# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Multani, Kanwarpal' 'Stanlake, Louisa' 'Stephan, Douglas W.' _publ_contact_author_name 'Stephan, Douglas W' _publ_contact_author_email dstephan@chem.utoronto.ca _publ_section_title ; Ti and Zr Complexes of Ferrocenyl Amidinates ; # Attachment '- all-cifs.txt' data_[CyNC(Fc)NCy]2ZrCl2 _database_code_depnum_ccdc_archive 'CCDC 778595' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H62 Cl2 Fe2 N4 Zr' _chemical_formula_weight 944.82 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.0872(3) _cell_length_b 18.5813(7) _cell_length_c 21.3216(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.434(2) _cell_angle_gamma 90.00 _cell_volume 4372.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 40303 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.61 _reflns_number_total 10062 _reflns_number_gt 6733 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10062 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C1 C 0.4794(2) 0.17149(16) 0.03374(13) 0.0202(6) Uani 1 1 d . . . C2 C 0.5499(2) 0.29681(16) 0.21507(13) 0.0171(6) Uani 1 1 d . . . C3 C 0.2872(2) 0.19762(18) 0.08293(14) 0.0263(7) Uani 1 1 d . . . H3 H 0.2485 0.1770 0.0438 0.032 Uiso 1 1 calc R . . C4 C 0.2552(3) 0.27714(19) 0.08465(16) 0.0336(8) Uani 1 1 d . . . H4A H 0.2797 0.3004 0.0472 0.040 Uiso 1 1 calc R . . H4B H 0.2999 0.2993 0.1210 0.040 Uiso 1 1 calc R . . C5 C 0.1192(3) 0.2893(2) 0.08817(18) 0.0456(10) Uani 1 1 d . . . H5A H 0.1034 0.3404 0.0924 0.055 Uiso 1 1 calc R . . H5B H 0.0746 0.2726 0.0496 0.055 Uiso 1 1 calc R . . C6 C 0.0770(3) 0.2494(3) 0.14353(17) 0.0592(14) Uani 1 1 d . . . H6A H -0.0099 0.2555 0.1438 0.071 Uiso 1 1 calc R . . H6B H 0.1155 0.2699 0.1822 0.071 Uiso 1 1 calc R . . C7 C 0.1062(3) 0.1702(3) 0.14131(17) 0.0509(12) Uani 1 1 d . . . H7A H 0.0615 0.1487 0.1047 0.061 Uiso 1 1 calc R . . H7B H 0.0808 0.1468 0.1785 0.061 Uiso 1 1 calc R . . C8 C 0.2417(3) 0.1575(2) 0.13813(15) 0.0376(9) Uani 1 1 d . . . H8A H 0.2858 0.1737 0.1770 0.045 Uiso 1 1 calc R . . H8B H 0.2567 0.1064 0.1337 0.045 Uiso 1 1 calc R . . C9 C 0.6860(2) 0.14022(16) 0.00838(13) 0.0193(6) Uani 1 1 d . . . H9 H 0.6481 0.1435 -0.0349 0.023 Uiso 1 1 calc R . . C10 C 0.8006(2) 0.18561(17) 0.01329(14) 0.0239(7) Uani 1 1 d . . . H10A H 0.8368 0.1856 0.0565 0.029 Uiso 1 1 calc R . . H10B H 0.7802 0.2349 0.0016 0.029 Uiso 1 1 calc R . . C11 C 0.8921(3) 0.15630(17) -0.02984(14) 0.0264(7) Uani 1 1 d . . . H11A H 0.8598 0.1621 -0.0734 0.032 Uiso 1 1 calc R . . H11B H 0.9665 0.1839 -0.0235 0.032 Uiso 1 1 calc R . . C12 C 0.9199(3) 0.07759(19) -0.01704(15) 0.0308(8) Uani 1 1 d . . . H12A H 0.9616 0.0725 0.0248 0.037 Uiso 1 1 calc R . . H12B H 0.9735 0.0602 -0.0471 0.037 Uiso 1 1 calc R . . C13 C 0.8051(3) 0.03212(18) -0.02183(14) 0.0294(7) Uani 1 1 d . . . H13A H 0.8253 -0.0173 -0.0105 0.035 Uiso 1 1 calc R . . H13B H 0.7678 0.0326 -0.0649 0.035 Uiso 1 1 calc R . . C14 C 0.7165(3) 0.06192(17) 0.02223(14) 0.0249(7) Uani 1 1 d . . . H14A H 0.6426 0.0337 0.0177 0.030 Uiso 1 1 calc R . . H14B H 0.7516 0.0574 0.0655 0.030 Uiso 1 1 calc R . . C15 C 0.4169(2) 0.15546(16) -0.02948(13) 0.0205(6) Uani 1 1 d . . . C16 C 0.3162(3) 0.19419(18) -0.05942(14) 0.0264(7) Uani 1 1 d . . . H16 H 0.2868 0.2409 -0.0460 0.032 Uiso 1 1 calc R . . C17 C 0.2655(3) 0.15374(17) -0.11164(14) 0.0269(7) Uani 1 1 d . . . H17 H 0.1951 0.1674 -0.1404 0.032 Uiso 1 1 calc R . . C18 C 0.3345(3) 0.09052(18) -0.11514(14) 0.0290(7) Uani 1 1 d . . . H18 H 0.3203 0.0526 -0.1469 0.035 Uiso 1 1 calc R . . C19 C 0.4284(3) 0.09149(17) -0.06572(14) 0.0248(7) Uani 1 1 d . . . H19 H 0.4904 0.0542 -0.0572 0.030 Uiso 1 1 calc R . . C20 C 0.4828(4) 0.2751(2) -0.16007(19) 0.0538(11) Uani 1 1 d . . . H20 H 0.4489 0.3219 -0.1496 0.065 Uiso 1 1 calc R . . C21 C 0.5889(3) 0.2438(3) -0.12988(19) 0.0553(12) Uani 1 1 d . . . H21 H 0.6417 0.2646 -0.0951 0.066 Uiso 1 1 calc R . . C22 C 0.6048(3) 0.1762(3) -0.15937(17) 0.0550(12) Uani 1 1 d . . . H22 H 0.6706 0.1420 -0.1484 0.066 Uiso 1 1 calc R . . C23 C 0.4341(3) 0.2283(2) -0.20758(17) 0.0488(11) Uani 1 1 d . . . H23 H 0.3606 0.2368 -0.2359 0.059 Uiso 1 1 calc R . . C24 C 0.5081(3) 0.1669(3) -0.20722(17) 0.0522(11) Uani 1 1 d . . . H24 H 0.4957 0.1253 -0.2353 0.063 Uiso 1 1 calc R . . C25 C 0.5125(2) 0.21312(16) 0.30276(12) 0.0182(6) Uani 1 1 d . . . H25 H 0.5151 0.2583 0.3265 0.022 Uiso 1 1 calc R . . C26 C 0.6191(2) 0.16657(17) 0.32924(13) 0.0238(7) Uani 1 1 d . . . H26A H 0.6220 0.1232 0.3041 0.029 Uiso 1 1 calc R . . H26B H 0.6941 0.1927 0.3264 0.029 Uiso 1 1 calc R . . C27 C 0.6084(3) 0.14603(19) 0.39772(14) 0.0302(8) Uani 1 1 d . . . H27A H 0.6753 0.1149 0.4125 0.036 Uiso 1 1 calc R . . H27B H 0.6129 0.1891 0.4236 0.036 Uiso 1 1 calc R . . C28 C 0.4890(3) 0.10741(18) 0.40448(15) 0.0313(8) Uani 1 1 d . . . H28A H 0.4870 0.0625 0.3813 0.038 Uiso 1 1 calc R . . H28B H 0.4826 0.0963 0.4485 0.038 Uiso 1 1 calc R . . C29 C 0.3826(3) 0.15404(18) 0.37964(14) 0.0258(7) Uani 1 1 d . . . H29A H 0.3802 0.1969 0.4055 0.031 Uiso 1 1 calc R . . H29B H 0.3078 0.1277 0.3824 0.031 Uiso 1 1 calc R . . C30 C 0.3925(2) 0.17604(17) 0.31121(13) 0.0218(6) Uani 1 1 d . . . H30A H 0.3847 0.1336 0.2847 0.026 Uiso 1 1 calc R . . H30B H 0.3264 0.2083 0.2977 0.026 Uiso 1 1 calc R . . C31 C 0.6315(3) 0.35679(17) 0.12507(13) 0.0237(7) Uani 1 1 d . . . H31 H 0.5949 0.3994 0.1426 0.028 Uiso 1 1 calc R . . C32 C 0.5869(3) 0.35144(18) 0.05518(14) 0.0314(8) Uani 1 1 d . . . H32A H 0.6193 0.3082 0.0376 0.038 Uiso 1 1 calc R . . H32B H 0.4992 0.3480 0.0505 0.038 Uiso 1 1 calc R . . C33 C 0.6263(4) 0.4171(2) 0.01923(17) 0.0506(11) Uani 1 1 d . . . H33A H 0.6007 0.4112 -0.0252 0.061 Uiso 1 1 calc R . . H33B H 0.5869 0.4597 0.0339 0.061 Uiso 1 1 calc R . . C34 C 0.7619(4) 0.4275(2) 0.0278(2) 0.0618(13) Uani 1 1 d . . . H34A H 0.7828 0.4716 0.0071 0.074 Uiso 1 1 calc R . . H34B H 0.8011 0.3879 0.0083 0.074 Uiso 1 1 calc R . . C35 C 0.8081(3) 0.4314(2) 0.0972(2) 0.0551(11) Uani 1 1 d . . . H35A H 0.7773 0.4746 0.1156 0.066 Uiso 1 1 calc R . . H35B H 0.8958 0.4340 0.1014 0.066 Uiso 1 1 calc R . . C36 C 0.7678(3) 0.36570(18) 0.13255(17) 0.0338(8) Uani 1 1 d . . . H36A H 0.8052 0.3230 0.1168 0.041 Uiso 1 1 calc R . . H36B H 0.7951 0.3705 0.1769 0.041 Uiso 1 1 calc R . . C37 C 0.5256(2) 0.36250(16) 0.25078(13) 0.0191(6) Uani 1 1 d . . . C38 C 0.4247(3) 0.37123(17) 0.28795(14) 0.0262(7) Uani 1 1 d . . . H38 H 0.3577 0.3372 0.2902 0.031 Uiso 1 1 calc R . . C39 C 0.4397(3) 0.43688(18) 0.32132(14) 0.0322(8) Uani 1 1 d . . . H39 H 0.3847 0.4560 0.3506 0.039 Uiso 1 1 calc R . . C40 C 0.5460(3) 0.47013(18) 0.30532(14) 0.0328(8) Uani 1 1 d . . . H40 H 0.5777 0.5165 0.3213 0.039 Uiso 1 1 calc R . . C41 C 0.5990(3) 0.42569(17) 0.26136(14) 0.0261(7) Uani 1 1 d . . . H41 H 0.6733 0.4363 0.2416 0.031 Uiso 1 1 calc R . . C42 C 0.2633(3) 0.4576(2) 0.17503(17) 0.0468(10) Uani 1 1 d . . . H42 H 0.1995 0.4211 0.1752 0.056 Uiso 1 1 calc R . . C43 C 0.3584(3) 0.4588(2) 0.13477(15) 0.0390(9) Uani 1 1 d . . . H43 H 0.3720 0.4231 0.1024 0.047 Uiso 1 1 calc R . . C44 C 0.4304(3) 0.5200(2) 0.15008(15) 0.0400(9) Uani 1 1 d . . . H44 H 0.5025 0.5346 0.1300 0.048 Uiso 1 1 calc R . . C45 C 0.3802(4) 0.5565(2) 0.19941(16) 0.0447(10) Uani 1 1 d . . . H45 H 0.4112 0.6012 0.2194 0.054 Uiso 1 1 calc R . . C46 C 0.2775(4) 0.5178(2) 0.21477(17) 0.0481(11) Uani 1 1 d . . . H46 H 0.2248 0.5310 0.2474 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.78876(6) 0.14717(5) 0.18156(4) 0.03009(19) Uani 1 1 d . . . Cl2 Cl 0.50711(7) 0.05558(4) 0.18402(4) 0.03254(19) Uani 1 1 d . . . Fe1 Fe 0.44168(4) 0.17873(3) -0.12197(2) 0.02629(12) Uani 1 1 d . . . Fe2 Fe 0.42774(4) 0.45535(2) 0.22739(2) 0.02512(11) Uani 1 1 d . . . N1 N 0.4196(2) 0.18913(14) 0.08325(11) 0.0229(6) Uani 1 1 d . . . N2 N 0.59833(19) 0.16621(14) 0.05095(11) 0.0205(5) Uani 1 1 d . . . N3 N 0.5243(2) 0.23043(13) 0.23588(10) 0.0193(5) Uani 1 1 d . . . N4 N 0.5962(2) 0.29347(13) 0.15994(11) 0.0211(5) Uani 1 1 d . . . Zr1 Zr 0.57610(2) 0.173846(16) 0.152617(13) 0.01882(8) 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 0.0233(14) 0.0185(15) 0.0198(15) -0.0001(13) 0.0066(12) 0.0023(13) C2 0.0136(13) 0.0221(16) 0.0157(14) 0.0011(12) 0.0014(11) 0.0019(12) C3 0.0156(14) 0.043(2) 0.0206(16) -0.0069(15) 0.0045(12) 0.0001(14) C4 0.0223(16) 0.043(2) 0.0348(19) -0.0121(17) 0.0006(14) 0.0035(15) C5 0.0215(17) 0.059(3) 0.056(3) -0.023(2) -0.0012(16) 0.0094(17) C6 0.0173(16) 0.122(5) 0.039(2) -0.022(3) 0.0053(16) 0.011(2) C7 0.0200(16) 0.099(4) 0.035(2) 0.011(2) 0.0080(15) -0.001(2) C8 0.0219(16) 0.064(3) 0.0271(18) 0.0019(18) 0.0037(13) -0.0011(17) C9 0.0181(14) 0.0240(17) 0.0166(14) 0.0000(13) 0.0054(11) 0.0039(13) C10 0.0223(14) 0.0286(19) 0.0215(16) -0.0034(14) 0.0058(12) 0.0023(13) C11 0.0195(15) 0.035(2) 0.0253(17) -0.0002(14) 0.0053(12) 0.0018(13) C12 0.0233(16) 0.043(2) 0.0263(17) -0.0059(16) 0.0049(13) 0.0086(15) C13 0.0331(17) 0.0291(19) 0.0264(17) -0.0030(15) 0.0050(14) 0.0107(15) C14 0.0222(15) 0.0296(19) 0.0233(16) 0.0009(14) 0.0037(12) 0.0008(14) C15 0.0192(14) 0.0282(18) 0.0148(14) 0.0009(13) 0.0047(11) 0.0005(13) C16 0.0260(16) 0.0312(19) 0.0220(16) 0.0008(14) 0.0027(13) 0.0052(14) C17 0.0211(15) 0.034(2) 0.0244(17) -0.0014(15) -0.0024(12) 0.0011(14) C18 0.0282(16) 0.033(2) 0.0252(17) -0.0035(15) 0.0002(13) -0.0032(15) C19 0.0256(15) 0.0249(18) 0.0238(17) 0.0005(14) 0.0021(13) 0.0006(14) C20 0.057(3) 0.048(3) 0.057(3) 0.028(2) 0.009(2) -0.010(2) C21 0.043(2) 0.075(3) 0.048(2) 0.028(2) 0.0009(19) -0.026(2) C22 0.0287(19) 0.103(4) 0.034(2) 0.027(2) 0.0113(16) 0.003(2) C23 0.041(2) 0.076(3) 0.030(2) 0.026(2) 0.0047(16) 0.000(2) C24 0.045(2) 0.086(3) 0.0272(19) 0.013(2) 0.0131(17) 0.012(2) C25 0.0223(14) 0.0187(16) 0.0140(14) 0.0016(12) 0.0032(11) -0.0003(12) C26 0.0214(14) 0.0274(18) 0.0231(16) 0.0027(14) 0.0053(12) 0.0015(13) C27 0.0314(17) 0.037(2) 0.0230(17) 0.0076(15) 0.0041(13) 0.0053(15) C28 0.0412(19) 0.0263(18) 0.0277(18) 0.0092(15) 0.0100(15) 0.0011(16) C29 0.0249(15) 0.0305(19) 0.0234(16) 0.0010(14) 0.0091(13) -0.0046(14) C30 0.0218(14) 0.0230(16) 0.0207(15) 0.0011(13) 0.0031(12) -0.0004(13) C31 0.0278(16) 0.0223(17) 0.0230(16) 0.0046(13) 0.0126(13) 0.0040(14) C32 0.0409(19) 0.033(2) 0.0217(17) 0.0049(15) 0.0118(14) 0.0121(16) C33 0.084(3) 0.042(2) 0.030(2) 0.0167(18) 0.025(2) 0.019(2) C34 0.086(3) 0.045(3) 0.063(3) 0.018(2) 0.053(3) 0.001(2) C35 0.049(2) 0.041(2) 0.080(3) 0.010(2) 0.034(2) -0.010(2) C36 0.0256(16) 0.031(2) 0.046(2) 0.0059(17) 0.0112(15) -0.0015(15) C37 0.0231(14) 0.0184(16) 0.0159(14) 0.0058(12) 0.0022(11) 0.0030(13) C38 0.0334(17) 0.0233(18) 0.0232(16) 0.0058(14) 0.0103(13) 0.0056(14) C39 0.046(2) 0.031(2) 0.0209(17) 0.0050(15) 0.0113(15) 0.0128(16) C40 0.048(2) 0.0241(19) 0.0247(18) -0.0032(15) -0.0044(15) 0.0030(16) C41 0.0296(16) 0.0242(17) 0.0241(17) 0.0016(14) 0.0004(13) 0.0010(14) C42 0.037(2) 0.055(3) 0.046(2) 0.004(2) -0.0058(17) 0.0175(19) C43 0.051(2) 0.041(2) 0.0234(18) 0.0039(16) -0.0031(16) 0.0222(19) C44 0.058(2) 0.034(2) 0.029(2) 0.0153(17) 0.0108(17) 0.0151(19) C45 0.078(3) 0.025(2) 0.031(2) 0.0055(16) 0.0058(19) 0.020(2) C46 0.055(2) 0.054(3) 0.037(2) 0.010(2) 0.0109(19) 0.034(2) Cl1 0.0212(4) 0.0413(5) 0.0277(4) -0.0026(4) 0.0015(3) 0.0088(3) Cl2 0.0376(4) 0.0240(4) 0.0378(5) -0.0012(4) 0.0130(4) -0.0005(4) Fe1 0.0251(2) 0.0336(3) 0.0203(2) 0.0047(2) 0.00288(18) 0.0002(2) Fe2 0.0315(2) 0.0224(2) 0.0221(2) 0.0035(2) 0.00582(18) 0.0077(2) N1 0.0166(12) 0.0337(16) 0.0189(13) -0.0023(11) 0.0036(10) 0.0008(11) N2 0.0162(11) 0.0283(15) 0.0174(12) -0.0019(11) 0.0037(9) 0.0044(11) N3 0.0218(12) 0.0201(14) 0.0170(12) 0.0018(11) 0.0068(10) 0.0008(11) N4 0.0224(13) 0.0218(14) 0.0200(13) 0.0007(11) 0.0071(10) 0.0007(11) Zr1 0.01786(13) 0.02270(16) 0.01636(14) -0.00157(13) 0.00402(10) 0.00226(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.338(3) . ? C1 N1 1.339(3) . ? C1 C15 1.487(4) . ? C2 N4 1.328(3) . ? C2 N3 1.350(4) . ? C2 C37 1.477(4) . ? C3 N1 1.475(3) . ? C3 C8 1.519(4) . ? C3 C4 1.521(5) . ? C4 C5 1.534(4) . ? C5 C6 1.506(5) . ? C6 C7 1.510(6) . ? C7 C8 1.528(4) . ? C9 N2 1.473(3) . ? C9 C14 1.516(4) . ? C9 C10 1.520(4) . ? C10 C11 1.532(4) . ? C11 C12 1.514(4) . ? C12 C13 1.523(4) . ? C13 C14 1.527(4) . ? C15 C16 1.427(4) . ? C15 C19 1.430(4) . ? C15 Fe1 2.063(3) . ? C16 C17 1.415(4) . ? C16 Fe1 2.037(3) . ? C17 C18 1.407(4) . ? C17 Fe1 2.040(3) . ? C18 C19 1.410(4) . ? C18 Fe1 2.038(3) . ? C19 Fe1 2.030(3) . ? C20 C23 1.404(6) . ? C20 C21 1.412(5) . ? C20 Fe1 2.037(4) . ? C21 C22 1.422(6) . ? C21 Fe1 2.051(4) . ? C22 C24 1.418(5) . ? C22 Fe1 2.045(3) . ? C23 C24 1.406(6) . ? C23 Fe1 2.039(3) . ? C24 Fe1 2.037(3) . ? C25 N3 1.480(3) . ? C25 C30 1.524(4) . ? C25 C26 1.529(4) . ? C26 C27 1.525(4) . ? C27 C28 1.525(4) . ? C28 C29 1.517(4) . ? C29 C30 1.529(4) . ? C31 N4 1.464(4) . ? C31 C36 1.514(4) . ? C31 C32 1.528(4) . ? C32 C33 1.527(5) . ? C33 C34 1.509(5) . ? C34 C35 1.521(6) . ? C35 C36 1.523(5) . ? C37 C41 1.434(4) . ? C37 C38 1.440(4) . ? C37 Fe2 2.074(3) . ? C38 C39 1.414(4) . ? C38 Fe2 2.030(3) . ? C39 C40 1.401(5) . ? C39 Fe2 2.024(3) . ? C40 C41 1.418(4) . ? C40 Fe2 2.035(3) . ? C41 Fe2 2.043(3) . ? C42 C46 1.404(5) . ? C42 C43 1.421(5) . ? C42 Fe2 2.046(3) . ? C43 C44 1.410(5) . ? C43 Fe2 2.051(3) . ? C44 C45 1.409(5) . ? C44 Fe2 2.042(3) . ? C45 C46 1.411(5) . ? C45 Fe2 2.027(3) . ? C46 Fe2 2.027(3) . ? Cl1 Zr1 2.4311(7) . ? Cl2 Zr1 2.4413(9) . ? N1 Zr1 2.189(2) . ? N2 Zr1 2.209(2) . ? N3 Zr1 2.186(2) . ? N4 Zr1 2.238(2) . ? 