(19) 0.84229(9) 0.0419(10) Uani 1 1 d . . . N10 N -0.2208(3) 0.21972(19) 0.89411(10) 0.0434(10) Uani 1 1 d . . . N11 N 0.2780(3) 0.70970(18) 0.92723(9) 0.0377(9) Uani 1 1 d . . . N12 N 0.1136(3) 0.72253(18) 0.98314(9) 0.0394(10) Uani 1 1 d . . . O1 O 0.3125(2) 0.42657(13) 0.80687(7) 0.0308(7) Uani 1 1 d . . . O2 O 0.4148(2) 0.49536(13) 0.83450(7) 0.0339(7) Uani 1 1 d . . . O3 O 0.5016(2) 0.27555(13) 0.76822(7) 0.0336(7) Uani 1 1 d . . . O4 O 0.5053(2) 0.26421(14) 0.71159(7) 0.0371(8) Uani 1 1 d . . . O5 O -0.1863(2) 0.11132(15) 0.85993(7) 0.0384(8) Uani 1 1 d . . . O6 O -0.0881(3) 0.04068(15) 0.83215(7) 0.0437(8) Uani 1 1 d . . . O7 O 0.0041(3) 0.25682(15) 0.90491(8) 0.0446(9) Uani 1 1 d . D . O8 O -0.0077(4) 0.26022(18) 0.96157(9) 0.0644(12) Uani 1 1 d . D . O9 O 0.2272(2) 0.60918(14) 0.96402(7) 0.0370(8) Uani 1 1 d . . . O10 O 0.1184(3) 0.55013(15) 0.99660(7) 0.0412(8) Uani 1 1 d . . . O11 O 0.0601(2) 0.76570(14) 0.92017(7) 0.0373(8) Uani 1 1 d . . . O12 O 0.0754(3) 0.76430(15) 0.86346(8) 0.0419(8) Uani 1 1 d . . . C1 C 0.5913(3) 0.46344(18) 0.74744(9) 0.0259(9) Uani 1 1 d . . . C2 C 0.5611(3) 0.46362(18) 0.77834(10) 0.0257(9) Uani 1 1 d . . . C3 C 0.6252(3) 0.4793(2) 0.80167(10) 0.0326(10) Uani 1 1 d . . . H3 H 0.6032 0.4809 0.8225 0.039 Uiso 1 1 calc R . . C4 C 0.7226(3) 0.4928(2) 0.79438(10) 0.0309(10) Uani 1 1 d . . . H4 H 0.7655 0.5061 0.8101 0.037 Uiso 1 1 calc R . . C5 C 0.7574(3) 0.4870(2) 0.76385(10) 0.0297(10) Uani 1 1 d . . . C6 C 0.6916(3) 0.47252(19) 0.74034(10) 0.0272(9) Uani 1 1 d . . . C7 C 0.7268(3) 0.4664(2) 0.70727(10) 0.0343(11) Uani 1 1 d . . . H7A H 0.7027 0.4992 0.6951 0.041 Uiso 1 1 calc R . . H7B H 0.6973 0.4318 0.6983 0.041 Uiso 1 1 calc R . . C8 C 0.8391(3) 0.4629(2) 0.70385(11) 0.0369(11) Uani 1 1 d . . . H8A H 0.8619 0.4248 0.7102 0.044 Uiso 1 1 calc R . . H8B H 0.8574 0.4687 0.6819 0.044 Uiso 1 1 calc R . . C9 C 0.8889(3) 0.5077(2) 0.72381(11) 0.0409(12) Uani 1 1 d . . . H9A H 0.8650 0.5458 0.7179 0.049 Uiso 1 1 calc R . . H9B H 0.9609 0.5065 0.7205 0.049 Uiso 1 1 calc R . . C10 C 0.8656(3) 0.4962(2) 0.75779(11) 0.0365(11) Uani 1 1 d . . . H10A H 0.9023 0.4622 0.7646 0.044 Uiso 1 1 calc R . . H10B H 0.8885 0.5286 0.7704 0.044 Uiso 1 1 calc R . . C11 C 0.5196(3) 0.4534(2) 0.72130(9) 0.0281(9) Uani 1 1 d . . . C12 C 0.4813(3) 0.39952(19) 0.71583(10) 0.0264(9) Uani 1 1 d . . . C13 C 0.4265(3) 0.3895(2) 0.68920(10) 0.0344(11) Uani 1 1 d . . . H13 H 0.4013 0.3528 0.6851 0.041 Uiso 1 1 calc R . . C14 C 0.4092(3) 0.4332(2) 0.66878(10) 0.0384(11) Uani 1 1 d . . . H14 H 0.3752 0.4255 0.6500 0.046 Uiso 1 1 calc R . . C15 C 0.4401(3) 0.4880(2) 0.67487(10) 0.0352(11) Uani 1 1 d . A . C16 C 0.4965(3) 0.4988(2) 0.70149(10) 0.0299(10) Uani 1 1 d . A . C17 C 0.5244(4) 0.5586(2) 0.71025(11) 0.0381(11) Uani 1 1 d D . . H17A H 0.5941 0.5624 0.7077 0.046 Uiso 0.570(7) 1 d PR A 1 H17B H 0.5103 0.5632 0.7319 0.046 Uiso 0.570(7) 1 d PR A 1 H17C H 0.5910 0.5590 0.7175 0.046 Uiso 0.430(7) 1 d PR A 2 H17D H 0.4827 0.5713 0.7268 0.046 Uiso 0.430(7) 1 d PR A 2 C18 C 0.4759(7) 0.6080(4) 0.69290(18) 0.0395(19) Uani 0.570(7) 1 d PD A 1 H18A H 0.4089 0.6147 0.7011 0.047 Uiso 0.570(7) 1 calc PR A 1 H18B H 0.5149 0.6430 0.6957 0.047 Uiso 0.570(7) 1 calc PR A 1 C19 C 0.4708(8) 0.5923(4) 0.65855(19) 0.049(2) Uani 0.570(7) 1 d PD A 1 H19A H 0.5385 0.5895 0.6503 0.059 Uiso 0.570(7) 1 calc PR A 1 H19B H 0.4369 0.6230 0.6472 0.059 Uiso 0.570(7) 1 calc PR A 1 C18' C 0.5156(8) 0.5986(6) 0.6825(3) 0.0395(19) Uani 0.430(7) 1 d PD A 2 H18C H 0.5245 0.6382 0.6895 0.047 Uiso 0.430(7) 1 calc PR A 2 H18D H 0.5678 0.5899 0.6673 0.047 Uiso 0.430(7) 1 calc PR A 2 C19' C 0.4159(9) 0.5924(4) 0.6672(3) 0.049(2) Uani 0.430(7) 1 d PD A 2 H19C H 0.3628 0.5953 0.6828 0.059 Uiso 0.430(7) 1 calc PR A 2 H19D H 0.4060 0.6224 0.6515 0.059 Uiso 0.430(7) 1 calc PR A 2 C20 C 0.4157(4) 0.5348(2) 0.65228(12) 0.0510(15) Uani 1 1 d D . . H20A H 0.3461 0.5413 0.6528 0.061 Uiso 0.570(7) 1 d PR A 1 H20B H 0.4326 0.5221 0.6318 0.061 Uiso 0.570(7) 1 d PR A 1 H20C H 0.3518 0.5276 0.6437 0.061 Uiso 0.430(7) 1 d PR A 2 H20D H 0.4624 0.5344 0.6356 0.061 Uiso 0.430(7) 1 d PR A 2 C21 C 0.3355(3) 0.53087(19) 0.78293(10) 0.0285(9) Uani 1 1 d . . . C22 C 0.2747(3) 0.5198(2) 0.75712(11) 0.0320(10) Uani 1 1 d . . . C23 C 0.2420(3) 0.5648(2) 0.73968(11) 0.0344(10) Uani 1 1 d . . . H23 H 0.2002 0.5575 0.7225 0.041 Uiso 1 1 calc R . . C24 C 0.2676(4) 0.6209(2) 0.74611(12) 0.0394(11) Uani 1 1 d . . . C25 C 0.3289(3) 0.6306(2) 0.77118(11) 0.0361(11) Uani 1 1 d . . . H25 H 0.3476 0.6684 0.7758 0.043 Uiso 1 1 calc R . . C26 C 0.3644(3) 0.58730(19) 0.78986(10) 0.0305(9) Uani 1 1 d . . . C27 C 0.2460(4) 0.4611(2) 0.74616(11) 0.0359(11) Uani 1 1 d . . . H27A H 0.2041 0.4642 0.7278 0.054 Uiso 1 1 calc R . . H27B H 0.2101 0.4415 0.7626 0.054 Uiso 1 1 calc R . . H27C H 0.3054 0.4396 0.7410 0.054 Uiso 1 1 calc R . . C28 C 0.2339(5) 0.6690(2) 0.72573(13) 0.0532(15) Uani 1 1 d . . . H28A H 0.1890 0.6935 0.7374 0.080 Uiso 1 1 calc R . . H28B H 0.1999 0.6538 0.7076 0.080 Uiso 1 1 calc R . . H28C H 0.2910 0.6911 0.7190 0.080 Uiso 1 1 calc R . . C29 C 0.4334(4) 0.6054(2) 0.81574(11) 0.0412(12) Uani 1 1 d . . . H29A H 0.4438 0.6464 0.8147 0.062 Uiso 1 1 calc R . . H29B H 0.4966 0.5859 0.8134 0.062 Uiso 1 1 calc R . . H29C H 0.4045 0.5955 0.8358 0.062 Uiso 1 1 calc R . . C30 C 0.6633(3) 0.30380(19) 0.73827(10) 0.0305(10) Uani 1 1 d . . . C31 C 0.7107(3) 0.3212(2) 0.76563(10) 0.0319(10) Uani 1 1 d . . . C32 C 0.8108(4) 0.3294(2) 0.76463(11) 0.0373(11) Uani 1 1 d . . . H32 H 0.8426 0.3420 0.7829 0.045 Uiso 1 1 calc R . . C33 C 0.8679(4) 0.3203(2) 0.73855(11) 0.0394(11) Uani 1 1 d . . . C34 C 0.8189(3) 0.3035(2) 0.71182(11) 0.0381(11) Uani 1 1 d . . . H34 H 0.8566 0.2967 0.6937 0.046 Uiso 1 1 calc R . . C35 C 0.7170(3) 0.29603(19) 0.71023(10) 0.0314(10) Uani 1 1 d . . . C36 C 0.6607(3) 0.3304(2) 0.79684(10) 0.0379(11) Uani 1 1 d . . . H36A H 0.7099 0.3413 0.8123 0.057 Uiso 1 1 calc R . . H36B H 0.6284 0.2952 0.8034 0.057 Uiso 1 1 calc R . . H36C H 0.6115 0.3605 0.7949 0.057 Uiso 1 1 calc R . . C37 C 0.9770(4) 0.3297(3) 0.73905(13) 0.0520(15) Uani 1 1 d . . . H37A H 1.0108 0.2931 0.7387 0.078 Uiso 1 1 calc R . . H37B H 0.9950 0.3504 0.7579 0.078 Uiso 1 1 calc R . . H37C H 0.9964 0.3518 0.7209 0.078 Uiso 1 1 calc R . . C38 C 0.6743(4) 0.2811(2) 0.67915(11) 0.0441(13) Uani 1 1 d . . . H38A H 0.7254 0.2843 0.6633 0.066 Uiso 1 1 calc R . . H38B H 0.6205 0.3072 0.6743 0.066 Uiso 1 1 calc R . . H38C H 0.6493 0.2422 0.6797 0.066 Uiso 1 1 calc R . . C39 C 0.0909(3) 0.0670(2) 0.91915(10) 0.0314(10) Uani 1 1 d . . . C40 C 0.0614(3) 0.0702(2) 0.88809(10) 0.0319(10) Uani 1 1 d . D . C41 C 0.1295(4) 0.0592(2) 0.86470(11) 0.0356(11) Uani 1 1 d . . . H41A H 0.1092 0.0593 0.8437 0.043 Uiso 1 1 calc R D . C42 C 0.2274(4) 0.0482(2) 0.87214(12) 0.0436(12) Uani 1 1 d . D . H42A H 0.2725 0.0392 0.8561 0.052 Uiso 1 1 calc R . . C43 C 0.2604(4) 0.0501(2) 0.90285(12) 0.0389(11) Uani 1 1 d . . . C44 C 0.1916(3) 0.0595(2) 0.92654(11) 0.0356(11) Uani 1 1 d . B . C45 C 0.2257(3) 0.0621(3) 0.95958(12) 0.0492(14) Uani 1 1 d D . . H45A H 0.1793 0.0424 0.9724 0.059 Uiso 0.595(10) 1 d PR B 1 H45B H 0.2273 0.1009 0.9661 0.059 Uiso 0.595(10) 1 d PR B 1 H45C H 0.1973 0.0309 0.9707 0.059 Uiso 0.405(10) 1 d PR B 2 H45D H 0.2007 0.0964 0.9686 0.059 Uiso 0.405(10) 1 d PR B 2 C46 C 0.3269(6) 0.0351(5) 0.9640(4) 0.059(3) Uani 0.595(10) 1 d PD B 1 H46A H 0.3225 -0.0062 0.9603 0.070 Uiso 0.595(10) 1 calc PR B 1 H46B H 0.3494 0.0412 0.9855 0.070 Uiso 0.595(10) 1 calc PR B 1 C47 C 0.4008(7) 0.0613(6) 0.9415(2) 0.062(3) Uani 0.595(10) 1 d PD B 1 H47A H 0.4680 0.0475 0.9460 0.074 Uiso 0.595(10) 1 calc PR B 1 H47B H 0.4002 0.1031 0.9432 0.074 Uiso 0.595(10) 1 calc PR B 1 C46' C 0.3373(7) 0.0608(8) 0.9649(6) 0.059(3) Uani 0.405(10) 1 d PD B 2 H46C H 0.3635 0.0997 0.9630 0.070 Uiso 0.405(10) 1 calc PR B 2 H46D H 0.3505 0.0476 0.9863 0.070 Uiso 0.405(10) 1 calc PR B 2 C47' C 0.3917(11) 0.0223(8) 0.9422(2) 0.062(3) Uani 0.405(10) 1 d PD B 2 H47C H 0.3698 -0.0174 0.9448 0.074 Uiso 0.405(10) 1 calc PR B 2 H47D H 0.4633 0.0240 0.9461 0.074 Uiso 0.405(10) 1 calc PR B 2 C48 C 0.3688(4) 0.0429(3) 0.90902(12) 0.0514(14) Uani 1 1 d D B . H48A H 0.4042 0.0653 0.8942 0.062 Uiso 0.595(10) 1 d PR B 1 H48B H 0.3865 0.0039 0.9058 0.062 Uiso 0.595(10) 1 d PR B 1 H48C H 0.4010 0.0785 0.9057 0.062 Uiso 0.405(10) 1 d PR B 2 H48D H 0.3950 0.0161 0.8945 0.062 Uiso 0.405(10) 1 d PR B 2 C49 C 0.0167(3) 0.0730(2) 0.94476(10) 0.0346(11) Uani 1 1 d . D . C50 C -0.0250(4) 0.1254(2) 0.95172(10) 0.0393(12) Uani 1 1 d . . . C51 C -0.0844(4) 0.1311(3) 0.97792(11) 0.0504(14) Uani 1 1 d . D . H51A H -0.1115 0.1668 0.9834 0.060 Uiso 1 1 calc R . . C52 C -0.1029(5) 0.0831(3) 0.99581(12) 0.0621(19) Uani 1 1 d . . . H52A H -0.1415 0.0870 1.0140 0.074 Uiso 1 1 calc R D . C53 C -0.0676(4) 0.0305(3) 0.98808(13) 0.0555(17) Uani 1 1 d . C . C54 C -0.0072(4) 0.0249(3) 0.96234(12) 0.0452(13) Uani 1 1 d . . . C55 C 0.0285(4) -0.0325(2) 0.95251(13) 0.0540(16) Uani 1 1 d D C . H55A H 0.0976 -0.0348 0.9568 0.065 Uiso 0.576(17) 1 d PR C 1 H55B H 0.0205 -0.0350 0.9305 0.065 Uiso 0.576(17) 1 d PR C 1 H55C H 0.0952 -0.0296 0.9454 0.065 Uiso 0.424(17) 1 d PR C 2 H55D H -0.0110 -0.0456 0.9356 0.065 Uiso 0.424(17) 1 d PR C 2 C56 C -0.0186(12) -0.0852(5) 0.9668(3) 0.078(4) Uani 0.576(17) 1 d PDU C 1 H56A H -0.0821 -0.0936 0.9566 0.093 Uiso 0.576(17) 1 calc PR C 1 H56B H 0.0252 -0.1184 0.9644 0.093 Uiso 0.576(17) 1 calc PR C 1 C57 C -0.0341(12) -0.0716(5) 1.0010(3) 0.075(3) Uani 0.576(17) 1 d PDU C 1 H57A H -0.0673 -0.1044 1.0107 0.090 Uiso 0.576(17) 1 calc PR C 1 H57B H 0.0313 -0.0680 1.0108 0.090 Uiso 0.576(17) 1 calc PR C 1 C56' C 0.0255(11) -0.0767(7) 0.9792(4) 0.067(5) Uani 0.424(17) 1 d PDU C 2 H56C H 0.0395 -0.1148 0.9707 0.081 Uiso 0.424(17) 1 calc PR C 2 H56D H 0.0775 -0.0676 0.9945 0.081 Uiso 0.424(17) 1 calc PR C 2 C57' C -0.0734(12) -0.0776(5) 0.9954(5) 0.075(3) Uani 0.424(17) 1 d PDU C 2 H57C H -0.0731 -0.1062 1.0122 0.090 Uiso 0.424(17) 1 calc PR C 2 H57D H -0.1258 -0.0877 0.9805 0.090 Uiso 0.424(17) 1 calc PR C 2 C58 C -0.0924(5) -0.0191(3) 1.00875(16) 0.092(3) Uani 1 1 d D . . H58A H -0.1611 -0.0275 1.0068 0.110 Uiso 0.576(17) 1 d PR C 1 H58B H -0.0796 -0.0089 1.0299 0.110 Uiso 0.576(17) 1 d PR C 1 H58C H -0.1613 -0.0168 1.0134 0.110 Uiso 0.424(17) 1 d PR C 2 H58D H -0.0573 -0.0146 1.0279 0.110 Uiso 0.424(17) 1 d PR C 2 C59 C -0.1707(3) 0.0068(2) 0.88338(11) 0.0339(10) Uani 1 1 d . . . C60 C -0.2314(3) 0.0189(2) 0.90919(11) 0.0364(11) Uani 1 1 d . D . C61 C -0.2673(4) -0.0255(2) 0.92675(12) 0.0422(12) Uani 1 1 d . . . H61A H -0.3086 -0.0173 0.9439 0.051 Uiso 1 1 calc R D . C62 C -0.2453(4) -0.0814(2) 0.92020(13) 0.0444(13) Uani 1 1 d . D . C63 C -0.1849(4) -0.0926(2) 0.89543(12) 0.0421(12) Uani 1 1 d . . . H63A H -0.1695 -0.1310 0.8909 0.050 Uiso 1 1 calc R D . C64 C -0.1453(4) -0.0504(2) 0.87665(12) 0.0410(12) Uani 1 1 d . D . C65 C -0.2611(4) 0.0791(2) 0.91899(12) 0.0462(13) Uani 1 1 d . . . H65A H -0.3000 0.0772 0.9380 0.069 Uiso 1 1 calc R D . H65B H -0.3002 0.0966 0.9025 0.069 Uiso 1 1 calc R . . H65C H -0.2019 0.1017 0.9227 0.069 Uiso 1 1 calc R . . C66 C -0.2841(5) -0.1290(2) 0.94036(14) 0.0611(17) Uani 1 1 d . . . H66A H -0.2298 -0.1541 0.9462 0.092 Uiso 1 1 calc R D . H66B H -0.3335 -0.1506 0.9288 0.092 Uiso 1 1 calc R . . H66C H -0.3140 -0.1130 0.9591 0.092 Uiso 1 1 calc R . . C67 C -0.0788(5) -0.0693(3) 0.85060(13) 0.0616(17) Uani 1 1 d . . . H67A H -0.0599 -0.1089 0.8538 0.092 Uiso 1 1 calc R D . H67B H -0.0197 -0.0456 0.8502 0.092 Uiso 1 1 calc R . . H67C H -0.1136 -0.0657 0.8308 0.092 Uiso 1 1 calc R . . C68 C 0.1643(5) 0.2230(9) 0.9363(3) 0.0434(19) Uani 0.530(17) 1 d PGDU D 1 C69 C 0.2151(8) 0.2313(8) 0.9638(3) 0.056(2) Uani 0.530(17) 1 d PGDU D 1 C70 C 0.3166(8) 0.2250(6) 0.9646(2) 0.059(3) Uani 0.530(17) 1 d PGU D 1 H70A H 0.3514 0.2307 0.9834 0.070 Uiso 0.530(17) 1 calc PR D 1 C71 C 0.3673(5) 0.2104(6) 0.9378(3) 0.053(3) Uani 0.530(17) 1 d PGDU D 1 C72 C 0.3165(7) 0.2021(6) 0.9103(2) 0.046(2) Uani 0.530(17) 1 d PGU D 1 H72A H 0.3511 0.1921 0.8920 0.055 Uiso 0.530(17) 1 calc PR D 1 C73 C 0.2150(7) 0.2083(8) 0.9095(3) 0.040(2) Uani 0.530(17) 1 d PGDU D 1 C74 C 0.1714(16) 0.2414(11) 0.9955(3) 0.101(7) Uani 0.530(17) 1 d PDU D 1 H74A H 0.2223 0.2365 1.0113 0.151 Uiso 0.530(17) 1 calc PR D 1 H74B H 0.1182 0.2142 0.9991 0.151 Uiso 0.530(17) 1 calc PR D 1 H74C H 0.1453 0.2800 0.9965 0.151 Uiso 0.530(17) 1 calc PR D 1 C75 C 0.4792(7) 0.2030(8) 0.9388(4) 0.080(5) Uani 0.530(17) 1 d PDU D 1 H75A H 0.4970 0.1782 0.9561 0.119 Uiso 0.530(17) 1 calc PR D 1 H75B H 0.5105 0.2400 0.9416 0.119 Uiso 0.530(17) 1 calc PR D 1 H75C H 0.5018 0.1861 0.9193 0.119 Uiso 0.530(17) 1 calc PR D 1 C76 C 0.171(2) 0.2012(13) 0.8778(4) 0.035(3) Uani 0.530(17) 1 d PDU D 1 H76A H 0.2231 0.1912 0.8631 0.053 Uiso 0.530(17) 1 calc PR D 1 H76B H 0.1401 0.2367 0.8714 0.053 Uiso 0.530(17) 1 calc PR D 1 H76C H 0.1218 0.1710 0.8783 0.053 Uiso 0.530(17) 1 calc PR D 1 C68' C 0.1547(5) 0.2281(11) 0.9409(4) 0.0434(19) Uani 0.470(17) 1 d PGD D 2 C69' C 0.1954(8) 0.2385(9) 0.9698(3) 0.056(2) Uani 0.470(17) 1 d PGD D 2 C70' C 0.2966(9) 0.2359(7) 0.9738(3) 0.059(3) Uani 0.470(17) 1 d PG D 2 H70B H 0.3245 0.2430 0.9936 0.070 Uiso 0.470(17) 1 calc PR D 2 C71' C 0.3571(5) 0.2230(7) 0.9489(3) 0.053(3) Uani 0.470(17) 1 d PGD D 2 C72' C 0.3164(8) 0.2126(7) 0.9199(3) 0.046(2) Uani 0.470(17) 1 d PG D 2 H72B H 0.3577 0.2038 0.9029 0.055 Uiso 0.470(17) 1 calc PR D 2 C73' C 0.2151(8) 0.2152(10) 0.9159(3) 0.040(2) Uani 0.470(17) 1 d PGD D 2 C74' C 0.1379(14) 0.2504(11) 0.9989(3) 0.080(5) Uani 0.470(17) 1 d PDU D 2 H74D H 0.1821 0.2493 1.0168 0.120 Uiso 0.470(17) 1 calc PR D 2 H74E H 0.0865 0.2217 1.0014 0.120 Uiso 0.470(17) 1 calc PR D 2 H74F H 0.1076 0.2880 0.9974 0.120 Uiso 0.470(17) 1 calc PR D 2 C75' C 0.4673(8) 0.2229(9) 0.9519(4) 0.074(5) Uani 0.470(17) 1 d PDU D 2 H75D H 0.4861 0.2036 0.9711 0.111 Uiso 0.470(17) 1 calc PR D 2 H75E H 0.4913 0.2621 0.9524 0.111 Uiso 0.470(17) 1 calc PR D 2 H75F H 0.4962 0.2031 0.9342 0.111 Uiso 0.470(17) 1 calc PR D 2 C76' C 0.179(3) 0.2038(16) 0.8836(4) 0.048(5) Uani 0.470(17) 1 d PDU D 2 H76D H 0.1275 0.1749 0.8842 0.072 Uiso 0.470(17) 1 calc PR D 2 H76E H 0.2339 0.1902 0.8708 0.072 Uiso 0.470(17) 1 calc PR D 2 H76F H 0.1528 0.2388 0.8747 0.072 Uiso 0.470(17) 1 calc PR D 2 C77 C -0.0712(3) 0.58268(19) 0.91219(10) 0.0285(10) Uani 1 1 d . . . C78 C -0.0327(3) 0.58357(19) 0.94202(11) 0.0313(10) Uani 1 1 d . . . C79 C -0.0938(4) 0.5748(2) 0.96758(10) 0.0371(11) Uani 1 1 d . . . H79 H -0.0670 0.5730 0.9879 0.045 Uiso 1 1 calc R . . C80 C -0.1943(4) 0.5689(3) 0.96295(12) 0.0476(14) Uani 1 1 d . . . H80 H -0.2355 0.5622 0.9803 0.057 Uiso 1 1 calc R . . C81 C -0.2364(4) 0.5726(2) 0.93370(12) 0.0398(12) Uani 1 1 d . . . C82 C -0.1748(3) 0.5793(2) 0.90789(11) 0.0330(10) Uani 1 1 d . . . C83 C -0.2192(3) 0.5865(2) 0.87621(11) 0.0350(11) Uani 1 1 d . . . H83A H -0.1772 0.5669 0.8609 0.042 Uiso 1 1 calc R . . H83B H -0.2194 0.6273 0.8709 0.042 Uiso 1 1 calc R . . C84 C -0.3240(4) 0.5638(3) 0.87337(13) 0.0504(14) Uani 1 1 d . . . H84A H -0.3520 0.5750 0.8531 0.061 Uiso 1 1 calc R . . H84B H -0.3231 0.5219 0.8744 0.061 Uiso 1 1 calc R . . C85 C -0.3862(4) 0.5866(3) 0.89890(13) 0.0595(17) Uani 1 1 d . . . H85A H -0.4543 0.5726 0.8965 0.071 Uiso 1 1 calc R . . H85B H -0.3877 0.6285 0.8977 0.071 Uiso 1 1 calc R . . C86 C -0.3468(4) 0.5688(3) 0.93027(13) 0.0530(15) Uani 1 1 d . . . H86A H -0.3776 0.5928 0.9463 0.064 Uiso 1 1 calc R . . H86B H -0.3671 0.5292 0.9342 0.064 Uiso 1 1 calc R . . C87 C -0.0030(3) 0.5827(2) 0.88455(10) 0.0287(9) Uani 1 1 d . . . C88 C 0.0495(3) 0.6311(2) 0.87603(10) 0.0304(10) Uani 1 1 d . . . C89 C 0.1060(3) 0.6319(2) 0.84887(10) 0.0354(11) Uani 1 1 d . . . H89 H 0.1413 0.6650 0.8431 0.042 Uiso 1 1 calc R . . C90 C 0.1094(3) 0.5837(2) 0.83058(10) 0.0383(12) Uani 1 1 d . . . H90 H 0.1450 0.5846 0.8117 0.046 Uiso 1 1 calc R . . C91 C 0.0625(3) 0.5344(2) 0.83916(11) 0.0342(11) Uani 1 1 d . . . C92 C 0.0062(3) 0.5334(2) 0.86656(10) 0.0325(10) Uani 1 1 d . . . C93 C -0.0407(4) 0.4787(2) 0.87761(12) 0.0425(12) Uani 1 1 d . . . H93A H -0.1127 0.4817 0.8749 0.051 Uiso 1 1 calc R . . H93B H -0.0274 0.4744 0.9000 0.051 Uiso 1 1 calc R . . C94 C -0.0050(6) 0.4259(3) 0.86093(15) 0.0688(19) Uani 1 1 d . . . H94A H 0.0607 0.4154 0.8689 0.083 Uiso 1 1 calc R . . H94B H -0.0505 0.3942 0.8654 0.083 Uiso 1 1 calc R . . C95 C 0.0006(5) 0.4346(3) 0.82734(14) 0.0608(17) Uani 1 1 d . . . H95A H -0.0654 0.4444 0.8193 0.073 Uiso 1 1 calc R . . H95B H 0.0218 0.3990 0.8173 0.073 Uiso 1 1 calc R . . C96 C 0.0730(3) 0.4822(2) 0.81892(12) 0.0451(13) Uani 1 1 d . . . H96A H 0.1409 0.4675 0.8208 0.054 Uiso 1 1 calc R . . H96B H 0.0626 0.4931 0.7970 0.054 Uiso 1 1 calc R . . C97 C 0.1799(3) 0.5041(2) 0.94482(10) 0.0320(10) Uani 1 1 d . . . C98 C 0.2380(3) 0.5086(2) 0.91788(11) 0.0343(10) Uani 1 1 d . . . C99 C 0.2564(3) 0.4596(2) 0.90103(11) 0.0369(11) Uani 1 1 d . . . H99 H 0.2952 0.4621 0.8828 0.044 Uiso 1 1 calc R . . C100 C 0.2204(4) 0.4075(2) 0.90987(12) 0.0396(12) Uani 1 1 d . . . C101 C 0.1638(4) 0.4034(2) 0.93645(12) 0.0439(13) Uani 1 1 d . . . H101 H 0.1387 0.3674 0.9424 0.053 Uiso 1 1 calc R . . C102 C 0.1423(4) 0.4507(2) 0.95488(11) 0.0399(12) Uani 1 1 d . . . C103 C 0.2801(4) 0.5624(2) 0.90494(11) 0.0415(12) Uani 1 1 d . . . H10C H 0.3323 0.5762 0.9186 0.062 Uiso 1 1 calc R . . H10D H 0.2282 0.5910 0.9034 0.062 Uiso 1 1 calc R . . H10E H 0.3072 0.5551 0.8843 0.062 Uiso 1 1 calc R . . C104 C 0.2396(5) 0.3550(2) 0.89030(14) 0.0584(16) Uani 1 1 d . . . H10F H 0.2827 0.3291 0.9017 0.088 Uiso 1 1 calc R . . H10G H 0.2712 0.3661 0.8708 0.088 Uiso 1 1 calc R . . H10H H 0.1771 0.3360 0.8858 0.088 Uiso 1 1 calc R . . C105 C 0.0778(5) 0.4406(2) 0.98293(13) 0.0591(17) Uani 1 1 d . . . H10I H 0.1173 0.4442 1.0018 0.089 Uiso 1 1 calc R . . H10J H 0.0497 0.4024 0.9819 0.089 Uiso 1 1 calc R . . H10K H 0.0247 0.4686 0.9833 0.089 Uiso 1 1 calc R . . C106 C -0.1011(3) 0.7460(2) 0.88566(11) 0.0361(10) Uani 1 1 d . . . C107 C -0.1630(4) 0.7369(2) 0.91123(11) 0.0403(12) Uani 1 1 d . . . C108 C -0.2654(4) 0.7387(2) 0.90647(13) 0.0438(12) Uani 1 1 d . . . H108 H -0.3076 0.7319 0.9236 0.053 Uiso 1 1 calc R . . C109 C -0.3071(4) 0.7502(2) 0.87780(13) 0.0437(12) Uani 1 1 d . . . C110 C -0.2444(4) 0.7580(2) 0.85311(12) 0.0420(12) Uani 1 1 d . . . H110 H -0.2719 0.7650 0.8333 0.050 Uiso 1 1 calc R . . C111 C -0.1417(4) 0.7562(2) 0.85594(11) 0.0378(11) Uani 1 1 d . . . C112 C -0.1262(4) 0.7263(3) 0.94357(11) 0.0522(14) Uani 1 1 d . . . H11A H -0.0819 0.6936 0.9435 0.078 Uiso 1 1 calc R . . H11B H -0.1820 0.7187 0.9573 0.078 Uiso 1 1 calc R . . H11C H -0.0906 0.7598 0.9510 0.078 Uiso 1 1 calc R . . C113 C -0.4171(4) 0.7523(3) 0.87347(14) 0.0587(16) Uani 1 1 d . . . H11D H -0.4384 0.7919 0.8719 0.088 Uiso 1 1 calc R . . H11E H -0.4494 0.7344 0.8912 0.088 Uiso 1 1 calc R . . H11F H -0.4350 0.7320 0.8545 0.088 Uiso 1 1 calc R . . C114 C -0.0830(4) 0.7647(3) 0.82620(11) 0.0493(14) Uani 1 1 d . . . H11G H -0.1282 0.7672 0.8086 0.074 Uiso 1 1 calc R . . H11H H -0.0384 0.7326 0.8232 0.074 Uiso 1 1 calc R . . H11I H -0.0448 0.7998 0.8277 0.074 Uiso 1 1 calc R . . C115 C 0.4215(5) 0.2598(2) 0.83407(13) 0.0557(15) Uani 1 1 d . . . H11J H 0.4870 0.2436 0.8373 0.083 Uiso 1 1 calc R . . H11K H 0.3901 0.2412 0.8163 0.083 Uiso 1 1 calc R . . H11L H 0.3814 0.2539 0.8526 0.083 Uiso 1 1 calc R . . C116 C 0.4856(4) 0.3481(2) 0.85269(11) 0.0448(13) Uani 1 1 d . . . H11M H 0.4519 0.3427 0.8725 0.067 Uiso 1 1 calc R . . H11N H 0.4900 0.3887 0.8481 0.067 Uiso 1 1 calc R . . H11O H 0.5518 0.3320 0.8539 0.067 Uiso 1 1 calc R . . C117 C 0.1994(4) 0.3112(3) 0.79380(12) 0.0484(13) Uani 1 1 d . . . H11P H 0.1487 0.3401 0.7907 0.073 Uiso 1 1 calc R . . H11Q H 0.2259 0.3144 0.8148 0.073 Uiso 1 1 calc R . . H11R H 0.1705 0.2735 0.7910 0.073 Uiso 1 1 calc R . . C118 C 0.2454(3) 0.3097(2) 0.73988(11) 0.0391(11) Uani 1 1 d . . . H11S H 0.2165 0.2718 0.7382 0.059 Uiso 1 1 calc R . . H11T H 0.3016 0.3127 0.7258 0.059 Uiso 1 1 calc R . . H11U H 0.1960 0.3381 0.7343 0.059 Uiso 1 1 calc R . . C119 C 0.0073(4) 0.1884(3) 0.81875(11) 0.0509(14) Uani 1 1 d . D . H11V H -0.0164 0.1998 0.7983 0.076 Uiso 1 1 calc R . . H11W H 0.0015 0.1473 0.8209 0.076 Uiso 1 1 calc R . . H11X H 0.0763 0.1995 0.8210 0.076 Uiso 1 1 calc R . . C120 C -0.0530(6) 0.2762(3) 0.83866(15) 0.070(2) Uani 1 1 d . D . H12P H -0.0828 0.2857 0.8187 0.105 Uiso 1 1 calc R . . H12Q H 0.0141 0.2912 0.8394 0.105 Uiso 1 1 calc R . . H12R H -0.0920 0.2930 0.8554 0.105 Uiso 1 1 calc R . . C121 C -0.2939(4) 0.2325(3) 0.87073(14) 0.0624(17) Uani 1 1 d . D . H12S H -0.3099 0.2729 0.8714 0.094 Uiso 1 1 calc R . . H12T H -0.3534 0.2102 0.8747 0.094 Uiso 1 1 calc R . . H12U H -0.2679 0.2229 0.8502 0.094 Uiso 1 1 calc R . . C122 C -0.2613(5) 0.2272(3) 0.92500(13) 0.0570(16) Uani 1 1 d . D . H12V H -0.2900 0.2651 0.9268 0.085 Uiso 1 1 calc R . . H12W H -0.2089 0.2228 0.9404 0.085 Uiso 1 1 calc R . . H12X H -0.3122 0.1986 0.9287 0.085 Uiso 1 1 calc R . . C123 C 0.3083(4) 0.7217(3) 0.89561(12) 0.0531(15) Uani 1 1 d . . . H12A H 0.3429 0.7581 0.8950 0.080 Uiso 1 1 calc R . . H12B H 0.2502 0.7234 0.8822 0.080 Uiso 1 1 calc R . . H12C H 0.3522 0.6916 0.8883 0.080 Uiso 1 1 calc R . . C124 C 0.3629(4) 0.7082(3) 0.94702(14) 0.070(2) Uani 1 1 d . . . H12D H 0.4067 0.6776 0.9404 0.104 Uiso 1 1 calc R . . H12E H 0.3422 0.7017 0.9684 0.104 Uiso 1 1 calc R . . H12F H 0.3978 0.7445 0.9457 0.104 Uiso 1 1 calc R . . C125 C 0.1601(8) 0.7742(4) 0.99306(17) 0.130(5) Uani 1 1 d . . . H12G H 0.1111 0.8046 0.9940 0.195 Uiso 1 1 calc R . . H12H H 0.2118 0.7845 0.9783 0.195 Uiso 1 1 calc R . . H12I H 0.1889 0.7687 1.0136 0.195 Uiso 1 1 calc R . . C126 C 0.0372(5) 0.7084(3) 1.00435(14) 0.071(2) Uani 1 1 d . . . H12J H 0.0655 0.7016 1.0249 0.106 Uiso 1 1 calc R . . H12K H 0.0034 0.6741 0.9972 0.106 Uiso 1 1 calc R . . H12L H -0.0099 0.7397 1.0055 0.106 Uiso 1 1 calc R . . C127 C 0.1934(9) 0.8910(3) 0.8764(2) 0.145(6) Uani 1 1 d . . . H12M H 0.1740 0.9307 0.8740 0.217 Uiso 1 1 calc R . . H12N H 0.1401 0.8699 0.8865 0.217 Uiso 1 1 calc R . . H12O H 0.2065 0.8745 0.8560 0.217 Uiso 1 1 calc R . . C128 C 0.2810(8) 0.8876(3) 0.89519(18) 0.084(3) Uani 1 1 d . . . C129 C 0.3790(8) 0.8959(3) 0.88539(18) 0.084(3) Uani 1 1 d . . . H129 H 0.3912 0.9027 0.8641 0.101 Uiso 1 1 calc R . . C130 C 0.4546(7) 0.8946(4) 0.90463(19) 0.091(3) Uani 1 1 d . . . H130 H 0.5189 0.9023 0.8972 0.109 Uiso 1 1 calc R . . C131 C 0.4403(6) 0.8826(4) 0.9345(2) 0.094(3) Uani 1 1 d . . . H131 H 0.4950 0.8821 0.9482 0.113 Uiso 1 1 calc R . . C132 C 0.3477(6) 0.8707(4) 0.94599(15) 0.080(2) Uani 1 1 d . . . H132 H 0.3402 0.8605 0.9671 0.096 Uiso 1 1 calc R . . C133 C 0.2666(6) 0.8734(3) 0.92731(15) 0.0675(19) Uani 1 1 d . . . H133 H 0.2028 0.8662 0.9353 0.081 Uiso 1 1 calc R . . C134 C 0.9674(4) 0.6415(3) 0.76557(14) 0.0594(16) Uani 1 1 d . . . H13A H 0.9968 0.6783 0.7607 0.089 Uiso 1 1 calc R . . H13B H 0.9862 0.6138 0.7497 0.089 Uiso 1 1 calc R . . H13C H 0.9908 0.6286 0.7859 0.089 Uiso 1 1 calc R . . C135 C 0.8564(4) 0.6471(2) 0.76628(12) 0.0475(13) Uani 1 1 d . . . C136 C 0.8022(4) 0.6546(2) 0.73969(13) 0.0499(14) Uani 1 1 d . . . H136 H 0.8359 0.6556 0.7204 0.060 Uiso 1 1 calc R . . C137 C 0.7024(5) 0.6605(2) 0.73954(16) 0.0594(16) Uani 1 1 d . . . H137 H 0.6681 0.6654 0.7206 0.071 Uiso 1 1 calc R . . C138 C 0.6514(5) 0.6595(3) 0.76751(18) 0.072(2) Uani 1 1 d . . . H138 H 0.5821 0.6639 0.7681 0.086 Uiso 1 1 calc R . . C139 C 0.7049(5) 0.6518(3) 0.79462(16) 0.0684(19) Uani 1 1 d . . . H139 H 0.6714 0.6510 0.8139 0.082 Uiso 1 1 calc R . . C140 C 0.8047(5) 0.6454(3) 0.79411(14) 0.0605(16) Uani 1 1 d . . . H140 H 0.8392 0.6397 0.8130 0.073 Uiso 1 1 calc R . . C141 C 0.8719(7) 0.3782(5) 0.9360(3) 0.082(5) Uani 0.491(10) 1 d PDU E 1 H14A H 0.8927 0.3636 0.9158 0.123 Uiso 0.491(10) 1 calc PR E 1 H14B H 0.8884 0.3506 0.9521 0.123 Uiso 0.491(10) 1 calc PR E 1 H14C H 0.9058 0.4140 0.9402 0.123 Uiso 0.491(10) 1 calc PR E 1 C142 C 0.7628(5) 0.3880(3) 0.93572(17) 0.058(4) Uani 0.491(10) 1 d PGDU E 1 C143 C 0.7165(6) 0.4076(4) 0.90911(16) 0.062(4) Uani 0.491(10) 1 d PGDU E 1 H143 H 0.7539 0.4149 0.8910 0.074 Uiso 0.491(10) 1 calc PR E 1 C144 C 0.6156(6) 0.4166(5) 0.9091(2) 0.073(5) Uani 0.491(10) 1 d PGDU E 1 H144 H 0.5840 0.4300 0.8909 0.087 Uiso 0.491(10) 1 calc PR E 1 C145 C 0.5609(5) 0.4060(5) 0.9356(2) 0.071(4) Uani 0.491(10) 1 d PGDU E 1 H145 H 0.4920 0.4121 0.9356 0.085 Uiso 0.491(10) 1 calc PR E 1 C146 C 0.6072(6) 0.3864(5) 0.9622(2) 0.085(5) Uani 0.491(10) 1 d PGDU E 1 H146 H 0.5699 0.3791 0.9804 0.102 Uiso 0.491(10) 1 calc PR E 1 C147 C 0.7081(6) 0.3774(4) 0.96228(16) 0.063(4) Uani 0.491(10) 1 d PGDU E 1 H147 H 0.7398 0.3640 0.9805 0.076 Uiso 0.491(10) 1 calc PR E 1 C148 C 0.5080(9) 0.4255(7) 0.9247(4) 0.138(9) Uani 0.509(10) 1 d PDU E 2 H14D H 0.4983 0.4462 0.9053 0.207 Uiso 0.509(10) 1 calc PR E 2 H14E H 0.4902 0.4499 0.9422 0.207 Uiso 0.509(10) 1 calc PR E 2 H14F H 0.4663 0.3916 0.9248 0.207 Uiso 0.509(10) 1 calc PR E 2 C149 C 0.6130(6) 0.4084(4) 0.9275(2) 0.094(6) Uani 0.509(10) 1 d PGDU E 2 C150 C 0.6690(7) 0.3988(4) 0.90114(18) 0.064(4) Uani 0.509(10) 1 d PGDU E 2 H15A H 0.6404 0.4032 0.8812 0.077 Uiso 0.509(10) 1 calc PR E 2 C151 C 0.7669(7) 0.3829(5) 0.9039(2) 0.084(5) Uani 0.509(10) 1 d PGDU E 2 H15B H 0.8052 0.3764 0.8858 0.101 Uiso 0.509(10) 1 calc PR E 2 C152 C 0.8089(6) 0.3765(5) 0.9330(3) 0.093(6) Uani 0.509(10) 1 d PGDU E 2 H15C H 0.8758 0.3656 0.9349 0.112 Uiso 0.509(10) 1 calc PR E 2 C153 C 0.7529(9) 0.3861(6) 0.9594(2) 0.099(7) Uani 0.509(10) 1 d PGDU E 2 H15D H 0.7815 0.3817 0.9793 0.119 Uiso 0.509(10) 1 calc PR E 2 C154 C 0.6549(8) 0.4020(5) 0.95667(19) 0.099(6) Uani 0.509(10) 1 d PGDU E 2 H15E H 0.6167 0.4085 0.9747 0.119 Uiso 0.509(10) 1 calc PR E 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 0.02236(19) 0.0284(2) 0.0287(2) -0.00109(18) 0.00178(17) -0.00079(17) Zr2 0.0324(2) 0.0336(2) 0.0315(2) -0.00109(19) -0.00261(18) 0.0001(2) Zr3 0.0301(2) 0.0330(2) 0.0319(2) -0.0031(2) -0.00497(18) 0.00305(19) S1 0.0273(6) 0.0286(6) 0.0269(5) -0.0024(5) 0.0039(4) 0.0012(4) S2 0.0271(6) 0.0290(6) 0.0348(6) -0.0060(5) 0.0025(4) -0.0015(4) S3 0.0347(6) 0.0370(7) 0.0323(6) -0.0057(5) -0.0055(5) -0.0022(5) S4 0.0539(8) 0.0420(8) 0.0421(7) -0.0134(6) -0.0068(6) -0.0054(6) S5 0.0343(6) 0.0353(6) 0.0285(5) -0.0006(5) -0.0040(5) 0.0061(5) S6 0.0299(6) 0.0320(6) 0.0385(6) 0.0042(5) -0.0053(5) 0.0010(5) N1 0.0216(17) 0.0271(19) 0.0261(17) -0.0030(16) 0.0009(14) -0.0010(14) N2 0.0243(18) 0.031(2) 0.0243(17) -0.0053(16) 0.0043(14) 0.0002(15) N3 0.041(2) 0.038(2) 0.0303(19) 0.0029(18) 0.0013(16) 0.0059(18) N4 0.0233(18) 0.038(2) 0.043(2) -0.0068(19) -0.0010(16) -0.0052(17) N5 0.039(2) 0.029(2) 0.0286(19) -0.0042(17) -0.0065(17) -0.0002(17) N6 0.038(2) 0.035(2) 0.0273(18) -0.0048(17) -0.0044(16) -0.0051(17) N7 0.028(2) 