Supplementary Material (ESI) for Dalton Transactions This journla is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Danopoulos, Andreas' 'Hursthouse, Michael B.' 'Porter, Robin M.' 'Winston, Scott' _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Chemistry University of Southampton Highfield Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'ad1@soton.ac.uk' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; (Alkyliminomethyl)phenylamido complexes of zirconium and titanium ; _publ_section_references ; ENTER OTHER REFERENCES WinGX - L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838 ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. PLATON/PLUTON - (a) A. L. Spek, Acta Crystallogr., Sect A 1990, 46, C34. (b) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998. ; data_Compound2 _database_code_CSD 181535 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sw003 _chemical_melting_point ? _chemical_formula_moiety 'C34 H54 Li2 N4 Si2' _chemical_formula_sum 'C34 H54 Li2 N4 Si2' _chemical_formula_weight 588.87 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 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 30.959(6) _cell_length_b 9.919(2) _cell_length_c 11.8838(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3649.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23163 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.37 _exptl_crystal_description Blocks _exptl_crystal_colour Clear _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9926 _exptl_absorpt_correction_T_max 0.9938 _exptl_absorpt_process_details 'sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17720 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_sigmaI/netI 0.1039 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4403 _reflns_number_gt 3079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(16) _refine_ls_number_reflns 4403 _refine_ls_number_parameters 387 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 0.805 _refine_ls_restrained_S_all 0.805 _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 C8 C 0.81135(12) 1.2488(4) 0.6738(4) 0.0348(12) Uani 1 1 d . . . H8A H 0.7892 1.1962 0.6345 0.052 Uiso 1 1 calc R . . H8B H 0.8332 1.2793 0.6198 0.052 Uiso 1 1 calc R . . H8C H 0.7979 1.3273 0.7097 0.052 Uiso 1 1 calc R . . C25 C 0.93279(14) 0.4658(5) 1.1275(4) 0.0414(14) Uani 1 1 d . . . H25A H 0.9379 0.3812 1.0870 0.062 Uiso 1 1 calc R . . H25B H 0.9111 0.4511 1.1863 0.062 Uiso 1 1 calc R . . H25C H 0.9598 0.4964 1.1620 0.062 Uiso 1 1 calc R . . C17 C 0.86092(14) 0.9132(5) 0.5663(4) 0.0346(13) Uani 1 1 d . . . H17A H 0.8306 0.9111 0.5899 0.052 Uiso 1 1 calc R . . H17B H 0.8644 0.8609 0.4969 0.052 Uiso 1 1 calc R . . H17C H 0.8697 1.0068 0.5527 0.052 Uiso 1 1 calc R . . C16 C 0.95072(13) 0.8091(5) 0.6191(4) 0.0425(14) Uani 1 1 d . . . H16A H 0.9657 0.8955 0.6104 0.064 Uiso 1 1 calc R . . H16B H 0.9480 0.7653 0.5455 0.064 Uiso 1 1 calc R . . H16C H 0.9673 0.7509 0.6699 0.064 Uiso 1 1 calc R . . C15 C 0.87291(14) 0.6700(5) 0.7176(4) 0.0383(13) Uani 1 1 d . . . H15A H 0.8904 0.6299 0.7777 0.057 Uiso 1 1 calc R . . H15B H 0.8735 0.6111 0.6513 0.057 Uiso 1 1 calc R . . H15C H 0.8431 0.6805 0.7435 0.057 Uiso 1 1 calc R . . C32 C 0.88499(18) 1.0762(5) 1.1239(5) 0.0627(18) Uani 1 1 d . . . H32A H 0.9140 1.0715 1.0910 0.094 Uiso 1 1 calc R . . H32B H 0.8859 1.1297 1.1932 0.094 Uiso 1 1 calc R . . H32C H 0.8652 1.1188 1.0701 0.094 Uiso 1 1 calc R . . C33 C 0.81364(14) 0.9179(5) 1.2372(5) 0.0428(14) Uani 1 1 d . . . H33A H 0.7938 0.9772 1.1962 0.064 Uiso 1 1 calc R . . H33B H 0.8195 0.9561 1.3117 0.064 Uiso 1 1 calc R . . H33C H 0.8005 0.8286 1.2456 0.064 Uiso 1 1 calc R . . C34 C 0.90507(15) 0.8201(6) 1.2540(4) 0.0546(17) Uani 1 1 d . . . H34A H 0.8952 0.7287 1.2719 0.082 Uiso 1 1 calc R . . H34B H 0.9073 0.8728 1.3235 0.082 Uiso 1 1 calc R . . H34C H 0.9334 0.8156 1.2177 0.082 Uiso 1 1 calc R . . N4 N 0.94097(9) 0.6573(3) 0.9964(3) 0.0205(9) Uani 1 1 d . . . C1 C 0.90910(13) 1.0679(4) 0.7958(4) 0.0227(11) Uani 1 1 d . . . C2 C 0.95289(13) 1.1022(5) 0.8126(4) 0.0271(12) Uani 1 1 d . . . H2 H 0.9732 1.0316 0.8233 0.033 Uiso 1 1 calc R . . C3 C 0.96751(13) 1.2341(5) 0.8141(4) 0.0302(12) Uani 1 1 d . . . H3 H 0.9970 1.2529 0.8296 0.036 Uiso 1 1 calc R . . C4 C 0.93922(13) 1.3377(5) 0.7932(4) 0.0281(11) Uani 1 1 d . . . H4 H 0.9491 1.4284 0.7920 0.034 Uiso 1 1 calc R . . C5 C 0.89635(13) 1.3083(5) 0.7739(4) 0.0280(12) Uani 1 1 d . . . H5 H 0.8770 1.3803 0.7586 0.034 Uiso 1 1 calc R . . C6 C 0.88029(12) 1.1766(4) 0.7759(4) 0.0197(10) Uani 1 1 d . . . C23 C 0.86968(13) 0.5714(4) 1.0222(4) 0.0237(11) Uani 1 1 d . . . C22 C 0.84976(15) 0.4473(5) 0.9988(4) 0.0361(13) Uani 1 1 d . . . H22 H 0.8666 0.3674 1.0022 0.043 Uiso 1 1 calc R . . C21 C 0.80683(16) 0.4371(5) 0.9714(5) 0.0418(14) Uani 1 1 d . . . H21 H 0.7946 0.3522 0.9525 0.050 Uiso 1 1 calc R . . C20 C 0.78181(15) 0.5513(5) 0.9715(4) 0.0383(13) Uani 1 1 d . . . H20 H 0.7519 0.5457 0.9539 0.046 Uiso 1 1 calc R . . C19 C 0.80021(12) 0.6744(5) 0.9971(4) 0.0279(12) Uani 1 1 d . . . H19 H 0.7820 0.7515 0.9998 0.033 Uiso 1 1 calc R . . C18 C 0.84416(12) 0.6910(4) 1.0192(4) 0.0227(11) Uani 1 1 d . . . C26 C 0.98804(12) 0.6653(4) 1.0163(4) 0.0242(11) Uani 1 1 d . . . H26 H 0.9939 0.6493 1.0980 0.029 Uiso 1 1 calc R . . C27 C 1.00171(12) 0.8082(4) 0.9859(4) 0.0289(12) Uani 1 1 d . . . H27A H 0.9925 0.8280 0.9079 0.035 Uiso 1 1 calc R . . H27B H 0.9868 0.8726 1.0364 0.035 Uiso 1 1 calc R . . C28 C 1.05029(13) 0.8289(5) 0.9955(4) 0.0336(13) Uani 1 1 d . . . H28A H 1.0590 0.8224 1.0754 0.040 Uiso 1 1 calc R . . H28B H 1.0578 0.9204 0.9684 0.040 Uiso 1 1 calc R . . C29 C 1.07501(13) 0.7249(5) 0.9272(5) 0.0395(14) Uani 1 1 d . . . H29A H 1.1064 0.7363 0.9403 0.047 Uiso 1 1 calc R . . H29B H 1.0694 0.7392 0.8461 0.047 Uiso 1 1 calc R . . C30 C 1.06161(13) 0.5828(5) 0.9599(5) 0.0388(13) Uani 1 1 d . . . H30A H 1.0769 0.5169 0.9116 0.047 Uiso 1 1 calc R . . H30B H 1.0700 0.5653 1.0390 0.047 Uiso 1 1 calc R . . C31 C 1.01331(12) 0.5639(4) 0.9470(4) 0.0321(13) Uani 1 1 d . . . H31A H 1.0054 0.4716 0.9710 0.038 Uiso 1 1 calc R . . H31B H 1.0054 0.5738 0.8668 0.038 Uiso 1 1 calc R . . C9 C 0.76489(13) 1.0729(5) 0.8255(5) 0.0423(15) Uani 1 1 d . . . H9 H 0.7530 1.1534 0.7855 0.051 Uiso 1 1 calc R . . C14 C 0.75168(14) 0.9464(6) 0.7636(5) 0.0524(17) Uani 1 1 d . . . H14A H 0.7615 0.9523 0.6845 0.063 Uiso 1 1 calc R . . H14B H 0.7660 0.8676 0.7986 0.063 Uiso 1 1 calc R . . C10 C 0.74798(15) 1.0707(5) 0.9468(5) 0.0511(16) Uani 1 1 d . . . H10A H 0.7620 0.9964 0.9886 0.061 Uiso 1 1 calc R . . H10B H 0.7556 1.1565 0.9844 0.061 Uiso 1 1 calc R . . C11 C 0.69917(17) 1.0516(7) 0.9496(7) 0.084(2) Uani 1 1 d . . . H11A H 0.6849 1.1313 0.9159 0.101 Uiso 1 1 calc R . . H11B H 0.6894 1.0439 1.0287 0.101 Uiso 1 1 calc R . . C12 C 0.68610(16) 0.9263(7) 0.8856(6) 0.077(2) Uani 1 1 d . . . H12A H 0.6974 0.8460 0.9254 0.092 Uiso 1 1 calc R . . H12B H 0.6542 0.9199 0.8845 0.092 Uiso 1 1 calc R . . C13 C 0.70265(16) 0.9257(7) 0.7661(6) 0.085(2) Uani 1 1 d . . . H13A H 0.6884 0.9984 0.7229 0.102 Uiso 1 1 calc R . . H13B H 0.6954 0.8386 0.7301 0.102 Uiso 1 1 calc R . . C7 C 0.83263(13) 1.1617(4) 0.7629(4) 0.0237(11) Uani 1 1 d . . . C24 C 0.91673(14) 0.5715(4) 1.0463(4) 0.0247(12) Uani 1 1 d . . . N1 N 0.89619(10) 0.9320(3) 0.7999(3) 0.0217(9) Uani 1 1 d . . . N2 N 0.81199(10) 1.0822(4) 0.8294(3) 0.0290(10) Uani 1 1 d . . . N3 N 0.86112(10) 0.8214(3) 1.0314(3) 0.0222(9) Uani 1 1 d . . . Si2 Si 0.86559(3) 0.90239(12) 1.15674(11) 0.0280(3) Uani 1 1 d . . . Si1 Si 0.89549(3) 0.83876(12) 0.67962(11) 0.0273(3) Uani 1 1 d . . . Li2 Li 0.9125(2) 0.8175(7) 0.9298(6) 0.0262(18) Uani 1 1 d . . . Li1 Li 0.8455(2) 0.9380(8) 0.9027(7) 0.032(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C8 0.024(2) 0.041(3) 0.039(3) 0.016(3) -0.002(3) 0.000(2) C25 0.041(3) 0.038(3) 0.045(4) 0.018(3) 0.004(3) 0.006(2) C17 0.036(3) 0.043(3) 0.024(3) 0.002(3) -0.003(2) -0.001(2) C16 0.045(3) 0.042(3) 0.041(4) 0.000(3) 0.004(3) 0.011(2) C15 0.060(3) 0.027(3) 0.027(3) 0.001(3) 0.000(2) -0.004(3) C32 0.087(4) 0.047(4) 0.054(4) -0.019(3) 0.012(3) -0.027(3) C33 0.044(3) 0.046(4) 0.039(3) -0.001(3) 0.007(3) 0.006(2) C34 0.043(3) 0.090(5) 0.031(4) -0.011(3) -0.004(3) 0.022(3) N4 0.020(2) 0.019(2) 0.023(2) -0.003(2) -0.0027(17) 0.0009(16) C1 0.026(3) 0.023(3) 0.019(3) -0.002(2) 0.006(2) 0.000(2) C2 0.017(2) 0.031(3) 0.033(3) 0.002(3) 0.007(2) 0.004(2) C3 0.025(3) 0.036(3) 0.030(3) 0.002(3) -0.004(2) -0.010(2) C4 0.032(3) 0.023(3) 0.029(3) 0.000(3) 0.003(2) -0.010(2) C5 0.032(3) 0.024(3) 0.028(3) 0.002(2) 0.004(2) 0.004(2) C6 0.023(2) 0.021(3) 0.015(3) 0.001(2) 0.002(2) 0.000(2) C23 0.025(3) 0.029(3) 0.017(3) 0.003(2) 0.009(2) -0.001(2) C22 0.038(3) 0.025(3) 0.045(4) -0.003(3) 0.016(3) 0.001(2) C21 0.044(3) 0.029(3) 0.052(4) -0.013(3) 0.014(3) -0.018(3) C20 0.032(3) 0.047(4) 0.036(3) -0.002(3) 0.004(2) -0.012(3) C19 0.023(3) 0.026(3) 0.034(3) -0.002(3) 0.006(2) 0.001(2) C18 0.021(2) 0.030(3) 0.017(3) 0.004(2) 0.003(2) -0.002(2) C26 0.024(2) 0.024(3) 0.025(3) 0.001(2) -0.004(2) 0.000(2) C27 0.022(3) 0.030(3) 0.035(3) -0.005(3) 0.001(2) 0.005(2) C28 0.028(3) 0.039(3) 0.034(3) 0.002(3) -0.003(2) 0.000(2) C29 0.022(3) 0.053(4) 0.044(4) -0.011(3) 0.003(2) -0.002(2) C30 0.029(3) 0.037(3) 0.050(4) -0.010(3) -0.001(3) 0.003(2) C31 0.030(3) 0.024(3) 0.043(3) -0.006(2) -0.003(2) 0.004(2) C9 0.018(3) 0.048(4) 0.060(4) 0.036(3) 0.002(3) 0.010(2) C14 0.032(3) 0.080(5) 0.045(4) 0.018(4) -0.009(3) -0.013(3) C10 0.040(3) 0.036(3) 0.078(5) 0.005(3) 0.027(3) 0.007(2) C11 0.042(4) 0.075(5) 0.134(7) 0.048(5) 0.040(4) 0.019(3) C12 0.019(3) 0.115(6) 0.098(6) 0.057(5) 0.006(3) -0.020(3) C13 0.036(3) 0.139(7) 0.079(6) 0.053(5) -0.019(3) -0.041(4) C7 0.024(2) 0.018(3) 0.029(3) -0.003(3) 0.005(2) 0.002(2) C24 0.034(3) 0.016(3) 0.025(3) 0.003(2) 0.003(2) 0.004(2) N1 0.0224(19) 0.016(2) 0.026(2) 0.0055(19) 0.0003(17) 0.0010(16) N2 0.018(2) 0.026(2) 0.044(3) 0.005(2) 0.0043(18) 0.0001(17) N3 0.024(2) 0.020(2) 0.022(2) 0.0018(19) 0.0009(17) -0.0002(17) Si2 0.0265(7) 0.0302(8) 0.0272(8) -0.0022(7) 0.0027(7) -0.0015(5) Si1 0.0337(7) 0.0225(7) 0.0256(8) 0.0013(7) 0.0027(7) 0.0010(6) Li2 0.024(4) 0.033(5) 0.022(5) 0.005(4) 0.002(3) -0.002(3) Li1 0.020(4) 0.038(5) 0.038(6) 0.014(4) 0.005(4) 0.001(3) _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 C8 C7 1.517(6) . ? C25 C24 1.510(6) . ? C17 Si1 1.872(5) . ? C16 Si1 1.878(4) . ? C15 Si1 1.869(5) . ? C32 Si2 1.867(5) . ? C33 Si2 1.877(5) . ? C34 Si2 1.870(5) . ? N4 C24 1.280(5) . ? N4 C26 1.479(5) . ? N4 Li2 1.982(8) . ? C1 N1 1.407(5) . ? C1 C2 1.412(5) . ? C1 C6 1.419(5) . ? C1 Li1 2.674(8) . ? C2 C3 1.385(6) . ? C3 C4 1.373(6) . ? C4 C5 1.378(5) . ? C5 C6 1.398(6) . ? C6 C7 1.491(5) . ? C23 C22 1.404(6) . ? C23 C18 1.426(6) . ? C23 C24 1.484(6) . ? C22 C21 1.372(6) . ? C21 C20 1.372(6) . ? C20 C19 1.382(6) . ? C19 C18 1.395(5) . ? C18 N3 1.404(5) . ? C18 Li2 2.679(8) . ? C26 C31 1.517(6) . ? C26 C27 1.523(5) . ? C27 C28 1.522(5) . ? C28 C29 1.519(6) . ? C29 C30 1.520(6) . ? C30 C31 1.515(5) . ? C9 N2 1.462(5) . ? C9 C14 1.510(7) . ? C9 C10 1.533(7) . ? C14 C13 1.532(6) . ? C10 C11 1.523(7) . ? C11 C12 1.513(8) . ? C12 C13 1.509(9) . ? C7 N2 1.287(5) . ? N1 Si1 1.703(4) . ? N1 Li1 1.989(8) . ? N1 Li2 1.982(8) . ? N2 Li1 1.970(8) . ? N3 Si2 1.698(4) . ? N3 Li2 1.997(8) . ? N3 Li1 1.978(8) . ? Si2 Li1 3.103(8) . ? Si2 Li2 3.176(7) . ? Si1 Li2 3.027(8) . ? Li2 Li1 2.415(9) . ? 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 C24 N4 C26 122.6(4) . . ? C24 N4 Li2 117.2(3) . . ? C26 N4 Li2 117.3(3) . . ? N1 C1 C2 119.9(4) . . ? N1 C1 C6 123.7(4) . . ? C2 C1 C6 116.4(4) . . ? N1 C1 Li1 46.6(2) . . ? C2 C1 Li1 139.1(3) . . ? C6 C1 Li1 89.0(3) . . ? C3 C2 C1 122.9(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 119.1(4) . . ? C6 C5 C4 122.5(4) . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C7 116.3(4) . . ? C1 C6 C7 124.3(4) . . ? C22 C23 C18 118.8(4) . . ? C22 C23 C24 118.0(4) . . ? C18 C23 C24 123.2(4) . . ? C21 C22 C23 122.5(4) . . ? C20 C21 C22 119.0(5) . . ? C21 C20 C19 119.8(4) . . ? C18 C19 C20 123.2(4) . . ? C19 C18 N3 119.5(4) . . ? C19 C18 C23 116.5(4) . . ? N3 C18 C23 123.9(3) . . ? C19 C18 Li2 138.7(4) . . ? N3 C18 Li2 46.7(2) . . ? C23 C18 Li2 87.8(3) . . ? N4 C26 C31 112.7(3) . . ? N4 C26 C27 106.6(3) . . ? C31 C26 C27 110.2(4) . . ? C28 C27 C26 112.5(3) . . ? C27 C28 C29 111.5(4) . . ? C28 C29 C30 110.9(4) . . ? C31 C30 C29 111.0(4) . . ? C30 C31 C26 111.9(4) . . ? N2 C9 C14 109.8(4) . . ? N2 C9 C10 108.1(4) . . ? C14 C9 C10 110.7(4) . . ? C13 C14 C9 111.7(5) . . ? C11 C10 C9 111.2(5) . . ? C10 C11 C12 110.9(5) . . ? C13 C12 C11 112.7(5) . . ? C12 C13 C14 110.7(5) . . ? N2 C7 C6 119.2(4) . . ? N2 C7 C8 124.2(4) . . ? C6 C7 C8 116.5(4) . . ? N4 C24 C23 119.1(4) . . ? N4 C24 C25 124.4(4) . . ? C23 C24 C25 116.5(4) . . ? C1 N1 Si1 119.6(3) . . ? C1 N1 Li1 102.5(3) . . ? Si1 N1 Li1 121.5(3) . . ? C1 N1 Li2 120.3(4) . . ? Si1 N1 Li2 110.3(3) . . ? Li1 N1 Li2 74.9(3) . . ? C7 N2 C9 121.0(4) . . ? C7 N2 Li1 117.1(3) . . ? C9 N2 Li1 119.6(4) . . ? C18 N3 Si2 123.9(3) . . ? C18 N3 Li2 102.5(3) . . ? Si2 N3 Li2 118.3(3) . . ? C18 N3 Li1 111.6(3) . . ? Si2 N3 Li1 115.0(3) . . ? Li2 N3 Li1 74.8(3) . . ? N3 Si2 C34 112.9(2) . . ? N3 Si2 C32 106.2(2) . . ? C34 Si2 C32 108.8(3) . . ? N3 Si2 C33 114.6(2) . . ? C34 Si2 C33 106.3(2) . . ? C32 Si2 C33 107.8(2) . . ? N3 Si2 Li1 35.30(18) . . ? C34 Si2 Li1 141.5(2) . . ? C32 Si2 Li1 75.9(2) . . ? C33 Si2 Li1 108.3(2) . . ? N3 Si2 Li2 33.61(16) . . ? C34 Si2 Li2 96.3(2) . . ? C32 Si2 Li2 85.4(2) . . ? C33 Si2 Li2 147.7(2) . . ? Li1 Si2 Li2 45.22(17) . . ? N1 Si1 C15 106.8(2) . . ? N1 Si1 C17 113.4(2) . . ? C15 Si1 C17 108.2(2) . . ? N1 Si1 C16 113.3(2) . . ? C15 Si1 C16 107.0(2) . . ? C17 Si1 C16 107.9(2) . . ? N1 Si1 Li2 37.90(18) . . ? C15 Si1 Li2 76.4(2) . . ? C17 Si1 Li2 146.5(2) . . ? C16 Si1 Li2 101.9(2) . . ? N3 Li2 N1 104.9(3) . . ? N3 Li2 N4 97.4(3) . . ? N1 Li2 N4 152.1(4) . . ? N3 Li2 Li1 52.2(3) . . ? N1 Li2 Li1 52.7(2) . . ? N4 Li2 Li1 146.3(4) . . ? N3 Li2 C18 30.76(16) . . ? N1 Li2 C18 112.1(3) . . ? N4 Li2 C18 79.5(3) . . ? Li1 Li2 C18 66.8(2) . . ? N3 Li2 Si1 117.0(3) . . ? N1 Li2 Si1 31.85(16) . . ? N4 Li2 Si1 121.7(3) . . ? Li1 Li2 Si1 71.6(3) . . ? C18 Li2 Si1 106.5(2) . . ? N3 Li2 Si2 28.07(15) . . ? N1 Li2 Si2 113.1(3) . . ? N4 Li2 Si2 94.4(3) . . ? Li1 Li2 Si2 65.8(2) . . ? C18 Li2 Si2 55.02(16) . . ? Si1 Li2 Si2 137.4(2) . . ? N2 Li1 N1 99.6(4) . . ? N2 Li1 N3 153.5(4) . . ? N1 Li1 N3 105.4(3) . . ? N2 Li1 Li2 150.6(4) . . ? N1 Li1 Li2 52.4(3) . . ? N3 Li1 Li2 53.0(3) . . ? N2 Li1 C1 80.1(3) . . ? N1 Li1 C1 30.92(16) . . ? N3 Li1 C1 118.0(3) . . ? Li2 Li1 C1 70.7(2) . . ? N2 Li1 Si2 128.2(4) . . ? N1 Li1 Si2 115.9(3) . . ? N3 Li1 Si2 29.74(16) . . ? Li2 Li1 Si2 69.0(2) . . ? C1 Li1 Si2 111.7(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.173 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.044 #==END data_Compound4 _database_code_CSD 181536 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 97WIL019 _chemical_melting_point ? _chemical_formula_moiety 'C14 H23 Cl3 N2 Si Zr' _chemical_formula_sum 'C14 H23 Cl3 N2 Si Zr' _chemical_formula_weight 445.00 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' 'Si' 'Si' 0.0817 0.0704 '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' -2.9650 0.5600 '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 15.31(5) _cell_length_b 8.01(3) _cell_length_c 17.37(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.47(15) _cell_angle_gamma 90.00 _cell_volume 2021(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7052 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 24.82 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 1.515 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'FAST TV area detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7052 _diffrn_reflns_av_R_equivalents 0.1360 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 24.82 _reflns_number_total 2892 _reflns_number_gt 2892 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4627 _refine_ls_number_parameters 196 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.1433 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 0.438 _refine_ls_restrained_S_all 0.438 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.228189(0) 0.248676(1) 0.133818(0) 0.02485(0) Uani 1 1 d . . . Cl1 Cl 0.224970(2) -0.009773(2) 0.206529(1) 0.05436(1) Uani 1 1 d . . . Cl2 Cl 0.340349(1) 0.155940(2) 0.074321(1) 0.03825(0) Uani 1 1 d . . . Cl3 Cl 0.072093(1) 0.204125(3) 0.046957(1) 0.04606(0) Uani 1 1 d . . . Si1 Si 0.387562(1) 0.400464(3) 0.311717(1) 0.03212(0) Uani 1 1 d . . . N1 N 0.278259(3) 0.381502(6) 0.238011(3) 0.01996(1) Uani 1 1 d . . . N2 N 0.206491(4) 0.517296(6) 0.078731(3) 0.02249(1) Uani 1 1 d . . . C1 C 0.196708(4) 0.444092(7) 0.247259(4) 0.02118(1) Uani 1 1 d . . . C2 C 0.171035(5) 0.410789(8) 0.316189(4) 0.02668(1) Uani 1 1 d . . . H2 H 0.2095 0.3460 0.3576 0.032 Uiso 1 1 calc R . . C3 C 0.089553(5) 0.471972(9) 0.324399(4) 0.03181(1) Uani 1 1 d . . . H3 H 0.0745 0.4472 0.3710 0.038 Uiso 1 1 calc R . . C4 C 0.031259(5) 0.567862(10) 0.265163(5) 0.03604(2) Uani 1 1 d . . . H4 H -0.0233 0.6078 0.2710 0.043 Uiso 1 1 calc R . . C5 C 0.054477(5) 0.604448(9) 0.196826(4) 0.03209(1) Uani 1 1 d . . . H5 H 0.0155 0.6717 0.1569 0.039 Uiso 1 1 calc R . . C6 C 0.135504(4) 0.542981(7) 0.185615(4) 0.02375(1) Uani 1 1 d . . . C7 C 0.157906(4) 0.599205(8) 0.113098(4) 0.02718(1) Uani 1 1 d . . . H7 H 0.1348 0.7020 0.0909 0.033 Uiso 1 1 calc R . . C8 C 0.390379(5) 0.601406(12) 0.367183(6) 0.05099(2) Uani 1 1 d . . . H8A H 0.4509 0.6185 0.4048 0.076 Uiso 1 1 calc R . . H8B H 0.3465 0.5970 0.3962 0.076 Uiso 1 1 calc R . . H8C H 0.3752 0.6919 0.3290 0.076 Uiso 1 1 calc R . . C9 C 0.411688(6) 0.225829(14) 0.383767(6) 0.05839(3) Uani 1 1 d . . . H9A H 0.4758 0.2261 0.4151 0.088 Uiso 1 1 calc R . . H9B H 0.3966 0.1225 0.3545 0.088 Uiso 1 1 calc R . . H9C H 0.3753 0.2375 0.4194 0.088 Uiso 1 1 calc R . . C10 C 0.473598(5) 0.403666(9) 0.255815(4) 0.03318(1) Uani 1 1 d . . . H10A H 0.5338 0.4250 0.2933 0.050 Uiso 1 1 calc R . . H10B H 0.4578 0.4900 0.2154 0.050 Uiso 1 1 calc R . . H10C H 0.4735 0.2976 0.2300 0.050 Uiso 1 1 calc R . . C11 C 0.230719(4) 0.593068(8) 0.008846(4) 0.02277(1) Uani 1 1 d . . . C12 C 0.188858(5) 0.763185(11) -0.015565(5) 0.04616(2) Uani 1 1 d . . . H12A H 0.1233 0.7567 -0.0274 0.069 Uiso 1 1 calc R . . H12B H 0.2027 0.8006 -0.0629 0.069 Uiso 1 1 calc R . . H12C H 0.2139 0.8406 0.0281 0.069 Uiso 1 1 calc R . . C13 C 0.196407(6) 0.473033(12) -0.061422(5) 0.04811(2) Uani 1 1 d . . . H13A H 0.1305 0.4799 -0.0831 0.072 Uiso 1 1 calc R . . H13B H 0.2140 0.3613 -0.0429 0.072 Uiso 1 1 calc R . . H13C H 0.2229 0.5016 -0.1029 0.072 Uiso 1 1 calc R . . C14 C 0.333574(5) 0.609447(10) 0.036070(5) 0.04109(2) Uani 1 1 d . . . H14A H 0.3522 0.6969 0.0757 0.062 Uiso 1 1 calc R . . H14B H 0.3533 0.6359 -0.0097 0.062 Uiso 1 1 calc R . . H14C H 0.3610 0.5060 0.0597 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.02624(0) 0.02420(0) 0.02759(0) -0.00296(0) 0.01349(0) -0.00294(0) Cl1 0.09096(2) 0.03202(1) 0.04542(1) 0.00634(1) 0.02917(1) -0.01344(1) Cl2 0.03876(1) 0.03850(1) 0.04591(1) 0.00028(1) 0.02535(1) 0.00973(1) Cl3 0.03005(1) 0.05637(1) 