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 N2 C1 N1 110.5(2) . . ? N2 C1 C15 126.6(2) . . ? N1 C1 C15 122.7(2) . . ? N4 C2 N3 111.0(3) . . ? N4 C2 C37 126.8(3) . . ? N3 C2 C37 122.1(2) . . ? N1 C3 C8 110.3(2) . . ? N1 C3 C4 109.8(2) . . ? C8 C3 C4 111.2(3) . . ? C3 C4 C5 112.2(3) . . ? C6 C5 C4 110.2(3) . . ? C5 C6 C7 111.8(3) . . ? C6 C7 C8 111.5(3) . . ? C3 C8 C7 111.1(3) . . ? N2 C9 C14 110.0(2) . . ? N2 C9 C10 111.8(2) . . ? C14 C9 C10 110.5(2) . . ? C9 C10 C11 111.0(2) . . ? C12 C11 C10 111.7(3) . . ? C11 C12 C13 111.6(2) . . ? C12 C13 C14 109.9(3) . . ? C9 C14 C13 111.9(2) . . ? C16 C15 C19 106.5(2) . . ? C16 C15 C1 125.6(3) . . ? C19 C15 C1 126.8(3) . . ? C16 C15 Fe1 68.66(16) . . ? C19 C15 Fe1 68.33(16) . . ? C1 C15 Fe1 137.1(2) . . ? C17 C16 C15 108.6(3) . . ? C17 C16 Fe1 69.79(17) . . ? C15 C16 Fe1 70.60(16) . . ? C18 C17 C16 107.9(3) . . ? C18 C17 Fe1 69.75(17) . . ? C16 C17 Fe1 69.59(17) . . ? C17 C18 C19 108.4(3) . . ? C17 C18 Fe1 69.87(19) . . ? C19 C18 Fe1 69.43(17) . . ? C18 C19 C15 108.5(3) . . ? C18 C19 Fe1 70.02(18) . . ? C15 C19 Fe1 70.78(17) . . ? C23 C20 C21 108.7(4) . . ? C23 C20 Fe1 70.0(2) . . ? C21 C20 Fe1 70.3(2) . . ? C20 C21 C22 107.2(4) . . ? C20 C21 Fe1 69.2(2) . . ? C22 C21 Fe1 69.4(2) . . ? C24 C22 C21 108.0(4) . . ? C24 C22 Fe1 69.4(2) . . ? C21 C22 Fe1 69.9(2) . . ? C20 C23 C24 108.3(4) . . ? C20 C23 Fe1 69.7(2) . . ? C24 C23 Fe1 69.7(2) . . ? C23 C24 C22 107.8(4) . . ? C23 C24 Fe1 69.9(2) . . ? C22 C24 Fe1 70.0(2) . . ? N3 C25 C30 111.7(2) . . ? N3 C25 C26 110.0(2) . . ? C30 C25 C26 110.7(2) . . ? C27 C26 C25 111.5(2) . . ? C28 C27 C26 110.8(3) . . ? C29 C28 C27 110.6(3) . . ? C28 C29 C30 111.3(2) . . ? C25 C30 C29 112.1(2) . . ? N4 C31 C36 110.3(2) . . ? N4 C31 C32 111.4(3) . . ? C36 C31 C32 109.7(2) . . ? C33 C32 C31 110.9(3) . . ? C34 C33 C32 111.8(3) . . ? C33 C34 C35 111.4(3) . . ? C34 C35 C36 110.8(3) . . ? C31 C36 C35 111.8(3) . . ? C41 C37 C38 106.3(3) . . ? C41 C37 C2 129.0(3) . . ? C38 C37 C2 124.5(3) . . ? C41 C37 Fe2 68.46(17) . . ? C38 C37 Fe2 67.84(16) . . ? C2 C37 Fe2 132.89(19) . . ? C39 C38 C37 108.3(3) . . ? C39 C38 Fe2 69.37(18) . . ? C37 C38 Fe2 71.10(16) . . ? C40 C39 C38 108.6(3) . . ? C40 C39 Fe2 70.24(18) . . ? C38 C39 Fe2 69.81(17) . . ? C39 C40 C41 108.4(3) . . ? C39 C40 Fe2 69.37(18) . . ? C41 C40 Fe2 69.94(17) . . ? C40 C41 C37 108.4(3) . . ? C40 C41 Fe2 69.37(18) . . ? C37 C41 Fe2 70.77(16) . . ? C46 C42 C43 107.7(4) . . ? C46 C42 Fe2 69.1(2) . . ? C43 C42 Fe2 69.9(2) . . ? C44 C43 C42 108.0(3) . . ? C44 C43 Fe2 69.51(19) . . ? C42 C43 Fe2 69.51(19) . . ? C45 C44 C43 107.8(3) . . ? C45 C44 Fe2 69.15(19) . . ? C43 C44 Fe2 70.20(19) . . ? C44 C45 C46 108.2(4) . . ? C44 C45 Fe2 70.3(2) . . ? C46 C45 Fe2 69.6(2) . . ? C42 C46 C45 108.2(3) . . ? C42 C46 Fe2 70.6(2) . . ? C45 C46 Fe2 69.6(2) . . ? C19 Fe1 C20 165.82(15) . . ? C19 Fe1 C24 119.59(16) . . ? C20 Fe1 C24 67.99(18) . . ? C19 Fe1 C16 68.50(12) . . ? C20 Fe1 C16 109.26(16) . . ? C24 Fe1 C16 157.95(14) . . ? C19 Fe1 C18 40.55(11) . . ? C20 Fe1 C18 152.91(14) . . ? C24 Fe1 C18 103.88(16) . . ? C16 Fe1 C18 68.12(13) . . ? C19 Fe1 C23 152.94(16) . . ? C20 Fe1 C23 40.29(16) . . ? C24 Fe1 C23 40.34(16) . . ? C16 Fe1 C23 123.33(14) . . ? C18 Fe1 C23 116.92(15) . . ? C19 Fe1 C17 68.32(12) . . ? C20 Fe1 C17 119.77(15) . . ? C24 Fe1 C17 120.19(14) . . ? C16 Fe1 C17 40.61(12) . . ? C18 Fe1 C17 40.38(12) . . ? C23 Fe1 C17 103.94(14) . . ? C19 Fe1 C22 109.18(15) . . ? C20 Fe1 C22 67.96(18) . . ? C24 Fe1 C22 40.67(14) . . ? C16 Fe1 C22 160.51(15) . . ? C18 Fe1 C22 123.56(17) . . ? C23 Fe1 C22 67.93(15) . . ? C17 Fe1 C22 158.15(16) . . ? C19 Fe1 C21 128.45(14) . . ? C20 Fe1 C21 40.43(15) . . ? C24 Fe1 C21 68.41(18) . . ? C16 Fe1 C21 124.70(17) . . ? C18 Fe1 C21 162.54(16) . . ? C23 Fe1 C21 68.02(15) . . ? C17 Fe1 C21 157.06(17) . . ? C22 Fe1 C21 40.63(17) . . ? C19 Fe1 C15 40.89(11) . . ? C20 Fe1 C15 128.38(15) . . ? C24 Fe1 C15 157.34(15) . . ? C16 Fe1 C15 40.74(11) . . ? C18 Fe1 C15 68.38(12) . . ? C23 Fe1 C15 162.28(15) . . ? C17 Fe1 C15 68.48(11) . . ? C22 Fe1 C15 124.81(13) . . ? C21 Fe1 C15 112.41(14) . . ? C39 Fe2 C45 116.07(14) . . ? C39 Fe2 C46 101.79(14) . . ? C45 Fe2 C46 40.75(15) . . ? C39 Fe2 C38 40.83(13) . . ? C45 Fe2 C38 151.90(13) . . ? C46 Fe2 C38 117.56(14) . . ? C39 Fe2 C40 40.39(13) . . ? C45 Fe2 C40 104.15(15) . . ? C46 Fe2 C40 119.25(15) . . ? C38 Fe2 C40 68.45(13) . . ? C39 Fe2 C44 153.36(15) . . ? C45 Fe2 C44 40.52(13) . . ? C46 Fe2 C44 68.30(15) . . ? C38 Fe2 C44 165.68(14) . . ? C40 Fe2 C44 121.48(15) . . ? C39 Fe2 C41 68.40(13) . . ? C45 Fe2 C41 124.16(15) . . ? C46 Fe2 C41 157.81(15) . . ? C38 Fe2 C41 68.74(12) . . ? C40 Fe2 C41 40.69(12) . . ? C44 Fe2 C41 111.17(14) . . ? C39 Fe2 C42 120.98(15) . . ? C45 Fe2 C42 68.11(17) . . ? C46 Fe2 C42 40.31(15) . . ? C38 Fe2 C42 107.18(15) . . ? C40 Fe2 C42 156.13(14) . . ? C44 Fe2 C42 68.14(16) . . ? C41 Fe2 C42 161.66(14) . . ? C39 Fe2 C43 160.28(15) . . ? C45 Fe2 C43 67.93(15) . . ? C46 Fe2 C43 68.03(14) . . ? C38 Fe2 C43 127.54(14) . . ? C40 Fe2 C43 159.31(15) . . ? C44 Fe2 C43 40.29(14) . . ? C41 Fe2 C43 126.94(13) . . ? C42 Fe2 C43 40.59(14) . . ? C39 Fe2 C37 68.73(12) . . ? C45 Fe2 C37 163.33(14) . . ? C46 Fe2 C37 155.92(15) . . ? C38 Fe2 C37 41.06(11) . . ? C40 Fe2 C37 68.53(12) . . ? C44 Fe2 C37 129.54(13) . . ? C41 Fe2 C37 40.77(11) . . ? C42 Fe2 C37 124.54(14) . . ? C43 Fe2 C37 113.43(13) . . ? C1 N1 C3 126.1(2) . . ? C1 N1 Zr1 94.63(16) . . ? C3 N1 Zr1 137.85(19) . . ? C1 N2 C9 123.1(2) . . ? C1 N2 Zr1 93.77(16) . . ? C9 N2 Zr1 140.10(18) . . ? C2 N3 C25 123.8(2) . . ? C2 N3 Zr1 95.34(16) . . ? C25 N3 Zr1 137.06(19) . . ? C2 N4 C31 123.8(2) . . ? C2 N4 Zr1 93.66(18) . . ? C31 N4 Zr1 142.39(19) . . ? N3 Zr1 N1 103.53(8) . . ? N3 Zr1 N2 152.86(9) . . ? N1 Zr1 N2 60.02(8) . . ? N3 Zr1 N4 59.86(8) . . ? N1 Zr1 N4 89.18(9) . . ? N2 Zr1 N4 96.46(9) . . ? N3 Zr1 Cl1 102.41(6) . . ? N1 Zr1 Cl1 152.32(6) . . ? N2 Zr1 Cl1 92.31(6) . . ? N4 Zr1 Cl1 95.57(6) . . ? N3 Zr1 Cl2 95.56(6) . . ? N1 Zr1 Cl2 93.05(7) . . ? N2 Zr1 Cl2 106.16(7) . . ? N4 Zr1 Cl2 155.05(6) . . ? Cl1 Zr1 Cl2 93.92(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.448 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.085 #===end data_[CyNC(Fc)NCy]2tiCl2 _database_code_depnum_ccdc_archive 'CCDC 778596' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C47 H64 Cl4 Fe2 N4 Ti' _chemical_formula_weight 986.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7232(5) _cell_length_b 22.1321(11) _cell_length_c 19.1676(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.048(2) _cell_angle_gamma 90.00 _cell_volume 4542.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7386 _exptl_absorpt_correction_T_max 0.9788 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75328 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.54 _reflns_number_total 10329 _reflns_number_gt 7262 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+3.4847P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10329 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Ti1 Ti 0.78344(4) 0.23563(2) 0.80890(2) 0.01369(10) Uani 1 1 d . . . Fe1 Fe 0.32519(3) 0.105795(18) 0.804124(19) 0.01880(10) Uani 1 1 d . . . Fe2 Fe 0.61205(3) 0.471916(17) 0.864076(19) 0.01829(9) Uani 1 1 d . . . Cl1 Cl 0.93039(6) 0.21471(3) 0.89791(3) 0.02222(15) Uani 1 1 d . . . Cl2 Cl 0.89752(6) 0.18995(3) 0.72391(3) 0.02170(15) Uani 1 1 d . . . Cl3 Cl 0.58810(10) 0.07490(5) 0.42527(4) 0.0570(3) Uani 1 1 d . . . Cl4 Cl 0.48563(8) 0.11612(4) 0.55522(4) 0.0410(2) Uani 1 1 d . . . N1 N 0.61817(18) 0.23111(10) 0.74731(10) 0.0148(4) Uani 1 1 d . . . N2 N 0.66526(19) 0.16669(10) 0.83074(10) 0.0154(5) Uani 1 1 d . . . N3 N 0.83248(19) 0.32296(10) 0.79087(10) 0.0156(5) Uani 1 1 d . . . N4 N 0.69701(19) 0.30170(9) 0.86866(10) 0.0148(4) Uani 1 1 d . . . C1 C 0.5828(2) 0.18041(12) 0.77768(12) 0.0152(5) Uani 1 1 d . . . C2 C 0.7598(2) 0.34617(12) 0.84058(12) 0.0139(5) Uani 1 1 d . . . C3 C 0.5618(2) 0.25730(12) 0.68246(12) 0.0161(5) Uani 1 1 d . . . H3A H 0.4866 0.2342 0.6684 0.019 Uiso 1 1 calc R . . C4 C 0.6532(2) 0.25337(13) 0.62429(12) 0.0202(6) Uani 1 1 d . . . H4A H 0.7305 0.2735 0.6390 0.024 Uiso 1 1 calc R . . H4B H 0.6719 0.2113 0.6152 0.024 Uiso 1 1 calc R . . C5 C 0.5983(3) 0.28287(14) 0.55759(13) 0.0277(7) Uani 1 1 d . . . H5A H 0.6587 0.2807 0.5218 0.033 Uiso 1 1 calc R . . H5B H 0.5245 0.2607 0.5410 0.033 Uiso 1 1 calc R . . C6 C 0.5637(3) 0.34822(13) 0.56930(14) 0.0283(7) Uani 1 1 d . . . H6A H 0.5265 0.3652 0.5264 0.034 Uiso 1 1 calc R . . H6B H 0.6382 0.3713 0.5824 0.034 Uiso 1 1 calc R . . C7 C 0.4721(3) 0.35236(14) 0.62660(14) 0.0291(7) Uani 1 1 d . . . H7A H 0.3949 0.3324 0.6114 0.035 Uiso 1 1 calc R . . H7B H 0.4534 0.3945 0.6353 0.035 Uiso 1 1 calc R . . C8 C 0.5248(3) 0.32300(13) 0.69449(13) 0.0241(6) Uani 1 1 d . . . H8A H 0.5973 0.3455 0.7123 0.029 Uiso 1 1 calc R . . H8B H 0.4624 0.3246 0.7293 0.029 Uiso 1 1 calc R . . C9 C 0.6692(2) 0.10859(12) 0.86793(12) 0.0163(5) Uani 1 1 d . . . H9A H 0.5894 0.0878 0.8583 0.020 Uiso 1 1 calc R . . C10 C 0.7738(2) 0.06924(12) 0.84090(13) 0.0206(6) Uani 1 1 d . . . H10A H 0.7576 0.0619 0.7914 0.025 Uiso 1 1 calc R . . H10B H 0.8525 0.0907 0.8469 0.025 Uiso 1 1 calc R . . C11 C 0.6887(3) 0.11712(12) 0.94709(12) 0.0205(6) Uani 1 1 d . . . H11A H 0.7640 0.1405 0.9571 0.025 Uiso 1 1 calc R . . H11B H 0.6189 0.1396 0.9642 0.025 Uiso 1 1 calc R . . C12 C 0.6997(3) 0.05681(13) 0.98483(13) 0.0249(6) Uani 1 1 d . . . H12A H 0.6211 0.0353 0.9787 0.030 Uiso 1 1 calc R . . H12B H 0.7159 0.0639 1.0344 0.030 Uiso 1 1 calc R . . C13 C 0.8040(3) 0.01782(13) 0.95773(14) 0.0290(7) Uani 1 1 d . . . H13A H 0.8840 0.0372 0.9682 0.035 Uiso 1 1 calc R . . H13B H 0.8049 -0.0211 0.9810 0.035 Uiso 1 1 calc R . . C14 C 0.7846(3) 0.00882(13) 0.87914(14) 0.0272(7) Uani 1 1 d . . . H14A H 0.7092 -0.0145 0.8692 0.033 Uiso 1 1 calc R . . H14B H 0.8543 -0.0138 0.8622 0.033 Uiso 1 1 calc R . . C15 C 0.4691(2) 0.14634(12) 0.75389(13) 0.0186(6) Uani 1 1 d . . . C16 C 0.3507(2) 0.17357(14) 0.73437(15) 0.0271(7) Uani 1 1 d . . . H16A H 0.3287 0.2161 0.7406 0.032 Uiso 1 1 calc R . . C17 C 0.2718(3) 0.12840(15) 0.70386(14) 0.0316(8) Uani 1 1 d . . . H17A H 0.1857 0.1344 0.6855 0.038 Uiso 1 1 calc R . . C18 C 0.3382(3) 0.07306(15) 0.70457(14) 0.0293(7) Uani 1 1 d . . . H18A H 0.3059 0.0342 0.6871 0.035 Uiso 1 1 calc R . . C19 C 0.4590(2) 0.08358(13) 0.73628(13) 0.0225(6) Uani 1 1 d . . . H19A H 0.5245 0.0531 0.7444 0.027 Uiso 1 1 calc R . . C20 C 0.1584(3) 0.09363(15) 0.84952(16) 0.0321(7) Uani 1 1 d . . . H20A H 0.0754 0.0972 0.8259 0.039 Uiso 1 1 calc R . . C21 C 0.2302(3) 0.04103(14) 0.85495(15) 0.0296(7) Uani 1 1 d . . . H21A H 0.2059 0.0013 0.8362 0.036 Uiso 1 1 calc R . . C22 C 0.3438(3) 0.05493(14) 0.89315(14) 0.0267(7) Uani 1 1 d . . . H22A H 0.4118 0.0266 0.9054 0.032 Uiso 1 1 calc R . . C23 C 0.3406(3) 0.11691(14) 0.91094(14) 0.0265(7) Uani 1 1 d . . . H23A H 0.4064 0.1393 0.9372 0.032 Uiso 1 1 calc R . . C24 C 0.2264(3) 0.14086(15) 0.88340(16) 0.0324(7) Uani 1 1 d . . . H24A H 0.1988 0.1829 0.8874 0.039 Uiso 1 1 calc R . . C25 C 0.9367(2) 0.35583(12) 0.76125(13) 0.0174(6) Uani 1 1 d . . . H25A H 0.9423 0.3958 0.7833 0.021 Uiso 1 1 calc R . . C26 C 0.9140(3) 0.36495(13) 0.68263(13) 0.0233(6) Uani 1 1 d . . . H26A H 0.8354 0.3859 0.6735 0.028 Uiso 1 1 calc R . . H26B H 0.9082 0.3259 0.6597 0.028 Uiso 1 1 calc R . . C27 C 1.0198(3) 0.40160(15) 0.65284(16) 0.0342(8) Uani 1 1 d . . . H27A H 1.0049 0.4057 0.6027 0.041 Uiso 1 1 calc R . . H27B H 1.0213 0.4418 0.6731 0.041 Uiso 1 1 calc R . . C28 C 1.1438(3) 0.37134(15) 0.66827(17) 0.0382(8) Uani 1 1 d . . . H28A H 1.2098 0.3967 0.6517 0.046 Uiso 1 1 calc R . . H28B H 1.1456 0.3332 0.6434 0.046 Uiso 1 1 calc R . . C29 C 1.1673(3) 0.35998(14) 0.74581(17) 0.0335(8) Uani 1 1 d . . . H29A H 1.1752 0.3984 0.7700 0.040 Uiso 1 1 calc R . . H29B H 1.2453 0.3382 0.7536 0.040 Uiso 1 1 calc R . . C30 C 