# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Haiyan Ma' _publ_contact_author_email HAIYANMA@ECUST.EDU.CN _publ_section_title ; Zirconium and Hafnium Complexes Supported by Linked Bis(?-diketiminate) Ligands: Synthesis, Characterization, and Catalytic Application in Ethylene Polymerization ; loop_ _publ_author_name 'Haiyan Ma' 'Shaogang Gong' 'Jiling Huang' # Attachment 'Gong-Dalton-Zr-revise-2009-6-19.cif' #============================================================================== data_cd27456 _database_code_depnum_ccdc_archive 'CCDC 724272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H56 Cl2 N4 Zr' _chemical_formula_weight 749.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 11.4820(11) _cell_length_b 31.485(3) _cell_length_c 11.7046(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.609(2) _cell_angle_gamma 90.00 _cell_volume 3933.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1850 _cell_measurement_theta_min 4.550 _cell_measurement_theta_max 51.730 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.498 _exptl_crystal_size_mid 0.419 _exptl_crystal_size_min 0.347 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1580 _exptl_absorpt_coefficient_mu 0.447 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75156 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22563 _diffrn_reflns_av_R_equivalents 0.0853 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8553 _reflns_number_gt 6286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00053(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8553 _refine_ls_number_parameters 446 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.50343(3) 0.124973(10) 0.17753(3) 0.02688(11) Uani 1 1 d . . . Cl1 Cl 0.50258(10) 0.20013(3) 0.13224(8) 0.0447(2) Uani 1 1 d . . . Cl2 Cl 0.66270(8) 0.08157(3) 0.14579(8) 0.0453(2) Uani 1 1 d . . . N1 N 0.3947(3) 0.11891(8) -0.0320(2) 0.0322(6) Uani 1 1 d . . . N2 N 0.3893(3) 0.06885(9) 0.1670(2) 0.0348(7) Uani 1 1 d . . . N3 N 0.6629(2) 0.14123(9) 0.3628(2) 0.0315(6) Uani 1 1 d . . . N4 N 0.4020(3) 0.13534(9) 0.2996(2) 0.0351(7) Uani 1 1 d . . . C1 C 0.3676(3) 0.08113(11) -0.0878(3) 0.0378(8) Uani 1 1 d . . . C2 C 0.3794(3) 0.04225(11) -0.0269(3) 0.0377(8) Uani 1 1 d . . . H2 H 0.3891 0.0182 -0.0686 0.045 Uiso 1 1 calc R . . C3 C 0.3778(3) 0.03635(11) 0.0888(3) 0.0378(8) Uani 1 1 d . . . C4 C 0.3092(4) 0.07774(13) -0.2267(3) 0.0601(12) Uani 1 1 d . . . H4A H 0.2196 0.0791 -0.2525 0.090 Uiso 1 1 calc R . . H4B H 0.3327 0.0512 -0.2525 0.090 Uiso 1 1 calc R . . H4C H 0.3382 0.1007 -0.2631 0.090 Uiso 1 1 calc R . . C5 C 0.3580(4) -0.00789(12) 0.1249(4) 0.0540(11) Uani 1 1 d . . . H5A H 0.4171 -0.0138 0.2059 0.081 Uiso 1 1 calc R . . H5B H 0.3696 -0.0277 0.0677 0.081 Uiso 1 1 calc R . . H5C H 0.2744 -0.0105 0.1242 0.081 Uiso 1 1 calc R . . C6 C 0.6490(3) 0.17071(11) 0.4395(3) 0.0337(8) Uani 1 1 d . . . C7 C 0.5331(3) 0.18813(11) 0.4286(3) 0.0370(8) Uani 1 1 d . . . H7 H 0.5340 0.2151 0.4612 0.044 Uiso 1 1 calc R . . C8 C 0.4181(3) 0.16906(11) 0.3743(3) 0.0354(8) Uani 1 1 d . . . C9 C 0.7586(4) 0.18567(14) 0.5498(3) 0.0547(11) Uani 1 1 d . . . H9A H 0.7525 0.1740 0.6232 0.082 Uiso 1 1 calc R . . H9B H 0.7577 0.2161 0.5539 0.082 Uiso 1 1 calc R . . H9C H 0.8353 0.1765 0.5426 0.082 Uiso 1 1 calc R . . C10 C 0.3119(4) 0.18566(14) 0.4069(4) 0.0553(11) Uani 1 1 d . . . H10A H 0.2363 0.1855 0.3352 0.083 Uiso 1 1 calc R . . H10B H 0.3302 0.2142 0.4373 0.083 Uiso 1 1 calc R . . H10C H 0.3014 0.1680 0.4692 0.083 Uiso 1 1 calc R . . C11 C 0.2974(3) 0.10626(13) 0.2879(4) 0.0488(10) Uani 1 1 d . . . H11A H 0.2222 0.1150 0.2206 0.059 Uiso 1 1 calc R . . H11B H 0.2802 0.1061 0.3631 0.059 Uiso 1 1 calc R . . C12 C 0.3381(4) 0.06344(12) 0.2637(3) 0.0452(9) Uani 1 1 d . . . H12A H 0.4015 0.0521 0.3376 0.054 Uiso 1 1 calc R . . H12B H 0.2675 0.0440 0.2370 0.054 Uiso 1 1 calc R . . C14 C 0.3515(4) 0.15504(11) -0.1141(3) 0.0378(9) Uani 1 1 d . . . C15 C 0.2286(4) 0.16826(11) -0.1455(3) 0.0450(10) Uani 1 1 d . . . C16 C 0.1856(5) 0.20105(14) -0.2305(4) 0.0660(13) Uani 1 1 d . . . H16 H 0.1031 0.2102 -0.2532 0.079 Uiso 1 1 calc R . . C17 C 0.2619(6) 0.22000(15) -0.2813(4) 0.0778(16) Uani 1 1 d . . . H17 H 0.2311 0.2418 -0.3382 0.093 Uiso 1 1 calc R . . C18 C 0.3836(5) 0.20708(14) -0.2488(4) 0.0674(14) Uani 1 1 d . . . H18 H 0.4345 0.2202 -0.2843 0.081 Uiso 1 1 calc R . . C19 C 0.4331(4) 0.17453(12) -0.1632(3) 0.0491(10) Uani 1 1 d . . . C20 C 0.1419(4) 0.14920(13) -0.0891(4) 0.0532(11) Uani 1 1 d . . . H20 H 0.1767 0.1217 -0.0539 0.064 Uiso 1 1 calc R . . C21 C 0.1370(4) 0.17749(16) 0.0161(4) 0.0743(14) Uani 1 1 d . . . H21A H 0.2200 0.1809 0.0763 0.111 Uiso 1 1 calc R . . H21B H 0.0845 0.1644 0.0538 0.111 Uiso 1 1 calc R . . H21C H 0.1034 0.2048 -0.0159 0.111 Uiso 1 1 calc R . . C22 C 0.0086(4) 0.14148(19) -0.1832(5) 0.0883(17) Uani 1 1 d . . . H22A H -0.0294 0.1682 -0.2162 0.132 Uiso 1 1 calc R . . H22B H -0.0407 0.1275 -0.1436 0.132 Uiso 1 1 calc R . . H22C H 0.0128 0.1239 -0.2487 0.132 Uiso 1 1 calc R . . C23 C 0.5689(5) 0.16178(14) -0.1282(4) 0.0611(12) Uani 1 1 d . . . H23 H 0.5952 0.1483 -0.0472 0.073 Uiso 1 1 calc R . . C24 C 0.5889(7) 0.12973(18) -0.2156(7) 