0.04871(1) -0.01790(1) 0.00817(1) -0.01314(1) Si1 0.02300(1) 0.04439(1) 0.02931(1) -0.00552(1) 0.00876(1) 0.00008(1) N1 0.01646(2) 0.01635(2) 0.02716(3) -0.00661(2) 0.00704(2) 0.00710(2) N2 0.02929(3) 0.01833(2) 0.02117(2) -0.00113(2) 0.00986(2) -0.00338(2) C1 0.02047(3) 0.01835(3) 0.02518(3) -0.00319(2) 0.00786(2) -0.00382(2) C2 0.03501(3) 0.03241(3) 0.01251(3) -0.00636(2) 0.00735(2) -0.00566(3) C3 0.03030(3) 0.04872(4) 0.02061(3) -0.00623(3) 0.01402(3) -0.01002(3) C4 0.02202(3) 0.05147(4) 0.03780(4) -0.01207(3) 0.01398(3) -0.00846(3) C5 0.02706(3) 0.03202(3) 0.03742(4) -0.00573(3) 0.01052(3) -0.00225(3) C6 0.02290(3) 0.02097(3) 0.02837(3) -0.00842(2) 0.00954(2) -0.00273(2) C7 0.02306(3) 0.02596(3) 0.03141(3) -0.00809(3) 0.00705(3) -0.00236(2) C8 0.02978(4) 0.06719(6) 0.05099(5) -0.02196(4) 0.00569(4) -0.00729(4) C9 0.04364(5) 0.08822(7) 0.04707(5) 0.01642(5) 0.01970(4) 0.01099(5) C10 0.02988(3) 0.03814(4) 0.02916(3) -0.00369(3) 0.00598(3) -0.00258(3) C11 0.02017(3) 0.02816(3) 0.01997(3) 0.00336(2) 0.00637(2) 0.00653(2) C12 0.03403(4) 0.06251(5) 0.04656(5) 0.03089(4) 0.01933(3) 0.00838(4) C13 0.05370(5) 0.06195(5) 0.02815(4) 0.00189(4) 0.01222(4) -0.01046(4) C14 0.03147(4) 0.04706(4) 0.04225(4) 0.01230(3) 0.00814(3) -0.01198(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.029(4) . ? Zr1 N2 2.335(7) . ? Zr1 Cl2 2.386(6) . ? Zr1 Cl3 2.415(8) . ? Zr1 Cl1 2.434(6) . ? Zr1 C1 2.677(5) . ? Si1 N1 1.762(5) . ? Si1 C9 1.835(4) . ? Si1 C10 1.868(5) . ? Si1 C8 1.869(5) . ? N1 C1 1.401(4) . ? N2 C7 1.273(3) . ? N2 C11 1.505(3) . ? C1 C2 1.399(3) . ? C1 C6 1.420(3) . ? C2 C3 1.389(4) . ? C3 C4 1.365(3) . ? C4 C5 1.374(2) . ? C5 C6 1.405(4) . ? C6 C7 1.477(3) . ? C11 C14 1.500(5) . ? C11 C12 1.508(4) . ? C11 C13 1.511(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 N1 Zr1 N2 81.19(19) . . ? N1 Zr1 Cl2 115.42(18) . . ? N2 Zr1 Cl2 97.92(11) . . ? N1 Zr1 Cl3 130.87(10) . . ? N2 Zr1 Cl3 84.03(10) . . ? Cl2 Zr1 Cl3 112.9(2) . . ? N1 Zr1 Cl1 92.7(2) . . ? N2 Zr1 Cl1 166.58(4) . . ? Cl2 Zr1 Cl1 95.49(14) . . ? Cl3 Zr1 Cl1 91.13(11) . . ? N1 Zr1 C1 30.91(12) . . ? N2 Zr1 C1 74.19(18) . . ? Cl2 Zr1 C1 145.38(8) . . ? Cl3 Zr1 C1 99.96(18) . . ? Cl1 Zr1 C1 94.4(2) . . ? N1 Si1 C9 111.68(12) . . ? N1 Si1 C10 106.7(2) . . ? C9 Si1 C10 110.02(12) . . ? N1 Si1 C8 108.07(10) . . ? C9 Si1 C8 109.8(2) . . ? C10 Si1 C8 110.56(9) . . ? C1 N1 Si1 124.16(19) . . ? C1 N1 Zr1 101.03(18) . . ? Si1 N1 Zr1 134.17(10) . . ? C7 N2 C11 120.02(17) . . ? C7 N2 Zr1 108.12(15) . . ? C11 N2 Zr1 131.50(5) . . ? C2 C1 N1 122.15(13) . . ? C2 C1 C6 117.03(18) . . ? N1 C1 C6 120.82(15) . . ? C2 C1 Zr1 133.11(15) . . ? N1 C1 Zr1 48.06(10) . . ? C6 C1 Zr1 90.05(19) . . ? C3 C2 C1 121.71(13) . . ? C4 C3 C2 121.01(15) . . ? C3 C4 C5 119.00(17) . . ? C4 C5 C6 121.78(13) . . ? C5 C6 C1 119.47(15) . . ? C5 C6 C7 117.74(13) . . ? C1 C6 C7 122.49(18) . . ? N2 C7 C6 124.81(15) . . ? C14 C11 N2 106.47(16) . . ? C14 C11 C12 108.66(13) . . ? N2 C11 C12 113.56(12) . . ? C14 C11 C13 111.84(11) . . ? N2 C11 C13 106.47(18) . . ? C12 C11 C13 109.85(19) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.027 _refine_diff_density_min -0.017 _refine_diff_density_rms 0.003 #==END data_Compound6 _database_code_CSD 181537 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 97wil014 _chemical_melting_point ? _chemical_formula_moiety 'C28 H45 Cl2 N4 Si2 Zr' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C28 H45 Cl2 N4 Si2 Zr' _chemical_formula_weight 655.98 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 18.111(3) _cell_length_b 15.285(3) _cell_length_c 24.458(6) _cell_angle_alpha 90 _cell_angle_beta 97.460(15) _cell_angle_gamma 90 _cell_volume 6713(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150 _cell_measurement_reflns_used 23008 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 25.05 _cell_special_details ; ? ; _exptl_crystal_description ' Prisms ' _exptl_crystal_colour ' Orange ' _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.581 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # cylinder 'cylindrical' # empirical 'empirical from intensities' # gaussian 'Gaussian from crystal shape' # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # refdelf 'refined from delta-F' # sphere 'spherical' _exptl_absorpt_correction_type ' multi-scan ' # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.9069 _exptl_absorpt_correction_T_max 0.9623 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'FAST TV area detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 23008 _diffrn_reflns_av_R_equivalents 0.2000 _diffrn_reflns_av_sigmaI/netI 0.0103 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _reflns_number_total 9770 _reflns_number_gt 9548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ' direct ' _atom_sites_solution_secondary ' difmap ' _atom_sites_solution_hydrogens ' geom ' _refine_ls_hydrogen_treatment 'mixed ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 9770 _refine_ls_number_parameters 691 _refine_ls_number_restraints 90 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.2800 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 0.412 _refine_ls_restrained_S_all 1.715 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.444 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.020 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Zr1 Zr Uani 0.23045 0.55255 0.37100 1.000 0.0310 . . Cl1 Cl Uani 0.24076 0.63031 0.45757 1.000 0.0440 . . Cl2 Cl Uani 0.24626 0.68598 0.31530 1.000 0.0525 . . Si1 Si Uani 0.42303 0.58150 0.38127 1.000 0.0490 . . Si2 Si Uani 0.17988 0.41239 0.47069 1.000 0.0457 . . N1 N Uani 0.09481 0.58485 0.35500 1.000 0.0406 . . N2 N Uani 0.18509 0.43834 0.40112 1.000 0.0179 . . N3 N Uani 0.34033 0.51784 0.38232 1.000 0.0275 . . N4 N Uani 0.23513 0.47177 0.28473 1.000 0.0362 . . C1 C Uani 0.13762 0.39418 0.36347 1.000 0.0255 . . C2 C Uani 0.14751 0.30520 0.35558 1.000 0.0323 . . C3 C Uani 0.10266 0.25329 0.31892 1.000 0.0471 . . C4 C Uani 0.04038 0.29215 0.28676 1.000 0.0508 . . C5 C Uani 0.02661 0.38223 0.29422 1.000 0.0483 . . C6 C Uani 0.07277 0.42868 0.33169 1.000 0.0222 . . C7 C Uani 0.04951 0.52123 0.33626 1.000 0.0263 . . C8 C Uani 0.05185 0.66999 0.35848 1.000 0.0448 . . C9 C Uani 0.03364 0.70773 0.30090 1.000 0.0730 . . C10 C Uani -0.01674 0.65839 0.38595 1.000 0.0971 . . C11 C Uani 0.09814 0.74106 0.39329 1.000 0.0576 . . C12 C Uani 0.10093 0.47710 0.49187 1.000 0.0816 . . C13 C Uani 0.16125 0.29145 0.48009 1.000 0.0619 . . C14 C Uani 0.27126 0.43428 0.51730 1.000 0.0531 . . C15 C Uani 0.35472 0.42432 0.38306 1.000 0.0286 . . C16 C Uani 0.39259 0.38412 0.42842 1.000 0.0391 . . C17 C Uani 0.40141 0.29052 0.43160 1.000 0.0542 . . C18 C Uani 0.37222 0.24253 0.38778 1.000 0.0344 . . C19 C Uani 0.33213 0.28194 0.34020 1.000 0.0424 . . C20 C Uani 0.32022 0.36908 0.33930 1.000 0.0300 . . C21 C Uani 0.27594 0.40255 0.29154 1.000 0.0373 . . C22 C Uani 0.20380 0.48656 0.22511 1.000 0.0491 . . C23 C Uani 0.17926 0.40935 0.19059 1.000 0.0613 . . C24 C Uani 0.13328 0.55100 0.22560 1.000 0.0635 . . C25 C Uani 0.26589 0.54318 0.20088 1.000 0.0522 . . C26 C Uani 0.43944 0.59960 0.30896 1.000 0.0727 . . C27 C Uani 0.41064 0.68890 0.41529 1.000 0.0760 . . C28 C Uani 0.50960 0.53720 0.41517 1.000 0.0632 . . Zr2 Zr Uani 0.72514 0.04525 0.34106 1.000 0.0343 . . Cl3 Cl Uani 0.60426 0.05447 0.27994 1.000 0.0411 . . Cl4 Cl Uani 0.75298 -0.09710 0.30436 1.000 0.0589 . . Si3 Si Uani 0.91319 0.00333 0.38435 1.000 0.0518 . . Si4 Si Uani 0.61053 -0.08838 0.40966 1.000 0.0960 . . N5 N Uani 0.77908 0.11850 0.26244 1.000 0.0331 . . N6 N Uani 0.83330 0.06938 0.37595 1.000 0.0260 . . N7 N Uani 0.68674 0.17241 0.38631 1.000 0.0343 . . N8 N Uani 0.68407 -0.01441 0.40850 1.000 0.0382 . . C30 C Uani 0.85031 0.16208 0.37900 1.000 0.0285 . . C31 C Uani 0.87926 0.20544 0.42863 1.000 0.0415 . . C32 C Uani 0.89609 0.29281 0.43251 1.000 0.0594 . . C33 C Uani 0.88820 0.34605 0.38644 1.000 0.0483 . . C34 C Uani 0.86138 0.30251 0.33668 1.000 0.0437 . . C35 C Uani 0.84386 0.21974 0.33212 1.000 0.0316 . . C36 C Uani 0.81974 0.18689 0.27552 1.000 0.0478 . . C37 C Uani 0.76760 0.10347 0.19982 1.000 0.0424 . . C38 C Uani 0.73079 0.01411 0.18666 1.000 0.0492 . . C39 C Uani 0.84507 0.10224 0.17879 1.000 0.0427 . . C40 C Uani 0.71721 0.17452 0.17312 1.000 0.0473 . . C41 C Uani 0.99368 0.05549 0.42563 1.000 0.0626 . . C42 C Uani 0.94598 -0.01314 0.31449 1.000 0.0647 . . C43 C Uani 0.89598 -0.10128 0.41868 1.000 0.0702 . . C44 C Uani 0.72230 0.01392 0.46178 1.000 0.0483 . . C45 C Uani 0.75541 -0.05248 0.49977 1.000 0.0380 . . C46 C Uani 0.78973 -0.02514 0.54868 1.000 0.0685 . . C47 C Uani 0.79677 0.06244 0.56460 1.000 0.0456 . . C48 C Uani 0.76541 0.12721 0.52811 1.000 0.0473 . . C49 C Uani 0.72954 0.10273 0.47475 1.000 0.0371 . . C50 C Uani 0.69586 0.17440 0.43964 1.000 0.0370 . . C51 C Uani 0.64294 0.25401 0.36192 1.000 0.0409 . . C52 C Uani 0.55765 0.23698 0.36448 1.000 0.0677 . . C53 C Uani 0.66989 0.33844 0.39576 1.000 0.0611 . . C54 C Uani 0.65279 0.27191 0.30196 1.000 0.0356 . . C55 C Uani 0.57316 -0.13058 0.34986 1.000 0.1012 . . C56 C Uani 0.53419 -0.01615 0.42945 1.000 0.3108 . . C57 C Uani 0.61092 -0.14690 0.46582 1.000 0.3273 . . H2 H Uiso 0.18761 0.27842 0.37672 1.000 0.0387 . . H3 H Uiso 0.11303 0.19412 0.31537 1.000 0.0565 . . H4 H Uiso 0.00933 0.25920 0.26137 1.000 0.0609 . . H5 H Uiso -0.01374 0.40940 0.27362 1.000 0.0580 . . H9A H Uiso 0.07863 0.72745 0.28797 1.000 0.1095 . . H9B H Uiso 0.00005 0.75614 0.30181 1.000 0.1095 . . H9C H Uiso 0.01073 0.66348 0.27650 1.000 0.1095 . . H10A H Uiso -0.00310 0.63671 0.42271 1.000 0.1457 . . H10B H Uiso -0.04949 0.61737 0.36531 1.000 0.1457 . . H10C H Uiso -0.04162 0.71364 0.38742 1.000 0.1457 . . H11A H Uiso 0.10977 0.72100 0.43061 1.000 0.0864 . . H11B H Uiso 0.06974 0.79415 0.39278 1.000 0.0864 . . H11C H Uiso 0.14345 0.75186 0.37795 1.000 0.0864 . . H12A H Uiso 0.09463 0.46281 0.52921 1.000 0.1225 . . H12B H Uiso 0.05609 0.46337 0.46799 1.000 0.1225 . . H12C H Uiso 0.11146 0.53841 0.48931 1.000 0.1225 . . H13A H Uiso 0.16196 0.27891 0.51862 1.000 0.0929 . . H13B H Uiso 0.19902 0.25765 0.46568 1.000 0.0929 . . H13C H Uiso 0.11334 0.27664 0.46072 1.000 0.0929 . . H14A H Uiso 0.29375 0.37965 0.52959 1.000 0.0797 . . H14B H Uiso 0.26138 0.46806 0.54864 1.000 0.0797 . . H14C H Uiso 0.30450 0.46612 0.49706 1.000 0.0797 . . H16 H Uiso 0.41318 0.41829 0.45799 1.000 0.0470 . . H17 H Uiso 0.42644 0.26402 0.46288 1.000 0.0650 . . H18 H Uiso 0.37846 0.18213 0.38868 1.000 0.0413 . . H19 H Uiso 0.31423 0.24780 0.30988 1.000 0.0508 . . H21 H Uiso 0.27656 0.36882 0.25996 1.000 0.0448 . . H23A H Uiso 0.15278 0.42864 0.15615 1.000 0.0920 . . H23B H Uiso 0.14714 0.37360 0.20953 1.000 0.0920 . . H23C H Uiso 0.22199 0.37591 0.18377 1.000 0.0920 . . H24A H Uiso 0.14954 0.60536 0.24279 1.000 0.0953 . . H24B H Uiso 0.09735 0.52417 0.24588 1.000 0.0953 . . H24C H Uiso 0.11101 0.56179 0.18842 1.000 0.0953 . . H25A H Uiso 0.27942 0.59205 0.22475 1.000 0.0784 . . H25B H Uiso 0.24667 0.56408 0.16481 1.000 0.0784 . . H25C H Uiso 0.30899 0.50753 0.19848 1.000 0.0784 . . H26A H Uiso 0.48128 0.63795 0.30825 1.000 0.1090 . . H26B H Uiso 0.39602 0.62562 0.28867 1.000 0.1090 . . H26C H Uiso 0.44953 0.54461 0.29247 1.000 0.1090 . . H27A H Uiso 0.45102 0.72714 0.40965 1.000 0.1140 . . H27B H Uiso 0.41015 0.68002 0.45410 1.000 0.1140 . . H27C H Uiso 0.36439 0.71477 0.39962 1.000 0.1140 . . H28A H Uiso 0.50744 0.53337 0.45411 1.000 0.0947 . . H28B H Uiso 0.54999 0.57477 0.40857 1.000 0.0947 . . H28C H Uiso 0.51735 0.47993 0.40084 1.000 0.0947 . . H31 H Uiso 0.88734 0.17218 0.46069 1.000 0.0497 . . H32 H Uiso 0.91314 0.31673 0.46679 1.000 0.0712 . . H33 H Uiso 0.89954 0.40541 0.38798 1.000 0.0580 . . H34 H Uiso 0.85578 0.33569 0.30454 1.000 0.0524 . . H36 H Uiso 0.83535 0.21851 0.24663 1.000 0.0574 . . H38A H Uiso 0.73422 -0.00089 0.14896 1.000 0.0738 . . H38B H Uiso 0.75578 -0.02954 0.21050 1.000 0.0738 . . H38C H Uiso 0.67936 0.01690 0.19229 1.000 0.0738 . . H39A H Uiso 0.83873 0.09091 0.13985 1.000 0.0640 . . H39B H Uiso 0.86894 0.15790 0.18593 1.000 0.0640 . . H39C H Uiso 0.87533 0.05715 0.19761 1.000 0.0640 . . H40A H Uiso 0.74096 0.23035 0.17979 1.000 0.0709 . . H40B H Uiso 0.70761 0.16426 0.13412 1.000 0.0709 . . H40C H Uiso 0.67106 0.17408 0.18849 1.000 0.0709 . . H41A H Uiso 1.03552 0.01643 0.42865 1.000 0.0940 . . H41B H Uiso 1.00603 0.10864 0.40797 1.000 0.0940 . . H41C H Uiso 0.98141 0.06858 0.46177 1.000 0.0940 . . H42A H Uiso 0.99773 -0.02890 0.31948 1.000 0.0971 . . H42B H Uiso 0.91746 -0.05900 0.29498 1.000 0.0971 . . H42C H Uiso 0.93934 0.04014 0.29365 1.000 0.0971 . . H43A H Uiso 0.94145 -0.13417 0.42495 1.000 0.1053 . . H43B H Uiso 0.87837 -0.08952 0.45331 1.000 0.1053 . . H43C H Uiso 0.85919 -0.13440 0.39558 1.000 0.1053 . . H45 H Uiso 0.75292 -0.11153 0.49057 1.000 0.0456 . . H46 H Uiso 0.81016 -0.06729 0.57360 1.000 0.0822 . . H47 H Uiso 0.82187 0.07764 0.59889 1.000 0.0547 . . H48 H Uiso 0.76793 0.18575 0.53856 1.000 0.0568 . . H52A H Uiso 0.55117 0.21338 0.39992 1.000 0.1015 . . H52B H Uiso 0.53079 0.29106 0.35888 1.000 0.1015 . . H52C H Uiso 0.53903 0.19612 0.33620 1.000 0.1015 . . H53A H Uiso 0.72280 0.34457 0.39676 1.000 0.0916 . . H53B H Uiso 0.64551 0.38894 0.37844 1.000 0.0916 . . H53C H Uiso 0.65778 0.33325 0.43269 1.000 0.0916 . . H54A H Uiso 0.69778 0.30459 0.30056 1.000 0.0534 . . H54B H Uiso 0.65572 0.21741 0.28285 1.000 0.0534 . . H54C H Uiso 0.61108 0.30500 0.28472 1.000 0.0534 . . H55A H Uiso 0.53127 -0.09575 0.33484 1.000 0.1518 . . H55B H Uiso 0.60960 -0.13107 0.32465 1.000 0.1518 . . H55C H Uiso 0.55700 -0.18932 0.35553 1.000 0.1518 . . H56A H Uiso 0.52011 -0.03552 0.46397 1.000 0.4662 . . H56B H Uiso 0.55163 0.04315 0.43300 1.000 0.4662 . . H56C H Uiso 0.49188 -0.01921 0.40146 1.000 0.4662 . . H57A H Uiso 0.60613 -0.10896 0.49644 1.000 0.4909 . . H57B H Uiso 0.56999 -0.18728 0.46121 1.000 0.4909 . . H57C H Uiso 0.65688 -0.17874 0.47271 1.000 0.4909 . . #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 Cl1 2.4141 . . yes Zr1 Cl2 2.4897 . . yes Zr1 N1 2.4864 . . yes Zr1 N2 2.1029 . . yes Zr1 N3 2.0434 . . yes Zr1 N4 2.4557 . . yes Zr2 N5 2.5285 . . yes Zr2 Cl3 2.4895 . . yes Zr2 Cl4 2.4314 . . yes Zr2 N8 2.1034 . . yes Zr2 N6 2.0658 . . yes Zr2 N7 2.3846 . . yes Si1 N3 1.7891 . . yes Si1 C27 1.8671 . . yes Si1 C28 1.8074 . . yes Si1 C26 1.8518 . . yes Si2 C14 1.9133 . . yes Si2 C13 1.8984 . . yes Si2 N2 1.7616 . . yes Si2 C12 1.8665 . . yes Si3 C41 1.8433 . . yes Si3 N6 1.7544 . . yes Si3 C42 1.8971 . . yes Si3 C43 1.8512 . . yes Si4 N8 1.7501 . . yes Si4 C55 1.6601 . . yes Si4 C56 1.8810 . . yes Si4 C57 1.6382 . . yes N1 C7 1.3157 . . yes N1 C8 1.5243 . . yes N2 C1 1.3554 . . yes N3 C15 1.4527 . . yes N4 C22 1.5115 . . yes N4 C21 1.2890 . . yes N5 C36 1.2947 . . yes N5 C37 1.5359 . . yes N6 C30 1.4499 . . yes N7 C50 1.2937 . . yes N7 C51 1.5549 . . yes N8 C44 1.4597 . . yes C1 C6 1.4229 . . no C1 C2 1.3885 . . no C2 C3 1.3799 . . no C3 C4 1.4189 . . no C4 C5 1.4153 . . no C5 C6 1.3579 . . no C6 C7 1.4844 . . no C8 C9 1.5180 . . no C8 C10 1.4975 . . no C8 C11 1.5564 . . no C15 C16 1.3715 . . no C15 C20 1.4406 . . no C16 C17 1.4405 . . no C17 C18 1.3487 . . no C18 C19 1.4230 . . no C19 C20 1.3490 . . no C20 C21 1.4234 . . no C22 C25 1.5931 . . no C22 C23 1.4852 . . no C22 C24 1.6142 . . no C2 H2 0.9300 . . no C3 H3 0.9300 . . no C4 H4 0.9300 . . no C5 H5 0.9300 . . no C9 H9B 0.9600 . . no C9 H9C 0.9600 . . no C9 H9A 0.9600 . . no C10 H10B 0.9600 . . no C10 H10C 0.9600 . . no C10 H10A 0.9600 . . no C11 H11C 0.9600 . . no C11 H11A 0.9600 . . no C11 H11B 0.9600 . . no C12 H12A 0.9600 . . no C12 H12B 0.9600 . . no C12 H12C 0.9600 . . no C13 H13C 0.9600 . . no C13 H13A 0.9600 . . no C13 H13B 0.9600 . . no C14 H14B 0.9600 . . no C14 H14C 0.9600 . . no C14 H14A 0.9600 . . no C16 H16 0.9300 . . no C17 H17 0.9300 . . no C18 H18 0.9300 . . no C19 H19 0.9300 . . no C21 H21 0.9300 . . no C23 H23A 0.9600 . . no C23 H23B 0.9600 . . no C23 H23C 0.9600 . . no C24 H24C 0.9600 . . no C24 H24A 0.9600 . . no C24 H24B 0.9600 . . no C25 H25C 0.9600 . . no C25 H25A 0.9600 . . no C25 H25B 0.9600 . . no C26 H26B 0.9600 . . no C26 H26A 0.9600 . . no C26 H26C 0.9600 . . no C27 H27A 0.9600 . . no C27 H27B 0.9600 . . no C27 H27C 0.9600 . . no C28 H28B 0.9600 . . no C28 H28C 0.9600 . . no C28 H28A 0.9600 . . no C30 C31 1.4221 . . no C30 C35 1.4388 . . no C31 C32 1.3703 . . no C32 C33 1.3822 . . no C33 C34 1.4165 . . no C34 C35 1.3056 . . no C35 C36 1.4840 . . no C37 C38 1.5355 . . no C37 C39 1.5559 . . no C37 C40 1.5113 . . no C44 C45 1.4520 . . no C44 C49 1.3963 . . no C45 C46 1.3413 . . no C46 C47 1.3953 . . no C47 C48 1.4027 . . no C48 C49 1.4301 . . no C49 C50 1.4743 . . no C51 C52 1.5757 . . no C51 C53 1.5760 . . no C51 C54 1.5249 . . no C31 H31 0.9300 . . no C32 H32 0.9300 . . no C33 H33 0.9300 . . no C34 H34 0.9300 . . no C36 H36 0.9300 . . no C38 H38A 0.9600 . . no C38 H38B 0.9600 . . no C38 H38C 0.9600 . . no C39 H39A 0.9600 . . no C39 H39B 0.9600 . . no C39 H39C 0.9600 . . no C40 H40A 0.9600 . . no C40 H40B 0.9600 . . no C40 H40C 0.9600 . . no C41 H41A 0.9600 . . no C41 H41B 0.9600 . . no C41 H41C 0.9600 . . no C42 H42A 0.9600 . . no C42 H42B 0.9600 . . no C42 H42C 0.9600 . . no C43 H43A 0.9600 . . no C43 H43B 0.9600 . . no C43 H43C 0.9600 . . no C45 H45 0.9300 . . no C46 H46 0.9300 . . no C47 H47 0.9300 . . no C48 H48 0.9300 . . no C52 H52A 0.9600 . . no C52 H52B 0.9600 . . no C52 H52C 0.9600 . . no C53 H53A 0.9600 . . no C53 H53B 0.9600 . . no C53 H53C 0.9600 . . no C54 H54A 0.9600 . . no C54 H54B 0.9600 . . no C54 H54C 0.9600 . . no C55 H55A 0.9600 . . no C55 H55B 0.9600 . . no C55 H55C 0.9600 . . no C56 H56A 0.9600 . . no C56 H56B 0.9600 . . no C56 H56C 0.9600 . . no C57 H57A 0.9600 . . no C57 H57B 0.9600 . . no C57 H57C 0.9600 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Zr1 Cl2 94.32 . . . yes Cl1 Zr1 N1 90.15 . . . yes Cl1 Zr1 N2 95.20 . . . yes Cl1 Zr1 N3 92.63 . . . yes Cl1 Zr1 N4 173.61 . . . yes Cl2 Zr1 N1 86.14 . . . yes Cl2 Zr1 N2 161.73 . . . yes Cl2 Zr1 N3 96.18 . . . yes Cl2 Zr1 N4 85.55 . . . yes N1 Zr1 N2 78.29 . . . yes N1 Zr1 N3 176.23 . . . yes N1 Zr1 N4 96.21 . . . yes N2 Zr1 N3 98.91 . . . yes N2 Zr1 N4 86.69 . . . yes N3 Zr1 N4 81.04 . . . yes N5 Zr2 N7 99.02 . . . yes N5 Zr2 N8 177.77 . . . yes N6 Zr2 N7 88.90 . . . yes N6 Zr2 N8 99.58 . . . yes N7 Zr2 N8 80.52 . . . yes Cl4 Zr2 N6 94.66 . . . yes Cl3 Zr2 Cl4 92.14 . . . yes Cl3 Zr2 N5 85.11 . . . yes Cl3 Zr2 N6 161.94 . . . yes Cl3 Zr2 N7 86.89 . . . yes Cl3 Zr2 N8 97.04 . . . yes Cl4 Zr2 N5 89.79 . . . yes N5 Zr2 N6 78.22 . . . yes Cl4 Zr2 N7 171.01 . . . yes Cl4 Zr2 N8 90.74 . . . yes C27 Si1 C28 105.80 . . . yes N3 Si1 C26 109.48 . . . yes N3 Si1 C27 108.81 . . . yes N3 Si1 C28 117.88 . . . yes C26 Si1 C27 109.74 . . . yes C26 Si1 C28 104.88 . . . yes N2 Si2 C12 106.73 . . . yes N2 Si2 C13 111.65 . . . yes N2 Si2 C14 112.67 . . . yes C12 Si2 C13 109.14 . . . yes C12 Si2 C14 112.12 . . . yes C13 Si2 C14 104.58 . . . yes C42 Si3 C43 112.63 . . . yes N6 Si3 C43 111.43 . . . yes N6 Si3 C41 113.38 . . . yes N6 Si3 C42 108.71 . . . yes C41 Si3 C42 103.47 . . . yes C41 Si3 C43 107.03 . . . yes N8 Si4 C57 116.48 . . . yes N8 Si4 C56 102.20 . . . yes N8 Si4 C55 117.44 . . . yes C55 Si4 C56 103.03 . . . yes C55 Si4 C57 118.90 . . . yes C56 Si4 C57 91.61 . . . yes C7 N1 C8 110.53 . . . yes Zr1 N1 C7 117.82 . . . yes Zr1 N1 C8 131.44 . . . yes Si2 N2 C1 115.80 . . . yes Zr1 N2 C1 114.68 . . . yes Zr1 N2 Si2 126.70 . . . yes Zr1 N3 C15 115.29 . . . yes Si1 N3 C15 112.72 . . . yes Zr1 N3 Si1 131.24 . . . yes Zr1 N4 C22 134.69 . . . yes C21 N4 C22 112.62 . . . yes Zr1 N4 C21 112.63 . . . yes C36 N5 C37 111.48 . . . yes Zr2 N5 C36 115.67 . . . yes Zr2 N5 C37 132.57 . . . yes Zr2 N6 Si3 131.99 . . . yes Zr2 N6 C30 112.30 . . . yes Si3 N6 C30 112.95 . . . yes C50 N7 C51 111.10 . . . yes Zr2 N7 C51 129.85 . . . yes Zr2 N7 C50 118.71 . . . yes Si4 N8 C44 116.80 . . . yes Zr2 N8 C44 113.35 . . . yes Zr2 N8 Si4 129.80 . . . yes C2 C1 C6 113.54 . . . no N2 C1 C6 126.32 . . . yes N2 C1 C2 120.02 . . . yes C1 C2 C3 125.30 . . . no C2 C3 C4 118.55 . . . no C3 C4 C5 118.45 . . . no C4 C5 C6 119.50 . . . no C1 C6 C7 122.29 . . . no C1 C6 C5 124.54 . . . no C5 C6 C7 113.16 . . . no N1 C7 C6 124.08 . . . yes N1 C8 C10 112.53 . . . yes N1 C8 C9 108.88 . . . yes C9 C8 C10 111.61 . . . no C9 C8 C11 106.20 . . . no N1 C8 C11 112.57 . . . yes C10 C8 C11 104.87 . . . no C16 C15 C20 117.48 . . . no N3 C15 C20 120.51 . . . yes N3 C15 C16 121.40 . . . yes C15 C16 C17 121.93 . . . no C16 C17 C18 117.90 . . . no C17 C18 C19 121.69 . . . no C18 C19 C20 119.66 . . . no C19 C20 C21 116.11 . . . no C15 C20 C19 120.90 . . . no C15 C20 C21 122.88 . . . no N4 C21 C20 130.81 . . . yes C24 C22 C25 105.59 . . . no N4 C22 C24 106.40 . . . yes N4 C22 C25 104.21 . . . yes N4 C22 C23 118.47 . . . yes C23 C22 C25 113.19 . . . no C23 C22 C24 108.09 . . . no C3 C2 H2 117.35 . . . no C1 C2 H2 117.35 . . . no C2 C3 H3 120.72 . . . no C4 C3 H3 120.72 . . . no C5 C4 H4 120.77 . . . no C3 C4 H4 120.77 . . . no C6 C5 H5 120.25 . . . no C4 C5 H5 120.25 . . . no C8 C9 H9A 109.47 . . . no C8 C9 H9C 109.47 . . . no H9A C9 H9B 109.47 . . . no C8 C9 H9B 109.47 . . . no H9A C9 H9C 109.47 . . . no H9B C9 H9C 109.47 . . . no C8 C10 H10A 109.47 . . . no C8 C10 H10B 109.47 . . . no C8 C10 H10C 109.47 . . . no H10A C10 H10B 109.47 . . . no H10A C10 H10C 109.47 . . . no H10B C10 H10C 109.47 . . . no C8 C11 H11B 109.47 . . . no C8 C11 H11C 109.47 . . . no H11A C11 H11B 109.47 . . . no H11A C11 H11C 109.47 . . . no H11B C11 H11C 109.47 . . . no C8 C11 H11A 109.47 . . . no Si2 C12 H12A 109.47 . . . no Si2 C12 H12C 109.47 . . . no H12A C12 H12B 109.47 . . . no Si2 C12 H12B 109.47 . . . no H12B C12 H12C 109.47 . . . no H12A C12 H12C 109.47 . . . no H13A C13 H13B 109.47 . . . no Si2 C13 H13C 109.47 . . . no Si2 C13 H13A 109.47 . . . no Si2 C13 H13B 109.47 . . . no H13A C13 H13C 109.47 . . . no H13B C13 H13C 109.47 . . . no Si2 C14 H14A 109.47 . . . no Si2 C14 H14B 109.47 . . . no Si2 C14 H14C 109.47 . . . no H14A C14 H14B 109.47 . . . no H14A C14 H14C 109.47 . . . no H14B C14 H14C 109.47 . . . no C17 C16 H16 119.03 . . . no C15 C16 H16 119.03 . . . no C16 C17 H17 121.05 . . . no C18 C17 H17 121.05 . . . no C19 C18 H18 119.15 . . . no C17 C18 H18 119.15 . . . no C18 C19 H19 120.17 . . . no C20 C19 H19 120.17 . . . no N4 C21 H21 114.59 . . . no C20 C21 H21 114.59 . . . no C22 C23 H23A 109.47 . . . no C22 C23 H23B 109.47 . . . no C22 C23 H23C 109.47 . . . no H23A C23 H23B 109.47 . . . no H23B C23 H23C 109.47 . . . no H23A C23 H23C 109.47 . . . no H24A C24 H24C 109.47 . . . no H24B C24 H24C 109.47 . . . no C22 C24 H24A 109.47 . . . no C22 C24 H24B 109.47 . . . no C22 C24 H24C 109.47 . . . no H24A C24 H24B 109.47 . . . no C22 C25 H25B 109.47 . . . no C22 C25 H25C 109.47 . . . no H25A C25 H25B 109.47 . . . no H25A C25 H25C 109.47 . . . no H25B C25 H25C 109.47 . . . no C22 C25 H25A 109.47 . . . no Si1 C26 H26B 109.47 . . . no Si1 C26 H26C 109.47 . . . no Si1 C26 H26A 109.47 . . . no H26A C26 H26B 109.47 . . . no H26A C26 H26C 109.47 . . . no H26B C26 H26C 109.47 . . . no Si1 C27 H27A 109.47 . . . no Si1 C27 H27B 109.47 . . . no Si1 C27 H27C 109.47 . . . no H27A C27 H27B 109.47 . . . no H27B C27 H27C 109.47 . . . no H27A C27 H27C 109.47 . . . no Si1 C28 H28B 109.47 . . . no Si1 C28 H28C 109.47 . . . no Si1 C28 H28A 109.47 . . . no H28A C28 H28C 109.47 . . . no H28B C28 H28C 109.47 . . . no H28A C28 H28B 109.47 . . . no N6 C30 C31 123.48 . . . yes N6 C30 C35 124.25 . . . yes C31 C30 C35 112.18 . . . no C30 C31 C32 124.57 . . . no C31 C32 C33 121.25 . . . no C32 C33 C34 114.29 . . . no C33 C34 C35 125.53 . . . no C30 C35 C34 122.13 . . . no C30 C35 C36 121.31 . . . no C34 C35 C36 116.51 . . . no N5 C36 C35 126.36 . . . yes N5 C37 C38 109.93 . . . yes N5 C37 C39 108.68 . . . yes N5 C37 C40 108.62 . . . yes C38 C37 C39 107.79 . . . no C38 C37 C40 109.10 . . . no C39 C37 C40 112.69 . . . no N8 C44 C45 118.20 . . . yes N8 C44 C49 120.72 . . . yes C45 C44 C49 121.02 . . . no C44 C45 C46 117.26 . . . no C45 C46 C47 124.25 . . . no C46 C47 C48 119.00 . . . no C47 C48 C49 119.63 . . . no C44 C49 C48 118.67 . . . no C44 C49 C50 124.79 . . . no C48 C49 C50 116.21 . . . no N7 C50 C49 123.97 . . . yes N7 C51 C52 107.83 . . . yes N7 C51 C53 110.34 . . . yes N7 C51 C54 113.29 . . . yes C52 C51 C53 110.66 . . . no C52 C51 C54 107.79 . . . no C53 C51 C54 106.93 . . . no C30 C31 H31 117.72 . . . no C32 C31 H31 117.72 . . . no C31 C32 H32 119.38 . . . no C33 C32 H32 119.38 . . . no C32 C33 H33 122.85 . . . no C34 C33 H33 122.85 . . . no C33 C34 H34 117.24 . . . no C35 C34 H34 117.24 . . . no N5 C36 H36 116.82 . . . no C35 C36 H36 116.82 . . . no C37 C38 H38A 109.47 . . . no C37 C38 H38B 109.47 . . . no C37 C38 H38C 109.47 . . . no H38A C38 H38B 109.47 . . . no H38A C38 H38C 109.47 . . . no H38B C38 H38C 109.47 . . . no C37 C39 H39A 109.47 . . . no C37 C39 H39B 109.47 . . . no C37 C39 H39C 109.47 . . . no H39A C39 H39B 109.47 . . . no H39A C39 H39C 109.47 . . . no H39B C39 H39C 109.47 . . . no C37 C40 H40A 109.47 . . . no C37 C40 H40B 109.47 . . . no C37 C40 H40C 109.47 . . . no H40A C40 H40B 109.47 . . . no H40A C40 H40C 109.47 . . . no H40B C40 H40C 109.47 . . . no Si3 C41 H41A 109.47 . . . no Si3 C41 H41B 109.47 . . . no Si3 C41 H41C 109.47 . . . no H41A C41 H41B 109.47 . . . no H41A C41 H41C 109.47 . . . no H41B C41 H41C 109.47 . . . no Si3 C42 H42A 109.47 . . . no Si3 C42 H42B 109.47 . . . no Si3 C42 H42C 109.47 . . . no H42A C42 H42B 109.47 . . . no H42A C42 H42C 109.47 . . . no H42B C42 H42C 109.47 . . . no Si3 C43 H43A 109.47 . . . no Si3 C43 H43B 109.47 . . . no Si3 C43 H43C 109.47 . . . no H43A C43 H43B 109.47 . . . no H43A C43 H43C 109.47 . . . no H43B C43 H43C 109.47 . . . no C44 C45 H45 121.37 . . . no C46 C45 H45 121.37 . . . no C45 C46 H46 117.88 . . . no C47 C46 H46 117.88 . . . no C46 C47 H47 120.50 . . . no C48 C47 H47 120.50 . . . no C47 C48 H48 120.18 . . . no C49 C48 H48 120.18 . . . no C51 C52 H52A 109.47 . . . no C51 C52 H52B 109.47 . . . no C51 C52 H52C 109.47 . . . no H52A C52 H52B 109.47 . . . no H52A C52 H52C 109.47 . . . no H52B C52 H52C 109.47 . . . no C51 C53 H53A 109.47 . . . no C51 C53 H53B 109.47 . . . no C51 C53 H53C 109.47 . . . no H53A C53 H53B 109.47 . . . no H53A C53 H53C 109.47 . . . no H53B C53 H53C 109.47 . . . no C51 C54 H54A 109.47 . . . no C51 C54 H54B 109.47 . . . no C51 C54 H54C 109.47 . . . no H54A C54 H54B 109.47 . . . no H54A C54 H54C 109.47 . . . no H54B C54 H54C 109.47 . . . no Si4 C55 H55A 109.47 . . . no Si4 C55 H55B 109.47 . . . no Si4 C55 H55C 109.47 . . . no H55A C55 H55B 109.47 . . . no H55A C55 H55C 109.47 . . . no H55B C55 H55C 109.47 . . . no Si4 C56 H56A 109.47 . . . no Si4 C56 H56B 109.47 . . . no Si4 C56 H56C 109.47 . . . no H56A C56 H56B 109.47 . . . no H56A C56 H56C 109.47 . . . no H56B C56 H56C 109.47 . . . no Si4 C57 H57A 109.47 . . . no Si4 C57 H57B 109.47 . . . no Si4 C57 H57C 109.47 . . . no H57A C57 H57B 109.47 . . . no H57A C57 H57C 109.47 . . . no H57B C57 H57C 109.47 . . . no 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 Cl1 Zr1 N1 C7 -136.54 . . . . no Cl2 Zr1 N1 C7 129.14 . . . . no N2 Zr1 N1 C7 -41.25 . . . . no N4 Zr1 N1 C7 44.05 . . . . no Cl1 Zr1 N1 C8 49.27 . . . . no Cl2 Zr1 N1 C8 -45.05 . . . . no N2 Zr1 N1 C8 144.56 . . . . no N4 Zr1 N1 C8 -130.14 . . . . no Cl1 Zr1 N2 Si2 -11.37 . . . . no N1 Zr1 N2 Si2 -100.44 . . . . no N3 Zr1 N2 Si2 82.12 . . . . no N4 Zr1 N2 Si2 162.51 . . . . no Cl1 Zr1 N2 C1 148.70 . . . . no N1 Zr1 N2 C1 59.63 . . . . no N3 Zr1 N2 C1 -117.81 . . . . no N4 Zr1 N2 C1 -37.42 . . . . no Cl2 Zr1 N3 Si1 24.48 . . . . no N2 Zr1 N3 Si1 -165.84 . . . . no N4 Zr1 N3 Si1 108.97 . . . . no Cl1 Zr1 N3 C15 120.66 . . . . no Cl2 Zr1 N3 C15 -144.71 . . . . no Cl2 Zr1 N4 C21 136.56 . . . . no Cl1 Zr1 N3 Si1 -70.15 . . . . no N1 Zr1 N4 C21 -137.82 . . . . no N2 Zr1 N4 C21 -59.99 . . . . no N3 Zr1 N4 C21 39.58 . . . . no Cl2 Zr1 N4 C22 -40.32 . . . . no N1 Zr1 N4 C22 45.30 . . . . no N2 Zr1 N3 C15 24.97 . . . . no N4 Zr1 N3 C15 -60.22 . . . . no N3 Zr1 N4 C22 -137.30 . . . . no N2 Zr1 N4 C22 123.13 . . . . no N6 Zr2 N5 C37 142.91 . . . . no N7 Zr2 N8 C44 -59.64 . . . . no N5 Zr2 N6 Si3 -96.81 . . . . no N7 Zr2 N5 C37 -130.13 . . . . no Cl4 Zr2 N6 Si3 -8.00 . . . . no N7 Zr2 N5 C36 43.11 . . . . no Cl3 Zr2 N5 C37 -44.06 . . . . no Cl4 Zr2 N5 C37 48.10 . . . . no Cl3 Zr2 N7 C50 134.82 . . . . no N5 Zr2 N7 C50 -140.63 . . . . no N6 Zr2 N7 C50 -62.75 . . . . no N7 Zr2 N6 Si3 163.74 . . . . no N6 Zr2 N5 C36 -43.86 . . . . no N7 Zr2 N8 Si4 118.03 . . . . no Cl3 Zr2 N8 C44 -145.28 . . . . no Cl4 Zr2 N8 C44 122.47 . . . . no N6 Zr2 N8 C44 27.62 . . . . no N7 Zr2 N6 C30 -36.84 . . . . no N8 Zr2 N6 C30 -117.03 . . . . no Cl4 Zr2 N8 Si4 -59.86 . . . . no N8 Zr2 N7 C50 37.15 . . . . no N8 Zr2 N6 Si3 83.54 . . . . no Cl4 Zr2 N6 C30 151.43 . . . . no N5 Zr2 N6 C30 62.61 . . . . no N6 Zr2 N7 C51 124.68 . . . . no N8 Zr2 N7 C51 -135.42 . . . . no Cl3 Zr2 N8 Si4 32.38 . . . . no N6 Zr2 N8 Si4 -154.72 . . . . no Cl3 Zr2 N5 C36 129.17 . . . . no Cl4 Zr2 N5 C36 -138.67 . . . . no N5 Zr2 N7 C51 46.79 . . . . no Cl3 Zr2 N7 C51 -37.76 . . . . no C26 Si1 N3 C15 88.64 . . . . no C27 Si1 N3 C15 -151.43 . . . . no C28 Si1 N3 Zr1 159.54 . . . . no C27 Si1 N3 Zr1 39.17 . . . . no C28 Si1 N3 C15 -31.05 . . . . no C26 Si1 N3 Zr1 -80.77 . . . . no C14 Si2 N2 C1 154.12 . . . . no C14 Si2 N2 Zr1 -46.00 . . . . no C13 Si2 N2 C1 36.78 . . . . no C13 Si2 N2 Zr1 -163.35 . . . . no C12 Si2 N2 C1 -82.40 . . . . no C12 Si2 N2 Zr1 77.48 . . . . no C43 Si3 N6 C30 147.82 . . . . no C42 Si3 N6 C30 -87.48 . . . . no C43 Si3 N6 Zr2 -52.86 . . . . no C41 Si3 N6 C30 26.99 . . . . no C42 Si3 N6 Zr2 71.84 . . . . no C41 Si3 N6 Zr2 -173.68 . . . . no C57 Si4 N8 Zr2 159.77 . . . . no C56 Si4 N8 Zr2 -102.19 . . . . no C55 Si4 N8 Zr2 9.66 . . . . no C55 Si4 N8 C44 -172.74 . . . . no C56 Si4 N8 C44 75.41 . . . . no C57 Si4 N8 C44 -22.63 . . . . no C7 N1 C8 C9 -76.53 . . . . no Zr1 N1 C7 C6 9.15 . . . . no Zr1 N1 C8 C10 -137.74 . . . . no C8 N1 C7 C6 -175.49 . . . . no Zr1 N1 C8 C9 97.98 . . . . no Zr1 N1 C8 C11 -19.50 . . . . no C7 N1 C8 C10 47.74 . . . . no C7 N1 C8 C11 165.99 . . . . no Zr1 N2 C1 C2 128.73 . . . . no Si2 N2 C1 C2 -68.95 . . . . no Zr1 N2 C1 C6 -55.55 . . . . no Si2 N2 C1 C6 106.77 . . . . no Si1 N3 C15 C16 69.36 . . . . no Zr1 N3 C15 C20 51.38 . . . . no Si1 N3 C15 C20 -119.82 . . . . no Zr1 N3 C15 C16 -119.44 . . . . no Zr1 N4 C22 C25 88.23 . . . . no Zr1 N4 C21 C20 -3.41 . . . . no C22 N4 C21 C20 174.19 . . . . no Zr1 N4 C22 C23 -144.94 . . . . no C21 N4 C22 C23 38.17 . . . . no Zr1 N4 C22 C24 -23.09 . . . . no C21 N4 C22 C24 160.03 . . . . no C21 N4 C22 C25 -88.65 . . . . no C36 N5 C37 C40 -70.23 . . . . no Zr2 N5 C37 C38 -16.10 . . . . no C36 N5 C37 C38 170.45 . . . . no Zr2 N5 C37 C39 -133.86 . . . . no C36 N5 C37 C39 52.70 . . . . no Zr2 N5 C37 C40 103.21 . . . . no Zr2 N5 C36 C35 7.09 . . . . no C37 N5 C36 C35 -178.26 . . . . no Zr2 N6 C30 C35 -57.76 . . . . no Zr2 N6 C30 C31 125.78 . . . . no Si3 N6 C30 C31 -70.69 . . . . no Si3 N6 C30 C35 105.76 . . . . no C50 N7 C51 C52 -80.35 . . . . no C50 N7 C51 C54 160.45 . . . . no C51 N7 C50 C49 174.55 . . . . no Zr2 N7 C50 C49 0.65 . . . . no Zr2 N7 C51 C52 92.67 . . . . no Zr2 N7 C51 C54 -26.52 . . . . no Zr2 N7 C51 C53 -146.37 . . . . no C50 N7 C51 C53 40.61 . . . . no Si4 N8 C44 C49 -125.28 . . . . no Si4 N8 C44 C45 57.46 . . . . no Zr2 N8 C44 C45 -124.55 . . . . no Zr2 N8 C44 C49 52.71 . . . . no C2 C1 C6 C5 -4.17 . . . . no N2 C1 C6 C7 0.58 . . . . no N2 C1 C2 C3 179.47 . . . . no C2 C1 C6 C7 176.53 . . . . no C6 C1 C2 C3 3.23 . . . . no N2 C1 C6 C5 179.87 . . . . no C1 C2 C3 C4 -0.98 . . . . no C2 C3 C4 C5 -0.72 . . . . no C3 C4 C5 C6 -0.17 . . . . no C4 C5 C6 C7 -177.85 . . . . no C4 C5 C6 C1 2.80 . . . . no C5 C6 C7 N1 -157.31 . . . . no C1 C6 C7 N1 22.06 . . . . no C16 C15 C20 C21 176.40 . . . . no C16 C15 C20 C19 -7.53 . . . . no N3 C15 C20 C21 5.23 . . . . no N3 C15 C16 C17 174.30 . . . . no C20 C15 C16 C17 3.22 . . . . no N3 C15 C20 C19 -178.70 . . . . no C15 C16 C17 C18 1.19 . . . . no C16 C17 C18 C19 -1.64 . . . . no C17 C18 C19 C20 -2.60 . . . . no C18 C19 C20 C21 -176.42 . . . . no C18 C19 C20 C15 7.25 . . . . no C19 C20 C21 N4 154.36 . . . . no C15 C20 C21 N4 -29.40 . . . . no C35 C30 C31 C32 2.84 . . . . no C31 C30 C35 C34 -1.65 . . . . no C31 C30 C35 C36 175.78 . . . . no N6 C30 C35 C34 -178.46 . . . . no N6 C30 C35 C36 -1.03 . . . . no N6 C30 C31 C32 179.68 . . . . no C30 C31 C32 C33 -2.34 . . . . no C31 C32 C33 C34 0.40 . . . . no C32 C33 C34 C35 0.75 . . . . no C33 C34 C35 C30 -0.04 . . . . no C33 C34 C35 C36 -177.59 . . . . no C34 C35 C36 N5 -156.93 . . . . no C30 C35 C36 N5 25.50 . . . . no C45 C44 C49 C48 -4.74 . . . . no N8 C44 C49 C48 178.08 . . . . no N8 C44 C49 C50 4.92 . . . . no N8 C44 C45 C46 -179.45 . . . . no C45 C44 C49 C50 -177.91 . . . . no C49 C44 C45 C46 3.30 . . . . no C44 C45 C46 C47 -1.37 . . . . no C45 C46 C47 C48 1.00 . . . . no C46 C47 C48 C49 -2.41 . . . . no C47 C48 C49 C50 178.02 . . . . no C47 C48 C49 C44 4.28 . . . . no C44 C49 C50 N7 -33.70 . . . . no C48 C49 C50 N7 152.99 . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Zr1 H11C 3.4441 . . no Zr1 H14C 3.4608 . . no Zr1 H24A 3.3822 . . no Zr1 H24B 3.6671 . . no Zr1 H27C 3.4758 . . no Zr2 H38C 3.6512 . . no Zr2 H54B 3.1730 . . no Zr2 H38B 3.5030 . . no Zr2 H55B 3.4036 . . no Cl1 C11 3.3098 . . no Cl1 C12 3.6267 . . no Cl1 C14 3.3478 . . no Cl1 C27 3.4876 . . no Cl2 C25 3.6029 . . no Cl2 C27 3.5994 . . no Cl2 C11 3.5878 . . no Cl2 C24 3.4772 . . no Cl3 C54 3.4620 . . no Cl3 C38 3.4921 . . no Cl3 C52 3.6364 . . no Cl3 C55 3.3900 . . no Cl4 C55 3.6122 . . no Cl4 C40 3.5642 . 2_645 no Cl4 C38 3.3223 . . no Cl4 C43 3.5565 . . no Cl1 H11A 2.7528 . . no Cl1 H53C 3.1001 . 3_666 no Cl1 H11C 3.0755 . . no Cl1 H12C 2.9209 . . no Cl1 H48 2.8183 . 3_666 no Cl1 H14C 2.8766 . . no Cl1 H27C 3.0842 . . no Cl2 H24A 2.6317 . . no Cl2 H23C 2.9589 . 2_555 no Cl2 H25A 2.7700 . . no Cl2 H26B 3.0151 . . no Cl2 H11C 2.7512 . . no Cl2 H9A 3.0884 . . no Cl2 H27C 2.8068 . . no Cl3 H5 2.9602 . 2_545 no Cl3 H55A 3.0468 . . no Cl3 H9C 2.8761 . 2_545 no Cl3 H52C 2.8981 . . no Cl3 H54B 2.6569 . . no Cl3 H55B 3.0365 . . no Cl3 H38C 2.7446 . . no Cl4 H55B 2.7557 . . no Cl4 H38B 2.5236 . . no Cl4 H43C 2.8086 . . no Cl4 H40A 2.6659 . 2_645 no Cl4 H42B 3.0730 . . no Si1 H16 3.1406 . . no Si2 H2 3.0950 . . no Si3 H31 3.2547 . . no Si4 H45 3.0605 . . no N1 C24 3.3678 . . no N2 C20 3.2183 . . no N4 C6 3.3580 . . no N6 C49 3.2878 . . no N7 C35 3.3700 . . no N1 H24B 2.8313 . . no N5 H54B 2.7957 . . no C1 C21 3.2452 . . no C1 C20 3.4556 . . no C2 C19 3.4314 . . no C2 C20 3.3496 . . no C2 C13 3.0303 . . no C2 C21 3.3202 . . no C5 C34 3.5107 . 1_455 no C6 N4 3.3580 . . no C6 C24 3.4882 . . no C7 C24 3.3015 . . no C11 Cl2 3.5878 . . no C11 C48 3.5529 . 3_666 no C11 Cl1 3.3098 . . no C12 Cl1 3.6267 . . no C13 C2 3.0303 . . no C14 C16 3.3738 . . no C14 Cl1 3.3478 . . no C16 C28 3.2014 . . no C16 C14 3.3738 . . no C17 C57 3.3630 . 3_656 no C17 C52 3.5465 . . no C18 C52 3.4795 . . no C19 C2 3.4314 . . no C20 C2 3.3496 . . no C20 N2 3.2183 . . no C20 C1 3.4556 . . no C21 C2 3.3202 . . no C21 C1 3.2452 . . no C24 C7 3.3015 . . no C24 C6 3.4882 . . no C24 Cl2 3.4772 . . no C24 N1 3.3678 . . no C25 Cl2 3.6029 . . no C27 Cl2 3.5994 . . no C27 Cl1 3.4876 . . no C28 C16 3.2014 . . no C30 C49 3.5244 . . no C30 C50 3.3372 . . no C31 C48 3.5922 . . no C31 C50 3.4004 . . no C31 C49 3.4473 . . no C31 C41 3.0972 . . no C34 C5 3.5107 . 1_655 no C35 C54 3.5344 . . no C35 N7 3.3700 . . no C36 C54 3.4288 . . no C38 Cl3 3.4921 . . no C38 Cl4 3.3223 . . no C40 Cl4 3.5642 . 2_655 no C41 C31 3.0972 . . no C43 Cl4 3.5565 . . no C43 C45 3.5046 . . no C45 C57 3.0093 . . no C45 C43 3.5046 . . no C48 C11 3.5529 . 3_666 no C48 C31 3.5922 . . no C49 C30 3.5244 . . no C49 N6 3.2878 . . no C49 C31 3.4473 . . no C50 C31 3.4004 . . no C50 C30 3.3372 . . no C52 C18 3.4795 . . no C52 Cl3 3.6364 . . no C52 C17 3.5465 . . no C54 C36 3.4288 . . no C54 Cl3 3.4620 . . no C54 C35 3.5344 . . no C55 Cl3 3.3900 . . no C55 Cl4 3.6122 . . no C57 C17 3.3630 . 3_656 no C57 C45 3.0093 . . no C1 H13C 3.0579 . . no C2 H13B 2.8280 . . no C2 H13C 2.7568 . . no C5 H24B 2.8530 . . no C6 H24B 2.6411 . . no C7 H24B 2.4770 . . no C7 H9C 2.6628 . . no C7 H10B 2.4920 . . no C7 H10A 3.0028 . . no C11 H48 2.9772 . 3_666 no C13 H2 2.6407 . . no C15 H28C 3.0421 . . no C16 H28C 2.8462 . . no C16 H28A 3.0962 . . no C16 H14C 2.7623 . . no C17 H57B 3.0463 . 3_656 no C19 H2 2.8737 . . no C20 H2 3.0160 . . no C21 H23C 2.7201 . . no C21 H25C 2.9100 . . no C21 H23B 2.9061 . . no C23 H21 2.3645 . . no C25 H21 3.0257 . . no C28 H16 2.8151 . . no C30 H41B 2.9333 . . no C31 H41C 2.8402 . . no C31 H41B 2.8315 . . no C33 H53A 3.0387 . . no C34 H54A 2.9802 . . no C35 H54A 2.9576 . . no C36 H40A 2.6631 . . no C36 H39B 2.5097 . . no C36 H39C 3.0126 . . no C36 H54B 3.0352 . . no C36 H54A 2.9736 . . no C39 H28B 3.0673 . 2_645 no C39 H36 2.4532 . . no C40 H36 2.6951 . . no C41 H31 2.8381 . . no C44 H57A 3.0226 . . no C45 H43B 2.6885 . . no C45 H57A 2.8292 . . no C45 H57C 2.6534 . . no C46 H25B 3.0992 . 4_555 no C48 H31 3.0022 . . no C50 H53A 2.8698 . . no C50 H52A 2.7395 . . no C50 H53C 2.5238 . . no C56 H56A 3.0087 . 3_656 no C57 H17 2.6478 . 3_656 no C57 H45 2.6208 . . no H2 C19 2.8737 . . no H2 H13B 2.1821 . . no H2 H13C 2.5979 . . no H2 C20 3.0160 . . no H2 Si2 3.0950 . . no H2 C13 2.6407 . . no H4 H26A 2.5374 . 2_545 no H5 Cl3 2.9602 . 2_555 no H9A H24A 2.5925 . . no H9A Cl2 3.0884 . . no H9A H11C 2.3852 . . no H9B H11B 2.4805 . . no H9B H10C 2.4055 . . no H9C C7 2.6628 . . no H9C Cl3 2.8761 . 2_555 no H10A H11A 2.4028 . . no H10A C7 3.0028 . . no H10B C7 2.4920 . . no H10B H40C 2.5649 . 2_555 no H10C H9B 2.4055 . . no H10C H11B 2.3517 . . no H10C H43A 2.5340 . 1_465 no H11A H10A 2.4028 . . no H11A Cl1 2.7528 . . no H11B H10C 2.3517 . . no H11B H9B 2.4805 . . no H11C Cl2 2.7512 . . no H11C H9A 2.3852 . . no H11C Cl1 3.0755 . . no H11C Zr1 3.4441 . . no H12C H32 2.5254 . 3_666 no H12C Cl1 2.9209 . . no H13B H2 2.1821 . . no H13B C2 2.8280 . . no H13B H45 2.5785 . 3_656 no H13C C2 2.7568 . . no H13C C1 3.0579 . . no H13C H2 2.5979 . . no H14C C16 2.7623 . . no H14C H16 2.4104 . . no H14C Zr1 3.4608 . . no H14C Cl1 2.8766 . . no H16 Si1 3.1406 . . no H16 C28 2.8151 . . no H16 H14C 2.4104 . . no H16 H28A 2.5362 . 