# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zrpmethox _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_sum 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_weight 749.20 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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1770(3) _cell_length_b 13.2410(4) _cell_length_c 15.1640(5) _cell_angle_alpha 64.6330(15) _cell_angle_beta 88.4740(15) _cell_angle_gamma 72.6430(15) _cell_volume 1922.11(10) _cell_formula_units_Z 2 _cell_measurement_temperature 230.0(1) _cell_measurement_reflns_used 11939 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8187 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14549 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8760 _reflns_number_gt 6170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1997), KappaCCD Collect Program' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus": a computer program for the solution and refinement of crystal structures from diffraction data University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The disordered methyl carbon C11 takes up two orientations with occupancies of 0.699 and 0.301. Hydrogens attached to C11 and C11A were placed at calculated positions. ; _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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8760 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1094 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.65525(2) 0.66850(2) -0.25369(2) 0.03101(9) Uani 1 1 d . . . Cl1 Cl 0.45638(7) 0.82662(7) -0.29963(7) 0.0553(2) Uani 1 1 d . . . Cl2 Cl 0.70198(9) 0.66731(8) -0.09804(6) 0.0551(2) Uani 1 1 d . . . Si1 Si 0.39520(7) 0.54021(7) -0.22993(6) 0.03701(19) Uani 1 1 d . . . Si2 Si 0.92456(7) 0.39964(7) -0.14365(6) 0.03658(19) Uani 1 1 d . . . Si3 Si 0.67405(7) 0.62294(7) -0.48487(6) 0.03732(19) Uani 1 1 d . . . Si4 Si 0.82492(8) 0.89042(7) -0.33650(6) 0.0389(2) Uani 1 1 d . . . O1 O 0.6522(2) -0.0144(2) 0.0566(2) 0.0651(7) Uani 1 1 d . . . O2 O 1.0253(2) 0.9047(2) -0.74455(16) 0.0505(6) Uani 1 1 d . . . N1 N 0.5532(2) 0.5380(2) -0.22115(17) 0.0349(5) Uani 1 1 d . . . N2 N 0.7655(2) 0.4795(2) -0.19025(17) 0.0324(5) Uani 1 1 d . . . N3 N 0.6990(2) 0.6783(2) -0.40236(17) 0.0352(5) Uani 1 1 d . . . N4 N 0.7710(2) 0.7780(2) -0.33779(17) 0.0356(5) Uani 1 1 d . . . C1 C 0.3117(3) 0.5925(3) -0.1430(3) 0.0491(8) Uani 1 1 d . . . H1A H 0.3211 0.6679 -0.1557 0.074 Uiso 1 1 calc R . . H1B H 0.3473 0.5356 -0.0762 0.074 Uiso 1 1 calc R . . H1C H 0.2228 0.6015 -0.1515 0.074 Uiso 1 1 calc R . . C2 C 0.3778(3) 0.3955(3) -0.2065(3) 0.0524(8) Uani 1 1 d . . . H2A H 0.4216 0.3687 -0.2524 0.079 Uiso 1 1 calc R . . H2B H 0.2890 0.4042 -0.2149 0.079 Uiso 1 1 calc R . . H2C H 0.4137 0.3383 -0.1398 0.079 Uiso 1 1 calc R . . C3 C 0.3229(3) 0.6445(3) -0.3583(2) 0.0518(8) Uani 1 1 d . . . H3A H 0.3676 0.6165 -0.4033 0.078 Uiso 1 1 calc R . . H3B H 0.3285 0.7218 -0.3734 0.078 Uiso 1 1 calc R . . H3C H 0.2350 0.6496 -0.3650 0.078 Uiso 1 1 calc R . . C4 C 0.6603(2) 0.4491(2) -0.1768(2) 0.0319(6) Uani 1 1 d . . . C5 C 0.6610(2) 0.3255(2) -0.1144(2) 0.0334(6) Uani 1 1 d . . . C6 C 0.7149(3) 0.2345(3) -0.1412(2) 0.0449(7) Uani 1 1 d . . . H6 H 0.7548 0.2498 -0.1988 0.054 Uiso 1 1 calc R . . C7 C 0.7101(3) 0.1222(3) -0.0837(3) 0.0497(8) Uani 1 1 d . . . H7 H 0.7451 0.0620 -0.1031 0.060 Uiso 1 1 calc R . . C8 C 0.6541(3) 0.0977(3) 0.0024(2) 0.0447(7) Uani 1 1 d . . . C9 C 0.6028(3) 0.1865(3) 0.0307(2) 0.0460(7) Uani 1 1 d . . . H9 H 0.5669 0.1700 0.0900 0.055 Uiso 1 1 calc R . . C10 C 0.6046(3) 0.2993(3) -0.0283(2) 0.0409(7) Uani 1 1 d . . . H10 H 0.5668 0.3597 -0.0097 0.049 Uiso 1 1 calc R . . C11 C 0.5747(6) -0.0419(5) 0.1335(4) 0.0672(18) Uani 0.699(7) 1 d P . . H11A H 0.5576 0.0168 0.1584 0.101 Uiso 0.699(7) 1 calc PR . . H11B H 0.6178 -0.1190 0.1861 0.101 Uiso 0.699(7) 1 calc PR . . H11C H 0.4959 -0.0421 0.1086 0.101 Uiso 0.699(7) 1 calc PR . . C11A C 0.6791(15) -0.0942(12) 0.0233(13) 0.089(6) Uani 0.301(7) 1 d P . . H11D H 0.6720 -0.1676 0.0737 0.134 Uiso 0.301(7) 1 calc PR . . H11E H 0.7646 -0.1069 0.0057 0.134 Uiso 0.301(7) 1 calc PR . . H11F H 0.6206 -0.0672 -0.0343 0.134 Uiso 0.301(7) 1 calc PR . . C12 C 0.9456(4) 0.2842(4) -0.0164(3) 0.0796(13) Uani 1 1 d . . . H12A H 0.9052 0.2278 -0.0140 0.119 Uiso 1 1 calc R . . H12B H 0.9078 0.3199 0.0259 0.119 Uiso 1 1 calc R . . H12C H 1.0350 0.2443 0.0057 0.119 Uiso 1 1 calc R . . C13 C 1.0018(3) 0.5063(3) -0.1482(3) 0.0705(12) Uani 1 1 d . . . H13A H 0.9910 0.5670 -0.2152 0.106 Uiso 1 1 calc R . . H13B H 1.0911 0.4661 -0.1259 0.106 Uiso 1 1 calc R . . H13C H 0.9640 0.5422 -0.1059 0.106 Uiso 1 1 calc R . . C14 C 0.9976(3) 0.3375(4) -0.2276(4) 0.0795(13) Uani 1 1 d . . . H14A H 0.9594 0.2802 -0.2265 0.119 Uiso 1 1 calc R . . H14B H 1.0874 0.2994 -0.2067 0.119 Uiso 1 1 calc R . . H14C H 0.9843 0.4003 -0.2939 0.119 Uiso 1 1 calc R . . C15 C 0.6471(3) 0.4795(3) -0.4123(2) 0.0475(8) Uani 1 1 d . . . H15A H 0.7212 0.4249 -0.3659 0.071 Uiso 1 1 calc R . . H15B H 0.6316 0.4477 -0.4562 0.071 Uiso 1 1 calc R . . H15C H 0.5746 0.4909 -0.3769 0.071 Uiso 1 1 calc R . . C16 C 0.8130(3) 0.5892(3) -0.5502(3) 0.0532(9) Uani 1 1 d . . . H16A H 0.8324 0.6611 -0.5901 0.080 Uiso 1 1 calc R . . H16B H 0.7938 0.5562 -0.5921 0.080 Uiso 1 1 calc R . . H16C H 0.8852 0.5328 -0.5025 0.080 Uiso 1 1 calc R . . C17 C 0.5356(3) 0.7303(3) -0.5751(3) 0.0560(9) Uani 1 1 d . . . H17A H 0.5522 0.8043 -0.6121 0.084 Uiso 1 1 calc R . . H17B H 0.4623 0.7433 -0.5408 0.084 Uiso 1 1 calc R . . H17C H 0.5196 0.6997 -0.6198 0.084 Uiso 1 1 calc R . . C18 C 0.7657(2) 0.7506(2) -0.4129(2) 0.0327(6) Uani 1 1 d . . . C19 C 0.8325(2) 0.7950(2) -0.5013(2) 0.0326(6) Uani 1 1 d . . . C20 C 0.9626(3) 0.7489(3) -0.4952(2) 0.0373(6) Uani 1 1 d . . . H20 H 1.0092 0.6918 -0.4346 0.045 Uiso 1 1 calc R . . C21 C 1.0239(3) 0.7862(3) -0.5775(2) 0.0398(7) Uani 1 1 d . . . H21 H 1.1119 0.7531 -0.5730 0.048 Uiso 1 1 calc R . . C22 C 0.9562(3) 0.8730(3) -0.6673(2) 0.0387(7) Uani 1 1 d . . . C23 C 0.8262(3) 0.9211(3) -0.6732(2) 0.0430(7) Uani 1 1 d . . . H23 H 0.7797 0.9807 -0.7331 0.052 Uiso 1 1 calc R . . C24 C 0.7656(3) 0.8810(2) -0.5904(2) 0.0384(7) Uani 1 1 d . . . H24 H 0.6774 0.9127 -0.5949 0.046 Uiso 1 1 calc R . . C25 C 0.9560(4) 0.9854(4) -0.8392(3) 0.0686(11) Uani 1 1 d . . . H25A H 1.0144 1.0010 -0.8880 0.103 Uiso 1 1 calc R . . H25B H 0.9070 1.0585 -0.8376 0.103 Uiso 1 1 calc R . . H25C H 0.8998 0.9512 -0.8560 0.103 Uiso 1 1 calc R . . C26 C 0.7371(4) 0.9421(4) -0.2510(3) 0.0767(13) Uani 1 1 d . . . H26A H 0.7510 0.8764 -0.1862 0.115 Uiso 1 1 calc R . . H26B H 0.6477 0.9747 -0.2743 0.115 Uiso 1 1 calc R . . H26C H 0.7664 1.0024 -0.2474 0.115 Uiso 1 1 calc R . . C27 C 0.9961(3) 0.8302(3) -0.2940(3) 0.0687(11) Uani 1 1 d . . . H27A H 1.0121 0.7623 -0.2304 0.103 Uiso 1 1 calc R . . H27B H 1.0241 0.8901 -0.2883 0.103 Uiso 1 1 calc R . . H27C H 1.0419 0.8068 -0.3409 0.103 Uiso 1 1 calc R . . C28 C 0.7948(4) 1.0195(3) -0.4580(3) 0.0702(11) Uani 1 1 d . . . H28A H 0.8401 0.9955 -0.5048 0.105 Uiso 1 1 calc R . . H28B H 0.8234 1.0792 -0.4527 0.105 Uiso 1 1 calc R . . H28C H 0.7050 1.0515 -0.4801 0.105 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 0.03137(14) 0.02993(15) 0.03103(16) -0.01199(12) 0.00530(10) -0.01112(11) Cl1 0.0391(4) 0.0429(4) 0.0717(6) -0.0211(4) 0.0015(4) -0.0020(3) Cl2 0.0736(6) 0.0564(5) 0.0386(4) -0.0245(4) 0.0042(4) -0.0196(4) Si1 0.0301(4) 0.0439(5) 0.0386(5) -0.0175(4) 0.0032(3) -0.0148(3) Si2 0.0299(4) 0.0339(4) 0.0403(5) -0.0117(4) 0.0043(3) -0.0095(3) Si3 0.0398(4) 0.0442(5) 0.0360(5) -0.0218(4) 0.0073(3) -0.0184(4) Si4 0.0451(4) 0.0368(4) 0.0407(5) -0.0178(4) 0.0057(4) -0.0199(4) O1 0.0787(17) 0.0401(13) 0.0674(18) -0.0087(13) 0.0124(14) -0.0294(13) O2 0.0503(13) 0.0550(14) 0.0425(13) -0.0147(11) 0.0176(11) -0.0227(11) N1 0.0331(12) 0.0344(12) 0.0370(14) -0.0136(11) 0.0045(10) -0.0136(10) N2 0.0312(11) 0.0323(12) 0.0324(13) -0.0115(10) 0.0052(10) -0.0126(10) N3 0.0430(13) 0.0364(13) 0.0321(13) -0.0166(11) 0.0098(10) -0.0191(11) N4 0.0408(13) 0.0369(13) 0.0333(13) -0.0164(11) 0.0075(10) -0.0168(11) C1 0.0388(16) 0.063(2) 0.050(2) -0.0284(18) 0.0106(14) -0.0186(15) C2 0.0474(18) 0.057(2) 0.059(2) -0.0239(18) 0.0021(16) -0.0272(16) C3 0.0409(17) 0.066(2) 0.0456(19) -0.0225(17) -0.0020(14) -0.0148(16) C4 0.0335(14) 0.0348(14) 0.0294(14) -0.0154(12) 0.0054(11) -0.0118(12) C5 0.0312(13) 0.0328(14) 0.0361(16) -0.0138(13) 0.0023(11) -0.0121(11) C6 0.0485(17) 0.0419(17) 0.050(2) -0.0233(16) 0.0190(15) -0.0189(14) C7 0.0531(19) 0.0386(17) 0.063(2) -0.0263(17) 0.0181(17) -0.0170(15) C8 0.0426(16) 0.0334(16) 0.052(2) -0.0098(15) 0.0003(14) -0.0163(13) C9 0.0535(18) 0.0472(18) 0.0351(17) -0.0125(15) 0.0078(14) -0.0215(15) C10 0.0469(16) 0.0415(16) 0.0384(17) -0.0193(14) 0.0077(13) -0.0175(14) C11 0.088(4) 0.062(3) 0.055(4) -0.010(3) 0.014(3) -0.053(3) C11A 0.080(10) 0.045(8) 0.122(15) -0.016(8) 0.015(9) -0.024(7) C12 0.050(2) 0.087(3) 0.055(2) 0.008(2) -0.0058(18) -0.017(2) C13 0.0402(18) 0.057(2) 0.109(4) -0.030(2) -0.004(2) -0.0179(17) C14 0.046(2) 0.113(4) 0.106(4) -0.078(3) 0.023(2) -0.017(2) C15 0.0598(19) 0.0517(19) 0.0465(19) -0.0292(17) 0.0132(15) -0.0279(16) C16 0.0535(19) 0.068(2) 0.060(2) -0.042(2) 0.0203(17) -0.0288(17) C17 0.054(2) 0.061(2) 0.051(2) -0.0211(18) -0.0027(16) -0.0214(17) C18 0.0292(13) 0.0302(14) 0.0333(15) -0.0102(12) 0.0015(11) -0.0076(11) C19 0.0353(14) 0.0331(14) 0.0316(15) -0.0137(12) 0.0048(11) -0.0146(12) C20 0.0358(14) 0.0376(15) 0.0354(16) -0.0116(13) 0.0031(12) -0.0144(12) C21 0.0339(14) 0.0405(16) 0.0441(18) -0.0174(15) 0.0080(13) -0.0128(13) C22 0.0436(16) 0.0384(16) 0.0380(17) -0.0160(14) 0.0137(13) -0.0204(13) C23 0.0435(16) 0.0386(16) 0.0367(17) -0.0083(14) 0.0037(13) -0.0119(13) C24 0.0321(14) 0.0354(15) 0.0401(17) -0.0121(13) 0.0050(12) -0.0073(12) C25 0.074(3) 0.071(3) 0.044(2) -0.011(2) 0.0229(19) -0.024(2) C26 0.099(3) 0.076(3) 0.097(3) -0.061(3) 0.046(3) -0.053(3) C27 0.056(2) 0.059(2) 0.101(3) -0.042(2) -0.011(2) -0.0198(18) C28 0.110(3) 0.0421(19) 0.057(2) -0.0123(18) -0.006(2) -0.034(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N4 2.202(2) . ? Zr1 N2 2.206(2) . ? Zr1 N1 2.224(2) . ? Zr1 N3 2.251(2) . ? Zr1 Cl1 2.4219(8) . ? Zr1 Cl2 2.4234(8) . ? Si1 N1 1.765(2) . ? Si1 C1 1.849(3) . ? Si1 C3 1.861(3) . ? Si1 C2 1.863(3) . ? Si2 N2 1.756(2) . ? Si2 C13 1.841(3) . ? Si2 C12 1.843(4) . ? Si2 C14 1.845(3) . ? Si3 N3 1.763(2) . ? Si3 C17 1.850(3) . ? Si3 C15 1.855(3) . ? Si3 C16 1.865(3) . ? Si4 N4 1.772(2) . ? Si4 C26 1.846(4) . ? Si4 C28 1.849(4) . ? Si4 C27 1.852(3) . ? O1 C11A 1.312(16) . ? O1 C8 1.361(4) . ? O1 C11 1.419(6) . ? O2 C22 1.367(3) . ? O2 C25 1.432(4) . ? N1 C4 1.340(3) . ? N2 C4 1.336(3) . ? N3 C18 1.336(3) . ? N4 C18 1.342(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.496(4) . ? C5 C10 1.387(4) . ? C5 C6 1.397(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9400 . ? C7 C8 1.383(5) . ? C7 H7 0.9400 . ? C8 C9 1.383(4) . ? C9 C10 1.380(4) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C11A H11D 0.9700 . ? C11A H11E 0.9700 . ? C11A H11F 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.495(4) . ? C19 C24 1.382(4) . ? C19 C20 1.387(4) . ? C20 C21 1.378(4) . ? C20 H20 0.9400 . ? C21 C22 1.394(4) . ? C21 H21 0.9400 . ? C22 C23 1.390(4) . ? C23 C24 1.384(4) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zr1 N2 110.97(8) . . ? N4 Zr1 N1 155.73(8) . . ? N2 Zr1 N1 61.30(8) . . ? N4 Zr1 N3 61.14(8) . . ? N2 Zr1 N3 87.70(8) . . ? N1 Zr1 N3 94.82(8) . . ? N4 Zr1 Cl1 96.78(6) . . ? N2 Zr1 Cl1 151.36(6) . . ? N1 Zr1 Cl1 90.46(6) . . ? N3 Zr1 Cl1 100.16(6) . . ? N4 Zr1 Cl2 96.44(6) . . ? N2 Zr1 Cl2 88.80(6) . . ? N1 Zr1 Cl2 105.98(7) . . ? N3 Zr1 Cl2 154.01(6) . . ? Cl1 Zr1 Cl2 95.17(3) . . ? N1 Si1 C1 108.56(13) . . ? N1 Si1 C3 107.41(13) . . ? C1 Si1 C3 110.12(16) . . ? N1 Si1 C2 114.15(13) . . ? C1 Si1 C2 109.94(16) . . ? C3 Si1 C2 106.59(16) . . ? N2 Si2 C13 106.92(14) . . ? N2 Si2 C12 113.15(15) . . ? C13 Si2 C12 109.4(2) . . ? N2 Si2 C14 108.17(16) . . ? C13 Si2 C14 107.4(2) . . ? C12 Si2 C14 111.6(2) . . ? N3 Si3 C17 108.82(14) . . ? N3 Si3 C15 107.77(13) . . ? C17 Si3 C15 111.21(16) . . ? N3 Si3 C16 114.01(13) . . ? C17 Si3 C16 109.91(17) . . ? C15 Si3 C16 105.09(15) . . ? N4 Si4 C26 107.67(15) . . ? N4 Si4 C28 112.85(15) . . ? C26 Si4 C28 107.2(2) . . ? N4 Si4 C27 109.64(14) . . ? C26 Si4 C27 110.0(2) . . ? C28 Si4 C27 109.4(2) . . ? C11A O1 C8 123.2(8) . . ? C11A O1 C11 110.6(7) . . ? C8 O1 C11 121.6(3) . . ? C22 O2 C25 116.8(2) . . ? C4 N1 Si1 131.5(2) . . ? Si1 N1 Zr1 137.26(12) . . ? C4 N2 Si2 132.6(2) . . ? Si2 N2 Zr1 133.70(12) . . ? C18 N3 Si3 127.7(2) . . ? Si3 N3 Zr1 141.60(13) . . ? C18 N4 Si4 127.2(2) . . ? Si4 N4 Zr1 138.61(12) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N1 115.1(2) . . ? N2 C4 C5 122.7(2) . . ? N1 C4 C5 122.1(2) . . ? C10 C5 C6 118.2(3) . . ? C10 C5 C4 119.9(2) . . ? C6 C5 C4 122.0(3) . . ? C7 C6 C5 120.5(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? O1 C8 C7 118.1(3) . . ? O1 C8 C9 122.3(3) . . ? C7 C8 C9 119.6(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C5 121.4(3) . . ? C9 C10 H10 119.3 . . ? C5 C10 H10 119.3 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C11A H11D 109.5 . . ? O1 C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? O1 C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 N4 115.5(2) . . ? N3 C18 C19 121.9(2) . . ? N4 C18 C19 122.5(2) . . ? N3 C18 Zr1 58.79(14) . . ? N4 C18 Zr1 56.72(14) . . ? C19 C18 Zr1 178.15(19) . . ? C24 C19 C20 119.1(3) . . ? C24 C19 C18 120.6(2) . . ? C20 C19 C18 120.3(2) . . ? C21 C20 C19 120.4(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? O2 C22 C23 124.6(3) . . ? O2 C22 C21 116.1(3) . . ? C23 C22 C21 119.4(3) . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C19 C24 C23 121.1(3) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? O2 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C1 Si1 N1 C4 102.8(3) . . . . ? C3 Si1 N1 C4 -138.2(3) . . . . ? C2 Si1 N1 C4 -20.2(3) . . . . ? C1 Si1 N1 Zr1 -65.9(2) . . . . ? C3 Si1 N1 Zr1 53.1(2) . . . . ? C2 Si1 N1 Zr1 171.08(18) . . . . ? N4 Zr1 N1 Si1 -104.2(2) . . . . ? N2 Zr1 N1 Si1 178.6(2) . . . . ? N3 Zr1 N1 Si1 -96.64(19) . . . . ? Cl1 Zr1 N1 Si1 3.59(18) . . . . ? Cl2 Zr1 N1 Si1 99.11(18) . . . . ? C13 Si2 N2 C4 -155.2(3) . . . . ? C12 Si2 N2 C4 -34.7(3) . . . . ? C14 Si2 N2 C4 89.4(3) . . . . ? C13 Si2 N2 Zr1 3.2(2) . . . . ? C12 Si2 N2 Zr1 123.7(2) . . . . ? C14 Si2 N2 Zr1 -112.2(2) . . . . ? N4 Zr1 N2 Si2 34.04(19) . . . . ? N1 Zr1 N2 Si2 -171.4(2) . . . . ? N3 Zr1 N2 Si2 91.85(17) . . . . ? Cl1 Zr1 N2 Si2 -161.01(9) . . . . ? Cl2 Zr1 N2 Si2 -62.40(16) . . . . ? C17 Si3 N3 C18 -86.7(3) . . . . ? C15 Si3 N3 C18 152.6(2) . . . . ? C16 Si3 N3 C18 36.4(3) . . . . ? C17 Si3 N3 Zr1 95.5(2) . . . . ? C15 Si3 N3 Zr1 -25.2(3) . . . . ? C16 Si3 N3 Zr1 -141.4(2) . . . . ? N4 Zr1 N3 Si3 178.6(2) . . . . ? N2 Zr1 N3 Si3 63.0(2) . . . . ? N1 Zr1 N3 Si3 2.1(2) . . . . ? Cl1 Zr1 N3 Si3 -89.2(2) . . . . ? Cl2 Zr1 N3 Si3 145.54(14) . . . . ? C26 Si4 N4 C18 149.8(3) . . . . ? C28 Si4 N4 C18 31.7(3) . . . . ? C27 Si4 N4 C18 -90.5(3) . . . . ? C26 Si4 N4 Zr1 -11.7(3) . . . . ? C28 Si4 N4 Zr1 -129.8(2) . . . . ? C27 Si4 N4 Zr1 108.0(2) . . . . ? N2 Zr1 N4 Si4 -120.03(19) . . . . ? N1 Zr1 N4 Si4 173.63(16) . . . . ? N3 Zr1 N4 Si4 165.1(2) . . . . ? Cl1 Zr1 N4 Si4 67.2(2) . . . . ? Cl2 Zr1 N4 Si4 -28.8(2) . . . . ? Si2 N2 C4 N1 176.0(2) . . . . ? Si2 N2 C4 C5 -2.2(4) . . . . ? Si1 N1 C4 N2 176.27(19) . . . . ? Si1 N1 C4 C5 -5.5(4) . . . . ? N2 C4 C5 C10 113.8(3) . . . . ? N1 C4 C5 C10 -64.3(4) . . . . ? N2 C4 C5 C6 -67.6(4) . . . . ? N1 C4 C5 C6 114.3(3) . . . . ? C10 C5 C6 C7 0.9(5) . . . . ? C4 C5 C6 C7 -177.7(3) . . . . ? C5 C6 C7 C8 -1.4(5) . . . . ? C11A O1 C8 C7 -13.0(9) . . . . ? C11 O1 C8 C7 -166.5(4) . . . . ? C11A O1 C8 C9 167.3(9) . . . . ? C11 O1 C8 C9 13.8(5) . . . . ? C6 C7 C8 O1 -179.8(3) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? O1 C8 C9 C10 -178.4(3) . . . . ? C7 C8 C9 C10 1.9(5) . . . . ? C8 C9 C10 C5 -2.3(5) . . . . ? C6 C5 C10 C9 1.0(4) . . . . ? C4 C5 C10 C9 179.6(3) . . . . ? Si3 N3 C18 N4 -179.10(19) . . . . ? Si3 N3 C18 C19 -0.7(4) . . . . ? Si3 N3 C18 Zr1 -178.7(3) . . . . ? Si4 N4 C18 N3 -167.4(2) . . . . ? Si4 N4 C18 C19 14.1(4) . . . . ? N3 C18 C19 C24 74.3(4) . . . . ? N4 C18 C19 C24 -107.4(3) . . . . ? N3 C18 C19 C20 -104.7(3) . . . . ? N4 C18 C19 C20 73.6(4) . . . . ? C24 C19 C20 C21 -1.5(4) . . . . ? C18 C19 C20 C21 177.4(3) . . . . ? C19 C20 C21 C22 1.5(4) . . . . ? C25 O2 C22 C23 -5.9(4) . . . . ? C25 O2 C22 C21 174.3(3) . . . . ? C20 C21 C22 O2 179.7(3) . . . . ? C20 C21 C22 C23 -0.2(4) . . . . ? O2 C22 C23 C24 179.0(3) . . . . ? C21 C22 C23 C24 -1.2(4) . . . . ? C20 C19 C24 C23 0.2(4) . . . . ? C18 C19 C24 C23 -178.8(3) . . . . ? C22 C23 C24 C19 1.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.538 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 946660' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zrpetdim _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H54 Cl2 N4 Si4 Zr' _chemical_formula_sum 'C30 H54 Cl2 N4 Si4 Zr' _chemical_formula_weight 745.25 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.3540(11) _cell_length_b 8.8490(5) _cell_length_c 20.4080(10) _cell_angle_alpha 90.00 _cell_angle_beta 128.046(3) _cell_angle_gamma 90.00 _cell_volume 4032.