0.120(3) Uani 1 1 d . . . H24A H 0.5401 0.1048 -0.2179 0.180 Uiso 1 1 calc R . . H24B H 0.6760 0.1222 -0.1879 0.180 Uiso 1 1 calc R . . H24C H 0.5633 0.1418 -0.2964 0.180 Uiso 1 1 calc R . . C25 C 0.6561(5) 0.19908(17) -0.1175(6) 0.0916(17) Uani 1 1 d . . . H25A H 0.6300 0.2141 -0.1942 0.137 Uiso 1 1 calc R . . H25B H 0.7401 0.1889 -0.0974 0.137 Uiso 1 1 calc R . . H25C H 0.6534 0.2179 -0.0539 0.137 Uiso 1 1 calc R . . C26 C 0.7865(3) 0.12165(12) 0.4003(3) 0.0380(8) Uani 1 1 d . . . C27 C 0.8821(3) 0.14185(14) 0.3750(4) 0.0509(10) Uani 1 1 d . . . C28 C 0.9983(4) 0.12245(17) 0.4147(5) 0.0689(13) Uani 1 1 d . . . H28 H 1.0640 0.1356 0.4002 0.083 Uiso 1 1 calc R . . C29 C 1.0183(4) 0.08456(19) 0.4745(5) 0.0766(16) Uani 1 1 d . . . H29 H 1.0974 0.0722 0.5007 0.092 Uiso 1 1 calc R . . C30 C 0.9237(4) 0.06450(15) 0.4965(4) 0.0607(12) Uani 1 1 d . . . H30 H 0.9386 0.0384 0.5366 0.073 Uiso 1 1 calc R . . C31 C 0.8042(3) 0.08258(12) 0.4596(3) 0.0414(9) Uani 1 1 d . . . C32 C 0.8639(4) 0.18343(16) 0.3051(5) 0.0742(15) Uani 1 1 d . . . H32 H 0.7765 0.1923 0.2831 0.089 Uiso 1 1 calc R . . C33 C 0.8881(6) 0.1770(2) 0.1868(5) 0.112(2) Uani 1 1 d . . . H33A H 0.9728 0.1676 0.2063 0.168 Uiso 1 1 calc R . . H33B H 0.8755 0.2033 0.1426 0.168 Uiso 1 1 calc R . . H33C H 0.8314 0.1560 0.1370 0.168 Uiso 1 1 calc R . . C34 C 0.9485(6) 0.21936(18) 0.3788(6) 0.107(2) Uani 1 1 d . . . H34A H 0.9210 0.2282 0.4433 0.160 Uiso 1 1 calc R . . H34B H 0.9440 0.2430 0.3254 0.160 Uiso 1 1 calc R . . H34C H 1.0334 0.2094 0.4139 0.160 Uiso 1 1 calc R . . C35 C 0.7006(4) 0.05952(13) 0.4835(4) 0.0539(11) Uani 1 1 d . . . H35 H 0.6228 0.0749 0.4389 0.065 Uiso 1 1 calc R . . C36 C 0.6818(6) 0.01447(17) 0.4374(6) 0.103(2) Uani 1 1 d . . . H36A H 0.6681 0.0141 0.3514 0.155 Uiso 1 1 calc R . . H36B H 0.6104 0.0025 0.4497 0.155 Uiso 1 1 calc R . . H36C H 0.7550 -0.0020 0.4817 0.155 Uiso 1 1 calc R . . C37 C 0.7185(8) 0.0606(2) 0.6166(6) 0.145(3) Uani 1 1 d . . . H37A H 0.7850 0.0416 0.6616 0.217 Uiso 1 1 calc R . . H37B H 0.6424 0.0520 0.6262 0.217 Uiso 1 1 calc R . . H37C H 0.7396 0.0890 0.6476 0.217 Uiso 1 1 calc R . . C38 C -0.0391(10) 0.0272(6) 0.1536(13) 0.174(5) Uani 1 1 d . . . C39 C -0.0137(17) 0.0538(6) 0.059(2) 0.159(10) Uani 0.50 1 d PD . . C40 C 0.0188(7) 0.0337(3) -0.0281(16) 0.136(4) Uani 1 1 d D . . C41 C 0.0479(17) 0.0181(11) -0.1221(17) 0.181(13) Uani 0.50 1 d PD . . C42 C 0.0089(10) -0.0098(5) -0.0553(17) 0.124(6) Uani 0.50 1 d PD . . 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 Zr 0.02806(18) 0.02859(19) 0.02415(17) -0.00130(14) 0.00982(12) -0.00016(14) Cl1 0.0646(6) 0.0313(5) 0.0368(5) -0.0018(4) 0.0171(4) -0.0005(4) Cl2 0.0378(5) 0.0543(6) 0.0428(5) -0.0119(4) 0.0137(4) 0.0080(4) N1 0.0397(16) 0.0268(15) 0.0272(14) 0.0022(12) 0.0089(12) 0.0035(13) N2 0.0359(16) 0.0349(16) 0.0341(15) 0.0026(13) 0.0133(13) -0.0013(13) N3 0.0260(14) 0.0374(16) 0.0308(14) -0.0006(13) 0.0104(12) 0.0015(12) N4 0.0316(15) 0.0432(18) 0.0348(15) -0.0050(13) 0.0172(13) -0.0049(13) C1 0.043(2) 0.036(2) 0.0314(18) -0.0014(16) 0.0102(16) 0.0035(17) C2 0.041(2) 0.030(2) 0.0372(19) -0.0068(16) 0.0093(16) 0.0019(16) C3 0.0347(19) 0.0304(19) 0.046(2) -0.0016(17) 0.0118(17) -0.0017(16) C4 0.090(3) 0.046(2) 0.032(2) -0.0106(18) 0.009(2) -0.002(2) C5 0.070(3) 0.037(2) 0.056(2) 0.0007(19) 0.024(2) -0.008(2) C6 0.0357(19) 0.036(2) 0.0283(17) 0.0009(15) 0.0105(15) -0.0014(16) C7 0.043(2) 0.038(2) 0.0325(18) -0.0074(16) 0.0170(16) 0.0026(17) C8 0.038(2) 0.043(2) 0.0291(17) 0.0003(16) 0.0169(15) 0.0047(17) C9 0.046(2) 0.068(3) 0.042(2) -0.023(2) 0.0061(19) -0.006(2) C10 0.053(3) 0.068(3) 0.057(2) -0.008(2) 0.034(2) 0.007(2) C11 0.039(2) 0.060(3) 0.055(2) -0.010(2) 0.0265(19) -0.0120(19) C12 0.049(2) 0.047(2) 0.047(2) 0.0006(19) 0.0262(19) -0.0122(19) C14 0.059(2) 0.0265(19) 0.0224(16) -0.0035(14) 0.0085(16) 0.0019(17) C15 0.056(2) 0.034(2) 0.0327(19) -0.0020(17) 0.0016(18) 0.0086(19) C16 0.075(3) 0.052(3) 0.054(3) 0.013(2) 0.004(2) 0.019(2) C17 0.113(5) 0.053(3) 0.053(3) 0.024(2) 0.013(3) 0.020(3) C18 0.108(4) 0.049(3) 0.046(2) 0.014(2) 0.029(3) 0.000(3) C19 0.079(3) 0.039(2) 0.0300(19) 0.0043(17) 0.020(2) 0.003(2) C20 0.045(2) 0.048(2) 0.052(2) 0.003(2) -0.0003(19) 0.012(2) C21 0.062(3) 0.090(4) 0.071(3) 0.000(3) 0.024(3) 0.019(3) C22 0.056(3) 0.098(4) 0.085(4) 0.002(3) -0.005(3) -0.002(3) C23 0.088(4) 0.056(3) 0.056(3) 0.016(2) 0.046(3) 0.012(2) C24 0.126(6) 0.092(5) 0.182(8) -0.038(5) 0.104(6) -0.002(4) C25 0.088(4) 0.078(4) 0.114(5) -0.003(3) 0.043(4) -0.012(3) C26 0.0301(18) 0.047(2) 0.0321(18) -0.0081(17) 0.0060(15) 0.0024(17) C27 0.031(2) 0.061(3) 0.056(2) -0.003(2) 0.0113(18) -0.0049(19) C28 0.034(2) 0.092(4) 0.077(3) -0.001(3) 0.017(2) 0.007(2) C29 0.039(3) 0.108(4) 0.070(3) -0.010(3) 0.006(2) 0.025(3) C30 0.055(3) 0.065(3) 0.051(2) 0.002(2) 0.006(2) 0.020(2) C31 0.037(2) 0.048(2) 0.0310(18) -0.0045(17) 0.0037(16) 0.0093(18) C32 0.039(2) 0.084(4) 0.099(4) 0.022(3) 0.025(3) -0.009(2) C33 0.110(5) 0.138(6) 0.086(4) 0.024(4) 0.034(4) -0.040(4) C34 0.106(5) 0.084(4) 0.145(6) -0.013(4) 0.063(5) -0.035(4) C35 0.059(3) 0.046(2) 0.055(2) 0.010(2) 0.019(2) 0.011(2) C36 0.130(6) 0.075(4) 0.110(5) -0.022(4) 