# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ana M Martins' 'Maria Duarte' 'Michael Fryzuk' 'Rui F. Munha' 'Luis Veiros' _publ_contact_author_name 'Ana M Martins' _publ_contact_author_email ANA.MARTINS@IST.UTL.PT _publ_section_title ; Synthesis and Structural Studies of Amido, Hydrazido and Imido Zirconium(IV) Complexes Incorporating a Diamido/Diamine Cyclam-Based Ligand ; # Attachment 'ZrCyclam_CIF_final.txt' data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 727732' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)Zr(NHtBu)2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H54 N6 Zr' _chemical_formula_sum 'C32 H54 N6 Zr' _chemical_formula_weight 614.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.69390(10) _cell_length_b 18.6721(2) _cell_length_c 18.6391(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.6300(10) _cell_angle_gamma 90.00 _cell_volume 3278.77(6) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2430 _cell_measurement_theta_max 32.6983 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8799 _exptl_absorpt_correction_T_max 0.9306 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; Solvent used: Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): Frames collected: Seconds exposure per frame: Degrees rotation per frame: Crystal-Detector distance (mm): ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 57862 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 30.51 _reflns_number_total 10001 _reflns_number_gt 7629 _reflns_threshold_expression >2\s(I) _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinoski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinoski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP3 _computing_publication_material SHELXL97 _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^ > 2\s(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^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10001 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.156939(12) 0.279245(6) -0.002923(6) 0.02191(4) Uani 1 1 d . . . N1 N 0.38800(11) 0.34890(5) 0.09321(5) 0.0230(2) Uani 1 1 d . . . N2 N 0.32536(11) 0.29538(5) -0.05428(5) 0.0225(2) Uani 1 1 d . . . N4 N 0.20153(12) 0.20741(5) 0.08524(5) 0.0238(2) Uani 1 1 d . . . N3 N 0.22360(11) 0.13257(5) -0.04751(5) 0.0254(2) Uani 1 1 d . . . C10 C 0.46913(14) 0.28793(7) 0.13319(7) 0.0266(3) Uani 1 1 d . . . H10A H 0.5643 0.3050 0.1595 0.032 Uiso 1 1 calc R . . H10B H 0.4825 0.2515 0.0968 0.032 Uiso 1 1 calc R . . C29 C -0.09997(15) 0.28210(7) -0.15610(8) 0.0324(3) Uani 1 1 d . . . C2 C 0.46426(13) 0.32466(7) -0.02235(7) 0.0259(3) Uani 1 1 d . . . H2A H 0.5017 0.3481 -0.0615 0.031 Uiso 1 1 calc R . . H2B H 0.5298 0.2854 -0.0012 0.031 Uiso 1 1 calc R . . N6 N -0.00656(12) 0.24976(7) -0.09028(6) 0.0306(2) Uani 1 1 d . . . C3 C 0.32833(14) 0.25299(7) -0.11999(7) 0.0280(3) Uani 1 1 d . . . H3A H 0.3703 0.2825 -0.1536 0.034 Uiso 1 1 calc R . . H3B H 0.2295 0.2415 -0.1461 0.034 Uiso 1 1 calc R . . N5 N 0.06515(12) 0.36725(6) 0.03498(6) 0.0282(2) Uani 1 1 d . . . C8 C 0.23831(14) 0.23962(7) 0.15854(6) 0.0271(3) Uani 1 1 d . . . H8A H 0.2042 0.2079 0.1933 0.033 Uiso 1 1 calc R . . H8B H 0.1875 0.2858 0.1569 0.033 Uiso 1 1 calc R . . C1 C 0.45844(13) 0.37823(7) 0.03703(7) 0.0265(3) Uani 1 1 d . . . H1A H 0.5562 0.3931 0.0615 0.032 Uiso 1 1 calc R . . H1B H 0.4062 0.4212 0.0143 0.032 Uiso 1 1 calc R . . C11 C 0.37035(14) 0.40761(7) 0.14399(7) 0.0278(3) Uani 1 1 d . . . H11A H 0.3281 0.3872 0.1829 0.033 Uiso 1 1 calc R . . H11B H 0.3015 0.4425 0.1158 0.033 Uiso 1 1 calc R . . C5 C 0.37702(14) 0.13897(7) -0.04132(7) 0.0302(3) Uani 1 1 d . . . H5A H 0.4181 0.0904 -0.0414 0.036 Uiso 1 1 calc R . . H5B H 0.4216 0.1618 0.0064 0.036 Uiso 1 1 calc R . . C12 C 0.50400(14) 0.44782(7) 0.18117(7) 0.0287(3) Uani 1 1 d . . . C6 C 0.19214(16) 0.09476(7) 0.01626(7) 0.0322(3) Uani 1 1 d . . . H6A H 0.2353 0.0465 0.0197 0.039 Uiso 1 1 calc R . . H6B H 0.0881 0.0886 0.0078 0.039 Uiso 1 1 calc R . . C19 C 0.18887(15) 0.01893(7) -0.12456(7) 0.0322(3) Uani 1 1 d . . . C9 C 0.39708(15) 0.25295(8) 0.18860(7) 0.0295(3) Uani 1 1 d . . . H9A H 0.4103 0.2840 0.2328 0.035 Uiso 1 1 calc R . . H9B H 0.4443 0.2067 0.2044 0.035 Uiso 1 1 calc R . . C18 C 0.14924(15) 0.09633(7) -0.11658(7) 0.0297(3) Uani 1 1 d . . . H18A H 0.1681 0.1235 -0.1588 0.036 Uiso 1 1 calc R . . H18B H 0.0459 0.0987 -0.1200 0.036 Uiso 1 1 calc R . . C4 C 0.41284(15) 0.18261(7) -0.10362(8) 0.0328(3) Uani 1 1 d . . . H4A H 0.3938 0.1531 -0.1490 0.039 Uiso 1 1 calc R . . H4B H 0.5155 0.1940 -0.0905 0.039 Uiso 1 1 calc R . . C7 C 0.24603(16) 0.13316(7) 0.08835(7) 0.0319(3) Uani 1 1 d . . . H7A H 0.2109 0.1083 0.1275 0.038 Uiso 1 1 calc R . . H7B H 0.3510 0.1310 0.1018 0.038 Uiso 1 1 calc R . . C25 C -0.05825(14) 0.38292(7) 0.06530(8) 0.0322(3) Uani 1 1 d . . . C17 C 0.59270(15) 0.42444(8) 0.24666(7) 0.0348(3) Uani 1 1 d . . . H17 H 0.5681 0.3831 0.2706 0.042 Uiso 1 1 calc R . . C13 C 0.54221(16) 0.50970(7) 0.14934(8) 0.0365(3) Uani 1 1 d . . . H13 H 0.4808 0.5276 0.1056 0.044 Uiso 1 1 calc R . . C15 C 0.75541(16) 0.52106(8) 0.24382(8) 0.0418(4) Uani 1 1 d . . . H15 H 0.8419 0.5451 0.2647 0.050 Uiso 1 1 calc R . . C20 C 0.11468(19) -0.03529(8) -0.09983(8) 0.0444(4) Uani 1 1 d . . . H20 H 0.0348 -0.0233 -0.0809 0.053 Uiso 1 1 calc R . . C14 C 0.66653(17) 0.54601(8) 0.17914(8) 0.0414(4) Uani 1 1 d . . . H14 H 0.6910 0.5877 0.1556 0.050 Uiso 1 1 calc R . . C26 C -0.13444(15) 0.31273(7) 0.07186(8) 0.0364(3) Uani 1 1 d . . . H26A H -0.1656 0.2908 0.0229 0.055 Uiso 1 1 calc R . . H26B H -0.2172 0.3221 0.0921 0.055 Uiso 1 1 calc R . . H26C H -0.0696 0.2801 0.1047 0.055 Uiso 1 1 calc R . . C16 C 0.71717(16) 0.46105(8) 0.27748(8) 0.0408(3) Uani 1 1 d . . . H16 H 0.7768 0.4445 0.3224 0.049 Uiso 1 1 calc R . . C32 C -0.25334(18) 0.28402(10) -0.14972(10) 0.0549(5) Uani 1 1 d . . . H32A H -0.2864 0.2351 -0.1447 0.082 Uiso 1 1 calc R . . H32B H -0.3126 0.3061 -0.1941 0.082 Uiso 1 1 calc R . . H32C H -0.2600 0.3121 -0.1062 0.082 Uiso 1 1 calc R . . C28 C -0.01197(19) 0.41708(9) 0.14207(9) 0.0495(4) Uani 1 1 d . . . H28A H 0.0518 0.3843 0.1754 0.074 Uiso 1 1 calc R . . H28B H -0.0958 0.4265 0.1615 0.074 Uiso 1 1 calc R . . H28C H 0.0376 0.4622 0.1384 0.074 Uiso 1 1 calc R . . C24 C 0.30081(17) -0.00005(8) -0.15524(9) 0.0450(4) Uani 1 1 d . . . H24 H 0.3502 0.0359 -0.1752 0.054 Uiso 1 1 calc R . . C23 C 0.3413(2) -0.07157(10) -0.15692(11) 0.0631(6) Uani 1 1 d . . . H23 H 0.4195 -0.0842 -0.1770 0.076 Uiso 1 1 calc R . . C31 C -0.09376(19) 0.23847(9) -0.22484(8) 0.0464(4) Uani 1 1 d . . . H31A H 0.0038 0.2380 -0.2311 0.070 Uiso 1 1 calc R . . H31B H -0.1566 0.2602 -0.2684 0.070 Uiso 1 1 calc R . . H31C H -0.1246 0.1893 -0.2190 0.070 Uiso 1 1 calc R . . C30 C -0.04706(19) 0.35811(8) -0.16438(9) 0.0477(4) Uani 1 1 d . . . H30A H -0.0474 0.3857 -0.1197 0.072 Uiso 1 1 calc R . . H30B H -0.1096 0.3813 -0.2071 0.072 Uiso 1 1 calc R . . H30C H 0.0497 0.3561 -0.1717 0.072 Uiso 1 1 calc R . . C27 C -0.16031(15) 0.43486(9) 0.01470(10) 0.0498(4) Uani 1 1 d . . . H27A H -0.1101 0.4794 0.0095 0.075 Uiso 1 1 calc R . . H27B H -0.2409 0.4454 0.0364 0.075 Uiso 1 1 calc R . . H27C H -0.1949 0.4129 -0.0340 0.075 Uiso 1 1 calc R . . C22 C 0.2680(2) -0.12386(9) -0.12951(11) 0.0678(6) Uani 1 1 d . . . H22 H 0.2971 -0.1724 -0.1298 0.081 Uiso 1 1 calc R . . C21 C 0.1531(2) -0.10634(9) -0.10177(10) 0.0608(5) Uani 1 1 d . . . H21 H 0.1008 -0.1426 -0.0842 0.073 Uiso 1 1 calc R . . H6 H -0.0148(18) 0.2085(8) -0.0900(9) 0.038(5) Uiso 1 1 d . . . H5 H 0.1087(17) 0.4003(8) 0.0385(8) 0.034(5) Uiso 1 1 d . . . 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 0.01807(6) 0.02615(7) 0.02281(6) 0.00592(4) 0.00743(5) 0.00093(5) N1 0.0200(5) 0.0257(5) 0.0242(5) -0.0013(4) 0.0073(4) 0.0005(4) N2 0.0214(5) 0.0258(5) 0.0221(5) -0.0013(4) 0.0086(4) -0.0040(4) N4 0.0265(6) 0.0238(5) 0.0225(5) 0.0021(4) 0.0083(4) -0.0002(4) N3 0.0253(5) 0.0251(5) 0.0266(5) 0.0027(4) 0.0075(4) -0.0015(4) C10 0.0226(6) 0.0308(7) 0.0245(6) -0.0015(5) 0.0021(5) 0.0039(5) C29 0.0259(7) 0.0393(8) 0.0284(7) 0.0044(5) -0.0007(5) -0.0011(6) C2 0.0217(6) 0.0324(6) 0.0259(6) -0.0016(5) 0.0103(5) -0.0055(5) N6 0.0293(6) 0.0291(6) 0.0310(6) 0.0034(5) 0.0027(5) 0.0014(5) C3 0.0315(7) 0.0314(6) 0.0239(6) -0.0019(5) 0.0123(5) -0.0063(6) N5 0.0192(5) 0.0296(6) 0.0374(6) 0.0019(5) 0.0098(5) -0.0015(5) C8 0.0332(7) 0.0285(6) 0.0217(6) 0.0034(5) 0.0107(5) 0.0008(5) C1 0.0226(6) 0.0290(6) 0.0288(6) -0.0021(5) 0.0080(5) -0.0068(5) C11 0.0244(6) 0.0295(6) 0.0308(6) -0.0048(5) 0.0092(5) 0.0008(5) C5 0.0270(7) 0.0282(6) 0.0360(7) -0.0036(5) 0.0086(6) 0.0012(5) C12 0.0260(7) 0.0302(6) 0.0304(6) -0.0072(5) 0.0076(5) 0.0008(5) C6 0.0424(8) 0.0233(6) 0.0338(7) 0.0038(5) 0.0148(6) -0.0010(6) C19 0.0317(7) 0.0297(7) 0.0321(7) -0.0059(5) 0.0015(6) -0.0020(6) C9 0.0330(7) 0.0331(7) 0.0210(6) 0.0022(5) 0.0033(5) 0.0027(6) C18 0.0290(7) 0.0288(6) 0.0315(7) 0.0001(5) 0.0072(6) -0.0017(5) C4 0.0305(7) 0.0335(7) 0.0397(7) -0.0101(6) 0.0187(6) -0.0061(6) C7 0.0433(8) 0.0257(6) 0.0284(6) 0.0072(5) 0.0117(6) 0.0038(6) C25 0.0243(7) 0.0287(7) 0.0480(8) 0.0050(6) 0.0172(6) 0.0054(5) C17 0.0362(8) 0.0389(8) 0.0290(7) -0.0057(6) 0.0070(6) -0.0008(6) C13 0.0376(8) 0.0297(7) 0.0388(8) -0.0037(6) 0.0023(6) -0.0032(6) C15 0.0328(8) 0.0460(9) 0.0463(9) -0.0232(7) 0.0084(7) -0.0079(7) C20 0.0574(10) 0.0309(7) 0.0460(9) -0.0056(6) 0.0141(8) -0.0075(7) C14 0.0447(9) 0.0313(7) 0.0479(9) -0.0093(6) 0.0102(7) -0.0086(7) C26 0.0288(7) 0.0350(8) 0.0500(9) 0.0102(6) 0.0185(6) 0.0025(6) C16 0.0359(8) 0.0516(9) 0.0313(7) -0.0117(6) 0.0005(6) 0.0008(7) C32 0.0268(8) 0.0756(13) 0.0574(11) -0.0017(9) 0.0001(8) 0.0026(8) C28 0.0502(10) 0.0442(9) 0.0630(11) -0.0125(8) 0.0313(9) 0.0029(8) C24 0.0377(9) 0.0428(8) 0.0538(10) -0.0179(7) 0.0092(7) -0.0034(7) C23 0.0427(10) 0.0582(11) 0.0787(13) -0.0381(10) -0.0049(9) 0.0131(9) C31 0.0456(10) 0.0565(10) 0.0316(8) 0.0008(7) -0.0016(7) -0.0011(8) C30 0.0548(10) 0.0426(9) 0.0383(8) 0.0109(7) -0.0041(7) -0.0054(8) C27 0.0268(8) 0.0404(8) 0.0852(13) 0.0242(8) 0.0192(8) 0.0100(6) C22 0.0780(14) 0.0317(9) 0.0723(12) -0.0185(8) -0.0251(11) 0.0148(9) C21 0.0916(16) 0.0301(8) 0.0545(11) -0.0043(7) 0.0051(10) -0.0036(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N6 2.0616(11) . ? Zr1 N5 2.0706(11) . ? Zr1 N4 2.0860(10) . ? Zr1 N2 2.0998(10) . ? N1 C10 1.4810(15) . ? N1 C1 1.4832(15) . ? N1 C11 1.4842(15) . ? N2 C2 1.4452(15) . ? N2 C3 1.4641(15) . ? N4 C7 1.4491(16) . ? N4 C8 1.4582(15) . ? N3 C5 1.4692(16) . ? N3 C6 1.4748(15) . ? N3 C18 1.4824(16) . ? C10 C9 1.5236(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C29 N6 1.4717(17) . ? C29 C32 1.520(2) . ? C29 C30 1.529(2) . ? C29 C31 1.532(2) . ? C2 C1 1.5027(16) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N6 H6 0.774(15) . ? C3 C4 1.541(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N5 C25 1.4679(16) . ? N5 H5 0.742(15) . ? C8 C9 1.5291(19) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 C12 1.5164(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C5 C4 1.5242(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C12 C17 1.3877(19) . ? C12 C13 1.3884(19) . ? C6 C7 1.5038(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C19 C20 1.382(2) . ? C19 C24 1.387(2) . ? C19 C18 1.5117(18) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C25 C26 1.5234(18) . ? C25 C28 1.534(2) . ? C25 C27 1.5393(19) . ? C17 C16 1.388(2) . ? C17 H17 0.9500 . ? C13 C14 1.380(2) . ? C13 H13 0.9500 . ? C15 C16 1.377(2) . ? C15 C14 1.387(2) . ? C15 H15 0.9500 . ? C20 C21 1.381(2) . ? C20 H20 0.9500 . ? C14 H14 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C16 H16 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C24 C23 1.394(2) . ? C24 H24 0.9500 . ? C23 C22 1.375(3) . ? C23 H23 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C22 C21 1.373(3) . ? C22 H22 0.9500 . ? C21 H21 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 N6 Zr1 N5 99.74(5) . . ? N6 Zr1 N4 115.37(4) . . ? N5 Zr1 N4 105.52(4) . . ? N6 Zr1 N2 102.35(4) . . ? N5 Zr1 N2 118.98(4) . . ? N4 Zr1 N2 114.35(4) . . ? C10 N1 C1 111.15(10) . . ? C10 N1 C11 111.98(9) . . ? C1 N1 C11 108.60(9) . . ? C2 N2 C3 110.42(10) . . ? C2 N2 Zr1 128.00(7) . . ? C3 N2 Zr1 118.33(8) . . ? C7 N4 C8 110.64(10) . . ? C7 N4 Zr1 130.63(8) . . ? C8 N4 Zr1 115.62(7) . . ? C5 N3 C6 111.93(10) . . ? C5 N3 C18 112.42(10) . . ? C6 N3 C18 109.31(10) . . ? N1 C10 C9 113.37(11) . . ? N1 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N6 C29 C32 111.45(12) . . ? N6 C29 C30 108.05(11) . . ? C32 C29 C30 110.10(13) . . ? N6 C29 C31 109.96(12) . . ? C32 C29 C31 108.06(13) . . ? C30 C29 C31 109.21(13) . . ? N2 C2 C1 111.23(10) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C29 N6 Zr1 139.14(9) . . ? C29 N6 H6 111.7(12) . . ? Zr1 N6 H6 108.8(12) . . ? N2 C3 C4 114.20(11) . . ? N2 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N2 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C25 N5 Zr1 138.10(9) . . ? C25 N5 H5 107.4(12) . . ? Zr1 N5 H5 114.1(12) . . ? N4 C8 C9 114.41(10) . . ? N4 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N4 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C1 C2 112.19(10) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N1 C11 C12 116.28(10) . . ? N1 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N1 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? N3 C5 C4 113.07(11) . . ? N3 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N3 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C17 C12 C13 117.73(13) . . ? C17 C12 C11 122.12(12) . . ? C13 C12 C11 120.14(12) . . ? N3 C6 C7 113.42(11) . . ? N3 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C20 C19 C24 118.01(13) . . ? C20 C19 C18 120.21(13) . . ? C24 C19 C18 121.78(13) . . ? C10 C9 C8 113.83(10) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N3 C18 C19 116.04(11) . . ? N3 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? N3 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C5 C4 C3 113.63(10) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N4 C7 C6 112.52(11) . . ? N4 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N4 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N5 C25 C26 108.29(10) . . ? N5 C25 C28 110.88(12) . . ? C26 C25 C28 108.89(12) . . ? N5 C25 C27 110.74(11) . . ? C26 C25 C27 109.72(12) . . ? C28 C25 C27 108.31(13) . . ? C12 C17 C16 120.47(13) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C14 C13 C12 122.17(14) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C16 C15 C14 119.39(14) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C21 C20 C19 122.01(17) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C13 C14 C15 119.31(14) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C15 C16 C17 120.88(14) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C24 C23 120.38(16) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C22 C23 C24 119.94(18) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C22 C23 120.44(16) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C21 C20 119.12(18) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? 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 N6 Zr1 N2 C2 172.32(10) . . . . ? N5 Zr1 N2 C2 63.70(11) . . . . ? N4 Zr1 N2 C2 -62.19(11) . . . . ? N6 Zr1 N2 C3 -30.16(10) . . . . ? N5 Zr1 N2 C3 -138.78(9) . . . . ? N4 Zr1 N2 C3 95.33(9) . . . . ? N6 Zr1 N4 C7 60.60(13) . . . . ? N5 Zr1 N4 C7 169.62(11) . . . . ? N2 Zr1 N4 C7 -57.73(12) . . . . ? N6 Zr1 N4 C8 -141.51(9) . . . . ? N5 Zr1 N4 C8 -32.49(10) . . . . ? N2 Zr1 N4 C8 100.17(9) . . . . ? C1 N1 C10 C9 -176.70(10) . . . . ? C11 N1 C10 C9 61.65(13) . . . . ? C3 N2 C2 C1 170.31(10) . . . . ? Zr1 N2 C2 C1 -30.73(15) . . . . ? C32 C29 N6 Zr1 -113.18(14) . . . . ? C30 C29 N6 Zr1 7.9(2) . . . . ? C31 C29 N6 Zr1 127.01(13) . . . . ? N5 Zr1 N6 C29 51.82(14) . . . . ? N4 Zr1 N6 C29 164.26(13) . . . . ? N2 Zr1 N6 C29 -70.92(14) . . . . ? C2 N2 C3 C4 69.31(13) . . . . ? Zr1 N2 C3 C4 -91.94(12) . . . . ? N6 Zr1 N5 C25 61.59(14) . . . . ? N4 Zr1 N5 C25 -58.33(14) . . . . ? N2 Zr1 N5 C25 171.66(12) . . . . ? C7 N4 C8 C9 71.59(14) . . . . ? Zr1 N4 C8 C9 -90.64(11) . . . . ? C10 N1 C1 C2 63.52(13) . . . . ? C11 N1 C1 C2 -172.87(10) . . . . ? N2 C2 C1 N1 52.53(14) . . . . ? C10 N1 C11 C12 68.10(14) . . . . ? C1 N1 C11 C12 -55.01(14) . . . . ? C6 N3 C5 C4 -175.76(10) . . . . ? C18 N3 C5 C4 60.75(13) . . . . ? N1 C11 C12 C17 -86.42(15) . . . . ? N1 C11 C12 C13 92.77(15) . . . . ? C5 N3 C6 C7 62.77(14) . . . . ? C18 N3 C6 C7 -172.01(11) . . . . ? N1 C10 C9 C8 45.48(15) . . . . ? N4 C8 C9 C10 46.31(15) . . . . ? C5 N3 C18 C19 64.46(14) . . . . ? C6 N3 C18 C19 -60.47(14) . . . . ? C20 C19 C18 N3 90.64(16) . . . . ? C24 C19 C18 N3 -88.20(16) . . . . ? N3 C5 C4 C3 46.10(15) . . . . ? N2 C3 C4 C5 47.40(15) . . . . ? C8 N4 C7 C6 171.81(11) . . . . ? Zr1 N4 C7 C6 -29.45(17) . . . . ? N3 C6 C7 N4 51.62(16) . . . . ? Zr1 N5 C25 C26 2.34(19) . . . . ? Zr1 N5 C25 C28 121.74(13) . . . . ? Zr1 N5 C25 C27 -118.00(13) . . . . ? C13 C12 C17 C16 -1.86(19) . . . . ? C11 C12 C17 C16 177.35(13) . . . . ? C17 C12 C13 C14 2.6(2) . . . . ? C11 C12 C13 C14 -176.60(13) . . . . ? C24 C19 C20 C21 3.1(2) . . . . ? C18 C19 C20 C21 -175.79(15) . . . . ? C12 C13 C14 C15 -1.4(2) . . . . ? C16 C15 C14 C13 -0.7(2) . . . . ? C14 C15 C16 C17 1.5(2) . . . . ? C12 C17 C16 C15 -0.1(2) . . . . ? C20 C19 C24 C23 -3.6(2) . . . . ? C18 C19 C24 C23 175.28(14) . . . . ? C19 C24 C23 C22 1.5(3) . . . . ? C24 C23 C22 C21 1.3(3) . . . . ? C23 C22 C21 C20 -1.8(3) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.421 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.076 #===end data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 727733' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)Zr(NH2,6Me-Ph)2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H54 N6 Zr, C6 H14' _chemical_formula_sum 'C46 H68 N6 Zr' _chemical_formula_weight 796.