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 230.0(1) _cell_measurement_reflns_used 6965 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8797 _exptl_absorpt_correction_T_max 0.9372 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6258 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3544 _reflns_number_gt 2506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1997), KappaCCD Collect Program' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus": a computer program for the solution and refinement of crystal structures from diffraction data University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00147(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3544 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 0.0000 0.45992(4) 0.2500 0.04044(16) Uani 1 2 d S . . Si1 Si -0.03798(4) 0.16117(11) 0.33668(6) 0.0526(3) Uani 1 1 d . . . Si2 Si 0.15866(4) 0.51848(11) 0.43000(6) 0.0523(3) Uani 1 1 d . . . Cl1 Cl -0.04049(4) 0.63963(10) 0.29212(6) 0.0740(3) Uani 1 1 d . . . N1 N 0.00963(10) 0.2840(3) 0.33380(14) 0.0431(6) Uani 1 1 d . . . N2 N 0.09021(10) 0.4201(3) 0.37114(14) 0.0411(6) Uani 1 1 d . . . C1 C 0.00041(17) -0.0048(4) 0.4041(2) 0.0665(10) Uani 1 1 d . . . H1A H 0.0197 -0.0608 0.3857 0.100 Uiso 1 1 calc R . . H1B H -0.0286 -0.0692 0.4010 0.100 Uiso 1 1 calc R . . H1C H 0.0303 0.0282 0.4611 0.100 Uiso 1 1 calc R . . C2 C -0.09342(17) 0.0953(5) 0.2276(2) 0.0921(15) Uani 1 1 d . . . H2A H -0.0730 0.0388 0.2110 0.138 Uiso 1 1 calc R . . H2B H -0.1134 0.1819 0.1912 0.138 Uiso 1 1 calc R . . H2C H -0.1228 0.0309 0.2236 0.138 Uiso 1 1 calc R . . C3 C -0.07419(18) 0.2658(5) 0.3727(3) 0.0945(14) Uani 1 1 d . . . H3A H -0.0948 0.3532 0.3374 0.142 Uiso 1 1 calc R . . H3B H -0.0440 0.2988 0.4296 0.142 Uiso 1 1 calc R . . H3C H -0.1028 0.2007 0.3702 0.142 Uiso 1 1 calc R . . C4 C 0.06579(13) 0.3246(3) 0.39353(18) 0.0395(7) Uani 1 1 d . . . C5 C 0.09925(12) 0.2722(3) 0.48143(17) 0.0417(7) Uani 1 1 d . . . C6 C 0.13529(15) 0.1452(4) 0.51023(19) 0.0522(8) Uani 1 1 d . . . H6 H 0.1392 0.0906 0.4743 0.063 Uiso 1 1 calc R . . C7 C 0.16569(14) 0.0981(4) 0.59194(19) 0.0556(8) Uani 1 1 d . . . H7 H 0.1899 0.0114 0.6108 0.067 Uiso 1 1 calc R . . C8 C 0.16083(14) 0.1772(4) 0.64594(19) 0.0510(8) Uani 1 1 d . . . C9 C 0.12406(15) 0.3024(4) 0.6161(2) 0.0569(9) Uani 1 1 d . . . H9 H 0.1198 0.3565 0.6519 0.068 Uiso 1 1 calc R . . C10 C 0.09336(14) 0.3497(3) 0.53481(18) 0.0499(8) Uani 1 1 d . . . H10 H 0.0683 0.4349 0.5157 0.060 Uiso 1 1 calc R . . C11 C 0.19789(16) 0.1312(4) 0.73733(19) 0.0674(10) Uani 1 1 d . . . H11A H 0.1796 0.1738 0.7613 0.081 Uiso 1 1 calc R . . H11B H 0.1974 0.0209 0.7411 0.081 Uiso 1 1 calc R . . C12 C 0.26130(19) 0.1844(5) 0.7866(2) 0.1094(17) Uani 1 1 d . . . H12A H 0.2832 0.1533 0.8442 0.164 Uiso 1 1 calc R . . H12B H 0.2620 0.2937 0.7838 0.164 Uiso 1 1 calc R . . H12C H 0.2798 0.1406 0.7639 0.164 Uiso 1 1 calc R . . C13 C 0.18860(16) 0.5168(5) 0.3705(2) 0.0839(13) Uani 1 1 d . . . H13A H 0.1961 0.4134 0.3635 0.126 Uiso 1 1 calc R . . H13B H 0.2257 0.5738 0.4006 0.126 Uiso 1 1 calc R . . H13C H 0.1596 0.5624 0.3163 0.126 Uiso 1 1 calc R . . C14 C 0.14339(17) 0.7142(4) 0.4442(2) 0.0871(13) Uani 1 1 d . . . H14A H 0.1280 0.7127 0.4755 0.131 Uiso 1 1 calc R . . H14B H 0.1140 0.7600 0.3902 0.131 Uiso 1 1 calc R . . H14C H 0.1802 0.7725 0.4743 0.131 Uiso 1 1 calc R . . C15 C 0.21833(14) 0.4356(4) 0.5338(2) 0.0721(11) Uani 1 1 d . . . H15A H 0.2266 0.3330 0.5268 0.108 Uiso 1 1 calc R . . H15B H 0.2050 0.4347 0.5676 0.108 Uiso 1 1 calc R . . H15C H 0.2544 0.4959 0.5611 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0354(3) 0.0396(3) 0.0416(3) 0.000 0.0214(2) 0.000 Si1 0.0485(6) 0.0548(6) 0.0565(6) 0.0013(4) 0.0333(5) -0.0097(4) Si2 0.0353(5) 0.0568(6) 0.0533(5) -0.0004(4) 0.0216(5) -0.0060(4) Cl1 0.0656(6) 0.0675(6) 0.0810(7) -0.0201(5) 0.0412(6) 0.0093(5) N1 0.0357(15) 0.0462(14) 0.0446(14) -0.0012(12) 0.0234(13) -0.0046(11) N2 0.0381(14) 0.0438(14) 0.0399(13) -0.0027(11) 0.0232(12) -0.0037(11) C1 0.073(3) 0.057(2) 0.071(2) 0.0000(18) 0.045(2) -0.0135(18) C2 0.078(3) 0.110(3) 0.065(2) 0.000(2) 0.033(2) -0.051(3) C3 0.088(3) 0.084(3) 0.152(4) 0.008(3) 0.095(3) 0.000(2) C4 0.0435(18) 0.0347(15) 0.0454(17) -0.0018(13) 0.0300(16) 0.0048(13) C5 0.0378(17) 0.0478(17) 0.0398(16) -0.0005(14) 0.0241(15) -0.0015(14) C6 0.060(2) 0.055(2) 0.0448(18) 0.0014(15) 0.0343(17) 0.0082(16) C7 0.055(2) 0.057(2) 0.0512(19) 0.0092(17) 0.0308(18) 0.0113(16) C8 0.049(2) 0.061(2) 0.0438(18) 0.0027(16) 0.0291(17) -0.0069(16) C9 0.064(2) 0.065(2) 0.053(2) -0.0077(18) 0.0419(19) -0.0028(18) C10 0.053(2) 0.0503(19) 0.0521(19) -0.0009(16) 0.0356(18) 0.0073(15) C11 0.073(3) 0.075(3) 0.048(2) 0.0083(18) 0.034(2) -0.008(2) C12 0.085(3) 0.142(4) 0.049(2) 0.014(3) 0.015(2) -0.041(3) C13 0.047(2) 0.127(4) 0.074(3) 0.004(2) 0.036(2) -0.018(2) C14 0.072(3) 0.053(2) 0.097(3) -0.014(2) 0.031(3) -0.014(2) C15 0.041(2) 0.091(3) 0.063(2) 0.002(2) 0.0215(19) -0.0080(19) _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 2.202(2) 2 ? Zr1 N1 2.202(2) . ? Zr1 N2 2.233(2) . ? Zr1 N2 2.233(2) 2 ? Zr1 Cl1 2.4089(9) . ? Zr1 Cl1 2.4089(9) 2 ? Si1 N1 1.762(2) . ? Si1 C1 1.840(3) . ? Si1 C3 1.839(4) . ? Si1 C2 1.859(3) . ? Si2 N2 1.759(2) . ? Si2 C14 1.851(4) . ? Si2 C13 1.863(4) . ? Si2 C15 1.863(3) . ? N1 C4 1.326(4) . ? N2 C4 1.339(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.495(4) . ? C5 C10 1.381(4) . ? C5 C6 1.383(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9400 . ? C7 C8 1.382(4) . ? C7 H7 0.9400 . ? C8 C9 1.380(4) . ? C8 C11 1.527(4) . ? C9 C10 1.381(4) . ? C9 H9 0.9400 . ? C10 H10 0.9400 . ? C11 C12 1.495(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 N1 89.99(12) 2 . ? N1 Zr1 N2 104.92(8) 2 . ? N1 Zr1 N2 61.27(8) . . ? N1 Zr1 N2 61.27(8) 2 2 ? N1 Zr1 N2 104.92(8) . 2 ? N2 Zr1 N2 161.84(12) . 2 ? N1 Zr1 Cl1 152.35(7) 2 . ? N1 Zr1 Cl1 92.74(6) . . ? N2 Zr1 Cl1 100.47(6) . . ? N2 Zr1 Cl1 91.52(6) 2 . ? N1 Zr1 Cl1 92.74(7) 2 2 ? N1 Zr1 Cl1 152.35(7) . 2 ? N2 Zr1 Cl1 91.52(6) . 2 ? N2 Zr1 Cl1 100.48(6) 2 2 ? Cl1 Zr1 Cl1 97.38(5) . 2 ? N1 Si1 C1 113.86(14) . . ? N1 Si1 C3 109.31(15) . . ? C1 Si1 C3 108.77(18) . . ? N1 Si1 C2 104.66(14) . . ? C1 Si1 C2 108.61(18) . . ? C3 Si1 C2 111.6(2) . . ? N2 Si2 C14 107.70(15) . . ? N2 Si2 C13 107.77(15) . . ? C14 Si2 C13 110.7(2) . . ? N2 Si2 C15 115.35(15) . . ? C14 Si2 C15 109.06(17) . . ? C13 Si2 C15 106.21(17) . . ? C4 N1 Si1 130.3(2) . . ? C4 N1 Zr1 91.49(17) . . ? Si1 N1 Zr1 136.99(13) . . ? C4 N2 Si2 131.6(2) . . ? C4 N2 Zr1 89.83(17) . . ? Si2 N2 Zr1 134.99(13) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 116.0(2) . . ? N1 C4 C5 122.2(2) . . ? N2 C4 C5 121.7(3) . . ? N1 C4 Zr1 57.85(15) . . ? N2 C4 Zr1 59.18(14) . . ? C5 C4 Zr1 168.17(19) . . ? C10 C5 C6 119.0(3) . . ? C10 C5 C4 119.8(3) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C7 118.3(3) . . ? C9 C8 C11 121.1(3) . . ? C7 C8 C11 120.5(3) . . ? C10 C9 C8 121.3(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C5 120.3(3) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? C12 C11 C8 112.0(3) . . ? C12 C11 H11A 109.2 . . ? C8 C11 H11A 109.2 . . ? C12 C11 H11B 109.2 . . ? C8 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 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 C1 Si1 N1 C4 -37.3(3) . . . . ? C3 Si1 N1 C4 84.6(3) . . . . ? C2 Si1 N1 C4 -155.7(3) . . . . ? C1 Si1 N1 Zr1 158.88(18) . . . . ? C3 Si1 N1 Zr1 -79.3(2) . . . . ? C2 Si1 N1 Zr1 40.4(2) . . . . ? N1 Zr1 N1 Si1 -78.08(18) 2 . . . ? N2 Zr1 N1 Si1 174.8(2) . . . . ? N2 Zr1 N1 Si1 -17.9(2) 2 . . . ? Cl1 Zr1 N1 Si1 74.39(18) . . . . ? Cl1 Zr1 N1 Si1 -173.99(9) 2 . . . ? C4 Zr1 N1 Si1 -49.7(2) 2 . . . ? C4 Zr1 N1 Si1 167.7(3) . . . . ? C14 Si2 N2 C4 -99.3(3) . . . . ? C13 Si2 N2 C4 141.2(3) . . . . ? C15 Si2 N2 C4 22.7(3) . . . . ? C14 Si2 N2 Zr1 52.7(2) . . . . ? C13 Si2 N2 Zr1 -66.8(2) . . . . ? C15 Si2 N2 Zr1 174.75(17) . . . . ? N1 Zr1 N2 C4 -88.62(15) 2 . . . ? N1 Zr1 N2 C4 -7.03(15) . . . . ? Cl1 Zr1 N2 C4 80.34(15) . . . . ? Cl1 Zr1 N2 C4 178.13(15) 2 . . . ? C4 Zr1 N2 C4 -84.5(2) 2 . . . ? N1 Zr1 N2 Si2 111.90(17) 2 . . . ? N1 Zr1 N2 Si2 -166.5(2) . . . . ? N2 Zr1 N2 Si2 150.31(17) 2 . . . ? Cl1 Zr1 N2 Si2 -79.14(17) . . . . ? Cl1 Zr1 N2 Si2 18.65(17) 2 . . . ? C4 Zr1 N2 Si2 116.00(18) 2 . . . ? C4 Zr1 N2 Si2 -159.5(3) . . . . ? Si1 N1 C4 N2 179.35(19) . . . . ? Zr1 N1 C4 N2 -11.6(2) . . . . ? Si1 N1 C4 C5 -3.0(4) . . . . ? Zr1 N1 C4 C5 166.0(2) . . . . ? Si1 N1 C4 Zr1 -169.0(3) . . . . ? Si2 N2 C4 N1 172.1(2) . . . . ? Zr1 N2 C4 N1 11.4(2) . . . . ? Si2 N2 C4 C5 -5.6(4) . . . . ? Zr1 N2 C4 C5 -166.2(2) . . . . ? Si2 N2 C4 Zr1 160.6(3) . . . . ? N1 Zr1 C4 N1 -68.9(2) 2 . . . ? N2 Zr1 C4 N1 -167.8(3) . . . . ? N2 Zr1 C4 N1 -7.8(2) 2 . . . ? Cl1 Zr1 C4 N1 88.52(16) . . . . ? Cl1 Zr1 C4 N1 -170.06(14) 2 . . . ? C4 Zr1 C4 N1 -46.61(15) 2 . . . ? N1 Zr1 C4 N2 98.97(15) 2 . . . ? N1 Zr1 C4 N2 167.8(3) . . . . ? N2 Zr1 C4 N2 160.07(14) 2 . . . ? Cl1 Zr1 C4 N2 -103.63(15) . . . . ? Cl1 Zr1 C4 N2 -2.21(17) 2 . . . ? C4 Zr1 C4 N2 121.24(16) 2 . . . ? N1 Zr1 C4 C5 -163.1(10) 2 . . . ? N1 Zr1 C4 C5 -94.2(10) . . . . ? N2 Zr1 C4 C5 98.0(10) . . . . ? N2 Zr1 C4 C5 -102.0(10) 2 . . . ? Cl1 Zr1 C4 C5 -5.7(10) . . . . ? Cl1 Zr1 C4 C5 95.7(10) 2 . . . ? C4 Zr1 C4 C5 -140.8(10) 2 . . . ? N1 C4 C5 C10 -84.8(4) . . . . ? N2 C4 C5 C10 92.6(3) . . . . ? Zr1 C4 C5 C10 1.9(12) . . . . ? N1 C4 C5 C6 93.8(4) . . . . ? N2 C4 C5 C6 -88.7(4) . . . . ? C10 C5 C6 C7 -1.0(5) . . . . ? C4 C5 C6 C7 -179.6(3) . . . . ? C5 C6 C7 C8 -0.3(5) . . . . ? C6 C7 C8 C9 1.3(5) . . . . ? C6 C7 C8 C11 -175.6(3) . . . . ? C7 C8 C9 C10 -0.9(5) . . . . ? C11 C8 C9 C10 175.9(3) . . . . ? C8 C9 C10 C5 -0.4(5) . . . . ? C6 C5 C10 C9 1.3(5) . . . . ? C4 C5 C10 C9 -180.0(3) . . . . ? C9 C8 C11 C12 -98.6(4) . . . . ? C7 C8 C11 C12 78.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.330 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 946661' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zrnbudim _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C34 H62 Cl2 N4 Si4 Zr)' _chemical_formula_sum 'C102 H186 Cl6 N12 Si12 Zr3' _chemical_formula_weight 2404.08 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' Cl Cl 0.1484 0.1585 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 18.8580(2) _cell_length_b 22.1300(3) _cell_length_c 32.6300(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.5150(11) _cell_angle_gamma 90.00 _cell_volume 13467.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 230.0(1) _cell_measurement_reflns_used 60215 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5088 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8776 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18861 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.28 _reflns_number_total 18861 _reflns_number_gt 9971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1997), KappaCCD Collect Program' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus": a computer program for the solution and refinement of crystal structures from diffraction data University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18861 _refine_ls_number_parameters 1204 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1640 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1A Zr -0.06400(3) 0.31975(3) 0.482213(16) 0.05869(19) Uani 1 1 d . . . Cl1A Cl -0.07728(9) 0.38630(8) 0.53951(5) 0.0826(5) Uani 1 1 d . . . Cl2A Cl -0.15995(9) 0.36298(9) 0.43392(5) 0.0894(6) Uani 1 1 d . . . Si1A Si 0.09885(10) 0.29947(9) 0.55633(5) 0.0738(6) Uani 1 1 d . . . Si2A Si 0.01249(10) 0.39926(10) 0.39820(5) 0.0767(6) Uani 1 1 d . . . Si3A Si -0.20255(11) 0.24901(9) 0.53529(5) 0.0743(6) Uani 1 1 d . . . Si4A Si -0.01664(10) 0.18282(9) 0.42390(6) 0.0761(6) Uani 1 1 d . . . N1A N 0.0512(2) 0.3153(2) 0.50719(13) 0.0630(14) Uani 1 1 d . . . N2A N 0.0137(2) 0.3592(2) 0.44506(13) 0.0599(13) Uani 1 1 d . . . N3A N -0.1321(3) 0.2498(2) 0.50593(13) 0.0630(13) Uani 1 1 d . . . N4A N -0.0601(3) 0.2258(2) 0.45832(14) 0.0628(13) Uani 1 1 d . . . C1A C 0.0363(4) 0.2528(3) 0.58226(19) 0.106(3) Uani 1 1 d . . . H1A1 H -0.0062 0.2762 0.5851 0.159 Uiso 1 1 calc R . . H1A2 H 0.0598 0.2407 0.6095 0.159 Uiso 1 1 calc R . . H1A3 H 0.0226 0.2170 0.5657 0.159 Uiso 1 1 calc R . . C2A C 0.1226(4) 0.3692(3) 0.58656(18) 0.094(2) Uani 1 1 d . . . H2A1 H 0.0795 0.3924 0.5883 0.141 Uiso 1 1 calc R . . H2A2 H 0.1554 0.3932 0.5730 0.141 Uiso 1 1 calc R . . H2A3 H 0.1453 0.3585 0.6142 0.141 Uiso 1 1 calc R . . C3A C 0.1804(4) 0.2539(4) 0.5518(2) 0.115(3) Uani 1 1 d . . . H3A1 H 0.1667 0.2176 0.5359 0.173 Uiso 1 1 calc R . . H3A2 H 0.2039 0.2429 0.5793 0.173 Uiso 1 1 calc R . . H3A3 H 0.2130 0.2776 0.5379 0.173 Uiso 1 1 calc R . . C4A C 0.0660(3) 0.3528(3) 0.47726(17) 0.0605(17) Uani 1 1 d . . . C5A C 0.1345(3) 0.3880(3) 0.48147(17) 0.0608(16) Uani 1 1 d . . . C6A C 0.1982(4) 0.3611(3) 0.47542(19) 0.083(2) Uani 1 1 d . . . H6A H 0.1993 0.3193 0.4703 0.099 Uiso 1 1 calc R . . C7A C 0.2607(4) 0.3947(4) 0.4768(2) 0.094(2) Uani 1 1 d . . . H7A H 0.3037 0.3753 0.4732 0.112 Uiso 1 1 calc R . . C8A C 0.2603(4) 0.4561(5) 0.4834(2) 0.095(3) Uani 1 1 d D . . C9A C 0.1974(4) 0.4830(3) 0.4915(2) 0.088(2) Uani 1 1 d . . . H9A H 0.1971 0.5242 0.4984 0.105 Uiso 1 1 calc R . . C10A C 0.1342(4) 0.4490(3) 0.48954(18) 0.0738(19) Uani 1 1 d . . . H10A H 0.0914 0.4680 0.4938 0.089 Uiso 1 1 calc R . . C15A C -0.0259(4) 0.4740(3) 0.4033(2) 0.104(3) Uani 1 1 d . . . H15A H 0.0040 0.4964 0.4248 0.157 Uiso 1 1 calc R . . H15B H -0.0737 0.4699 0.4105 0.157 Uiso 1 1 calc R . . H15C H -0.0284 0.4954 0.3772 0.157 Uiso 1 1 calc R . . C16A C -0.0429(4) 0.3546(3) 0.35680(17) 0.098(2) Uani 1 1 d . . . H16A H -0.0215 0.3151 0.3547 0.147 Uiso 1 1 calc R . . H16B H -0.0452 0.3755 0.3305 0.147 Uiso 1 1 calc R . . H16C H -0.0910 0.3499 0.3636 0.147 Uiso 1 1 calc R . . C17A C 0.1039(4) 0.4042(4) 0.38219(19) 0.116(3) Uani 1 1 d . . . H17A H 0.1229 0.3638 0.3799 0.174 Uiso 1 1 calc R . . H17B H 0.1356 0.4268 0.4028 0.174 Uiso 1 1 calc R . . H17C H 0.1005 0.4244 0.3556 0.174 Uiso 1 1 calc R . . C18A C -0.2635(4) 0.1817(3) 0.5265(2) 0.094(2) Uani 1 1 d . . . H18A H -0.2837 0.1794 0.4974 0.141 Uiso 1 1 calc R . . H18B H -0.3018 0.1856 0.5431 0.141 Uiso 1 1 calc R . . H18C H -0.2363 0.1452 0.5344 0.141 Uiso 1 1 calc R . . C19A C -0.2584(4) 0.3178(3) 0.5203(2) 0.106(3) Uani 1 1 d . . . H19A H -0.2780 0.3156 0.4911 0.160 Uiso 1 1 calc R . . H19B H -0.2288 0.3536 0.5253 0.160 Uiso 1 1 calc R . . H19C H -0.2973 0.3197 0.5366 0.160 Uiso 1 1 calc R . . C20A C -0.1654(4) 0.2517(4) 0.59111(17) 0.110(3) Uani 1 1 d . . . H20A H -0.1336 0.2862 0.5964 0.165 Uiso 1 1 calc R . . H20B H -0.1389 0.2149 0.5988 0.165 Uiso 1 1 calc R . . H20C H -0.2043 0.2555 0.6074 0.165 Uiso 1 1 calc R . . C21A C -0.1083(3) 0.2074(3) 0.48217(18) 0.0607(16) Uani 1 1 d . . . C22A C -0.1314(3) 0.1431(3) 0.48290(19) 0.0683(18) Uani 1 1 d . . . C23A C -0.1064(4) 0.1074(4) 0.5156(2) 0.102(3) Uani 1 1 d . . . H23A H -0.0750 0.1233 0.5380 0.123 Uiso 1 1 calc R . . C24A C -0.1275(4) 0.0470(4) 0.5159(3) 0.123(3) Uani 1 1 d . . . H24A H -0.1095 0.0220 0.5383 0.147 Uiso 1 1 calc R . . C25A C -0.1753(4) 0.0234(3) 0.4830(3) 0.104(3) Uani 1 1 d . . . C26A C -0.2016(4) 0.0603(4) 0.4515(2) 0.096(2) Uani 1 1 d . . . H26A H -0.2355 0.0453 0.4298 0.115 Uiso 1 1 calc R . . C27A C -0.1796(3) 0.1192(3) 0.45031(19) 0.0744(19) Uani 1 1 d . . . H27A H -0.1972 0.1437 0.4275 0.089 Uiso 1 1 calc R . . C32A C -0.0754(3) 0.1783(3) 0.37296(18) 0.095(2) Uani 1 1 d . . . H32A H -0.1195 0.1576 0.3763 0.143 Uiso 1 1 calc R . . H32B H -0.0510 0.1561 0.3535 0.143 Uiso 1 1 calc R . . H32C H -0.0864 0.2187 0.3625 0.143 Uiso 1 1 calc R . . C33A C 0.0682(3) 0.2220(3) 0.4187(2) 0.096(2) Uani 1 1 d . . . H33A H 0.0984 0.2237 0.4455 0.144 Uiso 1 1 calc R . . H33B H 0.0579 0.2627 0.4086 0.144 Uiso 1 1 calc R . . H33C H 0.0930 0.2002 0.3992 0.144 Uiso 1 1 calc R . . C34A C 0.0071(4) 0.1050(3) 0.4434(2) 0.104(3) Uani 1 1 d . . . H34A H -0.0363 0.0830 0.4464 0.157 Uiso 1 1 calc R . . H34B H 0.0376 0.1074 0.4700 0.157 Uiso 1 1 calc R . . H34C H 0.0324 0.0840 0.4238 0.157 Uiso 1 1 calc R . . Zr1B Zr -0.05132(3) 0.33738(3) 0.147151(16) 0.05675(19) Uani 1 1 d . . . Cl1B Cl -0.06139(9) 0.39736(8) 0.20786(5) 0.0833(5) Uani 1 1 d . . . Cl2B Cl -0.15274(9) 0.37917(9) 0.10209(5) 0.0900(6) Uani 1 1 d . . . Si1B Si 0.11878(10) 0.31016(9) 0.21371(5) 0.0716(5) Uani 1 1 d . . . Si2B Si 0.01271(10) 0.43425(9) 0.06686(5) 0.0675(5) Uani 1 1 d . . . Si3B Si -0.18123(10) 0.25794(10) 0.20188(5) 0.0747(6) Uani 1 1 d . . . Si4B Si -0.00613(10) 0.20783(9) 0.08187(5) 0.0677(5) Uani 1 1 d . . . N1B N 0.0648(2) 0.3337(2) 0.16815(13) 0.0549(12) Uani 1 1 d . . . N2B N 0.0207(2) 0.3864(2) 0.11038(13) 0.0570(13) Uani 1 1 d . . . N3B N -0.1132(2) 0.2634(2) 0.17036(13) 0.0611(13) Uani 1 1 d . . . N4B N -0.0472(2) 0.2458(2) 0.11905(13) 0.0573(13) Uani 1 1 d . . . C1B C 0.2036(4) 0.2750(4) 0.2017(2) 0.113(3) Uani 1 1 d . . . H1B1 H 0.2328 0.3056 0.1909 0.169 Uiso 1 1 calc R . . H1B2 H 0.1921 0.2434 0.1812 0.169 Uiso 1 1 calc R . . H1B3 H 0.2299 0.2577 0.2268 0.169 Uiso 1 1 calc R . . C2B C 0.1377(4) 0.3721(4) 0.25117(19) 0.110(3) Uani 1 1 d . . . H2B1 H 0.1667 0.4025 0.2400 0.164 Uiso 1 1 calc R . . H2B2 H 0.1636 0.3565 0.2769 0.164 Uiso 1 1 calc R . . H2B3 H 0.0930 0.3901 0.2564 0.164 Uiso 1 1 calc R . . C3B C 0.0647(4) 0.2522(4) 0.2348(2) 0.126(3) Uani 1 1 d . . . H3B1 H 0.0547 0.2196 0.2150 0.190 Uiso 1 1 calc R . . H3B2 H 0.0199 0.2699 0.2403 0.190 Uiso 1 1 calc R . . H3B3 H 0.0909 0.2365 0.2605 0.190 Uiso 1 1 calc R . . C4B C 0.0759(3) 0.3770(3) 0.14117(18) 0.0566(16) Uani 1 1 d . . . C5B C 0.1427(3) 0.4141(3) 0.14450(17) 0.0599(16) Uani 1 1 d . . . C6B C 0.2043(3) 0.3910(3) 0.13232(17) 0.0700(18) Uani 1 1 d . . . H6B H 0.2052 0.3507 0.1233 0.084 Uiso 1 1 calc R . . C7B C 0.2647(4) 0.4267(4) 0.1333(2) 0.093(2) Uani 1 1 d . . . H7B H 0.3061 0.4107 0.1245 0.112 Uiso 1 1 calc R . . C8B C 0.2650(4) 0.4858(5) 0.1472(2) 0.096(3) Uani 1 1 d D . . C9B C 0.2035(4) 0.5079(3) 0.1609(2) 0.092(2) Uani 1 1 d . . . H9B