0.050(4) -0.028(4) C37 0.217(9) 0.145(6) 0.130(6) -0.041(5) 0.129(6) -0.074(6) C38 0.085(6) 0.212(13) 0.214(13) -0.030(11) 0.042(7) 0.021(8) C39 0.076(12) 0.115(16) 0.20(2) -0.051(16) -0.049(13) 0.006(11) C40 0.069(5) 0.103(7) 0.206(12) 0.060(8) 0.016(6) -0.014(5) C41 0.058(10) 0.34(4) 0.119(16) 0.07(2) 0.008(10) -0.051(17) C42 0.030(6) 0.120(15) 0.18(2) -0.028(13) -0.003(9) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N4 2.174(3) . ? Zr N2 2.176(3) . ? Zr N1 2.314(3) . ? Zr N3 2.322(3) . ? Zr Cl2 2.4187(9) . ? Zr Cl1 2.4241(9) . ? N1 C1 1.337(4) . ? N1 C14 1.453(4) . ? N2 C3 1.347(4) . ? N2 C12 1.465(4) . ? N3 C6 1.341(4) . ? N3 C26 1.459(4) . ? N4 C8 1.344(4) . ? N4 C11 1.476(4) . ? C1 C2 1.398(5) . ? C1 C4 1.518(5) . ? C2 C3 1.374(5) . ? C2 H2 0.9300 . ? C3 C5 1.497(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.402(5) . ? C6 C9 1.508(5) . ? C7 C8 1.374(5) . ? C7 H7 0.9300 . ? C8 C10 1.500(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.488(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 C15 1.386(5) . ? C14 C19 1.407(5) . ? C15 C16 1.392(5) . ? C15 C20 1.507(6) . ? C16 C17 1.364(7) . ? C16 H16 0.9300 . ? C17 C18 1.368(7) . ? C17 H17 0.9300 . ? C18 C19 1.399(5) . ? C18 H18 0.9300 . ? C19 C23 1.514(6) . ? C20 C21 1.538(6) . ? C20 C22 1.541(6) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.513(6) . ? C23 C25 1.518(6) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C31 1.390(5) . ? C26 C27 1.391(5) . ? C27 C28 1.383(6) . ? C27 C32 1.517(6) . ? C28 C29 1.359(7) . ? C28 H28 0.9300 . ? C29 C30 1.360(7) . ? C29 H29 0.9300 . ? C30 C31 1.398(5) . ? C30 H30 0.9300 . ? C31 C35 1.505(6) . ? C32 C33 1.522(8) . ? C32 C34 1.534(7) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C37 1.495(7) . ? C35 C36 1.505(6) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C42 1.43(2) 3 ? C38 C41 1.47(3) 3 ? C38 C39 1.50(3) . ? C39 C40 1.366(16) . ? C39 C42 1.39(2) 3 ? C40 C41 1.353(17) . ? C40 C42 1.360(19) 3 ? C40 C42 1.401(15) . ? C41 C42 1.357(17) . ? C41 C38 1.47(3) 3 ? C42 C40 1.360(19) 3 ? C42 C39 1.39(2) 3 ? C42 C38 1.43(2) 3 ? C42 C42 1.51(4) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zr N2 72.68(11) . . ? N4 Zr N1 119.91(10) . . ? N2 Zr N1 78.15(10) . . ? N4 Zr N3 77.42(10) . . ? N2 Zr N3 118.89(10) . . ? N1 Zr N3 160.03(10) . . ? N4 Zr Cl2 143.50(8) . . ? N2 Zr Cl2 90.35(8) . . ? N1 Zr Cl2 86.20(7) . . ? N3 Zr Cl2 83.52(7) . . ? N4 Zr Cl1 92.13(8) . . ? N2 Zr Cl1 145.73(8) . . ? N1 Zr Cl1 83.77(7) . . ? N3 Zr Cl1 85.83(7) . . ? Cl2 Zr Cl1 117.40(4) . . ? C1 N1 C14 114.4(3) . . ? C1 N1 Zr 121.9(2) . . ? C14 N1 Zr 123.75(19) . . ? C3 N2 C12 118.1(3) . . ? C3 N2 Zr 124.2(2) . . ? C12 N2 Zr 117.1(2) . . ? C6 N3 C26 115.7(3) . . ? C6 N3 Zr 122.1(2) . . ? C26 N3 Zr 122.2(2) . . ? C8 N4 C11 117.5(3) . . ? C8 N4 Zr 124.6(2) . . ? C11 N4 Zr 117.4(2) . . ? N1 C1 C2 124.7(3) . . ? N1 C1 C4 121.1(3) . . ? C2 C1 C4 114.0(3) . . ? C3 C2 C1 125.9(3) . . ? C3 C2 H2 117.0 . . ? C1 C2 H2 117.0 . . ? N2 C3 C2 122.3(3) . . ? N2 C3 C5 120.1(3) . . ? C2 C3 C5 117.5(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 123.6(3) . . ? N3 C6 C9 121.5(3) . . ? C7 C6 C9 114.9(3) . . ? C8 C7 C6 126.1(3) . . ? C8 C7 H7 117.0 . . ? C6 C7 H7 117.0 . . ? N4 C8 C7 121.7(3) . . ? N4 C8 C10 120.7(3) . . ? C7 C8 C10 117.5(3) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 106.1(3) . . ? N4 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? N4 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N2 C12 C11 106.6(3) . . ? N2 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? N2 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C15 C14 C19 121.8(3) . . ? C15 C14 N1 118.5(3) . . ? C19 C14 N1 119.7(3) . . ? C14 C15 C16 118.1(4) . . ? C14 C15 C20 122.5(3) . . ? C16 C15 C20 119.4(4) . . ? C17 C16 C15 121.3(5) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 121.4(5) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C14 117.1(4) . . ? C18 C19 C23 119.6(4) . . ? C14 C19 C23 123.3(3) . . ? C15 C20 C21 110.2(3) . . ? C15 C20 C22 113.1(4) . . ? C21 C20 C22 110.2(4) . . ? C15 C20 H20 107.7 . . ? C21 C20 H20 107.7 . . ? C22 C20 H20 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 C24 113.1(5) . . ? C19 C23 C25 113.6(4) . . ? C24 C23 C25 108.2(4) . . ? C19 C23 H23 107.2 . . ? C24 C23 H23 107.2 . . ? C25 C23 H23 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 122.0(3) . . ? C31 C26 N3 118.1(3) . . ? C27 C26 N3 119.9(3) . . ? C28 C27 C26 117.7(4) . . ? C28 C27 C32 119.1(4) . . ? C26 C27 C32 123.1(4) . . ? C29 C28 C27 121.3(5) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C28 120.6(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.9(4) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C26 C31 C30 117.4(4) . . ? C26 C31 C35 122.7(3) . . ? C30 C31 C35 119.9(4) . . ? C27 C32 C33 109.9(5) . . ? C27 C32 C34 113.6(4) . . ? C33 C32 C34 108.7(4) . . ? C27 C32 H32 108.2 . . ? C33 C32 H32 108.2 . . ? C34 C32 H32 108.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C31 111.6(4) . . ? C37 C35 C36 110.0(5) . . ? C31 C35 C36 114.0(4) . . ? C37 C35 H35 106.9 . . ? C31 C35 H35 107.0 . . ? C36 C35 H35 107.0 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C42 C38 C41 55.9(9) 3 3 ? C42 C38 C39 56.6(12) 3 . ? C41 C38 C39 111.8(14) 3 . ? C40 C39 C42 59.2(12) . 