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.007(4) _cell_length_b 23.681(4) _cell_length_c 9.2392(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.377(16) _cell_angle_gamma 90.00 _cell_volume 4291.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2008 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 18.55 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9169 _exptl_absorpt_correction_T_max 0.9854 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23659 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.0900 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.76 _reflns_number_total 4081 _reflns_number_gt 2742 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP3 _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4081 _refine_ls_number_parameters 234 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.025 _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 C1 C 0.64437(18) 0.20238(15) 0.3630(3) 0.0275(9) Uani 1 1 d . . . H1A H 0.6702 0.2353 0.4041 0.033 Uiso 1 1 calc R . . H1B H 0.6759 0.1711 0.3673 0.033 Uiso 1 1 calc R . . C2 C 0.59266(18) 0.18855(15) 0.4560(4) 0.0275(9) Uani 1 1 d . . . H2A H 0.5731 0.1517 0.4281 0.033 Uiso 1 1 calc R . . H2B H 0.6152 0.1868 0.5590 0.033 Uiso 1 1 calc R . . C3 C 0.49579(17) 0.22327(17) 0.5485(3) 0.0294(8) Uani 1 1 d . . . H3A H 0.4663 0.2560 0.5446 0.035 Uiso 1 1 calc R . . H3B H 0.5248 0.2222 0.6459 0.035 Uiso 1 1 calc R . . C4 C 0.45182(18) 0.17017(16) 0.5276(4) 0.0296(9) Uani 1 1 d . . . H4A H 0.4174 0.1730 0.5879 0.036 Uiso 1 1 calc R . . H4B H 0.4801 0.1377 0.5614 0.036 Uiso 1 1 calc R . . C5 C 0.41692(18) 0.16116(15) 0.3668(4) 0.0283(9) Uani 1 1 d . . . H5A H 0.4500 0.1463 0.3127 0.034 Uiso 1 1 calc R . . H5B H 0.3812 0.1332 0.3628 0.034 Uiso 1 1 calc R . . C6 C 0.33501(18) 0.23868(15) 0.3688(4) 0.0282(9) Uani 1 1 d . . . H6A H 0.3243 0.2763 0.3294 0.034 Uiso 1 1 calc R . . H6B H 0.3551 0.2427 0.4728 0.034 Uiso 1 1 calc R . . C7 C 0.26859(18) 0.20609(15) 0.3561(4) 0.0277(9) Uani 1 1 d . . . C8 C 0.21227(18) 0.22156(17) 0.2508(4) 0.0323(9) Uani 1 1 d . . . H8 H 0.2151 0.2527 0.1910 0.039 Uiso 1 1 calc R . . C9 C 0.15215(19) 0.19160(17) 0.2333(4) 0.0347(10) Uani 1 1 d . . . H9 H 0.1150 0.2026 0.1616 0.042 Uiso 1 1 calc R . . C10 C 0.14657(19) 0.14532(18) 0.3212(4) 0.0379(10) Uani 1 1 d . . . H10 H 0.1062 0.1247 0.3078 0.045 Uiso 1 1 calc R . . C11 C 0.2019(2) 0.13003(17) 0.4297(4) 0.0377(10) Uani 1 1 d . . . H11 H 0.1985 0.0994 0.4910 0.045 Uiso 1 1 calc R . . C12 C 0.26230(19) 0.16034(16) 0.4469(4) 0.0337(9) Uani 1 1 d . . . H12 H 0.2991 0.1499 0.5202 0.040 Uiso 1 1 calc R . . C13 C 0.59685(19) 0.38920(15) 0.2020(4) 0.0281(9) Uani 1 1 d . . . C14 C 0.65674(19) 0.41456(16) 0.2848(4) 0.0311(9) Uani 1 1 d . . . C15 C 0.6754(2) 0.46760(16) 0.2480(4) 0.0377(10) Uani 1 1 d . . . H15 H 0.7134 0.4846 0.3057 0.045 Uiso 1 1 calc R . . C16 C 0.6392(2) 0.49660(18) 0.1276(4) 0.0421(10) Uani 1 1 d . . . H16 H 0.6527 0.5324 0.1037 0.051 Uiso 1 1 calc R . . C17 C 0.5820(2) 0.47071(16) 0.0431(4) 0.0347(9) Uani 1 1 d . . . H17 H 0.5579 0.4893 -0.0395 0.042 Uiso 1 1 calc R . . C18 C 0.56022(18) 0.41816(16) 0.0789(4) 0.0301(9) Uani 1 1 d . . . C19 C 0.7001(2) 0.38324(17) 0.4117(4) 0.0418(10) Uani 1 1 d . . . H19A H 0.7202 0.3508 0.3747 0.063 Uiso 1 1 calc R . . H19B H 0.6723 0.3712 0.4795 0.063 Uiso 1 1 calc R . . H19C H 0.7355 0.4077 0.4616 0.063 Uiso 1 1 calc R . . C20 C 0.49822(19) 0.39200(17) -0.0154(4) 0.0376(10) Uani 1 1 d . . . H20A H 0.4616 0.3917 0.0378 0.056 Uiso 1 1 calc R . . H20B H 0.5085 0.3540 -0.0400 0.056 Uiso 1 1 calc R . . H20C H 0.4850 0.4136 -0.1044 0.056 Uiso 1 1 calc R . . N1 N 0.38685(14) 0.21379(12) 0.2936(3) 0.0244(7) Uani 1 1 d . . . N2 N 0.53865(14) 0.23015(12) 0.4385(3) 0.0231(7) Uani 1 1 d . . . N3 N 0.57620(15) 0.33502(13) 0.2362(3) 0.0345(8) Uani 1 1 d . . . H3 H 0.6136 0.3170 0.2664 0.041 Uiso 1 1 calc R . . Zr1 Zr 0.5000 0.27674(2) 0.2500 0.02309(17) Uani 1 2 d S . . C23 C 0.3467 0.0019 0.5830 0.381(12) Uani 1 1 d DU . . H23A H 0.3165 0.0328 0.5498 0.571 Uiso 1 1 calc R . . H23B H 0.3205 -0.0315 0.5916 0.571 Uiso 1 1 calc R . . H23C H 0.3756 -0.0047 0.5131 0.571 Uiso 1 1 calc R . . C21 C 0.3891 0.0158 0.7280 0.406(15) Uani 1 1 d DU . . H21A H 0.3761 -0.0067 0.8059 0.487 Uiso 1 1 calc R . . H21B H 0.3856 0.0555 0.7510 0.487 Uiso 1 1 calc R . . C22 C 0.4663 -0.0002 0.7056 0.487(17) Uani 1 1 d DU . . H22A H 0.4611 -0.0387 0.6688 0.584 Uiso 1 1 calc R . . H22B H 0.4713 0.0225 0.6212 0.584 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 C1 0.027(2) 0.032(2) 0.0213(17) 0.0026(15) 0.0008(15) 0.0023(17) C2 0.031(2) 0.030(2) 0.0209(17) 0.0030(15) 0.0011(15) 0.0040(17) C3 0.028(2) 0.042(2) 0.0184(16) 0.0001(17) 0.0048(14) -0.0020(19) C4 0.028(2) 0.035(2) 0.0265(19) 0.0082(17) 0.0081(16) -0.0024(17) C5 0.031(2) 0.027(2) 0.0274(19) 0.0025(16) 0.0054(16) -0.0045(17) C6 0.030(2) 0.030(2) 0.0251(18) -0.0024(15) 0.0069(15) -0.0025(16) C7 0.029(2) 0.032(2) 0.0238(18) -0.0061(15) 0.0081(15) 0.0001(16) C8 0.038(2) 0.032(2) 0.0289(18) 0.0031(18) 0.0104(16) 0.006(2) C9 0.025(2) 0.052(3) 0.0265(19) -0.0039(19) 0.0036(16) -0.0027(19) C10 0.028(2) 0.049(3) 0.038(2) -0.007(2) 0.0104(18) -0.010(2) C11 0.040(2) 0.042(3) 0.034(2) 0.0026(19) 0.0139(18) -0.006(2) C12 0.030(2) 0.044(3) 0.0272(19) 0.0031(18) 0.0064(16) -0.0026(19) C13 0.032(2) 0.020(2) 0.036(2) -0.0010(17) 0.0165(17) 0.0053(17) C14 0.038(2) 0.030(2) 0.0274(19) -0.0004(17) 0.0116(17) 0.0021(18) C15 0.042(2) 0.030(2) 0.039(2) -0.0050(19) 0.0043(19) -0.0049(19) C16 0.047(3) 0.032(2) 0.048(2) 0.003(2) 0.010(2) -0.006(2) C17 0.037(2) 0.031(2) 0.036(2) 0.0074(18) 0.0062(18) 0.0039(19) C18 0.027(2) 0.031(2) 0.035(2) -0.0016(17) 0.0114(16) 0.0025(17) C19 0.048(3) 0.038(2) 0.039(2) -0.0006(19) 0.0064(19) 0.003(2) C20 0.033(2) 0.036(2) 0.045(2) 0.0001(19) 0.0094(18) 0.0007(18) N1 0.0269(16) 0.0256(18) 0.0204(14) -0.0027(13) 0.0039(12) -0.0023(13) N2 0.0252(16) 0.0257(17) 0.0195(13) -0.0002(13) 0.0069(11) -0.0004(13) N3 0.0289(18) 0.0258(18) 0.052(2) 0.0100(15) 0.0160(15) 0.0067(14) Zr1 0.0280(3) 0.0238(3) 0.0172(2) 0.000 0.00375(18) 0.000 C23 0.245(16) 0.38(2) 0.43(2) 0.141(19) -0.139(16) -0.027(16) C21 0.182(13) 0.33(2) 0.63(3) 0.17(2) -0.100(18) -0.088(14) C22 0.89(5) 0.328(19) 0.29(2) 0.116(19) 0.26(3) 0.06(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.483(4) 2_655 ? C1 C2 1.505(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.447(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.463(4) . ? C3 C4 1.525(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.527(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.488(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.480(4) . ? C6 C7 1.521(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.384(5) . ? C7 C12 1.391(5) . ? C8 C9 1.378(5) . ? C8 H8 0.9300 . ? C9 C10 1.382(5) . ? C9 H9 0.9300 . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 C12 1.387(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 N3 1.403(4) . ? C13 C18 1.404(5) . ? C13 C14 1.421(5) . ? C14 C15 1.372(5) . ? C14 C19 1.509(5) . ? C15 C16 1.384(5) . ? C15 H15 0.9300 . ? C16 C17 1.393(5) . ? C16 H16 0.9300 . ? C17 C18 1.380(5) . ? C17 H17 0.9300 . ? C18 C20 1.502(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N1 C1 1.483(4) 2_655 ? N2 Zr1 2.078(3) . ? N3 Zr1 2.079(3) . ? N3 H3 0.8600 . ? Zr1 N2 2.078(3) 2_655 ? Zr1 N3 2.079(3) 2_655 ? C23 C21 1.4745(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C21 C22 1.6421(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C22 1.4344(3) 2_656 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 C1 C2 113.1(3) 2_655 . ? N1 C1 H1A 109.0 2_655 . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 2_655 . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N2 C2 C1 111.7(3) . . ? N2 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 114.0(3) . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.6 . . ? C3 C4 C5 112.3(3) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C4 113.1(3) . . ? N1 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C6 C7 116.4(3) . . ? N1 C6 H6A 108.2 . . ? C7 C6 H6A 108.2 . . ? N1 C6 H6B 108.2 . . ? C7 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? C8 C7 C12 118.1(3) . . ? C8 C7 C6 119.8(3) . . ? C12 C7 C6 122.0(3) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 120.6(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 119.1(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.9(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? N3 C13 C18 119.9(3) . . ? N3 C13 C14 121.3(3) . . ? C18 C13 C14 118.7(3) . . ? C15 C14 C13 119.7(3) . . ? C15 C14 C19 120.0(3) . . ? C13 C14 C19 120.4(3) . . ? C14 C15 C16 121.9(4) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C17 118.2(4) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 121.8(4) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C13 119.7(3) . . ? C17 C18 C20 119.8(3) . . ? C13 C18 C20 120.5(3) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 N1 C1 109.3(3) . 2_655 ? C6 N1 C5 112.2(3) . . ? C1 N1 C5 110.2(3) 2_655 . ? C2 N2 C3 111.9(3) . . ? C2 N2 Zr1 127.0(2) . . ? C3 N2 Zr1 118.0(2) . . ? C13 N3 Zr1 150.8(2) . . ? C13 N3 H3 104.6 . . ? Zr1 N3 H3 104.6 . . ? N2 Zr1 N2 115.85(15) 2_655 . ? N2 Zr1 N3 117.21(11) 2_655 . ? N2 Zr1 N3 104.35(11) . . ? N2 Zr1 N3 104.35(11) 2_655 2_655 ? N2 Zr1 N3 117.21(11) . 2_655 ? N3 Zr1 N3 96.81(17) . 2_655 ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C21 C22 102.727(15) . . ? C23 C21 H21A 111.2 . . ? C22 C21 H21A 111.2 . . ? C23 C21 H21B 111.2 . . ? C22 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? C22 C22 C21 136.920(11) 2_656 . ? C22 C22 H22A 102.9 2_656 . ? C21 C22 H22A 102.9 . . ? C22 C22 H22B 102.9 2_656 . ? C21 C22 H22B 102.9 . . ? H22A C22 H22B 105.1 . . ? 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 C1 C2 N2 -50.9(4) 2_655 . . . ? N2 C3 C4 C5 -45.0(4) . . . . ? C3 C4 C5 N1 -44.1(4) . . . . ? N1 C6 C7 C8 -97.6(4) . . . . ? N1 C6 C7 C12 81.9(4) . . . . ? C12 C7 C8 C9 -1.9(5) . . . . ? C6 C7 C8 C9 177.7(3) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? C9 C10 C11 C12 -1.3(6) . . . . ? C10 C11 C12 C7 -0.3(6) . . . . ? C8 C7 C12 C11 1.9(5) . . . . ? C6 C7 C12 C11 -177.7(3) . . . . ? N3 C13 C14 C15 180.0(3) . . . . ? C18 C13 C14 C15 3.5(5) . . . . ? N3 C13 C14 C19 0.5(5) . . . . ? C18 C13 C14 C19 -176.0(3) . . . . ? C13 C14 C15 C16 -3.0(6) . . . . ? C19 C14 C15 C16 176.4(4) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? C15 C16 C17 C18 1.6(6) . . . . ? C16 C17 C18 C13 -1.1(6) . . . . ? C16 C17 C18 C20 179.9(4) . . . . ? N3 C13 C18 C17 -178.0(3) . . . . ? C14 C13 C18 C17 -1.5(5) . . . . ? N3 C13 C18 C20 1.0(5) . . . . ? C14 C13 C18 C20 177.6(3) . . . . ? C7 C6 N1 C1 53.0(4) . . . 2_655 ? C7 C6 N1 C5 -69.6(4) . . . . ? C4 C5 N1 C6 -59.5(4) . . . . ? C4 C5 N1 C1 178.4(3) . . . 2_655 ? C1 C2 N2 C3 -168.9(3) . . . . ? C1 C2 N2 Zr1 31.6(4) . . . . ? C4 C3 N2 C2 -69.3(4) . . . . ? C4 C3 N2 Zr1 92.2(3) . . . . ? C18 C13 N3 Zr1 -37.8(7) . . . . ? C14 C13 N3 Zr1 145.7(4) . . . . ? C2 N2 Zr1 N2 57.7(3) . . . 2_655 ? C3 N2 Zr1 N2 -100.6(2) . . . 2_655 ? C2 N2 Zr1 N3 -72.7(3) . . . . ? C3 N2 Zr1 N3 129.0(2) . . . . ? C2 N2 Zr1 N3 -178.3(3) . . . 2_655 ? C3 N2 Zr1 N3 23.3(3) . . . 2_655 ? C13 N3 Zr1 N2 86.7(5) . . . 2_655 ? C13 N3 Zr1 N2 -143.7(5) . . . . ? C13 N3 Zr1 N3 -23.3(5) . . . 2_655 ? C23 C21 C22 C22 -177.9 . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.595 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.079 #===end data_Compound5 _database_code_depnum_ccdc_archive 'CCDC 727734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)Zr(NHtBu)Cl ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H44 Cl N5 Zr, C6' _chemical_formula_sum 'C34 H44 Cl N5 Zr' _chemical_formula_weight 649.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.325(5) _cell_length_b 19.719(6) _cell_length_c 14.090(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.17(2) _cell_angle_gamma 90.00 _cell_volume 3410(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4566 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.45 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9190 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39955 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.63 _reflns_number_total 7089 _reflns_number_gt 4179 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7089 _refine_ls_number_parameters 401 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.021 _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 0.16448(3) 0.190681(16) 0.83011(2) 0.03912(12) Uani 1 1 d . . . Cl1 Cl -0.00544(8) 0.22764(6) 0.72934(7) 0.0661(3) Uani 1 1 d . . . N3 N 0.0291(2) 0.19885(13) 0.95214(18) 0.0421(7) Uani 1 1 d . . . N4 N 0.1971(2) 0.11486(13) 0.92897(18) 0.0427(7) Uani 1 1 d . . . N1 N 0.3672(2) 0.20500(13) 0.85460(18) 0.0391(7) Uani 1 1 d . . . C2 C 0.3034(3) 0.30795(17) 0.9277(3) 0.0530(10) Uani 1 1 d . . . H2A H 0.2907 0.3262 0.9897 0.064 Uiso 1 1 calc R . . H2B H 0.3365 0.3432 0.8920 0.064 Uiso 1 1 calc R . . N2 N 0.2016(2) 0.28786(14) 0.8782(2) 0.0462(7) Uani 1 1 d . . . C13 C 0.5225(3) 0.26525(18) 0.7760(2) 0.0444(9) Uani 1 1 d . . . C5 C -0.0208(3) 0.26595(18) 0.9660(3) 0.0516(10) Uani 1 1 d . . . H5A H -0.0601 0.2636 1.0225 0.062 Uiso 1 1 calc R . . H5B H -0.0741 0.2743 0.9123 0.062 Uiso 1 1 calc R . . C6 C 0.1004(3) 0.18050(17) 1.0381(2) 0.0485(9) Uani 1 1 d . . . H6A H 0.0565 0.1751 1.0914 0.058 Uiso 1 1 calc R . . H6B H 0.1519 0.2169 1.0534 0.058 Uiso 1 1 calc R . . C8 C 0.2830(3) 0.06492(17) 0.9212(3) 0.0517(9) Uani 1 1 d . . . H8A H 0.2778 0.0473 0.8567 0.062 Uiso 1 1 calc R . . H8B H 0.2719 0.0274 0.9638 0.062 Uiso 1 1 calc R . . N5 N 0.2103(2) 0.13931(14) 0.71136(18) 0.0505(8) Uani 1 1 d . . . H5 H 0.2730 0.1517 0.6953 0.061 Uiso 1 1 calc R . . C14 C 0.6045(3) 0.2227(2) 0.7472(3) 0.0544(10) Uani 1 1 d . . . H14 H 0.5873 0.1783 0.7293 0.065 Uiso 1 1 calc R . . C16 C 0.7356(3) 0.3101(3) 0.7697(3) 0.0694(12) Uani 1 1 d . . . H16 H 0.8067 0.3255 0.7675 0.083 Uiso 1 1 calc R . . C18 C 0.5512(3) 0.3300(2) 0.8004(3) 0.0569(10) Uani 1 1 d . . . H18 H 0.4984 0.3597 0.8190 0.068 Uiso 1 1 calc R . . C11 C 0.4056(3) 0.24188(17) 0.7706(2) 0.0453(9) Uani 1 1 d . . . H11A H 0.3596 0.2814 0.7587 0.054 Uiso 1 1 calc R . . H11B H 0.3931 0.2125 0.7154 0.054 Uiso 1 1 calc R . . C20 C -0.1264(3) 0.10187(19) 1.0847(3) 0.0606(11) Uani 1 1 d . . . H20 H -0.0642 0.0751 1.0934 0.073 Uiso 1 1 calc R . . C10 C 0.4332(3) 0.14218(17) 0.8705(2) 0.0494(9) Uani 1 1 d . . . H10A H 0.5081 0.1552 0.8887 0.059 Uiso 1 1 calc R . . H10B H 0.4320 0.1179 0.8106 0.059 Uiso 1 1 calc R . . C9 C 0.3970(3) 0.09404(18) 0.9455(3) 0.0542(10) Uani 1 1 d . . . H9A H 0.3985 0.1179 1.0058 0.065 Uiso 1 1 calc R . . H9B H 0.4486 0.0569 0.9536 0.065 Uiso 1 1 calc R . . C22 C -0.2953(4) 0.1377(2) 1.1397(3) 0.0684(12) Uani 1 1 d . . . H22 H -0.3459 0.1357 1.1847 0.082 Uiso 1 1 calc R . . C19 C -0.1427(3) 0.14290(19) 1.0064(2) 0.0507(9) Uani 1 1 d . . . C24 C -0.2380(3) 0.1801(2) 0.9957(3) 0.0670(12) Uani 1 1 d . . . H24 H -0.2514 0.2075 0.9422 0.080 Uiso 1 1 calc R . . C1 C 0.3791(3) 0.24811(17) 0.9400(2) 0.0493(9) Uani 1 1 d . . . H1A H 0.4537 0.2639 0.9507 0.059 Uiso 1 1 calc R . . H1B H 0.3625 0.2219 0.9952 0.059 Uiso 1 1 calc R . . C7 C 0.1613(3) 0.11622(17) 1.0241(2) 0.0511(9) Uani 1 1 d . . . H7A H 0.2238 0.1133 1.0709 0.061 Uiso 1 1 calc R . . H7B H 0.1145 0.0776 1.0329 0.061 Uiso 1 1 calc R . . C15 C 0.7097(3) 0.2451(2) 0.7447(3) 0.0638(12) Uani 1 1 d . . . H15 H 0.7630 0.2159 0.7260 0.077 Uiso 1 1 calc R . . C12 C -0.0603(3) 0.14840(19) 0.9326(2) 0.0530(10) Uani 1 1 d . . . H12A H -0.0276 0.1041 0.9260 0.064 Uiso 1 1 calc R . . H12B H -0.0994 0.1596 0.8718 0.064 Uiso 1 1 calc R . . C17 C 0.6578(4) 0.3528(2) 0.7980(3) 0.0691(12) Uani 1 1 d . . . H17 H 0.6759 0.3971 0.8157 0.083 Uiso 1 1 calc R . . C3 C 0.1165(3) 0.33872(18) 0.8891(3) 0.0572(10) Uani 1 1 d . . . H3A H 0.0657 0.3387 0.8324 0.069 Uiso 1 1 calc R . . H3B H 0.1498 0.3833 0.8948 0.069 Uiso 1 1 calc R . . C21 C -0.2032(4) 0.1002(2) 1.1516(3) 0.0679(12) Uani 1 1 d . . . H21 H -0.1908 0.0729 1.2053 0.081 Uiso 1 1 calc R . . C23 C -0.3139(3) 0.1780(2) 1.0620(3) 0.0738(13) Uani 1 1 d . . . H23 H -0.3771 0.2040 1.0535 0.089 Uiso 1 1 calc R . . C25 C 0.1588(4) 0.08596(19) 0.6480(3) 0.0619(11) Uani 1 1 d . . . C27 C 0.2472(4) 0.0342(2) 0.6276(3) 0.0939(16) Uani 1 1 d . . . H27A H 0.3022 0.0562 0.5946 0.141 Uiso 1 1 calc R . . H27B H 0.2150 -0.0018 0.5888 0.141 Uiso 1 1 calc R . . H27C H 0.2795 0.0159 0.6866 0.141 Uiso 1 1 calc R . . C4 C 0.0542(3) 0.32566(17) 0.9761(3) 0.0557(10) Uani 1 1 d . . . H4A H 0.1062 0.3186 1.0310 0.067 Uiso 1 1 calc R . . H4B H 0.0119 0.3657 0.9882 0.067 Uiso 1 1 calc R . . C28 C 0.0701(4) 0.0524(2) 0.6980(4) 0.0965(16) Uani 1 1 d . . . H28A H 0.1010 0.0325 0.7565 0.145 Uiso 1 1 calc R . . H28B H 0.0361 0.0177 0.6578 0.145 Uiso 1 1 calc R . . H28C H 0.0167 0.0856 0.7116 0.145 Uiso 1 1 calc R . . C26 C 0.1145(5) 0.1179(3) 0.5553(3) 0.115(2) Uani 1 1 d . . . H26A H 0.1727 0.1394 0.5258 0.172 Uiso 1 1 calc R . . H26B H 0.0605 0.1511 0.5674 0.172 Uiso 1 1 calc R . . H26C H 0.0821 0.0835 0.5136 0.172 Uiso 1 1 calc R . . C34 C 0.722(2) 0.0418(8) 0.6434(15) 0.101(5) Uani 0.61(4) 1 d PGDU A 1 C33 C 0.626(2) 0.0062(10) 0.6209(11) 0.105(6) Uani 0.61(4) 1 d PGDU A 1 C32 C 0.5658(10) -0.0169(7) 0.693(3) 0.100(6) Uani 0.61(4) 1 d PGDU A 1 C29 C 0.602(2) -0.0042(7) 0.788(2) 0.090(6) Uani 0.61(4) 1 d PGDU A 1 C30 C 0.698(3) 0.0314(10) 0.8104(6) 0.111(7) Uani 0.61(4) 1 d PGDU A 1 C31 C 0.7581(9) 0.0545(7) 0.738(2) 0.110(6) Uani 0.61(4) 1 d PGDU A 1 C35 C 0.642(2) 0.0091(15) 