3_666 no H16 H28A 2.4617 . . no H17 H57B 2.1901 . 3_656 no H17 C57 2.6478 . 3_656 no H19 H21 2.2720 . . no H21 C25 3.0257 . . no H21 C23 2.3645 . . no H21 H23C 1.9955 . . no H21 H19 2.2720 . . no H21 H23B 2.5038 . . no H23A H24C 2.3437 . . no H23B C21 2.9061 . . no H23B H21 2.5038 . . no H23C Cl2 2.9589 . 2_545 no H23C C21 2.7201 . . no H23C H25C 2.5520 . . no H23C H21 1.9955 . . no H24A Zr1 3.3822 . . no H24A Cl2 2.6317 . . no H24A H9A 2.5925 . . no H24A H25A 2.4575 . . no H24B N1 2.8313 . . no H24B C5 2.8530 . . no H24B C6 2.6411 . . no H24B Zr1 3.6671 . . no H24B C7 2.4770 . . no H24C H23A 2.3437 . . no H24C H25B 2.5961 . . no H25A H26B 2.5118 . . no H25A H24A 2.4575 . . no H25A Cl2 2.7700 . . no H25B C46 3.0992 . 4_454 no H25B H24C 2.5961 . . no H25C C21 2.9100 . . no H25C H23C 2.5520 . . no H26A H4 2.5374 . 2_555 no H26B H25A 2.5118 . . no H26B Cl2 3.0151 . . no H27C Zr1 3.4758 . . no H27C Cl1 3.0842 . . no H27C Cl2 2.8068 . . no H28A C16 3.0962 . . no H28A H16 2.4617 . . no H28A H28A 2.5119 . 3_666 no H28A H16 2.5362 . 3_666 no H28B C39 3.0673 . 2_655 no H28B H39A 2.4789 . 2_655 no H28C C16 2.8462 . . no H28C C15 3.0421 . . no H31 Si3 3.2547 . . no H31 C41 2.8381 . . no H31 C48 3.0022 . . no H31 H41C 2.3238 . . no H32 H12C 2.5254 . 3_666 no H34 H36 2.2836 . . no H36 C39 2.4532 . . no H36 C40 2.6951 . . no H36 H34 2.2836 . . no H36 H39B 1.9149 . . no H36 H40A 2.2141 . . no H38A H39A 2.3898 . . no H38A H40B 2.5867 . . no H38B Zr2 3.5030 . . no H38B Cl4 2.5236 . . no H38B H39C 2.5925 . . no H38C Zr2 3.6512 . . no H38C Cl3 2.7446 . . no H38C H40C 2.4083 . . no H39A H38A 2.3898 . . no H39A H28B 2.4789 . 2_645 no H39B C36 2.5097 . . no H39B H36 1.9149 . . no H39B H40A 2.5557 . . no H39C C36 3.0126 . . no H39C H38B 2.5925 . . no H39C H42C 2.4945 . . no H40A C36 2.6631 . . no H40A H36 2.2141 . . no H40A H39B 2.5557 . . no H40A Cl4 2.6659 . 2_655 no H40B H38A 2.5867 . . no H40C H38C 2.4083 . . no H40C H54B 2.4512 . . no H40C H10B 2.5649 . 2_545 no H41B C30 2.9333 . . no H41B C31 2.8315 . . no H41C C31 2.8402 . . no H41C H31 2.3238 . . no H42B Cl4 3.0730 . . no H42C H39C 2.4945 . . no H43A H10C 2.5340 . 1_645 no H43B C45 2.6885 . . no H43B H45 2.5774 . . no H43C Cl4 2.8086 . . no H45 Si4 3.0605 . . no H45 C57 2.6208 . . no H45 H43B 2.5774 . . no H45 H57C 2.0185 . . no H45 H13B 2.5785 . 3_656 no H48 Cl1 2.8183 . 3_666 no H48 C11 2.9772 . 3_666 no H52A C50 2.7395 . . no H52B H53B 2.5546 . . no H52B H54C 2.4769 . . no H52C Cl3 2.8981 . . no H52C H54C 2.5465 . . no H53A C33 3.0387 . . no H53A C50 2.8698 . . no H53A H54A 2.4162 . . no H53B H52B 2.5546 . . no H53B H54A 2.5797 . . no H53C C50 2.5238 . . no H53C Cl1 3.1001 . 3_666 no H54A C34 2.9802 . . no H54A C35 2.9576 . . no H54A C36 2.9736 . . no H54A H53A 2.4162 . . no H54A H53B 2.5797 . . no H54B Zr2 3.1730 . . no H54B Cl3 2.6569 . . no H54B N5 2.7957 . . no H54B C36 3.0352 . . no H54B H40C 2.4512 . . no H54C H52B 2.4769 . . no H54C H52C 2.5465 . . no H55A Cl3 3.0468 . . no H55A H56C 2.1989 . . no H55B Zr2 3.4036 . . no H55B Cl3 3.0365 . . no H55B Cl4 2.7557 . . no H55C H57B 2.5649 . . no H56A H57A 1.9991 . . no H56A H57B 2.4933 . . no H56A C56 3.0087 . 3_656 no H56A H56A 2.2692 . 3_656 no H56C H55A 2.1989 . . no H57A C44 3.0226 . . no H57A C45 2.8292 . . no H57A H56A 1.9991 . . no H57B H55C 2.5649 . . no H57B H56A 2.4933 . . no H57B C17 3.0463 . 3_656 no H57B H17 2.1901 . 3_656 no H57C C45 2.6534 . . no H57C H45 2.0185 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C11 H11A Cl1 0.9600 2.7528 3.3098 117.68 . yes C11 H11C Cl2 0.9600 2.7512 3.5878 146.04 . yes C24 H24A Cl2 0.9600 2.6317 3.4772 147.13 . yes C25 H25A Cl2 0.9600 2.7700 3.6029 145.56 . yes C27 H27C Cl2 0.9600 2.8068 3.5994 140.46 . yes C38 H38B Cl4 0.9600 2.5236 3.3223 140.66 . yes C38 H38C Cl3 0.9600 2.7446 3.4921 135.22 . yes C40 H40A Cl4 0.9600 2.6659 3.5642 155.95 2_655 yes C43 H43C Cl4 0.9600 2.8086 3.5565 135.39 . yes C48 H48 Cl1 0.9300 2.8183 3.7259 165.48 3_666 yes C54 H54B Cl3 0.9600 2.6569 3.4620 141.72 . yes C55 H55B Cl4 0.9600 2.7557 3.6122 148.95 . yes # End of Crystallographic Information File #==END data_Compound7 _database_code_CSD 181538 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sw008 _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 Cl2 N4 O Si2 Zr' _chemical_formula_sum 'C42 H66 Cl2 N4 O Si2 Zr' _chemical_formula_weight 861.29 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 10.494(2) _cell_length_b 31.860(6) _cell_length_c 14.365(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.39(3) _cell_angle_gamma 90.00 _cell_volume 4607.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 46183 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.37 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9572 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details 'sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _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 44974 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_av_sigmaI/netI 0.1433 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.31 _reflns_number_total 9201 _reflns_number_gt 4924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1295P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9201 _refine_ls_number_parameters 478 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1487 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.2141 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2100(5) 0.06792(17) 0.2475(4) 0.0370(14) Uani 1 1 d . . . C2 C 0.1646(6) 0.02677(18) 0.2537(4) 0.0442(15) Uani 1 1 d . . . H2 H 0.0718 0.0221 0.2402 0.053 Uiso 1 1 calc R . . C3 C 0.2487(6) -0.0067(2) 0.2782(5) 0.0592(19) Uani 1 1 d . . . H3 H 0.2138 -0.0341 0.2795 0.071 Uiso 1 1 calc R . . C4 C 0.3835(6) -0.0007(2) 0.3011(6) 0.064(2) Uani 1 1 d . . . H4 H 0.4430 -0.0237 0.3195 0.077 Uiso 1 1 calc R . . C5 C 0.4302(6) 0.0390(2) 0.2968(5) 0.0567(19) Uani 1 1 d . . . H5 H 0.5236 0.0431 0.3127 0.068 Uiso 1 1 calc R . . C6 C 0.3479(5) 0.07415(18) 0.2702(4) 0.0413(15) Uani 1 1 d . . . C7 C 0.4104(5) 0.1156(2) 0.2664(4) 0.0379(14) Uani 1 1 d . . . C8 C 0.5374(6) 0.1141(2) 0.2343(5) 0.0549(18) Uani 1 1 d . . . H8A H 0.5478 0.1406 0.2027 0.082 Uiso 1 1 calc R . . H8B H 0.5317 0.0909 0.1885 0.082 Uiso 1 1 calc R . . H8C H 0.6140 0.1098 0.2910 0.082 Uiso 1 1 calc R . . C9 C 0.4279(5) 0.19051(18) 0.2983(4) 0.0346(13) Uani 1 1 d . . . H9 H 0.3745 0.2092 0.3289 0.042 Uiso 1 1 calc R . . C10 C 0.4255(5) 0.21282(18) 0.2035(4) 0.0368(14) Uani 1 1 d . . . H10A H 0.4901 0.1996 0.1739 0.044 Uiso 1 1 calc R . . H10B H 0.3360 0.2107 0.1569 0.044 Uiso 1 1 calc R . . C11 C 0.4615(5) 0.25840(18) 0.2260(4) 0.0395(14) Uani 1 1 d . . . H11A H 0.3927 0.2718 0.2510 0.047 Uiso 1 1 calc R . . H11B H 0.4631 0.2731 0.1656 0.047 Uiso 1 1 calc R . . C12 C 0.5978(6) 0.2631(2) 0.3016(4) 0.0461(16) Uani 1 1 d . . . H12A H 0.6682 0.2534 0.2731 0.055 Uiso 1 1 calc R . . H12B H 0.6142 0.2930 0.3191 0.055 Uiso 1 1 calc R . . C13 C 0.6039(6) 0.2378(2) 0.3922(4) 0.0504(18) Uani 1 1 d . . . H13A H 0.6948 0.2393 0.4371 0.060 Uiso 1 1 calc R . . H13B H 0.5419 0.2500 0.4255 0.060 Uiso 1 1 calc R . . C14 C 0.5678(5) 0.1923(2) 0.3678(4) 0.0438(15) Uani 1 1 d . . . H14A H 0.5712 0.1765 0.4278 0.053 Uiso 1 1 calc R . . H14B H 0.6318 0.1795 0.3371 0.053 Uiso 1 1 calc R . . C15 C -0.0858(7) 0.0458(2) 0.0783(6) 0.076(2) Uani 1 1 d . . . H15A H -0.0195 0.0237 0.0819 0.114 Uiso 1 1 calc R . . H15B H -0.1488 0.0460 0.0133 0.114 Uiso 1 1 calc R . . H15C H -0.1336 0.0404 0.1266 0.114 Uiso 1 1 calc R . . C16 C -0.1356(5) 0.13646(18) 0.0935(4) 0.0401(14) Uani 1 1 d . . . H16A H -0.1787 0.1311 0.1446 0.060 Uiso 1 1 calc R . . H16B H -0.2012 0.1339 0.0299 0.060 Uiso 1 1 calc R . . H16C H -0.0982 0.1649 0.1010 0.060 Uiso 1 1 calc R . . C17 C 0.0790(6) 0.1067(2) 0.0001(4) 0.0555(19) Uani 1 1 d . . . C18 C 0.1687(9) 0.0698(3) -0.0070(7) 0.101(3) Uani 1 1 d . . . H18A H 0.2362 0.0660 0.0554 0.152 Uiso 1 1 calc R . . H18B H 0.2124 0.0755 -0.0576 0.152 Uiso 1 1 calc R . . H18C H 0.1152 0.0442 -0.0232 0.152 Uiso 1 1 calc R . . C19 C 0.1652(8) 0.1462(2) 0.0150(5) 0.066(2) Uani 1 1 d . . . H19A H 0.2346 0.1442 0.0769 0.099 Uiso 1 1 calc R . . H19B H 0.1098 0.1709 0.0156 0.099 Uiso 1 1 calc R . . H19C H 0.2063 0.1487 -0.0381 0.099 Uiso 1 1 calc R . . C20 C -0.0269(8) 0.1107(4) -0.0941(6) 0.146(6) Uani 1 1 d . . . H20A H -0.0775 0.1365 -0.0939 0.219 Uiso 1 1 calc R . . H20B H -0.0867 0.0864 -0.1026 0.219 Uiso 1 1 calc R . . H20C H 0.0140 0.1116 -0.1475 0.219 Uiso 1 1 calc R . . C21 C 0.3680(6) 0.1269(2) 0.5011(4) 0.0420(15) Uani 1 1 d . . . C22 C 0.4675(6) 0.0971(2) 0.5149(4) 0.0465(16) Uani 1 1 d . . . H22 H 0.4466 0.0699 0.4877 0.056 Uiso 1 1 calc R . . C23 C 0.5962(6) 0.1060(2) 0.5672(5) 0.0509(17) Uani 1 1 d . . . H23 H 0.6635 0.0853 0.5743 0.061 Uiso 1 1 calc R . . C24 C 0.6274(6) 0.1446(2) 0.6090(4) 0.0505(18) Uani 1 1 d . . . H24 H 0.7156 0.1504 0.6468 0.061 Uiso 1 1 calc R . . C25 C 0.5309(5) 0.1749(2) 0.5962(4) 0.0400(15) Uani 1 1 d . . . H25 H 0.5533 0.2016 0.6257 0.048 Uiso 1 1 calc R . . C26 C 0.3988(5) 0.16714(19) 0.5398(4) 0.0363(14) Uani 1 1 d . . . C27 C 0.3033(6) 0.20149(19) 0.5257(4) 0.0369(14) Uani 1 1 d . . . C28 C 0.3179(6) 0.2314(2) 0.6117(4) 0.0517(17) Uani 1 1 d . . . H28A H 0.2719 0.2578 0.5887 0.078 Uiso 1 1 calc R . . H28B H 0.4123 0.2370 0.6422 0.078 Uiso 1 1 calc R . . H28C H 0.2790 0.2185 0.6592 0.078 Uiso 1 1 calc R . . C29 C 0.1212(5) 0.24263(17) 0.4214(4) 0.0333(13) Uani 1 1 d . . . H29 H 0.0600 0.2367 0.3555 0.040 Uiso 1 1 calc R . . C30 C 0.1970(5) 0.28252(17) 0.4079(4) 0.0346(14) Uani 1 1 d . . . H30A H 0.2593 0.2908 0.4708 0.042 Uiso 1 1 calc R . . H30B H 0.2496 0.2767 0.3619 0.042 Uiso 1 1 calc R . . C31 C 0.1002(5) 0.31823(19) 0.3691(4) 0.0388(14) Uani 1 1 d . . . H31A H 0.0470 0.3115 0.3021 0.047 Uiso 1 1 calc R . . H31B H 0.1507 0.3443 0.3667 0.047 Uiso 1 1 calc R . . C32 C 0.0069(5) 0.32562(19) 0.4322(4) 0.0430(15) Uani 1 1 d . . . H32A H 0.0589 0.3353 0.4974 0.052 Uiso 1 1 calc R . . H32B H -0.0579 0.3479 0.4028 0.052 Uiso 1 1 calc R . . C33 C -0.0658(5) 0.2861(2) 0.4417(4) 0.0454(16) Uani 1 1 d . . . H33A H -0.1224 0.2777 0.3768 0.055 Uiso 1 1 calc R . . H33B H -0.1246 0.2915 0.4834 0.055 Uiso 1 1 calc R . . C34 C 0.0293(5) 0.24997(19) 0.4852(4) 0.0396(15) Uani 1 1 d . . . H34A H 0.0821 0.2572 0.5520 0.047 Uiso 1 1 calc R . . H34B H -0.0220 0.2242 0.4882 0.047 Uiso 1 1 calc R . . C35 C -0.0067(6) 0.06228(19) 0.4156(5) 0.0485(17) Uani 1 1 d . . . H35A H -0.0772 0.0789 0.4303 0.073 Uiso 1 1 calc R . . H35B H -0.0237 0.0324 0.4228 0.073 Uiso 1 1 calc R . . H35C H -0.0053 0.0679 0.3488 0.073 Uiso 1 1 calc R . . C36 C 0.2552(6) 0.0272(2) 0.5290(5) 0.064(2) Uani 1 1 d . . . H36A H 0.2816 0.0183 0.4719 0.096 Uiso 1 1 calc R . . H36B H 0.2012 0.0052 0.5469 0.096 Uiso 1 1 calc R . . H36C H 0.3347 0.0322 0.5832 0.096 Uiso 1 1 calc R . . C37 C 0.1261(8) 0.0958(3) 0.6185(5) 0.069(2) Uani 1 1 d . . . C38 C 0.0485(8) 0.0615(2) 0.6552(5) 0.085(3) Uani 1 1 d . . . H38A H 0.0325 0.0707 0.7161 0.127 Uiso 1 1 calc R . . H38B H 0.1003 0.0354 0.6664 0.127 Uiso 1 1 calc R . . H38C H -0.0368 0.0565 0.6066 0.127 Uiso 1 1 calc R . . C39 C 0.2536(9) 0.1044(3) 0.6959(5) 0.095(3) Uani 1 1 d . . . H39A H 0.3069 0.1246 0.6714 0.143 Uiso 1 1 calc R . . H39B H 0.3035 0.0782 0.7133 0.143 Uiso 1 1 calc R . . H39C H 0.2335 0.1160 0.7533 0.143 Uiso 1 1 calc R . . C40 C 0.0416(9) 0.1361(3) 0.6014(5) 0.083(3) Uani 1 1 d . . . H40A H 0.0254 0.1449 0.6625 0.125 Uiso 1 1 calc R . . H40B H -0.0434 0.1307 0.5529 0.125 Uiso 1 1 calc R . . H40C H 0.0892 0.1584 0.5781 0.125 Uiso 1 1 calc R . . N1 N 0.3607(4) 0.14905(14) 0.2912(3) 0.0291(10) Uani 1 1 d . . . N2 N 0.1163(4) 0.10093(14) 0.2184(3) 0.0315(11) Uani 1 1 d . . . N3 N 0.2119(4) 0.20578(14) 0.4431(3) 0.0304(11) Uani 1 1 d . . . N4 N 0.2332(4) 0.11578(14) 0.4481(3) 0.0364(12) Uani 1 1 d . . . Si1 Si -0.00096(15) 0.09775(5) 0.10291(12) 0.0386(4) Uani 1 1 d . . . Si2 Si 0.15597(18) 0.07681(6) 0.50066(13) 0.0480(5) Uani 1 1 d . . . Cl1 Cl -0.07414(13) 0.15946(5) 0.33579(11) 0.0395(4) Uani 1 1 d . . . Cl2 Cl 0.11626(12) 0.20979(4) 0.20487(9) 0.0314(3) Uani 1 1 d . . . Zr1 Zr 0.15033(5) 0.149947(17) 0.32123(4) 0.02921(19) Uani 1 1 d . . . C101 C 0.5400(12) 0.0527(4) 0.9726(9) 0.135(4) Uani 1 1 d U . . C100 C 0.5572(13) 0.0603(4) 0.8845(10) 0.156(5) Uani 1 1 d U . . O1 O 0.4887(16) 0.0044(5) 0.9390(10) 0.287(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.032(3) 0.046(4) 0.001(3) 0.016(3) 0.003(3) C2 0.032(3) 0.039(4) 0.062(4) 0.000(3) 0.015(3) 0.002(3) C3 0.048(4) 0.032(4) 0.107(6) 0.012(4) 0.037(4) 0.009(3) C4 0.039(4) 0.048(4) 0.111(6) 0.030(4) 0.028(4) 0.015(3) C5 0.025(3) 0.059(5) 0.088(5) 0.017(4) 0.018(3) 0.010(3) C6 0.029(3) 0.041(4) 0.055(4) 0.010(3) 0.014(3) 0.004(3) C7 0.023(3) 0.052(4) 0.040(3) 0.008(3) 0.011(3) 0.006(3) C8 0.033(3) 0.060(5) 0.079(5) 0.005(4) 0.027(4) 0.006(3) C9 0.030(3) 0.043(4) 0.033(3) 0.002(3) 0.013(3) -0.010(3) C10 0.029(3) 0.053(4) 0.032(3) -0.001(3) 0.014(3) -0.009(3) C11 0.042(3) 0.045(4) 0.035(3) 0.004(3) 0.016(3) -0.008(3) C12 0.044(4) 0.057(4) 0.038(3) -0.002(3) 0.012(3) -0.021(3) C13 0.032(3) 0.087(5) 0.032(3) -0.001(3) 0.009(3) -0.028(3) C14 0.026(3) 0.064(5) 0.041(3) 0.006(3) 0.009(3) -0.009(3) C15 0.067(5) 0.035(4) 0.101(6) -0.016(4) -0.016(4) -0.004(4) C16 0.034(3) 0.045(4) 0.035(3) -0.001(3) -0.001(3) 0.003(3) C17 0.051(4) 0.081(5) 0.029(3) -0.024(3) 0.002(3) 0.011(4) C18 0.091(6) 0.092(7) 0.143(9) -0.054(6) 0.069(7) -0.007(5) C19 0.084(6) 0.080(6) 0.040(4) -0.006(4) 0.029(4) -0.010(4) C20 0.070(6) 0.324(18) 0.045(5) -0.061(8) 0.018(5) 0.006(8) C21 0.048(4) 0.048(4) 0.030(3) 0.013(3) 0.010(3) -0.017(3) C22 0.046(4) 0.044(4) 0.046(4) 0.015(3) 0.007(3) -0.012(3) C23 0.038(4) 0.053(5) 0.052(4) 0.022(3) -0.003(3) -0.013(3) C24 0.037(4) 0.070(5) 0.041(4) 0.021(4) 0.005(3) -0.013(4) C25 0.035(3) 0.052(4) 0.032(3) 0.008(3) 0.009(3) -0.015(3) C26 0.032(3) 0.050(4) 0.028(3) 0.009(3) 0.010(3) -0.016(3) C27 0.035(3) 0.050(4) 0.029(3) -0.004(3) 0.013(3) -0.023(3) C28 0.047(4) 0.075(5) 0.029(3) -0.006(3) 0.004(3) -0.016(3) C29 0.026(3) 0.046(4) 0.029(3) -0.009(3) 0.009(3) -0.007(3) C30 0.032(3) 0.044(4) 0.031(3) -0.008(3) 0.014(3) -0.009(3) C31 0.041(3) 0.048(4) 0.026(3) -0.007(3) 0.008(3) -0.010(3) C32 0.030(3) 0.049(4) 0.047(4) -0.003(3) 0.008(3) -0.002(3) C33 0.030(3) 0.070(5) 0.038(3) -0.019(3) 0.012(3) -0.009(3) C34 0.038(3) 0.055(4) 0.033(3) -0.018(3) 0.022(3) -0.018(3) C35 0.052(4) 0.040(4) 0.062(4) -0.005(3) 0.029(4) -0.019(3) C36 0.052(4) 0.058(5) 0.073(5) 0.032(4) 0.002(4) -0.026(3) C37 0.094(6) 0.075(6) 0.044(4) -0.006(4) 0.029(4) -0.056(5) C38 0.121(7) 0.085(6) 0.064(5) -0.012(4) 0.052(5) -0.064(5) C39 0.133(8) 0.113(8) 0.043(4) -0.005(5) 0.030(5) -0.072(6) C40 0.147(8) 0.065(6) 0.059(5) -0.018(4) 0.064(6) -0.041(6) N1 0.019(2) 0.041(3) 0.026(2) 0.004(2) 0.005(2) -0.002(2) N2 0.025(2) 0.033(3) 0.037(3) -0.001(2) 0.010(2) 0.002(2) N3 0.032(3) 0.036(3) 0.027(2) -0.003(2) 0.015(2) -0.013(2) N4 0.031(3) 0.043(3) 0.034(3) 0.002(2) 0.008(2) -0.017(2) Si1 0.0317(9) 0.0325(10) 0.0476(10) -0.0140(8) 0.0049(8) 0.0012(7) Si2 0.0513(11) 0.0504(12) 0.0454(11) 0.0039(9) 0.0189(9) -0.0253(9) Cl1 0.0271(7) 0.0471(9) 0.0482(9) -0.0148(7) 0.0172(7) -0.0102(6) Cl2 0.0307(7) 0.0342(8) 0.0302(7) -0.0068(6) 0.0099(6) -0.0026(6) Zr1 0.0229(3) 0.0360(3) 0.0300(3) -0.0035(2) 0.0095(2) -0.0062(2) C101 0.135(4) 0.135(4) 0.136(4) -0.0003(10) 0.0387(15) -0.0003(10) C100 0.156(5) 0.155(5) 0.156(5) 0.0001(10) 0.0436(16) 0.0006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.406(8) . ? C1 C6 1.405(8) . ? C1 N2 1.420(7) . ? C2 C3 1.365(8) . ? C3 C4 1.373(9) . ? C4 C5 1.367(9) . ? C5 C6 1.399(8) . ? C6 C7 1.482(8) . ? C7 N1 1.280(7) . ? C7 C8 1.530(7) . ? C9 N1 1.487(7) . ? C9 C14 1.526(7) . ? C9 C10 1.531(7) . ? C10 C11 1.512(8) . ? C11 C12 1.539(8) . ? C12 C13 1.517(8) . ? C13 C14 1.512(8) . ? C15 Si1 1.865(7) . ? C16 Si1 1.851(6) . ? C17 C19 1.528(9) . ? C17 C20 1.494(10) . ? C17 C18 1.528(10) . ? C17 Si1 1.915(7) . ? C21 C22 1.384(8) . ? C21 C26 1.398(8) . ? C21 N4 1.449(7) . ? C22 C23 1.378(8) . ? C23 C24 1.366(9) . ? C24 C25 1.373(9) . ? C25 C26 1.416(7) . ? C26 C27 1.459(8) . ? C27 N3 1.305(7) . ? C27 C28 1.533(8) . ? C29 N3 1.489(7) . ? C29 C34 1.524(7) . ? C29 C30 1.541(7) . ? C30 C31 1.523(8) . ? C31 C32 1.529(7) . ? C32 C33 1.499(8) . ? C33 C34 1.536(8) . ? C35 Si2 1.856(6) . ? C36 Si2 1.872(7) . ? C37 C39 1.504(10) . ? C37 C38 1.542(8) . ? C37 C40 1.542(11) . ? C37 Si2 1.904(7) . ? N1 Zr1 2.366(4) . ? N2 Si1 1.768(5) . ? N2 Zr1 2.109(4) . ? N3 Zr1 2.451(4) . ? N4 Si2 1.765(4) . ? N4 Zr1 2.089(4) . ? Cl1 Zr1 2.4418(14) . ? Cl2 Zr1 2.4939(15) . ? C101 O1 1.656(18) . ? C101 C100 1.350(15) . ? C101 O1 2.29(2) 3_657 ? O1 O1 1.72(3) 3_657 ? O1 C101 2.29(2) 3_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.5(5) . . ? C2 C1 N2 119.4(5) . . ? C6 C1 N2 123.1(5) . . ? C3 C2 C1 122.6(6) . . ? C4 C3 C2 120.1(6) . . ? C3 C4 C5 118.4(6) . . ? C4 C5 C6 123.5(6) . . ? C1 C6 C5 117.8(5) . . ? C1 C6 C7 123.7(5) . . ? C5 C6 C7 118.5(5) . . ? N1 C7 C6 120.8(5) . . ? N1 C7 C8 124.6(5) . . ? C6 C7 C8 114.5(5) . . ? N1 C9 C14 115.4(5) . . ? N1 C9 C10 117.6(4) . . ? C14 C9 C10 109.6(4) . . ? C11 C10 C9 108.3(4) . . ? C10 C11 C12 111.7(5) . . ? C13 C12 C11 111.1(4) . . ? C14 C13 C12 111.3(5) . . ? C13 C14 C9 108.7(5) . . ? C19 C17 C20 108.5(7) . . ? C19 C17 C18 106.9(6) . . ? C20 C17 C18 108.6(7) . . ? C19 C17 Si1 112.7(4) . . ? C20 C17 Si1 109.6(5) . . ? C18 C17 Si1 110.4(6) . . ? C22 C21 C26 119.5(6) . . ? C22 C21 N4 119.5(6) . . ? C26 C21 N4 121.0(6) . . ? C21 C22 C23 121.3(6) . . ? C24 C23 C22 120.1(7) . . ? C23 C24 C25 119.8(6) . . ? C24 C25 C26 121.3(6) . . ? C21 C26 C25 117.8(6) . . ? C21 C26 C27 124.0(5) . . ? C25 C26 C27 118.2(6) . . ? N3 C27 C26 120.3(5) . . ? N3 C27 C28 123.3(6) . . ? C26 C27 C28 116.5(5) . . ? N3 C29 C34 118.1(4) . . ? N3 C29 C30 110.7(4) . . ? C34 C29 C30 112.8(5) . . ? C31 C30 C29 110.3(4) . . ? C30 C31 C32 111.8(5) . . ? C33 C32 C31 110.6(5) . . ? C32 C33 C34 112.2(5) . . ? C29 C34 C33 108.6(5) . . ? C39 C37 C38 108.8(6) . . ? C39 C37 C40 108.5(7) . . ? C38 C37 C40 108.1(7) . . ? C39 C37 Si2 112.3(6) . . ? C38 C37 Si2 108.4(5) . . ? C40 C37 Si2 110.8(5) . . ? C7 N1 C9 122.4(5) . . ? C7 N1 Zr1 122.3(4) . . ? C9 N1 Zr1 115.2(3) . . ? C1 N2 Si1 118.3(4) . . ? C1 N2 Zr1 112.1(3) . . ? Si1 N2 Zr1 129.4(2) . . ? C27 N3 C29 122.4(5) . . ? C27 N3 Zr1 123.5(4) . . ? C29 N3 Zr1 113.5(3) . . ? C21 N4 Si2 116.4(3) . . ? C21 N4 Zr1 115.8(3) . . ? Si2 N4 Zr1 127.7(2) . . ? N2 Si1 C16 110.2(2) . . ? N2 Si1 C15 113.4(3) . . ? C16 Si1 C15 105.3(3) . . ? N2 Si1 C17 112.0(2) . . ? C16 Si1 C17 109.6(3) . . ? C15 Si1 C17 106.0(3) . . ? N4 Si2 C35 110.0(3) . . ? N4 Si2 C36 113.1(3) . . ? C35 Si2 C36 106.5(3) . . ? N4 Si2 C37 111.6(3) . . ? C35 Si2 C37 108.2(3) . . ? C36 Si2 C37 107.2(4) . . ? N4 Zr1 N2 99.86(17) . . ? N4 Zr1 N1 88.44(15) . . ? N2 Zr1 N1 81.12(15) . . ? N4 Zr1 Cl1 99.43(12) . . ? N2 Zr1 Cl1 100.08(12) . . ? N1 Zr1 Cl1 171.66(11) . . ? N4 Zr1 N3 78.12(16) . . ? N2 Zr1 N3 174.69(15) . . ? N1 Zr1 N3 93.87(14) . . ? Cl1 Zr1 N3 85.13(10) . . ? N4 Zr1 Cl2 158.18(12) . . ? N2 Zr1 Cl2 97.64(13) . . ? N1 Zr1 Cl2 81.47(11) . . ? Cl1 Zr1 Cl2 90.19(5) . . ? N3 Zr1 Cl2 83.28(11) . . ? O1 C101 C100 90.7(11) . . ? O1 C101 O1 48.7(9) . 