1.0616(2) 0.32345(13) 0.77608(15) 0.0259(6) Uani 1 1 d . . . H30A H 1.0773 0.3188 0.8261 0.031 Uiso 1 1 calc R . . H30B H 1.0583 0.2835 0.7552 0.031 Uiso 1 1 calc R . . C31 C 0.6080(2) 0.30900(12) 0.92318(12) 0.0168(5) Uani 1 1 d . . . H31A H 0.5886 0.3521 0.9270 0.020 Uiso 1 1 calc R . . C32 C 0.4866(2) 0.27537(13) 0.90511(14) 0.0220(6) Uani 1 1 d . . . H32A H 0.5037 0.2326 0.9000 0.026 Uiso 1 1 calc R . . H32B H 0.4499 0.2901 0.8610 0.026 Uiso 1 1 calc R . . C33 C 0.3947(3) 0.28467(14) 0.96266(15) 0.0322(7) Uani 1 1 d . . . H33A H 0.3731 0.3271 0.9653 0.039 Uiso 1 1 calc R . . H33B H 0.3188 0.2622 0.9512 0.039 Uiso 1 1 calc R . . C34 C 0.4505(3) 0.26385(15) 1.03322(15) 0.0376(8) Uani 1 1 d . . . H34A H 0.3924 0.2724 1.0690 0.045 Uiso 1 1 calc R . . H34B H 0.4639 0.2205 1.0322 0.045 Uiso 1 1 calc R . . C35 C 0.5737(3) 0.29543(14) 1.05122(14) 0.0296(7) Uani 1 1 d . . . H35A H 0.6100 0.2792 1.0947 0.036 Uiso 1 1 calc R . . H35B H 0.5584 0.3382 1.0581 0.036 Uiso 1 1 calc R . . C36 C 0.6657(3) 0.28763(13) 0.99410(13) 0.0225(6) Uani 1 1 d . . . H36A H 0.6890 0.2454 0.9909 0.027 Uiso 1 1 calc R . . H36B H 0.7407 0.3108 1.0059 0.027 Uiso 1 1 calc R . . C37 C 0.7570(2) 0.41067(12) 0.85971(12) 0.0157(5) Uani 1 1 d . . . C38 C 0.7502(2) 0.43559(12) 0.92912(13) 0.0201(6) Uani 1 1 d . . . H38A H 0.7374 0.4124 0.9717 0.024 Uiso 1 1 calc R . . C39 C 0.7645(2) 0.49859(13) 0.92521(14) 0.0238(6) Uani 1 1 d . . . H39A H 0.7635 0.5267 0.9646 0.029 Uiso 1 1 calc R . . C40 C 0.7784(3) 0.51475(13) 0.85439(15) 0.0248(6) Uani 1 1 d . . . H40A H 0.7897 0.5558 0.8365 0.030 Uiso 1 1 calc R . . C41 C 0.7727(2) 0.46105(12) 0.81401(14) 0.0204(6) Uani 1 1 d . . . H41A H 0.7792 0.4587 0.7633 0.024 Uiso 1 1 calc R . . C42 C 0.4425(3) 0.43400(15) 0.83676(17) 0.0339(7) Uani 1 1 d . . . H42A H 0.4273 0.3912 0.8265 0.041 Uiso 1 1 calc R . . C43 C 0.4733(3) 0.47840(16) 0.78810(16) 0.0376(8) Uani 1 1 d . . . H43A H 0.4818 0.4722 0.7379 0.045 Uiso 1 1 calc R . . C44 C 0.4880(3) 0.53340(15) 0.82427(19) 0.0403(9) Uani 1 1 d . . . H44A H 0.5084 0.5725 0.8038 0.048 Uiso 1 1 calc R . . C45 C 0.4652(3) 0.52244(15) 0.89517(17) 0.0345(8) Uani 1 1 d . . . H45A H 0.4684 0.5525 0.9327 0.041 Uiso 1 1 calc R . . C46 C 0.4374(3) 0.46121(15) 0.90215(17) 0.0338(8) Uani 1 1 d . . . H46A H 0.4188 0.4407 0.9457 0.041 Uiso 1 1 calc R . . C47 C 0.5417(3) 0.13710(16) 0.47400(17) 0.0429(9) Uani 1 1 d . . . H47A H 0.4767 0.1589 0.4474 0.051 Uiso 1 1 calc R . . H47B H 0.6122 0.1642 0.4818 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 Ti1 0.0129(2) 0.0152(2) 0.0131(2) 0.00025(18) 0.00163(17) -0.00001(19) Fe1 0.01516(19) 0.0212(2) 0.02033(19) 0.00240(16) 0.00336(15) -0.00249(16) Fe2 0.0187(2) 0.0167(2) 0.01961(19) -0.00073(16) 0.00205(15) 0.00158(16) Cl1 0.0209(3) 0.0250(4) 0.0201(3) 0.0024(3) -0.0053(3) 0.0018(3) Cl2 0.0214(3) 0.0243(4) 0.0200(3) -0.0024(3) 0.0063(3) 0.0034(3) Cl3 0.0668(6) 0.0717(7) 0.0321(4) 0.0001(4) -0.0020(4) 0.0313(5) Cl4 0.0451(5) 0.0473(5) 0.0304(4) 0.0005(4) -0.0008(3) 0.0021(4) N1 0.0154(11) 0.0175(12) 0.0116(10) 0.0031(9) 0.0009(8) -0.0011(9) N2 0.0174(11) 0.0158(12) 0.0130(10) 0.0006(9) 0.0016(8) -0.0006(9) N3 0.0160(11) 0.0160(12) 0.0151(10) 0.0008(9) 0.0039(8) -0.0012(9) N4 0.0152(11) 0.0167(12) 0.0128(10) 0.0007(9) 0.0049(8) 0.0008(9) C1 0.0152(13) 0.0168(14) 0.0141(12) -0.0035(10) 0.0051(10) 0.0017(10) C2 0.0106(12) 0.0180(14) 0.0129(11) 0.0011(10) -0.0016(9) 0.0022(10) C3 0.0129(12) 0.0217(15) 0.0136(12) 0.0033(10) -0.0001(10) -0.0023(11) C4 0.0226(14) 0.0248(16) 0.0133(12) 0.0001(11) 0.0025(10) 0.0029(12) C5 0.0315(16) 0.0385(19) 0.0133(13) 0.0048(12) 0.0024(12) 0.0052(14) C6 0.0375(17) 0.0252(17) 0.0212(14) 0.0107(12) -0.0076(12) -0.0023(14) C7 0.0339(17) 0.0263(17) 0.0265(15) 0.0004(13) -0.0043(13) 0.0087(14) C8 0.0263(15) 0.0271(17) 0.0186(13) 0.0008(12) 0.0000(11) 0.0091(13) C9 0.0179(13) 0.0172(14) 0.0139(12) 0.0036(10) 0.0020(10) -0.0014(11) C10 0.0248(15) 0.0199(15) 0.0177(13) 0.0007(11) 0.0061(11) 0.0021(12) C11 0.0259(15) 0.0205(15) 0.0153(12) 0.0016(11) 0.0036(11) 0.0030(12) C12 0.0365(17) 0.0236(16) 0.0149(13) 0.0070(11) 0.0037(12) 0.0042(13) C13 0.0390(18) 0.0229(17) 0.0253(15) 0.0089(12) 0.0032(13) 0.0089(14) C14 0.0384(18) 0.0163(15) 0.0272(15) 0.0000(12) 0.0059(13) 0.0043(13) C15 0.0175(13) 0.0230(16) 0.0154(12) 0.0039(11) 0.0029(10) -0.0032(11) C16 0.0188(14) 0.0301(17) 0.0318(15) 0.0159(13) -0.0024(12) -0.0055(13) C17 0.0203(15) 0.049(2) 0.0247(15) 0.0168(14) -0.0074(12) -0.0143(15) C18 0.0287(16) 0.041(2) 0.0186(14) -0.0031(13) 0.0014(12) -0.0183(15) C19 0.0205(14) 0.0282(17) 0.0193(13) -0.0023(12) 0.0065(11) -0.0066(12) C20 0.0170(14) 0.046(2) 0.0348(17) -0.0016(15) 0.0101(12) -0.0057(14) C21 0.0348(17) 0.0290(18) 0.0257(15) 0.0036(13) 0.0075(13) -0.0156(14) C22 0.0278(16) 0.0303(18) 0.0229(14) 0.0091(13) 0.0083(12) -0.0018(13) C23 0.0224(15) 0.0369(19) 0.0211(14) -0.0040(13) 0.0085(11) -0.0080(13) C24 0.0273(16) 0.0340(19) 0.0371(17) -0.0075(14) 0.0141(13) 0.0035(14) C25 0.0152(13) 0.0158(14) 0.0219(13) -0.0020(11) 0.0072(10) -0.0040(11) C26 0.0224(14) 0.0262(17) 0.0221(14) 0.0025(12) 0.0077(11) -0.0047(12) C27 0.0383(18) 0.036(2) 0.0294(16) 0.0076(14) 0.0184(14) -0.0091(15) C28 0.0331(18) 0.0350(19) 0.049(2) -0.0052(16) 0.0272(15) -0.0108(15) C29 0.0145(14) 0.0305(18) 0.056(2) -0.0057(15) 0.0096(14) -0.0035(13) C30 0.0172(14) 0.0249(17) 0.0359(16) 0.0017(13) 0.0044(12) -0.0005(12) C31 0.0170(13) 0.0187(15) 0.0155(12) -0.0006(11) 0.0075(10) 0.0000(11) C32 0.0219(14) 0.0235(16) 0.0216(14) -0.0006(12) 0.0098(11) -0.0038(12) C33 0.0271(16) 0.0324(18) 0.0392(17) -0.0081(14) 0.0215(14) -0.0086(14) C34 0.053(2) 0.0344(19) 0.0276(16) -0.0073(14) 0.0265(15) -0.0138(16) C35 0.051(2) 0.0223(17) 0.0166(13) -0.0005(12) 0.0106(13) -0.0028(14) C36 0.0318(16) 0.0191(15) 0.0170(13) 0.0015(11) 0.0045(11) -0.0018(12) C37 0.0111(12) 0.0189(14) 0.0171(12) -0.0011(11) 0.0016(10) -0.0003(10) C38 0.0170(13) 0.0236(16) 0.0199(13) -0.0010(11) 0.0010(10) -0.0013(11) C39 0.0221(15) 0.0233(16) 0.0259(15) -0.0075(12) 0.0008(11) -0.0046(12) C40 0.0244(15) 0.0181(16) 0.0322(16) -0.0009(12) 0.0052(12) -0.0047(12) C41 0.0179(13) 0.0220(16) 0.0218(13) 0.0018(11) 0.0057(11) -0.0012(12) C42 0.0196(15) 0.0273(18) 0.054(2) -0.0088(15) -0.0082(14) 0.0021(13) C43 0.0246(16) 0.057(2) 0.0298(17) 0.0003(16) -0.0068(13) 0.0143(16) C44 0.0254(17) 0.0284(19) 0.067(2) 0.0193(17) 0.0015(16) 0.0082(14) C45 0.0253(16) 0.0311(19) 0.0472(19) -0.0144(15) 0.0024(14) 0.0123(14) C46 0.0197(15) 0.043(2) 0.0396(18) 0.0039(15) 0.0065(13) 0.0067(14) C47 0.050(2) 0.042(2) 0.0365(18) 0.0049(16) 0.0042(16) 0.0019(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N3 2.037(2) . ? Ti1 N2 2.041(2) . ? Ti1 N1 2.079(2) . ? Ti1 N4 2.103(2) . ? Ti1 Cl1 2.3069(8) . ? Ti1 Cl2 2.3204(7) . ? Fe1 C21 2.036(3) . ? Fe1 C16 2.038(3) . ? Fe1 C17 2.038(3) . ? Fe1 C22 2.045(3) . ? Fe1 C19 2.047(3) . ? Fe1 C20 2.048(3) . ? Fe1 C24 2.050(3) . ? Fe1 C18 2.053(3) . ? Fe1 C23 2.060(3) . ? Fe1 C15 2.067(2) . ? Fe2 C44 2.023(3) . ? Fe2 C41 2.030(3) . ? Fe2 C43 2.031(3) . ? Fe2 C40 2.037(3) . ? Fe2 C42 2.045(3) . ? Fe2 C45 2.046(3) . ? Fe2 C39 2.047(3) . ? Fe2 C38 2.049(3) . ? Fe2 C46 2.060(3) . ? Fe2 C37 2.067(3) . ? Cl3 C47 1.750(3) . ? Cl4 C47 1.761(3) . ? N1 C1 1.329(3) . ? N1 C3 1.472(3) . ? N2 C1 1.347(3) . ? N2 C9 1.470(3) . ? N3 C2 1.363(3) . ? N3 C25 1.473(3) . ? N4 C2 1.323(3) . ? N4 C31 1.461(3) . ? C1 C15 1.484(4) . ? C2 C37 1.474(4) . ? C3 C4 1.526(3) . ? C3 C8 1.528(4) . ? C4 C5 1.526(3) . ? C5 C6 1.513(4) . ? C6 C7 1.514(4) . ? C7 C8 1.535(4) . ? C9 C10 1.532(3) . ? C9 C11 1.532(3) . ? C10 C14 1.526(4) . ? C11 C12 1.520(4) . ? C12 C13 1.526(4) . ? C13 C14 1.523(4) . ? C15 C19 1.432(4) . ? C15 C16 1.437(4) . ? C16 C17 1.416(4) . ? C17 C18 1.416(4) . ? C18 C19 1.421(4) . ? C20 C21 1.397(4) . ? C20 C24 1.413(4) . ? C21 C22 1.422(4) . ? C22 C23 1.414(4) . ? C23 C24 1.411(4) . ? C25 C26 1.527(3) . ? C25 C30 1.532(4) . ? C26 C27 1.530(4) . ? C27 C28 1.504(4) . ? C28 C29 1.515(4) . ? C29 C30 1.531(4) . ? C31 C32 1.524(4) . ? C31 C36 1.538(3) . ? C32 C33 1.531(3) . ? C33 C34 1.521(4) . ? C34 C35 1.517(4) . ? C35 C36 1.522(4) . ? C37 C41 1.433(4) . ? C37 C38 1.446(3) . ? C38 C39 1.405(4) . ? C39 C40 1.419(4) . ? C40 C41 1.418(4) . ? C42 C46 1.394(4) . ? C42 C43 1.406(5) . ? C43 C44 1.406(5) . ? C44 C45 1.414(5) . ? C45 C46 1.396(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ti1 N2 155.87(9) . . ? N3 Ti1 N1 99.74(8) . . ? N2 Ti1 N1 63.94(8) . . ? N3 Ti1 N4 63.76(8) . . ? N2 Ti1 N4 96.41(8) . . ? N1 Ti1 N4 87.46(8) . . ? N3 Ti1 Cl1 98.25(6) . . ? N2 Ti1 Cl1 96.05(6) . . ? N1 Ti1 Cl1 159.79(6) . . ? N4 Ti1 Cl1 92.31(6) . . ? N3 Ti1 Cl2 98.27(6) . . ? N2 Ti1 Cl2 100.05(6) . . ? N1 Ti1 Cl2 92.62(6) . . ? N4 Ti1 Cl2 161.70(6) . . ? Cl1 Ti1 Cl2 93.84(3) . . ? C21 Fe1 C16 156.96(12) . . ? C21 Fe1 C17 120.09(12) . . ? C16 Fe1 C17 40.65(11) . . ? C21 Fe1 C22 40.77(11) . . ? C16 Fe1 C22 160.41(12) . . ? C17 Fe1 C22 158.74(12) . . ? C21 Fe1 C19 121.34(12) . . ? C16 Fe1 C19 68.71(12) . . ? C17 Fe1 C19 68.35(12) . . ? C22 Fe1 C19 110.92(12) . . ? C21 Fe1 C20 39.99(12) . . ? C16 Fe1 C20 121.76(12) . . ? C17 Fe1 C20 103.02(12) . . ? C22 Fe1 C20 67.79(12) . . ? C19 Fe1 C20 153.62(12) . . ? C21 Fe1 C24 67.71(12) . . ? C16 Fe1 C24 107.47(13) . . ? C17 Fe1 C24 118.40(13) . . ? C22 Fe1 C24 67.76(12) . . ? C19 Fe1 C24 165.67(12) . . ? C20 Fe1 C24 40.33(12) . . ? C21 Fe1 C18 104.87(12) . . ? C16 Fe1 C18 68.39(13) . . ? C17 Fe1 C18 40.50(13) . . ? C22 Fe1 C18 124.95(13) . . ? C19 Fe1 C18 40.55(11) . . ? C20 Fe1 C18 116.91(12) . . ? C24 Fe1 C18 152.34(12) . . ? C21 Fe1 C23 67.93(12) . . ? C16 Fe1 C23 123.90(12) . . ? C17 Fe1 C23 155.71(13) . . ? C22 Fe1 C23 40.30(11) . . ? C19 Fe1 C23 129.66(11) . . ? C20 Fe1 C23 67.60(11) . . ? C24 Fe1 C23 40.14(12) . . ? C18 Fe1 C23 163.79(13) . . ? C21 Fe1 C15 158.95(12) . . ? C16 Fe1 C15 40.98(10) . . ? C17 Fe1 C15 68.49(10) . . ? C22 Fe1 C15 125.82(11) . . ? C19 Fe1 C15 40.74(11) . . ? C20 Fe1 C15 161.02(12) . . ? C24 Fe1 C15 127.50(12) . . ? C18 Fe1 C15 68.34(11) . . ? C23 Fe1 C15 112.88(11) . . ? C44 Fe2 C41 117.29(12) . . ? C44 Fe2 C43 40.57(13) . . ? C41 Fe2 C43 106.08(12) . . ? C44 Fe2 C40 102.34(13) . . ? C41 Fe2 C40 40.81(11) . . ? C43 Fe2 C40 120.89(13) . . ? C44 Fe2 C42 67.78(13) . . ? C41 Fe2 C42 126.54(12) . . ? C43 Fe2 C42 40.36(13) . . ? C40 Fe2 C42 159.78(13) . . ? C44 Fe2 C45 40.68(13) . . ? C41 Fe2 C45 152.63(12) . . ? C43 Fe2 C45 67.94(13) . . ? C40 Fe2 C45 117.60(12) . . ? C42 Fe2 C45 67.13(13) . . ? C44 Fe2 C39 120.71(13) . . ? C41 Fe2 C39 68.46(11) . . ? C43 Fe2 C39 157.28(13) . . ? C40 Fe2 C39 40.67(11) . . ? C42 Fe2 C39 159.54(12) . . ? C45 Fe2 C39 106.22(12) . . ? C44 Fe2 C38 158.85(13) . . ? C41 Fe2 C38 68.72(10) . . ? C43 Fe2 C38 160.45(13) . . ? C40 Fe2 C38 68.28(11) . . ? C42 Fe2 C38 126.79(12) . . ? C45 Fe2 C38 125.45(12) . . ? C39 Fe2 C38 40.13(11) . . ? C44 Fe2 C46 67.62(13) . . ? C41 Fe2 C46 164.63(12) . . ? C43 Fe2 C46 67.47(13) . . ? C40 Fe2 C46 154.55(12) . . ? C42 Fe2 C46 39.71(12) . . ? C45 Fe2 C46 39.75(12) . . ? C39 Fe2 C46 122.96(12) . . ? C38 Fe2 C46 112.39(12) . . ? C44 Fe2 C37 154.97(12) . . ? C41 Fe2 C37 40.94(10) . . ? C43 Fe2 C37 122.75(12) . . ? C40 Fe2 C37 68.75(11) . . ? C42 Fe2 C37 112.37(11) . . ? C45 Fe2 C37 164.20(12) . . ? C39 Fe2 C37 68.47(11) . . ? C38 Fe2 C37 41.12(10) . . ? C46 Fe2 C37 129.70(12) . . ? C1 N1 C3 126.0(2) . . ? C1 N1 Ti1 92.67(15) . . ? C3 N1 Ti1 139.48(16) . . ? C1 N2 C9 124.3(2) . . ? C1 N2 Ti1 93.83(15) . . ? C9 N2 Ti1 138.73(16) . . ? C2 N3 C25 123.9(2) . . ? C2 N3 Ti1 94.40(15) . . ? C25 N3 Ti1 137.91(16) . . ? C2 N4 C31 125.1(2) . . ? C2 N4 Ti1 92.72(15) . . ? C31 N4 Ti1 142.19(17) . . ? N1 C1 N2 109.3(2) . . ? N1 C1 C15 122.9(2) . . ? N2 C1 C15 127.8(2) . . ? N4 C2 N3 109.0(2) . . ? N4 C2 C37 127.0(2) . . ? N3 C2 C37 123.9(2) . . ? N1 C3 C4 110.1(2) . . ? N1 C3 C8 110.2(2) . . ? C4 C3 C8 110.3(2) . . ? C5 C4 C3 110.7(2) . . ? C6 C5 C4 111.8(2) . . ? C5 C6 C7 109.8(2) . . ? C6 C7 C8 111.5(2) . . ? C3 C8 C7 111.2(2) . . ? N2 C9 C10 109.62(19) . . ? N2 C9 C11 111.8(2) . . ? C10 C9 C11 109.9(2) . . ? C14 C10 C9 112.0(2) . . ? C12 C11 C9 111.5(2) . . ? C11 C12 C13 112.0(2) . . ? C14 C13 C12 110.3(2) . . ? C13 C14 C10 111.3(2) . . ? C19 C15 C16 106.9(2) . . ? C19 C15 C1 128.0(2) . . ? C16 C15 C1 124.5(2) . . ? C19 C15 Fe1 68.87(14) . . ? C16 C15 Fe1 68.40(14) . . ? C1 C15 Fe1 134.32(17) . . ? C17 C16 C15 108.2(3) . . ? C17 C16 Fe1 69.70(16) . . ? C15 C16 Fe1 70.62(15) . . ? C16 C17 C18 108.6(3) . . ? C16 C17 Fe1 69.65(15) . . ? C18 C17 Fe1 70.31(16) . . ? C17 C18 C19 108.0(3) . . ? C17 C18 Fe1 69.19(17) . . ? C19 C18 Fe1 69.50(15) . . ? C18 C19 C15 108.4(3) . . ? C18 C19 Fe1 69.95(15) . . ? C15 C19 Fe1 