# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lutz Gade' _publ_contact_author_email LUTZ.GADE@UNI-HD.DE _publ_section_title ; Zirconium and Hafnium (1-Pyridinio)imido Complexes: Functionalized Terminal Hydrazinediido Analogues ; loop_ _publ_author_name 'Lutz Gade' 'Thorsten Gehrmann' 'Heike Herrmann' 'Hubert Wadepohl' # Attachment 'ga_hh12-ga_tg2b-ga_hh19-ga_hh17-ga_hh25-ga_hh28.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 679492' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H59 F3 N6 O3 S Si2 Zr' _chemical_formula_weight 896.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8684(11) _cell_length_b 13.9752(15) _cell_length_c 15.6286(17) _cell_angle_alpha 82.742(2) _cell_angle_beta 81.840(2) _cell_angle_gamma 75.184(2) _cell_volume 2261.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6318 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43129 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.73 _reflns_number_total 9610 _reflns_number_gt 7017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^)+(0.0760P)^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 9610 _refine_ls_number_parameters 508 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1083(3) 0.1364(2) 0.1294(2) 0.0238(7) Uani 1 1 d . . . H1A H 0.0190 0.1304 0.1318 0.029 Uiso 1 1 calc R . . H1B H 0.1649 0.0739 0.1092 0.029 Uiso 1 1 calc R . . C2 C 0.1263(3) 0.2219(3) 0.0589(2) 0.0228(7) Uani 1 1 d . . . C3 C 0.2638(3) 0.2350(3) 0.0439(2) 0.0305(8) Uani 1 1 d . . . H3A H 0.3204 0.1730 0.0228 0.037 Uiso 1 1 calc R . . H3B H 0.2675 0.2887 -0.0035 0.037 Uiso 1 1 calc R . . C4 C 0.1014(4) 0.1893(3) -0.0261(2) 0.0302(8) Uani 1 1 d . . . H4A H 0.0148 0.1784 -0.0197 0.045 Uiso 1 1 calc R . . H4B H 0.1642 0.1273 -0.0394 0.045 Uiso 1 1 calc R . . H4C H 0.1094 0.2412 -0.0735 0.045 Uiso 1 1 calc R . . C5 C 0.0306(3) 0.3183(2) 0.0808(2) 0.0227(7) Uani 1 1 d . . . C6 C -0.0640(4) 0.3690(3) 0.0286(3) 0.0414(10) Uani 1 1 d . . . H6 H -0.0710 0.3430 -0.0233 0.050 Uiso 1 1 calc R . . C7 C -0.1466(5) 0.4559(3) 0.0514(3) 0.0549(13) Uani 1 1 d . . . H7 H -0.2090 0.4913 0.0146 0.066 Uiso 1 1 calc R . . C8 C -0.1386(4) 0.4914(3) 0.1274(3) 0.0407(10) Uani 1 1 d . . . H8 H -0.1970 0.5504 0.1456 0.049 Uiso 1 1 calc R . . C9 C -0.0430(3) 0.4390(3) 0.1771(2) 0.0285(8) Uani 1 1 d . . . H9 H -0.0352 0.4642 0.2293 0.034 Uiso 1 1 calc R . . C10 C 0.1287(4) 0.0566(3) 0.4019(2) 0.0319(8) Uani 1 1 d . . . H10A H 0.1901 0.0953 0.4078 0.048 Uiso 1 1 calc R . . H10B H 0.1487 -0.0069 0.4379 0.048 Uiso 1 1 calc R . . H10C H 0.0418 0.0939 0.4208 0.048 Uiso 1 1 calc R . . C11 C 0.2970(4) -0.0582(3) 0.2593(3) 0.0384(9) Uani 1 1 d . . . H11A H 0.3076 -0.0700 0.1979 0.058 Uiso 1 1 calc R . . H11B H 0.2986 -0.1211 0.2954 0.058 Uiso 1 1 calc R . . H11C H 0.3669 -0.0309 0.2708 0.058 Uiso 1 1 calc R . . C12 C 0.0065(4) -0.0317(3) 0.2769(2) 0.0328(8) Uani 1 1 d . . . C13 C 0.0236(4) -0.0810(3) 0.1919(3) 0.0418(10) Uani 1 1 d . . . H13A H -0.0416 -0.1187 0.1942 0.063 Uiso 1 1 calc R . . H13B H 0.1090 -0.1261 0.1845 0.063 Uiso 1 1 calc R . . H13C H 0.0143 -0.0296 0.1428 0.063 Uiso 1 1 calc R . . C14 C -0.1254(4) 0.0426(3) 0.2864(3) 0.0456(11) Uani 1 1 d . . . H14A H -0.1290 0.0960 0.2389 0.068 Uiso 1 1 calc R . . H14B H -0.1385 0.0711 0.3421 0.068 Uiso 1 1 calc R . . H14C H -0.1927 0.0082 0.2841 0.068 Uiso 1 1 calc R . . C15 C 0.0084(5) -0.1147(3) 0.3517(3) 0.0490(12) Uani 1 1 d . . . H15A H -0.0624 -0.1459 0.3504 0.073 Uiso 1 1 calc R . . H15B H -0.0012 -0.0864 0.4072 0.073 Uiso 1 1 calc R . . H15C H 0.0899 -0.1648 0.3452 0.073 Uiso 1 1 calc R . . C16 C 0.4800(4) 0.3691(4) 0.0002(4) 0.0590(14) Uani 1 1 d . . . H16A H 0.4547 0.3476 -0.0505 0.089 Uiso 1 1 calc R . . H16B H 0.5676 0.3778 -0.0130 0.089 Uiso 1 1 calc R . . H16C H 0.4214 0.4323 0.0149 0.089 Uiso 1 1 calc R . . C17 C 0.5257(4) 0.3142(4) 0.1893(3) 0.0522(13) Uani 1 1 d . . . H17A H 0.4532 0.3601 0.2191 0.078 Uiso 1 1 calc R . . H17B H 0.5948 0.3480 0.1693 0.078 Uiso 1 1 calc R . . H17C H 0.5567 0.2561 0.2295 0.078 Uiso 1 1 calc R . . C18 C 0.5956(3) 0.1545(3) 0.0643(3) 0.0331(8) Uani 1 1 d . . . C19 C 0.5842(5) 0.1282(5) -0.0268(4) 0.0753(18) Uani 1 1 d . . . H19A H 0.6546 0.0715 -0.0425 0.113 Uiso 1 1 calc R . . H19B H 0.5888 0.1855 -0.0693 0.113 Uiso 1 1 calc R . . H19C H 0.5022 0.1111 -0.0265 0.113 Uiso 1 1 calc R . . C20 C 0.7307(4) 0.1702(4) 0.0589(3) 0.0529(12) Uani 1 1 d . . . H20A H 0.7451 0.1858 0.1155 0.079 Uiso 1 1 calc R . . H20B H 0.7400 0.2254 0.0151 0.079 Uiso 1 1 calc R . . H20C H 0.7936 0.1095 0.0427 0.079 Uiso 1 1 calc R . . C21 C 0.5823(5) 0.0695(4) 0.1307(4) 0.0653(15) Uani 1 1 d . . . H21A H 0.6497 0.0103 0.1164 0.098 Uiso 1 1 calc R . . H21B H 0.4982 0.0557 0.1311 0.098 Uiso 1 1 calc R . . H21C H 0.5904 0.0867 0.1882 0.098 Uiso 1 1 calc R . . C22 C 0.4988(4) 0.0990(3) 0.3857(3) 0.0352(9) Uani 1 1 d . . . H22 H 0.5003 0.0520 0.3464 0.042 Uiso 1 1 calc R . . C23 C 0.5845(4) 0.0759(3) 0.4461(3) 0.0434(11) Uani 1 1 d . . . H23 H 0.6451 0.0134 0.4474 0.052 Uiso 1 1 calc R . . C24 C 0.5845(4) 0.1407(4) 0.5042(3) 0.0506(12) Uani 1 1 d . . . H24 H 0.6424 0.1238 0.5470 0.061 Uiso 1 1 calc R . . C25 C 0.4977(4) 0.2313(4) 0.4988(3) 0.0542(13) Uani 1 1 d . . . H25 H 0.4958 0.2782 0.5382 0.065 Uiso 1 1 calc R . . C26 C 0.4132(4) 0.2553(3) 0.4371(3) 0.0436(10) Uani 1 1 d . . . H26 H 0.3557 0.3191 0.4334 0.052 Uiso 1 1 calc R . . C27 C -0.0881(3) 0.2812(3) 0.3427(2) 0.0292(8) Uani 1 1 d . . . H27 H -0.1001 0.2621 0.2889 0.035 Uiso 1 1 calc R . . C28 C -0.1879(4) 0.2908(3) 0.4084(3) 0.0404(10) Uani 1 1 d . . . H28 H -0.2668 0.2780 0.3999 0.048 Uiso 1 1 calc R . . C29 C -0.1717(5) 0.3196(3) 0.4871(3) 0.0500(12) Uani 1 1 d . . . H29 H -0.2394 0.3271 0.5334 0.060 Uiso 1 1 calc R . . C30 C -0.0565(5) 0.3369(3) 0.4966(3) 0.0449(11) Uani 1 1 d . . . H30 H -0.0431 0.3568 0.5498 0.054 Uiso 1 1 calc R . . C31 C 0.0405(4) 0.3253(3) 0.4282(2) 0.0328(8) Uani 1 1 d . . . H31 H 0.1204 0.3371 0.4357 0.039 Uiso 1 1 calc R . . C32 C 0.2361(6) 0.5976(3) 0.2223(3) 0.0537(13) Uani 1 1 d . . . C33 C 0.3431(5) 0.2844(6) 0.7148(4) 0.097(2) Uani 1 1 d D . . C34 C 0.2419(6) 0.3317(6) 0.6683(4) 0.099(3) Uani 1 1 d D . . H34 H 0.1681 0.3068 0.6692 0.119 Uiso 1 1 calc R . . C35 C 0.2579(6) 0.4172(6) 0.6211(6) 0.125(3) Uani 1 1 d D . . H35 H 0.1881 0.4532 0.5906 0.150 Uiso 1 1 calc R . . C36 C 0.3626(6) 0.4590(6) 0.6114(7) 0.163(5) Uani 1 1 d D . . H36 H 0.3753 0.5141 0.5720 0.196 Uiso 1 1 calc R . . C37 C 0.4436(11) 0.4065(6) 0.6689(6) 0.168(5) Uani 1 1 d D . . H37 H 0.5104 0.4369 0.6749 0.202 Uiso 1 1 calc R . . C38 C 0.4484(5) 0.3190(4) 0.7198(4) 0.0667(16) Uani 1 1 d D . . H38 H 0.5156 0.2867 0.7539 0.080 Uiso 1 1 calc R . . C39 C 0.3340(10) 0.1983(6) 0.7617(5) 0.138(4) Uani 1 1 d D . . H39A H 0.3707 0.1430 0.7258 0.207 Uiso 1 1 calc R . . H39B H 0.2437 0.2001 0.7811 0.207 Uiso 1 1 calc R . . H39C H 0.3811 0.1892 0.8124 0.207 Uiso 1 1 calc R . . F1 F 0.1610(5) 0.6233(3) 0.1609(2) 0.1177(17) Uani 1 1 d . . . F2 F 0.3554(4) 0.5646(2) 0.1869(2) 0.0833(11) Uani 1 1 d . . . F3 F 0.2328(3) 0.67927(18) 0.2594(2) 0.0667(8) Uani 1 1 d . . . N1 N 0.1325(3) 0.1418(2) 0.21874(17) 0.0213(6) Uani 1 1 d . . . N2 N 0.3186(3) 0.2584(2) 0.11755(18) 0.0229(6) Uani 1 1 d . . . N3 N 0.0392(2) 0.3544(2) 0.15475(17) 0.0220(6) Uani 1 1 d . . . N4 N 0.3279(3) 0.2095(2) 0.32374(19) 0.0299(7) Uani 1 1 d . . . N5 N 0.4114(3) 0.1884(2) 0.38119(19) 0.0301(7) Uani 1 1 d . . . N6 N 0.0257(3) 0.2977(2) 0.35159(18) 0.0274(6) Uani 1 1 d . . . O1 O 0.2033(2) 0.42279(18) 0.25118(17) 0.0323(6) Uani 1 1 d . . . O2 O 0.2740(3) 0.4895(2) 0.36613(17) 0.0400(7) Uani 1 1 d . . . O3 O 0.0558(3) 0.5497(2) 0.3303(2) 0.0545(9) Uani 1 1 d . . . S1 S 0.18646(9) 0.50576(7) 0.30299(6) 0.0287(2) Uani 1 1 d . . . Si1 Si 0.13971(9) 0.03241(7) 0.28552(6) 0.0242(2) Uani 1 1 d . . . Si2 Si 0.47301(9) 0.27345(7) 0.09387(7) 0.0270(2) Uani 1 1 d . . . Zr1 Zr 0.20766(3) 0.26082(2) 0.23823(2) 0.02071(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0305(18) 0.0225(17) 0.0193(17) -0.0038(13) -0.0065(14) -0.0052(14) C2 0.0229(17) 0.0303(18) 0.0159(16) -0.0042(13) -0.0013(13) -0.0071(14) C3 0.0264(18) 0.046(2) 0.0227(18) -0.0142(16) 0.0016(14) -0.0131(16) C4 0.036(2) 0.042(2) 0.0172(17) -0.0071(15) -0.0055(15) -0.0133(17) C5 0.0246(17) 0.0240(17) 0.0215(17) 0.0010(13) -0.0063(13) -0.0088(14) C6 0.051(3) 0.038(2) 0.037(2) -0.0048(18) -0.026(2) -0.0030(19) C7 0.058(3) 0.041(3) 0.063(3) -0.006(2) -0.038(3) 0.012(2) C8 0.037(2) 0.029(2) 0.052(3) -0.0081(18) -0.0142(19) 0.0054(17) C9 0.0268(18) 0.0235(18) 0.034(2) -0.0031(15) -0.0053(15) -0.0030(14) C10 0.040(2) 0.032(2) 0.0195(18) -0.0001(15) -0.0070(15) 0.0002(16) C11 0.043(2) 0.030(2) 0.034(2) -0.0065(17) -0.0073(18) 0.0091(17) C12 0.044(2) 0.033(2) 0.0230(19) -0.0017(15) -0.0012(16) -0.0146(17) C13 0.061(3) 0.039(2) 0.032(2) -0.0059(18) -0.004(2) -0.024(2) C14 0.031(2) 0.051(3) 0.057(3) -0.009(2) 0.000(2) -0.0154(19) C15 0.078(3) 0.043(3) 0.032(2) 0.0038(19) -0.005(2) -0.031(2) C16 0.038(2) 0.050(3) 0.086(4) 0.025(3) -0.006(2) -0.022(2) C17 0.028(2) 0.070(3) 0.070(3) -0.044(3) -0.003(2) -0.016(2) C18 0.0177(17) 0.040(2) 0.038(2) -0.0092(17) 0.0004(15) 0.0000(15) C19 0.049(3) 0.093(4) 0.077(4) -0.055(3) -0.010(3) 0.020(3) C20 0.023(2) 0.060(3) 0.068(3) -0.001(2) -0.001(2) -0.002(2) C21 0.047(3) 0.043(3) 0.088(4) 0.007(3) 0.013(3) 0.004(2) C22 0.0282(19) 0.043(2) 0.032(2) 0.0054(17) -0.0050(16) -0.0064(17) C23 0.028(2) 0.054(3) 0.042(2) 0.017(2) -0.0092(18) -0.0061(19) C24 0.038(2) 0.087(4) 0.030(2) 0.015(2) -0.0176(19) -0.023(2) C25 0.039(2) 0.084(4) 0.044(3) -0.016(2) -0.019(2) -0.011(2) C26 0.034(2) 0.057(3) 0.043(2) -0.017(2) -0.0182(19) -0.0018(19) C27 0.0273(18) 0.0281(19) 0.0286(19) -0.0065(15) 0.0001(15) -0.0003(15) C28 0.034(2) 0.036(2) 0.044(2) -0.0013(18) 0.0119(18) -0.0056(17) C29 0.054(3) 0.046(3) 0.035(2) -0.007(2) 0.022(2) 0.002(2) C30 0.062(3) 0.039(2) 0.025(2) -0.0106(17) 0.0049(19) 0.000(2) C31 0.041(2) 0.030(2) 0.0244(19) -0.0058(15) -0.0018(16) -0.0028(17) C32 0.084(4) 0.043(3) 0.044(3) 0.000(2) -0.029(3) -0.024(3) C33 0.098(5) 0.099(6) 0.094(5) -0.044(4) 0.036(4) -0.030(4) C34 0.060(4) 0.128(6) 0.082(5) -0.038(4) -0.034(3) 0.054(4) C35 0.036(3) 0.106(6) 0.233(11) -0.046(7) -0.020(5) -0.003(4) C36 0.095(6) 0.077(5) 0.257(13) 0.057(7) 0.032(7) 0.025(5) C37 0.232(12) 0.112(7) 0.145(9) -0.075(7) -0.101(8) 0.060(8) C38 0.045(3) 0.064(3) 0.096(4) -0.038(3) -0.033(3) 0.006(3) C39 0.207(10) 0.094(6) 0.070(5) -0.004(4) 0.069(6) -0.006(6) F1 0.207(5) 0.097(3) 0.083(3) 0.041(2) -0.102(3) -0.077(3) F2 0.119(3) 0.083(2) 0.0572(19) -0.0152(16) 0.0298(19) -0.058(2) F3 0.092(2) 0.0320(14) 0.085(2) -0.0027(14) -0.0306(18) -0.0216(14) N1 0.0225(14) 0.0243(15) 0.0164(13) -0.0051(11) -0.0031(11) -0.0022(11) N2 0.0188(14) 0.0288(15) 0.0215(14) -0.0075(12) -0.0018(11) -0.0043(12) N3 0.0203(14) 0.0234(15) 0.0215(14) -0.0015(11) -0.0032(11) -0.0034(11) N4 0.0245(15) 0.0393(18) 0.0268(16) -0.0083(13) -0.0088(13) -0.0037(13) N5 0.0224(15) 0.0426(19) 0.0253(16) -0.0023(14) -0.0062(12) -0.0068(13) N6 0.0322(16) 0.0260(16) 0.0195(15) -0.0066(12) 0.0008(12) 0.0011(13) O1 0.0319(14) 0.0300(14) 0.0373(15) -0.0160(11) -0.0024(11) -0.0063(11) O2 0.0475(17) 0.0429(16) 0.0339(15) -0.0058(12) -0.0159(13) -0.0113(13) O3 0.0324(16) 0.059(2) 0.075(2) -0.0419(18) -0.0037(15) -0.0008(14) S1 0.0296(5) 0.0306(5) 0.0283(5) -0.0124(4) -0.0046(4) -0.0064(4) Si1 0.0275(5) 0.0238(5) 0.0185(5) -0.0039(4) -0.0021(4) -0.0004(4) Si2 0.0202(5) 0.0286(5) 0.0331(5) -0.0067(4) 0.0004(4) -0.0077(4) Zr1 0.01763(17) 0.02610(19) 0.01823(18) -0.00784(12) -0.00398(12) -0.00116(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.473(4) . ? C1 C2 1.551(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.520(5) . ? C2 C3 1.534(5) . ? C2 C4 1.539(4) . ? C3 N2 1.474(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.342(4) . ? C5 C6 1.395(5) . ? C6 C7 1.367(6) . ? C6 H6 0.9500 . ? C7 C8 1.366(6) . ? C7 H7 0.9500 . ? C8 C9 1.385(5) . ? C8 H8 0.9500 . ? C9 N3 1.340(4) . ? C9 H9 0.9500 . ? C10 Si1 1.873(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.876(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.538(5) . ? C12 C13 1.539(5) . ? C12 C14 1.541(6) . ? C12 Si1 1.915(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.860(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.871(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.498(6) . ? C18 C20 1.529(5) . ? C18 C19 1.543(6) . ? C18 Si2 1.908(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N5 1.362(5) . ? C22 C23 1.372(5) . ? C22 H22 0.9500 . ? C23 C24 1.361(7) . ? C23 H23 0.9500 . ? C24 C25 1.373(7) . ? C24 H24 0.9500 . ? C25 C26 1.377(6) . ? C25 H25 0.9500 . ? C26 N5 1.363(5) . ? C26 H26 0.9500 . ? C27 N6 1.343(5) . ? C27 C28 1.375(5) . ? C27 H27 0.9500 . ? C28 C29 1.389(6) . ? C28 H28 0.9500 . ? C29 C30 1.366(7) . ? C29 H29 0.9500 . ? C30 C31 1.385(5) . ? C30 H30 0.9500 . ? C31 N6 1.346(4) . ? C31 H31 0.9500 . ? C32 F1 1.305(5) . ? C32 F2 1.326(6) . ? C32 F3 1.334(5) . ? C32 S1 1.811(5) . ? C33 C39 1.346(9) . ? C33 C38 1.367(5) . ? C33 C34 1.380(6) . ? C34 C35 1.361(8) . ? C34 H34 0.9500 . ? C35 C36 1.389(7) . ? C35 H35 0.9500 . ? C36 C37 1.359(7) . ? C36 H36 0.9500 . ? C37 C38 1.365(9) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? N1 Si1 1.730(3) . ? N1 Zr1 2.102(3) . ? N2 Si2 1.727(3) . ? N2 Zr1 2.088(3) . ? N3 Zr1 2.405(3) . ? N4 N5 1.321(4) . ? N4 Zr1 1.945(3) . ? N6 Zr1 2.456(3) . ? O1 S1 1.456(2) . ? O1 Zr1 2.286(2) . ? O2 S1 1.425(3) . ? O3 S1 1.422(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 119.1(3) . . ? N1 C1 H1A 107.5 . . ? C2 C1 H1A 107.5 . . ? N1 C1 H1B 107.5 . . ? C2 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C5 C2 C3 111.3(3) . . ? C5 C2 C4 110.6(3) . . ? C3 C2 C4 106.1(3) . . ? C5 C2 C1 110.3(3) . . ? C3 C2 C1 113.1(3) . . ? C4 C2 C1 105.3(3) . . ? N2 C3 C2 118.3(3) . . ? N2 C3 H3A 107.7 . . ? C2 C3 H3A 107.7 . . ? N2 C3 H3B 107.7 . . ? C2 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 119.6(3) . . ? N3 C5 C2 117.0(3) . . ? C6 C5 C2 123.3(3) . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 118.0(4) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? N3 C9 C8 122.8(3) . . ? N3 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 106.9(3) . . ? C15 C12 C14 108.1(3) . . ? C13 C12 C14 109.4(3) . . ? C15 C12 Si1 108.3(3) . . ? C13 C12 Si1 113.4(3) . . ? C14 C12 Si1 110.4(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C20 109.2(4) . . ? C21 C18 C19 110.2(4) . . ? C20 C18 C19 105.2(4) . . ? C21 C18 Si2 110.9(3) . . ? C20 C18 Si2 109.5(3) . . ? C19 C18 Si2 111.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 121.0(4) . . ? N5 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 121.4(4) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 117.5(4) . . ? C23 C24 H24 121.2 . . ? C25 C24 H24 121.2 . . ? C24 C25 C26 121.1(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? N5 C26 C25 120.7(4) . . ? N5 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N6 C27 C28 122.7(4) . . ? N6 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 118.6(4) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C29 C30 C31 119.5(4) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? N6 C31 C30 122.4(4) . . ? N6 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? F1 C32 F2 108.9(5) . . ? F1 C32 F3 107.8(4) . . ? F2 C32 F3 107.0(4) . . ? F1 C32 S1 111.7(4) . . ? F2 C32 S1 111.4(3) . . ? F3 C32 S1 109.9(3) . . ? C39 C33 C38 117.5(7) . . ? C39 C33 C34 116.5(7) . . ? C38 C33 C34 125.9(8) . . ? C35 C34 C33 113.7(8) . . ? C35 C34 H34 123.2 . . ? C33 C34 H34 123.2 . . ? C34 C35 C36 128.7(8) . . ? C34 C35 H35 115.7 . . ? C36 C35 H35 115.7 . . ? C37 C36 C35 107.3(9) . . ? C37 C36 H36 126.3 . . ? C35 C36 H36 126.3 . . ? C36 C37 C38 133.0(9) . . ? C36 C37 H37 113.5 . . ? C38 C37 H37 113.5 . . ? C37 C38 C33 110.5(7) . . ? C37 C38 H38 124.7 . . ? C33 C38 H38 124.7 . . ? C33 C39 H39A 109.5 . . ? C33 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C33 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C1 N1 Si1 114.5(2) . . ? C1 N1 Zr1 116.2(2) . . ? Si1 N1 Zr1 126.49(14) . . ? C3 N2 Si2 114.9(2) . . ? C3 N2 Zr1 117.3(2) . . ? Si2 N2 Zr1 127.65(15) . . ? C9 N3 C5 119.4(3) . . ? C9 N3 Zr1 124.2(2) . . ? C5 N3 Zr1 116.4(2) . . ? N5 N4 Zr1 171.4(3) . . ? N4 N5 C22 120.6(3) . . ? N4 N5 C26 121.1(3) . . ? C22 N5 C26 118.2(3) . . ? C27 N6 C31 117.7(3) . . ? C27 N6 Zr1 121.1(2) . . ? C31 N6 Zr1 120.9(2) . . ? S1 O1 Zr1 151.59(17) . . ? O3 S1 O2 116.84(18) . . ? O3 S1 O1 113.28(16) . . ? O2 S1 O1 114.45(16) . . ? O3 S1 C32 104.3(2) . . ? O2 S1 C32 104.37(19) . . ? O1 S1 C32 101.15(19) . . ? N1 Si1 C10 110.25(15) . . ? N1 Si1 C11 110.01(16) . . ? C10 Si1 C11 107.41(17) . . ? N1 Si1 C12 114.18(15) . . ? C10 Si1 C12 107.12(17) . . ? C11 Si1 C12 107.61(19) . . ? N2 Si2 C16 109.55(17) . . ? N2 Si2 C17 110.71(17) . . ? C16 Si2 C17 108.9(2) . . ? N2 Si2 C18 113.23(15) . . ? C16 Si2 C18 107.6(2) . . ? C17 Si2 C18 106.71(19) . . ? N4 Zr1 N2 105.85(12) . . ? N4 Zr1 N1 106.37(12) . . ? N2 Zr1 N1 93.85(10) . . ? N4 Zr1 O1 93.32(11) . . ? N2 Zr1 O1 93.74(10) . . ? N1 Zr1 O1 156.03(10) . . ? N4 Zr1 N3 166.64(11) . . ? N2 Zr1 N3 83.27(10) . . ? N1 Zr1 N3 82.28(10) . . ? O1 Zr1 N3 76.09(9) . . ? N4 Zr1 N6 92.05(11) . . ? N2 Zr1 N6 161.56(10) . . ? N1 Zr1 N6 85.11(10) . . ? O1 Zr1 N6 80.57(9) . . ? N3 Zr1 N6 78.34(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C5 -64.1(4) . . . . ? N1 C1 C2 C3 61.3(4) . . . . ? N1 C1 C2 C4 176.6(3) . . . . ? C5 C2 C3 N2 64.7(4) . . . . ? C4 C2 C3 N2 -175.0(3) . . . . ? C1 C2 C3 N2 -60.1(4) . . . . ? C3 C2 C5 N3 -63.9(4) . . . . ? C4 C2 C5 N3 178.5(3) . . . . ? C1 C2 C5 N3 62.5(4) . . . . ? C3 C2 C5 C6 116.6(4) . . . . ? C4 C2 C5 C6 -1.1(5) . . . . ? C1 C2 C5 C6 -117.1(4) . . . . ? N3 C5 C6 C7 1.0(6) . . . . ? C2 C5 C6 C7 -179.4(4) . . . . ? C5 C6 C7 C8 -2.0(7) . . . . ? C6 C7 C8 C9 2.3(7) . . . . ? C7 C8 C9 N3 -1.7(6) . . . . ? N5 C22 C23 C24 0.8(6) . . . . ? C22 C23 C24 C25 -1.7(6) . . . . ? C23 C24 C25 C26 0.4(7) . . . . ? C24 C25 C26 N5 1.8(7) . . . . ? N6 C27 C28 C29 0.6(6) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C28 C29 C30 C31 -0.2(6) . . . . ? C29 C30 C31 N6 0.4(6) . . . . ? C39 C33 C34 C35 -178.8(6) . . . . ? C38 C33 C34 C35 3.7(7) . . . . ? C33 C34 C35 C36 2.9(9) . . . . ? C34 C35 C36 C37 -8.9(11) . . . . ? C35 C36 C37 C38 11.0(14) . . . . ? C36 C37 C38 C33 -6.0(13) . . . . ? C39 C33 C38 C37 -180.0(6) . . . . ? C34 C33 C38 C37 -2.5(8) . . . . ? C2 C1 N1 Si1 -168.0(2) . . . . ? C2 C1 N1 Zr1 -5.9(4) . . . . ? C2 C3 N2 Si2 -179.1(3) . . . . ? C2 C3 N2 Zr1 