0.039(2) 0.0252(18) 0.0014(17) 0.0010(15) 0.0067(16) N8 0.0324(19) 0.031(2) 0.0273(18) -0.0017(16) -0.0011(15) 0.0013(16) N9 0.046(2) 0.044(3) 0.036(2) 0.005(2) 0.0003(19) 0.002(2) N10 0.037(2) 0.040(2) 0.053(3) -0.006(2) -0.0021(19) 0.0054(19) N11 0.028(2) 0.039(2) 0.046(2) 0.0048(19) -0.0070(17) -0.0009(18) N12 0.046(3) 0.037(2) 0.035(2) -0.0014(18) -0.0061(18) 0.0055(19) O1 0.0263(16) 0.0297(17) 0.0365(17) 0.0005(14) 0.0100(13) -0.0005(13) O2 0.0376(18) 0.0356(18) 0.0286(15) -0.0040(14) 0.0006(14) 0.0031(15) O3 0.0306(17) 0.0303(17) 0.0399(17) 0.0010(15) 0.0072(14) -0.0003(14) O4 0.0340(17) 0.0368(19) 0.0404(18) -0.0149(16) 0.0055(14) -0.0082(14) O5 0.0352(18) 0.042(2) 0.0376(18) -0.0044(16) -0.0083(14) -0.0006(15) O6 0.052(2) 0.043(2) 0.0358(17) -0.0086(16) -0.0030(16) -0.0075(18) O7 0.047(2) 0.0344(19) 0.052(2) -0.0013(17) -0.0105(17) -0.0026(16) O8 0.087(3) 0.055(3) 0.051(2) -0.024(2) -0.003(2) 0.002(2) O9 0.0354(18) 0.0364(19) 0.0393(18) -0.0009(16) -0.0094(15) 0.0062(15) O10 0.052(2) 0.044(2) 0.0276(16) 0.0017(15) -0.0049(14) 0.0037(17) O11 0.0371(18) 0.0334(19) 0.0414(18) 0.0004(16) -0.0104(14) 0.0010(14) O12 0.040(2) 0.040(2) 0.0458(19) 0.0121(16) -0.0048(15) -0.0069(16) C1 0.024(2) 0.026(2) 0.027(2) 0.0031(17) -0.0045(17) 0.0012(18) C2 0.022(2) 0.026(2) 0.029(2) -0.0001(18) 0.0018(15) 0.0018(16) C3 0.034(2) 0.038(3) 0.026(2) -0.003(2) 0.0010(18) 0.001(2) C4 0.023(2) 0.036(3) 0.034(2) -0.002(2) -0.0034(17) -0.0031(19) C5 0.018(2) 0.034(2) 0.037(2) 0.000(2) -0.0037(17) -0.0010(18) C6 0.023(2) 0.032(2) 0.027(2) -0.0026(19) -0.0017(17) 0.0003(17) C7 0.026(2) 0.047(3) 0.030(2) 0.003(2) 0.0025(18) 0.001(2) C8 0.037(3) 0.039(3) 0.034(2) 0.004(2) 0.007(2) 0.002(2) C9 0.026(3) 0.046(3) 0.050(3) 0.003(2) 0.003(2) -0.005(2) C10 0.025(2) 0.040(3) 0.044(3) 0.003(2) -0.001(2) -0.002(2) C11 0.024(2) 0.038(3) 0.022(2) 0.0007(19) -0.0018(16) -0.0008(18) C12 0.018(2) 0.036(2) 0.026(2) -0.0034(19) 0.0017(16) 0.0023(17) C13 0.027(2) 0.045(3) 0.031(2) -0.006(2) 0.0013(18) 0.004(2) C14 0.023(2) 0.065(3) 0.027(2) -0.005(2) -0.0031(19) 0.003(2) C15 0.026(2) 0.052(3) 0.028(2) 0.006(2) 0.0004(17) 0.010(2) C16 0.020(2) 0.042(3) 0.028(2) 0.008(2) 0.0015(16) 0.0057(19) C17 0.033(3) 0.040(3) 0.042(3) 0.008(2) -0.005(2) 0.003(2) C18 0.033(5) 0.042(4) 0.044(5) 0.013(4) -0.002(3) 0.009(4) C19 0.051(6) 0.051(4) 0.046(5) 0.015(4) 0.004(4) 0.016(5) C18' 0.033(5) 0.042(4) 0.044(5) 0.013(4) -0.002(3) 0.009(4) C19' 0.051(6) 0.051(4) 0.046(5) 0.015(4) 0.004(4) 0.016(5) C20 0.028(3) 0.082(4) 0.043(3) 0.017(3) -0.008(2) 0.009(3) C21 0.023(2) 0.030(2) 0.032(2) 0.002(2) 0.0040(17) -0.0019(17) C22 0.021(2) 0.035(3) 0.039(3) -0.006(2) 0.0007(18) 0.0009(18) C23 0.028(2) 0.034(3) 0.041(3) -0.005(2) -0.006(2) 0.001(2) C24 0.035(3) 0.035(3) 0.048(3) 0.001(2) -0.001(2) 0.005(2) C25 0.032(2) 0.034(3) 0.042(3) -0.003(2) -0.002(2) 0.000(2) C26 0.025(2) 0.030(2) 0.037(2) -0.004(2) 0.0031(18) -0.0007(18) C27 0.034(3) 0.038(3) 0.035(2) -0.008(2) 0.002(2) 0.001(2) C28 0.064(4) 0.035(3) 0.061(3) 0.009(3) -0.019(3) 0.004(3) C29 0.043(3) 0.034(3) 0.046(3) -0.003(2) -0.003(2) -0.006(2) C30 0.030(2) 0.027(2) 0.035(2) -0.001(2) 0.0015(18) 0.0055(18) C31 0.031(2) 0.027(2) 0.037(2) 0.002(2) -0.0001(18) 0.0042(19) C32 0.037(3) 0.041(3) 0.034(2) -0.001(2) -0.0056(19) 0.003(2) C33 0.032(2) 0.041(3) 0.045(3) 0.001(2) -0.001(2) 0.003(2) C34 0.034(2) 0.041(3) 0.039(3) -0.003(2) 0.009(2) 0.003(2) C35 0.030(2) 0.031(2) 0.033(2) 0.001(2) 0.0015(18) 0.0050(19) C36 0.032(2) 0.042(3) 0.040(3) -0.008(2) -0.002(2) 0.004(2) C37 0.026(3) 0.072(4) 0.058(3) -0.006(3) 0.003(2) 0.004(3) C38 0.038(3) 0.058(4) 0.036(3) -0.010(3) 0.008(2) -0.004(2) C39 0.021(2) 0.035(2) 0.038(2) 0.000(2) 0.0014(19) -0.0032(19) C40 0.032(2) 0.032(2) 0.031(2) -0.004(2) -0.0048(18) -0.0050(19) C41 0.039(3) 0.036(3) 0.032(2) -0.005(2) 0.001(2) -0.002(2) C42 0.037(3) 0.044(3) 0.050(3) -0.010(3) 0.013(2) -0.002(2) C43 0.028(2) 0.039(3) 0.049(3) -0.003(2) 0.002(2) -0.003(2) C44 0.028(2) 0.037(3) 0.041(3) 0.001(2) -0.001(2) -0.005(2) C45 0.026(2) 0.073(4) 0.048(3) 0.011(3) -0.009(2) -0.009(3) C46 0.048(4) 0.066(10) 0.062(4) 0.011(9) -0.023(4) 0.003(6) C47 0.027(3) 0.080(7) 0.078(5) -0.015(7) -0.008(4) 0.005(6) C46' 0.048(4) 0.066(10) 0.062(4) 0.011(9) -0.023(4) 0.003(6) C47' 0.027(3) 0.080(7) 0.078(5) -0.015(7) -0.008(4) 0.005(6) C48 0.031(3) 0.059(4) 0.064(4) -0.009(3) 0.002(3) 0.003(3) C49 0.027(2) 0.049(3) 0.028(2) 0.007(2) -0.0020(18) -0.007(2) C50 0.032(3) 0.060(4) 0.026(2) -0.001(2) 0.0027(19) -0.008(2) C51 0.044(3) 0.071(4) 0.036(3) -0.008(3) 0.010(2) -0.002(3) C52 0.048(3) 0.105(6) 0.033(3) 0.007(3) 0.013(3) -0.015(4) C53 0.034(3) 0.085(5) 0.048(3) 0.020(3) 0.004(2) -0.013(3) C54 0.027(2) 0.065(4) 0.043(3) 0.015(3) -0.002(2) -0.011(2) C55 0.039(3) 0.057(4) 0.066(4) 0.024(3) -0.010(3) -0.012(3) C56 0.067(7) 0.073(7) 0.093(8) 0.021(6) -0.008(6) -0.027(6) C57 0.069(7) 0.073(5) 0.083(5) 0.033(4) -0.006(5) -0.023(5) C56' 0.064(8) 0.071(9) 0.067(8) 0.012(7) 0.008(7) -0.010(7) C57' 0.069(7) 0.073(5) 0.083(5) 0.033(4) -0.006(5) -0.023(5) C58 0.061(4) 0.133(8) 0.081(5) 0.052(5) 0.023(4) -0.025(5) C59 0.025(2) 0.037(3) 0.040(2) -0.006(2) -0.0048(19) -0.0055(19) C60 0.030(2) 0.040(3) 0.040(3) -0.010(2) -0.002(2) -0.007(2) C61 0.030(3) 0.046(3) 0.050(3) -0.011(3) 0.007(2) -0.007(2) C62 0.033(3) 0.040(3) 0.061(3) -0.003(3) 0.004(2) -0.011(2) C63 0.041(3) 0.034(3) 0.051(3) -0.005(2) 0.008(2) -0.006(2) C64 0.032(3) 0.047(3) 0.044(3) -0.009(2) 0.005(2) -0.001(2) C65 0.049(3) 0.042(3) 0.048(3) -0.012(3) 0.008(3) -0.004(2) C66 0.068(4) 0.045(3) 0.071(4) -0.007(3) 0.022(3) -0.013(3) C67 0.076(4) 0.044(3) 0.065(4) -0.008(3) 0.034(3) -0.002(3) C68 0.046(3) 0.039(4) 0.045(4) -0.005(3) -0.011(3) -0.011(3) C69 0.064(5) 0.061(5) 0.043(4) -0.014(4) -0.006(4) -0.007(4) C70 0.059(5) 0.066(5) 0.051(5) -0.019(4) -0.030(4) -0.012(4) C71 0.055(4) 0.059(5) 0.044(6) -0.002(5) -0.017(4) -0.016(4) C72 0.043(3) 0.054(5) 0.042(5) 0.006(4) -0.015(4) -0.019(3) C73 0.043(3) 0.037(4) 0.040(4) 0.001(4) -0.013(3) -0.017(3) C74 0.095(9) 0.111(9) 0.096(9) -0.012(6) -0.013(6) 0.008(7) C75 0.067(7) 0.092(8) 0.080(7) 0.002(6) -0.010(5) -0.012(5) C76 0.035(6) 0.036(6) 0.034(5) -0.001(5) -0.007(4) -0.003(4) C68' 0.046(3) 0.039(4) 0.045(4) -0.005(3) -0.011(3) -0.011(3) C69' 0.064(5) 0.061(5) 0.043(4) -0.014(4) -0.006(4) -0.007(4) C70' 0.059(5) 0.066(5) 0.051(5) -0.019(4) -0.030(4) -0.012(4) C71' 0.055(4) 0.059(5) 0.044(6) -0.002(5) -0.017(4) -0.016(4) C72' 0.043(3) 0.054(5) 0.042(5) 0.006(4) -0.015(4) -0.019(3) C73' 0.043(3) 0.037(4) 0.040(4) 0.001(4) -0.013(3) -0.017(3) C74' 0.091(10) 0.110(10) 0.039(6) -0.029(6) -0.031(6) 0.007(8) C75' 0.057(7) 0.082(9) 0.083(9) -0.002(7) -0.022(6) -0.017(7) C76' 0.046(9) 0.042(8) 0.056(8) 0.007(8) 0.006(7) -0.013(7) C77 0.024(2) 0.031(2) 0.030(2) -0.0016(19) 0.0036(17) -0.0001(18) C78 0.030(2) 0.030(2) 0.034(2) 0.001(2) 0.0020(19) 0.0027(18) C79 0.039(3) 0.043(3) 0.030(2) 0.003(2) 0.002(2) 0.000(2) C80 0.050(3) 0.060(4) 0.033(3) 0.007(3) 0.015(2) 0.004(3) C81 0.033(3) 0.044(3) 0.043(3) 0.004(2) 0.005(2) -0.006(2) C82 0.030(2) 0.034(3) 0.035(2) 0.000(2) -0.0028(19) -0.0033(19) C83 0.027(2) 0.041(3) 0.037(2) -0.006(2) -0.0026(19) 0.001(2) C84 0.039(3) 0.061(4) 0.051(3) -0.006(3) -0.009(2) -0.002(3) C85 0.022(3) 0.089(5) 0.067(4) 0.005(4) -0.002(2) -0.006(3) C86 0.038(3) 0.066(4) 0.055(3) -0.001(3) 0.005(3) -0.007(3) C87 0.023(2) 0.034(2) 0.029(2) -0.002(2) -0.0012(17) 0.0024(18) C88 0.028(2) 0.040(3) 0.024(2) -0.0004(19) -0.0048(17) 0.0064(19) C89 0.026(2) 0.046(3) 0.034(2) 0.005(2) -0.0011(19) 0.001(2) C90 0.030(3) 0.060(3) 0.025(2) -0.008(2) 0.0020(18) 0.011(2) C91 0.023(2) 0.046(3) 0.034(2) -0.005(2) -0.0034(18) 0.009(2) C92 0.023(2) 0.039(3) 0.036(2) -0.005(2) 0.0002(18) 0.0063(19) C93 0.054(3) 0.029(3) 0.044(3) -0.002(2) -0.001(2) 0.001(2) C94 0.075(5) 0.049(4) 0.082(5) -0.016(4) 0.022(4) -0.005(3) C95 0.075(4) 0.050(4) 0.058(4) -0.013(3) -0.007(3) 0.008(3) C96 0.027(3) 0.065(4) 0.043(3) -0.021(3) -0.002(2) 0.012(2) C97 0.035(2) 0.033(3) 0.028(2) 0.001(2) -0.0027(18) 0.0019(19) C98 0.028(2) 0.040(3) 0.036(2) 0.008(2) -0.0016(19) 0.003(2) C99 0.030(2) 0.043(3) 0.037(3) 0.003(2) 0.005(2) 0.006(2) C100 0.040(3) 0.034(3) 0.045(3) -0.005(2) 0.003(2) 0.008(2) C101 0.048(3) 0.032(3) 0.053(3) 0.006(2) 0.004(2) 0.000(2) C102 0.045(3) 0.034(3) 0.040(3) 0.005(2) 0.002(2) -0.003(2) C103 0.050(3) 0.036(3) 0.039(3) 0.007(2) 0.008(2) 0.004(2) C104 0.075(4) 0.038(3) 0.063(4) -0.013(3) 0.010(3) 0.003(3) C105 0.080(5) 0.036(3) 0.061(4) 0.007(3) 0.030(3) -0.007(3) C106 0.029(2) 0.031(2) 0.048(3) 0.002(2) -0.002(2) 0.0024(19) C107 0.043(3) 0.037(3) 0.041(3) -0.002(2) 0.002(2) 0.007(2) C108 0.033(3) 0.039(3) 0.060(3) -0.003(3) 0.007(2) 0.006(2) C109 0.031(3) 0.041(3) 0.059(3) -0.003(3) -0.006(2) 0.007(2) C110 0.039(3) 0.035(3) 0.052(3) 0.001(2) -0.008(2) 0.007(2) C111 0.038(3) 0.032(3) 0.043(3) -0.001(2) -0.005(2) 0.004(2) C112 0.050(3) 0.064(4) 0.043(3) 0.003(3) 0.007(3) 0.006(3) C113 0.030(3) 0.064(4) 0.082(4) -0.004(3) 0.002(3) 0.011(3) C114 0.042(3) 0.062(4) 0.044(3) 0.003(3) -0.010(2) -0.001(3) C115 0.069(4) 0.054(4) 0.045(3) 0.010(3) 0.001(3) -0.009(3) C116 0.043(3) 0.053(3) 0.038(3) 0.000(3) -0.001(2) 0.007(3) C117 0.034(3) 0.057(4) 0.054(3) -0.012(3) 0.006(2) -0.013(3) C118 0.030(2) 0.041(3) 0.046(3) -0.009(2) 0.000(2) -0.006(2) C119 0.050(3) 0.068(4) 0.035(3) 0.004(3) -0.001(2) -0.011(3) C120 0.088(5) 0.059(4) 0.063(4) 0.026(4) -0.003(4) 0.010(4) C121 0.049(4) 0.068(4) 0.070(4) 0.005(3) -0.013(3) 0.013(3) C122 0.056(4) 0.062(4) 0.053(3) -0.007(3) 0.009(3) 0.010(3) C123 0.037(3) 0.073(4) 0.049(3) 0.005(3) 0.002(2) -0.010(3) C124 0.047(3) 0.090(5) 0.072(4) 0.024(4) -0.025(3) -0.022(4) C125 0.195(11) 0.126(9) 0.068(5) -0.052(5) 0.036(6) -0.100(8) C126 0.069(4) 0.086(5) 0.057(4) -0.026(4) 0.020(3) 0.001(4) C127 0.269(16) 0.054(5) 0.112(7) 0.009(5) -0.099(9) -0.048(7) C128 0.152(9) 0.025(3) 0.074(5) -0.004(3) -0.045(5) 0.009(4) C129 0.141(9) 0.050(4) 0.063(5) -0.006(4) 0.023(5) -0.011(5) C130 0.109(7) 0.085(6) 0.078(5) 0.023(5) 0.029(5) 0.038(5) C131 0.070(5) 0.107(7) 0.106(6) 0.038(5) 0.025(5) 0.027(5) C132 0.077(5) 0.107(7) 0.056(4) 0.027(4) 0.009(4) 0.025(5) C133 0.084(5) 0.057(4) 0.062(4) -0.008(3) -0.002(4) 0.019(4) C134 0.057(4) 0.059(4) 0.063(4) 0.007(3) -0.009(3) -0.006(3) C135 0.055(3) 0.037(3) 0.050(3) 0.003(3) 0.000(3) -0.004(3) C136 0.057(3) 0.043(3) 0.050(3) 0.007(3) -0.003(3) -0.010(3) C137 0.055(4) 0.041(3) 0.083(4) 0.008(3) -0.018(3) -0.002(3) C138 0.056(4) 0.041(4) 0.117(6) -0.001(4) 0.015(4) 0.003(3) C139 0.072(5) 0.056(4) 0.078(5) -0.013(4) 0.027(4) -0.018(4) C140 0.078(5) 0.054(4) 0.050(3) 0.002(3) 0.003(3) -0.013(3) C141 0.083(8) 0.081(8) 0.082(8) 0.024(7) 0.017(7) 0.024(7) C142 0.064(7) 0.048(6) 0.064(7) -0.002(6) 0.006(6) -0.007(6) C143 0.072(8) 0.056(7) 0.056(7) 0.006(6) -0.004(6) -0.014(6) C144 0.079(8) 0.067(8) 0.073(8) -0.004(7) -0.004(7) -0.009(7) C145 0.058(7) 0.080(8) 0.073(8) -0.008(7) 0.009(6) -0.004(6) C146 0.085(9) 0.084(9) 0.087(8) 0.000(7) 0.011(7) -0.016(7) C147 0.067(8) 0.066(8) 0.057(7) -0.004(6) 0.006(6) -0.001(7) C148 0.131(12) 0.137(12) 0.146(12) -0.017(9) 0.001(9) 0.001(9) C149 0.100(10) 0.080(9) 0.101(9) -0.017(8) 0.019(8) 0.001(8) C150 0.066(7) 0.054(7) 0.073(7) -0.028(6) 0.013(6) -0.028(6) C151 0.086(8) 0.077(8) 0.088(8) 0.004(7) -0.009(7) -0.016(7) C152 0.091(10) 0.071(9) 0.118(10) 0.009(8) -0.014(8) -0.014(8) C153 0.111(10) 0.098(10) 0.088(9) 0.004(8) 0.016(8) 0.001(8) C154 0.115(10) 0.096(10) 0.086(9) -0.002(7) 0.005(8) -0.005(8) _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 N4 2.015(4) . ? Zr1 N3 2.037(4) . ? Zr1 N2 2.247(3) . ? Zr1 N1 2.252(4) . ? Zr1 O1 2.344(3) . ? Zr1 O3 2.365(3) . ? Zr1 S1 2.9790(14) . ? Zr1 S2 2.9887(12) . ? Zr2 N10 2.038(4) . ? Zr2 N9 2.041(4) . ? Zr2 N6 2.239(4) . ? Zr2 N5 2.247(4) . ? Zr2 O5 2.338(3) . ? Zr2 O7 2.386(4) . ? Zr2 S3 2.9768(15) . ? Zr2 S4 2.9897(14) . ? Zr3 N11 2.041(4) . ? Zr3 N12 2.046(4) . ? Zr3 N8 2.226(4) . ? Zr3 N7 2.239(4) . ? Zr3 O9 2.346(3) . ? Zr3 O11 2.391(3) . ? Zr3 S5 2.9802(15) . ? Zr3 S6 2.9868(13) . ? S1 O2 1.432(3) . ? S1 O1 1.482(3) . ? S1 N1 1.589(4) . ? S1 C21 1.787(5) . ? S2 O4 1.425(3) . ? S2 O3 1.477(3) . ? S2 N2 1.574(4) . ? S2 C30 1.779(5) . ? S3 O6 1.422(3) . ? S3 O5 1.491(4) . ? S3 N5 1.574(4) . ? S3 C59 1.788(5) . ? S4 O8 1.425(4) . ? S4 O7 1.481(4) . ? S4 N6 1.578(4) . ? S4 C68' 1.737(7) . ? S4 C68 1.859(6) . ? S5 O10 1.446(3) . ? S5 O9 1.487(4) . ? S5 N7 1.566(4) . ? S5 C97 1.787(5) . ? S6 O12 1.438(3) . ? S6 O11 1.480(3) . ? S6 N8 1.582(4) . ? S6 C106 1.790(5) . ? N1 C2 1.414(5) . ? N2 C12 1.427(6) . ? N3 C115 1.442(7) . ? N3 C116 1.468(6) . ? N4 C117 1.451(6) . ? N4 C118 1.454(6) . ? N5 C40 1.422(6) . ? N6 C50 1.429(6) . ? N7 C78 1.450(6) . ? N8 C88 1.430(6) . ? N9 C120 1.433(8) . ? N9 C119 1.440(7) . ? N10 C121 1.450(7) . ? N10 C122 1.454(6) . ? N11 C124 1.438(6) . ? N11 C123 1.454(6) . ? N12 C126 1.426(7) . ? N12 C125 1.440(8) . ? C1 C2 1.397(6) . ? C1 C6 1.416(6) . ? C1 C11 1.511(6) . ? C2 C3 1.384(6) . ? C3 C4 1.399(6) . ? C3 H3 0.9500 . ? C4 C5 1.408(6) . ? C4 H4 0.9500 . ? C5 C6 1.396(6) . ? C5 C10 1.511(6) . ? C6 C7 1.513(6) . ? C7 C8 1.538(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.523(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.526(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.395(6) . ? C11 C16 1.407(6) . ? C12 C13 1.390(6) . ? C13 C14 1.376(7) . ? C13 H13 0.9500 . ? C14 C15 1.387(7) . ? C14 H14 0.9500 . ? C15 C16 1.405(6) . ? C15 C20 1.511(7) . ? C16 C17 1.510(7) . ? C17 C18' 1.532(8) . ? C17 C18 1.536(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9601 . ? C17 H17C 0.9601 . ? C17 H17D 0.9599 . ? C18 C19 1.531(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.575(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C18' C19' 1.516(9) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20 1.506(9) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20 H20A 0.9599 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 H20D 0.9601 . ? C21 C22 1.413(6) . ? C21 C26 1.421(6) . ? C22 C23 1.378(7) . ? C22 C27 1.515(7) . ? C23 C24 1.396(7) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 C28 1.509(7) . ? C25 C26 1.388(7) . ? C25 H25 0.9500 . ? C26 C29 1.522(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.407(6) . ? C30 C35 1.426(6) . ? C31 C32 1.377(7) . ? C31 C36 1.526(6) . ? C32 C33 1.385(7) . ? C32 H32 0.9500 . ? C33 C34 1.392(7) . ? C33 C37 1.502(7) . ? C34 C35 1.400(7) . ? C34 H34 0.9500 . ? C35 C38 1.504(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.403(6) . ? C39 C44 1.418(6) . ? C39 C49 1.504(6) . ? C40 C41 1.396(6) . ? C41 C42 1.395(7) . ? C41 H41A 0.9500 . ? C42 C43 1.401(7) . ? C42 H42A 0.9500 . ? C43 C44 1.405(7) . ? C43 C48 1.509(7) . ? C44 C45 1.502(7) . ? C45 C46 1.529(8) . ? C45 C46' 1.537(9) . ? C45 H45A 0.9602 . ? C45 H45B 0.9601 . ? C45 H45C 0.9602 . ? C45 H45D 0.9602 . ? C46 C47 1.530(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.531(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C46' C47' 1.529(10) . ? C46' H46C 0.9900 . ? C46' H46D 0.9900 . ? C47' C48 1.544(9) . ? C47' H47C 0.9900 . ? C47' H47D 0.9900 . ? C48 H48A 0.9602 . ? C48 H48B 0.9601 . ? C48 H48C 0.9600 . ? C48 H48D 0.9601 . ? C49 C50 1.394(7) . ? C49 C54 1.404(7) . ? C50 C51 1.398(6) . ? C51 C52 1.394(9) . ? C51 H51A 0.9500 . ? C52 C53 1.373(9) . ? C52 H52A 0.9500 . ? C53 C54 1.389(7) . ? C53 C58 1.512(8) . ? C54 C55 1.502(8) . ? C55 C56 1.530(8) . ? C55 C56' 1.556(9) . ? C55 H55A 0.9601 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C55 H55D 0.9600 . ? C56 C57 1.527(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.508(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C56' C57' 1.517(10) . ? C56' H56C 0.9900 . ? C56' H56D 0.9900 . ? C57' C58 1.518(9) . ? C57' H57C 0.9900 . ? C57' H57D 0.9900 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C58 H58D 0.9600 . ? C59 C60 1.417(6) . ? C59 C64 1.423(7) . ? C60 C61 1.384(7) . ? C60 C65 1.536(7) . ? C61 C62 1.382(7) . ? C61 H61A 0.9500 . ? C62 C63 1.375(7) . ? C62 C66 1.516(7) . ? C63 C64 1.395(7) . ? C63 H63A 0.9500 . ? C64 C67 1.512(7) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.3900 . ? C68 C73 1.3900 . ? C69 C70 1.3900 . ? C69 C74 1.509(9) . ? C70 C71 1.3900 . ? C70 H70A 0.9500 . ? C71 C72 1.3900 . ? C71 C75 1.534(9) . ? C72 C73 1.3900 . ? C72 H72A 0.9500 . ? C73 C76 1.503(9) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C68' C69' 1.3900 . ? C68' C73' 1.3900 . ? C69' C70' 1.3900 . ? C69' C74' 1.507(9) . ? C70' C71' 1.3900 . ? C70' H70B 0.9500 . ? C71' C72' 1.3900 . ? C71' C75' 1.506(9) . ? C72' C73' 1.3900 . ? C72' H72B 0.9500 . ? C73' C76' 1.505(9) . ? C74' H74D 0.9800 . ? C74' H74E 0.9800 . ? C74' H74F 0.9800 . ? C75' H75D 0.9800 . ? C75' H75E 0.9800 . ? C75' H75F 0.9800 . ? C76' H76D 0.9800 . ? C76' H76E 0.9800 . ? C76' H76F 0.9800 . ? C77 C78 1.391(6) . ? C77 C82 1.424(6) . ? C77 C87 1.513(6) . ? C78 C79 1.397(6) . ? C79 C80 1.389(7) . ? C79 H79 0.9500 . ? C80 C81 1.390(7) . ? C80 H80 0.9500 . ? C81 C82 1.404(6) . ? C81 C86 1.512(7) . ? C82 C83 1.506(6) . ? C83 C84 1.529(7) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 C85 1.491(8) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.517(8) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.398(7) . ? C87 C92 1.405(6) . ? C88 C89 1.403(6) . ? C89 C90 1.387(7) . ? C89 H89 0.9500 . ? C90 C91 1.378(7) . ? C90 H90 0.9500 . ? C91 C92 1.411(6) . ? C91 C96 1.519(7) . ? C92 C93 1.516(7) . ? C93 C94 1.520(8) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.467(8) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.538(8) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.411(6) . ? C97 C102 1.429(7) . ? C98 C99 1.389(7) . ? C98 C103 1.502(7) . ? C99 C100 1.378(7) . ? C99 H99 0.9500 . ? C100 C101 1.386(7) . ? C100 C104 1.523(7) . ? C101 C102 1.402(7) . ? C101 H101 0.9500 . ? C102 C105 1.515(7) . ? C103 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C104 H10F 0.9800 . ? C104 H10G 0.9800 . ? C104 H10H 0.9800 . ? C105 H10I 0.9800 . ? C105 H10J 0.9800 . ? C105 H10K 0.9800 . ? C106 C107 1.406(7) . ? C106 C111 1.417(6) . ? C107 C108 1.409(7) . ? C107 C112 1.505(7) . ? C108 C109 1.389(7) . ? C108 H108 0.9500 . ? C109 C110 1.378(7) . ? C109 C113 1.510(7) . ? C110 C111 1.404(7) . ? C110 H110 0.9500 . ? C111 C114 1.526(7) . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C113 H11D 0.9800 . ? C113 H11E 0.9800 . ? C113 H11F 0.9800 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C114 H11I 0.9800 . ? C115 H11J 0.9800 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C116 H11M 0.9800 . ? C116 H11N 0.9800 . ? C116 H11O 0.9800 . ? C117 H11P 0.9800 . ? C117 H11Q 0.9800 . ? C117 H11R 0.9800 . ? C118 H11S 0.9800 . ? C118 H11T 0.9800 . ? C118 H11U 0.9800 . ? C119 H11V 0.9800 . ? C119 H11W 0.9800 . ? C119 H11X 0.9800 . ? C120 H12P 0.9800 . ? C120 H12Q 0.9800 . ? C120 H12R 0.9800 . ? C121 H12S 0.9800 . ? C121 H12T 0.9800 . ? C121 H12U 0.9800 . ? C122 H12V 0.9800 . ? C122 H12W 0.9800 . ? C122 H12X 0.9800 . ? C123 H12A 0.9800 . ? C123 H12B 0.9800 . ? C123 H12C 0.9800 . ? C124 H12D 0.9800 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C126 H12L 0.9800 . ? C127 C128 1.444(12) . ? C127 H12M 0.9800 . ? C127 H12N 0.9800 . ? C127 H12O 0.9800 . ? C128 C129 1.414(12) . ? C128 C133 1.440(10) . ? C129 C130 1.322(12) . ? C129 H129 0.9500 . ? C130 C131 1.337(10) . ? C130 H130 0.9500 . ? C131 C132 1.384(10) . ? C131 H131 0.9500 . ? C132 C133 1.368(10) . ? C132 H132 0.9500 . ? C133 H133 0.9500 . ? C134 C135 1.517(8) . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C135 C136 1.376(8) . ? C135 C140 1.394(8) . ? C136 C137 1.366(9) . ? C136 H136 0.9500 . ? C137 C138 1.393(9) . ? C137 H137 0.9500 . ? C138 C139 1.391(10) . ? C138 H138 0.9500 . ? C139 C140 1.366(10) . ? C139 H139 0.9500 . ? C140 H140 0.9500 . ? C141 C142 1.503(7) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C142 C143 1.3900 . ? C142 C147 1.3900 . ? C143 C144 1.3900 . ? C143 H143 0.9500 . ? C144 C145 1.3900 . ? C144 H144 0.9500 . ? C145 C146 1.3900 . ? C145 H145 0.9500 . ? C146 C147 1.3900 . ? C146 H146 0.9500 . ? C147 H147 0.9500 . ? C148 C149 1.491(7) . ? C148 H14D 0.9800 . ? C148 H14E 0.9800 . ? C148 H14F 0.9800 . ? C149 C150 1.3900 . ? C149 C154 1.3900 . ? C150 C151 1.3900 . ? C150 H15A 0.9500 . ? C151 C152 1.3900 . ? C151 H15B 0.9500 . ? C152 C153 1.3900 . ? C152 H15C 0.9500 . ? C153 C154 1.3900 . ? C153 H15D 0.9500 . ? C154 H15E 0.9500 . ? 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 N4 Zr1 N3 104.48(17) . . ? N4 Zr1 N2 100.83(14) . . ? N3 Zr1 N2 137.19(14) . . ? N4 Zr1 N1 133.42(15) . . ? N3 Zr1 N1 107.71(15) . . ? N2 Zr1 N1 76.98(13) . . ? N4 Zr1 O1 86.39(14) . . ? N3 Zr1 O1 90.75(14) . . ? N2 Zr1 O1 125.03(12) . . ? N1 Zr1 O1 60.72(11) . . ? N4 Zr1 O3 94.31(14) . . ? N3 Zr1 O3 83.84(14) . . ? N2 Zr1 O3 60.16(12) . . ? N1 Zr1 O3 121.62(12) . . ? O1 Zr1 O3 174.55(11) . . ? N4 Zr1 S1 112.12(12) . . ? N3 Zr1 S1 97.30(12) . . ? N2 Zr1 S1 104.41(10) . . ? N1 Zr1 S1 31.66(9) . . ? O1 Zr1 S1 29.34(8) . . ? O3 Zr1 S1 152.14(8) . . ? N4 Zr1 S2 97.05(11) . . ? N3 Zr1 S2 111.05(12) . . ? N2 Zr1 S2 31.06(10) . . ? N1 Zr1 S2 101.70(9) . . ? O1 Zr1 S2 156.08(8) . . ? O3 Zr1 S2 29.18(8) . . ? S1 Zr1 S2 132.55(3) . . ? N10 Zr2 N9 104.35(18) . . ? N10 Zr2 N6 104.38(16) . . ? N9 Zr2 N6 134.54(16) . . ? N10 Zr2 N5 136.87(17) . . ? N9 Zr2 N5 103.85(16) . . ? N6 Zr2 N5 77.00(14) . . ? N10 Zr2 O5 85.96(15) . . ? N9 Zr2 O5 92.72(15) . . ? N6 Zr2 O5 123.73(13) . . ? N5 Zr2 O5 60.73(13) . . ? N10 Zr2 O7 92.96(16) . . ? N9 Zr2 O7 83.78(16) . . ? N6 Zr2 O7 60.29(13) . . ? N5 Zr2 O7 122.02(13) . . ? O5 Zr2 O7 175.98(12) . . ? N10 Zr2 S3 112.89(13) . . ? N9 Zr2 S3 97.17(13) . . ? N6 Zr2 S3 103.12(11) . . ? N5 Zr2 S3 31.29(10) . . ? O5 Zr2 S3 29.59(9) . . ? O7 Zr2 S3 152.80(9) . . ? N10 Zr2 S4 97.64(13) . . ? N9 Zr2 S4 110.41(13) . . ? N6 Zr2 S4 31.11(11) . . ? N5 Zr2 S4 102.28(10) . . ? O5 Zr2 S4 154.68(9) . . ? O7 Zr2 S4 29.33(9) . . ? S3 Zr2 S4 132.07(4) . . ? N11 Zr3 N12 107.98(17) . . ? N11 Zr3 N8 104.51(15) . . ? N12 Zr3 N8 133.22(15) . . ? N11 Zr3 N7 133.32(15) . . ? N12 Zr3 N7 102.98(15) . . ? N8 Zr3 N7 76.55(14) . . ? N11 Zr3 O9 83.81(14) . . ? N12 Zr3 O9 93.28(14) . . ? N8 Zr3 O9 123.15(13) . . ? N7 Zr3 O9 60.08(12) . . ? N11 Zr3 O11 94.40(14) . . ? N12 Zr3 O11 84.50(14) . . ? N8 Zr3 O11 60.09(12) . . ? N7 Zr3 O11 122.93(12) . . ? O9 Zr3 O11 176.59(12) . . ? N11 Zr3 S5 110.67(12) . . ? N12 Zr3 S5 95.88(12) . . ? N8 Zr3 S5 103.13(10) . . ? N7 Zr3 S5 30.98(9) . . ? O9 Zr3 S5 29.46(9) . . ? O11 Zr3 S5 153.29(9) . . ? N11 Zr3 S6 96.80(12) . . ? N12 Zr3 S6 111.32(12) . . ? N8 Zr3 S6 31.20(10) . . ? N7 Zr3 S6 103.52(10) . . ? O9 Zr3 S6 153.65(8) . . ? O11 Zr3 S6 29.38(8) . . ? S5 Zr3 S6 133.01(4) . . ? O2 S1 O1 114.39(19) . . ? O2 S1 N1 116.15(19) . . ? O1 S1 N1 98.34(18) . . ? O2 S1 C21 108.0(2) . . ? O1 S1 C21 110.4(2) . . ? N1 S1 C21 109.2(2) . . ? O2 S1 Zr1 124.66(14) . . ? O1 S1 Zr1 50.84(12) . . ? N1 S1 Zr1 48.06(13) . . ? C21 S1 Zr1 127.27(15) . . ? O4 S2 O3 116.0(2) . . ? O4 S2 N2 116.4(2) . . ? O3 S2 N2 98.61(18) . . ? O4 S2 C30 108.7(2) . . ? O3 S2 C30 107.9(2) . . ? N2 S2 C30 108.6(2) . . ? O4 S2 Zr1 129.38(14) . . ? O3 S2 Zr1 51.31(13) . . ? N2 S2 Zr1 47.46(13) . . ? C30 S2 Zr1 121.88(16) . . ? O6 S3 O5 114.6(2) . . ? O6 S3 N5 116.7(2) . . ? O5 S3 N5 98.3(2) . . ? O6 S3 C59 108.1(2) . . ? O5 S3 C59 109.1(2) . . ? N5 S3 C59 109.6(2) . . ? O6 S3 Zr2 126.94(16) . . ? O5 S3 Zr2 50.73(13) . . ? N5 S3 Zr2 47.85(14) . . ? C59 S3 Zr2 124.92(16) . . ? O8 S4 O7 115.2(2) . . ? O8 S4 N6 115.6(3) . . ? O7 S4 N6 99.0(2) . . ? O8 S4 C68' 104.1(6) . . ? O7 S4 C68' 111.2(7) . . ? N6 S4 C68' 112.0(8) . . ? O8 S4 C68 111.7(5) . . ? O7 S4 C68 106.7(6) . . ? N6 S4 C68 107.6(7) . . ? C68' S4 C68 7.6(9) . . ? O8 S4 Zr2 126.8(2) . . ? O7 S4 Zr2 52.12(14) . . ? N6 S4 Zr2 47.16(14) . . ? C68' S4 Zr2 129.0(6) . . ? C68 S4 Zr2 121.5(5) . . ? O10 S5 O9 115.0(2) . . ? O10 S5 N7 116.8(2) . . ? O9 S5 N7 97.6(2) . . ? O10 S5 C97 108.0(2) . . ? O9 S5 C97 110.4(2) . . ? N7 S5 C97 108.6(2) . . ? O10 S5 Zr3 124.85(15) . . ? O9 S5 Zr3 50.89(13) . . ? N7 S5 Zr3 47.39(15) . . ? C97 S5 Zr3 127.09(16) . . ? O12 S6 O11 114.8(2) . . ? O12 S6 N8 116.1(2) . . ? O11 S6 N8 98.24(19) . . ? O12 S6 C106 108.2(2) . . ? O11 S6 C106 110.6(2) . . ? N8 S6 C106 108.6(2) . . ? O12 S6 Zr3 123.03(15) . . ? O11 S6 Zr3 52.41(13) . . ? N8 S6 Zr3 46.79(13) . . ? C106 S6 Zr3 128.67(17) . . ? C2 N1 S1 126.0(3) . . ? C2 N1 Zr1 131.6(3) . . ? S1 N1 Zr1 100.28(17) . . ? C12 N2 S2 126.9(3) . . ? C12 N2 Zr1 130.2(3) . . ? S2 N2 Zr1 101.48(18) . . ? C115 N3 C116 111.1(4) . . ? C115 N3 Zr1 122.2(3) . . ? C116 N3 Zr1 124.1(3) . . ? C117 N4 C118 112.2(4) . . ? C117 N4 Zr1 119.8(3) . . ? C118 N4 Zr1 127.1(3) . . ? C40 N5 S3 127.1(3) . . ? C40 N5 Zr2 130.3(3) . . ? S3 N5 Zr2 100.86(19) . . ? C50 N6 S4 126.8(3) . . ? C50 N6 Zr2 130.1(3) . . ? S4 N6 Zr2 101.7(2) . . ? C78 N7 S5 125.2(3) . . ? C78 N7 Zr3 130.6(3) . . ? S5 N7 Zr3 101.63(19) . . ? C88 N8 S6 124.6(3) . . ? C88 N8 Zr3 130.8(3) . . ? S6 N8 Zr3 102.01(18) . . ? C120 N9 C119 112.5(5) . . ? C120 N9 Zr2 119.2(4) . . ? C119 N9 Zr2 125.8(4) . . ? C121 N10 C122 110.7(4) . . ? C121 N10 Zr2 122.3(4) . . ? C122 N10 Zr2 125.8(4) . . ? C124 N11 C123 109.6(4) . . ? C124 N11 Zr3 123.1(4) . . ? C123 N11 Zr3 126.6(3) . . ? C126 N12 C125 109.1(5) . . ? C126 N12 Zr3 126.9(4) . . ? C125 N12 Zr3 123.3(4) . . ? S1 O1 Zr1 99.82(15) . . ? S2 O3 Zr1 99.52(16) . . ? S3 O5 Zr2 99.68(16) . . ? S4 O7 Zr2 98.55(18) . . ? S5 O9 Zr3 99.65(16) . . ? S6 O11 Zr3 98.21(17) . . ? C2 C1 C6 119.4(4) . . ? C2 C1 C11 121.6(4) . . ? C6 C1 C11 119.0(4) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 N1 120.9(4) . . ? C1 C2 N1 118.1(4) . . ? C2 C3 C4 119.6(4) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.3(4) . . ? C6 C5 C10 122.3(4) . . ? C4 C5 C10 118.4(4) . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C7 120.5(4) . . ? C1 C6 C7 119.7(4) . . ? C6 C7 C8 114.2(4) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 110.5(4) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 109.2(4) . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? C5 C10 C9 113.3(4) . . ? C5 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C5 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 120.5(4) . . ? C12 C11 C1 120.8(4) . . ? C16 C11 C1 118.6(4) . . ? C13 C12 C11 119.7(4) . . ? C13 C12 N2 121.2(4) . . ? C11 C12 N2 118.5(4) . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 121.7(4) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 119.3(4) . . ? C14 C15 C20 119.6(4) . . ? C16 C15 C20 121.1(5) . . ? C15 C16 C11 118.8(5) . . ? C15 C16 C17 120.7(4) . . ? C11 C16 C17 120.2(4) . . ? C16 C17 C18' 111.2(6) . . ? C16 C17 C18 118.7(5) . . ? C18' C17 C18 27.8(5) . . ? C16 C17 H17A 107.9 . . ? C18' C17 H17A 86.1 . . ? C18 C17 H17A 107.4 . . ? C16 C17 H17B 107.5 . . ? C18' C17 H17B 132.5 . . ? C18 C17 H17B 107.6 . . ? H17A C17 H17B 107.3 . . ? C16 C17 H17C 109.3 . . ? C18' C17 H17C 108.8 . . ? C18 C17 H17C 123.9 . . ? H17A C17 H17C 25.9 . . ? H17B C17 H17C 82.5 . . ? C16 C17 H17D 109.4 . . ? C18' C17 H17D 109.9 . . ? C18 C17 H17D 82.5 . . ? H17A C17 H17D 129.7 . . ? H17B C17 H17D 28.7 . . ? H17C C17 H17D 108.2 . . ? C19 C18 C17 108.0(7) . . ? C19 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? C19 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C18 C19 C20 113.4(7) . . ? C18 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C19' C18' C17 110.6(9) . . ? C19' C18' H18C 109.5 . . ? C17 C18' H18C 109.5 . . ? C19' C18' H18D 109.5 . . ? C17 C18' H18D 109.5 . . ? H18C C18' H18D 108.1 . . ? C20 C19' C18' 106.0(9) . . ? C20 C19' H19C 110.5 . . ? C18' C19' H19C 110.5 . . ? C20 C19' H19D 110.5 . . ? C18' C19' H19D 110.5 . . ? H19C C19' H19D 108.7 . . ? C19' C20 C15 112.5(6) . . ? C19' C20 C19 31.4(5) . . ? C15 C20 C19 114.5(5) . . ? C19' C20 H20A 81.3 . . ? C15 C20 H20A 108.7 . . ? C19 C20 H20A 109.2 . . ? C19' C20 H20B 132.5 . . ? C15 C20 H20B 108.2 . . ? C19 C20 H20B 108.2 . . ? H20A C20 H20B 107.8 . . ? C19' C20 H20C 109.1 . . ? C15 C20 H20C 108.5 . . ? C19 C20 H20C 130.7 . . ? H20A C20 H20C 31.0 . . ? H20B C20 H20C 78.9 . . ? C19' C20 H20D 109.1 . . ? C15 C20 H20D 109.3 . . ? C19 C20 H20D 79.7 . . ? H20A C20 H20D 132.2 . . ? H20B C20 H20D 31.8 . . ? H20C C20 H20D 108.1 . . ? C22 C21 C26 120.1(4) . . ? C22 C21 S1 120.0(4) . . ? C26 C21 S1 119.6(3) . . ? C23 C22 C21 118.5(4) . . ? C23 C22 C27 116.9(4) . . ? C21 C22 C27 124.6(4) . . ? C22 C23 C24 122.9(4) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 117.5(5) . . ? C25 C24 C28 120.9(5) . . ? C23 C24 C28 121.5(5) . . ? C24 C25 C26 122.8(5) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C21 118.1(4) . . ? C25 C26 C29 115.8(4) . . ? C21 C26 C29 126.1(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 121.0(4) . . ? C31 C30 S2 119.5(3) . . ? C35 C30 S2 119.2(3) . . ? C32 C31 C30 117.9(4) . . ? C32 C31 C36 116.7(4) . . ? C30 C31 C36 125.4(4) . . ? C31 C32 C33 124.0(4) . . ? C31 C32 H32 118.0 . . ? C33 C32 H32 118.0 . . ? C32 C33 C34 116.7(4) . . ? C32 C33 C37 121.4(5) . . ? C34 C33 C37 121.9(5) . . ? C33 C34 C35 123.5(4) . . ? C33 C34 H34 118.3 . . ? C35 C34 H34 118.3 . . ? C34 C35 C30 116.7(4) . . ? C34 C35 C38 117.1(4) . . ? C30 C35 C38 126.2(4) . . ? 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 . . ? C33 C37 H37A 109.5 . . ? C33 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C33 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 119.9(4) . . ? C40 C39 C49 120.4(4) . . ? C44 C39 C49 119.7(4) . . ? C41 C40 C39 119.5(4) . . ? C41 C40 N5 121.2(4) . . ? C39 C40 N5 118.7(4) . . ? C42 C41 C40 120.2(4) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 121.3(5) . . ? C41 C42 H42A 119.4 . . ? C43 C42 H42A 119.4 . . ? C42 C43 C44 118.7(4) . . ? C42 C43 C48 118.5(5) . . ? C44 C43 C48 122.8(5) . . ? C43 C44 C39 120.0(4) . . ? C43 C44 C45 119.5(4) . . ? C39 C44 C45 120.5(4) . . ? C44 C45 C46 112.4(8) . . ? C44 C45 C46' 116.6(10) . . ? C46 C45 C46' 23.4(8) . . ? C44 C45 H45A 109.0 . . ? C46 C45 H45A 108.7 . . ? C46' C45 H45A 123.7 . . ? C44 C45 H45B 108.8 . . ? C46 C45 H45B 109.9 . . ? C46' C45 H45B 87.3 . . ? H45A C45 H45B 108.0 . . ? C44 C45 H45C 108.7 . . ? C46 C45 H45C 89.0 . . ? C46' C45 H45C 107.9 . . ? H45A C45 H45C 22.4 . . ? H45B C45 H45C 126.6 . . ? C44 C45 H45D 107.9 . . ? C46 C45 H45D 128.3 . . ? C46' C45 H45D 107.8 . . ? H45A C45 H45D 86.6 . . ? H45B C45 H45D 23.6 . . ? H45C C45 H45D 107.6 . . ? C45 C46 C47 110.2(8) . . ? C45 C46 H46A 109.6 . . ? C47 C46 H46A 109.6 . . ? C45 C46 H46B 109.6 . . ? C47 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C46 C47 C48 106.3(10) . . ? C46 C47 H47A 110.5 . . ? C48 C47 H47A 110.5 . . ? C46 C47 H47B 110.5 . . ? C48 C47 H47B 110.5 . . ? H47A C47 H47B 108.7 . . ? C47' C46' C45 113.2(12) . . ? C47' C46' H46C 108.9 . . ? C45 C46' H46C 108.9 . . ? C47' C46' H46D 108.9 . . ? C45 C46' H46D 108.9 . . ? H46C C46' H46D 107.8 . . ? C46' C47' C48 108.1(15) . . ? C46' C47' H47C 110.1 . . ? C48 C47' H47C 110.1 . . ? C46' C47' H47D 110.1 . . ? C48 C47' H47D 110.1 . . ? H47C C47' H47D 108.4 . . ? C43 C48 C47 114.1(5) . . ? C43 C48 C47' 113.4(7) . . ? C47 C48 C47' 35.2(7) . . ? C43 C48 H48A 108.1 . . ? C47 C48 H48A 108.1 . . ? C47' C48 H48A 133.7 . . ? C43 C48 H48B 109.2 . . ? C47 C48 H48B 109.5 . . ? C47' C48 H48B 77.4 . . ? H48A C48 H48B 107.8 . . ? C43 C48 H48C 108.7 . . ? C47 C48 H48C 76.1 . . ? C47' C48 H48C 108.9 . . ? H48A C48 H48C 35.5 . . ? H48B C48 H48C 134.6 . . ? C43 C48 H48D 108.8 . . ? C47 C48 H48D 132.9 . . ? C47' C48 H48D 109.0 . . ? H48A C48 H48D 75.0 . . ? H48B C48 H48D 35.1 . . ? H48C C48 H48D 107.9 . . ? C50 C49 C54 120.5(5) . . ? C50 C49 C39 121.0(4) . . ? C54 C49 C39 118.5(5) . . ? C49 C50 C51 119.7(5) . . ? C49 C50 N6 118.6(4) . . ? C51 C50 N6 121.1(5) . . ? C52 C51 C50 118.4(6) . . ? C52 C51 H51A 120.8 . . ? C50 C51 H51A 120.8 . . ? C53 C52 C51 122.5(5) . . ? C53 C52 H52A 118.8 . . ? C51 C52 H52A 118.8 . . ? C52 C53 C54 119.2(6) . . ? C52 C53 C58 118.6(6) . . ? C54 C53 C58 122.1(6) . . ? C53 C54 C49 119.5(6) . . ? C53 C54 C55 120.2(5) . . ? C49 C54 C55 120.2(5) . . ? C54 C55 C56 119.0(7) . . ? C54 C55 C56' 112.8(9) . . ? C56 C55 C56' 31.2(7) . . ? C54 C55 H55A 108.3 . . ? C56 C55 H55A 106.7 . . ? C56' C55 H55A 81.1 . . ? C54 C55 H55B 107.4 . . ? C56 C55 H55B 107.6 . . ? C56' C55 H55B 133.7 . . ? H55A C55 H55B 107.3 . . ? C54 C55 H55C 109.2 . . ? C56 C55 H55C 125.7 . . ? C56' C55 H55C 108.0 . . ? H55A C55 H55C 30.6 . . ? H55B C55 H55C 78.2 . . ? C54 C55 H55D 109.0 . . ? C56 C55 H55D 79.1 . . ? C56' C55 H55D 109.5 . . ? H55A C55 H55D 132.6 . . ? H55B C55 H55D 32.9 . . ? H55C C55 H55D 108.1 . . ? C57 C56 C55 106.1(10) . . ? C57 C56 H56A 110.5 . . ? C55 C56 H56A 110.5 . . ? C57 C56 H56B 110.5 . . ? C55 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? C58 C57 C56 117.4(11) . . ? C58 C57 H57A 108.0 . . ? C56 C57 H57A 108.0 . . ? C58 C57 H57B 107.9 . . ? C56 C57 H57B 107.9 . . ? H57A C57 H57B 107.2 . . ? C57' C56' C55 111.9(13) . . ? C57' C56' H56C 109.2 . . ? C55 C56' H56C 109.2 . . ? C57' C56' H56D 109.2 . . ? C55 C56' H56D 109.2 . . ? H56C C56' H56D 107.9 . . ? C56' C57' C58 108.3(13) . . ? C56' C57' H57C 110.0 . . ? C58 C57' H57C 110.0 . . ? C56' C57' H57D 110.0 . . ? C58 C57' H57D 110.0 . . ? H57C C57' H57D 108.4 . . ? C57 C58 C53 112.8(8) . . ? C57 C58 C57' 23.0(8) . . ? C53 C58 C57' 116.3(9) . . ? C57 C58 H58A 108.9 . . ? C53 C58 H58A 109.0 . . ? C57' C58 H58A 86.9 . . ? C57 C58 H58B 108.8 . . ? C53 C58 H58B 108.9 . . ? C57' C58 H58B 124.1 . . ? H58A C58 H58B 108.2 . . ? C57 C58 H58C 127.3 . . ? C53 C58 H58C 107.3 . . ? C57' C58 H58C 107.3 . . ? H58A C58 H58C 22.8 . . ? H58B C58 H58C 88.0 . . ? C57 C58 H58D 91.1 . . ? C53 C58 H58D 108.1 . . ? C57' C58 H58D 110.0 . . ? H58A C58 H58D 125.7 . . ? H58B C58 H58D 20.6 . . ? H58C C58 H58D 107.5 . . ? C60 C59 C64 119.6(5) . . ? C60 C59 S3 120.6(4) . . ? C64 C59 S3 119.5(4) . . ? C61 C60 C59 118.9(5) . . ? C61 C60 C65 117.2(4) . . ? C59 C60 C65 123.9(5) . . ? C62 C61 C60 122.3(5) . . ? C62 C61 H61A 118.8 . . ? C60 C61 H61A 118.8 . . ? C63 C62 C61 118.3(5) . . ? C63 C62 C66 120.8(5) . . ? C61 C62 C66 120.9(5) . . ? C62 C63 C64 123.1(5) . . ? C62 C63 H63A 118.5 . . ? C64 C63 H63A 118.5 . . ? C63 C64 C59 117.8(5) . . ? C63 C64 C67 116.9(5) . . ? C59 C64 C67 125.3(5) . . ? C60 C65 H65A 109.5 . . ? C60 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C60 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C62 C66 H66A 109.5 . . ? C62 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C62 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C73 120.0 . . ? C69 C68 S4 120.3(7) . . ? C73 C68 S4 119.7(7) . . ? C70 C69 C68 120.0 . . ? C70 C69 C74 112.8(11) . . ? C68 C69 C74 126.9(11) . . ? C71 C70 C69 120.0 . . ? C71 C70 H70A 120.0 . . ? C69 C70 H70A 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 C75 119.9(8) . . ? C72 C71 C75 120.1(8) . . ? C71 C72 C73 120.0 . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C72 C73 C68 120.0 . . ? C72 C73 C76 113.8(14) . . ? C68 C73 C76 126.1(14) . . ? C69 C74 H74A 109.5 . . ? C69 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C69 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C71 C75 H75A 109.5 . . ? C71 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C71 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C69' C68' C73' 120.0 . . ? C69' C68' S4 121.1(9) . . ? C73' C68' S4 118.9(9) . . ? C68' C69' C70' 120.0 . . ? C68' C69' C74' 125.1(11) . . ? C70' C69' C74' 114.8(11) . . ? C71' C70' C69' 120.0 . . ? C71' C70' H70B 120.0 . . ? C69' C70' H70B 120.0 . . ? C70' C71' C72' 120.0 . . ? C70' C71' C75' 121.6(9) . . ? C72' C71' C75' 118.4(9) . . ? C71' C72' C73' 120.0 . . ? C71' C72' H72B 120.0 . . ? C73' C72' H72B 120.0 . . ? C72' C73' C68' 120.0 . . ? C72' C73' C76' 115.5(16) . . ? C68' C73' C76' 124.5(17) . . ? C69' C74' H74D 109.5 . . ? C69' C74' H74E 109.5 . . ? H74D C74' H74E 109.5 . . ? C69' C74' H74F 109.5 . . ? H74D C74' H74F 109.5 . . ? H74E C74' H74F 109.5 . . ? C71' C75' H75D 109.5 . . ? C71' C75' H75E 109.5 . . ? H75D C75' H75E 109.5 . . ? C71' C75' H75F 109.5 . . ? H75D C75' H75F 109.5 . . ? H75E C75' H75F 109.5 . . ? C73' C76' H76D 109.5 . . ? C73' C76' H76E 109.5 . . ? H76D C76' H76E 109.5 . . ? C73' C76' H76F 109.5 . . ? H76D C76' H76F 109.5 . . ? H76E C76' H76F 109.5 . . ? C78 C77 C82 119.7(4) . . ? C78 C77 C87 120.0(4) . . ? C82 C77 C87 120.3(4) . . ? C77 C78 C79 120.3(4) . . ? C77 C78 N7 118.7(4) . . ? C79 C78 N7 120.6(4) . . ? C80 C79 C78 119.1(4) . . ? C80 C79 H79 120.4 . . ? C78 C79 H79 120.4 . . ? C79 C80 C81 122.1(5) . . ? C79 C80 H80 119.0 . . ? C81 C80 H80 119.0 . . ? C80 C81 C82 118.8(5) . . ? C80 C81 C86 119.7(5) . . ? C82 C81 C86 121.5(5) . . ? C81 C82 C77 119.6(4) . . ? C81 C82 C83 119.6(4) . . ? C77 C82 C83 120.7(4) . . ? C82 C83 C84 114.1(4) . . ? C82 C83 H83A 108.7 . . ? C84 C83 H83A 108.7 . . ? C82 C83 H83B 108.7 . . ? C84 C83 H83B 108.7 . . ? H83A C83 H83B 107.6 . . ? C85 C84 C83 110.1(4) . . ? C85 C84 H84A 109.7 . . ? C83 C84 H84A 109.6 . . ? C85 C84 H84B 109.6 . . ? C83 C84 H84B 109.7 . . ? H84A C84 H84B 108.2 . . ? C84 C85 C86 111.0(5) . . ? C84 C85 H85A 109.4 . . ? C86 C85 H85A 109.4 . . ? C84 C85 H85B 109.4 . . ? C86 C85 H85B 109.4 . . ? H85A C85 H85B 108.0 . . ? C81 C86 C85 115.0(5) . . ? C81 C86 H86A 108.5 . . ? C85 C86 H86A 108.5 . . ? C81 C86 H86B 108.5 . . ? C85 C86 H86B 108.5 . . ? H86A C86 H86B 107.5 . . ? C88 C87 C92 119.1(4) . . ? C88 C87 C77 121.4(4) . . ? C92 C87 C77 119.4(4) . . ? C87 C88 C89 120.8(4) . . ? C87 C88 N8 118.0(4) . . ? C89 C88 N8 120.6(4) . . ? C90 C89 C88 118.9(5) . . ? C90 C89 H89 120.6 . . ? C88 C89 H89 120.6 . . ? C91 C90 C89 121.7(4) . . ? C91 C90 H90 119.2 . . ? C89 C90 H90 119.2 . . ? C90 C91 C92 119.5(4) . . ? C90 C91 C96 119.2(4) . . ? C92 C91 C96 121.3(5) . . ? C87 C92 C91 119.9(5) . . ? C87 C92 C93 119.5(4) . . ? C91 C92 C93 120.5(4) . . ? C92 C93 C94 114.5(5) . . ? C92 C93 H93A 108.6 . . ? C94 C93 H93A 108.6 . . ? C92 C93 H93B 108.6 . . ? C94 C93 H93B 108.6 . . ? H93A C93 H93B 107.6 . . ? C95 C94 C93 111.7(6) . . ? C95 C94 H94A 109.3 . . ? C93 C94 H94A 109.3 . . ? C95 C94 H94B 109.3 . . ? C93 C94 H94B 109.3 . . ? H94A C94 H94B 107.9 . . ? C94 C95 C96 111.7(5) . . ? C94 C95 H95A 109.3 . . ? C96 C95 H95A 109.3 . . ? C94 C95 H95B 109.3 . . ? C96 C95 H95B 109.3 . . ? H95A C95 H95B 107.9 . . ? C91 C96 C95 113.4(4) . . ? C91 C96 H96A 108.9 . . ? C95 C96 H96A 108.9 . . ? C91 C96 H96B 108.9 . . ? C95 C96 H96B 108.9 . . ? H96A C96 H96B 107.7 . . ? C98 C97 C102 121.1(4) . . ? C98 C97 S5 119.7(4) . . ? C102 C97 S5 119.1(4) . . ? C99 C98 C97 118.1(5) . . ? C99 C98 C103 116.1(4) . . ? C97 C98 C103 125.7(5) . . ? C100 C99 C98 122.2(4) . . ? C100 C99 H99 118.9 . . ? C98 C99 H99 118.9 . . ? C99 C100 C101 119.4(5) . . ? C99 C100 C104 120.8(5) . . ? C101 C100 C104 119.9(5) . . ? C100 C101 C102 122.0(5) . . ? C100 C101 H101 119.0 . . ? C102 C101 H101 119.0 . . ? C101 C102 C97 117.2(5) . . ? C101 C102 C105 116.7(5) . . ? C97 C102 C105 126.1(5) . . ? C98 C103 H10C 109.5 . . ? C98 C103 H10D 109.5 . . ? H10C C103 H10D 109.5 . . ? C98 C103 H10E 109.5 . . ? H10C C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C100 C104 H10F 109.5 . . ? C100 C104 H10G 109.5 . . ? H10F C104 H10G 109.5 . . ? C100 C104 H10H 109.5 . . ? H10F C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? C102 C105 H10I 109.5 . . ? C102 C105 H10J 109.5 . . ? H10I C105 H10J 109.5 . . ? C102 C105 H10K 109.5 . . ? H10I C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? C107 C106 C111 120.3(4) . . ? C107 C106 S6 119.5(4) . . ? C111 C106 S6 120.1(4) . . ? C106 C107 C108 118.2(5) . . ? C106 C107 C112 123.7(5) . . ? C108 C107 C112 118.0(5) . . ? C109 C108 C107 122.7(5) . . ? C109 C108 H108 118.7 . . ? C107 C108 H108 118.7 . . ? C110 C109 C108 117.6(5) . . ? C110 C109 C113 120.9(5) . . ? C108 C109 C113 121.5(5) . . ? C109 C110 C111 123.0(5) . . ? C109 C110 H110 118.5 . . ? C111 C110 H110 118.5 . . ? C110 C111 C106 118.2(5) . . ? C110 C111 C114 116.3(4) . . ? C106 C111 C114 125.5(4) . . ? C107 C112 H11A 109.5 . . ? C107 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C107 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C109 C113 H11D 109.5 . . ? C109 C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C109 C113 H11F 109.5 . . ? H11D C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? C111 C114 H11G 109.5 . . ? C111 C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C111 C114 H11I 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? N3 C115 H11J 109.5 . . ? N3 C115 H11K 109.5 . . ? H11J C115 H11K 109.5 . . ? N3 C115 H11L 109.5 . . ? H11J C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? N3 C116 H11M 109.5 . . ? N3 C116 H11N 109.5 . . ? H11M C116 H11N 109.5 . . ? N3 C116 H11O 109.5 . . ? H11M C116 H11O 109.5 . . ? H11N C116 H11O 109.5 . . ? N4 C117 H11P 109.5 . . ? N4 C117 H11Q 109.5 . . ? H11P C117 H11Q 109.5 . . ? N4 C117 H11R 109.5 . . ? H11P C117 H11R 109.5 . . ? H11Q C117 H11R 109.5 . . ? N4 C118 H11S 109.5 . . ? N4 C118 H11T 109.5 . . ? H11S C118 H11T 109.5 . . ? N4 C118 H11U 109.5 . . ? H11S C118 H11U 109.5 . . ? H11T C118 H11U 109.5 . . ? N9 C119 H11V 109.5 . . ? N9 C119 H11W 109.5 . . ? H11V C119 H11W 109.5 . . ? N9 C119 H11X 109.5 . . ? H11V C119 H11X 109.5 . . ? H11W C119 H11X 109.5 . . ? N9 C120 H12P 109.5 . . ? N9 C120 H12Q 109.5 . . ? H12P C120 H12Q 109.5 . . ? N9 C120 H12R 109.5 . . ? H12P C120 H12R 109.5 . . ? H12Q C120 H12R 109.5 . . ? N10 C121 H12S 109.5 . . ? N10 C121 H12T 109.5 . . ? H12S C121 H12T 109.5 . . ? N10 C121 H12U 109.5 . . ? H12S C121 H12U 109.5 . . ? H12T C121 H12U 109.5 . . ? N10 C122 H12V 109.5 . . ? N10 C122 H12W 109.5 . . ? H12V C122 H12W 109.5 . . ? N10 C122 H12X 109.5 . . ? H12V C122 H12X 109.5 . . ? H12W C122 H12X 109.5 . . ? N11 C123 H12A 109.5 . . ? N11 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? N11 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? N11 C124 H12D 109.5 . . ? N11 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? N11 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? N12 C125 H12G 109.5 . . ? N12 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? N12 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? N12 C126 H12J 109.5 . . ? N12 C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? N12 C126 H12L 109.5 . . ? H12J C126 H12L 109.5 . . ? H12K C126 H12L 109.5 . . ? C128 C127 H12M 109.5 . . ? C128 C127 H12N 109.5 . . ? H12M C127 H12N 109.5 . . ? C128 C127 H12O 109.5 . . ? H12M C127 H12O 109.5 . . ? H12N C127 H12O 109.5 . . ? C129 C128 C133 116.6(7) . . ? C129 C128 C127 127.1(9) . . ? C133 C128 C127 116.2(10) . . ? C130 C129 C128 122.9(8) . . ? C130 C129 H129 118.6 . . ? C128 C129 H129 118.6 . . ? C129 C130 C131 120.0(9) . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C130 C131 C132 121.4(9) . . ? C130 C131 H131 119.3 . . ? C132 C131 H131 119.3 . . ? C133 C132 C131 121.0(7) . . ? C133 C132 H132 119.5 . . ? C131 C132 H132 119.5 . . ? C132 C133 C128 118.0(8) . . ? C132 C133 H133 121.0 . . ? C128 C133 H133 121.0 . . ? C135 C134 H13A 109.5 . . ? C135 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C135 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? C136 C135 C140 116.9(6) . . ? C136 C135 C134 121.9(5) . . ? C140 C135 C134 121.2(6) . . ? C137 C136 C135 123.4(6) . . ? C137 C136 H136 118.3 . . ? C135 C136 H136 118.3 . . ? C136 C137 C138 119.3(6) . . ? C136 C137 H137 120.4 . . ? C138 C137 H137 120.4 . . ? C139 C138 C137 118.2(6) . . ? C139 C138 H138 120.9 . . ? C137 C138 H138 120.9 . . ? C140 C139 C138 121.4(6) . . ? C140 C139 H139 119.3 . . ? C138 C139 H139 119.3 . . ? C139 C140 C135 120.8(6) . . ? C139 C140 H140 119.6 . . ? C135 C140 H140 119.6 . . ? C143 C142 C147 120.0 . . ? C143 C142 C141 120.3(4) . . ? C147 C142 C141 119.7(4) . . ? C144 C143 C142 120.0 . . ? C144 C143 H143 120.0 . . ? C142 C143 H143 120.0 . . ? C143 C144 C145 120.0 . . ? C143 C144 H144 120.0 . . ? C145 C144 H144 120.0 . . ? C146 C145 C144 120.0 . . ? C146 C145 H145 120.0 . . ? C144 C145 H145 120.0 . . ? C145 C146 C147 120.0 . . ? C145 C146 H146 120.0 . . ? C147 C146 H146 120.0 . . ? C146 C147 C142 120.0 . . ? C146 C147 H147 120.0 . . ? C142 C147 H147 120.0 . . ? C149 C148 H14D 109.5 . . ? C149 C148 H14E 109.5 . . ? H14D C148 H14E 109.5 . . ? C149 C148 H14F 109.5 . . ? H14D C148 H14F 109.5 . . ? H14E C148 H14F 109.5 . . ? C150 C149 C154 120.0 . . ? C150 C149 C148 120.2(4) . . ? C154 C149 C148 119.8(4) . . ? C149 C150 C151 120.0 . . ? C149 C150 H15A 120.0 . . ? C151 C150 H15A 120.0 . . ? C152 C151 C150 120.0 . . ? C152 C151 H15B 120.0 . . ? C150 C151 H15B 120.0 . . ? C153 C152 C151 120.0 . . ? C153 C152 H15C 120.0 . . ? C151 C152 H15C 120.0 . . ? C152 C153 C154 120.0 . . ? C152 C153 H15D 120.0 . . ? C154 C153 H15D 120.0 . . ? C153 C154 C149 120.0 . . ? C153 C154 H15E 120.0 . . ? C149 C154 H15E 120.0 . . ? 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 N4 Zr1 S1 O2 125.3(2) . . . . ? N3 Zr1 S1 O2 16.4(2) . . . . ? N2 Zr1 S1 O2 -126.4(2) . . . . ? N1 Zr1 S1 O2 -95.7(2) . . . . ? O1 Zr1 S1 O2 94.8(2) . . . . ? O3 Zr1 S1 O2 -74.2(2) . . . . ? S2 Zr1 S1 O2 -111.10(18) . . . . ? N4 Zr1 S1 O1 30.5(2) . . . . ? N3 Zr1 S1 O1 -78.4(2) . . . . ? N2 Zr1 S1 O1 138.79(19) . . . . ? N1 Zr1 S1 O1 169.5(2) . . . . ? O3 Zr1 S1 O1 -169.0(2) . . . . ? S2 Zr1 S1 O1 154.06(16) . . . . ? N4 Zr1 S1 N1 -139.0(2) . . . . ? N3 Zr1 S1 N1 112.1(2) . . . . ? N2 Zr1 S1 N1 -30.69(19) . . . . ? O1 Zr1 S1 N1 -169.5(2) . . . . ? O3 Zr1 S1 N1 21.5(2) . . . . ? S2 Zr1 S1 N1 -15.41(18) . . . . ? N4 Zr1 S1 C21 -56.3(2) . . . . ? N3 Zr1 S1 C21 -165.3(2) . . . . ? N2 Zr1 S1 C21 51.9(2) . . . . ? N1 Zr1 S1 C21 82.6(2) . . . . ? O1 Zr1 S1 C21 -86.8(2) . . . . ? O3 Zr1 S1 C21 104.1(2) . . . . ? S2 Zr1 S1 C21 67.22(19) . . . . ? N4 Zr1 S2 O4 7.7(2) . . . . ? N3 Zr1 S2 O4 116.2(2) . . . . ? N2 Zr1 S2 O4 -91.6(3) . . . . ? N1 Zr1 S2 O4 -129.4(2) . . . . ? O1 Zr1 S2 O4 -89.3(3) . . . . ? O3 Zr1 S2 O4 93.9(3) . . . . ? S1 Zr1 S2 O4 -121.2(2) . . . . ? N4 Zr1 S2 O3 -86.2(2) . . . . ? N3 Zr1 S2 O3 22.3(2) . . . . ? N2 Zr1 S2 O3 174.5(2) . . . . ? N1 Zr1 S2 O3 136.66(19) . . . . ? O1 Zr1 S2 O3 176.8(3) . . . . ? S1 Zr1 S2 O3 144.85(17) . . . . ? N4 Zr1 S2 N2 99.3(2) . . . . ? N3 Zr1 S2 N2 -152.2(2) . . . . ? N1 Zr1 S2 N2 -37.8(2) . . . . ? O1 Zr1 S2 N2 2.3(3) . . . . ? O3 Zr1 S2 N2 -174.5(2) . . . . ? S1 Zr1 S2 N2 -29.63(18) . . . . ? N4 Zr1 S2 C30 -174.2(2) . . . . ? N3 Zr1 S2 C30 -65.7(2) . . . . ? N2 Zr1 S2 C30 86.5(3) . . . . ? N1 Zr1 S2 C30 48.7(2) . . . . ? O1 Zr1 S2 C30 88.8(3) . . . . ? O3 Zr1 S2 C30 -88.0(2) . . . . ? S1 Zr1 S2 C30 56.85(19) . . . . ? N10 Zr2 S3 O6 119.4(2) . . . . ? N9 Zr2 S3 O6 10.5(2) . . . . ? N6 Zr2 S3 O6 -128.6(2) . . . . ? N5 Zr2 S3 O6 -94.5(3) . . . . ? O5 Zr2 S3 O6 93.3(3) . . . . ? O7 Zr2 S3 O6 -79.9(3) . . . . ? S4 Zr2 S3 O6 -115.5(2) . . . . ? N10 Zr2 S3 O5 26.1(2) . . . . ? N9 Zr2 S3 O5 -82.8(2) . . . . ? N6 Zr2 S3 O5 138.1(2) . . . . ? N5 Zr2 S3 O5 172.2(3) . . . . ? O7 Zr2 S3 O5 -173.2(3) . . . . ? S4 Zr2 S3 O5 151.21(17) . . . . ? N10 Zr2 S3 N5 -146.2(2) . . . . ? N9 Zr2 S3 N5 104.9(2) . . . . ? N6 Zr2 S3 N5 -34.1(2) . . . . ? O5 Zr2 S3 N5 -172.2(3) . . . . ? O7 Zr2 S3 N5 14.6(3) . . . . ? S4 Zr2 S3 N5 -21.0(2) . . . . ? N10 Zr2 S3 C59 -60.8(2) . . . . ? N9 Zr2 S3 C59 -169.7(2) . . . . ? N6 Zr2 S3 C59 51.3(2) . . . . ? N5 Zr2 S3 C59 85.4(3) . . . . ? O5 Zr2 S3 C59 -86.8(3) . . . . ? O7 Zr2 S3 C59 100.0(3) . . . . ? S4 Zr2 S3 C59 64.4(2) . . . . ? N10 Zr2 S4 O8 12.9(3) . . . . ? N9 Zr2 S4 O8 121.3(3) . . . . ? N6 Zr2 S4 O8 -92.4(3) . . . . ? N5 Zr2 S4 O8 -128.7(3) . . . . ? O5 Zr2 S4 O8 -83.9(3) . . . . ? O7 Zr2 S4 O8 95.3(3) . . . . ? S3 Zr2 S4 O8 -117.7(2) . . . . ? N10 Zr2 S4 O7 -82.4(2) . . . . ? N9 Zr2 S4 O7 26.1(2) . . . . ? N6 Zr2 S4 O7 172.4(3) . . . . ? N5 Zr2 S4 O7 136.1(2) . . . . ? O5 Zr2 S4 O7 -179.1(3) . . . . ? S3 Zr2 S4 O7 147.08(19) . . . . ? N10 Zr2 S4 N6 105.2(2) . . . . ? N9 Zr2 S4 N6 -146.3(2) . . . . ? N5 Zr2 S4 N6 -36.3(2) . . . . ? O5 Zr2 S4 N6 8.5(3) . . . . ? O7 Zr2 S4 N6 -172.4(3) . . . . ? S3 Zr2 S4 N6 -25.3(2) . . . . ? N10 Zr2 S4 C68' -170.1(11) . . . . ? N9 Zr2 S4 C68' -61.7(11) . . . . ? N6 Zr2 S4 C68' 84.6(11) . . . . ? N5 Zr2 S4 C68' 48.4(11) . . . . ? O5 Zr2 S4 C68' 93.1(11) . . . . ? O7 Zr2 S4 C68' -87.7(11) . . . . ? S3 Zr2 S4 C68' 59.3(11) . . . . ? N10 Zr2 S4 C68 -169.6(8) . . . . ? N9 Zr2 S4 C68 -61.2(8) . . . . ? N6 Zr2 S4 C68 85.2(8) . . . . ? N5 Zr2 S4 C68 48.9(8) . . . . ? O5 Zr2 S4 C68 93.6(8) . . . . ? O7 Zr2 S4 C68 -87.2(8) . . . . ? S3 Zr2 S4 C68 59.9(8) . . . . ? N11 Zr3 S5 O10 121.1(2) . . . . ? N12 Zr3 S5 O10 9.4(2) . . . . ? N8 Zr3 S5 O10 -127.6(2) . . . . ? N7 Zr3 S5 O10 -96.1(3) . . . . ? O9 Zr3 S5 O10 95.6(2) . . . . ? O11 Zr3 S5 O10 -80.1(3) . . . . ? S6 Zr3 S5 O10 -117.19(19) . . . . ? N11 Zr3 S5 O9 25.5(2) . . . . ? N12 Zr3 S5 O9 -86.3(2) . . . . ? N8 Zr3 S5 O9 136.78(19) . . . . ? N7 Zr3 S5 O9 168.3(3) . . . . ? O11 Zr3 S5 O9 -175.7(2) . . . . ? S6 Zr3 S5 O9 147.17(17) . . . . ? N11 Zr3 S5 N7 -142.8(2) . . . . ? N12 Zr3 S5 N7 105.5(2) . . . . ? N8 Zr3 S5 N7 -31.5(2) . . . . ? O9 Zr3 S5 N7 -168.3(3) . . . . ? O11 Zr3 S5 N7 16.0(3) . . . . ? S6 Zr3 S5 N7 -21.09(19) . . . . ? N11 Zr3 S5 C97 -61.6(2) . . . . ? N12 Zr3 S5 C97 -173.3(2) . . . . ? N8 Zr3 S5 C97 49.7(2) . . . . ? N7 Zr3 S5 C97 81.2(3) . . . . ? O9 Zr3 S5 C97 -87.1(3) . . . . ? O11 Zr3 S5 C97 97.2(3) . . . . ? S6 Zr3 S5 C97 60.1(2) . . . . ? N11 Zr3 S6 O12 10.6(2) . . . . ? N12 Zr3 S6 O12 122.9(2) . . . . ? N8 Zr3 S6 O12 -96.3(3) . . . . ? N7 Zr3 S6 O12 -127.1(2) . . . . ? O9 Zr3 S6 O12 -79.2(3) . . . . ? O11 Zr3 S6 O12 97.5(3) . . . . ? S5 Zr3 S6 O12 -116.11(19) . . . . ? N11 Zr3 S6 O11 -86.9(2) . . . . ? N12 Zr3 S6 O11 25.5(2) . . . . ? N8 Zr3 S6 O11 166.2(3) . . . . ? N7 Zr3 S6 O11 135.4(2) . . . . ? O9 Zr3 S6 O11 -176.7(3) . . . . ? S5 Zr3 S6 O11 146.42(17) . . . . ? N11 Zr3 S6 N8 106.9(2) . . . . ? N12 Zr3 S6 N8 -140.8(2) . . . . ? N7 Zr3 S6 N8 -30.8(2) . . . . ? O9 Zr3 S6 N8 17.1(3) . . . . ? O11 Zr3 S6 N8 -166.2(3) . . . . ? S5 Zr3 S6 N8 -19.82(19) . . . . ? N11 Zr3 S6 C106 -174.2(2) . . . . ? N12 Zr3 S6 C106 -61.8(3) . . . . ? N8 Zr3 S6 C106 79.0(3) . . . . ? N7 Zr3 S6 C106 48.2(2) . . . . ? O9 Zr3 S6 C106 96.1(3) . . . . ? O11 Zr3 S6 C106 -87.3(3) . . . . ? S5 Zr3 S6 C106 59.1(2) . . . . ? O2 S1 N1 C2 -50.8(4) . . . . ? O1 S1 N1 C2 -173.3(3) . . . . ? C21 S1 N1 C2 71.7(4) . . . . ? Zr1 S1 N1 C2 -165.0(4) . . . . ? O2 S1 N1 Zr1 114.25(19) . . . . ? O1 S1 N1 Zr1 -8.23(19) . . . . ? C21 S1 N1 Zr1 -123.32(18) . . . . ? N4 Zr1 N1 C2 -139.4(3) . . . . ? N3 Zr1 N1 C2 89.0(4) . . . . ? N2 Zr1 N1 C2 -46.7(4) . . . . ? O1 Zr1 N1 C2 169.6(4) . . . . ? O3 Zr1 N1 C2 -4.6(4) . . . . ? S1 Zr1 N1 C2 163.8(5) . . . . ? S2 Zr1 N1 C2 -27.8(4) . . . . ? N4 Zr1 N1 S1 56.8(3) . . . . ? N3 Zr1 N1 S1 -74.7(2) . . . . ? N2 Zr1 N1 S1 149.51(19) . . . . ? O1 Zr1 N1 S1 5.89(14) . . . . ? O3 Zr1 N1 S1 -168.40(13) . . . . ? S2 Zr1 N1 S1 168.46(13) . . . . ? O4 S2 N2 C12 -47.2(4) . . . . ? O3 S2 N2 C12 -172.0(4) . . . . ? C30 S2 N2 C12 75.8(4) . . . . ? Zr1 S2 N2 C12 -167.6(4) . . . . ? O4 S2 N2 Zr1 120.37(19) . . . . ? O3 S2 N2 Zr1 -4.4(2) . . . . ? C30 S2 N2 Zr1 -116.6(2) . . . . ? N4 Zr1 N2 C12 81.3(4) . . . . ? N3 Zr1 N2 C12 -153.1(3) . . . . ? N1 Zr1 N2 C12 -51.0(3) . . . . ? O1 Zr1 N2 C12 -11.9(4) . . . . ? O3 Zr1 N2 C12 170.1(4) . . . . ? S1 Zr1 N2 C12 -35.1(4) . . . . ? S2 Zr1 N2 C12 167.0(5) . . . . ? N4 Zr1 N2 S2 -85.7(2) . . . . ? N3 Zr1 N2 S2 39.9(3) . . . . ? N1 Zr1 N2 S2 141.95(19) . . . . ? O1 Zr1 N2 S2 -178.87(13) . . . . ? O3 Zr1 N2 S2 3.10(14) . . . . ? S1 Zr1 N2 S2 157.91(13) . . . . ? N4 Zr1 N3 C115 48.7(4) . . . . ? N2 Zr1 N3 C115 -75.7(5) . . . . ? N1 Zr1 N3 C115 -165.5(4) . . . . ? O1 Zr1 N3 C115 135.1(4) . . . . ? O3 Zr1 N3 C115 -44.2(4) . . . . ? S1 Zr1 N3 C115 163.8(4) . . . . ? S2 Zr1 N3 C115 -54.9(4) . . . . ? N4 Zr1 N3 C116 -151.2(4) . . . . ? N2 Zr1 N3 C116 84.5(4) . . . . ? N1 Zr1 N3 C116 -5.3(4) . . . . ? O1 Zr1 N3 C116 -64.7(4) . . . . ? O3 Zr1 N3 C116 115.9(4) . . . . ? S1 Zr1 N3 C116 -36.0(4) . . . . ? S2 Zr1 N3 C116 105.2(4) . . . . ? N3 Zr1 N4 C117 38.1(4) . . . . ? N2 Zr1 N4 C117 -176.8(4) . . . . ? N1 Zr1 N4 C117 -94.5(4) . . . . ? O1 Zr1 N4 C117 -51.8(4) . . . . ? O3 Zr1 N4 C117 122.8(4) . . . . ? S1 Zr1 N4 C117 -66.2(4) . . . . ? S2 Zr1 N4 C117 152.0(4) . . . . ? N3 Zr1 N4 C118 -153.1(4) . . . . ? N2 Zr1 N4 C118 -7.9(4) . . . . ? N1 Zr1 N4 C118 74.3(4) . . . . ? O1 Zr1 N4 C118 117.1(4) . . . . ? O3 Zr1 N4 C118 -68.3(4) . . . . ? S1 Zr1 N4 C118 102.6(4) . . . . ? S2 Zr1 N4 C118 -39.2(4) . . . . ? O6 S3 N5 C40 -49.4(5) . . . . ? O5 S3 N5 C40 -172.3(4) . . . . ? C59 S3 N5 C40 73.9(4) . . . . ? Zr2 S3 N5 C40 -166.2(5) . . . . ? O6 S3 N5 Zr2 116.9(2) . . . . ? O5 S3 N5 Zr2 -6.1(2) . . . . ? C59 S3 N5 Zr2 -119.8(2) . . . . ? N10 Zr2 N5 C40 -145.8(4) . . . . ? N9 Zr2 N5 C40 84.7(4) . . . . ? N6 Zr2 N5 C40 -48.5(4) . . . . ? O5 Zr2 N5 C40 170.0(4) . . . . ? O7 Zr2 N5 C40 -6.6(4) . . . . ? S3 Zr2 N5 C40 165.6(5) . . . . ? S4 Zr2 N5 C40 -30.2(4) . . . . ? N10 Zr2 N5 S3 48.6(3) . . . . ? N9 Zr2 N5 S3 -80.9(2) . . . . ? N6 Zr2 N5 S3 145.9(2) . . . . ? O5 Zr2 N5 S3 4.39(15) . . . . ? O7 Zr2 N5 S3 -172.19(15) . . . . ? S4 Zr2 N5 S3 164.19(15) . . . . ? O8 S4 N6 C50 -50.2(5) . . . . ? O7 S4 N6 C50 -173.9(4) . . . . ? C68' S4 N6 C50 68.8(7) . . . . ? C68 S4 N6 C50 75.3(6) . . . . ? Zr2 S4 N6 C50 -167.8(5) . . . . ? O8 S4 N6 Zr2 117.5(2) . . . . ? O7 S4 N6 Zr2 -6.1(2) . . . . ? C68' S4 N6 Zr2 -123.4(6) . . . . ? C68 S4 N6 Zr2 -116.9(5) . . . . ? N10 Zr2 N6 C50 86.3(4) . . . . ? N9 Zr2 N6 C50 -146.0(4) . . . . ? N5 Zr2 N6 C50 -49.2(4) . . . . ? O5 Zr2 N6 C50 -8.5(5) . . . . ? O7 Zr2 N6 C50 171.5(5) . . . . ? S3 Zr2 N6 C50 -31.8(4) . . . . ? S4 Zr2 N6 C50 167.2(5) . . . . ? N10 Zr2 N6 S4 -80.8(2) . . . . ? N9 Zr2 N6 S4 46.8(3) . . . . ? N5 Zr2 N6 S4 143.6(2) . . . . ? O5 Zr2 N6 S4 -175.65(15) . . . . ? O7 Zr2 N6 S4 4.30(16) . . . . ? S3 Zr2 N6 S4 161.00(16) . . . . ? O10 S5 N7 C78 -49.6(4) . . . . ? O9 S5 N7 C78 -172.7(4) . . . . ? C97 S5 N7 C78 72.8(4) . . . . ? Zr3 S5 N7 C78 -163.5(5) . . . . ? O10 S5 N7 Zr3 113.9(2) . . . . ? O9 S5 N7 Zr3 -9.2(2) . . . . ? C97 S5 N7 Zr3 -123.7(2) . . . . ? N11 Zr3 N7 C78 -146.7(4) . . . . ? N12 Zr3 N7 C78 82.5(4) . . . . ? N8 Zr3 N7 C78 -49.3(4) . . . . ? O9 Zr3 N7 C78 168.8(4) . . . . ? O11 Zr3 N7 C78 -9.3(4) . . . . ? S5 Zr3 N7 C78 162.2(5) . . . . ? S6 Zr3 N7 C78 -33.5(4) . . . . ? N11 Zr3 N7 S5 51.1(3) . . . . ? N12 Zr3 N7 S5 -79.7(2) . . . . ? N8 Zr3 N7 S5 148.5(2) . . . . ? O9 Zr3 N7 S5 6.63(15) . . . . ? O11 Zr3 N7 S5 -171.49(14) . . . . ? S6 Zr3 N7 S5 164.30(14) . . . . ? O12 S6 N8 C88 -51.3(4) . . . . ? O11 S6 N8 C88 -174.1(4) . . . . ? C106 S6 N8 C88 70.8(4) . . . . ? Zr3 S6 N8 C88 -163.1(5) . . . . ? O12 S6 N8 Zr3 111.9(2) . . . . ? O11 S6 N8 Zr3 -11.0(2) . . . . ? C106 S6 N8 Zr3 -126.0(2) . . . . ? N11 Zr3 N8 C88 82.6(4) . . . . ? N12 Zr3 N8 C88 -144.5(4) . . . . ? N7 Zr3 N8 C88 -49.2(4) . . . . ? O9 Zr3 N8 C88 -9.4(4) . . . . ? O11 Zr3 N8 C88 169.4(4) . . . . ? S5 Zr3 N8 C88 -33.1(4) . . . . ? S6 Zr3 N8 C88 161.6(5) . . . . ? N11 Zr3 N8 S6 -79.0(2) . . . . ? N12 Zr3 N8 S6 53.9(3) . . . . ? N7 Zr3 N8 S6 149.2(2) . . . . ? O9 Zr3 N8 S6 -171.03(15) . . . . ? O11 Zr3 N8 S6 7.73(14) . . . . ? S5 Zr3 N8 S6 165.25(14) . . . . ? N10 Zr2 N9 C120 48.6(5) . . . . ? N6 Zr2 N9 C120 -79.1(5) . . . . ? N5 Zr2 N9 C120 -164.4(5) . . . . ? O5 Zr2 N9 C120 135.1(5) . . . . ? O7 Zr2 N9 C120 -42.9(5) . . . . ? S3 Zr2 N9 C120 164.5(5) . . . . ? S4 Zr2 N9 C120 -55.4(5) . . . . ? N10 Zr2 N9 C119 -150.8(4) . . . . ? N6 Zr2 N9 C119 81.5(5) . . . . ? N5 Zr2 N9 C119 -3.8(4) . . . . ? O5 Zr2 N9 C119 -64.3(4) . . . . ? O7 Zr2 N9 C119 117.7(4) . . . . ? S3 Zr2 N9 C119 -34.9(4) . . . . ? S4 Zr2 N9 C119 105.2(4) . . . . ? N9 Zr2 N10 C121 38.4(5) . . . . ? N6 Zr2 N10 C121 -177.2(4) . . . . ? N5 Zr2 N10 C121 -91.0(5) . . . . ? O5 Zr2 N10 C121 -53.4(4) . . . . ? O7 Zr2 N10 C121 122.8(4) . . . . ? S3 Zr2 N10 C121 -65.9(5) . . . . ? S4 Zr2 N10 C121 151.8(4) . . . . ? N9 Zr2 N10 C122 -155.0(5) . . . . ? N6 Zr2 N10 C122 -10.6(5) . . . . ? N5 Zr2 N10 C122 75.6(5) . . . . ? O5 Zr2 N10 C122 113.2(5) . . . . ? O7 Zr2 N10 C122 -70.7(5) . . . . ? S3 Zr2 N10 C122 100.6(5) . . . . ? S4 Zr2 N10 C122 -41.6(5) . . . . ? N12 Zr3 N11 C124 48.1(5) . . . . ? N8 Zr3 N11 C124 -166.0(5) . . . . ? N7 Zr3 N11 C124 -81.0(5) . . . . ? O9 Zr3 N11 C124 -43.3(5) . . . . ? O11 Zr3 N11 C124 133.8(5) . . . . ? S5 Zr3 N11 C124 -55.6(5) . . . . ? S6 Zr3 N11 C124 163.2(5) . . . . ? N12 Zr3 N11 C123 -143.2(4) . . . . ? N8 Zr3 N11 C123 2.7(5) . . . . ? N7 Zr3 N11 C123 87.7(5) . . . . ? O9 Zr3 N11 C123 125.4(5) . . . . ? O11 Zr3 N11 C123 -57.5(5) . . . . ? S5 Zr3 N11 C123 113.1(4) . . . . ? S6 Zr3 N11 C123 -28.1(5) . . . . ? N11 Zr3 N12 C126 -166.1(5) . . . . ? N8 Zr3 N12 C126 62.1(5) . . . . ? N7 Zr3 N12 C126 -21.5(5) . . . . ? O9 Zr3 N12 C126 -81.5(5) . . . . ? O11 Zr3 N12 C126 101.1(5) . . . . ? S5 Zr3 N12 C126 -52.1(5) . . . . ? S6 Zr3 N12 C126 88.8(5) . . . . ? N11 Zr3 N12 C125 24.4(6) . . . . ? N8 Zr3 N12 C125 -107.3(6) . . . . ? N7 Zr3 N12 C125 169.0(6) . . . . ? O9 Zr3 N12 C125 109.0(6) . . . . ? O11 Zr3 N12 C125 -68.4(6) . . . . ? S5 Zr3 N12 C125 138.4(6) . . . . ? S6 Zr3 N12 C125 -80.6(6) . . . . ? O2 S1 O1 Zr1 -115.86(18) . . . . ? N1 S1 O1 Zr1 7.89(18) . . . . ? C21 S1 O1 Zr1 122.04(18) . . . . ? N4 Zr1 O1 S1 -151.89(19) . . . . ? N3 Zr1 O1 S1 103.65(19) . . . . ? N2 Zr1 O1 S1 -51.2(2) . . . . ? N1 Zr1 O1 S1 -6.31(14) . . . . ? O3 Zr1 O1 S1 110.5(11) . . . . ? S2 Zr1 O1 S1 -52.6(3) . . . . ? O4 S2 O3 Zr1 -120.95(19) . . . . ? N2 S2 O3 Zr1 4.11(18) . . . . ? C30 S2 O3 Zr1 116.90(19) . . . . ? N4 Zr1 O3 S2 96.74(19) . . . . ? N3 Zr1 O3 S2 -159.13(19) . . . . ? N2 Zr1 O3 S2 -3.28(15) . . . . ? N1 Zr1 O3 S2 -52.1(2) . . . . ? O1 Zr1 O3 S2 -166.0(11) . . . . ? S1 Zr1 O3 S2 -65.2(3) . . . . ? O6 S3 O5 Zr2 -118.7(2) . . . . ? N5 S3 O5 Zr2 5.8(2) . . . . ? C59 S3 O5 Zr2 119.96(19) . . . . ? N10 Zr2 O5 S3 -156.0(2) . . . . ? N9 Zr2 O5 S3 99.7(2) . . . . ? N6 Zr2 O5 S3 -51.4(2) . . . . ? N5 Zr2 O5 S3 -4.62(16) . . . . ? O7 Zr2 O5 S3 129.3(18) . . . . ? S4 Zr2 O5 S3 -56.7(3) . . . . ? O8 S4 O7 Zr2 -118.2(2) . . . . ? N6 S4 O7 Zr2 5.7(2) . . . . ? C68' S4 O7 Zr2 123.6(8) . . . . ? C68 S4 O7 Zr2 117.2(7) . . . . ? N10 Zr2 O7 S4 100.3(2) . . . . ? N9 Zr2 O7 S4 -155.5(2) . . . . ? N6 Zr2 O7 S4 -4.53(17) . . . . ? N5 Zr2 O7 S4 -53.1(2) . . . . ? O5 Zr2 O7 S4 174.8(17) . . . . ? S3 Zr2 O7 S4 -61.9(3) . . . . ? O10 S5 O9 Zr3 -115.67(19) . . . . ? N7 S5 O9 Zr3 8.69(19) . . . . ? C97 S5 O9 Zr3 121.78(18) . . . . ? N11 Zr3 O9 S5 -156.10(19) . . . . ? N12 Zr3 O9 S5 96.15(19) . . . . ? N8 Zr3 O9 S5 -52.8(2) . . . . ? N7 Zr3 O9 S5 -6.94(15) . . . . ? O11 Zr3 O9 S5 145(2) . . . . ? S6 Zr3 O9 S5 -63.3(3) . . . . ? O12 S6 O11 Zr3 -113.7(2) . . . . ? N8 S6 O11 Zr3 10.09(19) . . . . ? C106 S6 O11 Zr3 123.58(19) . . . . ? N11 Zr3 O11 S6 96.05(19) . . . . ? N12 Zr3 O11 S6 -156.3(2) . . . . ? N8 Zr3 O11 S6 -8.17(15) . . . . ? N7 Zr3 O11 S6 -54.4(2) . . . . ? O9 Zr3 O11 S6 154.2(19) . . . . ? S5 Zr3 O11 S6 -64.1(3) . . . . ? C6 C1 C2 C3 7.9(7) . . . . ? C11 C1 C2 C3 -172.5(4) . . . . ? C6 C1 C2 N1 -166.0(4) . . . . ? C11 C1 C2 N1 13.5(6) . . . . ? S1 N1 C2 C3 57.5(6) . . . . ? Zr1 N1 C2 C3 -102.6(5) . . . . ? S1 N1 C2 C1 -128.5(4) . . . . ? Zr1 N1 C2 C1 71.4(5) . . . . ? C1 C2 C3 C4 -2.7(7) . . . . ? N1 C2 C3 C4 171.1(4) . . . . ? C2 C3 C4 C5 -4.2(7) . . . . ? C3 C4 C5 C6 5.8(7) . . . . ? C3 C4 C5 C10 -173.7(4) . . . . ? C4 C5 C6 C1 -0.6(7) . . . . ? C10 C5 C6 C1 178.9(4) . . . . ? C4 C5 C6 C7 179.4(4) . . . . ? C10 C5 C6 C7 -1.1(7) . . . . ? C2 C1 C6 C5 -6.2(7) . . . . ? C11 C1 C6 C5 174.2(4) . . . . ? C2 C1 C6 C7 173.8(4) . . . . ? C11 C1 C6 C7 -5.8(7) . . . . ? C5 C6 C7 C8 14.2(7) . . . . ? C1 C6 C7 C8 -165.8(4) . . . . ? C6 C7 C8 C9 -45.1(6) . . . . ? C7 C8 C9 C10 62.8(5) . . . . ? C6 C5 C10 C9 19.2(7) . . . . ? C4 C5 C10 C9 -161.3(4) . . . . ? C8 C9 C10 C5 -49.3(6) . . . . ? C2 C1 C11 C12 -73.0(6) . . . . ? C6 C1 C11 C12 106.6(5) . . . . ? C2 C1 C11 C16 110.5(5) . . . . ? C6 C1 C11 C16 -70.0(6) . . . . ? C16 C11 C12 C13 5.4(6) . . . . ? C1 C11 C12 C13 -171.0(4) . . . . ? C16 C11 C12 N2 -165.4(4) . . . . ? C1 C11 C12 N2 18.1(6) . . . . ? S2 N2 C12 C13 63.8(5) . . . . ? Zr1 N2 C12 C13 -100.2(4) . . . . ? S2 N2 C12 C11 -125.5(4) . . . . ? Zr1 N2 C12 C11 70.5(5) . . . . ? C11 C12 C13 C14 -1.2(6) . . . . ? N2 C12 C13 C14 169.4(4) . . . . ? C12 C13 C14 C15 -3.8(7) . . . . ? C13 C14 C15 C16 4.5(7) . . . . ? C13 C14 C15 C20 -177.6(4) . . . . ? C14 C15 C16 C11 -0.2(6) . . . . ? C20 C15 C16 C11 -178.1(4) . . . . ? C14 C15 C16 C17 -175.0(4) . . . . ? C20 C15 C16 C17 7.2(7) . . . . ? C12 C11 C16 C15 -4.7(6) . . . . ? C1 C11 C16 C15 171.9(4) . . . . ? C12 C11 C16 C17 170.1(4) . . . . ? C1 C11 C16 C17 -13.4(6) . . . . ? C15 C16 C17 C18' -19.3(7) . . . . ? C11 C16 C17 C18' 166.0(6) . . . . ? C15 C16 C17 C18 10.3(7) . . . . ? C11 C16 C17 C18 -164.4(5) . . . . ? C16 C17 C18 C19 -41.2(9) . . . . ? C18' C17 C18 C19 40.0(12) . . . . ? C17 C18 C19 C20 56.0(10) . . . . ? C16 C17 C18' C19' 50.8(11) . . . . ? C18 C17 C18' C19' -60.7(12) . . . . ? C17 C18' C19' C20 -69.2(13) . . . . ? C18' C19' C20 C15 54.7(11) . . . . ? C18' C19' C20 C19 -45.7(9) . . . . ? C14 C15 C20 C19' 156.4(7) . . . . ? C16 C15 C20 C19' -25.7(8) . . . . ? C14 C15 C20 C19 -169.3(6) . . . . ? C16 C15 C20 C19 8.6(8) . . . . ? C18 C19 C20 C19' 51.9(11) . . . . ? C18 C19 C20 C15 -41.7(10) . . . . ? O2 S1 C21 C22 -161.5(3) . . . . ? O1 S1 C21 C22 -35.7(4) . . . . ? N1 S1 C21 C22 71.3(4) . . . . ? Zr1 S1 C21 C22 20.0(4) . . . . ? O2 S1 C21 C26 23.6(4) . . . . ? O1 S1 C21 C26 149.4(3) . . . . ? N1 S1 C21 C26 -103.6(4) . . . . ? Zr1 S1 C21 C26 -154.9(3) . . . . ? C26 C21 C22 C23 -2.1(6) . . . . ? S1 C21 C22 C23 -177.0(3) . . . . ? C26 C21 C22 C27 175.1(4) . . . . ? S1 C21 C22 C27 0.2(6) . . . . ? C21 C22 C23 C24 1.1(7) . . . . ? C27 C22 C23 C24 -176.3(4) . . . . ? C22 C23 C24 C25 0.2(7) . . . . ? C22 C23 C24 C28 177.3(5) . . . . ? C23 C24 C25 C26 -0.6(7) . . . . ? C28 C24 C25 C26 -177.7(5) . . . . ? C24 C25 C26 C21 -0.4(7) . . . . ? C24 C25 C26 C29 178.1(4) . . . . ? C22 C21 C26 C25 1.8(6) . . . . ? S1 C21 C26 C25 176.7(3) . . . . ? C22 C21 C26 C29 -176.6(4) . . . . ? S1 C21 C26 C29 -1.7(6) . . . . ? O4 S2 C30 C31 -163.1(4) . . . . ? O3 S2 C30 C31 -36.6(4) . . . . ? N2 S2 C30 C31 69.3(4) . . . . ? Zr1 S2 C30 C31 18.4(4) . . . . ? O4 S2 C30 C35 22.3(4) . . . . ? O3 S2 C30 C35 148.8(4) . . . . ? N2 S2 C30 C35 -105.3(4) . . . . ? Zr1 S2 C30 C35 -156.2(3) . . . . ? C35 C30 C31 C32 -1.2(7) . . . . ? S2 C30 C31 C32 -175.7(4) . . . . ? C35 C30 C31 C36 -179.6(4) . . . . ? S2 C30 C31 C36 5.9(7) . . . . ? C30 C31 C32 C33 -1.6(8) . . . . ? C36 C31 C32 C33 177.0(5) . . . . ? C31 C32 C33 C34 1.9(8) . . . . ? C31 C32 C33 C37 -179.6(5) . . . . ? C32 C33 C34 C35 0.5(8) . . . . ? C37 C33 C34 C35 -178.0(5) . . . . ? C33 C34 C35 C30 -3.1(7) . . . . ? C33 C34 C35 C38 176.4(5) . . . . ? C31 C30 C35 C34 3.4(7) . . . . ? S2 C30 C35 C34 177.9(4) . . . . ? C31 C30 C35 C38 -176.0(5) . . . . ? S2 C30 C35 C38 -1.5(7) . . . . ? C44 C39 C40 C41 7.5(7) . . . . ? C49 C39 C40 C41 -174.0(5) . . . . ? C44 C39 C40 N5 -163.8(4) . . . . ? C49 C39 C40 N5 14.8(7) . . . . ? S3 N5 C40 C41 63.0(6) . . . . ? Zr2 N5 C40 C41 -99.2(5) . . . . ? S3 N5 C40 C39 -125.9(4) . . . . ? Zr2 N5 C40 C39 71.9(6) . . . . ? C39 C40 C41 C42 -3.3(7) . . . . ? N5 C40 C41 C42 167.7(5) . . . . ? C40 C41 C42 C43 -2.6(8) . . . . ? C41 C42 C43 C44 4.3(8) . . . . ? C41 C42 C43 C48 -174.6(5) . . . . ? C42 C43 C44 C39 -0.1(8) . . . . ? C48 C43 C44 C39 178.8(5) . . . . ? C42 C43 C44 C45 -179.6(5) . . . . ? C48 C43 C44 C45 -0.7(8) . . . . ? C40 C39 C44 C43 -5.8(8) . . . . ? C49 C39 C44 C43 175.6(5) . . . . ? C40 C39 C44 C45 173.7(5) . . . . ? C49 C39 C44 C45 -4.8(8) . . . . ? C43 C44 C45 C46 -18.6(9) . . . . ? C39 C44 C45 C46 161.9(6) . . . . ? C43 C44 C45 C46' 6.8(12) . . . . ? C39 C44 C45 C46' -172.7(10) . . . . ? C44 C45 C46 C47 53.5(13) . . . . ? C46' C45 C46 C47 -52(3) . . . . ? C45 C46 C47 C48 -67.2(14) . . . . ? C44 C45 C46' C47' -37(2) . . . . ? C46 C45 C46' C47' 49(2) . . . . ? C45 C46' C47' C48 58(2) . . . . ? C42 C43 C48 C47 164.2(7) . . . . ? C44 C43 C48 C47 -14.6(10) . . . . ? C42 C43 C48 C47' -157.2(9) . . . . ? C44 C43 C48 C47' 23.9(11) . . . . ? C46 C47 C48 C43 46.8(11) . . . . ? C46 C47 C48 C47' -50.1(12) . . . . ? C46' C47' C48 C43 -50.9(15) . . . . ? C46' C47' C48 C47 48.2(12) . . . . ? C40 C39 C49 C50 -72.9(6) . . . . ? C44 C39 C49 C50 105.6(6) . . . . ? C40 C39 C49 C54 109.5(5) . . . . ? C44 C39 C49 C54 -72.0(6) . . . . ? C54 C49 C50 C51 5.4(7) . . . . ? C39 C49 C50 C51 -172.2(4) . . . . ? C54 C49 C50 N6 -166.2(4) . . . . ? C39 C49 C50 N6 16.2(7) . . . . ? S4 N6 C50 C49 -124.1(4) . . . . ? Zr2 N6 C50 C49 71.7(6) . . . . ? S4 N6 C50 C51 64.5(6) . . . . ? Zr2 N6 C50 C51 -99.8(5) . . . . ? C49 C50 C51 C52 -2.2(8) . . . . ? N6 C50 C51 C52 169.1(5) . . . . ? C50 C51 C52 C53 -2.1(9) . . . . ? C51 C52 C53 C54 3.1(9) . . . . ? C51 C52 C53 C58 -179.4(6) . . . . ? C52 C53 C54 C49 0.1(8) . . . . ? C58 C53 C54 C49 -177.3(6) . . . . ? C52 C53 C54 C55 -177.0(5) . . . . ? C58 C53 C54 C55 5.6(8) . . . . ? C50 C49 C54 C53 -4.3(7) . . . . ? C39 C49 C54 C53 173.4(4) . . . . ? C50 C49 C54 C55 172.8(5) . . . . ? C39 C49 C54 C55 -9.5(7) . . . . ? C53 C54 C55 C56 12.4(10) . . . . ? C49 C54 C55 C56 -164.7(8) . . . . ? C53 C54 C55 C56' -21.7(10) . . . . ? C49 C54 C55 C56' 161.2(9) . . . . ? C54 C55 C56 C57 -40.1(15) . . . . ? C56' C55 C56 C57 46.5(14) . . . . ? C55 C56 C57 C58 55.3(19) . . . . ? C54 C55 C56' C57' 50.0(19) . . . . ? C56 C55 C56' C57' -58.8(15) . . . . ? C55 C56' C57' C58 -60(2) . . . . ? C56 C57 C58 C53 -41.0(17) . . . . ? C56 C57 C58 C57' 63(2) . . . . ? C52 C53 C58 C57 -169.3(8) . . . . ? C54 C53 C58 C57 8.1(11) . . . . ? C52 C53 C58 C57' 165.6(11) . . . . ? C54 C53 C58 C57' -17.0(13) . . . . ? C56' C57' C58 C57 -43.6(19) . . . . ? C56' C57' C58 C53 43(2) . . . . ? O6 S3 C59 C60 -161.0(4) . . . . ? O5 S3 C59 C60 -35.8(4) . . . . ? N5 S3 C59 C60 70.8(4) . . . . ? Zr2 S3 C59 C60 19.1(4) . . . . ? O6 S3 C59 C64 25.0(5) . . . . ? O5 S3 C59 C64 150.2(4) . . . . ? N5 S3 C59 C64 -103.3(4) . . . . ? Zr2 S3 C59 C64 -154.9(3) . . . . ? C64 C59 C60 C61 -2.1(7) . . . . ? S3 C59 C60 C61 -176.1(4) . . . . ? C64 C59 C60 C65 178.4(5) . . . . ? S3 C59 C60 C65 4.4(6) . . . . ? C59 C60 C61 C62 0.7(8) . . . . ? C65 C60 C61 C62 -179.7(5) . . . . ? C60 C61 C62 C63 0.5(8) . . . . ? C60 C61 C62 C66 178.6(5) . . . . ? C61 C62 C63 C64 -0.1(8) . . . . ? C66 C62 C63 C64 -178.3(5) . . . . ? C62 C63 C64 C59 -1.2(8) . . . . ? C62 C63 C64 C67 179.0(5) . . . . ? C60 C59 C64 C63 2.3(7) . . . . ? S3 C59 C64 C63 176.4(4) . . . . ? C60 C59 C64 C67 -177.9(5) . . . . ? S3 C59 C64 C67 -3.9(7) . . . . ? O8 S4 C68 C69 16.4(12) . . . . ? O7 S4 C68 C69 143.1(8) . . . . ? N6 S4 C68 C69 -111.4(9) . . . . ? C68' S4 C68 C69 15(11) . . . . ? Zr2 S4 C68 C69 -161.5(7) . . . . ? O8 S4 C68 C73 -164.1(7) . . . . ? O7 S4 C68 C73 -37.3(10) . . . . ? N6 S4 C68 C73 68.1(10) . . . . ? C68' S4 C68 C73 -165(12) . . . . ? Zr2 S4 C68 C73 18.1(12) . . . . ? C73 C68 C69 C70 0.0 . . . . ? S4 C68 C69 C70 179.5(15) . . . . ? C73 C68 C69 C74 -173.3(19) . . . . ? S4 C68 C69 C74 6.2(18) . . . . ? C68 C69 C70 C71 0.0 . . . . ? C74 C69 C70 C71 174.2(17) . . . . ? C69 C70 C71 C72 0.0 . . . . ? C69 C70 C71 C75 -179.5(14) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C75 C71 C72 C73 179.5(14) . . . . ? C71 C72 C73 C68 0.0 . . . . ? C71 C72 C73 C76 176.7(19) . . . . ? C69 C68 C73 C72 0.0 . . . . ? S4 C68 C73 C72 -179.5(15) . . . . ? C69 C68 C73 C76 -176(2) . . . . ? S4 C68 C73 C76 4.2(19) . . . . ? O8 S4 C68' C69' 16.5(13) . . . . ? O7 S4 C68' C69' 141.2(9) . . . . ? N6 S4 C68' C69' -109.0(11) . . . . ? C68 S4 C68' C69' -164(12) . . . . ? Zr2 S4 C68' C69' -161.0(7) . . . . ? O8 S4 C68' C73' -163.7(9) . . . . ? O7 S4 C68' C73' -39.0(12) . . . . ? N6 S4 C68' C73' 70.7(11) . . . . ? C68 S4 C68' C73' 15(11) . . . . ? Zr2 S4 C68' C73' 18.8(16) . . . . ? C73' C68' C69' C70' 0.0 . . . . ? S4 C68' C69' C70' 179.8(18) . . . . ? C73' C68' C69' C74' -177(2) . . . . ? S4 C68' C69' C74' 2.6(19) . . . . ? C68' C69' C70' C71' 0.0 . . . . ? C74' C69' C70' C71' 177.5(18) . . . . ? C69' C70' C71' C72' 0.0 . . . . ? C69' C70' C71' C75' 176.6(17) . . . . ? C70' C71' C72' C73' 0.0 . . . . ? C75' C71' C72' C73' -176.7(16) . . . . ? C71' C72' C73' C68' 0.0 . . . . ? C71' C72' C73' C76' 179(2) . . . . ? C69' C68' C73' C72' 0.0 . . . . ? S4 C68' C73' C72' -179.8(18) . . . . ? C69' C68' C73' C76' -179(2) . . . . ? S4 C68' C73' C76' 1(2) . . . . ? C82 C77 C78 C79 7.2(7) . . . . ? C87 C77 C78 C79 -170.1(4) . . . . ? C82 C77 C78 N7 -165.7(4) . . . . ? C87 C77 C78 N7 17.0(6) . . . . ? S5 N7 C78 C77 -130.6(4) . . . . ? Zr3 N7 C78 C77 70.9(5) . . . . ? S5 N7 C78 C79 56.5(6) . . . . ? Zr3 N7 C78 C79 -102.0(5) . . . . ? C77 C78 C79 C80 -4.1(7) . . . . ? N7 C78 C79 C80 168.6(5) . . . . ? C78 C79 C80 C81 -1.4(9) . . . . ? C79 C80 C81 C82 3.7(9) . . . . ? C79 C80 C81 C86 -176.9(6) . . . . ? C80 C81 C82 C77 -0.5(8) . . . . ? C86 C81 C82 C77 -179.9(5) . . . . ? C80 C81 C82 C83 -176.8(5) . . . . ? C86 C81 C82 C83 3.9(8) . . . . ? C78 C77 C82 C81 -4.8(7) . . . . ? C87 C77 C82 C81 172.5(4) . . . . ? C78 C77 C82 C83 171.4(4) . . . . ? C87 C77 C82 C83 -11.3(7) . . . . ? C81 C82 C83 C84 -22.2(7) . . . . ? C77 C82 C83 C84 161.6(5) . . . . ? C82 C83 C84 C85 50.7(7) . . . . ? C83 C84 C85 C86 -60.8(7) . . . . ? C80 C81 C86 C85 166.5(6) . . . . ? C82 C81 C86 C85 -14.1(9) . . . . ? C84 C85 C86 C81 42.7(8) . . . . ? C78 C77 C87 C88 -72.5(6) . . . . ? C82 C77 C87 C88 110.2(5) . . . . ? C78 C77 C87 C92 109.0(5) . . . . ? C82 C77 C87 C92 -68.3(6) . . . . ? C92 C87 C88 C89 3.9(6) . . . . ? C77 C87 C88 C89 -174.5(4) . . . . ? C92 C87 C88 N8 -167.2(4) . . . . ? C77 C87 C88 N8 14.3(6) . . . . ? S6 N8 C88 C87 -128.3(4) . . . . ? Zr3 N8 C88 C87 73.7(5) . . . . ? S6 N8 C88 C89 60.5(5) . . . . ? Zr3 N8 C88 C89 -97.5(5) . . . . ? C87 C88 C89 C90 -0.3(7) . . . . ? N8 C88 C89 C90 170.6(4) . . . . ? C88 C89 C90 C91 -3.0(7) . . . . ? C89 C90 C91 C92 2.6(7) . . . . ? C89 C90 C91 C96 -177.1(4) . . . . ? C88 C87 C92 C91 -4.3(7) . . . . ? C77 C87 C92 C91 174.2(4) . . . . ? C88 C87 C92 C93 172.8(4) . . . . ? C77 C87 C92 C93 -8.6(6) . . . . ? C90 C91 C92 C87 1.1(7) . . . . ? C96 C91 C92 C87 -179.2(4) . . . . ? C90 C91 C92 C93 -176.0(4) . . . . ? C96 C91 C92 C93 3.7(7) . . . . ? C87 C92 C93 C94 -165.4(5) . . . . ? C91 C92 C93 C94 11.8(7) . . . . ? C92 C93 C94 C95 -44.2(8) . . . . ? C93 C94 C95 C96 60.9(8) . . . . ? C90 C91 C96 C95 -167.9(5) . . . . ? C92 C91 C96 C95 12.4(7) . . . . ? C94 C95 C96 C91 -44.6(7) . . . . ? O10 S5 C97 C98 -160.7(4) . . . . ? O9 S5 C97 C98 -34.1(4) . . . . ? N7 S5 C97 C98 71.8(4) . . . . ? Zr3 S5 C97 C98 21.7(5) . . . . ? O10 S5 C97 C102 22.7(4) . . . . ? O9 S5 C97 C102 149.3(4) . . . . ? N7 S5 C97 C102 -104.8(4) . . . . ? Zr3 S5 C97 C102 -154.9(3) . . . . ? C102 C97 C98 C99 1.1(7) . . . . ? S5 C97 C98 C99 -175.5(4) . . . . ? C102 C97 C98 C103 179.1(5) . . . . ? S5 C97 C98 C103 2.6(7) . . . . ? C97 C98 C99 C100 -0.3(7) . . . . ? C103 C98 C99 C100 -178.5(5) . . . . ? C98 C99 C100 C101 0.0(8) . . . . ? C98 C99 C100 C104 178.2(5) . . . . ? C99 C100 C101 C102 -0.4(8) . . . . ? C104 C100 C101 C102 -178.6(5) . . . . ? C100 C101 C102 C97 1.2(8) . . . . ? C100 C101 C102 C105 178.7(5) . . . . ? C98 C97 C102 C101 -1.5(7) . . . . ? S5 C97 C102 C101 175.1(4) . . . . ? C98 C97 C102 C105 -178.8(5) . . . . ? S5 C97 C102 C105 -2.2(7) . . . . ? O12 S6 C106 C107 -166.6(4) . . . . ? O11 S6 C106 C107 -40.1(5) . . . . ? N8 S6 C106 C107 66.6(4) . . . . ? Zr3 S6 C106 C107 17.6(5) . . . . ? O12 S6 C106 C111 17.3(5) . . . . ? O11 S6 C106 C111 143.7(4) . . . . ? N8 S6 C106 C111 -109.5(4) . . . . ? Zr3 S6 C106 C111 -158.5(3) . . . . ? C111 C106 C107 C108 -0.7(8) . . . . ? S6 C106 C107 C108 -176.8(4) . . . . ? C111 C106 C107 C112 -179.4(5) . . . . ? S6 C106 C107 C112 4.5(7) . . . . ? C106 C107 C108 C109 -1.2(8) . . . . ? C112 C107 C108 C109 177.6(5) . . . . ? C107 C108 C109 C110 2.2(8) . . . . ? C107 C108 C109 C113 -179.5(6) . . . . ? C108 C109 C110 C111 -1.5(8) . . . . ? C113 C109 C110 C111 -179.7(5) . . . . ? C109 C110 C111 C106 -0.3(8) . . . . ? C109 C110 C111 C114 179.0(5) . . . . ? C107 C106 C111 C110 1.4(7) . . . . ? S6 C106 C111 C110 177.5(4) . . . . ? C107 C106 C111 C114 -177.8(5) . . . . ? S6 C106 C111 C114 -1.7(7) . . . . ? C133 C128 C129 C130 -4.3(11) . . . . ? C127 C128 C129 C130 176.6(8) . . . . ? C128 C129 C130 C131 3.1(14) . . . . ? C129 C130 C131 C132 0.6(15) . . . . ? C130 C131 C132 C133 -3.0(14) . . . . ? C131 C132 C133 C128 1.5(12) . . . . ? C129 C128 C133 C132 1.9(10) . . . . ? C127 C128 C133 C132 -179.0(7) . . . . ? C140 C135 C136 C137 0.4(9) . . . . ? C134 C135 C136 C137 -179.1(6) . . . . ? C135 C136 C137 C138 0.4(10) . . . . ? C136 C137 C138 C139 -0.6(9) . . . . ? C137 C138 C139 C140 0.0(10) . . . . ? C138 C139 C140 C135 0.9(11) . . . . ? C136 C135 C140 C139 -1.0(9) . . . . ? C134 C135 C140 C139 178.5(6) . . . . ? C147 C142 C143 C144 0.0 . . . . ? C141 C142 C143 C144 -179.99(9) . . . . ? C142 C143 C144 C145 0.0 . . . . ? C143 C144 C145 C146 0.0 . . . . ? C144 C145 C146 C147 0.0 . . . . ? C145 C146 C147 C142 0.0 . . . . ? C143 C142 C147 C146 0.0 . . . . ? C141 C142 C147 C146 179.99(9) . . . . ? C154 C149 C150 C151 0.0 . . . . ? C148 C149 C150 C151 180.00(9) . . . . ? C149 C150 C151 C152 0.0 . . . . ? C150 C151 C152 C153 0.0 . . . . ? C151 C152 C153 C154 0.0 . . . . ? C152 C153 C154 C149 0.0 . . . . ? C150 C149 C154 C153 0.0 . . . . ? C148 C149 C154 C153 180.00(9) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.813 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.084 # Attachment 'compound_17.cif' data_compound17 _database_code_depnum_ccdc_archive 'CCDC 742603' #TrackingRef 'compound_17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C75 H60 N4 O8 S4 Zr' _chemical_formula_sum 'C75 H60 N4 O8 S4 Zr' _chemical_formula_weight 1364.73 _chemical_absolute_configuration rmad 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.8466(16) _cell_length_b 13.6505(15) _cell_length_c 15.9918(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.809(2) _cell_angle_gamma 90.00 _cell_volume 3133.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11157 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9567 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39786 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.88 _reflns_number_total 14305 _reflns_number_gt 13560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0371P)^2^+0.4928P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(16) _refine_ls_number_reflns 14305 _refine_ls_number_parameters 839 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.033 _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 0.278786(12) 0.642778(13) 0.667359(11) 0.01112(4) Uani 1 1 d . . . S1 S 0.10659(3) 0.75901(4) 0.61915(3) 0.01242(10) Uani 1 1 d . . . S2 S 0.38203(3) 0.53469(4) 0.56360(3) 0.01396(10) Uani 1 1 d . . . S3 S 0.39310(3) 0.81230(4) 0.74839(3) 0.01290(10) Uani 1 1 d . . . S4 S 0.22018(3) 0.46380(4) 0.74258(3) 0.01374(10) Uani 1 1 d . . . N1 N 0.19297(11) 0.74705(12) 0.57940(10) 0.0120(3) Uani 1 1 d . . . N2 N 0.28747(11) 0.59364(12) 0.53819(10) 0.0123(3) Uani 1 1 d . . . N3 N 0.32553(11) 0.73995(12) 0.77945(11) 0.0117(3) Uani 1 1 d . . . N4 N 0.29153(12) 0.54634(13) 0.78295(11) 0.0133(4) Uani 1 1 d . . . O1 O 0.13545(10) 0.68457(10) 0.68896(9) 0.0142(3) Uani 1 1 d . . . O2 O 0.08679(10) 0.85537(11) 0.64489(9) 0.0166(3) Uani 1 1 d . . . O3 O 0.40978(10) 0.56177(11) 0.65746(9) 0.0154(3) Uani 1 1 d . . . O4 O 0.37978(11) 0.43147(11) 0.54654(10) 0.0199(3) Uani 1 1 d . . . O5 O 0.38885(10) 0.76422(11) 0.66409(9) 0.0143(3) Uani 1 1 d . . . O6 O 0.37036(10) 0.91444(11) 0.74662(10) 0.0180(3) Uani 1 1 d . . . O7 O 0.19306(10) 0.49881(10) 0.65116(9) 0.0148(3) Uani 1 1 d . . . O8 O 0.25175(11) 0.36428(11) 0.75613(10) 0.0194(3) Uani 1 1 d . . . C1 C 0.21815(14) 0.76465(15) 0.43596(13) 0.0126(4) Uani 1 1 d . . . C2 C 0.21402(13) 0.80674(15) 0.51366(12) 0.0132(4) Uani 1 1 d . . . C3 C 0.23944(14) 0.90592(16) 0.53318(14) 0.0166(4) Uani 1 1 d . . . H3 H 0.2341 0.9337 0.5862 0.020 Uiso 1 1 calc R . . C4 C 0.27149(15) 0.96155(16) 0.47598(14) 0.0184(4) Uani 1 1 d . . . H4 H 0.2847 1.0289 0.4880 0.022 Uiso 1 1 calc R . . C5 C 0.28535(15) 0.92018(16) 0.39881(14) 0.0178(4) Uani 1 1 d . . . C6 C 0.25837(14) 0.82072(16) 0.37859(13) 0.0157(4) Uani 1 1 d . . . C7 C 0.27606(16) 0.77953(17) 0.30286(14) 0.0204(5) Uani 1 1 d . . . H7 H 0.2585 0.7137 0.2878 0.025 Uiso 1 1 calc R . . C8 C 0.31835(17) 0.83375(19) 0.25094(15) 0.0271(5) Uani 1 1 d . . . H8 H 0.3297 0.8049 0.2005 0.033 Uiso 1 1 calc R . . C9 C 0.34476(18) 0.93122(19) 0.27196(16) 0.0282(5) Uani 1 1 d . . . H9 H 0.3744 0.9678 0.2360 0.034 Uiso 1 1 calc R . . C10 C 0.32812(16) 0.97365(18) 0.34347(15) 0.0237(5) Uani 1 1 d . . . H10 H 0.3454 1.0400 0.3565 0.028 Uiso 1 1 calc R . . C11 C 0.18160(14) 0.66423(14) 0.41118(12) 0.0130(4) Uani 1 1 d . . . C12 C 0.21885(14) 0.58179(15) 0.45813(13) 0.0135(4) Uani 1 1 d . . . C13 C 0.18484(14) 0.48668(15) 0.43210(13) 0.0152(4) Uani 1 1 d . . . H13 H 0.2115 0.4315 0.4656 0.018 Uiso 1 1 calc R . . C14 C 0.11428(14) 0.47352(16) 0.35956(13) 0.0167(4) Uani 1 1 d . . . H14 H 0.0943 0.4091 0.3414 0.020 Uiso 1 1 calc R . . C15 C 0.07035(15) 0.55517(17) 0.31082(14) 0.0158(4) Uani 1 1 d . . . C16 C 0.10309(13) 0.65111(17) 0.33759(12) 0.0142(4) Uani 1 1 d . . . C17 C 0.05368(15) 0.73158(17) 0.29129(14) 0.0179(5) Uani 1 1 d . . . H17 H 0.0732 0.7964 0.3087 0.021 Uiso 1 1 calc R . . C18 C -0.02185(16) 0.71779(19) 0.22187(15) 0.0221(5) Uani 1 1 d . . . H18 H -0.0544 0.7728 0.1924 0.027 Uiso 1 1 calc R . . C19 C -0.05102(15) 0.62229(17) 0.19441(14) 0.0227(5) Uani 1 1 d . . . H19 H -0.1019 0.6129 0.1452 0.027 Uiso 1 1 calc R . . C20 C -0.00639(16) 0.54345(18) 0.23821(15) 0.0204(5) Uani 1 1 d . . . H20 H -0.0272 0.4793 0.2196 0.025 Uiso 1 1 calc R . . C21 C 0.00848(14) 0.71536(16) 0.54195(13) 0.0142(4) Uani 1 1 d . . . C22 C -0.05847(15) 0.78172(16) 0.49920(14) 0.0191(4) Uani 1 1 d . . . H22 H -0.0551 0.8487 0.5158 0.023 Uiso 1 1 calc R . . C23 C -0.13058(15) 0.74804(17) 0.43142(14) 0.0205(5) Uani 1 1 d . . . H23 H -0.1772 0.7926 0.4021 0.025 Uiso 1 1 calc R . . C24 C -0.13563(13) 0.65047(18) 0.40593(12) 0.0176(4) Uani 1 1 d . . . C25 C -0.06690(15) 0.58544(16) 0.45090(14) 0.0176(4) Uani 1 1 d . . . H25 H -0.0699 0.5184 0.4345 0.021 Uiso 1 1 calc R . . C26 C 0.00526(15) 0.61736(15) 0.51873(14) 0.0161(4) Uani 1 1 d . . . H26 H 0.0516 0.5729 0.5487 0.019 Uiso 1 1 calc R . . C27 C -0.21178(16) 0.61537(17) 0.33120(15) 0.0248(5) Uani 1 1 d . . . H27A H -0.2660 0.5963 0.3518 0.037 Uiso 1 1 calc R . . H27B H -0.1898 0.5588 0.3043 0.037 Uiso 1 1 calc R . . H27C H -0.2294 0.6681 0.2885 0.037 Uiso 1 1 calc R . . C28 C 0.45391(15) 0.58939(17) 0.50487(15) 0.0182(5) Uani 1 1 d . . . C29 C 0.4602(2) 0.6910(2) 0.50326(19) 0.0348(7) Uani 1 1 d . . . H29 H 0.4378 0.7294 0.5432 0.042 Uiso 1 1 calc R . . C30 C 0.4989(2) 0.7356(2) 0.4435(2) 0.0405(8) Uani 1 1 d . . . H30 H 0.5027 0.8050 0.4423 0.049 Uiso 1 1 calc R . . C31 C 0.53251(17) 0.6806(2) 0.38493(17) 0.0263(5) Uani 1 1 d . . . C32 C 0.52758(19) 0.5800(2) 0.38834(17) 0.0301(6) Uani 1 1 d . . . H32 H 0.5511 0.5416 0.3491 0.036 Uiso 1 1 calc R . . C33 C 0.48865(18) 0.5336(2) 0.44831(16) 0.0258(5) Uani 1 1 d . . . H33 H 0.4860 0.4641 0.4503 0.031 Uiso 1 1 calc R . . C34 C 0.5675(2) 0.7318(2) 0.31634(19) 0.0400(7) Uani 1 1 d . . . H34A H 0.5805 0.6834 0.2757 0.060 Uiso 1 1 calc R . . H34B H 0.6247 0.7677 0.3434 0.060 Uiso 1 1 calc R . . H34C H 0.5200 0.7779 0.2852 0.060 Uiso 1 1 calc R . . C35 C 0.32029(14) 0.68239(16) 0.92149(13) 0.0139(4) Uani 1 1 d . . . C36 C 0.29251(14) 0.74971(16) 0.85535(13) 0.0139(4) Uani 1 1 d . . . C37 C 0.22367(15) 0.82179(17) 0.85600(14) 0.0178(4) Uani 1 1 d . . . H37 H 0.2090 0.8701 0.8118 0.021 Uiso 1 1 calc R . . C38 C 0.17863(15) 0.82115(18) 0.92061(15) 0.0215(5) Uani 1 1 d . . . H38 H 0.1322 0.8690 0.9207 0.026 Uiso 1 1 calc R . . C39 C 0.20021(15) 0.74992(17) 0.98780(14) 0.0202(5) Uani 1 1 d . . . C40 C 0.27364(15) 0.68214(16) 0.99015(13) 0.0167(4) Uani 1 1 d . . . C41 C 0.29392(17) 0.61170(17) 1.05753(14) 0.0218(5) Uani 1 1 d . . . H41 H 0.3446 0.5679 1.0620 0.026 Uiso 1 1 calc R . . C42 C 0.24103(18) 0.60611(19) 1.11655(16) 0.0271(5) Uani 1 1 d . . . H42 H 0.2554 0.5582 1.1611 0.033 Uiso 1 1 calc R . . C43 C 0.16629(17) 0.67020(19) 1.11166(15) 0.0277(6) Uani 1 1 d . . . H43 