3_657 ? C100 C101 O1 137.5(12) . 3_657 ? O1 O1 C101 85.1(13) 3_657 . ? O1 O1 C101 46.2(9) 3_657 3_657 ? C101 O1 C101 131.3(9) . 3_657 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.871 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.107 #==END data_Compound9 _database_code_CSD 181539 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02sw035 _chemical_melting_point ? _chemical_formula_moiety 'C24 H45 Cl N4 Si Zr' _chemical_formula_sum 'C24 H45 Cl N4 Si Zr' _chemical_formula_weight 544.40 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.293(5) _cell_length_b 11.022(6) _cell_length_c 15.424(9) _cell_angle_alpha 77.235(17) _cell_angle_beta 87.70(2) _cell_angle_gamma 66.486(13) _cell_volume 1410.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23724 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9476 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_process_details 'Sortav - Blessing' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode'' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Chi scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8991 _diffrn_reflns_av_R_equivalents 0.1214 _diffrn_reflns_av_sigmaI/netI 0.2582 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5852 _reflns_number_gt 2682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1058P)^2^+0.1694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5852 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2220 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.2614 _refine_ls_wR_factor_gt 0.2078 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4312(11) 0.7674(8) 0.1067(6) 0.031(2) Uani 1 1 d . . . C2 C 0.4949(11) 0.8193(8) 0.0340(6) 0.037(2) Uani 1 1 d . . . H2 H 0.6010 0.8087 0.0394 0.045 Uiso 1 1 calc R . . C3 C 0.4117(11) 0.8870(8) -0.0476(6) 0.039(2) Uani 1 1 d . . . H3 H 0.4608 0.9209 -0.0965 0.047 Uiso 1 1 calc R . . C4 C 0.2562(12) 0.9043(8) -0.0567(6) 0.037(2) Uani 1 1 d . . . H4 H 0.1976 0.9496 -0.1119 0.044 Uiso 1 1 calc R . . C5 C 0.1897(12) 0.8550(8) 0.0150(6) 0.039(2) Uani 1 1 d . . . H5 H 0.0847 0.8637 0.0080 0.047 Uiso 1 1 calc R . . C6 C 0.2693(11) 0.7918(8) 0.0990(6) 0.032(2) Uani 1 1 d . . . C7 C 0.1779(11) 0.7641(8) 0.1745(6) 0.036(2) Uani 1 1 d . . . C8 C 0.0576(12) 0.7082(9) 0.1605(6) 0.046(3) Uani 1 1 d . . . H8A H 0.0831 0.6670 0.1087 0.070 Uiso 1 1 calc R . . H8B H -0.0473 0.7821 0.1503 0.070 Uiso 1 1 calc R . . H8C H 0.0592 0.6394 0.2135 0.070 Uiso 1 1 calc R . . C9 C 0.0893(10) 0.7868(8) 0.3206(6) 0.031(2) Uani 1 1 d . . . H9 H -0.0078 0.7897 0.2929 0.037 Uiso 1 1 calc R . . C10 C 0.0454(11) 0.9162(8) 0.3565(6) 0.037(2) Uani 1 1 d . . . H10A H 0.1405 0.9174 0.3823 0.045 Uiso 1 1 calc R . . H10B H -0.0004 0.9976 0.3074 0.045 Uiso 1 1 calc R . . C11 C -0.0712(11) 0.9174(8) 0.4262(6) 0.040(2) Uani 1 1 d . . . H11A H -0.1702 0.9268 0.3982 0.048 Uiso 1 1 calc R . . H11B H -0.0946 0.9970 0.4526 0.048 Uiso 1 1 calc R . . C12 C -0.0110(12) 0.7886(9) 0.4996(6) 0.044(3) Uani 1 1 d . . . H12A H 0.0817 0.7839 0.5319 0.053 Uiso 1 1 calc R . . H12B H -0.0936 0.7912 0.5427 0.053 Uiso 1 1 calc R . . C13 C 0.0341(13) 0.6633(9) 0.4617(6) 0.048(3) Uani 1 1 d . . . H13A H 0.0769 0.5809 0.5103 0.058 Uiso 1 1 calc R . . H13B H -0.0605 0.6639 0.4339 0.058 Uiso 1 1 calc R . . C14 C 0.1558(11) 0.6591(8) 0.3929(6) 0.035(2) Uani 1 1 d . . . H14A H 0.2531 0.6530 0.4209 0.042 Uiso 1 1 calc R . . H14B H 0.1819 0.5784 0.3673 0.042 Uiso 1 1 calc R . . C15 C 0.7886(11) 0.5333(9) 0.0925(6) 0.045(3) Uani 1 1 d . . . H15A H 0.8698 0.4415 0.0972 0.067 Uiso 1 1 calc R . . H15B H 0.8381 0.5983 0.0847 0.067 Uiso 1 1 calc R . . H15C H 0.7162 0.5565 0.0412 0.067 Uiso 1 1 calc R . . C16 C 0.8178(13) 0.5057(10) 0.2904(7) 0.059(3) Uani 1 1 d . . . H16A H 0.9229 0.4438 0.2786 0.088 Uiso 1 1 calc R . . H16B H 0.7834 0.4641 0.3456 0.088 Uiso 1 1 calc R . . H16C H 0.8211 0.5912 0.2966 0.088 Uiso 1 1 calc R . . C17 C 0.5999(11) 0.4012(8) 0.2177(6) 0.037(2) Uani 1 1 d . . . C18 C 0.5076(12) 0.4117(9) 0.1335(7) 0.051(3) Uani 1 1 d . . . H18A H 0.5778 0.3992 0.0841 0.077 Uiso 1 1 calc R . . H18B H 0.4206 0.5014 0.1180 0.077 Uiso 1 1 calc R . . H18C H 0.4657 0.3413 0.1450 0.077 Uiso 1 1 calc R . . C19 C 0.7393(12) 0.2607(9) 0.2360(7) 0.054(3) Uani 1 1 d . . . H19A H 0.8090 0.2558 0.1864 0.081 Uiso 1 1 calc R . . H19B H 0.6994 0.1895 0.2423 0.081 Uiso 1 1 calc R . . H19C H 0.7978 0.2480 0.2911 0.081 Uiso 1 1 calc R . . C20 C 0.4998(14) 0.4112(10) 0.2953(8) 0.065(4) Uani 1 1 d . . . H20A H 0.4124 0.5008 0.2843 0.097 Uiso 1 1 calc R . . H20B H 0.5625 0.3988 0.3486 0.097 Uiso 1 1 calc R . . H20C H 0.4582 0.3407 0.3042 0.097 Uiso 1 1 calc R . . C21 C 0.5493(17) 0.6567(13) 0.4362(8) 0.090(4) Uani 1 1 d . . . H21A H 0.5753 0.6034 0.3903 0.135 Uiso 1 1 calc R . . H21B H 0.4973 0.6175 0.4840 0.135 Uiso 1 1 calc R . . H21C H 0.6458 0.6552 0.4606 0.135 Uiso 1 1 calc R . . C22 C 0.4303(18) 0.8689(12) 0.4680(8) 0.090(5) Uani 1 1 d . . . H22A H 0.3678 0.9649 0.4418 0.134 Uiso 1 1 calc R . . H22B H 0.5335 0.8580 0.4895 0.134 Uiso 1 1 calc R . . H22C H 0.3760 0.8370 0.5180 0.134 Uiso 1 1 calc R . . C23 C 0.2790(13) 1.1361(9) 0.2645(7) 0.058(3) Uani 1 1 d . . . H23A H 0.3515 1.0857 0.3168 0.087 Uiso 1 1 calc R . . H23B H 0.1720 1.1779 0.2837 0.087 Uiso 1 1 calc R . . H23C H 0.3102 1.2069 0.2301 0.087 Uiso 1 1 calc R . . C24 C 0.1902(12) 1.1122(9) 0.1294(7) 0.050(3) Uani 1 1 d . . . H24A H 0.2128 1.0494 0.0897 0.074 Uiso 1 1 calc R . . H24B H 0.2142 1.1900 0.1005 0.074 Uiso 1 1 calc R . . H24C H 0.0788 1.1440 0.1426 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.6723(3) 0.8888(2) 0.25910(16) 0.0423(6) Uani 1 1 d . . . N1 N 0.2011(8) 0.7916(6) 0.2498(4) 0.0286(17) Uani 1 1 d . . . N2 N 0.5204(8) 0.6980(6) 0.1886(5) 0.0287(17) Uani 1 1 d . . . N3 N 0.4506(8) 0.7879(7) 0.3994(5) 0.0296(17) Uani 1 1 d . . . N4 N 0.2838(9) 1.0446(7) 0.2099(5) 0.0346(19) Uani 1 1 d . . . Si1 Si 0.6774(3) 0.5400(2) 0.19627(17) 0.0374(7) Uani 1 1 d . . . Zr1 Zr 0.42830(11) 0.84428(8) 0.26390(6) 0.0326(3) 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 0.042(6) 0.024(4) 0.030(5) -0.013(4) 0.008(5) -0.014(4) C2 0.037(6) 0.030(5) 0.046(6) -0.014(4) 0.008(5) -0.013(5) C3 0.037(6) 0.029(5) 0.047(6) -0.014(4) 0.009(5) -0.008(5) C4 0.048(7) 0.026(4) 0.035(6) -0.002(4) -0.003(5) -0.015(5) C5 0.040(6) 0.031(5) 0.049(7) -0.016(4) -0.006(5) -0.012(5) C6 0.034(6) 0.021(4) 0.047(6) -0.014(4) 0.003(5) -0.013(4) C7 0.037(6) 0.025(4) 0.037(6) -0.002(4) 0.009(5) -0.007(4) C8 0.051(7) 0.050(6) 0.047(7) -0.018(5) -0.007(5) -0.025(5) C9 0.014(5) 0.038(5) 0.047(6) -0.013(4) 0.009(4) -0.014(4) C10 0.039(6) 0.029(5) 0.037(6) -0.005(4) 0.006(5) -0.009(4) C11 0.043(6) 0.036(5) 0.045(6) -0.016(4) 0.004(5) -0.015(5) C12 0.045(7) 0.045(6) 0.046(6) -0.014(5) 0.010(5) -0.020(5) C13 0.059(8) 0.038(5) 0.044(6) -0.007(5) 0.002(5) -0.017(5) C14 0.038(6) 0.030(5) 0.048(6) -0.014(4) 0.004(5) -0.022(4) C15 0.028(6) 0.038(5) 0.064(7) -0.019(5) 0.017(5) -0.007(5) C16 0.064(8) 0.048(6) 0.066(8) -0.008(5) -0.018(6) -0.025(6) C17 0.036(6) 0.027(5) 0.042(6) -0.008(4) 0.009(5) -0.008(4) C18 0.050(7) 0.023(5) 0.068(7) -0.012(5) -0.011(6) 0.002(5) C19 0.064(8) 0.034(5) 0.065(7) -0.024(5) -0.004(6) -0.012(5) C20 0.078(9) 0.038(6) 0.086(9) -0.020(6) 0.031(7) -0.029(6) C21 0.091(11) 0.100(11) 0.084(10) -0.028(8) 0.001(8) -0.039(9) C22 0.125(13) 0.077(8) 0.072(9) -0.038(7) 0.021(9) -0.036(9) C23 0.070(8) 0.037(5) 0.066(8) -0.026(5) -0.001(6) -0.011(6) C24 0.053(7) 0.032(5) 0.060(7) -0.017(5) -0.003(6) -0.009(5) Cl1 0.0371(15) 0.0466(13) 0.0493(16) -0.0125(11) 0.0011(12) -0.0219(12) N1 0.032(5) 0.031(4) 0.026(4) -0.012(3) 0.003(3) -0.012(3) N2 0.022(4) 0.030(4) 0.032(4) -0.006(3) 0.005(3) -0.009(3) N3 0.013(4) 0.027(4) 0.056(5) -0.021(3) 0.005(3) -0.010(3) N4 0.034(5) 0.029(4) 0.042(5) -0.017(3) 0.007(4) -0.011(4) Si1 0.0343(16) 0.0320(13) 0.0427(17) -0.0119(12) 0.0003(13) -0.0078(12) Zr1 0.0310(6) 0.0292(5) 0.0394(6) -0.0124(4) 0.0041(4) -0.0117(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.366(12) . ? C1 C6 1.424(12) . ? C1 N2 1.421(10) . ? C1 Zr1 2.736(8) . ? C2 C3 1.393(12) . ? C3 C4 1.389(13) . ? C4 C5 1.359(12) . ? C5 C6 1.406(12) . ? C6 C7 1.463(12) . ? C7 N1 1.310(11) . ? C7 C8 1.519(13) . ? C9 N1 1.484(10) . ? C9 C14 1.508(11) . ? C9 C10 1.541(11) . ? C10 C11 1.494(12) . ? C11 C12 1.522(12) . ? C12 C13 1.518(12) . ? C13 C14 1.513(12) . ? C15 Si1 1.869(9) . ? C16 Si1 1.863(10) . ? C17 C20 1.483(13) . ? C17 C18 1.542(13) . ? C17 C19 1.546(12) . ? C17 Si1 1.899(10) . ? C21 N3 1.369(13) . ? C22 N3 1.490(12) . ? C23 N4 1.437(11) . ? C24 N4 1.419(11) . ? Cl1 Zr1 2.499(3) . ? N1 Zr1 2.431(7) . ? N2 Si1 1.752(7) . ? N2 Zr1 2.081(7) . ? N3 Zr1 2.038(8) . ? N4 Zr1 2.069(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.6(8) . . ? C2 C1 N2 121.4(9) . . ? C6 C1 N2 121.0(8) . . ? C2 C1 Zr1 120.5(6) . . ? C6 C1 Zr1 98.2(5) . . ? N2 C1 Zr1 48.3(4) . . ? C1 C2 C3 123.1(9) . . ? C4 C3 C2 119.4(9) . . ? C5 C4 C3 118.5(9) . . ? C4 C5 C6 123.0(9) . . ? C5 C6 C1 118.1(9) . . ? C5 C6 C7 117.9(9) . . ? C1 C6 C7 123.8(8) . . ? N1 C7 C6 118.7(8) . . ? N1 C7 C8 123.3(8) . . ? C6 C7 C8 118.0(8) . . ? N1 C9 C14 112.3(7) . . ? N1 C9 C10 106.9(7) . . ? C14 C9 C10 112.5(7) . . ? C11 C10 C9 108.7(7) . . ? C10 C11 C12 111.9(8) . . ? C13 C12 C11 111.1(8) . . ? C14 C13 C12 110.7(8) . . ? C9 C14 C13 108.5(7) . . ? C20 C17 C18 111.0(9) . . ? C20 C17 C19 109.3(8) . . ? C18 C17 C19 106.9(7) . . ? C20 C17 Si1 110.6(7) . . ? C18 C17 Si1 109.5(6) . . ? C19 C17 Si1 109.6(7) . . ? C7 N1 C9 118.2(8) . . ? C7 N1 Zr1 117.1(6) . . ? C9 N1 Zr1 124.7(5) . . ? C1 N2 Si1 120.0(5) . . ? C1 N2 Zr1 101.0(4) . . ? Si1 N2 Zr1 138.4(4) . . ? C21 N3 C22 107.7(9) . . ? C21 N3 Zr1 116.9(7) . . ? C22 N3 Zr1 131.1(6) . . ? C24 N4 C23 112.6(7) . . ? C24 N4 Zr1 133.9(5) . . ? C23 N4 Zr1 113.5(6) . . ? N2 Si1 C16 110.3(4) . . ? N2 Si1 C15 111.7(4) . . ? C16 Si1 C15 107.7(5) . . ? N2 Si1 C17 109.5(4) . . ? C16 Si1 C17 108.4(4) . . ? C15 Si1 C17 109.3(4) . . ? N3 Zr1 N4 116.2(3) . . ? N3 Zr1 N2 119.9(3) . . ? N4 Zr1 N2 123.2(3) . . ? N3 Zr1 N1 95.5(2) . . ? N4 Zr1 N1 86.9(3) . . ? N2 Zr1 N1 80.2(2) . . ? N3 Zr1 Cl1 91.0(2) . . ? N4 Zr1 Cl1 94.0(2) . . ? N2 Zr1 Cl1 92.9(2) . . ? N1 Zr1 Cl1 172.30(17) . . ? N3 Zr1 C1 147.2(2) . . ? N4 Zr1 C1 93.1(3) . . ? N2 Zr1 C1 30.7(2) . . ? N1 Zr1 C1 70.4(3) . . ? Cl1 Zr1 C1 101.9(2) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.157 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.142 #==END data_Compound10 _database_code_CSD 181540 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02sw023b _chemical_melting_point ? _chemical_formula_moiety 'C25 H47 Cl N4 Si Zr' _chemical_formula_sum 'C25 H47 Cl N4 Si Zr' _chemical_formula_weight 558.43 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' 'Si' 'Si' 0.0817 0.0704 '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)/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 17.2365(7) _cell_length_b 9.3683(5) _cell_length_c 18.9138(13) _cell_angle_alpha 90.00 _cell_angle_beta 106.866(2) _cell_angle_gamma 90.00 _cell_volume 2922.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11695 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9895 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details 'Sortav - Blessing' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12359 _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6448 _reflns_number_gt 4058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdiff-99.2 (1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1063P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6448 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2078 _refine_ls_wR_factor_gt 0.1800 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0948(3) 0.1922(5) 0.0965(3) 0.0283(12) Uani 1 1 d . . . C2 C -0.1010(3) 0.0985(6) 0.0368(3) 0.0342(13) Uani 1 1 d . . . H2 H -0.1105 -0.0002 0.0424 0.041 Uiso 1 1 calc R . . C3 C -0.0936(3) 0.1481(6) -0.0299(3) 0.0370(13) Uani 1 1 d . . . H3 H -0.0978 0.0832 -0.0695 0.044 Uiso 1 1 calc R . . C4 C -0.0801(3) 0.2900(6) -0.0393(3) 0.0353(13) Uani 1 1 d . . . H4 H -0.0747 0.3237 -0.0850 0.042 Uiso 1 1 calc R . . C5 C -0.0743(3) 0.3835(6) 0.0184(3) 0.0344(13) Uani 1 1 d . . . H5 H -0.0672 0.4823 0.0108 0.041 Uiso 1 1 calc R . . C6 C -0.0785(3) 0.3382(5) 0.0872(3) 0.0289(11) Uani 1 1 d . . . C7 C -0.0657(3) 0.4416(5) 0.1492(3) 0.0284(12) Uani 1 1 d . . . C8 C -0.1064(3) 0.5854(6) 0.1294(3) 0.0382(13) Uani 1 1 d . . . H8A H -0.1307 0.6149 0.1679 0.057 Uiso 1 1 calc R . . H8B H -0.1488 0.5781 0.0820 0.057 Uiso 1 1 calc R . . H8C H -0.0661 0.6562 0.1253 0.057 Uiso 1 1 calc R . . C9 C 0.0003(3) 0.5098(6) 0.2734(3) 0.0330(13) Uani 1 1 d . . . H9 H -0.0182 0.6053 0.2513 0.040 Uiso 1 1 calc R . . C10 C -0.0413(3) 0.4799(6) 0.3322(3) 0.0371(14) Uani 1 1 d . . . H10A H -0.0273 0.3822 0.3517 0.045 Uiso 1 1 calc R . . H10B H -0.1007 0.4841 0.3096 0.045 Uiso 1 1 calc R . . C11 C -0.0169(4) 0.5860(6) 0.3957(4) 0.0424(15) Uani 1 1 d . . . H11A H -0.0378 0.6817 0.3775 0.051 Uiso 1 1 calc R . . H11B H -0.0422 0.5576 0.4343 0.051 Uiso 1 1 calc R . . C12 C 0.0739(4) 0.5942(7) 0.4292(4) 0.0476(16) Uani 1 1 d . . . H12A H 0.0942 0.5024 0.4534 0.057 Uiso 1 1 calc R . . H12B H 0.0872 0.6701 0.4673 0.057 Uiso 1 1 calc R . . C13 C 0.1155(4) 0.6268(7) 0.3691(4) 0.0447(15) Uani 1 1 d . . . H13A H 0.1751 0.6260 0.3913 0.054 Uiso 1 1 calc R . . H13B H 0.0994 0.7231 0.3485 0.054 Uiso 1 1 calc R . . C14 C 0.0914(3) 0.5151(6) 0.3067(3) 0.0374(14) Uani 1 1 d . . . H14A H 0.1171 0.5396 0.2678 0.045 Uiso 1 1 calc R . . H14B H 0.1114 0.4199 0.3266 0.045 Uiso 1 1 calc R . . C15 C -0.2683(5) 0.2429(12) 0.1126(8) 0.147(6) Uani 1 1 d . . . H15A H -0.2360 0.3288 0.1119 0.220 Uiso 1 1 calc R . . H15B H -0.3098 0.2645 0.1371 0.220 Uiso 1 1 calc R . . H15C H -0.2944 0.2116 0.0619 0.220 Uiso 1 1 calc R . . C16 C -0.2369(5) -0.0706(10) 0.1184(7) 0.106(4) Uani 1 1 d . . . H16A H -0.2322 -0.0696 0.0680 0.160 Uiso 1 1 calc R . . H16B H -0.2936 -0.0859 0.1168 0.160 Uiso 1 1 calc R . . H16C H -0.2035 -0.1478 0.1465 0.160 Uiso 1 1 calc R . . C17 C -0.2139(5) 0.1039(16) 0.2568(5) 0.133(5) Uani 1 1 d . . . H17A H -0.1835 0.0246 0.2857 0.200 Uiso 1 1 calc R . . H17B H -0.2715 0.0945 0.2536 0.200 Uiso 1 1 calc R . . H17C H -0.1932 0.1945 0.2809 0.200 Uiso 1 1 calc R . . C18 C -0.0486(4) 0.1068(7) 0.4183(4) 0.0556(18) Uani 1 1 d . . . H18A H -0.0058 0.1253 0.4643 0.083 Uiso 1 1 calc R . . H18B H -0.0887 0.0415 0.4281 0.083 Uiso 1 1 calc R . . H18C H -0.0751 0.1969 0.3986 0.083 Uiso 1 1 calc R . . C19 C -0.0117(4) 0.0395(6) 0.3620(4) 0.0443(15) Uani 1 1 d . . . H19A H 0.0144 -0.0516 0.3825 0.053 Uiso 1 1 calc R . . H19B H -0.0560 0.0168 0.3169 0.053 Uiso 1 1 calc R . . C20 C 0.1235(4) 0.1532(6) 0.3998(4) 0.0456(16) Uani 1 1 d . . . H20A H 0.1106 0.2030 0.4411 0.055 Uiso 1 1 calc R . . H20B H 0.1578 0.2179 0.3803 0.055 Uiso 1 1 calc R . . C21 C 0.1717(4) 0.0202(7) 0.4295(4) 0.0516(17) Uani 1 1 d . . . H21A H 0.1387 -0.0439 0.4499 0.077 Uiso 1 1 calc R . . H21B H 0.2209 0.0467 0.4684 0.077 Uiso 1 1 calc R . . H21C H 0.1866 -0.0282 0.3894 0.077 Uiso 1 1 calc R . . C22 C 0.1879(3) 0.1340(6) 0.2369(3) 0.0328(12) Uani 1 1 d . . . H22A H 0.2045 0.0765 0.1998 0.039 Uiso 1 1 calc R . . H22B H 0.1719 0.0668 0.2705 0.039 Uiso 1 1 calc R . . C23 C 0.2607(3) 0.2201(7) 0.2814(4) 0.0461(16) Uani 1 1 d . . . H23A H 0.2852 0.2700 0.2477 0.069 Uiso 1 1 calc R . . H23B H 0.3007 0.1557 0.3132 0.069 Uiso 1 1 calc R . . H23C H 0.2430 0.2900 0.3121 0.069 Uiso 1 1 calc R . . C24 C 0.1321(3) 0.3185(6) 0.1436(3) 0.0352(13) Uani 1 1 d . . . H24A H 0.1830 0.3714 0.1662 0.042 Uiso 1 1 calc R . . H24B H 0.0874 0.3889 0.1296 0.042 Uiso 1 1 calc R . . C25 C 0.1388(3) 0.2428(7) 0.0742(3) 0.0410(14) Uani 1 1 d . . . H25A H 0.1787 0.1658 0.0881 0.061 Uiso 1 1 calc R . . H25B H 0.1559 0.3113 0.0425 0.061 Uiso 1 1 calc R . . H25C H 0.0859 0.2028 0.0473 0.061 Uiso 1 1 calc R . . N1 N -0.0211(2) 0.4027(4) 0.2140(3) 0.0279(10) Uani 1 1 d . . . N2 N -0.1038(3) 0.1415(4) 0.1647(3) 0.0310(10) Uani 1 1 d . . . N3 N 0.1170(2) 0.2200(4) 0.1985(2) 0.0293(10) Uani 1 1 d . . . N4 N 0.0477(3) 0.1269(4) 0.3413(3) 0.0307(10) Uani 1 1 d . . . Si1 Si -0.20198(9) 0.10067(17) 0.16320(10) 0.0351(4) Uani 1 1 d . . . Cl1 Cl 0.03367(8) -0.10908(13) 0.20324(8) 0.0347(3) Uani 1 1 d . . . Zr1 Zr 0.01883(3) 0.14993(5) 0.22891(3) 0.02699(19) 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) 0.033(3) 0.029(3) 0.000(2) 0.003(2) -0.002(2) C2 0.027(3) 0.043(3) 0.031(3) -0.001(3) 0.007(2) -0.005(2) C3 0.039(3) 0.042(3) 0.028(3) -0.005(3) 0.007(3) -0.001(2) C4 0.036(3) 0.051(3) 0.019(3) 0.005(3) 0.007(2) -0.006(3) C5 0.031(3) 0.040(3) 0.029(3) 0.006(3) 0.004(2) -0.004(2) C6 0.026(3) 0.034(3) 0.025(3) 0.007(2) 0.004(2) 0.004(2) C7 0.027(3) 0.029(3) 0.030(3) 0.004(2) 0.011(2) -0.003(2) C8 0.042(3) 0.037(3) 0.032(3) 0.004(3) 0.004(3) 0.008(2) C9 0.038(3) 0.029(3) 0.031(3) 0.004(2) 0.008(3) 0.003(2) C10 0.035(3) 0.037(3) 0.042(4) 0.000(3) 0.017(3) 0.000(2) C11 0.046(4) 0.041(3) 0.044(4) -0.008(3) 0.021(3) 0.001(3) C12 0.056(4) 0.049(4) 0.036(4) -0.010(3) 0.012(3) -0.002(3) C13 0.039(3) 0.052(4) 0.041(4) -0.012(3) 0.009(3) -0.009(3) C14 0.028(3) 0.045(3) 0.039(4) -0.012(3) 0.009(3) -0.012(2) C15 0.038(5) 0.131(8) 0.277(18) 0.122(10) 0.054(8) 0.027(5) C16 0.079(6) 0.093(6) 0.171(12) -0.072(7) 0.074(7) -0.048(5) C17 0.052(5) 0.304(16) 0.053(6) -0.036(8) 0.032(5) -0.051(7) C18 0.070(5) 0.062(4) 0.040(4) 0.008(4) 0.025(4) 0.001(4) C19 0.053(4) 0.042(3) 0.039(4) 0.004(3) 0.017(3) 0.007(3) C20 0.061(4) 0.040(3) 0.027(3) 0.001(3) 0.000(3) 0.004(3) C21 0.056(4) 0.053(4) 0.037(4) 0.006(3) 0.000(3) 0.012(3) C22 0.028(3) 0.036(3) 0.035(3) -0.006(3) 0.010(2) -0.001(2) C23 0.030(3) 0.048(4) 0.050(4) -0.001(3) -0.005(3) 0.002(3) C24 0.030(3) 0.039(3) 0.037(3) 0.002(3) 0.010(3) -0.003(2) C25 0.034(3) 0.052(3) 0.040(4) 0.009(3) 0.015(3) 0.002(3) N1 0.025(2) 0.027(2) 0.029(3) 0.000(2) 0.0055(19) -0.0031(18) N2 0.027(2) 0.035(2) 0.030(3) 0.004(2) 0.007(2) -0.0032(18) N3 0.026(2) 0.032(2) 0.029(3) 0.002(2) 0.006(2) -0.0015(17) N4 0.033(2) 0.029(2) 0.028(3) 0.003(2) 0.005(2) 0.0010(18) Si1 0.0291(8) 0.0393(8) 0.0373(10) -0.0015(7) 0.0102(7) -0.0050(6) Cl1 0.0395(8) 0.0268(6) 0.0381(8) 0.0001(6) 0.0117(6) -0.0010(5) Zr1 0.0303(3) 0.0268(3) 0.0220(3) 0.0016(2) 0.0047(2) -0.0004(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 C2 1.409(8) . ? C1 C6 1.417(7) . ? C1 N2 1.425(7) . ? C1 Zr1 2.724(5) . ? C2 C3 1.385(8) . ? C3 C4 1.369(8) . ? C4 C5 1.380(8) . ? C5 C6 1.391(8) . ? C6 C7 1.487(7) . ? C7 N1 1.295(7) . ? C7 C8 1.514(7) . ? C9 N1 1.472(7) . ? C9 C14 1.513(8) . ? C9 C10 1.514(8) . ? C10 C11 1.522(8) . ? C11 C12 1.511(9) . ? C12 C13 1.540(9) . ? C13 C14 1.542(8) . ? C15 Si1 1.834(9) . ? C16 Si1 1.832(8) . ? C17 Si1 1.841(9) . ? C18 C19 1.526(9) . ? C19 N4 1.451(7) . ? C20 N4 1.467(7) . ? C20 C21 1.512(8) . ? C22 N3 1.468(7) . ? C22 C23 1.524(8) . ? C24 N3 1.468(7) . ? C24 C25 1.526(8) . ? N1 Zr1 2.460(4) . ? N2 Si1 1.727(4) . ? N2 Zr1 2.112(4) . ? N3 Zr1 2.047(4) . ? N4 Zr1 2.049(5) . ? Cl1 Zr1 2.5022(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.3(5) . . ? C2 C1 N2 120.9(5) . . ? C6 C1 N2 120.7(5) . . ? C2 C1 Zr1 120.9(4) . . ? C6 C1 Zr1 98.0(3) . . ? N2 C1 Zr1 50.0(2) . . ? C3 C2 C1 