4.5(4) . . . . ? C8 C9 N3 C5 0.7(5) . . . . ? C8 C9 N3 Zr1 179.7(3) . . . . ? C6 C5 N3 C9 -0.4(5) . . . . ? C2 C5 N3 C9 -179.9(3) . . . . ? C6 C5 N3 Zr1 -179.4(3) . . . . ? C2 C5 N3 Zr1 1.0(4) . . . . ? Zr1 N4 N5 C22 -145.3(16) . . . . ? Zr1 N4 N5 C26 34.3(19) . . . . ? C23 C22 N5 N4 -178.9(3) . . . . ? C23 C22 N5 C26 1.5(5) . . . . ? C25 C26 N5 N4 177.7(4) . . . . ? C25 C26 N5 C22 -2.7(6) . . . . ? C28 C27 N6 C31 -0.4(5) . . . . ? C28 C27 N6 Zr1 172.9(3) . . . . ? C30 C31 N6 C27 -0.1(5) . . . . ? C30 C31 N6 Zr1 -173.4(3) . . . . ? Zr1 O1 S1 O3 -76.9(4) . . . . ? Zr1 O1 S1 O2 60.4(4) . . . . ? Zr1 O1 S1 C32 172.0(3) . . . . ? F1 C32 S1 O3 -54.5(4) . . . . ? F2 C32 S1 O3 -176.5(3) . . . . ? F3 C32 S1 O3 65.1(4) . . . . ? F1 C32 S1 O2 -177.6(4) . . . . ? F2 C32 S1 O2 60.4(3) . . . . ? F3 C32 S1 O2 -58.0(4) . . . . ? F1 C32 S1 O1 63.3(4) . . . . ? F2 C32 S1 O1 -58.7(3) . . . . ? F3 C32 S1 O1 -177.1(3) . . . . ? C1 N1 Si1 C10 -165.6(2) . . . . ? Zr1 N1 Si1 C10 34.5(2) . . . . ? C1 N1 Si1 C11 76.1(3) . . . . ? Zr1 N1 Si1 C11 -83.8(2) . . . . ? C1 N1 Si1 C12 -45.0(3) . . . . ? Zr1 N1 Si1 C12 155.09(17) . . . . ? C15 C12 Si1 N1 -168.7(3) . . . . ? C13 C12 Si1 N1 72.8(3) . . . . ? C14 C12 Si1 N1 -50.5(3) . . . . ? C15 C12 Si1 C10 -46.3(3) . . . . ? C13 C12 Si1 C10 -164.9(3) . . . . ? C14 C12 Si1 C10 71.9(3) . . . . ? C15 C12 Si1 C11 68.9(3) . . . . ? C13 C12 Si1 C11 -49.6(3) . . . . ? C14 C12 Si1 C11 -172.9(3) . . . . ? C3 N2 Si2 C16 54.6(3) . . . . ? Zr1 N2 Si2 C16 -129.4(2) . . . . ? C3 N2 Si2 C17 174.7(3) . . . . ? Zr1 N2 Si2 C17 -9.3(3) . . . . ? C3 N2 Si2 C18 -65.5(3) . . . . ? Zr1 N2 Si2 C18 110.5(2) . . . . ? C21 C18 Si2 N2 -50.3(4) . . . . ? C20 C18 Si2 N2 -170.9(3) . . . . ? C19 C18 Si2 N2 73.0(4) . . . . ? C21 C18 Si2 C16 -171.5(3) . . . . ? C20 C18 Si2 C16 67.9(3) . . . . ? C19 C18 Si2 C16 -48.2(4) . . . . ? C21 C18 Si2 C17 71.7(4) . . . . ? C20 C18 Si2 C17 -48.8(3) . . . . ? C19 C18 Si2 C17 -164.9(4) . . . . ? N5 N4 Zr1 N2 85.1(17) . . . . ? N5 N4 Zr1 N1 -175.9(17) . . . . ? N5 N4 Zr1 O1 -9.8(17) . . . . ? N5 N4 Zr1 N3 -47(2) . . . . ? N5 N4 Zr1 N6 -90.4(17) . . . . ? C3 N2 Zr1 N4 144.7(3) . . . . ? Si2 N2 Zr1 N4 -31.2(2) . . . . ? C3 N2 Zr1 N1 36.5(3) . . . . ? Si2 N2 Zr1 N1 -139.40(19) . . . . ? C3 N2 Zr1 O1 -120.8(3) . . . . ? Si2 N2 Zr1 O1 63.35(19) . . . . ? C3 N2 Zr1 N3 -45.3(2) . . . . ? Si2 N2 Zr1 N3 138.8(2) . . . . ? C3 N2 Zr1 N6 -49.6(5) . . . . ? Si2 N2 Zr1 N6 134.5(3) . . . . ? C1 N1 Zr1 N4 -143.1(2) . . . . ? Si1 N1 Zr1 N4 16.5(2) . . . . ? C1 N1 Zr1 N2 -35.4(2) . . . . ? Si1 N1 Zr1 N2 124.27(18) . . . . ? C1 N1 Zr1 O1 72.8(3) . . . . ? Si1 N1 Zr1 O1 -127.5(2) . . . . ? C1 N1 Zr1 N3 47.3(2) . . . . ? Si1 N1 Zr1 N3 -153.07(18) . . . . ? C1 N1 Zr1 N6 126.2(2) . . . . ? Si1 N1 Zr1 N6 -74.20(18) . . . . ? S1 O1 Zr1 N4 -52.7(3) . . . . ? S1 O1 Zr1 N2 -158.9(3) . . . . ? S1 O1 Zr1 N1 92.9(4) . . . . ? S1 O1 Zr1 N3 119.0(3) . . . . ? S1 O1 Zr1 N6 38.8(3) . . . . ? C9 N3 Zr1 N4 0.7(6) . . . . ? C5 N3 Zr1 N4 179.7(4) . . . . ? C9 N3 Zr1 N2 -133.1(3) . . . . ? C5 N3 Zr1 N2 45.8(2) . . . . ? C9 N3 Zr1 N1 132.0(3) . . . . ? C5 N3 Zr1 N1 -49.0(2) . . . . ? C9 N3 Zr1 O1 -37.6(3) . . . . ? C5 N3 Zr1 O1 141.4(2) . . . . ? C9 N3 Zr1 N6 45.4(3) . . . . ? C5 N3 Zr1 N6 -135.6(2) . . . . ? C27 N6 Zr1 N4 -140.4(3) . . . . ? C31 N6 Zr1 N4 32.6(3) . . . . ? C27 N6 Zr1 N2 53.3(5) . . . . ? C31 N6 Zr1 N2 -133.6(3) . . . . ? C27 N6 Zr1 N1 -34.2(3) . . . . ? C31 N6 Zr1 N1 138.9(3) . . . . ? C27 N6 Zr1 O1 126.5(3) . . . . ? C31 N6 Zr1 O1 -60.4(3) . . . . ? C27 N6 Zr1 N3 48.9(3) . . . . ? C31 N6 Zr1 N3 -138.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.157 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.092 _audit_block_code ga_hh12 _audit_block_refno 419 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 687175' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H59 F3 Hf N6 O3 S Si2' _chemical_formula_weight 983.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8631(7) _cell_length_b 13.8086(9) _cell_length_c 31.0427(19) _cell_angle_alpha 83.6470(10) _cell_angle_beta 82.7360(10) _cell_angle_gamma 75.6280(10) _cell_volume 4459.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 2.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4157 _exptl_absorpt_correction_T_max 0.4949 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 111883 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 0.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15688 _reflns_number_gt 14493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'DIRDIF (Beurskens, 1999-2007)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^)+(0.0071P)^2^+32.2440P] 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 15688 _refine_ls_number_parameters 1015 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.335 _refine_ls_restrained_S_all 1.335 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7277(6) 0.7503(5) 0.23208(18) 0.0203(13) Uani 1 1 d . . . H1A H 0.7316 0.6940 0.2550 0.024 Uiso 1 1 calc R . . H1B H 0.6715 0.8107 0.2447 0.024 Uiso 1 1 calc R . . C2 C 0.8633(5) 0.7687(4) 0.22156(18) 0.0178(12) Uani 1 1 d . . . C3 C 0.8718(6) 0.8528(4) 0.18469(18) 0.0194(12) Uani 1 1 d . . . H3A H 0.8119 0.9153 0.1940 0.023 Uiso 1 1 calc R . . H3B H 0.9590 0.8641 0.1821 0.023 Uiso 1 1 calc R . . C4 C 0.8935(6) 0.8069(5) 0.26239(19) 0.0225(13) Uani 1 1 d . . . H4A H 0.8892 0.7566 0.2871 0.034 Uiso 1 1 calc R . . H4B H 0.8312 0.8696 0.2688 0.034 Uiso 1 1 calc R . . H4C H 0.9796 0.8190 0.2576 0.034 Uiso 1 1 calc R . . C5 C 0.9588(5) 0.6721(4) 0.21043(19) 0.0184(12) Uani 1 1 d . . . C6 C 1.0599(6) 0.6256(5) 0.2353(2) 0.0254(14) Uani 1 1 d . . . H6 H 1.0714 0.6549 0.2604 0.030 Uiso 1 1 calc R . . C7 C 1.1420(6) 0.5378(5) 0.2235(2) 0.0324(16) Uani 1 1 d . . . H7 H 1.2102 0.5061 0.2404 0.039 Uiso 1 1 calc R . . C8 C 1.1256(6) 0.4960(5) 0.1873(2) 0.0286(15) Uani 1 1 d . . . H8 H 1.1825 0.4357 0.1784 0.034 Uiso 1 1 calc R . . C9 C 1.0245(6) 0.5435(5) 0.1641(2) 0.0259(14) Uani 1 1 d . . . H9 H 1.0119 0.5139 0.1393 0.031 Uiso 1 1 calc R . . C10 C 0.4568(7) 0.6469(5) 0.1722(2) 0.0336(16) Uani 1 1 d . . . H10A H 0.4742 0.6733 0.1420 0.050 Uiso 1 1 calc R . . H10B H 0.3651 0.6511 0.1787 0.050 Uiso 1 1 calc R . . H10C H 0.5042 0.5768 0.1761 0.050 Uiso 1 1 calc R . . C11 C 0.4880(7) 0.6605(5) 0.2667(2) 0.0347(16) Uani 1 1 d . . . H11A H 0.5484 0.5948 0.2688 0.052 Uiso 1 1 calc R . . H11B H 0.4005 0.6519 0.2733 0.052 Uiso 1 1 calc R . . H11C H 0.5046 0.7028 0.2876 0.052 Uiso 1 1 calc R . . C12 C 0.3914(6) 0.8502(5) 0.2100(2) 0.0238(14) Uani 1 1 d . . . C13 C 0.3866(7) 0.8982(6) 0.1626(3) 0.047(2) Uani 1 1 d . . . H13A H 0.3308 0.9659 0.1624 0.070 Uiso 1 1 calc R . . H13B H 0.3531 0.8572 0.1453 0.070 Uiso 1 1 calc R . . H13C H 0.4729 0.9019 0.1500 0.070 Uiso 1 1 calc R . . C14 C 0.2564(6) 0.8411(5) 0.2270(3) 0.0358(17) Uani 1 1 d . . . H14A H 0.2548 0.8137 0.2575 0.054 Uiso 1 1 calc R . . H14B H 0.2300 0.7963 0.2096 0.054 Uiso 1 1 calc R . . H14C H 0.1975 0.9075 0.2249 0.054 Uiso 1 1 calc R . . C15 C 0.4315(7) 0.9211(6) 0.2364(3) 0.050(2) Uani 1 1 d . . . H15A H 0.3678 0.9853 0.2361 0.075 Uiso 1 1 calc R . . H15B H 0.5146 0.9321 0.2236 0.075 Uiso 1 1 calc R . . H15C H 0.4380 0.8918 0.2665 0.075 Uiso 1 1 calc R . . C16 C 0.6791(6) 1.0397(5) 0.1201(2) 0.0262(14) Uani 1 1 d . . . H16A H 0.6082 1.0183 0.1104 0.039 Uiso 1 1 calc R . . H16B H 0.6828 1.1059 0.1057 0.039 Uiso 1 1 calc R . . H16C H 0.6657 1.0433 0.1517 0.039 Uiso 1 1 calc R . . C17 C 0.8340(6) 0.9157(5) 0.04798(19) 0.0258(14) Uani 1 1 d . . . H17A H 0.9198 0.8783 0.0376 0.039 Uiso 1 1 calc R . . H17B H 0.8103 0.9778 0.0292 0.039 Uiso 1 1 calc R . . H17C H 0.7726 0.8748 0.0472 0.039 Uiso 1 1 calc R . . C18 C 0.9670(6) 1.0139(5) 0.1058(2) 0.0254(14) Uani 1 1 d . . . C19 C 0.9603(7) 1.0667(5) 0.1475(2) 0.0302(15) Uani 1 1 d . . . H19A H 1.0191 1.1113 0.1429 0.045 Uiso 1 1 calc R . . H19B H 0.9845 1.0163 0.1717 0.045 Uiso 1 1 calc R . . H19C H 0.8730 1.1061 0.1545 0.045 Uiso 1 1 calc R . . C20 C 1.0989(6) 0.9402(5) 0.0989(3) 0.0364(17) Uani 1 1 d . . . H20A H 1.1059 0.9093 0.0714 0.055 Uiso 1 1 calc R . . H20B H 1.1085 0.8879 0.1231 0.055 Uiso 1 1 calc R . . H20C H 1.1663 0.9767 0.0976 0.055 Uiso 1 1 calc R . . C21 C 0.9569(7) 1.0950(5) 0.0674(2) 0.0361(17) Uani 1 1 d . . . H21A H 1.0220 1.1328 0.0678 0.054 Uiso 1 1 calc R . . H21B H 0.8719 1.1407 0.0701 0.054 Uiso 1 1 calc R . . H21C H 0.9702 1.0632 0.0400 0.054 Uiso 1 1 calc R . . C22 C 0.5006(6) 0.8796(5) 0.0522(2) 0.0308(15) Uani 1 1 d . . . H22 H 0.5114 0.9320 0.0677 0.037 Uiso 1 1 calc R . . C23 C 0.4202(7) 0.9025(6) 0.0200(2) 0.0401(19) Uani 1 1 d . . . H23 H 0.3758 0.9701 0.0137 0.048 Uiso 1 1 calc R . . C24 C 0.4030(7) 0.8290(7) -0.0034(2) 0.046(2) Uani 1 1 d . . . H24 H 0.3491 0.8448 -0.0262 0.055 Uiso 1 1 calc R . . C25 C 0.4674(7) 0.7301(7) 0.0076(3) 0.045(2) Uani 1 1 d . . . H25 H 0.4559 0.6773 -0.0075 0.055 Uiso 1 1 calc R . . C26 C 0.5467(7) 0.7088(6) 0.0400(2) 0.0367(17) Uani 1 1 d . . . H26 H 0.5896 0.6411 0.0471 0.044 Uiso 1 1 calc R . . C27 C 1.0526(6) 0.6972(5) 0.0801(2) 0.0272(15) Uani 1 1 d . . . H27 H 1.0683 0.7178 0.1067 0.033 Uiso 1 1 calc R . . C28 C 1.1485(7) 0.6893(5) 0.0455(2) 0.0336(16) Uani 1 1 d . . . H28 H 1.2275 0.7050 0.0481 0.040 Uiso 1 1 calc R . . C29 C 1.1250(7) 0.6579(5) 0.0070(2) 0.0372(18) Uani 1 1 d . . . H29 H 1.1885 0.6510 -0.0172 0.045 Uiso 1 1 calc R . . C30 C 1.0102(7) 0.6370(5) 0.0041(2) 0.0353(17) Uani 1 1 d . . . H30 H 0.9928 0.6152 -0.0219 0.042 Uiso 1 1 calc R . . C31 C 0.9201(7) 0.6483(5) 0.0397(2) 0.0312(15) Uani 1 1 d . . . H31 H 0.8397 0.6349 0.0373 0.037 Uiso 1 1 calc R . . C32 C 0.7386(8) 0.3719(6) 0.1429(2) 0.0400(18) Uani 1 1 d . . . C51 C 0.1014(5) 0.1330(4) 0.31189(18) 0.0154(12) Uani 1 1 d . . . H51A H 0.0125 0.1268 0.3121 0.019 Uiso 1 1 calc R . . H51B H 0.1582 0.0703 0.3015 0.019 Uiso 1 1 calc R . . C52 C 0.1207(5) 0.2207(4) 0.27759(18) 0.0145(11) Uani 1 1 d . . . C53 C 0.2605(5) 0.2332(4) 0.27251(18) 0.0174(12) Uani 1 1 d . . . H53A H 0.3175 0.1695 0.2633 0.021 Uiso 1 1 calc R . . H53B H 0.2681 0.2855 0.2484 0.021 Uiso 1 1 calc R . . C54 C 0.0999(6) 0.1876(5) 0.23396(18) 0.0194(12) Uani 1 1 d . . . H54A H 0.0130 0.1780 0.2355 0.029 Uiso 1 1 calc R . . H54B H 0.1617 0.1244 0.2280 0.029 Uiso 1 1 calc R . . H54C H 0.1117 0.2393 0.2106 0.029 Uiso 1 1 calc R . . C55 C 0.0246(5) 0.3169(4) 0.28887(18) 0.0151(12) Uani 1 1 d . . . C56 C -0.0664(6) 0.3696(4) 0.26117(19) 0.0205(13) Uani 1 1 d . . . H56 H -0.0688 0.3459 0.2338 0.025 Uiso 1 1 calc R . . C57 C -0.1522(6) 0.4555(5) 0.2737(2) 0.0259(14) Uani 1 1 d . . . H57 H -0.2145 0.4911 0.2551 0.031 Uiso 1 1 calc R . . C58 C -0.1471(6) 0.4896(4) 0.3135(2) 0.0234(13) Uani 1 1 d . . . H58 H -0.2063 0.5483 0.3230 0.028 Uiso 1 1 calc R . . C59 C -0.0538(5) 0.4363(4) 0.33900(19) 0.0174(12) Uani 1 1 d . . . H59 H -0.0495 0.4600 0.3662 0.021 Uiso 1 1 calc R . . C60 C 0.1235(6) 0.0501(4) 0.44874(18) 0.0196(12) Uani 1 1 d . . . H60A H 0.1899 0.0845 0.4524 0.029 Uiso 1 1 calc R . . H60B H 0.1375 -0.0142 0.4665 0.029 Uiso 1 1 calc R . . H60C H 0.0394 0.0919 0.4581 0.029 Uiso 1 1 calc R . . C61 C 0.2844(6) -0.0660(5) 0.3760(2) 0.0268(14) Uani 1 1 d . . . H61A H 0.2924 -0.0773 0.3450 0.040 Uiso 1 1 calc R . . H61B H 0.2849 -0.1294 0.3937 0.040 Uiso 1 1 calc R . . H61C H 0.3563 -0.0401 0.3818 0.040 Uiso 1 1 calc R . . C62 C -0.0054(6) -0.0354(4) 0.38569(19) 0.0203(13) Uani 1 1 d . . . C63 C -0.1346(6) 0.0413(5) 0.3895(2) 0.0272(14) Uani 1 1 d . . . H63A H -0.2033 0.0076 0.3880 0.041 Uiso 1 1 calc R . . H63B H -0.1361 0.0939 0.3655 0.041 Uiso 1 1 calc R . . H63C H -0.1471 0.0714 0.4173 0.041 Uiso 1 1 calc R . . C64 C 0.0101(7) -0.0859(5) 0.3429(2) 0.0267(14) Uani 1 1 d . . . H64A H 0.0947 -0.1319 0.3394 0.040 Uiso 1 1 calc R . . H64B H 0.0014 -0.0344 0.3183 0.040 Uiso 1 1 calc R . . H64C H -0.0560 -0.1234 0.3438 0.040 Uiso 1 1 calc R . . C65 C -0.0072(7) -0.1172(5) 0.4231(2) 0.0298(15) Uani 1 1 d . . . H65A H -0.0230 -0.0869 0.4510 0.045 Uiso 1 1 calc R . . H65B H 0.0754 -0.1662 0.4217 0.045 Uiso 1 1 calc R . . H65C H -0.0751 -0.1509 0.4205 0.045 Uiso 1 1 calc R . . C66 C 0.5141(6) 0.3114(5) 0.3515(2) 0.0235(13) Uani 1 1 d . . . H66A H 0.4424 0.3558 0.3674 0.035 Uiso 1 1 calc R . . H66B H 0.5843 0.3452 0.3438 0.035 Uiso 1 1 calc R . . H66C H 0.5434 0.2495 0.3698 0.035 Uiso 1 1 calc R . . C67 C 0.4638(6) 0.3893(5) 0.2589(2) 0.0247(14) Uani 1 1 d . . . H67A H 0.4292 0.3779 0.2328 0.037 Uiso 1 1 calc R . . H67B H 0.5518 0.3958 0.2514 0.037 Uiso 1 1 calc R . . H67C H 0.4115 0.4509 0.2709 0.037 Uiso 1 1 calc R . . C68 C 0.5869(5) 0.1674(4) 0.27986(19) 0.0186(12) Uani 1 1 d . . . C69 C 0.5728(6) 0.0727(5) 0.3085(2) 0.0291(15) Uani 1 1 d . . . H69A H 0.6389 0.0152 0.2984 0.044 Uiso 1 1 calc R . . H69B H 0.4883 0.0610 0.3068 0.044 Uiso 1 1 calc R . . H69C H 0.5820 0.0812 0.3388 0.044 Uiso 1 1 calc R . . C70 C 0.5803(6) 0.1524(5) 0.2321(2) 0.0276(14) Uani 1 1 d . . . H70A H 0.6498 0.0960 0.2229 0.041 Uiso 1 1 calc R . . H70B H 0.5889 0.2135 0.2138 0.041 Uiso 1 1 calc R . . H70C H 0.4980 0.1382 0.2289 0.041 Uiso 1 1 calc R . . C71 C 0.7208(6) 0.1830(5) 0.2827(2) 0.0274(14) Uani 1 1 d . . . H71A H 0.7294 0.1934 0.3128 0.041 Uiso 1 1 calc R . . H71B H 0.7329 0.2420 0.2635 0.041 Uiso 1 1 calc R . . H71C H 0.7854 0.1237 0.2735 0.041 Uiso 1 1 calc R . . C72 C 0.4915(6) 0.0920(5) 0.4403(2) 0.0250(14) Uani 1 1 d . . . H72 H 0.4902 0.0462 0.4197 0.030 Uiso 1 1 calc R . . C73 C 0.5817(6) 0.0667(5) 0.4692(2) 0.0271(15) Uani 1 1 d . . . H73 H 0.6422 0.0039 0.4685 0.033 Uiso 1 1 calc R . . C74 C 0.5855(6) 0.1315(5) 0.4994(2) 0.0288(15) Uani 1 1 d . . . H74 H 0.6474 0.1141 0.5197 0.035 Uiso 1 1 calc R . . C75 C 0.4971(6) 0.2223(5) 0.4993(2) 0.0294(15) Uani 1 1 d . . . H75 H 0.4971 0.2678 0.5201 0.035 Uiso 1 1 calc R . . C76 C 0.4087(6) 0.2479(5) 0.4694(2) 0.0244(14) Uani 1 1 d . . . H76 H 0.3510 0.3121 0.4689 0.029 Uiso 1 1 calc R . . C77 C -0.0968(6) 0.2774(4) 0.4202(2) 0.0196(12) Uani 1 1 d . . . H77 H -0.1098 0.2601 0.3926 0.024 Uiso 1 1 calc R . . C78 C -0.1962(6) 0.2858(4) 0.4528(2) 0.0235(13) Uani 1 1 d . . . H78 H -0.2758 0.2744 0.4478 0.028 Uiso 1 1 calc R . . C79 C -0.1784(6) 0.3108(5) 0.4928(2) 0.0301(15) Uani 1 1 d . . . H79 H -0.2452 0.3164 0.5160 0.036 Uiso 1 1 calc R . . C80 C -0.0615(6) 0.3278(4) 0.4988(2) 0.0253(14) Uani 1 1 d . . . H80 H -0.0470 0.3460 0.5260 0.030 Uiso 1 1 calc R . . C81 C 0.0337(6) 0.3179(4) 0.46441(18) 0.0194(12) Uani 1 1 d . . . H81 H 0.1139 0.3294 0.4686 0.023 Uiso 1 1 calc R . . C82 C 0.2293(7) 0.5928(5) 0.3649(2) 0.0287(15) Uani 1 1 d . . . C91 C 0.3444(8) 0.3677(8) 0.0933(3) 0.063(3) Uani 1 1 d D . . C92 C 0.2519(10) 0.3536(10) 0.0719(4) 0.104(5) Uani 1 1 d D . . H92 H 0.2097 0.4052 0.0522 0.125 Uiso 1 1 calc R . . C93 C 0.2188(15) 0.2613(11) 0.0792(6) 0.244(16) Uani 1 1 d D . . H93 H 0.1531 0.2512 0.0640 0.293 Uiso 1 1 calc R . . C94 C 0.2759(12) 0.1854(11) 0.1069(5) 0.127(6) Uani 1 1 d D . . H94 H 0.2545 0.1222 0.1100 0.152 Uiso 1 1 calc R . . C95 C 0.3631(9) 0.2026(8) 0.1298(3) 0.067(3) Uani 1 1 d D . . H95 H 0.3998 0.1536 0.1515 0.080 Uiso 1 1 calc R . . C96 C 0.4005(10) 0.2946(7) 0.1214(3) 0.073(3) Uani 1 1 d D . . H96 H 0.4672 0.3047 0.1362 0.087 Uiso 1 1 calc R . . C97 C 0.3790(12) 0.4637(8) 0.0844(5) 0.099(4) Uani 1 1 d D . . H97A H 0.3348 0.5082 0.1069 0.149 Uiso 1 1 calc R . . H97B H 0.3539 0.4942 0.0558 0.149 Uiso 1 1 calc R . . H97C H 0.4715 0.4534 0.0845 0.149 Uiso 1 1 calc R . . C101 C 0.6437(5) 0.7107(5) 0.3927(2) 0.0274(14) Uani 1 1 d D . . C102 C 0.5387(6) 0.6707(5) 0.3953(2) 0.0285(15) Uani 1 1 d D . . H102 H 0.4715 0.7013 0.3777 0.034 Uiso 1 1 calc R . . C103 C 0.5291(7) 0.5861(5) 0.4231(2) 0.0364(17) Uani 1 1 d D . . H103 H 0.4557 0.5597 0.4247 0.044 Uiso 1 1 calc R . . C104 C 0.6268(6) 0.5404(6) 0.4485(3) 0.045(2) Uani 1 1 d D . . H104 H 0.6201 0.4837 0.4683 0.054 Uiso 1 1 calc R . . C105 C 0.7347(6) 0.5785(5) 0.4448(3) 0.0409(18) Uani 1 1 d D . . H105 H 0.8035 0.5464 0.4614 0.049 Uiso 1 1 calc R . . C106 C 0.7430(6) 0.6629(5) 0.4172(2) 0.0325(16) Uani 1 1 d D . . H106 H 0.8174 0.6883 0.4150 0.039 Uiso 1 1 calc R . . C107 C 0.6500(8) 0.8040(6) 0.3638(3) 0.0442(19) Uani 1 1 d D . . H10D H 0.5982 0.8626 0.3781 0.066 Uiso 1 1 calc R . . H10E H 0.6170 0.8009 0.3361 0.066 Uiso 1 1 calc R . . H10F H 0.7389 0.8096 0.3581 0.066 Uiso 1 1 calc R . . F1 F 0.6203(5) 0.4045(4) 0.16102(15) 0.0589(14) Uani 1 1 d . . . F2 F 0.8139(6) 0.3429(4) 0.17421(16) 0.0733(18) Uani 1 1 d . . . F3 F 0.7419(4) 0.2933(3) 0.12158(14) 0.0442(11) Uani 1 1 d . . . F51 F 0.3494(4) 0.5567(3) 0.34899(13) 0.0406(10) Uani 1 1 d . . . F52 F 0.1576(6) 0.6180(4) 0.33221(15) 0.0631(15) Uani 1 1 d . . . F53 F 0.2255(4) 0.6768(3) 0.38326(14) 0.0392(10) Uani 1 1 d . . . Hf1 Hf 0.76870(2) 0.716741(18) 0.135243(8) 0.01834(7) Uani 1 1 d . . . Hf51 Hf 0.19582(2) 0.258103(17) 0.369506(7) 0.01218(6) Uani 1 1 d . . . N1 N 0.6662(5) 0.7274(4) 0.19605(15) 0.0176(10) Uani 1 1 d . . . N2 N 0.8446(4) 0.8379(4) 0.14093(15) 0.0166(10) Uani 1 1 d . . . N3 N 0.9423(4) 0.6303(4) 0.17476(16) 0.0196(11) Uani 1 1 d . . . N4 N 0.6437(5) 0.7623(4) 0.09377(17) 0.0244(12) Uani 1 1 d . . . N5 N 0.5657(5) 0.7833(4) 0.06247(17) 0.0280(12) Uani 1 1 d . . . N6 N 0.9396(5) 0.6772(4) 0.07782(16) 0.0253(12) Uani 1 1 d . . . N51 N 0.1243(4) 0.1380(3) 0.35730(15) 0.0139(10) Uani 1 1 d . . . N52 N 0.3089(4) 0.2599(3) 0.31060(15) 0.0145(10) Uani 1 1 d . . . N53 N 0.0318(4) 0.3521(3) 0.32721(14) 0.0138(10) Uani 1 1 d . . . N54 N 0.3150(4) 0.2056(4) 0.41278(14) 0.0158(10) Uani 1 1 d . . . N55 N 0.4029(4) 0.1822(4) 0.44029(15) 0.0170(10) Uani 1 1 d . . . N56 N 0.0174(4) 0.2926(3) 0.42529(14) 0.0135(10) Uani 1 1 d . . . O1 O 0.7701(4) 0.5518(3) 0.13302(14) 0.0264(10) Uani 1 1 d . . . O2 O 0.7046(5) 0.4870(3) 0.07199(15) 0.0344(11) Uani 1 1 d . . . O3 O 0.9208(5) 0.4264(4) 0.09241(16) 0.0408(13) Uani 1 1 d . . . O51 O 0.1894(4) 0.4183(3) 0.37828(13) 0.0182(9) Uani 1 1 d . . . O52 O 0.2579(4) 0.4851(3) 0.43774(13) 0.0238(9) Uani 1 1 d . . . O53 O 0.0422(4) 0.5497(3) 0.41668(16) 0.0321(11) Uani 1 1 d . . . S1 S 0.78963(17) 0.46942(12) 0.10514(5) 0.0280(4) Uani 1 1 d . . . S51 S 0.17296(13) 0.50281(10) 0.40472(5) 0.0164(3) Uani 1 1 d . . . Si1 Si 0.50784(16) 0.72216(12) 0.20979(5) 0.0192(3) Uani 1 1 d . . . Si2 Si 0.83284(16) 0.94713(13) 0.10543(5) 0.0207(4) Uani 1 1 d . . . Si51 Si 0.13064(15) 0.02745(11) 0.39012(5) 0.0142(3) Uani 1 1 d . . . Si52 Si 0.46146(14) 0.28056(12) 0.30057(5) 0.0148(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.028(3) 0.013(3) -0.004(2) -0.001(2) -0.006(3) C2 0.018(3) 0.021(3) 0.014(3) -0.002(2) -0.001(2) -0.006(2) C3 