3 ? C40 C39 C38 118.4(16) . . ? C42 C39 C38 59.2(14) 3 . ? C41 C40 C42 125.1(16) . 3 ? C41 C40 C39 173.3(17) . . ? C42 C40 C39 61.2(12) 3 . ? C41 C40 C42 59.0(9) . . ? C42 C40 C42 66.4(15) 3 . ? C39 C40 C42 126.9(17) . . ? C40 C41 C42 62.2(10) . . ? C40 C41 C38 122.8(16) . 3 ? C42 C41 C38 60.6(15) . 3 ? C41 C42 C40 170.4(17) . 3 ? C41 C42 C39 127(2) . 3 ? C40 C42 C39 59.6(11) 3 3 ? C41 C42 C40 58.7(11) . . ? C40 C42 C40 113.6(15) 3 . ? C39 C42 C40 169.3(16) 3 . ? C41 C42 C38 63.6(18) . 3 ? C40 C42 C38 123.8(14) 3 3 ? C39 C42 C38 64.2(14) 3 3 ? C40 C42 C38 122.3(17) . 3 ? C41 C42 C42 113.9(18) . 3 ? C40 C42 C42 58.1(14) 3 3 ? C39 C42 C42 117(2) 3 3 ? C40 C42 C42 55.5(10) . 3 ? C38 C42 C42 174.1(14) 3 3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Zr N1 C1 -98.3(3) . . . . ? N2 Zr N1 C1 -36.4(3) . . . . ? N3 Zr N1 C1 113.8(3) . . . . ? Cl2 Zr N1 C1 54.7(3) . . . . ? Cl1 Zr N1 C1 172.9(3) . . . . ? N4 Zr N1 C14 82.4(3) . . . . ? N2 Zr N1 C14 144.3(3) . . . . ? N3 Zr N1 C14 -65.5(4) . . . . ? Cl2 Zr N1 C14 -124.6(3) . . . . ? Cl1 Zr N1 C14 -6.5(3) . . . . ? N4 Zr N2 C3 174.3(3) . . . . ? N1 Zr N2 C3 47.5(3) . . . . ? N3 Zr N2 C3 -121.4(3) . . . . ? Cl2 Zr N2 C3 -38.6(3) . . . . ? Cl1 Zr N2 C3 107.1(3) . . . . ? N4 Zr N2 C12 -15.5(2) . . . . ? N1 Zr N2 C12 -142.3(3) . . . . ? N3 Zr N2 C12 48.9(3) . . . . ? Cl2 Zr N2 C12 131.6(2) . . . . ? Cl1 Zr N2 C12 -82.6(3) . . . . ? N4 Zr N3 C6 -37.9(3) . . . . ? N2 Zr N3 C6 -99.8(3) . . . . ? N1 Zr N3 C6 113.9(3) . . . . ? Cl2 Zr N3 C6 173.4(3) . . . . ? Cl1 Zr N3 C6 55.2(2) . . . . ? N4 Zr N3 C26 145.3(3) . . . . ? N2 Zr N3 C26 83.4(3) . . . . ? N1 Zr N3 C26 -62.9(4) . . . . ? Cl2 Zr N3 C26 -3.4(2) . . . . ? Cl1 Zr N3 C26 -121.6(2) . . . . ? N2 Zr N4 C8 174.7(3) . . . . ? N1 Zr N4 C8 -120.6(3) . . . . ? N3 Zr N4 C8 48.7(3) . . . . ? Cl2 Zr N4 C8 109.0(3) . . . . ? Cl1 Zr N4 C8 -36.5(3) . . . . ? N2 Zr N4 C11 -13.4(3) . . . . ? N1 Zr N4 C11 51.3(3) . . . . ? N3 Zr N4 C11 -139.4(3) . . . . ? Cl2 Zr N4 C11 -79.2(3) . . . . ? Cl1 Zr N4 C11 135.3(3) . . . . ? C14 N1 C1 C2 -168.2(3) . . . . ? Zr N1 C1 C2 12.4(5) . . . . ? C14 N1 C1 C4 6.2(5) . . . . ? Zr N1 C1 C4 -173.2(3) . . . . ? N1 C1 C2 C3 23.7(6) . . . . ? C4 C1 C2 C3 -151.1(4) . . . . ? C12 N2 C3 C2 155.9(3) . . . . ? Zr N2 C3 C2 -34.0(5) . . . . ? C12 N2 C3 C5 -21.9(5) . . . . ? Zr N2 C3 C5 148.3(3) . . . . ? C1 C2 C3 N2 -13.5(6) . . . . ? C1 C2 C3 C5 164.3(4) . . . . ? C26 N3 C6 C7 -170.0(3) . . . . ? Zr N3 C6 C7 13.1(4) . . . . ? C26 N3 C6 C9 6.3(5) . . . . ? Zr N3 C6 C9 -170.7(3) . . . . ? N3 C6 C7 C8 25.5(5) . . . . ? C9 C6 C7 C8 -151.0(4) . . . . ? C11 N4 C8 C7 154.5(3) . . . . ? Zr N4 C8 C7 -33.7(4) . . . . ? C11 N4 C8 C10 -21.9(5) . . . . ? Zr N4 C8 C10 149.9(3) . . . . ? C6 C7 C8 N4 -16.1(5) . . . . ? C6 C7 C8 C10 160.4(3) . . . . ? C8 N4 C11 C12 -149.4(3) . . . . ? Zr N4 C11 C12 38.1(4) . . . . ? C3 N2 C12 C11 -149.0(3) . . . . ? Zr N2 C12 C11 40.2(4) . . . . ? N4 C11 C12 N2 -47.3(4) . . . . ? C1 N1 C14 C15 83.5(4) . . . . ? Zr N1 C14 C15 -97.1(3) . . . . ? C1 N1 C14 C19 -94.0(4) . . . . ? Zr N1 C14 C19 85.4(3) . . . . ? C19 C14 C15 C16 1.7(5) . . . . ? N1 C14 C15 C16 -175.8(3) . . . . ? C19 C14 C15 C20 -176.9(3) . . . . ? N1 C14 C15 C20 5.7(5) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C20 C15 C16 C17 178.2(4) . . . . ? C15 C16 C17 C18 -0.3(7) . . . . ? C16 C17 C18 C19 -0.2(7) . . . . ? C17 C18 C19 C14 1.4(6) . . . . ? C17 C18 C19 C23 -178.9(4) . . . . ? C15 C14 C19 C18 -2.1(5) . . . . ? N1 C14 C19 C18 175.3(3) . . . . ? C15 C14 C19 C23 178.2(4) . . . . ? N1 C14 C19 C23 -4.4(5) . . . . ? C14 C15 C20 C21 98.0(4) . . . . ? C16 C15 C20 C21 -80.5(4) . . . . ? C14 C15 C20 C22 -138.2(4) . . . . ? C16 C15 C20 C22 43.2(5) . . . . ? C18 C19 C23 C24 -85.3(5) . . . . ? C14 C19 C23 C24 94.4(5) . . . . ? C18 C19 C23 C25 38.5(6) . . . . ? C14 C19 C23 C25 -141.8(4) . . . . ? C6 N3 C26 C31 97.6(4) . . . . ? Zr N3 C26 C31 -85.4(3) . . . . ? C6 N3 C26 C27 -83.2(4) . . . . ? Zr N3 C26 C27 93.8(4) . . . . ? C31 C26 C27 C28 -2.2(6) . . . . ? N3 C26 C27 C28 178.6(3) . . . . ? C31 C26 C27 C32 177.0(4) . . . . ? N3 C26 C27 C32 -2.2(6) . . . . ? C26 C27 C28 C29 1.2(7) . . . . ? C32 C27 C28 C29 -178.0(5) . . . . ? C27 C28 C29 C30 0.3(8) . . . . ? C28 C29 C30 C31 -0.8(7) . . . . ? C27 C26 C31 C30 1.7(5) . . . . ? N3 C26 C31 C30 -179.1(3) . . . . ? C27 C26 C31 C35 -177.7(4) . . . . ? N3 C26 C31 C35 1.5(5) . . . . ? C29 C30 C31 C26 -0.2(6) . . . . ? C29 C30 C31 C35 179.2(4) . . . . ? C28 C27 C32 C33 61.2(6) . . . . ? C26 C27 C32 C33 -117.9(5) . . . . ? C28 C27 C32 C34 -60.8(6) . . . . ? C26 C27 C32 C34 120.1(5) . . . . ? C26 C31 C35 C37 -107.9(5) . . . . ? C30 C31 C35 C37 72.8(6) . . . . ? C26 C31 C35 C36 126.8(4) . . . . ? C30 C31 C35 C36 -52.6(5) . . . . ? C42 C38 C39 C40 -2.4(12) 3 . . . ? C41 C38 C39 C40 -11(2) 3 . . . ? C41 C38 C39 C42 -8.6(13) 3 . . 3 ? C42 C39 C40 C41 162(11) 3 . . . ? C38 C39 C40 C41 164(10) . . . . ? C38 C39 C40 C42 2.4(12) . . . 3 ? C42 C39 C40 C42 10.7(15) 3 . . . ? C38 C39 C40 C42 13(2) . . . . ? C42 C40 C41 C42 7.2(16) 3 . . . ? C39 C40 C41 C42 -153(11) . . . . ? C42 C40 C41 C38 7(2) 3 . . 