121.0(5) . . ? C4 C3 C2 120.5(6) . . ? C3 C4 C5 119.4(5) . . ? C4 C5 C6 122.3(5) . . ? C5 C6 C1 118.4(5) . . ? C5 C6 C7 120.2(5) . . ? C1 C6 C7 121.4(5) . . ? N1 C7 C6 118.3(4) . . ? N1 C7 C8 126.1(5) . . ? C6 C7 C8 115.6(5) . . ? N1 C9 C14 109.9(4) . . ? N1 C9 C10 111.5(4) . . ? C14 C9 C10 110.9(5) . . ? C9 C10 C11 112.2(5) . . ? C12 C11 C10 112.3(5) . . ? C11 C12 C13 110.4(6) . . ? C12 C13 C14 110.6(5) . . ? C9 C14 C13 110.9(5) . . ? N4 C19 C18 115.2(5) . . ? N4 C20 C21 114.5(5) . . ? N3 C22 C23 114.7(5) . . ? N3 C24 C25 112.9(4) . . ? C7 N1 C9 118.6(4) . . ? C7 N1 Zr1 116.7(3) . . ? C9 N1 Zr1 124.6(3) . . ? C1 N2 Si1 115.0(4) . . ? C1 N2 Zr1 98.9(3) . . ? Si1 N2 Zr1 146.1(3) . . ? C24 N3 C22 113.7(4) . . ? C24 N3 Zr1 136.9(3) . . ? C22 N3 Zr1 108.8(3) . . ? C19 N4 C20 115.8(5) . . ? C19 N4 Zr1 111.2(4) . . ? C20 N4 Zr1 131.3(4) . . ? N2 Si1 C17 111.3(3) . . ? N2 Si1 C16 113.0(3) . . ? C17 Si1 C16 110.2(6) . . ? N2 Si1 C15 107.9(3) . . ? C17 Si1 C15 105.2(6) . . ? C16 Si1 C15 108.9(6) . . ? N3 Zr1 N4 110.69(17) . . ? N3 Zr1 N2 128.44(18) . . ? N4 Zr1 N2 119.61(17) . . ? N3 Zr1 N1 83.45(15) . . ? N4 Zr1 N1 101.32(16) . . ? N2 Zr1 N1 76.69(15) . . ? N3 Zr1 Cl1 96.71(12) . . ? N4 Zr1 Cl1 95.25(12) . . ? N2 Zr1 Cl1 89.63(12) . . ? N1 Zr1 Cl1 162.24(11) . . ? N3 Zr1 C1 97.32(16) . . ? N4 Zr1 C1 149.63(16) . . ? N2 Zr1 C1 31.14(15) . . ? N1 Zr1 C1 69.61(15) . . ? Cl1 Zr1 C1 92.82(11) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.209 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.133 #==END data_compound11 _database_code_CSD 181541 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 02sw022 _chemical_melting_point ? _chemical_formula_moiety 'C28 H50 Cl N3 O Si Zr' _chemical_formula_sum 'C28 H50 Cl N3 O Si Zr' _chemical_formula_weight 599.47 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 14.4679(4) _cell_length_b 12.2609(3) _cell_length_c 18.0837(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.3480(10) _cell_angle_gamma 90.00 _cell_volume 3107.80(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9688 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Cube _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9285 _exptl_absorpt_correction_T_max 0.9515 _exptl_absorpt_process_details 'Sortav - Blessing' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12852 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7048 _reflns_number_gt 4856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdiff-99.2 (1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7048 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.67831(19) 0.79346(19) 0.08372(14) 0.0148(6) Uani 1 1 d . . . C2 C 0.6366(2) 0.7541(2) 0.14055(14) 0.0200(6) Uani 1 1 d . . . H2 H 0.6761 0.7314 0.1867 0.024 Uiso 1 1 calc R . . C3 C 0.5397(2) 0.7478(2) 0.13069(15) 0.0223(7) Uani 1 1 d . . . H3 H 0.5142 0.7232 0.1701 0.027 Uiso 1 1 calc R . . C4 C 0.4801(2) 0.7786(2) 0.06122(15) 0.0233(7) Uani 1 1 d . . . H4 H 0.4142 0.7748 0.0536 0.028 Uiso 1 1 calc R . . C5 C 0.5194(2) 0.8146(2) 0.00373(15) 0.0220(6) Uani 1 1 d . . . H5 H 0.4788 0.8340 -0.0428 0.026 Uiso 1 1 calc R . . C6 C 0.61776(19) 0.8232(2) 0.01241(14) 0.0159(6) Uani 1 1 d . . . C7 C 0.65440(19) 0.8628(2) -0.05343(14) 0.0183(6) Uani 1 1 d . . . C8 C 0.6143(2) 0.9533(2) -0.09020(14) 0.0242(7) Uani 1 1 d . . . H8A H 0.6323 0.9774 -0.1333 0.029 Uiso 1 1 calc R . . H8B H 0.5686 0.9914 -0.0725 0.029 Uiso 1 1 calc R . . C9 C 0.73170(19) 0.80807(19) -0.15162(13) 0.0166(6) Uani 1 1 d . . . H9 H 0.6697 0.8332 -0.1822 0.020 Uiso 1 1 calc R . . C10 C 0.8062(2) 0.8922(2) -0.16177(14) 0.0206(6) Uani 1 1 d . . . H10A H 0.7914 0.9625 -0.1429 0.025 Uiso 1 1 calc R . . H10B H 0.8687 0.8702 -0.1320 0.025 Uiso 1 1 calc R . . C11 C 0.8079(2) 0.9028(2) -0.24530(13) 0.0212(6) Uani 1 1 d . . . H11A H 0.7470 0.9305 -0.2745 0.025 Uiso 1 1 calc R . . H11B H 0.8569 0.9546 -0.2499 0.025 Uiso 1 1 calc R . . C12 C 0.8279(2) 0.7930(2) -0.27785(15) 0.0216(6) Uani 1 1 d . . . H12A H 0.8258 0.8011 -0.3316 0.026 Uiso 1 1 calc R . . H12B H 0.8913 0.7683 -0.2518 0.026 Uiso 1 1 calc R . . C13 C 0.7551(2) 0.7089(2) -0.26836(14) 0.0204(6) Uani 1 1 d . . . H13A H 0.7711 0.6389 -0.2869 0.024 Uiso 1 1 calc R . . H13B H 0.6926 0.7300 -0.2988 0.024 Uiso 1 1 calc R . . C14 C 0.7516(2) 0.69760(19) -0.18453(14) 0.0194(6) Uani 1 1 d . . . H14A H 0.7020 0.6462 -0.1808 0.023 Uiso 1 1 calc R . . H14B H 0.8120 0.6692 -0.1549 0.023 Uiso 1 1 calc R . . C15 C 0.9775(2) 0.8442(2) 0.17307(17) 0.0306(8) Uani 1 1 d . . . H15A H 0.9865 0.7751 0.1989 0.046 Uiso 1 1 calc R . . H15B H 1.0193 0.8973 0.2031 0.046 Uiso 1 1 calc R . . H15C H 0.9917 0.8370 0.1242 0.046 Uiso 1 1 calc R . . C16 C 0.8212(2) 0.8867(3) 0.25409(15) 0.0350(8) Uani 1 1 d . . . H16A H 0.7554 0.9062 0.2476 0.053 Uiso 1 1 calc R . . H16B H 0.8609 0.9379 0.2878 0.053 Uiso 1 1 calc R . . H16C H 0.8319 0.8148 0.2755 0.053 Uiso 1 1 calc R . . C17 C 0.8376(2) 1.0335(2) 0.12045(16) 0.0273(7) Uani 1 1 d . . . C18 C 0.7350(2) 1.0749(2) 0.11141(17) 0.0357(8) Uani 1 1 d . . . H18A H 0.7199 1.0743 0.1602 0.053 Uiso 1 1 calc R . . H18B H 0.6914 1.0282 0.0768 0.053 Uiso 1 1 calc R . . H18C H 0.7296 1.1479 0.0916 0.053 Uiso 1 1 calc R . . C19 C 0.9055(2) 1.1099(2) 0.17580(18) 0.0411(9) Uani 1 1 d . . . H19A H 0.9703 1.0880 0.1799 0.062 Uiso 1 1 calc R . . H19B H 0.8922 1.1063 0.2252 0.062 Uiso 1 1 calc R . . H19C H 0.8966 1.1834 0.1570 0.062 Uiso 1 1 calc R . . C20 C 0.8619(2) 1.0363(2) 0.04300(17) 0.0385(9) Uani 1 1 d . . . H20A H 0.8546 1.1094 0.0233 0.058 Uiso 1 1 calc R . . H20B H 0.8197 0.9885 0.0082 0.058 Uiso 1 1 calc R . . H20C H 0.9266 1.0129 0.0488 0.058 Uiso 1 1 calc R . . C21 C 0.62365(19) 0.5381(2) -0.01408(14) 0.0210(7) Uani 1 1 d . . . H21A H 0.6005 0.5882 0.0188 0.025 Uiso 1 1 calc R . . H21B H 0.6159 0.4647 0.0035 0.025 Uiso 1 1 calc R . . C22 C 0.5620(2) 0.5503(2) -0.09529(14) 0.0308(8) Uani 1 1 d . . . H22A H 0.5690 0.6226 -0.1135 0.046 Uiso 1 1 calc R . . H22B H 0.4963 0.5378 -0.0957 0.046 Uiso 1 1 calc R . . H22C H 0.5817 0.4980 -0.1278 0.046 Uiso 1 1 calc R . . C23 C 0.7753(2) 0.4720(2) -0.03655(16) 0.0263(7) Uani 1 1 d . . . H23A H 0.8380 0.4985 -0.0380 0.032 Uiso 1 1 calc R . . H23B H 0.7404 0.4571 -0.0887 0.032 Uiso 1 1 calc R . . C24 C 0.7873(2) 0.3653(2) 0.00818(17) 0.0366(9) Uani 1 1 d . . . H24A H 0.8239 0.3783 0.0594 0.055 Uiso 1 1 calc R . . H24B H 0.8198 0.3133 -0.0159 0.055 Uiso 1 1 calc R . . H24C H 0.7256 0.3373 0.0092 0.055 Uiso 1 1 calc R . . C25 C 0.9994(2) 0.5472(2) 0.12573(16) 0.0276(7) Uani 1 1 d . . . H25A H 1.0477 0.6035 0.1312 0.033 Uiso 1 1 calc R . . H25B H 1.0020 0.5017 0.0824 0.033 Uiso 1 1 calc R . . C26 C 1.0148(3) 0.4802(3) 0.19707(18) 0.0538(11) Uani 1 1 d . . . H26A H 1.0216 0.4039 0.1852 0.065 Uiso 1 1 calc R . . H26B H 1.0728 0.5034 0.2333 0.065 Uiso 1 1 calc R . . C27 C 0.9369(3) 0.4934(4) 0.2289(2) 0.0927(18) Uani 1 1 d . . . H27A H 0.9573 0.5291 0.2782 0.111 Uiso 1 1 calc R . . H27B H 0.9107 0.4227 0.2366 0.111 Uiso 1 1 calc R . . C28 C 0.8629(2) 0.5604(2) 0.17700(14) 0.0278(7) Uani 1 1 d . . . H28A H 0.8058 0.5176 0.1569 0.033 Uiso 1 1 calc R . . H28B H 0.8462 0.6230 0.2038 0.033 Uiso 1 1 calc R . . N1 N 0.77945(15) 0.79746(16) 0.09558(11) 0.0145(5) Uani 1 1 d . . . N2 N 0.72336(15) 0.79686(15) -0.07248(11) 0.0143(5) Uani 1 1 d . . . N3 N 0.72547(16) 0.55851(16) -0.00572(11) 0.0177(5) Uani 1 1 d . . . Si3 Si 0.85120(6) 0.88896(6) 0.15962(4) 0.02061(19) Uani 1 1 d . . . Cl2 Cl 0.95812(5) 0.70895(5) -0.02267(4) 0.02353(17) Uani 1 1 d . . . Zr1 Zr 0.806485(19) 0.694544(19) 0.013974(13) 0.01422(8) Uani 1 1 d . . . O1 O 0.90481(13) 0.59542(14) 0.11557(9) 0.0199(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 0.0146(14) 0.0108(13) 0.0185(13) -0.0045(11) 0.0033(11) 0.0003(12) C2 0.0198(17) 0.0220(15) 0.0172(14) -0.0005(12) 0.0025(12) 0.0006(13) C3 0.0235(17) 0.0213(15) 0.0253(15) -0.0006(13) 0.0119(13) -0.0030(14) C4 0.0116(15) 0.0282(16) 0.0304(16) -0.0055(13) 0.0057(13) -0.0010(13) C5 0.0171(15) 0.0267(16) 0.0206(14) -0.0033(12) 0.0015(12) 0.0047(13) C6 0.0149(15) 0.0136(14) 0.0183(14) -0.0043(11) 0.0027(11) 0.0001(12) C7 0.0192(16) 0.0191(15) 0.0148(14) -0.0015(12) 0.0005(12) 0.0009(13) C8 0.0296(18) 0.0247(16) 0.0192(14) 0.0024(12) 0.0080(13) 0.0115(14) C9 0.0178(15) 0.0167(14) 0.0144(13) 0.0011(11) 0.0024(11) 0.0034(13) C10 0.0257(17) 0.0153(14) 0.0209(14) 0.0014(12) 0.0057(12) 0.0004(13) C11 0.0235(17) 0.0201(15) 0.0199(14) 0.0060(12) 0.0051(12) -0.0005(13) C12 0.0198(16) 0.0284(16) 0.0182(14) 0.0061(12) 0.0074(12) 0.0059(13) C13 0.0212(16) 0.0200(15) 0.0207(14) -0.0027(12) 0.0065(12) 0.0025(13) C14 0.0228(16) 0.0163(14) 0.0199(14) 0.0035(12) 0.0066(12) -0.0026(13) C15 0.0182(17) 0.0298(17) 0.0376(18) -0.0127(14) -0.0050(14) -0.0007(14) C16 0.032(2) 0.047(2) 0.0238(16) -0.0135(15) 0.0028(14) -0.0067(16) C17 0.0220(18) 0.0221(16) 0.0344(17) -0.0084(13) 0.0005(14) -0.0018(13) C18 0.031(2) 0.0231(16) 0.049(2) -0.0054(15) 0.0022(16) 0.0038(15) C19 0.032(2) 0.0267(17) 0.060(2) -0.0175(16) 0.0018(17) -0.0079(16) C20 0.049(2) 0.0226(17) 0.045(2) 0.0018(15) 0.0135(18) -0.0051(16) C21 0.0212(17) 0.0184(14) 0.0244(15) 0.0001(12) 0.0077(13) -0.0019(13) C22 0.0209(18) 0.0424(19) 0.0282(16) -0.0018(14) 0.0044(14) -0.0058(15) C23 0.0235(18) 0.0215(15) 0.0332(17) -0.0064(13) 0.0055(14) -0.0005(13) C24 0.029(2) 0.0165(15) 0.060(2) -0.0023(15) 0.0029(17) 0.0016(14) C25 0.0188(17) 0.0267(16) 0.0357(17) -0.0008(14) 0.0039(14) 0.0073(14) C26 0.049(3) 0.078(3) 0.0342(19) 0.0214(19) 0.0094(18) 0.037(2) C27 0.037(3) 0.150(4) 0.097(3) 0.097(3) 0.026(2) 0.040(3) C28 0.0251(18) 0.0363(18) 0.0228(15) 0.0090(14) 0.0078(13) 0.0043(15) N1 0.0127(12) 0.0152(11) 0.0151(11) 0.0006(9) 0.0024(9) 0.0019(10) N2 0.0160(12) 0.0126(11) 0.0148(11) 0.0013(9) 0.0048(9) 0.0009(10) N3 0.0196(13) 0.0148(12) 0.0184(11) -0.0004(9) 0.0041(10) -0.0004(10) Si3 0.0163(4) 0.0230(4) 0.0205(4) -0.0068(3) 0.0007(3) 0.0006(4) Cl2 0.0181(4) 0.0274(4) 0.0271(4) 0.0032(3) 0.0096(3) 0.0019(3) Zr1 0.01456(14) 0.01325(14) 0.01503(13) 0.00013(11) 0.00401(10) 0.00113(12) O1 0.0157(11) 0.0230(10) 0.0217(10) 0.0045(8) 0.0056(8) 0.0047(9) _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 C2 1.400(4) . ? C1 C6 1.416(3) . ? C1 N1 1.426(3) . ? C1 Zr1 2.768(3) . ? C2 C3 1.371(4) . ? C3 C4 1.388(4) . ? C4 C5 1.375(4) . ? C5 C6 1.397(4) . ? C6 C7 1.499(4) . ? C7 C8 1.348(3) . ? C7 N2 1.392(3) . ? C9 N2 1.472(3) . ? C9 C10 1.535(4) . ? C9 C14 1.535(3) . ? C10 C11 1.522(3) . ? C11 C12 1.526(3) . ? C12 C13 1.514(4) . ? C13 C14 1.535(3) . ? C15 Si3 1.865(3) . ? C16 Si3 1.864(3) . ? C17 C20 1.527(4) . ? C17 C19 1.536(4) . ? C17 C18 1.539(4) . ? C17 Si3 1.901(3) . ? C21 N3 1.465(3) . ? C21 C22 1.525(3) . ? C23 N3 1.468(3) . ? C23 C24 1.524(4) . ? C25 O1 1.461(3) . ? C25 C26 1.499(4) . ? C26 C27 1.397(5) . ? C27 C28 1.485(4) . ? C28 O1 1.456(3) . ? N1 Si3 1.755(2) . ? N1 Zr1 2.052(2) . ? N2 Zr1 2.1289(19) . ? N3 Zr1 2.019(2) . ? Cl2 Zr1 2.4502(7) . ? Zr1 O1 2.3624(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.4(2) . . ? C2 C1 N1 121.0(2) . . ? C6 C1 N1 120.6(2) . . ? C2 C1 Zr1 129.99(18) . . ? C6 C1 Zr1 91.78(16) . . ? N1 C1 Zr1 45.99(11) . . ? C3 C2 C1 122.5(2) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 119.4(3) . . ? C4 C5 C6 122.7(2) . . ? C5 C6 C1 117.8(2) . . ? C5 C6 C7 119.1(2) . . ? C1 C6 C7 123.1(2) . . ? C8 C7 N2 127.1(3) . . ? C8 C7 C6 117.7(3) . . ? N2 C7 C6 115.1(2) . . ? N2 C9 C10 114.1(2) . . ? N2 C9 C14 111.28(19) . . ? C10 C9 C14 110.0(2) . . ? C11 C10 C9 111.2(2) . . ? C12 C11 C10 111.0(2) . . ? C13 C12 C11 110.7(2) . . ? C12 C13 C14 111.5(2) . . ? C9 C14 C13 111.0(2) . . ? C20 C17 C19 109.2(3) . . ? C20 C17 C18 109.3(2) . . ? C19 C17 C18 108.2(2) . . ? C20 C17 Si3 109.69(19) . . ? C19 C17 Si3 109.62(19) . . ? C18 C17 Si3 110.8(2) . . ? N3 C21 C22 114.6(2) . . ? N3 C23 C24 114.8(2) . . ? O1 C25 C26 105.4(3) . . ? C27 C26 C25 109.2(3) . . ? C26 C27 C28 109.4(3) . . ? O1 C28 C27 105.9(3) . . ? C1 N1 Si3 122.56(17) . . ? C1 N1 Zr1 104.01(14) . . ? Si3 N1 Zr1 132.89(13) . . ? C7 N2 C9 115.00(19) . . ? C7 N2 Zr1 118.02(16) . . ? C9 N2 Zr1 126.97(16) . . ? C21 N3 C23 114.4(2) . . ? C21 N3 Zr1 133.20(17) . . ? C23 N3 Zr1 110.23(18) . . ? N1 Si3 C15 107.34(11) . . ? N1 Si3 C16 111.18(12) . . ? C15 Si3 C16 108.60(14) . . ? N1 Si3 C17 111.12(11) . . ? C15 Si3 C17 109.32(14) . . ? C16 Si3 C17 109.22(14) . . ? N3 Zr1 N1 115.41(9) . . ? N3 Zr1 N2 99.19(8) . . ? N1 Zr1 N2 89.54(8) . . ? N3 Zr1 O1 85.62(7) . . ? N1 Zr1 O1 86.70(7) . . ? N2 Zr1 O1 174.85(7) . . ? N3 Zr1 Cl2 122.10(7) . . ? N1 Zr1 Cl2 119.56(6) . . ? N2 Zr1 Cl2 98.03(6) . . ? O1 Zr1 Cl2 80.82(5) . . ? N3 Zr1 C1 90.98(8) . . ? N1 Zr1 C1 30.00(7) . . ? N2 Zr1 C1 75.88(8) . . ? O1 Zr1 C1 102.32(7) . . ? Cl2 Zr1 C1 146.89(5) . . ? C28 O1 C25 109.8(2) . . ? C28 O1 Zr1 117.43(15) . . ? C25 O1 Zr1 132.15(16) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.585 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.083 data_Compound12 _database_code_CSD 181542 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 99skl007 _chemical_melting_point ? _chemical_formula_moiety 'C16 H29 Cl2 N3 Si Zr' _chemical_formula_sum 'C16 H29 Cl2 N3 Si Zr' _chemical_formula_weight 453.63 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 9.1721(18) _cell_length_b 13.137(3) _cell_length_c 17.476(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.88(3) _cell_angle_gamma 90.00 _cell_volume 2101.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20200 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.373 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.837 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8504 _exptl_absorpt_correction_T_max 0.9210 _exptl_absorpt_process_details 'Sortav' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48241 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.36 _reflns_number_total 4292 _reflns_number_gt 3557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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^)+(0.0372P)^2^+0.6224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4292 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.51288(2) 0.596627(15) 0.096731(11) 0.01952(8) Uani 1 1 d . . . Si4 Si 0.67795(7) 0.50827(5) 0.26231(4) 0.02853(16) Uani 1 1 d . . . N1 N 0.52963(19) 0.57582(13) 0.21547(10) 0.0227(4) Uani 1 1 d . . . Cl1 Cl 0.51063(6) 0.40424(4) 0.05849(3) 0.02321(13) Uani 1 1 d . . . Cl2 Cl 0.75875(6) 0.66192(5) 0.08310(3) 0.03294(15) Uani 1 1 d . . . C7 C 0.2632(2) 0.66675(16) 0.14447(12) 0.0224(5) Uani 1 1 d . . . H7 H 0.1679 0.7020 0.1319 0.027 Uiso 1 1 calc R . . N2 N 0.38107(18) 0.71804(13) 0.10511(10) 0.0216(4) Uani 1 1 d . . . C5 C 0.1913(3) 0.70102(17) 0.27719(14) 0.0302(5) Uani 1 1 d . . . H5 H 0.1012 0.7259 0.2545 0.036 Uiso 1 1 calc R . . C6 C 0.2945(2) 0.66212(16) 0.22978(12) 0.0239(5) Uani 1 1 d . . . C1 C 0.4278(2) 0.62244(17) 0.26243(13) 0.0248(5) Uani 1 1 d . . . C4 C 0.2160(3) 0.70446(18) 0.35549(14) 0.0374(6) Uani 1 1 d . . . H4 H 0.1430 0.7294 0.3867 0.045 Uiso 1 1 calc R . . C2 C 0.4523(3) 0.63099(19) 0.34234(13) 0.0338(6) Uani 1 1 d . . . H2 H 0.5431 0.6085 0.3658 0.041 Uiso 1 1 calc R . . C3 C 0.3489(3) 0.6710(2) 0.38820(14) 0.0409(6) Uani 1 1 d . . . H3 H 0.3693 0.6755 0.4421 0.049 Uiso 1 1 calc R . . C8 C 0.3637(2) 0.82801(17) 0.08771(13) 0.0266(5) Uani 1 1 d . . . C9 C 0.3391(3) 0.88920(17) 0.16017(14) 0.0328(6) Uani 1 1 d . . . H9A H 0.2469 0.8682 0.1806 0.049 Uiso 1 1 calc R . . H9B H 0.3348 0.9619 0.1477 0.049 Uiso 1 1 calc R . . H9C H 0.4198 0.8767 0.1987 0.049 Uiso 1 1 calc R . . C12 C 0.6089(3) 0.4166(2) 0.33326(17) 0.0458(7) Uani 1 1 d . . . H12A H 0.6265 0.4441 0.3852 0.069 Uiso 1 1 calc R . . H12B H 0.6601 0.3515 0.3296 0.069 Uiso 1 1 calc R . . H12C H 0.5038 0.4060 0.3222 0.069 Uiso 1 1 calc R . . C10 C 0.2366(3) 0.8452(2) 0.02805(15) 0.0439(7) Uani 1 1 d . . . H10A H 0.2548 0.8080 -0.0190 0.066 Uiso 1 1 calc R . . H10B H 0.2275 0.9180 0.0167 0.066 Uiso 1 1 calc R . . H10C H 0.1459 0.8205 0.0482 0.066 Uiso 1 1 calc R . . C13 C 0.8138(3) 0.6006(2) 0.30589(16) 0.0412(7) Uani 1 1 d . . . H13A H 0.8531 0.6419 0.2654 0.062 Uiso 1 1 calc R . . H13B H 0.8936 0.5634 0.3336 0.062 Uiso 1 1 calc R . . H13C H 0.7660 0.6451 0.3416 0.062 Uiso 1 1 calc R . . C11 C 0.5061(3) 0.8636(2) 0.05578(17) 0.0444(7) Uani 1 1 d . . . H11A H 0.5877 0.8509 0.0937 0.067 Uiso 1 1 calc R . . H11B H 0.4999 0.9367 0.0446 0.067 Uiso 1 1 calc R . . H11C H 0.5221 0.8262 0.0086 0.067 Uiso 1 1 calc R . . C14 C 0.7768(3) 0.4287(2) 0.19440(16) 0.0430(7) Uani 1 1 d . . . H14A H 0.7124 0.3741 0.1742 0.064 Uiso 1 1 calc R . . H14B H 0.8638 0.3991 0.2213 0.064 Uiso 1 1 calc R . . H14C H 0.8061 0.4712 0.1520 0.064 Uiso 1 1 calc R . . N3 N 0.26224(18) 0.56353(14) 0.10698(11) 0.0243(4) Uani 1 1 d . . . C15 C 0.2077(3) 0.48049(18) 0.15413(15) 0.0350(6) Uani 1 1 d . . . H15A H 0.1098 0.4977 0.1694 0.053 Uiso 1 1 calc R . . H15B H 0.2739 0.4713 0.2000 0.053 Uiso 1 1 calc R . . H15C H 0.2031 0.4173 0.1243 0.053 Uiso 1 1 calc R . . C16 C 0.1693(2) 0.5692(2) 0.03435(14) 0.0334(6) Uani 1 1 d . . . H16A H 0.1788 0.5060 0.0054 0.050 Uiso 1 1 calc R . . H16B H 0.2007 0.6268 0.0038 0.050 Uiso 1 1 calc R . . H16C H 0.0671 0.5788 0.0458 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01729(12) 0.02054(13) 0.02122(13) -0.00298(8) 0.00490(8) -0.00116(8) Si4 0.0241(3) 0.0309(4) 0.0301(3) 0.0009(3) -0.0017(3) 0.0002(3) N1 0.0210(9) 0.0245(10) 0.0231(10) 0.0005(8) 0.0041(7) 0.0006(7) Cl1 0.0282(3) 0.0203(3) 0.0218(3) -0.0002(2) 0.0061(2) -0.0013(2) Cl2 0.0229(3) 0.0354(3) 0.0416(4) -0.0104(3) 0.0099(2) -0.0081(2) C7 0.0192(11) 0.0196(11) 0.0290(12) -0.0008(9) 0.0057(9) 0.0005(8) N2 0.0232(9) 0.0218(10) 0.0202(9) -0.0006(8) 0.0048(7) -0.0006(7) C5 0.0328(13) 0.0228(13) 0.0368(14) 0.0029(11) 0.0155(10) 0.0034(10) C6 0.0263(11) 0.0197(12) 0.0267(12) 0.0010(9) 0.0097(9) -0.0024(9) C1 0.0281(12) 0.0222(12) 0.0250(12) -0.0011(10) 0.0095(9) -0.0012(9) C4 0.0524(16) 0.0296(14) 0.0333(14) -0.0005(11) 0.0263(12) 0.0058(12) C2 0.0402(14) 0.0384(15) 0.0235(13) 0.0023(11) 0.0061(10) 0.0034(11) C3 0.0609(18) 0.0402(16) 0.0231(13) -0.0014(11) 0.0149(12) 0.0001(13) C8 0.0321(12) 0.0212(12) 0.0268(12) 0.0050(10) 0.0047(10) 0.0030(9) C9 0.0378(14) 0.0224(13) 0.0385(15) -0.0018(11) 0.0046(11) 0.0016(10) C12 0.0417(16) 0.0428(17) 0.0519(18) 0.0177(14) -0.0034(13) 0.0020(12) C10 0.0556(17) 0.0396(17) 0.0353(15) 0.0100(12) -0.0053(12) 0.0093(13) C13 0.0363(15) 0.0494(18) 0.0372(15) -0.0032(13) -0.0021(12) -0.0059(12) C11 0.0522(16) 0.0272(14) 0.0567(19) 0.0115(13) 0.0252(14) 0.0003(12) C14 0.0293(13) 0.0516(17) 0.0465(16) -0.0063(13) -0.0094(12) 0.0153(12) N3 0.0196(9) 0.0225(10) 0.0312(10) -0.0053(8) 0.0061(8) -0.0025(7) C15 0.0308(13) 0.0259(13) 0.0500(15) -0.0015(12) 0.0150(11) -0.0056(10) C16 0.0194(11) 0.0425(15) 0.0383(14) -0.0138(12) 0.0025(10) -0.0033(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N2 2.0128(17) . ? Zr1 N1 2.0884(18) . ? Zr1 N3 2.3583(17) . ? Zr1 Cl2 2.4394(7) . ? Zr1 Cl1 2.6140(7) . ? Zr1 C7 2.655(2) . ? Zr1 Cl1 2.7068(8) 3_665 ? Si4 N1 1.7769(19) . ? Si4 C14 1.862(3) . ? Si4 C13 1.864(3) . ? Si4 C12 1.870(3) . ? N1 C1 1.423(3) . ? Cl1 Zr1 2.7068(8) 3_665 ? C7 N2 1.482(3) . ? C7 C6 1.500(3) . ? C7 N3 1.506(3) . ? C7 H7 1.0000 . ? N2 C8 1.483(3) . ? C5 C4 1.373(3) . ? C5 C6 1.396(3) . ? C5 H5 0.9500 . ? C6 C1 1.414(3) . ? C1 C2 1.404(3) . ? C4 C3 1.382(4) . ? C4 H4 0.9500 . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C8 C10 1.527(3) . ? C8 C11 1.528(3) . ? C8 C9 1.530(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N3 C15 1.475(3) . ? N3 C16 1.482(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zr1 N1 92.04(7) . . ? N2 Zr1 N3 63.07(7) . . ? N1 Zr1 N3 84.67(7) . . ? N2 Zr1 Cl2 106.99(5) . . ? N1 Zr1 Cl2 97.85(6) . . ? N3 Zr1 Cl2 169.93(5) . . ? N2 Zr1 Cl1 142.22(5) . . ? N1 Zr1 Cl1 97.25(5) . . ? N3 Zr1 Cl1 81.39(5) . . ? Cl2 Zr1 Cl1 107.84(2) . . ? N2 Zr1 C7 33.59(6) . . ? N1 Zr1 C7 74.94(7) . . ? N3 Zr1 C7 34.32(6) . . ? Cl2 Zr1 C7 137.01(5) . . ? Cl1 Zr1 C7 115.08(5) . . ? N2 Zr1 Cl1 93.94(5) . 3_665 ? N1 Zr1 Cl1 172.23(5) . 3_665 ? N3 Zr1 Cl1 93.63(5) . 3_665 ? Cl2 Zr1 Cl1 85.13(3) . 3_665 ? Cl1 Zr1 Cl1 74.990(18) . 3_665 ? C7 Zr1 Cl1 107.73(5) . 3_665 ? N1 Si4 C14 112.15(10) . . ? N1 Si4 C13 109.45(11) . . ? C14 Si4 C13 106.55(13) . . ? N1 Si4 C12 110.13(11) . . ? C14 Si4 C12 105.21(14) . . ? C13 Si4 C12 113.29(13) . . ? C1 N1 Si4 117.46(15) . . ? C1 N1 Zr1 120.64(14) . . ? Si4 N1 Zr1 121.72(10) . . ? Zr1 Cl1 Zr1 105.010(18) . 3_665 ? N2 C7 C6 112.55(17) . . ? N2 C7 N3 100.98(15) . . ? C6 C7 N3 113.02(17) . . ? N2 C7 Zr1 48.71(9) . . ? C6 C7 Zr1 100.80(13) . . ? N3 C7 Zr1 62.01(9) . . ? N2 C7 H7 110.0 . . ? C6 C7 H7 110.0 . . ? N3 C7 H7 110.0 . . ? Zr1 C7 H7 148.4 . . ? C7 N2 C8 117.83(16) . . ? C7 N2 Zr1 97.70(12) . . ? C8 N2 Zr1 144.47(14) . . ? C4 C5 C6 122.1(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.9(2) . . ? C5 C6 C7 118.91(19) . . ? C1 C6 C7 121.20(19) . . ? C2 C1 C6 116.6(2) . . ? C2 C1 N1 122.7(2) . . ? C6 C1 N1 120.63(19) . . ? C5 C4 C3 118.9(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C3 C2 C1 122.4(2) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C4 C3 C2 120.0(2) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? N2 C8 C10 110.50(19) . . ? N2 C8 C11 106.92(18) . . ? C10 C8 C11 109.7(2) . . ? N2 C8 C9 111.23(18) . . ? C10 C8 C9 109.80(19) . . ? C11 C8 C9 108.6(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 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 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 N3 C16 108.59(18) . . ? C15 N3 C7 114.53(17) . . ? C16 N3 C7 108.26(17) . . ? C15 N3 Zr1 123.24(14) . . ? C16 N3 Zr1 115.63(13) . . ? C7 N3 Zr1 83.67(10) . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 C14 Si4 N1 C1 167.41(17) . . . . ? C13 Si4 N1 C1 -74.57(18) . . . . ? C12 Si4 N1 C1 50.61(19) . . . . ? C14 Si4 N1 Zr1 -17.40(16) . . . . ? C13 Si4 N1 Zr1 100.63(13) . . . . ? C12 Si4 N1 Zr1 -134.20(13) . . . . ? N2 Zr1 N1 C1 17.01(16) . . . . ? N3 Zr1 N1 C1 -45.70(15) . . . . ? Cl2 Zr1 N1 C1 124.48(15) . . . . ? Cl1 Zr1 N1 C1 -126.29(15) . . . . ? C7 Zr1 N1 C1 -12.20(15) . . . . ? Cl1 Zr1 N1 C1 -123.3(3) 3_665 . . . ? N2 Zr1 N1 Si4 -158.03(11) . . . . ? N3 Zr1 N1 Si4 139.25(11) . . . . ? Cl2 Zr1 N1 Si4 -50.57(11) . . . . ? Cl1 Zr1 N1 Si4 58.66(10) . . . . ? C7 Zr1 N1 Si4 172.76(12) . . . . ? Cl1 Zr1 N1 Si4 61.6(4) 3_665 . . . ? N2 Zr1 Cl1 Zr1 76.71(9) . . . 3_665 ? N1 Zr1 Cl1 Zr1 179.59(5) . . . 3_665 ? N3 Zr1 Cl1 Zr1 96.14(6) . . . 3_665 ? Cl2 Zr1 Cl1 Zr1 -79.71(4) . . . 3_665 ? C7 Zr1 Cl1 Zr1 102.86(6) . . . 3_665 ? Cl1 Zr1 Cl1 Zr1 0.0 3_665 . . 3_665 ? N1 Zr1 C7 N2 118.16(13) . . . . ? N3 Zr1 C7 N2 -138.94(18) . . . . ? Cl2 Zr1 C7 N2 32.81(15) . . . . ? Cl1 Zr1 C7 N2 -150.79(10) . . . . ? Cl1 Zr1 C7 N2 -69.45(12) 3_665 . . . ? N2 Zr1 C7 C6 -110.61(18) . . . . ? N1 Zr1 C7 C6 7.54(12) . . . . ? N3 Zr1 C7 C6 110.45(17) . . . . ? Cl2 Zr1 C7 C6 -77.80(14) . . . . ? Cl1 Zr1 C7 C6 98.60(12) . . . . ? Cl1 Zr1 C7 C6 179.94(11) 3_665 . . . ? N2 Zr1 C7 N3 138.94(18) . . . . ? N1 Zr1 C7 N3 -102.91(12) . . . . ? Cl2 Zr1 C7 N3 171.74(9) . . . . ? Cl1 Zr1 C7 N3 -11.85(12) . . . . ? Cl1 Zr1 C7 N3 69.49(11) 3_665 . . . ? C6 C7 N2 C8 -95.3(2) . . . . ? N3 C7 N2 C8 143.94(17) . . . . ? Zr1 C7 N2 C8 -179.8(2) . . . . ? C6 C7 N2 Zr1 84.57(16) . . . . ? N3 C7 N2 Zr1 -36.22(14) . . . . ? N1 Zr1 N2 C7 -58.42(12) . . . . ? N3 Zr1 N2 C7 24.55(11) . . . . ? Cl2 Zr1 N2 C7 -157.27(10) . . . . ? Cl1 Zr1 N2 C7 46.19(15) . . . . ? Cl1 Zr1 N2 C7 116.62(11) 3_665 . . . ? N1 Zr1 N2 C8 121.3(2) . . . . ? N3 Zr1 N2 C8 -155.7(3) . . . . ? Cl2 Zr1 N2 C8 22.5(2) . . . . ? Cl1 Zr1 N2 C8 -134.1(2) . . . . ? C7 Zr1 N2 C8 179.8(3) . . . . ? Cl1 Zr1 N2 C8 -63.6(2) 3_665 . . . ? C4 C5 C6 C1 1.5(3) . . . . ? C4 C5 C6 C7 -176.3(2) . . . . ? N2 C7 C6 C5 125.4(2) . . . . ? N3 C7 C6 C5 -121.0(2) . . . . ? Zr1 C7 C6 C5 175.01(16) . . . . ? N2 C7 C6 C1 -52.4(3) . . . . ? N3 C7 C6 C1 61.2(3) . . . . ? Zr1 C7 C6 C1 -2.8(2) . . . . ? C5 C6 C1 C2 -4.1(3) . . . . ? C7 C6 C1 C2 173.7(2) . . . . ? C5 C6 C1 N1 175.44(19) . . . . ? C7 C6 C1 N1 -6.8(3) . . . . ? Si4 N1 C1 C2 10.4(3) . . . . ? Zr1 N1 C1 C2 -164.80(18) . . . . ? Si4 N1 C1 C6 -169.02(16) . . . . ? Zr1 N1 C1 C6 15.7(3) . . . . ? C6 C5 C4 C3 1.9(4) . . . . ? C6 C1 C2 C3 3.4(4) . . . . ? N1 C1 C2 C3 -176.1(2) . . . . ? C5 C4 C3 C2 -2.6(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C7 N2 C8 C10 -66.8(2) . . . . ? Zr1 N2 C8 C10 113.5(2) . . . . ? C7 N2 C8 C11 173.87(19) . . . . ? Zr1 N2 C8 C11 -5.9(3) . . . . ? C7 N2 C8 C9 55.4(2) . . . . ? Zr1 N2 C8 C9 -124.3(2) . . . . ? N2 C7 N3 C15 153.94(17) . . . . ? C6 C7 N3 C15 33.5(2) . . . . ? Zr1 C7 N3 C15 123.75(17) . . . . ? N2 C7 N3 C16 -84.76(18) . . . . ? C6 C7 N3 C16 154.78(17) . . . . ? Zr1 C7 N3 C16 -114.94(15) . . . . ? N2 C7 N3 Zr1 30.19(12) . . . . ? C6 C7 N3 Zr1 -90.27(15) . . . . ? N2 Zr1 N3 C15 -139.32(18) . . . . ? N1 Zr1 N3 C15 -44.29(17) . . . . ? Cl2 Zr1 N3 C15 -149.3(2) . . . . ? Cl1 Zr1 N3 C15 53.89(16) . . . . ? C7 Zr1 N3 C15 -115.3(2) . . . . ? Cl1 Zr1 N3 C15 128.10(16) 3_665 . . . ? N2 Zr1 N3 C16 83.19(16) . . . . ? N1 Zr1 N3 C16 178.22(16) . . . . ? Cl2 Zr1 N3 C16 73.2(3) . . . . ? Cl1 Zr1 N3 C16 -83.60(15) . . . . ? C7 Zr1 N3 C16 107.2(2) . . . . ? Cl1 Zr1 N3 C16 -9.38(15) 3_665 . . . ? N2 Zr1 N3 C7 -24.05(11) . . . . ? N1 Zr1 N3 C7 70.97(12) . . . . ? Cl2 Zr1 N3 C7 -34.0(3) . . . . ? Cl1 Zr1 N3 C7 169.15(11) . . . . ? Cl1 Zr1 N3 C7 -116.63(11) 3_665 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.415 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.086 #==END data_Compound14 _database_code_CSD 181543 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sw038 _chemical_melting_point ? _chemical_formula_moiety 'C36 H60 N8 Zr2' _chemical_formula_sum 'C36 H60 N8 Zr2' _chemical_formula_weight 787.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 8.7107(2) _cell_length_b 18.7443(4) _cell_length_c 11.8704(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.1300(10) _cell_angle_gamma 90.00 _cell_volume 1887.48(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19939 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Cube _exptl_crystal_colour Orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.9170 _exptl_absorpt_correction_T_max 0.9712 _exptl_absorpt_process_details 'Sortav - Blessing' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Chi scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27335 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4320 _reflns_number_gt 3714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0853P)^2^+5.6896P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4320 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 0.577 _refine_ls_restrained_S_all 0.577 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8729(2) 0.90602(10) 0.12429(16) 0.0211(4) Uani 1 1 d . . . C2 C 0.9259(3) 0.91336(11) 0.24706(17) 0.0285(4) Uani 1 1 d . . . H2 H 1.0143 0.9432 0.2759 0.034 Uiso 1 1 calc R . . C3 C 0.8565(3) 0.87981(11) 0.32557(17) 0.0303(5) Uani 1 1 d . . . H3 H 0.8939 0.8884 0.4060 0.036 Uiso 1 1 calc R . . C4 C 0.7312(3) 0.83319(12) 0.28679(18) 0.0311(5) Uani 1 1 d . . . H4 H 0.6798 0.8109 0.3399 0.037 Uiso 1 1 calc R . . C5 C 0.6837(2) 0.82016(11) 0.17060(18) 0.0270(4) Uani 1 1 d . . . H5 H 0.6008 0.7869 0.1451 0.032 Uiso 1 1 calc R . . C6 C 0.7513(2) 0.85360(10) 0.08622(16) 0.0206(4) Uani 1 1 d . . . C7 C 0.6988(2) 0.83043(10) -0.03473(16) 0.0212(4) Uani 1 1 d . . . C8 C 0.5897(3) 0.76681(12) -0.05616(18) 0.0297(4) Uani 1 1 d . . . H8A H 0.4870 0.7802 -0.0419 0.045 Uiso 1 1 calc R . . H8B H 0.6350 0.7279 -0.0039 0.045 Uiso 1 1 calc R . . H8C H 0.5763 0.7510 -0.1365 0.045 Uiso 1 1 calc R . . C9 C 1.2971(2) 1.16022(11) 0.24041(16) 0.0222(4) Uani 1 1 d . . . H9 H 1.2456 1.1240 0.2814 0.027 Uiso 1 1 calc R . . C10 C 1.4726(2) 1.15379(13) 0.29876(18) 0.0293(4) Uani 1 1 d . . . H10A H 1.5109 1.1053 0.2863 0.035 Uiso 1 1 calc R . . H10B H 1.5341 1.1887 0.2645 0.035 Uiso 1 1 calc R . . C11 C 1.4952(3) 1.16805(14) 0.42842(19) 0.0340(5) Uani 1 1 d . . . H11A H 1.4417 1.1302 0.4634 0.041 Uiso 1 1 calc R . . H11B H 1.6090 1.1664 0.4658 0.041 Uiso 1 1 calc R . . C12 C 1.4289(3) 1.24018(14) 0.45037(18) 0.0344(5) Uani 1 1 d . . . H12A H 1.4857 1.2782 0.4186 0.041 Uiso 1 1 calc R . . H12B H 1.4452 1.2480 0.5347 0.041 Uiso 1 1 calc R . . C13 C 1.2535(3) 1.24461(13) 0.39434(18) 0.0309(5) Uani 1 1 d . . . H13A H 1.2136 1.2925 0.4084 0.037 Uiso 1 1 calc R . . H13B H 1.1959 1.2089 0.4304 0.037 Uiso 1 1 calc R . . C14 C 1.2217(3) 1.23110(12) 0.26442(17) 0.0270(4) Uani 1 1 d . . . H14A H 1.2659 1.2707 0.2264 0.032 Uiso 1 1 calc R . . H14B H 1.1066 1.2293 0.2318 0.032 Uiso 1 1 calc R . . C15 C 1.3514(4) 0.95927(15) 0.3248(2) 0.0468(7) Uani 1 1 d . . . H15A H 1.3604 0.9072 0.3230 0.070 Uiso 1 1 calc R . . H15B H 1.2743 0.9726 0.3697 0.070 Uiso 1 1 calc R . . H15C H 1.4542 0.9799 0.3609 0.070 Uiso 1 1 calc R . . C16 C 1.4150(3) 0.97113(13) 0.1393(2) 0.0385(5) Uani 1 1 d . . . H16A H 1.5184 0.9895 0.1792 0.058 Uiso 1 1 calc R . . H16B H 1.3820 0.9943 0.0636 0.058 Uiso 1 1 calc R . . H16C H 1.4220 0.9195 0.1286 0.058 Uiso 1 1 calc R . . C17 C 0.9450(3) 1.08882(13) 0.32870(19) 0.0340(5) Uani 1 1 d . . . H17A H 0.9373 1.1383 0.3534 0.051 Uiso 1 1 calc R . . H17B H 1.0427 1.0676 0.3735 0.051 Uiso 1 1 calc R . . H17C H 0.8545 1.0616 0.3417 0.051 Uiso 1 1 calc R . . C18 C 0.8030(3) 1.11821(13) 0.1374(2) 0.0332(5) Uani 1 1 d . . . H18A H 0.7117 1.0905 0.1478 0.050 Uiso 1 1 calc R . . H18B H 0.8078 1.1174 0.0558 0.050 Uiso 1 1 calc R . . H18C H 0.7928 1.1676 0.1617 0.050 Uiso 1 1 calc R . . N1 N 1.25264(18) 1.13745(9) 0.11708(13) 0.0200(3) Uani 1 1 d . . . N2 N 0.9410(2) 0.94688(9) 0.05475(14) 0.0208(3) Uani 1 1 d . . . N4 N 1.3004(2) 0.98606(10) 0.20803(16) 0.0288(4) Uani 1 1 d . . . N5 N 0.9458(2) 1.08734(9) 0.20698(14) 0.0230(3) Uani 1 1 d . . . Zr1 Zr 1.09869(2) 1.037832(9) 0.121741(14) 0.01786(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 0.0277(10) 0.0181(8) 0.0190(9) 0.0019(7) 0.0080(7) 0.0032(7) C2 0.0410(12) 0.0246(10) 0.0194(9) 0.0015(7) 0.0059(8) -0.0046(9) C3 0.0466(13) 0.0279(10) 0.0172(9) 0.0037(8) 0.0090(9) 0.0023(9) C4 0.0385(12) 0.0332(11) 0.0252(10) 0.0084(8) 0.0148(9) 0.0015(9) C5 0.0265(10) 0.0304(10) 0.0266(10) 0.0054(8) 0.0111(8) 0.0011(8) C6 0.0215(9) 0.0217(9) 0.0200(9) 0.0033(7) 0.0077(7) 0.0040(7) C7 0.0189(9) 0.0227(9) 0.0223(9) 0.0014(7) 0.0053(7) 0.0029(7) C8 0.0316(11) 0.0328(11) 0.0254(10) 0.0021(8) 0.0077(8) -0.0081(9) C9 0.0235(9) 0.0260(9) 0.0173(9) -0.0016(7) 0.0054(7) -0.0018(8) C10 0.0216(10) 0.0407(12) 0.0251(10) 0.0006(9) 0.0046(8) 0.0005(9) C11 0.0275(11) 0.0476(13) 0.0235(10) 0.0039(9) -0.0012(8) -0.0064(10) C12 0.0335(12) 0.0476(14) 0.0215(10) -0.0051(9) 0.0048(9) -0.0159(10) C13 0.0298(11) 0.0401(12) 0.0239(10) -0.0102(9) 0.0083(8) -0.0059(9) C14 0.0272(10) 0.0309(10) 0.0227(10) -0.0050(8) 0.0055(8) 0.0011(8) C15 0.0453(15) 0.0490(16) 0.0385(14) 0.0171(11) -0.0063(12) 0.0013(11) C16 0.0333(12) 0.0384(13) 0.0426(14) -0.0053(10) 0.0059(10) 0.0106(10) C17 0.0435(13) 0.0370(12) 0.0264(11) -0.0054(9) 0.0181(9) -0.0058(10) C18 0.0300(11) 0.0340(12) 0.0376(12) -0.0007(9) 0.0117(9) 0.0045(9) N1 0.0200(8) 0.0224(8) 0.0179(7) -0.0007(6) 0.0048(6) 0.0015(6) N2 0.0253(8) 0.0209(7) 0.0172(8) 0.0008(6) 0.0066(6) -0.0010(6) N4 0.0287(9) 0.0269(9) 0.0288(9) 0.0052(7) 0.0022(7) 0.0033(7) N5 0.0273(8) 0.0236(8) 0.0205(8) -0.0023(6) 0.0102(6) -0.0024(7) Zr1 0.02178(11) 0.01821(11) 0.01415(11) 0.00092(6) 0.00525(7) 0.00068(6) _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 1.358(2) . ? C1 C2 1.432(3) . ? C1 C6 1.440(3) . ? C2 C3 1.373(3) . ? C3 C4 1.392(3) . ? C4 C5 1.369(3) . ? C5 C6 1.418(3) . ? C6 C7 1.470(3) . ? C7 N1 1.298(2) 3_775 ? C7 C8 1.510(3) . ? C9 N1 1.489(2) . ? C9 C10 1.533(3) . ? C9 C14 1.537(3) . ? C10 C11 1.530(3) . ? C11 C12 1.516(4) . ? C12 C13 1.524(3) . ? C13 C14 1.525(3) . ? C15 N4 1.446(3) . ? C16 N4 1.453(3) . ? C17 N5 1.447(3) . ? C18 N5 1.448(3) . ? N1 C7 1.298(2) 3_775 ? N1 Zr1 2.3069(16) . ? N2 Zr1 2.0644(16) 3_775 ? N2 Zr1 2.2200(17) . ? N4 Zr1 2.0642(18) . ? N5 Zr1 2.0664(16) . ? Zr1 N2 2.0644(16) 3_775 ? Zr1 Zr1 3.3262(3) 3_775 ? 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 C2 118.69(18) . . ? N2 C1 C6 125.88(17) . . ? C2 C1 C6 115.42(17) . . ? C3 C2 C1 123.8(2) . . ? C2 C3 C4 119.73(19) . . ? C5 C4 C3 118.70(19) . . ? C4 C5 C6 123.6(2) . . ? C5 C6 C1 118.28(17) . . ? C5 C6 C7 118.17(18) . . ? C1 C6 C7 123.49(17) . . ? N1 C7 C6 121.06(17) 3_775 . ? N1 C7 C8 122.67(17) 3_775 . ? C6 C7 C8 116.25(17) . . ? N1 C9 C10 115.58(16) . . ? N1 C9 C14 113.78(16) . . ? C10 C9 C14 114.11(17) . . ? C11 C10 C9 109.14(17) . . ? C12 C11 C10 111.21(19) . . ? C11 C12 C13 110.92(18) . . ? C12 C13 C14 111.48(18) . . ? C13 C14 C9 110.12(18) . . ? C7 N1 C9 123.42(17) 3_775 . ? C7 N1 Zr1 133.18(13) 3_775 . ? C9 N1 Zr1 103.37(11) . . ? C1 N2 Zr1 134.41(14) . 3_775 ? C1 N2 Zr1 122.40(13) . . ? Zr1 N2 Zr1 101.79(7) 3_775 . ? C15 N4 C16 111.8(2) . . ? C15 N4 Zr1 132.88(18) . . ? C16 N4 Zr1 115.34(15) . . ? C17 N5 C18 111.30(17) . . ? C17 N5 Zr1 130.35(15) . . ? C18 N5 Zr1 117.77(13) . . ? N4 Zr1 N5 122.60(7) . . ? N4 Zr1 N2 119.76(7) . 3_775 ? N5 Zr1 N2 117.16(7) . 3_775 ? N4 Zr1 N2 101.79(7) . . ? N5 Zr1 N2 96.05(6) . . ? N2 Zr1 N2 78.21(7) 3_775 . ? N4 Zr1 N1 87.62(7) . . ? N5 Zr1 N1 95.22(6) . . ? N2 Zr1 N1 80.07(6) 3_775 . ? N2 Zr1 N1 158.22(6) . . ? N4 Zr1 Zr1 116.39(5) . 3_775 ? N5 Zr1 Zr1 110.71(5) . 3_775 ? N2 Zr1 Zr1 40.80(5) 3_775 3_775 ? N2 Zr1 Zr1 37.41(4) . 3_775 ? N1 Zr1 Zr1 120.85(4) . 3_775 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.771 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.063 #==END data_Compound15 _database_code_CSD 181544 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 99skl003 _chemical_melting_point ? _chemical_formula_moiety 'C31 H43 Cl N6 O Ti' _chemical_formula_sum 'C31 H43 Cl N6 O Ti' _chemical_formula_weight 599.06 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.205(2) _cell_length_b 10.252(2) _cell_length_c 14.980(3) _cell_angle_alpha 87.61(3) _cell_angle_beta 84.12(3) _cell_angle_gamma 76.98(3) _cell_volume 1518.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5193 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 26.022 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9801 _exptl_absorpt_correction_T_max 0.9801 _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 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13977 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5918 _reflns_number_gt 3822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1400P)^2^+1.8895P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5918 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 0.712 _refine_ls_restrained_S_all 0.712 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.26658(6) 0.31681(5) 0.16111(4) 0.02167(19) Uani 1 1 d . . . Cl1 Cl 0.29287(9) 0.50131(8) 0.06551(6) 0.0339(2) Uani 1 1 d . . . N11 N 0.0992(3) 0.2900(2) 0.23076(17) 0.0221(6) Uani 1 1 d . . . N12 N 0.1508(3) 0.2541(3) 0.04499(18) 0.0267(6) Uani 1 1 d . . . C17 C 0.1784(3) 0.1179(3) 0.0891(2) 0.0250(7) Uani 1 1 d . . . H17 H 0.1974 0.0461 0.0434 0.030 Uiso 1 1 calc R . . C18 C 0.2313(4) 0.2479(4) -0.0430(2) 0.0370(9) Uani 1 1 d . . . H18A H 0.1983 0.1923 -0.0833 0.056 Uiso 1 1 calc R . . H18B H 0.3264 0.2088 -0.0352 0.056 Uiso 1 1 calc R . . H18C H 0.2227 0.3385 -0.0689 0.056 Uiso 1 1 calc R . . C19 C 0.0068(4) 0.3077(4) 0.0331(2) 0.0346(9) Uani 1 1 d . . . H19A H -0.0040 0.3947 0.0017 0.052 Uiso 1 1 calc R . . H19B H -0.0455 0.3185 0.0920 0.052 Uiso 1 1 calc R . . H19C H -0.0258 0.2454 -0.0023 0.052 Uiso 1 1 calc R . . C11 C 0.0368(3) 0.1829(3) 0.2341(2) 0.0206(7) Uani 1 1 d . . . C12 C -0.0572(3) 0.1580(3) 0.3030(2) 0.0262(7) Uani 1 1 d . . . H12 H -0.0797 0.2144 0.3536 0.031 Uiso 1 1 calc R . . C15 C 0.0077(4) -0.0101(3) 0.1569(2) 0.0292(8) Uani 1 1 d . . . H15 H 0.0304 -0.0682 0.1073 0.035 Uiso 1 1 calc R . . C16 C 0.0697(3) 0.0968(3) 0.1598(2) 0.0238(7) Uani 1 1 d . . . C14 C -0.0867(4) -0.0333(3) 0.2253(3) 0.0320(8) Uani 1 1 d . . . H14 H -0.1293 -0.1062 0.2224 0.038 Uiso 1 1 calc R . . C13 C -0.1183(4) 0.0506(3) 0.2977(2) 0.0312(8) Uani 1 1 d . . . H13 H -0.1829 0.0347 0.3448 0.037 Uiso 1 1 calc R . . N21 N 0.3017(3) 0.1254(2) 0.12872(17) 0.0213(6) Uani 1 1 d . . . N22 N 0.5069(3) 0.2614(3) 0.14903(18) 0.0254(6) Uani 1 1 d . . . C27 C 0.4905(3) 0.1802(3) 0.2329(2) 0.0252(7) Uani 1 1 d . . . H27 H 0.5626 0.1829 0.2729 0.030 Uiso 1 1 calc R . . C28 C 0.5916(4) 0.1874(4) 0.0732(2) 0.0318(8) Uani 1 1 d . . . H28A H 0.5983 0.2489 0.0219 0.048 Uiso 1 1 calc R . . H28B H 0.5506 0.1156 0.0562 0.048 Uiso 1 1 calc R . . H28C H 0.6821 0.1488 0.0912 0.048 Uiso 1 1 calc R . . C29 C 0.5667(4) 0.3741(3) 0.1694(2) 0.0331(8) Uani 1 1 d . . . H29A H 0.6592 0.3392 0.1851 0.050 Uiso 1 1 calc R . . H29B H 0.5125 0.4238 0.2201 0.050 Uiso 1 1 calc R . . H29C H 0.5680 0.4338 0.1167 0.050 Uiso 1 1 calc R . . C21 C 0.3810(3) 0.0151(3) 0.1670(2) 0.0228(7) Uani 1 1 d . . . C22 C 0.3695(4) -0.1178(3) 0.1572(2) 0.0278(8) Uani 1 1 d . . . H22 H 0.2997 -0.1352 0.1252 0.033 Uiso 1 1 calc R . . C23 C 0.4592(4) -0.2236(3) 0.1941(2) 0.0326(8) Uani 1 1 d . . . H23 H 0.4512 -0.3128 0.1859 0.039 Uiso 1 1 calc R . . C25 C 0.5706(4) -0.0696(3) 0.2536(2) 0.0284(8) Uani 1 1 d . . . H25 H 0.6394 -0.0537 0.2872 0.034 Uiso 1 1 calc R . . C24 C 0.5595(4) -0.2013(3) 0.2422(2) 0.0324(8) Uani 1 1 d . . . H24 H 0.6203 -0.2742 0.2674 0.039 Uiso 1 1 calc R . . C26 C 0.4836(3) 0.0379(3) 0.2169(2) 0.0235(7) Uani 1 1 d . . . N31 N 0.3602(3) 0.2580(2) 0.27002(17) 0.0216(6) Uani 1 1 d . . . N32 N 0.1473(3) 0.4844(2) 0.26142(18) 0.0265(6) Uani 1 1 d . . . C37 C 0.0898(3) 0.3744(3) 0.3081(2) 0.0236(7) Uani 1 1 d . . . H37 H -0.0065 0.4085 0.3320 0.028 Uiso 1 1 calc R . . C38 C 0.0375(4) 0.5802(3) 0.2204(3) 0.0371(9) Uani 1 1 d . . . H38A H -0.0281 0.6258 0.2678 0.056 Uiso 1 1 calc R . . H38B H -0.0077 0.5318 0.1826 0.056 Uiso 1 1 calc R . . H38C H 0.0756 0.6465 0.1836 0.056 Uiso 1 1 calc R . . C39 C 0.2115(4) 0.5582(4) 0.3191(2) 0.0373(9) Uani 1 1 d . . . H39A H 0.2380 0.6333 0.2849 0.056 Uiso 1 1 calc R . . H39B H 0.2919 0.4984 0.3403 0.056 Uiso 1 1 calc R . . H39C H 0.1477 0.5925 0.3707 0.056 Uiso 1 1 calc R . . C31 C 0.3083(3) 0.2400(3) 0.3569(2) 0.0212(7) Uani 1 1 d . . . C36 C 0.1722(3) 0.3029(3) 0.3807(2) 0.0232(7) Uani 1 1 d . . . C32 C 0.3830(4) 0.1684(3) 0.4237(2) 0.0269(7) Uani 1 1 d . . . H32 H 0.4748 0.1246 0.4091 0.032 Uiso 1 1 calc R . . C35 C 0.1140(4) 0.2931(3) 0.4684(2) 0.0276(8) Uani 