0.023(3) 0.019(3) 0.015(3) 0.001(2) -0.002(2) -0.004(2) C4 0.024(3) 0.028(3) 0.016(3) -0.002(3) -0.003(2) -0.006(3) C5 0.016(3) 0.020(3) 0.018(3) 0.003(2) -0.001(2) -0.004(2) C6 0.027(3) 0.027(3) 0.025(3) 0.004(3) -0.010(3) -0.010(3) C7 0.026(4) 0.027(4) 0.041(4) 0.005(3) -0.014(3) 0.001(3) C8 0.024(3) 0.023(3) 0.034(4) 0.000(3) -0.002(3) 0.003(3) C9 0.027(3) 0.026(3) 0.022(3) -0.004(3) -0.001(3) -0.001(3) C10 0.033(4) 0.036(4) 0.034(4) -0.014(3) 0.003(3) -0.011(3) C11 0.041(4) 0.034(4) 0.030(4) 0.009(3) 0.000(3) -0.019(3) C12 0.015(3) 0.020(3) 0.037(4) -0.003(3) 0.002(3) -0.007(2) C13 0.031(4) 0.044(5) 0.054(5) 0.020(4) 0.000(4) 0.002(3) C14 0.021(3) 0.034(4) 0.052(5) -0.001(3) 0.006(3) -0.010(3) C15 0.035(4) 0.025(4) 0.091(7) -0.022(4) -0.008(4) -0.001(3) C16 0.023(3) 0.028(3) 0.022(3) -0.001(3) 0.000(3) 0.003(3) C17 0.033(4) 0.027(3) 0.013(3) 0.004(2) -0.003(3) -0.002(3) C18 0.023(3) 0.024(3) 0.028(3) 0.004(3) 0.002(3) -0.007(3) C19 0.038(4) 0.027(4) 0.028(4) 0.005(3) -0.005(3) -0.015(3) C20 0.023(4) 0.039(4) 0.048(5) -0.003(3) 0.005(3) -0.012(3) C21 0.045(4) 0.032(4) 0.032(4) 0.006(3) 0.007(3) -0.019(3) C22 0.029(4) 0.039(4) 0.025(3) 0.007(3) -0.003(3) -0.013(3) C23 0.034(4) 0.048(5) 0.036(4) 0.025(4) -0.016(3) -0.012(4) C24 0.039(4) 0.072(6) 0.026(4) 0.014(4) -0.017(3) -0.015(4) C25 0.041(4) 0.063(5) 0.037(4) -0.013(4) -0.016(4) -0.012(4) C26 0.035(4) 0.044(4) 0.032(4) -0.008(3) -0.011(3) -0.005(3) C27 0.034(4) 0.021(3) 0.019(3) 0.001(3) -0.002(3) 0.004(3) C28 0.029(4) 0.035(4) 0.030(4) -0.005(3) 0.002(3) 0.004(3) C29 0.047(5) 0.032(4) 0.025(4) -0.005(3) 0.013(3) -0.003(3) C30 0.045(4) 0.035(4) 0.022(3) -0.010(3) -0.001(3) 0.000(3) C31 0.036(4) 0.030(4) 0.025(4) -0.008(3) -0.006(3) 0.001(3) C32 0.058(5) 0.035(4) 0.027(4) -0.001(3) -0.011(4) -0.009(4) C51 0.019(3) 0.014(3) 0.015(3) -0.003(2) -0.004(2) -0.005(2) C52 0.016(3) 0.015(3) 0.014(3) 0.000(2) -0.001(2) -0.007(2) C53 0.015(3) 0.024(3) 0.015(3) -0.003(2) 0.003(2) -0.010(2) C54 0.019(3) 0.025(3) 0.016(3) -0.002(2) -0.002(2) -0.008(2) C55 0.018(3) 0.015(3) 0.015(3) 0.002(2) -0.002(2) -0.011(2) C56 0.026(3) 0.022(3) 0.017(3) 0.004(2) -0.009(2) -0.010(3) C57 0.027(3) 0.023(3) 0.027(3) 0.007(3) -0.012(3) -0.005(3) C58 0.020(3) 0.013(3) 0.035(4) 0.001(3) -0.003(3) -0.001(2) C59 0.018(3) 0.017(3) 0.018(3) -0.002(2) 0.001(2) -0.007(2) C60 0.024(3) 0.021(3) 0.016(3) 0.004(2) -0.006(2) -0.008(3) C61 0.026(3) 0.022(3) 0.028(3) 0.001(3) 0.002(3) -0.001(3) C62 0.029(3) 0.016(3) 0.018(3) 0.002(2) -0.003(2) -0.011(3) C63 0.021(3) 0.033(4) 0.030(4) -0.004(3) 0.000(3) -0.013(3) C64 0.044(4) 0.022(3) 0.020(3) -0.001(3) -0.004(3) -0.018(3) C65 0.044(4) 0.027(3) 0.022(3) 0.000(3) -0.001(3) -0.017(3) C66 0.017(3) 0.035(4) 0.024(3) -0.007(3) -0.001(2) -0.015(3) C67 0.022(3) 0.026(3) 0.027(3) 0.005(3) -0.004(3) -0.009(3) C68 0.015(3) 0.021(3) 0.019(3) 0.000(2) 0.000(2) -0.005(2) C69 0.026(3) 0.021(3) 0.036(4) -0.001(3) 0.002(3) -0.001(3) C70 0.023(3) 0.030(4) 0.027(3) -0.010(3) 0.007(3) -0.003(3) C71 0.017(3) 0.031(4) 0.032(4) 0.003(3) 0.001(3) -0.005(3) C72 0.022(3) 0.027(3) 0.023(3) 0.001(3) 0.001(3) -0.005(3) C73 0.018(3) 0.032(4) 0.028(3) 0.013(3) -0.002(3) -0.007(3) C74 0.021(3) 0.045(4) 0.022(3) 0.015(3) -0.010(3) -0.015(3) C75 0.024(3) 0.047(4) 0.021(3) 0.000(3) -0.005(3) -0.015(3) C76 0.021(3) 0.028(3) 0.023(3) -0.005(3) -0.003(3) -0.003(3) C77 0.020(3) 0.015(3) 0.024(3) -0.001(2) 0.003(2) -0.006(2) C78 0.021(3) 0.019(3) 0.028(3) 0.002(3) 0.007(3) -0.005(3) C79 0.028(4) 0.027(4) 0.028(4) -0.002(3) 0.012(3) -0.001(3) C80 0.039(4) 0.019(3) 0.015(3) -0.001(2) 0.004(3) -0.003(3) C81 0.023(3) 0.018(3) 0.015(3) 0.000(2) 0.000(2) -0.001(2) C82 0.047(4) 0.021(3) 0.024(3) 0.003(3) -0.014(3) -0.015(3) C91 0.047(5) 0.069(6) 0.065(6) -0.013(5) 0.002(5) 0.001(5) C92 0.069(8) 0.136(12) 0.128(11) 0.030(9) -0.075(8) -0.050(8) C93 0.23(2) 0.190(19) 0.38(3) 0.20(2) -0.26(2) -0.167(18) C94 0.104(11) 0.108(11) 0.189(16) 0.070(11) -0.069(11) -0.074(9) C95 0.056(6) 0.075(7) 0.049(6) -0.001(5) -0.009(5) 0.021(5) C96 0.076(7) 0.046(6) 0.091(8) -0.021(5) -0.053(6) 0.025(5) C97 0.089(9) 0.056(7) 0.157(13) -0.014(8) -0.003(9) -0.029(6) C101 0.026(3) 0.030(4) 0.024(3) -0.007(3) 0.003(3) -0.005(3) C102 0.026(3) 0.032(4) 0.029(4) -0.008(3) -0.004(3) -0.006(3) C103 0.030(4) 0.029(4) 0.055(5) -0.008(3) -0.004(3) -0.013(3) C104 0.036(4) 0.028(4) 0.068(6) 0.009(4) -0.001(4) -0.010(3) C105 0.025(4) 0.036(4) 0.059(5) 0.004(4) -0.009(3) -0.002(3) C106 0.017(3) 0.042(4) 0.039(4) -0.009(3) 0.000(3) -0.006(3) C107 0.041(4) 0.047(5) 0.040(4) 0.007(4) 0.002(4) -0.008(4) F1 0.082(4) 0.046(3) 0.046(3) -0.012(2) 0.023(3) -0.021(3) F2 0.128(5) 0.062(3) 0.046(3) 0.020(3) -0.052(3) -0.041(3) F3 0.066(3) 0.028(2) 0.039(2) -0.0072(18) -0.011(2) -0.007(2) F51 0.056(3) 0.041(2) 0.030(2) -0.0052(18) 0.018(2) -0.032(2) F52 0.105(4) 0.053(3) 0.047(3) 0.025(2) -0.052(3) -0.039(3) F53 0.050(3) 0.0141(18) 0.058(3) -0.0019(18) -0.014(2) -0.0137(18) Hf1 0.01850(13) 0.02111(13) 0.01342(12) -0.00402(10) -0.00307(10) 0.00091(10) Hf51 0.01264(12) 0.01340(12) 0.01077(12) -0.00163(8) -0.00068(9) -0.00357(9) N1 0.020(3) 0.018(2) 0.016(2) -0.0035(19) -0.002(2) -0.005(2) N2 0.013(2) 0.025(3) 0.012(2) 0.000(2) -0.0017(18) -0.005(2) N3 0.014(2) 0.024(3) 0.019(3) -0.005(2) -0.001(2) 0.001(2) N4 0.025(3) 0.023(3) 0.026(3) 0.002(2) -0.014(2) -0.005(2) N5 0.025(3) 0.035(3) 0.021(3) 0.000(2) -0.005(2) -0.001(2) N6 0.026(3) 0.027(3) 0.019(3) -0.004(2) -0.004(2) 0.004(2) N51 0.017(2) 0.012(2) 0.013(2) -0.0020(18) -0.0013(19) -0.0037(19) N52 0.016(2) 0.015(2) 0.014(2) -0.0032(19) -0.0021(19) -0.0048(19) N53 0.017(2) 0.012(2) 0.012(2) 0.0023(18) 0.0018(18) -0.0055(19) N54 0.015(2) 0.025(3) 0.008(2) -0.0045(19) 0.0021(18) -0.007(2) N55 0.014(2) 0.023(3) 0.015(2) 0.003(2) 0.0004(19) -0.008(2) N56 0.018(2) 0.012(2) 0.012(2) 0.0012(18) 0.0027(18) -0.0069(19) O1 0.033(3) 0.023(2) 0.023(2) -0.0081(18) 0.0008(19) -0.0047(19) O2 0.050(3) 0.030(3) 0.023(2) -0.004(2) -0.008(2) -0.007(2) O3 0.041(3) 0.042(3) 0.037(3) -0.020(2) 0.002(2) 0.000(2) O51 0.021(2) 0.017(2) 0.018(2) -0.0056(16) 0.0014(17) -0.0065(17) O52 0.028(2) 0.029(2) 0.016(2) -0.0014(18) -0.0066(18) -0.0088(19) O53 0.019(2) 0.035(3) 0.044(3) -0.022(2) -0.001(2) -0.002(2) S1 0.0365(9) 0.0271(8) 0.0187(8) -0.0094(6) -0.0008(7) -0.0020(7) S51 0.0182(7) 0.0155(7) 0.0170(7) -0.0037(5) -0.0015(6) -0.0058(6) Si1 0.0202(8) 0.0163(8) 0.0221(9) -0.0039(6) -0.0010(7) -0.0059(7) Si2 0.0218(9) 0.0211(8) 0.0155(8) 0.0006(6) -0.0012(7) 0.0009(7) Si51 0.0158(8) 0.0132(7) 0.0136(7) 0.0013(6) -0.0011(6) -0.0044(6) Si52 0.0135(8) 0.0175(8) 0.0140(7) 0.0003(6) 0.0006(6) -0.0066(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.473(7) . ? C1 C2 1.545(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.516(8) . ? C2 C4 1.526(8) . ? C2 C3 1.549(8) . ? C3 N2 1.472(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.354(8) . ? C5 C6 1.404(8) . ? C6 C7 1.371(9) . ? C6 H6 0.9500 . ? C7 C8 1.369(10) . ? C7 H7 0.9500 . ? C8 C9 1.376(9) . ? C8 H8 0.9500 . ? C9 N3 1.350(8) . ? C9 H9 0.9500 . ? C10 Si1 1.861(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.886(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.516(10) . ? C12 C14 1.525(8) . ? C12 C13 1.549(10) . ? C12 Si1 1.901(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.873(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.879(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.536(9) . ? C18 C19 1.541(9) . ? C18 C20 1.544(9) . ? C18 Si2 1.910(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N5 1.367(9) . ? C22 C23 1.370(9) . ? C22 H22 0.9500 . ? C23 C24 1.371(12) . ? C23 H23 0.9500 . ? C24 C25 1.399(12) . ? C24 H24 0.9500 . ? C25 C26 1.366(10) . ? C25 H25 0.9500 . ? C26 N5 1.374(9) . ? C26 H26 0.9500 . ? C27 N6 1.335(9) . ? C27 C28 1.392(9) . ? C27 H27 0.9500 . ? C28 C29 1.388(10) . ? C28 H28 0.9500 . ? C29 C30 1.363(11) . ? C29 H29 0.9500 . ? C30 C31 1.374(10) . ? C30 H30 0.9500 . ? C31 N6 1.347(8) . ? C31 H31 0.9500 . ? C32 F2 1.315(9) . ? C32 F3 1.323(8) . ? C32 F1 1.326(9) . ? C32 S1 1.830(8) . ? C51 N51 1.474(7) . ? C51 C52 1.558(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C55 1.516(8) . ? C52 C54 1.536(8) . ? C52 C53 1.557(8) . ? C53 N52 1.470(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N53 1.352(7) . ? C55 C56 1.402(8) . ? C56 C57 1.374(9) . ? C56 H56 0.9500 . ? C57 C58 1.382(9) . ? C57 H57 0.9500 . ? C58 C59 1.379(8) . ? C58 H58 0.9500 . ? C59 N53 1.350(7) . ? C59 H59 0.9500 . ? C60 Si51 1.869(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 Si51 1.876(6) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C65 1.529(8) . ? C62 C63 1.535(9) . ? C62 C64 1.539(8) . ? C62 Si51 1.915(6) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 Si52 1.871(6) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 Si52 1.872(6) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.527(8) . ? C68 C70 1.534(8) . ? C68 C71 1.537(8) . ? C68 Si52 1.913(6) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.369(9) . ? C72 N55 1.372(8) . ? C72 H72 0.9500 . ? C73 C74 1.376(10) . ? C73 H73 0.9500 . ? C74 C75 1.378(10) . ? C74 H74 0.9500 . ? C75 C76 1.376(9) . ? C75 H75 0.9500 . ? C76 N55 1.366(8) . ? C76 H76 0.9500 . ? C77 N56 1.338(7) . ? C77 C78 1.377(8) . ? C77 H77 0.9500 . ? C78 C79 1.374(9) . ? C78 H78 0.9500 . ? C79 C80 1.385(10) . ? C79 H79 0.9500 . ? C80 C81 1.382(8) . ? C80 H80 0.9500 . ? C81 N56 1.345(7) . ? C81 H81 0.9500 . ? C82 F52 1.321(7) . ? C82 F51 1.328(8) . ? C82 F53 1.338(7) . ? C82 S51 1.815(7) . ? C91 C92 1.335(9) . ? C91 C96 1.336(9) . ? C91 C97 1.455(14) . ? C92 C93 1.396(13) . ? C92 H92 0.9500 . ? C93 C94 1.356(12) . ? C93 H93 0.9500 . ? C94 C95 1.332(11) . ? C94 H94 0.9500 . ? C95 C96 1.415(12) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C101 C102 1.376(7) . ? C101 C106 1.386(7) . ? C101 C107 1.498(10) . ? C102 C103 1.392(8) . ? C102 H102 0.9500 . ? C103 C104 1.385(8) . ? C103 H103 0.9500 . ? C104 C105 1.386(8) . ? C104 H104 0.9500 . ? C105 C106 1.383(8) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10D 0.9800 . ? C107 H10E 0.9800 . ? C107 H10F 0.9800 . ? Hf1 N4 1.933(5) . ? Hf1 N1 2.067(5) . ? Hf1 N2 2.074(5) . ? Hf1 O1 2.283(4) . ? Hf1 N3 2.373(5) . ? Hf1 N6 2.408(5) . ? Hf51 N54 1.940(5) . ? Hf51 N52 2.072(5) . ? Hf51 N51 2.086(4) . ? Hf51 O51 2.241(4) . ? Hf51 N53 2.377(5) . ? Hf51 N56 2.420(4) . ? N1 Si1 1.737(5) . ? N2 Si2 1.754(5) . ? N4 N5 1.331(7) . ? N51 Si51 1.730(5) . ? N52 Si52 1.735(5) . ? N54 N55 1.318(6) . ? O1 S1 1.463(4) . ? O2 S1 1.430(5) . ? O3 S1 1.425(5) . ? O51 S51 1.463(4) . ? O52 S51 1.426(4) . ? O53 S51 1.428(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 117.7(5) . . ? N1 C1 H1A 107.9 . . ? C2 C1 H1A 107.9 . . ? N1 C1 H1B 107.9 . . ? C2 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C5 C2 C4 111.0(5) . . ? C5 C2 C1 110.2(5) . . ? C4 C2 C1 106.2(5) . . ? C5 C2 C3 110.4(5) . . ? C4 C2 C3 105.7(5) . . ? C1 C2 C3 113.2(5) . . ? N2 C3 C2 118.2(5) . . ? N2 C3 H3A 107.8 . . ? C2 C3 H3A 107.8 . . ? N2 C3 H3B 107.8 . . ? C2 C3 H3B 107.8 . . ? H3A C3 H3B 107.1 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 120.1(5) . . ? N3 C5 C2 116.8(5) . . ? C6 C5 C2 123.1(5) . . ? C7 C6 C5 119.9(6) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 120.0(6) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 118.2(6) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N3 C9 C8 123.4(6) . . ? N3 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 109.6(6) . . ? C15 C12 C13 107.5(6) . . ? C14 C12 C13 107.1(6) . . ? C15 C12 Si1 112.5(5) . . ? C14 C12 Si1 111.3(4) . . ? C13 C12 Si1 108.7(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C19 107.2(5) . . ? C21 C18 C20 107.7(5) . . ? C19 C18 C20 109.0(6) . . ? C21 C18 Si2 107.9(5) . . ? C19 C18 Si2 114.0(4) . . ? C20 C18 Si2 110.8(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 121.5(7) . . ? N5 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 120.9(7) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 117.8(7) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C26 C25 C24 120.5(8) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 N5 121.3(7) . . ? C25 C26 H26 119.4 . . ? N5 C26 H26 119.4 . . ? N6 C27 C28 123.3(6) . . ? N6 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C29 C28 C27 117.8(7) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? C30 C29 C28 119.6(7) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 118.7(7) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N6 C31 C30 123.6(7) . . ? N6 C31 H31 118.2 . . ? C30 C31 H31 118.2 . . ? F2 C32 F3 108.6(6) . . ? F2 C32 F1 108.0(7) . . ? F3 C32 F1 108.2(7) . . ? F2 C32 S1 111.1(6) . . ? F3 C32 S1 109.7(5) . . ? F1 C32 S1 111.2(5) . . ? N51 C51 C52 118.7(4) . . ? N51 C51 H51A 107.6 . . ? C52 C51 H51A 107.6 . . ? N51 C51 H51B 107.6 . . ? C52 C51 H51B 107.6 . . ? H51A C51 H51B 107.1 . . ? C55 C52 C54 111.4(5) . . ? C55 C52 C53 112.0(4) . . ? C54 C52 C53 106.1(4) . . ? C55 C52 C51 110.1(4) . . ? C54 C52 C51 104.9(4) . . ? C53 C52 C51 112.0(5) . . ? N52 C53 C52 117.9(4) . . ? N52 C53 H53A 107.8 . . ? C52 C53 H53A 107.8 . . ? N52 C53 H53B 107.8 . . ? C52 C53 H53B 107.8 . . ? H53A C53 H53B 107.2 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N53 C55 C56 120.4(5) . . ? N53 C55 C52 116.7(5) . . ? C56 C55 C52 122.9(5) . . ? C57 C56 C55 120.0(6) . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C56 C57 C58 119.4(6) . . ? C56 C57 H57 120.3 . . ? C58 C57 H57 120.3 . . ? C59 C58 C57 118.2(6) . . ? C59 C58 H58 120.9 . . ? C57 C58 H58 120.9 . . ? N53 C59 C58 123.2(5) . . ? N53 C59 H59 118.4 . . ? C58 C59 H59 118.4 . . ? Si51 C60 H60A 109.5 . . ? Si51 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? Si51 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? Si51 C61 H61A 109.5 . . ? Si51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C65 C62 C63 108.1(5) . . ? C65 C62 C64 107.2(5) . . ? C63 C62 C64 109.0(5) . . ? C65 C62 Si51 109.1(4) . . ? C63 C62 Si51 110.5(4) . . ? C64 C62 Si51 112.8(4) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si52 C66 H66A 109.5 . . ? Si52 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? Si52 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? Si52 C67 H67A 109.5 . . ? Si52 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? Si52 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 C70 109.8(5) . . ? C69 C68 C71 108.3(5) . . ? C70 C68 C71 106.5(5) . . ? C69 C68 Si52 109.7(4) . . ? C70 C68 Si52 113.3(4) . . ? C71 C68 Si52 109.1(4) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 N55 121.4(6) . . ? C73 C72 H72 119.3 . . ? N55 C72 H72 119.3 . . ? C72 C73 C74 120.5(6) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C73 C74 C75 118.2(6) . . ? C73 C74 H74 120.9 . . ? C75 C74 H74 120.9 . . ? C76 C75 C74 120.8(6) . . ? C76 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? N55 C76 C75 120.9(6) . . ? N55 C76 H76 119.6 . . ? C75 C76 H76 119.6 . . ? N56 C77 C78 123.3(6) . . ? N56 C77 H77 118.3 . . ? C78 C77 H77 118.3 . . ? C79 C78 C77 118.8(6) . . ? C79 C78 H78 120.6 . . ? C77 C78 H78 120.6 . . ? C78 C79 C80 118.9(6) . . ? C78 C79 H79 120.6 . . ? C80 C79 H79 120.6 . . ? C81 C80 C79 118.8(6) . . ? C81 C80 H80 120.6 . . ? C79 C80 H80 120.6 . . ? N56 C81 C80 122.6(6) . . ? N56 C81 H81 118.7 . . ? C80 C81 H81 118.7 . . ? F52 C82 F51 108.7(6) . . ? F52 C82 F53 107.4(5) . . ? F51 C82 F53 107.4(5) . . ? F52 C82 S51 111.5(5) . . ? F51 C82 S51 111.3(4) . . ? F53 C82 S51 110.4(5) . . ? C92 C91 C96 119.6(11) . . ? C92 C91 C97 117.2(10) . . ? C96 C91 C97 123.2(10) . . ? C91 C92 C93 118.3(11) . . ? C91 C92 H92 120.9 . . ? C93 C92 H92 120.9 . . ? C94 C93 C92 123.2(12) . . ? C94 C93 H93 118.4 . . ? C92 C93 H93 118.4 . . ? C95 C94 C93 117.7(13) . . ? C95 C94 H94 121.2 . . ? C93 C94 H94 121.2 . . ? C94 C95 C96 119.3(9) . . ? C94 C95 H95 120.4 . . ? C96 C95 H95 120.4 . . ? C91 C96 C95 121.7(9) . . ? C91 C96 H96 119.1 . . ? C95 C96 H96 119.1 . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C102 C101 C106 118.8(6) . . ? C102 C101 C107 120.3(6) . . ? C106 C101 C107 120.9(6) . . ? C101 C102 C103 121.1(6) . . ? C101 C102 H102 119.5 . . ? C103 C102 H102 119.5 . . ? C104 C103 C102 119.9(6) . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C105 119.0(7) . . ? C103 C104 H104 120.5 . . ? C105 C104 H104 120.5 . . ? C106 C105 C104 120.6(6) . . ? C106 C105 H105 119.7 . . ? C104 C105 H105 119.7 . . ? C105 C106 C101 120.5(6) . . ? C105 C106 H106 119.7 . . ? C101 C106 H106 119.7 . . ? C101 C107 H10D 109.5 . . ? C101 C107 H10E 109.5 . . ? H10D C107 H10E 109.5 . . ? C101 C107 H10F 109.5 . . ? H10D C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? N4 Hf1 N1 105.7(2) . . ? N4 Hf1 N2 106.2(2) . . ? N1 Hf1 N2 93.29(18) . . ? N4 Hf1 O1 93.45(19) . . ? N1 Hf1 O1 93.85(17) . . ? N2 Hf1 O1 156.36(17) . . ? N4 Hf1 N3 166.3(2) . . ? N1 Hf1 N3 84.31(18) . . ? N2 Hf1 N3 81.98(18) . . ? O1 Hf1 N3 76.35(16) . . ? N4 Hf1 N6 91.7(2) . . ? N1 Hf1 N6 162.33(18) . . ? N2 Hf1 N6 84.52(18) . . ? O1 Hf1 N6 81.88(17) . . ? N3 Hf1 N6 78.03(17) . . ? N54 Hf51 N52 104.95(18) . . ? N54 Hf51 N51 105.98(19) . . ? N52 Hf51 N51 94.75(17) . . ? N54 Hf51 O51 93.52(17) . . ? N52 Hf51 O51 93.02(16) . . ? N51 Hf51 O51 156.31(16) . . ? N54 Hf51 N53 166.99(17) . . ? N52 Hf51 N53 83.35(16) . . ? N51 Hf51 N53 82.90(16) . . ? O51 Hf51 N53 75.82(15) . . ? N54 Hf51 N56 91.72(17) . . ? N52 Hf51 N56 162.34(17) . . ? N51 Hf51 N56 86.00(16) . . ? O51 Hf51 N56 79.98(14) . . ? N53 Hf51 N56 79.23(15) . . ? C1 N1 Si1 114.1(4) . . ? C1 N1 Hf1 118.2(4) . . ? Si1 N1 Hf1 127.6(3) . . ? C3 N2 Si2 112.4(4) . . ? C3 N2 Hf1 117.2(4) . . ? Si2 N2 Hf1 127.0(2) . . ? C9 N3 C5 118.6(5) . . ? C9 N3 Hf1 124.7(4) . . ? C5 N3 Hf1 116.8(4) . . ? N5 N4 Hf1 172.5(5) . . ? N4 N5 C22 120.8(6) . . ? N4 N5 C26 121.1(6) . . ? C22 N5 C26 118.1(6) . . ? C27 N6 C31 117.0(6) . . ? C27 N6 Hf1 120.8(4) . . ? C31 N6 Hf1 121.6(5) . . ? C51 N51 Si51 114.8(3) . . ? C51 N51 Hf51 116.4(3) . . ? Si51 N51 Hf51 126.2(2) . . ? C53 N52 Si52 114.3(4) . . ? C53 N52 Hf51 117.4(3) . . ? Si52 N52 Hf51 128.1(2) . . ? C59 N53 C55 118.6(5) . . ? C59 N53 Hf51 124.7(4) . . ? C55 N53 Hf51 116.6(4) . . ? N55 N54 Hf51 171.2(4) . . ? N54 N55 C76 120.7(5) . . ? N54 N55 C72 121.1(5) . . ? C76 N55 C72 118.2(5) . . ? C77 N56 C81 117.5(5) . . ? C77 N56 Hf51 121.7(4) . . ? C81 N56 Hf51 120.5(4) . . ? S1 O1 Hf1 145.5(3) . . ? S51 O51 Hf51 153.1(3) . . ? O3 S1 O2 116.7(3) . . ? O3 S1 O1 113.4(3) . . ? O2 S1 O1 114.6(3) . . ? O3 S1 C32 103.9(4) . . ? O2 S1 C32 103.8(3) . . ? O1 S1 C32 102.1(3) . . ? O52 S51 O53 117.2(3) . . ? O52 S51 O51 114.1(2) . . ? O53 S51 O51 113.3(2) . . ? O52 S51 C82 104.6(3) . . ? O53 S51 C82 104.5(3) . . ? O51 S51 C82 100.7(3) . . ? N1 Si1 C10 111.2(3) . . ? N1 Si1 C11 109.7(3) . . ? C10 Si1 C11 107.8(3) . . ? N1 Si1 C12 113.8(3) . . ? C10 Si1 C12 108.2(3) . . ? C11 Si1 C12 105.9(3) . . ? N2 Si2 C16 109.9(3) . . ? N2 Si2 C17 109.7(3) . . ? C16 Si2 C17 108.2(3) . . ? N2 Si2 C18 114.6(3) . . ? C16 Si2 C18 106.9(3) . . ? C17 Si2 C18 107.3(3) . . ? N51 Si51 C60 110.6(2) . . ? N51 Si51 C61 110.2(3) . . ? C60 Si51 C61 107.7(3) . . ? N51 Si51 C62 114.3(2) . . ? C60 Si51 C62 106.6(3) . . ? C61 Si51 C62 107.2(3) . . ? N52 Si52 C66 110.5(2) . . ? N52 Si52 C67 110.3(3) . . ? C66 Si52 C67 107.6(3) . . ? N52 Si52 C68 113.3(2) . . ? C66 Si52 C68 107.2(3) . . ? C67 Si52 C68 107.