H 0.1288 0.6640 1.1514 0.033 Uiso 1 1 calc R . . C44 C 0.14718(17) 0.74189(19) 1.04954(16) 0.0267(5) Uani 1 1 d . . . H44 H 0.0978 0.7867 1.0479 0.032 Uiso 1 1 calc R . . C45 C 0.39099(14) 0.60563(16) 0.91788(13) 0.0140(4) Uani 1 1 d . . . C46 C 0.37244(14) 0.53614(15) 0.85318(12) 0.0130(4) Uani 1 1 d . . . C47 C 0.43739(15) 0.46057(16) 0.84981(13) 0.0165(4) Uani 1 1 d . . . H47 H 0.4234 0.4135 0.8046 0.020 Uiso 1 1 calc R . . C48 C 0.51960(15) 0.45591(16) 0.91144(14) 0.0193(4) Uani 1 1 d . . . H48 H 0.5617 0.4039 0.9099 0.023 Uiso 1 1 calc R . . C49 C 0.54361(15) 0.52657(17) 0.97752(14) 0.0176(4) Uani 1 1 d . . . C50 C 0.47976(15) 0.60389(16) 0.98016(13) 0.0162(4) Uani 1 1 d . . . C51 C 0.50826(16) 0.67858(18) 1.04360(13) 0.0205(5) Uani 1 1 d . . . H51 H 0.4673 0.7315 1.0458 0.025 Uiso 1 1 calc R . . C52 C 0.59396(17) 0.67507(19) 1.10146(14) 0.0266(5) Uani 1 1 d . . . H52 H 0.6125 0.7264 1.1424 0.032 Uiso 1 1 calc R . . C53 C 0.65497(17) 0.5961(2) 1.10089(15) 0.0287(6) Uani 1 1 d . . . H53 H 0.7129 0.5927 1.1433 0.034 Uiso 1 1 calc R . . C54 C 0.63132(16) 0.52483(19) 1.04004(15) 0.0250(5) Uani 1 1 d . . . H54 H 0.6738 0.4731 1.0391 0.030 Uiso 1 1 calc R . . C55 C 0.50595(14) 0.79699(16) 0.81587(13) 0.0155(4) Uani 1 1 d . . . C56 C 0.55689(15) 0.71280(17) 0.80950(15) 0.0192(4) Uani 1 1 d . . . H56 H 0.5332 0.6652 0.7661 0.023 Uiso 1 1 calc R . . C57 C 0.64312(16) 0.69998(18) 0.86816(15) 0.0234(5) Uani 1 1 d . . . H57 H 0.6789 0.6434 0.8640 0.028 Uiso 1 1 calc R . . C58 C 0.67800(15) 0.76847(19) 0.93285(14) 0.0234(5) Uani 1 1 d . . . C59 C 0.62507(16) 0.85120(18) 0.93816(14) 0.0234(5) Uani 1 1 d . . . H59 H 0.6480 0.8979 0.9826 0.028 Uiso 1 1 calc R . . C60 C 0.53901(15) 0.86695(17) 0.87961(14) 0.0200(5) Uani 1 1 d . . . H60 H 0.5037 0.9242 0.8831 0.024 Uiso 1 1 calc R . . C61 C 0.77168(17) 0.7538(2) 0.99659(17) 0.0346(6) Uani 1 1 d . . . H61A H 0.7909 0.6853 0.9951 0.052 Uiso 1 1 calc R . . H61B H 0.7669 0.7702 1.0550 0.052 Uiso 1 1 calc R . . H61C H 0.8180 0.7964 0.9810 0.052 Uiso 1 1 calc R . . C62 C 0.12112(14) 0.47735(15) 0.78390(13) 0.0161(4) Uani 1 1 d . . . C63 C 0.03193(15) 0.47033(17) 0.72987(14) 0.0206(5) Uani 1 1 d . . . H63 H 0.0227 0.4590 0.6696 0.025 Uiso 1 1 calc R . . C64 C -0.04369(16) 0.48023(17) 0.76575(16) 0.0251(5) Uani 1 1 d . . . H64 H -0.1051 0.4754 0.7293 0.030 Uiso 1 1 calc R . . C65 C -0.03139(17) 0.49706(18) 0.85371(17) 0.0258(5) Uani 1 1 d . . . C66 C 0.05800(18) 0.50229(19) 0.90598(16) 0.0277(5) Uani 1 1 d . . . H66 H 0.0673 0.5126 0.9663 0.033 Uiso 1 1 calc R . . C67 C 0.13514(17) 0.49271(18) 0.87192(15) 0.0238(5) Uani 1 1 d . . . H67 H 0.1965 0.4967 0.9086 0.029 Uiso 1 1 calc R . . C68 C -0.11517(19) 0.5125(2) 0.8899(2) 0.0385(7) Uani 1 1 d . . . H68A H -0.0946 0.5174 0.9530 0.058 Uiso 1 1 calc R . . H68B H -0.1580 0.4570 0.8738 0.058 Uiso 1 1 calc R . . H68C H -0.1471 0.5731 0.8661 0.058 Uiso 1 1 calc R . . C69 C 0.3351(3) 0.3745(4) 0.3076(3) 0.0493(15) Uani 0.631(5) 1 d PD A 1 H69A H 0.3257 0.4353 0.3369 0.074 Uiso 0.631(5) 1 calc PR A 1 H69B H 0.3548 0.3904 0.2551 0.074 Uiso 0.631(5) 1 calc PR A 1 H69C H 0.3834 0.3351 0.3463 0.074 Uiso 0.631(5) 1 calc PR A 1 C70 C 0.2457(2) 0.3176(3) 0.2837(2) 0.0319(11) Uani 0.631(5) 1 d PGD A 1 C71 C 0.2235(3) 0.2495(4) 0.3398(3) 0.0406(13) Uani 0.631(5) 1 d PGD A 1 H71 H 0.2675 0.2342 0.3927 0.049 Uiso 0.631(5) 1 calc PR A 1 C72 C 0.1370(4) 0.2038(7) 0.3187(5) 0.0530(12) Uani 0.631(5) 1 d PG A 1 H72 H 0.1218 0.1572 0.3571 0.064 Uiso 0.631(5) 1 calc PR A 1 C73 C 0.0726(4) 0.2262(9) 0.2414(6) 0.0563(11) Uani 0.631(5) 1 d PG A 1 H73 H 0.0135 0.1949 0.2269 0.068 Uiso 0.631(5) 1 calc PR A 1 C74 C 0.0948(4) 0.2943(7) 0.1852(5) 0.0461(10) Uani 0.631(5) 1 d PG A 1 H74 H 0.0508 0.3097 0.1323 0.055 Uiso 0.631(5) 1 calc PR A 1 C75 C 0.1813(3) 0.3401(4) 0.2063(3) 0.0367(13) Uani 0.631(5) 1 d PGD A 1 H75 H 0.1965 0.3866 0.1679 0.044 Uiso 0.631(5) 1 calc PR A 1 C76 C 0.3189(6) 0.2546(7) 0.3846(5) 0.064(3) Uani 0.369(5) 1 d PD A 2 H76A H 0.3040 0.2130 0.4291 0.096 Uiso 0.369(5) 1 calc PR A 2 H76B H 0.3402 0.3188 0.4094 0.096 Uiso 0.369(5) 1 calc PR A 2 H76C H 0.3682 0.2237 0.3631 0.096 Uiso 0.369(5) 1 calc PR A 2 C77 C 0.2338(5) 0.2674(7) 0.3114(5) 0.0406(13) Uani 0.369(5) 1 d PGD A 2 C78 C 0.1537(7) 0.2146(12) 0.3110(8) 0.0530(12) Uani 0.369(5) 1 d PGD A 2 H78 H 0.1531 0.1707 0.3570 0.064 Uiso 0.369(5) 1 calc PR A 2 C79 C 0.0743(8) 0.2259(16) 0.2433(11) 0.0563(11) Uani 0.369(5) 1 d PG A 2 H79 H 0.0196 0.1898 0.2430 0.068 Uiso 0.369(5) 1 calc PR A 2 C80 C 0.0752(7) 0.2901(13) 0.1760(9) 0.0461(10) Uani 0.369(5) 1 d PG A 2 H80 H 0.0209 0.2978 0.1297 0.055 Uiso 0.369(5) 1 calc PR A 2 C81 C 0.1553(7) 0.3429(7) 0.1764(4) 0.0367(13) Uani 0.369(5) 1 d PG A 2 H81 H 0.1559 0.3867 0.1304 0.044 Uiso 0.369(5) 1 calc PR A 2 C82 C 0.2347(5) 0.3315(6) 0.2441(4) 0.0319(11) Uani 0.369(5) 1 d PGD A 2 H82 H 0.2894 0.3676 0.2444 0.038 Uiso 0.369(5) 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 0.01212(9) 0.01084(9) 0.00997(8) -0.00012(8) 0.00205(6) 0.00027(8) S1 0.0126(2) 0.0118(2) 0.0124(2) -0.00042(19) 0.00213(18) 0.00095(18) S2 0.0135(2) 0.0140(3) 0.0147(2) -0.00066(19) 0.00429(18) 0.00164(19) S3 0.0144(2) 0.0118(2) 0.0124(2) -0.00057(18) 0.00304(18) -0.00114(18) S4 0.0162(2) 0.0109(2) 0.0135(2) -0.00060(18) 0.00275(18) -0.00178(19) N1 0.0124(8) 0.0108(8) 0.0130(8) 0.0008(6) 0.0034(6) 0.0028(6) N2 0.0132(8) 0.0130(9) 0.0108(8) 0.0005(7) 0.0035(6) 0.0017(7) N3 0.0124(8) 0.0114(9) 0.0112(8) -0.0007(6) 0.0027(6) -0.0022(6) N4 0.0155(9) 0.0122(9) 0.0108(8) -0.0013(7) 0.0012(7) -0.0019(7) O1 0.0141(7) 0.0153(7) 0.0127(7) 0.0030(6) 0.0028(5) 0.0013(5) O2 0.0180(7) 0.0129(7) 0.0183(7) -0.0027(6) 0.0034(6) 0.0018(6) O3 0.0152(7) 0.0173(8) 0.0126(7) 0.0012(6) 0.0016(6) 0.0030(6) O4 0.0230(8) 0.0130(8) 0.0240(8) -0.0029(6) 0.0063(6) 0.0031(6) O5 0.0157(7) 0.0161(7) 0.0107(7) -0.0023(6) 0.0024(5) -0.0017(6) O6 0.0201(8) 0.0125(7) 0.0197(8) -0.0004(6) 0.0021(6) -0.0015(6) O7 0.0185(7) 0.0136(7) 0.0115(7) -0.0014(5) 0.0022(5) -0.0014(6) O8 0.0242(8) 0.0122(8) 0.0204(8) 0.0002(6) 0.0030(6) -0.0003(6) C1 0.0133(9) 0.0110(10) 0.0123(9) 0.0005(8) 0.0008(7) -0.0005(8) C2 0.0128(9) 0.0133(10) 0.0127(9) 0.0036(8) 0.0017(7) 0.0011(8) C3 0.0187(11) 0.0139(10) 0.0161(10) -0.0018(8) 0.0023(8) 0.0013(8) C4 0.0213(11) 0.0115(10) 0.0209(11) -0.0006(8) 0.0026(8) -0.0027(8) C5 0.0183(11) 0.0170(11) 0.0164(10) 0.0019(8) 0.0012(8) -0.0031(8) C6 0.0152(10) 0.0176(11) 0.0130(9) 0.0008(8) 0.0011(7) -0.0011(8) C7 0.0254(12) 0.0206(12) 0.0161(10) -0.0008(9) 0.0067(9) -0.0052(9) C8 0.0315(13) 0.0332(14) 0.0195(11) 0.0006(10) 0.0117(10) -0.0049(10) C9 0.0311(13) 0.0313(14) 0.0243(12) 0.0054(10) 0.0108(10) -0.0099(11) C10 0.0268(12) 0.0193(12) 0.0239(11) 0.0033(9) 0.0042(9) -0.0086(9) C11 0.0140(9) 0.0142(11) 0.0117(9) -0.0017(7) 0.0047(7) -0.0010(7) C12 0.0124(10) 0.0149(11) 0.0132(9) 0.0001(8) 0.0036(8) 0.0004(8) C13 0.0165(10) 0.0122(10) 0.0176(10) 0.0003(8) 0.0055(8) 0.0001(8) C14 0.0176(10) 0.0137(10) 0.0194(10) -0.0026(8) 0.0058(8) -0.0021(8) C15 0.0148(10) 0.0193(11) 0.0128(10) -0.0032(8) 0.0027(8) -0.0007(8) C16 0.0149(9) 0.0163(11) 0.0118(8) -0.0009(9) 0.0043(7) -0.0009(9) C17 0.0188(11) 0.0175(12) 0.0172(11) -0.0020(8) 0.0043(9) 0.0023(8) C18 0.0205(12) 0.0252(13) 0.0181(11) 0.0009(9) 0.0003(9) 0.0020(9) C19 0.0183(11) 0.0304(15) 0.0165(10) -0.0053(9) -0.0008(8) -0.0002(9) C20 0.0203(11) 0.0211(12) 0.0188(11) -0.0055(9) 0.0028(9) -0.0014(9) C21 0.0133(10) 0.0163(10) 0.0123(9) 0.0007(8) 0.0017(7) -0.0005(8) C22 0.0206(11) 0.0152(11) 0.0203(11) -0.0008(8) 0.0034(9) 0.0031(8) C23 0.0165(11) 0.0209(12) 0.0204(11) 0.0037(9) -0.0022(8) 0.0037(9) C24 0.0170(9) 0.0182(11) 0.0164(9) 0.0020(9) 0.0024(7) -0.0060(9) C25 0.0167(10) 0.0141(11) 0.0210(11) 0.0000(8) 0.0031(8) -0.0005(8) C26 0.0141(10) 0.0144(12) 0.0190(10) 0.0013(8) 0.0026(8) 0.0018(7) C27 0.0237(12) 0.0239(13) 0.0203(11) 0.0025(9) -0.0059(9) -0.0044(9) C28 0.0136(10) 0.0239(13) 0.0182(11) -0.0012(9) 0.0063(8) -0.0011(9) C29 0.0482(18) 0.0295(15) 0.0376(16) -0.0137(12) 0.0308(14) -0.0145(12) C30 0.056(2) 0.0313(16) 0.0469(18) -0.0109(13) 0.0370(16) -0.0174(13) C31 0.0191(12) 0.0345(14) 0.0295(13) -0.0007(11) 0.0139(10) -0.0032(10) C32 0.0354(15) 0.0337(16) 0.0278(13) -0.0013(11) 0.0200(11) 0.0083(11) C33 0.0285(13) 0.0230(13) 0.0296(13) 0.0021(10) 0.0145(10) 0.0067(10) C34 0.0430(17) 0.0460(18) 0.0408(16) 0.0060(13) 0.0287(14) 0.0028(13) C35 0.0135(10) 0.0159(10) 0.0119(9) -0.0030(8) 0.0026(7) -0.0037(8) C36 0.0122(9) 0.0166(10) 0.0126(9) -0.0030(8) 0.0026(7) -0.0028(8) C37 0.0174(10) 0.0186(11) 0.0169(10) -0.0038(8) 0.0035(8) -0.0001(8) C38 0.0177(11) 0.0236(12) 0.0241(11) -0.0053(9) 0.0069(9) 0.0023(9) C39 0.0199(11) 0.0243(12) 0.0173(10) -0.0083(9) 0.0067(8) -0.0034(9) C40 0.0182(11) 0.0199(11) 0.0127(9) -0.0041(8) 0.0055(8) -0.0036(8) C41 0.0295(12) 0.0202(12) 0.0175(10) -0.0031(8) 0.0092(9) -0.0043(9) C42 0.0354(14) 0.0299(13) 0.0194(11) -0.0013(9) 0.0130(10) -0.0090(10) C43 0.0303(13) 0.0376(16) 0.0199(11) -0.0082(10) 0.0153(10) -0.0099(10) C44 0.0220(12) 0.0348(14) 0.0260(12) -0.0111(11) 0.0111(10) -0.0047(10) C45 0.0162(10) 0.0159(10) 0.0099(9) 0.0030(7) 0.0032(8) -0.0012(8) C46 0.0139(10) 0.0138(10) 0.0113(9) 0.0032(8) 0.0031(7) 0.0006(8) C47 0.0196(10) 0.0143(10) 0.0162(10) 0.0001(8) 0.0056(8) -0.0003(8) C48 0.0184(11) 0.0165(11) 0.0233(11) 0.0043(9) 0.0060(9) 0.0042(8) C49 0.0163(10) 0.0206(11) 0.0154(10) 0.0063(8) 0.0031(8) 0.0004(8) C50 0.0170(10) 0.0205(11) 0.0111(9) 0.0021(8) 0.0038(8) -0.0019(8) C51 0.0207(11) 0.0271(12) 0.0131(10) -0.0002(9) 0.0033(8) -0.0035(9) C52 0.0265(13) 0.0390(15) 0.0136(10) -0.0027(9) 0.0035(9) -0.0096(10) C53 0.0191(12) 0.0454(15) 0.0174(11) 0.0060(10) -0.0031(9) -0.0033(10) C54 0.0189(11) 0.0323(14) 0.0214(11) 0.0101(10) 0.0007(9) 0.0023(10) C55 0.0151(10) 0.0186(11) 0.0128(9) -0.0001(8) 0.0036(8) -0.0020(8) C56 0.0178(11) 0.0180(11) 0.0209(11) -0.0021(9) 0.0034(8) -0.0032(9) C57 0.0172(11) 0.0267(13) 0.0256(12) 0.0011(10) 0.0040(9) 0.0027(9) C58 0.0163(11) 0.0334(14) 0.0183(11) 0.0051(10) 0.0004(8) -0.0026(9) C59 0.0226(12) 0.0284(13) 0.0162(10) -0.0044(9) -0.0009(9) -0.0061(9) C60 0.0201(11) 0.0199(12) 0.0182(10) -0.0028(9) 0.0019(9) -0.0026(9) C61 0.0208(12) 0.0498(17) 0.0278(13) 0.0063(12) -0.0035(10) -0.0004(12) C62 0.0192(10) 0.0115(10) 0.0190(10) 0.0007(8) 0.0075(8) -0.0029(8) C63 0.0210(11) 0.0189(11) 0.0201(11) -0.0015(9) 0.0023(8) -0.0028(9) C64 0.0216(11) 0.0173(12) 0.0365(13) 0.0010(10) 0.0073(10) -0.0023(9) C65 0.0270(13) 0.0173(12) 0.0376(14) -0.0005(10) 0.0165(11) -0.0016(9) C66 0.0298(13) 0.0329(14) 0.0239(12) -0.0066(10) 0.0131(10) -0.0043(10) C67 0.0230(12) 0.0299(13) 0.0185(11) -0.0018(10) 0.0051(9) -0.0050(10) C68 0.0344(15) 0.0355(16) 0.0539(18) -0.0019(13) 0.0265(14) 0.0017(12) C69 0.033(3) 0.067(4) 0.053(3) -0.024(3) 0.020(2) -0.011(2) C70 0.035(2) 0.041(2) 0.029(3) -0.015(3) 0.023(2) -0.0047(17) C71 0.050(2) 0.039(3) 0.039(3) -0.009(3) 0.023(2) 0.011(2) C72 0.074(4) 0.026(3) 0.074(3) -0.0183(19) 0.046(3) -0.006(2) C73 0.0451(19) 0.0388(19) 0.098(3) -0.040(2) 0.042(2) -0.0184(15) C74 0.034(3) 0.045(2) 0.059(3) -0.030(2) 0.011(2) -0.003(2) C75 0.037(4) 0.045(2) 0.029(3) -0.022(3) 0.010(3) -0.012(2) C76 0.062(6) 0.048(6) 0.062(6) -0.033(5) -0.018(5) 0.011(5) C77 0.050(2) 0.039(3) 0.039(3) -0.009(3) 0.023(2) 0.011(2) C78 0.074(4) 0.026(3) 0.074(3) -0.0183(19) 0.046(3) -0.006(2) C79 0.0451(19) 0.0388(19) 0.098(3) -0.040(2) 0.042(2) -0.0184(15) C80 0.034(3) 0.045(2) 0.059(3) -0.030(2) 0.011(2) -0.003(2) C81 0.037(4) 0.045(2) 0.029(3) -0.022(3) 0.010(3) -0.012(2) C82 0.035(2) 0.041(2) 0.029(3) -0.015(3) 0.023(2) -0.0047(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 2.1707(16) . ? Zr1 N3 2.1951(17) . ? Zr1 N2 2.2067(16) . ? Zr1 N4 2.2376(17) . ? Zr1 O3 2.2776(15) . ? Zr1 O1 2.3129(14) . ? Zr1 O7 2.3196(15) . ? Zr1 O5 2.3377(15) . ? Zr1 S2 2.9292(6) . ? Zr1 S1 2.9394(6) . ? Zr1 S4 2.9509(6) . ? Zr1 S3 2.9649(6) . ? S1 O2 1.4311(15) . ? S1 O1 1.4892(14) . ? S1 N1 1.5788(17) . ? S1 C21 1.755(2) . ? S2 O4 1.4339(16) . ? S2 O3 1.4978(15) . ? S2 N2 1.5786(17) . ? S2 C28 1.758(2) . ? S3 O6 1.4331(16) . ? S3 O5 1.4862(15) . ? S3 N3 1.5758(17) . ? S3 C55 1.758(2) . ? S4 O8 1.4354(16) . ? S4 O7 1.4923(15) . ? S4 N4 1.5681(18) . ? S4 C62 1.769(2) . ? N1 C2 1.426(3) . ? N2 C12 1.427(2) . ? N3 C36 1.427(3) . ? N4 C46 1.426(2) . ? C1 C2 1.385(3) . ? C1 C6 1.437(3) . ? C1 C11 1.490(3) . ? C2 C3 1.419(3) . ? C3 C4 1.365(3) . ? C3 H3 0.9500 . ? C4 C5 1.419(3) . ? C4 H4 0.9500 . ? C5 C10 1.416(3) . ? C5 C6 1.429(3) . ? C6 C7 1.419(3) . ? C7 C8 1.378(3) . ? C7 H7 0.9500 . ? C8 C9 1.403(4) . ? C8 H8 0.9500 . ? C9 C10 1.360(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 C16 1.440(3) . ? C12 C13 1.416(3) . ? C13 C14 1.362(3) . ? C13 H13 0.9500 . ? C14 C15 1.420(3) . ? C14 H14 0.9500 . ? C15 C20 1.413(3) . ? C15 C16 1.424(3) . ? C16 C17 1.420(3) . ? C17 C18 1.374(3) . ? C17 H17 0.9500 . ? C18 C19 1.408(3) . ? C18 H18 0.9500 . ? C19 C20 1.360(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.386(3) . ? C21 C22 1.389(3) . ? C22 C23 1.393(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.404(3) . ? C24 C27 1.498(3) . ? C25 C26 1.386(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.380(3) . ? C28 C29 1.390(3) . ? C29 C30 1.378(4) . ? C29 H29 0.9500 . ? C30 C31 1.389(4) . ? C30 H30 0.9500 . ? C31 C32 1.377(4) . ? C31 C34 1.501(4) . ? C32 C33 1.392(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.382(3) . ? C35 C40 1.440(3) . ? C35 C45 1.495(3) . ? C36 C37 1.421(3) . ? C37 C38 1.367(3) . ? C37 H37 0.9500 . ? C38 C39 1.424(3) . ? C38 H38 0.9500 . ? C39 C44 1.416(3) . ? C39 C40 1.423(3) . ? C40 C41 1.418(3) . ? C41 C42 1.375(3) . ? C41 H41 0.9500 . ? C42 C43 1.399(4) . ? C42 H42 0.9500 . ? C43 C44 1.372(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.379(3) . ? C45 C50 1.435(3) . ? C46 C47 1.422(3) . ? C47 C48 1.360(3) . ? C47 H47 0.9500 . ? C48 C49 1.408(3) . ? C48 H48 0.9500 . ? C49 C54 1.425(3) . ? C49 C50 1.426(3) . ? C50 C51 1.424(3) . ? C51 C52 1.369(3) . ? C51 H51 0.9500 . ? C52 C53 1.410(4) . ? C52 H52 0.9500 . ? C53 C54 1.357(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.391(3) . ? C55 C56 1.394(3) . ? C56 C57 1.391(3) . ? C56 H56 0.9500 . ? C57 C58 1.392(3) . ? C57 H57 0.9500 . ? C58 C59 1.391(3) . ? C58 C61 1.513(3) . ? C59 C60 1.394(3) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C67 1.385(3) . ? C62 C63 1.387(3) . ? C63 C64 1.392(3) . ? C63 H63 0.9500 . ? C64 C65 1.391(4) . ? C64 H64 0.9500 . ? C65 C66 1.378(4) . ? C65 C68 1.514(3) . ? C66 C67 1.394(3) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.501(4) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.3900 . ? C70 C75 1.3900 . ? C71 C72 1.3900 . ? C71 H71 0.9500 . ? C72 C73 1.3900 . ? C72 H72 0.9500 . ? C73 C74 1.3900 . ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.496(6) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.3900 . ? C77 C82 1.3900 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 C80 1.3900 . ? C79 H79 0.9500 . ? C80 C81 1.3900 . ? C80 H80 0.9500 . ? C81 C82 1.3900 . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? 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 98.26(6) . . ? N1 Zr1 N2 75.98(6) . . ? N3 Zr1 N2 150.02(6) . . ? N1 Zr1 N4 146.39(6) . . ? N3 Zr1 N4 74.84(6) . . ? N2 Zr1 N4 125.57(6) . . ? N1 Zr1 O3 130.05(6) . . ? N3 Zr1 O3 104.64(6) . . ? N2 Zr1 O3 62.10(6) . . ? N4 Zr1 O3 83.01(6) . . ? N1 Zr1 O1 61.64(6) . . ? N3 Zr1 O1 80.79(6) . . ? N2 Zr1 O1 119.40(6) . . ? N4 Zr1 O1 84.75(6) . . ? O3 Zr1 O1 164.74(5) . . ? N1 Zr1 O7 105.59(6) . . ? N3 Zr1 O7 130.78(6) . . ? N2 Zr1 O7 78.44(6) . . ? N4 Zr1 O7 61.44(6) . . ? O3 Zr1 O7 91.99(5) . . ? O1 Zr1 O7 74.11(5) . . ? N1 Zr1 O5 79.53(6) . . ? N3 Zr1 O5 60.85(5) . . ? N2 Zr1 O5 89.21(6) . . ? N4 Zr1 O5 121.58(6) . . ? O3 Zr1 O5 74.25(6) . . ? O1 Zr1 O5 120.24(5) . . ? O7 Zr1 O5 164.80(5) . . ? N1 Zr1 S2 105.58(5) . . ? N3 Zr1 S2 131.68(5) . . ? N2 Zr1 S2 32.05(4) . . ? N4 Zr1 S2 103.04(5) . . ? O3 Zr1 S2 30.27(4) . . ? O1 Zr1 S2 147.52(4) . . ? O7 Zr1 S2 82.04(4) . . ? O5 Zr1 S2 82.79(4) . . ? N1 Zr1 S1 31.68(4) . . ? N3 Zr1 S1 87.72(5) . . ? N2 Zr1 S1 100.00(4) . . ? N4 Zr1 S1 114.74(5) . . ? O3 Zr1 S1 160.86(4) . . ? O1 Zr1 S1 30.03(4) . . ? O7 Zr1 S1 90.71(4) . . ? O5 Zr1 S1 100.22(4) . . ? S2 Zr1 S1 132.014(16) . . ? N1 Zr1 S4 128.44(5) . . ? N3 Zr1 S4 103.42(5) . . ? N2 Zr1 S4 102.93(5) . . ? N4 Zr1 S4 31.53(4) . . ? O3 Zr1 S4 88.41(4) . . ? O1 Zr1 S4 76.40(4) . . ? O7 Zr1 S4 29.95(4) . . ? O5 Zr1 S4 151.27(4) . . ? S2 Zr1 S4 93.748(17) . . ? S1 Zr1 S4 103.091(16) . . ? N1 Zr1 S3 86.96(5) . . ? N3 Zr1 S3 31.27(4) . . ? N2 Zr1 S3 118.85(5) . . ? N4 Zr1 S3 100.37(5) . . ? O3 Zr1 S3 90.33(4) . . ? O1 Zr1 S3 100.83(4) . . ? O7 Zr1 S3 161.18(4) . . ? O5 Zr1 S3 29.65(3) . . ? S2 Zr1 S3 108.467(16) . . ? S1 Zr1 S3 93.192(16) . . ? S4 Zr1 S3 131.570(16) . . ? O2 S1 O1 116.90(9) . . ? O2 S1 N1 117.29(9) . . ? O1 S1 N1 97.10(8) . . ? O2 S1 C21 108.65(10) . . ? O1 S1 C21 108.89(9) . . ? N1 S1 C21 107.16(9) . . ? O2 S1 Zr1 130.50(7) . . ? O1 S1 Zr1 51.01(6) . . ? N1 S1 Zr1 46.23(6) . . ? C21 S1 Zr1 120.73(7) . . ? O4 S2 O3 114.85(9) . . ? O4 S2 N2 118.42(10) . . ? O3 S2 N2 97.52(9) . . ? O4 S2 C28 107.67(10) . . ? O3 S2 C28 112.43(10) . . ? N2 S2 C28 105.51(10) . . ? O4 S2 Zr1 127.77(7) . . ? O3 S2 Zr1 50.04(6) . . ? N2 S2 Zr1 47.88(6) . . ? C28 S2 Zr1 124.45(8) . . ? O6 S3 O5 117.16(9) . . ? O6 S3 N3 116.76(9) . . ? O5 S3 N3 97.26(9) . . ? O6 S3 C55 108.09(10) . . ? O5 S3 C55 108.49(9) . . ? N3 S3 C55 108.40(9) . . ? O6 S3 Zr1 130.17(7) . . ? O5 S3 Zr1 51.10(6) . . ? N3 S3 Zr1 46.31(6) . . ? C55 S3 Zr1 121.65(7) . . ? O8 S4 O7 116.55(9) . . ? O8 S4 N4 117.24(10) . . ? O7 S4 N4 99.09(9) . . ? O8 S4 C62 108.24(10) . . ? O7 S4 C62 106.89(9) . . ? N4 S4 C62 108.03(10) . . ? O8 S4 Zr1 136.57(7) . . ? O7 S4 Zr1 50.90(6) . . ? N4 S4 Zr1 48.27(6) . . ? C62 S4 Zr1 115.18(7) . . ? C2 N1 S1 126.25(14) . . ? C2 N1 Zr1 130.49(13) . . ? S1 N1 Zr1 102.09(8) . . ? C12 N2 S2 123.86(14) . . ? C12 N2 Zr1 132.47(13) . . ? S2 N2 Zr1 100.07(8) . . ? C36 N3 S3 126.48(14) . . ? C36 N3 Zr1 130.20(13) . . ? S3 N3 Zr1 102.43(8) . . ? C46 N4 S4 126.76(15) . . ? C46 N4 Zr1 125.75(13) . . ? S4 N4 Zr1 100.19(8) . . ? S1 O1 Zr1 98.96(7) . . ? S2 O3 Zr1 99.70(7) . . ? S3 O5 Zr1 99.25(7) . . ? S4 O7 Zr1 99.15(7) . . ? C2 C1 C6 118.23(19) . . ? C2 C1 C11 121.58(18) . . ? C6 C1 C11 120.19(18) . . ? C1 C2 C3 121.54(19) . . ? C1 C2 N1 119.52(18) . . ? C3 C2 N1 118.63(18) . . ? C4 C3 C2 120.2(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C10 C5 C4 121.7(2) . . ? C10 C5 C6 119.5(2) . . ? C4 C5 C6 118.70(19) . . ? C7 C6 C5 117.85(19) . . ? C7 C6 C1 122.1(2) . . ? C5 C6 C1 119.99(19) . . ? C8 C7 C6 120.9(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C5 120.9(2) . . ? C9 C10 H10 119.6 . . ? C5 C10 H10 119.6 . . ? C12 C11 C16 117.96(18) . . ? C12 C11 C1 122.33(18) . . ? C16 C11 C1 119.69(18) . . ? C11 C12 C13 121.45(18) . . ? C11 C12 N2 119.22(18) . . ? C13 C12 N2 119.12(18) . . ? C14 C13 C12 120.67(19) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 120.6(2) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C20 C15 C14 121.6(2) . . ? C20 C15 C16 119.5(2) . . ? C14 C15 C16 118.90(19) . . ? C17 C16 C15 117.62(18) . . ? C17 C16 C11 122.2(2) . . ? C15 C16 C11 120.18(19) . . ? C18 C17 C16 121.4(2) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 120.1(2) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C15 121.2(2) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? C26 C21 C22 121.77(19) . . ? C26 C21 S1 118.79(16) . . ? C22 C21 S1 119.06(17) . . ? C21 C22 C23 118.6(2) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 118.56(19) . . ? C23 C24 C27 120.9(2) . . ? C25 C24 C27 120.5(2) . . ? C26 C25 C24 121.2(2) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 118.69(19) . . ? C25 C26 H26 120.7 . . ? C21 C26 H26 120.7 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 120.0(2) . . ? C33 C28 S2 119.70(19) . . ? C29 C28 S2 119.09(19) . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.9(3) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 118.8(2) . . ? C32 C31 C34 121.7(2) . . ? C30 C31 C34 119.4(3) . . ? C31 C32 C33 121.1(2) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C28 C33 C32 119.4(2) . . ? C28 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 118.52(19) . . ? C36 C35 C45 120.77(18) . . ? C40 C35 C45 120.47(19) . . ? C35 C36 C37 121.96(19) . . ? C35 C36 N3 119.26(18) . . ? C37 C36 N3 118.37(18) . . ? C38 C37 C36 119.5(2) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 121.0(2) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C44 C39 C40 119.4(2) . . ? C44 C39 C38 121.4(2) . . ? C40 C39 C38 119.16(19) . . ? C41 C40 C39 118.25(19) . . ? C41 C40 C35 122.1(2) . . ? C39 C40 C35 119.5(2) . . ? C42 C41 C40 120.8(2) . . ? C42 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C41 C42 C43 120.7(2) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C39 120.8(2) . . ? C43 C44 H44 119.6 . . ? C39 C44 H44 119.6 . . ? C46 C45 C50 118.78(19) . . ? C46 C45 C35 120.25(18) . . ? C50 C45 C35 120.96(18) . . ? C45 C46 C47 121.34(19) . . ? C45 C46 N4 119.36(18) . . ? C47 C46 N4 118.92(18) . . ? C48 C47 C46 119.9(2) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C47 C48 C49 121.3(2) . . ? C47 C48 H48 119.3 . . ? C49 C48 H48 119.3 . . ? C48 C49 C54 121.7(2) . . ? C48 C49 C50 119.12(19) . . ? C54 C49 C50 119.1(2) . . ? C51 C50 C49 118.17(19) . . ? C51 C50 C45 122.4(2) . . ? C49 C50 C45 119.41(19) . . ? C52 C51 C50 120.8(2) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 120.7(2) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 120.3(2) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C49 120.9(2) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? C60 C55 C56 121.5(2) . . ? C60 C55 S3 118.06(17) . . ? C56 C55 S3 120.19(16) . . ? C57 C56 C55 118.5(2) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C56 C57 C58 121.3(2) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C59 C58 C57 118.8(2) . . ? C59 C58 C61 120.2(2) . . ? C57 C58 C61 121.0(2) . . ? C58 C59 C60 121.3(2) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C55 C60 C59 118.5(2) . . ? C55 C60 H60 120.7 . . ? C59 C60 H60 120.7 . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C67 C62 C63 121.0(2) . . ? C67 C62 S4 118.16(17) . . ? C63 C62 S4 120.82(16) . . ? C62 C63 C64 118.6(2) . . ? C62 C63 H63 120.7 . . ? C64 C63 H63 120.7 . . ? C65 C64 C63 121.5(2) . . ? C65 C64 H64 119.3 . . ? C63 C64 H64 119.3 . . ? C66 C65 C64 118.6(2) . . ? C66 C65 C68 121.3(2) . . ? C64 C65 C68 120.1(2) . . ? C65 C66 C67 121.2(2) . . ? C65 C66 H66 119.4 . . ? C67 C66 H66 119.4 . . ? C62 C67 C66 119.1(2) . . ? C62 C67 H67 120.5 . . ? C66 C67 H67 120.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C71 C70 C75 120.0 . . ? C71 C70 C69 121.5(3) . . ? C75 C70 C69 118.4(3) . . ? C70 C71 C72 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C73 C72 C71 120.0 . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 H74 120.0 . . ? C75 C74 H74 120.0 . . ? C74 C75 C70 120.0 . . ? C74 C75 H75 120.0 . . ? C70 C75 H75 120.0 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C82 120.0 . . ? C78 C77 C76 119.6(4) . . ? C82 C77 C76 120.4(4) . . ? C79 C78 C77 120.0 . . ? C79 C78 H78 120.0 . . ? C77 C78 H78 120.0 . . ? C80 C79 C78 120.0 . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C79 C80 C81 120.0 . . ? C79 C80 H80 120.0 . . ? C81 C80 H80 120.0 . . ? C82 C81 C80 120.0 . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C77 120.0 . . ? C81 C82 H82 120.0 . . ? C77 C82 H82 120.0 . . ? 