3 ? C39 C40 C41 C38 -153(10) . . . 3 ? C42 C40 C41 C38 -0.1(13) . . . 3 ? C40 C41 C42 C40 -38(10) . . . 3 ? C38 C41 C42 C40 142(9) 3 . . 3 ? C40 C41 C42 C39 -169.0(15) . . . 3 ? C38 C41 C42 C39 10.9(16) 3 . . 3 ? C38 C41 C42 C40 179.9(13) 3 . . . ? C40 C41 C42 C38 -179.9(13) . . . 3 ? C40 C41 C42 C42 -5.8(13) . . . 3 ? C38 C41 C42 C42 174.1(15) 3 . . 3 ? C42 C40 C42 C41 -173.5(14) 3 . . . ? C39 C40 C42 C41 176.2(16) . . . . ? C41 C40 C42 C40 173.5(14) . . . 3 ? C42 C40 C42 C40 0.0 3 . . 3 ? C39 C40 C42 C40 -10.2(14) . . . 3 ? C41 C40 C42 C39 125(10) . . . 3 ? C42 C40 C42 C39 -49(9) 3 . . 3 ? C39 C40 C42 C39 -59(10) . . . 3 ? C41 C40 C42 C38 0.1(13) . . . 3 ? C42 C40 C42 C38 -173.4(16) 3 . . 3 ? C39 C40 C42 C38 176.4(13) . . . 3 ? C41 C40 C42 C42 173.5(14) . . . 3 ? C39 C40 C42 C42 -10.2(14) . . . 3 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.691 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.078 #===END data_cd27338 _database_code_depnum_ccdc_archive 'CCDC 724273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H58 Cl2 N4 Zr' _chemical_formula_weight 763.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 11.6509(13) _cell_length_b 31.598(4) _cell_length_c 11.6510(13) _cell_angle_alpha 90.00 _cell_angle_beta 110.906(2) _cell_angle_gamma 90.00 _cell_volume 4006.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1912 _cell_measurement_theta_min 4.436 _cell_measurement_theta_max 47.569 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.293 _exptl_crystal_size_mid 0.262 _exptl_crystal_size_min 0.204 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1614 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77096 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21032 _diffrn_reflns_av_R_equivalents 0.1133 _diffrn_reflns_av_sigmaI/netI 0.1710 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7437 _reflns_number_gt 3356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7437 _refine_ls_number_parameters 426 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1296 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.822 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.01479(5) 0.127047(17) 0.67027(5) 0.03841(17) Uani 1 1 d . . . Cl1 Cl 0.17294(13) 0.08602(5) 0.63147(14) 0.0560(4) Uani 1 1 d . . . Cl2 Cl 0.01807(13) 0.20131(5) 0.61797(13) 0.0562(4) Uani 1 1 d . . . N1 N 0.1667(4) 0.14083(13) 0.8569(4) 0.0386(11) Uani 1 1 d . . . N2 N -0.1036(4) 0.14447(14) 0.7728(4) 0.0427(12) Uani 1 1 d . . . N3 N -0.1033(4) 0.11826(14) 0.4680(4) 0.0444(12) Uani 1 1 d . . . N4 N -0.0717(4) 0.06656(14) 0.6878(4) 0.0459(12) Uani 1 1 d . . . C1 C 0.1517(5) 0.16918(18) 0.9345(5) 0.0433(14) Uani 1 1 d . . . C2 C 0.0390(5) 0.18741(17) 0.9266(5) 0.0468(15) Uani 1 1 d . . . H2 H 0.0446 0.2119 0.9725 0.056 Uiso 1 1 calc R . . C3 C -0.0799(5) 0.17384(19) 0.8594(5) 0.0492(16) Uani 1 1 d . . . C4 C 0.2589(5) 0.18253(19) 1.0484(5) 0.069(2) Uani 1 1 d . . . H4A H 0.2798 0.1598 1.1069 0.104 Uiso 1 1 calc R . . H4B H 0.2360 0.2070 1.0841 0.104 Uiso 1 1 calc R . . H4C H 0.3284 0.1892 1.0259 0.104 Uiso 1 1 calc R . . C5 C -0.1785(5) 0.1941(2) 0.8962(5) 0.0683(19) Uani 1 1 d . . . H5A H -0.2470 0.2015 0.8239 0.102 Uiso 1 1 calc R . . H5B H -0.1464 0.2192 0.9433 0.102 Uiso 1 1 calc R . . H5C H -0.2049 0.1746 0.9450 0.102 Uiso 1 1 calc R . . C6 C -0.1352(5) 0.0797(2) 0.4163(5) 0.0524(16) Uani 1 1 d . . . C7 C -0.1206(5) 0.04229(19) 0.4826(6) 0.0550(16) Uani 1 1 d . . . H7 H -0.1237 0.0178 0.4372 0.066 Uiso 1 1 calc R . . C8 C -0.1023(5) 0.03557(19) 0.6046(6) 0.0481(15) Uani 1 1 d . . . C9 C -0.1983(6) 0.0751(2) 0.2787(5) 0.077(2) Uani 1 1 d . . . H9A H -0.2829 0.0832 0.2556 0.115 Uiso 1 1 calc R . . H9B H -0.1933 0.0462 0.2556 0.115 Uiso 1 1 calc R . . H9C H -0.1585 0.0930 0.2377 0.115 Uiso 1 1 calc R . . C10 C -0.1258(6) -0.00891(18) 0.6384(6) 0.073(2) Uani 1 1 d . . . H10A H -0.0622 -0.0170 0.7139 0.110 Uiso 1 1 calc R . . H10B H -0.1261 -0.0280 0.5743 0.110 Uiso 1 1 calc R . . H10C H -0.2039 -0.0100 0.6486 0.110 Uiso 1 1 calc R . . C11 C -0.0891(5) 0.06014(18) 0.8052(5) 0.0572(17) Uani 1 1 d . . . H11A H -0.0202 0.0723 0.8711 0.069 Uiso 1 1 calc R . . H11B H -0.0914 0.0301 0.8208 0.069 Uiso 1 1 calc R . . C12 C -0.2071(5) 0.0805(2) 0.8039(6) 0.0659(19) Uani 1 1 d . . . H12A H -0.2035 0.0852 0.8874 0.079 Uiso 1 1 calc R . . H12B H -0.2762 0.0620 0.7631 0.079 Uiso 1 1 calc R . . C13 C -0.2230(5) 0.1222(2) 0.7362(5) 0.0583(17) Uani 1 1 d . . . H13A H -0.2536 0.1171 0.6483 0.070 Uiso 1 1 calc R . . H13B H -0.2823 0.1396 0.7554 0.070 Uiso 1 1 calc R . . C14 C 0.2932(5) 0.1235(2) 0.8914(5) 0.0463(14) Uani 1 1 d . . . C15 C 0.3249(5) 0.08653(19) 0.9568(5) 0.0512(16) Uani 1 1 d . . . C16 C 0.4452(6) 0.0721(2) 0.9910(6) 0.077(2) Uani 1 1 d . . . H16 H 0.4671 0.0470 1.0351 0.093 Uiso 1 1 calc R . . C17 C 0.5312(6) 0.0936(3) 0.9614(7) 0.091(3) Uani 1 1 d . . . H17 H 0.6111 0.0834 0.9849 0.109 Uiso 1 1 calc R . . C18 C 0.4995(6) 0.1309(3) 0.8963(7) 0.087(2) Uani 1 1 d . . . H18 H 0.5592 0.1457 0.8767 0.104 Uiso 1 1 calc R . . C19 C 0.3797(5) 0.1472(2) 0.8587(6) 0.0606(18) Uani 1 1 d . . . C20 C 0.2348(6) 