1 1 d . . . H35 H 0.0217 0.3346 0.4833 0.033 Uiso 1 1 calc R . . C34 C 0.1899(4) 0.2233(3) 0.5341(2) 0.0304(8) Uani 1 1 d . . . H34 H 0.1506 0.2183 0.5940 0.037 Uiso 1 1 calc R . . C33 C 0.3245(4) 0.1607(3) 0.5108(2) 0.0303(8) Uani 1 1 d . . . H33 H 0.3768 0.1122 0.5553 0.036 Uiso 1 1 calc R . . O4 O 0.2493(3) 0.7153(2) 0.50643(17) 0.0364(6) Uani 1 1 d . . . C41 C 0.2889(4) 0.8186(4) 0.4531(3) 0.0442(10) Uani 1 1 d . . . H41A H 0.3577 0.7792 0.4044 0.053 Uiso 1 1 calc R . . H41B H 0.3303 0.8731 0.4902 0.053 Uiso 1 1 calc R . . C42 C 0.1720(5) 0.9056(4) 0.4136(3) 0.0469(11) Uani 1 1 d . . . H42A H 0.1341 0.8528 0.3741 0.070 Uiso 1 1 calc R . . H42B H 0.2016 0.9786 0.3788 0.070 Uiso 1 1 calc R . . H42C H 0.1030 0.9431 0.4617 0.070 Uiso 1 1 calc R . . C43 C 0.3573(5) 0.6339(5) 0.5480(4) 0.0597(13) Uani 1 1 d . . . H43A H 0.3913 0.6886 0.5895 0.072 Uiso 1 1 calc R . . H43B H 0.4319 0.5987 0.5018 0.072 Uiso 1 1 calc R . . C44 C 0.3161(5) 0.5216(4) 0.5983(3) 0.0577(12) Uani 1 1 d . . . H44A H 0.2499 0.5559 0.6487 0.086 Uiso 1 1 calc R . . H44B H 0.3954 0.4623 0.6212 0.086 Uiso 1 1 calc R . . H44C H 0.2755 0.4716 0.5585 0.086 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 0.0252(3) 0.0207(3) 0.0191(3) 0.0006(2) -0.0003(2) -0.0061(2) Cl1 0.0410(5) 0.0295(5) 0.0307(5) 0.0095(3) -0.0003(4) -0.0101(4) N11 0.0256(15) 0.0194(13) 0.0206(14) -0.0041(10) -0.0007(11) -0.0034(11) N12 0.0308(16) 0.0293(15) 0.0192(15) 0.0017(11) -0.0023(12) -0.0053(12) C17 0.0312(19) 0.0248(17) 0.0188(17) -0.0038(13) -0.0016(14) -0.0059(14) C18 0.046(2) 0.046(2) 0.0207(19) 0.0016(15) -0.0003(16) -0.0155(18) C19 0.037(2) 0.035(2) 0.032(2) 0.0033(15) -0.0112(17) -0.0049(16) C11 0.0204(16) 0.0186(15) 0.0218(17) 0.0003(12) -0.0023(13) -0.0026(12) C12 0.0246(18) 0.0280(17) 0.0252(18) -0.0019(13) -0.0020(14) -0.0039(14) C15 0.0279(19) 0.0291(18) 0.032(2) -0.0097(14) -0.0081(15) -0.0056(15) C16 0.0225(17) 0.0233(16) 0.0257(18) -0.0012(13) -0.0049(14) -0.0046(13) C14 0.0271(19) 0.0289(18) 0.043(2) -0.0028(15) -0.0013(16) -0.0128(15) C13 0.0249(19) 0.0312(19) 0.038(2) 0.0024(15) 0.0007(16) -0.0094(15) N21 0.0228(14) 0.0236(14) 0.0182(14) -0.0025(10) -0.0027(11) -0.0058(11) N22 0.0277(16) 0.0271(14) 0.0225(15) 0.0022(11) 0.0010(12) -0.0105(12) C27 0.0271(18) 0.0285(17) 0.0214(17) -0.0021(13) 0.0002(14) -0.0097(14) C28 0.033(2) 0.0362(19) 0.0241(18) -0.0005(14) 0.0059(15) -0.0077(16) C29 0.036(2) 0.0325(19) 0.034(2) 0.0005(15) -0.0028(17) -0.0153(16) C21 0.0231(17) 0.0255(17) 0.0182(16) -0.0018(13) 0.0062(13) -0.0054(13) C22 0.0275(19) 0.0250(17) 0.0295(19) -0.0054(14) 0.0064(15) -0.0062(14) C23 0.035(2) 0.0235(17) 0.036(2) 0.0007(15) 0.0099(17) -0.0053(15) C25 0.0251(18) 0.0307(18) 0.0264(18) 0.0024(14) 0.0036(15) -0.0027(14) C24 0.033(2) 0.0254(18) 0.032(2) 0.0088(14) 0.0039(16) 0.0017(15) C26 0.0213(17) 0.0276(17) 0.0199(17) 0.0019(13) 0.0035(13) -0.0049(13) N31 0.0236(15) 0.0244(14) 0.0181(14) -0.0018(10) -0.0013(11) -0.0082(11) N32 0.0368(17) 0.0189(13) 0.0240(15) -0.0011(11) 0.0009(13) -0.0082(12) C37 0.0263(18) 0.0219(16) 0.0212(17) -0.0024(12) 0.0026(14) -0.0046(13) C38 0.043(2) 0.0232(17) 0.039(2) 0.0018(15) 0.0017(18) 0.0015(16) C39 0.053(3) 0.0276(19) 0.033(2) -0.0077(15) 0.0058(18) -0.0156(17) C31 0.0269(18) 0.0198(15) 0.0189(16) -0.0021(12) -0.0002(13) -0.0101(13) C36 0.0286(18) 0.0196(16) 0.0231(17) -0.0022(12) 0.0027(14) -0.0108(13) C32 0.0265(18) 0.0284(17) 0.0265(18) 0.0000(13) -0.0027(14) -0.0080(14) C35 0.0322(19) 0.0259(17) 0.0258(18) -0.0018(13) 0.0019(15) -0.0108(14) C34 0.045(2) 0.0306(18) 0.0179(17) -0.0008(14) 0.0033(16) -0.0157(16) C33 0.043(2) 0.0295(18) 0.0201(18) 0.0056(13) -0.0089(16) -0.0094(16) O4 0.0356(15) 0.0313(13) 0.0394(15) 0.0033(11) -0.0017(12) -0.0028(11) C41 0.040(2) 0.042(2) 0.051(3) 0.0084(19) -0.005(2) -0.0107(18) C42 0.060(3) 0.034(2) 0.050(3) 0.0019(18) -0.018(2) -0.011(2) C43 0.037(3) 0.055(3) 0.083(4) 0.025(2) -0.005(2) -0.008(2) C44 0.056(3) 0.045(2) 0.068(3) 0.011(2) 0.001(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N11 1.976(3) . ? Ti1 N31 1.979(3) . ? Ti1 N21 1.985(3) . ? Ti1 N32 2.365(3) . ? Ti1 Cl1 2.3717(12) . ? Ti1 N22 2.379(3) . ? Ti1 N12 2.385(3) . ? Ti1 C27 2.698(4) . ? Ti1 C37 2.696(3) . ? N11 C11 1.384(4) . ? N11 C37 1.458(4) . ? N12 C18 1.476(4) . ? N12 C19 1.475(5) . ? N12 C17 1.500(4) . ? C17 N21 1.464(4) . ? C17 C16 1.499(5) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C11 C12 1.392(5) . ? C11 C16 1.415(5) . ? C12 C13 1.391(5) . ? C12 H12 0.9500 . ? C15 C16 1.388(5) . ? C15 C14 1.383(5) . ? C15 H15 0.9500 . ? C14 C13 1.378(5) . ? C14 H14 0.9500 . ? C13 H13 0.9500 . ? N21 C21 1.376(4) . ? N22 C29 1.478(4) . ? N22 C28 1.480(4) . ? N22 C27 1.495(4) . ? C27 N31 1.457(4) . ? C27 C26 1.506(4) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C21 C26 1.413(5) . ? C21 C22 1.408(5) . ? C22 C23 1.387(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(5) . ? C23 H23 0.9500 . ? C25 C26 1.384(5) . ? C25 C24 1.398(5) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? N31 C31 1.375(4) . ? N32 C39 1.464(5) . ? N32 C38 1.481(5) . ? N32 C37 1.501(4) . ? C37 C36 1.506(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C31 C32 1.401(5) . ? C31 C36 1.409(5) . ? C36 C35 1.395(5) . ? C32 C33 1.385(5) . ? C32 H32 0.9500 . ? C35 C34 1.388(5) . ? C35 H35 0.9500 . ? C34 C33 1.395(5) . ? C34 H34 0.9500 . ? C33 H33 0.9500 . ? O4 C43 1.408(5) . ? O4 C41 1.407(4) . ? C41 C42 1.480(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.466(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ti1 N31 87.34(11) . . ? N11 Ti1 N21 87.13(11) . . ? N31 Ti1 N21 87.75(11) . . ? N11 Ti1 N32 61.16(10) . . ? N31 Ti1 N32 80.02(11) . . ? N21 Ti1 N32 146.24(10) . . ? N11 Ti1 Cl1 127.29(8) . . ? N31 Ti1 Cl1 126.34(8) . . ? N21 Ti1 Cl1 127.60(8) . . ? N32 Ti1 Cl1 83.94(7) . . ? N11 Ti1 N22 145.72(10) . . ? N31 Ti1 N22 60.87(10) . . ? N21 Ti1 N22 79.63(11) . . ? N32 Ti1 N22 119.58(10) . . ? Cl1 Ti1 N22 84.82(7) . . ? N11 Ti1 N12 79.36(10) . . ? N31 Ti1 N12 146.25(10) . . ? N21 Ti1 N12 60.93(10) . . ? N32 Ti1 N12 118.48(10) . . ? Cl1 Ti1 N12 85.50(7) . . ? N22 Ti1 N12 119.46(10) . . ? N11 Ti1 C27 112.22(11) . . ? N31 Ti1 C27 31.83(10) . . ? N21 Ti1 C27 70.48(11) . . ? N32 Ti1 C27 109.20(10) . . ? Cl1 Ti1 C27 116.20(8) . . ? N22 Ti1 C27 33.50(9) . . ? N12 Ti1 C27 129.51(10) . . ? N11 Ti1 C37 31.87(10) . . ? N31 Ti1 C37 70.45(11) . . ? N21 Ti1 C37 112.53(10) . . ? N32 Ti1 C37 33.71(9) . . ? Cl1 Ti1 C37 115.88(7) . . ? N22 Ti1 C37 129.40(10) . . ? N12 Ti1 C37 108.32(10) . . ? C27 Ti1 C37 101.84(10) . . ? C11 N11 C37 121.7(3) . . ? C11 N11 Ti1 130.5(2) . . ? C37 N11 Ti1 102.42(19) . . ? C18 N12 C19 109.6(3) . . ? C18 N12 C17 109.0(3) . . ? C19 N12 C17 113.4(3) . . ? C18 N12 Ti1 111.9(2) . . ? C19 N12 Ti1 124.8(2) . . ? C17 N12 Ti1 85.17(18) . . ? N21 C17 C16 111.4(3) . . ? N21 C17 N12 98.3(2) . . ? C16 C17 N12 113.9(3) . . ? N21 C17 H17 110.9 . . ? C16 C17 H17 110.9 . . ? N12 C17 H17 110.9 . . ? N12 C18 H18A 109.5 . . ? N12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 H19A 109.5 . . ? N12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N11 C11 C12 124.7(3) . . ? N11 C11 C16 116.3(3) . . ? C12 C11 C16 119.0(3) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C11 119.6(3) . . ? C15 C16 C17 121.5(3) . . ? C11 C16 C17 118.8(3) . . ? C13 C14 C15 119.3(3) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C21 N21 C17 121.8(3) . . ? C21 N21 Ti1 129.6(2) . . ? C17 N21 Ti1 102.48(19) . . ? C29 N22 C28 108.2(3) . . ? C29 N22 C27 108.9(3) . . ? C28 N22 C27 115.3(3) . . ? C29 N22 Ti1 113.4(2) . . ? C28 N22 Ti1 123.8(2) . . ? C27 N22 Ti1 85.03(18) . . ? N31 C27 C26 111.2(3) . . ? N31 C27 N22 98.4(2) . . ? C26 C27 N22 114.1(3) . . ? N31 C27 Ti1 45.74(14) . . ? C26 C27 Ti1 101.1(2) . . ? N22 C27 Ti1 61.47(16) . . ? N31 C27 H27 110.9 . . ? C26 C27 H27 110.9 . . ? N22 C27 H27 110.9 . . ? Ti1 C27 H27 146.7 . . ? N22 C28 H28A 109.5 . . ? N22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N22 C29 H29A 109.5 . . ? N22 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N22 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N21 C21 C26 116.9(3) . . ? N21 C21 C22 124.6(3) . . ? C26 C21 C22 118.5(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C26 C25 C24 121.4(3) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C23 C24 C25 119.1(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C25 C26 C21 119.7(3) . . ? C25 C26 C27 121.6(3) . . ? C21 C26 C27 118.7(3) . . ? C31 N31 C27 122.3(3) . . ? C31 N31 Ti1 130.2(2) . . ? C27 N31 Ti1 102.42(19) . . ? C39 N32 C38 108.6(3) . . ? C39 N32 C37 114.9(3) . . ? C38 N32 C37 108.7(3) . . ? C39 N32 Ti1 124.3(2) . . ? C38 N32 Ti1 112.6(2) . . ? C37 N32 Ti1 85.35(16) . . ? N11 C37 C36 111.9(3) . . ? N11 C37 N32 98.0(2) . . ? C36 C37 N32 113.4(3) . . ? N11 C37 Ti1 45.71(14) . . ? C36 C37 Ti1 101.4(2) . . ? N32 C37 Ti1 60.94(15) . . ? N11 C37 H37 111.0 . . ? C36 C37 H37 111.0 . . ? N32 C37 H37 111.0 . . ? Ti1 C37 H37 146.5 . . ? N32 C38 H38A 109.5 . . ? N32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N32 C39 H39A 109.5 . . ? N32 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N32 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N31 C31 C32 124.4(3) . . ? N31 C31 C36 117.3(3) . . ? C32 C31 C36 118.2(3) . . ? C35 C36 C31 120.5(3) . . ? C35 C36 C37 121.0(3) . . ? C31 C36 C37 118.4(3) . . ? C31 C32 C33 120.7(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C36 C35 C34 120.6(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C34 C33 C32 120.9(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C43 O4 C41 112.5(3) . . ? O4 C41 C42 111.1(3) . . ? O4 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? O4 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O4 C43 C44 111.7(4) . . ? O4 C43 H43A 109.3 . . ? C44 C43 H43A 109.3 . . ? O4 C43 H43B 109.3 . . ? C44 C43 H43B 109.3 . . ? H43A C43 H43B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? 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 N31 Ti1 N11 C11 -97.6(3) . . . . ? N21 Ti1 N11 C11 -9.7(3) . . . . ? N32 Ti1 N11 C11 -177.7(3) . . . . ? Cl1 Ti1 N11 C11 127.1(2) . . . . ? N22 Ti1 N11 C11 -76.6(3) . . . . ? N12 Ti1 N11 C11 51.2(3) . . . . ? C27 Ti1 N11 C11 -77.3(3) . . . . ? C37 Ti1 N11 C11 -153.6(4) . . . . ? N31 Ti1 N11 C37 55.95(19) . . . . ? N21 Ti1 N11 C37 143.83(19) . . . . ? N32 Ti1 N11 C37 -24.11(17) . . . . ? Cl1 Ti1 N11 C37 -79.3(2) . . . . ? N22 Ti1 N11 C37 77.0(2) . . . . ? N12 Ti1 N11 C37 -155.22(19) . . . . ? C27 Ti1 N11 C37 76.3(2) . . . . ? N11 Ti1 N12 C18 -178.3(2) . . . . ? N31 Ti1 N12 C18 -109.8(3) . . . . ? N21 Ti1 N12 C18 -85.6(2) . . . . ? N32 Ti1 N12 C18 133.0(2) . . . . ? Cl1 Ti1 N12 C18 52.4(2) . . . . ? N22 Ti1 N12 C18 -29.0(2) . . . . ? C27 Ti1 N12 C18 -68.2(2) . . . . ? C37 Ti1 N12 C18 168.2(2) . . . . ? N11 Ti1 N12 C19 45.6(2) . . . . ? N31 Ti1 N12 C19 114.1(3) . . . . ? N21 Ti1 N12 C19 138.2(3) . . . . ? N32 Ti1 N12 C19 -3.1(3) . . . . ? Cl1 Ti1 N12 C19 -83.7(2) . . . . ? N22 Ti1 N12 C19 -165.2(2) . . . . ? C27 Ti1 N12 C19 155.7(2) . . . . ? C37 Ti1 N12 C19 32.1(3) . . . . ? N11 Ti1 N12 C17 -69.74(18) . . . . ? N31 Ti1 N12 C17 -1.2(3) . . . . ? N21 Ti1 N12 C17 22.90(17) . . . . ? N32 Ti1 N12 C17 -118.41(18) . . . . ? Cl1 Ti1 N12 C17 160.98(17) . . . . ? N22 Ti1 N12 C17 79.51(19) . . . . ? C27 Ti1 N12 C17 40.4(2) . . . . ? C37 Ti1 N12 C17 -83.22(19) . . . . ? C18 N12 C17 N21 83.8(3) . . . . ? C19 N12 C17 N21 -153.8(3) . . . . ? Ti1 N12 C17 N21 -27.78(19) . . . . ? C18 N12 C17 C16 -158.3(3) . . . . ? C19 N12 C17 C16 -35.9(4) . . . . ? Ti1 N12 C17 C16 90.1(3) . . . . ? C37 N11 C11 C12 11.3(5) . . . . ? Ti1 N11 C11 C12 160.6(2) . . . . ? C37 N11 C11 C16 -170.8(3) . . . . ? Ti1 N11 C11 C16 -21.5(4) . . . . ? N11 C11 C12 C13 177.2(3) . . . . ? C16 C11 C12 C13 -0.7(5) . . . . ? C14 C15 C16 C11 0.5(5) . . . . ? C14 C15 C16 C17 176.0(3) . . . . ? N11 C11 C16 C15 -177.9(3) . . . . ? C12 C11 C16 C15 0.1(5) . . . . ? N11 C11 C16 C17 6.5(4) . . . . ? C12 C11 C16 C17 -175.5(3) . . . . ? N21 C17 C16 C15 -124.4(3) . . . . ? N12 C17 C16 C15 125.4(3) . . . . ? N21 C17 C16 C11 51.1(4) . . . . ? N12 C17 C16 C11 -59.0(4) . . . . ? C16 C15 C14 C13 -0.7(5) . . . . ? C15 C14 C13 C12 0.1(5) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C16 C17 N21 C21 69.9(4) . . . . ? N12 C17 N21 C21 -170.3(3) . . . . ? C16 C17 N21 Ti1 -85.0(2) . . . . ? N12 C17 N21 Ti1 34.9(2) . . . . ? N11 Ti1 N21 C21 -96.7(3) . . . . ? N31 Ti1 N21 C21 -9.2(3) . . . . ? N32 Ti1 N21 C21 -77.5(3) . . . . ? Cl1 Ti1 N21 C21 126.7(2) . . . . ? N22 Ti1 N21 C21 51.6(3) . . . . ? N12 Ti1 N21 C21 -176.1(3) . . . . ? C27 Ti1 N21 C21 18.1(3) . . . . ? C37 Ti1 N21 C21 -77.0(3) . . . . ? N11 Ti1 N21 C17 55.40(19) . . . . ? N31 Ti1 N21 C17 142.85(19) . . . . ? N32 Ti1 N21 C17 74.6(3) . . . . ? Cl1 Ti1 N21 C17 -81.2(2) . . . . ? N22 Ti1 N21 C17 -156.37(19) . . . . ? N12 Ti1 N21 C17 -24.01(17) . . . . ? C27 Ti1 N21 C17 170.2(2) . . . . ? C37 Ti1 N21 C17 75.1(2) . . . . ? N11 Ti1 N22 C29 -109.6(2) . . . . ? N31 Ti1 N22 C29 -85.4(2) . . . . ? N21 Ti1 N22 C29 -178.6(2) . . . . ? N32 Ti1 N22 C29 -28.4(2) . . . . ? Cl1 Ti1 N22 C29 51.7(2) . . . . ? N12 Ti1 N22 C29 133.5(2) . . . . ? C27 Ti1 N22 C29 -108.4(3) . . . . ? C37 Ti1 N22 C29 -67.9(2) . . . . ? N11 Ti1 N22 C28 116.0(3) . . . . ? N31 Ti1 N22 C28 140.3(3) . . . . ? N21 Ti1 N22 C28 47.0(2) . . . . ? N32 Ti1 N22 C28 -162.7(2) . . . . ? Cl1 Ti1 N22 C28 -82.7(2) . . . . ? N12 Ti1 N22 C28 -0.8(3) . . . . ? C27 Ti1 N22 C28 117.2(3) . . . . ? C37 Ti1 N22 C28 157.8(2) . . . . ? N11 Ti1 N22 C27 -1.2(3) . . . . ? N31 Ti1 N22 C27 23.05(16) . . . . ? N21 Ti1 N22 C27 -70.18(17) . . . . ? N32 Ti1 N22 C27 80.05(18) . . . . ? Cl1 Ti1 N22 C27 160.07(16) . . . . ? N12 Ti1 N22 C27 -118.07(17) . . . . ? C37 Ti1 N22 C27 40.5(2) . . . . ? C29 N22 C27 N31 85.0(3) . . . . ? C28 N22 C27 N31 -153.2(3) . . . . ? Ti1 N22 C27 N31 -28.00(19) . . . . ? C29 N22 C27 C26 -157.2(3) . . . . ? C28 N22 C27 C26 -35.4(4) . . . . ? Ti1 N22 C27 C26 89.8(3) . . . . ? C29 N22 C27 Ti1 113.0(2) . . . . ? C28 N22 C27 Ti1 -125.2(3) . . . . ? N11 Ti1 C27 N31 -41.2(2) . . . . ? N21 Ti1 C27 N31 -119.5(2) . . . . ? N32 Ti1 C27 N31 24.7(2) . . . . ? Cl1 Ti1 C27 N31 117.35(17) . . . . ? N22 Ti1 C27 N31 139.6(3) . . . . ? N12 Ti1 C27 N31 -135.64(18) . . . . ? C37 Ti1 C27 N31 -9.54(19) . . . . ? N11 Ti1 C27 C26 67.7(2) . . . . ? N31 Ti1 C27 C26 108.9(3) . . . . ? N21 Ti1 C27 C26 -10.63(18) . . . . ? N32 Ti1 C27 C26 133.52(18) . . . . ? Cl1 Ti1 C27 C26 -133.80(17) . . . . ? N22 Ti1 C27 C26 -111.6(3) . . . . ? N12 Ti1 C27 C26 -26.8(2) . . . . ? C37 Ti1 C27 C26 99.31(19) . . . . ? N11 Ti1 C27 N22 179.27(16) . . . . ? N31 Ti1 C27 N22 -139.6(3) . . . . ? N21 Ti1 C27 N22 100.94(18) . . . . ? N32 Ti1 C27 N22 -114.91(17) . . . . ? Cl1 Ti1 C27 N22 -22.23(18) . . . . ? N12 Ti1 C27 N22 84.78(19) . . . . ? C37 Ti1 C27 N22 -149.12(17) . . . . ? C17 N21 C21 C26 -169.1(3) . . . . ? Ti1 N21 C21 C26 -21.7(4) . . . . ? C17 N21 C21 C22 13.1(5) . . . . ? Ti1 N21 C21 C22 160.5(2) . . . . ? N21 C21 C22 C23 176.2(3) . . . . ? C26 C21 C22 C23 -1.5(5) . . . . ? C21 C22 C23 C24 1.2(5) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C26 C25 C24 C23 -0.5(5) . . . . ? C24 C25 C26 C21 0.1(5) . . . . ? C24 C25 C26 C27 176.8(3) . . . . ? N21 C21 C26 C25 -177.1(3) . . . . ? C22 C21 C26 C25 0.8(5) . . . . ? N21 C21 C26 C27 6.2(4) . . . . ? C22 C21 C26 C27 -175.9(3) . . . . ? N31 C27 C26 C25 -124.9(3) . . . . ? N22 C27 C26 C25 125.0(3) . . . . ? Ti1 C27 C26 C25 -171.5(3) . . . . ? N31 C27 C26 C21 51.8(4) . . . . ? N22 C27 C26 C21 -58.4(4) . . . . ? Ti1 C27 C26 C21 5.2(3) . . . . ? C26 C27 N31 C31 72.3(4) . . . . ? N22 C27 N31 C31 -167.7(3) . . . . ? Ti1 C27 N31 C31 157.1(3) . . . . ? C26 C27 N31 Ti1 -84.8(3) . . . . ? N22 C27 N31 Ti1 35.2(2) . . . . ? N11 Ti1 N31 C31 -12.1(3) . . . . ? N21 Ti1 N31 C31 -99.4(3) . . . . ? N32 Ti1 N31 C31 49.0(3) . . . . ? Cl1 Ti1 N31 C31 123.8(2) . . . . ? N22 Ti1 N31 C31 -178.7(3) . . . . ? N12 Ti1 N31 C31 -78.4(3) . . . . ? C27 Ti1 N31 C31 -154.6(4) . . . . ? C37 Ti1 N31 C31 15.5(2) . . . . ? N11 Ti1 N31 C27 142.42(19) . . . . ? N21 Ti1 N31 C27 55.20(19) . . . . ? N32 Ti1 N31 C27 -156.40(19) . . . . ? Cl1 Ti1 N31 C27 -81.62(19) . . . . ? N22 Ti1 N31 C27 -24.19(17) . . . . ? N12 Ti1 N31 C27 76.1(3) . . . . ? C37 Ti1 N31 C27 170.1(2) . . . . ? N11 Ti1 N32 C39 139.9(3) . . . . ? N31 Ti1 N32 C39 47.5(2) . . . . ? N21 Ti1 N32 C39 117.9(3) . . . . ? Cl1 Ti1 N32 C39 -81.1(2) . . . . ? N22 Ti1 N32 C39 -0.6(3) . . . . ? N12 Ti1 N32 C39 -162.7(2) . . . . ? C27 Ti1 N32 C39 34.5(3) . . . . ? C37 Ti1 N32 C39 117.1(3) . . . . ? N11 Ti1 N32 C38 -85.4(2) . . . . ? N31 Ti1 N32 C38 -177.9(2) . . . . ? N21 Ti1 N32 C38 -107.5(3) . . . . ? Cl1 Ti1 N32 C38 53.5(2) . . . . ? N22 Ti1 N32 C38 134.0(2) . . . . ? N12 Ti1 N32 C38 -28.0(2) . . . . ? C27 Ti1 N32 C38 169.2(2) . . . . ? C37 Ti1 N32 C38 -108.3(3) . . . . ? N11 Ti1 N32 C37 22.87(17) . . . . ? N31 Ti1 N32 C37 -69.60(18) . . . . ? N21 Ti1 N32 C37 0.8(3) . . . . ? Cl1 Ti1 N32 C37 161.81(17) . . . . ? N22 Ti1 N32 C37 -117.66(18) . . . . ? N12 Ti1 N32 C37 80.28(19) . . . . ? C27 Ti1 N32 C37 -82.52(19) . . . . ? C11 N11 C37 C36 72.0(4) . . . . ? Ti1 N11 C37 C36 -84.6(3) . . . . ? C11 N11 C37 N32 -168.7(3) . . . . ? Ti1 N11 C37 N32 34.7(2) . . . . ? C11 N11 C37 Ti1 156.6(3) . . . . ? C39 N32 C37 N11 -153.6(3) . . . . ? C38 N32 C37 N11 84.6(3) . . . . ? Ti1 N32 C37 N11 -27.78(19) . . . . ? C39 N32 C37 C36 -35.5(4) . . . . ? C38 N32 C37 C36 -157.4(3) . . . . ? Ti1 N32 C37 C36 90.3(2) . . . . ? C39 N32 C37 Ti1 -125.8(3) . . . . ? C38 N32 C37 Ti1 112.3(2) . . . . ? N31 Ti1 C37 N11 -118.6(2) . . . . ? N21 Ti1 C37 N11 -39.6(2) . . . . ? N32 Ti1 C37 N11 139.9(3) . . . . ? Cl1 Ti1 C37 N11 119.67(17) . . . . ? N22 Ti1 C37 N11 -134.74(18) . . . . ? N12 Ti1 C37 N11 25.7(2) . . . . ? C27 Ti1 C37 N11 -113.23(19) . . . . ? N11 Ti1 C37 C36 109.5(3) . . . . ? N31 Ti1 C37 C36 -9.02(17) . . . . ? N21 Ti1 C37 C36 69.9(2) . . . . ? N32 Ti1 C37 C36 -110.6(3) . . . . ? Cl1 Ti1 C37 C36 -130.79(16) . . . . ? N22 Ti1 C37 C36 -25.2(2) . . . . ? N12 Ti1 C37 C36 135.26(18) . . . . ? C27 Ti1 C37 C36 -3.69(19) . . . . ? N11 Ti1 C37 N32 -139.9(3) . . . . ? N31 Ti1 C37 N32 101.59(19) . . . . ? N21 Ti1 C37 N32 -179.50(17) . . . . ? Cl1 Ti1 C37 N32 -20.18(19) . . . . ? N22 Ti1 C37 N32 85.4(2) . . . . ? N12 Ti1 C37 N32 -114.13(18) . . . . ? C27 Ti1 C37 N32 106.92(18) . . . . ? C27 N31 C31 C32 13.8(5) . . . . ? Ti1 N31 C31 C32 164.0(2) . . . . ? C27 N31 C31 C36 -168.9(3) . . . . ? Ti1 N31 C31 C36 -18.7(4) . . . . ? N31 C31 C36 C35 -177.7(3) . . . . ? C32 C31 C36 C35 -0.3(4) . . . . ? N31 C31 C36 C37 5.4(4) . . . . ? C32 C31 C36 C37 -177.1(3) . . . . ? N11 C37 C36 C35 -125.9(3) . . . . ? N32 C37 C36 C35 124.4(3) . . . . ? Ti1 C37 C36 C35 -172.5(2) . . . . ? N11 C37 C36 C31 50.9(4) . . . . ? N32 C37 C36 C31 -58.8(4) . . . . ? Ti1 C37 C36 C31 4.3(3) . . . . ? N31 C31 C32 C33 176.8(3) . . . . ? C36 C31 C32 C33 -0.5(5) . . . . ? C31 C36 C35 C34 1.2(5) . . . . ? C37 C36 C35 C34 177.9(3) . . . . ? C36 C35 C34 C33 -1.3(5) . . . . ? C35 C34 C33 C32 0.5(5) . . . . ? C31 C32 C33 C34 0.4(5) . . . . ? C43 O4 C41 C42 -177.5(4) . . . . ? C41 O4 C43 C44 -176.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.343 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.067 #==END