70.39(15) . . ? C21 C20 C24 108.3(3) . . ? C21 C20 Fe1 69.57(16) . . ? C24 C20 Fe1 69.95(16) . . ? C20 C21 C22 108.2(3) . . ? C20 C21 Fe1 70.44(16) . . ? C22 C21 Fe1 69.95(15) . . ? C23 C22 C21 107.6(3) . . ? C23 C22 Fe1 70.42(16) . . ? C21 C22 Fe1 69.28(16) . . ? C24 C23 C22 107.8(3) . . ? C24 C23 Fe1 69.57(16) . . ? C22 C23 Fe1 69.28(16) . . ? C23 C24 C20 108.1(3) . . ? C23 C24 Fe1 70.29(16) . . ? C20 C24 Fe1 69.73(16) . . ? N3 C25 C26 111.2(2) . . ? N3 C25 C30 111.8(2) . . ? C26 C25 C30 109.7(2) . . ? C25 C26 C27 110.9(2) . . ? C28 C27 C26 110.9(3) . . ? C27 C28 C29 111.4(2) . . ? C28 C29 C30 111.8(2) . . ? C29 C30 C25 109.9(2) . . ? N4 C31 C32 111.5(2) . . ? N4 C31 C36 110.5(2) . . ? C32 C31 C36 110.5(2) . . ? C31 C32 C33 110.2(2) . . ? C34 C33 C32 111.2(3) . . ? C35 C34 C33 111.1(2) . . ? C34 C35 C36 111.9(2) . . ? C35 C36 C31 110.8(2) . . ? C41 C37 C38 106.2(2) . . ? C41 C37 C2 126.6(2) . . ? C38 C37 C2 126.9(2) . . ? C41 C37 Fe2 68.12(14) . . ? C38 C37 Fe2 68.76(14) . . ? C2 C37 Fe2 132.06(17) . . ? C39 C38 C37 108.6(2) . . ? C39 C38 Fe2 69.86(16) . . ? C37 C38 Fe2 70.12(14) . . ? C38 C39 C40 108.6(2) . . ? C38 C39 Fe2 70.01(15) . . ? C40 C39 Fe2 69.28(16) . . ? C41 C40 C39 107.9(2) . . ? C41 C40 Fe2 69.33(15) . . ? C39 C40 Fe2 70.06(16) . . ? C40 C41 C37 108.8(2) . . ? C40 C41 Fe2 69.86(15) . . ? C37 C41 Fe2 70.94(14) . . ? C46 C42 C43 108.4(3) . . ? C46 C42 Fe2 70.71(17) . . ? C43 C42 Fe2 69.29(17) . . ? C44 C43 C42 107.6(3) . . ? C44 C43 Fe2 69.43(18) . . ? C42 C43 Fe2 70.35(17) . . ? C43 C44 C45 107.7(3) . . ? C43 C44 Fe2 70.01(17) . . ? C45 C44 Fe2 70.50(17) . . ? C46 C45 C44 107.9(3) . . ? C46 C45 Fe2 70.67(17) . . ? C44 C45 Fe2 68.82(17) . . ? C42 C46 C45 108.3(3) . . ? C42 C46 Fe2 69.57(17) . . ? C45 C46 Fe2 69.58(17) . . ? Cl3 C47 Cl4 112.60(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.512 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.078 #===end data_CpZr[CyNC(Fc)NCy]Cl2 _database_code_depnum_ccdc_archive 'CCDC 778597' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H36 Cl2 Fe N2 Zr' _chemical_formula_weight 618.56 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1426(13) _cell_length_b 18.5720(14) _cell_length_c 7.4148(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.285(4) _cell_angle_gamma 90.00 _cell_volume 2620.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7576 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62637 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 31.51 _reflns_number_total 8714 _reflns_number_gt 7318 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+1.3750P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8714 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C1 C 0.14320(9) 0.64897(10) 0.4958(2) 0.0275(3) Uani 1 1 d . . . H1 H 0.1695 0.6529 0.6164 0.033 Uiso 1 1 calc R . . C2 C 0.14355(8) 0.69981(9) 0.3547(3) 0.0267(3) Uani 1 1 d . . . H2 H 0.1699 0.7451 0.3613 0.032 Uiso 1 1 calc R . . C3 C 0.09198(8) 0.67954(9) 0.2141(2) 0.0248(3) Uani 1 1 d . . . H3 H 0.0762 0.7086 0.1071 0.030 Uiso 1 1 calc R . . C4 C 0.05912(8) 0.61609(9) 0.2686(2) 0.0242(3) Uani 1 1 d . . . H4 H 0.0170 0.5937 0.2053 0.029 Uiso 1 1 calc R . . C5 C 0.09092(9) 0.59750(9) 0.4430(2) 0.0253(3) Uani 1 1 d . . . H5 H 0.0750 0.5595 0.5206 0.030 Uiso 1 1 calc R . . C6 C 0.24459(7) 0.48129(8) 0.44523(19) 0.0144(2) Uani 1 1 d . . . C7 C 0.33971(7) 0.57122(8) 0.5100(2) 0.0172(3) Uani 1 1 d . . . H7 H 0.3550 0.5369 0.6066 0.021 Uiso 1 1 calc R . . C8 C 0.33080(9) 0.64450(9) 0.5973(2) 0.0257(3) Uani 1 1 d . . . H8A H 0.2963 0.6406 0.6835 0.031 Uiso 1 1 calc R . . H8B H 0.3132 0.6787 0.5045 0.031 Uiso 1 1 calc R . . C9 C 0.40014(10) 0.67243(10) 0.6951(3) 0.0340(4) Uani 1 1 d . . . H9A H 0.3931 0.7207 0.7398 0.041 Uiso 1 1 calc R . . H9B H 0.4143 0.6418 0.7988 0.041 Uiso 1 1 calc R . . C10 C 0.45857(10) 0.67383(10) 0.5709(3) 0.0361(4) Uani 1 1 d . . . H10A H 0.4480 0.7102 0.4779 0.043 Uiso 1 1 calc R . . H10B H 0.5026 0.6868 0.6410 0.043 Uiso 1 1 calc R . . C11 C 0.46652(8) 0.60097(10) 0.4815(3) 0.0295(4) Uani 1 1 d . . . H11A H 0.4830 0.5659 0.5734 0.035 Uiso 1 1 calc R . . H11B H 0.5014 0.6046 0.3964 0.035 Uiso 1 1 calc R . . C12 C 0.39703(8) 0.57510(9) 0.3812(2) 0.0224(3) Uani 1 1 d . . . H12A H 0.4035 0.5279 0.3298 0.027 Uiso 1 1 calc R . . H12B H 0.3824 0.6079 0.2824 0.027 Uiso 1 1 calc R . . C13 C 0.14084(7) 0.40702(8) 0.3334(2) 0.0160(3) Uani 1 1 d . . . H13 H 0.1425 0.3849 0.4538 0.019 Uiso 1 1 calc R . . C14 C 0.06367(7) 0.42119(9) 0.2646(2) 0.0210(3) Uani 1 1 d . . . H14A H 0.0432 0.4531 0.3483 0.025 Uiso 1 1 calc R . . H14B H 0.0608 0.4448 0.1474 0.025 Uiso 1 1 calc R . . C15 C 0.02212(8) 0.35092(9) 0.2471(2) 0.0225(3) Uani 1 1 d . . . H15A H 0.0205 0.3302 0.3667 0.027 Uiso 1 1 calc R . . H15B H -0.0258 0.3610 0.1963 0.027 Uiso 1 1 calc R . . C16 C 0.05456(8) 0.29658(9) 0.1268(2) 0.0232(3) Uani 1 1 d . . . H16A H 0.0289 0.2515 0.1267 0.028 Uiso 1 1 calc R . . H16B H 0.0507 0.3145 0.0032 0.028 Uiso 1 1 calc R . . C17 C 0.13152(8) 0.28336(8) 0.1936(2) 0.0209(3) Uani 1 1 d . . . H17A H 0.1518 0.2511 0.1105 0.025 Uiso 1 1 calc R . . H17B H 0.1350 0.2604 0.3117 0.025 Uiso 1 1 calc R . . C18 C 0.17269(7) 0.35382(8) 0.2074(2) 0.0190(3) Uani 1 1 d . . . H18A H 0.1722 0.3750 0.0877 0.023 Uiso 1 1 calc R . . H18B H 0.2212 0.3442 0.2536 0.023 Uiso 1 1 calc R . . C19 C 0.27956(7) 0.42071(8) 0.55056(19) 0.0151(2) Uani 1 1 d . . . C20 C 0.34629(7) 0.39061(8) 0.5190(2) 0.0178(3) Uani 1 1 d . . . H20 H 0.3804 0.4126 0.4463 0.021 Uiso 1 1 calc R . . C21 C 0.35428(8) 0.32373(9) 0.6110(2) 0.0232(3) Uani 1 1 d . . . H21 H 0.3948 0.2914 0.6122 0.028 Uiso 1 1 calc R . . C22 C 0.29419(8) 0.31203(9) 0.7036(2) 0.0240(3) Uani 1 1 d . . . H22 H 0.2857 0.2701 0.7783 0.029 Uiso 1 1 calc R . . C23 C 0.24819(7) 0.37201(8) 0.6683(2) 0.0196(3) Uani 1 1 d . . . H23 H 0.2027 0.3785 0.7152 0.024 Uiso 1 1 calc R . . C24 C 0.42240(9) 0.47030(10) 0.9036(2) 0.0260(3) Uani 1 1 d . . . H24 H 0.4562 0.4960 0.8368 0.031 Uiso 1 1 calc R . . C25 C 0.35638(9) 0.49720(9) 0.9443(2) 0.0246(3) Uani 1 1 d . . . H25 H 0.3366 0.5446 0.9101 0.030 Uiso 1 1 calc R . . C26 C 0.32360(9) 0.44290(10) 1.0404(2) 0.0262(3) Uani 1 1 d . . . H26 H 0.2774 0.4464 1.0853 0.031 Uiso 1 1 calc R . . C27 C 0.36960(10) 0.38286(10) 1.0611(2) 0.0290(4) Uani 1 1 d . . . H27 H 0.3607 0.3377 1.1228 0.035 Uiso 1 1 calc R . . C28 C 0.43073(9) 0.39947(10) 0.9761(2) 0.0298(4) Uani 1 1 d . . . H28 H 0.4713 0.3679 0.9690 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.26327(2) 0.66306(2) 0.08757(6) 0.02625(8) Uani 1 1 d . . . Cl2 Cl 0.14173(2) 0.53220(2) -0.06564(5) 0.02842(9) Uani 1 1 d . . . Fe1 Fe 0.342941(10) 0.404422(11) 0.79238(3) 0.01546(5) Uani 1 1 d . . . N1 N 0.18077(6) 0.47469(7) 0.35204(17) 0.0165(2) Uani 1 1 d . . . N2 N 0.27220(6) 0.54636(7) 0.41933(17) 0.0162(2) Uani 1 1 d . . . Zr1 Zr 0.183412(7) 0.583743(8) 0.228917(19) 0.01532(4) 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 0.0257(7) 0.0329(9) 0.0238(8) -0.0099(7) 0.0031(6) 0.0076(7) C2 0.0224(7) 0.0192(7) 0.0387(10) -0.0079(7) 0.0041(6) 0.0033(6) C3 0.0201(7) 0.0202(7) 0.0335(9) 0.0015(6) 0.0002(6) 0.0076(6) C4 0.0158(6) 0.0239(8) 0.0327(9) -0.0023(7) 0.0023(6) 0.0036(6) C5 0.0244(7) 0.0260(8) 0.0271(8) -0.0002(6) 0.0100(6) 0.0057(6) C6 0.0140(5) 0.0171(6) 0.0120(6) -0.0001(5) 0.0008(4) 0.0006(5) C7 0.0149(6) 0.0174(7) 0.0180(7) 0.0008(5) -0.0035(5) -0.0025(5) C8 0.0247(7) 0.0212(8) 0.0294(8) -0.0061(6) -0.0056(6) 0.0005(6) C9 0.0357(9) 0.0252(9) 0.0373(10) -0.0081(7) -0.0138(8) -0.0042(7) C10 0.0321(9) 0.0293(9) 0.0430(11) 0.0109(8) -0.0138(8) -0.0147(7) C11 0.0176(7) 0.0382(10) 0.0316(9) 0.0096(7) -0.0028(6) -0.0068(6) C12 0.0175(6) 0.0273(8) 0.0221(7) 0.0031(6) 0.0002(5) -0.0030(6) C13 0.0128(5) 0.0168(6) 0.0175(6) 0.0004(5) -0.0020(5) -0.0014(5) C14 0.0134(6) 0.0217(7) 0.0271(8) -0.0037(6) -0.0019(5) 0.0007(5) C15 0.0153(6) 0.0247(8) 0.0272(8) -0.0026(6) 0.0005(5) -0.0024(5) C16 0.0190(6) 0.0231(7) 0.0266(8) -0.0050(6) -0.0027(6) -0.0028(5) C17 0.0217(7) 0.0184(7) 0.0217(7) -0.0025(6) -0.0021(5) 0.0006(5) C18 0.0148(6) 0.0198(7) 0.0218(7) -0.0015(6) -0.0010(5) 0.0003(5) C19 0.0141(5) 0.0155(6) 0.0148(6) 0.0000(5) -0.0022(4) -0.0020(5) C20 0.0172(6) 0.0205(7) 0.0149(6) -0.0017(5) -0.0013(5) 0.0026(5) C21 0.0255(7) 0.0173(7) 0.0247(8) -0.0030(6) -0.0062(6) 0.0038(6) C22 0.0262(7) 0.0169(7) 0.0265(8) 0.0043(6) -0.0076(6) -0.0056(6) C23 0.0157(6) 0.0215(7) 0.0205(7) 0.0041(6) -0.0036(5) -0.0049(5) C24 0.0257(7) 0.0325(9) 0.0180(7) -0.0016(6) -0.0053(6) -0.0115(6) C25 0.0356(8) 0.0220(8) 0.0154(7) -0.0032(6) -0.0006(6) -0.0058(6) C26 0.0345(8) 0.0283(8) 0.0161(7) -0.0016(6) 0.0047(6) -0.0064(7) C27 0.0419(9) 0.0283(9) 0.0150(7) 0.0053(6) -0.0051(6) -0.0057(7) C28 0.0250(7) 0.0376(10) 0.0237(8) 0.0013(7) -0.0115(6) 0.0007(7) Cl1 0.02483(17) 0.02495(19) 0.0293(2) 0.01018(16) 0.00428(14) 0.00116(14) Cl2 0.0361(2) 0.0305(2) 0.01704(17) -0.00164(15) -0.00454(14) 0.00278(16) Fe1 0.01520(9) 0.01670(10) 0.01361(10) 0.00125(7) -0.00229(7) -0.00177(7) N1 0.0142(5) 0.0154(6) 0.0190(6) 0.0002(5) -0.0026(4) -0.0001(4) N2 0.0147(5) 0.0156(6) 0.0174(6) 0.0008(4) -0.0022(4) -0.0007(4) Zr1 0.01505(6) 0.01560(7) 0.01488(7) 0.00084(5) -0.00032(4) 0.00313(5) _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 C1 C5 1.408(2) . ? C1 C2 1.410(3) . ? C1 Zr1 2.5121(16) . ? C2 C3 1.407(2) . ? C2 Zr1 2.5010(16) . ? C3 C4 1.415(2) . ? C3 Zr1 2.4897(15) . ? C4 C5 1.411(2) . ? C4 Zr1 2.5022(15) . ? C5 Zr1 2.5172(16) . ? C6 N2 1.3412(18) . ? C6 N1 1.3417(17) . ? C6 C19 1.4865(19) . ? C7 N2 1.4645(17) . ? C7 C8 1.525(2) . ? C7 C12 1.533(2) . ? C8 C9 1.532(2) . ? C9 C10 1.525(3) . ? C10 C11 1.522(3) . ? C11 C12 1.529(2) . ? C13 N1 1.4695(18) . ? C13 C18 1.532(2) . ? C13 C14 1.5320(19) . ? C14 C15 1.527(2) . ? C15 C16 1.524(2) . ? C16 C17 1.522(2) . ? C17 C18 1.525(2) . ? C19 C23 1.434(2) . ? C19 C20 1.4369(19) . ? C19 Fe1 2.0742(13) . ? C20 C21 1.418(2) . ? C20 Fe1 2.0514(15) . ? C21 C22 1.419(2) . ? C21 Fe1 2.0410(16) . ? C22 C23 1.426(2) . ? C22 Fe1 2.0284(15) . ? C23 Fe1 2.0331(14) . ? C24 C25 1.422(3) . ? C24 C28 1.423(3) . ? C24 Fe1 2.0534(15) . ? C25 C26 1.420(2) . ? C25 Fe1 2.0593(16) . ? C26 C27 1.419(3) . ? C26 Fe1 2.0443(17) . ? C27 C28 1.422(3) . ? C27 Fe1 2.0413(16) . ? C28 Fe1 2.0460(15) . ? Cl1 Zr1 2.4405(4) . ? Cl2 Zr1 2.4375(4) . ? N1 Zr1 2.2245(12) . ? N2 Zr1 2.1998(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 108.02(15) . . ? C5 C1 Zr1 73.94(9) . . ? C2 C1 Zr1 73.23(9) . . ? C3 C2 C1 108.12(15) . . ? C3 C2 Zr1 73.19(9) . . ? C1 C2 Zr1 74.10(10) . . ? C2 C3 C4 108.01(15) . . ? C2 C3 Zr1 74.07(9) . . ? C4 C3 Zr1 74.02(9) . . ? C5 C4 C3 107.73(15) . . ? C5 C4 Zr1 74.26(9) . . ? C3 C4 Zr1 73.04(9) . . ? C1 C5 C4 108.12(16) . . ? C1 C5 Zr1 73.54(9) . . ? C4 C5 Zr1 73.09(9) . . ? N2 C6 N1 111.07(12) . . ? N2 C6 C19 126.54(12) . . ? N1 C6 C19 122.25(12) . . ? N2 C7 C8 110.01(12) . . ? N2 C7 C12 112.63(12) . . ? C8 C7 C12 110.09(13) . . ? C7 C8 C9 111.83(14) . . ? C10 C9 C8 112.02(15) . . ? C11 C10 C9 111.28(14) . . ? C10 C11 C12 111.60(15) . . ? C11 C12 C7 110.85(13) . . ? N1 C13 C18 111.80(12) . . ? N1 C13 C14 110.92(12) . . ? C18 C13 C14 109.96(12) . . ? C15 C14 C13 110.85(13) . . ? C16 C15 C14 111.97(13) . . ? C17 C16 C15 111.00(12) . . ? C16 C17 C18 110.99(13) . . ? C17 C18 C13 110.94(12) . . ? C23 C19 C20 107.04(13) . . ? C23 C19 C6 127.08(12) . . ? C20 C19 C6 124.47(13) . . ? C23 C19 Fe1 68.04(8) . . ? C20 C19 Fe1 68.77(8) . . ? C6 C19 Fe1 138.74(10) . . ? C21 C20 C19 108.26(13) . . ? C21 C20 Fe1 69.34(9) . . ? C19 C20 Fe1 70.47(8) . . ? C20 C21 C22 108.45(14) . . ? C20 C21 Fe1 70.13(9) . . ? C22 C21 Fe1 69.11(9) . . ? C21 C22 C23 107.96(14) . . ? C21 C22 Fe1 70.06(9) . . ? C23 C22 Fe1 69.62(9) . . ? C22 C23 C19 108.25(13) . . ? C22 C23 Fe1 69.26(8) . . ? C19 C23 Fe1 71.12(8) . . ? C25 C24 C28 108.06(15) . . ? C25 C24 Fe1 70.00(9) . . ? C28 C24 Fe1 69.40(9) . . ? C26 C25 C24 108.00(16) . . ? C26 C25 Fe1 69.19(9) . . ? C24 C25 Fe1 69.55(9) . . ? C27 C26 C25 108.01(16) . . ? C27 C26 Fe1 69.57(10) . . ? C25 C26 Fe1 70.32(9) . . ? C26 C27 C28 108.22(16) . . ? C26 C27 Fe1 69.79(9) . . ? C28 C27 Fe1 69.81(9) . . ? C27 C28 C24 107.71(16) . . ? C27 C28 Fe1 69.46(9) . . ? C24 C28 Fe1 69.97(9) . . ? C22 Fe1 C23 41.12(6) . . ? C22 Fe1 C21 40.83(7) . . ? C23 Fe1 C21 68.80(6) . . ? C22 Fe1 C27 101.99(7) . . ? C23 Fe1 C27 119.93(7) . . ? C21 Fe1 C27 117.76(7) . . ? C22 Fe1 C26 117.74(7) . . ? C23 Fe1 C26 105.68(7) . . ? C21 Fe1 C26 153.16(7) . . ? C27 Fe1 C26 40.64(7) . . ? C22 Fe1 C28 119.55(7) . . ? C23 Fe1 C28 156.20(7) . . ? C21 Fe1 C28 105.47(7) . . ? C27 Fe1 C28 40.73(8) . . ? C26 Fe1 C28 68.49(8) . . ? C22 Fe1 C20 68.69(7) . . ? C23 Fe1 C20 68.81(6) . . ? C21 