0.0607(2) 0.9925(6) 0.0639(18) Uani 1 1 d . . . H20 H 0.1566 0.0760 0.9665 0.077 Uiso 1 1 calc R . . C21 C 0.2122(7) 0.0181(2) 0.9312(7) 0.112(3) Uani 1 1 d . . . H21A H 0.1841 0.0217 0.8437 0.168 Uiso 1 1 calc R . . H21B H 0.1509 0.0032 0.9528 0.168 Uiso 1 1 calc R . . H21C H 0.2872 0.0021 0.9579 0.168 Uiso 1 1 calc R . . C22 C 0.2776(7) 0.0542(3) 1.1313(7) 0.121(3) Uani 1 1 d . . . H22A H 0.3519 0.0378 1.1581 0.181 Uiso 1 1 calc R . . H22B H 0.2152 0.0394 1.1513 0.181 Uiso 1 1 calc R . . H22C H 0.2926 0.0812 1.1717 0.181 Uiso 1 1 calc R . . C23 C 0.3499(6) 0.1879(2) 0.7841(7) 0.081(2) Uani 1 1 d . . . H23 H 0.2613 0.1931 0.7589 0.097 Uiso 1 1 calc R . . C24 C 0.3815(8) 0.1855(3) 0.6736(7) 0.138(4) Uani 1 1 d . . . H24A H 0.4691 0.1832 0.6968 0.208 Uiso 1 1 calc R . . H24B H 0.3533 0.2105 0.6252 0.208 Uiso 1 1 calc R . . H24C H 0.3431 0.1611 0.6265 0.208 Uiso 1 1 calc R . . C25 C 0.4181(9) 0.2264(3) 0.8594(9) 0.151(4) Uani 1 1 d . . . H25A H 0.4904 0.2169 0.9248 0.226 Uiso 1 1 calc R . . H25B H 0.3651 0.2409 0.8933 0.226 Uiso 1 1 calc R . . H25C H 0.4413 0.2453 0.8069 0.226 Uiso 1 1 calc R . . C26 C -0.1429(6) 0.15298(18) 0.3786(5) 0.0493(16) Uani 1 1 d . . . C27 C -0.2612(6) 0.1687(2) 0.3457(5) 0.0595(18) Uani 1 1 d . . . C28 C -0.2987(7) 0.1997(2) 0.2568(7) 0.086(2) Uani 1 1 d . . . H28 H -0.3784 0.2101 0.2341 0.103 Uiso 1 1 calc R . . C29 C -0.2247(9) 0.2154(3) 0.2023(7) 0.106(3) Uani 1 1 d . . . H29 H -0.2523 0.2364 0.1430 0.127 Uiso 1 1 calc R . . C30 C -0.1074(8) 0.1999(2) 0.2352(6) 0.089(2) Uani 1 1 d . . . H30 H -0.0561 0.2105 0.1965 0.107 Uiso 1 1 calc R . . C31 C -0.0630(7) 0.1689(2) 0.3242(6) 0.071(2) Uani 1 1 d . . . C32 C -0.3500(6) 0.1543(2) 0.4056(6) 0.0669(19) Uani 1 1 d . . . H32 H -0.3181 0.1279 0.4495 0.080 Uiso 1 1 calc R . . C33 C -0.4803(6) 0.1452(2) 0.3126(7) 0.107(3) Uani 1 1 d . . . H33A H -0.5147 0.1707 0.2692 0.160 Uiso 1 1 calc R . . H33B H -0.5315 0.1351 0.3557 0.160 Uiso 1 1 calc R . . H33C H -0.4758 0.1241 0.2552 0.160 Uiso 1 1 calc R . . C34 C -0.3563(6) 0.1868(2) 0.5005(6) 0.087(2) Uani 1 1 d . . . H34A H -0.2754 0.1913 0.5600 0.130 Uiso 1 1 calc R . . H34B H -0.4094 0.1765 0.5410 0.130 Uiso 1 1 calc R . . H34C H -0.3878 0.2131 0.4599 0.130 Uiso 1 1 calc R . . C35 C 0.0685(8) 0.1535(3) 0.3552(8) 0.108(3) Uani 1 1 d . . . H35 H 0.0928 0.1381 0.4332 0.130 Uiso 1 1 calc R . . C36 C 0.0781(9) 0.1239(3) 0.2589(10) 0.121(5) Uani 1 1 d . . . H36A H 0.0384 0.0977 0.2634 0.162 Uiso 1 1 calc R . . H36B H 0.1631 0.1188 0.2723 0.162 Uiso 1 1 calc R . . H36C H 0.0389 0.1363 0.1792 0.162 Uiso 1 1 calc R . . C37 C 0.1592(7) 0.1902(3) 0.3700(8) 0.144(4) Uani 1 1 d . . . H37A H 0.2418 0.1797 0.4048 0.176 Uiso 1 1 calc R . . H37B H 0.1460 0.2112 0.4233 0.176 Uiso 1 1 calc R . . H37C H 0.1465 0.2025 0.2911 0.176 Uiso 1 1 calc R . . C38 C 0.4504(11) 0.0141(5) 0.5983(12) 0.191(5) Uiso 1 1 d D . . C39 C 0.4888(10) 0.0431(3) 0.5281(11) 0.198(5) Uiso 1 1 d D . . H39 H 0.4844 0.0721 0.5395 0.238 Uiso 1 1 calc R . . C40 C 0.5328(9) 0.0276(3) 0.4428(9) 0.162(4) Uiso 1 1 d D . . H40 H 0.5577 0.0488 0.4015 0.195 Uiso 1 1 calc R . . C41 C 0.437(2) 0.0253(8) 0.7037(18) 0.273(15) Uiso 0.50 1 d PD . . H41A H 0.3608 0.0147 0.7051 0.409 Uiso 0.50 1 calc PR . . H41B H 0.4386 0.0556 0.7102 0.409 Uiso 0.50 1 calc PR . . H41C H 0.5038 0.0137 0.7716 0.409 Uiso 0.50 1 calc PR . . 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 Zr 0.0394(3) 0.0366(3) 0.0396(3) -0.0001(3) 0.0145(2) 0.0000(3) Cl1 0.0502(9) 0.0589(11) 0.0610(10) -0.0073(8) 0.0224(8) 0.0077(8) Cl2 0.0699(11) 0.0424(10) 0.0552(10) 0.0030(7) 0.0211(8) -0.0012(8) N1 0.037(3) 0.037(3) 0.044(3) 0.000(2) 0.018(2) 0.001(2) N2 0.036(3) 0.047(3) 0.044(3) -0.004(2) 0.012(2) 0.000(2) N3 0.050(3) 0.036(3) 0.044(3) 0.003(2) 0.014(2) 0.010(2) N4 0.047(3) 0.043(3) 0.048(3) 0.004(3) 0.018(2) 0.003(2) C1 0.042(4) 0.043(4) 0.042(4) 0.000(3) 0.012(3) -0.006(3) C2 0.054(4) 0.036(4) 0.051(4) -0.009(3) 0.020(3) -0.001(3) C3 0.048(4) 0.053(4) 0.051(4) 0.006(3) 0.023(3) 0.007(3) C4 0.056(4) 0.075(5) 0.059(4) -0.023(4) 0.000(3) -0.004(3) C5 0.059(4) 0.080(5) 0.074(5) -0.012(4) 0.035(4) 0.009(4) C6 0.063(4) 0.048(4) 0.046(4) -0.003(3) 0.019(3) 0.011(3) C7 0.064(4) 0.038(4) 0.062(4) -0.011(3) 0.021(3) 0.005(3) C8 0.041(4) 0.042(4) 0.065(4) -0.001(3) 0.024(3) 0.002(3) C9 0.109(6) 0.067(5) 0.044(4) -0.016(3) 0.015(4) 0.003(4) C10 0.092(5) 0.041(4) 0.090(5) -0.002(4) 0.036(4) -0.012(4) C11 0.066(4) 0.048(4) 0.058(4) 0.007(3) 0.023(3) -0.008(3) C12 0.054(4) 0.079(5) 0.072(5) -0.002(4) 0.033(4) -0.016(4) C13 0.035(3) 0.075(5) 0.063(4) -0.010(4) 0.015(3) 0.001(3) C14 0.033(3) 0.060(4) 0.044(3) -0.003(3) 0.012(3) 0.001(3) C15 0.047(4) 0.053(4) 0.050(4) 0.001(3) 0.012(3) 0.014(3) C16 0.060(5) 0.091(6) 0.074(5) 0.023(4) 0.016(4) 0.024(4) C17 0.051(5) 0.117(8) 0.108(7) 0.027(5) 0.033(5) 0.032(5) C18 0.039(4) 0.125(8) 0.100(6) 0.008(5) 0.030(4) -0.007(5) C19 0.041(4) 0.071(5) 0.067(5) -0.001(4) 0.016(3) -0.005(3) C20 0.056(4) 0.050(5) 0.079(5) 0.015(4) 0.016(4) 0.004(3) C21 0.151(8) 0.068(6) 0.118(7) -0.011(5) 0.047(6) -0.033(5) C22 0.174(9) 0.109(8) 0.103(7) -0.007(6) 0.078(7) -0.047(6) C23 0.048(4) 0.083(6) 0.107(6) 0.028(5) 