H 0.2036 0.5474 0.1714 0.111 Uiso 1 1 calc R . . C10B C 0.1417(3) 0.4725(3) 0.15929(19) 0.0749(19) Uani 1 1 d . . . H10B H 0.1002 0.4882 0.1681 0.090 Uiso 1 1 calc R . . C15B C -0.0377(4) 0.3909(3) 0.02376(17) 0.089(2) Uani 1 1 d . . . H15D H -0.0840 0.3794 0.0309 0.134 Uiso 1 1 calc R . . H15E H -0.0109 0.3549 0.0188 0.134 Uiso 1 1 calc R . . H15F H -0.0446 0.4157 -0.0010 0.134 Uiso 1 1 calc R . . C16B C -0.0361(4) 0.5035(3) 0.07835(19) 0.096(2) Uani 1 1 d . . . H16D H -0.0080 0.5252 0.1010 0.144 Uiso 1 1 calc R . . H16E H -0.0820 0.4924 0.0861 0.144 Uiso 1 1 calc R . . H16F H -0.0437 0.5290 0.0539 0.144 Uiso 1 1 calc R . . C17B C 0.1003(3) 0.4551(3) 0.05086(18) 0.097(2) Uani 1 1 d . . . H17D H 0.1284 0.4782 0.0728 0.146 Uiso 1 1 calc R . . H17E H 0.0920 0.4793 0.0258 0.146 Uiso 1 1 calc R . . H17F H 0.1262 0.4187 0.0456 0.146 Uiso 1 1 calc R . . C18B C -0.1378(4) 0.2514(3) 0.25688(16) 0.092(2) Uani 1 1 d . . . H18D H -0.1050 0.2849 0.2636 0.139 Uiso 1 1 calc R . . H18E H -0.1116 0.2136 0.2607 0.139 Uiso 1 1 calc R . . H18F H -0.1743 0.2523 0.2749 0.139 Uiso 1 1 calc R . . C19B C -0.2353(3) 0.3289(3) 0.1930(2) 0.104(3) Uani 1 1 d . . . H19D H -0.2043 0.3636 0.1997 0.156 Uiso 1 1 calc R . . H19E H -0.2726 0.3288 0.2105 0.156 Uiso 1 1 calc R . . H19F H -0.2570 0.3310 0.1641 0.156 Uiso 1 1 calc R . . C20B C -0.2442(4) 0.1936(4) 0.1888(2) 0.111(3) Uani 1 1 d . . . H20D H -0.2670 0.1971 0.1603 0.167 Uiso 1 1 calc R . . H20E H -0.2806 0.1942 0.2070 0.167 Uiso 1 1 calc R . . H20F H -0.2179 0.1558 0.1925 0.167 Uiso 1 1 calc R . . C21B C -0.0907(3) 0.2244(3) 0.14383(16) 0.0581(16) Uani 1 1 d . . . C22B C -0.1130(3) 0.1586(3) 0.14263(17) 0.0589(16) Uani 1 1 d . . . C23B C -0.0841(3) 0.1209(3) 0.17504(19) 0.0748(19) Uani 1 1 d . . . H23B H -0.0518 0.1362 0.1973 0.090 Uiso 1 1 calc R . . C24B C -0.1032(4) 0.0614(4) 0.1741(2) 0.091(2) Uani 1 1 d . . . H24B H -0.0828 0.0359 0.1958 0.109 Uiso 1 1 calc R . . C25B C -0.1515(4) 0.0374(3) 0.1424(2) 0.081(2) Uani 1 1 d . . . C26B C -0.1808(3) 0.0760(3) 0.1103(2) 0.0756(19) Uani 1 1 d . . . H26B H -0.2144 0.0610 0.0884 0.091 Uiso 1 1 calc R . . C27B C -0.1605(3) 0.1360(3) 0.11060(17) 0.0648(17) Uani 1 1 d . . . H27B H -0.1795 0.1615 0.0886 0.078 Uiso 1 1 calc R . . C32B C 0.0204(4) 0.1289(3) 0.0964(2) 0.094(2) Uani 1 1 d . . . H32D H -0.0219 0.1055 0.0995 0.141 Uiso 1 1 calc R . . H32E H 0.0529 0.1290 0.1224 0.141 Uiso 1 1 calc R . . H32F H 0.0442 0.1111 0.0749 0.141 Uiso 1 1 calc R . . C33B C 0.0763(3) 0.2499(3) 0.0764(2) 0.094(2) Uani 1 1 d . . . H33D H 0.1083 0.2495 0.1026 0.140 Uiso 1 1 calc R . . H33E H 0.0642 0.2913 0.0685 0.140 Uiso 1 1 calc R . . H33F H 0.0999 0.2310 0.0552 0.140 Uiso 1 1 calc R . . C34B C -0.0667(4) 0.2076(4) 0.03179(17) 0.102(3) Uani 1 1 d . . . H34D H -0.1098 0.1851 0.0347 0.153 Uiso 1 1 calc R . . H34E H -0.0427 0.1887 0.0108 0.153 Uiso 1 1 calc R . . H34F H -0.0794 0.2488 0.0237 0.153 Uiso 1 1 calc R . . Zr1C Zr 0.44729(3) 0.20144(3) 0.302666(17) 0.0614(2) Uani 1 1 d . . . Cl1C Cl 0.42713(11) 0.13698(9) 0.35948(6) 0.1039(7) Uani 1 1 d . . . Cl2C Cl 0.34387(10) 0.16836(10) 0.25599(6) 0.1081(7) Uani 1 1 d . . . Si1C Si 0.33452(11) 0.28877(10) 0.36431(5) 0.0795(6) Uani 1 1 d . . . Si2C Si 0.49911(9) 0.32779(8) 0.23712(5) 0.0629(5) Uani 1 1 d . . . Si3C Si 0.61798(11) 0.22246(10) 0.37107(6) 0.0852(6) Uani 1 1 d . . . Si4C Si 0.50833(10) 0.10034(9) 0.22425(5) 0.0735(5) Uani 1 1 d . . . N1C N 0.3969(2) 0.2798(2) 0.32955(13) 0.0601(13) Uani 1 1 d . . . N2C N 0.4588(2) 0.2932(2) 0.27601(12) 0.0546(12) Uani 1 1 d . . . N3C N 0.5630(2) 0.1999(2) 0.32548(14) 0.0640(14) Uani 1 1 d . . . N4C N 0.5181(2) 0.1492(2) 0.26702(13) 0.0599(13) Uani 1 1 d . . . C1C C 0.3825(4) 0.2722(4) 0.41707(17) 0.108(3) Uani 1 1 d . . . H1C1 H 0.4199 0.3020 0.4245 0.163 Uiso 1 1 calc R . . H1C2 H 0.4037 0.2322 0.4174 0.163 Uiso 1 1 calc R . . H1C3 H 0.3489 0.2738 0.4369 0.163 Uiso 1 1 calc R . . C2C C 0.2614(4) 0.2351(4) 0.3480(2) 0.108(3) Uani 1 1 d . . . H2C1 H 0.2375 0.2460 0.3206 0.162 Uiso 1 1 calc R . . H2C2 H 0.2273 0.2364 0.3675 0.162 Uiso 1 1 calc R . . H2C3 H 0.2809 0.1946 0.3473 0.162 Uiso 1 1 calc R . . C3C C 0.2944(4) 0.3657(4) 0.3655(2) 0.119(3) Uani 1 1 d . . . H3C1 H 0.3320 0.3950 0.3741 0.178 Uiso 1 1 calc R . . H3C2 H 0.2602 0.3662 0.3849 0.178 Uiso 1 1 calc R . . H3C3 H 0.2702 0.3761 0.3381 0.178 Uiso 1 1 calc R . . C4C C 0.4179(3) 0.3183(3) 0.30195(16) 0.0544(16) Uani 1 1 d . . . C5C C 0.3983(3) 0.3836(3) 0.30030(17) 0.0533(15) Uani 1 1 d . . . C6C C 0.4330(3) 0.4234(3) 0.32844(18) 0.0696(18) Uani 1 1 d . . . H6C H 0.4705 0.4096 0.3485 0.084 Uiso 1 1 calc R . . C7C C 0.4135(3) 0.4833(3) 0.3277(2) 0.0744(19) Uani 1 1 d . . . H7C H 0.4392 0.5102 0.3466 0.089 Uiso 1 1 calc R . . C8C C 0.3570(4) 0.5049(3) 0.2997(2) 0.0673(17) Uani 1 1 d D . . C9C C 0.3223(3) 0.4638(3) 0.27105(18) 0.0694(18) Uani 1 1 d . . . H9C H 0.2839 0.4770 0.2514 0.083 Uiso 1 1 calc R . . C10C C 0.3436(3) 0.4032(3) 0.27111(17) 0.0627(17) Uani 1 1 d . . . H10C H 0.3204 0.3761 0.2513 0.075 Uiso 1 1 calc R . . C15C C 0.4335(3) 0.3309(3) 0.18848(16) 0.088(2) Uani 1 1 d . . . H15G H 0.3926 0.3553 0.1930 0.133 Uiso 1 1 calc R . . H15H H 0.4175 0.2903 0.1806 0.133 Uiso 1 1 calc R . . H15I H 0.4562 0.3487 0.1666 0.133 Uiso 1 1 calc R . . C16C C 0.5779(3) 0.2818(3) 0.2298(2) 0.090(2) Uani 1 1 d . . . H16G H 0.6112 0.2806 0.2555 0.136 Uiso 1 1 calc R . . H16H H 0.6013 0.2995 0.2082 0.136 Uiso 1 1 calc R . . H16I H 0.5626 0.2410 0.2220 0.136 Uiso 1 1 calc R . . C17C C 0.5325(4) 0.4059(3) 0.2518(2) 0.096(2) Uani 1 1 d . . . H17G H 0.4924 0.4313 0.2563 0.144 Uiso 1 1 calc R . . H17H H 0.5555 0.4227 0.2297 0.144 Uiso 1 1 calc R . . H17I H 0.5668 0.4040 0.2770 0.144 Uiso 1 1 calc R . . C18C C 0.5758(4) 0.2914(4) 0.3871(3) 0.175(5) Uani 1 1 d . . . H18G H 0.5763 0.3223 0.3661 0.262 Uiso 1 1 calc R . . H18H H 0.6020 0.3056 0.4132 0.262 Uiso 1 1 calc R . . H18I H 0.5266 0.2827 0.3907 0.262 Uiso 1 1 calc R . . C19C C 0.6177(5) 0.1634(5) 0.4107(2) 0.168(5) Uani 1 1 d . . . H19G H 0.6394 0.1270 0.4017 0.252 Uiso 1 1 calc R . . H19H H 0.5687 0.1550 0.4147 0.252 Uiso 1 1 calc R . . H19I H 0.6448 0.1772 0.4366 0.252 Uiso 1 1 calc R . . C20C C 0.7111(4) 0.2411(4) 0.3634(3) 0.152(4) Uani 1 1 d . . . H20G H 0.7101 0.2728 0.3428 0.227 Uiso 1 1 calc R . . H20H H 0.7338 0.2054 0.3539 0.227 Uiso 1 1 calc R . . H20I H 0.7380 0.2547 0.3894 0.227 Uiso 1 1 calc R . . C21C C 0.5725(3) 0.1565(3) 0.29798(18) 0.0616(16) Uani 1 1 d . . . C22C C 0.6370(3) 0.1171(3) 0.30346(17) 0.0587(16) Uani 1 1 d . . . C23C C 0.7011(3) 0.1358(3) 0.29149(18) 0.0728(19) Uani 1 1 d . . . H23C H 0.7044 0.1746 0.2802 0.087 Uiso 1 1 calc R . . C24C C 0.7594(4) 0.0983(3) 0.29591(19) 0.0743(19) Uani 1 1 d . . . H24C H 0.8024 0.1123 0.2879 0.089 Uiso 1 1 calc R . . C25C C 0.7571(3) 0.0406(3) 0.31177(18) 0.0706(18) Uani 1 1 d D . . C26C C 0.6932(4) 0.0221(3) 0.3247(2) 0.081(2) Uani 1 1 d . . . H26C H 0.6903 -0.0161 0.3369 0.097 Uiso 1 1 calc R . . C27C C 0.6338(3) 0.0600(3) 0.31944(19) 0.0730(18) Uani 1 1 d . . . H27C H 0.5904 0.0462 0.3270 0.088 Uiso 1 1 calc R . . C32C C 0.4567(4) 0.0342(3) 0.23575(19) 0.096(2) Uani 1 1 d . . . H32G H 0.4831 0.0123 0.2589 0.143 Uiso 1 1 calc R . . H32H H 0.4488 0.0081 0.2116 0.143 Uiso 1 1 calc R . . H32I H 0.4109 0.0471 0.2428 0.143 Uiso 1 1 calc R . . C33C C 0.4599(4) 0.1434(3) 0.17968(18) 0.111(3) Uani 1 1 d . . . H33G H 0.4885 0.1780 0.1739 0.167 Uiso 1 1 calc R . . H33H H 0.4142 0.1573 0.1865 0.167 Uiso 1 1 calc R . . H33I H 0.4517 0.1175 0.1555 0.167 Uiso 1 1 calc R . . C34C C 0.5951(4) 0.0769(4) 0.20921(19) 0.123(3) Uani 1 1 d . . . H34G H 0.6220 0.1124 0.2033 0.185 Uiso 1 1 calc R . . H34H H 0.5865 0.0516 0.1847 0.185 Uiso 1 1 calc R . . H34I H 0.6224 0.0543 0.2317 0.185 Uiso 1 1 calc R . . C11A C 0.3263(4) 0.4956(5) 0.4815(3) 0.139(4) Uani 1 1 d D . . H11X H 0.3582 0.4741 0.4653 0.167 Uiso 1 1 calc R . . H11Y H 0.3105 0.5326 0.4662 0.167 Uiso 1 1 calc R . . C12A C 0.3663(4) 0.5123(4) 0.5193(2) 0.129(3) Uani 1 1 d D . . H12X H 0.3855 0.4754 0.5334 0.154 Uiso 1 1 calc R . . H12Y H 0.3334 0.5305 0.5364 0.154 Uiso 1 1 calc R . . C13A C 0.4296(4) 0.5569(4) 0.5181(2) 0.116(3) Uani 1 1 d D . . H13X H 0.4575 0.5438 0.4966 0.139 Uiso 1 1 calc R . . H13Y H 0.4104 0.5972 0.5105 0.139 Uiso 1 1 calc R . . C14A C 0.4767(5) 0.5607(5) 0.5575(2) 0.151(4) Uani 1 1 d D . . H14X H 0.5147 0.5896 0.5553 0.227 Uiso 1 1 calc R . . H14Y H 0.4975 0.5213 0.5646 0.227 Uiso 1 1 calc R . . H14Z H 0.4494 0.5737 0.5789 0.227 Uiso 1 1 calc R . . C28A C -0.1938(3) -0.0424(3) 0.48208(19) 0.147(4) Uani 1 1 d G . . H28X H -0.1499 -0.0667 0.4857 0.177 Uiso 1 1 calc R . . H28Y H -0.2220 -0.0529 0.4554 0.177 Uiso 1 1 calc R . . C29A C -0.2370(3) -0.0553(3) 0.51713(19) 0.162(5) Uani 1 1 d R . . H29X H -0.2098 -0.0408 0.5432 0.194 Uiso 1 1 calc R . . H29Y H -0.2818 -0.0323 0.5121 0.194 Uiso 1 1 calc R . . C30A C -0.2550(3) -0.1219(3) 0.52209(19) 0.225(7) Uani 1 1 d R . . H30X H -0.2851 -0.1360 0.4968 0.270 Uiso 1 1 calc R . . H30Y H -0.2106 -0.1456 0.5256 0.270 Uiso 1 1 calc R . . C31A C -0.2940(3) -0.1325(3) 0.55909(19) 0.308(11) Uani 1 1 d R . . H31X H -0.3045 -0.1752 0.5612 0.462 Uiso 1 1 calc R . . H31Y H -0.3385 -0.1098 0.5554 0.462 Uiso 1 1 calc R . . H31Z H -0.2640 -0.1193 0.5842 0.462 Uiso 1 1 calc R . . C11B C 0.3306(5) 0.5270(5) 0.1444(3) 0.164(5) Uani 1 1 d D . . H11U H 0.3584 0.5088 0.1244 0.196 Uiso 1 1 calc R . . H11V H 0.3128 0.5660 0.1330 0.196 Uiso 1 1 calc R . . C12B C 0.3754(5) 0.5374(5) 0.1798(2) 0.150(4) Uani 1 1 d D . . H12U H 0.3955 0.4984 0.1899 0.180 Uiso 1 1 calc R . . H12V H 0.3465 0.5523 0.2003 0.180 Uiso 1 1 calc R . . C13B C 0.4377(4) 0.5811(4) 0.1793(2) 0.135(4) Uani 1 1 d D . . H13U H 0.4672 0.5671 0.1588 0.162 Uiso 1 1 calc R . . H13V H 0.4186 0.6209 0.1703 0.162 Uiso 1 1 calc R . . C14B C 0.4819(4) 0.5873(4) 0.2181(2) 0.132(3) Uani 1 1 d D . . H14U H 0.5199 0.6160 0.2156 0.198 Uiso 1 1 calc R . . H14V H 0.5027 0.5484 0.2267 0.198 Uiso 1 1 calc R . . H14W H 0.4534 0.6016 0.2385 0.198 Uiso 1 1 calc R . . C28B C -0.1719(4) -0.0301(3) 0.13692(19) 0.139(4) Uani 1 1 d G . . H28U H -0.2002 -0.0335 0.1093 0.167 Uiso 1 1 calc R . . H28V H -0.1269 -0.0516 0.1356 0.167 Uiso 1 1 calc R . . C29B C -0.2117(4) -0.0672(3) 0.16568(19) 0.363(14) Uani 1 1 d R . . H29U H -0.2376 -0.0999 0.1496 0.435 Uiso 1 1 calc R . . H29V H -0.1765 -0.0858 0.1871 0.435 Uiso 1 1 calc R . . C30B C -0.2650(4) -0.0312(3) 0.18682(19) 0.233(7) Uani 1 1 d R . . H30U H -0.2390 -0.0001 0.2045 0.280 Uiso 1 1 calc R . . H30V H -0.2989 -0.0106 0.1657 0.280 Uiso 1 1 calc R . . C31B C -0.3063(4) -0.0712(3) 0.21298(19) 0.274(9) Uani 1 1 d R . . H31U H -0.3395 -0.0466 0.2259 0.411 Uiso 1 1 calc R . . H31V H -0.2730 -0.0910 0.2343 0.411 Uiso 1 1 calc R . . H31W H -0.3328 -0.1015 0.1955 0.411 Uiso 1 1 calc R . . C11C C 0.3324(4) 0.5689(3) 0.3010(2) 0.092(2) Uani 1 1 d D . . H11P H 0.3745 0.5953 0.3034 0.111 Uiso 1 1 calc R . . H11R H 0.3026 0.5782 0.2745 0.111 Uiso 1 1 calc R . . C12C C 0.2913(5) 0.5840(4) 0.3346(3) 0.147(4) Uani 1 1 d D . . H12P H 0.3263 0.5870 0.3599 0.176 Uiso 1 1 calc R . . H12R H 0.2722 0.6248 0.3288 0.176 Uiso 1 1 calc R . . C13C C 0.2358(6) 0.5502(4) 0.3447(4) 0.184(5) Uani 1 1 d D . . H13P H 0.2532 0.5085 0.3481 0.220 Uiso 1 1 calc R . . H13R H 0.1985 0.5504 0.3203 0.220 Uiso 1 1 calc R . . C14C C 0.1993(4) 0.5639(4) 0.3814(2) 0.131(3) Uani 1 1 d D . . H14P H 0.1604 0.5356 0.3823 0.197 Uiso 1 1 calc R . . H14R H 0.1804 0.6047 0.3791 0.197 Uiso 1 1 calc R . . H14S H 0.2336 0.5604 0.4066 0.197 Uiso 1 1 calc R . . C28C C 0.8200(3) -0.0022(3) 0.3154(2) 0.090(2) Uani 1 1 d D . . H28M H 0.8041 -0.0403 0.3016 0.108 Uiso 1 1 calc R . . H28N H 0.8567 0.0151 0.3005 0.108 Uiso 1 1 calc R . . C29C C 0.8534(4) -0.0158(3) 0.3586(2) 0.110(3) Uani 1 1 d D . . H29M H 0.8169 -0.0336 0.3735 0.132 Uiso 1 1 calc R . . H29N H 0.8692 0.0222 0.3725 0.132 Uiso 1 1 calc R . . C30C C 0.9168(4) -0.0586(4) 0.3617(2) 0.129(3) Uani 1 1 d D . . H30M H 0.9006 -0.0967 0.3482 0.155 Uiso 1 1 calc R . . H30N H 0.9525 -0.0411 0.3461 0.155 Uiso 1 1 calc R . . C31C C 0.9510(6) -0.0716(5) 0.4028(3) 0.223(7) Uani 1 1 d D . . H31M H 0.9908 -0.0989 0.4016 0.335 Uiso 1 1 calc R . . H31N H 0.9167 -0.0902 0.4183 0.335 Uiso 1 1 calc R . . H31O H 0.9686 -0.0343 0.4163 0.335 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 Zr1A 0.0583(4) 0.0564(4) 0.0590(3) -0.0001(3) 0.0009(3) 0.0034(3) Cl1A 0.0852(13) 0.0721(13) 0.0913(11) -0.0203(9) 0.0153(9) 0.0021(10) Cl2A 0.0664(11) 0.1013(15) 0.0949(12) 0.0278(11) -0.0064(9) 0.0068(10) Si1A 0.0749(13) 0.0744(14) 0.0654(10) 0.0060(10) -0.0117(9) 0.0114(11) Si2A 0.0759(14) 0.0919(17) 0.0597(10) 0.0113(10) 0.0009(9) -0.0041(12) Si3A 0.0846(14) 0.0728(14) 0.0667(11) -0.0001(10) 0.0149(10) -0.0077(11) Si4A 0.0680(13) 0.0731(15) 0.0839(12) -0.0171(10) 0.0004(10) 0.0162(11) N1A 0.061(3) 0.071(4) 0.055(3) 0.003(3) -0.001(2) 0.006(3) N2A 0.054(3) 0.064(4) 0.058(3) -0.002(2) -0.002(2) 0.006(3) N3A 0.077(4) 0.058(4) 0.055(3) -0.004(3) 0.014(3) 0.003(3) N4A 0.061(3) 0.055(3) 0.068(3) -0.003(3) -0.003(3) 0.007(3) C1A 0.118(6) 0.109(7) 0.086(5) 0.033(4) -0.004(4) 0.001(5) C2A 0.097(6) 0.101(6) 0.074(4) -0.010(4) -0.016(4) 0.012(5) C3A 0.117(7) 0.116(7) 0.103(5) 0.006(5) -0.017(5) 0.055(6) C4A 0.069(5) 0.059(5) 0.053(4) -0.010(3) 0.006(3) 0.018(4) C5A 0.053(4) 0.067(5) 0.062(4) -0.003(3) 0.005(3) 0.004(4) C6A 0.069(5) 0.087(6) 0.090(5) -0.024(4) 0.008(4) 0.000(5) C7A 0.068(6) 0.098(7) 0.112(6) -0.020(5) 0.007(4) 0.010(5) C8A 0.046(5) 0.143(9) 0.096(5) -0.011(5) 0.011(4) -0.005(5) C9A 0.075(6) 0.083(6) 0.103(5) -0.005(4) 0.006(4) -0.021(5) C10A 0.065(5) 0.072(6) 0.084(4) 0.004(4) 0.011(4) 0.002(4) C15A 0.131(7) 0.080(6) 0.096(5) 0.019(4) -0.008(5) -0.006(5) C16A 0.112(6) 0.109(7) 0.067(4) 0.003(4) -0.007(4) 0.002(5) C17A 0.095(6) 0.179(9) 0.077(5) 0.017(5) 0.028(4) -0.008(6) C18A 0.099(6) 0.094(6) 0.095(5) -0.008(4) 0.032(4) -0.023(5) C19A 0.086(6) 0.104(7) 0.137(6) 0.024(5) 0.042(5) 0.008(5) C20A 0.136(7) 0.131(8) 0.066(4) -0.017(4) 0.023(4) -0.022(6) C21A 0.056(4) 0.057(5) 0.063(4) 0.010(3) -0.014(3) 0.002(4) C22A 0.068(5) 0.056(5) 0.075(4) 0.005(4) -0.009(4) 0.005(4) C23A 0.116(7) 0.064(6) 0.112(6) 0.022(5) -0.034(5) -0.023(5) C24A 0.125(7) 0.089(7) 0.136(7) 0.027(6) -0.044(6) -0.009(6) C25A 0.103(6) 0.044(5) 0.151(7) -0.013(5) -0.024(6) -0.025(5) C26A 0.091(6) 0.066(6) 0.120(6) -0.014(5) -0.016(5) 0.006(5) C27A 0.081(5) 0.064(5) 0.073(4) -0.010(4) -0.006(4) 0.012(4) C32A 0.088(5) 0.113(7) 0.083(4) -0.018(4) 0.009(4) 0.013(5) C33A 0.080(5) 0.099(6) 0.113(5) -0.029(5) 0.023(4) 0.014(5) C34A 0.092(6) 0.082(6) 0.136(6) -0.009(5) 0.007(5) 0.030(5) Zr1B 0.0487(4) 0.0599(4) 0.0594(3) 0.0035(3) 0.0004(3) -0.0022(3) Cl1B 0.0759(12) 0.0833(14) 0.0904(11) -0.0199(10) 0.0117(9) -0.0038(10) Cl2B 0.0577(11) 0.1152(17) 0.0914(11) 0.0272(11) -0.0077(9) 0.0097(10) Si1B 0.0601(12) 0.0724(14) 0.0749(11) 0.0164(10) -0.0148(9) -0.0011(10) Si2B 0.0692(13) 0.0656(14) 0.0652(10) 0.0130(9) 0.0013(9) -0.0005(10) Si3B 0.0707(13) 0.0891(16) 0.0664(11) -0.0094(10) 0.0177(9) -0.0194(11) Si4B 0.0651(12) 0.0704(14) 0.0680(10) -0.0034(9) 0.0111(9) -0.0003(10) N1B 0.051(3) 0.048(3) 0.063(3) 0.011(3) -0.002(2) -0.005(2) N2B 0.046(3) 0.057(3) 0.064(3) 0.006(2) -0.004(2) 0.003(2) N3B 0.064(3) 0.069(4) 0.052(3) -0.007(3) 0.012(2) -0.008(3) N4B 0.053(3) 0.065(4) 0.055(3) 0.005(2) 0.010(2) -0.009(3) C1B 0.097(6) 0.112(7) 0.119(6) 0.019(5) -0.017(5) 0.040(5) C2B 0.107(6) 0.128(7) 0.082(5) -0.010(5) -0.026(4) 0.020(5) C3B 0.098(6) 0.138(8) 0.129(6) 0.079(6) -0.030(5) -0.029(6) C4B 0.042(4) 0.052(4) 0.075(4) -0.004(3) 0.004(3) 0.007(3) C5B 0.049(4) 0.067(5) 0.062(4) 0.009(3) 0.000(3) 0.000(4) C6B 0.056(5) 0.070(5) 0.082(4) 0.009(4) 0.000(4) 0.000(4) C7B 0.052(5) 0.114(7) 0.113(6) -0.004(5) 0.012(4) -0.007(5) C8B 0.069(6) 0.122(8) 0.092(5) 0.011(5) -0.007(4) -0.037(6) C9B 0.097(6) 0.068(6) 0.106(5) -0.002(4) -0.008(5) -0.014(5) C10B 0.059(5) 0.073(6) 0.091(5) -0.009(4) 0.006(4) -0.011(4) C15B 0.103(6) 0.092(6) 0.068(4) 0.010(4) -0.007(4) -0.001(5) C16B 0.110(6) 0.081(6) 0.091(5) 0.014(4) -0.004(4) 0.003(5) C17B 0.093(6) 0.115(7) 0.083(4) 0.041(4) 0.010(4) -0.011(5) C18B 0.110(6) 0.107(6) 0.064(4) 0.000(4) 0.025(4) -0.011(5) C19B 0.070(5) 0.114(7) 0.133(6) 0.005(5) 0.030(5) 0.003(5) C20B 0.093(6) 0.142(8) 0.109(5) -0.033(5) 0.048(5) -0.058(5) C21B 0.053(4) 0.066(5) 0.049(3) 0.001(3) -0.014(3) 0.003(4) C22B 0.056(4) 0.058(5) 0.062(4) 0.003(3) 0.004(3) -0.005(3) C23B 0.070(5) 0.062(5) 0.086(5) 0.010(4) -0.011(4) -0.009(4) C24B 0.093(6) 0.077(6) 0.095(5) 0.015(4) -0.007(4) -0.007(5) C25B 0.102(6) 0.056(5) 0.090(5) -0.003(4) 0.033(5) -0.013(5) C26B 0.061(4) 0.081(6) 0.083(5) -0.006(4) 0.002(3) -0.007(4) C27B 0.068(5) 0.057(5) 0.065(4) -0.005(3) -0.003(3) -0.005(4) C32B 0.100(6) 0.077(6) 0.112(5) 0.003(4) 0.036(4) 0.013(5) C33B 0.090(5) 0.101(6) 0.100(5) -0.014(4) 0.051(4) -0.008(5) C34B 0.111(6) 0.126(7) 0.069(4) -0.008(4) 0.009(4) 0.006(5) Zr1C 0.0532(4) 0.0545(4) 0.0721(4) 0.0024(3) -0.0059(3) 0.0020(3) Cl1C 0.1000(15) 0.0851(15) 0.1283(15) 0.0387(12) 0.0228(12) 0.0030(12) Cl2C 0.0656(12) 0.1077(17) 0.1373(16) -0.0412(13) -0.0296(11) 0.0111(11) Si1C 0.0844(14) 0.0954(17) 0.0625(11) 0.0073(10) 0.0229(10) 0.0023(12) Si2C 0.0586(12) 0.0606(13) 0.0696(10) 0.0012(9) 0.0098(9) -0.0039(9) Si3C 0.0707(14) 0.0808(16) 0.0922(13) -0.0203(11) -0.0271(11) 0.0075(12) Si4C 0.0773(14) 0.0750(15) 0.0643(10) -0.0097(10) -0.0029(9) -0.0006(11) N1C 0.056(3) 0.066(4) 0.057(3) 0.001(3) 0.007(2) 0.001(3) N2C 0.054(3) 0.056(3) 0.055(3) -0.003(2) 0.009(2) 0.001(3) N3C 0.056(3) 0.057(4) 0.072(3) 0.000(3) -0.014(3) 0.002(3) N4C 0.059(3) 0.058(4) 0.057(3) 0.004(2) -0.009(2) 0.006(3) C1C 0.125(7) 0.139(8) 0.061(4) 0.007(4) 0.014(4) -0.015(6) C2C 