Fe1 C20 40.53(6) . . ? C27 Fe1 C20 155.29(7) . . ? C26 Fe1 C20 163.96(7) . . ? C28 Fe1 C20 122.68(7) . . ? C22 Fe1 C24 158.24(7) . . ? C23 Fe1 C24 160.59(7) . . ? C21 Fe1 C24 125.07(7) . . ? C27 Fe1 C24 68.28(7) . . ? C26 Fe1 C24 68.25(7) . . ? C28 Fe1 C24 40.63(7) . . ? C20 Fe1 C24 111.69(7) . . ? C22 Fe1 C25 155.63(7) . . ? C23 Fe1 C25 123.17(7) . . ? C21 Fe1 C25 163.52(7) . . ? C27 Fe1 C25 68.12(7) . . ? C26 Fe1 C25 40.49(7) . . ? C28 Fe1 C25 68.23(7) . . ? C20 Fe1 C25 129.03(6) . . ? C24 Fe1 C25 40.45(7) . . ? C22 Fe1 C19 68.77(6) . . ? C23 Fe1 C19 40.84(6) . . ? C21 Fe1 C19 68.40(6) . . ? C27 Fe1 C19 158.80(7) . . ? C26 Fe1 C19 125.47(7) . . ? C28 Fe1 C19 160.40(7) . . ? C20 Fe1 C19 40.76(5) . . ? C24 Fe1 C19 126.72(6) . . ? C25 Fe1 C19 112.16(6) . . ? C6 N1 C13 124.16(12) . . ? C6 N1 Zr1 93.89(9) . . ? C13 N1 Zr1 140.81(9) . . ? C6 N2 C7 124.07(12) . . ? C6 N2 Zr1 95.01(8) . . ? C7 N2 Zr1 140.90(10) . . ? N2 Zr1 N1 59.99(4) . . ? N2 Zr1 Cl2 127.25(4) . . ? N1 Zr1 Cl2 89.44(3) . . ? N2 Zr1 Cl1 89.42(3) . . ? N1 Zr1 Cl1 140.29(3) . . ? Cl2 Zr1 Cl1 90.643(16) . . ? N2 Zr1 C3 138.07(5) . . ? N1 Zr1 C3 128.41(5) . . ? Cl2 Zr1 C3 94.68(4) . . ? Cl1 Zr1 C3 91.15(4) . . ? N2 Zr1 C2 106.17(5) . . ? N1 Zr1 C2 127.59(6) . . ? Cl2 Zr1 C2 126.12(4) . . ? Cl1 Zr1 C2 82.59(4) . . ? C3 Zr1 C2 32.74(5) . . ? N2 Zr1 C4 132.70(5) . . ? N1 Zr1 C4 96.07(5) . . ? Cl2 Zr1 C4 88.70(4) . . ? Cl1 Zr1 C4 123.64(4) . . ? C3 Zr1 C4 32.94(6) . . ? C2 Zr1 C4 54.30(5) . . ? N2 Zr1 C1 85.89(5) . . ? N1 Zr1 C1 95.34(6) . . ? Cl2 Zr1 C1 142.83(4) . . ? Cl1 Zr1 C1 107.91(5) . . ? C3 Zr1 C1 54.24(6) . . ? C2 Zr1 C1 32.66(6) . . ? C4 Zr1 C1 54.15(5) . . ? N2 Zr1 C5 100.06(5) . . ? N1 Zr1 C5 77.55(5) . . ? Cl2 Zr1 C5 114.91(4) . . ? Cl1 Zr1 C5 136.59(4) . . ? C3 Zr1 C5 54.24(6) . . ? C2 Zr1 C5 54.04(6) . . ? C4 Zr1 C5 32.65(6) . . ? C1 Zr1 C5 32.52(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.531 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.073 #===end data_Cp*Zr[CyNC(Fc)NCy]Cl2 _database_code_depnum_ccdc_archive 'CCDC 778598' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C36 H53 Cl2 Fe N2 Zr' _chemical_formula_weight 731.88 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 19.7051(12) _cell_length_b 14.5964(10) _cell_length_c 24.6497(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7089.8(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6882 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 113245 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.55 _reflns_number_total 15687 _reflns_number_gt 12881 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+3.4139P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.502(13) _refine_ls_number_reflns 15687 _refine_ls_number_parameters 769 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 C1 C 0.52102(17) 0.9429(2) 0.18030(14) 0.0305(8) Uani 1 1 d . . . C2 C 0.55758(15) 0.8773(2) 0.21146(16) 0.0322(8) Uani 1 1 d . . . C3 C 0.53891(16) 0.8882(2) 0.26646(15) 0.0319(8) Uani 1 1 d . . . C4 C 0.48961(17) 0.9588(2) 0.26881(15) 0.0338(8) Uani 1 1 d . . . C5 C 0.47875(16) 0.9926(2) 0.21567(16) 0.0326(8) Uani 1 1 d . . . C6 C 0.31240(16) 0.8856(2) 0.24285(13) 0.0230(7) Uani 1 1 d . . . C7 C 0.32698(17) 0.8009(2) 0.32829(13) 0.0255(7) Uani 1 1 d . . . H7 H 0.2898 0.8402 0.3409 0.031 Uiso 1 1 calc R . . C8 C 0.38111(18) 0.7983(3) 0.37243(14) 0.0359(8) Uani 1 1 d . . . H8A H 0.3985 0.8596 0.3787 0.043 Uiso 1 1 calc R . . H8B H 0.4186 0.7598 0.3609 0.043 Uiso 1 1 calc R . . C9 C 0.3505(2) 0.7604(3) 0.42484(15) 0.0438(10) Uani 1 1 d . . . H9A H 0.3856 0.7575 0.4524 0.053 Uiso 1 1 calc R . . H9B H 0.3156 0.8020 0.4376 0.053 Uiso 1 1 calc R . . C10 C 0.3202(2) 0.6662(3) 0.41735(16) 0.0479(10) Uani 1 1 d . . . H10A H 0.2982 0.6473 0.4507 0.057 Uiso 1 1 calc R . . H10B H 0.3560 0.6226 0.4095 0.057 Uiso 1 1 calc R . . C11 C 0.2689(2) 0.6654(3) 0.37159(16) 0.0408(9) Uani 1 1 d . . . H11A H 0.2296 0.7012 0.3821 0.049 Uiso 1 1 calc R . . H11B H 0.2541 0.6030 0.3651 0.049 Uiso 1 1 calc R . . C12 C 0.29874(17) 0.7047(2) 0.31947(15) 0.0300(8) Uani 1 1 d . . . H12A H 0.2638 0.7068 0.2918 0.036 Uiso 1 1 calc R . . H12B H 0.3347 0.6649 0.3067 0.036 Uiso 1 1 calc R . . C13 C 0.29908(16) 0.9134(2) 0.14545(13) 0.0270(8) Uani 1 1 d . . . H13 H 0.2640 0.9585 0.1546 0.032 Uiso 1 1 calc R . . C14 C 0.33978(19) 0.9504(2) 0.09830(14) 0.0337(8) Uani 1 1 d . . . H14A H 0.3776 0.9096 0.0910 0.040 Uiso 1 1 calc R . . H14B H 0.3581 1.0099 0.1079 0.040 Uiso 1 1 calc R . . C15 C 0.2963(2) 0.9595(3) 0.04725(16) 0.0446(10) Uani 1 1 d . . . H15A H 0.2613 1.0050 0.0534 0.053 Uiso 1 1 calc R . . H15B H 0.3245 0.9805 0.0175 0.053 Uiso 1 1 calc R . . C16 C 0.2636(2) 0.8697(3) 0.03190(16) 0.0443(10) Uani 1 1 d . . . H16A H 0.2984 0.8252 0.0230 0.053 Uiso 1 1 calc R . . H16B H 0.2352 0.8783 0.0002 0.053 Uiso 1 1 calc R . . C17 C 0.22093(19) 0.8343(3) 0.07854(17) 0.0462(10) Uani 1 1 d . . . H17A H 0.2017 0.7753 0.0689 0.055 Uiso 1 1 calc R . . H17B H 0.1838 0.8764 0.0854 0.055 Uiso 1 1 calc R . . C18 C 0.26400(18) 0.8243(2) 0.12976(14) 0.0326(8) Uani 1 1 d . . . H18A H 0.2352 0.8045 0.1595 0.039 Uiso 1 1 calc R . . H18B H 0.2980 0.7773 0.1239 0.039 Uiso 1 1 calc R . . C19 C 0.24468(15) 0.9249(2) 0.25548(13) 0.0237(7) Uani 1 1 d . . . C20 C 0.22509(17) 1.0151(2) 0.23886(14) 0.0282(8) Uani 1 1 d . . . H20 H 0.2551 1.0610 0.2225 0.034 Uiso 1 1 calc R . . C21 C 0.15539(17) 1.0271(3) 0.25026(14) 0.0325(8) Uani 1 1 d . . . H21 H 0.1286 1.0823 0.2428 0.039 Uiso 1 1 calc R . . C22 C 0.13111(16) 0.9457(3) 0.27380(15) 0.0362(8) Uani 1 1 d . . . H22 H 0.0844 0.9347 0.2859 0.043 Uiso 1 1 calc R . . C23 C 0.18563(16) 0.8827(2) 0.27811(14) 0.0303(8) Uani 1 1 d . . . H23 H 0.1831 0.8208 0.2934 0.036 Uiso 1 1 calc R . . C24 C 0.2626(2) 1.0963(3) 0.35991(16) 0.0420(9) Uani 1 1 d . . . H24 H 0.2969 1.1364 0.3436 0.050 Uiso 1 1 calc R . . C25 C 0.27470(19) 1.0097(2) 0.38293(15) 0.0341(8) Uani 1 1 d . . . H25 H 0.3187 0.9788 0.3853 0.041 Uiso 1 1 calc R . . C26 C 0.2123(2) 0.9749(3) 0.40127(15) 0.0428(10) Uani 1 1 d . . . H26 H 0.2052 0.9156 0.4190 0.051 Uiso 1 1 calc R . . C27 C 0.1614(2) 1.0411(3) 0.38998(17) 0.0533(11) Uani 1 1 d . . . H27 H 0.1130 1.0358 0.3987 0.064 Uiso 1 1 calc R . . C28 C 0.1932(2) 1.1159(3) 0.36449(17) 0.0492(11) Uani 1 1 d . . . H28 H 0.1707 1.1720 0.3520 0.059 Uiso 1 1 calc R . . C29 C 0.4615(2) 1.0035(3) 0.31898(19) 0.0506(11) Uani 1 1 d . . . H29A H 0.4726 0.9670 0.3501 0.076 Uiso 1 1 calc R . . H29B H 0.4131 1.0085 0.3159 0.076 Uiso 1 1 calc R . . H29C H 0.4808 1.0635 0.3230 0.076 Uiso 1 1 calc R . . C30 C 0.5702(2) 0.8402(3) 0.31415(16) 0.0463(10) Uani 1 1 d . . . H30A H 0.6093 0.8739 0.3262 0.069 Uiso 1 1 calc R . . H30B H 0.5838 0.7796 0.3036 0.069 Uiso 1 1 calc R . . H30C H 0.5377 0.8365 0.3431 0.069 Uiso 1 1 calc R . . C31 C 0.61022(18) 0.8130(3) 0.18965(17) 0.0450(10) Uani 1 1 d . . . H31A H 0.6539 0.8419 0.1909 0.067 Uiso 1 1 calc R . . H31B H 0.5994 0.7975 0.1528 0.067 Uiso 1 1 calc R . . H31C H 0.6110 0.7583 0.2113 0.067 Uiso 1 1 calc R . . C32 C 0.5314(2) 0.9602(3) 0.12115(16) 0.0436(10) Uani 1 1 d . . . H32A H 0.5756 0.9864 0.1155 0.065 Uiso 1 1 calc R . . H32B H 0.4974 1.0019 0.1083 0.065 Uiso 1 1 calc R . . H32C H 0.5281 0.9035 0.1016 0.065 Uiso 1 1 calc R . . C33 C 0.43634(19) 1.0755(2) 0.20281(19) 0.0444(11) Uani 1 1 d . . . H33A H 0.4564 1.1287 0.2192 0.067 Uiso 1 1 calc R . . H33B H 0.3913 1.0670 0.2169 0.067 Uiso 1 1 calc R . . H33C H 0.4342 1.0837 0.1642 0.067 Uiso 1 1 calc R . . C34 C 0.24661(17) 0.4654(2) 0.11110(14) 0.0333(8) Uani 1 1 d . . . C35 C 0.19580(17) 0.3961(3) 0.11157(16) 0.0380(9) Uani 1 1 d . . . C36 C 0.17397(15) 0.3843(2) 0.16515(17) 0.0361(8) Uani 1 1 d . . . C37 C 0.20904(17) 0.4482(2) 0.19856(15) 0.0322(8) Uani 1 1 d . . . C38 C 0.25458(15) 0.4974(2) 0.16493(15) 0.0288(7) Uani 1 1 d . . . C39 C 0.41955(16) 0.3854(2) 0.14308(12) 0.0211(7) Uani 1 1 d . . . C40 C 0.42796(16) 0.4147(2) 0.24120(13) 0.0257(7) Uani 1 1 d . . . H40 H 0.4620 0.4619 0.2335 0.031 Uiso 1 1 calc R . . C41 C 0.46460(17) 0.3271(2) 0.25835(14) 0.0311(8) Uani 1 1 d . . . H41A H 0.4316 0.2783 0.2626 0.037 Uiso 1 1 calc R . . H41B H 0.4960 0.3091 0.2299 0.037 Uiso 1 1 calc R . . C42 C 0.5035(2) 0.3387(3) 0.31115(15) 0.0414(9) Uani 1 1 d . . . H42A H 0.5237 0.2807 0.3215 0.050 Uiso 1 1 calc R . . H42B H 0.5398 0.3827 0.3060 0.050 Uiso 1 1 calc R . . C43 C 0.4570(2) 0.3716(3) 0.35609(15) 0.0418(9) Uani 1 1 d . . . H43A H 0.4232 0.3251 0.3637 0.050 Uiso 1 1 calc R . . H43B H 0.4832 0.3817 0.3889 0.050 Uiso 1 1 calc R . . C44 C 0.4222(2) 0.4595(3) 0.33981(15) 0.0428(9) Uani 1 1 d . . . H44A H 0.4559 0.5073 0.3354 0.051 Uiso 1 1 calc R . . H44B H 0.3914 0.4782 0.3684 0.051 Uiso 1 1 calc R . . C45 C 0.38268(18) 0.4485(2) 0.28697(13) 0.0321(8) Uani 1 1 d . . . H45A H 0.3459 0.4054 0.2925 0.039 Uiso 1 1 calc R . . H45B H 0.3630 0.5070 0.2769 0.039 Uiso 1 1 calc R . . C46 C 0.40905(16) 0.3019(2) 0.05781(13) 0.0247(7) Uani 1 1 d . . . H46 H 0.4471 0.3410 0.0469 0.030 Uiso 1 1 calc R . . C47 C 0.35841(17) 0.2999(2) 0.01115(14) 0.0307(8) Uani 1 1 d . . . H47A H 0.3418 0.3614 0.0043 0.037 Uiso 1 1 calc R . . H47B H 0.3200 0.2617 0.0209 0.037 Uiso 1 1 calc R . . C48 C 0.39177(19) 0.2622(3) -0.04008(14) 0.0399(9) Uani 1 1 d . . . H48A H 0.3584 0.2596 -0.0690 0.048 Uiso 1 1 calc R . . H48B H 0.4278 0.3033 -0.0514 0.048 Uiso 1 1 calc R . . C49 C 0.4206(2) 0.1683(3) -0.03088(16) 0.0486(10) Uani 1 1 d . . . H49A H 0.4441 0.1484 -0.0634 0.058 Uiso 1 1 calc R . . H49B H 0.3838 0.1257 -0.0240 0.058 Uiso 1 1 calc R . . C50 C 0.4695(2) 0.1663(3) 0.01649(15) 0.0410(9) Uani 1 1 d . . . H50A H 0.5096 0.2018 0.0075 0.049 Uiso 1 1 calc R . . H50B H 0.4835 0.1037 0.0233 0.049 Uiso 1 1 calc R . . C51 C 0.43665(17) 0.2057(2) 0.06768(15) 0.0290(8) Uani 1 1 d . . . H51A H 0.3999 0.1659 0.0791 0.035 Uiso 1 1 calc R . . H51B H 0.4700 0.2077 0.0966 0.035 Uiso 1 1 calc R . . C52 C 0.48754(16) 0.4256(2) 0.13213(12) 0.0232(7) Uani 1 1 d . . . C53 C 0.54812(16) 0.3833(2) 0.11223(13) 0.0271(7) Uani 1 1 d . . . H53 H 0.5519 0.3209 0.0979 0.033 Uiso 1 1 calc R . . C54 C 0.60175(17) 0.4468(2) 0.11773(14) 0.0335(8) Uani 1 1 d . . . H54 H 0.6492 0.4360 0.1078 0.040 Uiso 1 1 calc R . . C55 C 0.57525(18) 0.5285(3) 0.13921(14) 0.0302(8) Uani 1 1 d . . . H55 H 0.6012 0.5842 0.1469 0.036 Uiso 1 1 calc R . . C56 C 0.50540(17) 0.5169(2) 0.14790(12) 0.0264(7) Uani 1 1 d . . . H56 H 0.4743 0.5630 0.1626 0.032 Uiso 1 1 calc R . . C57 C 0.4766(2) 0.5951(2) 0.02374(14) 0.0386(9) Uani 1 1 d . . . H57 H 0.4419 0.6370 0.0377 0.046 Uiso 1 1 calc R . . C58 C 0.46506(18) 0.5074(2) 0.00185(13) 0.0307(8) Uani 1 1 d . . . H58 H 0.4207 0.4775 -0.0016 0.037 Uiso 1 1 calc R . . C59 C 0.52767(18) 0.4691(3) -0.01340(14) 0.0344(8) Uani 1 1 d . . . H59 H 0.5346 0.4086 -0.0298 0.041 Uiso 1 1 calc R . . C60 C 0.5787(2) 0.5342(3) -0.00121(15) 0.0437(10) Uani 1 1 d . . . H60 H 0.6275 0.5269 -0.0078 0.052 Uiso 1 1 calc R . . C61 C 0.5469(2) 0.6120(3) 0.02209(16) 0.0425(10) Uani 1 1 d . . . H61 H 0.5697 0.6679 0.0343 0.051 Uiso 1 1 calc R . . C62 C 0.1665(2) 0.3501(3) 0.0620(2) 0.0627(14) Uani 1 1 d . . . H62A H 0.1521 0.2892 0.0713 0.094 Uiso 1 1 calc R . . H62B H 0.2005 0.3471 0.0341 0.094 Uiso 1 1 calc R . . H62C H 0.1283 0.3846 0.0491 0.094 Uiso 1 1 calc R . . C63 C 0.2803(2) 0.5098(3) 0.06316(18) 0.0527(11) Uani 1 1 d . . . H63A H 0.2659 0.5724 0.0605 0.079 Uiso 1 1 calc R . . H63B H 0.2679 0.4777 0.0306 0.079 Uiso 1 1 calc R . . H63C H 0.3287 0.5076 0.0677 0.079 Uiso 1 1 calc R . . C64 C 0.29734(18) 0.5781(2) 0.18018(17) 0.0408(10) Uani 1 1 d . . . H64A H 0.2791 0.6324 0.1637 0.061 Uiso 1 1 calc R . . H64B H 0.3430 0.5687 0.1677 0.061 Uiso 1 1 calc R . . H64C H 0.2974 0.5851 0.2189 0.061 Uiso 1 1 calc R . . C65 C 0.1949(2) 0.4645(3) 0.25726(18) 0.0455(11) Uani 1 1 d . . . H65A H 0.2297 0.5029 0.2723 0.068 Uiso 1 1 calc R . . H65B H 0.1942 0.4070 0.2761 0.068 Uiso 1 1 calc R . . H65C H 0.1517 0.4941 0.2611 0.068 Uiso 1 1 calc R . . C66 C 0.11902(19) 0.3199(3) 0.1841(2) 0.0557(12) Uani 1 1 d . . . H66A H 0.0760 0.3402 0.1705 0.083 Uiso 1 1 calc R . . H66B H 0.1179 0.3193 0.2231 0.083 Uiso 1 1 calc R . . H66C H 0.1282 0.2593 0.1710 0.083 Uiso 1 1 calc R . . Cl1 Cl 0.46742(4) 0.68286(6) 0.25997(4) 0.03391(19) Uani 1 1 d . . . Cl2 Cl 0.44566(4) 0.75688(6) 0.12882(4) 0.0349(2) Uani 1 1 d . . . Cl3 Cl 0.27880(5) 0.25668(6) 0.25110(4) 0.0400(2) Uani 1 1 d . . . Cl4 Cl 0.26272(5) 0.18734(6) 0.11922(4) 0.0404(2) Uani 1 1 d . . . Fe1 Fe 0.20706(2) 0.99978(3) 0.319905(19) 0.02636(10) Uani 1 1 d . . . Fe3 Fe 0.52836(2) 0.49860(3) 0.067903(19) 0.02443(10) Uani 1 1 d . . . N1 N 0.34101(13) 0.89761(19) 0.19430(11) 0.0243(6) Uani 1 1 d . . . N2 N 0.35261(13) 0.83840(18) 0.27684(11) 