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 N1 Zr1 S1 O2 -90.96(12) . . . . ? N3 Zr1 S1 O2 18.81(10) . . . . ? N2 Zr1 S1 O2 -132.03(9) . . . . ? N4 Zr1 S1 O2 90.96(10) . . . . ? O3 Zr1 S1 O2 -112.26(14) . . . . ? O1 Zr1 S1 O2 94.25(11) . . . . ? O7 Zr1 S1 O2 149.59(9) . . . . ? O5 Zr1 S1 O2 -41.02(9) . . . . ? S2 Zr1 S1 O2 -130.50(8) . . . . ? S4 Zr1 S1 O2 122.06(9) . . . . ? S3 Zr1 S1 O2 -11.99(9) . . . . ? N1 Zr1 S1 O1 174.79(12) . . . . ? N3 Zr1 S1 O1 -75.45(9) . . . . ? N2 Zr1 S1 O1 133.72(9) . . . . ? N4 Zr1 S1 O1 -3.29(9) . . . . ? O3 Zr1 S1 O1 153.49(14) . . . . ? O7 Zr1 S1 O1 55.34(8) . . . . ? O5 Zr1 S1 O1 -135.27(8) . . . . ? S2 Zr1 S1 O1 135.25(7) . . . . ? S4 Zr1 S1 O1 27.80(7) . . . . ? S3 Zr1 S1 O1 -106.24(7) . . . . ? N3 Zr1 S1 N1 109.76(10) . . . . ? N2 Zr1 S1 N1 -41.07(10) . . . . ? N4 Zr1 S1 N1 -178.08(10) . . . . ? O3 Zr1 S1 N1 -21.30(15) . . . . ? O1 Zr1 S1 N1 -174.79(12) . . . . ? O7 Zr1 S1 N1 -119.45(9) . . . . ? O5 Zr1 S1 N1 49.94(9) . . . . ? S2 Zr1 S1 N1 -39.54(9) . . . . ? S4 Zr1 S1 N1 -146.99(9) . . . . ? S3 Zr1 S1 N1 78.97(9) . . . . ? N1 Zr1 S1 C21 84.60(12) . . . . ? N3 Zr1 S1 C21 -165.63(9) . . . . ? N2 Zr1 S1 C21 43.53(9) . . . . ? N4 Zr1 S1 C21 -93.47(10) . . . . ? O3 Zr1 S1 C21 63.30(15) . . . . ? O1 Zr1 S1 C21 -90.19(11) . . . . ? O7 Zr1 S1 C21 -34.85(9) . . . . ? O5 Zr1 S1 C21 134.54(9) . . . . ? S2 Zr1 S1 C21 45.06(9) . . . . ? S4 Zr1 S1 C21 -62.38(8) . . . . ? S3 Zr1 S1 C21 163.57(8) . . . . ? N1 Zr1 S2 O4 -119.53(10) . . . . ? N3 Zr1 S2 O4 123.86(10) . . . . ? N2 Zr1 S2 O4 -96.37(12) . . . . ? N4 Zr1 S2 O4 42.67(10) . . . . ? O3 Zr1 S2 O4 92.53(12) . . . . ? O1 Zr1 S2 O4 -58.22(11) . . . . ? O7 Zr1 S2 O4 -15.47(9) . . . . ? O5 Zr1 S2 O4 163.50(9) . . . . ? S1 Zr1 S2 O4 -99.22(9) . . . . ? S4 Zr1 S2 O4 12.16(9) . . . . ? S3 Zr1 S2 O4 148.46(9) . . . . ? N1 Zr1 S2 O3 147.94(9) . . . . ? N3 Zr1 S2 O3 31.33(10) . . . . ? N2 Zr1 S2 O3 171.09(12) . . . . ? N4 Zr1 S2 O3 -49.87(9) . . . . ? O1 Zr1 S2 O3 -150.76(10) . . . . ? O7 Zr1 S2 O3 -108.01(8) . . . . ? O5 Zr1 S2 O3 70.96(9) . . . . ? S1 Zr1 S2 O3 168.25(8) . . . . ? S4 Zr1 S2 O3 -80.37(8) . . . . ? S3 Zr1 S2 O3 55.93(8) . . . . ? N1 Zr1 S2 N2 -23.15(10) . . . . ? N3 Zr1 S2 N2 -139.77(10) . . . . ? N4 Zr1 S2 N2 139.04(10) . . . . ? O3 Zr1 S2 N2 -171.09(12) . . . . ? O1 Zr1 S2 N2 38.15(11) . . . . ? O7 Zr1 S2 N2 80.90(9) . . . . ? O5 Zr1 S2 N2 -100.13(9) . . . . ? S1 Zr1 S2 N2 -2.84(9) . . . . ? S4 Zr1 S2 N2 108.54(9) . . . . ? S3 Zr1 S2 N2 -115.17(9) . . . . ? N1 Zr1 S2 C28 56.29(10) . . . . ? N3 Zr1 S2 C28 -60.32(11) . . . . ? N2 Zr1 S2 C28 79.44(13) . . . . ? N4 Zr1 S2 C28 -141.52(10) . . . . ? O3 Zr1 S2 C28 -91.65(12) . . . . ? O1 Zr1 S2 C28 117.60(11) . . . . ? O7 Zr1 S2 C28 160.34(10) . . . . ? O5 Zr1 S2 C28 -20.68(10) . . . . ? S1 Zr1 S2 C28 76.60(10) . . . . ? S4 Zr1 S2 C28 -172.02(9) . . . . ? S3 Zr1 S2 C28 -35.72(10) . . . . ? N1 Zr1 S3 O6 20.89(10) . . . . ? N3 Zr1 S3 O6 -90.48(12) . . . . ? N2 Zr1 S3 O6 93.06(10) . . . . ? N4 Zr1 S3 O6 -126.05(10) . . . . ? O3 Zr1 S3 O6 150.99(10) . . . . ? O1 Zr1 S3 O6 -39.47(10) . . . . ? O7 Zr1 S3 O6 -111.85(14) . . . . ? O5 Zr1 S3 O6 94.96(12) . . . . ? S2 Zr1 S3 O6 126.32(9) . . . . ? S1 Zr1 S3 O6 -10.18(9) . . . . ? S4 Zr1 S3 O6 -120.84(9) . . . . ? N1 Zr1 S3 O5 -74.07(9) . . . . ? N3 Zr1 S3 O5 174.56(12) . . . . ? N2 Zr1 S3 O5 -1.90(9) . . . . ? N4 Zr1 S3 O5 138.99(9) . . . . ? O3 Zr1 S3 O5 56.03(9) . . . . ? O1 Zr1 S3 O5 -134.43(8) . . . . ? O7 Zr1 S3 O5 153.19(13) . . . . ? S2 Zr1 S3 O5 31.35(8) . . . . ? S1 Zr1 S3 O5 -105.15(7) . . . . ? S4 Zr1 S3 O5 144.20(7) . . . . ? N1 Zr1 S3 N3 111.37(10) . . . . ? N2 Zr1 S3 N3 -176.45(10) . . . . ? N4 Zr1 S3 N3 -35.57(9) . . . . ? O3 Zr1 S3 N3 -118.53(9) . . . . ? O1 Zr1 S3 N3 51.01(9) . . . . ? O7 Zr1 S3 N3 -21.37(15) . . . . ? O5 Zr1 S3 N3 -174.56(12) . . . . ? S2 Zr1 S3 N3 -143.20(9) . . . . ? S1 Zr1 S3 N3 80.30(9) . . . . ? S4 Zr1 S3 N3 -30.35(9) . . . . ? N1 Zr1 S3 C55 -162.99(9) . . . . ? N3 Zr1 S3 C55 85.63(12) . . . . ? N2 Zr1 S3 C55 -90.82(9) . . . . ? N4 Zr1 S3 C55 50.06(9) . . . . ? O3 Zr1 S3 C55 -32.89(9) . . . . ? O1 Zr1 S3 C55 136.64(9) . . . . ? O7 Zr1 S3 C55 64.26(14) . . . . ? O5 Zr1 S3 C55 -88.92(11) . . . . ? S2 Zr1 S3 C55 -57.57(8) . . . . ? S1 Zr1 S3 C55 165.93(8) . . . . ? S4 Zr1 S3 C55 55.28(8) . . . . ? N1 Zr1 S4 O8 135.18(11) . . . . ? N3 Zr1 S4 O8 -112.62(11) . . . . ? N2 Zr1 S4 O8 52.94(11) . . . . ? N4 Zr1 S4 O8 -87.13(13) . . . . ? O3 Zr1 S4 O8 -7.94(10) . . . . ? O1 Zr1 S4 O8 170.50(10) . . . . ? O7 Zr1 S4 O8 88.82(12) . . . . ? O5 Zr1 S4 O8 -59.96(13) . . . . ? S2 Zr1 S4 O8 21.87(10) . . . . ? S1 Zr1 S4 O8 156.61(10) . . . . ? S3 Zr1 S4 O8 -96.97(10) . . . . ? N1 Zr1 S4 O7 46.36(9) . . . . ? N3 Zr1 S4 O7 158.56(9) . . . . ? N2 Zr1 S4 O7 -35.87(9) . . . . ? N4 Zr1 S4 O7 -175.95(12) . . . . ? O3 Zr1 S4 O7 -96.76(8) . . . . ? O1 Zr1 S4 O7 81.68(8) . . . . ? O5 Zr1 S4 O7 -148.78(10) . . . . ? S2 Zr1 S4 O7 -66.95(8) . . . . ? S1 Zr1 S4 O7 67.79(8) . . . . ? S3 Zr1 S4 O7 174.21(7) . . . . ? N1 Zr1 S4 N4 -137.69(10) . . . . ? N3 Zr1 S4 N4 -25.49(9) . . . . ? N2 Zr1 S4 N4 140.08(10) . . . . ? O3 Zr1 S4 N4 79.19(9) . . . . ? O1 Zr1 S4 N4 -102.37(9) . . . . ? O7 Zr1 S4 N4 175.95(12) . . . . ? O5 Zr1 S4 N4 27.17(12) . . . . ? S2 Zr1 S4 N4 109.00(9) . . . . ? S1 Zr1 S4 N4 -116.26(9) . . . . ? S3 Zr1 S4 N4 -9.84(9) . . . . ? N1 Zr1 S4 C62 -45.45(10) . . . . ? N3 Zr1 S4 C62 66.75(9) . . . . ? N2 Zr1 S4 C62 -127.69(9) . . . . ? N4 Zr1 S4 C62 92.24(12) . . . . ? O3 Zr1 S4 C62 171.43(9) . . . . ? O1 Zr1 S4 C62 -10.13(9) . . . . ? O7 Zr1 S4 C62 -91.81(11) . . . . ? O5 Zr1 S4 C62 119.40(11) . . . . ? S2 Zr1 S4 C62 -158.76(8) . . . . ? S1 Zr1 S4 C62 -24.02(8) . . . . ? S3 Zr1 S4 C62 82.40(8) . . . . ? O2 S1 N1 C2 -47.5(2) . . . . ? O1 S1 N1 C2 -172.74(17) . . . . ? C21 S1 N1 C2 74.94(18) . . . . ? Zr1 S1 N1 C2 -168.7(2) . . . . ? O2 S1 N1 Zr1 121.19(9) . . . . ? O1 S1 N1 Zr1 -4.08(9) . . . . ? C21 S1 N1 Zr1 -116.40(9) . . . . ? N3 Zr1 N1 C2 96.13(17) . . . . ? N2 Zr1 N1 C2 -53.86(17) . . . . ? N4 Zr1 N1 C2 171.12(15) . . . . ? O3 Zr1 N1 C2 -21.0(2) . . . . ? O1 Zr1 N1 C2 170.93(19) . . . . ? O7 Zr1 N1 C2 -127.35(17) . . . . ? O5 Zr1 N1 C2 37.96(17) . . . . ? S2 Zr1 N1 C2 -41.44(18) . . . . ? S1 Zr1 N1 C2 168.0(2) . . . . ? S4 Zr1 N1 C2 -149.38(15) . . . . ? S3 Zr1 N1 C2 66.89(17) . . . . ? N3 Zr1 N1 S1 -71.84(9) . . . . ? N2 Zr1 N1 S1 138.17(10) . . . . ? N4 Zr1 N1 S1 3.15(17) . . . . ? O3 Zr1 N1 S1 171.05(6) . . . . ? O1 Zr1 N1 S1 2.96(7) . . . . ? O7 Zr1 N1 S1 64.68(9) . . . . ? O5 Zr1 N1 S1 -130.01(9) . . . . ? S2 Zr1 N1 S1 150.59(7) . . . . ? S4 Zr1 N1 S1 42.65(10) . . . . ? S3 Zr1 N1 S1 -101.08(8) . . . . ? O4 S2 N2 C12 -44.2(2) . . . . ? O3 S2 N2 C12 -167.77(16) . . . . ? C28 S2 N2 C12 76.38(18) . . . . ? Zr1 S2 N2 C12 -160.9(2) . . . . ? O4 S2 N2 Zr1 116.72(9) . . . . ? O3 S2 N2 Zr1 -6.88(9) . . . . ? C28 S2 N2 Zr1 -122.72(9) . . . . ? N1 Zr1 N2 C12 -44.59(17) . . . . ? N3 Zr1 N2 C12 -126.74(18) . . . . ? N4 Zr1 N2 C12 106.66(18) . . . . ? O3 Zr1 N2 C12 163.5(2) . . . . ? O1 Zr1 N2 C12 0.8(2) . . . . ? O7 Zr1 N2 C12 64.91(18) . . . . ? O5 Zr1 N2 C12 -124.00(18) . . . . ? S2 Zr1 N2 C12 158.4(2) . . . . ? S1 Zr1 N2 C12 -23.76(18) . . . . ? S4 Zr1 N2 C12 82.29(18) . . . . ? S3 Zr1 N2 C12 -123.06(17) . . . . ? N1 Zr1 N2 S2 157.02(9) . . . . ? N3 Zr1 N2 S2 74.87(15) . . . . ? N4 Zr1 N2 S2 -51.73(11) . . . . ? O3 Zr1 N2 S2 5.07(7) . . . . ? O1 Zr1 N2 S2 -157.61(7) . . . . ? O7 Zr1 N2 S2 -93.47(8) . . . . ? O5 Zr1 N2 S2 77.62(8) . . . . ? S1 Zr1 N2 S2 177.86(7) . . . . ? S4 Zr1 N2 S2 -76.10(8) . . . . ? S3 Zr1 N2 S2 78.56(8) . . . . ? O6 S3 N3 C36 -48.9(2) . . . . ? O5 S3 N3 C36 -174.31(17) . . . . ? C55 S3 N3 C36 73.40(19) . . . . ? Zr1 S3 N3 C36 -170.0(2) . . . . ? O6 S3 N3 Zr1 121.16(9) . . . . ? O5 S3 N3 Zr1 -4.27(9) . . . . ? C55 S3 N3 Zr1 -116.55(9) . . . . ? N1 Zr1 N3 C36 99.52(17) . . . . ? N2 Zr1 N3 C36 175.74(15) . . . . ? N4 Zr1 N3 C36 -46.84(17) . . . . ? O3 Zr1 N3 C36 -125.25(17) . . . . ? O1 Zr1 N3 C36 40.17(17) . . . . ? O7 Zr1 N3 C36 -19.4(2) . . . . ? O5 Zr1 N3 C36 172.59(19) . . . . ? S2 Zr1 N3 C36 -140.96(15) . . . . ? S1 Zr1 N3 C36 69.56(17) . . . . ? S4 Zr1 N3 C36 -33.36(18) . . . . ? S3 Zr1 N3 C36 169.5(2) . . . . ? N1 Zr1 N3 S3 -69.99(9) . . . . ? N2 Zr1 N3 S3 6.22(17) . . . . ? N4 Zr1 N3 S3 143.64(9) . . . . ? O3 Zr1 N3 S3 65.24(9) . . . . ? O1 Zr1 N3 S3 -129.34(9) . . . . ? O7 Zr1 N3 S3 171.07(6) . . . . ? O5 Zr1 N3 S3 3.08(7) . . . . ? S2 Zr1 N3 S3 49.53(11) . . . . ? S1 Zr1 N3 S3 -99.96(8) . . . . ? S4 Zr1 N3 S3 157.13(7) . . . . ? O8 S4 N4 C46 -21.6(2) . . . . ? O7 S4 N4 C46 -147.91(17) . . . . ? C62 S4 N4 C46 100.90(18) . . . . ? Zr1 S4 N4 C46 -151.1(2) . . . . ? O8 S4 N4 Zr1 129.45(9) . . . . ? O7 S4 N4 Zr1 3.18(9) . . . . ? C62 S4 N4 Zr1 -108.01(9) . . . . ? N1 Zr1 N4 C46 -136.23(15) . . . . ? N3 Zr1 N4 C46 -54.20(16) . . . . ? N2 Zr1 N4 C46 101.24(16) . . . . ? O3 Zr1 N4 C46 53.08(16) . . . . ? O1 Zr1 N4 C46 -136.06(16) . . . . ? O7 Zr1 N4 C46 149.19(18) . . . . ? O5 Zr1 N4 C46 -13.57(18) . . . . ? S2 Zr1 N4 C46 75.92(16) . . . . ? S1 Zr1 N4 C46 -134.41(15) . . . . ? S4 Zr1 N4 C46 151.5(2) . . . . ? S3 Zr1 N4 C46 -35.97(16) . . . . ? N1 Zr1 N4 S4 72.27(14) . . . . ? N3 Zr1 N4 S4 154.30(9) . . . . ? N2 Zr1 N4 S4 -50.26(11) . . . . ? O3 Zr1 N4 S4 -98.42(8) . . . . ? O1 Zr1 N4 S4 72.45(8) . . . . ? O7 Zr1 N4 S4 -2.30(7) . . . . ? O5 Zr1 N4 S4 -165.07(6) . . . . ? S2 Zr1 N4 S4 -75.57(8) . . . . ? S1 Zr1 N4 S4 74.10(8) . . . . ? S3 Zr1 N4 S4 172.53(7) . . . . ? O2 S1 O1 Zr1 -121.76(8) . . . . ? N1 S1 O1 Zr1 3.79(8) . . . . ? C21 S1 O1 Zr1 114.70(9) . . . . ? N1 Zr1 O1 S1 -3.11(7) . . . . ? N3 Zr1 O1 S1 101.54(8) . . . . ? N2 Zr1 O1 S1 -54.78(9) . . . . ? N4 Zr1 O1 S1 177.00(8) . . . . ? O3 Zr1 O1 S1 -146.21(16) . . . . ? O7 Zr1 O1 S1 -121.23(8) . . . . ? O5 Zr1 O1 S1 53.28(9) . . . . ? S2 Zr1 O1 S1 -76.88(10) . . . . ? S4 Zr1 O1 S1 -152.13(7) . . . . ? S3 Zr1 O1 S1 77.42(7) . . . . ? O4 S2 O3 Zr1 -119.52(9) . . . . ? N2 S2 O3 Zr1 6.65(9) . . . . ? C28 S2 O3 Zr1 116.91(10) . . . . ? N1 Zr1 O3 S2 -41.91(11) . . . . ? N3 Zr1 O3 S2 -156.34(7) . . . . ? N2 Zr1 O3 S2 -5.33(7) . . . . ? N4 Zr1 O3 S2 131.37(8) . . . . ? O1 Zr1 O3 S2 94.4(2) . . . . ? O7 Zr1 O3 S2 70.46(8) . . . . ? O5 Zr1 O3 S2 -102.98(8) . . . . ? S1 Zr1 O3 S2 -27.48(17) . . . . ? S4 Zr1 O3 S2 100.20(7) . . . . ? S3 Zr1 O3 S2 -128.22(7) . . . . ? O6 S3 O5 Zr1 -121.17(8) . . . . ? N3 S3 O5 Zr1 3.96(8) . . . . ? C55 S3 O5 Zr1 116.18(9) . . . . ? N1 Zr1 O5 S3 102.45(8) . . . . ? N3 Zr1 O5 S3 -3.23(7) . . . . ? N2 Zr1 O5 S3 178.34(8) . . . . ? N4 Zr1 O5 S3 -49.26(10) . . . . ? O3 Zr1 O5 S3 -120.50(8) . . . . ? O1 Zr1 O5 S3 54.27(9) . . . . ? O7 Zr1 O5 S3 -146.29(16) . . . . ? S2 Zr1 O5 S3 -150.17(7) . . . . ? S1 Zr1 O5 S3 78.32(7) . . . . ? S4 Zr1 O5 S3 -65.54(11) . . . . ? O8 S4 O7 Zr1 -129.80(8) . . . . ? N4 S4 O7 Zr1 -3.06(9) . . . . ? C62 S4 O7 Zr1 109.04(9) . . . . ? N1 Zr1 O7 S4 -143.95(7) . . . . ? N3 Zr1 O7 S4 -28.00(11) . . . . ? N2 Zr1 O7 S4 144.34(8) . . . . ? N4 Zr1 O7 S4 2.41(7) . . . . ? O3 Zr1 O7 S4 83.35(7) . . . . ? O1 Zr1 O7 S4 -90.26(8) . . . . ? O5 Zr1 O7 S4 108.12(18) . . . . ? S2 Zr1 O7 S4 112.01(7) . . . . ? S1 Zr1 O7 S4 -115.60(7) . . . . ? S3 Zr1 O7 S4 -13.54(17) . . . . ? C6 C1 C2 C3 6.5(3) . . . . ? C11 C1 C2 C3 -173.07(18) . . . . ? C6 C1 C2 N1 -166.99(18) . . . . ? C11 C1 C2 N1 13.4(3) . . . . ? S1 N1 C2 C1 -118.96(19) . . . . ? Zr1 N1 C2 C1 75.7(2) . . . . ? S1 N1 C2 C3 67.3(2) . . . . ? Zr1 N1 C2 C3 -98.0(2) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? N1 C2 C3 C4 171.59(19) . . . . ? C2 C3 C4 C5 -3.8(3) . . . . ? C3 C4 C5 C10 -172.9(2) . . . . ? C3 C4 C5 C6 4.8(3) . . . . ? C10 C5 C6 C7 0.1(3) . . . . ? C4 C5 C6 C7 -177.6(2) . . . . ? C10 C5 C6 C1 177.7(2) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C2 C1 C6 C7 172.0(2) . . . . ? C11 C1 C6 C7 -8.4(3) . . . . ? C2 C1 C6 C5 -5.4(3) . . . . ? C11 C1 C6 C5 174.15(18) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C1 C6 C7 C8 -177.2(2) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C5 1.0(4) . . . . ? C4 C5 C10 C9 176.9(2) . . . . ? C6 C5 C10 C9 -0.8(3) . . . . ? C2 C1 C11 C12 -63.1(3) . . . . ? C6 C1 C11 C12 117.4(2) . . . . ? C2 C1 C11 C16 115.0(2) . . . . ? C6 C1 C11 C16 -64.5(3) . . . . ? C16 C11 C12 C13 3.7(3) . . . . ? C1 C11 C12 C13 -178.18(19) . . . . ? C16 C11 C12 N2 -170.98(17) . . . . ? C1 C11 C12 N2 7.2(3) . . . . ? S2 N2 C12 C11 -132.14(18) . . . . ? Zr1 N2 C12 C11 73.8(2) . . . . ? S2 N2 C12 C13 53.1(2) . . . . ? Zr1 N2 C12 C13 -101.0(2) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? N2 C12 C13 C14 174.88(18) . . . . ? C12 C13 C14 C15 -3.0(3) . . . . ? C13 C14 C15 C20 -176.4(2) . . . . ? C13 C14 C15 C16 1.8(3) . . . . ? C20 C15 C16 C17 2.6(3) . . . . ? C14 C15 C16 C17 -175.6(2) . . . . ? C20 C15 C16 C11 -179.63(19) . . . . ? C14 C15 C16 C11 2.2(3) . . . . ? C12 C11 C16 C17 172.88(19) . . . . ? C1 C11 C16 C17 -5.3(3) . . . . ? C12 C11 C16 C15 -4.8(3) . . . . ? C1 C11 C16 C15 176.99(18) . . . . ? C15 C16 C17 C18 -1.4(3) . . . . ? C11 C16 C17 C18 -179.1(2) . . . . ? C16 C17 C18 C19 -0.9(4) . . . . ? C17 C18 C19 C20 2.1(3) . . . . ? C18 C19 C20 C15 -0.9(3) . . . . ? C14 C15 C20 C19 176.7(2) . . . . ? C16 C15 C20 C19 -1.5(3) . . . . ? O2 S1 C21 C26 -168.88(16) . . . . ? O1 S1 C21 C26 -40.55(19) . . . . ? N1 S1 C21 C26 63.48(19) . . . . ? Zr1 S1 C21 C26 14.7(2) . . . . ? O2 S1 C21 C22 18.1(2) . . . . ? O1 S1 C21 C22 146.48(17) . . . . ? N1 S1 C21 C22 -109.49(18) . . . . ? Zr1 S1 C21 C22 -158.29(15) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? S1 C21 C22 C23 172.92(17) . . . . ? C21 C22 C23 C24 -0.7(3) . . . . ? C22 C23 C24 C25 0.9(3) . . . . ? C22 C23 C24 C27 -178.1(2) . . . . ? C23 C24 C25 C26 -0.7(3) . . . . ? C27 C24 C25 C26 178.4(2) . . . . ? C24 C25 C26 C21 0.2(3) . . . . ? C22 C21 C26 C25 0.1(3) . . . . ? S1 C21 C26 C25 -172.71(16) . . . . ? O4 S2 C28 C33 5.9(2) . . . . ? O3 S2 C28 C33 133.4(2) . . . . ? N2 S2 C28 C33 -121.5(2) . . . . ? Zr1 S2 C28 C33 -170.67(16) . . . . ? O4 S2 C28 C29 173.5(2) . . . . ? O3 S2 C28 C29 -59.0(3) . . . . ? N2 S2 C28 C29 46.1(3) . . . . ? Zr1 S2 C28 C29 -3.1(3) . . . . ? C33 C28 C29 C30 1.7(5) . . . . ? S2 C28 C29 C30 -165.8(2) . . . . ? C28 C29 C30 C31 -0.4(5) . . . . ? C29 C30 C31 C32 -0.9(5) . . . . ? C29 C30 C31 C34 175.3(3) . . . . ? C30 C31 C32 C33 0.9(5) . . . . ? C34 C31 C32 C33 -175.2(3) . . . . ? C29 C28 C33 C32 -1.7(4) . . . . ? S2 C28 C33 C32 165.8(2) . . . . ? C31 C32 C33 C28 0.4(4) . . . . ? C40 C35 C36 C37 3.8(3) . . . . ? C45 C35 C36 C37 178.30(19) . . . . ? C40 C35 C36 N3 -168.75(18) . . . . ? C45 C35 C36 N3 5.7(3) . . . . ? S3 N3 C36 C35 -113.3(2) . . . . ? Zr1 N3 C36 C35 79.4(2) . . . . ? S3 N3 C36 C37 73.8(2) . . . . ? Zr1 N3 C36 C37 -93.4(2) . . . . ? C35 C36 C37 C38 -4.5(3) . . . . ? N3 C36 C37 C38 168.14(19) . . . . ? C36 C37 C38 C39 0.6(3) . . . . ? C37 C38 C39 C44 -173.0(2) . . . . ? C37 C38 C39 C40 3.7(3) . . . . ? C44 C39 C40 C41 -3.1(3) . . . . ? C38 C39 C40 C41 -179.9(2) . . . . ? C44 C39 C40 C35 172.5(2) . . . . ? C38 C39 C40 C35 -4.3(3) . . . . ? C36 C35 C40 C41 176.0(2) . . . . ? C45 C35 C40 C41 1.6(3) . . . . ? C36 C35 C40 C39 0.6(3) . . . . ? C45 C35 C40 C39 -173.90(19) . . . . ? C39 C40 C41 C42 3.1(3) . . . . ? C35 C40 C41 C42 -172.4(2) . . . . ? C40 C41 C42 C43 -0.3(4) . . . . ? C41 C42 C43 C44 -2.4(4) . . . . ? C42 C43 C44 C39 2.3(4) . . . . ? C40 C39 C44 C43 0.5(3) . . . . ? C38 C39 C44 C43 177.2(2) . . . . ? C36 C35 C45 C46 -62.9(3) . . . . ? C40 C35 C45 C46 111.5(2) . . . . ? C36 C35 C45 C50 115.8(2) . . . . ? C40 C35 C45 C50 -69.8(3) . . . . ? C50 C45 C46 C47 3.2(3) . . . . ? C35 C45 C46 C47 -178.08(19) . . . . ? C50 C45 C46 N4 -169.70(18) . . . . ? C35 C45 C46 N4 9.0(3) . . . . ? S4 N4 C46 C45 -135.06(18) . . . . ? Zr1 N4 C46 C45 80.8(2) . . . . ? S4 N4 C46 C47 51.9(3) . . . . ? Zr1 N4 C46 C47 -92.2(2) . . . . ? C45 C46 C47 C48 0.1(3) . . . . ? N4 C46 C47 C48 173.07(19) . . . . ? C46 C47 C48 C49 -2.1(3) . . . . ? C47 C48 C49 C54 -177.1(2) . . . . ? C47 C48 C49 C50 0.7(3) . . . . ? C48 C49 C50 C51 -175.42(19) . . . . ? C54 C49 C50 C51 2.4(3) . . . . ? C48 C49 C50 C45 2.7(3) . . . . ? C54 C49 C50 C45 -179.46(19) . . . . ? C46 C45 C50 C51 173.4(2) . . . . ? C35 C45 C50 C51 -5.3(3) . . . . ? C46 C45 C50 C49 -4.6(3) . . . . ? C35 C45 C50 C49 176.71(19) . . . . ? C49 C50 C51 C52 -1.2(3) . . . . ? C45 C50 C51 C52 -179.3(2) . . . . ? C50 C51 C52 C53 -1.6(3) . . . . ? C51 C52 C53 C54 3.3(4) . . . . ? C52 C53 C54 C49 -2.1(4) . . . . ? C48 C49 C54 C53 177.0(2) . . . . ? C50 C49 C54 C53 -0.8(3) . . . . ? O6 S3 C55 C60 24.7(2) . . . . ? O5 S3 C55 C60 152.70(17) . . . . ? N3 S3 C55 C60 -102.73(18) . . . . ? Zr1 S3 C55 C60 -152.17(14) . . . . ? O6 S3 C55 C56 -160.43(17) . . . . ? O5 S3 C55 C56 -32.4(2) . . . . ? N3 S3 C55 C56 72.14(19) . . . . ? Zr1 S3 C55 C56 22.7(2) . . . . ? C60 C55 C56 C57 -0.7(3) . . . . ? S3 C55 C56 C57 -175.38(17) . . . . ? C55 C56 C57 C58 0.9(3) . . . . ? C56 C57 C58 C59 -0.2(4) . . . . ? C56 C57 C58 C61 179.8(2) . . . . ? C57 C58 C59 C60 -0.8(3) . . . . ? C61 C58 C59 C60 179.3(2) . . . . ? C56 C55 C60 C59 -0.2(3) . . . . ? S3 C55 C60 C59 174.57(17) . . . . ? C58 C59 C60 C55 1.0(3) . . . . ? O8 S4 C62 C67 82.0(2) . . . . ? O7 S4 C62 C67 -151.70(18) . . . . ? N4 S4 C62 C67 -45.9(2) . . . . ? Zr1 S4 C62 C67 -97.54(18) . . . . ? O8 S4 C62 C63 -96.42(19) . . . . ? O7 S4 C62 C63 29.9(2) . . . . ? N4 S4 C62 C63 135.69(18) . . . . ? Zr1 S4 C62 C63 84.04(18) . . . . ? C67 C62 C63 C64 0.8(3) . . . . ? S4 C62 C63 C64 179.14(17) . . . . ? C62 C63 C64 C65 0.2(3) . . . . ? C63 C64 C65 C66 -1.1(4) . . . . ? C63 C64 C65 C68 176.9(2) . . . . ? C64 C65 C66 C67 1.1(4) . . . . ? C68 C65 C66 C67 -176.9(2) . . . . ? C63 C62 C67 C66 -0.7(4) . . . . ? S4 C62 C67 C66 -179.16(19) . . . . ? C65 C66 C67 C62 -0.2(4) . . . . ? C75 C70 C71 C72 0.0 . . . . ? C69 C70 C71 C72 174.9(6) . . . . ? C70 C71 C72 C73 0.0 . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C70 0.0 . . . . ? C71 C70 C75 C74 0.0 . . . . ? C69 C70 C75 C74 -175.0(6) . . . . ? C82 C77 C78 C79 0.0 . . . . ? C76 C77 C78 C79 -180.0(9) . . . . ? C77 C78 C79 C80 0.0 . . . . ? C78 C79 C80 C81 0.0 . . . . ? C79 C80 C81 C82 0.0 . . . . ? C80 C81 C82 C77 0.0 . . . . ? C78 C77 C82 C81 0.0 . . . . ? C76 C77 C82 C81 180.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.300 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.059 # Attachment 'compound_18.cif' data_compound18 _database_code_depnum_ccdc_archive 'CCDC 742604' #TrackingRef 'compound_18.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C101 H108 N4 O4 Zr' _chemical_formula_sum 'C101 H108 N4 O4 Zr' _chemical_formula_weight 1533.13 _chemical_absolute_configuration rmad 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 'P 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.2722(4) _cell_length_b 30.1590(11) _cell_length_c 12.0617(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.946(2) _cell_angle_gamma 90.00 _cell_volume 4099.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10650 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9665 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32274 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.83 _reflns_number_total 17782 _reflns_number_gt 16985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0365P)^2^+0.5280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(14) _refine_ls_number_reflns 17782 _refine_ls_number_parameters 1066 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.615679(13) 0.656860(6) 0.475413(12) 0.01596(4) Uani 1 1 d . . . N1 N 0.54195(13) 0.62396(5) 0.31940(12) 0.0158(3) Uani 1 1 d . . . N2 N 0.58138(13) 0.58591(6) 0.52653(12) 0.0188(3) Uani 1 1 d . . . N3 N 0.64532(14) 0.72107(6) 0.57138(13) 0.0184(3) Uani 1 1 d . . . N4 N 0.69134(13) 0.70474(5) 0.34958(12) 0.0152(3) Uani 1 1 d . . . O1 O 0.44106(11) 0.67527(5) 0.40398(10) 0.0195(3) Uani 1 1 d . . . O2 O 0.71973(12) 0.62399(5) 0.61506(11) 0.0230(3) Uani 1 1 d . . . O3 O 0.50837(11) 0.67386(5) 0.62398(10) 0.0203(3) Uani 1 1 d . . . O4 O 0.79315(11) 0.64734(4) 0.40819(11) 0.0209(3) Uani 1 1 d . . . C1 C 0.54110(15) 0.54225(6) 0.31443(15) 0.0174(4) Uani 1 1 d . . . C2 C 0.57205(15) 0.58321(6) 0.26798(15) 0.0167(3) Uani 1 1 d . . . C3 C 0.65238(16) 0.58471(7) 0.18122(15) 0.0202(4) Uani 1 1 d . . . H3 H 0.6715 0.6124 0.1482 0.024 Uiso 1 1 calc R . . C4 C 0.70453(16) 0.54610(7) 0.14288(16) 0.0226(4) Uani 1 1 d . . . H4 H 0.7566 0.5475 0.0819 0.027 Uiso 1 1 calc R . . C5 C 0.68170(17) 0.50531(7) 0.19246(16) 0.0224(4) Uani 1 1 d . . . C6 C 0.59833(17) 0.50323(7) 0.27810(16) 0.0211(4) Uani 1 1 d . . . C7 C 0.57991(19) 0.46016(7) 0.34055(19) 0.0278(4) Uani 1 1 d . . . H7A H 0.4936 0.4544 0.3444 0.033 Uiso 1 1 calc R . . H7B H 0.6101 0.4641 0.4175 0.033 Uiso 1 1 calc R . . C8 C 0.6391(2) 0.41935(8) 0.2914(2) 0.0389(5) Uani 1 1 d . . . H8A H 0.6466 0.3961 0.3491 0.047 Uiso 1 1 calc R . . H8B H 0.5887 0.4075 0.2303 0.047 Uiso 1 1 calc R . . C9 C 0.7611(2) 0.43036(9) 0.2476(2) 0.0376(5) Uani 1 1 d . . . H9A H 0.8121 0.4420 0.3086 0.045 Uiso 1 1 calc R . . H9B H 0.7986 0.4032 0.2184 0.045 Uiso 1 1 calc R . . C10 C 0.7502(2) 0.46464(8) 0.15635(19) 0.0321(5) Uani 1 1 d . . . H10A H 0.7094 0.4512 0.0912 0.038 Uiso 1 1 calc R . . H10B H 0.8305 0.4737 0.1335 0.038 Uiso 1 1 calc R . . C11 C 0.45641(16) 0.53859(6) 0.40904(15) 0.0180(4) Uani 1 1 d . . . C12 C 0.48953(16) 0.55416(6) 0.51477(15) 0.0186(4) Uani 1 1 d . . . C13 C 0.42057(18) 0.54302(7) 0.60681(17) 0.0241(4) Uani 1 1 d . . . H13 H 0.4441 0.5524 0.6791 0.029 Uiso 1 1 calc R . . C14 C 0.31823(18) 0.51826(7) 0.59136(18) 0.0281(4) Uani 1 1 d . . . H14 H 0.2745 0.5093 0.6542 0.034 Uiso 1 1 calc R . . C15 C 0.27780(18) 0.50615(7) 0.48601(18) 0.0265(4) Uani 1 1 d . . . C16 C 0.34622(16) 0.51640(7) 0.39348(17) 0.0219(4) Uani 1 1 d . . . C17 C 0.30338(18) 0.50521(8) 0.27713(18) 0.0283(4) Uani 1 1 d . . . H17A H 0.3543 0.4815 0.2471 0.034 Uiso 1 1 calc R . . H17B H 0.3128 0.5317 0.2295 0.034 Uiso 1 1 calc R . . C18 C 0.1737(2) 0.48998(9) 0.2704(2) 0.0394(6) Uani 1 1 d . . . H18A H 0.1210 0.5162 0.2726 0.047 Uiso 1 1 calc R . . H18B H 0.1591 0.4746 0.1990 0.047 Uiso 1 1 calc R . . C19 C 0.1436(2) 0.45904(9) 0.3650(2) 0.0436(6) Uani 1 1 d . . . H19A H 0.0605 0.4488 0.3564 0.052 Uiso 1 1 calc R . . H19B H 0.1960 0.4327 0.3632 0.052 Uiso 1 1 calc R . . C20 C 0.1591(2) 0.48247(8) 0.4739(2) 0.0376(6) Uani 1 1 d . . . H20A H 0.1518 0.4606 0.5346 0.045 Uiso 1 1 calc R . . H20B H 0.0944 0.5044 0.4817 0.045 Uiso 1 1 calc R . . C21 C 0.43873(15) 0.64320(6) 0.33126(15) 0.0169(4) Uani 1 1 d . . . C22 C 0.32423(15) 0.63178(6) 0.27384(15) 0.0182(4) Uani 1 1 d . . . C23 C 0.22512(16) 0.62152(7) 0.33949(17) 0.0215(4) Uani 1 1 d . . . C24 C 0.11856(17) 0.61068(7) 0.28559(19) 0.0272(4) Uani 1 1 d . . . H24 H 0.0519 0.6032 0.3289 0.033 Uiso 1 1 calc R . . C25 C 0.10647(17) 0.61047(7) 0.17009(19) 0.0289(5) Uani 1 1 d . . . C26 C 0.20427(17) 0.62235(7) 0.10788(18) 0.0259(4) Uani 1 1 d . . . H26 H 0.1965 0.6235 0.0294 0.031 Uiso 1 1 calc R . . C27 C 0.31358(16) 0.63270(7) 0.15760(16) 0.0213(4) Uani 1 1 d . . . C28 C 0.23141(18) 0.62232(8) 0.46442(17) 0.0265(4) Uani 1 1 d . . . H28A H 0.2348 0.6531 0.4902 0.040 Uiso 1 1 calc R . . H28B H 0.3027 0.6065 0.4901 0.040 Uiso 1 1 calc R . . H28C H 0.1609 0.6079 0.4941 0.040 Uiso 1 1 calc R . . C29 C -0.0095(2) 0.59757(10) 0.1152(2) 0.0444(6) Uani 1 1 d . . . H29A H -0.0110 0.5654 0.1033 0.067 Uiso 1 1 calc R . . H29B H -0.0176 0.6128 0.0437 0.067 Uiso 1 1 calc R . . H29C H -0.0752 0.6061 0.1629 0.067 Uiso 1 1 calc R . . C30 C 0.41421(18) 0.64648(7) 0.08338(16) 0.0288(5) Uani 1 1 d . . . H30A H 0.4527 0.6200 0.0536 0.043 Uiso 1 1 calc R . . H30B H 0.4723 0.6638 0.1264 0.043 Uiso 1 1 calc R . . H30C H 0.3828 0.6646 0.0221 0.043 Uiso 1 1 calc R . . C31 C 0.66578(17) 0.58668(7) 0.60384(16) 0.0210(4) Uani 1 1 d . . . C32 C 0.70435(17) 0.54701(7) 0.66953(16) 0.0214(4) Uani 1 1 d . . . C33 C 0.77323(16) 0.51466(7) 0.61697(15) 0.0218(4) Uani 1 1 d . . . C34 C 0.80593(17) 0.47701(7) 0.67582(17) 0.0263(4) Uani 1 1 d . . . H34 H 0.8525 0.4551 0.6406 0.032 Uiso 1 1 calc R . . C35 C 0.77222(19) 0.47042(7) 0.78570(17) 0.0271(4) Uani 1 1 d . . . C36 C 0.70877(19) 0.50387(7) 0.83737(17) 0.0267(4) Uani 1 1 d . . . H36 H 0.6884 0.5004 0.9130 0.032 Uiso 1 1 calc R . . C37 C 0.67400(19) 0.54251(7) 0.78134(16) 0.0252(4) Uani 1 1 d . . . C38 C 0.81638(19) 0.52216(9) 0.49963(17) 0.0286(5) Uani 1 1 d . . . H38A H 0.8625 0.4964 0.4759 0.043 Uiso 1 1 calc R . . H38B H 0.8665 0.5487 0.4980 0.043 Uiso 1 1 calc R . . H38C H 0.7480 0.5262 0.4494 0.043 Uiso 1 1 calc R . . C39 C 0.8066(2) 0.42886(8) 0.8479(2) 0.0370(5) Uani 1 1 d . . . H39A H 0.8705 0.4356 0.9013 0.056 Uiso 1 1 calc R . . H39B H 0.8340 0.4064 0.7954 0.056 Uiso 1 1 calc R . . H39C H 0.7377 0.4175 0.8874 0.056 Uiso 1 1 calc R . . C40 C 0.6080(2) 0.57848(9) 0.84221(18) 0.0379(6) Uani 1 1 d . . . H40A H 0.5439 0.5652 0.8849 0.057 Uiso 1 1 calc R . . H40B H 0.5744 0.5996 0.7885 0.057 Uiso 1 1 calc R . . H40C H 0.6629 0.5940 0.8927 0.057 Uiso 1 1 calc R . . C41 C 0.76493(16) 0.78052(6) 0.49107(15) 0.0174(4) Uani 1 1 d . . . C42 C 0.73220(15) 0.75506(6) 0.58332(14) 0.0177(4) Uani 1 1 d . . . C43 C 0.79818(17) 0.75851(7) 0.68226(15) 0.0225(4) Uani 1 1 d . . . H43 H 0.7748 0.7422 0.7457 0.027 Uiso 1 1 calc R . . C44 C 0.89736(17) 0.78557(8) 0.68822(17) 0.0257(4) Uani 1 1 d . . . H44 H 0.9388 0.7889 0.7570 0.031 Uiso 1 1 calc R . . C45 C 0.93758(17) 0.80814(7) 0.59478(17) 0.0236(4) Uani 1 1 d . A . C46 C 0.87147(16) 0.80544(7) 0.49521(16) 0.0204(4) Uani 1 1 d . A . C47 C 0.91655(17) 0.82721(7) 0.39034(17) 0.0242(4) Uani 1 1 d D . . H47A H 0.8501 0.8393 0.3497 0.029 Uiso 0.677(8) 1 d PR A 1 H47B H 0.9521 0.8049 0.3449 0.029 Uiso 0.677(8) 1 d PR A 1 H47C H 0.8689 0.8528 0.3733 0.029 Uiso 0.323(8) 1 d PR A 2 H47D H 0.9087 0.8067 0.3297 0.029 Uiso 0.323(8) 1 d PR A 2 C48 C 1.0071(3) 0.86433(14) 0.4116(3) 0.0302(10) Uani 0.677(8) 1 d PD A 1 H48A H 1.0424 0.8738 0.3408 0.036 Uiso 0.677(8) 1 calc PR A 1 H48B H 0.9677 0.8902 0.4453 0.036 Uiso 0.677(8) 1 calc PR A 1 C49 C 1.1039(3) 0.84653(17) 0.4901(4) 0.0336(10) Uani 0.677(8) 1 d PD A 1 H49A H 1.1666 0.8692 0.5000 0.040 Uiso 0.677(8) 1 calc PR A 1 H49B H 1.1404 0.8199 0.4571 0.040 Uiso 0.677(8) 1 calc PR A 1 C48' C 1.0495(6) 0.8412(3) 0.4033(5) 0.026(2) Uani 0.323(8) 1 d PD A 2 H48C H 1.1001 0.8144 0.4017 0.031 Uiso 0.323(8) 1 calc PR A 2 H48D H 1.0714 0.8602 0.3399 0.031 Uiso 0.323(8) 1 calc PR A 2 C49' C 1.0732(9) 0.8663(3) 0.5115(5) 0.033(2) Uani 0.323(8) 1 d PD A 2 H49C H 1.1560 0.8773 0.5145 0.040 Uiso 0.323(8) 1 calc PR A 2 H49D H 1.0191 0.8920 0.5171 0.040 Uiso 0.323(8) 1 calc PR A 2 C50 C 1.05230(19) 0.83455(8) 0.60399(19) 0.0328(5) Uani 1 1 d D . . H50A H 1.1101 0.8174 0.6446 0.039 Uiso 0.677(8) 1 d PR A 1 H50B H 1.0380 0.8612 0.6451 0.039 Uiso 0.677(8) 1 d PR A 1 H50C H 1.1177 0.8142 0.6064 0.039 Uiso 0.323(8) 1 d PR A 2 H50D H 1.0526 0.8505 0.6728 0.039 Uiso 0.323(8) 1 d PR A 2 C51 C 0.68400(15) 0.78458(6) 0.39232(14) 0.0166(3) Uani 1 1 d . . . C52 C 0.65949(15) 0.74884(6) 0.32122(14) 0.0159(3) Uani 1 1 d . . . C53 C 0.58430(16) 0.75495(7) 0.22878(15) 0.0202(4) Uani 1 1 d . . . H53 H 0.5682 0.7309 0.1799 0.024 Uiso 1 1 calc R . . C54 C 0.53360(17) 0.79590(7) 0.20873(16) 0.0230(4) Uani 1 1 d . . . H54 H 0.4857 0.8000 0.1440 0.028 Uiso 1 1 calc R . . C55 C 0.55107(17) 0.83152(7) 0.28133(16) 0.0223(4) Uani 1 1 d . B . C56 C 0.62660(16) 0.82596(7) 0.37334(15) 0.0195(4) Uani 1 1 d . B . C57 C 0.64042(19) 0.86343(7) 0.45759(17) 0.0254(4) Uani 1 1 d D . . H57A H 0.7173 0.8767 0.4497 0.030 Uiso 0.686(8) 1 d PR B 1 H57B H 0.6365 0.8512 0.5309 0.030 Uiso 0.686(8) 1 d PR B 1 H57C H 0.7228 0.8661 0.4780 0.030 Uiso 0.314(8) 1 d PR B 2 H57D H 0.5978 0.8558 0.5231 0.030 Uiso 0.314(8) 1 d PR B 2 C58 C 0.5466(4) 0.89937(13) 0.4446(3) 0.0318(10) Uani 0.686(8) 1 d PD B 1 H58A H 0.5697 0.9252 0.4907 0.038 Uiso 0.686(8) 1 calc PR B 1 H58B H 0.4701 0.8880 0.4722 0.038 Uiso 0.686(8) 1 calc PR B 1 C59 C 0.5298(4) 0.91435(12) 0.3244(3) 0.0351(10) Uani 0.686(8) 1 d PD B 1 H59A H 0.6063 0.9245 0.2942 0.042 Uiso 0.686(8) 1 calc PR B 1 H59B H 0.4724 0.9391 0.3198 0.042 Uiso 0.686(8) 1 calc PR B 1 C58' C 0.5976(8) 0.9081(2) 0.4150(7) 0.028(2) Uani 0.314(8) 1 d PD B 2 H58C H 0.6535 0.9194 0.3592 0.034 Uiso 0.314(8) 1 calc PR B 2 H58D H 0.5956 0.9295 0.4771 0.034 Uiso 0.314(8) 1 calc PR B 2 C59' C 0.4738(8) 0.9038(3) 0.3627(7) 0.037(2) Uani 0.314(8) 1 d PD B 2 H59C H 0.4429 0.9335 0.3420 0.045 Uiso 0.314(8) 1 calc PR B 2 H59D H 0.4188 0.8903 0.4162 0.045 Uiso 0.314(8) 1 calc PR B 2 C60 C 0.4830(2) 0.87421(8) 0.25824(19) 0.0318(5) Uani 1 1 d D . . H60A H 0.4012 0.8697 0.2758 0.038 Uiso 0.686(8) 1 d PR B 1 H60B H 0.4870 0.8808 0.1805 0.038 Uiso 0.686(8) 1 d PR B 1 H60C H 0.4047 0.8669 0.2317 0.038 Uiso 0.314(8) 1 d PR B 2 H60D H 0.5220 0.8906 0.2011 0.038 Uiso 0.314(8) 1 d PR B 2 C61 C 0.55794(16) 0.71197(6) 0.63920(14) 0.0181(4) Uani 1 1 d . . . C62 C 0.50545(15) 0.74317(6) 0.72123(15) 0.0175(4) Uani 1 1 d . . . C63 C 0.42470(16) 0.77522(7) 0.68134(15) 0.0197(4) Uani 1 1 d . . . C64 C 0.36829(16) 0.80226(7) 0.75739(16) 0.0220(4) Uani 1 1 d . . . H64 H 0.3143 0.8242 0.7312 0.026 Uiso 1 1 calc R . . C65 C 0.38900(17) 0.79797(7) 0.87153(16) 0.0244(4) Uani 1 1 d . . . C66 C 0.46726(18) 0.76533(7) 0.90858(16) 0.0239(4) Uani 1 1 d . . . H66 H 0.4809 0.7619 0.9860 0.029 Uiso 1 1 calc R . . C67 C 0.52635(16) 0.73746(7) 0.83531(15) 0.0203(4) Uani 1 1 d . . . C68 C 0.39641(18) 0.77919(8) 0.55915(17) 0.0280(5) Uani 1 1 d . . . H68A H 0.3282 0.7990 0.5482 0.042 Uiso 1 1 calc R . . H68B H 0.3774 0.7498 0.5289 0.042 Uiso 1 1 calc R . . H68C H 0.4652 0.7914 0.5209 0.042 Uiso 1 1 calc R . . C69 C 0.3257(2) 0.82830(9) 0.9514(2) 0.0389(6) Uani 1 1 d . . . H69A H 0.3045 0.8116 1.0178 0.058 Uiso 1 1 calc R . . H69B H 0.2536 0.8400 0.9156 0.058 Uiso 1 1 calc R . . H69C H 0.3781 0.8529 0.9723 0.058 Uiso 1 1 calc R . . C70 C 0.60910(19) 0.70202(8) 0.87951(16) 0.0278(4) Uani 1 1 d . . . H70A H 0.6436 0.6858 0.8174 0.042 Uiso 1 1 calc R . . H70B H 0.5648 0.6814 0.9260 0.042 Uiso 1 1 calc R . . H70C H 0.6727 0.7158 0.9238 0.042 