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C5 -68.7(6) . . . . ? N1 C1 C2 C4 171.0(5) . . . . ? N1 C1 C2 C3 55.5(7) . . . . ? C5 C2 C3 N2 61.0(7) . . . . ? C4 C2 C3 N2 -178.9(5) . . . . ? C1 C2 C3 N2 -63.1(7) . . . . ? C4 C2 C5 N3 179.9(5) . . . . ? C1 C2 C5 N3 62.6(6) . . . . ? C3 C2 C5 N3 -63.3(7) . . . . ? C4 C2 C5 C6 0.4(8) . . . . ? C1 C2 C5 C6 -116.9(6) . . . . ? C3 C2 C5 C6 117.3(6) . . . . ? N3 C5 C6 C7 0.1(9) . . . . ? C2 C5 C6 C7 179.5(6) . . . . ? C5 C6 C7 C8 0.3(10) . . . . ? C6 C7 C8 C9 -1.0(10) . . . . ? C7 C8 C9 N3 1.4(10) . . . . ? N5 C22 C23 C24 -0.5(11) . . . . ? C22 C23 C24 C25 1.7(12) . . . . ? C23 C24 C25 C26 -1.4(12) . . . . ? C24 C25 C26 N5 -0.2(12) . . . . ? N6 C27 C28 C29 -0.8(10) . . . . ? C27 C28 C29 C30 0.6(10) . . . . ? C28 C29 C30 C31 0.3(11) . . . . ? C29 C30 C31 N6 -1.3(11) . . . . ? N51 C51 C52 C55 -64.4(6) . . . . ? N51 C51 C52 C54 175.6(5) . . . . ? N51 C51 C52 C53 60.9(6) . . . . ? C55 C52 C53 N52 61.3(6) . . . . ? C54 C52 C53 N52 -176.9(5) . . . . ? C51 C52 C53 N52 -63.0(6) . . . . ? C54 C52 C55 N53 178.5(5) . . . . ? C53 C52 C55 N53 -62.9(6) . . . . ? C51 C52 C55 N53 62.5(6) . . . . ? C54 C52 C55 C56 -2.9(7) . . . . ? C53 C52 C55 C56 115.8(6) . . . . ? C51 C52 C55 C56 -118.9(6) . . . . ? N53 C55 C56 C57 -2.5(9) . . . . ? C52 C55 C56 C57 178.9(5) . . . . ? C55 C56 C57 C58 0.5(9) . . . . ? C56 C57 C58 C59 1.0(9) . . . . ? C57 C58 C59 N53 -0.6(9) . . . . ? N55 C72 C73 C74 0.2(9) . . . . ? C72 C73 C74 C75 -0.6(9) . . . . ? C73 C74 C75 C76 -0.9(10) . . . . ? C74 C75 C76 N55 2.9(10) . . . . ? N56 C77 C78 C79 0.0(9) . . . . ? C77 C78 C79 C80 0.6(9) . . . . ? C78 C79 C80 C81 -0.7(9) . . . . ? C79 C80 C81 N56 0.2(9) . . . . ? C96 C91 C92 C93 -1.3(13) . . . . ? C97 C91 C92 C93 178.7(11) . . . . ? C91 C92 C93 C94 0.1(18) . . . . ? C92 C93 C94 C95 4(2) . . . . ? C93 C94 C95 C96 -6(2) . . . . ? C92 C91 C96 C95 -1.0(15) . . . . ? C97 C91 C96 C95 179.0(10) . . . . ? C94 C95 C96 C91 4.7(17) . . . . ? C106 C101 C102 C103 2.5(9) . . . . ? C107 C101 C102 C103 -177.7(6) . . . . ? C101 C102 C103 C104 -0.5(9) . . . . ? C102 C103 C104 C105 -1.8(11) . . . . ? C103 C104 C105 C106 2.1(12) . . . . ? C104 C105 C106 C101 -0.1(12) . . . . ? C102 C101 C106 C105 -2.2(10) . . . . ? C107 C101 C106 C105 178.0(7) . . . . ? C2 C1 N1 Si1 -173.0(4) . . . . ? C2 C1 N1 Hf1 2.3(7) . . . . ? N4 Hf1 N1 C1 -148.3(4) . . . . ? N2 Hf1 N1 C1 -40.4(4) . . . . ? O1 Hf1 N1 C1 117.0(4) . . . . ? N3 Hf1 N1 C1 41.2(4) . . . . ? N6 Hf1 N1 C1 41.8(8) . . . . ? N4 Hf1 N1 Si1 26.3(4) . . . . ? N2 Hf1 N1 Si1 134.1(3) . . . . ? O1 Hf1 N1 Si1 -68.4(3) . . . . ? N3 Hf1 N1 Si1 -144.3(3) . . . . ? N6 Hf1 N1 Si1 -143.6(5) . . . . ? C2 C3 N2 Si2 170.3(4) . . . . ? C2 C3 N2 Hf1 9.9(6) . . . . ? N4 Hf1 N2 C3 141.3(4) . . . . ? N1 Hf1 N2 C3 33.9(4) . . . . ? O1 Hf1 N2 C3 -73.5(6) . . . . ? N3 Hf1 N2 C3 -49.9(4) . . . . ? N6 Hf1 N2 C3 -128.5(4) . . . . ? N4 Hf1 N2 Si2 -15.9(4) . . . . ? N1 Hf1 N2 Si2 -123.3(3) . . . . ? O1 Hf1 N2 Si2 129.3(4) . . . . ? N3 Hf1 N2 Si2 152.9(3) . . . . ? N6 Hf1 N2 Si2 74.2(3) . . . . ? C8 C9 N3 C5 -1.0(9) . . . . ? C8 C9 N3 Hf1 178.9(5) . . . . ? C6 C5 N3 C9 0.2(9) . . . . ? C2 C5 N3 C9 -179.2(5) . . . . ? C6 C5 N3 Hf1 -179.6(4) . . . . ? C2 C5 N3 Hf1 0.9(7) . . . . ? N4 Hf1 N3 C9 -3.9(11) . . . . ? N1 Hf1 N3 C9 134.0(5) . . . . ? N2 Hf1 N3 C9 -131.9(5) . . . . ? O1 Hf1 N3 C9 38.6(5) . . . . ? N6 Hf1 N3 C9 -45.8(5) . . . . ? N4 Hf1 N3 C5 176.0(8) . . . . ? N1 Hf1 N3 C5 -46.1(4) . . . . ? N2 Hf1 N3 C5 48.0(4) . . . . ? O1 Hf1 N3 C5 -141.5(4) . . . . ? N6 Hf1 N3 C5 134.0(4) . . . . ? N1 Hf1 N4 N5 -134(4) . . . . ? N2 Hf1 N4 N5 127(4) . . . . ? O1 Hf1 N4 N5 -39(4) . . . . ? N3 Hf1 N4 N5 2(4) . . . . ? N6 Hf1 N4 N5 43(4) . . . . ? Hf1 N4 N5 C22 -154(3) . . . . ? Hf1 N4 N5 C26 27(4) . . . . ? C23 C22 N5 N4 179.8(6) . . . . ? C23 C22 N5 C26 -1.1(10) . . . . ? C25 C26 N5 N4 -179.5(7) . . . . ? C25 C26 N5 C22 1.4(10) . . . . ? C28 C27 N6 C31 -0.1(9) . . . . ? C28 C27 N6 Hf1 -170.6(5) . . . . ? C30 C31 N6 C27 1.1(10) . . . . ? C30 C31 N6 Hf1 171.6(5) . . . . ? N4 Hf1 N6 C27 139.8(5) . . . . ? N1 Hf1 N6 C27 -49.9(9) . . . . ? N2 Hf1 N6 C27 33.6(5) . . . . ? O1 Hf1 N6 C27 -127.0(5) . . . . ? N3 Hf1 N6 C27 -49.3(5) . . . . ? N4 Hf1 N6 C31 -30.3(5) . . . . ? N1 Hf1 N6 C31 140.0(6) . . . . ? N2 Hf1 N6 C31 -136.5(5) . . . . ? O1 Hf1 N6 C31 62.9(5) . . . . ? N3 Hf1 N6 C31 140.6(5) . . . . ? C52 C51 N51 Si51 -168.0(4) . . . . ? C52 C51 N51 Hf51 -5.1(6) . . . . ? N54 Hf51 N51 C51 -142.9(4) . . . . ? N52 Hf51 N51 C51 -35.8(4) . . . . ? O51 Hf51 N51 C51 72.9(6) . . . . ? N53 Hf51 N51 C51 46.9(4) . . . . ? N56 Hf51 N51 C51 126.5(4) . . . . ? N54 Hf51 N51 Si51 17.9(3) . . . . ? N52 Hf51 N51 Si51 125.0(3) . . . . ? O51 Hf51 N51 Si51 -126.3(4) . . . . ? N53 Hf51 N51 Si51 -152.3(3) . . . . ? N56 Hf51 N51 Si51 -72.7(3) . . . . ? C52 C53 N52 Si52 -175.8(4) . . . . ? C52 C53 N52 Hf51 8.6(6) . . . . ? N54 Hf51 N52 C53 142.1(4) . . . . ? N51 Hf51 N52 C53 34.2(4) . . . . ? O51 Hf51 N52 C53 -123.4(4) . . . . ? N53 Hf51 N52 C53 -48.1(4) . . . . ? N56 Hf51 N52 C53 -57.6(7) . . . . ? N54 Hf51 N52 Si52 -32.9(4) . . . . ? N51 Hf51 N52 Si52 -140.8(3) . . . . ? O51 Hf51 N52 Si52 61.6(3) . . . . ? N53 Hf51 N52 Si52 136.9(3) . . . . ? N56 Hf51 N52 Si52 127.4(5) . . . . ? C58 C59 N53 C55 -1.3(8) . . . . ? C58 C59 N53 Hf51 179.3(4) . . . . ? C56 C55 N53 C59 2.8(8) . . . . ? C52 C55 N53 C59 -178.5(5) . . . . ? C56 C55 N53 Hf51 -177.8(4) . . . . ? C52 C55 N53 Hf51 0.9(6) . . . . ? N54 Hf51 N53 C59 -3.3(10) . . . . ? N52 Hf51 N53 C59 -133.8(4) . . . . ? N51 Hf51 N53 C59 130.5(4) . . . . ? O51 Hf51 N53 C59 -39.0(4) . . . . ? N56 Hf51 N53 C59 43.3(4) . . . . ? N54 Hf51 N53 C55 177.3(7) . . . . ? N52 Hf51 N53 C55 46.8(4) . . . . ? N51 Hf51 N53 C55 -48.9(4) . . . . ? O51 Hf51 N53 C55 141.6(4) . . . . ? N56 Hf51 N53 C55 -136.1(4) . . . . ? N52 Hf51 N54 N55 63(3) . . . . ? N51 Hf51 N54 N55 162(3) . . . . ? O51 Hf51 N54 N55 -31(3) . . . . ? N53 Hf51 N54 N55 -66(3) . . . . ? N56 Hf51 N54 N55 -111(3) . . . . ? Hf51 N54 N55 C76 55(3) . . . . ? Hf51 N54 N55 C72 -124(2) . . . . ? C75 C76 N55 N54 177.4(5) . . . . ? C75 C76 N55 C72 -3.2(9) . . . . ? C73 C72 N55 N54 -179.0(5) . . . . ? C73 C72 N55 C76 1.7(9) . . . . ? C78 C77 N56 C81 -0.5(8) . . . . ? C78 C77 N56 Hf51 172.8(4) . . . . ? C80 C81 N56 C77 0.4(8) . . . . ? C80 C81 N56 Hf51 -172.9(4) . . . . ? N54 Hf51 N56 C77 -141.3(4) . . . . ? N52 Hf51 N56 C77 57.7(7) . . . . ? N51 Hf51 N56 C77 -35.4(4) . . . . ? O51 Hf51 N56 C77 125.4(4) . . . . ? N53 Hf51 N56 C77 48.1(4) . . . . ? N54 Hf51 N56 C81 31.8(4) . . . . ? N52 Hf51 N56 C81 -129.2(6) . . . . ? N51 Hf51 N56 C81 137.7(4) . . . . ? O51 Hf51 N56 C81 -61.5(4) . . . . ? N53 Hf51 N56 C81 -138.8(4) . . . . ? N4 Hf1 O1 S1 56.4(5) . . . . ? N1 Hf1 O1 S1 162.4(5) . . . . ? N2 Hf1 O1 S1 -90.3(6) . . . . ? N3 Hf1 O1 S1 -114.4(5) . . . . ? N6 Hf1 O1 S1 -34.8(5) . . . . ? N54 Hf51 O51 S51 -51.5(6) . . . . ? N52 Hf51 O51 S51 -156.7(6) . . . . ? N51 Hf51 O51 S51 94.3(7) . . . . ? N53 Hf51 O51 S51 120.9(6) . . . . ? N56 Hf51 O51 S51 39.6(6) . . . . ? Hf1 O1 S1 O3 77.0(6) . . . . ? Hf1 O1 S1 O2 -60.3(6) . . . . ? Hf1 O1 S1 C32 -171.9(5) . . . . ? F2 C32 S1 O3 53.6(6) . . . . ? F3 C32 S1 O3 -66.4(6) . . . . ? F1 C32 S1 O3 174.0(5) . . . . ? F2 C32 S1 O2 176.1(5) . . . . ? F3 C32 S1 O2 56.1(6) . . . . ? F1 C32 S1 O2 -63.5(6) . . . . ? F2 C32 S1 O1 -64.5(6) . . . . ? F3 C32 S1 O1 175.5(5) . . . . ? F1 C32 S1 O1 55.9(6) . . . . ? Hf51 O51 S51 O52 57.3(6) . . . . ? Hf51 O51 S51 O53 -80.2(6) . . . . ? Hf51 O51 S51 C82 168.7(5) . . . . ? F52 C82 S51 O52 -179.0(5) . . . . ? F51 C82 S51 O52 59.5(5) . . . . ? F53 C82 S51 O52 -59.7(5) . . . . ? F52 C82 S51 O53 -55.2(6) . . . . ? F51 C82 S51 O53 -176.7(4) . . . . ? F53 C82 S51 O53 64.1(5) . . . . ? F52 C82 S51 O51 62.4(6) . . . . ? F51 C82 S51 O51 -59.1(5) . . . . ? F53 C82 S51 O51 -178.3(4) . . . . ? C1 N1 Si1 C10 -157.8(4) . . . . ? Hf1 N1 Si1 C10 27.4(4) . . . . ? C1 N1 Si1 C11 -38.7(5) . . . . ? Hf1 N1 Si1 C11 146.5(3) . . . . ? C1 N1 Si1 C12 79.7(5) . . . . ? Hf1 N1 Si1 C12 -95.0(4) . . . . ? C15 C12 Si1 N1 -50.4(6) . . . . ? C14 C12 Si1 N1 -173.9(5) . . . . ? C13 C12 Si1 N1 68.4(5) . . . . ? C15 C12 Si1 C10 -174.5(5) . . . . ? C14 C12 Si1 C10 62.0(6) . . . . ? C13 C12 Si1 C10 -55.7(5) . . . . ? C15 C12 Si1 C11 70.2(6) . . . . ? C14 C12 Si1 C11 -53.3(6) . . . . ? C13 C12 Si1 C11 -171.0(5) . . . . ? C3 N2 Si2 C16 -73.4(4) . . . . ? Hf1 N2 Si2 C16 84.7(4) . . . . ? C3 N2 Si2 C17 167.8(4) . . . . ? Hf1 N2 Si2 C17 -34.1(4) . . . . ? C3 N2 Si2 C18 47.0(5) . . . . ? Hf1 N2 Si2 C18 -154.8(3) . . . . ? C21 C18 Si2 N2 169.5(4) . . . . ? C19 C18 Si2 N2 -71.5(5) . . . . ? C20 C18 Si2 N2 51.9(5) . . . . ? C21 C18 Si2 C16 -68.4(5) . . . . ? C19 C18 Si2 C16 50.6(5) . . . . ? C20 C18 Si2 C16 174.0(5) . . . . ? C21 C18 Si2 C17 47.5(5) . . . . ? C19 C18 Si2 C17 166.5(4) . . . . ? C20 C18 Si2 C17 -70.2(5) . . . . ? C51 N51 Si51 C60 -167.4(4) . . . . ? Hf51 N51 Si51 C60 31.5(4) . . . . ? C51 N51 Si51 C61 73.6(4) . . . . ? Hf51 N51 Si51 C61 -87.5(4) . . . . ? C51 N51 Si51 C62 -47.1(5) . . . . ? Hf51 N51 Si51 C62 151.8(3) . . . . ? C65 C62 Si51 N51 -167.1(4) . . . . ? C63 C62 Si51 N51 -48.4(5) . . . . ? C64 C62 Si51 N51 73.9(5) . . . . ? C65 C62 Si51 C60 -44.5(5) . . . . ? C63 C62 Si51 C60 74.2(5) . . . . ? C64 C62 Si51 C60 -163.6(4) . . . . ? C65 C62 Si51 C61 70.5(5) . . . . ? C63 C62 Si51 C61 -170.8(4) . . . . ? C64 C62 Si51 C61 -48.5(5) . . . . ? C53 N52 Si52 C66 -178.9(4) . . . . ? Hf51 N52 Si52 C66 -3.8(4) . . . . ? C53 N52 Si52 C67 62.2(5) . . . . ? Hf51 N52 Si52 C67 -122.7(3) . . . . ? C53 N52 Si52 C68 -58.6(4) . . . . ? Hf51 N52 Si52 C68 116.5(3) . . . . ? C69 C68 Si52 N52 -47.7(5) . . . . ? C70 C68 Si52 N52 75.3(5) . . . . ? C71 C68 Si52 N52 -166.3(4) . . . . ? C69 C68 Si52 C66 74.5(5) . . . . ? C70 C68 Si52 C66 -162.5(4) . . . . ? C71 C68 Si52 C66 -44.1(5) . . . . ? C69 C68 Si52 C67 -170.0(4) . . . . ? C70 C68 Si52 C67 -47.0(5) . . . . ? C71 C68 Si52 C67 71.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.441 _refine_diff_density_min -2.388 _refine_diff_density_rms 0.117 _audit_block_code ga_tg2b _audit_block_refno 678 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 687176' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H64 N6 Si2 Zr' _chemical_formula_weight 848.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0651(8) _cell_length_b 14.2917(11) _cell_length_c 15.7951(11) _cell_angle_alpha 71.3620(10) _cell_angle_beta 80.6460(10) _cell_angle_gamma 74.071(2) _cell_volume 2268.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6832 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37559 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7996 _reflns_number_gt 5613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^)+(0.0718P)^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 7996 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3618(3) 0.2356(3) 0.0269(2) 0.0231(8) Uani 1 1 d . . . H1A H 0.3429 0.2996 -0.0224 0.028 Uiso 1 1 calc R . . H1B H 0.3361 0.1834 0.0099 0.028 Uiso 1 1 calc R . . C2 C 0.5058(3) 0.2026(3) 0.0319(2) 0.0223(8) Uani 1 1 d . . . C3 C 0.5469(4) 0.1028(3) 0.1081(2) 0.0250(9) Uani 1 1 d . . . H3A H 0.5120 0.0503 0.0989 0.030 Uiso 1 1 calc R . . H3B H 0.6399 0.0800 0.1006 0.030 Uiso 1 1 calc R . . C4 C 0.5605(4) 0.1745(3) -0.0551(2) 0.0274(9) Uani 1 1 d . . . H4A H 0.5344 0.2333 -0.1068 0.041 Uiso 1 1 calc R . . H4B H 0.5291 0.1176 -0.0572 0.041 Uiso 1 1 calc R . . H4C H 0.6527 0.1548 -0.0567 0.041 Uiso 1 1 calc R . . C5 C 0.5548(3) 0.2876(3) 0.0403(2) 0.0220(8) Uani 1 1 d . . . C6 C 0.6378(3) 0.3348(3) -0.0242(2) 0.0233(8) Uani 1 1 d . . . H6 H 0.6680 0.3122 -0.0759 0.028 Uiso 1 1 calc R . . C7 C 0.6761(3) 0.4129(3) -0.0141(2) 0.0260(9) Uani 1 1 d . . . H7 H 0.7320 0.4454 -0.0588 0.031 Uiso 1 1 calc R . . C8 C 0.6330(3) 0.4449(3) 0.0617(2) 0.0248(9) Uani 1 1 d . . . H8 H 0.6598 0.4984 0.0709 0.030 Uiso 1 1 calc R . . C9 C 0.5500(3) 0.3966(3) 0.1234(2) 0.0231(8) Uani 1 1 d . . . H9 H 0.5186 0.4188 0.1751 0.028 Uiso 1 1 calc R . . C16 C 0.5212(4) -0.0010(3) 0.3946(2) 0.0255(9) Uani 1 1 d . . . H16A H 0.5966 0.0171 0.4034 0.038 Uiso 1 1 calc R . . H16B H 0.5138 -0.0658 0.4388 0.038 Uiso 1 1 calc R . . H16C H 0.4463 0.0522 0.4024 0.038 Uiso 1 1 calc R . . C17 C 0.4118(4) -0.0821(3) 0.2774(3) 0.0293(9) Uani 1 1 d . . . H17A H 0.3291 -0.0472 0.2991 0.044 Uiso 1 1 calc R . . H17B H 0.4341 -0.1522 0.3161 0.044 Uiso 1 1 calc R . . H17C H 0.4085 -0.0825 0.2159 0.044 Uiso 1 1 calc R . . C18 C 0.6953(4) -0.1015(3) 0.2643(2) 0.0268(9) Uani 1 1 d . . . C21 C 0.7975(3) -0.0430(3) 0.2491(3) 0.0302(9) Uani 1 1 d . . . H21A H 0.7885 -0.0123 0.2978 0.045 Uiso 1 1 calc R . . H21B H 0.7888 0.0106 0.1917 0.045 Uiso 1 1 calc R . . H21C H 0.8808 -0.0898 0.2480 0.045 Uiso 1 1 calc R . . C20 C 0.7190(4) -0.1896(3) 0.3504(3) 0.0338(10) Uani 1 1 d . . . H20A H 0.8040 -0.2326 0.3446 0.051 Uiso 1 1 calc R . . H20B H 0.6567 -0.2301 0.3604 0.051 Uiso 1 1 calc R . . H20C H 0.7115 -0.1626 0.4012 0.051 Uiso 1 1 calc R . . C19 C 0.7051(4) -0.1484(3) 0.1868(3) 0.0354(10) Uani 1 1 d . . . H19A H 0.7882 -0.1948 0.1835 0.053 Uiso 1 1 calc R . . H19B H 0.6937 -0.0941 0.1301 0.053 Uiso 1 1 calc R . . H19C H 0.6394 -0.1861 0.1979 0.053 Uiso 1 1 calc R . . C10 C 0.0298(4) 0.3549(3) 0.1741(3) 0.0313(10) Uani 1 1 d . . . H10A H 0.0461 0.3152 0.2361 0.047 Uiso 1 1 calc R . . H10B H -0.0604 0.3693 0.1669 0.047 Uiso 1 1 calc R . . H10C H 0.0553 0.4190 0.1600 0.047 Uiso 1 1 calc R . . C11 C 0.0876(4) 0.3633(3) -0.0208(2) 0.0300(9) Uani 1 1 d . . . H11A H 0.1232 0.4228 -0.0351 0.045 Uiso 1 1 calc R . . H11B H -0.0038 0.3857 -0.0249 0.045 Uiso 1 1 calc R . . H11C H 0.1257 0.3241 -0.0633 0.045 Uiso 1 1 calc R . . C12 C 0.0584(3) 0.1634(3) 0.1199(2) 0.0241(8) Uani 1 1 d . . . C15 C 0.0551(4) 0.1074(3) 0.2209(2) 0.0308(9) Uani 1 1 d . . . H15A H 0.0185 0.0488 0.2328 0.046 Uiso 1 1 calc R . . H15B H 0.0035 0.1537 0.2543 0.046 Uiso 1 1 calc R . . H15C H 0.1410 0.0840 0.2398 0.046 Uiso 1 1 calc R . . C14 C 0.1380(4) 0.0895(3) 0.0692(3) 0.0343(10) Uani 1 1 d . . . H14A H 0.2224 0.0627 0.0909 0.051 Uiso 1 1 calc R . . H14B H 0.1449 0.1252 0.0050 0.051 Uiso 1 1 calc R . . H14C H 0.0979 0.0333 0.0791 0.051 Uiso 1 1 calc R . . C13 C -0.0768(4) 0.1957(3) 0.0910(3) 0.0409(11) Uani 1 1 d . . . H13A H -0.0760 0.2303 0.0265 0.061 Uiso 1 1 calc R . . H13B H -0.1302 0.2419 0.1238 0.061 Uiso 1 1 calc R . . H13C H -0.1104 0.1353 0.1043 0.061 Uiso 1 1 calc R . . C22 C 0.1617(4) 0.0825(3) 0.4533(2) 0.0260(9) Uani 1 1 d . . . H22 H 0.2123 0.0223 0.4405 0.031 Uiso 1 1 calc R . . C23 C 0.0773(4) 0.0752(3) 0.5280(3) 0.0336(10) Uani 1 1 d . . . H23 H 0.0712 0.0100 0.5665 0.040 Uiso 1 1 calc R . . C24 C 0.0016(4) 0.1606(4) 0.5477(3) 0.0393(11) Uani 1 1 d . . . H24 H -0.0570 0.1553 0.5992 0.047 Uiso 1 1 calc R . . C25 C 0.0129(4) 0.2540(4) 0.4910(3) 0.0378(11) Uani 1 1 d . . . H25 H -0.0382 0.3142 0.5034 0.045 Uiso 1 1 calc R . . C26 C 0.0975(4) 0.2609(3) 0.4166(3) 0.0296(9) Uani 1 1 d . . . H26 H 0.1036 0.3260 0.3778 0.035 Uiso 1 1 calc R . . C32 C 0.2915(4) 0.3989(3) 0.2384(2) 0.0268(9) Uani 1 1 d . . . C33 C 0.2522(3) 0.4849(3) 0.2453(2) 0.0230(8) Uani 1 1 d . . . C34 C 0.2146(3) 0.5894(3) 0.2440(2) 0.0213(8) Uani 1 1 d . . . C39 C 0.2819(4) 0.6278(3) 0.2863(3) 0.0346(10) Uani 1 1 d . . . H39 H 0.3496 0.5835 0.3203 0.042 Uiso 1 1 calc R . . C38 C 0.2505(5) 0.7308(4) 0.2791(3) 0.0511(13) Uani 1 1 d . . . H38 H 0.2968 0.7565 0.3084 0.061 Uiso 1 1 calc R . . C37 C 0.1546(5) 0.7951(3) 0.2306(3) 0.0503(14) Uani 1 1 d . . . H37 H 0.1347 0.8655 0.2258 0.060 Uiso 1 1 calc R . . C36 C 0.0868(4) 0.7595(3) 0.1890(3) 0.0430(12) Uani 1 1 d . . . H36 H 0.0196 0.8049 0.1551 0.052 Uiso 1 1 calc R . . C35 C 0.1154(4) 0.6568(3) 0.1959(3) 0.0309(10) Uani 1 1 d . . . H35 H 0.0667 0.6321 0.1674 0.037 Uiso 1 1 calc R . . C31 C 0.6442(4) 0.2135(3) 0.3042(3) 0.0264(9) Uani 1 1 d . . . H31 H 0.6778 0.1931 0.2519 0.032 Uiso 1 1 calc R . . C30 C 0.7261(4) 0.2160(3) 0.3590(3) 0.0362(10) Uani 1 1 d . . . H30 H 0.8145 0.1978 0.3445 0.043 Uiso 1 1 calc R . . C29 C 0.6792(4) 0.2454(3) 0.4361(3) 0.0412(11) Uani 1 1 d . . . H29 H 0.7343 0.2482 0.4750 0.049 Uiso 1 1 calc R . . C28 C 0.5512(4) 0.2701(3) 0.4542(3) 0.0357(10) Uani 1 1 d . . . H28 H 0.5158 0.2892 0.5070 0.043 Uiso 1 1 calc R . . C27 C 0.4746(4) 0.2672(3) 0.3957(2) 0.0267(9) Uani 1 1 d . . . H27 H 0.3859 0.2864 0.4086 0.032 Uiso 1 1 calc R . . N1 N 0.2815(3) 0.2519(2) 0.10740(19) 0.0213(7) Uani 1 1 d . . . N2 N 0.5116(3) 0.1045(2) 0.20182(18) 0.0196(7) Uani 1 1 d . . . N3 N 0.5114(3) 0.3202(2) 0.11396(19) 0.0218(7) Uani 1 1 d . . . N4 N 0.2558(3) 0.1825(2) 0.32500(19) 0.0225(7) Uani 1 1 d . . . N5 N 0.1736(3) 0.1751(2) 0.3974(2) 0.0239(7) Uani 1 1 d . . . N6 N 0.5184(3) 0.2386(2) 0.32086(19) 0.0205(7) Uani 1 1 d . . . Si1 Si 0.12195(10) 0.28093(8) 0.09662(7) 0.0224(2) Uani 1 1 d . . . Si2 Si 0.53428(10) -0.01351(8) 0.27944(7) 0.0218(2) Uani 1 1 d . . . Zr Zr 0.36823(3) 0.23396(3) 0.22192(2) 0.01854(12) Uani 1 1 d . . . C40 C 0.7238(4) 0.5245(3) 0.3322(3) 0.0409(11) Uani 1 1 d . . . C41 C 0.8453(4) 0.5343(3) 0.3223(3) 0.0469(12) Uani 1 1 d . . . H41 H 0.8941 0.5343 0.2669 0.056 Uiso 1 1 calc R . . C42 C 0.8976(5) 0.5442(4) 0.3905(4) 0.0562(14) Uani 1 1 d . . . H42 H 0.9823 0.5503 0.3827 0.067 Uiso 1 1 calc R . . C43 C 0.8275(6) 0.5452(4) 0.4705(4) 0.0554(14) Uani 1 1 d . . . H43 H 0.8635 0.5532 0.5176 0.066 Uiso 1 1 calc R . . C45 C 0.6564(5) 0.5244(4) 0.4134(3) 0.0495(13) Uani 1 1 d . . . H45 H 0.5722 0.5170 0.4219 0.059 Uiso 1 1 calc R . . C46 C 0.6678(6) 0.5139(5) 0.2563(4) 0.0708(17) Uani 1 1 d . . . H46A H 0.7357 0.4880 0.2154 0.106 Uiso 1 1 calc R . . H46B H 0.6185 0.5805 0.2237 0.106 Uiso 1 1 calc R . . H46C H 0.6129 0.4665 0.2801 0.106 Uiso 1 1 calc R . . C44 C 0.7075(5) 0.5349(3) 0.4825(3) 0.0500(13) Uani 1 1 d . . . H44 H 0.6592 0.5349 