0.084(6) 0.142(8) 0.102(5) 0.010(5) 0.030(4) -0.013(5) C3C 0.145(7) 0.117(7) 0.112(6) 0.020(5) 0.078(5) 0.049(6) C4C 0.049(4) 0.068(5) 0.042(3) -0.001(3) -0.008(3) -0.006(3) C5C 0.051(4) 0.046(4) 0.063(4) -0.001(3) 0.009(3) 0.001(3) C6C 0.063(4) 0.064(5) 0.076(4) -0.009(4) -0.009(3) 0.005(4) C7C 0.070(5) 0.057(5) 0.095(5) -0.019(4) 0.008(4) -0.002(4) C8C 0.075(5) 0.053(5) 0.079(4) 0.004(4) 0.027(4) 0.004(4) C9C 0.066(5) 0.071(5) 0.071(4) 0.014(4) 0.010(3) 0.012(4) C10C 0.055(4) 0.070(5) 0.059(4) -0.003(3) -0.002(3) 0.004(4) C15C 0.083(5) 0.117(6) 0.065(4) 0.009(4) 0.011(4) -0.004(5) C16C 0.077(5) 0.089(6) 0.114(5) 0.007(4) 0.041(4) 0.000(4) C17C 0.111(6) 0.073(6) 0.110(5) -0.008(4) 0.039(5) -0.024(5) C18C 0.112(7) 0.192(11) 0.192(9) -0.123(8) -0.070(6) 0.068(7) C19C 0.208(11) 0.184(11) 0.087(5) 0.036(6) -0.059(6) -0.047(9) C20C 0.078(6) 0.181(11) 0.180(8) -0.072(8) -0.030(6) -0.023(6) C21C 0.064(5) 0.054(5) 0.065(4) 0.007(3) 0.004(3) -0.006(4) C22C 0.054(4) 0.057(5) 0.063(4) 0.006(3) 0.002(3) 0.002(4) C23C 0.061(5) 0.067(5) 0.090(5) 0.015(4) 0.006(4) -0.004(4) C24C 0.056(5) 0.068(5) 0.098(5) 0.010(4) 0.011(4) -0.008(4) C25C 0.049(4) 0.082(6) 0.078(4) -0.007(4) -0.001(3) 0.011(4) C26C 0.064(5) 0.060(5) 0.114(5) 0.014(4) -0.002(4) 0.010(4) C27C 0.056(4) 0.069(5) 0.095(5) 0.017(4) 0.013(3) 0.004(4) C32C 0.112(6) 0.078(6) 0.089(5) 0.004(4) -0.014(4) -0.002(5) C33C 0.146(7) 0.110(7) 0.067(4) 0.005(4) -0.020(4) -0.033(6) C34C 0.109(6) 0.182(10) 0.078(5) -0.053(5) 0.012(4) 0.003(6) C11A 0.078(6) 0.205(11) 0.134(7) -0.008(7) 0.013(5) -0.041(7) C12A 0.120(7) 0.166(10) 0.101(6) -0.011(6) 0.018(5) -0.050(7) C13A 0.095(6) 0.112(7) 0.137(7) 0.001(6) 0.007(5) -0.039(6) C14A 0.150(9) 0.166(11) 0.138(8) -0.040(7) 0.024(7) -0.037(8) C28A 0.125(8) 0.096(8) 0.211(10) 0.005(7) -0.010(7) -0.020(6) C29A 0.218(12) 0.061(7) 0.193(10) 0.027(7) -0.019(9) -0.047(7) C30A 0.130(10) 0.260(19) 0.260(15) 0.080(14) -0.052(10) -0.030(11) C31A 0.34(2) 0.33(2) 0.236(15) 0.096(15) -0.019(14) -0.177(19) C11B 0.129(8) 0.203(12) 0.143(8) 0.032(8) -0.030(7) -0.088(8) C12B 0.151(9) 0.203(11) 0.094(6) 0.012(6) 0.012(6) -0.095(8) C13B 0.109(7) 0.187(10) 0.103(6) 0.022(6) 0.001(5) -0.101(7) C14B 0.139(8) 0.133(8) 0.120(6) 0.013(6) 0.008(6) -0.064(7) C28B 0.185(10) 0.080(7) 0.163(9) 0.017(6) 0.056(8) -0.012(7) C29B 0.33(2) 0.50(4) 0.234(17) -0.17(2) -0.052(17) 0.11(3) C30B 0.249(16) 0.127(11) 0.334(18) -0.047(12) 0.078(14) 0.040(11) C31B 0.277(17) 0.279(19) 0.247(14) 0.085(13) -0.026(12) -0.157(15) C11C 0.099(6) 0.059(5) 0.125(6) 0.005(4) 0.039(5) 0.010(4) C12C 0.136(9) 0.069(7) 0.254(12) 0.000(7) 0.095(9) 0.022(6) C13C 0.191(12) 0.088(8) 0.295(14) -0.022(9) 0.111(11) 0.045(8) C14C 0.124(7) 0.150(9) 0.130(7) 0.000(6) 0.050(6) 0.039(7) C28C 0.061(5) 0.095(6) 0.110(5) 0.005(5) 0.000(4) 0.023(4) C29C 0.106(6) 0.099(7) 0.113(6) -0.026(5) -0.024(5) 0.043(5) C30C 0.118(7) 0.120(8) 0.134(7) -0.016(6) -0.028(6) 0.061(6) C31C 0.268(15) 0.174(12) 0.189(10) -0.038(9) -0.090(10) 0.131(11) _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 Zr1A N1A 2.207(5) . ? Zr1A N2A 2.215(5) . ? Zr1A N3A 2.223(5) . ? Zr1A N4A 2.225(5) . ? Zr1A Cl2A 2.4142(17) . ? Zr1A Cl1A 2.4220(16) . ? Zr1A C4A 2.587(7) . ? Zr1A C21A 2.623(7) . ? Si1A N1A 1.753(5) . ? Si1A C2A 1.850(7) . ? Si1A C3A 1.862(7) . ? Si1A C1A 1.864(7) . ? Si2A N2A 1.765(5) . ? Si2A C15A 1.822(7) . ? Si2A C16A 1.865(6) . ? Si2A C17A 1.877(7) . ? Si3A N3A 1.750(5) . ? Si3A C20A 1.853(6) . ? Si3A C19A 1.874(7) . ? Si3A C18A 1.878(7) . ? Si4A N4A 1.764(5) . ? Si4A C33A 1.851(7) . ? Si4A C32A 1.859(6) . ? Si4A C34A 1.868(7) . ? N1A C4A 1.343(7) . ? N2A C4A 1.338(7) . ? N3A C21A 1.335(7) . ? N4A C21A 1.345(7) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C1A H1A3 0.9700 . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C2A H2A3 0.9700 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C3A H3A3 0.9700 . ? C4A C5A 1.496(8) . ? C5A C10A 1.375(8) . ? C5A C6A 1.381(8) . ? C6A C7A 1.389(9) . ? C6A H6A 0.9400 . ? C7A C8A 1.375(10) . ? C7A H7A 0.9400 . ? C8A C9A 1.388(9) . ? C8A C11A 1.530(10) . ? C9A C10A 1.402(8) . ? C9A H9A 0.9400 . ? C10A H10A 0.9400 . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C15A H15C 0.9700 . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C16A H16C 0.9700 . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C17A H17C 0.9700 . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18A H18C 0.9700 . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C19A H19C 0.9700 . ? C20A H20A 0.9700 . ? C20A H20B 0.9700 . ? C20A H20C 0.9700 . ? C21A C22A 1.490(8) . ? C22A C23A 1.354(8) . ? C22A C27A 1.397(8) . ? C23A C24A 1.396(10) . ? C23A H23A 0.9400 . ? C24A C25A 1.398(9) . ? C24A H24A 0.9400 . ? C25A C26A 1.347(10) . ? C25A C28A 1.496(9) . ? C26A C27A 1.370(9) . ? C26A H26A 0.9400 . ? C27A H27A 0.9400 . ? C32A H32A 0.9700 . ? C32A H32B 0.9700 . ? C32A H32C 0.9700 . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C33A H33C 0.9700 . ? C34A H34A 0.9700 . ? C34A H34B 0.9700 . ? C34A H34C 0.9700 . ? Zr1B N1B 2.197(4) . ? Zr1B N3B 2.208(5) . ? Zr1B N2B 2.223(4) . ? Zr1B N4B 2.230(5) . ? Zr1B Cl1B 2.4153(17) . ? Zr1B Cl2B 2.4171(16) . ? Zr1B C4B 2.589(6) . ? Zr1B C21B 2.605(7) . ? Si1B N1B 1.752(4) . ? Si1B C3B 1.835(7) . ? Si1B C2B 1.837(7) . ? Si1B C1B 1.872(7) . ? Si2B N2B 1.761(5) . ? Si2B C15B 1.845(6) . ? Si2B C16B 1.853(7) . ? Si2B C17B 1.863(6) . ? Si3B N3B 1.763(5) . ? Si3B C20B 1.864(7) . ? Si3B C18B 1.864(6) . ? Si3B C19B 1.871(7) . ? Si4B N4B 1.748(5) . ? Si4B C33B 1.843(6) . ? Si4B C34B 1.850(6) . ? Si4B C32B 1.858(7) . ? N1B C4B 1.338(7) . ? N2B C4B 1.351(6) . ? N3B C21B 1.336(7) . ? N4B C21B 1.323(7) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C1B H1B3 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C2B H2B3 0.9700 . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C3B H3B3 0.9700 . ? C4B C5B 1.494(8) . ? C5B C6B 1.380(8) . ? C5B C10B 1.381(8) . ? C6B C7B 1.384(9) . ? C6B H6B 0.9400 . ? C7B C8B 1.383(10) . ? C7B H7B 0.9400 . ? C8B C9B 1.391(10) . ? C8B C11B 1.549(10) . ? C9B C10B 1.399(9) . ? C9B H9B 0.9400 . ? C10B H10B 0.9400 . ? C15B H15D 0.9700 . ? C15B H15E 0.9700 . ? C15B H15F 0.9700 . ? C16B H16D 0.9700 . ? C16B H16E 0.9700 . ? C16B H16F 0.9700 . ? C17B H17D 0.9700 . ? C17B H17E 0.9700 . ? C17B H17F 0.9700 . ? C18B H18D 0.9700 . ? C18B H18E 0.9700 . ? C18B H18F 0.9700 . ? C19B H19D 0.9700 . ? C19B H19E 0.9700 . ? C19B H19F 0.9700 . ? C20B H20D 0.9700 . ? C20B H20E 0.9700 . ? C20B H20F 0.9700 . ? C21B C22B 1.516(8) . ? C22B C27B 1.366(7) . ? C22B C23B 1.393(8) . ? C23B C24B 1.364(9) . ? C23B H23B 0.9400 . ? C24B C25B 1.381(9) . ? C24B H24B 0.9400 . ? C25B C26B 1.400(9) . ? C25B C28B 1.546(9) . ? C26B C27B 1.383(8) . ? C26B H26B 0.9400 . ? C27B H27B 0.9400 . ? C32B H32D 0.9700 . ? C32B H32E 0.9700 . ? C32B H32F 0.9700 . ? C33B H33D 0.9700 . ? C33B H33E 0.9700 . ? C33B H33F 0.9700 . ? C34B H34D 0.9700 . ? C34B H34E 0.9700 . ? C34B H34F 0.9700 . ? Zr1C N3C 2.199(4) . ? Zr1C N1C 2.220(5) . ? Zr1C N4C 2.221(5) . ? Zr1C N2C 2.232(5) . ? Zr1C Cl2C 2.4041(18) . ? Zr1C Cl1C 2.4135(18) . ? Zr1C C21C 2.587(6) . ? Zr1C C4C 2.644(6) . ? Si1C N1C 1.762(5) . ? Si1C C2C 1.838(7) . ? Si1C C1C 1.859(6) . ? Si1C C3C 1.866(7) . ? Si2C N2C 1.749(4) . ? Si2C C16C 1.846(6) . ? Si2C C15C 1.864(6) . ? Si2C C17C 1.877(7) . ? Si3C N3C 1.755(5) . ? Si3C C18C 1.832(8) . ? Si3C C19C 1.839(8) . ? Si3C C20C 1.856(8) . ? Si4C N4C 1.753(5) . ? Si4C C32C 1.827(7) . ? Si4C C34C 1.851(7) . ? Si4C C33C 1.862(6) . ? N1C C4C 1.342(7) . ? N2C C4C 1.347(6) . ? N3C C21C 1.344(7) . ? N4C C21C 1.339(7) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C1C H1C3 0.9700 . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C2C H2C3 0.9700 . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C3C H3C3 0.9700 . ? C4C C5C 1.491(8) . ? C5C C6C 1.367(8) . ? C5C C10C 1.367(7) . ? C6C C7C 1.375(8) . ? C6C H6C 0.9400 . ? C7C C8C 1.380(8) . ? C7C H7C 0.9400 . ? C8C C9C 1.397(8) . ? C8C C11C 1.494(8) . ? C9C C10C 1.400(8) . ? C9C H9C 0.9400 . ? C10C H10C 0.9400 . ? C15C H15G 0.9700 . ? C15C H15H 0.9700 . ? C15C H15I 0.9700 . ? C16C H16G 0.9700 . ? C16C H16H 0.9700 . ? C16C H16I 0.9700 . ? C17C H17G 0.9700 . ? C17C H17H 0.9700 . ? C17C H17I 0.9700 . ? C18C H18G 0.9700 . ? C18C H18H 0.9700 . ? C18C H18I 0.9700 . ? C19C H19G 0.9700 . ? C19C H19H 0.9700 . ? C19C H19I 0.9700 . ? C20C H20G 0.9700 . ? C20C H20H 0.9700 . ? C20C H20I 0.9700 . ? C21C C22C 1.486(8) . ? C22C C27C 1.372(8) . ? C22C C23C 1.387(8) . ? C23C C24C 1.369(8) . ? C23C H23C 0.9400 . ? C24C C25C 1.381(8) . ? C24C H24C 0.9400 . ? C25C C26C 1.395(8) . ? C25C C28C 1.510(8) . ? C26C C27C 1.390(8) . ? C26C H26C 0.9400 . ? C27C H27C 0.9400 . ? C32C H32G 0.9700 . ? C32C H32H 0.9700 . ? C32C H32I 0.9700 . ? C33C H33G 0.9700 . ? C33C H33H 0.9700 . ? C33C H33I 0.9700 . ? C34C H34G 0.9700 . ? C34C H34H 0.9700 . ? C34C H34I 0.9700 . ? C11A C12A 1.398(8) . ? C11A H11X 0.9800 . ? C11A H11Y 0.9800 . ? C12A C13A 1.555(9) . ? C12A H12X 0.9800 . ? C12A H12Y 0.9800 . ? C13A C14A 1.454(8) . ? C13A H13X 0.9800 . ? C13A H13Y 0.9800 . ? C14A H14X 0.9700 . ? C14A H14Y 0.9700 . ? C14A H14Z 0.9700 . ? C28A C29A 1.5264 . ? C28A H28X 0.9800 . ? C28A H28Y 0.9800 . ? C29A C30A 1.5254 . ? C29A H29X 0.9800 . ? C29A H29Y 0.9800 . ? C30A C31A 1.5228 . ? C30A H30X 0.9800 . ? C30A H30Y 0.9800 . ? C31A H31X 0.9700 . ? C31A H31Y 0.9700 . ? C31A H31Z 0.9700 . ? C11B C12B 1.347(8) . ? C11B H11U 0.9800 . ? C11B H11V 0.9800 . ? C12B C13B 1.525(9) . ? C12B H12U 0.9800 . ? C12B H12V 0.9800 . ? C13B C14B 1.415(8) . ? C13B H13U 0.9800 . ? C13B H13V 0.9800 . ? C14B H14U 0.9700 . ? C14B H14V 0.9700 . ? C14B H14W 0.9700 . ? C28B C29B 1.5264 . ? C28B H28U 0.9800 . ? C28B H28V 0.9800 . ? C29B C30B 1.5254 . ? C29B H29U 0.9800 . ? C29B H29V 0.9800 . ? C30B C31B 1.5228 . ? C30B H30U 0.9800 . ? C30B H30V 0.9800 . ? C31B H31U 0.9700 . ? C31B H31V 0.9700 . ? C31B H31W 0.9700 . ? C11C C12C 1.473(8) . ? C11C H11P 0.9800 . ? C11C H11R 0.9800 . ? C12C C13C 1.365(10) . ? C12C H12P 0.9800 . ? C12C H12R 0.9800 . ? C13C C14C 1.499(9) . ? C13C H13P 0.9800 . ? C13C H13R 0.9800 . ? C14C H14P 0.9700 . ? C14C H14R 0.9700 . ? C14C H14S 0.9700 . ? C28C C29C 1.487(7) . ? C28C H28M 0.9800 . ? C28C H28N 0.9800 . ? C29C C30C 1.517(8) . ? C29C H29M 0.9800 . ? C29C H29N 0.9800 . ? C30C C31C 1.429(9) . ? C30C H30M 0.9800 . ? C30C H30N 0.9800 . ? C31C H31M 0.9700 . ? C31C H31N 0.9700 . ? C31C H31O 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Zr1A N2A 61.63(16) . . ? N1A Zr1A N3A 115.35(18) . . ? N2A Zr1A N3A 158.17(18) . . ? N1A Zr1A N4A 90.35(18) . . ? N2A Zr1A N4A 96.76(18) . . ? N3A Zr1A N4A 61.41(17) . . ? N1A Zr1A Cl2A 149.38(14) . . ? N2A Zr1A Cl2A 88.81(13) . . ? N3A Zr1A Cl2A 95.03(13) . . ? N4A Zr1A Cl2A 101.64(12) . . ? N1A Zr1A Cl1A 87.18(12) . . ? N2A Zr1A Cl1A 109.59(13) . . ? N3A Zr1A Cl1A 91.37(13) . . ? N4A Zr1A Cl1A 148.33(14) . . ? Cl2A Zr1A Cl1A 96.30(7) . . ? N1A Zr1A C4A 31.27(16) . . ? N2A Zr1A C4A 31.15(15) . . ? N3A Zr1A C4A 145.15(19) . . ? N4A Zr1A C4A 99.32(18) . . ? Cl2A Zr1A C4A 118.22(14) . . ? Cl1A Zr1A C4A 94.79(13) . . ? N1A Zr1A C21A 104.73(18) . . ? N2A Zr1A C21A 127.59(19) . . ? N3A Zr1A C21A 30.58(16) . . ? N4A Zr1A C21A 30.83(17) . . ? Cl2A Zr1A C21A 99.62(13) . . ? Cl1A Zr1A C21A 120.49(15) . . ? C4A Zr1A C21A 124.98(19) . . ? N1A Si1A C2A 111.8(3) . . ? N1A Si1A C3A 110.7(3) . . ? C2A Si1A C3A 110.9(3) . . ? N1A Si1A C1A 104.6(3) . . ? C2A Si1A C1A 109.9(3) . . ? C3A Si1A C1A 108.8(4) . . ? N2A Si2A C15A 109.4(3) . . ? N2A Si2A C16A 107.2(3) . . ? C15A Si2A C16A 111.1(3) . . ? N2A Si2A C17A 112.1(3) . . ? C15A Si2A C17A 111.5(4) . . ? C16A Si2A C17A 105.6(3) . . ? N3A Si3A C20A 109.3(3) . . ? N3A Si3A C19A 107.0(3) . . ? C20A Si3A C19A 110.3(4) . . ? N3A Si3A C18A 114.9(3) . . ? C20A Si3A C18A 108.1(3) . . ? C19A Si3A C18A 107.3(3) . . ? N4A Si4A C33A 107.2(3) . . ? N4A Si4A C32A 109.1(3) . . ? C33A Si4A C32A 110.6(3) . . ? N4A Si4A C34A 113.1(3) . . ? C33A Si4A C34A 107.2(3) . . ? C32A Si4A C34A 109.6(3) . . ? C4A N1A Si1A 130.9(4) . . ? C4A N1A Zr1A 90.2(4) . . ? Si1A N1A Zr1A 133.6(3) . . ? C4A N2A Si2A 130.3(4) . . ? C4A N2A Zr1A 90.0(4) . . ? Si2A N2A Zr1A 138.4(3) . . ? C21A N3A Si3A 131.2(5) . . ? C21A N3A Zr1A 91.5(4) . . ? Si3A N3A Zr1A 136.2(3) . . ? C21A N4A Si4A 128.5(5) . . ? C21A N4A Zr1A 91.2(4) . . ? Si4A N4A Zr1A 140.3(3) . . ? Si1A C1A H1A1 109.5 . . ? Si1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Si1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? Si1A C2A H2A1 109.5 . . ? Si1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? Si1A C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? Si1A C3A H3A1 109.5 . . ? Si1A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? Si1A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? N2A C4A N1A 115.3(6) . . ? N2A C4A C5A 122.9(5) . . ? N1A C4A C5A 121.6(5) . . ? N2A C4A Zr1A 58.9(3) . . ? N1A C4A Zr1A 58.6(3) . . ? C5A C4A Zr1A 162.6(4) . . ? C10A C5A C6A 118.6(6) . . ? C10A C5A C4A 120.0(6) . . ? C6A C5A C4A 121.3(6) . . ? C5A C6A C7A 121.1(7) . . ? C5A C6A H6A 119.4 . . ? C7A C6A H6A 119.4 . . ? C8A C7A C6A 120.7(7) . . ? C8A C7A H7A 119.7 . . ? C6A C7A H7A 119.7 . . ? C7A C8A C9A 118.5(7) . . ? C7A C8A C11A 122.4(8) . . ? C9A C8A C11A 119.1(9) . . ? C8A C9A C10A 120.4(7) . . ? C8A C9A H9A 119.8 . . ? C10A C9A H9A 119.8 . . ? C5A C10A C9A 120.6(7) . . ? C5A C10A H10A 119.7 . . ? C9A C10A H10A 119.7 . . ? Si2A C15A H15A 109.5 . . ? Si2A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? Si2A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? Si2A C16A H16A 109.5 . . ? Si2A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? Si2A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? Si2A C17A H17A 109.5 . . ? Si2A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? Si2A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? Si3A C18A H18A 109.5 . . ? Si3A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? Si3A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? Si3A C19A H19A 109.5 . . ? Si3A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? Si3A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? Si3A C20A H20A 109.5 . . ? Si3A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? Si3A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? N3A C21A N4A 115.9(6) . . ? N3A C21A C22A 122.5(6) . . ? N4A C21A C22A 121.5(6) . . ? N3A C21A Zr1A 57.9(3) . . ? N4A C21A Zr1A 58.0(3) . . ? C22A C21A Zr1A 178.2(4) . . ? C23A C22A C27A 119.4(7) . . ? C23A C22A C21A 120.1(6) . . ? C27A C22A C21A 120.5(6) . . ? C22A C23A C24A 119.9(7) . . ? C22A C23A H23A 120.1 . . ? C24A C23A H23A 120.1 . . ? C23A C24A C25A 120.2(7) . . ? C23A C24A H24A 119.9 . . ? C25A C24A H24A 119.9 . . ? C26A C25A C24A 118.9(7) . . ? C26A C25A C28A 121.1(7) . . ? C24A C25A C28A 119.9(8) . . ? C25A C26A C27A 121.3(7) . . ? C25A C26A H26A 119.4 . . ? C27A C26A H26A 119.4 . . ? C26A C27A C22A 120.3(7) . . ? C26A C27A H27A 119.9 . . ? C22A C27A H27A 119.9 . . ? Si4A C32A H32A 109.5 . . ? Si4A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? Si4A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? Si4A C33A H33A 109.5 . . ? Si4A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? Si4A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? Si4A C34A H34A 109.5 . . ? Si4A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? Si4A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? N1B Zr1B N3B 114.76(17) . . ? N1B Zr1B N2B 61.69(15) . . ? N3B Zr1B N2B 160.52(17) . . ? N1B Zr1B N4B 90.04(16) . . ? N3B Zr1B N4B 61.34(16) . . ? N2B Zr1B N4B 99.18(16) . . ? N1B Zr1B Cl1B 87.72(12) . . ? N3B Zr1B Cl1B 90.93(13) . . ? N2B Zr1B Cl1B 107.65(12) . . ? N4B Zr1B Cl1B 148.03(12) . . ? N1B Zr1B Cl2B 150.01(13) . . ? N3B Zr1B Cl2B 94.67(13) . . ? N2B Zr1B Cl2B 88.67(12) . . ? N4B Zr1B Cl2B 99.81(12) . . ? Cl1B Zr1B Cl2B 97.90(7) . . ? N1B Zr1B C4B 31.12(16) . . ? N3B Zr1B C4B 145.06(18) . . ? N2B Zr1B C4B 31.46(15) . . ? N4B Zr1B C4B 100.80(17) . . ? Cl1B Zr1B C4B 93.55(13) . . ? Cl2B Zr1B C4B 118.89(14) . . ? N1B Zr1B C21B 104.04(17) . . ? N3B Zr1B C21B 30.83(16) . . ? N2B Zr1B C21B 129.68(18) . . ? N4B Zr1B C21B 30.51(15) . . ? Cl1B Zr1B C21B 120.32(14) . . ? Cl2B Zr1B C21B 98.44(12) . . ? C4B Zr1B C21B 125.70(19) . . ? N1B Si1B C3B 104.0(3) . . ? N1B Si1B C2B 111.9(3) . . ? C3B Si1B C2B 109.6(4) . . ? N1B Si1B C1B 110.7(3) . . ? C3B Si1B C1B 109.1(4) . . ? C2B Si1B C1B 111.2(3) . . ? N2B Si2B C15B 105.9(3) . . ? N2B Si2B C16B 108.7(3) . . ? C15B Si2B C16B 111.6(3) . . ? N2B Si2B C17B 113.7(3) . . ? C15B Si2B C17B 107.1(3) . . ? C16B Si2B C17B 109.8(3) . . ? N3B Si3B C20B 114.4(3) . . ? N3B Si3B C18B 108.3(3) . . ? C20B Si3B C18B 109.5(3) . . ? N3B Si3B C19B 106.1(3) . . ? C20B Si3B C19B 107.0(4) . . ? C18B Si3B C19B 111.5(3) . . ? N4B Si4B C33B 106.9(3) . . ? N4B Si4B C34B 109.6(3) . . ? C33B Si4B C34B 109.6(3) . . ? N4B Si4B C32B 113.9(3) . . ? C33B Si4B C32B 107.4(3) . . ? C34B Si4B C32B 109.3(3) . . ? C4B N1B Si1B 130.0(4) . . ? C4B N1B Zr1B 90.8(3) . . ? Si1B N1B Zr1B 134.6(2) . . ? C4B N2B Si2B 131.0(4) . . ? C4B N2B Zr1B 89.4(3) . . ? Si2B N2B Zr1B 138.0(2) . . ? C21B N3B Si3B 131.4(4) . . ? C21B N3B Zr1B 91.3(3) . . ? Si3B N3B Zr1B 135.9(3) . . ? C21B N4B Si4B 129.1(4) . . ? C21B N4B Zr1B 90.6(4) . . ? Si4B N4B Zr1B 140.2(3) . . ? Si1B C1B H1B1 109.5 . . ? Si1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? Si1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? Si1B C2B H2B1 109.5 . . ? Si1B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? Si1B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? Si1B C3B H3B1 109.5 . . ? Si1B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? Si1B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? N1B C4B N2B 114.9(5) . . ? N1B C4B C5B 123.9(5) . . ? N2B C4B C5B 121.2(5) . . ? N1B C4B Zr1B 58.1(3) . . ? N2B C4B Zr1B 59.2(3) . . ? C5B C4B Zr1B 164.0(4) . . ? C6B C5B C10B 120.3(6) . . ? C6B C5B C4B 120.8(6) . . ? C10B C5B C4B 119.0(6) . . ? C5B C6B C7B 120.4(7) . . ? C5B C6B H6B 119.8 . . ? C7B C6B H6B 119.8 . . ? C8B C7B C6B 120.7(7) . . ? C8B C7B H7B 119.6 . . ? C6B C7B H7B 119.6 . . ? C7B C8B C9B 118.3(7) . . ? C7B C8B C11B 120.0(9) . . ? C9B C8B C11B 121.5(9) . . ? C8B C9B C10B 121.5(7) . . ? C8B C9B H9B 119.3 . . ? C10B C9B H9B 119.3 . . ? C5B C10B C9B 118.7(6) . . ? C5B C10B H10B 120.6 . . ? C9B C10B H10B 120.6 . . ? Si2B C15B H15D 109.5 . . ? Si2B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? Si2B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? Si2B C16B H16D 109.5 . . ? Si2B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? Si2B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? Si2B C17B H17D 109.5 . . ? Si2B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? Si2B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? Si3B C18B H18D 109.5 . . ? Si3B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? Si3B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? Si3B C19B H19D 109.5 . . ? Si3B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? Si3B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? Si3B C20B H20D 109.5 . . ? Si3B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? Si3B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? N4B C21B N3B 116.8(6) . . ? N4B C21B C22B 121.5(5) . . ? N3B C21B C22B 121.7(5) . . ? N4B C21B Zr1B 58.9(3) . . ? N3B C21B Zr1B 57.9(3) . . ? C22B C21B Zr1B 179.0(4) . . ? C27B C22B C23B 120.0(6) . . ? C27B C22B C21B 121.3(5) . . ? C23B C22B C21B 118.7(5) . . ? C24B C23B C22B 119.3(6) . . ? C24B C23B H23B 120.4 . . ? C22B C23B H23B 120.4 . . ? C23B C24B C25B 122.0(7) . . ? C23B C24B H24B 119.0 . . ? C25B C24B H24B 119.0 . . ? C24B C25B C26B 118.1(7) . . ? C24B C25B C28B 125.6(7) . . ? C26B C25B C28B 116.0(7) . . ? C27B C26B C25B 120.1(6) . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C22B C27B C26B 120.5(6) . . ? C22B C27B H27B 119.8 . . ? C26B C27B H27B 119.8 . . ? Si4B C32B H32D 109.5 . . ? Si4B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? Si4B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? Si4B C33B H33D 109.5 . . ? Si4B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? Si4B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? Si4B C34B H34D 109.5 . . ? Si4B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? Si4B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? N3C Zr1C N1C 109.88(18) . . ? N3C Zr1C N4C 61.70(17) . . ? N1C Zr1C N4C 159.99(18) . . ? N3C Zr1C N2C 89.83(17) . . ? N1C Zr1C N2C 61.03(16) . . ? N4C Zr1C N2C 99.72(16) . . ? N3C Zr1C Cl2C 151.76(14) . . ? N1C Zr1C Cl2C 97.67(12) . . ? N4C Zr1C Cl2C 90.22(13) . . ? N2C Zr1C Cl2C 98.43(12) . . ? N3C Zr1C Cl1C 89.55(13) . . ? N1C Zr1C Cl1C 91.87(13) . . ? N4C Zr1C Cl1C 105.65(12) . . ? N2C Zr1C Cl1C 150.75(12) . . ? Cl2C Zr1C Cl1C 95.82(8) . . ? N3C Zr1C C21C 31.31(16) . . ? N1C Zr1C C21C 140.51(19) . . ? N4C Zr1C C21C 31.16(16) . . ? N2C Zr1C C21C 100.62(17) . . ? Cl2C Zr1C C21C 120.48(15) . . ? Cl1C Zr1C C21C 93.85(13) . . ? N3C Zr1C C4C 102.37(18) . . ? N1C Zr1C C4C 30.46(15) . . ? N4C Zr1C C4C 130.25(17) . . ? N2C Zr1C C4C 30.60(15) . . ? Cl2C Zr1C C4C 98.22(12) . . ? Cl1C Zr1C C4C 121.88(13) . . ? C21C Zr1C C4C 124.57(18) . . ? N1C Si1C C2C 106.5(3) . . ? N1C Si1C C1C 107.1(3) . . ? C2C Si1C C1C 112.5(3) . . ? N1C Si1C C3C 115.3(3) . . ? C2C Si1C C3C 107.9(4) . . ? C1C Si1C C3C 107.7(4) . . ? N2C Si2C C16C 107.2(3) . . ? N2C Si2C C15C 109.2(2) . . ? C16C Si2C C15C 110.9(3) . . ? N2C Si2C C17C 112.6(3) . . ? C16C Si2C C17C 107.2(3) . . ? C15C Si2C C17C 109.8(3) . . ? N3C Si3C C18C 104.6(3) . . ? N3C Si3C C19C 109.3(3) . . ? C18C Si3C C19C 110.1(5) . . ? N3C Si3C C20C 113.6(3) . . ? C18C Si3C C20C 108.3(4) . . ? C19C Si3C C20C 110.8(4) . . ? N4C Si4C C32C 109.1(3) . . ? N4C Si4C C34C 113.0(3) . . ? C32C Si4C C34C 110.4(4) . . ? N4C Si4C C33C 106.7(3) . . ? C32C Si4C C33C 110.9(3) . . ? C34C Si4C C33C 106.7(4) . . ? C4C N1C Si1C 130.7(4) . . ? C4C N1C Zr1C 92.5(3) . . ? Si1C N1C Zr1C 135.1(3) . . ? C4C N2C Si2C 128.8(4) . . ? C4C N2C Zr1C 91.9(3) . . ? Si2C N2C Zr1C 139.4(3) . . ? C21C N3C Si3C 130.5(4) . . ? C21C N3C Zr1C 90.5(4) . . ? Si3C N3C Zr1C 135.6(3) . . ? C21C N4C Si4C 130.8(4) . . ? C21C N4C Zr1C 89.7(4) . . ? Si4C N4C Zr1C 137.5(3) . . ? Si1C C1C H1C1 109.5 . . ? Si1C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? Si1C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? Si1C C2C H2C1 109.5 . . ? Si1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? Si1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? Si1C C3C H3C1 109.5 . . ? Si1C C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? Si1C C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? N1C C4C N2C 114.5(5) . . ? N1C C4C C5C 122.9(5) . . ? N2C C4C C5C 122.6(5) . . ? N1C C4C Zr1C 57.0(3) . . ? N2C C4C Zr1C 57.5(3) . . ? C5C C4C Zr1C 177.4(4) . . ? C6C C5C C10C 120.1(6) . . ? C6C C5C C4C 120.5(5) . . ? C10C C5C C4C 119.3(5) . . ? C5C C6C C7C 120.6(6) . . ? C5C C6C H6C 119.7 . . ? C7C C6C H6C 119.7 . . ? C6C C7C C8C 121.6(6) . . ? C6C C7C H7C 119.2 . . ? C8C C7C H7C 119.2 . . ? C7C C8C C9C 117.2(6) . . ? C7C C8C C11C 121.6(7) . . ? C9C C8C C11C 121.2(7) . . ? C8C C9C C10C 121.1(6) . . ? C8C C9C H9C 119.4 . . ? C10C C9C H9C 119.4 . . ? C5C C10C C9C 119.4(6) . . ? C5C C10C H10C 120.3 . . ? C9C C10C H10C 120.3 . . ? Si2C C15C H15G 109.5 . . ? Si2C C15C H15H 109.5 . . ? H15G C15C H15H 109.5 . . ? Si2C C15C H15I 109.5 . . ? H15G C15C H15I 109.5 . . ? H15H C15C H15I 109.5 . . ? Si2C C16C H16G 109.5 . . ? Si2C C16C H16H 109.5 . . ? H16G C16C H16H 109.5 . . ? Si2C C16C H16I 109.5 . . ? H16G C16C H16I 109.5 . . ? H16H C16C H16I 109.5 . . ? Si2C C17C H17G 109.5 . . ? Si2C C17C H17H 109.5 . . ? H17G C17C H17H 109.5 . . ? Si2C C17C H17I 109.5 . . ? H17G C17C H17I 109.5 . . ? H17H C17C H17I 109.5 . . ? Si3C C18C H18G 109.5 . . ? Si3C C18C H18H 109.5 . . ? H18G C18C H18H 109.5 . . ? Si3C C18C H18I 109.5 . . ? H18G C18C H18I 109.5 . . ? H18H C18C H18I 109.5 . . ? Si3C C19C H19G 109.5 . . ? Si3C C19C H19H 109.5 . . ? H19G C19C H19H 109.5 . . ? Si3C C19C H19I 109.5 . . ? H19G C19C H19I 109.5 . . ? H19H C19C H19I 109.5 . . ? Si3C C20C H20G 109.5 . . ? Si3C C20C H20H 109.5 . . ? H20G C20C H20H 109.5 . . ? Si3C C20C H20I 109.5 . . ? H20G C20C H20I 109.5 . . ? H20H C20C H20I 109.5 . . ? N4C C21C N3C 115.3(5) . . ? N4C C21C C22C 122.8(6) . . ? N3C C21C C22C 121.8(5) . . ? N4C C21C Zr1C 59.1(3) . . ? N3C C21C Zr1C 58.2(3) . . ? C22C C21C Zr1C 163.0(4) . . ? C27C C22C C23C 118.1(6) . . ? C27C C22C C21C 120.3(6) . . ? C23C C22C C21C 121.5(6) . . ? C24C C23C C22C 120.7(6) . . ? C24C C23C H23C 119.7 . . ? C22C C23C H23C 119.7 . . ? C23C C24C C25C 122.0(6) . . ? C23C C24C H24C 119.0 . . ? C25C C24C H24C 119.0 . . ? C24C C25C C26C 117.4(6) . . ? C24C C25C C28C 122.8(6) . . ? C26C C25C C28C 119.8(7) . . ? C27C C26C C25C 120.2(6) . . ? C27C C26C H26C 119.9 . . ? C25C C26C H26C 119.9 . . ? C22C C27C C26C 121.5(6) . . ? C22C C27C H27C 119.3 . . ? C26C C27C H27C 119.3 . . ? Si4C C32C H32G 109.5 . . ? Si4C C32C H32H 109.5 . . ? H32G C32C H32H 109.5 . . ? Si4C C32C H32I 109.5 . . ? H32G C32C H32I 109.5 . . ? H32H C32C H32I 109.5 . . ? Si4C C33C H33G 109.5 . . ? Si4C C33C H33H 109.5 . . ? H33G C33C H33H 109.5 . . ? Si4C C33C H33I 109.5 . . ? H33G C33C H33I 109.5 . . ? H33H C33C H33I 109.5 . . ? Si4C C34C H34G 109.5 . . ? Si4C C34C H34H 109.5 . . ? H34G C34C H34H 109.5 . . ? Si4C C34C H34I 109.5 . . ? H34G C34C H34I 109.5 . . ? H34H C34C H34I 109.5 . . ? C12A C11A C8A 116.7(7) . . ? C12A C11A H11X 108.1 . . ? C8A C11A H11X 108.1 . . ? C12A C11A H11Y 108.1 . . ? C8A C11A H11Y 108.1 . . ? H11X C11A H11Y 107.3 . . ? C11A C12A C13A 117.4(7) . . ? C11A C12A H12X 108.0 . . ? C13A C12A H12X 108.0 . . ? C11A C12A H12Y 108.0 . . ? C13A C12A H12Y 108.0 . . ? H12X C12A H12Y 107.2 . . ? C14A C13A C12A 112.6(7) . . ? C14A C13A H13X 109.1 . . ? C12A C13A H13X 109.1 . . ? C14A C13A H13Y 109.1 . . ? C12A C13A H13Y 109.1 . . ? H13X C13A H13Y 107.8 . . ? C13A C14A H14X 109.5 . . ? C13A C14A H14Y 109.5 . . ? H14X C14A H14Y 109.5 . . ? C13A C14A H14Z 109.5 . . ? H14X C14A H14Z 109.5 . . ? H14Y C14A H14Z 109.5 . . ? C25A C28A C29A 108.5(4) . . ? C25A C28A H28X 110.0 . . ? C29A C28A H28X 110.0 . . ? C25A C28A H28Y 110.0 . . ? C29A C28A H28Y 110.0 . . ? H28X C28A H28Y 108.4 . . ? C30A C29A C28A 114.4 . . ? C30A C29A H29X 108.7 . . ? C28A C29A H29X 108.7 . . ? C30A C29A H29Y 108.7 . . ? C28A C29A H29Y 108.7 . . ? H29X C29A H29Y 107.6 . . ? C31A C30A C29A 112.0 . . ? C31A C30A H30X 109.2 . . ? C29A C30A H30X 109.2 . . ? C31A C30A H30Y 109.2 . . ? C29A C30A H30Y 109.2 . . ? H30X C30A H30Y 107.9 . . ? C30A C31A H31X 109.5 . . ? C30A C31A H31Y 109.5 . . ? H31X C31A H31Y 109.5 . . ? C30A C31A H31Z 109.5 . . ? H31X C31A H31Z 109.5 . . ? H31Y C31A H31Z 109.5 . . ? C12B C11B C8B 117.0(7) . . ? C12B C11B H11U 108.0 . . ? C8B C11B H11U 108.0 . . ? C12B C11B H11V 108.0 . . ? C8B C11B H11V 108.0 . . ? H11U C11B H11V 107.3 . . ? C11B C12B C13B 119.1(7) . . ? C11B C12B H12U 107.5 . . ? C13B C12B H12U 107.5 . . ? C11B C12B H12V 107.5 . . ? C13B C12B H12V 107.5 . . ? H12U C12B H12V 107.0 . . ? C14B C13B C12B 113.9(6) . . ? C14B C13B H13U 108.8 . . ? C12B C13B H13U 108.8 . . ? C14B C13B H13V 108.8 . . ? C12B C13B H13V 108.8 . . ? H13U C13B H13V 107.7 . . ? C13B C14B H14U 109.5 . . ? C13B C14B H14V 109.5 . . ? H14U C14B H14V 109.5 . . ? C13B C14B H14W 109.5 . . ? H14U C14B H14W 109.5 . . ? H14V C14B H14W 109.5 . . ? C29B C28B C25B 125.9(4) . . ? C29B C28B H28U 105.9 . . ? C25B C28B H28U 105.9 . . ? C29B C28B H28V 105.9 . . ? C25B C28B H28V 105.9 . . ? H28U C28B H28V 106.2 . . ? C30B C29B C28B 114.4 . . ? C30B C29B H29U 108.7 . . ? C28B C29B H29U 108.7 . . ? C30B C29B H29V 108.7 . . ? C28B C29B H29V 108.7 . . ? H29U C29B H29V 107.6 . . ? C31B C30B C29B 112.0 . . ? C31B C30B H30U 109.2 . . ? C29B C30B H30U 109.2 . . ? C31B C30B H30V 109.2 . . ? C29B C30B H30V 109.2 . . ? H30U C30B H30V 107.9 . . ? C30B C31B H31U 109.5 . . ? C30B C31B H31V 109.5 . . ? H31U C31B H31V 109.5 . . ? C30B C31B H31W 109.5 . . ? H31U C31B H31W 109.5 . . ? H31V C31B H31W 109.5 . . ? C12C C11C C8C 115.7(6) . . ? C12C C11C H11P 108.3 . . ? C8C C11C H11P 108.3 . . ? C12C C11C H11R 108.3 . . ? C8C C11C H11R 108.3 . . ? H11P C11C H11R 107.4 . . ? C13C C12C C11C 124.2(9) . . ? C13C C12C H12P 106.3 . . ? C11C C12C H12P 106.3 . . ? C13C C12C H12R 106.3 . . ? C11C C12C H12R 106.3 . . ? H12P C12C H12R 106.4 . . ? C12C C13C C14C 122.6(9) . . ? C12C C13C H13P 106.7 . . ? C14C C13C H13P 106.7 . . ? C12C C13C H13R 106.7 . . ? C14C C13C H13R 106.7 . . ? H13P C13C H13R 106.6 . . ? C13C C14C H14P 109.5 . . ? C13C C14C H14R 109.5 . . ? H14P C14C H14R 109.5 . . ? C13C C14C H14S 109.5 . . ? H14P C14C H14S 109.5 . . ? H14R C14C H14S 109.5 . . ? C29C C28C C25C 114.7(6) . . ? C29C C28C H28M 108.6 . . ? C25C C28C H28M 108.6 . . ? C29C C28C H28N 108.6 . . ? C25C C28C H28N 108.6 . . ? H28M C28C H28N 107.6 . . ? C28C C29C C30C 114.0(6) . . ? C28C C29C H29M 108.8 . . ? C30C C29C H29M 108.8 . . ? C28C C29C H29N 108.8 . . ? C30C C29C H29N 108.8 . . ? H29M C29C H29N 107.6 . . ? C31C C30C C29C 115.4(7) . . ? C31C C30C H30M 108.4 . . ? C29C C30C H30M 108.4 . . ? C31C C30C H30N 108.4 . . ? C29C C30C H30N 108.4 . . ? H30M C30C H30N 107.5 . . ? C30C C31C H31M 109.5 . . ? C30C C31C H31N 109.5 . . ? H31M C31C H31N 109.5 . . ? C30C C31C H31O 109.5 . . ? H31M C31C H31O 109.5 . . ? H31N C31C H31O 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 C2A Si1A N1A C4A 52.0(6) . . . . ? C3A Si1A N1A C4A -72.1(6) . . . . ? C1A Si1A N1A C4A 170.9(5) . . . . ? C2A Si1A N1A Zr1A -94.3(4) . . . . ? C3A Si1A N1A Zr1A 141.6(4) . . . . ? C1A Si1A N1A Zr1A 24.6(5) . . . . ? N2A Zr1A N1A C4A 10.1(3) . . . . ? N3A Zr1A N1A C4A 165.8(3) . . . . ? N4A Zr1A N1A C4A 107.6(3) . . . . ? Cl2A Zr1A N1A C4A -6.4(5) . . . . ? Cl1A Zr1A N1A C4A -104.0(3) . . . . ? C21A Zr1A N1A C4A 135.2(3) . . . . ? N2A Zr1A N1A Si1A 165.3(4) . . . . ? N3A Zr1A N1A Si1A -39.0(4) . . . . ? N4A Zr1A N1A Si1A -97.2(4) . . . . ? Cl2A Zr1A N1A Si1A 148.8(2) . . . . ? Cl1A Zr1A N1A Si1A 51.2(4) . . . . ? C4A Zr1A N1A Si1A 155.2(6) . . . . ? C21A Zr1A N1A Si1A -69.6(4) . . . . ? C15A Si2A N2A C4A -95.3(6) . . . . ? C16A Si2A N2A C4A 144.2(5) . . . . ? C17A Si2A N2A C4A 28.9(6) . . . . ? C15A Si2A N2A Zr1A 67.1(5) . . . . ? C16A Si2A N2A Zr1A -53.4(5) . . . . ? C17A Si2A N2A Zr1A -168.8(4) . . . . ? N1A Zr1A N2A C4A -10.1(3) . . . . ? N3A Zr1A N2A C4A -97.8(5) . . . . ? N4A Zr1A N2A C4A -96.8(3) . . . . ? Cl2A Zr1A N2A C4A 161.6(3) . . . . ? Cl1A Zr1A N2A C4A 65.3(3) . . . . ? C21A Zr1A N2A C4A -97.2(4) . . . . ? N1A Zr1A N2A Si2A -176.8(5) . . . . ? N3A Zr1A N2A Si2A 95.5(6) . . . . ? N4A Zr1A N2A Si2A 96.5(4) . . . . ? Cl2A Zr1A N2A Si2A -5.1(4) . . . . ? Cl1A Zr1A N2A Si2A -101.3(4) . . . . ? C4A Zr1A N2A Si2A -166.6(6) . . . . ? C21A Zr1A N2A Si2A 96.2(4) . . . . ? C20A Si3A N3A C21A 112.0(6) . . . . ? C19A Si3A N3A C21A -128.7(5) . . . . ? C18A Si3A N3A C21A -9.7(6) . . . . ? C20A Si3A N3A Zr1A -83.6(4) . . . . ? C19A Si3A N3A Zr1A 35.8(5) . . . . ? C18A Si3A N3A Zr1A 154.8(4) . . . . ? N1A Zr1A N3A C21A -75.6(3) . . . . ? N2A Zr1A N3A C21A 1.0(6) . . . . ? N4A Zr1A N3A C21A -0.1(3) . . . . ? Cl2A Zr1A N3A C21A 100.4(3) . . . . ? Cl1A Zr1A N3A C21A -163.1(3) . . . . ? C4A Zr1A N3A C21A -62.7(4) . . . . ? N1A Zr1A N3A Si3A 116.0(4) . . . . ? N2A Zr1A N3A Si3A -167.4(3) . . . . ? N4A Zr1A N3A Si3A -168.5(4) . . . . ? Cl2A Zr1A N3A Si3A -68.0(3) . . . . ? Cl1A Zr1A N3A Si3A 28.5(3) . . . . ? C4A Zr1A N3A Si3A 128.9(4) . . . . ? C21A Zr1A N3A Si3A -168.4(6) . . . . ? C33A Si4A N4A C21A -155.4(5) . . . . ? C32A Si4A N4A C21A 84.8(5) . . . . ? C34A Si4A N4A C21A -37.4(6) . . . . ? C33A Si4A N4A Zr1A 23.5(5) . . . . ? C32A Si4A N4A Zr1A -96.3(4) . . . . ? C34A Si4A N4A Zr1A 141.5(4) . . . . ? N1A Zr1A N4A C21A 119.1(3) . . . . ? N2A Zr1A N4A C21A -179.5(3) . . . . ? N3A Zr1A N4A C21A 0.1(3) . . . . ? Cl2A Zr1A N4A C21A -89.3(3) . . . . ? Cl1A Zr1A N4A C21A 33.9(4) . . . . ? C4A Zr1A N4A C21A 149.2(3) . . . . ? N1A Zr1A N4A Si4A -60.1(4) . . . . ? N2A Zr1A N4A Si4A 1.4(4) . . . . ? N3A Zr1A N4A Si4A -179.0(5) . . . . ? Cl2A Zr1A N4A Si4A 91.6(4) . . . . ? Cl1A Zr1A N4A Si4A -145.2(3) . . . . ? C4A Zr1A N4A Si4A -30.0(4) . . . . ? C21A Zr1A N4A Si4A -179.1(6) . . . . ? Si2A N2A C4A N1A -175.3(4) . . . . ? Zr1A N2A C4A N1A 16.3(5) . . . . ? Si2A N2A C4A C5A 8.8(8) . . . . ? Zr1A N2A C4A C5A -159.6(5) . . . . ? Si2A N2A C4A Zr1A 168.4(5) . . . . ? Si1A N1A C4A N2A -172.7(4) . . . . ? Zr1A N1A C4A N2A -16.4(5) . . . . ? Si1A N1A C4A C5A 3.3(8) . . . . ? Zr1A N1A C4A C5A 159.6(5) . . . . ? Si1A N1A C4A Zr1A -156.3(5) . . . . ? N1A Zr1A C4A N2A 162.7(5) . . . . ? N3A Zr1A C4A N2A 139.9(3) . . . . ? N4A Zr1A C4A N2A 87.7(3) . . . . ? Cl2A Zr1A C4A N2A -21.0(4) . . . . ? Cl1A Zr1A C4A N2A -120.8(3) . . . . ? C21A Zr1A C4A N2A 106.4(4) . . . . ? N2A Zr1A C4A N1A -162.7(5) . . . . ? N3A Zr1A C4A N1A -22.8(5) . . . . ? N4A Zr1A C4A N1A -75.0(3) . . . . ? Cl2A Zr1A C4A N1A 176.3(3) . . . . ? Cl1A Zr1A C4A N1A 76.5(3) . . . . ? C21A Zr1A C4A N1A -56.3(4) . . . . ? N1A Zr1A C4A C5A -96.0(15) . . . . ? N2A Zr1A C4A C5A 101.3(15) . . . . ? N3A Zr1A C4A C5A -118.8(14) . . . . ? N4A Zr1A C4A C5A -171.1(14) . . . . ? Cl2A Zr1A C4A C5A 80.3(14) . . . . ? Cl1A Zr1A C4A C5A -19.5(14) . . . . ? C21A Zr1A C4A C5A -152.3(14) . . . . ? N2A C4A C5A C10A 70.1(7) . . . . ? N1A C4A C5A C10A -105.6(7) . . . . ? Zr1A C4A C5A C10A -20.3(17) . . . . ? N2A C4A C5A C6A -106.8(7) . . . . ? N1A C4A C5A C6A 77.6(7) . . . . ? Zr1A C4A C5A C6A 162.8(12) . . . . ? C10A C5A C6A C7A -0.9(10) . . . . ? C4A C5A C6A C7A 176.0(6) . . . . ? C5A C6A C7A C8A -1.4(11) . . . . ? C6A C7A C8A C9A 4.5(11) . . . . ? C6A C7A C8A C11A -174.5(7) . . . . ? C7A C8A C9A C10A -5.3(11) . . . . ? C11A C8A C9A C10A 173.8(6) . . . . ? C6A C5A C10A C9A 0.0(9) . . . . ? C4A C5A C10A C9A -176.9(5) . . . . ? C8A C9A C10A C5A 3.1(10) . . . . ? Si3A N3A C21A N4A 169.5(4) . . . . ? Zr1A N3A C21A N4A 0.2(5) . . . . ? Si3A N3A C21A C22A -12.7(8) . . . . ? Zr1A N3A C21A C22A 178.0(5) . . . . ? Si3A N3A C21A Zr1A 169.3(5) . . . . ? Si4A N4A C21A N3A 179.1(4) . . . . ? Zr1A N4A C21A N3A -0.2(5) . . . . ? Si4A N4A C21A C22A 1.3(8) . . . . ? Zr1A N4A C21A C22A -178.0(5) . . . . ? Si4A N4A C21A Zr1A 179.3(5) . . . . ? N1A Zr1A C21A N3A 115.2(3) . . . . ? N2A Zr1A C21A N3A -179.5(3) . . . . ? N4A Zr1A C21A N3A 179.8(5) . . . . ? Cl2A Zr1A C21A N3A -83.6(3) . . . . ? Cl1A Zr1A C21A N3A 19.7(4) . . . . ? C4A Zr1A C21A N3A 141.7(3) . . . . ? N1A Zr1A C21A N4A -64.7(3) . . . . ? N2A Zr1A C21A N4A 0.7(4) . . . . ? N3A Zr1A C21A N4A -179.8(5) . . . . ? Cl2A Zr1A C21A N4A 96.6(3) . . . . ? Cl1A Zr1A C21A N4A -160.1(3) . . . . ? C4A Zr1A C21A N4A -38.1(4) . . . . ? N1A Zr1A C21A C22A 10(17) . . . . ? N2A Zr1A C21A C22A 76(17) . . . . ? N3A Zr1A C21A C22A -105(17) . . . . ? N4A Zr1A C21A C22A 75(17) . . . . ? Cl2A Zr1A C21A C22A 172(100) . . . . ? Cl1A Zr1A C21A C22A -85(17) . . . . ? C4A Zr1A C21A C22A 37(17) . . . . ? N3A C21A C22A C23A -73.2(9) . . . . ? N4A C21A C22A C23A 104.5(8) . . . . ? Zr1A C21A C22A C23A 31(17) . . . . ? N3A C21A C22A C27A 105.8(7) . . . . ? N4A C21A C22A C27A -76.5(8) . . . . ? Zr1A C21A C22A C27A -150(17) . . . . ? C27A C22A C23A C24A 1.8(12) . . . . ? C21A C22A C23A C24A -179.2(8) . . . . ? C22A C23A C24A C25A -1.2(14) . . . . ? C23A C24A C25A C26A -1.2(14) . . . . ? C23A