Uiso 1 1 calc R . . C71 C 0.79626(15) 0.68558(6) 0.35817(14) 0.0172(3) Uani 1 1 d . . . C72 C 0.91177(15) 0.70325(6) 0.32016(15) 0.0186(4) Uani 1 1 d . . . C73 C 1.00553(16) 0.70793(7) 0.39865(16) 0.0210(4) Uani 1 1 d . . . C74 C 1.11374(17) 0.72458(7) 0.36197(18) 0.0254(4) Uani 1 1 d . . . H74 H 1.1767 0.7289 0.4142 0.030 Uiso 1 1 calc R . . C75 C 1.13218(17) 0.73508(8) 0.25093(19) 0.0290(5) Uani 1 1 d . . . C76 C 1.03958(17) 0.72881(7) 0.17498(17) 0.0259(4) Uani 1 1 d . . . H76 H 1.0521 0.7354 0.0990 0.031 Uiso 1 1 calc R . . C77 C 0.92864(16) 0.71313(7) 0.20711(16) 0.0213(4) Uani 1 1 d . . . C78 C 0.99389(17) 0.69468(8) 0.51801(16) 0.0261(4) Uani 1 1 d . . . H78A H 0.9899 0.6623 0.5234 0.039 Uiso 1 1 calc R . . H78B H 0.9214 0.7076 0.5479 0.039 Uiso 1 1 calc R . . H78C H 1.0628 0.7055 0.5606 0.039 Uiso 1 1 calc R . . C79 C 1.25154(19) 0.75254(9) 0.2159(2) 0.0416(6) Uani 1 1 d . . . H79A H 1.2506 0.7850 0.2173 0.062 Uiso 1 1 calc R . . H79B H 1.2681 0.7423 0.1406 0.062 Uiso 1 1 calc R . . H79C H 1.3133 0.7416 0.2670 0.062 Uiso 1 1 calc R . . C80 C 0.83412(18) 0.70461(8) 0.11951(16) 0.0264(4) Uani 1 1 d . . . H80A H 0.7887 0.7319 0.1061 0.040 Uiso 1 1 calc R . . H80B H 0.7807 0.6812 0.1450 0.040 Uiso 1 1 calc R . . H80C H 0.8716 0.6952 0.0506 0.040 Uiso 1 1 calc R . . C81 C 0.6810(2) 0.86111(10) 0.8053(2) 0.0449(6) Uani 1 1 d . . . H81A H 0.6574 0.8924 0.8043 0.067 Uiso 1 1 calc R . . H81B H 0.6120 0.8427 0.8220 0.067 Uiso 1 1 calc R . . H81C H 0.7118 0.8528 0.7327 0.067 Uiso 1 1 calc R . . C82 C 0.7764(2) 0.85406(8) 0.8935(2) 0.0333(5) Uani 1 1 d . . . C83 C 0.8894(2) 0.87240(9) 0.8810(2) 0.0370(5) Uani 1 1 d . . . H83 H 0.9059 0.8898 0.8174 0.044 Uiso 1 1 calc R . . C84 C 0.9771(2) 0.86547(10) 0.9605(2) 0.0468(7) Uani 1 1 d . . . H84 H 1.0540 0.8775 0.9504 0.056 Uiso 1 1 calc R . . C85 C 0.9530(3) 0.84083(10) 1.0557(3) 0.0554(8) Uani 1 1 d . . . H85 H 1.0129 0.8363 1.1109 0.067 Uiso 1 1 calc R . . C86 C 0.8415(3) 0.82321(10) 1.0685(3) 0.0568(8) Uani 1 1 d . . . H86 H 0.8238 0.8067 1.1332 0.068 Uiso 1 1 calc R . . C87 C 0.7553(3) 0.82944(9) 0.9877(2) 0.0438(6) Uani 1 1 d . . . H87 H 0.6793 0.8165 0.9971 0.053 Uiso 1 1 calc R . . C88 C 0.5572(3) 0.95980(15) 0.0026(3) 0.0638(11) Uani 0.814(4) 1 d PDU C 1 H88A H 0.4984 0.9572 0.0612 0.096 Uiso 0.814(4) 1 calc PR C 1 H88B H 0.5627 0.9316 -0.0373 0.096 Uiso 0.814(4) 1 calc PR C 1 H88C H 0.5330 0.9833 -0.0492 0.096 Uiso 0.814(4) 1 calc PR C 1 C89 C 0.67696(15) 0.97115(8) 0.05373(16) 0.0453(9) Uani 0.814(4) 1 d PGDU C 1 C90 C 0.72238(19) 1.01381(7) 0.04449(19) 0.0475(9) Uani 0.814(4) 1 d PGDU C 1 H90A H 0.6783 1.0360 0.0059 0.057 Uiso 0.814(4) 1 calc PR C 1 C91 C 0.8323(2) 1.02405(6) 0.0917(2) 0.0529(10) Uani 0.814(4) 1 d PGDU C 1 H91A H 0.8634 1.0532 0.0854 0.063 Uiso 0.814(4) 1 calc PR C 1 C92 C 0.89685(16) 0.99163(8) 0.1481(2) 0.0526(10) Uani 0.814(4) 1 d PGDU C 1 H92A H 0.9720 0.9986 0.1804 0.063 Uiso 0.814(4) 1 calc PR C 1 C93 C 0.8514(2) 0.94897(7) 0.1574(2) 0.0567(10) Uani 0.814(4) 1 d PGDU C 1 H93A H 0.8955 0.9268 0.1959 0.068 Uiso 0.814(4) 1 calc PR C 1 C94 C 0.7415(2) 0.93872(6) 0.1102(2) 0.0469(9) Uani 0.814(4) 1 d PGDU C 1 H94A H 0.7104 0.9096 0.1165 0.056 Uiso 0.814(4) 1 calc PR C 1 C88' C 0.8795(11) 0.9513(5) 0.1880(11) 0.0567(10) Uani 0.186(4) 1 d PDU C 2 H88D H 0.8539 0.9245 0.2271 0.085 Uiso 0.186(4) 1 calc PR C 2 H88E H 0.9050 0.9737 0.2422 0.085 Uiso 0.186(4) 1 calc PR C 2 H88F H 0.9457 0.9440 0.1397 0.085 Uiso 0.186(4) 1 calc PR C 2 C89' C 0.7776(7) 0.9692(3) 0.1190(7) 0.050(4) Uani 0.186(4) 1 d PGDU C 2 C90' C 0.6931(10) 0.9405(3) 0.0745(10) 0.0469(9) Uani 0.186(4) 1 d PGDU C 2 H90B H 0.6994 0.9095 0.0875 0.056 Uiso 0.186(4) 1 calc PR C 2 C91' C 0.5992(9) 0.9570(4) 0.0108(10) 0.0638(11) Uani 0.186(4) 1 d PGDU C 2 H91B H 0.5414 0.9374 -0.0196 0.077 Uiso 0.186(4) 1 calc PR C 2 C92' C 0.5899(8) 1.0024(4) -0.0083(8) 0.046(4) Uani 0.186(4) 1 d PGDU C 2 H92B H 0.5257 1.0137 -0.0518 0.055 Uiso 0.186(4) 1 calc PR C 2 C93' C 0.6744(9) 1.0311(3) 0.0362(9) 0.054(4) Uani 0.186(4) 1 d PGDU C 2 H93B H 0.6680 1.0621 0.0231 0.065 Uiso 0.186(4) 1 calc PR C 2 C94' C 0.7683(8) 1.0145(3) 0.0998(9) 0.048(4) Uani 0.186(4) 1 d PGDU C 2 H94B H 0.8261 1.0342 0.1302 0.057 Uiso 0.186(4) 1 calc PR C 2 C95 C 0.0046(4) 0.58842(14) 0.7105(4) 0.0623(12) Uani 0.791(5) 1 d PD D 1 H95A H 0.0656 0.5686 0.6814 0.093 Uiso 0.791(5) 1 calc PR D 1 H95B H -0.0494 0.5975 0.6502 0.093 Uiso 0.791(5) 1 calc PR D 1 H95C H -0.0402 0.5729 0.7676 0.093 Uiso 0.791(5) 1 calc PR D 1 C96 C 0.0628(2) 0.62879(8) 0.7604(2) 0.0391(8) Uani 0.791(5) 1 d PGD D 1 C97 C 0.18429(19) 0.63581(10) 0.7534(2) 0.0460(9) Uani 0.791(5) 1 d PGD D 1 H97 H 0.2331 0.6142 0.7197 0.055 Uiso 0.791(5) 1 calc PR D 1 C98 C 0.23435(18) 0.67450(12) 0.7958(3) 0.0677(16) Uani 0.791(5) 1 d PGU D 1 H98 H 0.3174 0.6793 0.7910 0.081 Uiso 0.791(5) 1 calc PR D 1 C99 C 0.1629(3) 0.70618(9) 0.8452(3) 0.0736(18) Uani 0.791(5) 1 d PGU D 1 H99 H 0.1971 0.7326 0.8742 0.088 Uiso 0.791(5) 1 calc PR D 1 C100 C 0.0414(3) 0.69916(9) 0.8522(2) 0.0580(12) Uani 0.791(5) 1 d PGU D 1 H100 H -0.0075 0.7208 0.8859 0.070 Uiso 0.791(5) 1 calc PR D 1 C101 C -0.00869(15) 0.66046(10) 0.8098(2) 0.0438(9) Uani 0.791(5) 1 d PGD D 1 H101 H -0.0917 0.6557 0.8146 0.053 Uiso 0.791(5) 1 calc PR D 1 C102 C -0.0598(11) 0.5993(4) 0.7799(15) 0.0623(12) Uani 0.209(5) 1 d PD D 2 H10C H -0.0265 0.5708 0.7572 0.093 Uiso 0.209(5) 1 calc PR D 2 H10D H -0.1189 0.6091 0.7247 0.093 Uiso 0.209(5) 1 calc PR D 2 H10E H -0.0975 0.5960 0.8521 0.093 Uiso 0.209(5) 1 calc PR D 2 C103 C 0.0378(8) 0.6331(4) 0.7888(11) 0.0391(8) Uani 0.209(5) 1 d PGD D 2 C104 C 0.0152(9) 0.6746(4) 0.8342(11) 0.0438(9) Uani 0.209(5) 1 d PGD D 2 H104 H -0.0624 0.6818 0.8577 0.053 Uiso 0.209(5) 1 calc PR D 2 C105 C 0.1063(13) 0.7054(3) 0.8450(11) 0.0580(12) Uani 0.209(5) 1 d PG D 2 H105 H 0.0908 0.7338 0.8760 0.070 Uiso 0.209(5) 1 calc PR D 2 C106 C 0.2198(10) 0.6948(4) 0.8106(12) 0.0736(18) Uani 0.209(5) 1 d PG D 2 H106 H 0.2821 0.7159 0.8180 0.088 Uiso 0.209(5) 1 calc PR D 2 C107 C 0.2424(7) 0.6534(5) 0.7652(10) 0.0677(16) Uani 0.209(5) 1 d PG D 2 H107 H 0.3200 0.6461 0.7416 0.081 Uiso 0.209(5) 1 calc PR D 2 C108 C 0.1514(9) 0.6225(4) 0.7543(9) 0.0460(9) Uani 0.209(5) 1 d PGD D 2 H108 H 0.1668 0.5942 0.7233 0.055 Uiso 0.209(5) 1 calc PR D 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 0.01828(7) 0.01467(8) 0.01494(7) -0.00021(7) 0.00068(5) -0.00112(7) N1 0.0163(7) 0.0135(8) 0.0175(7) -0.0004(6) -0.0002(5) -0.0012(6) N2 0.0215(7) 0.0178(8) 0.0170(7) 0.0023(6) -0.0014(6) 0.0004(6) N3 0.0192(7) 0.0188(9) 0.0174(8) -0.0028(6) 0.0023(6) -0.0033(6) N4 0.0159(7) 0.0147(8) 0.0151(7) -0.0012(6) 0.0004(5) 0.0002(6) O1 0.0200(6) 0.0187(7) 0.0199(6) -0.0032(5) 0.0008(5) 0.0025(5) O2 0.0277(7) 0.0216(7) 0.0196(6) 0.0024(5) -0.0047(5) -0.0027(6) O3 0.0236(6) 0.0194(7) 0.0180(6) -0.0021(5) 0.0049(5) -0.0044(5) O4 0.0201(6) 0.0171(8) 0.0255(6) 0.0034(5) 0.0026(5) 0.0016(5) C1 0.0151(8) 0.0168(9) 0.0203(8) -0.0012(7) -0.0001(7) -0.0006(7) C2 0.0144(8) 0.0181(10) 0.0176(8) -0.0036(7) -0.0018(6) 0.0005(7) C3 0.0221(9) 0.0184(10) 0.0203(9) -0.0002(7) 0.0009(7) -0.0037(7) C4 0.0197(8) 0.0240(11) 0.0241(9) -0.0062(8) 0.0031(7) -0.0014(7) C5 0.0205(9) 0.0213(11) 0.0252(9) -0.0067(8) -0.0013(7) 0.0028(7) C6 0.0209(9) 0.0167(10) 0.0255(9) -0.0010(8) -0.0019(7) 0.0001(7) C7 0.0297(10) 0.0183(11) 0.0355(11) 0.0013(9) -0.0003(9) 0.0023(8) C8 0.0462(13) 0.0224(12) 0.0479(14) -0.0011(10) 0.0006(11) 0.0077(10) C9 0.0371(12) 0.0311(14) 0.0445(13) -0.0089(10) -0.0034(10) 0.0137(10) C10 0.0314(11) 0.0277(12) 0.0371(12) -0.0097(9) 0.0020(9) 0.0082(9) C11 0.0184(8) 0.0128(9) 0.0228(9) 0.0026(7) 0.0016(7) 0.0008(7) C12 0.0187(8) 0.0153(10) 0.0218(9) 0.0039(7) 0.0015(7) 0.0022(7) C13 0.0284(10) 0.0214(11) 0.0225(10) 0.0066(8) 0.0040(8) 0.0011(8) C14 0.0292(10) 0.0240(11) 0.0314(11) 0.0074(9) 0.0092(8) -0.0008(8) C15 0.0220(9) 0.0187(11) 0.0391(11) 0.0052(9) 0.0056(8) -0.0025(8) C16 0.0204(9) 0.0150(10) 0.0304(10) 0.0021(8) 0.0007(7) -0.0006(7) C17 0.0257(10) 0.0270(12) 0.0321(11) 0.0000(9) -0.0020(8) -0.0072(8) C18 0.0311(11) 0.0379(14) 0.0488(14) 0.0043(11) -0.0083(10) -0.0119(10) C19 0.0313(12) 0.0380(15) 0.0617(17) 0.0020(13) 0.0027(11) -0.0144(10) C20 0.0279(11) 0.0285(13) 0.0566(15) 0.0017(11) 0.0095(10) -0.0110(10) C21 0.0176(8) 0.0168(10) 0.0163(8) 0.0021(6) 0.0032(6) 0.0001(6) C22 0.0166(8) 0.0152(10) 0.0229(9) -0.0007(7) -0.0010(7) 0.0022(7) C23 0.0187(8) 0.0158(10) 0.0300(10) 0.0026(8) 0.0019(7) 0.0044(7) C24 0.0178(9) 0.0194(11) 0.0445(12) 0.0033(9) 0.0044(8) 0.0008(7) C25 0.0184(9) 0.0230(11) 0.0451(12) -0.0036(9) -0.0073(8) 0.0003(8) C26 0.0246(9) 0.0226(11) 0.0303(10) -0.0017(8) -0.0065(8) -0.0005(8) C27 0.0207(9) 0.0192(10) 0.0239(9) 0.0006(8) -0.0005(7) -0.0001(7) C28 0.0240(9) 0.0268(11) 0.0290(10) 0.0051(8) 0.0081(8) 0.0056(8) C29 0.0237(11) 0.0442(16) 0.0649(17) -0.0067(13) -0.0129(11) -0.0021(10) C30 0.0265(9) 0.0385(16) 0.0213(9) 0.0019(8) 0.0003(7) -0.0050(8) C31 0.0224(9) 0.0220(11) 0.0186(9) 0.0005(8) 0.0041(7) 0.0007(8) C32 0.0219(9) 0.0213(10) 0.0207(9) 0.0019(7) -0.0036(7) 0.0023(7) C33 0.0188(8) 0.0260(11) 0.0204(9) -0.0026(8) -0.0038(7) 0.0017(8) C34 0.0248(9) 0.0258(12) 0.0282(10) -0.0048(8) -0.0029(8) 0.0072(8) C35 0.0320(10) 0.0220(11) 0.0270(10) 0.0024(8) -0.0061(8) 0.0026(8) C36 0.0357(11) 0.0231(11) 0.0213(9) 0.0036(8) -0.0017(8) 0.0036(9) C37 0.0342(10) 0.0209(11) 0.0204(9) 0.0017(8) 0.0001(8) 0.0047(8) C38 0.0233(10) 0.0423(14) 0.0202(10) -0.0025(9) 0.0007(8) 0.0057(9) C39 0.0468(13) 0.0268(13) 0.0373(12) 0.0086(10) -0.0025(10) 0.0093(10) C40 0.0594(16) 0.0317(13) 0.0227(10) 0.0040(9) 0.0049(10) 0.0161(12) C41 0.0161(8) 0.0161(10) 0.0199(9) -0.0042(7) -0.0008(7) 0.0009(7) C42 0.0155(8) 0.0195(10) 0.0180(8) -0.0037(7) 0.0010(6) -0.0002(7) C43 0.0237(9) 0.0263(11) 0.0175(9) -0.0018(8) -0.0004(7) -0.0016(8) C44 0.0234(9) 0.0313(12) 0.0220(9) -0.0050(8) -0.0069(7) -0.0003(8) C45 0.0182(8) 0.0239(11) 0.0285(10) -0.0059(8) -0.0029(7) -0.0007(7) C46 0.0188(8) 0.0185(10) 0.0239(9) -0.0041(8) 0.0000(7) -0.0012(7) C47 0.0210(9) 0.0238(11) 0.0276(10) -0.0019(8) 0.0000(7) -0.0055(8) C48 0.0267(18) 0.024(2) 0.0397(19) 0.0020(15) 0.0010(14) -0.0071(15) C49 0.0214(18) 0.030(3) 0.050(2) -0.0004(19) -0.0035(16) -0.0087(15) C48' 0.024(4) 0.029(5) 0.026(3) -0.005(3) 0.004(3) -0.015(3) C49' 0.030(4) 0.031(5) 0.038(4) -0.007(4) -0.003(3) -0.013(4) C50 0.0229(10) 0.0375(14) 0.0379(12) -0.0077(10) -0.0065(9) -0.0074(9) C51 0.0157(8) 0.0180(10) 0.0160(8) -0.0017(7) -0.0004(6) -0.0031(7) C52 0.0151(8) 0.0148(9) 0.0179(8) -0.0009(7) 0.0021(6) -0.0005(6) C53 0.0210(8) 0.0190(10) 0.0204(9) -0.0027(7) -0.0018(7) -0.0015(7) C54 0.0236(9) 0.0226(11) 0.0225(9) -0.0002(8) -0.0066(7) 0.0006(8) C55 0.0219(9) 0.0204(11) 0.0246(9) -0.0010(8) 0.0005(7) 0.0027(8) C56 0.0192(8) 0.0176(10) 0.0217(9) -0.0012(7) 0.0020(7) -0.0013(7) C57 0.0294(10) 0.0186(11) 0.0280(10) -0.0062(8) -0.0012(8) 0.0005(8) C58 0.039(2) 0.0201(19) 0.036(2) -0.0090(15) 0.0011(16) 0.0042(16) C59 0.044(2) 0.0185(19) 0.043(2) -0.0023(15) -0.0051(17) 0.0045(15) C58' 0.043(5) 0.017(4) 0.026(4) -0.004(3) 0.001(3) -0.003(3) C59' 0.050(6) 0.020(4) 0.041(5) -0.008(3) -0.012(4) 0.016(4) C60 0.0364(12) 0.0232(12) 0.0354(11) -0.0030(9) -0.0097(9) 0.0084(9) C61 0.0188(8) 0.0188(10) 0.0167(8) 0.0006(7) -0.0008(6) -0.0007(7) C62 0.0177(8) 0.0183(10) 0.0165(8) 0.0001(7) 0.0008(6) -0.0016(7) C63 0.0184(8) 0.0219(10) 0.0186(9) 0.0018(7) -0.0004(7) -0.0029(7) C64 0.0208(9) 0.0202(10) 0.0250(9) 0.0018(8) 0.0011(7) 0.0021(7) C65 0.0264(9) 0.0224(11) 0.0244(9) -0.0030(8) 0.0035(8) 0.0021(8) C66 0.0301(10) 0.0246(11) 0.0171(8) -0.0021(7) -0.0002(7) 0.0035(8) C67 0.0214(9) 0.0217(10) 0.0178(9) 0.0002(7) 0.0000(7) 0.0005(7) C68 0.0250(10) 0.0366(13) 0.0222(10) 0.0024(9) -0.0035(8) 0.0054(9) C69 0.0502(15) 0.0395(15) 0.0272(11) -0.0025(10) 0.0048(10) 0.0208(12) C70 0.0358(11) 0.0300(12) 0.0176(9) 0.0035(8) -0.0003(8) 0.0115(9) C71 0.0185(8) 0.0168(9) 0.0162(8) -0.0026(7) -0.0007(6) 0.0007(7) C72 0.0166(8) 0.0175(10) 0.0218(9) -0.0004(7) 0.0016(7) 0.0026(7) C73 0.0186(8) 0.0183(10) 0.0262(9) -0.0033(8) -0.0006(7) 0.0031(7) C74 0.0190(9) 0.0202(11) 0.0369(11) -0.0016(8) -0.0033(8) 0.0021(7) C75 0.0187(9) 0.0254(12) 0.0429(12) 0.0056(9) 0.0051(8) 0.0007(8) C76 0.0251(9) 0.0245(11) 0.0283(10) 0.0058(8) 0.0064(8) 0.0028(8) C77 0.0215(9) 0.0178(10) 0.0246(9) 0.0011(7) 0.0031(7) 0.0017(7) C78 0.0216(9) 0.0315(12) 0.0250(10) -0.0026(8) -0.0026(7) 0.0050(8) C79 0.0228(10) 0.0416(16) 0.0607(16) 0.0121(12) 0.0091(10) -0.0039(10) C80 0.0267(10) 0.0321(12) 0.0206(9) 0.0027(8) 0.0026(8) -0.0012(9) C81 0.0424(14) 0.0450(16) 0.0469(14) 0.0048(12) -0.0067(11) 0.0031(12) C82 0.0368(12) 0.0250(12) 0.0378(12) -0.0027(9) -0.0022(9) -0.0002(9) C83 0.0375(12) 0.0337(14) 0.0398(13) -0.0089(10) 0.0028(10) 0.0007(10) C84 0.0397(13) 0.0407(16) 0.0597(17) -0.0167(13) -0.0079(12) -0.0021(11) C85 0.0706(19) 0.0332(15) 0.0613(18) -0.0113(13) -0.0373(15) 0.0055(14) C86 0.090(2) 0.0321(16) 0.0470(16) 0.0062(12) -0.0218(15) -0.0143(15) C87 0.0522(15) 0.0314(14) 0.0474(14) 0.0020(11) -0.0073(12) -0.0111(12) C88 0.053(2) 0.078(3) 0.060(2) -0.0064(19) 0.0012(19) 0.004(2) C89 0.0427(17) 0.060(3) 0.0336(16) -0.0015(15) 0.0068(14) 0.0043(16) C90 0.056(2) 0.049(2) 0.0377(18) 0.0085(17) -0.0022(16) 0.0064(18) C91 0.056(2) 0.044(2) 0.058(2) -0.0021(17) -0.0017(19) -0.0033(18) C92 0.0460(19) 0.055(2) 0.056(2) -0.0074(17) -0.0048(16) 0.0092(16) C93 0.054(2) 0.056(2) 0.060(2) -0.0097(18) -0.0020(18) 0.0169(18) C94 0.048(2) 0.0404(19) 0.052(2) -0.0036(16) 0.0077(16) 0.0074(16) C88' 0.054(2) 0.056(2) 0.060(2) -0.0097(18) -0.0020(18) 0.0169(18) C89' 0.047(7) 0.061(8) 0.042(6) -0.012(6) 0.000(5) 0.023(6) C90' 0.048(2) 0.0404(19) 0.052(2) -0.0036(16) 0.0077(16) 0.0074(16) C91' 0.053(2) 0.078(3) 0.060(2) -0.0064(19) 0.0012(19) 0.004(2) C92' 0.044(6) 0.064(8) 0.029(5) -0.005(5) 0.003(5) -0.003(6) C93' 0.058(8) 0.046(8) 0.058(7) 0.029(6) 0.007(6) 0.004(6) C94' 0.037(7) 0.052(8) 0.054(7) 0.005(6) -0.008(6) -0.008(6) C95 0.059(2) 0.056(3) 0.070(3) 0.010(2) -0.0299(19) -0.011(2) C96 0.0291(17) 0.058(2) 0.0303(19) 0.0074(14) -0.0047(12) -0.0129(14) C97 0.0225(17) 0.085(3) 0.0302(13) 0.0095(16) -0.0023(12) -0.0174(16) C98 0.0493(17) 0.109(5) 0.044(2) 0.029(2) -0.0137(15) -0.050(2) C99 0.115(4) 0.067(3) 0.038(2) 0.016(2) -0.022(3) -0.049(3) C100 0.090(3) 0.055(2) 0.0291(15) 0.0084(15) 0.0047(19) -0.010(2) C101 0.0452(16) 0.050(3) 0.0365(16) 0.0084(18) 0.0079(13) -0.0048(18) C102 0.059(2) 0.056(3) 0.070(3) 0.010(2) -0.0299(19) -0.011(2) C103 0.0291(17) 0.058(2) 0.0303(19) 0.0074(14) -0.0047(12) -0.0129(14) C104 0.0452(16) 0.050(3) 0.0365(16) 0.0084(18) 0.0079(13) -0.0048(18) C105 0.090(3) 0.055(2) 0.0291(15) 0.0084(15) 0.0047(19) -0.010(2) C106 0.115(4) 0.067(3) 0.038(2) 0.016(2) -0.022(3) -0.049(3) C107 0.0493(17) 0.109(5) 0.044(2) 0.029(2) -0.0137(15) -0.050(2) C108 0.0225(17) 0.085(3) 0.0302(13) 0.0095(16) -0.0023(12) -0.0174(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O4 2.1899(12) . ? Zr1 O1 2.2066(13) . ? Zr1 O3 2.2380(12) . ? Zr1 N2 2.2619(16) . ? Zr1 O2 2.2649(14) . ? Zr1 N4 2.2714(15) . ? Zr1 N1 2.2726(15) . ? Zr1 N3 2.2778(17) . ? Zr1 C71 2.6436(18) . ? Zr1 C21 2.6564(18) . ? Zr1 C61 2.6706(18) . ? Zr1 C31 2.678(2) . ? N1 C21 1.310(2) . ? N1 C2 1.420(2) . ? N2 C31 1.321(2) . ? N2 C12 1.416(2) . ? N3 C61 1.320(2) . ? N3 C42 1.423(2) . ? N4 C71 1.319(2) . ? N4 C52 1.418(2) . ? O1 C21 1.306(2) . ? O2 C31 1.285(3) . ? O3 C61 1.290(2) . ? O4 C71 1.302(2) . ? C1 C2 1.403(3) . ? C1 C6 1.415(3) . ? C1 C11 1.504(2) . ? C2 C3 1.396(2) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.394(3) . ? C4 H4 0.9500 . ? C5 C6 1.409(3) . ? C5 C10 1.517(3) . ? C6 C7 1.518(3) . ? C7 C8 1.524(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.518(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.514(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.404(3) . ? C11 C16 1.421(3) . ? C12 C13 1.406(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.402(3) . ? C15 C20 1.522(3) . ? C16 C17 1.515(3) . ? C17 C18 1.534(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.516(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.499(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.495(3) . ? C22 C27 1.405(3) . ? C22 C23 1.414(3) . ? C23 C24 1.395(3) . ? C23 C28 1.508(3) . ? C24 C25 1.398(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(3) . ? C25 C29 1.506(3) . ? C26 C27 1.397(3) . ? C26 H26 0.9500 . ? C27 C30 1.515(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.496(3) . ? C32 C37 1.403(3) . ? C32 C33 1.405(3) . ? C33 C34 1.386(3) . ? C33 C38 1.521(3) . ? C34 C35 1.399(3) . ? C34 H34 0.9500 . ? C35 C36 1.390(3) . ? C35 C39 1.508(3) . ? C36 C37 1.400(3) . ? C36 H36 0.9500 . ? C37 C40 1.513(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.406(3) . ? C41 C46 1.417(3) . ? C41 C51 1.493(3) . ? C42 C43 1.400(3) . ? C43 C44 1.385(3) . ? C43 H43 0.9500 . ? C44 C45 1.399(3) . ? C44 H44 0.9500 . ? C45 C46 1.405(3) . ? C45 C50 1.521(3) . ? C46 C47 1.520(3) . ? C47 C48 1.534(4) . ? C47 C48' 1.563(6) . ? C47 H47A 0.9599 . ? C47 H47B 0.9600 . ? C47 H47C 0.9599 . ? C47 H47D 0.9599 . ? C48 C49 1.530(5) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.544(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C48' C49' 1.529(8) . ? C48' H48C 0.9900 . ? C48' H48D 0.9900 . ? C49' C50 1.492(7) . ? C49' H49C 0.9900 . ? C49' H49D 0.9900 . ? C50 H50A 0.9601 . ? C50 H50B 0.9600 . ? C50 H50C 0.9601 . ? C50 H50D 0.9600 . ? C51 C52 1.402(2) . ? C51 C56 1.423(3) . ? C52 C53 1.402(3) . ? C53 C54 1.381(3) . ? C53 H53 0.9500 . ? C54 C55 1.398(3) . ? C54 H54 0.9500 . ? C55 C56 1.398(3) . ? C55 C60 1.522(3) . ? C56 C57 1.526(3) . ? C57 C58' 1.517(6) . ? C57 C58 1.521(4) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9601 . ? C57 H57D 0.9599 . ? C58 C59 1.527(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.539(4) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C58' C59' 1.528(9) . ? C58' H58C 0.9900 . ? C58' H58D 0.9900 . ? C59' C60 1.549(7) . ? C59' H59C 0.9900 . ? C59' H59D 0.9900 . ? C60 H60A 0.9599 . ? C60 H60B 0.9600 . ? C60 H60C 0.9599 . ? C60 H60D 0.9601 . ? C61 C62 1.494(3) . ? C62 C67 1.403(2) . ? C62 C63 1.407(3) . ? C63 C64 1.389(3) . ? C63 C68 1.507(3) . ? C64 C65 1.399(3) . ? C64 H64 0.9500 . ? C65 C66 1.391(3) . ? C65 C69 1.515(3) . ? C66 C67 1.397(3) . ? C66 H66 0.9500 . ? C67 C70 1.510(3) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.486(2) . ? C72 C77 1.412(3) . ? C72 C73 1.414(3) . ? C73 C74 1.398(3) . ? C73 C78 1.502(3) . ? C74 C75 1.395(3) . ? C74 H74 0.9500 . ? C75 C76 1.390(3) . ? C75 C79 1.512(3) . ? C76 C77 1.398(3) . ? C76 H76 0.9500 . ? C77 C80 1.510(3) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.514(3) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C87 1.382(4) . ? C82 C83 1.399(3) . ? C83 C84 1.382(4) . ? C83 H83 0.9500 . ? C84 C85 1.398(5) . ? C84 H84 0.9500 . ? C85 C86 1.376(5) . ? C85 H85 0.9500 . ? C86 C87 1.377(4) . ? C86 H86 0.9500 . ? C87 H87 0.9500 . ? C88 C89 1.514(4) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C90 1.3900 . ? C89 C94 1.3900 . ? C90 C91 1.3900 . ? C90 H90A 0.9500 . ? C91 C92 1.3900 . ? C91 H91A 0.9500 . ? C92 C93 1.3900 . ? C92 H92A 0.9500 . ? C93 C94 1.3900 . ? C93 H93A 0.9500 . ? C94 H94A 0.9500 . ? C88' C89' 1.508(7) . ? C88' H88D 0.9800 . ? C88' H88E 0.9800 . ? C88' H88F 0.9800 . ? C89' C90' 1.3900 . ? C89' C94' 1.3900 . ? C90' C91' 1.3900 . ? C90' H90B 0.9500 . ? C91' C92' 1.3900 . ? C91' H91B 0.9500 . ? C92' C93' 1.3900 . ? C92' H92B 0.9500 . ? C93' C94' 1.3900 . ? C93' H93B 0.9500 . ? C94' H94B 0.9500 . ? C95 C96 1.504(4) . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C97 1.3900 . ? C96 C101 1.3900 . ? C97 C98 1.3900 . ? C97 H97 0.9500 . ? C98 C99 1.3900 . ? C98 H98 0.9500 . ? C99 C100 1.3900 . ? C99 H99 0.9500 . ? C100 C101 1.3900 . ? C100 H100 0.9500 . ? C101 H101 0.9500 . ? C102 C103 1.502(6) . ? C102 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C103 C104 1.3900 . ? C103 C108 1.3900 . ? C104 C105 1.3900 . ? C104 H104 0.9500 . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 C107 1.3900 . ? C106 H106 0.9500 . ? C107 C108 1.3900 . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zr1 O1 134.66(5) . . ? O4 Zr1 O3 146.68(5) . . ? O1 Zr1 O3 76.38(5) . . ? O4 Zr1 N2 97.94(5) . . ? O1 Zr1 N2 100.90(5) . . ? O3 Zr1 N2 84.34(5) . . ? O4 Zr1 O2 75.70(5) . . ? O1 Zr1 O2 148.01(5) . . ? O3 Zr1 O2 77.58(5) . . ? N2 Zr1 O2 58.13(5) . . ? O4 Zr1 N4 58.71(5) . . ? O1 Zr1 N4 85.50(5) . . ? O3 Zr1 N4 127.10(5) . . ? N2 Zr1 N4 148.36(5) . . ? O2 Zr1 N4 125.42(5) . . ? O4 Zr1 N1 87.70(5) . . ? O1 Zr1 N1 58.32(5) . . ? O3 Zr1 N1 124.61(5) . . ? N2 Zr1 N1 75.58(6) . . ? O2 Zr1 N1 127.05(6) . . ? N4 Zr1 N1 81.98(5) . . ? O4 Zr1 N3 99.93(5) . . ? O1 Zr1 N3 96.14(5) . . ? O3 Zr1 N3 58.33(5) . . ? N2 Zr1 N3 133.63(6) . . ? O2 Zr1 N3 85.66(6) . . ? N4 Zr1 N3 75.26(6) . . ? N1 Zr1 N3 147.19(6) . . ? O4 Zr1 C71 29.39(5) . . ? O1 Zr1 C71 113.48(5) . . ? O3 Zr1 C71 141.66(5) . . ? N2 Zr1 C71 126.32(6) . . ? O2 Zr1 C71 98.47(5) . . ? N4 Zr1 C71 29.93(5) . . ? N1 Zr1 C71 88.53(5) . . ? N3 Zr1 C71 83.43(6) . . ? O4 Zr1 C21 114.70(5) . . ? O1 Zr1 C21 29.32(5) . . ? O3 Zr1 C21 98.61(5) . . ? N2 Zr1 C21 84.37(6) . . ? O2 Zr1 C21 142.46(5) . . ? N4 Zr1 C21 86.98(5) . . ? N1 Zr1 C21 29.54(5) . . ? N3 Zr1 C21 124.52(6) . . ? C71 Zr1 C21 106.09(5) . . ? O4 Zr1 C61 126.22(5) . . ? O1 Zr1 C61 84.58(5) . . ? O3 Zr1 C61 28.78(5) . . ? N2 Zr1 C61 110.02(6) . . ? O2 Zr1 C61 81.48(5) . . ? N4 Zr1 C61 101.39(6) . . ? N1 Zr1 C61 142.56(5) . . ? N3 Zr1 C61 29.59(5) . . ? C71 Zr1 C61 113.02(6) . . ? C21 Zr1 C61 113.03(5) . . ? O4 Zr1 C31 85.72(5) . . ? O1 Zr1 C31 127.09(6) . . ? O3 Zr1 C31 80.19(5) . . ? N2 Zr1 C31 29.52(6) . . ? O2 Zr1 C31 28.62(6) . . ? N4 Zr1 C31 144.21(6) . . ? N1 Zr1 C31 101.81(6) . . ? N3 Zr1 C31 110.50(6) . . ? C71 Zr1 C31 114.30(6) . . ? C21 Zr1 C31 113.89(6) . . ? C61 Zr1 C31 96.64(6) . . ? C21 N1 C2 130.53(16) . . ? C21 N1 Zr1 91.69(11) . . ? C2 N1 Zr1 130.74(12) . . ? C31 N2 C12 126.83(16) . . ? C31 N2 Zr1 92.95(12) . . ? C12 N2 Zr1 137.78(12) . . ? C61 N3 C42 127.32(16) . . ? C61 N3 Zr1 91.93(12) . . ? C42 N3 Zr1 139.34(12) . . ? C71 N4 C52 130.79(16) . . ? C71 N4 Zr1 90.85(11) . . ? C52 N4 Zr1 131.38(11) . . ? C21 O1 Zr1 94.81(10) . . ? C31 O2 Zr1 93.82(11) . . ? C61 O3 Zr1 94.57(10) . . ? C71 O4 Zr1 95.00(10) . . ? C2 C1 C6 119.40(16) . . ? C2 C1 C11 122.20(16) . . ? C6 C1 C11 118.18(17) . . ? C3 C2 C1 119.79(17) . . ? C3 C2 N1 117.50(17) . . ? C1 C2 N1 121.66(15) . . ? C4 C3 C2 120.42(18) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.05(17) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 118.93(18) . . ? C4 C5 C10 119.48(18) . . ? C6 C5 C10 121.55(19) . . ? C5 C6 C1 120.20(18) . . ? C5 C6 C7 120.00(18) . . ? C1 C6 C7 119.43(17) . . ? C6 C7 C8 115.72(18) . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? C8 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 111.3(2) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 109.81(19) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C5 112.29(18) . . ? C9 C10 H10A 109.1 . . ? C5 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C5 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C16 119.76(16) . . ? C12 C11 C1 120.15(16) . . ? C16 C11 C1 119.93(17) . . ? C11 C12 C13 119.68(18) . . ? C11 C12 N2 120.03(16) . . ? C13 C12 N2 119.68(18) . . ? C14 C13 C12 119.5(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.61(18) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C16 119.54(19) . . ? C14 C15 C20 119.04(19) . . ? C16 C15 C20 121.4(2) . . ? C15 C16 C11 119.35(19) . . ? C15 C16 C17 121.16(18) . . ? C11 C16 C17 119.48(17) . . ? C16 C17 C18 113.87(18) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 111.7(2) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 110.2(2) . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C19 C20 C15 113.27(19) . . ? C19 C20 H20A 108.9 . . ? C15 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C15 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? O1 C21 N1 113.17(16) . . ? O1 C21 C22 119.31(15) . . ? N1 C21 C22 127.51(16) . . ? O1 C21 Zr1 55.87(9) . . ? N1 C21 Zr1 58.77(10) . . ? C22 C21 Zr1 166.45(12) . . ? C27 C22 C23 120.50(17) . . ? C27 C22 C21 121.10(16) . . ? C23 C22 C21 118.36(16) . . ? C24 C23 C22 118.19(18) . . ? C24 C23 C28 119.70(17) . . ? C22 C23 C28 122.11(17) . . ? C23 C24 C25 122.32(18) . . ? C23 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C26 C25 C24 118.13(18) . . ? C26 C25 C29 121.3(2) . . ? C24 C25 C29 120.6(2) . . ? C25 C26 C27 121.8(2) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C26 C27 C22 118.96(17) . . ? C26 C27 C30 118.13(18) . . ? C22 C27 C30 122.86(17) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O2 C31 N2 115.06(18) . . ? O2 C31 C32 120.79(17) . . ? N2 C31 C32 124.02(18) . . ? O2 C31 Zr1 57.56(10) . . ? N2 C31 Zr1 57.52(10) . . ? C32 C31 Zr1 174.57(13) . . ? C37 C32 C33 120.80(18) . . ? C37 C32 C31 120.87(18) . . ? C33 C32 C31 118.33(17) . . ? C34 C33 C32 118.83(18) . . ? C34 C33 C38 120.79(18) . . ? C32 C33 C38 120.29(19) . . ? C33 C34 C35 121.84(19) . . ? C33 C34 H34 119.1 . . ? C35 C34 H34 119.1 . . ? C36 C35 C34 118.14(19) . . ? C36 C35 C39 120.67(19) . . ? C34 C35 C39 121.2(2) . . ? C35 C36 C37 121.98(19) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C36 C37 C32 118.27(19) . . ? C36 C37 C40 119.92(18) . . ? C32 C37 C40 121.79(19) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 119.68(17) . . ? C42 C41 C51 120.73(16) . . ? C46 C41 C51 119.40(17) . . ? C43 C42 C41 119.43(17) . . ? C43 C42 N3 119.66(17) . . ? C41 C42 N3 120.16(16) . . ? C44 C43 C42 120.34(18) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 121.13(18) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C46 119.09(18) . . ? C44 C45 C50 118.85(18) . . ? C46 C45 C50 122.06(19) . . ? C45 C46 C41 119.87(18) . . ? C45 C46 C47 120.42(17) . . ? C41 C46 C47 119.64(17) . . ? C46 C47 C48 114.0(2) . . ? C46 C47 C48' 111.5(3) . . ? C48 C47 C48' 32.0(3) . . ? C46 C47 H47A 108.7 . . ? C48 C47 H47A 108.7 . . ? C48' C47 H47A 133.5 . . ? C46 C47 H47B 108.7 . . ? C48 C47 H47B 108.9 . . ? C48' C47 H47B 80.6 . . ? H47A C47 H47B 107.7 . . ? C46 C47 H47C 109.3 . . ? C48 C47 H47C 79.6 . . ? C48' C47 H47C 109.8 . . ? H47A C47 H47C 32.6 . . ? H47B C47 H47C 132.7 . . ? C46 C47 H47D 109.1 . . ? C48 C47 H47D 130.5 . . ? C48' C47 H47D 109.0 . . ? H47A C47 H47D 78.1 . . ? H47B C47 H47D 31.6 . . ? H47C C47 H47D 108.0 . . ? C49 C48 C47 108.2(3) . . ? C49 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 . . ? C49 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 . . ? H48A C48 H48B 108.4 . . ? C48 C49 C50 111.0(3) . . ? C48 C49 H49A 109.4 . . ? C50 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? C50 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C49' C48' C47 111.9(6) . . ? C49' C48' H48C 109.2 . . ? C47 C48' H48C 109.2 . . ? C49' C48' H48D 109.2 . . ? C47 C48' H48D 109.2 . . ? H48C C48' H48D 107.9 . . ? C50 C49' C48' 107.0(6) . . ? C50 C49' H49C 110.3 . . ? C48' C49' H49C 110.3 . . ? C50 C49' H49D 110.3 . . ? C48' C49' H49D 110.3 . . ? H49C C49' H49D 108.6 . . ? C49' C50 C45 115.2(3) . . ? C49' C50 C49 28.1(3) . . ? C45 C50 C49 112.9(2) . . ? C49' C50 H50A 127.9 . . ? C45 C50 H50A 108.8 . . ? C49 C50 H50A 108.6 . . ? C49' C50 H50B 83.0 . . ? C45 C50 H50B 109.1 . . ? C49 C50 H50B 109.4 . . ? H50A C50 H50B 107.9 . . ? C49' C50 H50C 107.7 . . ? C45 C50 H50C 108.6 . . ? C49 C50 H50C 82.9 . . ? H50A C50 H50C 28.9 . . ? H50B C50 H50C 131.0 . . ? C49' C50 H50D 109.0 . . ? C45 C50 H50D 108.5 . . ? C49 C50 H50D 131.0 . . ? H50A C50 H50D 80.6 . . ? H50B C50 H50D 29.6 . . ? H50C C50 H50D 107.6 . . ? C52 C51 C56 119.44(16) . . ? C52 C51 C41 122.45(17) . . ? C56 C51 C41 118.06(16) . . ? C53 C52 C51 119.74(17) . . ? C53 C52 N4 117.55(16) . . ? C51 C52 N4 121.80(16) . . ? C54 C53 C52 120.00(18) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 121.62(18) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 118.87(18) . . ? C56 C55 C60 123.04(18) . . ? C54 C55 C60 118.05(18) . . ? C55 C56 C51 120.17(17) . . ? C55 C56 C57 119.61(18) . . ? C51 C56 C57 120.09(17) . . ? C58' C57 C58 27.8(3) . . ? C58' C57 C56 113.8(3) . . ? C58 C57 C56 113.3(2) . . ? C58' C57 H57A 83.1 . . ? C58 C57 H57A 108.7 . . ? C56 C57 H57A 108.9 . . ? C58' C57 H57B 129.3 . . ? C58 C57 H57B 109.0 . . ? C56 C57 H57B 108.9 . . ? H57A C57 H57B 107.8 . . ? C58' C57 H57C 108.3 . . ? C58 C57 H57C 129.4 . . ? C56 C57 H57C 108.7 . . ? H57A C57 H57C 28.3 . . ? H57B C57 H57C 81.6 . . ? C58' C57 H57D 109.3 . . ? C58 C57 H57D 84.2 . . ? C56 C57 H57D 108.9 . . ? H57A C57 H57D 130.3 . . ? H57B C57 H57D 28.1 . . ? H57C C57 H57D 107.7 . . ? C57 C58 C59 112.6(3) . . ? C57 C58 H58A 109.1 . . ? C59 C58 H58A 109.1 . . ? C57 C58 H58B 109.1 . . ? C59 C58 H58B 109.1 . . ? H58A C58 H58B 107.8 . . ? C58 C59 C60 107.2(3) . . ? C58 C59 H59A 110.3 . . ? C60 C59 H59A 110.3 . . ? C58 C59 H59B 110.3 . . ? C60 C59 H59B 110.3 . . ? H59A C59 H59B 108.5 . . ? C57 C58' C59' 110.4(6) . . ? C57 C58' H58C 109.6 . . ? C59' C58' H58C 109.6 . . ? C57 C58' H58D 109.6 . . ? C59' C58' H58D 109.6 . . ? H58C C58' H58D 108.1 . . ? C58' C59' C60 108.1(6) . . ? C58' C59' H59C 110.1 . . ? C60 C59' H59C 110.1 . . ? C58' C59' H59D 110.1 . . ? C60 C59' H59D 110.1 . . ? H59C C59' H59D 108.4 . . ? C55 C60 C59 113.8(2) . . ? C55 C60 C59' 112.3(3) . . ? C59 C60 C59' 32.0(4) . . ? C55 C60 H60A 108.8 . . ? C59 C60 H60A 108.7 . . ? C59' C60 H60A 80.0 . . ? C55 C60 H60B 108.8 . . ? C59 C60 H60B 108.8 . . ? C59' C60 H60B 132.8 . . ? H60A C60 H60B 107.8 . . ? C55 C60 H60C 109.0 . . ? C59 C60 H60C 131.2 . . ? C59' C60 H60C 109.2 . . ? H60A C60 H60C 32.7 . . ? H60B C60 H60C 77.2 . . ? C55 C60 H60D 109.3 . . ? C59 C60 H60D 79.1 . . ? C59' C60 H60D 109.0 . . ? H60A C60 H60D 133.2 . . ? H60B C60 H60D 33.2 . . ? H60C C60 H60D 107.9 . . ? O3 C61 N3 115.02(16) . . ? O3 C61 C62 118.69(15) . . ? N3 C61 C62 125.97(17) . . ? O3 C61 Zr1 56.65(9) . . ? N3 C61 Zr1 58.48(10) . . ? C62 C61 Zr1 170.25(13) . . ? C67 C62 C63 121.13(17) . . ? C67 C62 C61 120.67(17) . . ? C63 C62 C61 117.84(16) . . ? C64 C63 C62 118.55(17) . . ? C64 C63 C68 120.48(18) . . ? C62 C63 C68 120.93(17) . . ? C63 C64 C65 121.67(18) . . ? C63 C64 H64 119.2 . . ? C65 C64 H64 119.2 . . ? C66 C65 C64 118.45(18) . . ? C66 C65 C69 121.74(19) . . ? C64 C65 C69 119.81(19) . . ? C65 C66 C67 121.96(18) . . ? C65 C66 H66 119.0 . . ? C67 C66 H66 119.0 . . ? C66 C67 C62 118.21(18) . . ? C66 C67 C70 120.06(17) . . ? C62 C67 C70 121.73(17) . . ? C63 C68 H68A 109.5 . . ? C63 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C63 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C65 C69 H69A 109.5 . . ? C65 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C65 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O4 C71 N4 113.18(16) . . ? O4 C71 C72 119.40(16) . . ? N4 C71 C72 127.41(17) . . ? O4 C71 Zr1 55.61(8) . . ? N4 C71 Zr1 59.22(9) . . ? C72 C71 Zr1 165.62(13) . . ? C77 C72 C73 120.96(17) . . ? C77 C72 C71 120.42(16) . . ? C73 C72 C71 118.56(16) . . ? C74 C73 C72 118.06(18) . . ? C74 C73 C78 119.31(17) . . ? C72 C73 C78 122.61(17) . . ? C75 C74 C73 122.01(19) . . ? C75 C74 H74 119.0 . . ? C73 C74 H74 119.0 . . ? C76 C75 C74 118.65(18) . . ? C76 C75 C79 121.7(2) . . ? C74 C75 C79 119.7(2) . . ? C75 C76 C77 121.92(19) . . ? C75 C76 H76 119.0 . . ? C77 C76 H76 119.0 . . ? C76 C77 C72 118.34(18) . . ? C76 C77 C80 119.19(17) . . ? C72 C77 C80 122.36(17) . . ? C73 C78 H78A 109.5 . . ? C73 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C73 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C75 C79 H79A 109.5 . . ? C75 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C75 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C87 C82 C83 118.0(2) . . ? C87 C82 C81 121.5(2) . . ? C83 C82 C81 120.4(2) . . ? C84 C83 C82 120.5(3) . . ? C84 C83 H83 119.7 . . ? C82 C83 H83 119.7 . . ? C83 C84 C85 120.3(3) . . ? C83 C84 H84 119.9 . . ? C85 C84 H84 119.9 . . ? C86 C85 C84 119.2(3) . . ? C86 C85 H85 120.4 . . ? C84 C85 H85 120.4 . . ? C85 C86 C87 120.2(3) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C86 C87 C82 121.8(3) . . ? C86 C87 H87 119.1 . . ? C82 C87 H87 119.1 . . ? C90 C89 C94 120.0 . . ? C90 C89 C88 120.2(2) . . ? C94 C89 C88 119.8(2) . . ? C91 C90 C89 120.0 . . ? C91 C90 H90A 120.0 . . ? C89 C90 H90A 120.0 . . ? C90 C91 C92 120.0 . . ? C90 C91 H91A 120.0 . . ? C92 C91 H91A 120.0 . . ? C93 C92 C91 120.0 . . ? C93 C92 H92A 120.0 . . ? C91 C92 H92A 120.0 . . ? C92 C93 C94 120.0 . . ? C92 C93 H93A 120.0 . . ? C94 C93 H93A 120.0 . . ? C93 C94 C89 120.0 . . ? C93 C94 H94A 120.0 . . ? C89 C94 H94A 120.0 . . ? C89' C88' H88D 109.5 . . ? C89' C88' H88E 109.5 . . ? H88D C88' H88E 109.5 . . ? C89' C88' H88F 109.5 . . ? H88D C88' H88F 109.5 . . ? H88E C88' H88F 109.5 . . ? C90' C89' C94' 120.0 . . ? C90' C89' C88' 120.0(4) . . ? C94' C89' C88' 120.0(4) . . ? C89' C90' C91' 120.0 . . ? C89' C90' H90B 120.0 . . ? C91' C90' H90B 120.0 . . ? C92' C91' C90' 120.0 . . ? C92' C91' H91B 120.0 . . ? C90' C91' H91B 120.0 . . ? C91' C92' C93' 120.0 . . ? C91' C92' H92B 120.0 . . ? C93' C92' H92B 120.0 . . ? C94' C93' C92' 120.0 . . ? C94' C93' H93B 120.0 . . ? C92' C93' H93B 120.0 . . ? C93' C94' C89' 120.0 . . ? C93' C94' H94B 120.0 . . ? C89' C94' H94B 120.0 . . ? C97 C96 C101 120.0 . . ? C97 C96 C95 121.5(2) . . ? C101 C96 C95 118.4(2) . . ? C98 C97 C96 120.0 . . ? C98 C97 H97 120.0 . . ? C96 C97 H97 120.0 . . ? C99 C98 C97 120.0 . . ? C99 C98 H98 120.0 . . ? C97 C98 H98 120.0 . . ? C98 C99 C100 120.0 . . ? C98 C99 H99 120.0 . . ? C100 C99 H99 120.0 . . ? C101 C100 C99 120.0 . . ? C101 C100 H100 120.0 . . ? C99 C100 H100 120.0 . . ? C100 C101 C96 120.0 . . ? C100 C101 H101 120.0 . . ? C96 C101 H101 120.0 . . ? C103 C102 H10C 109.5 . . ? C103 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C103 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C104 C103 C108 120.0 . . ? C104 C103 C102 120.0(4) . . ? C108 C103 C102 120.0(4) . . ? C105 C104 C103 120.0 . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C104 C105 C106 120.0 . . ? C104 C105 H105 120.0 . . ? C106 C105 H105 120.0 . . ? C105 C106 C107 120.0 . . ? C105 C106 H106 120.0 . . ? C107 C106 H106 120.0 . . ? C108 C107 C106 120.0 . . ? C108 C107 H107 120.0 . . ? C106 C107 H107 120.0 . . ? C107 C108 C103 120.0 . . ? C107 C108 H108 120.0 . . ? C103 C108 H108 120.0 . . ? 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 O4 Zr1 N1 C21 -156.81(11) . . . . ? O1 Zr1 N1 C21 -8.45(10) . . . . ? O3 Zr1 N1 C21 31.91(13) . . . . ? N2 Zr1 N1 C21 104.38(11) . . . . ? O2 Zr1 N1 C21 133.07(10) . . . . ? N4 Zr1 N1 C21 -98.10(11) . . . . ? N3 Zr1 N1 C21 -51.96(15) . . . . ? C71 Zr1 N1 C21 -127.42(11) . . . . ? C61 Zr1 N1 C21 0.17(15) . . . . ? C31 Zr1 N1 C21 118.05(11) . . . . ? O4 Zr1 N1 C2 51.12(15) . . . . ? O1 Zr1 N1 C2 -160.53(17) . . . . ? O3 Zr1 N1 C2 -120.16(14) . . . . ? N2 Zr1 N1 C2 -47.69(15) . . . . ? O2 Zr1 N1 C2 -19.00(17) . . . . ? N4 Zr1 N1 C2 109.83(15) . . . . ? N3 Zr1 N1 C2 155.97(13) . . . . ? C71 Zr1 N1 C2 80.51(15) . . . . ? C21 Zr1 N1 C2 -152.1(2) . . . . ? C61 Zr1 N1 C2 -151.90(14) . . . . ? C31 Zr1 N1 C2 -34.02(16) . . . . ? O4 Zr1 N2 C31 66.46(11) . . . . ? O1 Zr1 N2 C31 -154.98(11) . . . . ? O3 Zr1 N2 C31 -80.06(11) . . . . ? O2 Zr1 N2 C31 -1.18(10) . . . . ? N4 Zr1 N2 C31 105.80(13) . . . . ? N1 Zr1 N2 C31 152.01(12) . . . . ? N3 Zr1 N2 C31 -45.47(14) . . . . ? C71 Zr1 N2 C31 74.83(12) . . . . ? C21 Zr1 N2 C31 -179.32(12) . . . . ? C61 Zr1 N2 C31 -66.83(12) . . . . ? O4 Zr1 N2 C12 -131.72(17) . . . . ? O1 Zr1 N2 C12 6.84(18) . . . . ? O3 Zr1 N2 C12 81.77(18) . . . . ? O2 Zr1 N2 C12 160.6(2) . . . . ? N4 Zr1 N2 C12 -92.4(2) . . . . ? N1 Zr1 N2 C12 -46.17(17) . . . . ? N3 Zr1 N2 C12 116.35(18) . . . . ? C71 Zr1 N2 C12 -123.35(17) . . . . ? C21 Zr1 N2 C12 -17.50(17) . . . . ? C61 Zr1 N2 C12 94.99(18) . . . . ? C31 Zr1 N2 C12 161.8(2) . . . . ? O4 Zr1 N3 C61 -155.01(11) . . . . ? O1 Zr1 N3 C61 67.55(12) . . . . ? O3 Zr1 N3 C61 -2.29(10) . . . . ? N2 Zr1 N3 C61 -43.87(15) . . . . ? O2 Zr1 N3 C61 -80.37(11) . . . . ? N4 Zr1 N3 C61 151.24(12) . . . . ? N1 Zr1 N3 C61 103.65(13) . . . . ? C71 Zr1 N3 C61 -179.43(12) . . . . ? C21 Zr1 N3 C61 75.54(13) . . . . ? C31 Zr1 N3 C61 -65.90(12) . . . . ? O4 Zr1 N3 C42 11.0(2) . . . . ? O1 Zr1 N3 C42 -126.5(2) . . . . ? O3 Zr1 N3 C42 163.7(2) . . . . ? N2 Zr1 N3 C42 122.12(19) . . . . ? O2 Zr1 N3 C42 85.6(2) . . . . ? N4 Zr1 N3 C42 -42.77(19) . . . . ? N1 Zr1 N3 C42 -90.4(2) . . . . ? C71 Zr1 N3 C42 -13.44(19) . . . . ? C21 Zr1 N3 C42 -118.47(19) . . . . ? C61 Zr1 N3 C42 166.0(3) . . . . ? C31 Zr1 N3 C42 100.1(2) . . . . ? O4 Zr1 N4 C71 -8.93(10) . . . . ? O1 Zr1 N4 C71 -159.73(11) . . . . ? O3 Zr1 N4 C71 131.10(10) . . . . ? N2 Zr1 N4 C71 -56.21(16) . . . . ? O2 Zr1 N4 C71 29.15(13) . . . . ? N1 Zr1 N4 C71 -101.12(11) . . . . ? N3 Zr1 N4 C71 102.70(11) . . . . ? C21 Zr1 N4 C71 -130.38(11) . . . . ? C61 Zr1 N4 C71 116.73(11) . . . . ? C31 Zr1 N4 C71 -2.03(16) . . . . ? O4 Zr1 N4 C52 -161.04(17) . . . . ? O1 Zr1 N4 C52 48.16(15) . . . . ? O3 Zr1 N4 C52 -21.01(17) . . . . ? N2 Zr1 N4 C52 151.67(14) . . . . ? O2 Zr1 N4 C52 -122.96(15) . . . . ? N1 Zr1 N4 C52 106.77(15) . . . . ? N3 Zr1 N4 C52 -49.41(15) . . . . ? C71 Zr1 N4 C52 -152.1(2) . . . . ? C21 Zr1 N4 C52 77.51(15) . . . . ? C61 Zr1 N4 C52 -35.38(16) . . . . ? C31 Zr1 N4 C52 -154.14(14) . . . . ? O4 Zr1 O1 C21 55.98(12) . . . . ? O3 Zr1 O1 C21 -138.23(10) . . . . ? N2 Zr1 O1 C21 -56.85(10) . . . . ? O2 Zr1 O1 C21 -101.89(12) . . . . ? N4 Zr1 O1 C21 91.85(10) . . . . ? N1 Zr1 O1 C21 8.51(9) . . . . ? N3 Zr1 O1 C21 166.48(10) . . . . ? C71 Zr1 O1 C21 80.99(11) . . . . ? C61 Zr1 O1 C21 -166.24(10) . . . . ? C31 Zr1 O1 C21 -72.00(11) . . . . ? O4 Zr1 O2 C31 -107.84(11) . . . . ? O1 Zr1 O2 C31 56.11(15) . . . . ? O3 Zr1 O2 C31 92.25(11) . . . . ? N2 Zr1 O2 C31 1.21(11) . . . . ? N4 Zr1 O2 C31 -140.79(11) . . . . ? N1 Zr1 O2 C31 -31.98(13) . . . . ? N3 Zr1 O2 C31 150.75(11) . . . . ? C71 Zr1 O2 C31 -126.56(11) . . . . ? C21 Zr1 O2 C31 4.25(15) . . . . ? C61 Zr1 O2 C31 121.26(11) . . . . ? O4 Zr1 O3 C61 57.63(14) . . . . ? O1 Zr1 O3 C61 -103.83(11) . . . . ? N2 Zr1 O3 C61 153.49(11) . . . . ? O2 Zr1 O3 C61 94.92(11) . . . . ? N4 Zr1 O3 C61 -30.36(13) . . . . ? N1 Zr1 O3 C61 -138.38(11) . . . . ? N3 Zr1 O3 C61 2.35(10) . . . . ? C71 Zr1 O3 C61 6.94(15) . . . . ? C21 Zr1 O3 C61 -123.10(11) . . . . ? C31 Zr1 O3 C61 123.97(11) . . . . ? O1 Zr1 O4 C71 52.20(13) . . . . ? O3 Zr1 O4 C71 -102.05(12) . . . . ? N2 Zr1 O4 C71 166.17(10) . . . . ? O2 Zr1 O4 C71 -139.68(11) . . . . ? N4 Zr1 O4 C71 9.07(10) . . . . ? N1 Zr1 O4 C71 91.08(11) . . . . ? N3 Zr1 O4 C71 -56.80(11) . . . . ? C21 Zr1 O4 C71 78.74(11) . . . . ? C61 Zr1 O4 C71 -71.79(12) . . . . ? C31 Zr1 O4 C71 -166.89(11) . . . . ? C6 C1 C2 C3 4.6(3) . . . . ? C11 C1 C2 C3 179.13(17) . . . . ? C6 C1 C2 N1 -163.39(17) . . . . ? C11 C1 C2 N1 11.2(3) . . . . ? C21 N1 C2 C3 121.8(2) . . . . ? Zr1 N1 C2 C3 -96.18(19) . . . . ? C21 N1 C2 C1 -69.9(3) . . . . ? Zr1 N1 C2 C1 72.0(2) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? N1 C2 C3 C4 166.49(17) . . . . ? C2 C3 C4 C5 -2.5(3) . . . . ? C3 C4 C5 C6 4.1(3) . . . . ? C3 C4 C5 C10 -173.55(19) . . . . ? C4 C5 C6 C1 -1.4(3) . . . . ? C10 C5 C6 C1 176.20(18) . . . . ? C4 C5 C6 C7 -174.47(18) . . . . ? C10 C5 C6 C7 3.2(3) . . . . ? C2 C1 C6 C5 -2.9(3) . . . . ? C11 C1 C6 C5 -177.66(17) . . . . ? C2 C1 C6 C7 170.20(18) . . . . ? C11 C1 C6 C7 -4.6(3) . . . . ? C5 C6 C7 C8 -10.4(3) . . . . ? C1 C6 C7 C8 176.52(19) . . . . ? C6 C7 C8 C9 39.3(3) . . . . ? C7 C8 C9 C10 -61.1(3) . . . . ? C8 C9 C10 C5 53.3(3) . . . . ? C4 C5 C10 C9 152.6(2) . . . . ? C6 C5 C10 C9 -25.1(3) . . . . ? C2 C1 C11 C12 -68.9(2) . . . . ? C6 C1 C11 C12 105.7(2) . . . . ? C2 C1 C11 C16 115.8(2) . . . . ? C6 C1 C11 C16 -69.6(2) . . . . ? C16 C11 C12 C13 7.7(3) . . . . ? C1 C11 C12 C13 -167.63(18) . . . . ? C16 C11 C12 N2 -163.28(17) . . . . ? C1 C11 C12 N2 21.4(3) . . . . ? C31 N2 C12 C11 -139.2(2) . . . . ? Zr1 N2 C12 C11 63.7(2) . . . . ? C31 N2 C12 C13 49.8(3) . . . . ? Zr1 N2 C12 C13 -107.3(2) . . . . ? C11 C12 C13 C14 -2.5(3) . . . . ? N2 C12 C13 C14 168.52(18) . . . . ? C12 C13 C14 C15 -3.7(3) . . . . ? C13 C14 C15 C16 4.6(3) . . . . ? C13 C14 C15 C20 -174.6(2) . . . . ? C14 C15 C16 C11 0.7(3) . . . . ? C20 C15 C16 C11 179.9(2) . . . . ? C14 C15 C16 C17 -177.9(2) . . . . ? C20 C15 C16 C17 1.4(3) . . . . ? C12 C11 C16 C15 -6.8(3) . . . . ? C1 C11 C16 C15 168.56(18) . . . . ? C12 C11 C16 C17 171.78(18) . . . . ? C1 C11 C16 C17 -12.9(3) . . . . ? C15 C16 C17 C18 10.2(3) . . . . ? C11 C16 C17 C18 -168.4(2) . . . . ? C16 C17 C18 C19 -41.4(3) . . . . ? C17 C18 C19 C20 61.8(3) . . . . ? C18 C19 C20 C15 -49.5(3) . . . . ? C14 C15 C20 C19 -161.9(2) . . . . ? C16 C15 C20 C19 18.8(3) . . . . ? Zr1 O1 C21 N1 -13.74(15) . . . . ? Zr1 O1 C21 C22 165.10(14) . . . . ? C2 N1 C21 O1 165.46(17) . . . . ? Zr1 N1 C21 O1 13.30(15) . . . . ? C2 N1 C21 C22 -13.3(3) . . . . ? Zr1 N1 C21 C22 -165.43(17) . . . . ? C2 N1 C21 Zr1 152.2(2) . . . . ? O4 Zr1 C21 O1 -139.54(9) . . . . ? O3 Zr1 C21 O1 40.90(10) . . . . ? N2 Zr1 C21 O1 124.29(10) . . . . ? O2 Zr1 C21 O1 121.70(11) . . . . ? N4 Zr1 C21 O1 -86.18(10) . . . . ? N1 Zr1 C21 O1 -165.20(16) . . . . ? N3 Zr1 C21 O1 -16.39(12) . . . . ? C71 Zr1 C21 O1 -109.48(10) . . . . ? C61 Zr1 C21 O1 14.91(11) . . . . ? C31 Zr1 C21 O1 123.93(10) . . . . ? O4 Zr1 C21 N1 25.66(12) . . . . ? O1 Zr1 C21 N1 165.20(16) . . . . ? O3 Zr1 C21 N1 -153.89(10) . . . . ? N2 Zr1 C21 N1 -70.51(11) . . . . ? O2 Zr1 C21 N1 -73.10(13) . . . . ? N4 Zr1 C21 N1 79.02(11) . . . . ? N3 Zr1 C21 N1 148.81(10) . . . . ? C71 Zr1 C21 N1 55.72(12) . . . . ? C61 Zr1 C21 N1 -179.89(10) . . . . ? C31 Zr1 C21 N1 -70.87(11) . . . . ? O4 Zr1 C21 C22 147.2(5) . . . . ? O1 Zr1 C21 C22 -73.2(5) . . . . ? O3 Zr1 C21 C22 -32.3(6) . . . . ? N2 Zr1 C21 C22 51.1(6) . . . . ? O2 Zr1 C21 C22 48.5(6) . . . . ? N4 Zr1 C21 C22 -159.4(6) . . . . ? N1 Zr1 C21 C22 121.6(6) . . . . ? N3 Zr1 C21 C22 -89.6(6) . . . . ? C71 Zr1 C21 C22 177.3(5) . . . . ? C61 Zr1 C21 C22 -58.3(6) . . . . ? C31 Zr1 C21 C22 50.7(6) . . . . ? O1 C21 C22 C27 122.68(19) . . . . ? N1 C21 C22 C27 -58.7(3) . . . . ? Zr1 C21 C22 C27 -172.0(5) . . . . ? O1 C21 C22 C23 -55.1(2) . . . . ? N1 C21 C22 C23 123.6(2) . . . . ? Zr1 C21 C22 C23 10.3(7) . . . . ? C27 C22 C23 C24 2.5(3) . . . . ? C21 C22 C23 C24 -179.71(18) . . . . ? C27 C22 C23 C28 -177.02(19) . . . . ? C21 C22 C23 C28 0.7(3) . . . . ? C22 C23 C24 C25 -1.2(3) . . . . ? C28 C23 C24 C25 178.4(2) . . . . ? C23 C24 C25 C26 -1.2(3) . . . . ? C23 C24 C25 C29 178.6(2) . . . . ? C24 C25 C26 C27 2.4(3) . . . . ? C29 C25 C26 C27 -177.4(2) . . . . ? C25 C26 C27 C22 -1.1(3) . . . . ? C25 C26 C27 C30 -178.4(2) . . . . ? C23 C22 C27 C26 -1.4(3) . . . . ? C21 C22 C27 C26 -179.13(18) . . . . ? C23 C22 C27 C30 175.73(19) . . . . ? C21 C22 C27 C30 -2.0(3) . . . . ? Zr1 O2 C31 N2 -1.95(17) . . . . ? Zr1 O2 C31 C32 173.93(15) . . . . ? C12 N2 C31 O2 -162.87(17) . . . . ? Zr1 N2 C31 O2 1.95(17) . . . . ? C12 N2 C31 C32 21.4(3) . . . . ? Zr1 N2 C31 C32 -173.78(16) . . . . ? C12 N2 C31 Zr1 -164.8(2) . . . . ? O4 Zr1 C31 O2 67.67(11) . . . . ? O1 Zr1 C31 O2 -146.54(10) . . . . ? O3 Zr1 C31 O2 -82.03(11) . . . . ? N2 Zr1 C31 O2 -177.91(18) . . . . ? N4 Zr1 C31 O2 61.76(15) . . . . ? N1 Zr1 C31 O2 154.42(11) . . . . ? N3 Zr1 C31 O2 -31.34(12) . . . . ? C71 Zr1 C31 O2 60.65(12) . . . . ? C21 Zr1 C31 O2 -177.17(10) . . . . ? C61 Zr1 C31 O2 -58.33(11) . . . . ? O4 Zr1 C31 N2 -114.42(11) . . . . ? O1 Zr1 C31 N2 31.37(13) . . . . ? O3 Zr1 C31 N2 95.88(11) . . . . ? O2 Zr1 C31 N2 177.91(18) . . . . ? N4 Zr1 C31 N2 -120.33(12) . . . . ? N1 Zr1 C31 N2 -27.67(12) . . . . ? N3 Zr1 C31 N2 146.57(11) . . . . ? C71 Zr1 C31 N2 -121.44(11) . . . . ? C21 Zr1 C31 N2 0.74(13) . . . . ? C61 Zr1 C31 N2 119.58(11) . . . . ? O4 Zr1 C31 C32 -6.2(15) . . . . ? O1 Zr1 C31 C32 139.6(15) . . . . ? O3 Zr1 C31 C32 -155.9(15) . . . . ? N2 Zr1 C31 C32 108.2(16) . . . . ? O2 Zr1 C31 C32 -73.9(15) . . . . ? N4 Zr1 C31 C32 -12.1(16) . . . . ? N1 Zr1 C31 C32 80.5(15) . . . . ? N3 Zr1 C31 C32 -105.2(15) . . . . ? C71 Zr1 C31 C32 -13.2(15) . . . . ? C21 Zr1 C31 C32 108.9(15) . . . . ? C61 Zr1 C31 C32 -132.2(15) . . . . ? O2 C31 C32 C37 77.7(3) . . . . ? N2 C31 C32 C37 -106.8(2) . . . . ? Zr1 C31 C32 C37 148.4(14) . . . . ? O2 C31 C32 C33 -101.3(2) . . . . ? N2 C31 C32 C33 74.2(3) . . . . ? Zr1 C31 C32 C33 -30.6(16) . . . . ? C37 C32 C33 C34 3.2(3) . . . . ? C31 C32 C33 C34 -177.74(18) . . . . ? C37 C32 C33 C38 -173.59(19) . . . . ? C31 C32 C33 C38 5.5(3) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C38 C33 C34 C35 176.8(2) . . . . ? C33 C34 C35 C36 -3.0(3) . . . . ? C33 C34 C35 C39 178.8(2) . . . . ? C34 C35 C36 C37 2.8(3) . . . . ? C39 C35 C36 C37 -179.0(2) . . . . ? C35 C36 C37 C32 0.3(3) . . . . ? C35 C36 C37 C40 -178.3(2) . . . . ? C33 C32 C37 C36 -3.3(3) . . . . ? C31 C32 C37 C36 177.61(19) . . . . ? C33 C32 C37 C40 175.2(2) . . . . ? C31 C32 C37 C40 -3.8(3) . . . . ? C46 C41 C42 C43 7.1(3) . . . . ? C51 C41 C42 C43 -167.88(17) . . . . ? C46 C41 C42 N3 -162.93(17) . . . . ? C51 C41 C42 N3 22.1(3) . . . . ? C61 N3 C42 C43 52.4(3) . . . . ? Zr1 N3 C42 C43 -109.9(2) . . . . ? C61 N3 C42 C41 -137.6(2) . . . . ? Zr1 N3 C42 C41 60.1(3) . . . . ? C41 C42 C43 C44 -2.3(3) . . . . ? N3 C42 C43 C44 167.81(18) . . . . ? C42 C43 C44 C45 -3.4(3) . . . . ? C43 C44 C45 C46 4.1(3) . . . . ? C43 C44 C45 C50 -175.3(2) . . . . ? C44 C45 C46 C41 0.8(3) . . . . ? C50 C45 C46 C41 -179.77(19) . . . . ? C44 C45 C46 C47 -176.23(19) . . . . ? C50 C45 C46 C47 3.2(3) . . . . ? C42 C41 C46 C45 -6.4(3) . . . . ? C51 C41 C46 C45 168.68(17) . . . . ? C42 C41 C46 C47 170.67(18) . . . . ? C51 C41 C46 C47 -14.3(3) . . . . ? C45 C46 C47 C48 -21.4(3) . . . . ? C41 C46 C47 C48 161.6(2) . . . . ? C45 C46 C47 C48' 13.2(4) . . . . ? C41 C46 C47 C48' -163.8(4) . . . . ? C46 C47 C48 C49 50.7(4) . . . . ? C48' C47 C48 C49 -41.8(5) . . . . ? C47 C48 C49 C50 -63.6(5) . . . . ? C46 C47 C48' C49' -48.1(8) . . . . ? C48 C47 C48' C49' 53.2(6) . . . . ? C47 C48' C49' C50 65.3(10) . . . . ? C48' C49' C50 C45 -47.7(9) . . . . ? C48' C49' C50 C49 44.2(6) . . . . ? C44 C45 C50 C49' -165.4(5) . . . . ? C46 C45 C50 C49' 15.2(5) . . . . ? C44 C45 C50 C49 163.9(3) . . . . ? C46 C45 C50 C49 -15.6(4) . . . . ? C48 C49 C50 C49' -55.0(7) . . . . ? C48 C49 C50 C45 46.0(5) . . . . ? C42 C41 C51 C52 -68.8(2) . . . . ? C46 C41 C51 C52 116.2(2) . . . . ? C42 C41 C51 C56 108.6(2) . . . . ? C46 C41 C51 C56 -66.4(2) . . . . ? C56 C51 C52 C53 3.7(3) . . . . ? C41 C51 C52 C53 -178.92(16) . . . . ? C56 C51 C52 N4 -165.13(16) . . . . ? C41 C51 C52 N4 12.2(3) . . . . ? C71 N4 C52 C53 121.2(2) . . . . ? Zr1 N4 C52 C53 -96.96(18) . . . . ? C71 N4 C52 C51 -69.7(2) . . . . ? Zr1 N4 C52 C51 72.1(2) . . . . ? C51 C52 C53 C54 -0.7(3) . . . . ? N4 C52 C53 C54 168.55(17) . . . . ? C52 C53 C54 C55 -2.8(3) . . . . ? C53 C54 C55 C56 3.3(3) . . . . ? C53 C54 C55 C60 -174.61(19) . . . . ? C54 C55 C56 C51 -0.2(3) . . . . ? C60 C55 C56 C51 177.55(18) . . . . ? C54 C55 C56 C57 -175.98(18) . . . . ? C60 C55 C56 C57 1.8(3) . . . . ? C52 C51 C56 C55 -3.2(3) . . . . ? C41 C51 C56 C55 179.29(16) . . . . ? C52 C51 C56 C57 172.52(16) . . . . ? C41 C51 C56 C57 -5.0(3) . . . . ? C55 C56 C57 C58' -17.0(5) . . . . ? C51 C56 C57 C58' 167.2(4) . . . . ? C55 C56 C57 C58 13.4(3) . . . . ? C51 C56 C57 C58 -162.3(3) . . . . ? C58' C57 C58 C59 49.8(7) . . . . ? C56 C57 C58 C59 -47.4(4) . . . . ? C57 C58 C59 C60 63.9(5) . . . . ? C58 C57 C58' C59' -46.0(7) . . . . ? C56 C57 C58' C59' 49.2(8) . . . . ? C57 C58' C59' C60 -65.5(10) . . . . ? C56 C55 C60 C59 16.2(3) . . . . ? C54 C55 C60 C59 -166.0(3) . . . . ? C56 C55 C60 C59' -18.6(5) . . . . ? C54 C55 C60 C59' 159.2(5) . . . . ? C58 C59 C60 C55 -46.9(4) . . . . ? C58 C59 C60 C59' 47.4(6) . . . . ? C58' C59' C60 C55 49.0(9) . . . . ? C58' C59' C60 C59 -50.6(6) . . . . ? Zr1 O3 C61 N3 -3.81(17) . . . . ? Zr1 O3 C61 C62 170.00(14) . . . . ? C42 N3 C61 O3 -164.82(18) . . . . ? Zr1 N3 C61 O3 3.74(16) . . . . ? C42 N3 C61 C62 21.9(3) . . . . ? Zr1 N3 C61 C62 -169.56(17) . . . . ? C42 N3 C61 Zr1 -168.6(2) . . . . ? O4 Zr1 C61 O3 -144.90(10) . . . . ? O1 Zr1 C61 O3 71.43(11) . . . . ? N2 Zr1 C61 O3 -28.21(12) . . . . ? O2 Zr1 C61 O3 -79.69(11) . . . . ? N4 Zr1 C61 O3 155.72(10) . . . . ? N1 Zr1 C61 O3 64.06(14) . . . . ? N3 Zr1 C61 O3 -175.94(18) . . . . ? C71 Zr1 C61 O3 -175.33(10) . . . . ? C21 Zr1 C61 O3 64.16(11) . . . . ? C31 Zr1 C61 O3 -55.35(11) . . . . ? O4 Zr1 C61 N3 31.05(13) . . . . ? O1 Zr1 C61 N3 -112.63(12) . . . . ? O3 Zr1 C61 N3 175.94(18) . . . . ? N2 Zr1 C61 N3 147.73(11) . . . . ? O2 Zr1 C61 N3 96.25(12) . . . . ? N4 Zr1 C61 N3 -28.34(12) . . . . ? N1 Zr1 C61 N3 -119.99(12) . . . . ? C71 Zr1 C61 N3 0.62(13) . . . . ? C21 Zr1 C61 N3 -119.90(11) . . . . ? C31 Zr1 C61 N3 120.59(12) . . . . ? O4 Zr1 C61 C62 151.0(8) . . . . ? O1 Zr1 C61 C62 7.3(8) . . . . ? O3 Zr1 C61 C62 -64.1(8) . . . . ? N2 Zr1 C61 C62 -92.3(8) . . . . ? O2 Zr1 C61 C62 -143.8(8) . . . . ? N4 Zr1 C61 C62 91.6(8) . . . . ? N1 Zr1 C61 C62 -0.1(8) . . . . ? N3 Zr1 C61 C62 119.9(8) . . . . ? C71 Zr1 C61 C62 120.6(8) . . . . ? C21 Zr1 C61 C62 0.0(8) . . . . ? C31 Zr1 C61 C62 -119.5(8) . . . . ? O3 C61 C62 C67 78.6(2) . . . . ? N3 C61 C62 C67 -108.3(2) . . . . ? Zr1 C61 C62 C67 137.5(7) . . . . ? O3 C61 C62 C63 -94.7(2) . . . . ? N3 C61 C62 C63 78.4(2) . . . . ? Zr1 C61 C62 C63 -35.7(9) . . . . ? C67 C62 C63 C64 2.0(3) . . . . ? C61 C62 C63 C64 175.18(17) . . . . ? C67 C62 C63 C68 -175.89(18) . . . . ? C61 C62 C63 C68 -2.7(3) . . . . ? C62 C63 C64 C65 -0.7(3) . . . . ? C68 C63 C64 C65 177.17(19) . . . . ? C63 C64 C65 C66 -0.7(3) . . . . ? C63 C64 C65 C69 179.8(2) . . . . ? C64 C65 C66 C67 0.9(3) . . . . ? C69 C65 C66 C67 -179.6(2) . . . . ? C65 C66 C67 C62 0.3(3) . . . . ? C65 C66 C67 C70 -179.1(2) . . . . ? C63 C62 C67 C66 -1.8(3) . . . . ? C61 C62 C67 C66 -174.79(18) . . . . ? C63 C62 C67 C70 177.58(19) . . . . ? C61 C62 C67 C70 4.5(3) . . . . ? Zr1 O4 C71 N4 -14.62(15) . . . . ? Zr1 O4 C71 C72 164.09(14) . . . . ? C52 N4 C71 O4 166.42(16) . . . . ? Zr1 N4 C71 O4 14.04(15) . . . . ? C52 N4 C71 C72 -12.2(3) . . . . ? Zr1 N4 C71 C72 -164.55(17) . . . . ? C52 N4 C71 Zr1 152.4(2) . . . . ? O1 Zr1 C71 O4 -142.21(10) . . . . ? O3 Zr1 C71 O4 120.00(11) . . . . ? N2 Zr1 C71 O4 -17.09(13) . . . . ? O2 Zr1 C71 O4 39.34(11) . . . . ? N4 Zr1 C71 O4 -164.33(17) . . . . ? N1 Zr1 C71 O4 -87.93(11) . . . . ? N3 Zr1 C71 O4 123.93(11) . . . . ? C21 Zr1 C71 O4 -111.98(10) . . . . ? C61 Zr1 C71 O4 123.63(10) . . . . ? C31 Zr1 C71 O4 14.37(12) . . . . ? O4 Zr1 C71 N4 164.33(17) . . . . ? O1 Zr1 C71 N4 22.12(12) . . . . ? O3 Zr1 C71 N4 -75.67(13) . . . . ? N2 Zr1 C71 N4 147.24(10) . . . . ? O2 Zr1 C71 N4 -156.34(11) . . . . ? N1 Zr1 C71 N4 76.40(11) . . . . ? N3 Zr1 C71 N4 -71.74(11) . . . . ? C21 Zr1 C71 N4 52.35(12) . . . . ? C61 Zr1 C71 N4 -72.05(11) . . . . ? C31 Zr1 C71 N4 178.70(10) . . . . ? O4 Zr1 C71 C72 -74.1(5) . . . . ? O1 Zr1 C71 C72 143.7(5) . . . . ? O3 Zr1 C71 C72 45.9(6) . . . . ? N2 Zr1 C71 C72 -91.2(5) . . . . ? O2 Zr1 C71 C72 -34.8(5) . . . . ? N4 Zr1 C71 C72 121.6(6) . . . . ? N1 Zr1 C71 C72 -162.0(5) . . . . ? N3 Zr1 C71 C72 49.8(5) . . . . ? C21 Zr1 C71 C72 173.9(5) . . . . ? C61 Zr1 C71 C72 49.5(6) . . . . ? C31 Zr1 C71 C72 -59.7(5) . . . . ? O4 C71 C72 C77 121.4(2) . . . . ? N4 C71 C72 C77 -60.1(3) . . . . ? Zr1 C71 C72 C77 -173.0(4) . . . . ? O4 C71 C72 C73 -55.7(2) . . . . ? N4 C71 C72 C73 122.8(2) . . . . ? Zr1 C71 C72 C73 9.9(6) . . . . ? C77 C72 C73 C74 2.9(3) . . . . ? C71 C72 C73 C74 180.00(18) . . . . ? C77 C72 C73 C78 -175.47(19) . . . . ? C71 C72 C73 C78 1.6(3) . . . . ? C72 C73 C74 C75 -2.2(3) . . . . ? C78 C73 C74 C75 176.3(2) . . . . ? C73 C74 C75 C76 0.2(3) . . . . ? C73 C74 C75 C79 -179.4(2) . . . . ? C74 C75 C76 C77 1.2(3) . . . . ? C79 C75 C76 C77 -179.3(2) . . . . ? C75 C76 C77 C72 -0.4(3) . . . . ? C75 C76 C77 C80 -176.6(2) . . . . ? C73 C72 C77 C76 -1.7(3) . . . . ? C71 C72 C77 C76 -178.70(18) . . . . ? C73 C72 C77 C80 174.35(18) . . . . ? C71 C72 C77 C80 -2.7(3) . . . . ? C87 C82 C83 C84 0.7(4) . . . . ? C81 C82 C83 C84 -179.0(2) . . . . ? C82 C83 C84 C85 -1.5(4) . . . . ? C83 C84 C85 C86 0.7(4) . . . . ? C84 C85 C86 C87 0.7(5) . . . . ? C85 C86 C87 C82 -1.5(5) . . . . ? C83 C82 C87 C86 0.7(4) . . . . ? C81 C82 C87 C86 -179.5(3) . . . . ? C94 C89 C90 C91 0.0 . . . . ? C88 C89 C90 C91 179.95(8) . . . . ? C89 C90 C91 C92 0.0 . . . . ? C90 C91 C92 C93 0.0 . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C89 0.0 . . . . ? C90 C89 C94 C93 0.0 . . . . ? C88 C89 C94 C93 -179.95(8) . . . . ? C94' C89' C90' C91' 0.0 . . . . ? C88' C89' C90' C91' 179.98(9) . . . . ? C89' C90' C91' C92' 0.0 . . . . ? C90' C91' C92' C93' 0.0 . . . . ? C91' C92' C93' C94' 0.0 . . . . ? C92' C93' C94' C89' 0.0 . . . . ? C90' C89' C94' C93' 0.0 . . . . ? C88' C89' C94' C93' -179.98(9) . . . . ? C101 C96 C97 C98 0.0 . . . . ? C95 C96 C97 C98 176.9(3) . . . . ? C96 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C100 0.0 . . . . ? C98 C99 C100 C101 0.0 . . . . ? C99 C100 C101 C96 0.0 . . . . ? C97 C96 C101 C100 0.0 . . . . ? C95 C96 C101 C100 -177.0(3) . . . . ? C108 C103 C104 C105 0.0 . . . . ? C102 C103 C104 C105 178.3(13) . . . . ? C103 C104 C105 C106 0.0 . . . . ? C104 C105 C106 C107 0.0 . . . . ? C105 C106 C107 C108 0.0 . . . . ? C106 C107 C108 C103 0.0 . . . . ? C104 C103 C108 C107 0.0 . . . . ? C102 C103 C108 C107 -178.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.83 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.407 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.044