0.5381 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(2) 0.025(2) 0.0160(19) -0.0057(16) 0.0027(16) -0.0117(17) C2 0.030(2) 0.0191(19) 0.0151(19) -0.0047(15) 0.0025(16) -0.0048(16) C3 0.033(2) 0.021(2) 0.019(2) -0.0083(16) 0.0003(16) -0.0015(17) C4 0.032(2) 0.029(2) 0.020(2) -0.0104(17) 0.0017(17) -0.0033(18) C5 0.0197(19) 0.023(2) 0.0161(19) -0.0005(16) -0.0004(15) -0.0003(16) C6 0.0174(19) 0.030(2) 0.019(2) -0.0049(17) -0.0036(15) -0.0016(16) C7 0.023(2) 0.030(2) 0.018(2) 0.0040(17) -0.0017(16) -0.0071(17) C8 0.023(2) 0.021(2) 0.027(2) 0.0012(17) -0.0072(17) -0.0072(17) C9 0.026(2) 0.022(2) 0.021(2) -0.0044(16) -0.0017(16) -0.0084(17) C16 0.033(2) 0.021(2) 0.021(2) -0.0055(16) 0.0006(17) -0.0060(17) C17 0.027(2) 0.029(2) 0.030(2) -0.0061(18) 0.0006(17) -0.0080(18) C18 0.029(2) 0.026(2) 0.024(2) -0.0078(17) 0.0003(17) -0.0049(17) C21 0.023(2) 0.030(2) 0.037(2) -0.0113(19) -0.0012(18) -0.0042(18) C20 0.037(2) 0.032(2) 0.033(2) -0.0098(19) -0.0078(19) -0.0035(19) C19 0.041(3) 0.028(2) 0.034(2) -0.0139(19) 0.003(2) -0.001(2) C10 0.031(2) 0.026(2) 0.030(2) -0.0056(18) 0.0017(18) 0.0008(18) C11 0.031(2) 0.028(2) 0.024(2) -0.0010(18) -0.0042(17) -0.0034(18) C12 0.024(2) 0.026(2) 0.019(2) -0.0013(16) 0.0004(16) -0.0063(17) C15 0.026(2) 0.034(2) 0.028(2) -0.0008(18) -0.0025(17) -0.0087(18) C14 0.041(3) 0.032(2) 0.033(2) -0.0084(19) 0.0002(19) -0.017(2) C13 0.028(2) 0.040(3) 0.044(3) 0.009(2) -0.008(2) -0.013(2) C22 0.030(2) 0.029(2) 0.022(2) -0.0064(17) 0.0020(17) -0.0142(18) C23 0.037(2) 0.047(3) 0.021(2) -0.0024(19) -0.0011(18) -0.025(2) C24 0.033(2) 0.072(3) 0.019(2) -0.018(2) 0.0102(18) -0.023(2) C25 0.030(2) 0.058(3) 0.031(2) -0.023(2) 0.0006(19) -0.008(2) C26 0.029(2) 0.038(2) 0.027(2) -0.0174(19) 0.0036(18) -0.0105(19) C32 0.028(2) 0.030(2) 0.024(2) -0.0089(18) 0.0053(17) -0.0131(18) C33 0.024(2) 0.023(2) 0.022(2) -0.0066(16) 0.0045(16) -0.0095(17) C34 0.025(2) 0.022(2) 0.0180(19) -0.0064(16) 0.0047(16) -0.0108(16) C39 0.045(3) 0.029(2) 0.033(2) -0.0084(19) -0.001(2) -0.016(2) C38 0.079(4) 0.042(3) 0.051(3) -0.026(3) 0.008(3) -0.038(3) C37 0.075(4) 0.018(2) 0.049(3) -0.009(2) 0.021(3) -0.013(2) C36 0.042(3) 0.028(2) 0.041(3) -0.004(2) 0.009(2) 0.006(2) C35 0.023(2) 0.033(2) 0.033(2) -0.0112(19) 0.0010(18) -0.0008(18) C31 0.029(2) 0.021(2) 0.026(2) -0.0049(17) 0.0024(17) -0.0050(17) C30 0.024(2) 0.037(3) 0.045(3) -0.014(2) 0.002(2) -0.0039(19) C29 0.036(3) 0.050(3) 0.045(3) -0.022(2) -0.010(2) -0.008(2) C28 0.039(3) 0.044(3) 0.032(2) -0.021(2) -0.003(2) -0.010(2) C27 0.030(2) 0.026(2) 0.028(2) -0.0125(17) 0.0040(17) -0.0103(17) N1 0.0284(17) 0.0172(16) 0.0171(16) -0.0048(13) 0.0035(13) -0.0069(13) N2 0.0267(17) 0.0198(16) 0.0119(15) -0.0064(13) 0.0020(12) -0.0049(13) N3 0.0268(17) 0.0188(16) 0.0169(16) -0.0010(13) 0.0005(13) -0.0070(14) N4 0.0288(18) 0.0246(17) 0.0167(16) -0.0080(13) 0.0037(13) -0.0115(14) N5 0.0263(17) 0.0299(19) 0.0183(16) -0.0072(14) 0.0002(13) -0.0120(15) N6 0.0247(17) 0.0138(15) 0.0230(17) -0.0079(13) 0.0044(13) -0.0055(13) Si1 0.0252(6) 0.0178(5) 0.0203(6) -0.0032(4) -0.0012(4) -0.0018(4) Si2 0.0305(6) 0.0184(5) 0.0165(5) -0.0059(4) 0.0001(4) -0.0060(5) Zr 0.0253(2) 0.01516(19) 0.01495(19) -0.00520(14) 0.00381(14) -0.00670(15) C40 0.046(3) 0.038(3) 0.041(3) -0.012(2) -0.001(2) -0.013(2) C41 0.043(3) 0.043(3) 0.045(3) -0.008(2) 0.006(2) -0.004(2) C42 0.037(3) 0.053(3) 0.076(4) -0.014(3) -0.012(3) -0.009(2) C43 0.073(4) 0.042(3) 0.057(3) -0.012(3) -0.031(3) -0.011(3) C45 0.051(3) 0.049(3) 0.055(3) -0.021(3) 0.015(3) -0.026(2) C46 0.068(4) 0.091(5) 0.069(4) -0.042(4) -0.020(3) -0.014(3) C44 0.078(4) 0.030(3) 0.034(3) -0.006(2) 0.003(3) -0.010(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 C1 N1 1.473(4) . ? C1 C2 1.540(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.509(5) . ? C2 C4 1.538(5) . ? C2 C3 1.553(5) . ? C3 N2 1.475(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.357(4) . ? C5 C6 1.390(5) . ? C6 C7 1.359(5) . ? C6 H6 0.9500 . ? C7 C8 1.384(5) . ? C7 H7 0.9500 . ? C8 C9 1.378(5) . ? C8 H8 0.9500 . ? C9 N3 1.332(4) . ? C9 H9 0.9500 . ? C16 Si2 1.863(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.888(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.529(5) . ? C18 C20 1.531(5) . ? C18 C19 1.549(5) . ? C18 Si2 1.907(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C10 Si1 1.867(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.886(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.528(5) . ? C12 C15 1.538(5) . ? C12 C13 1.539(5) . ? C12 Si1 1.903(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C22 N5 1.364(5) . ? C22 C23 1.376(5) . ? C22 H22 0.9500 . ? C23 C24 1.373(6) . ? C23 H23 0.9500 . ? C24 C25 1.375(6) . ? C24 H24 0.9500 . ? C25 C26 1.374(5) . ? C25 H25 0.9500 . ? C26 N5 1.376(5) . ? C26 H26 0.9500 . ? C32 C33 1.220(5) . ? C32 Zr 2.359(4) . ? C33 C34 1.431(5) . ? C34 C39 1.387(5) . ? C34 C35 1.389(5) . ? C39 C38 1.388(6) . ? C39 H39 0.9500 . ? C38 C37 1.355(7) . ? C38 H38 0.9500 . ? C37 C36 1.356(7) . ? C37 H37 0.9500 . ? C36 C35 1.385(6) . ? C36 H36 0.9500 . ? C35 H35 0.9500 . ? C31 N6 1.343(5) . ? C31 C30 1.365(6) . ? C31 H31 0.9500 . ? C30 C29 1.389(6) . ? C30 H30 0.9500 . ? C29 C28 1.367(6) . ? C29 H29 0.9500 . ? C28 C27 1.368(5) . ? C28 H28 0.9500 . ? C27 N6 1.347(4) . ? C27 H27 0.9500 . ? N1 Si1 1.723(3) . ? N1 Zr 2.095(3) . ? N2 Si2 1.720(3) . ? N2 Zr 2.154(3) . ? N3 Zr 2.406(3) . ? N4 N5 1.335(4) . ? N4 Zr 1.954(3) . ? N6 Zr 2.486(3) . ? C40 C41 1.369(6) . ? C40 C45 1.373(6) . ? C40 C46 1.501(6) . ? C41 C42 1.364(7) . ? C41 H41 0.9500 . ? C42 C43 1.373(7) . ? C42 H42 0.9500 . ? C43 C44 1.352(7) . ? C43 H43 0.9500 . ? C45 C44 1.374(7) . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C44 H44 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.3(3) . . ? N1 C1 H1A 107.7 . . ? C2 C1 H1A 107.7 . . ? N1 C1 H1B 107.7 . . ? C2 C1 H1B 107.7 . . ? H1A C1 H1B 107.1 . . ? C5 C2 C4 111.7(3) . . ? C5 C2 C1 110.5(3) . . ? C4 C2 C1 105.7(3) . . ? C5 C2 C3 111.7(3) . . ? C4 C2 C3 104.7(3) . . ? C1 C2 C3 112.4(3) . . ? N2 C3 C2 118.4(3) . . ? N2 C3 H3A 107.7 . . ? C2 C3 H3A 107.7 . . ? N2 C3 H3B 107.7 . . ? C2 C3 H3B 107.7 . . ? H3A C3 H3B 107.1 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 119.6(3) . . ? N3 C5 C2 117.1(3) . . ? C6 C5 C2 123.3(3) . . ? C7 C6 C5 120.7(4) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.5(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 117.7(4) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? N3 C9 C8 123.2(3) . . ? N3 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C20 107.8(3) . . ? C21 C18 C19 110.6(3) . . ? C20 C18 C19 107.3(3) . . ? C21 C18 Si2 109.2(3) . . ? C20 C18 Si2 109.0(3) . . ? C19 C18 Si2 112.9(3) . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 108.6(3) . . ? C14 C12 C13 108.0(3) . . ? C15 C12 C13 108.5(3) . . ? C14 C12 Si1 112.4(3) . . ? C15 C12 Si1 109.9(3) . . ? C13 C12 Si1 109.4(3) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C22 C23 120.7(4) . . ? N5 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 121.2(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 118.2(4) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 N5 121.1(4) . . ? C25 C26 H26 119.5 . . ? N5 C26 H26 119.5 . . ? C33 C32 Zr 178.9(3) . . ? C32 C33 C34 173.4(4) . . ? C39 C34 C35 118.0(4) . . ? C39 C34 C33 120.4(4) . . ? C35 C34 C33 121.5(3) . . ? C34 C39 C38 120.0(4) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C37 C38 C39 120.8(4) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C37 C36 120.4(4) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C36 C35 120.0(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C35 C34 120.8(4) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? N6 C31 C30 123.1(4) . . ? N6 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? C31 C30 C29 119.5(4) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C28 C29 C30 117.9(4) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N6 C27 C28 123.4(4) . . ? N6 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? C1 N1 Si1 114.5(2) . . ? C1 N1 Zr 118.6(2) . . ? Si1 N1 Zr 126.88(16) . . ? C3 N2 Si2 114.5(2) . . ? C3 N2 Zr 116.2(2) . . ? Si2 N2 Zr 123.01(15) . . ? C9 N3 C5 119.3(3) . . ? C9 N3 Zr 123.5(2) . . ? C5 N3 Zr 117.2(2) . . ? N5 N4 Zr 163.0(2) . . ? N4 N5 C22 120.9(3) . . ? N4 N5 C26 120.7(3) . . ? C22 N5 C26 118.4(3) . . ? C31 N6 C27 116.6(3) . . ? C31 N6 Zr 123.4(2) . . ? C27 N6 Zr 120.0(2) . . ? N1 Si1 C10 111.58(17) . . ? N1 Si1 C11 109.67(16) . . ? C10 Si1 C11 106.72(18) . . ? N1 Si1 C12 112.80(15) . . ? C10 Si1 C12 107.63(18) . . ? C11 Si1 C12 108.20(17) . . ? N2 Si2 C16 110.21(16) . . ? N2 Si2 C17 111.60(16) . . ? C16 Si2 C17 107.16(17) . . ? N2 Si2 C18 114.22(16) . . ? C16 Si2 C18 106.23(17) . . ? C17 Si2 C18 107.04(17) . . ? N4 Zr N1 106.51(12) . . ? N4 Zr N2 106.88(12) . . ? N1 Zr N2 92.51(11) . . ? N4 Zr C32 89.99(12) . . ? N1 Zr C32 100.04(12) . . ? N2 Zr C32 155.25(12) . . ? N4 Zr N3 167.46(11) . . ? N1 Zr N3 82.98(11) . . ? N2 Zr N3 80.36(10) . . ? C32 Zr N3 80.11(11) . . ? N4 Zr N6 91.65(11) . . ? N1 Zr N6 161.76(10) . . ? N2 Zr N6 83.70(10) . . ? C32 Zr N6 77.71(11) . . ? N3 Zr N6 78.79(10) . . ? C41 C40 C45 117.8(4) . . ? C41 C40 C46 120.3(4) . . ? C45 C40 C46 121.9(5) . . ? C42 C41 C40 121.1(5) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 119.9(5) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.4(5) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C40 C45 C44 121.8(5) . . ? C40 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C44 C45 119.1(5) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? 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 N1 C1 C2 C5 -68.4(4) . . . . ? N1 C1 C2 C4 170.6(3) . . . . ? N1 C1 C2 C3 57.1(4) . . . . ? C5 C2 C3 N2 57.5(4) . . . . ? C4 C2 C3 N2 178.5(3) . . . . ? C1 C2 C3 N2 -67.3(4) . . . . ? C4 C2 C5 N3 178.9(3) . . . . ? C1 C2 C5 N3 61.6(4) . . . . ? C3 C2 C5 N3 -64.2(4) . . . . ? C4 C2 C5 C6 0.9(5) . . . . ? C1 C2 C5 C6 -116.5(4) . . . . ? C3 C2 C5 C6 117.7(4) . . . . ? N3 C5 C6 C7 0.2(5) . . . . ? C2 C5 C6 C7 178.2(3) . . . . ? C5 C6 C7 C8 0.8(5) . . . . ? C6 C7 C8 C9 -1.4(5) . . . . ? C7 C8 C9 N3 1.1(5) . . . . ? N5 C22 C23 C24 0.8(6) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 0.3(6) . . . . ? C24 C25 C26 N5 -0.6(6) . . . . ? Zr C32 C33 C34 -21(20) . . . . ? C32 C33 C34 C39 -92(4) . . . . ? C32 C33 C34 C35 84(4) . . . . ? C35 C34 C39 C38 -0.8(6) . . . . ? C33 C34 C39 C38 175.2(4) . . . . ? C34 C39 C38 C37 -0.2(7) . . . . ? C39 C38 C37 C36 0.6(7) . . . . ? C38 C37 C36 C35 0.0(7) . . . . ? C37 C36 C35 C34 -1.1(6) . . . . ? C39 C34 C35 C36 1.4(6) . . . . ? C33 C34 C35 C36 -174.5(4) . . . . ? N6 C31 C30 C29 0.2(6) . . . . ? C31 C30 C29 C28 0.5(7) . . . . ? C30 C29 C28 C27 -1.3(7) . . . . ? C29 C28 C27 N6 1.6(6) . . . . ? C2 C1 N1 Si1 -176.2(2) . . . . ? C2 C1 N1 Zr 1.9(4) . . . . ? C2 C3 N2 Si2 168.0(3) . . . . ? C2 C3 N2 Zr 14.9(4) . . . . ? C8 C9 N3 C5 -0.2(5) . . . . ? C8 C9 N3 Zr 179.3(3) . . . . ? C6 C5 N3 C9 -0.5(5) . . . . ? C2 C5 N3 C9 -178.6(3) . . . . ? C6 C5 N3 Zr 180.0(2) . . . . ? C2 C5 N3 Zr 1.8(4) . . . . ? Zr N4 N5 C22 -161.7(7) . . . . ? Zr N4 N5 C26 19.3(10) . . . . ? C23 C22 N5 N4 179.8(3) . . . . ? C23 C22 N5 C26 -1.1(5) . . . . ? C25 C26 N5 N4 -179.9(3) . . . . ? C25 C26 N5 C22 1.0(5) . . . . ? C30 C31 N6 C27 0.0(5) . . . . ? C30 C31 N6 Zr -179.8(3) . . . . ? C28 C27 N6 C31 -1.0(5) . . . . ? C28 C27 N6 Zr 178.9(3) . . . . ? C1 N1 Si1 C10 -154.5(2) . . . . ? Zr N1 Si1 C10 27.6(2) . . . . ? C1 N1 Si1 C11 -36.5(3) . . . . ? Zr N1 Si1 C11 145.6(2) . . . . ? C1 N1 Si1 C12 84.2(3) . . . . ? Zr N1 Si1 C12 -93.8(2) . . . . ? C14 C12 Si1 N1 -48.9(3) . . . . ? C15 C12 Si1 N1 72.1(3) . . . . ? C13 C12 Si1 N1 -168.9(3) . . . . ? C14 C12 Si1 C10 -172.4(3) . . . . ? C15 C12 Si1 C10 -51.4(3) . . . . ? C13 C12 Si1 C10 67.6(3) . . . . ? C14 C12 Si1 C11 72.6(3) . . . . ? C15 C12 Si1 C11 -166.4(3) . . . . ? C13 C12 Si1 C11 -47.4(3) . . . . ? C3 N2 Si2 C16 167.3(3) . . . . ? Zr N2 Si2 C16 -41.7(2) . . . . ? C3 N2 Si2 C17 -73.8(3) . . . . ? Zr N2 Si2 C17 77.3(2) . . . . ? C3 N2 Si2 C18 47.8(3) . . . . ? Zr N2 Si2 C18 -161.17(17) . . . . ? C21 C18 Si2 N2 46.2(3) . . . . ? C20 C18 Si2 N2 163.7(2) . . . . ? C19 C18 Si2 N2 -77.3(3) . . . . ? C21 C18 Si2 C16 -75.5(3) . . . . ? C20 C18 Si2 C16 42.0(3) . . . . ? C19 C18 Si2 C16 161.0(3) . . . . ? C21 C18 Si2 C17 170.2(3) . . . . ? C20 C18 Si2 C17 -72.3(3) . . . . ? C19 C18 Si2 C17 46.8(3) . . . . ? N5 N4 Zr N1 -108.9(9) . . . . ? N5 N4 Zr N2 153.2(8) . . . . ? N5 N4 Zr C32 -8.4(9) . . . . ? N5 N4 Zr N3 29.2(12) . . . . ? N5 N4 Zr N6 69.3(9) . . . . ? C1 N1 Zr N4 -147.4(2) . . . . ? Si1 N1 Zr N4 30.4(2) . . . . ? C1 N1 Zr N2 -39.0(3) . . . . ? Si1 N1 Zr N2 138.83(19) . . . . ? C1 N1 Zr C32 119.6(2) . . . . ? Si1 N1 Zr C32 -62.6(2) . . . . ? C1 N1 Zr N3 40.9(2) . . . . ? Si1 N1 Zr N3 -141.2(2) . . . . ? C1 N1 Zr N6 38.4(5) . . . . ? Si1 N1 Zr N6 -143.8(3) . . . . ? C3 N2 Zr N4 138.1(2) . . . . ? Si2 N2 Zr N4 -12.4(2) . . . . ? C3 N2 Zr N1 30.0(3) . . . . ? Si2 N2 Zr N1 -120.54(19) . . . . ? C3 N2 Zr C32 -90.8(4) . . . . ? Si2 N2 Zr C32 118.7(3) . . . . ? C3 N2 Zr N3 -52.4(2) . . . . ? Si2 N2 Zr N3 157.0(2) . . . . ? C3 N2 Zr N6 -132.1(3) . . . . ? Si2 N2 Zr N6 77.36(18) . . . . ? C33 C32 Zr N4 -152(17) . . . . ? C33 C32 Zr N1 -45(17) . . . . ? C33 C32 Zr N2 75(17) . . . . ? C33 C32 Zr N3 36(17) . . . . ? C33 C32 Zr N6 117(17) . . . . ? C9 N3 Zr N4 -5.7(7) . . . . ? C5 N3 Zr N4 173.8(5) . . . . ? C9 N3 Zr N1 134.2(3) . . . . ? C5 N3 Zr N1 -46.3(3) . . . . ? C9 N3 Zr N2 -132.0(3) . . . . ? C5 N3 Zr N2 47.5(3) . . . . ? C9 N3 Zr C32 32.7(3) . . . . ? C5 N3 Zr C32 -147.8(3) . . . . ? C9 N3 Zr N6 -46.6(3) . . . . ? C5 N3 Zr N6 132.9(3) . . . . ? C31 N6 Zr N4 141.7(3) . . . . ? C27 N6 Zr N4 -38.2(3) . . . . ? C31 N6 Zr N1 -43.9(5) . . . . ? C27 N6 Zr N1 136.2(3) . . . . ? C31 N6 Zr N2 34.8(3) . . . . ? C27 N6 Zr N2 -145.0(3) . . . . ? C31 N6 Zr C32 -128.7(3) . . . . ? C27 N6 Zr C32 51.4(3) . . . . ? C31 N6 Zr N3 -46.5(3) . . . . ? C27 N6 Zr N3 133.6(3) . . . . ? C45 C40 C41 C42 -0.3(7) . . . . ? C46 C40 C41 C42 179.9(5) . . . . ? C40 C41 C42 C43 -0.6(8) . . . . ? C41 C42 C43 C44 1.1(8) . . . . ? C41 C40 C45 C44 0.7(7) . . . . ? C46 C40 C45 C44 -179.5(5) . . . . ? C42 C43 C44 C45 -0.7(7) . . . . ? C40 C45 C44 C43 -0.2(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.053 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.087 _audit_block_code ga_hh19 _audit_block_refno 574 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 679493' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H55 F3 N6 O3 S Si2 Zr' _chemical_formula_weight 808.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4937(5) _cell_length_b 19.0633(9) _cell_length_c 20.8233(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.1230(10) _cell_angle_gamma 90.00 _cell_volume 4072.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6932 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98728 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12423 _reflns_number_gt 8972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^)+(0.0436P)^2^+2.7786P] 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 12423 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2255(2) 0.10686(12) 0.07563(11) 0.0289(5) Uani 1 1 d . . . H1A H 0.3217 0.1041 0.0882 0.035 Uiso 1 1 calc R . . H1B H 0.1986 0.0843 0.0321 0.035 Uiso 1 1 calc R . . C2 C 0.1690(2) 0.06351(11) 0.12559(11) 0.0215(4) Uani 1 1 d . . . C3 C 0.0184(2) 0.06775(12) 0.11193(12) 0.0279(5) Uani 1 1 d . . . H3A H -0.0155 0.0534 0.0658 0.034 Uiso 1 1 calc R . . H3B H -0.0129 0.0329 0.1403 0.034 Uiso 1 1 calc R . . C4 C 0.2010(2) -0.01347(12) 0.11342(12) 0.0297(5) Uani 1 1 d . . . H4A H 0.2949 -0.0184 0.1163 0.045 Uiso 1 1 calc R . . H4B H 0.1539 -0.0277 0.0696 0.045 Uiso 1 1 calc R . . H4C H 0.1744 -0.0433 0.1466 0.045 Uiso 1 1 calc R . . C5 C 0.22780(18) 0.08556(11) 0.19543(10) 0.0186(4) Uani 1 1 d . . . C6 C 0.3044(2) 0.04131(12) 0.24090(12) 0.0266(5) Uani 1 1 d . . . H6 H 0.3261 -0.0043 0.2282 0.032 Uiso 1 1 calc R . . C7 C 0.3490(2) 0.06406(13) 0.30485(12) 0.0318(5) Uani 1 1 d . . . H7 H 0.4010 0.0341 0.3363 0.038 Uiso 1 1 calc R . . C8 C 0.3177(2) 0.13045(13) 0.32264(11) 0.0290(5) Uani 1 1 d . . . H8 H 0.3451 0.1465 0.3666 0.035 Uiso 1 1 calc R . . C9 C 0.2459(2) 0.17283(12) 0.27522(10) 0.0229(4) Uani 1 1 d . . . H9 H 0.2261 0.2191 0.2871 0.027 Uiso 1 1 calc R . . C10 C 0.3927(2) 0.18320(15) -0.00938(12) 0.0326(5) Uani 1 1 d . . . H10A H 0.4572 0.1895 0.0317 0.049 Uiso 1 1 calc R . . H10B H 0.4223 0.2075 -0.0451 0.049 Uiso 1 1 calc R . . H10C H 0.3823 0.1331 -0.0196 0.049 Uiso 1 1 calc R . . C11 C 0.2586(2) 0.31707(12) 0.01151(11) 0.0273(5) Uani 1 1 d . . . H11A H 0.1768 0.3392 0.0163 0.041 Uiso 1 1 calc R . . H11B H 0.2864 0.3369 -0.0268 0.041 Uiso 1 1 calc R . . H11C H 0.3258 0.3258 0.0511 0.041 Uiso 1 1 calc R . . C12 C 0.1066(2) 0.20327(11) -0.07858(10) 0.0220(4) Uani 1 1 d . . . C13 C 0.1212(3) 0.12967(14) -0.10609(13) 0.0394(6) Uani 1 1 d . . . H13A H 0.1080 0.0944 -0.0739 0.059 Uiso 1 1 calc R . . H13B H 0.2088 0.1245 -0.1150 0.059 Uiso 1 1 calc R . . H13C H 0.0561 0.1232 -0.1469 0.059 Uiso 1 1 calc R . . C14 C 0.1256(3) 0.25619(15) -0.13142(12) 0.0366(6) Uani 1 1 d . . . H14A H 0.0616 0.2470 -0.1721 0.055 Uiso 1 1 calc R . . H14B H 0.2138 0.2514 -0.1396 0.055 Uiso 1 1 calc R . . H14C H 0.1136 0.3039 -0.1162 0.055 Uiso 1 1 calc R . . C15 C -0.0317(2) 0.21087(15) -0.06751(12) 0.0354(6) Uani 1 1 d . . . H15A H -0.0444 0.2586 -0.0526 0.053 Uiso 1 1 calc R . . H15B H -0.0456 0.1772 -0.0341 0.053 Uiso 1 1 calc R . . H15C H -0.0942 0.2017 -0.1087 0.053 Uiso 1 1 calc R . . C16 C -0.2766(2) 0.21992(11) 0.10651(13) 0.0277(5) Uani 1 1 d . . . H16A H -0.2292 0.2530 0.1390 0.042 Uiso 1 1 calc R . . H16B H -0.3686 0.2189 0.1095 0.042 Uiso 1 1 calc R . . H16C H -0.2696 0.2348 0.0624 0.042 Uiso 1 1 calc R . . C17 C -0.2893(2) 0.07188(13) 0.05494(14) 0.0360(6) Uani 1 1 d . . . H17A H -0.2779 0.0908 0.0127 0.054 Uiso 1 1 calc R . . H17B H -0.3824 0.0694 0.0553 0.054 Uiso 1 1 calc R . . H17C H -0.2514 0.0248 0.0612 0.054 Uiso 1 1 calc R . . C18 C -0.2351(2) 0.09515(12) 0.20422(13) 0.0291(5) Uani 1 1 d . . . C19 C -0.1531(6) 0.1332(4) 0.26084(18) 0.137(3) Uani 1 1 d . . . H19A H -0.1781 0.1188 0.3017 0.205 Uiso 1 1 calc R . . H19B H -0.1663 0.1839 0.2547 0.205 Uiso 1 1 calc R . . H19C H -0.0610 0.1220 0.2633 0.205 Uiso 1 1 calc R . . C20 C -0.2086(7) 0.0185(2) 0.2130(2) 0.123(3) Uani 1 1 d . . . H20A H -0.1158 0.0096 0.2150 0.185 Uiso 1 1 calc R . . H20B H -0.2608 -0.0072 0.1759 