0.8137(6) 0.079(8) Uani 0.39(4) 1 d PGDU A 2 C36 C 0.5581(12) -0.0108(9) 0.747(2) 0.078(7) Uani 0.39(4) 1 d PGDU A 2 C40 C 0.5664(19) 0.0002(13) 0.6506(17) 0.083(7) Uani 0.39(4) 1 d PGDU A 2 C39 C 0.659(3) 0.0312(15) 0.6207(11) 0.072(8) Uani 0.39(4) 1 d PGDU A 2 C37 C 0.7427(16) 0.0511(11) 0.687(3) 0.088(9) Uani 0.39(4) 1 d PGDU A 2 C38 C 0.7344(16) 0.0401(15) 0.784(2) 0.091(9) Uani 0.39(4) 1 d PGDU 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 0.03520(19) 0.0478(2) 0.0353(2) 0.00029(16) 0.00805(14) 0.00219(16) Cl1 0.0448(6) 0.1073(8) 0.0468(6) 0.0076(5) 0.0071(4) 0.0178(5) N3 0.0391(16) 0.0519(18) 0.0357(16) -0.0038(13) 0.0064(13) -0.0017(14) N4 0.0487(18) 0.0429(17) 0.0373(17) 0.0000(13) 0.0081(13) 0.0017(14) N1 0.0354(15) 0.0444(17) 0.0378(16) 0.0023(13) 0.0053(12) 0.0040(12) C2 0.056(2) 0.051(2) 0.055(2) -0.0069(19) 0.0212(19) -0.005(2) N2 0.0405(17) 0.0455(17) 0.0546(19) 0.0000(14) 0.0143(15) 0.0014(14) C13 0.038(2) 0.059(2) 0.036(2) 0.0097(17) 0.0038(16) -0.0021(18) C5 0.046(2) 0.063(3) 0.048(2) -0.0034(19) 0.0171(18) 0.0026(19) C6 0.053(2) 0.058(2) 0.036(2) -0.0030(17) 0.0112(17) -0.0073(18) C8 0.060(3) 0.047(2) 0.049(2) 0.0070(18) 0.0120(19) 0.0026(19) N5 0.0400(17) 0.069(2) 0.0427(17) -0.0094(15) 0.0026(14) 0.0013(15) C14 0.044(2) 0.070(3) 0.050(2) 0.0162(19) 0.0073(18) 0.004(2) C16 0.045(2) 0.110(4) 0.054(3) 0.022(3) 0.002(2) -0.013(3) C18 0.055(3) 0.067(3) 0.050(2) 0.001(2) 0.0118(19) -0.005(2) C11 0.042(2) 0.055(2) 0.041(2) 0.0044(17) 0.0089(16) 0.0045(17) C20 0.065(3) 0.053(2) 0.066(3) -0.005(2) 0.015(2) -0.013(2) C10 0.039(2) 0.056(2) 0.053(2) 0.0066(19) 0.0043(17) 0.0074(17) C9 0.056(2) 0.054(2) 0.053(2) 0.0130(19) 0.0057(19) 0.0148(19) C22 0.067(3) 0.083(3) 0.060(3) -0.014(2) 0.029(2) -0.029(3) C19 0.049(2) 0.066(3) 0.038(2) -0.0075(19) 0.0096(18) -0.020(2) C24 0.050(3) 0.107(4) 0.044(2) 0.011(2) 0.006(2) -0.007(2) C1 0.050(2) 0.054(2) 0.044(2) -0.0023(18) 0.0072(17) -0.0037(18) C7 0.057(2) 0.054(2) 0.042(2) 0.0072(18) 0.0069(18) -0.0032(19) C15 0.040(2) 0.099(4) 0.054(3) 0.028(2) 0.0105(19) 0.010(2) C12 0.047(2) 0.072(3) 0.041(2) -0.0131(19) 0.0087(17) -0.0132(19) C17 0.075(3) 0.077(3) 0.056(3) 0.001(2) 0.012(2) -0.026(3) C3 0.057(2) 0.046(2) 0.072(3) 0.003(2) 0.026(2) 0.0105(19) C21 0.086(3) 0.061(3) 0.059(3) 0.004(2) 0.021(3) -0.024(2) C23 0.049(3) 0.111(4) 0.065(3) 0.004(3) 0.019(2) -0.006(2) C25 0.083(3) 0.059(3) 0.042(2) -0.009(2) -0.003(2) 0.015(2) C27 0.116(4) 0.087(3) 0.081(3) -0.020(3) 0.017(3) 0.019(3) C4 0.057(2) 0.048(2) 0.066(3) -0.0053(19) 0.026(2) 0.0084(18) C28 0.080(4) 0.078(3) 0.128(5) -0.017(3) -0.005(3) -0.013(3) C26 0.174(6) 0.109(4) 0.055(3) -0.014(3) -0.024(3) 0.030(4) C34 0.115(15) 0.083(9) 0.105(11) 0.008(8) 0.013(9) 0.009(9) C33 0.133(15) 0.085(11) 0.095(11) -0.009(7) -0.004(9) 0.006(9) C32 0.103(9) 0.088(9) 0.105(15) -0.011(11) -0.010(9) -0.015(6) C29 0.097(13) 0.073(8) 0.101(12) -0.009(9) 0.015(10) 0.003(9) C30 0.139(17) 0.090(12) 0.101(9) -0.003(8) -0.007(11) 0.020(12) C31 0.133(12) 0.081(9) 0.111(13) -0.010(10) -0.022(10) 0.002(8) C35 0.079(15) 0.078(16) 0.074(10) -0.007(10) -0.030(10) 0.004(11) C36 0.079(11) 0.085(11) 0.065(14) -0.019(11) -0.028(10) -0.012(8) C40 0.097(14) 0.102(13) 0.052(11) 0.006(9) 0.018(10) 0.009(10) C39 0.090(17) 0.057(13) 0.070(11) 0.008(8) 0.014(10) 0.027(11) C37 0.081(13) 0.080(13) 0.10(2) 0.001(14) 0.012(13) -0.005(9) C38 0.058(11) 0.089(14) 0.121(19) -0.016(15) -0.012(13) -0.009(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.058(3) . ? Zr1 N2 2.070(3) . ? Zr1 N5 2.077(3) . ? Zr1 N1 2.507(3) . ? Zr1 N3 2.507(3) . ? Zr1 Cl1 2.5292(13) . ? N3 C6 1.476(4) . ? N3 C5 1.479(4) . ? N3 C12 1.491(4) . ? N4 C7 1.448(4) . ? N4 C8 1.457(4) . ? N1 C1 1.470(4) . ? N1 C10 1.488(4) . ? N1 C11 1.502(4) . ? C2 N2 1.435(4) . ? C2 C1 1.505(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N2 C3 1.469(4) . ? C13 C18 1.362(5) . ? C13 C14 1.400(5) . ? C13 C11 1.509(4) . ? C5 C4 1.496(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.495(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.529(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N5 C25 1.485(5) . ? N5 H5 0.8600 . ? C14 C15 1.373(5) . ? C14 H14 0.9300 . ? C16 C15 1.360(5) . ? C16 C17 1.362(6) . ? C16 H16 0.9300 . ? C18 C17 1.392(5) . ? C18 H18 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C20 C19 1.369(5) . ? C20 C21 1.394(5) . ? C20 H20 0.9300 . ? C10 C9 1.517(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C22 C21 1.351(6) . ? C22 C23 1.355(6) . ? C22 H22 0.9300 . ? C19 C24 1.382(5) . ? C19 C12 1.521(5) . ? C24 C23 1.382(5) . ? C24 H24 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C15 H15 0.9300 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C17 H17 0.9300 . ? C3 C4 1.525(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C21 H21 0.9300 . ? C23 H23 0.9300 . ? C25 C28 1.506(6) . ? C25 C26 1.507(5) . ? C25 C27 1.539(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C34 C33 1.3900 . ? C34 C31 1.3900 . ? C33 C32 1.3900 . ? C32 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C35 C36 1.3900 . ? C35 C38 1.3900 . ? C36 C40 1.3900 . ? C40 C39 1.3900 . ? C39 C37 1.3900 . ? C37 C38 1.3900 . ? 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 N2 115.29(11) . . ? N4 Zr1 N5 98.06(11) . . ? N2 Zr1 N5 130.32(11) . . ? N4 Zr1 N1 81.80(10) . . ? N2 Zr1 N1 70.29(10) . . ? N5 Zr1 N1 79.99(10) . . ? N4 Zr1 N3 71.58(10) . . ? N2 Zr1 N3 81.79(9) . . ? N5 Zr1 N3 146.08(10) . . ? N1 Zr1 N3 127.96(9) . . ? N4 Zr1 Cl1 133.67(8) . . ? N2 Zr1 Cl1 93.69(9) . . ? N5 Zr1 Cl1 87.69(8) . . ? N1 Zr1 Cl1 144.03(7) . . ? N3 Zr1 Cl1 78.33(7) . . ? C6 N3 C5 109.6(3) . . ? C6 N3 C12 111.3(3) . . ? C5 N3 C12 108.2(3) . . ? C6 N3 Zr1 99.39(19) . . ? C5 N3 Zr1 117.26(19) . . ? C12 N3 Zr1 110.92(18) . . ? C7 N4 C8 111.5(3) . . ? C7 N4 Zr1 123.7(2) . . ? C8 N4 Zr1 122.6(2) . . ? C1 N1 C10 110.2(3) . . ? C1 N1 C11 110.5(2) . . ? C10 N1 C11 108.4(2) . . ? C1 N1 Zr1 101.69(19) . . ? C10 N1 Zr1 116.86(19) . . ? C11 N1 Zr1 109.09(18) . . ? N2 C2 C1 110.2(3) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 N2 C3 111.2(3) . . ? C2 N2 Zr1 124.9(2) . . ? C3 N2 Zr1 121.9(2) . . ? C18 C13 C14 117.2(3) . . ? C18 C13 C11 121.6(3) . . ? C14 C13 C11 120.9(3) . . ? N3 C5 C4 117.1(3) . . ? N3 C5 H5A 108.0 . . ? C4 C5 H5A 108.0 . . ? N3 C5 H5B 108.0 . . ? C4 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? N3 C6 C7 111.6(3) . . ? N3 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N3 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N4 C8 C9 112.9(3) . . ? N4 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N4 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C25 N5 Zr1 134.2(2) . . ? C25 N5 H5 112.9 . . ? Zr1 N5 H5 112.9 . . ? C15 C14 C13 121.5(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C13 C18 C17 121.4(4) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? N1 C11 C13 118.4(3) . . ? N1 C11 H11A 107.7 . . ? C13 C11 H11A 107.7 . . ? N1 C11 H11B 107.7 . . ? C13 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? N1 C10 C9 115.8(3) . . ? N1 C10 H10A 108.3 . . ? C9 C10 H10A 108.3 . . ? N1 C10 H10B 108.3 . . ? C9 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C9 C8 113.6(3) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C20 C19 C24 117.6(3) . . ? C20 C19 C12 122.4(4) . . ? C24 C19 C12 120.1(3) . . ? C23 C24 C19 122.1(4) . . ? C23 C24 H24 118.9 . . ? C19 C24 H24 118.9 . . ? N1 C1 C2 110.1(3) . . ? N1 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? H1A C1 H1B 108.2 . . ? N4 C7 C6 109.7(3) . . ? N4 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? N4 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? N3 C12 C19 116.7(3) . . ? N3 C12 H12A 108.1 . . ? C19 C12 H12A 108.1 . . ? N3 C12 H12B 108.1 . . ? C19 C12 H12B 108.1 . . ? H12A C12 H12B 107.3 . . ? C16 C17 C18 119.9(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N2 C3 C4 112.6(3) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C22 C21 C20 121.1(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C22 C23 C24 119.2(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? N5 C25 C28 108.6(3) . . ? N5 C25 C26 109.1(3) . . ? C28 C25 C26 111.6(4) . . ? N5 C25 C27 108.1(3) . . ? C28 C25 C27 110.6(3) . . ? C26 C25 C27 108.8(4) . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C5 C4 C3 114.1(3) . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C33 C34 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C32 C29 120.0 . . ? C30 C29 C32 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C34 120.0 . . ? C36 C35 C38 120.0 . . ? C40 C36 C35 120.0 . . ? C36 C40 C39 120.0 . . ? C40 C39 C37 120.0 . . ? C38 C37 C39 120.0 . . ? C37 C38 C35 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 N3 C6 37.02(18) . . . . ? N2 Zr1 N3 C6 -83.2(2) . . . . ? N5 Zr1 N3 C6 113.7(2) . . . . ? N1 Zr1 N3 C6 -26.2(2) . . . . ? Cl1 Zr1 N3 C6 -178.70(19) . . . . ? N4 Zr1 N3 C5 154.9(2) . . . . ? N2 Zr1 N3 C5 34.7(2) . . . . ? N5 Zr1 N3 C5 -128.5(2) . . . . ? N1 Zr1 N3 C5 91.6(2) . . . . ? Cl1 Zr1 N3 C5 -60.8(2) . . . . ? N4 Zr1 N3 C12 -80.2(2) . . . . ? N2 Zr1 N3 C12 159.6(2) . . . . ? N5 Zr1 N3 C12 -3.5(3) . . . . ? N1 Zr1 N3 C12 -143.4(2) . . . . ? Cl1 Zr1 N3 C12 64.1(2) . . . . ? N2 Zr1 N4 C7 50.3(3) . . . . ? N5 Zr1 N4 C7 -167.6(3) . . . . ? N1 Zr1 N4 C7 113.8(3) . . . . ? N3 Zr1 N4 C7 -20.8(2) . . . . ? Cl1 Zr1 N4 C7 -73.0(3) . . . . ? N2 Zr1 N4 C8 -111.5(2) . . . . ? N5 Zr1 N4 C8 30.6(3) . . . . ? N1 Zr1 N4 C8 -47.9(2) . . . . ? N3 Zr1 N4 C8 177.4(3) . . . . ? Cl1 Zr1 N4 C8 125.2(2) . . . . ? N4 Zr1 N1 C1 -83.8(2) . . . . ? N2 Zr1 N1 C1 36.84(19) . . . . ? N5 Zr1 N1 C1 176.4(2) . . . . ? N3 Zr1 N1 C1 -25.0(2) . . . . ? Cl1 Zr1 N1 C1 104.67(19) . . . . ? N4 Zr1 N1 C10 36.1(2) . . . . ? N2 Zr1 N1 C10 156.8(2) . . . . ? N5 Zr1 N1 C10 -63.6(2) . . . . ? N3 Zr1 N1 C10 95.0(2) . . . . ? Cl1 Zr1 N1 C10 -135.37(19) . . . . ? N4 Zr1 N1 C11 159.4(2) . . . . ? N2 Zr1 N1 C11 -79.9(2) . . . . ? N5 Zr1 N1 C11 59.7(2) . . . . ? N3 Zr1 N1 C11 -141.74(18) . . . . ? Cl1 Zr1 N1 C11 -12.1(2) . . . . ? C1 C2 N2 C3 163.6(3) . . . . ? C1 C2 N2 Zr1 -0.2(4) . . . . ? N4 Zr1 N2 C2 49.5(3) . . . . ? N5 Zr1 N2 C2 -77.7(3) . . . . ? N1 Zr1 N2 C2 -20.8(2) . . . . ? N3 Zr1 N2 C2 114.5(3) . . . . ? Cl1 Zr1 N2 C2 -167.8(3) . . . . ? N4 Zr1 N2 C3 -112.8(3) . . . . ? N5 Zr1 N2 C3 120.0(2) . . . . ? N1 Zr1 N2 C3 176.9(3) . . . . ? N3 Zr1 N2 C3 -47.7(2) . . . . ? Cl1 Zr1 N2 C3 30.0(2) . . . . ? C6 N3 C5 C4 65.0(4) . . . . ? C12 N3 C5 C4 -173.5(3) . . . . ? Zr1 N3 C5 C4 -47.2(4) . . . . ? C5 N3 C6 C7 -174.4(3) . . . . ? C12 N3 C6 C7 66.0(3) . . . . ? Zr1 N3 C6 C7 -50.9(3) . . . . ? C7 N4 C8 C9 -89.6(3) . . . . ? Zr1 N4 C8 C9 74.2(3) . . . . ? N4 Zr1 N5 C25 77.1(3) . . . . ? N2 Zr1 N5 C25 -149.6(3) . . . . ? N1 Zr1 N5 C25 157.2(3) . . . . ? N3 Zr1 N5 C25 8.3(4) . . . . ? Cl1 Zr1 N5 C25 -56.7(3) . . . . ? C18 C13 C14 C15 0.8(5) . . . . ? C11 C13 C14 C15 174.9(3) . . . . ? C14 C13 C18 C17 -0.8(5) . . . . ? C11 C13 C18 C17 -174.9(3) . . . . ? C1 N1 C11 C13 60.2(4) . . . . ? C10 N1 C11 C13 -60.6(4) . . . . ? Zr1 N1 C11 C13 171.2(2) . . . . ? C18 C13 C11 N1 -97.6(4) . . . . ? C14 C13 C11 N1 88.6(4) . . . . ? C1 N1 C10 C9 66.0(4) . . . . ? C11 N1 C10 C9 -173.1(3) . . . . ? Zr1 N1 C10 C9 -49.4(4) . . . . ? N1 C10 C9 C8 63.0(4) . . . . ? N4 C8 C9 C10 -71.7(4) . . . . ? C21 C20 C19 C24 -1.8(5) . . . . ? C21 C20 C19 C12 178.2(3) . . . . ? C20 C19 C24 C23 1.5(6) . . . . ? C12 C19 C24 C23 -178.4(4) . . . . ? C10 N1 C1 C2 -174.1(3) . . . . ? C11 N1 C1 C2 66.2(3) . . . . ? Zr1 N1 C1 C2 -49.5(3) . . . . ? N2 C2 C1 N1 37.9(4) . . . . ? C8 N4 C7 C6 162.6(3) . . . . ? Zr1 N4 C7 C6 -0.9(4) . . . . ? N3 C6 C7 N4 40.1(4) . . . . ? C17 C16 C15 C14 0.6(6) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C6 N3 C12 C19 64.6(4) . . . . ? C5 N3 C12 C19 -55.8(4) . . . . ? Zr1 N3 C12 C19 174.3(3) . . . . ? C20 C19 C12 N3 -86.5(4) . . . . ? C24 C19 C12 N3 93.5(4) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C13 C18 C17 C16 0.8(6) . . . . ? C2 N2 C3 C4 -89.9(4) . . . . ? Zr1 N2 C3 C4 74.5(4) . . . . ? C23 C22 C21 C20 -0.5(6) . . . . ? C19 C20 C21 C22 1.3(6) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C19 C24 C23 C22 -0.7(7) . . . . ? Zr1 N5 C25 C28 -17.9(5) . . . . ? Zr1 N5 C25 C26 103.9(4) . . . . ? Zr1 N5 C25 C27 -137.9(3) . . . . ? N3 C5 C4 C3 61.6(4) . . . . ? N2 C3 C4 C5 -71.7(4) . . . . ? C31 C34 C33 C32 0.0 . . . . ? C34 C33 C32 C29 0.0 . . . . ? C33 C32 C29 C30 0.0 . . . . ? C32 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C34 0.0 . . . . ? C33 C34 C31 C30 0.0 . . . . ? C38 C35 C36 C40 0.0 . . . . ? C35 C36 C40 C39 0.0 . . . . ? C36 C40 C39 C37 0.0 . . . . ? C40 C39 C37 C38 0.0 . . . . ? C39 C37 C38 C35 0.0 . . . . ? C36 C35 C38 C37 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.63 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.337 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.065 #===end data_Compound6 _database_code_depnum_ccdc_archive 'CCDC 727735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)Zr(NH2,6iPrPh)Cl ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H52 Cl N5 Zr), 3(C4 H10 O)' _chemical_formula_sum 'C84 H134 Cl2 N10 O3 Zr2' _chemical_formula_weight 1585.35 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7286(8) _cell_length_b 28.7142(17) _cell_length_c 20.8751(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.543(3) _cell_angle_gamma 90.00 _cell_volume 8545.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6194 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 24.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3384 _exptl_absorpt_coefficient_mu 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9651 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82745 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.76 _reflns_number_total 16261 _reflns_number_gt 11937 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0558P)^2^+19.6424P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16261 _refine_ls_number_parameters 929 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr11 Zr 0.98105(3) 0.319129(13) 0.489377(18) 0.02016(10) Uani 1 1 d . . . Cl11 Cl 1.13104(7) 0.28886(4) 0.56176(5) 0.0325(2) Uani 1 1 d . . . N11 N 0.8286(2) 0.36285(11) 0.48496(15) 0.0198(7) Uani 1 1 d . . . N12 N 0.8935(2) 0.27835(12) 0.52964(16) 0.0238(7) Uani 1 1 d . . . N13 N 0.9977(2) 0.24564(12) 0.43046(16) 0.0246(7) Uani 1 1 d . . . N14 N 0.9368(2) 0.33119(12) 0.38842(15) 0.0238(7) Uani 1 1 d . . . N15 N 1.0320(2) 0.38758(12) 0.51913(16) 0.0247(7) Uani 1 1 d . . . H15 H 0.9847 0.4055 0.5219 0.030 Uiso 1 1 calc R . . Zr21 Zr 0.50920(3) 0.199314(15) 0.299861(19) 0.02454(11) Uani 1 1 d . . . Cl21 Cl 0.65507(7) 0.23749(4) 0.36422(6) 0.0381(3) Uani 1 1 d . . . N21 N 0.4289(2) 0.12276(12) 0.27194(16) 0.0271(8) Uani 1 1 d . . . N22 N 0.4653(2) 0.17474(13) 0.38104(17) 0.0328(9) Uani 1 1 d . . . N23 N 0.4427(2) 0.27312(13) 0.33139(17) 0.0309(8) Uani 1 1 d . . . N24 N 0.4033(2) 0.22116(12) 0.22095(17) 0.0276(8) Uani 1 1 d . . . N25 N 0.5997(2) 0.16759(12) 0.24719(16) 0.0264(8) Uani 1 1 d . . . H25 H 0.5784 0.1404 0.2304 0.032 Uiso 1 1 calc R . . C11 C 0.7626(3) 0.32312(14) 0.4657(2) 0.0247(9) Uani 1 1 d . . . H11A H 0.7621 0.3128 0.4203 0.030 Uiso 1 1 calc R . . H11B H 0.6983 0.3331 0.4658 0.030 Uiso 1 1 calc R . . C12 C 0.7924(3) 0.28330(14) 0.5135(2) 0.0248(9) Uani 1 1 d . . . H12A H 0.7717 0.2893 0.5543 0.030 Uiso 1 1 calc R . . H12B H 0.7625 0.2541 0.4934 0.030 Uiso 1 1 calc R . . C13 C 0.9228(3) 0.23210(15) 0.5572(2) 0.0307(10) Uani 1 1 d . . . H13A H 0.8808 0.2222 0.5850 0.037 Uiso 1 1 calc R . . H13B H 0.9873 0.2341 0.5860 0.037 Uiso 1 1 calc R . . C14 C 0.9204(3) 0.19548(15) 0.5039(2) 0.0332(10) Uani 1 1 d . . . H14A H 0.8588 0.1969 0.4713 0.040 Uiso 1 1 calc R . . H14B H 0.9264 0.1642 0.5246 0.040 Uiso 1 1 calc R . . C15 C 0.9976(3) 0.20135(15) 0.4675(2) 0.0314(10) Uani 1 1 d . . . H15A H 1.0590 0.1985 0.5002 0.038 Uiso 1 1 calc R . . H15B H 0.9929 0.1752 0.4358 0.038 Uiso 1 1 calc R . . C16 C 0.9142(3) 0.24783(15) 0.3735(2) 0.0277(9) Uani 1 1 d . . . H16A H 0.8569 0.2426 0.3891 0.033 Uiso 1 1 calc R . . H16B H 0.9181 0.2229 0.3415 0.033 Uiso 1 1 calc R . . C17 C 0.9078(3) 0.29416(15) 0.3396(2) 0.0278(9) Uani 1 1 d . . . H17A H 0.9486 0.2943 0.3085 0.033 Uiso 1 1 calc R . . H17B H 0.8424 0.2997 0.3139 0.033 Uiso 1 1 calc R . . C18 C 0.9088(3) 0.37684(15) 0.3611(2) 0.0286(9) Uani 1 1 d . . . H18A H 0.9107 0.3773 0.3140 0.034 Uiso 1 1 calc R . . H18B H 0.9544 0.4002 0.3849 0.034 Uiso 1 1 calc R . . C19 C 0.8107(3) 0.39055(15) 0.36591(19) 0.0285(9) Uani 1 1 d . . . H19A H 0.7904 0.4183 0.3379 0.034 Uiso 1 1 calc R . . H19B H 0.7669 0.3649 0.3478 0.034 Uiso 1 1 calc R . . C110 C 0.8033(3) 0.40125(14) 0.43563(19) 0.0252(9) Uani 1 1 d . . . H11C H 0.8443 0.4282 0.4523 0.030 Uiso 1 1 calc R . . H11D H 0.7380 0.4109 0.4333 0.030 Uiso 1 1 calc R . . C111 C 0.8238(3) 0.38100(14) 0.55172(18) 0.0219(8) Uani 1 1 d . . . H11E H 0.8701 0.4065 0.5643 0.026 Uiso 1 1 calc R . . H11F H 0.8433 0.3557 0.5845 0.026 Uiso 1 1 calc R . . C112 C 0.7288(3) 0.39910(14) 0.55712(18) 0.0231(9) Uani 1 1 d . . . C113 C 0.7045(3) 0.44530(15) 0.5433(2) 0.0283(9) Uani 1 1 d . . . H113 H 0.7480 0.4658 0.5311 0.034 Uiso 1 1 calc R . . C114 C 0.6177(3) 0.46208(16) 0.5469(2) 0.0336(10) Uani 1 1 d . . . H114 H 0.6021 0.4938 0.5370 0.040 Uiso 1 1 calc R . . C115 C 0.5540(3) 0.43301(16) 0.5648(2) 0.0351(11) Uani 1 1 d . . . H115 H 0.4939 0.4443 0.5662 0.042 Uiso 1 1 calc R . . C116 C 0.5783(3) 0.38739(17) 0.5807(2) 0.0381(11) Uani 1 1 d . . . H116 H 0.5356 0.3674 0.5947 0.046 Uiso 1 1 calc R . . C117 C 0.6646(3) 0.37040(15) 0.5765(2) 0.0288(9) Uani 1 1 d . . . H117 H 0.6801 0.3387 0.5870 0.035 Uiso 1 1 calc R . . C118 C 1.0874(3) 0.24849(16) 0.4074(2) 0.0287(10) Uani 1 1 d . . . H11G H 1.1409 0.2429 0.4461 0.034 Uiso 1 1 calc R . . H11H H 1.0935 0.2807 0.3921 0.034 Uiso 1 1 calc R . . C119 C 1.0962(3) 0.21508(17) 0.3523(2) 0.0337(11) Uani 1 1 d . . . C120 C 1.1135(3) 0.16764(18) 0.3630(3) 0.0453(13) Uani 1 1 d . . . H120 H 1.1212 0.1549 0.4060 0.054 Uiso 1 1 calc R . . C121 C 1.1195(4) 0.1391(2) 0.3104(3) 0.0557(16) Uani 1 1 d . . . H121 H 1.1291 0.1066 0.3176 0.067 Uiso 1 1 calc R . . C122 C 1.1119(3) 0.1570(3) 0.2486(3) 0.0596(17) Uani 1 1 d . . . H122 H 1.1154 0.1370 0.2131 0.071 Uiso 1 1 calc R . . C123 C 1.0991(3) 0.2039(3) 0.2379(3) 0.0559(16) Uani 1 1 d . . . H123 H 1.0960 0.2166 0.1954 0.067 Uiso 1 1 calc R . . C124 C 1.0909(3) 0.23276(19) 0.2897(2) 0.0403(12) Uani 1 1 d . . . H124 H 1.0814 0.2652 0.2819 0.048 Uiso 1 1 calc R . . C125 C 1.1153(3) 0.41343(14) 0.53571(18) 0.0216(8) Uani 1 1 d . . . C126 C 1.1312(3) 0.44595(14) 0.58934(19) 0.0251(9) Uani 1 1 d . . . C127 C 1.2143(3) 0.47127(15) 0.6049(2) 0.0286(9) Uani 1 1 d . . . H127 H 1.2249 0.4928 0.6406 0.034 Uiso 1 1 calc R . . C128 C 1.2816(3) 0.46600(15) 0.5702(2) 0.0308(10) Uani 1 1 d . . . H128 H 1.3377 0.4838 0.5815 0.037 Uiso 1 1 calc R . . C129 C 1.2664(3) 0.43462(15) 0.5189(2) 0.0309(10) Uani 1 1 d . . . H129 H 1.3129 0.4310 0.4950 0.037 Uiso 1 1 calc R . . C130 C 1.1853(3) 0.40795(14) 0.5008(2) 0.0264(9) Uani 1 1 d . . . C131 C 1.0569(3) 0.45381(15) 0.6272(2) 0.0295(10) Uani 1 1 d . . . H131 H 1.0260 0.4232 0.6304 0.035 Uiso 1 1 calc R . . C132 C 1.0954(4) 0.4720(2) 0.6971(2) 0.0506(14) Uani 1 1 d . . . H13C H 1.0438 0.4761 0.7185 0.076 Uiso 1 1 calc R . . H13D H 1.1266 0.5019 0.6955 0.076 Uiso 1 1 calc R . . H13E H 1.1406 0.4496 0.7225 0.076 Uiso 1 1 calc R . . C133 C 0.9811(3) 0.48748(16) 0.5892(2) 0.0396(11) Uani 1 1 d . . . H13F H 0.9335 0.4920 0.6141 0.059 Uiso 1 1 calc R . . H13G H 0.9515 0.4744 0.5456 0.059 Uiso 1 1 calc R . . H13H H 1.0099 0.5175 0.5837 0.059 Uiso 1 1 calc R . . C134 C 1.1739(3) 0.37559(17) 0.4424(2) 0.0350(11) Uani 1 1 d . . . H134 H 1.1165 0.3564 0.4401 0.042 Uiso 1 1 calc R . . C135 C 1.1582(4) 0.4028(2) 0.3769(2) 0.0543(15) Uani 1 1 d . . . H13I H 1.1507 0.3809 0.3400 0.081 Uiso 1 1 calc R . . H13J H 1.2123 0.4230 0.3783 0.081 Uiso 1 1 calc R . . H13K H 1.1015 0.4219 0.3707 0.081 Uiso 1 1 calc R . . C136 C 1.2568(3) 0.34197(19) 0.4506(3) 0.0512(14) Uani 1 1 d . . . H13L H 1.2466 0.3215 0.4118 0.077 Uiso 1 1 calc R . . H13M H 1.2620 0.3231 0.4905 0.077 Uiso 1 1 calc R . . H13N H 1.3148 0.3598 0.4547 0.077 Uiso 1 1 calc R . . C21 C 0.3506(3) 0.12907(18) 0.3040(2) 0.0355(11) Uani 1 1 d . . . H21A H 0.3146 0.0997 0.3014 0.043 Uiso 1 1 calc R . . H21B H 0.3076 0.1536 0.2805 0.043 Uiso 1 1 calc R . . C22 C 0.3880(3) 0.14267(18) 0.3751(2) 0.0402(12) Uani 1 1 d . . . H22A H 0.3377 0.1576 0.3917 0.048 Uiso 1 1 calc R . . H22B H 0.4095 0.1146 0.4022 0.048 Uiso 1 1 calc R . . C23 C 0.4867(3) 0.19949(18) 0.4446(2) 0.0419(12) Uani 1 1 d . . . H23A H 0.5537 0.2084 0.4566 0.050 Uiso 1 1 calc R . . H23B H 0.4760 0.1783 0.4794 0.050 Uiso 1 1 calc R . . C24 C 0.4275(4) 0.24258(19) 0.4427(2) 0.0452(13) Uani 1 1 d . . . H24A H 0.3609 0.2345 0.4233 0.054 Uiso 1 1 calc R . . H24B H 0.4331 0.2534 0.4886 0.054 Uiso 1 1 calc R . . C25 C 0.4547(3) 0.28188(18) 0.4034(2) 0.0397(12) Uani 1 1 d . . . H25A H 0.4170 0.3096 0.4084 0.048 Uiso 1 1 calc R . . H25B H 0.5213 0.2897 0.4232 0.048 Uiso 1 1 calc R . . C26 C 0.3427(3) 0.26743(17) 0.2976(2) 0.0325(10) Uani 1 1 d . . . H26A H 0.3090 0.2969 0.3002 0.039 Uiso 1 1 calc R . . H26B H 0.3149 0.2429 0.3201 0.039 Uiso 1 1 calc R . . C27 C 0.3307(3) 0.25425(16) 0.2258(2) 0.0319(10) Uani 1 1 d . . . H27A H 0.2681 0.2402 0.2080 0.038 Uiso 1 1 calc R . . H27B H 0.3354 0.2824 0.1994 0.038 Uiso 1 1 calc R . . C28 C 0.3820(3) 0.19656(15) 0.15708(19) 0.0280(9) Uani 1 1 d . . . H28A H 0.4413 0.1904 0.1444 0.034 Uiso 1 1 calc R . . H28B H 0.3428 0.2169 0.1227 0.034 Uiso 1 1 calc R . . C29 C 0.3314(3) 0.15107(16) 0.1587(2) 0.0330(10) Uani 1 1 d . . . H29A H 0.3085 0.1395 0.1128 0.040 Uiso 1 1 calc R . . H29B H 0.2759 0.1569 0.1763 0.040 Uiso 1 1 calc R . . C210 C 0.3909(3) 0.11321(15) 0.2004(2) 0.0309(10) Uani 1 1 d . . . H21C H 0.3525 0.0845 0.1960 0.037 Uiso 1 1 calc R . . H21D H 0.4444 0.1065 0.1810 0.037 Uiso 1 1 calc R . . C211 C 0.4896(3) 0.08290(16) 0.3029(2) 0.0333(10) Uani 1 1 d . . . H21E H 0.5162 0.0903 0.3502 0.040 Uiso 1 1 calc R . . H21F H 0.5427 0.0807 0.2818 0.040 Uiso 1 1 calc R . . C212 C 0.4434(3) 0.03541(17) 0.2987(2) 0.0375(11) Uani 1 1 d . . . C213 C 0.4453(3) 0.00527(16) 0.2473(3) 0.0413(12) Uani 1 1 d . . . H213 H 0.4755 0.0150 0.2144 0.050 Uiso 1 1 calc R . . C214 C 0.4048(4) -0.03844(19) 0.2423(3) 0.0530(14) Uani 1 1 d . . . H214 H 0.4080 -0.0586 0.2069 0.064 Uiso 1 1 calc R . . C215 C 0.3599(4) -0.0522(2) 0.2891(3) 0.0605(16) Uani 1 1 d . . . H215 H 0.3303 -0.0819 0.2855 0.073 Uiso 1 1 calc R . . C216 C 0.3572(5) -0.0239(2) 0.3408(3) 0.0671(17) Uani 1 1 d . . . H216 H 0.3270 -0.0339 0.3736 0.081 Uiso 1 1 calc R . . C217 C 0.3991(4) 0.0200(2) 0.3456(3) 0.0560(15) Uani 1 1 d . . . H217 H 0.3969 0.0397 0.3818 0.067 Uiso 1 1 calc R . . C218 C 0.4843(3) 0.31352(16) 0.3030(2) 0.0349(11) Uani 1 1 d . . . H21G H 0.4746 0.3081 0.2550 0.042 Uiso 1 1 calc R . . H21H H 0.5529 0.3135 0.3229 0.042 Uiso 1 1 calc R . . C219 C 0.4476(3) 0.36153(16) 0.3123(2) 0.0361(11) Uani 1 1 d . . . C220 C 0.3740(3) 0.38154(18) 0.2654(2) 0.0429(12) Uani 1 1 d . . . H220 H 0.3449 0.3642 0.2269 0.052 Uiso 1 1 calc R . . C221 C 0.3419(4) 0.42571(18) 0.2730(3) 0.0457(12) Uani 1 1 d . . . H221 H 0.2913 0.4385 0.2402 0.055 Uiso 1 1 calc R . . C222 C 0.3831(4) 0.45131(18) 0.3282(3) 0.0469(13) Uani 1 1 d . . . H222 H 0.3609 0.4817 0.3338 0.056 Uiso 1 1 calc R . . C223 C 0.4566(4) 0.43276(18) 0.3753(3) 0.0460(13) Uani 1 1 d . . . H223 H 0.4855 0.4505 0.4134 0.055 Uiso 1 1 calc R . . C224 C 0.4889(3) 0.38806(18) 0.3676(2) 0.0416(12) Uani 1 1 d . . . H224 H 0.5398 0.3756 0.4005 0.050 Uiso 1 1 calc R . . C225 C 0.6853(3) 0.17953(15) 0.23264(19) 0.0268(9) Uani 1 1 d . . . C226 C 0.7603(3) 0.14728(17) 0.2453(2) 0.0361(11) Uani 1 1 d . B . C227 C 0.8430(3) 0.15904(18) 0.2285(2) 0.0376(11) Uani 1 1 d . . . H227 H 0.8933 0.1373 0.2368 0.045 Uiso 1 1 calc R . . C228 C 0.8538(3) 0.20129(18) 0.2002(2) 0.0359(11) Uani 1 1 d . . . H228 H 0.9104 0.2084 0.1882 0.043 Uiso 1 1 calc R . . C229 C 0.7812(3) 0.23317(17) 0.1895(2) 0.0331(10) Uani 1 1 d . . . H229 H 0.7890 0.2627 0.1709 0.040 Uiso 1 1 calc R . . C230 C 0.6967(3) 0.22297(15) 0.20521(19) 0.0274(9) Uani 1 1 d . . . C231 C 0.6192(3) 0.25853(16) 0.1856(2) 0.0321(10) Uani 1 1 d . . . H231 H 0.5680 0.2490 0.2065 0.038 Uiso 1 1 calc R . . C232 C 0.6493(3) 0.30828(17) 0.2098(3) 0.0431(12) Uani 1 1 d . . . H23C H 0.5958 0.3295 0.1958 0.065 Uiso 1 1 calc R . . H23D H 0.7004 0.3186 0.1908 0.065 Uiso 1 1 calc R . . H23E H 0.6708 0.3084 0.2582 0.065 Uiso 1 1 calc R . . C233 C 0.5783(3) 0.25843(18) 0.1112(2) 0.0428(12) Uani 1 1 d . . . H23F H 0.5279 0.2816 0.0996 0.064 Uiso 1 1 calc R . . H23G H 0.5529 0.2275 0.0971 0.064 Uiso 1 1 calc R . . H23H H 0.6275 0.2662 0.0890 0.064 Uiso 1 1 calc R . . C234 C 0.7537(4) 0.1013(2) 0.2783(3) 0.0550(15) Uani 1 1 d . . . H234 H 0.6876 0.0913 0.2586 0.066 Uiso 1 1 calc R A 1 C35A C 0.7592(8) 0.1036(4) 0.3442(5) 0.070(3) Uani 0.614(10) 1 d P B 1 H35A H 0.7543 0.0721 0.3613 0.105 Uiso 0.614(10) 1 calc PR B 1 H35B H 0.7079 0.1229 0.3516 0.105 Uiso 0.614(10) 1 calc PR B 1 H35C H 0.8194 0.1173 0.3673 0.105 Uiso 0.614(10) 1 calc PR B 1 C36A C 0.8136(8) 0.0624(4) 0.2550(6) 0.071(3) Uani 0.614(10) 1 d P B 1 H36A H 0.8036 0.0640 0.2069 0.107 Uiso 0.614(10) 1 calc PR B 1 H36B H 0.7942 0.0318 0.2674 0.107 Uiso 0.614(10) 1 calc PR B 1 H36C H 0.8802 0.0673 0.2763 0.107 Uiso 0.614(10) 1 calc PR B 1 C35B C 0.8473(10) 0.0917(6) 0.3395(8) 0.064(5) Uani 0.386(10) 1 d P B 2 H35D H 0.8657 0.1206 0.3643 0.096 Uiso 0.386(10) 1 calc PR B 2 H35E H 0.8990 0.0809 0.3215 0.096 Uiso 0.386(10) 1 calc PR B 2 H35F H 0.8329 0.0679 0.3692 0.096 Uiso 0.386(10) 1 calc PR B 2 C36B C 0.7233(11) 0.0622(5) 0.2416(7) 0.055(4) Uani 0.386(10) 1 d P B 2 H36D H 0.7236 0.0357 0.2712 0.082 Uiso 0.386(10) 1 calc PR B 2 H36E H 0.7651 0.0556 0.2129 0.082 Uiso 0.386(10) 1 calc PR B 2 H36F H 0.6595 0.0673 0.2143 0.082 Uiso 0.386(10) 1 calc PR B 2 O41 O 0.7749(5) 0.0879(3) 0.5829(4) 0.156(3) Uani 1 1 d . . . C41 C 0.9041(9) 0.0627(6) 0.6714(7) 0.219(8) Uani 1 1 d U . . H41A H 0.9553 0.0728 0.7084 0.329 Uiso 1 1 calc R . . H41B H 0.9297 0.0449 0.6399 0.329 Uiso 1 1 calc R . . H41C H 0.8607 0.0430 0.6881 0.329 Uiso 1 1 calc R . . C42 C 0.8515(9) 0.1053(6) 0.6366(8) 0.206(7) Uani 1 1 d . . . H42A H 0.8262 0.1240 0.6681 0.247 Uiso 1 1 calc R . . H42B H 0.8942 0.1252 0.6187 0.247 Uiso 1 1 calc R . . C43 C 0.7210(7) 0.1234(4) 0.5408(6) 0.126(4) Uani 1 1 d . . . H43A H 0.6923 0.1446 0.5676 0.151 Uiso 1 1 calc R . . H43B H 0.7626 0.1420 0.5201 0.151 Uiso 1 1 calc R . . C44 C 0.6549(11) 0.1036(5) 0.4946(6) 0.200(7) Uani 1 1 d U . . H44A H 0.6180 0.1276 0.4663 0.300 Uiso 1 1 calc R . . H44B H 0.6138 0.0853 0.5153 0.300 Uiso 1 1 calc R . . H44C H 0.6836 0.0830 0.4677 0.300 Uiso 1 1 calc R . . O51 O 0.3247(6) 0.4054(3) 0.0697(5) 0.175(3) Uani 1 1 d . . . C51 C 0.3347(16) 0.4890(6) 0.0804(16) 0.42(2) Uani 1 1 d U . . H51A H 0.3765 0.5158 0.0933 0.627 Uiso 1 1 calc R . . H51B H 0.2903 0.4877 0.1084 0.627 Uiso 1 1 calc R . . H51C H 0.3001 0.4922 0.0340 0.627 Uiso 1 1 calc R . . C52 C 0.3926(10) 0.4443(6) 0.0892(8) 0.228(8) Uani 1 1 d U . . H52A H 0.4371 0.4448 0.0607 0.273 Uiso 1 1 calc R . . H52B H 0.4286 0.4407 0.1358 0.273 Uiso 1 1 calc R . . C53 C 0.3680(8) 0.3621(5) 0.0753(5) 0.140(4) Uani 1 1 d . . . H53A H 0.3999 0.3553 0.1220 0.168 Uiso 1 1 calc R . . H53B H 0.4150 0.3610 0.0487 0.168 Uiso 1 1 calc R . . C54 C 0.2910(8) 0.3278(4) 0.0496(5) 0.132(4) Uani 1 1 d . . . H54A H 0.3172 0.2963 0.0527 0.198 Uiso 1 1 calc R . . H54B H 0.2606 0.3349 0.0033 0.198 Uiso 1 1 calc R . . H54C H 0.2447 0.3297 0.0760 0.198 Uiso 1 1 calc R . . O61 O 0.0659(5) 0.1087(3) 0.5861(4) 0.160(3) Uani 1 1 d . . . C61 C 0.1143(7) 0.1579(3) 0.6763(5) 0.132(4) Uani 1 1 d . . . H61A H 0.1593 0.1612 0.7194 0.198 Uiso 1 1 calc R . . H61B H 0.0503 0.1588 0.6820 0.198 Uiso 1 1 calc R . . H61C H 0.1230 0.1834 0.6471 0.198 Uiso 1 1 calc R . . C62 C 0.1300(7) 0.1131(4) 0.6465(5) 0.135(4) Uani 1 1 d . . . H62A H 0.1946 0.1118 0.6406 0.162 Uiso 1 1 calc R . . H62B H 0.1222 0.0871 0.6760 0.162 Uiso 1 1 calc R . . C63 C 0.0817(12) 0.0651(4) 0.5485(9) 0.215(7) Uani 1 1 d U . . H63A H 0.0775 0.0373 0.5758 0.258 Uiso 1 1 calc R . . H63B H 0.1458 0.0660 0.5417 0.258 Uiso 1 1 calc R . . C64 C 0.0104(15) 0.0601(5) 0.4809(8) 0.337(16) Uani 1 1 d U . . H64A H 0.0235 0.0315 0.4592 0.505 Uiso 1 1 calc R . . H64B H 0.0155 0.0870 0.4531 0.505 Uiso 1 1 calc R . . H64C H -0.0532 0.0586 0.4873 0.505 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 Zr11 0.01865(19) 0.0214(2) 0.02167(19) -0.00422(15) 0.00740(14) -0.00171(16) Cl11 0.0249(5) 0.0379(6) 0.0320(5) -0.0050(5) 0.0023(4) 0.0034(5) N11 0.0186(16) 0.0204(18) 0.0214(16) -0.0031(13) 0.0067(13) -0.0012(13) N12 0.0236(17) 0.0225(19) 0.0271(17) 0.0007(14) 0.0095(14) 0.0011(14) N13 0.0210(17) 0.0244(19) 0.0298(18) -0.0043(15) 0.0089(14) -0.0009(14) N14 0.0262(18) 0.026(2) 0.0219(17) -0.0053(14) 0.0107(14) -0.0036(15) N15 0.0189(17) 0.0251(19) 0.0320(19) -0.0050(15) 0.0100(14) -0.0020(14) Zr21 0.01697(19) 0.0303(2) 0.0264(2) -0.00834(17) 0.00559(15) -0.00118(17) Cl21 0.0212(5) 0.0474(7) 0.0430(6) -0.0204(5) 0.0029(4) -0.0037(5) N21 0.0225(18) 0.032(2) 0.0272(18) -0.0034(15) 0.0062(14) -0.0018(15) N22 0.031(2) 0.040(2) 0.0271(18) -0.0059(16) 0.0074(15) -0.0003(17) N23 0.0235(18) 0.037(2) 0.034(2) -0.0094(16) 0.0105(15) -0.0001(16) N24 0.0215(18) 0.028(2) 0.0322(19) -0.0060(15) 0.0052(14) 0.0016(15) N25 0.0179(17) 0.030(2) 0.0310(18) -0.0095(15) 0.0065(14) -0.0036(15) C11 0.020(2) 0.025(2) 0.030(2) -0.0045(17) 0.0079(16) -0.0010(17) C12 0.023(2) 0.025(2) 0.030(2) -0.0039(17) 0.0109(17) -0.0027(17) C13 0.033(2) 0.026(2) 0.036(2) 0.0037(19) 0.0134(19) 0.0008(19) C14 0.036(2) 0.020(2) 0.049(3) 0.003(2) 0.020(2) 0.0009(19) C15 0.031(2) 0.024(2) 0.043(3) -0.0038(19) 0.0139(19) 0.0027(19) C16 0.020(2) 0.031(2) 0.032(2) -0.0107(18) 0.0066(17) -0.0022(18) C17 0.026(2) 0.031(3) 0.026(2) -0.0104(18) 0.0056(17) 0.0020(18) C18 0.036(2) 0.029(2) 0.022(2) 0.0023(17) 0.0087(18) 0.0040(19) C19 0.034(2) 0.028(2) 0.023(2) 0.0024(17) 0.0076(17) 0.0043(19) C110 0.024(2) 0.022(2) 0.032(2) -0.0023(17) 0.0096(17) -0.0005(17) C111 0.022(2) 0.023(2) 0.0209(19) -0.0024(16) 0.0063(15) -0.0006(17) C112 0.024(2) 0.028(2) 0.0203(19) -0.0030(16) 0.0101(16) 0.0017(17) C113 0.030(2) 0.026(2) 0.033(2) -0.0022(18) 0.0153(18) 0.0014(19) C114 0.040(3) 0.029(3) 0.036(2) 0.0029(19) 0.017(2) 0.010(2) C115 0.027(2) 0.039(3) 0.043(3) 0.001(2) 0.017(2) 0.012(2) C116 0.033(2) 0.045(3) 0.043(3) 0.003(2) 0.022(2) 0.000(2) C117 0.031(2) 0.027(2) 0.034(2) 0.0026(18) 0.0186(19) 0.0068(19) C118 0.020(2) 0.034(3) 0.034(2) -0.0097(19) 0.0109(17) -0.0007(18) C119 0.019(2) 0.043(3) 0.041(3) -0.015(2) 0.0112(18) -0.0035(19) C120 0.039(3) 0.042(3) 0.061(3) -0.011(2) 0.025(2) 0.004(2) C121 0.038(3) 0.055(4) 0.081(4) -0.030(3) 0.029(3) -0.002(3) C122 0.031(3) 0.084(5) 0.066(4) -0.042(4) 0.016(3) -0.002(3) C123 0.025(3) 0.103(5) 0.042(3) -0.020(3) 0.012(2) 0.000(3) C124 0.029(2) 0.055(3) 0.041(3) -0.009(2) 0.015(2) 0.002(2) C125 0.022(2) 0.018(2) 0.025(2) -0.0007(16) 0.0061(16) 0.0010(16) C126 0.029(2) 0.021(2) 0.024(2) 0.0019(17) 0.0030(16) -0.0003(17) C127 0.029(2) 0.022(2) 0.030(2) 0.0017(17) -0.0019(18) -0.0012(18) C128 0.020(2) 0.026(2) 0.043(3) 0.007(2) 0.0017(18) -0.0041(18) C129 0.028(2) 0.029(3) 0.039(2) 0.003(2) 0.0140(19) 0.0003(19) C130 0.023(2) 0.025(2) 0.034(2) 0.0009(18) 0.0118(17) -0.0020(17) C131 0.037(2) 0.027(2) 0.028(2) -0.0044(18) 0.0131(18) -0.0089(19) C132 0.063(4) 0.052(3) 0.042(3) -0.015(2) 0.023(3) -0.020(3) C133 0.038(3) 0.026(3) 0.060(3) -0.004(2) 0.022(2) 0.001(2) C134 0.027(2) 0.040(3) 0.044(3) -0.013(2) 0.019(2) -0.009(2) C135 0.057(3) 0.072(4) 0.039(3) -0.010(3) 0.021(3) -0.014(3) C136 0.038(3) 0.048(3) 0.075(4) -0.021(3) 0.027(3) -0.001(2) C21 0.023(2) 0.048(3) 0.039(3) -0.005(2) 0.0130(19) -0.007(2) C22 0.041(3) 0.046(3) 0.041(3) -0.002(2) 0.025(2) -0.002(2) C23 0.044(3) 0.054(3) 0.028(2) -0.009(2) 0.012(2) -0.001(2) C24 0.045(3) 0.062(4) 0.032(3) -0.014(2) 0.017(2) 0.000(3) C25 0.029(2) 0.049(3) 0.041(3) -0.022(2) 0.010(2) 0.003(2) C26 0.022(2) 0.039(3) 0.039(2) -0.010(2) 0.0118(18) 0.0059(19) C27 0.024(2) 0.033(3) 0.038(2) -0.006(2) 0.0061(18) 0.0012(19) C28 0.027(2) 0.031(2) 0.024(2) -0.0052(18) 0.0035(17) 0.0001(19) C29 0.030(2) 0.035(3) 0.030(2) -0.0057(19) 0.0005(18) -0.003(2) C210 0.029(2) 0.028(2) 0.033(2) -0.0092(19) 0.0038(18) -0.0069(19) C211 0.030(2) 0.036(3) 0.033(2) 0.000(2) 0.0051(19) 0.001(2) C212 0.034(3) 0.037(3) 0.039(3) 0.002(2) 0.005(2) -0.002(2) C213 0.040(3) 0.030(3) 0.054(3) 0.004(2) 0.012(2) -0.002(2) C214 0.054(3) 0.035(3) 0.066(4) -0.001(3) 0.007(3) -0.002(3) C215 0.057(4) 0.041(3) 0.081(4) 0.009(3) 0.012(3) -0.010(3) C216 0.076(4) 0.060(4) 0.073(4) 0.015(3) 0.033(3) -0.017(3) C217 0.077(4) 0.043(3) 0.055(3) 0.001(3) 0.030(3) -0.011(3) C218 0.027(2) 0.036(3) 0.042(3) -0.014(2) 0.0095(19) 0.000(2) C219 0.035(3) 0.033(3) 0.044(3) -0.009(2) 0.017(2) -0.002(2) C220 0.041(3) 0.042(3) 0.043(3) -0.009(2) 0.007(2) 0.000(2) C221 0.042(3) 0.036(3) 0.057(3) -0.006(2) 0.009(2) 0.002(2) C222 0.048(3) 0.034(3) 0.065(3) -0.012(3) 0.024(3) 0.005(2) C223 0.044(3) 0.044(3) 0.050(3) -0.019(2) 0.012(2) 0.000(2) C224 0.035(3) 0.042(3) 0.047(3) -0.014(2) 0.008(2) 0.001(2) C225 0.021(2) 0.033(2) 0.027(2) -0.0108(18) 0.0064(16) -0.0018(18) C226 0.026(2) 0.037(3) 0.044(3) -0.007(2) 0.0061(19) 0.002(2) C227 0.024(2) 0.047(3) 0.041(3) -0.014(2) 0.0062(19) 0.007(2) C228 0.023(2) 0.055(3) 0.031(2) -0.014(2) 0.0101(18) -0.008(2) C229 0.031(2) 0.041(3) 0.030(2) -0.010(2) 0.0122(18) -0.006(2) C230 0.023(2) 0.034(3) 0.025(2) -0.0120(18) 0.0044(16) -0.0035(18) C231 0.026(2) 0.033(3) 0.039(2) -0.005(2) 0.0113(19) -0.0030(19) C232 0.039(3) 0.036(3) 0.058(3) -0.007(2) 0.020(2) -0.002(2) C233 0.041(3) 0.045(3) 0.040(3) 0.002(2) 0.007(2) 0.006(2) C234 0.033(3) 0.045(3) 0.088(5) 0.008(3) 0.017(3) 0.011(2) C35A 0.068(7) 0.083(8) 0.056(6) 0.019(5) 0.011(5) 0.009(6) C36A 0.070(8) 0.053(7) 0.098(8) 0.016(6) 0.032(6) 0.022(5) C35B 0.040(9) 0.068(11) 0.073(11) 0.030(9) -0.007(7) 0.004(7) C36B 0.063(11) 0.035(8) 0.062(9) -0.012(7) 0.008(7) 0.002(7) O41 0.100(5) 0.221(9) 0.132(6) 0.072(6) 0.004(4) -0.009(5) C41 0.174(13) 0.30(2) 0.174(12) 0.144(13) 0.025(10) 0.067(13) C42 0.106(9) 0.267(19) 0.234(16) 0.090(15) 0.020(10) -0.026(11) C43 0.105(7) 0.114(8) 0.148(9) 0.054(7) 0.014(7) -0.007(6) C44 0.241(16) 0.174(13) 0.119(9) 0.011(9) -0.076(10) 0.024(11) O51 0.119(6) 0.133(7) 0.249(10) 0.002(6) 0.004(6) -0.019(5) C51 0.27(2) 0.146(16) 0.74(5) 0.13(2) -0.05(3) 0.004(16) C52 0.151(12) 0.257(19) 0.233(16) 0.004(14) -0.030(11) -0.129(14) C53 0.158(11) 0.169(12) 0.106(7) -0.012(8) 0.056(7) 0.071(10) C54 0.163(10) 0.117(8) 0.102(7) 0.003(6) 0.005(7) -0.019(8) O61 0.140(6) 0.118(6) 0.185(8) 0.002(5) -0.029(5) 0.009(5) C61 0.120(8) 0.089(7) 0.161(10) -0.002(7) -0.015(7) 0.010(6) C62 0.100(7) 0.142(10) 0.123(8) 0.006(7) -0.048(6) 0.014(7) C63 0.252(18) 0.081(9) 0.29(2) -0.032(11) 0.036(15) 0.019(10) C64 0.49(3) 0.164(14) 0.209(16) 0.018(12) -0.19(2) -0.072(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Zr11 N12 2.070(3) . ? Zr11 N14 2.073(3) . ? Zr11 N15 2.140(3) . ? Zr11 N13 2.485(3) . ? Zr11 Cl11 2.4984(11) . ? Zr11 N11 2.554(3) . ? N11 C11 1.487(5) . ? N11 C110 1.491(5) . ? N11 C111 1.506(5) . ? N12 C12 1.450(5) . ? N12 C13 1.468(5) . ? N13 C16 1.482(5) . ? N13 C15 1.488(5) . ? N13 C118 1.518(5) . ? N14 C18 1.448(5) . ? N14 C17 1.461(5) . ? N15 C125 1.401(5) . ? N15 H15 0.8800 . ? Zr21 N24 2.062(3) . ? Zr21 N22 2.083(4) . ? Zr21 N25 2.133(3) . ? Zr21 Cl21 2.4845(11) . ? Zr21 N23 2.492(4) . ? Zr21 N21 2.495(3) . ? N21 C210 1.484(5) . ? N21 C21 1.484(5) . ? N21 C211 1.495(5) . ? N22 C22 1.445(6) . ? N22 C23 1.468(5) . ? N23 C26 1.474(5) . ? N23 C25 1.491(5) . ? N23 C218 1.502(6) . ? N24 C27 1.453(5) . ? N24 C28 1.471(5) . ? N25 C225 1.411(5) . ? N25 H25 0.8800 . ? C11 C12 1.509(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.526(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.528(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.498(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.525(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C110 1.518(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C110 H11C 0.9900 . ? C110 H11D 0.9900 . ? C111 C112 1.523(5) . ? C111 H11E 0.9900 . ? C111 H11F 0.9900 . ? C112 C113 1.386(6) . ? C112 C117 1.389(6) . ? C113 C114 1.386(6) . ? C113 H113 0.9500 . ? C114 C115 1.375(6) . ? C114 H114 0.9500 . ? C115 C116 1.376(7) . ? C115 H115 0.9500 . ? C116 C117 1.384(6) . ? C116 H116 0.9500 . ? C117 H117 0.9500 . ? C118 C119 1.528(6) . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C119 C124 1.386(7) . ? C119 C120 1.394(7) . ? C120 C121 1.390(7) . ? C120 H120 0.9500 . ? C121 C122 1.368(9) . ? C121 H121 0.9500 . ? C122 C123 1.369(9) . ? C122 H122 0.9500 . ? C123 C124 1.392(7) . ? C123 H123 0.9500 . ? C124 H124 0.9500 . ? C125 C130 1.412(5) . ? C125 C126 1.431(5) . ? C126 C127 1.390(6) . ? C126 C131 1.518(6) . ? C127 C128 1.376(6) . ? C127 H127 0.9500 . ? C128 C129 1.374(6) . ? C128 H128 0.9500 . ? C129 C130 1.389(6) . ? C129 H129 0.9500 . ? C130 C134 1.508(6) . ? C131 C132 1.520(6) . ? C131 C133 1.538(6) . ? C131 H131 1.0000 . ? C132 H13C 0.9800 . ? C132 H13D 0.9800 . ? C132 H13E 0.9800 . ? C133 H13F 0.9800 . ? C133 H13G 0.9800 . ? C133 H13H 0.9800 . ? C134 C136 1.532(7) . ? C134 C135 1.542(7) . ? C134 H134 1.0000 . ? C135 H13I 0.9800 . ? C135 H13J 0.9800 . ? C135 H13K 0.9800 . ? C136 H13L 0.9800 . ? C136 H13M 0.9800 . ? C136 H13N 0.9800 . ? C21 C22 1.499(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.509(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.507(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.513(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.509(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C210 1.524(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C210 H21C 0.9900 . ? C210 H21D 0.9900 . ? C211 C212 1.517(6) . ? C211 H21E 0.9900 . ? C211 H21F 0.9900 . ? C212 C217 1.378(7) . ? C212 C213 1.384(7) . ? C213 C214 1.382(7) . ? C213 H213 0.9500 . ? C214 C215 1.369(8) . ? C214 H214 0.9500 . ? C215 C216 1.361(9) . ? C215 H215 0.9500 . ? C216 C217 1.396(8) . ? C216 H216 0.9500 . ? C217 H217 0.9500 . ? C218 C219 1.511(6) . ? C218 H21G 0.9900 . ? C218 H21H 0.9900 . ? C219 C224 1.389(6) . ? C219 C220 1.390(7) . ? C220 C221 1.376(7) . ? C220 H220 0.9500 . ? C221 C222 1.373(7) . ? C221 H221 0.9500 . ? C222 C223 1.374(7) . ? C222 H222 0.9500 . ? C223 C224 1.392(7) . ? C223 H223 0.9500 . ? C224 H224 0.9500 . ? C225 C230 1.400(6) . ? C225 C226 1.415(6) . ? C226 C227 1.391(6) . ? C226 C234 1.504(7) . ? C227 C228 1.376(7) . ? C227 H227 0.9500 . ? C228 C229 1.383(6) . ? C228 H228 0.9500 . ? C229 C230 1.397(6) . ? C229 H229 0.9500 . ? C230 C231 1.510(6) . ? C231 C233 1.517(6) . ? C231 C232 1.543(6) . ? C231 H231 1.0000 . ? C232 H23C 0.9800 . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C233 H23F 0.9800 . ? C233 H23G 0.9800 . ? C233 H23H 0.9800 . ? C234 C35A 1.360(11) . ? C234 C36B 1.369(14) . ? C234 C36A 1.573(11) . ? C234 C35B 1.651(14) . ? C234 H234 1.0000 . ? C35A H35A 0.9800 . ? C35A H35B 0.9800 . ? C35A H35C 0.9800 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C35B H35D 0.9800 . ? C35B H35E 0.9800 . ? C35B H35F 0.9800 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? O41 C43 1.446(10) . ? O41 C42 1.465(15) . ? C41 C42 1.531(17) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.316(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O51 C53 1.390(11) . ? O51 C52 1.485(13) . ? C51 C52 1.53(2) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.497(14) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O61 C62 1.379(10) . ? O61 C63 1.527(14) . ? C61 C62 1.471(13) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.540(17) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 N12 Zr11 N14 116.02(13) . . ? N12 Zr11 N15 127.63(13) . . ? N14 Zr11 N15 98.01(13) . . ? N12 Zr11 N13 82.49(12) . . ? N14 Zr11 N13 71.56(12) . . ? N15 Zr11 N13 148.52(12) . . ? N12 Zr11 Cl11 95.96(9) . . ? N14 Zr11 Cl11 132.65(9) . . ? N15 Zr11 Cl11 87.24(9) . . ? N13 Zr11 Cl11 79.75(8) . . ? N12 Zr11 N11 70.19(11) . . ? N14 Zr11 N11 80.34(11) . . ? N15 Zr11 N11 78.45(11) . . ? N13 Zr11 N11 126.47(10) . . ? Cl11 Zr11 N11 145.96(7) . . ? C11 N11 C110 110.3(3) . . ? C11 N11 C111 109.7(3) . . ? C110 N11 C111 108.8(3) . . ? C11 N11 Zr11 98.1(2) . . ? C110 N11 Zr11 117.0(2) . . ? C111 N11 Zr11 112.4(2) . . ? C12 N12 C13 111.3(3) . . ? C12 N12 Zr11 124.0(3) . . ? C13 N12 Zr11 121.3(3) . . ? C16 N13 C15 110.2(3) . . ? C16 N13 C118 110.8(3) . . ? C15 N13 C118 108.9(3) . . ? C16 N13 Zr11 101.3(2) . . ? C15 N13 Zr11 117.1(2) . . ? C118 N13 Zr11 108.2(2) . . ? C18 N14 C17 112.3(3) . . ? C18 N14 Zr11 122.5(2) . . ? C17 N14 Zr11 123.4(3) . . ? C125 N15 Zr11 141.2(3) . . ? C125 N15 H15 109.4 . . ? Zr11 N15 H15 109.4 . . ? N24 Zr21 N22 115.21(14) . . ? N24 Zr21 N25 99.40(13) . . ? N22 Zr21 N25 129.53(14) . . ? N24 Zr21 Cl21 132.53(10) . . ? N22 Zr21 Cl21 96.47(10) . . ? N25 Zr21 Cl21 84.26(9) . . ? N24 Zr21 N23 71.55(12) . . ? N22 Zr21 N23 81.38(13) . . ? N25 Zr21 N23 146.86(13) . . ? Cl21 Zr21 N23 79.97(8) . . ? N24 Zr21 N21 82.08(12) . . ? N22 Zr21 N21 70.47(13) . . ? N25 Zr21 N21 79.87(12) . . ? Cl21 Zr21 N21 144.09(8) . . ? N23 Zr21 N21 128.05(11) . . ? C210 N21 C21 109.7(3) . . ? C210 N21 C211 109.1(3) . . ? C21 N21 C211 110.3(3) . . ? C210 N21 Zr21 115.8(3) . . ? C21 N21 Zr21 99.4(3) . . ? C211 N21 Zr21 112.1(2) . . ? C22 N22 C23 111.8(4) . . ? C22 N22 Zr21 123.0(3) . . ? C23 N22 Zr21 122.1(3) . . ? C26 N23 C25 110.6(3) . . ? C26 N23 C218 110.8(4) . . ? C25 N23 C218 108.1(3) . . ? C26 N23 Zr21 101.0(2) . . ? C25 N23 Zr21 117.1(3) . . ? C218 N23 Zr21 109.0(2) . . ? C27 N24 C28 112.6(3) . . ? C27 N24 Zr21 124.4(3) . . ? C28 N24 Zr21 121.6(3) . . ? C225 N25 Zr21 135.6(3) . . ? C225 N25 H25 112.2 . . ? Zr21 N25 H25 112.2 . . ? N11 C11 C12 109.9(3) . . ? N11 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N11 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N12 C12 C11 109.8(3) . . ? N12 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? N12 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N12 C13 C14 112.7(3) . . ? N12 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N12 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 113.8(4) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N13 C15 C14 116.7(3) . . ? N13 C15 H15A 108.1 . . ? C14 C15 H15A 108.1 . . ? N13 C15 H15B 108.1 . . ? C14 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? N13 C16 C17 111.0(3) . . ? N13 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N13 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N14 C17 C16 110.1(3) . . ? N14 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? N14 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N14 C18 C19 112.9(3) . . ? N14 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? N14 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C110 C19 C18 114.4(3) . . ? C110 C19 H19A 108.7 . . ? C18 C19 H19A 108.7 . . ? C110 C19 H19B 108.7 . . ? C18 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? N11 C110 C19 116.6(3) . . ? N11 C110 H11C 108.2 . . ? C19 C110 H11C 108.2 . . ? N11 C110 H11D 108.2 . . ? C19 C110 H11D 108.2 . . ? H11C C110 H11D 107.3 . . ? N11 C111 C112 116.4(3) . . ? N11 C111 H11E 108.2 . . ? C112 C111 H11E 108.2 . . ? N11 C111 H11F 108.2 . . ? C112 C111 H11F 108.2 . . ? H11E C111 H11F 107.4 . . ? C113 C112 C117 118.0(4) . . ? C113 C112 C111 120.4(4) . . ? C117 C112 C111 121.6(4) . . ? C112 C113 C114 121.0(4) . . ? C112 C113 H113 119.5 . . ? C114 C113 H113 119.5 . . ? C115 C114 C113 120.3(4) . . ? C115 C114 H114 119.8 . . ? C113 C114 H114 119.8 . . ? C114 C115 C116 119.3(4) . . ? C114 C115 H115 120.3 . . ? C116 C115 H115 120.3 . . ? C115 C116 C117 120.5(4) . . ? C115 C116 H116 119.8 . . ? C117 C116 H116 119.8 . . ? C116 C117 C112 120.8(4) . . ? C116 C117 H117 119.6 . . ? C112 C117 H117 119.6 . . ? N13 C118 C119 116.8(3) . . ? N13 C118 H11G 108.1 . . ? C119 C118 H11G 108.1 . . ? N13 C118 H11H 108.1 . . ? C119 C118 H11H 108.1 . . ? H11G C118 H11H 107.3 . . ? C124 C119 C120 118.3(4) . . ? C124 C119 C118 119.0(4) . . ? C120 C119 C118 122.7(4) . . ? C121 C120 C119 119.6(5) . . ? C121 C120 H120 120.2 . . ? C119 C120 H120 120.2 . . ? C122 C121 C120 121.2(6) . . ? C122 C121 H121 119.4 . . ? C120 C121 H121 119.4 . . ? C121 C122 C123 119.9(5) . . ? C121 C122 H122 120.1 . . ? C123 C122 H122 120.1 . . ? C122 C123 C124 119.6(6) . . ? C122 C123 H123 120.2 . . ? C124 C123 H123 120.2 . . ? C119 C124 C123 121.3(5) . . ? C119 C124 H124 119.4 . . ? C123 C124 H124 119.4 . . ? N15 C125 C130 121.4(3) . . ? N15 C125 C126 120.0(3) . . ? C130 C125 C126 118.6(4) . . ? C127 C126 C125 119.1(4) . . ? C127 C126 C131 120.5(4) . . ? C125 C126 C131 120.4(4) . . ? C128 C127 C126 121.8(4) . . ? C128 C127 H127 119.1 . . ? C126 C127 H127 119.1 . . ? C129 C128 C127 119.0(4) . . ? C129 C128 H128 120.5 . . ? C127 C128 H128 120.5 . . ? C128 C129 C130 122.3(4) . . ? C128 C129 H129 118.8 . . ? C130 C129 H129 118.8 . . ? C129 C130 C125 119.2(4) . . ? C129 C130 C134 118.2(4) . . ? C125 C130 C134 122.6(4) . . ? C126 C131 C132 114.1(4) . . ? C126 C131 C133 110.5(3) . . ? C132 C131 C133 109.1(4) . . ? C126 C131 H131 107.7 . . ? C132 C131 H131 107.7 . . ? C133 C131 H131 107.7 . . ? C131 C132 H13C 109.5 . . ? C131 C132 H13D 109.5 . . ? H13C C132 H13D 109.5 . . ? C131 C132 H13E 109.5 . . ? H13C C132 H13E 109.5 . . ? H13D C132 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? C131 C133 H13G 109.5 . . ? H13F C133 H13G 109.5 . . ? C131 C133 H13H 109.5 . . ? H13F C133 H13H 109.5 . . ? H13G C133 H13H 109.5 . . ? C130 C134 C136 112.0(4) . . ? C130 C134 C135 111.5(4) . . ? C136 C134 C135 110.9(4) . . ? C130 C134 H134 107.4 . . ? C136 C134 H134 107.4 . . ? C135 C134 H134 107.4 . . ? C134 C135 H13I 109.5 . . ? C134 C135 H13J 109.5 . . ? H13I C135 H13J 109.5 . . ? C134 C135 H13K 109.5 . . ? H13I C135 H13K 109.5 . . ? H13J C135 H13K 109.5 . . ? C134 C136 H13L 109.5 . . ? C134 C136 H13M 109.5 . . ? H13L C136 H13M 109.5 . . ? C134 C136 H13N 109.5 . . ? H13L C136 H13N 109.5 . . ? H13M C136 H13N 109.5 . . ? N21 C21 C22 110.2(3) . . ? N21 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? N21 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N22 C22 C21 109.7(4) . . ? N22 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? N22 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N22 C23 C24 112.5(4) . . ? N22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 113.4(4) . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N23 C25 C24 116.3(4) . . ? N23 C25 H25A 108.2 . . ? C24 C25 H25A 108.2 . . ? N23 C25 H25B 108.2 . . ? C24 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? N23 C26 C27 110.8(3) . . ? N23 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? N23 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? N24 C27 C26 109.2(3) . . ? N24 C27 H27A 109.8 . . ? C26 C27 H27A 109.8 . . ? N24 C27 H27B 109.8 . . ? C26 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? N24 C28 C29 112.9(3) . . ? N24 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N24 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C210 114.5(3) . . ? C28 C29 H29A 108.6 . . ? C210 C29 H29A 108.6 . . ? C28 C29 H29B 108.6 . . ? C210 C29 H29B 108.6 . . ? H29A C29 H29B 107.6 . . ? N21 C210 C29 117.4(4) . . ? N21 C210 H21C 108.0 . . ? C29 C210 H21C 108.0 . . ? N21 C210 H21D 108.0 . . ? C29 C210 H21D 108.0 . . ? H21C C210 H21D 107.2 . . ? N21 C211 C212 116.9(4) . . ? N21 C211 H21E 108.1 . . ? C212 C211 H21E 108.1 . . ? N21 C211 H21F 108.1 . . ? C212 C211 H21F 108.1 . . ? H21E C211 H21F 107.3 . . ? C217 C212 C213 117.1(5) . . ? C217 C212 C211 122.2(5) . . ? C213 C212 C211 120.7(4) . . ? C214 C213 C212 122.3(5) . . ? C214 C213 H213 118.9 . . ? C212 C213 H213 118.9 . . ? C215 C214 C213 119.0(6) . . ? C215 C214 H214 120.5 . . ? C213 C214 H214 120.5 . . ? C216 C215 C214 120.6(6) . . ? C216 C215 H215 119.7 . . ? C214 C215 H215 119.7 . . ? C215 C216 C217 119.8(6) . . ? C215 C216 H216 120.1 . . ? C217 C216 H216 120.1 . . ? C212 C217 C216 121.2(5) . . ? C212 C217 H217 119.4 . . ? C216 C217 H217 119.4 . . ? N23 C218 C219 117.3(4) . . ? N23 C218 H21G 108.0 . . ? C219 C218 H21G 108.0 . . ? N23 C218 H21H 108.0 . . ? C219 C218 H21H 108.0 . . ? H21G C218 H21H 107.2 . . ? C224 C219 C220 117.4(4) . . ? C224 C219 C218 120.7(4) . . ? C220 C219 C218 121.9(4) . . ? C221 C220 C219 122.0(5) . . ? C221 C220 H220 119.0 . . ? C219 C220 H220 119.0 . . ? C222 C221 C220 119.9(5) . . ? C222 C221 H221 120.1 . . ? C220 C221 H221 120.1 . . ? C221 C222 C223 119.7(5) . . ? C221 C222 H222 120.1 . . ? C223 C222 H222 120.1 . . ? C222 C223 C224 120.3(5) . . ? C222 C223 H223 119.8 . . ? C224 C223 H223 119.8 . . ? C219 C224 C223 120.7(5) . . ? C219 C224 H224 119.7 . . ? C223 C224 H224 119.7 . . ? C230 C225 N25 120.7(4) . . ? C230 C225 C226 119.4(4) . . ? N25 C225 C226 119.9(4) . . ? C227 C226 C225 119.1(4) . . ? C227 C226 C234 119.3(4) . . ? C225 C226 C234 121.5(4) . . ? C228 C227 C226 121.7(4) . . ? C228 C227 H227 119.2 . . ? C226 C227 H227 119.2 . . ? C227 C228 C229 119.0(4) . . ? C227 C228 H228 120.5 . . ? C229 C228 H228 120.5 . . ? C228 C229 C230 121.5(5) . . ? C228 C229 H229 119.3 . . ? C230 C229 H229 119.3 . . ? C229 C230 C225 119.3(4) . . ? C229 C230 C231 116.9(4) . . ? C225 C230 C231 123.6(4) . . ? C230 C231 C233 110.8(4) . . ? C230 C231 C232 113.7(4) . . ? C233 C231 C232 110.2(4) . . ? C230 C231 H231 107.3 . . ? C233 C231 H231 107.3 . . ? C232 C231 H231 107.3 . . ? C231 C232 H23C 109.5 . . ? C231 C232 H23D 109.5 . . ? H23C C232 H23D 109.5 . . ? C231 C232 H23E 109.5 . . ? H23C C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? C231 C233 H23G 109.5 . . ? H23F C233 H23G 109.5 . . ? C231 C233 H23H 109.5 . . ? H23F C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? C35A C234 C36B 122.2(9) . . ? C35A C234 C226 115.3(7) . . ? C36B C234 C226 120.9(8) . . ? C35A C234 C36A 116.8(7) . . ? C36B C234 C36A 51.4(8) . . ? C226 C234 C36A 112.1(6) . . ? C35A C234 C35B 53.0(8) . . ? C36B C234 C35B 112.9(9) . . ? C226 C234 C35B 111.3(7) . . ? C36A C234 C35B 72.4(8) . . ? C35A C234 H234 103.5 . . ? C36B C234 H234 52.2 . . ? C226 C234 H234 103.5 . . ? C36A C234 H234 103.5 . . ? C35B C234 H234 143.9 . . ? C234 C35A H35A 109.5 . . ? C234 C35A H35B 109.5 . . ? H35A C35A H35B 109.5 . . ? C234 C35A H35C 109.5 . . ? H35A C35A H35C 109.5 . . ? H35B C35A H35C 109.5 . . ? C234 C36A H36A 109.5 . . ? C234 C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C234 C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C234 C35B H35D 109.5 . . ? C234 C35B H35E 109.5 . . ? H35D C35B H35E 109.5 . . ? C234 C35B H35F 109.5 . . ? H35D C35B H35F 109.5 . . ? H35E C35B H35F 109.5 . . ? C234 C36B H36D 109.5 . . ? C234 C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C234 C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? C43 O41 C42 115.1(10) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O41 C42 C41 106.9(13) . . ? O41 C42 H42A 110.3 . . ? C41 C42 H42A 110.3 . . ? O41 C42 H42B 110.3 . . ? C41 C42 H42B 110.3 . . ? H42A C42 H42B 108.6 . . ? C44 C43 O41 109.4(10) . . ? C44 C43 H43A 109.8 . . ? O41 C43 H43A 109.8 . . ? C44 C43 H43B 109.8 . . ? O41 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C53 O51 C52 112.7(11) . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O51 C52 C51 106.4(13) . . ? O51 C52 H52A 110.5 . . ? C51 C52 H52A 110.5 . . ? O51 C52 H52B 110.5 . . ? C51 C52 H52B 110.5 . . ? H52A C52 H52B 108.6 . . ? O51 C53 C54 105.6(9) . . ? O51 C53 H53A 110.6 . . ? C54 C53 H53A 110.6 . . ? O51 C53 H53B 110.6 . . ? C54 C53 H53B 110.6 . . ? H53A C53 H53B 108.8 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C62 O61 C63 112.8(9) . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O61 C62 C61 108.8(8) . . ? O61 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? O61 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? O61 C63 C64 113.0(13) . . ? O61 C63 H63A 109.0 . . ? C64 C63 H63A 109.0 . . ? O61 C63 H63B 109.0 . . ? C64 C63 H63B 109.0 . . ? H63A C63 H63B 107.8 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 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 N12 Zr11 N11 C11 -40.6(2) . . . . ? N14 Zr11 N11 C11 81.7(2) . . . . ? N15 Zr11 N11 C11 -178.0(2) . . . . ? N13 Zr11 N11 C11 23.4(3) . . . . ? Cl11 Zr11 N11 C11 -111.0(2) . . . . ? N12 Zr11 N11 C110 -158.4(3) . . . . ? N14 Zr11 N11 C110 -36.1(3) . . . . ? N15 Zr11 N11 C110 64.2(3) . . . . ? N13 Zr11 N11 C110 -94.4(3) . . . . ? Cl11 Zr11 N11 C110 131.2(2) . . . . ? N12 Zr11 N11 C111 74.7(2) . . . . ? N14 Zr11 N11 C111 -163.0(3) . . . . ? N15 Zr11 N11 C111 -62.7(2) . . . . ? N13 Zr11 N11 C111 138.7(2) . . . . ? Cl11 Zr11 N11 C111 4.3(3) . . . . ? N14 Zr11 N12 C12 -43.5(3) . . . . ? N15 Zr11 N12 C12 81.4(3) . . . . ? N13 Zr11 N12 C12 -108.7(3) . . . . ? Cl11 Zr11 N12 C12 172.5(3) . . . . ? N11 Zr11 N12 C12 24.5(3) . . . . ? N14 Zr11 N12 C13 113.7(3) . . . . ? N15 Zr11 N12 C13 -121.4(3) . . . . ? N13 Zr11 N12 C13 48.5(3) . . . . ? Cl11 Zr11 N12 C13 -30.3(3) . . . . ? N11 Zr11 N12 C13 -178.3(3) . . . . ? N12 Zr11 N13 C16 84.1(2) . . . . ? N14 Zr11 N13 C16 -36.6(2) . . . . ? N15 Zr11 N13 C16 -111.3(3) . . . . ? Cl11 Zr11 N13 C16 -178.4(2) . . . . ? N11 Zr11 N13 C16 25.6(3) . . . . ? N12 Zr11 N13 C15 -35.7(3) . . . . ? N14 Zr11 N13 C15 -156.4(3) . . . . ? N15 Zr11 N13 C15 128.8(3) . . . . ? Cl11 Zr11 N13 C15 61.7(3) . . . . ? N11 Zr11 N13 C15 -94.2(3) . . . . ? N12 Zr11 N13 C118 -159.3(3) . . . . ? N14 Zr11 N13 C118 80.0(3) . . . . ? N15 Zr11 N13 C118 5.3(4) . . . . ? Cl11 Zr11 N13 C118 -61.8(2) . . . . ? N11 Zr11 N13 C118 142.2(2) . . . . ? N12 Zr11 N14 C18 112.6(3) . . . . ? N15 Zr11 N14 C18 -26.4(3) . . . . ? N13 Zr11 N14 C18 -175.8(3) . . . . ? Cl11 Zr11 N14 C18 -120.0(3) . . . . ? N11 Zr11 N14 C18 50.4(3) . . . . ? N12 Zr11 N14 C17 -50.9(3) . . . . ? N15 Zr11 N14 C17 170.1(3) . . . . ? N13 Zr11 N14 C17 20.6(3) . . . . ? Cl11 Zr11 N14 C17 76.4(3) . . . . ? N11 Zr11 N14 C17 -113.2(3) . . . . ? N12 Zr11 N15 C125 130.1(4) . . . . ? N14 Zr11 N15 C125 -98.0(4) . . . . ? N13 Zr11 N15 C125 -30.4(5) . . . . ? Cl11 Zr11 N15 C125 34.7(4) . . . . ? N11 Zr11 N15 C125 -176.3(4) . . . . ? N24 Zr21 N21 C210 37.5(3) . . . . ? N22 Zr21 N21 C210 157.9(3) . . . . ? N25 Zr21 N21 C210 -63.5(3) . . . . ? Cl21 Zr21 N21 C210 -128.7(2) . . . . ? N23 Zr21 N21 C210 96.6(3) . . . . ? N24 Zr21 N21 C21 -79.9(3) . . . . ? N22 Zr21 N21 C21 40.5(2) . . . . ? N25 Zr21 N21 C21 179.1(3) . . . . ? Cl21 Zr21 N21 C21 113.9(2) . . . . ? N23 Zr21 N21 C21 -20.8(3) . . . . ? N24 Zr21 N21 C211 163.6(3) . . . . ? N22 Zr21 N21 C211 -76.0(3) . . . . ? N25 Zr21 N21 C211 62.5(3) . . . . ? Cl21 Zr21 N21 C211 -2.7(3) . . . . ? N23 Zr21 N21 C211 -137.4(3) . . . . ? N24 Zr21 N22 C22 45.8(4) . . . . ? N25 Zr21 N22 C22 -82.7(4) . . . . ? Cl21 Zr21 N22 C22 -170.6(3) . . . . ? N23 Zr21 N22 C22 110.7(4) . . . . ? N21 Zr21 N22 C22 -25.0(3) . . . . ? N24 Zr21 N22 C23 -112.7(3) . . . . ? N25 Zr21 N22 C23 118.8(3) . . . . ? Cl21 Zr21 N22 C23 30.9(3) . . . . ? N23 Zr21 N22 C23 -47.9(3) . . . . ? N21 Zr21 N22 C23 176.4(4) . . . . ? N24 Zr21 N23 C26 36.0(3) . . . . ? N22 Zr21 N23 C26 -84.3(3) . . . . ? N25 Zr21 N23 C26 114.7(3) . . . . ? Cl21 Zr21 N23 C26 177.5(3) . . . . ? N21 Zr21 N23 C26 -27.5(3) . . . . ? N24 Zr21 N23 C25 156.2(3) . . . . ? N22 Zr21 N23 C25 35.9(3) . . . . ? N25 Zr21 N23 C25 -125.1(3) . . . . ? Cl21 Zr21 N23 C25 -62.3(3) . . . . ? N21 Zr21 N23 C25 92.7(3) . . . . ? N24 Zr21 N23 C218 -80.7(3) . . . . ? N22 Zr21 N23 C218 159.0(3) . . . . ? N25 Zr21 N23 C218 -2.0(4) . . . . ? Cl21 Zr21 N23 C218 60.8(2) . . . . ? N21 Zr21 N23 C218 -144.3(2) . . . . ? N22 Zr21 N24 C27 51.9(4) . . . . ? N25 Zr21 N24 C27 -165.8(3) . . . . ? Cl21 Zr21 N24 C27 -75.0(4) . . . . ? N23 Zr21 N24 C27 -18.7(3) . . . . ? N21 Zr21 N24 C27 115.9(3) . . . . ? N22 Zr21 N24 C28 -113.9(3) . . . . ? N25 Zr21 N24 C28 28.4(3) . . . . ? Cl21 Zr21 N24 C28 119.2(3) . . . . ? N23 Zr21 N24 C28 175.5(3) . . . . ? N21 Zr21 N24 C28 -49.9(3) . . . . ? N24 Zr21 N25 C225 104.7(4) . . . . ? N22 Zr21 N25 C225 -121.2(4) . . . . ? Cl21 Zr21 N25 C225 -27.5(4) . . . . ? N23 Zr21 N25 C225 34.2(5) . . . . ? N21 Zr21 N25 C225 -175.2(4) . . . . ? C110 N11 C11 C12 176.5(3) . . . . ? C111 N11 C11 C12 -63.8(4) . . . . ? Zr11 N11 C11 C12 53.7(3) . . . . ? C13 N12 C12 C11 -161.2(3) . . . . ? Zr11 N12 C12 C11 -2.0(4) . . . . ? N11 C11 C12 N12 -41.1(4) . . . . ? C12 N12 C13 C14 84.9(4) . . . . ? Zr11 N12 C13 C14 -74.9(4) . . . . ? N12 C13 C14 C15 71.4(5) . . . . ? C16 N13 C15 C14 -67.4(5) . . . . ? C118 N13 C15 C14 170.8(4) . . . . ? Zr11 N13 C15 C14 47.6(4) . . . . ? C13 C14 C15 N13 -61.1(5) . . . . ? C15 N13 C16 C17 174.3(3) . . . . ? C118 N13 C16 C17 -65.1(4) . . . . ? Zr11 N13 C16 C17 49.6(3) . . . . ? C18 N14 C17 C16 -164.6(3) . . . . ? Zr11 N14 C17 C16 0.5(4) . . . . ? N13 C16 C17 N14 -38.0(4) . . . . ? C17 N14 C18 C19 88.0(4) . . . . ? Zr11 N14 C18 C19 -77.2(4) . . . . ? N14 C18 C19 C110 71.0(5) . . . . ? C11 N11 C110 C19 -63.8(4) . . . . ? C111 N11 C110 C19 175.9(3) . . . . ? Zr11 N11 C110 C19 47.2(4) . . . . ? C18 C19 C110 N11 -60.1(5) . . . . ? C11 N11 C111 C112 -60.3(4) . . . . ? C110 N11 C111 C112 60.4(4) . . . . ? Zr11 N11 C111 C112 -168.4(3) . . . . ? N11 C111 C112 C113 -88.8(5) . . . . ? N11 C111 C112 C117 91.9(5) . . . . ? C117 C112 C113 C114 -1.7(6) . . . . ? C111 C112 C113 C114 178.9(4) . . . . ? C112 C113 C114 C115 0.4(7) . . . . ? C113 C114 C115 C116 1.7(7) . . . . ? C114 C115 C116 C117 -2.3(7) . . . . ? C115 C116 C117 C112 1.0(7) . . . . ? C113 C112 C117 C116 1.1(6) . . . . ? C111 C112 C117 C116 -179.6(4) . . . . ? C16 N13 C118 C119 -50.8(5) . . . . ? C15 N13 C118 C119 70.6(5) . . . . ? Zr11 N13 C118 C119 -161.1(3) . . . . ? N13 C118 C119 C124 108.9(5) . . . . ? N13 C118 C119 C120 -73.9(5) . . . . ? C124 C119 C120 C121 -3.7(7) . . . . ? C118 C119 C120 C121 179.1(4) . . . . ? C119 C120 C121 C122 2.2(7) . . . . ? C120 C121 C122 C123 0.8(8) . . . . ? C121 C122 C123 C124 -2.2(8) . . . . ? C120 C119 C124 C123 2.3(7) . . . . ? C118 C119 C124 C123 179.6(4) . . . . ? C122 C123 C124 C119 0.7(7) . . . . ? Zr11 N15 C125 C130 39.9(6) . . . . ? Zr11 N15 C125 C126 -139.6(4) . . . . ? N15 C125 C126 C127 -179.9(4) . . . . ? C130 C125 C126 C127 0.5(6) . . . . ? N15 C125 C126 C131 -1.9(6) . . . . ? C130 C125 C126 C131 178.6(4) . . . . ? C125 C126 C127 C128 0.1(6) . . . . ? C131 C126 C127 C128 -177.9(4) . . . . ? C126 C127 C128 C129 -0.4(6) . . . . ? C127 C128 C129 C130 0.0(6) . . . . ? C128 C129 C130 C125 0.6(6) . . . . ? C128 C129 C130 C134 178.1(4) . . . . ? N15 C125 C130 C129 179.6(4) . . . . ? C126 C125 C130 C129 -0.9(6) . . . . ? N15 C125 C130 C134 2.2(6) . . . . ? C126 C125 C130 C134 -178.2(4) . . . . ? C127 C126 C131 C132 -26.4(6) . . . . ? C125 C126 C131 C132 155.6(4) . . . . ? C127 C126 C131 C133 96.9(4) . . . . ? C125 C126 C131 C133 -81.1(5) . . . . ? C129 C130 C134 C136 55.2(6) . . . . ? C125 C130 C134 C136 -127.5(4) . . . . ? C129 C130 C134 C135 -69.8(5) . . . . ? C125 C130 C134 C135 107.6(5) . . . . ? C210 N21 C21 C22 -175.3(4) . . . . ? C211 N21 C21 C22 64.5(5) . . . . ? Zr21 N21 C21 C22 -53.4(4) . . . . ? C23 N22 C22 C21 163.4(4) . . . . ? Zr21 N22 C22 C21 2.9(5) . . . . ? N21 C21 C22 N22 39.2(5) . . . . ? C22 N22 C23 C24 -86.0(5) . . . . ? Zr21 N22 C23 C24 74.7(5) . . . . ? N22 C23 C24 C25 -72.5(5) . . . . ? C26 N23 C25 C24 65.5(5) . . . . ? C218 N23 C25 C24 -173.0(4) . . . . ? Zr21 N23 C25 C24 -49.5(5) . . . . ? C23 C24 C25 N23 63.5(5) . . . . ? C25 N23 C26 C27 -174.9(4) . . . . ? C218 N23 C26 C27 65.2(5) . . . . ? Zr21 N23 C26 C27 -50.2(4) . . . . ? C28 N24 C27 C26 163.7(4) . . . . ? Zr21 N24 C27 C26 -3.2(5) . . . . ? N23 C26 C27 N24 40.1(5) . . . . ? C27 N24 C28 C29 -92.6(4) . . . . ? Zr21 N24 C28 C29 74.7(4) . . . . ? N24 C28 C29 C210 -69.3(5) . . . . ? C21 N21 C210 C29 62.5(5) . . . . ? C211 N21 C210 C29 -176.6(4) . . . . ? Zr21 N21 C210 C29 -49.0(4) . . . . ? C28 C29 C210 N21 61.0(5) . . . . ? C210 N21 C211 C212 -59.9(5) . . . . ? C21 N21 C211 C212 60.6(5) . . . . ? Zr21 N21 C211 C212 170.4(3) . . . . ? N21 C211 C212 C217 -87.9(6) . . . . ? N21 C211 C212 C213 92.9(5) . . . . ? C217 C212 C213 C214 0.1(7) . . . . ? C211 C212 C213 C214 179.3(4) . . . . ? C212 C213 C214 C215 1.1(8) . . . . ? C213 C214 C215 C216 -1.7(9) . . . . ? C214 C215 C216 C217 1.3(10) . . . . ? C213 C212 C217 C216 -0.6(8) . . . . ? C211 C212 C217 C216 -179.8(5) . . . . ? C215 C216 C217 C212 -0.1(10) . . . . ? C26 N23 C218 C219 65.2(5) . . . . ? C25 N23 C218 C219 -56.1(5) . . . . ? Zr21 N23 C218 C219 175.6(3) . . . . ? N23 C218 C219 C224 89.9(5) . . . . ? N23 C218 C219 C220 -92.4(5) . . . . ? C224 C219 C220 C221 -0.6(7) . . . . ? C218 C219 C220 C221 -178.4(5) . . . . ? C219 C220 C221 C222 0.1(8) . . . . ? C220 C221 C222 C223 0.4(8) . . . . ? C221 C222 C223 C224 -0.5(8) . . . . ? C220 C219 C224 C223 0.5(7) . . . . ? C218 C219 C224 C223 178.3(5) . . . . ? C222 C223 C224 C219 0.0(8) . . . . ? Zr21 N25 C225 C230 -50.9(5) . . . . ? Zr21 N25 C225 C226 129.6(4) . . . . ? C230 C225 C226 C227 -1.8(6) . . . . ? N25 C225 C226 C227 177.7(4) . . . . ? C230 C225 C226 C234 176.4(4) . . . . ? N25 C225 C226 C234 -4.0(6) . . . . ? C225 C226 C227 C228 0.4(7) . . . . ? C234 C226 C227 C228 -177.9(5) . . . . ? C226 C227 C228 C229 1.3(7) . . . . ? C227 C228 C229 C230 -1.6(6) . . . . ? C228 C229 C230 C225 0.2(6) . . . . ? C228 C229 C230 C231 -174.5(4) . . . . ? N25 C225 C230 C229 -178.0(4) . . . . ? C226 C225 C230 C229 1.5(6) . . . . ? N25 C225 C230 C231 -3.8(6) . . . . ? C226 C225 C230 C231 175.8(4) . . . . ? C229 C230 C231 C233 72.3(5) . . . . ? C225 C230 C231 C233 -102.0(5) . . . . ? C229 C230 C231 C232 -52.4(5) . . . . ? C225 C230 C231 C232 133.3(4) . . . . ? C227 C226 C234 C35A 104.8(7) . . . . ? C225 C226 C234 C35A -73.4(8) . . . . ? C227 C226 C234 C36B -89.2(10) . . . . ? C225 C226 C234 C36B 92.5(10) . . . . ? C227 C226 C234 C36A -32.1(8) . . . . ? C225 C226 C234 C36A 149.7(6) . . . . ? C227 C226 C234 C35B 46.8(9) . . . . ? C225 C226 C234 C35B -131.4(8) . . . . ? C43 O41 C42 C41 -175.6(10) . . . . ? C42 O41 C43 C44 179.8(12) . . . . ? C53 O51 C52 C51 180.0(17) . . . . ? C52 O51 C53 C54 -176.2(10) . . . . ? C63 O61 C62 C61 175.2(11) . . . . ? C62 O61 C63 C64 -179.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.674 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.084 #===end data_Compound7 _database_code_depnum_ccdc_archive 'CCDC 727736' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)Zr(N2,6iPr-Ph) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H51 N5 Zr' _chemical_formula_sum 'C36 H51 N5 Zr' _chemical_formula_weight 645.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2564(15) _cell_length_b 10.6519(16) _cell_length_c 19.043(4) _cell_angle_alpha 101.146(11) _cell_angle_beta 95.359(12) _cell_angle_gamma 110.215(8) _cell_volume 1702.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4264 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 25.80 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9326 _exptl_absorpt_correction_T_max 0.9895 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21535 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.80 _reflns_number_total 6378 _reflns_number_gt 4878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0773P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6378 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.77224(3) 0.19606(3) 0.763943(15) 0.01788(10) Uani 1 1 d . . . N1 N 0.7167(3) 0.2810(2) 0.87827(13) 0.0243(6) Uani 1 1 d . . . N3 N 0.8581(3) 0.2597(2) 0.65928(12) 0.0218(5) Uani 1 1 d . . . N2 N 0.5761(3) 0.2467(2) 0.73625(13) 0.0256(6) Uani 1 1 d . . . C25 C 0.7248(3) -0.1281(3) 0.74339(14) 0.0170(6) Uani 1 1 d . . . N5 N 0.7407(3) 0.0079(2) 0.75190(12) 0.0209(5) Uani 1 1 d . . . C19 C 0.9935(4) 0.1823(3) 0.55702(16) 0.0259(7) Uani 1 1 d . . . C26 C 0.5882(3) -0.2377(3) 0.70113(15) 0.0211(6) Uani 1 1 d . B . N4 N 1.0039(3) 0.3394(2) 0.80399(13) 0.0259(6) Uani 1 1 d . . . C11 C 0.6104(3) 0.1602(3) 0.90253(15) 0.0241(7) Uani 1 1 d . . . H11A H 0.6644 0.0977 0.9065 0.029 Uiso 1 1 calc R . . H11B H 0.5188 0.1112 0.8649 0.029 Uiso 1 1 calc R . . C28 C 0.6921(4) -0.4058(3) 0.72714(16) 0.0273(7) Uani 1 1 d . . . H28 H 0.6808 -0.4974 0.7222 0.033 Uiso 1 1 calc R . . C27 C 0.5758(3) -0.3727(3) 0.69352(15) 0.0235(7) Uani 1 1 d . . . H27 H 0.4871 -0.4432 0.6651 0.028 Uiso 1 1 calc R . . C30 C 0.8442(3) -0.1642(3) 0.77739(15) 0.0216(7) Uani 1 1 d . . . C18 C 0.9231(4) 0.1567(3) 0.62338(15) 0.0257(7) Uani 1 1 d . . . H18A H 1.0024 0.1530 0.6591 0.031 Uiso 1 1 calc R . . H18B H 0.8395 0.0665 0.6100 0.031 Uiso 1 1 calc R . . C17 C 0.4314(4) 0.2367(3) 0.97809(16) 0.0298(7) Uani 1 1 d . . . H17 H 0.3779 0.2433 0.9360 0.036 Uiso 1 1 calc R . . C31 C 0.4589(3) -0.2052(3) 0.66256(15) 0.0255(7) Uani 1 1 d . . . H31 H 0.4736 -0.1098 0.6852 0.031 Uiso 1 1 calc R A 1 C12 C 0.5564(3) 0.1945(3) 0.97364(16) 0.0241(7) Uani 1 1 d . . . C9 C 0.9903(4) 0.3027(3) 0.92605(16) 0.0316(8) Uani 1 1 d . . . H9A H 0.9421 0.2031 0.9091 0.038 Uiso 1 1 calc R . . H9B H 1.0532 0.3240 0.9736 0.038 Uiso 1 1 calc R . . C4 C 0.5689(4) 0.1598(3) 0.60737(16) 0.0300(7) Uani 1 1 d . . . H4A H 0.5816 0.0763 0.6147 0.036 Uiso 1 1 calc R . . H4B H 0.5053 0.1373 0.5599 0.036 Uiso 1 1 calc R . . C20 C 0.9057(4) 0.1144(3) 0.48806(16) 0.0330(8) Uani 1 1 d . . . H20 H 0.8033 0.0533 0.4833 0.040 Uiso 1 1 calc R . . C29 C 0.8252(4) -0.3008(3) 0.76810(15) 0.0254(7) Uani 1 1 d . . . H29 H 0.9042 -0.3230 0.7900 0.031 Uiso 1 1 calc R . . C5 C 0.7288(3) 0.2665(3) 0.60796(16) 0.0253(7) Uani 1 1 d . . . H5A H 0.7528 0.2534 0.5592 0.030 Uiso 1 1 calc R . . H5B H 0.7248 0.3577 0.6215 0.030 Uiso 1 1 calc R . . C34 C 0.9908(3) -0.0529(3) 0.82424(16) 0.0281(7) Uani 1 1 d . . . H34 H 0.9873 0.0365 0.8205 0.034 Uiso 1 1 calc R . . C8 C 1.0959(4) 0.3597(3) 0.87365(16) 0.0323(8) Uani 1 1 d . . . H8A H 1.1552 0.4574 0.8936 0.039 Uiso 1 1 calc R . . H8B H 1.1693 0.3135 0.8676 0.039 Uiso 1 1 calc R . . C13 C 0.6303(4) 0.1820(3) 1.03706(17) 0.0326(8) Uani 1 1 d . . . H13 H 0.7136 0.1523 1.0355 0.039 Uiso 1 1 calc R . . C2 C 0.5084(4) 0.3051(3) 0.79418(17) 0.0309(8) Uani 1 1 d . . . H2A H 0.4210 0.2331 0.8045 0.037 Uiso 1 1 calc R . . H2B H 0.4709 0.3724 0.7796 0.037 Uiso 1 1 calc R . . C3 C 0.4822(4) 0.2069(3) 0.66529(16) 0.0290(7) Uani 1 1 d . . . H3A H 0.4586 0.2843 0.6554 0.035 Uiso 1 1 calc R . . H3B H 0.3842 0.1324 0.6637 0.035 Uiso 1 1 calc R . . C6 C 0.9814(4) 0.3993(3) 0.68860(16) 0.0284(7) Uani 1 1 d . . . H6A H 0.9323 0.4650 0.7031 0.034 Uiso 1 1 calc R . . H6B H 1.0395 0.4263 0.6507 0.034 Uiso 1 1 calc R . . C10 C 0.8628(4) 0.3622(3) 0.93277(16) 0.0312(8) Uani 1 1 d . . . H10A H 0.8374 0.3659 0.9812 0.037 Uiso 1 1 calc R . . H10B H 0.9029 0.4559 0.9269 0.037 Uiso 1 1 calc R . . C1 C 0.6364(4) 0.3742(3) 0.86177(16) 0.0298(7) Uani 1 1 d . . . H1A H 0.7127 0.4573 0.8541 0.036 Uiso 1 1 calc R . . H1B H 0.5903 0.4007 0.9031 0.036 Uiso 1 1 calc R . . C7 C 1.0938(4) 0.4041(3) 0.75346(16) 0.0310(7) Uani 1 1 d . . . H7A H 1.1610 0.3557 0.7375 0.037 Uiso 1 1 calc R . . H7B H 1.1591 0.4990 0.7771 0.037 Uiso 1 1 calc R . . C32 C 0.2952(4) -0.2974(4) 0.6697(2) 0.0549(11) Uani 1 1 d . B 1 H32A H 0.2885 -0.2911 0.7202 0.082 Uiso 1 1 calc R B 1 H32B H 0.2753 -0.3912 0.6456 0.082 Uiso 1 1 calc R B 1 H32C H 0.2190 -0.2678 0.6477 0.082 Uiso 1 1 calc R B 1 C24 C 1.1460(4) 0.2702(4) 0.56184(19) 0.0401(9) Uani 1 1 d . . . H24 H 1.2078 0.3149 0.6074 0.048 Uiso 1 1 calc R . . C16 C 0.3840(4) 0.2694(4) 1.04370(18) 0.0380(8) Uani 1 1 d . . . H16 H 0.3005 0.2989 1.0454 0.046 Uiso 1 1 calc R . . C15 C 0.4605(4) 0.2584(4) 1.10638(18) 0.0402(9) Uani 1 1 d . . . H15 H 0.4300 0.2814 1.1507 0.048 Uiso 1 1 calc R . . C33 C 0.4678(5) -0.2145(4) 0.58405(19) 0.0545(11) Uani 1 1 d . B . H33A H 0.3850 -0.1930 0.5615 0.082 Uiso 1 1 calc R . . H33B H 0.4573 -0.3063 0.5607 0.082 Uiso 1 1 calc R . . H33C H 0.5668 -0.1502 0.5794 0.082 Uiso 1 1 calc R . . C14 C 0.5825(4) 0.2129(4) 1.10275(17) 0.0396(9) Uani 1 1 d . . . H14 H 0.6331 0.2030 1.1447 0.047 Uiso 1 1 calc R . . C23 C 1.2089(5) 0.2931(4) 0.4999(2) 0.0515(10) Uani 1 1 d . . . H23 H 1.3114 0.3536 0.5043 0.062 Uiso 1 1 calc R . . C35 C 1.1388(4) -0.0612(4) 0.7991(2) 0.0642(13) Uani 1 1 d . . . H35A H 1.2283 0.0112 0.8302 0.096 Uiso 1 1 calc R . . H35B H 1.1377 -0.0512 0.7500 0.096 Uiso 1 1 calc R . . H35C H 1.1441 -0.1489 0.8011 0.096 Uiso 1 1 calc R . . C36 C 0.9974(5) -0.0578(4) 0.90355(19) 0.0572(11) Uani 1 1 d . . . H36A H 1.0910 0.0139 0.9319 0.086 Uiso 1 1 calc R . . H36B H 0.9975 -0.1457 0.9085 0.086 Uiso 1 1 calc R . . H36C H 0.9078 -0.0446 0.9204 0.086 Uiso 1 1 calc R . . C22 C 1.1198(5) 0.2263(4) 0.4319(2) 0.0502(10) Uani 1 1 d . . . H22 H 1.1612 0.2416 0.3903 0.060 Uiso 1 1 calc R . . C21 C 0.9688(5) 0.1367(4) 0.42656(18) 0.0429(9) Uani 1 1 d . . . H21 H 0.9083 0.0905 0.3809 0.051 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 0.01723(16) 0.01520(15) 0.01915(16) 0.00220(10) 0.00170(11) 0.00494(11) N1 0.0249(14) 0.0192(13) 0.0275(14) 0.0046(11) 0.0071(11) 0.0064(11) N3 0.0222(14) 0.0206(13) 0.0220(13) 0.0030(10) 0.0042(11) 0.0082(11) N2 0.0242(14) 0.0289(14) 0.0254(14) 0.0078(11) 0.0033(11) 0.0117(12) C25 0.0213(16) 0.0189(15) 0.0121(14) 0.0037(11) 0.0073(12) 0.0078(13) N5 0.0235(14) 0.0228(13) 0.0166(12) 0.0045(10) 0.0023(10) 0.0091(11) C19 0.0275(18) 0.0308(17) 0.0241(17) 0.0046(13) 0.0070(14) 0.0171(15) C26 0.0242(17) 0.0218(15) 0.0174(15) 0.0062(12) 0.0054(13) 0.0076(13) N4 0.0226(14) 0.0271(14) 0.0242(14) 0.0040(11) 0.0007(11) 0.0066(12) C11 0.0261(17) 0.0190(15) 0.0258(17) 0.0052(12) 0.0047(14) 0.0067(13) C28 0.038(2) 0.0209(16) 0.0274(17) 0.0057(13) 0.0091(15) 0.0154(15) C27 0.0261(17) 0.0182(15) 0.0213(16) 0.0033(12) 0.0020(13) 0.0038(13) C30 0.0239(17) 0.0228(16) 0.0186(15) 0.0038(12) 0.0053(13) 0.0095(13) C18 0.0284(18) 0.0247(16) 0.0251(17) 0.0029(13) 0.0035(14) 0.0133(14) C17 0.0279(18) 0.0397(19) 0.0245(17) 0.0116(14) 0.0056(14) 0.0137(15) C31 0.0269(18) 0.0192(15) 0.0252(16) 0.0034(12) -0.0059(14) 0.0060(14) C12 0.0243(17) 0.0186(15) 0.0275(17) 0.0078(13) 0.0066(14) 0.0042(13) C9 0.0289(19) 0.0342(19) 0.0249(17) -0.0010(14) -0.0027(14) 0.0096(15) C4 0.0288(18) 0.0329(18) 0.0258(17) 0.0056(14) -0.0023(14) 0.0112(15) C20 0.036(2) 0.0382(19) 0.0277(18) 0.0013(14) 0.0033(15) 0.0217(16) C29 0.0288(18) 0.0279(17) 0.0260(17) 0.0067(13) 0.0045(14) 0.0183(15) C5 0.0285(18) 0.0278(17) 0.0228(16) 0.0074(13) 0.0027(14) 0.0143(14) C34 0.0255(18) 0.0295(17) 0.0265(17) 0.0016(13) -0.0023(14) 0.0112(14) C8 0.0213(18) 0.0394(19) 0.0297(18) -0.0029(14) -0.0028(14) 0.0111(15) C13 0.0311(19) 0.0393(19) 0.0310(19) 0.0118(15) 0.0026(15) 0.0166(16) C2 0.0277(18) 0.0321(18) 0.039(2) 0.0131(15) 0.0077(15) 0.0159(15) C3 0.0252(18) 0.0270(17) 0.0335(18) 0.0116(14) -0.0016(14) 0.0073(14) C6 0.0280(18) 0.0249(17) 