C24A C25A C28A 175.8(8) . . . . ? C24A C25A C26A C27A 3.1(13) . . . . ? C28A C25A C26A C27A -173.9(7) . . . . ? C25A C26A C27A C22A -2.6(12) . . . . ? C23A C22A C27A C26A 0.1(10) . . . . ? C21A C22A C27A C26A -178.9(6) . . . . ? C3B Si1B N1B C4B 176.8(6) . . . . ? C2B Si1B N1B C4B 58.5(6) . . . . ? C1B Si1B N1B C4B -66.2(6) . . . . ? C3B Si1B N1B Zr1B 27.9(5) . . . . ? C2B Si1B N1B Zr1B -90.4(4) . . . . ? C1B Si1B N1B Zr1B 145.0(4) . . . . ? N3B Zr1B N1B C4B 169.3(3) . . . . ? N2B Zr1B N1B C4B 10.8(3) . . . . ? N4B Zr1B N1B C4B 111.2(3) . . . . ? Cl1B Zr1B N1B C4B -100.7(3) . . . . ? Cl2B Zr1B N1B C4B 1.2(5) . . . . ? C21B Zr1B N1B C4B 138.6(3) . . . . ? N3B Zr1B N1B Si1B -34.0(4) . . . . ? N2B Zr1B N1B Si1B 167.5(4) . . . . ? N4B Zr1B N1B Si1B -92.1(4) . . . . ? Cl1B Zr1B N1B Si1B 56.0(3) . . . . ? Cl2B Zr1B N1B Si1B 157.9(2) . . . . ? C4B Zr1B N1B Si1B 156.7(6) . . . . ? C21B Zr1B N1B Si1B -64.7(4) . . . . ? C15B Si2B N2B C4B 140.5(5) . . . . ? C16B Si2B N2B C4B -99.4(5) . . . . ? C17B Si2B N2B C4B 23.2(6) . . . . ? C15B Si2B N2B Zr1B -58.9(4) . . . . ? C16B Si2B N2B Zr1B 61.2(4) . . . . ? C17B Si2B N2B Zr1B -176.2(4) . . . . ? N1B Zr1B N2B C4B -10.7(3) . . . . ? N3B Zr1B N2B C4B -95.1(6) . . . . ? N4B Zr1B N2B C4B -95.7(3) . . . . ? Cl1B Zr1B N2B C4B 66.7(3) . . . . ? Cl2B Zr1B N2B C4B 164.6(3) . . . . ? C21B Zr1B N2B C4B -95.6(3) . . . . ? N1B Zr1B N2B Si2B -176.2(4) . . . . ? N3B Zr1B N2B Si2B 99.4(6) . . . . ? N4B Zr1B N2B Si2B 98.8(4) . . . . ? Cl1B Zr1B N2B Si2B -98.8(4) . . . . ? Cl2B Zr1B N2B Si2B -0.9(4) . . . . ? C4B Zr1B N2B Si2B -165.5(6) . . . . ? C21B Zr1B N2B Si2B 98.9(4) . . . . ? C20B Si3B N3B C21B -13.6(6) . . . . ? C18B Si3B N3B C21B 108.8(5) . . . . ? C19B Si3B N3B C21B -131.4(5) . . . . ? C20B Si3B N3B Zr1B 148.9(4) . . . . ? C18B Si3B N3B Zr1B -88.6(4) . . . . ? C19B Si3B N3B Zr1B 31.2(4) . . . . ? N1B Zr1B N3B C21B -75.4(3) . . . . ? N2B Zr1B N3B C21B -0.6(7) . . . . ? N4B Zr1B N3B C21B 0.0(3) . . . . ? Cl1B Zr1B N3B C21B -163.3(3) . . . . ? Cl2B Zr1B N3B C21B 98.7(3) . . . . ? C4B Zr1B N3B C21B -65.8(4) . . . . ? N1B Zr1B N3B Si3B 117.6(3) . . . . ? N2B Zr1B N3B Si3B -167.6(4) . . . . ? N4B Zr1B N3B Si3B -167.0(4) . . . . ? Cl1B Zr1B N3B Si3B 29.6(3) . . . . ? Cl2B Zr1B N3B Si3B -68.4(3) . . . . ? C4B Zr1B N3B Si3B 127.2(4) . . . . ? C21B Zr1B N3B Si3B -167.0(6) . . . . ? C33B Si4B N4B C21B -153.7(5) . . . . ? C34B Si4B N4B C21B 87.6(5) . . . . ? C32B Si4B N4B C21B -35.2(6) . . . . ? C33B Si4B N4B Zr1B 23.6(5) . . . . ? C34B Si4B N4B Zr1B -95.1(4) . . . . ? C32B Si4B N4B Zr1B 142.2(4) . . . . ? N1B Zr1B N4B C21B 118.5(3) . . . . ? N3B Zr1B N4B C21B 0.0(3) . . . . ? N2B Zr1B N4B C21B 179.8(3) . . . . ? Cl1B Zr1B N4B C21B 32.7(4) . . . . ? Cl2B Zr1B N4B C21B -90.0(3) . . . . ? C4B Zr1B N4B C21B 147.9(3) . . . . ? N1B Zr1B N4B Si4B -59.5(4) . . . . ? N3B Zr1B N4B Si4B -178.0(4) . . . . ? N2B Zr1B N4B Si4B 1.8(4) . . . . ? Cl1B Zr1B N4B Si4B -145.2(3) . . . . ? Cl2B Zr1B N4B Si4B 92.0(4) . . . . ? C4B Zr1B N4B Si4B -30.1(4) . . . . ? C21B Zr1B N4B Si4B -178.0(6) . . . . ? Si1B N1B C4B N2B -175.8(4) . . . . ? Zr1B N1B C4B N2B -17.3(5) . . . . ? Si1B N1B C4B C5B 2.7(8) . . . . ? Zr1B N1B C4B C5B 161.1(5) . . . . ? Si1B N1B C4B Zr1B -158.4(5) . . . . ? Si2B N2B C4B N1B -175.7(4) . . . . ? Zr1B N2B C4B N1B 17.1(5) . . . . ? Si2B N2B C4B C5B 5.8(8) . . . . ? Zr1B N2B C4B C5B -161.4(5) . . . . ? Si2B N2B C4B Zr1B 167.2(5) . . . . ? N3B Zr1B C4B N1B -17.1(5) . . . . ? N2B Zr1B C4B N1B -161.6(5) . . . . ? N4B Zr1B C4B N1B -71.7(3) . . . . ? Cl1B Zr1B C4B N1B 79.6(3) . . . . ? Cl2B Zr1B C4B N1B -179.3(3) . . . . ? C21B Zr1B C4B N1B -52.2(4) . . . . ? N1B Zr1B C4B N2B 161.6(5) . . . . ? N3B Zr1B C4B N2B 144.5(3) . . . . ? N4B Zr1B C4B N2B 90.0(3) . . . . ? Cl1B Zr1B C4B N2B -118.7(3) . . . . ? Cl2B Zr1B C4B N2B -17.7(4) . . . . ? C21B Zr1B C4B N2B 109.4(3) . . . . ? N1B Zr1B C4B C5B -102.2(16) . . . . ? N3B Zr1B C4B C5B -119.3(15) . . . . ? N2B Zr1B C4B C5B 96.2(16) . . . . ? N4B Zr1B C4B C5B -173.8(15) . . . . ? Cl1B Zr1B C4B C5B -22.5(15) . . . . ? Cl2B Zr1B C4B C5B 78.5(15) . . . . ? C21B Zr1B C4B C5B -154.4(15) . . . . ? N1B C4B C5B C6B 78.6(7) . . . . ? N2B C4B C5B C6B -103.0(7) . . . . ? Zr1B C4B C5B C6B 170.4(13) . . . . ? N1B C4B C5B C10B -102.6(7) . . . . ? N2B C4B C5B C10B 75.8(7) . . . . ? Zr1B C4B C5B C10B -10.7(18) . . . . ? C10B C5B C6B C7B -2.4(9) . . . . ? C4B C5B C6B C7B 176.4(6) . . . . ? C5B C6B C7B C8B 1.1(10) . . . . ? C6B C7B C8B C9B 1.2(11) . . . . ? C6B C7B C8B C11B -174.4(6) . . . . ? C7B C8B C9B C10B -2.4(11) . . . . ? C11B C8B C9B C10B 173.1(6) . . . . ? C6B C5B C10B C9B 1.3(9) . . . . ? C4B C5B C10B C9B -177.6(5) . . . . ? C8B C9B C10B C5B 1.2(10) . . . . ? Si4B N4B C21B N3B 178.3(4) . . . . ? Zr1B N4B C21B N3B 0.0(5) . . . . ? Si4B N4B C21B C22B -0.7(8) . . . . ? Zr1B N4B C21B C22B -179.0(5) . . . . ? Si4B N4B C21B Zr1B 178.3(5) . . . . ? Si3B N3B C21B N4B 167.9(4) . . . . ? Zr1B N3B C21B N4B 0.0(5) . . . . ? Si3B N3B C21B C22B -13.0(8) . . . . ? Zr1B N3B C21B C22B 179.0(5) . . . . ? Si3B N3B C21B Zr1B 168.0(5) . . . . ? N1B Zr1B C21B N4B -65.0(3) . . . . ? N3B Zr1B C21B N4B 180.0(5) . . . . ? N2B Zr1B C21B N4B -0.3(4) . . . . ? Cl1B Zr1B C21B N4B -160.6(3) . . . . ? Cl2B Zr1B C21B N4B 95.0(3) . . . . ? C4B Zr1B C21B N4B -40.1(4) . . . . ? N1B Zr1B C21B N3B 115.1(3) . . . . ? N2B Zr1B C21B N3B 179.7(3) . . . . ? N4B Zr1B C21B N3B -180.0(5) . . . . ? Cl1B Zr1B C21B N3B 19.4(3) . . . . ? Cl2B Zr1B C21B N3B -85.0(3) . . . . ? C4B Zr1B C21B N3B 140.0(3) . . . . ? N1B Zr1B C21B C22B 51(31) . . . . ? N3B Zr1B C21B C22B -64(31) . . . . ? N2B Zr1B C21B C22B 115(31) . . . . ? N4B Zr1B C21B C22B 116(31) . . . . ? Cl1B Zr1B C21B C22B -45(31) . . . . ? Cl2B Zr1B C21B C22B -149(31) . . . . ? C4B Zr1B C21B C22B 76(31) . . . . ? N4B C21B C22B C27B -73.1(8) . . . . ? N3B C21B C22B C27B 108.0(6) . . . . ? Zr1B C21B C22B C27B 172(100) . . . . ? N4B C21B C22B C23B 107.0(6) . . . . ? N3B C21B C22B C23B -72.0(8) . . . . ? Zr1B C21B C22B C23B -8(32) . . . . ? C27B C22B C23B C24B 0.7(10) . . . . ? C21B C22B C23B C24B -179.4(6) . . . . ? C22B C23B C24B C25B -1.3(11) . . . . ? C23B C24B C25B C26B 0.5(11) . . . . ? C23B C24B C25B C28B 174.9(7) . . . . ? C24B C25B C26B C27B 0.9(10) . . . . ? C28B C25B C26B C27B -174.1(6) . . . . ? C23B C22B C27B C26B 0.7(9) . . . . ? C21B C22B C27B C26B -179.2(6) . . . . ? C25B C26B C27B C22B -1.5(10) . . . . ? C2C Si1C N1C C4C 115.6(5) . . . . ? C1C Si1C N1C C4C -123.8(5) . . . . ? C3C Si1C N1C C4C -4.0(6) . . . . ? C2C Si1C N1C Zr1C -45.6(4) . . . . ? C1C Si1C N1C Zr1C 75.0(4) . . . . ? C3C Si1C N1C Zr1C -165.2(4) . . . . ? N3C Zr1C N1C C4C 80.5(3) . . . . ? N4C Zr1C N1C C4C 19.2(6) . . . . ? N2C Zr1C N1C C4C 2.2(3) . . . . ? Cl2C Zr1C N1C C4C -93.2(3) . . . . ? Cl1C Zr1C N1C C4C 170.7(3) . . . . ? C21C Zr1C N1C C4C 72.3(4) . . . . ? N3C Zr1C N1C Si1C -113.7(3) . . . . ? N4C Zr1C N1C Si1C -175.0(3) . . . . ? N2C Zr1C N1C Si1C 168.1(4) . . . . ? Cl2C Zr1C N1C Si1C 72.7(3) . . . . ? Cl1C Zr1C N1C Si1C -23.5(3) . . . . ? C21C Zr1C N1C Si1C -121.8(3) . . . . ? C4C Zr1C N1C Si1C 165.8(6) . . . . ? C16C Si2C N2C C4C 154.1(5) . . . . ? C15C Si2C N2C C4C -85.6(5) . . . . ? C17C Si2C N2C C4C 36.5(6) . . . . ? C16C Si2C N2C Zr1C -27.9(5) . . . . ? C15C Si2C N2C Zr1C 92.4(4) . . . . ? C17C Si2C N2C Zr1C -145.5(4) . . . . ? N3C Zr1C N2C C4C -115.2(3) . . . . ? N1C Zr1C N2C C4C -2.2(3) . . . . ? N4C Zr1C N2C C4C -176.4(3) . . . . ? Cl2C Zr1C N2C C4C 91.9(3) . . . . ? Cl1C Zr1C N2C C4C -26.4(4) . . . . ? C21C Zr1C N2C C4C -144.8(3) . . . . ? N3C Zr1C N2C Si2C 66.3(4) . . . . ? N1C Zr1C N2C Si2C 179.3(4) . . . . ? N4C Zr1C N2C Si2C 5.1(4) . . . . ? Cl2C Zr1C N2C Si2C -86.5(4) . . . . ? Cl1C Zr1C N2C Si2C 155.1(2) . . . . ? C21C Zr1C N2C Si2C 36.8(4) . . . . ? C4C Zr1C N2C Si2C -178.4(6) . . . . ? C18C Si3C N3C C21C 171.5(6) . . . . ? C19C Si3C N3C C21C -70.6(7) . . . . ? C20C Si3C N3C C21C 53.7(7) . . . . ? C18C Si3C N3C Zr1C -36.0(6) . . . . ? C19C Si3C N3C Zr1C 81.8(5) . . . . ? C20C Si3C N3C Zr1C -153.9(4) . . . . ? N1C Zr1C N3C C21C -170.0(3) . . . . ? N4C Zr1C N3C C21C -9.9(3) . . . . ? N2C Zr1C N3C C21C -111.1(3) . . . . ? Cl2C Zr1C N3C C21C -3.4(5) . . . . ? Cl1C Zr1C N3C C21C 98.2(3) . . . . ? C4C Zr1C N3C C21C -139.2(3) . . . . ? N1C Zr1C N3C Si3C 30.6(4) . . . . ? N4C Zr1C N3C Si3C -169.3(4) . . . . ? N2C Zr1C N3C Si3C 89.5(4) . . . . ? Cl2C Zr1C N3C Si3C -162.7(2) . . . . ? Cl1C Zr1C N3C Si3C -61.2(4) . . . . ? C21C Zr1C N3C Si3C -159.4(6) . . . . ? C4C Zr1C N3C Si3C 61.4(4) . . . . ? C32C Si4C N4C C21C 98.1(6) . . . . ? C34C Si4C N4C C21C -25.1(6) . . . . ? C33C Si4C N4C C21C -142.1(5) . . . . ? C32C Si4C N4C Zr1C -60.8(4) . . . . ? C34C Si4C N4C Zr1C 176.0(4) . . . . ? C33C Si4C N4C Zr1C 59.0(5) . . . . ? N3C Zr1C N4C C21C 10.0(3) . . . . ? N1C Zr1C N4C C21C 79.5(6) . . . . ? N2C Zr1C N4C C21C 94.5(3) . . . . ? Cl2C Zr1C N4C C21C -166.9(3) . . . . ? Cl1C Zr1C N4C C21C -70.8(3) . . . . ? C4C Zr1C N4C C21C 92.1(4) . . . . ? N3C Zr1C N4C Si4C 174.2(4) . . . . ? N1C Zr1C N4C Si4C -116.3(5) . . . . ? N2C Zr1C N4C Si4C -101.3(4) . . . . ? Cl2C Zr1C N4C Si4C -2.7(4) . . . . ? Cl1C Zr1C N4C Si4C 93.4(3) . . . . ? C21C Zr1C N4C Si4C 164.2(6) . . . . ? C4C Zr1C N4C Si4C -103.7(4) . . . . ? Si1C N1C C4C N2C -170.4(4) . . . . ? Zr1C N1C C4C N2C -3.6(5) . . . . ? Si1C N1C C4C C5C 10.1(8) . . . . ? Zr1C N1C C4C C5C 176.9(5) . . . . ? Si1C N1C C4C Zr1C -166.8(5) . . . . ? Si2C N2C C4C N1C -177.7(4) . . . . ? Zr1C N2C C4C N1C 3.6(5) . . . . ? Si2C N2C C4C C5C 1.7(8) . . . . ? Zr1C N2C C4C C5C -177.0(5) . . . . ? Si2C N2C C4C Zr1C 178.7(5) . . . . ? N3C Zr1C C4C N1C -108.3(3) . . . . ? N4C Zr1C C4C N1C -171.5(3) . . . . ? N2C Zr1C C4C N1C -176.1(5) . . . . ? Cl2C Zr1C C4C N1C 91.2(3) . . . . ? Cl1C Zr1C C4C N1C -11.0(3) . . . . ? C21C Zr1C C4C N1C -132.6(3) . . . . ? N3C Zr1C C4C N2C 67.9(3) . . . . ? N1C Zr1C C4C N2C 176.1(5) . . . . ? N4C Zr1C C4C N2C 4.6(4) . . . . ? Cl2C Zr1C C4C N2C -92.7(3) . . . . ? Cl1C Zr1C C4C N2C 165.2(3) . . . . ? C21C Zr1C C4C N2C 43.5(4) . . . . ? N3C Zr1C C4C C5C 163(10) . . . . ? N1C Zr1C C4C C5C -89(10) . . . . ? N4C Zr1C C4C C5C 100(10) . . . . ? N2C Zr1C C4C C5C 95(10) . . . . ? Cl2C Zr1C C4C C5C 2(10) . . . . ? Cl1C Zr1C C4C C5C -100(10) . . . . ? C21C Zr1C C4C C5C 139(10) . . . . ? N1C C4C C5C C6C 77.4(7) . . . . ? N2C C4C C5C C6C -102.1(6) . . . . ? Zr1C C4C C5C C6C 164(9) . . . . ? N1C C4C C5C C10C -100.6(6) . . . . ? N2C C4C C5C C10C 80.0(7) . . . . ? Zr1C C4C C5C C10C -13(10) . . . . ? C10C C5C C6C C7C -0.1(9) . . . . ? C4C C5C C6C C7C -178.1(6) . . . . ? C5C C6C C7C C8C 2.4(10) . . . . ? C6C C7C C8C C9C -2.6(9) . . . . ? C6C C7C C8C C11C 175.4(6) . . . . ? C7C C8C C9C C10C 0.7(9) . . . . ? C11C C8C C9C C10C -177.3(5) . . . . ? C6C C5C C10C C9C -1.7(9) . . . . ? C4C C5C C10C C9C 176.3(5) . . . . ? C8C C9C C10C C5C 1.4(9) . . . . ? Si4C N4C C21C N3C 178.0(4) . . . . ? Zr1C N4C C21C N3C -16.0(5) . . . . ? Si4C N4C C21C C22C -5.8(9) . . . . ? Zr1C N4C C21C C22C 160.1(5) . . . . ? Si4C N4C C21C Zr1C -165.9(5) . . . . ? Si3C N3C C21C N4C 177.3(4) . . . . ? Zr1C N3C C21C N4C 16.2(5) . . . . ? Si3C N3C C21C C22C 1.1(9) . . . . ? Zr1C N3C C21C C22C -160.0(5) . . . . ? Si3C N3C C21C Zr1C 161.1(5) . . . . ? N3C Zr1C C21C N4C -162.9(5) . . . . ? N1C Zr1C C21C N4C -148.1(3) . . . . ? N2C Zr1C C21C N4C -91.3(3) . . . . ? Cl2C Zr1C C21C N4C 15.2(4) . . . . ? Cl1C Zr1C C21C N4C 114.3(3) . . . . ? C4C Zr1C C21C N4C -112.1(3) . . . . ? N1C Zr1C C21C N3C 14.9(5) . . . . ? N4C Zr1C C21C N3C 162.9(5) . . . . ? N2C Zr1C C21C N3C 71.7(3) . . . . ? Cl2C Zr1C C21C N3C 178.2(3) . . . . ? Cl1C Zr1C C21C N3C -82.8(3) . . . . ? C4C Zr1C C21C N3C 50.8(4) . . . . ? N3C Zr1C C21C C22C 95.2(16) . . . . ? N1C Zr1C C21C C22C 110.1(15) . . . . ? N4C Zr1C C21C C22C -101.8(16) . . . . ? N2C Zr1C C21C C22C 166.9(15) . . . . ? Cl2C Zr1C C21C C22C -86.6(15) . . . . ? Cl1C Zr1C C21C C22C 12.5(15) . . . . ? C4C Zr1C C21C C22C 146.0(15) . . . . ? N4C C21C C22C C27C -76.4(8) . . . . ? N3C C21C C22C C27C 99.5(7) . . . . ? Zr1C C21C C22C C27C 14.8(19) . . . . ? N4C C21C C22C C23C 101.5(7) . . . . ? N3C C21C C22C C23C -82.6(7) . . . . ? Zr1C C21C C22C C23C -167.2(12) . . . . ? C27C C22C C23C C24C -0.5(9) . . . . ? C21C C22C C23C C24C -178.5(6) . . . . ? C22C C23C C24C C25C 0.9(10) . . . . ? C23C C24C C25C C26C -2.2(10) . . . . ? C23C C24C C25C C28C 177.6(6) . . . . ? C24C C25C C26C C27C 3.2(9) . . . . ? C28C C25C C26C C27C -176.6(6) . . . . ? C23C C22C C27C C26C 1.7(9) . . . . ? C21C C22C C27C C26C 179.7(6) . . . . ? C25C C26C C27C C22C -3.1(10) . . . . ? C7A C8A C11A C12A -101.0(11) . . . . ? C9A C8A C11A C12A 80.0(11) . . . . ? C8A C11A C12A C13A -174.9(8) . . . . ? C11A C12A C13A C14A -167.2(9) . . . . ? C26A C25A C28A C29A -115.2(8) . . . . ? C24A C25A C28A C29A 67.9(8) . . . . ? C25A C28A C29A C30A -175.7(4) . . . . ? C28A C29A C30A C31A 176.5 . . . . ? C7B C8B C11B C12B -104.1(12) . . . . ? C9B C8B C11B C12B 80.5(13) . . . . ? C8B C11B C12B C13B -175.7(9) . . . . ? C11B C12B C13B C14B -178.6(11) . . . . ? C24B C25B C28B C29B 66.2(8) . . . . ? C26B C25B C28B C29B -119.2(5) . . . . ? C25B C28B C29B C30B 31.2(5) . . . . ? C28B C29B C30B C31B 176.5 . . . . ? C7C C8C C11C C12C -74.7(9) . . . . ? C9C C8C C11C C12C 103.1(8) . . . . ? C8C C11C C12C C13C -47.4(14) . . . . ? C11C C12C C13C C14C 174.6(9) . . . . ? C24C C25C C28C C29C 111.8(8) . . . . ? C26C C25C C28C C29C -68.4(9) . . . . ? C25C C28C C29C C30C -179.6(7) . . . . ? C28C C29C C30C C31C 178.8(9) . . . . ? # start Validation Reply Form _vrf_PLAT234_I ; PROBLEM: Large Hirshfeld Difference C29B -- C30B .. 0.32 Ang. RESPONSE: . Two of the six butyl fragments have high ADPs suggesting librations of the fragments ; _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for C29B RESPONSE: Two of the six butyl fragments have high ADPs suggesting librations of the fragments ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.676 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 946662' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zrdimomet _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_sum 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_weight 749.20 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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.409(2) _cell_length_b 11.8110(14) _cell_length_c 17.5870(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.611(8) _cell_angle_gamma 90.00 _cell_volume 4023.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 230.0(1) _cell_measurement_reflns_used 76564 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8132 _exptl_absorpt_correction_T_max 0.8517 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10204 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.1295 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6108 _reflns_number_gt 2875 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1997), KappaCCD Collect Program' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus": a computer program for the solution and refinement of crystal structures from diffraction data University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6108 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 0.833 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.002 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 0.72906(3) 0.08510(6) 0.27812(3) 0.0580(2) Uani 1 1 d . . . Cl1 Cl 0.76366(12) 0.2000(2) 0.17317(11) 0.1196(8) Uani 1 1 d . . . Cl2 Cl 0.63033(8) -0.00093(18) 0.20911(9) 0.0840(6) Uani 1 1 d . . . Si1 Si 0.69630(9) 0.38917(18) 0.31457(10) 0.0733(6) Uani 1 1 d . . . Si2 Si 0.63159(9) -0.03912(17) 0.42722(9) 0.0626(5) Uani 1 1 d . . . Si3 Si 0.87063(9) 0.1072(2) 0.43117(10) 0.0950(8) Uani 1 1 d . . . Si4 Si 0.79822(13) -0.1562(3) 0.17420(13) 0.1223(11) Uani 1 1 d . . . O1 O 0.53502(19) 0.2135(4) 0.3098(2) 0.0714(12) Uani 1 1 d . . . O2 O 0.8679(3) -0.2251(6) 0.3703(3) 0.112(2) Uani 1 1 d . . . N1 N 0.6984(2) 0.2447(4) 0.3347(2) 0.0559(13) Uani 1 1 d . . . N2 N 0.6724(2) 0.0703(4) 0.3814(2) 0.0507(12) Uani 1 1 d . . . N3 N 0.8264(2) 0.0577(6) 0.3476(3) 0.0756(18) Uani 1 1 d . . . N4 N 0.7971(2) -0.0552(5) 0.2476(3) 0.0779(18) Uani 1 1 d . . . C1 C 0.7869(4) 0.4298(8) 0.2974(5) 0.125(3) Uani 1 1 d . . . H1A H 0.8164 0.4152 0.3430 0.187 Uiso 1 1 calc R . . H1B H 0.7886 0.5096 0.2848 0.187 Uiso 1 1 calc R . . H1C H 0.8028 0.3855 0.2555 0.187 Uiso 1 1 calc R . . C2 C 0.6669(4) 0.4792(7) 0.3933(5) 0.121(3) Uani 1 1 d . . . H2A H 0.6966 0.4665 0.4389 0.182 Uiso 1 1 calc R . . H2B H 0.6198 0.4596 0.4031 0.182 Uiso 1 1 calc R . . H2C H 0.6690 0.5582 0.3787 0.182 Uiso 1 1 calc R . . C3 C 0.6377(4) 0.4133(7) 0.2302(4) 0.115(3) Uani 1 1 d . . . H3A H 0.5913 0.3912 0.2412 0.172 Uiso 1 1 calc R . . H3B H 0.6527 0.3685 0.1880 0.172 Uiso 1 1 calc R . . H3C H 0.6382 0.4929 0.2167 0.172 Uiso 1 1 calc R . . C4 C 0.6604(3) 0.1803(6) 0.3801(3) 0.0525(16) Uani 1 1 d . . . C5 C 0.6031(3) 0.2340(5) 0.4229(3) 0.0550(16) Uani 1 1 d . . . C6 C 0.6128(3) 0.2684(6) 0.4980(3) 0.0680(18) Uani 1 1 d . . . H6 H 0.6556 0.2563 0.5250 0.082 Uiso 1 1 calc R . . C7 C 0.5592(4) 0.3209(7) 0.5334(4) 0.092(2) Uani 1 1 d . . . H7 H 0.5654 0.3444 0.5844 0.110 Uiso 1 1 calc R . . C8 C 0.4983(4) 0.3376(6) 0.4938(5) 0.089(2) Uani 1 1 d . . . H8 H 0.4629 0.3751 0.5179 0.106 Uiso 1 1 calc R . . C9 C 0.4857(3) 0.3020(6) 0.4193(4) 0.078(2) Uani 1 1 d . . . H9 H 0.4420 0.3117 0.3938 0.093 Uiso 1 1 calc R . . C10 C 0.5390(3) 0.2520(6) 0.3837(4) 0.0632(17) Uani 1 1 d . . . C11 C 0.4704(3) 0.2151(7) 0.2673(4) 0.100(3) Uani 1 1 d . . . H11A H 0.4761 0.1860 0.2165 0.150 Uiso 1 1 calc R . . H11B H 0.4533 0.2922 0.2639 0.150 Uiso 1 1 calc R . . H11C H 0.4377 0.1681 0.2925 0.150 Uiso 1 1 calc R . . C12 