0.185 Uiso 1 1 calc R . . H20C H -0.2316 0.0027 0.2539 0.185 Uiso 1 1 calc R . . C21 C -0.3755(4) 0.1062(3) 0.2088(3) 0.0997(19) Uani 1 1 d . . . H21A H -0.4331 0.0858 0.1701 0.150 Uiso 1 1 calc R . . H21B H -0.3931 0.1565 0.2108 0.150 Uiso 1 1 calc R . . H21C H -0.3914 0.0833 0.2486 0.150 Uiso 1 1 calc R . . C22 C -0.0783(2) 0.35190(12) 0.04350(11) 0.0245(4) Uani 1 1 d . . . C23 C -0.2283(2) 0.44913(13) 0.02151(13) 0.0310(5) Uani 1 1 d . . . C24 C -0.2846(3) 0.48687(15) -0.04247(13) 0.0413(7) Uani 1 1 d . . . H24A H -0.2137 0.5083 -0.0597 0.062 Uiso 1 1 calc R . . H24B H -0.3449 0.5235 -0.0344 0.062 Uiso 1 1 calc R . . H24C H -0.3313 0.4532 -0.0745 0.062 Uiso 1 1 calc R . . C25 C -0.1519(3) 0.50049(15) 0.07101(14) 0.0467(7) Uani 1 1 d . . . H25A H -0.1122 0.4753 0.1113 0.070 Uiso 1 1 calc R . . H25B H -0.2109 0.5367 0.0812 0.070 Uiso 1 1 calc R . . H25C H -0.0834 0.5225 0.0524 0.070 Uiso 1 1 calc R . . C26 C -0.3338(3) 0.41359(18) 0.0491(2) 0.0569(9) Uani 1 1 d . . . H26A H -0.3806 0.3801 0.0169 0.085 Uiso 1 1 calc R . . H26B H -0.3950 0.4489 0.0587 0.085 Uiso 1 1 calc R . . H26C H -0.2944 0.3887 0.0896 0.085 Uiso 1 1 calc R . . C27 C 0.39268(19) 0.26848(11) 0.18067(10) 0.0212(4) Uani 1 1 d . . . H27 H 0.4007 0.2191 0.1771 0.025 Uiso 1 1 calc R . . C28 C 0.5052(2) 0.30814(13) 0.19534(11) 0.0250(4) Uani 1 1 d . . . H28 H 0.5883 0.2862 0.2026 0.030 Uiso 1 1 calc R . . C29 C 0.4949(2) 0.38015(13) 0.19936(11) 0.0278(5) Uani 1 1 d . . . H29 H 0.5705 0.4088 0.2087 0.033 Uiso 1 1 calc R . . C30 C 0.3716(2) 0.40951(13) 0.18945(11) 0.0276(5) Uani 1 1 d . . . H30 H 0.3615 0.4589 0.1920 0.033 Uiso 1 1 calc R . . C31 C 0.2634(2) 0.36644(11) 0.17591(10) 0.0223(4) Uani 1 1 d . . . H31 H 0.1795 0.3872 0.1697 0.027 Uiso 1 1 calc R . . C32 C 0.0372(3) 0.33312(13) 0.32716(12) 0.0330(5) Uani 1 1 d . . . F1 F 0.0142(2) 0.27235(9) 0.35371(8) 0.0628(6) Uani 1 1 d . . . F3 F -0.00363(18) 0.38482(8) 0.36086(8) 0.0467(4) Uani 1 1 d . . . F11 F 0.16549(16) 0.33972(8) 0.33400(8) 0.0461(4) Uani 1 1 d . . . N1 N 0.18853(17) 0.18167(9) 0.06844(8) 0.0199(3) Uani 1 1 d . . . N2 N -0.03973(16) 0.13628(9) 0.12208(9) 0.0196(3) Uani 1 1 d . . . N3 N 0.20209(16) 0.15193(9) 0.21264(8) 0.0184(3) Uani 1 1 d . . . N4 N -0.01454(17) 0.30634(10) 0.07477(9) 0.0223(4) Uani 1 1 d . . . N5 N -0.1384(2) 0.39557(12) 0.00555(11) 0.0407(6) Uani 1 1 d . . . N6 N 0.27195(16) 0.29629(9) 0.17115(8) 0.0188(3) Uani 1 1 d . . . O1 O 0.01791(14) 0.27612(8) 0.21574(7) 0.0209(3) Uani 1 1 d . . . O2 O -0.00363(17) 0.40317(9) 0.21975(8) 0.0314(4) Uani 1 1 d . . . O3 O -0.17750(16) 0.32808(11) 0.24019(12) 0.0522(6) Uani 1 1 d . . . S S -0.04266(5) 0.33707(3) 0.24124(3) 0.02300(11) Uani 1 1 d . . . Si1 Si 0.23325(5) 0.22050(3) -0.00003(3) 0.01863(11) Uani 1 1 d . . . Si2 Si -0.20531(5) 0.13060(3) 0.12314(3) 0.02266(13) Uani 1 1 d . . . Zr1 Zr 0.079328(17) 0.223135(10) 0.129938(9) 0.01583(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0382(13) 0.0260(11) 0.0244(11) 0.0016(9) 0.0108(9) 0.0184(10) C2 0.0220(10) 0.0187(9) 0.0230(10) -0.0021(8) 0.0028(8) 0.0085(8) C3 0.0227(10) 0.0211(10) 0.0363(13) -0.0117(9) -0.0022(9) 0.0061(8) C4 0.0324(12) 0.0213(11) 0.0348(13) -0.0036(9) 0.0055(10) 0.0125(9) C5 0.0142(8) 0.0191(9) 0.0224(10) 0.0037(8) 0.0039(7) 0.0021(7) C6 0.0229(10) 0.0240(11) 0.0318(12) 0.0081(9) 0.0036(9) 0.0026(8) C7 0.0291(11) 0.0305(12) 0.0307(12) 0.0150(10) -0.0054(9) -0.0018(9) C8 0.0285(11) 0.0339(12) 0.0202(10) 0.0062(9) -0.0047(9) -0.0089(9) C9 0.0204(9) 0.0270(11) 0.0189(10) 0.0018(8) -0.0010(8) -0.0026(8) C10 0.0230(11) 0.0512(16) 0.0234(11) -0.0052(11) 0.0041(9) 0.0075(10) C11 0.0316(11) 0.0270(11) 0.0231(11) -0.0048(9) 0.0057(9) -0.0055(9) C12 0.0264(10) 0.0217(10) 0.0161(9) -0.0029(8) 0.0001(8) 0.0020(8) C13 0.0446(15) 0.0316(13) 0.0338(14) -0.0116(11) -0.0103(11) 0.0063(11) C14 0.0454(15) 0.0422(14) 0.0183(11) 0.0028(10) -0.0021(10) -0.0027(12) C15 0.0243(11) 0.0535(17) 0.0244(11) -0.0053(11) -0.0042(9) 0.0043(11) C16 0.0168(9) 0.0215(10) 0.0409(13) -0.0085(9) -0.0033(9) 0.0050(8) C17 0.0291(12) 0.0271(12) 0.0451(15) -0.0160(11) -0.0078(11) 0.0018(10) C18 0.0215(10) 0.0217(11) 0.0450(14) -0.0071(10) 0.0091(10) 0.0003(8) C19 0.153(5) 0.230(7) 0.0340(19) -0.030(3) 0.035(2) -0.154(5) C20 0.257(7) 0.051(2) 0.096(3) 0.041(2) 0.113(4) 0.085(3) C21 0.045(2) 0.128(4) 0.140(4) 0.080(4) 0.052(3) 0.033(2) C22 0.0240(10) 0.0250(11) 0.0247(11) -0.0031(8) 0.0056(8) 0.0063(8) C23 0.0299(12) 0.0272(12) 0.0341(13) 0.0038(10) 0.0029(10) 0.0136(9) C24 0.0484(16) 0.0343(14) 0.0346(14) 0.0037(11) -0.0065(12) 0.0181(12) C25 0.0588(18) 0.0378(15) 0.0361(15) 0.0017(12) -0.0066(13) 0.0099(13) C26 0.0399(16) 0.0473(18) 0.086(3) 0.0187(17) 0.0195(16) 0.0164(14) C27 0.0187(9) 0.0261(10) 0.0189(9) 0.0013(8) 0.0038(7) 0.0060(8) C28 0.0168(9) 0.0384(13) 0.0198(10) 0.0016(9) 0.0043(8) 0.0036(8) C29 0.0220(10) 0.0403(13) 0.0207(10) -0.0032(9) 0.0037(8) -0.0093(9) C30 0.0278(11) 0.0273(11) 0.0278(11) -0.0067(9) 0.0064(9) -0.0030(9) C31 0.0202(9) 0.0247(10) 0.0213(10) -0.0026(8) 0.0029(8) 0.0032(8) C32 0.0535(16) 0.0245(11) 0.0229(11) -0.0088(9) 0.0125(11) -0.0098(11) F1 0.1318(19) 0.0311(9) 0.0338(9) -0.0055(7) 0.0360(11) -0.0179(10) F3 0.0776(12) 0.0345(8) 0.0346(8) -0.0200(7) 0.0272(8) -0.0132(8) F11 0.0412(9) 0.0407(9) 0.0453(9) -0.0157(7) -0.0162(7) 0.0007(7) N1 0.0220(8) 0.0197(8) 0.0173(8) -0.0012(6) 0.0022(7) 0.0076(6) N2 0.0180(8) 0.0170(8) 0.0218(8) -0.0062(7) -0.0004(6) 0.0055(6) N3 0.0153(7) 0.0203(8) 0.0185(8) 0.0001(6) 0.0013(6) 0.0013(6) N4 0.0212(8) 0.0216(9) 0.0226(9) -0.0022(7) 0.0013(7) 0.0071(7) N5 0.0487(13) 0.0424(13) 0.0317(11) 0.0112(10) 0.0102(10) 0.0278(11) N6 0.0167(8) 0.0234(8) 0.0159(8) -0.0004(6) 0.0024(6) 0.0039(6) O1 0.0186(7) 0.0227(7) 0.0218(7) -0.0074(6) 0.0050(5) 0.0024(6) O2 0.0396(9) 0.0240(8) 0.0311(9) -0.0039(7) 0.0083(7) 0.0080(7) O3 0.0171(8) 0.0534(12) 0.0885(17) -0.0479(12) 0.0167(9) -0.0097(8) S 0.0150(2) 0.0265(3) 0.0280(3) -0.0135(2) 0.00559(19) -0.00161(19) Si1 0.0184(2) 0.0224(3) 0.0143(2) -0.0030(2) 0.00146(19) 0.0030(2) Si2 0.0154(2) 0.0169(3) 0.0322(3) -0.0086(2) -0.0026(2) 0.0022(2) Zr1 0.01409(8) 0.01658(9) 0.01553(9) -0.00306(7) 0.00015(6) 0.00507(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.477(3) . ? C1 C2 1.541(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.515(3) . ? C2 C4 1.538(3) . ? C2 C3 1.548(3) . ? C3 N2 1.476(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.357(3) . ? C5 C6 1.391(3) . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C8 1.378(4) . ? C7 H7 0.9500 . ? C8 C9 1.372(3) . ? C8 H8 0.9500 . ? C9 N3 1.348(3) . ? C9 H9 0.9500 . ? C10 Si1 1.865(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.868(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.524(3) . ? C12 C13 1.535(3) . ? C12 C14 1.536(3) . ? C12 Si1 1.907(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.863(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.876(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.492(4) . ? C18 C19 1.494(4) . ? C18 C21 1.511(4) . ? C18 Si2 1.904(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N4 1.201(3) . ? C22 N5 1.227(3) . ? C23 N5 1.475(3) . ? C23 C26 1.511(4) . ? C23 C24 1.520(3) . ? C23 C25 1.522(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N6 1.349(2) . ? C27 C28 1.381(3) . ? C27 H27 0.9500 . ? C28 C29 1.381(3) . ? C28 H28 0.9500 . ? C29 C30 1.384(3) . ? C29 H29 0.9500 . ? C30 C31 1.382(3) . ? C30 H30 0.9500 . ? C31 N6 1.345(3) . ? C31 H31 0.9500 . ? C32 F1 1.328(3) . ? C32 F11 1.329(3) . ? C32 F3 1.332(3) . ? C32 S 1.811(3) . ? N1 Si1 1.7555(19) . ? N1 Zr1 2.0480(17) . ? N2 Si2 1.7456(18) . ? N2 Zr1 2.0599(18) . ? N3 Zr1 2.3530(17) . ? N4 Zr1 2.0810(18) . ? N6 Zr1 2.4573(17) . ? O1 S 1.4757(15) . ? O1 Zr1 2.2608(14) . ? O2 S 1.4258(18) . ? O3 S 1.4209(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 117.13(17) . . ? N1 C1 H1A 108.0 . . ? C2 C1 H1A 108.0 . . ? N1 C1 H1B 108.0 . . ? C2 C1 H1B 108.0 . . ? H1A C1 H1B 107.3 . . ? C5 C2 C4 111.35(17) . . ? C5 C2 C1 111.25(18) . . ? C4 C2 C1 105.79(18) . . ? C5 C2 C3 110.87(17) . . ? C4 C2 C3 105.61(18) . . ? C1 C2 C3 111.73(18) . . ? N2 C3 C2 117.19(17) . . ? N2 C3 H3A 108.0 . . ? C2 C3 H3A 108.0 . . ? N2 C3 H3B 108.0 . . ? C2 C3 H3B 108.0 . . ? H3A C3 H3B 107.2 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 120.3(2) . . ? N3 C5 C2 116.66(17) . . ? C6 C5 C2 123.08(19) . . ? C7 C6 C5 119.7(2) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C8 C7 C6 119.6(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 118.3(2) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? N3 C9 C8 123.1(2) . . ? N3 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 108.4(2) . . ? C15 C12 C14 108.5(2) . . ? C13 C12 C14 107.2(2) . . ? C15 C12 Si1 111.59(15) . . ? C13 C12 Si1 111.81(15) . . ? C14 C12 Si1 109.23(16) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 108.5(4) . . ? C20 C18 C21 106.7(3) . . ? C19 C18 C21 106.9(4) . . ? C20 C18 Si2 113.3(2) . . ? C19 C18 Si2 110.6(2) . . ? C21 C18 Si2 110.5(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 N5 172.7(2) . . ? N5 C23 C26 109.3(2) . . ? N5 C23 C24 106.2(2) . . ? C26 C23 C24 111.4(2) . . ? N5 C23 C25 109.1(2) . . ? C26 C23 C25 110.8(3) . . ? C24 C23 C25 110.0(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 C28 123.4(2) . . ? N6 C27 H27 118.3 . . ? C28 C27 H27 118.3 . . ? C27 C28 C29 118.9(2) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 118.4(2) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C31 C30 C29 119.5(2) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? N6 C31 C30 122.8(2) . . ? N6 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? F1 C32 F11 107.9(2) . . ? F1 C32 F3 108.6(2) . . ? F11 C32 F3 107.72(19) . . ? F1 C32 S 111.14(17) . . ? F11 C32 S 110.50(17) . . ? F3 C32 S 110.87(19) . . ? C1 N1 Si1 112.34(14) . . ? C1 N1 Zr1 118.60(14) . . ? Si1 N1 Zr1 128.70(9) . . ? C3 N2 Si2 112.93(14) . . ? C3 N2 Zr1 117.43(13) . . ? Si2 N2 Zr1 129.61(9) . . ? C9 N3 C5 118.98(18) . . ? C9 N3 Zr1 124.07(14) . . ? C5 N3 Zr1 116.94(13) . . ? C22 N4 Zr1 174.57(18) . . ? C22 N5 C23 126.2(2) . . ? C31 N6 C27 117.04(18) . . ? C31 N6 Zr1 121.82(13) . . ? C27 N6 Zr1 120.43(14) . . ? S O1 Zr1 148.43(10) . . ? O3 S O2 116.90(12) . . ? O3 S O1 113.72(10) . . ? O2 S O1 114.15(9) . . ? O3 S C32 105.25(14) . . ? O2 S C32 104.06(11) . . ? O1 S C32 100.24(11) . . ? N1 Si1 C10 108.83(10) . . ? N1 Si1 C11 111.48(9) . . ? C10 Si1 C11 106.41(12) . . ? N1 Si1 C12 111.54(9) . . ? C10 Si1 C12 108.87(10) . . ? C11 Si1 C12 109.55(10) . . ? N2 Si2 C16 107.65(10) . . ? N2 Si2 C17 109.75(10) . . ? C16 Si2 C17 107.34(11) . . ? N2 Si2 C18 112.49(10) . . ? C16 Si2 C18 110.78(11) . . ? C17 Si2 C18 108.71(12) . . ? N1 Zr1 N2 92.85(7) . . ? N1 Zr1 N4 102.19(7) . . ? N2 Zr1 N4 111.10(7) . . ? N1 Zr1 O1 163.02(6) . . ? N2 Zr1 O1 98.80(6) . . ? N4 Zr1 O1 85.14(6) . . ? N1 Zr1 N3 86.72(6) . . ? N2 Zr1 N3 79.87(6) . . ? N4 Zr1 N3 165.17(6) . . ? O1 Zr1 N3 83.25(6) . . ? N1 Zr1 N6 84.85(6) . . ? N2 Zr1 N6 157.60(6) . . ? N4 Zr1 N6 91.12(6) . . ? O1 Zr1 N6 79.66(5) . . ? N3 Zr1 N6 77.76(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C5 -69.5(2) . . . . ? N1 C1 C2 C4 169.46(19) . . . . ? N1 C1 C2 C3 55.0(3) . . . . ? C5 C2 C3 N2 57.3(3) . . . . ? C4 C2 C3 N2 178.1(2) . . . . ? C1 C2 C3 N2 -67.4(3) . . . . ? C4 C2 C5 N3 -177.72(18) . . . . ? C1 C2 C5 N3 64.5(2) . . . . ? C3 C2 C5 N3 -60.5(2) . . . . ? C4 C2 C5 C6 2.1(3) . . . . ? C1 C2 C5 C6 -115.6(2) . . . . ? C3 C2 C5 C6 119.4(2) . . . . ? N3 C5 C6 C7 3.2(3) . . . . ? C2 C5 C6 C7 -176.6(2) . . . . ? C5 C6 C7 C8 -0.4(3) . . . . ? C6 C7 C8 C9 -2.0(4) . . . . ? C7 C8 C9 N3 1.7(3) . . . . ? N6 C27 C28 C29 -1.3(3) . . . . ? C27 C28 C29 C30 1.0(3) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C29 C30 C31 N6 -0.7(3) . . . . ? C2 C1 N1 Si1 -168.71(16) . . . . ? C2 C1 N1 Zr1 5.0(3) . . . . ? C2 C3 N2 Si2 -166.59(16) . . . . ? C2 C3 N2 Zr1 15.2(3) . . . . ? C8 C9 N3 C5 1.1(3) . . . . ? C8 C9 N3 Zr1 -179.81(16) . . . . ? C6 C5 N3 C9 -3.6(3) . . . . ? C2 C5 N3 C9 176.28(18) . . . . ? C6 C5 N3 Zr1 177.29(15) . . . . ? C2 C5 N3 Zr1 -2.9(2) . . . . ? N5 C22 N4 Zr1 -113(2) . . . . ? N4 C22 N5 C23 177(2) . . . . ? C26 C23 N5 C22 -56.0(4) . . . . ? C24 C23 N5 C22 -176.3(3) . . . . ? C25 C23 N5 C22 65.3(4) . . . . ? C30 C31 N6 C27 0.4(3) . . . . ? C30 C31 N6 Zr1 -170.06(17) . . . . ? C28 C27 N6 C31 0.6(3) . . . . ? C28 C27 N6 Zr1 171.21(16) . . . . ? Zr1 O1 S O3 94.7(2) . . . . ? Zr1 O1 S O2 -42.9(2) . . . . ? Zr1 O1 S C32 -153.47(17) . . . . ? F1 C32 S O3 59.1(2) . . . . ? F11 C32 S O3 178.85(17) . . . . ? F3 C32 S O3 -61.8(2) . . . . ? F1 C32 S O2 -177.38(19) . . . . ? F11 C32 S O2 -57.66(19) . . . . ? F3 C32 S O2 61.7(2) . . . . ? F1 C32 S O1 -59.1(2) . . . . ? F11 C32 S O1 60.63(18) . . . . ? F3 C32 S O1 179.99(17) . . . . ? C1 N1 Si1 C10 -36.68(18) . . . . ? Zr1 N1 Si1 C10 150.44(13) . . . . ? C1 N1 Si1 C11 -153.74(16) . . . . ? Zr1 N1 Si1 C11 33.38(15) . . . . ? C1 N1 Si1 C12 83.44(17) . . . . ? Zr1 N1 Si1 C12 -89.44(13) . . . . ? C15 C12 Si1 N1 41.91(19) . . . . ? C13 C12 Si1 N1 -79.71(19) . . . . ? C14 C12 Si1 N1 161.86(16) . . . . ? C15 C12 Si1 C10 162.01(18) . . . . ? C13 C12 Si1 C10 40.4(2) . . . . ? C14 C12 Si1 C10 -78.04(19) . . . . ? C15 C12 Si1 C11 -82.00(19) . . . . ? C13 C12 Si1 C11 156.38(18) . . . . ? C14 C12 Si1 C11 37.95(19) . . . . ? C3 N2 Si2 C16 -160.33(16) . . . . ? Zr1 N2 Si2 C16 17.60(16) . . . . ? C3 N2 Si2 C17 -43.80(19) . . . . ? Zr1 N2 Si2 C17 134.12(14) . . . . ? C3 N2 Si2 C18 77.35(17) . . . . ? Zr1 N2 Si2 C18 -104.72(14) . . . . ? C20 C18 Si2 N2 -72.9(3) . . . . ? C19 C18 Si2 N2 49.2(4) . . . . ? C21 C18 Si2 N2 167.4(3) . . . . ? C20 C18 Si2 C16 166.6(3) . . . . ? C19 C18 Si2 C16 -71.3(4) . . . . ? C21 C18 Si2 C16 46.8(3) . . . . ? C20 C18 Si2 C17 48.9(4) . . . . ? C19 C18 Si2 C17 170.9(3) . . . . ? C21 C18 Si2 C17 -70.9(3) . . . . ? C1 N1 Zr1 N2 -42.17(16) . . . . ? Si1 N1 Zr1 N2 130.32(12) . . . . ? C1 N1 Zr1 N4 -154.47(16) . . . . ? Si1 N1 Zr1 N4 18.02(13) . . . . ? C1 N1 Zr1 O1 91.3(3) . . . . ? Si1 N1 Zr1 O1 -96.2(2) . . . . ? C1 N1 Zr1 N3 37.50(16) . . . . ? Si1 N1 Zr1 N3 -150.00(12) . . . . ? C1 N1 Zr1 N6 115.49(16) . . . . ? Si1 N1 Zr1 N6 -72.01(12) . . . . ? C3 N2 Zr1 N1 31.39(16) . . . . ? Si2 N2 Zr1 N1 -146.46(13) . . . . ? C3 N2 Zr1 N4 135.62(15) . . . . ? Si2 N2 Zr1 N4 -42.23(14) . . . . ? C3 N2 Zr1 O1 -136.22(15) . . . . ? Si2 N2 Zr1 O1 45.93(13) . . . . ? C3 N2 Zr1 N3 -54.76(15) . . . . ? Si2 N2 Zr1 N3 127.39(13) . . . . ? C3 N2 Zr1 N6 -52.0(3) . . . . ? Si2 N2 Zr1 N6 130.15(14) . . . . ? C22 N4 Zr1 N1 123.4(18) . . . . ? C22 N4 Zr1 N2 25.5(19) . . . . ? C22 N4 Zr1 O1 -72.1(18) . . . . ? C22 N4 Zr1 N3 -110.6(18) . . . . ? C22 N4 Zr1 N6 -151.6(18) . . . . ? S O1 Zr1 N1 110.7(2) . . . . ? S O1 Zr1 N2 -116.54(17) . . . . ? S O1 Zr1 N4 -5.90(17) . . . . ? S O1 Zr1 N3 164.86(18) . . . . ? S O1 Zr1 N6 86.13(17) . . . . ? C9 N3 Zr1 N1 139.48(17) . . . . ? C5 N3 Zr1 N1 -41.43(14) . . . . ? C9 N3 Zr1 N2 -127.03(17) . . . . ? C5 N3 Zr1 N2 52.06(14) . . . . ? C9 N3 Zr1 N4 11.9(4) . . . . ? C5 N3 Zr1 N4 -169.0(2) . . . . ? C9 N3 Zr1 O1 -26.79(16) . . . . ? C5 N3 Zr1 O1 152.30(14) . . . . ? C9 N3 Zr1 N6 54.05(16) . . . . ? C5 N3 Zr1 N6 -126.86(15) . . . . ? C31 N6 Zr1 N1 128.92(16) . . . . ? C27 N6 Zr1 N1 -41.22(15) . . . . ? C31 N6 Zr1 N2 -146.11(18) . . . . ? C27 N6 Zr1 N2 43.7(2) . . . . ? C31 N6 Zr1 N4 26.78(16) . . . . ? C27 N6 Zr1 N4 -143.36(16) . . . . ? C31 N6 Zr1 O1 -58.07(16) . . . . ? C27 N6 Zr1 O1 131.79(16) . . . . ? C31 N6 Zr1 N3 -143.33(17) . . . . ? C27 N6 Zr1 N3 46.53(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.923 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.089 _audit_block_code ga_hh17 _audit_block_refno 527 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_13 _database_code_depnum_ccdc_archive 'CCDC 679494' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38.50 H58 F3 N5 O4 S Si2 Zr' _chemical_formula_weight 891.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9979(6) _cell_length_b 13.3201(9) _cell_length_c 18.5380(11) _cell_angle_alpha 92.1600(10) _cell_angle_beta 103.4830(10) _cell_angle_gamma 110.4440(10) _cell_volume 2230.