0.0248(6) Uani 1 1 d . . . N3 N 0.38073(13) 0.33957(18) 0.10784(11) 0.0249(6) Uani 1 1 d . . . N4 N 0.38886(12) 0.39694(18) 0.19125(10) 0.0228(6) Uani 1 1 d . . . Zr1 Zr 0.436701(13) 0.828148(19) 0.217374(12) 0.02293(7) Uani 1 1 d . . . Zr2 Zr 0.293427(14) 0.33087(2) 0.163847(13) 0.02441(7) Uani 1 1 d . . . C81 C 0.5710(4) 0.9106(7) 0.9675(3) 0.135(3) Uani 1 1 d . . . H81A H 0.5832 0.9394 0.9334 0.162 Uiso 1 1 calc R . . H81B H 0.5598 0.9590 0.9929 0.162 Uiso 1 1 calc R . . C82 C 0.5097(4) 0.8535(8) 0.9586(4) 0.160(4) Uani 1 1 d . . . H82A H 0.5243 0.8022 0.9365 0.192 Uiso 1 1 calc R . . H82B H 0.4981 0.8283 0.9938 0.192 Uiso 1 1 calc R . . C83 C 0.4526(6) 0.8815(10) 0.9374(3) 0.231(8) Uani 1 1 d . . . H83A H 0.4650 0.9120 0.9039 0.278 Uiso 1 1 calc R . . H83B H 0.4361 0.9291 0.9615 0.278 Uiso 1 1 calc R . . C85 C 0.3392(9) 0.8808(11) 0.8979(4) 0.262(9) Uani 1 1 d . . . H85A H 0.3242 0.9288 0.9217 0.393 Uiso 1 1 calc R . . H85B H 0.3019 0.8404 0.8903 0.393 Uiso 1 1 calc R . . H85C H 0.3555 0.9070 0.8647 0.393 Uiso 1 1 calc R . . C80 C 0.6296(4) 0.8611(5) 0.9879(3) 0.125(3) Uani 1 1 d . . . H80A H 0.6219 0.8440 1.0250 0.187 Uiso 1 1 calc R . . H80B H 0.6690 0.8995 0.9857 0.187 Uiso 1 1 calc R . . H80C H 0.6366 0.8070 0.9664 0.187 Uiso 1 1 calc R . . C84 C 0.3957(6) 0.8274(10) 0.9248(5) 0.236(9) Uani 1 1 d . . . H84A H 0.3785 0.8000 0.9579 0.283 Uiso 1 1 calc R . . H84B H 0.4097 0.7781 0.9009 0.283 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 0.0256(17) 0.0321(19) 0.034(2) 0.0016(14) 0.0045(14) -0.0071(15) C2 0.0188(15) 0.0374(18) 0.041(2) -0.0022(17) 0.0052(15) -0.0014(14) C3 0.0245(17) 0.037(2) 0.0347(19) 0.0005(16) -0.0032(14) -0.0047(15) C4 0.0270(18) 0.038(2) 0.036(2) -0.0097(16) 0.0070(15) -0.0115(15) C5 0.0286(17) 0.0305(18) 0.039(2) -0.0008(17) 0.0024(16) -0.0042(14) C6 0.0214(15) 0.0200(16) 0.0276(18) -0.0039(13) 0.0019(13) -0.0007(13) C7 0.0277(17) 0.0286(18) 0.0202(17) 0.0016(14) 0.0028(13) 0.0026(14) C8 0.0329(19) 0.044(2) 0.031(2) -0.0030(17) -0.0015(15) 0.0033(16) C9 0.049(2) 0.059(3) 0.0229(19) -0.0019(17) -0.0026(16) 0.015(2) C10 0.058(2) 0.051(3) 0.034(2) 0.0140(18) 0.0090(19) 0.009(2) C11 0.047(2) 0.036(2) 0.039(2) 0.0080(17) 0.0112(18) -0.0006(18) C12 0.0323(19) 0.0261(18) 0.0316(19) -0.0001(15) 0.0005(15) 0.0016(14) C13 0.0259(18) 0.0288(19) 0.0263(18) -0.0005(13) -0.0019(13) 0.0052(14) C14 0.040(2) 0.0303(19) 0.0310(19) 0.0032(15) 0.0004(15) 0.0027(16) C15 0.058(3) 0.046(2) 0.030(2) 0.0053(18) 0.0028(18) 0.016(2) C16 0.047(2) 0.054(3) 0.032(2) -0.0111(18) -0.0078(17) 0.015(2) C17 0.033(2) 0.062(3) 0.044(2) -0.015(2) -0.0056(17) -0.0024(19) C18 0.0301(18) 0.036(2) 0.0311(19) -0.0024(15) -0.0006(15) -0.0037(15) C19 0.0203(15) 0.0257(17) 0.0251(16) -0.0039(13) -0.0006(13) 0.0008(13) C20 0.0272(17) 0.0296(19) 0.0279(18) -0.0051(14) -0.0007(14) 0.0009(14) C21 0.0287(18) 0.038(2) 0.0311(19) -0.0058(15) -0.0049(14) 0.0125(16) C22 0.0183(16) 0.046(2) 0.044(2) -0.0085(17) 0.0021(15) 0.0010(15) C23 0.0260(16) 0.0282(18) 0.037(2) -0.0056(15) 0.0015(14) -0.0047(14) C24 0.055(2) 0.035(2) 0.035(2) -0.0079(17) -0.0073(18) -0.0060(18) C25 0.0378(19) 0.036(2) 0.0290(19) -0.0063(15) -0.0032(15) 0.0013(16) C26 0.055(3) 0.050(2) 0.0236(19) 0.0026(17) 0.0061(17) -0.0061(19) C27 0.042(2) 0.081(3) 0.037(2) -0.014(2) 0.0116(18) 0.014(2) C28 0.069(3) 0.044(2) 0.035(2) -0.0138(19) -0.002(2) 0.025(2) C29 0.047(2) 0.051(3) 0.054(3) -0.022(2) 0.017(2) -0.018(2) C30 0.036(2) 0.064(3) 0.039(2) 0.009(2) -0.0084(17) -0.0057(19) C31 0.029(2) 0.049(2) 0.057(3) -0.0033(19) 0.0049(18) 0.0104(17) C32 0.044(2) 0.047(2) 0.040(2) 0.0091(19) 0.0047(19) -0.0116(18) C33 0.039(2) 0.0225(19) 0.071(3) -0.0031(19) 0.000(2) -0.0013(16) C34 0.0306(18) 0.0355(19) 0.034(2) -0.0005(16) -0.0010(15) 0.0148(15) C35 0.0238(17) 0.045(2) 0.046(2) -0.0131(18) -0.0088(16) 0.0078(16) C36 0.0189(15) 0.0383(19) 0.051(2) -0.0129(19) 0.0012(17) -0.0013(14) C37 0.0260(17) 0.0331(19) 0.038(2) -0.0064(16) -0.0014(14) 0.0092(15) C38 0.0245(16) 0.0230(16) 0.0389(19) -0.0015(17) -0.0038(15) 0.0077(13) C39 0.0202(15) 0.0174(15) 0.0257(17) 0.0002(12) -0.0046(12) 0.0048(13) C40 0.0289(17) 0.0276(18) 0.0204(16) -0.0021(13) -0.0011(13) -0.0049(14) C41 0.0305(18) 0.0333(19) 0.0296(18) -0.0020(15) 0.0016(14) 0.0041(15) C42 0.039(2) 0.053(2) 0.033(2) 0.0117(18) -0.0093(16) 0.0011(19) C43 0.046(2) 0.051(2) 0.028(2) 0.0054(17) -0.0060(17) -0.0038(18) C44 0.063(3) 0.042(2) 0.0227(19) 0.0003(16) -0.0036(17) -0.002(2) C45 0.045(2) 0.0306(19) 0.0210(17) -0.0005(14) 0.0003(15) 0.0090(16) C46 0.0255(16) 0.0240(16) 0.0245(18) -0.0029(13) -0.0019(13) -0.0010(13) C47 0.0332(18) 0.0300(18) 0.0288(18) -0.0054(14) -0.0056(15) -0.0003(15) C48 0.047(2) 0.048(2) 0.025(2) -0.0061(17) -0.0058(15) -0.0033(18) C49 0.074(3) 0.041(2) 0.031(2) -0.0150(18) 0.007(2) 0.000(2) C50 0.050(2) 0.035(2) 0.038(2) 0.0010(17) 0.0084(18) 0.0143(18) C51 0.0304(19) 0.0294(19) 0.0271(18) -0.0028(15) 0.0015(15) 0.0000(14) C52 0.0268(16) 0.0253(17) 0.0174(15) 0.0030(13) -0.0024(13) 0.0004(13) C53 0.0244(16) 0.0293(18) 0.0276(18) 0.0030(14) -0.0015(13) 0.0054(14) C54 0.0218(17) 0.045(2) 0.0341(19) 0.0114(17) -0.0059(14) -0.0001(15) C55 0.0301(19) 0.036(2) 0.0244(18) 0.0051(15) -0.0053(14) -0.0097(16) C56 0.0338(18) 0.0266(17) 0.0189(16) -0.0011(12) -0.0007(13) -0.0026(14) C57 0.058(2) 0.032(2) 0.0254(19) 0.0060(15) -0.0101(17) 0.0035(18) C58 0.035(2) 0.036(2) 0.0213(17) 0.0060(14) -0.0077(14) -0.0023(16) C59 0.039(2) 0.044(2) 0.0204(18) -0.0011(15) 0.0016(14) -0.0015(17) C60 0.039(2) 0.063(3) 0.029(2) 0.0096(18) 0.0044(16) -0.007(2) C61 0.056(2) 0.037(2) 0.035(2) 0.0129(17) -0.0116(18) -0.0208(19) C62 0.045(2) 0.079(3) 0.064(3) -0.037(3) -0.025(2) 0.018(2) C63 0.061(3) 0.052(3) 0.046(3) 0.016(2) 0.009(2) 0.024(2) C64 0.038(2) 0.0258(19) 0.058(3) 0.0017(18) -0.0077(18) 0.0055(15) C65 0.050(2) 0.042(2) 0.045(2) -0.008(2) 0.011(2) 0.0104(19) C66 0.027(2) 0.057(3) 0.083(3) -0.014(2) 0.010(2) -0.0055(19) Cl1 0.0332(4) 0.0306(5) 0.0379(5) 0.0043(4) 0.0030(4) 0.0092(4) Cl2 0.0396(5) 0.0333(5) 0.0318(5) -0.0071(4) 0.0026(4) 0.0079(4) Cl3 0.0485(5) 0.0318(5) 0.0395(5) 0.0061(4) 0.0090(4) -0.0058(4) Cl4 0.0355(5) 0.0314(5) 0.0544(6) -0.0137(4) 0.0083(4) -0.0109(4) Fe1 0.0240(2) 0.0299(3) 0.0252(2) -0.00300(19) 0.00328(19) 0.0018(2) Fe3 0.0246(2) 0.0270(2) 0.0216(2) 0.00195(19) -0.00030(19) -0.00178(19) N1 0.0217(14) 0.0268(15) 0.0245(14) 0.0028(12) 0.0007(11) 0.0031(12) N2 0.0215(13) 0.0279(15) 0.0251(14) 0.0015(12) 0.0026(11) 0.0027(11) N3 0.0228(13) 0.0245(14) 0.0275(15) -0.0042(12) 0.0007(11) -0.0024(11) N4 0.0218(14) 0.0273(15) 0.0192(14) -0.0017(11) -0.0002(11) 0.0015(11) Zr1 0.02008(14) 0.02294(15) 0.02577(15) -0.00166(15) 0.00162(12) 0.00209(12) Zr2 0.02102(14) 0.02266(15) 0.02955(16) -0.00247(15) 0.00197(13) -0.00158(12) C81 0.104(6) 0.201(9) 0.099(6) 0.061(6) -0.014(4) 0.001(6) C82 0.077(5) 0.260(12) 0.141(8) 0.063(8) 0.026(5) -0.017(7) C83 0.240(13) 0.386(19) 0.067(5) 0.051(8) -0.011(7) -0.221(15) C85 0.44(3) 0.286(17) 0.060(6) 0.005(8) 0.040(11) -0.054(19) C80 0.139(7) 0.115(6) 0.121(6) 0.048(5) 0.003(5) -0.009(5) C84 0.176(11) 0.308(19) 0.224(15) -0.180(14) 0.116(10) -0.132(12) _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 C1 C5 1.407(5) . ? C1 C2 1.423(5) . ? C1 C32 1.494(5) . ? C1 Zr1 2.530(3) . ? C2 C3 1.414(5) . ? C2 C31 1.499(5) . ? C2 Zr1 2.492(3) . ? C3 C4 1.418(5) . ? C3 C30 1.501(5) . ? C3 Zr1 2.508(3) . ? C4 C5 1.415(5) . ? C4 C29 1.504(5) . ? C4 Zr1 2.517(3) . ? C5 C33 1.505(5) . ? C5 Zr1 2.539(3) . ? C6 N1 1.334(4) . ? C6 N2 1.343(4) . ? C6 C19 1.486(4) . ? C7 N2 1.471(4) . ? C7 C8 1.524(5) . ? C7 C12 1.526(5) . ? C8 C9 1.529(5) . ? C9 C10 1.512(6) . ? C10 C11 1.514(6) . ? C11 C12 1.525(5) . ? C13 N1 1.478(4) . ? C13 C14 1.512(5) . ? C13 C18 1.523(5) . ? C14 C15 1.528(5) . ? C15 C16 1.509(6) . ? C16 C17 1.516(6) . ? C17 C18 1.528(5) . ? C19 C23 1.430(5) . ? C19 C20 1.432(5) . ? C19 Fe1 2.065(3) . ? C20 C21 1.413(5) . ? C20 Fe1 2.041(4) . ? C21 C22 1.407(5) . ? C21 Fe1 2.035(3) . ? C22 C23 1.418(5) . ? C22 Fe1 2.038(3) . ? C23 Fe1 2.040(3) . ? C24 C28 1.402(6) . ? C24 C25 1.405(5) . ? C24 Fe1 2.039(4) . ? C25 C26 1.405(5) . ? C25 Fe1 2.052(4) . ? C26 C27 1.420(6) . ? C26 Fe1 2.041(4) . ? C27 C28 1.407(6) . ? C27 Fe1 2.039(4) . ? C28 Fe1 2.038(4) . ? C34 C38 1.416(5) . ? C34 C35 1.423(5) . ? C34 C63 1.502(5) . ? C34 Zr2 2.529(3) . ? C35 C36 1.400(6) . ? C35 C62 1.509(5) . ? C35 Zr2 2.503(4) . ? C36 C37 1.424(5) . ? C36 C66 1.508(5) . ? C36 Zr2 2.480(3) . ? C37 C38 1.417(5) . ? C37 C65 1.492(5) . ? C37 Zr2 2.536(3) . ? C38 C64 1.497(5) . ? C38 Zr2 2.548(3) . ? C39 N3 1.337(4) . ? C39 N4 1.343(4) . ? C39 C52 1.487(4) . ? C40 N4 1.476(4) . ? C40 C45 1.521(5) . ? C40 C41 1.528(5) . ? C41 C42 1.520(5) . ? C42 C43 1.515(5) . ? C43 C44 1.509(6) . ? C44 C45 1.526(5) . ? C46 N3 1.461(4) . ? C46 C47 1.523(4) . ? C46 C51 1.526(5) . ? C47 C48 1.526(5) . ? C48 C49 1.501(6) . ? C49 C50 1.514(6) . ? C50 C51 1.530(5) . ? C52 C53 1.430(4) . ? C52 C56 1.432(5) . ? C52 Fe3 2.071(3) . ? C53 C54 1.412(5) . ? C53 Fe3 2.043(3) . ? C54 C55 1.405(5) . ? C54 Fe3 2.042(3) . ? C55 C56 1.403(5) . ? C55 Fe3 2.033(4) . ? C56 Fe3 2.041(3) . ? C57 C61 1.406(5) . ? C57 C58 1.408(5) . ? C57 Fe3 2.052(4) . ? C58 C59 1.406(5) . ? C58 Fe3 2.055(3) . ? C59 C60 1.416(5) . ? C59 Fe3 2.050(3) . ? C60 C61 1.419(6) . ? C60 Fe3 2.039(4) . ? C61 Fe3 2.036(4) . ? Cl1 Zr1 2.4426(9) . ? Cl2 Zr1 2.4245(9) . ? Cl3 Zr2 2.4252(10) . ? Cl4 Zr2 2.4424(9) . ? N1 Zr1 2.215(2) . ? N2 Zr1 2.217(3) . ? N3 Zr2 2.209(3) . ? N4 Zr2 2.219(2) . ? C81 C80 1.452(10) . ? C81 C82 1.484(12) . ? C82 C83 1.305(14) . ? C83 C84 1.406(13) . ? C85 C84 1.513(18) . ? 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 C5 C1 C2 108.2(3) . . ? C5 C1 C32 126.8(3) . . ? C2 C1 C32 124.8(3) . . ? C5 C1 Zr1 74.25(18) . . ? C2 C1 Zr1 72.09(18) . . ? C32 C1 Zr1 123.7(2) . . ? C3 C2 C1 108.1(3) . . ? C3 C2 C31 126.5(3) . . ? C1 C2 C31 125.3(3) . . ? C3 C2 Zr1 74.19(18) . . ? C1 C2 Zr1 75.01(18) . . ? C31 C2 Zr1 120.1(2) . . ? C2 C3 C4 107.4(3) . . ? C2 C3 C30 126.3(3) . . ? C4 C3 C30 126.1(3) . . ? C2 C3 Zr1 72.96(19) . . ? C4 C3 Zr1 73.96(19) . . ? C30 C3 Zr1 123.0(2) . . ? C5 C4 C3 108.6(3) . . ? C5 C4 C29 123.7(4) . . ? C3 C4 C29 127.0(4) . . ? C5 C4 Zr1 74.61(19) . . ? C3 C4 Zr1 73.3(2) . . ? C29 C4 Zr1 126.2(2) . . ? C1 C5 C4 107.7(3) . . ? C1 C5 C33 127.8(4) . . ? C4 C5 C33 124.0(3) . . ? C1 C5 Zr1 73.52(18) . . ? C4 C5 Zr1 72.88(19) . . ? C33 C5 Zr1 125.6(2) . . ? N1 C6 N2 112.2(3) . . ? N1 C6 C19 121.1(3) . . ? N2 C6 C19 126.7(3) . . ? N2 C7 C8 112.6(3) . . ? N2 C7 C12 110.2(3) . . ? C8 C7 C12 109.5(3) . . ? C7 C8 C9 109.6(3) . . ? C10 C9 C8 112.5(3) . . ? C9 C10 C11 111.2(3) . . ? C10 C11 C12 111.6(3) . . ? C11 C12 C7 111.5(3) . . ? N1 C13 C14 112.7(3) . . ? N1 C13 C18 109.1(3) . . ? C14 C13 C18 110.5(3) . . ? C13 C14 C15 111.5(3) . . ? C16 C15 C14 111.8(3) . . ? C15 C16 C17 110.1(3) . . ? C16 C17 C18 110.6(3) . . ? C13 C18 C17 112.4(3) . . ? C23 C19 C20 106.8(3) . . ? C23 C19 C6 130.3(3) . . ? C20 C19 C6 122.5(3) . . ? C23 C19 Fe1 68.67(18) . . ? C20 C19 Fe1 68.69(18) . . ? C6 C19 Fe1 133.5(2) . . ? C21 C20 C19 108.6(3) . . ? C21 C20 Fe1 69.5(2) . . ? C19 C20 Fe1 70.5(2) . . ? C22 C21 C20 107.9(3) . . ? C22 C21 Fe1 69.9(2) . . ? C20 C21 Fe1 69.96(19) . . ? C21 C22 C23 108.8(3) . . ? C21 C22 Fe1 69.7(2) . . ? C23 C22 Fe1 69.72(19) . . ? C22 C23 C19 107.9(3) . . ? C22 C23 Fe1 69.6(2) . . ? C19 C23 Fe1 70.56(19) . . ? C28 C24 C25 108.4(4) . . ? C28 C24 Fe1 69.9(2) . . ? C25 C24 Fe1 70.4(2) . . ? C26 C25 C24 107.9(4) . . ? C26 C25 Fe1 69.5(2) . . ? C24 C25 Fe1 69.4(2) . . ? C25 C26 C27 108.0(4) . . ? C25 C26 Fe1 70.4(2) . . ? C27 C26 Fe1 69.5(2) . . ? C28 C27 C26 107.5(4) . . ? C28 C27 Fe1 69.8(2) . . ? C26 C27 Fe1 69.7(2) . . ? C24 C28 C27 108.2(4) . . ? C24 C28 Fe1 69.9(2) . . ? C27 C28 Fe1 69.8(2) . . ? C38 C34 C35 107.7(3) . . ? C38 C34 C63 123.1(4) . . ? C35 C34 C63 128.6(4) . . ? C38 C34 Zr2 74.56(18) . . ? C35 C34 Zr2 72.6(2) . . ? C63 C34 Zr2 125.3(2) . . ? C36 C35 C34 108.1(3) . . ? C36 C35 C62 126.3(4) . . ? C34 C35 C62 125.4(4) . . ? C36 C35 Zr2 72.8(2) . . ? C34 C35 Zr2 74.57(19) . . ? C62 C35 Zr2 122.8(3) . . ? C35 C36 C37 108.4(3) . . ? C35 C36 C66 126.2(3) . . ? C37 C36 C66 125.3(4) . . ? C35 C36 Zr2 74.62(19) . . ? C37 C36 Zr2 75.69(18) . . ? C66 C36 Zr2 119.3(3) . . ? C38 C37 C36 107.5(3) . . ? C38 C37 C65 127.2(3) . . ? C36 C37 C65 125.1(4) . . ? C38 C37 Zr2 74.29(18) . . ? C36 C37 Zr2 71.35(18) . . ? C65 C37 Zr2 123.9(3) . . ? C34 C38 C37 108.1(3) . . ? C34 C38 C64 123.9(3) . . ? C37 C38 C64 127.5(3) . . ? C34 C38 Zr2 73.07(18) . . ? C37 C38 Zr2 73.35(18) . . ? C64 C38 Zr2 125.8(2) . . ? N3 C39 N4 112.3(3) . . ? N3 C39 C52 126.5(3) . . ? N4 C39 