0.0289(17) 0.0055(13) 0.0077(14) 0.0055(14) C10 0.0312(19) 0.0272(17) 0.0244(17) -0.0049(13) 0.0021(14) 0.0043(15) C1 0.040(2) 0.0275(17) 0.0306(18) 0.0102(14) 0.0167(15) 0.0179(16) C7 0.0241(18) 0.0303(18) 0.0303(18) 0.0020(14) 0.0054(14) 0.0028(14) C32 0.037(2) 0.067(3) 0.072(3) 0.032(2) 0.014(2) 0.023(2) C24 0.032(2) 0.053(2) 0.034(2) 0.0014(17) 0.0113(16) 0.0174(18) C16 0.035(2) 0.048(2) 0.039(2) 0.0159(17) 0.0175(17) 0.0196(18) C15 0.045(2) 0.045(2) 0.0292(19) 0.0106(16) 0.0186(17) 0.0117(18) C33 0.053(3) 0.086(3) 0.038(2) 0.024(2) 0.0060(19) 0.038(2) C14 0.048(2) 0.046(2) 0.0236(18) 0.0121(15) 0.0020(16) 0.0159(19) C23 0.040(2) 0.056(3) 0.058(3) 0.012(2) 0.027(2) 0.015(2) C35 0.029(2) 0.076(3) 0.059(3) -0.010(2) 0.005(2) 0.000(2) C36 0.051(3) 0.065(3) 0.032(2) 0.0072(19) -0.0048(19) -0.001(2) C22 0.070(3) 0.064(3) 0.041(2) 0.023(2) 0.036(2) 0.042(2) C21 0.058(3) 0.056(2) 0.0251(19) 0.0063(17) 0.0101(18) 0.036(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 Zr1 N5 1.887(2) . ? Zr1 N2 2.115(2) . ? Zr1 N4 2.119(2) . ? Zr1 N3 2.347(2) . ? Zr1 N1 2.365(2) . ? N1 C1 1.491(4) . ? N1 C10 1.496(4) . ? N1 C11 1.509(4) . ? N3 C6 1.488(4) . ? N3 C5 1.504(3) . ? N3 C18 1.508(3) . ? N2 C3 1.437(4) . ? N2 C2 1.460(4) . ? C25 N5 1.379(3) . ? C25 C26 1.427(4) . ? C25 C30 1.430(4) . ? C19 C24 1.381(5) . ? C19 C20 1.391(4) . ? C19 C18 1.504(4) . ? C26 C27 1.380(4) . ? C26 C31 1.521(4) . ? N4 C8 1.443(4) . ? N4 C7 1.450(4) . ? C11 C12 1.509(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C28 C29 1.381(4) . ? C28 C27 1.383(4) . ? C28 H28 0.9300 . ? C27 H27 0.9300 . ? C30 C29 1.378(4) . ? C30 C34 1.515(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17 C12 1.383(4) . ? C17 C16 1.384(4) . ? C17 H17 0.9300 . ? C31 C33 1.491(4) . ? C31 C32 1.530(5) . ? C31 H31 0.9800 . ? C12 C13 1.384(4) . ? C9 C10 1.525(4) . ? C9 C8 1.525(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C4 C5 1.520(4) . ? C4 C3 1.531(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C20 C21 1.382(5) . ? C20 H20 0.9300 . ? C29 H29 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C34 C36 1.518(4) . ? C34 C35 1.518(5) . ? C34 H34 0.9800 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C13 C14 1.383(4) . ? C13 H13 0.9300 . ? C2 C1 1.532(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 C7 1.520(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C24 C23 1.389(5) . ? C24 H24 0.9300 . ? C16 C15 1.376(5) . ? C16 H16 0.9300 . ? C15 C14 1.377(5) . ? C15 H15 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C14 H14 0.9300 . ? C23 C22 1.380(5) . ? C23 H23 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C22 C21 1.374(5) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Zr1 N2 117.89(10) . . ? N5 Zr1 N4 116.62(10) . . ? N2 Zr1 N4 125.49(9) . . ? N5 Zr1 N3 106.99(9) . . ? N2 Zr1 N3 87.36(9) . . ? N4 Zr1 N3 76.89(9) . . ? N5 Zr1 N1 109.57(9) . . ? N2 Zr1 N1 76.76(9) . . ? N4 Zr1 N1 85.83(9) . . ? N3 Zr1 N1 143.43(8) . . ? C1 N1 C10 109.6(2) . . ? C1 N1 C11 112.2(2) . . ? C10 N1 C11 112.2(2) . . ? C1 N1 Zr1 102.74(17) . . ? C10 N1 Zr1 111.68(17) . . ? C11 N1 Zr1 108.13(16) . . ? C6 N3 C5 110.3(2) . . ? C6 N3 C18 112.2(2) . . ? C5 N3 C18 111.2(2) . . ? C6 N3 Zr1 103.19(17) . . ? C5 N3 Zr1 111.80(17) . . ? C18 N3 Zr1 107.88(17) . . ? C3 N2 C2 113.9(2) . . ? C3 N2 Zr1 125.96(18) . . ? C2 N2 Zr1 119.16(18) . . ? N5 C25 C26 121.3(2) . . ? N5 C25 C30 121.1(2) . . ? C26 C25 C30 117.6(2) . . ? C25 N5 Zr1 177.4(2) . . ? C24 C19 C20 117.9(3) . . ? C24 C19 C18 122.0(3) . . ? C20 C19 C18 120.1(3) . . ? C27 C26 C25 120.0(2) . . ? C27 C26 C31 120.2(3) . . ? C25 C26 C31 119.8(2) . . ? C8 N4 C7 113.8(2) . . ? C8 N4 Zr1 126.3(2) . . ? C7 N4 Zr1 118.55(18) . . ? N1 C11 C12 116.0(2) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C29 C28 C27 119.1(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C26 C27 C28 121.6(3) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C29 C30 C25 119.9(3) . . ? C29 C30 C34 119.8(3) . . ? C25 C30 C34 120.3(2) . . ? C19 C18 N3 116.9(2) . . ? C19 C18 H18A 108.1 . . ? N3 C18 H18A 108.1 . . ? C19 C18 H18B 108.1 . . ? N3 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? C12 C17 C16 121.6(3) . . ? C12 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C33 C31 C26 111.7(3) . . ? C33 C31 C32 109.1(3) . . ? C26 C31 C32 113.1(3) . . ? C33 C31 H31 107.6 . . ? C26 C31 H31 107.6 . . ? C32 C31 H31 107.6 . . ? C17 C12 C13 117.6(3) . . ? C17 C12 C11 122.1(3) . . ? C13 C12 C11 120.3(3) . . ? C10 C9 C8 112.1(3) . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C5 C4 C3 113.9(2) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? N3 C5 C4 113.6(2) . . ? N3 C5 H5A 108.8 . . ? C4 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C4 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C30 C34 C36 111.3(3) . . ? C30 C34 C35 112.5(3) . . ? C36 C34 C35 109.8(3) . . ? C30 C34 H34 107.7 . . ? C36 C34 H34 107.7 . . ? C35 C34 H34 107.7 . . ? N4 C8 C9 110.4(2) . . ? N4 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N4 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? N2 C2 C1 107.7(2) . . ? N2 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N2 C3 C4 110.3(2) . . ? N2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N3 C6 C7 112.1(2) . . ? N3 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N3 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N1 C10 C9 113.5(2) . . ? N1 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N1 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N1 C1 C2 111.8(2) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N4 C7 C6 108.7(2) . . ? N4 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? N4 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C19 C24 C23 121.2(3) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C15 C16 C17 120.0(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C15 C14 119.3(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C21 C22 C23 118.9(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Zr1 N1 C1 -141.01(18) . . . . ? N2 Zr1 N1 C1 -25.78(18) . . . . ? N4 Zr1 N1 C1 102.19(19) . . . . ? N3 Zr1 N1 C1 40.9(2) . . . . ? N5 Zr1 N1 C10 101.59(19) . . . . ? N2 Zr1 N1 C10 -143.2(2) . . . . ? N4 Zr1 N1 C10 -15.21(19) . . . . ? N3 Zr1 N1 C10 -76.5(2) . . . . ? N5 Zr1 N1 C11 -22.28(19) . . . . ? N2 Zr1 N1 C11 92.96(18) . . . . ? N4 Zr1 N1 C11 -139.08(18) . . . . ? N3 Zr1 N1 C11 159.60(16) . . . . ? N5 Zr1 N3 C6 -139.68(17) . . . . ? N2 Zr1 N3 C6 101.93(17) . . . . ? N4 Zr1 N3 C6 -25.48(16) . . . . ? N1 Zr1 N3 C6 38.5(2) . . . . ? N5 Zr1 N3 C5 101.74(18) . . . . ? N2 Zr1 N3 C5 -16.65(17) . . . . ? N4 Zr1 N3 C5 -144.06(19) . . . . ? N1 Zr1 N3 C5 -80.1(2) . . . . ? N5 Zr1 N3 C18 -20.79(19) . . . . ? N2 Zr1 N3 C18 -139.18(18) . . . . ? N4 Zr1 N3 C18 93.41(18) . . . . ? N1 Zr1 N3 C18 157.37(16) . . . . ? N5 Zr1 N2 C3 -61.8(3) . . . . ? N4 Zr1 N2 C3 117.8(2) . . . . ? N3 Zr1 N2 C3 46.0(2) . . . . ? N1 Zr1 N2 C3 -167.2(3) . . . . ? N5 Zr1 N2 C2 106.1(2) . . . . ? N4 Zr1 N2 C2 -74.2(2) . . . . ? N3 Zr1 N2 C2 -146.1(2) . . . . ? N1 Zr1 N2 C2 0.7(2) . . . . ? N5 C25 C26 C27 179.9(3) . . . . ? C30 C25 C26 C27 -0.8(4) . . . . ? N5 C25 C26 C31 1.9(4) . . . . ? C30 C25 C26 C31 -178.8(2) . . . . ? N5 Zr1 N4 C8 -61.9(2) . . . . ? N2 Zr1 N4 C8 118.4(2) . . . . ? N3 Zr1 N4 C8 -164.5(2) . . . . ? N1 Zr1 N4 C8 47.9(2) . . . . ? N5 Zr1 N4 C7 104.1(2) . . . . ? N2 Zr1 N4 C7 -75.6(2) . . . . ? N3 Zr1 N4 C7 1.44(19) . . . . ? N1 Zr1 N4 C7 -146.1(2) . . . . ? C1 N1 C11 C12 -65.1(3) . . . . ? C10 N1 C11 C12 58.7(3) . . . . ? Zr1 N1 C11 C12 -177.69(19) . . . . ? C25 C26 C27 C28 1.2(4) . . . . ? C31 C26 C27 C28 179.2(3) . . . . ? C29 C28 C27 C26 -1.4(4) . . . . ? N5 C25 C30 C29 179.9(3) . . . . ? C26 C25 C30 C29 0.6(4) . . . . ? N5 C25 C30 C34 0.5(4) . . . . ? C26 C25 C30 C34 -178.8(2) . . . . ? C24 C19 C18 N3 83.7(3) . . . . ? C20 C19 C18 N3 -97.7(3) . . . . ? C6 N3 C18 C19 -63.7(3) . . . . ? C5 N3 C18 C19 60.4(3) . . . . ? Zr1 N3 C18 C19 -176.7(2) . . . . ? C27 C26 C31 C33 -78.3(4) . . . . ? C25 C26 C31 C33 99.7(3) . . . . ? C27 C26 C31 C32 45.3(4) . . . . ? C25 C26 C31 C32 -136.7(3) . . . . ? C16 C17 C12 C13 1.9(5) . . . . ? C16 C17 C12 C11 -179.2(3) . . . . ? N1 C11 C12 C17 82.4(4) . . . . ? N1 C11 C12 C13 -98.7(3) . . . . ? C24 C19 C20 C21 -1.2(4) . . . . ? C18 C19 C20 C21 -179.9(3) . . . . ? C25 C30 C29 C28 -0.7(4) . . . . ? C34 C30 C29 C28 178.6(3) . . . . ? C27 C28 C29 C30 1.1(5) . . . . ? C6 N3 C5 C4 -148.5(2) . . . . ? C18 N3 C5 C4 86.3(3) . . . . ? Zr1 N3 C5 C4 -34.3(3) . . . . ? C3 C4 C5 N3 87.1(3) . . . . ? C29 C30 C34 C36 -67.3(4) . . . . ? C25 C30 C34 C36 112.0(3) . . . . ? C29 C30 C34 C35 56.3(4) . . . . ? C25 C30 C34 C35 -124.4(3) . . . . ? C7 N4 C8 C9 173.6(2) . . . . ? Zr1 N4 C8 C9 -19.8(3) . . . . ? C10 C9 C8 N4 -54.2(3) . . . . ? C17 C12 C13 C14 -1.1(5) . . . . ? C11 C12 C13 C14 180.0(3) . . . . ? C3 N2 C2 C1 -166.3(2) . . . . ? Zr1 N2 C2 C1 24.4(3) . . . . ? C2 N2 C3 C4 174.6(2) . . . . ? Zr1 N2 C3 C4 -16.9(4) . . . . ? C5 C4 C3 N2 -56.0(3) . . . . ? C5 N3 C6 C7 166.3(2) . . . . ? C18 N3 C6 C7 -69.1(3) . . . . ? Zr1 N3 C6 C7 46.7(3) . . . . ? C1 N1 C10 C9 -151.0(3) . . . . ? C11 N1 C10 C9 83.7(3) . . . . ? Zr1 N1 C10 C9 -37.8(3) . . . . ? C8 C9 C10 N1 89.1(3) . . . . ? C10 N1 C1 C2 166.7(3) . . . . ? C11 N1 C1 C2 -68.0(3) . . . . ? Zr1 N1 C1 C2 47.8(3) . . . . ? N2 C2 C1 N1 -49.8(3) . . . . ? C8 N4 C7 C6 -169.2(2) . . . . ? Zr1 N4 C7 C6 23.1(3) . . . . ? N3 C6 C7 N4 -48.3(3) . . . . ? C20 C19 C24 C23 1.6(5) . . . . ? C18 C19 C24 C23 -179.7(3) . . . . ? C12 C17 C16 C15 -0.9(5) . . . . ? C17 C16 C15 C14 -0.8(5) . . . . ? C16 C15 C14 C13 1.6(5) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C19 C24 C23 C22 -0.9(5) . . . . ? C24 C23 C22 C21 -0.3(5) . . . . ? C23 C22 C21 C20 0.7(5) . . . . ? C19 C20 C21 C22 0.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.80 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.002 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.072 #===end data_Compound9 _database_code_depnum_ccdc_archive 'CCDC 727737' _vrf_PLAT220_Compound9 ; Problem: Large Non-Solvent C Ueq(max)/Ueq(min)...4.91 Ratio Response: This is due to the large thermal motion of some of the C atoms of the n-Butyl group (C39 and C40) and some C atoms of the co-crystallised toluene (C41 C43 C44), see Fig. 6. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Bn2Cyclam)ZrCl(NPhNPhBu) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H53 Cl N6 Zr, C7 H8' _chemical_formula_sum 'C47 H61 Cl N6 Zr' _chemical_formula_weight 836.69 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.978(6) _cell_length_b 15.349(8) _cell_length_c 26.502(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.019(18) _cell_angle_gamma 90.00 _cell_volume 4383(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2379 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 22.16 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _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 1768 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9331 _exptl_absorpt_correction_T_max 0.9658 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37951 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.59 _reflns_number_total 8176 _reflns_number_gt 5365 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP3 _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8176 _refine_ls_number_parameters 497 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1089 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.004 _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 C1 C 0.7395(3) 1.0723(2) 0.35237(14) 0.0280(8) Uani 1 1 d . . . H1A H 0.7595 1.1110 0.3827 0.034 Uiso 1 1 calc R . . H1B H 0.7494 1.1061 0.3216 0.034 Uiso 1 1 calc R . . C2 C 0.8281(3) 0.9945(2) 0.35907(14) 0.0294(9) Uani 1 1 d . . . H2A H 0.9080 1.0116 0.3498 0.035 Uiso 1 1 calc R . . H2B H 0.8446 0.9753 0.3954 0.035 Uiso 1 1 calc R . . C3 C 0.8667(3) 0.8572(2) 0.31993(15) 0.0304(9) Uani 1 1 d . . . H3A H 0.8258 0.8004 0.3107 0.036 Uiso 1 1 calc R . . H3B H 0.9245 0.8501 0.3533 0.036 Uiso 1 1 calc R . . C4 C 0.9411(3) 0.8831(2) 0.27843(15) 0.0321(9) Uani 1 1 d . . . H4A H 0.9738 0.9428 0.2858 0.038 Uiso 1 1 calc R . . H4B H 1.0131 0.8434 0.2809 0.038 Uiso 1 1 calc R . . C5 C 0.8668(3) 0.8806(2) 0.22331(15) 0.0320(9) Uani 1 1 d . . . H5A H 0.9236 0.8961 0.1999 0.038 Uiso 1 1 calc R . . H5B H 0.8396 0.8198 0.2155 0.038 Uiso 1 1 calc R . . C6 C 0.7913(3) 1.0315(2) 0.21521(15) 0.0276(9) Uani 1 1 d . . . H6A H 0.8406 1.0461 0.1888 0.033 Uiso 1 1 calc R . . H6B H 0.8433 1.0426 0.2494 0.033 Uiso 1 1 calc R . . C7 C 0.6762(3) 1.0885(2) 0.20804(14) 0.0281(9) Uani 1 1 d . . . H7A H 0.6980 1.1464 0.2237 0.034 Uiso 1 1 calc R . . H7B H 0.6434 1.0970 0.1709 0.034 Uiso 1 1 calc R . . C8 C 0.4840(3) 1.1114(2) 0.23725(14) 0.0284(9) Uani 1 1 d . . . H8A H 0.4052 1.0803 0.2376 0.034 Uiso 1 1 calc R . . H8B H 0.4708 1.1506 0.2070 0.034 Uiso 1 1 calc R . . C9 C 0.5181(4) 1.1658(2) 0.28615(14) 0.0325(9) Uani 1 1 d . . . H9A H 0.4580 1.2143 0.2843 0.039 Uiso 1 1 calc R . . H9B H 0.6011 1.1918 0.2871 0.039 Uiso 1 1 calc R . . C10 C 0.5204(3) 1.1160(2) 0.33655(14) 0.0299(9) Uani 1 1 d . . . H10A H 0.5407 1.1577 0.3654 0.036 Uiso 1 1 calc R . . H10B H 0.4360 1.0934 0.3365 0.036 Uiso 1 1 calc R . . C11 C 0.5899(3) 0.9961(2) 0.39546(13) 0.0274(9) Uani 1 1 d . . . H11A H 0.6496 0.9473 0.4026 0.033 Uiso 1 1 calc R . . H11B H 0.5055 0.9705 0.3888 0.033 Uiso 1 1 calc R . . C12 C 0.6035(3) 1.0523(2) 0.44399(14) 0.0289(9) Uani 1 1 d . . . C13 C 0.4997(4) 1.0903(2) 0.45764(15) 0.0357(10) Uani 1 1 d . . . H13 H 0.4204 1.0817 0.4365 0.043 Uiso 1 1 calc R . . C14 C 0.5101(4) 1.1408(2) 0.50200(16) 0.0435(11) Uani 1 1 d . . . H14 H 0.4382 1.1672 0.5103 0.052 Uiso 1 1 calc R . . C15 C 0.6228(4) 1.1528(2) 0.53374(16) 0.0447(11) Uani 1 1 d . . . H15 H 0.6292 1.1871 0.5640 0.054 Uiso 1 1 calc R . . C16 C 0.7275(4) 1.1144(3) 0.52125(16) 0.0481(12) Uani 1 1 d . . . H16 H 0.8061 1.1222 0.5431 0.058 Uiso 1 1 calc R . . C17 C 0.7177(4) 1.0643(2) 0.47661(15) 0.0381(10) Uani 1 1 d . . . H17 H 0.7899 1.0380 0.4684 0.046 Uiso 1 1 calc R . . C18 C 0.6872(3) 0.9169(2) 0.15702(14) 0.0283(9) Uani 1 1 d . . . H18A H 0.6175 0.9584 0.1480 0.034 Uiso 1 1 calc R . . H18B H 0.6508 0.8579 0.1576 0.034 Uiso 1 1 calc R . . C19 C 0.7621(3) 0.9191(2) 0.11443(15) 0.0322(9) Uani 1 1 d . . . C20 C 0.7697(4) 0.9932(3) 0.08524(16) 0.0435(11) Uani 1 1 d . . . H20 H 0.7284 1.0449 0.0923 0.052 Uiso 1 1 calc R . . C21 C 0.8375(4) 0.9926(3) 0.04560(17) 0.0559(13) Uani 1 1 d . . . H21 H 0.8426 1.0438 0.0260 0.067 Uiso 1 1 calc R . . C22 C 0.8969(4) 0.9172(3) 0.03503(18) 0.0601(14) Uani 1 1 d . . . H22 H 0.9434 0.9167 0.0082 0.072 Uiso 1 1 calc R . . C23 C 0.8889(4) 0.8434(3) 0.06318(18) 0.0578(13) Uani 1 1 d . . . H23 H 0.9294 0.7916 0.0557 0.069 Uiso 1 1 calc R . . C24 C 0.8225(4) 0.8437(3) 0.10238(16) 0.0430(11) Uani 1 1 d . . . H24 H 0.8177 0.7920 0.1216 0.052 Uiso 1 1 calc R . . C25 C 0.4245(3) 0.8052(2) 0.32841(13) 0.0220(8) Uani 1 1 d . . . C26 C 0.3080(3) 0.7669(2) 0.32683(14) 0.0274(9) Uani 1 1 d . . . H26 H 0.2357 0.7929 0.3072 0.033 Uiso 1 1 calc R . . C27 C 0.2984(4) 0.6899(2) 0.35432(14) 0.0326(9) Uani 1 1 d . . . H27 H 0.2190 0.6644 0.3532 0.039 Uiso 1 1 calc R . . C28 C 0.4013(4) 0.6503(2) 0.38287(15) 0.0384(10) Uani 1 1 d . . . H28 H 0.3931 0.5981 0.4012 0.046 Uiso 1 1 calc R . . C29 C 0.5168(4) 0.6873(2) 0.38465(15) 0.0359(10) Uani 1 1 d . . . H29 H 0.5884 0.6605 0.4044 0.043 Uiso 1 1 calc R . . C30 C 0.5286(3) 0.7633(2) 0.35768(14) 0.0283(9) Uani 1 1 d . . . H30 H 0.6087 0.7876 0.3590 0.034 Uiso 1 1 calc R . . C31 C 0.2644(3) 0.9756(2) 0.28475(14) 0.0228(8) Uani 1 1 d . . . C32 C 0.1879(3) 1.0310(2) 0.24987(15) 0.0309(9) Uani 1 1 d . . . H32 H 0.1868 1.0260 0.2141 0.037 Uiso 1 1 calc R . . C33 C 0.1145(3) 1.0927(2) 0.26761(16) 0.0317(10) Uani 1 1 d . . . H33 H 0.0648 1.1305 0.2438 0.038 Uiso 1 1 calc R . . C34 C 0.1119(3) 1.1003(2) 0.31993(16) 0.0345(10) Uani 1 1 d . . . H34 H 0.0630 1.1440 0.3319 0.041 Uiso 1 1 calc R . . C35 C 0.1826(3) 1.0427(2) 0.35404(16) 0.0317(9) Uani 1 1 d . . . H35 H 0.1793 1.0455 0.3896 0.038 Uiso 1 1 calc R . . C36 C 0.2586(3) 0.9806(2) 0.33660(14) 0.0271(9) Uani 1 1 d . . . H36 H 0.3064 0.9417 0.3604 0.033 Uiso 1 1 calc R . . C37 C 0.2947(3) 0.8643(2) 0.22001(14) 0.0288(9) Uani 1 1 d . . . H37A H 0.2038 0.8608 0.2177 0.035 Uiso 1 1 calc R . . H37B H 0.3284 0.8045 0.2256 0.035 Uiso 1 1 calc R . . C38 C 0.3203(4) 0.8977(2) 0.16873(14) 0.0397(10) Uani 1 1 d . . . H38A H 0.4110 0.8996 0.1702 0.048 Uiso 1 1 calc R . . H38B H 0.2876 0.9577 0.1628 0.048 Uiso 1 1 calc R . . C39 C 0.2595(5) 0.8390(3) 0.12372(18) 0.0717(16) Uani 1 1 d U . . H39A H 0.2986 0.7807 0.1281 0.086 Uiso 1 1 calc R . . H39B H 0.1705 0.8319 0.1249 0.086 Uiso 1 1 calc R . . C40 C 0.2710(7) 0.8742(4) 0.0726(2) 0.109(2) Uani 1 1 d U . . H40A H 0.2318 0.8339 0.0457 0.163 Uiso 1 1 calc R . . H40B H 0.3589 0.8808 0.0710 0.163 Uiso 1 1 calc R . . H40C H 0.2298 0.9310 0.0674 0.163 Uiso 1 1 calc R . . C41 C 1.0664(6) 0.6316(5) 0.4557(3) 0.129(3) Uani 1 1 d U . . H41A H 1.0169 0.6069 0.4242 0.194 Uiso 1 1 calc R . . H41B H 1.0834 0.5864 0.4822 0.194 Uiso 1 1 calc R . . H41C H 1.1450 0.6538 0.4484 0.194 Uiso 1 1 calc R . . C42 C 0.9956(5) 0.7052(4) 0.4745(2) 0.0711(16) Uani 1 1 d . . . C43 C 1.0361(5) 0.7447(5) 0.5223(2) 0.093(2) Uani 1 1 d U . . H43 H 1.1109 0.7255 0.5436 0.111 Uiso 1 1 calc R . . C44 C 0.9687(6) 0.8115(5) 0.5392(3) 0.095(2) Uani 1 1 d U . . H44 H 0.9972 0.8375 0.5719 0.114 Uiso 1 1 calc R . . C45 C 0.8641(6) 0.8389(3) 0.5095(2) 0.0786(17) Uani 1 1 d . . . H45 H 0.8173 0.8845 0.5209 0.094 Uiso 1 1 calc R . . C46 C 0.8240(5) 0.8008(3) 0.4620(2) 0.0687(15) Uani 1 1 d . . . H46 H 0.7493 0.8209 0.4411 0.082 Uiso 1 1 calc R . . C47 C 0.8882(4) 0.7353(3) 0.44424(19) 0.0527(12) Uani 1 1 d . . . H47 H 0.8589 0.7107 0.4113 0.063 Uiso 1 1 calc R . . N1 N 0.6099(3) 1.04148(16) 0.34653(11) 0.0248(7) Uani 1 1 d . . . N2 N 0.7720(2) 0.92232(16) 0.32567(11) 0.0246(7) Uani 1 1 d . . . N3 N 0.7550(3) 0.93797(16) 0.21083(11) 0.0252(7) Uani 1 1 d . . . N4 N 0.5810(3) 1.04761(16) 0.23228(11) 0.0237(7) Uani 1 1 d . . . N5 N 0.4475(2) 0.88171(16) 0.30276(11) 0.0216(7) Uani 1 1 d . . . N6 N 0.3485(2) 0.91885(16) 0.26558(11) 0.0220(7) Uani 1 1 d . . . Zr01 Zr 0.60497(3) 0.933090(19) 0.274659(14) 0.02173(11) Uani 1 1 d . . . Cl1 Cl 0.60315(8) 0.77862(5) 0.23786(4) 0.0303(2) Uani 1 1 d . . . 