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52847 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13011 _reflns_number_gt 10278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'DIRDIF (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^+1.0288P] 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 13011 _refine_ls_number_parameters 509 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3323(2) 0.27399(15) 0.39005(10) 0.0148(3) Uani 1 1 d . . . H1A H 0.2967 0.2075 0.4135 0.018 Uiso 1 1 calc R . . H1B H 0.4055 0.3311 0.4301 0.018 Uiso 1 1 calc R . . C2 C 0.41376(19) 0.25208(14) 0.33319(10) 0.0137(3) Uani 1 1 d . . . C3 C 0.3154(2) 0.15358(15) 0.27316(10) 0.0161(3) Uani 1 1 d . . . H3A H 0.3719 0.1484 0.2368 0.019 Uiso 1 1 calc R . . H3B H 0.2978 0.0875 0.2981 0.019 Uiso 1 1 calc R . . C4 C 0.5382(2) 0.21980(16) 0.37871(11) 0.0180(4) Uani 1 1 d . . . H4A H 0.5914 0.2016 0.3452 0.027 Uiso 1 1 calc R . . H4B H 0.4957 0.1570 0.4033 0.027 Uiso 1 1 calc R . . H4C H 0.6069 0.2803 0.4166 0.027 Uiso 1 1 calc R . . C5 C 0.4742(2) 0.35105(14) 0.29567(10) 0.0141(3) Uani 1 1 d . . . C6 C 0.6244(2) 0.40689(16) 0.30413(11) 0.0187(4) Uani 1 1 d . . . H6 H 0.6950 0.3836 0.3352 0.022 Uiso 1 1 calc R . . C7 C 0.6715(2) 0.49620(17) 0.26755(11) 0.0213(4) Uani 1 1 d . . . H7 H 0.7741 0.5347 0.2734 0.026 Uiso 1 1 calc R . . C8 C 0.5671(2) 0.52844(16) 0.22239(11) 0.0195(4) Uani 1 1 d . . . H8 H 0.5963 0.5894 0.1965 0.023 Uiso 1 1 calc R . . C9 C 0.4195(2) 0.47021(15) 0.21568(10) 0.0165(3) Uani 1 1 d . . . H9 H 0.3477 0.4923 0.1846 0.020 Uiso 1 1 calc R . . C10 C -0.0269(2) 0.37886(16) 0.38883(11) 0.0197(4) Uani 1 1 d . . . H10A H -0.0221 0.4135 0.3433 0.030 Uiso 1 1 calc R . . H10B H -0.0482 0.4230 0.4248 0.030 Uiso 1 1 calc R . . H10C H -0.1054 0.3070 0.3764 0.030 Uiso 1 1 calc R . . C11 C 0.2946(2) 0.50284(16) 0.47090(12) 0.0232(4) Uani 1 1 d . . . H11A H 0.3879 0.4964 0.4971 0.035 Uiso 1 1 calc R . . H11B H 0.2590 0.5369 0.5062 0.035 Uiso 1 1 calc R . . H11C H 0.3109 0.5473 0.4305 0.035 Uiso 1 1 calc R . . C12 C 0.1298(2) 0.28008(16) 0.51030(11) 0.0201(4) Uani 1 1 d . . . C13 C 0.0404(3) 0.31876(19) 0.55492(12) 0.0281(5) Uani 1 1 d . . . H13A H -0.0598 0.3027 0.5233 0.042 Uiso 1 1 calc R . . H13B H 0.0892 0.3968 0.5705 0.042 Uiso 1 1 calc R . . H13C H 0.0351 0.2813 0.5992 0.042 Uiso 1 1 calc R . . C14 C 0.2767(3) 0.29126(19) 0.56514(12) 0.0278(5) Uani 1 1 d . . . H14A H 0.2569 0.2473 0.6054 0.042 Uiso 1 1 calc R . . H14B H 0.3313 0.3672 0.5864 0.042 Uiso 1 1 calc R . . H14C H 0.3358 0.2664 0.5386 0.042 Uiso 1 1 calc R . . C15 C 0.0421(3) 0.16041(17) 0.47857(13) 0.0285(5) Uani 1 1 d . . . H15A H 0.0985 0.1343 0.4509 0.043 Uiso 1 1 calc R . . H15B H -0.0533 0.1529 0.4449 0.043 Uiso 1 1 calc R . . H15C H 0.0252 0.1177 0.5198 0.043 Uiso 1 1 calc R . . C16 C -0.0838(2) 0.04133(17) 0.09599(11) 0.0247(4) Uani 1 1 d . . . H16A H -0.1371 0.0833 0.1125 0.037 Uiso 1 1 calc R . . H16B H -0.1542 -0.0305 0.0721 0.037 Uiso 1 1 calc R . . H16C H -0.0323 0.0786 0.0601 0.037 Uiso 1 1 calc R . . C17 C 0.1695(3) -0.03510(18) 0.14125(13) 0.0271(4) Uani 1 1 d . . . H17A H 0.2318 0.0168 0.1153 0.041 Uiso 1 1 calc R . . H17B H 0.1048 -0.1001 0.1062 0.041 Uiso 1 1 calc R . . H17C H 0.2324 -0.0547 0.1828 0.041 Uiso 1 1 calc R . . C18 C -0.0498(2) -0.06636(16) 0.23918(11) 0.0224(4) Uani 1 1 d . . . C19 C -0.1652(3) -0.0277(2) 0.25982(14) 0.0317(5) Uani 1 1 d . . . H19A H -0.2342 -0.0230 0.2140 0.048 Uiso 1 1 calc R . . H19B H -0.1154 0.0437 0.2898 0.048 Uiso 1 1 calc R . . H19C H -0.2200 -0.0791 0.2888 0.048 Uiso 1 1 calc R . . C20 C 0.0562(3) -0.07090(18) 0.31242(12) 0.0284(5) Uani 1 1 d . . . H20A H 0.0014 -0.1241 0.3404 0.043 Uiso 1 1 calc R . . H20B H 0.1004 0.0004 0.3425 0.043 Uiso 1 1 calc R . . H20C H 0.1345 -0.0919 0.3012 0.043 Uiso 1 1 calc R . . C21 C -0.1283(3) -0.18140(18) 0.19684(15) 0.0363(6) Uani 1 1 d . . . H21A H -0.1816 -0.2292 0.2281 0.055 Uiso 1 1 calc R . . H21B H -0.0548 -0.2078 0.1851 0.055 Uiso 1 1 calc R . . H21C H -0.1985 -0.1805 0.1503 0.055 Uiso 1 1 calc R . . C22 C -0.2367(2) 0.19475(17) 0.22040(11) 0.0210(4) Uani 1 1 d . . . C23 C -0.0104(2) 0.33335(17) 0.07494(11) 0.0216(4) Uani 1 1 d . . . H23 H -0.0807 0.3429 0.0985 0.026 Uiso 1 1 calc R . . C24 C -0.0241(2) 0.34918(17) 0.00051(12) 0.0249(4) Uani 1 1 d . . . H24 H -0.1019 0.3695 -0.0262 0.030 Uiso 1 1 calc R . . C25 C 0.0774(3) 0.33485(17) -0.03408(12) 0.0267(4) Uani 1 1 d . . . H25 H 0.0716 0.3466 -0.0848 0.032 Uiso 1 1 calc R . . C26 C 0.1877(2) 0.30308(17) 0.00631(11) 0.0245(4) Uani 1 1 d . . . H26 H 0.2578 0.2914 -0.0165 0.029 Uiso 1 1 calc R . . C27 C 0.1940(2) 0.28868(16) 0.07999(11) 0.0199(4) Uani 1 1 d . . . H27 H 0.2693 0.2662 0.1073 0.024 Uiso 1 1 calc R . . C28 C 0.2267(3) 0.66335(17) 0.28509(13) 0.0284(5) Uani 1 1 d . . . C51 C 0.4555(3) 0.7940(2) 0.03347(16) 0.0440(7) Uani 1 1 d D . . C52 C 0.4533(3) 0.7865(2) -0.04349(15) 0.0408(6) Uani 1 1 d D . . H52 H 0.4735 0.8495 -0.0679 0.049 Uiso 1 1 calc R . . C53 C 0.4217(3) 0.6871(2) -0.08263(14) 0.0336(5) Uani 1 1 d D . . H53 H 0.4198 0.6810 -0.1341 0.040 Uiso 1 1 calc R . . C54 C 0.3928(3) 0.5967(2) -0.04611(15) 0.0402(6) Uani 1 1 d D . . H54 H 0.3682 0.5278 -0.0730 0.048 Uiso 1 1 calc R . . C55 C 0.3991(3) 0.6052(3) 0.02898(16) 0.0499(7) Uani 1 1 d D . . H55 H 0.3816 0.5426 0.0538 0.060 Uiso 1 1 calc R . . C56 C 0.4300(3) 0.7023(3) 0.06750(16) 0.0447(7) Uani 1 1 d D . . H56 H 0.4342 0.7070 0.1193 0.054 Uiso 1 1 calc R . . C57 C 0.4777(4) 0.8995(3) 0.07519(19) 0.0549(8) Uani 1 1 d D . . H57A H 0.3926 0.9201 0.0551 0.082 Uiso 1 1 calc R . . H57B H 0.5679 0.9553 0.0694 0.082 Uiso 1 1 calc R . . H57C H 0.4872 0.8921 0.1284 0.082 Uiso 1 1 calc R . . C61 C 0.4314(5) 0.0274(3) 0.5480(2) 0.0682(11) Uani 1 1 d D . . H61 H 0.3824 0.0463 0.5814 0.082 Uiso 0.50 1 d PR . . C62 C 0.3509(4) -0.0411(3) 0.4831(2) 0.0647(11) Uani 1 1 d D . . H62 H 0.2460 -0.0694 0.4722 0.078 Uiso 1 1 calc R . . C63 C 0.5843(5) 0.0687(3) 0.5644(2) 0.0739(13) Uani 1 1 d D . . H63 H 0.6416 0.1161 0.6092 0.089 Uiso 1 1 calc R . . C64 C 0.3697(8) 0.0484(5) 0.5994(4) 0.0516(16) Uani 0.50 1 d PD . . H64A H 0.2704 0.0464 0.5752 0.077 Uiso 0.50 1 calc PR . . H64B H 0.4303 0.1204 0.6270 0.077 Uiso 0.50 1 calc PR . . H64C H 0.3627 -0.0058 0.6340 0.077 Uiso 0.50 1 calc PR . . F1 F 0.1775(2) 0.65902(13) 0.34610(8) 0.0435(4) Uani 1 1 d . . . F2 F 0.36261(16) 0.66316(12) 0.30457(9) 0.0388(3) Uani 1 1 d . . . F3 F 0.2334(2) 0.75656(11) 0.25931(9) 0.0479(4) Uani 1 1 d . . . N1 N 0.20560(17) 0.30718(12) 0.36113(8) 0.0142(3) Uani 1 1 d . . . N2 N 0.16937(17) 0.15342(12) 0.23066(9) 0.0155(3) Uani 1 1 d . . . N3 N 0.37275(17) 0.38321(12) 0.25126(8) 0.0142(3) Uani 1 1 d . . . N4 N -0.11049(18) 0.23258(14) 0.22187(9) 0.0203(3) Uani 1 1 d . . . N5 N 0.09813(18) 0.30506(13) 0.11527(9) 0.0181(3) Uani 1 1 d . . . O1 O -0.36411(18) 0.15533(15) 0.21844(10) 0.0374(4) Uani 1 1 d . . . O2 O 0.12528(15) 0.45843(11) 0.24787(8) 0.0185(3) Uani 1 1 d . . . O3 O 0.16683(17) 0.57282(12) 0.15038(8) 0.0235(3) Uani 1 1 d . . . O4 O -0.03881(18) 0.55420(14) 0.20494(10) 0.0326(4) Uani 1 1 d . . . S S 0.10491(5) 0.55123(4) 0.21296(3) 0.01840(10) Uani 1 1 d . . . Si1 Si 0.15410(5) 0.36575(4) 0.43070(3) 0.01340(10) Uani 1 1 d . . . Si2 Si 0.05382(6) 0.02740(4) 0.17847(3) 0.01716(11) Uani 1 1 d . . . Zr Zr 0.123715(19) 0.288532(14) 0.247501(9) 0.01281(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(8) 0.0173(8) 0.0149(8) 0.0044(6) 0.0040(6) 0.0076(7) C2 0.0128(8) 0.0139(8) 0.0147(8) 0.0015(6) 0.0026(6) 0.0061(6) C3 0.0144(8) 0.0150(8) 0.0183(9) 0.0001(7) 0.0023(7) 0.0059(7) C4 0.0155(8) 0.0205(9) 0.0199(9) 0.0047(7) 0.0029(7) 0.0096(7) C5 0.0135(8) 0.0159(8) 0.0131(8) -0.0004(6) 0.0041(6) 0.0056(7) C6 0.0140(8) 0.0220(9) 0.0194(9) 0.0011(7) 0.0039(7) 0.0062(7) C7 0.0140(9) 0.0242(10) 0.0229(10) 0.0015(8) 0.0066(7) 0.0027(7) C8 0.0181(9) 0.0187(9) 0.0204(9) 0.0028(7) 0.0088(7) 0.0030(7) C9 0.0184(9) 0.0178(9) 0.0157(8) 0.0037(7) 0.0065(7) 0.0080(7) C10 0.0172(9) 0.0246(10) 0.0215(9) 0.0045(7) 0.0067(7) 0.0118(8) C11 0.0204(10) 0.0192(9) 0.0278(10) -0.0015(8) 0.0052(8) 0.0059(8) C12 0.0266(10) 0.0214(9) 0.0179(9) 0.0061(7) 0.0107(8) 0.0118(8) C13 0.0406(13) 0.0331(12) 0.0235(10) 0.0107(9) 0.0193(9) 0.0215(10) C14 0.0369(12) 0.0360(12) 0.0181(9) 0.0093(8) 0.0070(9) 0.0222(10) C15 0.0370(12) 0.0216(10) 0.0317(11) 0.0095(8) 0.0208(10) 0.0082(9) C16 0.0236(10) 0.0255(10) 0.0177(9) 0.0002(8) 0.0004(8) 0.0037(8) C17 0.0303(11) 0.0232(10) 0.0277(11) -0.0034(8) 0.0098(9) 0.0092(9) C18 0.0228(10) 0.0173(9) 0.0219(10) 0.0022(7) 0.0053(8) 0.0015(8) C19 0.0297(12) 0.0325(12) 0.0362(13) 0.0115(10) 0.0163(10) 0.0097(10) C20 0.0336(12) 0.0229(10) 0.0250(11) 0.0086(8) 0.0059(9) 0.0066(9) C21 0.0401(14) 0.0190(10) 0.0376(13) -0.0020(9) 0.0105(11) -0.0036(10) C22 0.0209(10) 0.0270(10) 0.0153(9) 0.0013(7) 0.0043(7) 0.0096(8) C23 0.0206(9) 0.0252(10) 0.0188(9) 0.0043(7) 0.0035(7) 0.0093(8) C24 0.0288(11) 0.0228(10) 0.0193(9) 0.0042(8) -0.0012(8) 0.0097(8) C25 0.0366(12) 0.0253(10) 0.0150(9) 0.0038(8) 0.0041(8) 0.0093(9) C26 0.0295(11) 0.0244(10) 0.0185(9) 0.0019(8) 0.0083(8) 0.0075(9) C27 0.0204(9) 0.0209(9) 0.0176(9) 0.0026(7) 0.0041(7) 0.0071(8) C28 0.0421(13) 0.0199(10) 0.0289(11) 0.0056(8) 0.0128(10) 0.0161(9) C51 0.0299(13) 0.0530(17) 0.0449(15) -0.0203(13) -0.0033(11) 0.0213(12) C52 0.0442(15) 0.0379(14) 0.0401(14) 0.0014(11) -0.0015(12) 0.0233(12) C53 0.0382(13) 0.0399(13) 0.0272(11) 0.0021(10) 0.0094(10) 0.0196(11) C54 0.0423(15) 0.0382(14) 0.0354(13) 0.0045(11) 0.0118(11) 0.0082(12) C55 0.0422(16) 0.0602(19) 0.0364(15) 0.0106(13) 0.0128(12) 0.0037(14) C56 0.0339(14) 0.068(2) 0.0326(13) 0.0064(13) 0.0119(11) 0.0171(13) C57 0.0560(19) 0.0503(18) 0.0537(19) -0.0100(14) 0.0091(15) 0.0190(15) C61 0.095(3) 0.0430(18) 0.0510(19) 0.0277(15) 0.0038(19) 0.0139(18) C62 0.064(2) 0.0469(18) 0.0481(19) 0.0222(15) -0.0134(17) -0.0057(16) C63 0.080(3) 0.0431(18) 0.049(2) 0.0188(15) -0.0267(19) -0.0104(17) C64 0.077(5) 0.053(4) 0.054(4) 0.021(3) 0.042(3) 0.043(3) F1 0.0707(11) 0.0429(9) 0.0287(7) 0.0009(6) 0.0202(7) 0.0307(8) F2 0.0321(8) 0.0324(7) 0.0421(8) -0.0041(6) 0.0005(6) 0.0070(6) F3 0.0780(12) 0.0202(7) 0.0486(9) 0.0084(6) 0.0175(9) 0.0211(8) N1 0.0132(7) 0.0165(7) 0.0146(7) 0.0031(6) 0.0041(6) 0.0072(6) N2 0.0139(7) 0.0160(7) 0.0148(7) 0.0025(6) 0.0020(6) 0.0043(6) N3 0.0141(7) 0.0153(7) 0.0138(7) 0.0029(5) 0.0045(6) 0.0056(6) N4 0.0134(7) 0.0249(8) 0.0210(8) 0.0030(6) 0.0023(6) 0.0066(6) N5 0.0185(8) 0.0189(8) 0.0151(7) 0.0039(6) 0.0022(6) 0.0061(6) O1 0.0174(8) 0.0526(11) 0.0411(10) 0.0074(8) 0.0132(7) 0.0077(7) O2 0.0213(7) 0.0191(7) 0.0186(6) 0.0071(5) 0.0071(5) 0.0098(5) O3 0.0266(8) 0.0285(8) 0.0215(7) 0.0114(6) 0.0104(6) 0.0141(6) O4 0.0267(8) 0.0448(10) 0.0391(9) 0.0200(8) 0.0144(7) 0.0232(8) S 0.0200(2) 0.0209(2) 0.0199(2) 0.00874(17) 0.00806(18) 0.01185(19) Si1 0.0130(2) 0.0143(2) 0.0139(2) 0.00240(17) 0.00343(18) 0.00617(18) Si2 0.0185(3) 0.0155(2) 0.0145(2) -0.00025(18) 0.00312(19) 0.0038(2) Zr 0.01120(8) 0.01500(9) 0.01222(8) 0.00346(6) 0.00253(6) 0.00502(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.477(2) . ? C1 C2 1.550(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.515(3) . ? C2 C4 1.535(2) . ? C2 C3 1.551(2) . ? C3 N2 1.488(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.353(2) . ? C5 C6 1.390(3) . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 C8 1.381(3) . ? C7 H7 0.9500 . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 N3 1.349(2) . ? C9 H9 0.9500 . ? C10 Si1 1.8663(19) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.866(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.534(3) . ? C12 C15 1.539(3) . ? C12 C13 1.544(3) . ? C12 Si1 1.908(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.867(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.873(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.533(3) . ? C18 C19 1.533(3) . ? C18 C21 1.537(3) . ? C18 Si2 1.909(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N4 1.177(3) . ? C22 O1 1.187(3) . ? C23 N5 1.344(2) . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.380(3) . ? C24 H24 0.9500 . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C27 1.376(3) . ? C26 H26 0.9500 . ? C27 N5 1.350(3) . ? C27 H27 0.9500 . ? C28 F2 1.323(3) . ? C28 F1 1.330(3) . ? C28 F3 1.333(2) . ? C28 S 1.822(2) . ? C51 C56 1.368(4) . ? C51 C52 1.421(4) . ? C51 C57 1.497(4) . ? C52 C53 1.382(3) . ? C52 H52 0.9500 . ? C53 C54 1.378(4) . ? C53 H53 0.9500 . ? C54 C55 1.377(4) . ? C54 H54 0.9500 . ? C55 C56 1.351(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 C64 1.319(7) . ? C61 C62 1.370(5) . ? C61 C63 1.384(5) . ? C61 H61 0.9500 . ? C62 C63 1.320(6) 2_656 ? C62 H62 0.9500 . ? C63 C62 1.320(6) 2_656 ? C63 H63 0.9500 . ? C64 H61 0.3870 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N1 Si1 1.7469(16) . ? N1 Zr 2.0453(15) . ? N2 Si2 1.7579(16) . ? N2 Zr 2.0353(16) . ? N3 Zr 2.3480(15) . ? N4 Zr 2.1212(16) . ? N5 Zr 2.4312(16) . ? O2 S 1.4707(14) . ? O2 Zr 2.2573(13) . ? O3 S 1.4309(15) . ? O4 S 1.4244(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 117.27(14) . . ? N1 C1 H1A 108.0 . . ? C2 C1 H1A 108.0 . . ? N1 C1 H1B 108.0 . . ? C2 C1 H1B 108.0 . . ? H1A C1 H1B 107.2 . . ? C5 C2 C4 111.53(15) . . ? C5 C2 C1 111.29(14) . . ? C4 C2 C1 105.51(14) . . ? C5 C2 C3 109.96(14) . . ? C4 C2 C3 105.50(14) . . ? C1 C2 C3 112.85(15) . . ? N2 C3 C2 116.99(14) . . ? N2 C3 H3A 108.1 . . ? C2 C3 H3A 108.1 . . ? N2 C3 H3B 108.1 . . ? C2 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 120.29(17) . . ? N3 C5 C2 116.16(15) . . ? C6 C5 C2 123.55(17) . . ? C7 C6 C5 120.35(18) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 118.93(18) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 118.50(18) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? N3 C9 C8 122.90(18) . . ? N3 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 109.45(18) . . ? C14 C12 C13 107.42(17) . . ? C15 C12 C13 108.57(17) . . ? C14 C12 Si1 113.34(14) . . ? C15 C12 Si1 110.14(14) . . ? C13 C12 Si1 107.77(13) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 107.42(18) . . ? C20 C18 C21 108.19(19) . . ? C19 C18 C21 108.92(19) . . ? C20 C18 Si2 111.30(14) . . ? C19 C18 Si2 111.17(15) . . ? C21 C18 Si2 109.74(15) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 O1 179.1(3) . . ? N5 C23 C24 122.83(19) . . ? N5 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 118.8(2) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 118.94(19) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 118.9(2) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? N5 C27 C26 122.98(19) . . ? N5 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? F2 C28 F1 108.16(19) . . ? F2 C28 F3 108.0(2) . . ? F1 C28 F3 108.31(18) . . ? F2 C28 S 111.39(14) . . ? F1 C28 S 111.29(17) . . ? F3 C28 S 109.56(16) . . ? C56 C51 C52 118.8(2) . . ? C56 C51 C57 120.8(3) . . ? C52 C51 C57 120.3(3) . . ? C53 C52 C51 119.6(3) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C54 C53 C52 119.2(2) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 120.7(3) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C56 C55 C54 120.3(3) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C51 121.4(3) . . ? C55 C56 H56 119.3 . . ? C51 C56 H56 119.3 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C64 C61 C62 122.5(5) . . ? C64 C61 C63 117.6(5) . . ? C62 C61 C63 119.6(4) . . ? C64 C61 H61 5.9 . . ? C62 C61 H61 120.2 . . ? C63 C61 H61 120.3 . . ? C63 C62 C61 121.5(4) 2_656 . ? C63 C62 H62 119.2 2_656 . ? C61 C62 H62 119.2 . . ? C62 C63 C61 118.9(4) 2_656 . ? C62 C63 H63 120.6 2_656 . ? C61 C63 H63 120.6 . . ? C61 C64 H61 14.6 . . ? C61 C64 H64A 109.5 . . ? H61 C64 H64A 97.4 . . ? C61 C64 H64B 109.5 . . ? H61 C64 H64B 107.4 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H61 C64 H64C 122.7 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C1 N1 Si1 113.82(11) . . ? C1 N1 Zr 117.16(11) . . ? Si1 N1 Zr 128.89(8) . . ? C3 N2 Si2 112.57(12) . . ? C3 N2 Zr 117.75(11) . . ? Si2 N2 Zr 129.40(9) . . ? C9 N3 C5 119.03(16) . . ? C9 N3 Zr 123.97(12) . . ? C5 N3 Zr 116.88(12) . . ? C22 N4 Zr 167.54(16) . . ? C23 N5 C27 117.50(17) . . ? C23 N5 Zr 121.07(13) . . ? C27 N5 Zr 121.42(13) . . ? S O2 Zr 154.70(9) . . ? O4 S O3 117.26(9) . . ? O4 S O2 113.79(9) . . ? O3 S O2 113.31(8) . . ? O4 S C28 104.73(11) . . ? O3 S C28 103.89(10) . . ? O2 S C28 101.51(9) . . ? N1 Si1 C11 110.93(9) . . ? N1 Si1 C10 108.91(8) . . ? C11 Si1 C10 108.70(9) . . ? N1 Si1 C12 112.24(8) . . ? C11 Si1 C12 108.36(10) . . ? C10 Si1 C12 107.59(9) . . ? N2 Si2 C16 111.70(9) . . ? N2 Si2 C17 109.01(9) . . ? C16 Si2 C17 106.92(10) . . ? N2 Si2 C18 110.74(8) . . ? C16 Si2 C18 108.81(10) . . ? C17 Si2 C18 109.58(10) . . ? N2 Zr N1 93.78(6) . . ? N2 Zr N4 104.67(6) . . ? N1 Zr N4 108.58(6) . . ? N2 Zr O2 162.89(6) . . ? N1 Zr O2 93.08(5) . . ? N4 Zr O2 87.91(6) . . ? N2 Zr N3 85.17(6) . . ? N1 Zr N3 83.00(6) . . ? N4 Zr N3 163.89(6) . . ? O2 Zr N3 80.14(5) . . ? N2 Zr N5 88.43(6) . . ? N1 Zr N5 163.19(6) . . ? N4 Zr N5 86.87(6) . . ? O2 Zr N5 80.59(5) . . ? N3 Zr N5 80.58(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 N1 C1 C2 C5 58.8(2) . . . . ? N1 C1 C2 C4 179.93(15) . . . . ? N1 C1 C2 C3 -65.4(2) . . . . ? C5 C2 C3 N2 -71.54(19) . . . . ? C4 C2 C3 N2 168.07(15) . . . . ? C1 C2 C3 N2 53.4(2) . . . . ? C4 C2 C5 N3 177.05(15) . . . . ? C1 C2 C5 N3 -65.42(19) . . . . ? C3 C2 C5 N3 60.38(19) . . . . ? C4 C2 C5 C6 -2.1(2) . . . . ? C1 C2 C5 C6 115.46(19) . . . . ? C3 C2 C5 C6 -118.75(19) . . . . ? N3 C5 C6 C7 0.3(3) . . . . ? C2 C5 C6 C7 179.41(17) . . . . ? C5 C6 C7 C8 -0.3(3) . . . . ? C6 C7 C8 C9 0.1(3) . . . . ? C7 C8 C9 N3 0.0(3) . . . . ? N5 C23 C24 C25 0.3(3) . . . . ? C23 C24 C25 C26 1.2(3) . . . . ? C24 C25 C26 C27 -1.1(3) . . . . ? C25 C26 C27 N5 -0.6(3) . . . . ? C56 C51 C52 C53 1.8(4) . . . . ? C57 C51 C52 C53 -175.2(3) . . . . ? C51 C52 C53 C54 0.0(4) . . . . ? C52 C53 C54 C55 -1.8(4) . . . . ? C53 C54 C55 C56 1.7(5) . . . . ? C54 C55 C56 C51 0.1(5) . . . . ? C52 C51 C56 C55 -1.9(4) . . . . ? C57 C51 C56 C55 175.1(3) . . . . ? C64 C61 C62 C63 -173.9(4) . . . 2_656 ? C63 C61 C62 C63 -0.2(6) . . . 2_656 ? C64 C61 C63 C62 174.2(4) . . . 2_656 ? C62 C61 C63 C62 0.2(5) . . . 2_656 ? C2 C1 N1 Si1 -163.05(12) . . . . ? C2 C1 N1 Zr 13.1(2) . . . . ? C2 C3 N2 Si2 -168.02(13) . . . . ? C2 C3 N2 Zr 6.4(2) . . . . ? C8 C9 N3 C5 0.0(3) . . . . ? C8 C9 N3 Zr 175.95(14) . . . . ? C6 C5 N3 C9 -0.2(3) . . . . ? C2 C5 N3 C9 -179.36(15) . . . . ? C6 C5 N3 Zr -176.40(13) . . . . ? C2 C5 N3 Zr 4.45(19) . . . . ? O1 C22 N4 Zr -91(18) . . . . ? C24 C23 N5 C27 -2.0(3) . . . . ? C24 C23 N5 Zr 176.51(15) . . . . ? C26 C27 N5 C23 2.2(3) . . . . ? C26 C27 N5 Zr -176.35(15) . . . . ? Zr O2 S O4 92.0(2) . . . . ? Zr O2 S O3 -45.3(2) . . . . ? Zr O2 S C28 -156.0(2) . . . . ? F2 C28 S O4 172.90(15) . . . . ? F1 C28 S O4 52.11(18) . . . . ? F3 C28 S O4 -67.65(18) . . . . ? F2 C28 S O3 -63.53(17) . . . . ? F1 C28 S O3 175.68(15) . . . . ? F3 C28 S O3 55.92(18) . . . . ? F2 C28 S O2 54.27(17) . . . . ? F1 C28 S O2 -66.52(17) . . . . ? F3 C28 S O2 173.72(16) . . . . ? C1 N1 Si1 C11 71.21(15) . . . . ? Zr N1 Si1 C11 -104.39(12) . . . . ? C1 N1 Si1 C10 -169.20(13) . . . . ? Zr N1 Si1 C10 15.20(14) . . . . ? C1 N1 Si1 C12 -50.18(15) . . . . ? Zr N1 Si1 C12 134.23(11) . . . . ? C14 C12 Si1 N1 78.32(16) . . . . ? C15 C12 Si1 N1 -44.67(17) . . . . ? C13 C12 Si1 N1 -162.95(14) . . . . ? C14 C12 Si1 C11 -44.53(16) . . . . ? C15 C12 Si1 C11 -167.52(14) . . . . ? C13 C12 Si1 C11 74.21(17) . . . . ? C14 C12 Si1 C10 -161.88(14) . . . . ? C15 C12 Si1 C10 75.12(16) . . . . ? C13 C12 Si1 C10 -43.15(17) . . . . ? C3 N2 Si2 C16 -154.17(13) . . . . ? Zr N2 Si2 C16 32.17(14) . . . . ? C3 N2 Si2 C17 -36.24(15) . . . . ? Zr N2 Si2 C17 150.09(12) . . . . ? C3 N2 Si2 C18 84.38(14) . . . . ? Zr N2 Si2 C18 -89.28(13) . . . . ? C20 C18 Si2 N2 -50.37(17) . . . . ? C19 C18 Si2 N2 69.34(17) . . . . ? C21 C18 Si2 N2 -170.10(15) . . . . ? C20 C18 Si2 C16 -173.50(15) . . . . ? C19 C18 Si2 C16 -53.79(17) . . . . ? C21 C18 Si2 C16 66.77(18) . . . . ? C20 C18 Si2 C17 69.91(17) . . . . ? C19 C18 Si2 C17 -170.37(15) . . . . ? C21 C18 Si2 C17 -49.82(19) . . . . ? C3 N2 Zr N1 -43.57(13) . . . . ? Si2 N2 Zr N1 129.81(11) . . . . ? C3 N2 Zr N4 -153.90(13) . . . . ? Si2 N2 Zr N4 19.49(12) . . . . ? C3 N2 Zr O2 69.9(2) . . . . ? Si2 N2 Zr O2 -116.74(18) . . . . ? C3 N2 Zr N3 39.07(13) . . . . ? Si2 N2 Zr N3 -147.55(11) . . . . ? C3 N2 Zr N5 119.74(13) . . . . ? Si2 N2 Zr N5 -66.87(11) . . . . ? C1 N1 Zr N2 33.30(13) . . . . ? Si1 N1 Zr N2 -151.23(11) . . . . ? C1 N1 Zr N4 140.15(12) . . . . ? Si1 N1 Zr N4 -44.38(12) . . . . ? C1 N1 Zr O2 -131.02(12) . . . . ? Si1 N1 Zr O2 44.45(11) . . . . ? C1 N1 Zr N3 -51.36(12) . . . . ? Si1 N1 Zr N3 124.11(11) . . . . ? C1 N1 Zr N5 -63.8(2) . . . . ? Si1 N1 Zr N5 111.63(19) . . . . ? C22 N4 Zr N2 75.9(8) . . . . ? C22 N4 Zr N1 -23.3(8) . . . . ? C22 N4 Zr O2 -115.9(8) . . . . ? C22 N4 Zr N3 -157.8(7) . . . . ? C22 N4 Zr N5 163.4(8) . . . . ? S O2 Zr N2 63.0(3) . . . . ? S O2 Zr N1 176.6(2) . . . . ? S O2 Zr N4 -74.9(2) . . . . ? S O2 Zr N3 94.2(2) . . . . ? S O2 Zr N5 12.2(2) . . . . ? C9 N3 Zr N2 135.30(14) . . . . ? C5 N3 Zr N2 -48.71(13) . . . . ? C9 N3 Zr N1 -130.28(14) . . . . ? C5 N3 Zr N1 45.71(12) . . . . ? C9 N3 Zr N4 6.8(3) . . . . ? C5 N3 Zr N4 -177.25(19) . . . . ? C9 N3 Zr O2 -35.90(14) . . . . ? C5 N3 Zr O2 140.08(13) . . . . ? C9 N3 Zr N5 46.09(14) . . . . ? C5 N3 Zr N5 -137.92(13) . . . . ? C23 N5 Zr N2 138.94(15) . . . . ? C27 N5 Zr N2 -42.59(15) . . . . ? C23 N5 Zr N1 -123.1(2) . . . . ? C27 N5 Zr N1 55.3(3) . . . . ? C23 N5 Zr N4 34.16(15) . . . . ? C27 N5 Zr N4 -147.38(15) . . . . ? C23 N5 Zr O2 -54.24(15) . . . . ? C27 N5 Zr O2 124.23(15) . . . . ? C23 N5 Zr N3 -135.70(15) . . . . ? C27 N5 Zr N3 42.77(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.565 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.087 _audit_block_code ga_hh25 _audit_block_refno 623 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #===end=== data_complex_14 _database_code_depnum_ccdc_archive 'CCDC 687177' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H92 F6 N10 O6 S2 Si4 Zr2' _chemical_formula_weight 1450.