0.023(4) -0.019(4) C24 0.185(10) 0.128(9) 0.110(7) 0.037(6) 0.062(7) -0.016(7) C25 0.195(10) 0.098(8) 0.169(10) -0.001(7) 0.077(8) -0.047(7) C26 0.065(4) 0.038(4) 0.040(4) -0.002(3) 0.013(3) 0.009(3) C27 0.081(5) 0.043(4) 0.042(4) -0.003(3) 0.007(4) 0.011(4) C28 0.104(6) 0.067(6) 0.071(6) 0.012(4) 0.010(5) 0.038(5) C29 0.166(10) 0.068(6) 0.074(6) 0.034(5) 0.030(6) 0.045(6) C30 0.136(7) 0.075(6) 0.063(5) 0.020(4) 0.042(5) 0.004(5) C31 0.102(6) 0.069(5) 0.049(4) 0.018(4) 0.036(4) 0.014(4) C32 0.060(4) 0.059(5) 0.061(5) -0.002(4) -0.004(4) 0.009(4) C33 0.069(5) 0.116(7) 0.107(6) -0.010(5) -0.002(5) 0.003(5) C34 0.086(5) 0.094(6) 0.075(5) -0.003(5) 0.022(4) 0.034(4) C35 0.111(7) 0.136(9) 0.100(7) 0.060(6) 0.066(6) 0.032(7) C36 0.136(10) 0.061(7) 0.189(14) 0.027(8) 0.107(11) 0.039(7) C37 0.111(8) 0.214(12) 0.120(8) -0.015(8) 0.058(6) -0.030(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr N2 2.193(4) . ? Zr N4 2.204(4) . ? Zr N3 2.282(4) . ? Zr N1 2.303(4) . ? Zr Cl1 2.4238(14) . ? Zr Cl2 2.4282(16) . ? N1 C1 1.328(6) . ? N1 C14 1.488(6) . ? N2 C3 1.325(6) . ? N2 C13 1.479(6) . ? N3 C6 1.351(7) . ? N3 C26 1.469(6) . ? N4 C8 1.334(6) . ? N4 C11 1.467(6) . ? C1 C2 1.406(7) . ? C1 C4 1.521(7) . ? C2 C3 1.393(7) . ? C2 H2 0.9300 . ? C3 C5 1.505(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.390(7) . ? C6 C9 1.513(7) . ? C7 C8 1.377(7) . ? C7 H7 0.9300 . ? C8 C10 1.511(7) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.512(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.513(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.371(7) . ? C14 C19 1.413(7) . ? C15 C16 1.391(7) . ? C15 C20 1.501(7) . ? C16 C17 1.354(8) . ? C16 H16 0.9300 . ? C17 C18 1.379(9) . ? C17 H17 0.9300 . ? C18 C19 1.404(8) . ? C18 H18 0.9300 . ? C19 C23 1.521(8) . ? C20 C21 1.503(8) . ? C20 C22 1.526(8) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.462(9) . ? C23 C25 1.542(10) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.384(7) . ? C26 C31 1.393(8) . ? C27 C28 1.379(8) . ? C27 C32 1.511(8) . ? C28 C29 1.335(9) . ? C28 H28 0.9300 . ? C29 C30 1.372(10) . ? C29 H29 0.9300 . ? C30 C31 1.385(8) . ? C30 H30 0.9300 . ? C31 C35 1.523(9) . ? C32 C34 1.529(8) . ? C32 C33 1.545(8) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.495(11) . ? C35 C37 1.535(10) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C41 1.338(15) . ? C38 C39 1.403(11) . ? C38 C40 1.439(10) 3_656 ? C39 C40 1.362(9) . ? C39 H39 0.9300 . ? C40 C38 1.439(10) 3_656 ? C40 H40 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zr N4 76.71(16) . . ? N2 Zr N3 109.16(15) . . ? N4 Zr N3 82.13(16) . . ? N2 Zr N1 81.89(15) . . ? N4 Zr N1 107.41(15) . . ? N3 Zr N1 167.15(14) . . ? N2 Zr Cl1 154.65(12) . . ? N4 Zr Cl1 87.50(12) . . ? N3 Zr Cl1 87.76(11) . . ? N1 Zr Cl1 84.16(11) . . ? N2 Zr Cl2 87.90(12) . . ? N4 Zr Cl2 155.52(11) . . ? N3 Zr Cl2 85.19(12) . . ? N1 Zr Cl2 88.77(11) . . ? Cl1 Zr Cl2 112.89(5) . . ? C1 N1 C14 115.0(4) . . ? C1 N1 Zr 121.8(3) . . ? C14 N1 Zr 122.6(3) . . ? C3 N2 C13 118.2(4) . . ? C3 N2 Zr 126.1(4) . . ? C13 N2 Zr 115.6(3) . . ? C6 N3 C26 112.9(5) . . ? C6 N3 Zr 122.6(4) . . ? C26 N3 Zr 124.2(3) . . ? C8 N4 C11 119.1(5) . . ? C8 N4 Zr 125.6(4) . . ? C11 N4 Zr 115.2(4) . . ? N1 C1 C2 125.3(5) . . ? N1 C1 C4 120.9(5) . . ? C2 C1 C4 113.6(5) . . ? C3 C2 C1 128.9(5) . . ? C3 C2 H2 115.5 . . ? C1 C2 H2 115.5 . . ? N2 C3 C2 122.6(5) . . ? N2 C3 C5 122.8(5) . . ? C2 C3 C5 114.5(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 C7 124.0(5) . . ? N3 C6 C9 120.8(5) . . ? C7 C6 C9 115.1(6) . . ? C8 C7 C6 130.4(6) . . ? C8 C7 H7 114.8 . . ? C6 C7 H7 114.8 . . ? N4 C8 C7 122.7(6) . . ? N4 C8 C10 121.3(5) . . ? C7 C8 C10 115.9(5) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 C12 111.1(5) . . ? N4 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N4 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 108.4(4) . . ? C11 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? C11 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N2 C13 C12 109.7(5) . . ? N2 C13 H13A 109.7 . . ? C12 C13 H13A 109.7 . . ? N2 C13 H13B 109.7 . . ? C12 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C19 121.7(5) . . ? C15 C14 N1 120.5(5) . . ? C19 C14 N1 117.7(5) . . ? C14 C15 C16 118.8(6) . . ? C14 C15 C20 122.8(5) . . ? C16 C15 C20 118.4(6) . . ? C17 C16 C15 121.6(7) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 119.6(6) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 121.7(6) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 C14 116.5(6) . . ? C18 C19 C23 119.2(6) . . ? C14 C19 C23 124.3(6) . . ? C15 C20 C21 112.1(6) . . ? C15 C20 C22 111.7(5) . . ? C21 C20 C22 108.6(6) . . ? C15 C20 H20 108.1 . . ? C21 C20 H20 108.1 . . ? C22 C20 H20 108.