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 C1 0.030(2) 0.0242(18) 0.030(2) -0.0025(17) 0.0055(18) -0.0069(17) C2 0.024(2) 0.0312(19) 0.032(2) -0.0056(17) 0.0029(18) -0.0040(16) C3 0.025(2) 0.0268(19) 0.035(2) -0.0007(17) -0.0046(19) -0.0024(16) C4 0.020(2) 0.0295(19) 0.046(3) -0.0002(18) 0.0054(19) 0.0047(16) C5 0.023(2) 0.0306(19) 0.043(3) -0.0045(18) 0.009(2) 0.0031(16) C6 0.025(2) 0.0241(18) 0.035(2) -0.0035(16) 0.0093(18) -0.0070(15) C7 0.030(2) 0.0241(18) 0.031(2) 0.0020(16) 0.0091(18) -0.0026(16) C8 0.027(2) 0.0242(18) 0.034(2) 0.0032(17) 0.0049(18) -0.0009(16) C9 0.034(2) 0.0218(18) 0.042(3) 0.0001(18) 0.010(2) 0.0016(16) C10 0.033(2) 0.0241(18) 0.034(2) -0.0017(17) 0.0097(19) 0.0007(16) C11 0.027(2) 0.0240(18) 0.030(2) 0.0009(16) 0.0032(18) -0.0047(16) C12 0.035(2) 0.0233(19) 0.030(2) 0.0005(16) 0.0094(19) -0.0073(16) C13 0.040(3) 0.032(2) 0.035(3) -0.0018(18) 0.008(2) -0.0045(18) C14 0.056(3) 0.037(2) 0.040(3) -0.001(2) 0.015(2) 0.003(2) C15 0.067(3) 0.038(2) 0.032(3) -0.005(2) 0.016(3) -0.005(2) C16 0.054(3) 0.051(3) 0.035(3) -0.003(2) -0.004(2) -0.015(2) C17 0.040(2) 0.042(2) 0.031(2) -0.002(2) 0.005(2) -0.003(2) C18 0.026(2) 0.0285(19) 0.030(2) -0.0047(16) 0.0045(18) -0.0030(16) C19 0.028(2) 0.039(2) 0.030(2) -0.0120(18) 0.0075(18) -0.0093(18) C20 0.055(3) 0.041(2) 0.037(3) -0.011(2) 0.016(2) -0.012(2) C21 0.070(4) 0.062(3) 0.039(3) -0.007(2) 0.019(3) -0.027(3) C22 0.051(3) 0.093(4) 0.041(3) -0.024(3) 0.023(3) -0.020(3) C23 0.054(3) 0.074(3) 0.047(3) -0.020(3) 0.012(3) 0.006(3) C24 0.042(3) 0.046(2) 0.042(3) -0.011(2) 0.008(2) 0.003(2) C25 0.025(2) 0.0210(17) 0.019(2) -0.0041(15) 0.0005(16) -0.0019(15) C26 0.026(2) 0.0288(19) 0.025(2) -0.0021(17) 0.0009(17) -0.0042(16) C27 0.038(2) 0.035(2) 0.026(2) -0.0072(18) 0.008(2) -0.0160(18) C28 0.055(3) 0.027(2) 0.033(3) 0.0031(18) 0.005(2) -0.0082(19) C29 0.040(3) 0.029(2) 0.035(3) 0.0056(18) 0.000(2) 0.0034(18) C30 0.025(2) 0.0272(19) 0.031(2) -0.0015(17) 0.0026(18) 0.0019(16) C31 0.0162(19) 0.0226(17) 0.029(2) 0.0011(16) 0.0041(17) -0.0035(15) C32 0.026(2) 0.0280(19) 0.039(3) 0.0043(18) 0.0082(19) -0.0013(17) C33 0.022(2) 0.0218(18) 0.052(3) 0.0067(18) 0.008(2) -0.0011(16) C34 0.024(2) 0.0249(19) 0.055(3) -0.0046(19) 0.009(2) -0.0001(16) C35 0.024(2) 0.035(2) 0.037(3) -0.0103(18) 0.0099(19) -0.0088(17) C36 0.025(2) 0.0247(18) 0.031(2) -0.0018(17) 0.0016(18) -0.0002(16) C37 0.024(2) 0.0308(19) 0.030(2) -0.0035(17) 0.0003(18) -0.0003(16) C38 0.043(3) 0.047(2) 0.027(2) 0.0013(19) 0.000(2) 0.009(2) C39 0.113(5) 0.064(3) 0.033(3) -0.006(3) -0.001(3) 0.018(3) C40 0.172(7) 0.103(5) 0.045(4) -0.003(3) 0.004(4) 0.044(5) C41 0.083(5) 0.161(7) 0.151(7) 0.021(6) 0.041(5) 0.044(5) C42 0.042(3) 0.089(4) 0.083(5) 0.023(3) 0.013(3) 0.005(3) C43 0.035(3) 0.164(7) 0.070(5) 0.035(4) -0.014(3) 0.001(4) C44 0.063(4) 0.143(6) 0.073(5) -0.012(4) -0.002(4) -0.022(4) C45 0.085(5) 0.073(4) 0.072(4) -0.006(3) 0.001(4) -0.005(3) C46 0.080(4) 0.059(3) 0.055(4) 0.002(3) -0.018(3) 0.009(3) C47 0.058(3) 0.049(3) 0.047(3) 0.010(2) 0.001(3) -0.004(2) N1 0.0230(17) 0.0200(14) 0.0319(19) 0.0022(13) 0.0064(15) -0.0023(12) N2 0.0177(16) 0.0224(15) 0.0324(18) -0.0039(13) 0.0016(14) -0.0020(12) N3 0.0202(16) 0.0225(14) 0.0324(18) -0.0022(14) 0.0036(14) -0.0008(13) N4 0.0204(16) 0.0247(15) 0.0268(18) 0.0026(13) 0.0059(14) 0.0027(12) N5 0.0191(16) 0.0222(14) 0.0217(17) 0.0013(13) -0.0006(13) 0.0020(12) N6 0.0212(16) 0.0232(15) 0.0210(17) -0.0009(13) 0.0027(13) 0.0023(12) Zr01 0.01900(19) 0.01833(16) 0.0273(2) -0.00082(16) 0.00303(15) -0.00086(15) Cl1 0.0276(5) 0.0224(4) 0.0418(6) -0.0039(4) 0.0089(5) -0.0025(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.479(4) . ? C1 C2 1.529(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.477(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.471(4) . ? C3 C4 1.542(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.531(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.495(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.489(4) . ? C6 C7 1.518(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N4 1.468(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.471(4) . ? C8 C9 1.527(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.535(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N1 1.498(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N1 1.524(4) . ? C11 C12 1.533(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.388(5) . ? C12 C17 1.392(5) . ? C13 C14 1.395(5) . ? C13 H13 0.9500 . ? C14 C15 1.369(6) . ? C14 H14 0.9500 . ? C15 C16 1.387(6) . ? C15 H15 0.9500 . ? C16 C17 1.398(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 N3 1.512(4) . ? C18 C19 1.518(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.387(5) . ? C19 C24 1.400(5) . ? C20 C21 1.399(5) . ? C20 H20 0.9500 . ? C21 C22 1.384(6) . ? C21 H21 0.9500 . ? C22 C23 1.369(6) . ? C22 H22 0.9500 . ? C23 C24 1.379(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.401(4) . ? C25 N5 1.404(4) . ? C25 C30 1.408(5) . ? C26 C27 1.403(5) . ? C26 H26 0.9500 . ? C27 C28 1.375(5) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 H28 0.9500 . ? C29 C30 1.387(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.390(5) . ? C31 C32 1.410(5) . ? C31 N6 1.432(4) . ? C32 C33 1.382(5) . ? C32 H32 0.9500 . ? C33 C34 1.397(5) . ? C33 H33 0.9500 . ? C34 C35 1.391(5) . ? C34 H34 0.9500 . ? C35 C36 1.403(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 N6 1.495(4) . ? C37 C38 1.528(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.541(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.485(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.509(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C47 1.372(6) . ? C42 C43 1.399(8) . ? C43 C44 1.387(8) . ? C43 H43 0.9500 . ? C44 C45 1.331(7) . ? C44 H44 0.9500 . ? C45 C46 1.380(7) . ? C45 H45 0.9500 . ? C46 C47 1.363(6) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? N1 Zr01 2.522(3) . ? N2 Zr01 2.066(3) . ? N3 Zr01 2.578(3) . ? N4 Zr01 2.075(3) . ? N5 N6 1.437(4) . ? N5 Zr01 2.158(3) . ? N6 Zr01 2.788(3) . ? Zr01 Cl1 2.5624(15) . ? 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 C1 C2 109.9(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 109.4(3) . . ? N2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 112.3(3) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 114.5(3) . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? N3 C5 C4 117.5(3) . . ? N3 C5 H5A 107.9 . . ? C4 C5 H5A 107.9 . . ? N3 C5 H5B 107.9 . . ? C4 C5 H5B 107.9 . . ? H5A C5 H5B 107.2 . . ? N3 C6 C7 110.0(3) . . ? N3 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N3 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N4 C7 C6 110.1(3) . . ? N4 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? N4 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 112.1(3) . . ? N4 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N4 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C10 115.3(3) . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N1 C10 C9 115.8(3) . . ? N1 C10 H10A 108.3 . . ? C9 C10 H10A 108.3 . . ? N1 C10 H10B 108.3 . . ? C9 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? N1 C11 C12 116.7(3) . . ? N1 C11 H11A 108.1 . . ? C12 C11 H11A 108.1 . . ? N1 C11 H11B 108.1 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C13 C12 C17 118.0(4) . . ? C13 C12 C11 120.1(3) . . ? C17 C12 C11 121.8(3) . . ? C12 C13 C14 120.9(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.3(4) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 120.8(4) . . ? C12 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? N3 C18 C19 117.2(3) . . ? N3 C18 H18A 108.0 . . ? C19 C18 H18A 108.0 . . ? N3 C18 H18B 108.0 . . ? C19 C18 H18B 108.0 . . ? H18A C18 H18B 107.2 . . ? C20 C19 C24 117.9(4) . . ? C20 C19 C18 122.1(3) . . ? C24 C19 C18 119.9(3) . . ? C19 C20 C21 120.7(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 119.8(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 121.2(4) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C26 C25 N5 125.7(3) . . ? C26 C25 C30 117.7(3) . . ? N5 C25 C30 116.6(3) . . ? C25 C26 C27 119.8(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.5(4) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.2(4) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 121.5(3) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? C36 C31 C32 118.8(3) . . ? C36 C31 N6 122.6(3) . . ? C32 C31 N6 118.6(3) . . ? C33 C32 C31 120.2(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 118.5(3) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C31 C36 C35 120.4(3) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? N6 C37 C38 114.8(3) . . ? N6 C37 H37A 108.6 . . ? C38 C37 H37A 108.6 . . ? N6 C37 H37B 108.6 . . ? C38 C37 H37B 108.6 . . ? H37A C37 H37B 107.5 . . ? C37 C38 C39 111.5(3) . . ? C37 C38 H38A 109.3 . . ? C39 C38 H38A 109.3 . . ? C37 C38 H38B 109.3 . . ? C39 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C38 113.2(5) . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C47 C42 C43 118.1(5) . . ? C47 C42 C41 119.9(6) . . ? C43 C42 C41 121.9(6) . . ? C44 C43 C42 121.1(5) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C45 C44 C43 119.8(6) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.6(6) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C47 C46 C45 122.2(5) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C46 C47 C42 119.3(5) . . ? C46 C47 H47 120.3 . . ? C42 C47 H47 120.3 . . ? C1 N1 C10 111.1(2) . . ? C1 N1 C11 110.4(3) . . ? C10 N1 C11 107.7(3) . . ? C1 N1 Zr01 99.85(19) . . ? C10 N1 Zr01 116.9(2) . . ? C11 N1 Zr01 110.80(18) . . ? C3 N2 C2 110.5(3) . . ? C3 N2 Zr01 122.9(2) . . ? C2 N2 Zr01 123.3(2) . . ? C6 N3 C5 110.8(3) . . ? C6 N3 C18 110.9(3) . . ? C5 N3 C18 108.5(3) . . ? C6 N3 Zr01 99.88(19) . . ? C5 N3 Zr01 116.0(2) . . ? C18 N3 Zr01 110.58(19) . . ? C7 N4 C8 110.0(2) . . ? C7 N4 Zr01 124.9(2) . . ? C8 N4 Zr01 122.3(2) . . ? C25 N5 N6 118.8(3) . . ? C25 N5 Zr01 134.6(2) . . ? N6 N5 Zr01 99.72(18) . . ? C31 N6 N5 116.9(3) . . ? C31 N6 C37 116.4(3) . . ? N5 N6 C37 117.5(2) . . ? C31 N6 Zr01 129.13(19) . . ? N5 N6 Zr01 49.74(14) . . ? C37 N6 Zr01 110.50(19) . . ? N2 Zr01 N4 115.24(11) . . ? N2 Zr01 N5 114.48(11) . . ? N4 Zr01 N5 117.99(11) . . ? N2 Zr01 N1 70.76(10) . . ? N4 Zr01 N1 80.34(11) . . ? N5 Zr01 N1 83.29(10) . . ? N2 Zr01 Cl1 96.68(8) . . ? N4 Zr01 Cl1 125.93(9) . . ? N5 Zr01 Cl1 81.07(7) . . ? N1 Zr01 Cl1 153.56(7) . . ? N2 Zr01 N3 80.40(11) . . ? N4 Zr01 N3 69.57(10) . . ? N5 Zr01 N3 153.07(9) . . ? N1 Zr01 N3 123.53(9) . . ? Cl1 Zr01 N3 74.73(6) . . ? N2 Zr01 N6 143.65(10) . . ? N4 Zr01 N6 89.91(9) . . ? N5 Zr01 N6 30.54(9) . . ? N1 Zr01 N6 89.56(8) . . ? Cl1 Zr01 N6 87.73(6) . . ? N3 Zr01 N6 134.99(9) . . ? 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 C1 C2 N2 38.0(4) . . . . ? N2 C3 C4 C5 -69.1(4) . . . . ? C3 C4 C5 N3 59.8(4) . . . . ? N3 C6 C7 N4 37.7(4) . . . . ? N4 C8 C9 C10 -68.6(4) . . . . ? C8 C9 C10 N1 60.0(4) . . . . ? N1 C11 C12 C13 94.7(4) . . . . ? N1 C11 C12 C17 -87.9(4) . . . . ? C17 C12 C13 C14 1.7(5) . . . . ? C11 C12 C13 C14 179.2(3) . . . . ? C12 C13 C14 C15 -1.3(6) . . . . ? C13 C14 C15 C16 0.3(6) . . . . ? C14 C15 C16 C17 0.2(6) . . . . ? C13 C12 C17 C16 -1.2(5) . . . . ? C11 C12 C17 C16 -178.6(3) . . . . ? C15 C16 C17 C12 0.2(6) . . . . ? N3 C18 C19 C20 -92.7(4) . . . . ? N3 C18 C19 C24 89.6(4) . . . . ? C24 C19 C20 C21 -1.0(6) . . . . ? C18 C19 C20 C21 -178.7(4) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C20 C21 C22 C23 0.3(7) . . . . ? C21 C22 C23 C24 -0.5(7) . . . . ? C22 C23 C24 C19 -0.1(7) . . . . ? C20 C19 C24 C23 0.8(6) . . . . ? C18 C19 C24 C23 178.6(4) . . . . ? N5 C25 C26 C27 179.8(3) . . . . ? C30 C25 C26 C27 0.6(5) . . . . ? C25 C26 C27 C28 -0.3(5) . . . . ? C26 C27 C28 C29 0.1(6) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C28 C29 C30 C25 0.6(6) . . . . ? C26 C25 C30 C29 -0.8(5) . . . . ? N5 C25 C30 C29 180.0(3) . . . . ? C36 C31 C32 C33 3.9(5) . . . . ? N6 C31 C32 C33 -173.6(3) . . . . ? C31 C32 C33 C34 -1.4(5) . . . . ? C32 C33 C34 C35 -1.8(5) . . . . ? C33 C34 C35 C36 2.6(5) . . . . ? C32 C31 C36 C35 -3.2(5) . . . . ? N6 C31 C36 C35 174.3(3) . . . . ? C34 C35 C36 C31 -0.1(5) . . . . ? N6 C37 C38 C39 -178.8(3) . . . . ? C37 C38 C39 C40 174.0(4) . . . . ? C47 C42 C43 C44 1.0(9) . . . . ? C41 C42 C43 C44 -179.1(6) . . . . ? C42 C43 C44 C45 -0.3(10) . . . . ? C43 C44 C45 C46 -0.2(9) . . . . ? C44 C45 C46 C47 0.1(9) . . . . ? C45 C46 C47 C42 0.7(8) . . . . ? C43 C42 C47 C46 -1.2(7) . . . . ? C41 C42 C47 C46 178.9(5) . . . . ? C2 C1 N1 C10 -176.4(3) . . . . ? C2 C1 N1 C11 64.3(3) . . . . ? C2 C1 N1 Zr01 -52.4(3) . . . . ? C9 C10 N1 C1 63.9(4) . . . . ? C9 C10 N1 C11 -175.1(3) . . . . ? C9 C10 N1 Zr01 -49.7(4) . . . . ? C12 C11 N1 C1 64.3(4) . . . . ? C12 C11 N1 C10 -57.1(4) . . . . ? C12 C11 N1 Zr01 174.0(2) . . . . ? C4 C3 N2 C2 -82.3(4) . . . . ? C4 C3 N2 Zr01 77.5(3) . . . . ? C1 C2 N2 C3 163.9(3) . . . . ? C1 C2 N2 Zr01 4.2(4) . . . . ? C7 C6 N3 C5 -174.0(3) . . . . ? C7 C6 N3 C18 65.5(4) . . . . ? C7 C6 N3 Zr01 -51.2(3) . . . . ? C4 C5 N3 C6 65.2(4) . . . . ? C4 C5 N3 C18 -172.9(3) . . . . ? C4 C5 N3 Zr01 -47.8(4) . . . . ? C19 C18 N3 C6 68.8(4) . . . . ? C19 C18 N3 C5 -53.1(4) . . . . ? C19 C18 N3 Zr01 178.6(2) . . . . ? C6 C7 N4 C8 165.4(3) . . . . ? C6 C7 N4 Zr01 4.1(4) . . . . ? C9 C8 N4 C7 -85.3(3) . . . . ? C9 C8 N4 Zr01 76.6(3) . . . . ? C26 C25 N5 N6 -9.7(5) . . . . ? C30 C25 N5 N6 169.5(3) . . . . ? C26 C25 N5 Zr01 -154.1(3) . . . . ? C30 C25 N5 Zr01 25.1(5) . . . . ? C36 C31 N6 N5 -14.2(4) . . . . ? C32 C31 N6 N5 163.2(3) . . . . ? C36 C31 N6 C37 131.9(3) . . . . ? C32 C31 N6 C37 -50.7(4) . . . . ? C36 C31 N6 Zr01 -72.8(4) . . . . ? C32 C31 N6 Zr01 104.7(3) . . . . ? C25 N5 N6 C31 85.0(3) . . . . ? Zr01 N5 N6 C31 -119.9(2) . . . . ? C25 N5 N6 C37 -60.8(4) . . . . ? Zr01 N5 N6 C37 94.4(3) . . . . ? C25 N5 N6 Zr01 -155.2(3) . . . . ? C38 C37 N6 C31 101.8(4) . . . . ? C38 C37 N6 N5 -112.3(3) . . . . ? C38 C37 N6 Zr01 -58.0(3) . . . . ? C3 N2 Zr01 N4 -113.8(2) . . . . ? C2 N2 Zr01 N4 43.4(3) . . . . ? C3 N2 Zr01 N5 104.5(3) . . . . ? C2 N2 Zr01 N5 -98.3(3) . . . . ? C3 N2 Zr01 N1 177.3(3) . . . . ? C2 N2 Zr01 N1 -25.4(2) . . . . ? C3 N2 Zr01 Cl1 21.3(2) . . . . ? C2 N2 Zr01 Cl1 178.5(2) . . . . ? C3 N2 Zr01 N3 -51.9(2) . . . . ? C2 N2 Zr01 N3 105.3(3) . . . . ? C3 N2 Zr01 N6 116.5(3) . . . . ? C2 N2 Zr01 N6 -86.2(3) . . . . ? C7 N4 Zr01 N2 43.2(3) . . . . ? C8 N4 Zr01 N2 -115.9(3) . . . . ? C7 N4 Zr01 N5 -176.5(2) . . . . ? C8 N4 Zr01 N5 24.4(3) . . . . ? C7 N4 Zr01 N1 106.5(3) . . . . ? C8 N4 Zr01 N1 -52.6(2) . . . . ? C7 N4 Zr01 Cl1 -76.8(3) . . . . ? C8 N4 Zr01 Cl1 124.1(2) . . . . ? C7 N4 Zr01 N3 -24.9(2) . . . . ? C8 N4 Zr01 N3 176.0(3) . . . . ? C7 N4 Zr01 N6 -163.9(3) . . . . ? C8 N4 Zr01 N6 36.9(2) . . . . ? C25 N5 Zr01 N2 -45.3(3) . . . . ? N6 N5 Zr01 N2 165.89(16) . . . . ? C25 N5 Zr01 N4 174.1(3) . . . . ? N6 N5 Zr01 N4 25.3(2) . . . . ? C25 N5 Zr01 N1 -110.6(3) . . . . ? N6 N5 Zr01 N1 100.60(17) . . . . ? C25 N5 Zr01 Cl1 48.1(3) . . . . ? N6 N5 Zr01 Cl1 -100.79(17) . . . . ? C25 N5 Zr01 N3 74.2(4) . . . . ? N6 N5 Zr01 N3 -74.7(3) . . . . ? C25 N5 Zr01 N6 148.8(4) . . . . ? C1 N1 Zr01 N2 40.98(19) . . . . ? C10 N1 Zr01 N2 160.8(2) . . . . ? C11 N1 Zr01 N2 -75.4(2) . . . . ? C1 N1 Zr01 N4 -80.2(2) . . . . ? C10 N1 Zr01 N4 39.6(2) . . . . ? C11 N1 Zr01 N4 163.4(2) . . . . ? C1 N1 Zr01 N5 159.9(2) . . . . ? C10 N1 Zr01 N5 -80.3(2) . . . . ? C11 N1 Zr01 N5 43.4(2) . . . . ? C1 N1 Zr01 Cl1 105.8(2) . . . . ? C10 N1 Zr01 Cl1 -134.4(2) . . . . ? C11 N1 Zr01 Cl1 -10.6(3) . . . . ? C1 N1 Zr01 N3 -22.7(2) . . . . ? C10 N1 Zr01 N3 97.1(2) . . . . ? C11 N1 Zr01 N3 -139.1(2) . . . . ? C1 N1 Zr01 N6 -170.17(19) . . . . ? C10 N1 Zr01 N6 -50.4(2) . . . . ? C11 N1 Zr01 N6 73.4(2) . . . . ? C6 N3 Zr01 N2 -82.0(2) . . . . ? C5 N3 Zr01 N2 37.1(2) . . . . ? C18 N3 Zr01 N2 161.2(2) . . . . ? C6 N3 Zr01 N4 39.7(2) . . . . ? C5 N3 Zr01 N4 158.7(2) . . . . ? C18 N3 Zr01 N4 -77.2(2) . . . . ? C6 N3 Zr01 N5 151.5(2) . . . . ? C5 N3 Zr01 N5 -89.4(3) . . . . ? C18 N3 Zr01 N5 34.7(3) . . . . ? C6 N3 Zr01 N1 -22.8(2) . . . . ? C5 N3 Zr01 N1 96.2(2) . . . . ? C18 N3 Zr01 N1 -139.68(19) . . . . ? C6 N3 Zr01 Cl1 178.3(2) . . . . ? C5 N3 Zr01 Cl1 -62.6(2) . . . . ? C18 N3 Zr01 Cl1 61.48(18) . . . . ? C6 N3 Zr01 N6 107.7(2) . . . . ? C5 N3 Zr01 N6 -133.3(2) . . . . ? C18 N3 Zr01 N6 -9.2(2) . . . . ? C31 N6 Zr01 N2 72.3(3) . . . . ? N5 N6 Zr01 N2 -22.0(2) . . . . ? C37 N6 Zr01 N2 -131.2(2) . . . . ? C31 N6 Zr01 N4 -63.5(3) . . . . ? N5 N6 Zr01 N4 -157.83(18) . . . . ? C37 N6 Zr01 N4 92.9(2) . . . . ? C31 N6 Zr01 N5 94.3(3) . . . . ? C37 N6 Zr01 N5 -109.2(3) . . . . ? C31 N6 Zr01 N1 16.8(3) . . . . ? N5 N6 Zr01 N1 -77.48(18) . . . . ? C37 N6 Zr01 N1 173.3(2) . . . . ? C31 N6 Zr01 Cl1 170.5(3) . . . . ? N5 N6 Zr01 Cl1 76.21(17) . . . . ? C37 N6 Zr01 Cl1 -33.02(19) . . . . ? C31 N6 Zr01 N3 -123.9(3) . . . . ? N5 N6 Zr01 N3 141.85(17) . . . . ? C37 N6 Zr01 N3 32.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.385 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.081 #===end