C52 121.1(3) . . ? N4 C40 C45 111.7(3) . . ? N4 C40 C41 109.3(3) . . ? C45 C40 C41 110.1(3) . . ? C42 C41 C40 112.4(3) . . ? C43 C42 C41 110.9(3) . . ? C44 C43 C42 110.5(3) . . ? C43 C44 C45 111.7(3) . . ? C40 C45 C44 111.6(3) . . ? N3 C46 C47 113.2(3) . . ? N3 C46 C51 110.4(3) . . ? C47 C46 C51 109.6(3) . . ? C46 C47 C48 110.5(3) . . ? C49 C48 C47 111.5(3) . . ? C48 C49 C50 112.0(3) . . ? C49 C50 C51 111.1(3) . . ? C46 C51 C50 111.4(3) . . ? C53 C52 C56 106.8(3) . . ? C53 C52 C39 130.1(3) . . ? C56 C52 C39 122.6(3) . . ? C53 C52 Fe3 68.62(18) . . ? C56 C52 Fe3 68.47(17) . . ? C39 C52 Fe3 133.8(2) . . ? C54 C53 C52 108.0(3) . . ? C54 C53 Fe3 69.74(19) . . ? C52 C53 Fe3 70.71(18) . . ? C55 C54 C53 108.3(3) . . ? C55 C54 Fe3 69.47(19) . . ? C53 C54 Fe3 69.83(18) . . ? C56 C55 C54 108.6(3) . . ? C56 C55 Fe3 70.14(19) . . ? C54 C55 Fe3 70.2(2) . . ? C55 C56 C52 108.2(3) . . ? C55 C56 Fe3 69.56(19) . . ? C52 C56 Fe3 70.77(18) . . ? C61 C57 C58 107.9(3) . . ? C61 C57 Fe3 69.3(2) . . ? C58 C57 Fe3 70.07(19) . . ? C59 C58 C57 108.8(3) . . ? C59 C58 Fe3 69.8(2) . . ? C57 C58 Fe3 69.82(19) . . ? C58 C59 C60 107.4(4) . . ? C58 C59 Fe3 70.2(2) . . ? C60 C59 Fe3 69.3(2) . . ? C59 C60 C61 108.0(3) . . ? C59 C60 Fe3 70.2(2) . . ? C61 C60 Fe3 69.5(2) . . ? C57 C61 C60 107.9(3) . . ? C57 C61 Fe3 70.5(2) . . ? C60 C61 Fe3 69.7(2) . . ? C21 Fe1 C28 102.98(16) . . ? C21 Fe1 C22 40.40(15) . . ? C28 Fe1 C22 121.62(16) . . ? C21 Fe1 C27 115.84(15) . . ? C28 Fe1 C27 40.37(18) . . ? C22 Fe1 C27 105.25(17) . . ? C21 Fe1 C24 122.76(16) . . ? C28 Fe1 C24 40.24(16) . . ? C22 Fe1 C24 158.71(15) . . ? C27 Fe1 C24 67.84(18) . . ? C21 Fe1 C23 68.58(15) . . ? C28 Fe1 C23 160.26(16) . . ? C22 Fe1 C23 40.70(14) . . ? C27 Fe1 C23 125.76(17) . . ? C24 Fe1 C23 159.15(15) . . ? C21 Fe1 C26 152.77(15) . . ? C28 Fe1 C26 67.97(17) . . ? C22 Fe1 C26 121.09(16) . . ? C27 Fe1 C26 40.75(17) . . ? C24 Fe1 C26 67.69(17) . . ? C23 Fe1 C26 110.95(16) . . ? C21 Fe1 C20 40.55(13) . . ? C28 Fe1 C20 117.36(16) . . ? C22 Fe1 C20 67.96(14) . . ? C27 Fe1 C20 150.86(17) . . ? C24 Fe1 C20 107.69(15) . . ? C23 Fe1 C20 68.53(14) . . ? C26 Fe1 C20 166.50(15) . . ? C21 Fe1 C25 161.71(15) . . ? C28 Fe1 C25 67.67(15) . . ? C22 Fe1 C25 157.88(15) . . ? C27 Fe1 C25 67.93(16) . . ? C24 Fe1 C25 40.19(14) . . ? C23 Fe1 C25 125.17(14) . . ? C26 Fe1 C25 40.15(15) . . ? C20 Fe1 C25 128.31(14) . . ? C21 Fe1 C19 68.58(13) . . ? C28 Fe1 C19 154.51(16) . . ? C22 Fe1 C19 68.27(13) . . ? C27 Fe1 C19 165.08(17) . . ? C24 Fe1 C19 123.01(15) . . ? C23 Fe1 C19 40.77(13) . . ? C26 Fe1 C19 130.03(15) . . ? C20 Fe1 C19 40.82(13) . . ? C25 Fe1 C19 112.73(13) . . ? C55 Fe3 C61 102.92(15) . . ? C55 Fe3 C60 116.52(15) . . ? C61 Fe3 C60 40.76(17) . . ? C55 Fe3 C56 40.30(13) . . ? C61 Fe3 C56 117.99(15) . . ? C60 Fe3 C56 151.89(15) . . ? C55 Fe3 C54 40.34(15) . . ? C61 Fe3 C54 120.50(15) . . ? C60 Fe3 C54 104.59(15) . . ? C56 Fe3 C54 67.93(14) . . ? C55 Fe3 C53 68.15(14) . . ? C61 Fe3 C53 158.66(14) . . ? C60 Fe3 C53 124.31(16) . . ? C56 Fe3 C53 68.48(14) . . ? C54 Fe3 C53 40.43(13) . . ? C55 Fe3 C59 153.30(15) . . ? C61 Fe3 C59 68.28(16) . . ? C60 Fe3 C59 40.53(15) . . ? C56 Fe3 C59 166.09(14) . . ? C54 Fe3 C59 120.98(15) . . ? C53 Fe3 C59 110.54(15) . . ? C55 Fe3 C57 122.49(15) . . ? C61 Fe3 C57 40.24(15) . . ? C60 Fe3 C57 67.90(17) . . ? C56 Fe3 C57 108.23(15) . . ? C54 Fe3 C57 157.68(15) . . ? C53 Fe3 C57 160.69(14) . . ? C59 Fe3 C57 67.81(15) . . ? C55 Fe3 C58 161.33(15) . . ? C61 Fe3 C58 67.58(14) . . ? C60 Fe3 C58 67.52(15) . . ? C56 Fe3 C58 128.53(14) . . ? C54 Fe3 C58 158.33(15) . . ? C53 Fe3 C58 126.21(14) . . ? C59 Fe3 C58 40.05(14) . . ? C57 Fe3 C58 40.11(14) . . ? C55 Fe3 C52 68.05(13) . . ? C61 Fe3 C52 155.74(16) . . ? C60 Fe3 C52 163.50(16) . . ? C56 Fe3 C52 40.76(13) . . ? C54 Fe3 C52 67.96(13) . . ? C53 Fe3 C52 40.67(12) . . ? C59 Fe3 C52 129.53(14) . . ? C57 Fe3 C52 124.48(14) . . ? C58 Fe3 C52 113.71(13) . . ? C6 N1 C13 121.0(2) . . ? C6 N1 Zr1 93.97(19) . . ? C13 N1 Zr1 139.1(2) . . ? C6 N2 C7 121.7(3) . . ? C6 N2 Zr1 93.62(19) . . ? C7 N2 Zr1 143.3(2) . . ? C39 N3 C46 121.2(3) . . ? C39 N3 Zr2 93.92(19) . . ? C46 N3 Zr2 143.5(2) . . ? C39 N4 C40 121.6(2) . . ? C39 N4 Zr2 93.32(19) . . ? C40 N4 Zr2 140.6(2) . . ? N1 Zr1 N2 60.18(9) . . ? N1 Zr1 Cl2 91.56(7) . . ? N2 Zr1 Cl2 132.73(7) . . ? N1 Zr1 Cl1 135.95(7) . . ? N2 Zr1 Cl1 87.69(7) . . ? Cl2 Zr1 Cl1 89.80(3) . . ? N1 Zr1 C2 131.81(11) . . ? N2 Zr1 C2 137.18(11) . . ? Cl2 Zr1 C2 90.08(9) . . ? Cl1 Zr1 C2 92.20(8) . . ? N1 Zr1 C3 130.35(11) . . ? N2 Zr1 C3 104.93(11) . . ? Cl2 Zr1 C3 121.73(9) . . ? Cl1 Zr1 C3 84.10(9) . . ? C2 Zr1 C3 32.85(12) . . ? N1 Zr1 C4 97.76(11) . . ? N2 Zr1 C4 85.72(10) . . ? Cl2 Zr1 C4 138.47(8) . . ? Cl1 Zr1 C4 109.81(9) . . ? C2 Zr1 C4 54.21(11) . . ? C3 Zr1 C4 32.77(12) . . ? N1 Zr1 C1 99.40(11) . . ? N2 Zr1 C1 133.23(10) . . ? Cl2 Zr1 C1 84.90(8) . . ? Cl1 Zr1 C1 124.56(8) . . ? C2 Zr1 C1 32.90(11) . . ? C3 Zr1 C1 54.22(11) . . ? C4 Zr1 C1 53.71(11) . . ? N1 Zr1 C5 80.85(10) . . ? N2 Zr1 C5 101.01(10) . . ? Cl2 Zr1 C5 111.52(9) . . ? Cl1 Zr1 C5 138.31(8) . . ? C2 Zr1 C5 54.18(11) . . ? C3 Zr1 C5 54.22(11) . . ? C4 Zr1 C5 32.51(12) . . ? C1 Zr1 C5 32.23(11) . . ? N3 Zr2 N4 60.35(9) . . ? N3 Zr2 Cl3 132.25(7) . . ? N4 Zr2 Cl3 91.43(7) . . ? N3 Zr2 Cl4 87.75(7) . . ? N4 Zr2 Cl4 136.05(7) . . ? Cl3 Zr2 Cl4 89.25(3) . . ? N3 Zr2 C36 136.81(12) . . ? N4 Zr2 C36 131.60(10) . . ? Cl3 Zr2 C36 90.92(10) . . ? Cl4 Zr2 C36 92.32(8) . . ? N3 Zr2 C35 104.76(12) . . ? N4 Zr2 C35 129.99(12) . . ? Cl3 Zr2 C35 122.34(10) . . ? Cl4 Zr2 C35 84.49(9) . . ? C36 Zr2 C35 32.62(13) . . ? N3 Zr2 C34 85.30(11) . . ? N4 Zr2 C34 97.37(11) . . ? Cl3 Zr2 C34 139.40(8) . . ? Cl4 Zr2 C34 110.12(9) . . ? C36 Zr2 C34 54.29(12) . . ? C35 Zr2 C34 32.85(12) . . ? N3 Zr2 C37 133.04(11) . . ? N4 Zr2 C37 99.17(10) . . ? Cl3 Zr2 C37 85.66(9) . . ? Cl4 Zr2 C37 124.67(8) . . ? C36 Zr2 C37 32.95(11) . . ? C35 Zr2 C37 54.05(12) . . ? C34 Zr2 C37 53.84(12) . . ? N3 Zr2 C38 100.70(10) . . ? N4 Zr2 C38 80.61(10) . . ? Cl3 Zr2 C38 112.39(9) . . ? Cl4 Zr2 C38 138.45(8) . . ? C36 Zr2 C38 54.18(11) . . ? C35 Zr2 C38 53.98(11) . . ? C34 Zr2 C38 32.37(11) . . ? C37 Zr2 C38 32.36(11) . . ? C80 C81 C82 114.8(8) . . ? C83 C82 C81 125.7(11) . . ? C82 C83 C84 126.8(15) . . ? C83 C84 C85 113.3(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.521 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.062 #===end data_[CyNC(Fc)NCy]2ZrMe2 _database_code_depnum_ccdc_archive 'CCDC 778599' #TrackingRef '- all-cifs.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C48 H68 Fe2 N4 Zr' _chemical_formula_weight 903.98 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.6543(10) _cell_length_b 11.9951(6) _cell_length_c 19.4642(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4355.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.8809 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36680 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.51 _reflns_number_total 9775 _reflns_number_gt 6316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.55(2) _refine_ls_number_reflns 9775 _refine_ls_number_parameters 498 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 C1 C 0.0477(3) 0.6727(4) 0.7561(3) 0.0182(12) Uani 1 1 d . . . C2 C 0.0297(3) 0.8245(5) 0.5330(3) 0.0230(13) Uani 1 1 d . . . C3 C 0.1027(3) 0.8620(4) 0.7468(3) 0.0201(12) Uani 1 1 d . . . H3 H 0.1234 0.8428 0.7926 0.024 Uiso 1 1 calc R . . C4 C 0.0583(3) 0.9684(5) 0.7537(3) 0.0301(15) Uani 1 1 d . . . H4A H 0.0216 0.9585 0.7899 0.036 Uiso 1 1 calc R . . H4B H 0.0335 0.9843 0.7098 0.036 Uiso 1 1 calc R . . C5 C 0.1081(4) 1.0667(5) 0.7726(4) 0.0445(18) Uani 1 1 d . . . H5A H 0.0792 1.1358 0.7757 0.053 Uiso 1 1 calc R . . H5B H 0.1294 1.0527 0.8184 0.053 Uiso 1 1 calc R . . C6 C 0.1669(4) 1.0838(5) 0.7217(4) 0.0428(18) Uani 1 1 d . . . H6A H 0.1981 1.1460 0.7367 0.051 Uiso 1 1 calc R . . H6B H 0.1464 1.1032 0.6764 0.051 Uiso 1 1 calc R . . C7 C 0.2107(3) 0.9772(5) 0.7160(4) 0.0463(19) Uani 1 1 d . . . H7A H 0.2342 0.9617 0.7606 0.056 Uiso 1 1 calc R . . H7B H 0.2486 0.9872 0.6810 0.056 Uiso 1 1 calc R . . C8 C 0.1633(3) 0.8777(5) 0.6960(3) 0.0358(16) Uani 1 1 d . . . H8A H 0.1431 0.8902 0.6496 0.043 Uiso 1 1 calc R . . H8B H 0.1928 0.8092 0.6945 0.043 Uiso 1 1 calc R . . C9 C -0.0276(3) 0.5048(4) 0.7547(3) 0.0227(12) Uani 1 1 d . . . H9 H 0.0066 0.4801 0.7912 0.027 Uiso 1 1 calc R . . C10 C -0.1009(3) 0.5204(5) 0.7869(3) 0.0281(14) Uani 1 1 d . . . H10A H -0.1335 0.5545 0.7527 0.034 Uiso 1 1 calc R . . H10B H -0.0967 0.5725 0.8261 0.034 Uiso 1 1 calc R . . C11 C -0.1336(3) 0.4101(5) 0.8122(3) 0.0394(17) Uani 1 1 d . . . H11A H -0.1049 0.3808 0.8510 0.047 Uiso 1 1 calc R . . H11B H -0.1830 0.4235 0.8289 0.047 Uiso 1 1 calc R . . C12 C -0.1352(3) 0.3250(6) 0.7549(4) 0.0427(19) Uani 1 1 d . . . H12A H -0.1546 0.2537 0.7725 0.051 Uiso 1 1 calc R . . H12B H -0.1671 0.3515 0.7176 0.051 Uiso 1 1 calc R . . C13 C -0.0611(3) 0.3070(5) 0.7273(3) 0.0374(16) Uani 1 1 d . . . H13A H -0.0626 0.2497 0.6907 0.045 Uiso 1 1 calc R . . H13B H -0.0296 0.2793 0.7645 0.045 Uiso 1 1 calc R . . C14 C -0.0302(3) 0.4144(4) 0.6983(3) 0.0290(14) Uani 1 1 d . . . H14A H -0.0603 0.4406 0.6596 0.035 Uiso 1 1 calc R . . H14B H 0.0187 0.4005 0.6806 0.035 Uiso 1 1 calc R . . C15 C 0.0909(3) 0.6432(4) 0.8182(3) 0.0193(13) Uani 1 1 d . . . C16 C 0.0628(3) 0.6122(4) 0.8833(3) 0.0259(14) Uani 1 1 d . . . H16 H 0.0119 0.5927 0.8937 0.031 Uiso 1 1 calc R . . C17 C 0.1217(3) 0.6141(5) 0.9319(3) 0.0290(15) Uani 1 1 d . . . H17 H 0.1184 0.5970 0.9821 0.035 Uiso 1 1 calc R . . C18 C 0.1842(3) 0.6447(5) 0.8963(3) 0.0296(15) Uani 1 1 d . . . H18 H 0.2331 0.6533 0.9168 0.035 Uiso 1 1 calc R . . C19 C 0.1657(3) 0.6620(4) 0.8260(3) 0.0215(13) Uani 1 1 d . . . H19 H 0.1996 0.6836 0.7886 0.026 Uiso 1 1 calc R . . C20 C 0.2054(3) 0.3940(5) 0.8000(4) 0.0390(17) Uani 1 1 d . . . H20 H 0.2396 0.4156 0.7628 0.047 Uiso 1 1 calc R . . C21 C 0.2219(4) 0.3853(5) 0.8693(4) 0.0421(18) Uani 1 1 d . . . H21 H 0.2701 0.4000 0.8899 0.051 Uiso 1 1 calc R . . C22 C 0.1600(4) 0.3557(5) 0.9064(4) 0.047(2) Uani 1 1 d . . . H22 H 0.1565 0.3428 0.9571 0.057 Uiso 1 1 calc R . . C23 C 0.1040(3) 0.3434(4) 0.8575(4) 0.0381(16) Uani 1 1 d . . . H23 H 0.0535 0.3213 0.8679 0.046 Uiso 1 1 calc R . . C24 C 0.1321(3) 0.3683(5) 0.7908(4) 0.0336(17) Uani 1 1 d . . . H24 H 0.1053 0.3666 0.7463 0.040 Uiso 1 1 calc R . . C25 C -0.0601(3) 0.9752(4) 0.5394(3) 0.0262(13) Uani 1 1 d . . . H25 H -0.0277 1.0109 0.5049 0.031 Uiso 1 1 calc R . . C26 C -0.1285(3) 0.9419(5) 0.5024(3) 0.0307(15) Uani 1 1 d . . . H26A H -0.1611 0.9038 0.5348 0.037 Uiso 1 1 calc R . . H26B H -0.1169 0.8893 0.4648 0.037 Uiso 1 1 calc R . . C27 C -0.1656(3) 1.0447(5) 0.4728(3) 0.0407(17) Uani 1 1 d . . . H27A H -0.1349 1.0783 0.4369 0.049 Uiso 1 1 calc R . . H27B H -0.2113 1.0221 0.4510 0.049 Uiso 1 1 calc R . . C28 C -0.1805(3) 1.1296(5) 0.5272(3) 0.0457(18) Uani 1 1 d . . . H28A H -0.2155 1.0986 0.5603 0.055 Uiso 1 1 calc R . . H28B H -0.2023 1.1963 0.5057 0.055 Uiso 1 1 calc R . . C29 C -0.1139(4) 1.1636(6) 0.5651(4) 0.0460(19) Uani 1 1 d . . . H29A H -0.1268 1.2155 0.6027 0.055 Uiso 1 1 calc R . . H29B H -0.0812 1.2031 0.5333 0.055 Uiso 1 1 calc R . . C30 C -0.0758(3) 1.0613(5) 0.5950(3) 0.0354(15) Uani 1 1 d . . . H30A H -0.0302 1.0848 0.6167 0.042 Uiso 1 1 calc R . . H30B H -0.1063 1.0272 0.6309 0.042 Uiso 1 1 calc R . . C31 C 0.0959(3) 0.6433(4) 0.5365(3) 0.0226(13) Uani 1 1 d . . . H31 H 0.1157 0.6695 0.4916 0.027 Uiso 1 1 calc R . . C32 C 0.0569(3) 0.5354(4) 0.5246(3) 0.0297(14) Uani 1 1 d . . . H32A H 0.0194 0.5469 0.4894 0.036 Uiso 1 1 calc R . . H32B H 0.0330 0.5122 0.5677 0.036 Uiso 1 1 calc R . . C33 C 0.1072(4) 0.4430(5) 0.5010(4) 0.0433(18) Uani 1 1 d . . . H33A H 0.0798 0.3726 0.4963 0.052 Uiso 1 1 calc R . . H33B H 0.1271 0.4623 0.4554 0.052 Uiso 1 1 calc R . . C34 C 0.1675(3) 0.4262(5) 0.5510(4) 0.0390(17) Uani 1 1 d . . . H34A H 0.2009 0.3693 0.5327 0.047 Uiso 1 1 calc R . . H34B H 0.1480 0.3983 0.5951 0.047 Uiso 1 1 calc R . . C35 C 0.2082(3) 0.5345(5) 0.5636(4) 0.0408(18) Uani 1 1 d . . . H35A H 0.2333 0.5570 0.5210 0.049 Uiso 1 1 calc R . . H35B H 0.2447 0.5224 0.5998 0.049 Uiso 1 1 calc R . . C36 C 0.1573(3) 0.6275(5) 0.5859(3) 0.0330(16) Uani 1 1 d . . . H36A H 0.1379 0.6098 0.6320 0.040 Uiso 1 1 calc R . . H36B H 0.1845 0.6981 0.5895 0.040 Uiso 1 1 calc R . . C37 C 0.0662(3) 0.8628(4) 0.4693(3) 0.0231(13) Uani 1 1 d . . . C38 C 0.0351(3) 0.8951(4) 0.4040(3) 0.0273(14) Uani 1 1 d . . . H38 H -0.0171 0.9064 0.3944 0.033 Uiso 1 1 calc R . . C39 C 0.0911(3) 0.9071(5) 0.3567(3) 0.0319(15) Uani 1 1 d . . . H39 H 0.0855 0.9285 0.3074 0.038 Uiso 1 1 calc R . . C40 C 0.1566(3) 0.8850(5) 0.3899(3) 