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.451(3) _cell_length_b 10.513(3) _cell_length_c 16.952(5) _cell_angle_alpha 101.762(6) _cell_angle_beta 90.268(6) _cell_angle_gamma 109.007(5) _cell_volume 1719.0(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6316 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector (Bruker AXS Smart 1000)' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26268 _diffrn_reflns_av_R_equivalents 0.0961 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6069 _reflns_number_gt 4074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 1997-2003)' _computing_cell_refinement 'SAINT (Bruker AXS, 1997-2006)' _computing_data_reduction 'SAINT (Bruker AXS, 1997-2006)' _computing_structure_solution 'SIR-2004 (Giacovazzo, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2005)' _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^)+(0.0863P)^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 6069 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3913(5) -0.1562(5) 0.2811(3) 0.0246(12) Uani 1 1 d . . . H1A H 0.3583 -0.2514 0.2480 0.030 Uiso 1 1 calc R . . H1B H 0.3509 -0.1587 0.3336 0.030 Uiso 1 1 calc R . . C2 C 0.5476(5) -0.1136(5) 0.2971(3) 0.0226(12) Uani 1 1 d . . . C3 C 0.6156(5) 0.0433(5) 0.3334(3) 0.0239(12) Uani 1 1 d . . . H3A H 0.5693 0.0673 0.3822 0.029 Uiso 1 1 calc R . . H3B H 0.7109 0.0594 0.3514 0.029 Uiso 1 1 calc R . . C4 C 0.5714(6) -0.1859(6) 0.3636(4) 0.0400(16) Uani 1 1 d . . . H4A H 0.5285 -0.2858 0.3452 0.060 Uiso 1 1 calc R . . H4B H 0.5316 -0.1539 0.4128 0.060 Uiso 1 1 calc R . . H4C H 0.6691 -0.1639 0.3752 0.060 Uiso 1 1 calc R . . C5 C 0.6113(5) -0.1560(5) 0.2217(3) 0.0223(12) Uani 1 1 d . . . C6 C 0.6904(5) -0.2430(5) 0.2151(4) 0.0283(13) Uani 1 1 d . . . H6 H 0.7065 -0.2776 0.2604 0.034 Uiso 1 1 calc R . . C7 C 0.7439(6) -0.2778(6) 0.1441(4) 0.0393(17) Uani 1 1 d . . . H7 H 0.7971 -0.3365 0.1400 0.047 Uiso 1 1 calc R . . C8 C 0.7211(6) -0.2283(6) 0.0785(4) 0.0394(16) Uani 1 1 d . . . H8 H 0.7588 -0.2506 0.0288 0.047 Uiso 1 1 calc R . . C9 C 0.6402(6) -0.1437(6) 0.0871(4) 0.0294(13) Uani 1 1 d . . . H9 H 0.6226 -0.1096 0.0419 0.035 Uiso 1 1 calc R . . C10 C 0.0888(6) -0.0277(6) 0.1829(3) 0.0295(13) Uani 1 1 d . . . H10A H 0.1589 0.0302 0.1550 0.044 Uiso 1 1 calc R . . H10B H 0.0336 0.0255 0.2096 0.044 Uiso 1 1 calc R . . H10C H 0.0308 -0.1083 0.1436 0.044 Uiso 1 1 calc R . . C11 C 0.0709(6) -0.2720(6) 0.2549(5) 0.049(2) Uani 1 1 d . . . H11A H 0.0796 -0.3274 0.2025 0.073 Uiso 1 1 calc R . . H11B H -0.0249 -0.2822 0.2611 0.073 Uiso 1 1 calc R . . H11C H 0.1058 -0.3035 0.2983 0.073 Uiso 1 1 calc R . . C12 C 0.1538(6) 0.0140(8) 0.3634(4) 0.0442(17) Uani 1 1 d . . . C13 C 0.2266(8) -0.0174(13) 0.4314(4) 0.096(4) Uani 1 1 d . . . H13A H 0.3250 0.0221 0.4289 0.144 Uiso 1 1 calc R . . H13B H 0.2009 -0.1175 0.4253 0.144 Uiso 1 1 calc R . . H13C H 0.2007 0.0228 0.4836 0.144 Uiso 1 1 calc R . . C14 C 0.2122(7) 0.1689(8) 0.3662(5) 0.068(3) Uani 1 1 d . . . H14A H 0.2230 0.2202 0.4224 0.102 Uiso 1 1 calc R . . H14B H 0.1503 0.1957 0.3347 0.102 Uiso 1 1 calc R . . H14C H 0.3008 0.1901 0.3434 0.102 Uiso 1 1 calc R . . C15 C 0.0010(7) -0.0231(9) 0.3793(4) 0.059(2) Uani 1 1 d . . . H15A H -0.0344 -0.1186 0.3857 0.088 Uiso 1 1 calc R . . H15B H -0.0494 -0.0128 0.3335 0.088 Uiso 1 1 calc R . . H15C H -0.0094 0.0388 0.4286 0.088 Uiso 1 1 calc R . . C16 C 0.9107(6) 0.2888(6) 0.3003(5) 0.0460(19) Uani 1 1 d . . . H16A H 0.9198 0.2190 0.3284 0.069 Uiso 1 1 calc R . . H16B H 0.9790 0.3781 0.3242 0.069 Uiso 1 1 calc R . . H16C H 0.9243 0.2623 0.2430 0.069 Uiso 1 1 calc R . . C17 C 0.7111(6) 0.4156(5) 0.2451(4) 0.0414(17) Uani 1 1 d . . . H17A H 0.7052 0.3690 0.1882 0.062 Uiso 1 1 calc R . . H17B H 0.7879 0.5021 0.2555 0.062 Uiso 1 1 calc R . . H17C H 0.6270 0.4353 0.2569 0.062 Uiso 1 1 calc R . . C18 C 0.7292(6) 0.3894(6) 0.4197(4) 0.0440(18) Uani 1 1 d . . . C19 C 0.8171(8) 0.5456(7) 0.4319(6) 0.075(3) Uani 1 1 d . . . H19A H 0.8228 0.5907 0.4890 0.112 Uiso 1 1 calc R . . H19B H 0.7748 0.5900 0.3991 0.112 Uiso 1 1 calc R . . H19C H 0.9085 0.5535 0.4152 0.112 Uiso 1 1 calc R . . C20 C 0.5844(7) 0.3767(8) 0.4370(4) 0.059(2) Uani 1 1 d . . . H20A H 0.5286 0.2790 0.4266 0.088 Uiso 1 1 calc R . . H20B H 0.5491 0.4231 0.4020 0.088 Uiso 1 1 calc R . . H20C H 0.5816 0.4196 0.4937 0.088 Uiso 1 1 calc R . . C21 C 0.7894(8) 0.3293(8) 0.4804(5) 0.061(2) Uani 1 1 d . . . H21A H 0.7852 0.3784 0.5355 0.092 Uiso 1 1 calc R . . H21B H 0.8841 0.3401 0.4701 0.092 Uiso 1 1 calc R . . H21C H 0.7372 0.2312 0.4741 0.092 Uiso 1 1 calc R . . C22 C 0.4342(6) 0.3951(5) 0.1127(3) 0.0256(12) Uani 1 1 d . . . H22 H 0.5123 0.3807 0.0895 0.031 Uiso 1 1 calc R . . C23 C 0.3926(6) 0.4995(5) 0.0971(3) 0.0292(13) Uani 1 1 d . . . H23 H 0.4425 0.5563 0.0630 0.035 Uiso 1 1 calc R . . C24 C 0.2817(6) 0.5229(6) 0.1295(4) 0.0395(17) Uani 1 1 d . . . H24 H 0.2537 0.5957 0.1190 0.047 Uiso 1 1 calc R . . C25 C 0.2126(7) 0.4397(7) 0.1768(7) 0.079(3) Uani 1 1 d . . . H25 H 0.1326 0.4516 0.1985 0.095 Uiso 1 1 calc R . . C26 C 0.2565(7) 0.3370(7) 0.1944(7) 0.083(3) Uani 1 1 d . . . H26 H 0.2094 0.2832 0.2306 0.099 Uiso 1 1 calc R . . C27 C 0.8613(6) 0.2302(7) 0.0280(4) 0.0368(15) Uani 1 1 d . . . F1 F 0.9071(4) 0.3284(4) 0.0946(2) 0.0568(11) Uani 1 1 d . . . F2 F 0.9166(3) 0.2817(4) -0.0339(2) 0.0486(10) Uani 1 1 d . . . F3 F 0.9035(3) 0.1272(4) 0.0338(2) 0.0498(10) Uani 1 1 d . . . N1 N 0.3377(4) -0.0699(4) 0.2405(3) 0.0184(9) Uani 1 1 d . . . N2 N 0.6163(4) 0.1399(4) 0.2811(3) 0.0201(10) Uani 1 1 d . . . N3 N 0.5868(4) -0.1090(4) 0.1564(3) 0.0202(10) Uani 1 1 d . . . N4 N 0.4023(5) 0.2081(4) 0.1753(3) 0.0319(12) Uani 1 1 d . . . N5 N 0.3642(4) 0.3125(4) 0.1611(3) 0.0325(12) Uani 1 1 d . . . O1 O 0.6391(3) 0.1352(4) 0.0907(2) 0.0240(8) Uani 1 1 d . . . O2 O 0.6384(4) 0.0627(4) -0.0535(2) 0.0320(9) Uani 1 1 d . . . O3 O 0.6523(4) 0.2993(4) 0.0061(3) 0.0382(10) Uani 1 1 d . . . S1 S 0.67739(13) 0.17745(15) 0.01612(9) 0.0268(3) Uani 1 1 d . . . Si1 Si 0.17099(14) -0.08593(14) 0.26002(9) 0.0208(3) Uani 1 1 d . . . Si2 Si 0.73645(15) 0.30207(14) 0.31083(10) 0.0275(4) Uani 1 1 d . . . Zr Zr 0.47515(5) 0.06353(5) 0.18155(3) 0.01709(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.024(3) 0.030(3) 0.014(2) 0.002(2) 0.010(2) C2 0.024(3) 0.017(3) 0.027(3) 0.013(2) -0.004(2) 0.001(2) C3 0.024(3) 0.022(3) 0.025(3) 0.005(2) -0.002(2) 0.007(2) C4 0.026(3) 0.041(4) 0.056(5) 0.038(3) -0.001(3) 0.000(3) C5 0.019(3) 0.013(2) 0.031(3) 0.005(2) -0.004(2) 0.001(2) C6 0.027(3) 0.012(3) 0.042(4) 0.001(2) -0.012(3) 0.005(2) C7 0.030(3) 0.027(3) 0.057(5) -0.013(3) -0.016(3) 0.018(3) C8 0.031(3) 0.041(4) 0.039(4) -0.019(3) -0.011(3) 0.020(3) C9 0.029(3) 0.029(3) 0.028(3) -0.005(2) -0.005(3) 0.014(3) C10 0.032(3) 0.033(3) 0.028(3) 0.010(3) 0.004(3) 0.015(3) C11 0.027(3) 0.031(3) 0.097(6) 0.036(4) -0.001(4) 0.008(3) C12 0.032(4) 0.080(5) 0.022(4) 0.004(3) 0.004(3) 0.023(3) C13 0.050(5) 0.234(13) 0.028(5) 0.029(6) 0.004(4) 0.080(7) C14 0.042(4) 0.071(5) 0.068(6) -0.046(4) -0.002(4) 0.025(4) C15 0.037(4) 0.123(7) 0.031(4) 0.023(4) 0.015(3) 0.042(4) C16 0.025(3) 0.020(3) 0.088(6) 0.008(3) 0.015(3) 0.002(3) C17 0.028(3) 0.012(3) 0.082(5) 0.014(3) 0.010(3) 0.002(2) C18 0.039(4) 0.025(3) 0.056(5) -0.023(3) -0.013(3) 0.014(3) C19 0.063(5) 0.027(4) 0.107(7) -0.034(4) -0.031(5) 0.010(4) C20 0.062(5) 0.067(5) 0.044(5) -0.021(4) 0.003(4) 0.036(4) C21 0.066(5) 0.063(5) 0.051(5) -0.021(4) -0.018(4) 0.036(4) C22 0.032(3) 0.018(3) 0.031(3) 0.012(2) 0.005(3) 0.011(2) C23 0.043(3) 0.019(3) 0.028(3) 0.003(2) -0.005(3) 0.013(3) C24 0.025(3) 0.019(3) 0.077(5) 0.014(3) -0.003(3) 0.009(2) C25 0.043(4) 0.048(4) 0.179(10) 0.067(6) 0.054(6) 0.032(4) C26 0.051(4) 0.049(4) 0.191(11) 0.077(6) 0.071(6) 0.042(4) C27 0.030(3) 0.049(4) 0.028(4) 0.008(3) 0.003(3) 0.008(3) F1 0.036(2) 0.069(3) 0.043(3) -0.003(2) 0.0063(18) -0.0037(19) F2 0.035(2) 0.063(2) 0.044(2) 0.0226(19) 0.0184(18) 0.0053(18) F3 0.029(2) 0.072(3) 0.058(3) 0.026(2) 0.0081(18) 0.0229(19) N1 0.023(2) 0.011(2) 0.020(2) 0.0012(17) -0.0030(19) 0.0061(17) N2 0.023(2) 0.008(2) 0.026(3) 0.0052(18) 0.005(2) 0.0015(17) N3 0.026(2) 0.015(2) 0.020(3) -0.0017(18) -0.0027(19) 0.0110(18) N4 0.026(2) 0.018(2) 0.059(4) 0.021(2) 0.013(2) 0.010(2) N5 0.022(2) 0.018(2) 0.065(4) 0.024(2) 0.006(2) 0.009(2) O1 0.0227(19) 0.033(2) 0.019(2) 0.0110(16) 0.0057(16) 0.0093(16) O2 0.027(2) 0.049(3) 0.018(2) 0.0087(19) -0.0004(17) 0.0099(19) O3 0.046(3) 0.044(2) 0.040(3) 0.026(2) 0.012(2) 0.024(2) S1 0.0207(7) 0.0388(8) 0.0241(8) 0.0145(6) 0.0043(6) 0.0095(6) Si1 0.0197(7) 0.0170(7) 0.0264(9) 0.0087(6) 0.0018(6) 0.0046(6) Si2 0.0207(8) 0.0108(7) 0.0457(11) -0.0021(7) 0.0016(7) 0.0030(6) Zr 0.0202(3) 0.0122(2) 0.0218(3) 0.00709(19) 0.0049(2) 0.00721(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 C1 N1 1.481(6) . ? C1 C2 1.553(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.498(8) . ? C2 C4 1.543(7) . ? C2 C3 1.556(7) . ? C3 N2 1.477(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.355(7) . ? C5 C6 1.409(7) . ? C6 C7 1.362(9) . ? C6 H6 0.9500 . ? C7 C8 1.370(9) . ? C7 H7 0.9500 . ? C8 C9 1.401(8) . ? C8 H8 0.9500 . ? C9 N3 1.338(7) . ? C9 H9 0.9500 . ? C10 Si1 1.866(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.877(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.526(10) . ? C12 C14 1.532(11) . ? C12 C15 1.554(8) . ? C12 Si1 1.893(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si2 1.878(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.866(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.511(9) . ? C18 C21 1.540(10) . ? C18 C19 1.569(9) . ? C18 Si2 1.900(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 N5 1.358(7) . ? C22 C23 1.375(7) . ? C22 H22 0.9500 . ? C23 C24 1.358(8) . ? C23 H23 0.9500 . ? C24 C25 1.346(10) . ? C24 H24 0.9500 . ? C25 C26 1.384(9) . ? C25 H25 0.9500 . ? C26 N5 1.337(8) . ? C26 H26 0.9500 . ? C27 F3 1.315(7) . ? C27 F2 1.327(7) . ? C27 F1 1.329(7) . ? C27 S1 1.817(6) . ? N1 Si1 1.736(4) . ? N1 Zr 2.073(4) . ? N2 Si2 1.729(4) . ? N2 Zr 2.079(4) . ? N3 Zr 2.429(4) . ? N4 N5 1.347(6) . ? N4 Zr 1.928(4) . ? O1 S1 1.440(4) . ? O1 Zr 2.352(3) . ? O2 S1 1.452(4) . ? O2 Zr 2.379(4) 2_655 ? O3 S1 1.430(4) . ? Zr O2 2.379(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.0(4) . . ? N1 C1 H1A 107.8 . . ? C2 C1 H1A 107.8 . . ? N1 C1 H1B 107.8 . . ? C2 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? C5 C2 C4 111.2(5) . . ? C5 C2 C1 110.9(4) . . ? C4 C2 C1 106.2(4) . . ? C5 C2 C3 110.5(4) . . ? C4 C2 C3 105.2(5) . . ? C1 C2 C3 112.7(4) . . ? N2 C3 C2 117.7(4) . . ? N2 C3 H3A 107.9 . . ? C2 C3 H3A 107.9 . . ? N2 C3 H3B 107.9 . . ? C2 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 119.5(5) . . ? N3 C5 C2 116.7(4) . . ? C6 C5 C2 123.8(5) . . ? C7 C6 C5 120.2(6) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.2(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 117.8(6) . . ? C7 C8 H8 121.1 . . ? C9 C8 H8 121.1 . . ? N3 C9 C8 122.6(6) . . ? N3 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 108.4(7) . . ? C13 C12 C15 108.0(6) . . ? C14 C12 C15 108.6(6) . . ? C13 C12 Si1 112.9(5) . . ? C14 C12 Si1 109.6(5) . . ? C15 C12 Si1 109.2(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C21 109.5(6) . . ? C20 C18 C19 109.5(6) . . ? C21 C18 C19 107.2(6) . . ? C20 C18 Si2 110.2(4) . . ? C21 C18 Si2 112.2(4) . . ? C19 C18 Si2 108.0(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N5 C22 C23 120.3(5) . . ? N5 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 121.2(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 117.9(5) . . ? C25 C24 H24 121.1 . . ? C23 C24 H24 121.1 . . ? C24 C25 C26 120.9(6) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? N5 C26 C25 120.9(7) . . ? N5 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? F3 C27 F2 108.3(5) . . ? F3 C27 F1 108.4(5) . . ? F2 C27 F1 107.5(5) . . ? F3 C27 S1 112.0(4) . . ? F2 C27 S1 110.9(4) . . ? F1 C27 S1 109.5(4) . . ? C1 N1 Si1 112.6(3) . . ? C1 N1 Zr 116.5(3) . . ? Si1 N1 Zr 130.5(2) . . ? C3 N2 Si2 115.1(4) . . ? C3 N2 Zr 116.3(3) . . ? Si2 N2 Zr 128.6(2) . . ? C9 N3 C5 119.6(4) . . ? C9 N3 Zr 124.1(4) . . ? C5 N3 Zr 115.6(3) . . ? N5 N4 Zr 170.8(4) . . ? C26 N5 N4 120.6(5) . . ? C26 N5 C22 118.6(5) . . ? N4 N5 C22 120.8(4) . . ? S1 O1 Zr 151.2(2) . . ? S1 O2 Zr 155.3(3) . 2_655 ? O3 S1 O1 115.8(2) . . ? O3 S1 O2 115.9(3) . . ? O1 S1 O2 112.6(2) . . ? O3 S1 C27 103.7(3) . . ? O1 S1 C27 102.0(3) . . ? O2 S1 C27 104.6(3) . . ? N1 Si1 C10 111.1(2) . . ? N1 Si1 C11 109.5(2) . . ? C10 Si1 C11 107.3(3) . . ? N1 Si1 C12 113.5(2) . . ? C10 Si1 C12 108.1(3) . . ? C11 Si1 C12 107.2(3) . . ? N2 Si2 C17 109.4(3) . . ? N2 Si2 C16 109.4(2) . . ? C17 Si2 C16 109.1(3) . . ? N2 Si2 C18 113.7(3) . . ? C17 Si2 C18 107.6(3) . . ? C16 Si2 C18 107.5(3) . . ? N4 Zr N1 106.22(17) . . ? N4 Zr N2 106.09(19) . . ? N1 Zr N2 92.47(16) . . ? N4 Zr O1 92.15(16) . . ? N1 Zr O1 158.33(14) . . ? N2 Zr O1 93.36(14) . . ? N4 Zr O2 89.86(19) . 2_655 ? N1 Zr O2 91.44(15) . 2_655 ? N2 Zr O2 161.76(14) . 2_655 ? O1 Zr O2 76.92(13) . 2_655 ? N4 Zr N3 165.50(18) . . ? N1 Zr N3 85.83(15) . . ? N2 Zr N3 80.89(15) . . ? O1 Zr N3 74.54(14) . . ? O2 Zr N3 81.64(14) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C5 -78.4(6) . . . . ? N1 C1 C2 C4 160.7(5) . . . . ? N1 C1 C2 C3 46.0(6) . . . . ? C5 C2 C3 N2 56.4(6) . . . . ? C4 C2 C3 N2 176.5(4) . . . . ? C1 C2 C3 N2 -68.2(6) . . . . ? C4 C2 C5 N3 174.2(4) . . . . ? C1 C2 C5 N3 56.2(6) . . . . ? C3 C2 C5 N3 -69.4(6) . . . . ? C4 C2 C5 C6 -4.2(7) . . . . ? C1 C2 C5 C6 -122.1(5) . . . . ? C3 C2 C5 C6 112.2(5) . . . . ? N3 C5 C6 C7 1.1(8) . . . . ? C2 C5 C6 C7 179.4(5) . . . . ? C5 C6 C7 C8 0.0(8) . . . . ? C6 C7 C8 C9 -0.9(9) . . . . ? C7 C8 C9 N3 0.8(9) . . . . ? N5 C22 C23 C24 0.2(9) . . . . ? C22 C23 C24 C25 -0.7(10) . . . . ? C23 C24 C25 C26 2.5(14) . . . . ? C24 C25 C26 N5 -3.9(16) . . . . ? C2 C1 N1 Si1 -157.0(4) . . . . ? C2 C1 N1 Zr 16.6(6) . . . . ? C2 C3 N2 Si2 -159.9(4) . . . . ? C2 C3 N2 Zr 19.5(6) . . . . ? C8 C9 N3 C5 0.3(8) . . . . ? C8 C9 N3 Zr 170.4(4) . . . . ? C6 C5 N3 C9 -1.3(7) . . . . ? C2 C5 N3 C9 -179.7(5) . . . . ? C6 C5 N3 Zr -172.1(4) . . . . ? C2 C5 N3 Zr 9.5(5) . . . . ? C25 C26 N5 N4 -176.7(8) . . . . ? C25 C26 N5 C22 3.3(13) . . . . ? Zr N4 N5 C26 167(2) . . . . ? Zr N4 N5 C22 -13(3) . . . . ? C23 C22 N5 C26 -1.5(10) . . . . ? C23 C22 N5 N4 178.5(5) . . . . ? Zr O1 S1 O3 60.2(5) . . . . ? Zr O1 S1 O2 -76.3(5) . . . . ? Zr O1 S1 C27 172.0(5) . . . . ? Zr O2 S1 O3 -15.6(7) 2_655 . . . ? Zr O2 S1 O1 121.0(5) 2_655 . . . ? Zr O2 S1 C27 -129.0(6) 2_655 . . . ? F3 C27 S1 O3 -176.6(4) . . . . ? F2 C27 S1 O3 -55.4(5) . . . . ? F1 C27 S1 O3 63.1(5) . . . . ? F3 C27 S1 O1 62.9(5) . . . . ? F2 C27 S1 O1 -176.0(4) . . . . ? F1 C27 S1 O1 -57.5(5) . . . . ? F3 C27 S1 O2 -54.7(5) . . . . ? F2 C27 S1 O2 66.5(5) . . . . ? F1 C27 S1 O2 -175.0(4) . . . . ? C1 N1 Si1 C10 -160.4(4) . . . . ? Zr N1 Si1 C10 27.2(4) . . . . ? C1 N1 Si1 C11 -42.1(4) . . . . ? Zr N1 Si1 C11 145.5(3) . . . . ? C1 N1 Si1 C12 77.6(4) . . . . ? Zr N1 Si1 C12 -94.8(4) . . . . ? C13 C12 Si1 N1 -52.2(6) . . . . ? C14 C12 Si1 N1 68.8(5) . . . . ? C15 C12 Si1 N1 -172.3(5) . . . . ? C13 C12 Si1 C10 -175.8(6) . . . . ? C14 C12 Si1 C10 -54.8(5) . . . . ? C15 C12 Si1 C10 64.0(6) . . . . ? C13 C12 Si1 C11 68.8(6) . . . . ? C14 C12 Si1 C11 -170.2(4) . . . . ? C15 C12 Si1 C11 -51.4(6) . . . . ? C3 N2 Si2 C17 -174.0(4) . . . . ? Zr N2 Si2 C17 6.6(4) . . . . ? C3 N2 Si2 C16 66.5(4) . . . . ? Zr N2 Si2 C16 -112.9(4) . . . . ? C3 N2 Si2 C18 -53.7(4) . . . . ? Zr N2 Si2 C18 126.9(3) . . . . ? C20 C18 Si2 N2 -46.8(6) . . . . ? C21 C18 Si2 N2 75.5(5) . . . . ? C19 C18 Si2 N2 -166.5(4) . . . . ? C20 C18 Si2 C17 74.5(5) . . . . ? C21 C18 Si2 C17 -163.2(5) . . . . ? C19 C18 Si2 C17 -45.1(5) . . . . ? C20 C18 Si2 C16 -168.1(5) . . . . ? C21 C18 Si2 C16 -45.7(6) . . . . ? C19 C18 Si2 C16 72.3(5) . . . . ? N5 N4 Zr N1 -159(3) . . . . ? N5 N4 Zr N2 104(3) . . . . ? N5 N4 Zr O1 10(3) . . . . ? N5 N4 Zr O2 -67(3) . . . 2_655 ? N5 N4 Zr N3 -13(3) . . . . ? C1 N1 Zr N4 -156.7(4) . . . . ? Si1 N1 Zr N4 15.4(3) . . . . ? C1 N1 Zr N2 -49.2(4) . . . . ? Si1 N1 Zr N2 123.0(3) . . . . ? C1 N1 Zr O1 56.3(6) . . . . ? Si1 N1 Zr O1 -131.5(3) . . . . ? C1 N1 Zr O2 113.0(4) . . . 2_655 ? Si1 N1 Zr O2 -74.8(3) . . . 2_655 ? C1 N1 Zr N3 31.5(3) . . . . ? Si1 N1 Zr N3 -156.4(3) . . . . ? C3 N2 Zr N4 138.0(3) . . . . ? Si2 N2 Zr N4 -42.6(3) . . . . ? C3 N2 Zr N1 30.4(3) . . . . ? Si2 N2 Zr N1 -150.3(3) . . . . ? C3 N2 Zr O1 -128.8(3) . . . . ? Si2 N2 Zr O1 50.6(3) . . . . ? C3 N2 Zr O2 -71.9(6) . . . 2_655 ? Si2 N2 Zr O2 107.5(4) . . . 2_655 ? C3 N2 Zr N3 -55.0(3) . . . . ? Si2 N2 Zr N3 124.3(3) . . . . ? S1 O1 Zr N4 -47.5(5) . . . . ? S1 O1 Zr N1 100.9(6) . . . . ? S1 O1 Zr N2 -153.7(5) . . . . ? S1 O1 Zr O2 41.9(5) . . . 2_655 ? S1 O1 Zr N3 126.7(5) . . . . ? C9 N3 Zr N4 -6.4(9) . . . . ? C5 N3 Zr N4 164.0(6) . . . . ? C9 N3 Zr N1 140.4(4) . . . . ? C5 N3 Zr N1 -49.2(3) . . . . ? C9 N3 Zr N2 -126.4(4) . . . . ? C5 N3 Zr N2 44.0(3) . . . . ? C9 N3 Zr O1 -30.3(4) . . . . ? C5 N3 Zr O1 140.1(4) . . . . ? C9 N3 Zr O2 48.3(4) . . . 2_655 ? C5 N3 Zr O2 -141.3(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.806 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.123 _audit_block_code ga_hh28 _audit_block_refno 640 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end==