C 0.6738(3) -0.1689(6) 0.3937(4) 0.087(2) Uani 1 1 d . . . H12A H 0.7228 -0.1660 0.4081 0.131 Uiso 1 1 calc R . . H12B H 0.6669 -0.1741 0.3387 0.131 Uiso 1 1 calc R . . H12C H 0.6537 -0.2348 0.4168 0.131 Uiso 1 1 calc R . . C13 C 0.5380(3) -0.0435(6) 0.4003(4) 0.078(2) Uani 1 1 d . . . H13A H 0.5163 0.0246 0.4182 0.117 Uiso 1 1 calc R . . H13B H 0.5177 -0.1093 0.4231 0.117 Uiso 1 1 calc R . . H13C H 0.5309 -0.0480 0.3453 0.117 Uiso 1 1 calc R . . C14 C 0.6482(4) -0.0278(7) 0.5323(3) 0.095(3) Uani 1 1 d . . . H14A H 0.6976 -0.0263 0.5448 0.142 Uiso 1 1 calc R . . H14B H 0.6281 -0.0925 0.5567 0.142 Uiso 1 1 calc R . . H14C H 0.6276 0.0413 0.5502 0.142 Uiso 1 1 calc R . . C15 C 0.8127(3) 0.1984(8) 0.4818(4) 0.115(3) Uani 1 1 d . . . H15A H 0.7721 0.1557 0.4939 0.172 Uiso 1 1 calc R . . H15B H 0.7989 0.2625 0.4499 0.172 Uiso 1 1 calc R . . H15C H 0.8364 0.2253 0.5286 0.172 Uiso 1 1 calc R . . C16 C 0.9481(3) 0.1881(10) 0.4093(5) 0.143(4) Uani 1 1 d . . . H16A H 0.9788 0.1400 0.3821 0.215 Uiso 1 1 calc R . . H16B H 0.9717 0.2139 0.4564 0.215 Uiso 1 1 calc R . . H16C H 0.9346 0.2529 0.3779 0.215 Uiso 1 1 calc R . . C17 C 0.8934(5) -0.0147(9) 0.4966(4) 0.141(4) Uani 1 1 d . . . H17A H 0.9247 -0.0654 0.4724 0.212 Uiso 1 1 calc R . . H17B H 0.8518 -0.0555 0.5074 0.212 Uiso 1 1 calc R . . H17C H 0.9156 0.0137 0.5438 0.212 Uiso 1 1 calc R . . C18 C 0.8429(3) -0.0246(8) 0.3030(4) 0.085(2) Uani 1 1 d . . . C19 C 0.91591(18) -0.0741(5) 0.3087(3) 0.111(3) Uani 1 1 d G . . C20 C 0.9711(2) -0.0182(4) 0.2787(2) 0.078(2) Uani 1 1 d G . . H20 H 0.9641 0.0520 0.2542 0.093 Uiso 1 1 calc R . . C21 C 1.0366(2) -0.0661(5) 0.2849(3) 0.128(4) Uani 1 1 d G . . H21 H 1.0739 -0.0283 0.2646 0.154 Uiso 1 1 calc R . . C22 C 1.0470(2) -0.1698(5) 0.3211(3) 0.150(5) Uani 1 1 d G . . H22 H 1.0913 -0.2022 0.3253 0.180 Uiso 1 1 calc R . . C23 C 0.9918(4) -0.2257(4) 0.3512(3) 0.120(4) Uani 1 1 d G . . H23 H 0.9988 -0.2959 0.3757 0.144 Uiso 1 1 calc R . . C24 C 0.9263(3) -0.1778(5) 0.3449(3) 0.106(3) Uani 1 1 d G . . C25 C 0.8827(6) -0.3316(10) 0.4115(5) 0.171(5) Uani 1 1 d . . . H25A H 0.8402 -0.3627 0.4287 0.256 Uiso 1 1 calc R . . H25B H 0.9146 -0.3170 0.4552 0.256 Uiso 1 1 calc R . . H25C H 0.9033 -0.3853 0.3779 0.256 Uiso 1 1 calc R . . C26 C 0.8779(4) -0.2309(11) 0.1661(6) 0.212(7) Uani 1 1 d . . . H26A H 0.8938 -0.2606 0.2156 0.318 Uiso 1 1 calc R . . H26B H 0.9123 -0.1796 0.1481 0.318 Uiso 1 1 calc R . . H26C H 0.8708 -0.2929 0.1304 0.318 Uiso 1 1 calc R . . C27 C 0.7345(6) -0.2749(10) 0.1994(7) 0.195(5) Uani 1 1 d . . . H27A H 0.6893 -0.2424 0.2055 0.292 Uiso 1 1 calc R . . H27B H 0.7511 -0.3113 0.2465 0.292 Uiso 1 1 calc R . . H27C H 0.7313 -0.3305 0.1587 0.292 Uiso 1 1 calc R . . C28 C 0.7598(5) -0.0966(10) 0.0878(4) 0.159(5) Uani 1 1 d . . . H28A H 0.7166 -0.0601 0.0982 0.239 Uiso 1 1 calc R . . H28B H 0.7510 -0.1562 0.0505 0.239 Uiso 1 1 calc R . . H28C H 0.7909 -0.0412 0.0680 0.239 Uiso 1 1 calc R . . C29 C 1.013(2) -0.047(4) 0.055(2) 0.150 Uiso 0.260(7) 1 d P . . C30 C 0.951(2) 0.003(4) 0.086(2) 0.150 Uiso 0.260(7) 1 d P . . C31 C 0.908(2) 0.066(4) 0.026(2) 0.150 Uiso 0.260(7) 1 d P . . C32 C 0.883(2) -0.035(4) 0.102(2) 0.150 Uiso 0.260(7) 1 d P . . 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 0.0498(3) 0.0809(5) 0.0440(3) -0.0005(3) 0.0082(2) -0.0020(3) Cl1 0.163(2) 0.123(2) 0.0788(13) 0.0111(12) 0.0536(13) -0.0237(16) Cl2 0.0702(11) 0.1069(17) 0.0732(11) -0.0185(10) -0.0080(8) -0.0012(10) Si1 0.0715(12) 0.0718(16) 0.0777(12) 0.0070(10) 0.0125(9) -0.0123(10) Si2 0.0616(10) 0.0692(14) 0.0586(10) 0.0115(9) 0.0161(8) 0.0029(9) Si3 0.0506(11) 0.174(3) 0.0595(11) -0.0296(13) -0.0027(8) -0.0023(13) Si4 0.1058(18) 0.173(3) 0.0842(15) -0.0608(17) -0.0238(13) 0.0643(19) O1 0.056(3) 0.088(4) 0.070(3) 0.003(2) -0.003(2) 0.009(2) O2 0.078(3) 0.146(6) 0.113(4) -0.008(4) 0.011(3) -0.001(4) N1 0.047(3) 0.070(4) 0.050(3) 0.002(3) 0.005(2) -0.004(3) N2 0.045(3) 0.050(4) 0.058(3) 0.001(2) 0.006(2) 0.002(2) N3 0.044(3) 0.135(6) 0.048(3) -0.019(3) 0.005(2) 0.011(3) N4 0.050(3) 0.125(5) 0.058(3) -0.021(3) -0.005(2) 0.016(3) C1 0.096(6) 0.106(8) 0.173(8) 0.016(6) 0.018(6) -0.046(5) C2 0.168(8) 0.066(6) 0.135(7) -0.017(5) 0.054(6) -0.010(6) C3 0.127(7) 0.094(7) 0.121(6) 0.036(5) -0.014(5) 0.002(6) C4 0.044(3) 0.075(5) 0.038(3) -0.005(3) 0.002(2) -0.007(3) C5 0.053(4) 0.054(4) 0.060(4) 0.003(3) 0.015(3) 0.001(3) C6 0.080(4) 0.069(5) 0.056(4) -0.006(3) 0.014(3) -0.003(4) C7 0.124(7) 0.087(6) 0.070(5) -0.005(4) 0.048(5) 0.008(5) C8 0.082(5) 0.073(6) 0.115(7) 0.004(5) 0.042(5) 0.018(4) C9 0.072(5) 0.073(6) 0.090(5) 0.006(4) 0.026(4) 0.011(4) C10 0.051(4) 0.067(5) 0.072(4) 0.005(4) 0.009(3) -0.001(3) C11 0.076(5) 0.121(8) 0.100(5) 0.000(5) -0.019(4) 0.013(5) C12 0.090(5) 0.066(5) 0.109(5) 0.013(4) 0.031(4) 0.023(4) C13 0.068(4) 0.078(6) 0.091(5) 0.020(4) 0.019(4) -0.012(4) C14 0.099(5) 0.125(7) 0.061(4) 0.027(4) 0.011(4) 0.001(5) C15 0.078(5) 0.193(10) 0.073(5) -0.047(5) 0.004(4) 0.007(5) C16 0.065(5) 0.246(14) 0.118(6) -0.041(7) 0.004(4) -0.036(6) C17 0.152(8) 0.194(12) 0.073(5) -0.020(6) -0.031(5) 0.033(8) C18 0.035(4) 0.154(8) 0.064(4) -0.015(5) -0.002(3) 0.022(4) C19 0.119(7) 0.147(10) 0.064(5) -0.033(5) -0.014(4) 0.027(7) C20 0.044(4) 0.127(7) 0.065(4) -0.002(4) 0.024(3) 0.000(4) C21 0.046(5) 0.216(12) 0.124(7) -0.041(7) 0.012(4) 0.029(6) C22 0.114(8) 0.195(13) 0.133(8) -0.060(8) -0.057(6) 0.101(9) C23 0.055(5) 0.206(11) 0.097(6) -0.060(6) -0.010(4) 0.024(6) C24 0.138(9) 0.106(8) 0.071(5) -0.021(5) -0.018(5) 0.023(7) C25 0.258(14) 0.132(11) 0.118(8) 0.040(7) -0.020(8) -0.028(10) C26 0.138(8) 0.329(19) 0.163(9) -0.164(11) -0.027(7) 0.106(10) C27 0.190(11) 0.149(12) 0.243(14) -0.071(10) -0.003(10) -0.023(10) C28 0.177(9) 0.219(13) 0.078(6) -0.059(7) -0.024(6) 0.069(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 Zr1 N2 2.189(4) . ? Zr1 N3 2.207(4) . ? Zr1 N4 2.207(5) . ? Zr1 N1 2.230(5) . ? Zr1 Cl1 2.420(2) . ? Zr1 Cl2 2.4259(17) . ? Zr1 C4 2.561(5) . ? Zr1 C18 2.575(6) . ? Si1 N1 1.743(5) . ? Si1 C3 1.834(7) . ? Si1 C2 1.863(7) . ? Si1 C1 1.866(7) . ? Si2 N2 1.740(5) . ? Si2 C13 1.849(6) . ? Si2 C12 1.852(7) . ? Si2 C14 1.861(6) . ? Si3 N3 1.756(5) . ? Si3 C15 1.829(7) . ? Si3 C16 1.843(8) . ? Si3 C17 1.879(10) . ? Si4 N4 1.759(6) . ? Si4 C28 1.794(8) . ? Si4 C26 1.795(8) . ? Si4 C27 1.939(11) . ? O1 C10 1.375(7) . ? O1 C11 1.419(7) . ? O2 C24 1.363(6) . ? O2 C25 1.472(11) . ? N1 C4 1.353(7) . ? N2 C4 1.320(7) . ? N3 C18 1.301(8) . ? N4 C18 1.327(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.521(7) . ? C5 C6 1.383(7) . ? C5 C10 1.399(8) . ? C6 C7 1.391(9) . ? C6 H6 0.9400 . ? C7 C8 1.348(9) . ? C7 H7 0.9400 . ? C8 C9 1.383(9) . ? C8 H8 0.9400 . ? C9 C10 1.376(8) . ? C9 H9 0.9400 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.530(7) . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9400 . ? C21 C22 1.3900 . ? C21 H21 0.9400 . ? C22 C23 1.3900 . ? C22 H22 0.9400 . ? C23 C24 1.3900 . ? C23 H23 0.9400 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C30 1.47(5) . ? C30 C32 1.44(5) . ? C30 C31 1.51(5) . ? C31 C32 1.88(6) . ? 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 N3 89.23(16) . . ? N2 Zr1 N4 118.79(19) . . ? N3 Zr1 N4 61.31(19) . . ? N2 Zr1 N1 62.26(17) . . ? N3 Zr1 N1 96.90(19) . . ? N4 Zr1 N1 157.55(17) . . ? N2 Zr1 Cl1 148.84(15) . . ? N3 Zr1 Cl1 103.62(15) . . ? N4 Zr1 Cl1 92.11(15) . . ? N1 Zr1 Cl1 87.79(13) . . ? N2 Zr1 Cl2 87.66(12) . . ? N3 Zr1 Cl2 146.81(18) . . ? N4 Zr1 Cl2 91.72(14) . . ? N1 Zr1 Cl2 110.63(12) . . ? Cl1 Zr1 Cl2 95.84(8) . . ? N2 Zr1 C4 31.02(17) . . ? N3 Zr1 C4 98.14(17) . . ? N4 Zr1 C4 147.8(2) . . ? N1 Zr1 C4 31.86(18) . . ? Cl1 Zr1 C4 118.00(17) . . ? Cl2 Zr1 C4 96.02(12) . . ? N2 Zr1 C18 106.84(19) . . ? N3 Zr1 C18 30.35(19) . . ? N4 Zr1 C18 31.0(2) . . ? N1 Zr1 C18 126.9(2) . . ? Cl1 Zr1 C18 97.78(17) . . ? Cl2 Zr1 C18 121.12(19) . . ? C4 Zr1 C18 125.49(19) . . ? N1 Si1 C3 108.8(3) . . ? N1 Si1 C2 114.3(3) . . ? C3 Si1 C2 108.0(4) . . ? N1 Si1 C1 106.0(3) . . ? C3 Si1 C1 111.8(4) . . ? C2 Si1 C1 108.0(4) . . ? N2 Si2 C13 111.7(3) . . ? N2 Si2 C12 104.2(3) . . ? C13 Si2 C12 110.0(3) . . ? N2 Si2 C14 110.6(3) . . ? C13 Si2 C14 111.3(3) . . ? C12 Si2 C14 108.8(3) . . ? N3 Si3 C15 108.7(3) . . ? N3 Si3 C16 111.1(3) . . ? C15 Si3 C16 109.3(5) . . ? N3 Si3 C17 110.0(4) . . ? C15 Si3 C17 106.3(4) . . ? C16 Si3 C17 111.2(4) . . ? N4 Si4 C28 109.4(4) . . ? N4 Si4 C26 116.2(3) . . ? C28 Si4 C26 116.2(5) . . ? N4 Si4 C27 106.6(4) . . ? C28 Si4 C27 103.9(5) . . ? C26 Si4 C27 103.2(6) . . ? C10 O1 C11 119.3(5) . . ? C24 O2 C25 111.7(7) . . ? C4 N1 Si1 131.6(4) . . ? C4 N1 Zr1 87.7(4) . . ? Si1 N1 Zr1 137.7(2) . . ? C4 N2 Si2 130.9(4) . . ? C4 N2 Zr1 90.2(3) . . ? Si2 N2 Zr1 135.3(3) . . ? C18 N3 Si3 128.8(4) . . ? C18 N3 Zr1 90.7(3) . . ? Si3 N3 Zr1 140.5(3) . . ? C18 N4 Si4 133.3(5) . . ? C18 N4 Zr1 90.0(4) . . ? Si4 N4 Zr1 136.3(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N1 117.5(5) . . ? N2 C4 C5 122.3(5) . . ? N1 C4 C5 120.0(6) . . ? N2 C4 Zr1 58.8(3) . . ? N1 C4 Zr1 60.5(3) . . ? C5 C4 Zr1 163.6(4) . . ? C6 C5 C10 119.3(5) . . ? C6 C5 C4 122.3(5) . . ? C10 C5 C4 118.4(5) . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 119.4(7) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 122.9(7) . . ? C7 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C10 C9 C8 117.8(7) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C9 C10 O1 124.9(6) . . ? C9 C10 C5 120.8(6) . . ? O1 C10 C5 114.2(5) . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 N4 117.8(5) . . ? N3 C18 C19 120.6(5) . . ? N4 C18 C19 121.2(6) . . ? N3 C18 Zr1 59.0(3) . . ? N4 C18 Zr1 59.0(3) . . ? C19 C18 Zr1 169.9(5) . . ? C20 C19 C24 120.0 . . ? C20 C19 C18 121.7(5) . . ? C24 C19 C18 118.3(5) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? O2 C24 C23 125.7(5) . . ? O2 C24 C19 114.3(5) . . ? C23 C24 C19 120.0 . . ? O2 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C30 C29 136(5) . . ? C32 C30 C31 79(3) . . ? C29 C30 C31 112(4) . . ? C30 C31 C32 49(2) . . ? C30 C32 C31 52(2) . . ? 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 C3 Si1 N1 C4 -91.5(5) . . . . ? C2 Si1 N1 C4 29.3(6) . . . . ? C1 Si1 N1 C4 148.2(5) . . . . ? C3 Si1 N1 Zr1 62.0(5) . . . . ? C2 Si1 N1 Zr1 -177.2(4) . . . . ? C1 Si1 N1 Zr1 -58.3(5) . . . . ? N2 Zr1 N1 C4 -8.9(3) . . . . ? N3 Zr1 N1 C4 -94.3(3) . . . . ? N4 Zr1 N1 C4 -107.6(5) . . . . ? Cl1 Zr1 N1 C4 162.2(3) . . . . ? Cl2 Zr1 N1 C4 66.8(3) . . . . ? C18 Zr1 N1 C4 -99.7(3) . . . . ? N2 Zr1 N1 Si1 -169.3(4) . . . . ? N3 Zr1 N1 Si1 105.2(4) . . . . ? N4 Zr1 N1 Si1 91.9(6) . . . . ? Cl1 Zr1 N1 Si1 1.7(3) . . . . ? Cl2 Zr1 N1 Si1 -93.7(3) . . . . ? C4 Zr1 N1 Si1 -160.5(5) . . . . ? C18 Zr1 N1 Si1 99.8(4) . . . . ? C13 Si2 N2 C4 56.4(6) . . . . ? C12 Si2 N2 C4 175.2(5) . . . . ? C14 Si2 N2 C4 -68.1(6) . . . . ? C13 Si2 N2 Zr1 -95.6(4) . . . . ? C12 Si2 N2 Zr1 23.1(4) . . . . ? C14 Si2 N2 Zr1 139.9(4) . . . . ? N3 Zr1 N2 C4 107.3(3) . . . . ? N4 Zr1 N2 C4 163.6(3) . . . . ? N1 Zr1 N2 C4 9.1(3) . . . . ? Cl1 Zr1 N2 C4 -8.4(5) . . . . ? Cl2 Zr1 N2 C4 -105.8(3) . . . . ? C18 Zr1 N2 C4 132.4(3) . . . . ? N3 Zr1 N2 Si2 -93.5(4) . . . . ? N4 Zr1 N2 Si2 -37.2(4) . . . . ? N1 Zr1 N2 Si2 168.3(4) . . . . ? Cl1 Zr1 N2 Si2 150.9(2) . . . . ? Cl2 Zr1 N2 Si2 53.5(3) . . . . ? C4 Zr1 N2 Si2 159.2(6) . . . . ? C18 Zr1 N2 Si2 -68.4(4) . . . . ? C15 Si3 N3 C18 -165.6(7) . . . . ? C16 Si3 N3 C18 74.0(8) . . . . ? C17 Si3 N3 C18 -49.5(7) . . . . ? C15 Si3 N3 Zr1 9.5(6) . . . . ? C16 Si3 N3 Zr1 -110.9(5) . . . . ? C17 Si3 N3 Zr1 125.5(5) . . . . ? N2 Zr1 N3 C18 126.6(5) . . . . ? N4 Zr1 N3 C18 2.8(4) . . . . ? N1 Zr1 N3 C18 -171.5(4) . . . . ? Cl1 Zr1 N3 C18 -82.1(5) . . . . ? Cl2 Zr1 N3 C18 42.1(5) . . . . ? C4 Zr1 N3 C18 156.4(4) . . . . ? N2 Zr1 N3 Si3 -49.6(5) . . . . ? N4 Zr1 N3 Si3 -173.4(6) . . . . ? N1 Zr1 N3 Si3 12.4(5) . . . . ? Cl1 Zr1 N3 Si3 101.8(5) . . . . ? Cl2 Zr1 N3 Si3 -134.1(4) . . . . ? C4 Zr1 N3 Si3 -19.7(5) . . . . ? C18 Zr1 N3 Si3 -176.2(8) . . . . ? C28 Si4 N4 C18 -138.0(8) . . . . ? C26 Si4 N4 C18 -4.0(10) . . . . ? C27 Si4 N4 C18 110.2(8) . . . . ? C28 Si4 N4 Zr1 32.1(6) . . . . ? C26 Si4 N4 Zr1 166.0(6) . . . . ? C27 Si4 N4 Zr1 -79.7(6) . . . . ? N2 Zr1 N4 C18 -74.2(5) . . . . ? N3 Zr1 N4 C18 -2.7(4) . . . . ? N1 Zr1 N4 C18 12.3(7) . . . . ? Cl1 Zr1 N4 C18 101.6(4) . . . . ? Cl2 Zr1 N4 C18 -162.4(4) . . . . ? C4 Zr1 N4 C18 -58.3(6) . . . . ? N2 Zr1 N4 Si4 113.0(4) . . . . ? N3 Zr1 N4 Si4 -175.5(6) . . . . ? N1 Zr1 N4 Si4 -160.5(4) . . . . ? Cl1 Zr1 N4 Si4 -71.1(5) . . . . ? Cl2 Zr1 N4 Si4 24.8(5) . . . . ? C4 Zr1 N4 Si4 128.9(4) . . . . ? C18 Zr1 N4 Si4 -172.8(8) . . . . ? Si2 N2 C4 N1 -175.8(4) . . . . ? Zr1 N2 C4 N1 -15.0(5) . . . . ? Si2 N2 C4 C5 0.0(8) . . . . ? Zr1 N2 C4 C5 160.7(5) . . . . ? Si2 N2 C4 Zr1 -160.7(5) . . . . ? Si1 N1 C4 N2 177.3(4) . . . . ? Zr1 N1 C4 N2 14.8(5) . . . . ? Si1 N1 C4 C5 1.5(7) . . . . ? Zr1 N1 C4 C5 -161.0(4) . . . . ? Si1 N1 C4 Zr1 162.5(5) . . . . ? N3 Zr1 C4 N2 -74.7(3) . . . . ? N4 Zr1 C4 N2 -27.7(5) . . . . ? N1 Zr1 C4 N2 -164.7(5) . . . . ? Cl1 Zr1 C4 N2 175.1(3) . . . . ? Cl2 Zr1 C4 N2 75.2(3) . . . . ? C18 Zr1 C4 N2 -60.3(4) . . . . ? N2 Zr1 C4 N1 164.7(5) . . . . ? N3 Zr1 C4 N1 90.0(3) . . . . ? N4 Zr1 C4 N1 136.9(4) . . . . ? Cl1 Zr1 C4 N1 -20.2(3) . . . . ? Cl2 Zr1 C4 N1 -120.1(3) . . . . ? C18 Zr1 C4 N1 104.4(4) . . . . ? N2 Zr1 C4 C5 -98.9(17) . . . . ? N3 Zr1 C4 C5 -173.6(17) . . . . ? N4 Zr1 C4 C5 -126.6(16) . . . . ? N1 Zr1 C4 C5 96.4(17) . . . . ? Cl1 Zr1 C4 C5 76.2(17) . . . . ? Cl2 Zr1 C4 C5 -23.7(17) . . . . ? C18 Zr1 C4 C5 -159.2(16) . . . . ? N2 C4 C5 C6 87.8(7) . . . . ? N1 C4 C5 C6 -96.6(7) . . . . ? Zr1 C4 C5 C6 176.5(13) . . . . ? N2 C4 C5 C10 -94.2(7) . . . . ? N1 C4 C5 C10 81.4(7) . . . . ? Zr1 C4 C5 C10 -5(2) . . . . ? C10 C5 C6 C7 -0.4(9) . . . . ? C4 C5 C6 C7 177.6(6) . . . . ? C5 C6 C7 C8 0.0(11) . . . . ? C6 C7 C8 C9 1.8(12) . . . . ? C7 C8 C9 C10 -3.0(12) . . . . ? C8 C9 C10 O1 -179.2(6) . . . . ? C8 C9 C10 C5 2.4(10) . . . . ? C11 O1 C10 C9 -5.7(10) . . . . ? C11 O1 C10 C5 172.7(6) . . . . ? C6 C5 C10 C9 -0.8(9) . . . . ? C4 C5 C10 C9 -178.9(6) . . . . ? C6 C5 C10 O1 -179.3(6) . . . . ? C4 C5 C10 O1 2.6(8) . . . . ? Si3 N3 C18 N4 172.3(5) . . . . ? Zr1 N3 C18 N4 -4.6(7) . . . . ? Si3 N3 C18 C19 -14.9(11) . . . . ? Zr1 N3 C18 C19 168.2(6) . . . . ? Si3 N3 C18 Zr1 176.9(7) . . . . ? Si4 N4 C18 N3 177.8(6) . . . . ? Zr1 N4 C18 N3 4.6(7) . . . . ? Si4 N4 C18 C19 5.0(11) . . . . ? Zr1 N4 C18 C19 -168.2(6) . . . . ? Si4 N4 C18 Zr1 173.2(7) . . . . ? N2 Zr1 C18 N3 -57.0(5) . . . . ? N4 Zr1 C18 N3 -175.2(7) . . . . ? N1 Zr1 C18 N3 10.6(5) . . . . ? Cl1 Zr1 C18 N3 103.7(4) . . . . ? Cl2 Zr1 C18 N3 -154.6(4) . . . . ? C4 Zr1 C18 N3 -29.1(6) . . . . ? N2 Zr1 C18 N4 118.2(4) . . . . ? N3 Zr1 C18 N4 175.2(7) . . . . ? N1 Zr1 C18 N4 -174.1(4) . . . . ? Cl1 Zr1 C18 N4 -81.1(4) . . . . ? Cl2 Zr1 C18 N4 20.6(5) . . . . ? C4 Zr1 C18 N4 146.1(4) . . . . ? N2 Zr1 C18 C19 -148(3) . . . . ? N3 Zr1 C18 C19 -91(3) . . . . ? N4 Zr1 C18 C19 94(3) . . . . ? N1 Zr1 C18 C19 -80(3) . . . . ? Cl1 Zr1 C18 C19 13(3) . . . . ? Cl2 Zr1 C18 C19 115(3) . . . . ? C4 Zr1 C18 C19 -120(3) . . . . ? N3 C18 C19 C20 -76.7(7) . . . . ? N4 C18 C19 C20 95.9(8) . . . . ? Zr1 C18 C19 C20 8(3) . . . . ? N3 C18 C19 C24 103.4(7) . . . . ? N4 C18 C19 C24 -84.0(7) . . . . ? Zr1 C18 C19 C24 -172(3) . . . . ? C24 C19 C20 C21 0.0 . . . . ? C18 C19 C20 C21 -179.9(5) . . . . ? C19 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C25 O2 C24 C23 4.5(8) . . . . ? C25 O2 C24 C19 -177.0(5) . . . . ? C22 C23 C24 O2 178.4(5) . . . . ? C22 C23 C24 C19 0.0 . . . . ? C20 C19 C24 O2 -178.6(5) . . . . ? C18 C19 C24 O2 1.3(5) . . . . ? C20 C19 C24 C23 0.0 . . . . ? C18 C19 C24 C23 179.9(5) . . . . ? C29 C30 C31 C32 135(5) . . . . ? C29 C30 C32 C31 -110(6) . . . . ? _diffrn_measured_fraction_theta_max 0.95 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.95 _refine_diff_density_max 0.684 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 946663' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zrmmtxdim _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_sum 'C28 H50 Cl2 N4 O2 Si4 Zr' _chemical_formula_weight 749.20 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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7290(4) _cell_length_b 17.8860(6) _cell_length_c 18.8940(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.6470(13) _cell_angle_gamma 90.00 _cell_volume 3959.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 230.0(1) _cell_measurement_reflns_used 17889 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8631 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 230.