0.0298(15) Uani 1 1 d . . . H40 H 0.2052 0.8870 0.3681 0.036 Uiso 1 1 calc R . . C41 C 0.1415(3) 0.8581(5) 0.4595(3) 0.0281(14) Uani 1 1 d . . . H41 H 0.1778 0.8392 0.4954 0.034 Uiso 1 1 calc R . . C42 C 0.1644(4) 1.1264(5) 0.4920(4) 0.051(2) Uani 1 1 d . . . H42 H 0.2030 1.1074 0.5256 0.061 Uiso 1 1 calc R . . C43 C 0.1743(4) 1.1470(5) 0.4204(5) 0.054(2) Uani 1 1 d . . . H43 H 0.2208 1.1455 0.3948 0.065 Uiso 1 1 calc R . . C44 C 0.1059(5) 1.1700(5) 0.3926(4) 0.057(2) Uani 1 1 d . . . H44 H 0.0957 1.1865 0.3432 0.069 Uiso 1 1 calc R . . C45 C 0.0543(4) 1.1646(5) 0.4450(4) 0.0425(17) Uani 1 1 d . . . H45 H 0.0017 1.1776 0.4397 0.051 Uiso 1 1 calc R . . C46 C 0.0908(4) 1.1381(5) 0.5074(4) 0.0423(18) Uani 1 1 d . . . H46 H 0.0682 1.1288 0.5536 0.051 Uiso 1 1 calc R . . C47 C -0.1176(3) 0.6286(5) 0.6027(4) 0.0346(16) Uani 1 1 d . . . H47A H -0.0943 0.5700 0.5757 0.052 Uiso 1 1 calc R . . H47B H -0.1495 0.6720 0.5730 0.052 Uiso 1 1 calc R . . H47C H -0.1456 0.5945 0.6398 0.052 Uiso 1 1 calc R . . C48 C -0.1228(3) 0.8389(6) 0.7010(3) 0.0349(17) Uani 1 1 d . . . H48A H -0.1612 0.8536 0.6679 0.052 Uiso 1 1 calc R . . H48B H -0.1041 0.9097 0.7185 0.052 Uiso 1 1 calc R . . H48C H -0.1419 0.7947 0.7393 0.052 Uiso 1 1 calc R . . Fe1 Fe 0.14270(4) 0.50256(7) 0.85608(4) 0.02457(19) Uani 1 1 d . . . Fe2 Fe 0.10617(5) 1.01491(7) 0.43590(4) 0.0325(2) Uani 1 1 d . . . N1 N 0.0553(3) 0.7711(4) 0.7247(3) 0.0209(11) Uani 1 1 d . . . N2 N -0.0020(2) 0.6102(4) 0.7262(2) 0.0223(11) Uani 1 1 d . . . N3 N -0.0223(2) 0.8772(4) 0.5675(2) 0.0250(11) Uani 1 1 d . . . N4 N 0.0457(2) 0.7281(4) 0.5621(3) 0.0206(11) Uani 1 1 d . . . Zr1 Zr -0.03299(2) 0.74256(4) 0.64847(4) 0.02059(11) 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 0.021(3) 0.015(3) 0.019(3) -0.001(2) 0.002(2) -0.005(2) C2 0.024(3) 0.018(3) 0.026(3) -0.001(3) -0.003(3) -0.007(3) C3 0.020(3) 0.011(3) 0.030(3) -0.001(2) -0.004(3) -0.007(2) C4 0.026(3) 0.022(3) 0.041(4) 0.000(3) 0.006(3) 0.001(3) C5 0.052(4) 0.018(3) 0.064(5) -0.002(3) 0.003(4) -0.003(3) C6 0.049(4) 0.029(4) 0.051(5) -0.005(3) 0.002(4) -0.018(3) C7 0.036(4) 0.045(5) 0.058(5) -0.013(4) 0.017(3) -0.027(3) C8 0.041(4) 0.024(3) 0.043(4) -0.013(3) 0.008(3) -0.013(3) C9 0.020(3) 0.016(3) 0.032(3) 0.001(2) -0.001(2) -0.010(2) C10 0.020(3) 0.022(3) 0.042(4) 0.000(3) 0.006(3) -0.003(3) C11 0.030(3) 0.047(4) 0.041(4) 0.014(3) 0.007(3) -0.006(3) C12 0.044(4) 0.031(4) 0.053(5) 0.007(3) -0.015(4) -0.018(3) C13 0.043(4) 0.024(3) 0.045(4) -0.001(3) -0.007(3) -0.008(3) C14 0.037(3) 0.020(3) 0.031(3) 0.000(3) -0.003(3) -0.002(3) C15 0.022(3) 0.014(3) 0.022(3) -0.006(2) 0.000(2) 0.001(2) C16 0.030(3) 0.017(3) 0.031(4) 0.001(3) 0.003(3) 0.006(3) C17 0.047(4) 0.022(3) 0.018(3) -0.004(3) -0.002(3) 0.008(3) C18 0.030(3) 0.020(3) 0.039(4) -0.004(3) -0.012(3) 0.000(3) C19 0.022(3) 0.014(3) 0.028(3) 0.005(2) -0.003(3) 0.000(2) C20 0.030(3) 0.021(3) 0.066(5) -0.009(3) 0.002(3) 0.010(3) C21 0.042(4) 0.024(3) 0.060(5) -0.001(3) -0.014(4) 0.015(3) C22 0.069(5) 0.022(4) 0.050(5) 0.011(3) -0.012(4) 0.012(4) C23 0.038(4) 0.014(3) 0.062(5) -0.001(3) 0.002(4) -0.003(3) C24 0.046(4) 0.021(3) 0.035(4) -0.014(3) -0.001(3) 0.010(3) C25 0.029(3) 0.022(3) 0.027(3) 0.002(3) -0.001(3) 0.004(3) C26 0.025(3) 0.032(4) 0.035(4) 0.007(3) -0.005(3) 0.009(3) C27 0.039(4) 0.036(4) 0.046(4) 0.009(3) -0.009(3) 0.005(3) C28 0.043(4) 0.046(4) 0.048(4) 0.021(4) -0.005(3) 0.018(3) C29 0.062(5) 0.037(4) 0.039(4) -0.005(3) -0.007(4) 0.016(4) C30 0.047(4) 0.026(3) 0.033(4) 0.000(3) -0.007(3) 0.013(3) C31 0.030(3) 0.015(3) 0.022(3) -0.002(2) 0.005(3) 0.001(3) C32 0.033(3) 0.021(3) 0.035(4) -0.007(3) 0.001(3) 0.008(3) C33 0.058(4) 0.018(3) 0.053(5) -0.009(3) -0.005(4) 0.004(3) C34 0.044(4) 0.022(3) 0.052(5) 0.000(3) 0.012(4) 0.015(3) C35 0.031(4) 0.043(4) 0.048(4) 0.005(3) 0.003(3) 0.015(3) C36 0.033(4) 0.025(3) 0.041(4) -0.011(3) -0.004(3) 0.006(3) C37 0.029(3) 0.013(3) 0.027(3) 0.000(2) -0.001(3) 0.000(3) C38 0.041(4) 0.018(3) 0.023(3) 0.003(2) -0.007(3) 0.003(3) C39 0.044(4) 0.024(3) 0.028(3) 0.004(3) -0.002(3) 0.002(3) C40 0.034(4) 0.022(3) 0.033(4) -0.001(3) 0.011(3) -0.002(3) C41 0.037(3) 0.018(3) 0.029(4) 0.001(3) -0.006(3) -0.001(3) C42 0.059(5) 0.017(3) 0.076(6) -0.009(4) 0.007(4) -0.017(3) C43 0.050(5) 0.020(4) 0.094(7) -0.005(4) 0.022(5) -0.013(3) C44 0.105(7) 0.014(4) 0.053(5) 0.008(3) 0.019(5) -0.006(4) C45 0.059(4) 0.017(3) 0.051(5) -0.001(3) 0.005(4) 0.001(3) C46 0.050(4) 0.019(4) 0.058(5) -0.008(3) -0.005(4) -0.004(3) C47 0.035(4) 0.036(4) 0.033(4) 0.007(3) -0.007(3) -0.010(3) C48 0.028(4) 0.038(4) 0.039(4) 0.005(3) 0.002(3) 0.010(3) Fe1 0.0298(4) 0.0162(4) 0.0276(5) -0.0002(4) -0.0028(4) 0.0044(4) Fe2 0.0456(5) 0.0162(4) 0.0358(6) 0.0006(4) 0.0021(5) -0.0051(4) N1 0.023(2) 0.015(2) 0.025(3) 0.003(2) 0.001(2) -0.003(2) N2 0.026(3) 0.017(2) 0.024(3) 0.002(2) -0.009(2) -0.001(2) N3 0.032(3) 0.019(3) 0.024(3) 0.008(2) 0.000(2) 0.012(2) N4 0.028(3) 0.014(2) 0.020(3) -0.001(2) 0.003(2) 0.002(2) Zr1 0.01966(19) 0.0191(2) 0.0231(2) 0.0014(3) -0.0021(3) 0.0008(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 C1 N2 1.327(6) . ? C1 N1 1.337(7) . ? C1 C15 1.494(8) . ? C2 N4 1.322(7) . ? C2 N3 1.337(7) . ? C2 C37 1.488(8) . ? C3 N1 1.469(7) . ? C3 C8 1.512(8) . ? C3 C4 1.527(7) . ? C4 C5 1.546(8) . ? C5 C6 1.491(9) . ? C6 C7 1.521(9) . ? C7 C8 1.535(8) . ? C9 N2 1.461(6) . ? C9 C10 1.515(7) . ? C9 C14 1.545(7) . ? C10 C11 1.539(8) . ? C11 C12 1.511(9) . ? C12 C13 1.500(8) . ? C13 C14 1.519(7) . ? C15 C16 1.421(8) . ? C15 C19 1.422(7) . ? C15 Fe1 2.080(5) . ? C16 C17 1.450(8) . ? C16 Fe1 2.056(5) . ? C17 C18 1.404(8) . ? C17 Fe1 2.030(6) . ? C18 C19 1.426(8) . ? C18 Fe1 2.030(6) . ? C19 Fe1 2.045(5) . ? C20 C21 1.387(9) . ? C20 C24 1.413(8) . ? C20 Fe1 2.063(6) . ? C21 C22 1.408(10) . ? C21 Fe1 2.056(6) . ? C22 C23 1.421(10) . ? C22 Fe1 2.041(6) . ? C23 C24 1.431(10) . ? C23 Fe1 2.041(6) . ? C24 Fe1 2.061(6) . ? C25 N3 1.476(7) . ? C25 C26 1.518(7) . ? C25 C30 1.525(8) . ? C26 C27 1.527(8) . ? C27 C28 1.494(9) . ? C28 C29 1.501(8) . ? C29 C30 1.534(8) . ? C31 N4 1.469(7) . ? C31 C32 1.502(7) . ? C31 C36 1.508(8) . ? C32 C33 1.522(8) . ? C33 C34 1.500(9) . ? C34 C35 1.524(8) . ? C35 C36 1.528(8) . ? C37 C41 1.419(7) . ? C37 C38 1.450(8) . ? C37 Fe2 2.075(5) . ? C38 C39 1.399(8) . ? C38 Fe2 2.052(6) . ? C39 C40 1.408(8) . ? C39 Fe2 2.032(6) . ? C40 C41 1.421(8) . ? C40 Fe2 2.030(6) . ? C41 Fe2 2.045(6) . ? C42 C46 1.412(9) . ? C42 C43 1.428(10) . ? C42 Fe2 2.039(7) . ? C43 C44 1.413(10) . ? C43 Fe2 2.054(6) . ? C44 C45 1.403(9) . ? C44 Fe2 2.042(7) . ? C45 C46 1.428(9) . ? C45 Fe2 2.047(6) . ? C46 Fe2 2.050(6) . ? C47 Zr1 2.270(6) . ? C48 Zr1 2.278(6) . ? N1 Zr1 2.242(5) . ? N2 Zr1 2.268(4) . ? N3 Zr1 2.265(5) . ? N4 Zr1 2.238(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 111.8(5) . . ? N2 C1 C15 126.7(5) . . ? N1 C1 C15 121.5(5) . . ? N4 C2 N3 111.3(5) . . ? N4 C2 C37 121.6(5) . . ? N3 C2 C37 127.1(5) . . ? N1 C3 C8 110.6(5) . . ? N1 C3 C4 108.6(4) . . ? C8 C3 C4 111.0(5) . . ? C3 C4 C5 109.4(5) . . ? C6 C5 C4 112.9(6) . . ? C5 C6 C7 109.1(5) . . ? C6 C7 C8 111.3(5) . . ? C3 C8 C7 111.2(5) . . ? N2 C9 C10 110.3(4) . . ? N2 C9 C14 110.3(5) . . ? C10 C9 C14 110.6(4) . . ? C9 C10 C11 112.6(5) . . ? C12 C11 C10 110.6(5) . . ? C13 C12 C11 110.1(5) . . ? C12 C13 C14 111.2(5) . . ? C13 C14 C9 110.1(5) . . ? C16 C15 C19 107.8(5) . . ? C16 C15 C1 125.8(5) . . ? C19 C15 C1 125.3(5) . . ? C16 C15 Fe1 69.0(3) . . ? C19 C15 Fe1 68.5(3) . . ? C1 C15 Fe1 136.8(4) . . ? C15 C16 C17 107.4(5) . . ? C15 C16 Fe1 70.8(3) . . ? C17 C16 Fe1 68.2(3) . . ? C18 C17 C16 108.1(6) . . ? C18 C17 Fe1 69.8(3) . . ? C16 C17 Fe1 70.2(3) . . ? C17 C18 C19 108.1(5) . . ? C17 C18 Fe1 69.8(3) . . ? C19 C18 Fe1 70.1(3) . . ? C15 C19 C18 108.5(5) . . ? C15 C19 Fe1 71.2(3) . . ? C18 C19 Fe1 68.9(3) . . ? C21 C20 C24 108.7(6) . . ? C21 C20 Fe1 70.0(4) . . ? C24 C20 Fe1 69.9(3) . . ? C20 C21 C22 109.6(6) . . ? C20 C21 Fe1 70.6(3) . . ? C22 C21 Fe1 69.3(4) . . ? C21 C22 C23 106.5(7) . . ? C21 C22 Fe1 70.5(4) . . ? C23 C22 Fe1 69.6(3) . . ? C22 C23 C24 108.5(6) . . ? C22 C23 Fe1 69.6(3) . . ? C24 C23 Fe1 70.3(3) . . ? C20 C24 C23 106.5(6) . . ? C20 C24 Fe1 70.0(4) . . ? C23 C24 Fe1 68.9(4) . . ? N3 C25 C26 111.6(5) . . ? N3 C25 C30 111.6(5) . . ? C26 C25 C30 110.7(5) . . ? C25 C26 C27 110.4(5) . . ? C28 C27 C26 111.5(5) . . ? C27 C28 C29 112.3(5) . . ? C28 C29 C30 110.7(6) . . ? C25 C30 C29 111.2(5) . . ? N4 C31 C32 109.9(4) . . ? N4 C31 C36 110.8(5) . . ? C32 C31 C36 110.9(5) . . ? C31 C32 C33 112.1(5) . . ? C34 C33 C32 111.3(6) . . ? C33 C34 C35 111.4(5) . . ? C34 C35 C36 111.0(5) . . ? C31 C36 C35 112.5(5) . . ? C41 C37 C38 106.8(5) . . ? C41 C37 C2 123.6(5) . . ? C38 C37 C2 129.1(5) . . ? C41 C37 Fe2 68.7(3) . . ? C38 C37 Fe2 68.6(3) . . ? C2 C37 Fe2 134.2(4) . . ? C39 C38 C37 107.8(5) . . ? C39 C38 Fe2 69.2(3) . . ? C37 C38 Fe2 70.3(3) . . ? C38 C39 C40 109.1(6) . . ? C38 C39 Fe2 70.8(4) . . ? C40 C39 Fe2 69.6(3) . . ? C39 C40 C41 107.9(5) . . ? C39 C40 Fe2 69.8(3) . . ? C41 C40 Fe2 70.2(3) . . ? C37 C41 C40 108.4(5) . . ? C37 C41 Fe2 71.0(3) . . ? C40 C41 Fe2 69.0(3) . . ? C46 C42 C43 108.5(7) . . ? C46 C42 Fe2 70.2(4) . . ? C43 C42 Fe2 70.1(4) . . ? C44 C43 C42 106.8(7) . . ? C44 C43 Fe2 69.4(4) . . ? C42 C43 Fe2 69.0(4) . . ? C45 C44 C43 109.4(7) . . ? C45 C44 Fe2 70.1(4) . . ? C43 C44 Fe2 70.3(4) . . ? C44 C45 C46 107.5(7) . . ? C44 C45 Fe2 69.7(4) . . ? C46 C45 Fe2 69.7(4) . . ? C42 C46 C45 107.7(7) . . ? C42 C46 Fe2 69.4(4) . . ? C45 C46 Fe2 69.5(4) . . ? C17 Fe1 C18 40.5(2) . . ? C17 Fe1 C22 104.5(3) . . ? C18 Fe1 C22 118.6(3) . . ? C17 Fe1 C23 122.6(3) . . ? C18 Fe1 C23 156.3(3) . . ? C22 Fe1 C23 40.7(3) . . ? C17 Fe1 C19 68.4(2) . . ? C18 Fe1 C19 41.0(2) . . ? C22 Fe1 C19 155.6(3) . . ? C23 Fe1 C19 162.3(3) . . ? C17 Fe1 C21 119.9(3) . . ? C18 Fe1 C21 104.6(3) . . ? C22 Fe1 C21 40.2(3) . . ? C23 Fe1 C21 67.2(3) . . ? C19 Fe1 C21 121.7(3) . . ? C17 Fe1 C16 41.6(2) . . ? C18 Fe1 C16 68.9(2) . . ? C22 Fe1 C16 122.8(3) . . ? C23 Fe1 C16 109.8(2) . . ? C19 Fe1 C16 68.1(2) . . ? C21 Fe1 C16 157.8(3) . . ? C17 Fe1 C24 160.9(2) . . ? C18 Fe1 C24 158.6(3) . . ? C22 Fe1 C24 68.7(3) . . ? C23 Fe1 C24 40.8(3) . . ? C19 Fe1 C24 125.1(3) . . ? C21 Fe1 C24 67.1(3) . . ? C16 Fe1 C24 126.1(2) . . ? C17 Fe1 C20 155.5(2) . . ? C18 Fe1 C20 121.2(2) . . ? C22 Fe1 C20 67.7(3) . . ? C23 Fe1 C20 67.5(3) . . ? C19 Fe1 C20 108.7(2) . . ? C21 Fe1 C20 39.4(2) . . ? C16 Fe1 C20 161.9(3) . . ? C24 Fe1 C20 40.1(2) . . ? C17 Fe1 C15 68.5(2) . . ? C18 Fe1 C15 68.5(2) . . ? C22 Fe1 C15 160.7(3) . . ? C23 Fe1 C15 126.8(2) . . ? C19 Fe1 C15 40.3(2) . . ? C21 Fe1 C15 159.0(3) . . ? C16 Fe1 C15 40.2(2) . . ? C24 Fe1 C15 111.7(2) . . ? C20 Fe1 C15 126.0(3) . . ? C40 Fe2 C39 40.6(2) . . ? C40 Fe2 C42 119.5(3) . . ? C39 Fe2 C42 153.8(3) . . ? C40 Fe2 C44 121.2(3) . . ? C39 Fe2 C44 105.5(3) . . ? C42 Fe2 C44 68.0(3) . . ? C40 Fe2 C41 40.8(2) . . ? C39 Fe2 C41 68.2(2) . . ? C42 Fe2 C41 108.1(3) . . ? C44 Fe2 C41 158.6(3) . . ? C40 Fe2 C45 158.6(3) . . ? C39 Fe2 C45 124.0(3) . . ? C42 Fe2 C45 68.3(3) . . ? C44 Fe2 C45 40.1(3) . . ? C41 Fe2 C45 160.0(3) . . ? C40 Fe2 C46 156.7(3) . . ? C39 Fe2 C46 162.7(3) . . ? C42 Fe2 C46 40.4(2) . . ? C44 Fe2 C46 67.9(3) . . ? C41 Fe2 C46 123.8(3) . . ? C45 Fe2 C46 40.8(3) . . ? C40 Fe2 C38 68.2(2) . . ? C39 Fe2 C38 40.1(2) . . ? C42 Fe2 C38 164.9(3) . . ? C44 Fe2 C38 120.8(3) . . ? C41 Fe2 C38 68.4(2) . . ? C45 Fe2 C38 109.6(3) . . ? C46 Fe2 C38 128.3(3) . . ? C40 Fe2 C43 103.9(3) . . ? C39 Fe2 C43 117.7(3) . . ? C42 Fe2 C43 40.8(3) . . ? C44 Fe2 C43 40.4(3) . . ? C41 Fe2 C43 122.9(3) . . ? C45 Fe2 C43 68.2(3) . . ? C46 Fe2 C43 68.3(3) . . ? C38 Fe2 C43 153.6(3) . . ? C40 Fe2 C37 68.3(2) . . ? C39 Fe2 C37 68.2(2) . . ? C42 Fe2 C37 126.9(3) . . ? C44 Fe2 C37 158.3(3) . . ? C41 Fe2 C37 40.3(2) . . ? C45 Fe2 C37 125.1(2) . . ? C46 Fe2 C37 111.8(3) . . ? C38 Fe2 C37 41.1(2) . . ? C43 Fe2 C37 161.2(3) . . ? C1 N1 C3 125.8(5) . . ? C1 N1 Zr1 95.2(3) . . ? C3 N1 Zr1 138.6(4) . . ? C1 N2 C9 123.4(5) . . ? C1 N2 Zr1 94.3(3) . . ? C9 N2 Zr1 140.9(3) . . ? C2 N3 C25 122.5(5) . . ? C2 N3 Zr1 94.4(3) . . ? C25 N3 Zr1 141.6(4) . . ? C2 N4 C31 127.2(5) . . ? C2 N4 Zr1 96.0(4) . . ? C31 N4 Zr1 136.6(4) . . ? N4 Zr1 N1 91.57(15) . . ? N4 Zr1 N3 58.33(17) . . ? N1 Zr1 N3 106.65(17) . . ? N4 Zr1 N2 106.20(17) . . ? N1 Zr1 N2 58.57(16) . . ? N3 Zr1 N2 160.14(15) . . ? N4 Zr1 C47 96.6(2) . . ? N1 Zr1 C47 149.5(2) . . ? N3 Zr1 C47 102.6(2) . . ? N2 Zr1 C47 91.0(2) . . ? N4 Zr1 C48 149.2(2) . . ? N1 Zr1 C48 99.5(2) . . ? N3 Zr1 C48 90.9(2) . . ? N2 Zr1 C48 104.1(2) . . ? C47 Zr1 C48 88.3(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.662 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.091 #===end