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 112.4(7) . . ? C24 C23 C25 107.5(6) . . ? C19 C23 C25 112.0(7) . . ? C24 C23 H23 108.3 . . ? C19 C23 H23 108.3 . . ? C25 C23 H23 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 120.3(6) . . ? C27 C26 N3 119.6(5) . . ? C31 C26 N3 120.1(5) . . ? C28 C27 C26 118.7(7) . . ? C28 C27 C32 118.4(7) . . ? C26 C27 C32 122.9(6) . . ? C29 C28 C27 122.3(8) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 118.9(7) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C29 C30 C31 122.0(7) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C30 C31 C26 117.7(7) . . ? C30 C31 C35 118.6(6) . . ? C26 C31 C35 123.7(6) . . ? C27 C32 C34 110.4(5) . . ? C27 C32 C33 113.3(6) . . ? C34 C32 C33 110.1(6) . . ? C27 C32 H32 107.6 . . ? C34 C32 H32 107.6 . . ? C33 C32 H32 107.6 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C31 111.1(8) . . ? C36 C35 C37 108.9(7) . . ? C31 C35 C37 112.3(8) . . ? C36 C35 H35 108.1 . . ? C31 C35 H35 108.1 . . ? C37 C35 H35 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C41 C38 C39 121.8(16) . . ? C41 C38 C40 128.3(18) . 3_656 ? C39 C38 C40 107.1(9) . 3_656 ? C40 C39 C38 118.1(8) . . ? C40 C39 H39 120.9 . . ? C38 C39 H39 120.9 . . ? C39 C40 C38 134.8(8) . 3_656 ? C39 C40 H40 112.6 . . ? C38 C40 H40 112.6 3_656 . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zr N1 C1 -30.2(4) . . . . ? N4 Zr N1 C1 -103.5(4) . . . . ? N3 Zr N1 C1 119.7(7) . . . . ? Cl1 Zr N1 C1 171.0(4) . . . . ? Cl2 Zr N1 C1 57.9(4) . . . . ? N2 Zr N1 C14 158.7(4) . . . . ? N4 Zr N1 C14 85.4(4) . . . . ? N3 Zr N1 C14 -51.4(9) . . . . ? Cl1 Zr N1 C14 -0.1(4) . . . . ? Cl2 Zr N1 C14 -113.2(4) . . . . ? N4 Zr N2 C3 145.8(5) . . . . ? N3 Zr N2 C3 -137.5(4) . . . . ? N1 Zr N2 C3 35.7(5) . . . . ? Cl1 Zr N2 C3 92.9(5) . . . . ? Cl2 Zr N2 C3 -53.4(5) . . . . ? N4 Zr N2 C13 -37.0(4) . . . . ? N3 Zr N2 C13 39.6(4) . . . . ? N1 Zr N2 C13 -147.2(4) . . . . ? Cl1 Zr N2 C13 -89.9(4) . . . . ? Cl2 Zr N2 C13 123.8(4) . . . . ? N2 Zr N3 C6 -102.1(4) . . . . ? N4 Zr N3 C6 -29.1(4) . . . . ? N1 Zr N3 C6 109.6(8) . . . . ? Cl1 Zr N3 C6 58.7(4) . . . . ? Cl2 Zr N3 C6 171.9(4) . . . . ? N2 Zr N3 C26 83.8(4) . . . . ? N4 Zr N3 C26 156.7(4) . . . . ? N1 Zr N3 C26 -64.5(9) . . . . ? Cl1 Zr N3 C26 -115.5(4) . . . . ? Cl2 Zr N3 C26 -2.3(4) . . . . ? N2 Zr N4 C8 146.1(5) . . . . ? N3 Zr N4 C8 34.2(4) . . . . ? N1 Zr N4 C8 -137.0(4) . . . . ? Cl1 Zr N4 C8 -53.9(4) . . . . ? Cl2 Zr N4 C8 93.6(5) . . . . ? N2 Zr N4 C11 -37.5(4) . . . . ? N3 Zr N4 C11 -149.4(4) . . . . ? N1 Zr N4 C11 39.5(4) . . . . ? Cl1 Zr N4 C11 122.6(4) . . . . ? Cl2 Zr N4 C11 -89.9(4) . . . . ? C14 N1 C1 C2 -174.7(5) . . . . ? Zr N1 C1 C2 13.5(7) . . . . ? C14 N1 C1 C4 0.8(7) . . . . ? Zr N1 C1 C4 -170.9(4) . . . . ? N1 C1 C2 C3 16.8(9) . . . . ? C4 C1 C2 C3 -159.1(6) . . . . ? C13 N2 C3 C2 160.0(5) . . . . ? Zr N2 C3 C2 -22.9(8) . . . . ? C13 N2 C3 C5 -17.8(8) . . . . ? Zr N2 C3 C5 159.3(4) . . . . ? C1 C2 C3 N2 -12.8(9) . . . . ? C1 C2 C3 C5 165.2(5) . . . . ? C26 N3 C6 C7 -172.6(5) . . . . ? Zr N3 C6 C7 12.6(8) . . . . ? C26 N3 C6 C9 3.4(7) . . . . ? Zr N3 C6 C9 -171.3(4) . . . . ? N3 C6 C7 C8 17.6(10) . . . . ? C9 C6 C7 C8 -158.6(6) . . . . ? C11 N4 C8 C7 162.1(5) . . . . ? Zr N4 C8 C7 -21.6(7) . . . . ? C11 N4 C8 C10 -14.6(8) . . . . ? Zr N4 C8 C10 161.7(4) . . . . ? C6 C7 C8 N4 -13.5(9) . . . . ? C6 C7 C8 C10 163.3(6) . . . . ? C8 N4 C11 C12 -98.7(6) . . . . ? Zr N4 C11 C12 84.6(5) . . . . ? N4 C11 C12 C13 -38.9(7) . . . . ? C3 N2 C13 C12 -96.9(6) . . . . ? Zr N2 C13 C12 85.7(5) . . . . ? C11 C12 C13 N2 -41.9(6) . . . . ? C1 N1 C14 C15 94.1(6) . . . . ? Zr N1 C14 C15 -94.2(5) . . . . ? C1 N1 C14 C19 -83.5(6) . . . . ? Zr N1 C14 C19 88.2(5) . . . . ? C19 C14 C15 C16 -0.4(9) . . . . ? N1 C14 C15 C16 -177.9(5) . . . . ? C19 C14 C15 C20 -179.9(5) . . . . ? N1 C14 C15 C20 2.6(9) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C20 C15 C16 C17 179.7(6) . . . . ? C15 C16 C17 C18 0.2(12) . . . . ? C16 C17 C18 C19 -0.4(12) . . . . ? C17 C18 C19 C14 0.2(10) . . . . ? C17 C18 C19 C23 -178.4(7) . . . . ? C15 C14 C19 C18 0.2(9) . . . . ? N1 C14 C19 C18 177.8(5) . . . . ? C15 C14 C19 C23 178.7(6) . . . . ? N1 C14 C19 C23 -3.7(9) . . . . ? C14 C15 C20 C21 114.9(7) . . . . ? C16 C15 C20 C21 -64.6(8) . . . . ? C14 C15 C20 C22 -122.9(7) . . . . ? C16 C15 C20 C22 57.6(8) . . . . ? C18 C19 C23 C24 54.8(9) . . . . ? C14 C19 C23 C24 -123.7(7) . . . . ? C18 C19 C23 C25 -66.4(9) . . . . ? C14 C19 C23 C25 115.2(7) . . . . ? C6 N3 C26 C27 84.2(6) . . . . ? Zr N3 C26 C27 -101.1(5) . . . . ? C6 N3 C26 C31 -93.6(6) . . . . ? Zr N3 C26 C31 81.1(6) . . . . ? C31 C26 C27 C28 1.2(9) . . . . ? N3 C26 C27 C28 -176.6(6) . . . . ? C31 C26 C27 C32 -176.9(6) . . . . ? N3 C26 C27 C32 5.3(9) . . . . ? C26 C27 C28 C29 -0.6(11) . . . . ? C32 C27 C28 C29 177.6(7) . . . . ? C27 C28 C29 C30 0.4(13) . . . . ? C28 C29 C30 C31 -0.8(13) . . . . ? C29 C30 C31 C26 1.4(11) . . . . ? C29 C30 C31 C35 -180.0(8) . . . . ? C27 C26 C31 C30 -1.6(9) . . . . ? N3 C26 C31 C30 176.2(6) . . . . ? C27 C26 C31 C35 179.9(7) . . . . ? N3 C26 C31 C35 -2.3(10) . . . . ? C28 C27 C32 C34 -77.0(7) . . . . ? C26 C27 C32 C34 101.1(7) . . . . ? C28 C27 C32 C33 47.0(8) . . . . ? C26 C27 C32 C33 -134.9(6) . . . . ? C30 C31 C35 C36 -77.0(10) . . . . ? C26 C31 C35 C36 101.5(8) . . . . ? C30 C31 C35 C37 45.3(10) . . . . ? C26 C31 C35 C37 -136.2(7) . . . . ? C41 C38 C39 C40 161.8(18) . . . . ? C40 C38 C39 C40 -0.9(19) 3_656 . . . ? C38 C39 C40 C38 1(3) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.824 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.077 #===END