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5500 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5500 _reflns_number_gt 4226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius (1997), KappaCCD Collect Program' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland "maXus": a computer program for the solution and refinement of crystal structures from diffraction data University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan (1998) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Molecular Structure Corporation (1999). ORTEP. TEXRAY Structure Analysis Package. MSC, 3200 Research Forest Drive, The Woodlands,TX 77381, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0274P)^2^+2.9489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5500 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Zr1 Zr 0.64697(3) -0.134465(19) 0.250042(19) 0.04146(12) Uani 1 1 d . . . Cl1 Cl 0.78435(10) -0.20085(7) 0.32609(7) 0.0804(4) Uani 1 1 d . . . Cl2 Cl 0.59528(11) -0.23589(7) 0.17039(8) 0.0926(5) Uani 1 1 d . . . Si1 Si 0.50607(9) -0.19026(6) 0.41405(6) 0.0487(3) Uani 1 1 d . . . Si2 Si 0.40216(10) -0.04693(7) 0.15395(6) 0.0551(3) Uani 1 1 d . . . Si3 Si 0.85388(9) -0.12067(6) 0.10931(6) 0.0485(3) Uani 1 1 d . . . Si4 Si 0.69950(9) 0.05257(6) 0.33386(6) 0.0475(3) Uani 1 1 d . . . O1 O 0.0982(2) 0.00454(18) 0.38614(16) 0.0691(8) Uani 1 1 d . . . O2 O 0.8509(2) 0.17501(16) 0.05009(15) 0.0671(8) Uani 1 1 d . . . N1 N 0.5192(2) -0.14053(16) 0.33429(15) 0.0412(7) Uani 1 1 d . . . N2 N 0.4769(2) -0.08534(16) 0.22873(15) 0.0438(7) Uani 1 1 d . . . N3 N 0.7710(2) -0.08661(15) 0.17811(15) 0.0415(7) Uani 1 1 d . . . N4 N 0.7160(2) -0.02007(15) 0.27235(15) 0.0417(7) Uani 1 1 d . . . C1 C 0.6223(4) -0.1587(3) 0.4759(2) 0.0741(13) Uani 1 1 d . . . H1A H 0.6140 -0.1056 0.4849 0.111 Uiso 1 1 calc R . . H1B H 0.6952 -0.1679 0.4553 0.111 Uiso 1 1 calc R . . H1C H 0.6189 -0.1860 0.5202 0.111 Uiso 1 1 calc R . . C2 C 0.5170(5) -0.2913(2) 0.3945(3) 0.0893(16) Uani 1 1 d . . . H2A H 0.4545 -0.3060 0.3621 0.134 Uiso 1 1 calc R . . H2B H 0.5133 -0.3195 0.4382 0.134 Uiso 1 1 calc R . . H2C H 0.5891 -0.3013 0.3731 0.134 Uiso 1 1 calc R . . C3 C 0.3701(4) -0.1735(3) 0.4587(2) 0.0817(15) Uani 1 1 d . . . H3A H 0.3063 -0.1891 0.4278 0.122 Uiso 1 1 calc R . . H3B H 0.3630 -0.1207 0.4693 0.122 Uiso 1 1 calc R . . H3C H 0.3703 -0.2020 0.5024 0.122 Uiso 1 1 calc R . . C4 C 0.4399(3) -0.11184(18) 0.28905(19) 0.0394(8) Uani 1 1 d . . . C5 C 0.3145(3) -0.11097(19) 0.30325(19) 0.0413(9) Uani 1 1 d . . . C6 C 0.2456(3) -0.1680(2) 0.2781(2) 0.0537(10) Uani 1 1 d . . . H6 H 0.2770 -0.2078 0.2530 0.064 Uiso 1 1 calc R . . C7 C 0.1295(3) -0.1669(2) 0.2899(2) 0.0613(11) Uani 1 1 d . . . H7 H 0.0824 -0.2061 0.2728 0.074 Uiso 1 1 calc R . . C8 C 0.0836(3) -0.1089(2) 0.3261(2) 0.0598(11) Uani 1 1 d . . . H8 H 0.0051 -0.1085 0.3339 0.072 Uiso 1 1 calc R . . C9 C 0.1514(3) -0.0511(2) 0.3513(2) 0.0494(10) Uani 1 1 d . . . C10 C 0.2683(3) -0.0516(2) 0.34017(19) 0.0443(9) Uani 1 1 d . . . H10 H 0.3152 -0.0124 0.3573 0.053 Uiso 1 1 calc R . . C11 C 0.1629(4) 0.0667(3) 0.4097(3) 0.0894(16) Uani 1 1 d . . . H11A H 0.1140 0.1016 0.4334 0.134 Uiso 1 1 calc R . . H11B H 0.1954 0.0911 0.3695 0.134 Uiso 1 1 calc R . . H11C H 0.2237 0.0502 0.4426 0.134 Uiso 1 1 calc R . . C12 C 0.2953(4) 0.0239(3) 0.1778(2) 0.0820(15) Uani 1 1 d . . . H12A H 0.2355 0.0001 0.2034 0.123 Uiso 1 1 calc R . . H12B H 0.2625 0.0468 0.1350 0.123 Uiso 1 1 calc R . . H12C H 0.3321 0.0620 0.2074 0.123 Uiso 1 1 calc R . . C13 C 0.5138(4) 0.0002(3) 0.1051(2) 0.0669(12) Uani 1 1 d . . . H13A H 0.5706 -0.0362 0.0921 0.100 Uiso 1 1 calc R . . H13B H 0.5498 0.0384 0.1348 0.100 Uiso 1 1 calc R . . H13C H 0.4798 0.0230 0.0626 0.100 Uiso 1 1 calc R . . C14 C 0.3341(5) -0.1226(3) 0.0988(3) 0.0992(18) Uani 1 1 d . . . H14A H 0.2754 -0.1468 0.1252 0.149 Uiso 1 1 calc R . . H14B H 0.3913 -0.1591 0.0870 0.149 Uiso 1 1 calc R . . H14C H 0.3001 -0.1012 0.0556 0.149 Uiso 1 1 calc R . . C15 C 0.7685(4) -0.1139(3) 0.0246(2) 0.0941(18) Uani 1 1 d . . . H15A H 0.6965 -0.1398 0.0289 0.141 Uiso 1 1 calc R . . H15B H 0.8103 -0.1367 -0.0130 0.141 Uiso 1 1 calc R . . H15C H 0.7540 -0.0618 0.0134 0.141 Uiso 1 1 calc R . . C16 C 0.9924(4) -0.0719(3) 0.1015(3) 0.0834(15) Uani 1 1 d . . . H16A H 1.0367 -0.0757 0.1460 0.125 Uiso 1 1 calc R . . H16B H 0.9787 -0.0196 0.0904 0.125 Uiso 1 1 calc R . . H16C H 1.0342 -0.0948 0.0641 0.125 Uiso 1 1 calc R . . C17 C 0.8879(4) -0.2197(2) 0.1312(3) 0.0774(14) Uani 1 1 d . . . H17A H 0.9328 -0.2218 0.1756 0.116 Uiso 1 1 calc R . . H17B H 0.9311 -0.2414 0.0938 0.116 Uiso 1 1 calc R . . H17C H 0.8176 -0.2474 0.1357 0.116 Uiso 1 1 calc R . . C18 C 0.7785(3) -0.02269(19) 0.21486(19) 0.0397(8) Uani 1 1 d . . . C19 C 0.8514(3) 0.04094(19) 0.19316(18) 0.0400(8) Uani 1 1 d . . . C20 C 0.9496(3) 0.0604(2) 0.2327(2) 0.0493(10) Uani 1 1 d . . . H20 H 0.9702 0.0344 0.2746 0.059 Uiso 1 1 calc R . . C21 C 1.0166(3) 0.1182(2) 0.2100(2) 0.0567(11) Uani 1 1 d . . . H21 H 1.0837 0.1309 0.2365 0.068 Uiso 1 1 calc R . . C22 C 0.9874(3) 0.1578(2) 0.1494(2) 0.0533(10) Uani 1 1 d . . . H22 H 1.0342 0.1969 0.1344 0.064 Uiso 1 1 calc R . . C23 C 0.8887(3) 0.1393(2) 0.11083(19) 0.0479(9) Uani 1 1 d . . . C24 C 0.8212(3) 0.08052(19) 0.13196(19) 0.0438(9) Uani 1 1 d . . . H24 H 0.7549 0.0675 0.1048 0.053 Uiso 1 1 calc R . . C25 C 0.9139(4) 0.2370(2) 0.0262(2) 0.0736(13) Uani 1 1 d . . . H25A H 0.8778 0.2562 -0.0173 0.110 Uiso 1 1 calc R . . H25B H 0.9912 0.2213 0.0174 0.110 Uiso 1 1 calc R . . H25C H 0.9159 0.2758 0.0620 0.110 Uiso 1 1 calc R . . C26 C 0.5534(4) 0.0456(2) 0.3668(3) 0.0718(13) Uani 1 1 d . . . H26A H 0.5427 -0.0035 0.3871 0.108 Uiso 1 1 calc R . . H26B H 0.4980 0.0532 0.3277 0.108 Uiso 1 1 calc R . . H26C H 0.5432 0.0835 0.4026 0.108 Uiso 1 1 calc R . . C27 C 0.7125(5) 0.1470(2) 0.2970(3) 0.0932(18) Uani 1 1 d . . . H27A H 0.7880 0.1534 0.2791 0.140 Uiso 1 1 calc R . . H27B H 0.7006 0.1837 0.3338 0.140 Uiso 1 1 calc R . . H27C H 0.6555 0.1538 0.2587 0.140 Uiso 1 1 calc R . . C28 C 0.8055(4) 0.0370(3) 0.4088(2) 0.0944(18) Uani 1 1 d . . . H28A H 0.7965 -0.0131 0.4274 0.142 Uiso 1 1 calc R . . H28B H 0.7932 0.0732 0.4459 0.142 Uiso 1 1 calc R . . H28C H 0.8820 0.0428 0.3922 0.142 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 0.0368(2) 0.0383(2) 0.0498(2) -0.00109(17) 0.00809(15) 0.00214(17) Cl1 0.0569(7) 0.0904(9) 0.0953(9) 0.0366(7) 0.0170(6) 0.0301(6) Cl2 0.0801(9) 0.0828(8) 0.1172(11) -0.0544(8) 0.0281(8) -0.0209(7) Si1 0.0479(6) 0.0511(6) 0.0470(6) 0.0062(5) 0.0024(5) -0.0008(5) Si2 0.0455(6) 0.0690(8) 0.0504(7) 0.0101(6) -0.0032(5) 0.0040(6) Si3 0.0493(6) 0.0497(6) 0.0475(6) -0.0071(5) 0.0122(5) 0.0010(5) Si4 0.0466(6) 0.0429(6) 0.0537(7) -0.0100(5) 0.0096(5) -0.0006(5) O1 0.0440(17) 0.084(2) 0.079(2) -0.0177(17) 0.0074(15) 0.0129(16) O2 0.074(2) 0.0648(18) 0.0627(19) 0.0160(15) 0.0042(15) -0.0135(16) N1 0.0371(16) 0.0429(17) 0.0436(17) 0.0035(14) 0.0008(14) 0.0047(14) N2 0.0395(17) 0.0483(18) 0.0435(19) 0.0054(14) 0.0006(14) 0.0021(14) N3 0.0429(18) 0.0394(17) 0.0428(17) -0.0040(14) 0.0079(14) -0.0003(14) N4 0.0416(17) 0.0398(17) 0.0444(18) -0.0040(14) 0.0085(15) 0.0026(14) C1 0.071(3) 0.096(4) 0.055(3) 0.011(2) -0.005(2) -0.007(3) C2 0.130(5) 0.054(3) 0.084(4) 0.012(3) 0.009(3) -0.006(3) C3 0.063(3) 0.121(4) 0.063(3) 0.026(3) 0.018(2) 0.010(3) C4 0.039(2) 0.0314(18) 0.048(2) -0.0062(16) 0.0025(18) -0.0008(16) C5 0.035(2) 0.042(2) 0.047(2) 0.0050(17) 0.0007(17) -0.0001(17) C6 0.052(3) 0.041(2) 0.068(3) -0.003(2) 0.003(2) -0.0016(19) C7 0.049(3) 0.058(3) 0.076(3) 0.006(2) -0.003(2) -0.020(2) C8 0.039(2) 0.068(3) 0.072(3) 0.014(2) 0.000(2) -0.006(2) C9 0.038(2) 0.059(3) 0.051(2) 0.001(2) 0.0006(18) 0.005(2) C10 0.035(2) 0.045(2) 0.052(2) -0.0005(18) -0.0022(17) -0.0015(17) C11 0.079(4) 0.090(4) 0.100(4) -0.038(3) 0.007(3) 0.020(3) C12 0.062(3) 0.113(4) 0.072(3) 0.031(3) 0.008(2) 0.037(3) C13 0.061(3) 0.082(3) 0.058(3) 0.019(2) 0.008(2) 0.017(2) C14 0.108(4) 0.109(4) 0.076(4) -0.004(3) -0.032(3) -0.018(4) C15 0.096(4) 0.137(5) 0.049(3) -0.027(3) -0.002(3) 0.037(3) C16 0.066(3) 0.080(3) 0.107(4) -0.027(3) 0.045(3) -0.006(3) C17 0.084(3) 0.063(3) 0.088(4) -0.004(3) 0.040(3) 0.015(3) C18 0.0335(19) 0.040(2) 0.046(2) -0.0003(17) -0.0004(17) 0.0009(16) C19 0.038(2) 0.038(2) 0.044(2) -0.0062(17) 0.0060(17) -0.0008(16) C20 0.045(2) 0.048(2) 0.055(2) 0.0019(18) -0.0025(19) 0.0009(19) C21 0.038(2) 0.059(3) 0.073(3) -0.012(2) -0.003(2) -0.005(2) C22 0.045(2) 0.046(2) 0.071(3) -0.007(2) 0.017(2) -0.0091(18) C23 0.050(2) 0.047(2) 0.047(2) 0.0004(19) 0.0081(18) -0.0007(19) C24 0.040(2) 0.046(2) 0.046(2) -0.0040(18) 0.0033(17) -0.0054(17) C25 0.090(4) 0.061(3) 0.073(3) 0.010(2) 0.034(3) -0.004(3) C26 0.066(3) 0.064(3) 0.087(3) -0.029(2) 0.028(3) -0.003(2) C27 0.130(5) 0.044(3) 0.110(4) -0.008(3) 0.054(4) 0.005(3) C28 0.071(3) 0.146(5) 0.066(3) -0.035(3) -0.002(3) 0.025(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 N2 2.200(3) . ? Zr1 N3 2.208(3) . ? Zr1 N4 2.234(3) . ? Zr1 N1 2.239(3) . ? Zr1 Cl2 2.4164(12) . ? Zr1 Cl1 2.4202(12) . ? Zr1 C4 2.602(3) . ? Zr1 C18 2.629(3) . ? Si1 N1 1.763(3) . ? Si1 C1 1.843(4) . ? Si1 C2 1.850(5) . ? Si1 C3 1.862(4) . ? Si2 N2 1.767(3) . ? Si2 C13 1.841(4) . ? Si2 C12 1.852(4) . ? Si2 C14 1.864(5) . ? Si3 N3 1.767(3) . ? Si3 C15 1.853(5) . ? Si3 C16 1.856(4) . ? Si3 C17 1.857(4) . ? Si4 N4 1.760(3) . ? Si4 C27 1.836(4) . ? Si4 C26 1.854(4) . ? Si4 C28 1.862(5) . ? O1 C9 1.361(5) . ? O1 C11 1.407(5) . ? O2 C23 1.369(4) . ? O2 C25 1.418(5) . ? N1 C4 1.336(4) . ? N2 C4 1.326(4) . ? N3 C18 1.338(4) . ? N4 C18 1.338(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.508(5) . ? C5 C6 1.372(5) . ? C5 C10 1.394(5) . ? C6 C7 1.390(5) . ? C6 H6 0.9400 . ? C7 C8 1.367(6) . ? C7 H7 0.9400 . ? C8 C9 1.377(5) . ? C8 H8 0.9400 . ? C9 C10 1.396(5) . ? C10 H10 0.9400 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 H13C 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 C19 1.493(5) . ? C19 C20 1.388(5) . ? C19 C24 1.388(5) . ? C20 C21 1.380(5) . ? C20 H20 0.9400 . ? C21 C22 1.376(6) . ? C21 H21 0.9400 . ? C22 C23 1.379(5) . ? C22 H22 0.9400 . ? C23 C24 1.387(5) . ? C24 H24 0.9400 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zr1 N3 110.47(11) . . ? N2 Zr1 N4 89.23(11) . . ? N3 Zr1 N4 61.16(10) . . ? N2 Zr1 N1 61.20(10) . . ? N3 Zr1 N1 159.69(10) . . ? N4 Zr1 N1 99.16(10) . . ? N2 Zr1 Cl2 89.23(8) . . ? N3 Zr1 Cl2 93.50(8) . . ? N4 Zr1 Cl2 152.08(8) . . ? N1 Zr1 Cl2 104.44(8) . . ? N2 Zr1 Cl1 151.39(8) . . ? N3 Zr1 Cl1 96.68(8) . . ? N4 Zr1 Cl1 96.41(8) . . ? N1 Zr1 Cl1 90.20(8) . . ? Cl2 Zr1 Cl1 98.19(5) . . ? N2 Zr1 C4 30.62(10) . . ? N3 Zr1 C4 139.80(11) . . ? N4 Zr1 C4 98.01(10) . . ? N1 Zr1 C4 30.89(10) . . ? Cl2 Zr1 C4 94.73(8) . . ? Cl1 Zr1 C4 120.84(9) . . ? N2 Zr1 C18 100.80(11) . . ? N3 Zr1 C18 30.57(10) . . ? N4 Zr1 C18 30.59(10) . . ? N1 Zr1 C18 129.53(11) . . ? Cl2 Zr1 C18 123.14(8) . . ? Cl1 Zr1 C18 98.11(8) . . ? C4 Zr1 C18 121.30(10) . . ? N1 Si1 C1 107.27(17) . . ? N1 Si1 C2 108.23(19) . . ? C1 Si1 C2 111.7(2) . . ? N1 Si1 C3 114.61(18) . . ? C1 Si1 C3 106.7(2) . . ? C2 Si1 C3 108.5(2) . . ? N2 Si2 C13 103.94(17) . . ? N2 Si2 C12 112.83(18) . . ? C13 Si2 C12 108.3(2) . . ? N2 Si2 C14 110.4(2) . . ? C13 Si2 C14 110.4(2) . . ? C12 Si2 C14 110.8(3) . . ? N3 Si3 C15 108.62(18) . . ? N3 Si3 C16 114.20(17) . . ? C15 Si3 C16 109.9(3) . . ? N3 Si3 C17 106.54(17) . . ? C15 Si3 C17 110.9(2) . . ? C16 Si3 C17 106.6(2) . . ? N4 Si4 C27 114.52(19) . . ? N4 Si4 C26 107.68(17) . . ? C27 Si4 C26 106.4(2) . . ? N4 Si4 C28 107.55(19) . . ? C27 Si4 C28 111.2(3) . . ? C26 Si4 C28 109.3(2) . . ? C9 O1 C11 118.5(3) . . ? C23 O2 C25 118.6(3) . . ? C4 N1 Si1 130.9(2) . . ? C4 N1 Zr1 89.7(2) . . ? Si1 N1 Zr1 136.04(15) . . ? C4 N2 Si2 131.0(3) . . ? C4 N2 Zr1 91.7(2) . . ? Si2 N2 Zr1 135.56(16) . . ? C18 N3 Si3 130.6(2) . . ? C18 N3 Zr1 92.4(2) . . ? Si3 N3 Zr1 136.00(15) . . ? C18 N4 Si4 130.0(2) . . ? C18 N4 Zr1 91.3(2) . . ? Si4 N4 Zr1 138.66(16) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N1 116.2(3) . . ? N2 C4 C5 120.7(3) . . ? N1 C4 C5 123.1(3) . . ? N2 C4 Zr1 57.67(18) . . ? N1 C4 Zr1 59.37(17) . . ? C5 C4 Zr1 169.5(2) . . ? C6 C5 C10 120.2(3) . . ? C6 C5 C4 119.6(3) . . ? C10 C5 C4 120.1(3) . . ? C5 C6 C7 120.0(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.1(4) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.6(4) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? O1 C9 C8 116.5(4) . . ? O1 C9 C10 123.6(4) . . ? C8 C9 C10 119.9(4) . . ? C5 C10 C9 119.1(4) . . ? C5 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 N3 115.2(3) . . ? N4 C18 C19 122.6(3) . . ? N3 C18 C19 122.2(3) . . ? N4 C18 Zr1 58.15(17) . . ? N3 C18 Zr1 57.07(17) . . ? C19 C18 Zr1 178.6(3) . . ? C20 C19 C24 119.7(3) . . ? C20 C19 C18 121.0(3) . . ? C24 C19 C18 119.3(3) . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 121.4(4) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? O2 C23 C22 124.2(3) . . ? O2 C23 C24 115.3(3) . . ? C22 C23 C24 120.4(4) . . ? C23 C24 C19 120.0(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? O2 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C1 Si1 N1 C4 -141.7(3) . . . . ? C2 Si1 N1 C4 97.6(4) . . . . ? C3 Si1 N1 C4 -23.5(4) . . . . ? C1 Si1 N1 Zr1 65.3(3) . . . . ? C2 Si1 N1 Zr1 -55.4(3) . . . . ? C3 Si1 N1 Zr1 -176.5(2) . . . . ? N2 Zr1 N1 C4 6.28(18) . . . . ? N3 Zr1 N1 C4 76.7(4) . . . . ? N4 Zr1 N1 C4 90.3(2) . . . . ? Cl2 Zr1 N1 C4 -74.66(19) . . . . ? Cl1 Zr1 N1 C4 -173.17(19) . . . . ? C18 Zr1 N1 C4 86.1(2) . . . . ? N2 Zr1 N1 Si1 166.2(3) . . . . ? N3 Zr1 N1 Si1 -123.4(3) . . . . ? N4 Zr1 N1 Si1 -109.7(2) . . . . ? Cl2 Zr1 N1 Si1 85.3(2) . . . . ? Cl1 Zr1 N1 Si1 -13.2(2) . . . . ? C4 Zr1 N1 Si1 160.0(4) . . . . ? C18 Zr1 N1 Si1 -113.9(2) . . . . ? C13 Si2 N2 C4 164.5(3) . . . . ? C12 Si2 N2 C4 47.4(4) . . . . ? C14 Si2 N2 C4 -77.2(4) . . . . ? C13 Si2 N2 Zr1 -34.9(3) . . . . ? C12 Si2 N2 Zr1 -152.0(3) . . . . ? C14 Si2 N2 Zr1 83.4(3) . . . . ? N3 Zr1 N2 C4 -165.90(19) . . . . ? N4 Zr1 N2 C4 -107.2(2) . . . . ? N1 Zr1 N2 C4 -6.34(19) . . . . ? Cl2 Zr1 N2 C4 100.65(19) . . . . ? Cl1 Zr1 N2 C4 -5.2(3) . . . . ? C18 Zr1 N2 C4 -135.7(2) . . . . ? N3 Zr1 N2 Si2 28.6(3) . . . . ? N4 Zr1 N2 Si2 87.3(2) . . . . ? N1 Zr1 N2 Si2 -171.8(3) . . . . ? Cl2 Zr1 N2 Si2 -64.9(2) . . . . ? Cl1 Zr1 N2 Si2 -170.69(12) . . . . ? C4 Zr1 N2 Si2 -165.5(4) . . . . ? C18 Zr1 N2 Si2 58.8(2) . . . . ? C15 Si3 N3 C18 -106.5(4) . . . . ? C16 Si3 N3 C18 16.5(4) . . . . ? C17 Si3 N3 C18 134.0(3) . . . . ? C15 Si3 N3 Zr1 88.5(3) . . . . ? C16 Si3 N3 Zr1 -148.5(3) . . . . ? C17 Si3 N3 Zr1 -31.0(3) . . . . ? N2 Zr1 N3 C18 76.2(2) . . . . ? N4 Zr1 N3 C18 -0.98(19) . . . . ? N1 Zr1 N3 C18 14.4(4) . . . . ? Cl2 Zr1 N3 C18 166.7(2) . . . . ? Cl1 Zr1 N3 C18 -94.6(2) . . . . ? C4 Zr1 N3 C18 65.1(3) . . . . ? N2 Zr1 N3 Si3 -115.2(2) . . . . ? N4 Zr1 N3 Si3 167.7(3) . . . . ? N1 Zr1 N3 Si3 -176.9(2) . . . . ? Cl2 Zr1 N3 Si3 -24.7(2) . . . . ? Cl1 Zr1 N3 Si3 74.0(2) . . . . ? C4 Zr1 N3 Si3 -126.2(2) . . . . ? C18 Zr1 N3 Si3 168.7(4) . . . . ? C27 Si4 N4 C18 30.5(4) . . . . ? C26 Si4 N4 C18 148.6(3) . . . . ? C28 Si4 N4 C18 -93.7(4) . . . . ? C27 Si4 N4 Zr1 -145.5(3) . . . . ? C26 Si4 N4 Zr1 -27.3(3) . . . . ? C28 Si4 N4 Zr1 90.3(3) . . . . ? N2 Zr1 N4 C18 -113.0(2) . . . . ? N3 Zr1 N4 C18 0.98(19) . . . . ? N1 Zr1 N4 C18 -173.67(19) . . . . ? Cl2 Zr1 N4 C18 -26.1(3) . . . . ? Cl1 Zr1 N4 C18 95.09(19) . . . . ? C4 Zr1 N4 C18 -142.4(2) . . . . ? N2 Zr1 N4 Si4 63.9(2) . . . . ? N3 Zr1 N4 Si4 177.9(3) . . . . ? N1 Zr1 N4 Si4 3.2(3) . . . . ? Cl2 Zr1 N4 Si4 150.80(16) . . . . ? Cl1 Zr1 N4 Si4 -88.0(2) . . . . ? C4 Zr1 N4 Si4 34.5(3) . . . . ? C18 Zr1 N4 Si4 176.9(4) . . . . ? Si2 N2 C4 N1 177.0(2) . . . . ? Zr1 N2 C4 N1 10.4(3) . . . . ? Si2 N2 C4 C5 -1.3(5) . . . . ? Zr1 N2 C4 C5 -167.8(3) . . . . ? Si2 N2 C4 Zr1 166.6(3) . . . . ? Si1 N1 C4 N2 -171.9(2) . . . . ? Zr1 N1 C4 N2 -10.2(3) . . . . ? Si1 N1 C4 C5 6.3(5) . . . . ? Zr1 N1 C4 C5 168.0(3) . . . . ? Si1 N1 C4 Zr1 -161.6(3) . . . . ? N3 Zr1 C4 N2 20.7(3) . . . . ? N4 Zr1 C4 N2 74.7(2) . . . . ? N1 Zr1 C4 N2 169.1(3) . . . . ? Cl2 Zr1 C4 N2 -80.4(2) . . . . ? Cl1 Zr1 C4 N2 177.11(17) . . . . ? C18 Zr1 C4 N2 53.4(2) . . . . ? N2 Zr1 C4 N1 -169.1(3) . . . . ? N3 Zr1 C4 N1 -148.44(19) . . . . ? N4 Zr1 C4 N1 -94.5(2) . . . . ? Cl2 Zr1 C4 N1 110.44(19) . . . . ? Cl1 Zr1 C4 N1 8.0(2) . . . . ? C18 Zr1 C4 N1 -115.8(2) . . . . ? N2 Zr1 C4 C5 84.2(14) . . . . ? N3 Zr1 C4 C5 104.9(14) . . . . ? N4 Zr1 C4 C5 158.8(14) . . . . ? N1 Zr1 C4 C5 -106.7(15) . . . . ? Cl2 Zr1 C4 C5 3.8(14) . . . . ? Cl1 Zr1 C4 C5 -98.7(14) . . . . ? C18 Zr1 C4 C5 137.6(14) . . . . ? N2 C4 C5 C6 84.4(4) . . . . ? N1 C4 C5 C6 -93.7(4) . . . . ? Zr1 C4 C5 C6 6.6(16) . . . . ? N2 C4 C5 C10 -94.0(4) . . . . ? N1 C4 C5 C10 87.9(4) . . . . ? Zr1 C4 C5 C10 -171.8(12) . . . . ? C10 C5 C6 C7 -0.4(6) . . . . ? C4 C5 C6 C7 -178.8(4) . . . . ? C5 C6 C7 C8 0.3(6) . . . . ? C6 C7 C8 C9 0.1(6) . . . . ? C11 O1 C9 C8 -176.9(4) . . . . ? C11 O1 C9 C10 2.8(6) . . . . ? C7 C8 C9 O1 179.4(4) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C6 C5 C10 C9 0.1(5) . . . . ? C4 C5 C10 C9 178.5(3) . . . . ? O1 C9 C10 C5 -179.4(3) . . . . ? C8 C9 C10 C5 0.2(6) . . . . ? Si4 N4 C18 N3 -178.9(3) . . . . ? Zr1 N4 C18 N3 -1.6(3) . . . . ? Si4 N4 C18 C19 1.2(5) . . . . ? Zr1 N4 C18 C19 178.5(3) . . . . ? Si4 N4 C18 Zr1 -177.3(3) . . . . ? Si3 N3 C18 N4 -168.0(2) . . . . ? Zr1 N3 C18 N4 1.6(3) . . . . ? Si3 N3 C18 C19 11.9(5) . . . . ? Zr1 N3 C18 C19 -178.5(3) . . . . ? Si3 N3 C18 Zr1 -169.6(3) . . . . ? N2 Zr1 C18 N4 69.5(2) . . . . ? N3 Zr1 C18 N4 -178.3(3) . . . . ? N1 Zr1 C18 N4 8.1(2) . . . . ? Cl2 Zr1 C18 N4 165.75(17) . . . . ? Cl1 Zr1 C18 N4 -88.90(19) . . . . ? C4 Zr1 C18 N4 44.9(2) . . . . ? N2 Zr1 C18 N3 -112.2(2) . . . . ? N4 Zr1 C18 N3 178.3(3) . . . . ? N1 Zr1 C18 N3 -173.57(19) . . . . ? Cl2 Zr1 C18 N3 -15.9(2) . . . . ? Cl1 Zr1 C18 N3 89.4(2) . . . . ? C4 Zr1 C18 N3 -136.7(2) . . . . ? N4 C18 C19 C20 69.6(5) . . . . ? N3 C18 C19 C20 -110.3(4) . . . . ? N4 C18 C19 C24 -111.2(4) . . . . ? N3 C18 C19 C24 68.9(5) . . . . ? C24 C19 C20 C21 -0.9(5) . . . . ? C18 C19 C20 C21 178.3(3) . . . . ? C19 C20 C21 C22 0.9(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C25 O2 C23 C22 -2.7(6) . . . . ? C25 O2 C23 C24 178.4(3) . . . . ? C21 C22 C23 O2 179.6(4) . . . . ? C21 C22 C23 C24 -1.6(6) . . . . ? O2 C23 C24 C19 -179.6(3) . . . . ? C22 C23 C24 C19 1.5(5) . . . . ? C20 C19 C24 C23 -0.3(5) . . . . ? C18 C19 C24 C23 -179.4(3) . . . . ? loop_ # start Validation Reply Form _vrf_THETM01_I ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: . The Scattering power is null after 23 degrees ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.312 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 946664'