Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lutz Gade' 'Heike Herrmann' 'Hubert Wadepohl' _publ_contact_author_name 'Lutz Gade' _publ_contact_author_address ; Anorganisch-Chemisches Institut University of Heidelberg Im Neuenheimer Feld 270 Heidelberg 69120 GERMANY ; _publ_contact_author_email LUTZ.GADE@UNI-HD.DE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; En Route to Zirconium Hydrazides(2-) ; data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 674839' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H41 Cl2 N3 Si2 Zr' _chemical_formula_weight 553.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.056(2) _cell_length_b 21.423(3) _cell_length_c 18.016(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.690(3) _cell_angle_gamma 90.00 _cell_volume 5810.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6838 _exptl_absorpt_correction_T_max 0.7464 _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 120143 _diffrn_reflns_av_R_equivalents 0.0903 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13856 _reflns_number_gt 9446 _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^)+(0.0646P)^2^+8.9328P] 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 13856 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.8827(3) 0.28615(19) 0.1641(2) 0.0269(8) Uani 1 1 d . . . H1A H 0.8195 0.2767 0.1534 0.032 Uiso 1 1 calc R . . H1B H 0.8860 0.3304 0.1797 0.032 Uiso 1 1 calc R . . C2 C 0.9132(2) 0.24501(18) 0.2310(2) 0.0223(7) Uani 1 1 d . . . C3 C 0.8889(3) 0.17478(18) 0.2200(2) 0.0242(8) Uani 1 1 d . . . H3A H 0.9026 0.1525 0.2669 0.029 Uiso 1 1 calc R . . H3B H 0.8240 0.1718 0.2114 0.029 Uiso 1 1 calc R . . C4 C 0.8562(3) 0.2669(2) 0.2961(2) 0.0291(9) Uani 1 1 d . . . H4A H 0.8687 0.2408 0.3396 0.044 Uiso 1 1 calc R . . H4B H 0.7932 0.2635 0.2824 0.044 Uiso 1 1 calc R . . H4C H 0.8704 0.3105 0.3077 0.044 Uiso 1 1 calc R . . C5 C 1.0114(2) 0.25290(16) 0.2460(2) 0.0211(7) Uani 1 1 d . . . C6 C 1.0453(3) 0.27782(18) 0.3107(2) 0.0268(8) Uani 1 1 d . . . H6 H 1.0057 0.2924 0.3476 0.032 Uiso 1 1 calc R . . C7 C 1.1352(3) 0.2821(2) 0.3231(2) 0.0348(10) Uani 1 1 d . . . H7 H 1.1582 0.2988 0.3681 0.042 Uiso 1 1 calc R . . C8 C 1.1912(3) 0.2613(2) 0.2681(2) 0.0367(10) Uani 1 1 d . . . H8 H 1.2538 0.2631 0.2748 0.044 Uiso 1 1 calc R . . C9 C 1.1545(3) 0.2380(2) 0.2032(2) 0.0301(9) Uani 1 1 d . . . H9 H 1.1931 0.2247 0.1651 0.036 Uiso 1 1 calc R . . C10 C 1.0244(3) 0.3276(2) -0.0333(3) 0.0410(11) Uani 1 1 d . . . H10A H 1.0789 0.3067 -0.0163 0.061 Uiso 1 1 calc R . . H10B H 1.0398 0.3655 -0.0607 0.061 Uiso 1 1 calc R . . H10C H 0.9906 0.2994 -0.0659 0.061 Uiso 1 1 calc R . . C11 C 1.0232(4) 0.3992(2) 0.1115(3) 0.0540(14) Uani 1 1 d . . . H11A H 0.9933 0.4029 0.1593 0.081 Uiso 1 1 calc R . . H11B H 1.0297 0.4407 0.0893 0.081 Uiso 1 1 calc R . . H11C H 1.0821 0.3806 0.1193 0.081 Uiso 1 1 calc R . . C12 C 0.8510(3) 0.3904(2) 0.0163(3) 0.0400(11) Uani 1 1 d . . . C13 C 0.8769(5) 0.4435(4) -0.0359(5) 0.119(4) Uani 1 1 d . . . H13A H 0.8261 0.4716 -0.0431 0.178 Uiso 1 1 calc R . . H13B H 0.8943 0.4262 -0.0839 0.178 Uiso 1 1 calc R . . H13C H 0.9268 0.4668 -0.0142 0.178 Uiso 1 1 calc R . . C14 C 0.8014(4) 0.4205(3) 0.0800(4) 0.0704(19) Uani 1 1 d . . . H14A H 0.7527 0.4461 0.0600 0.106 Uiso 1 1 calc R . . H14B H 0.8423 0.4468 0.1088 0.106 Uiso 1 1 calc R . . H14C H 0.7771 0.3879 0.1121 0.106 Uiso 1 1 calc R . . C15 C 0.7891(5) 0.3448(4) -0.0208(5) 0.099(3) Uani 1 1 d . . . H15A H 0.7755 0.3109 0.0138 0.148 Uiso 1 1 calc R . . H15B H 0.8174 0.3276 -0.0650 0.148 Uiso 1 1 calc R . . H15C H 0.7341 0.3662 -0.0353 0.148 Uiso 1 1 calc R . . C16 C 1.0045(3) 0.0453(2) 0.2602(2) 0.0424(11) Uani 1 1 d . . . H16A H 1.0489 0.0776 0.2708 0.064 Uiso 1 1 calc R . . H16B H 1.0337 0.0044 0.2587 0.064 Uiso 1 1 calc R . . H16C H 0.9597 0.0453 0.2992 0.064 Uiso 1 1 calc R . . C17 C 1.0275(3) 0.0377(2) 0.0939(2) 0.0356(10) Uani 1 1 d . . . H17A H 1.0009 0.0474 0.0454 0.053 Uiso 1 1 calc R . . H17B H 1.0389 -0.0072 0.0973 0.053 Uiso 1 1 calc R . . H17C H 1.0835 0.0606 0.0999 0.053 Uiso 1 1 calc R . . C18 C 0.8419(3) 0.0163(2) 0.1595(3) 0.0423(11) Uani 1 1 d . . . C19 C 0.7990(4) 0.0288(3) 0.0851(4) 0.083(2) Uani 1 1 d . . . H19A H 0.7487 0.0004 0.0776 0.124 Uiso 1 1 calc R . . H19B H 0.8425 0.0223 0.0458 0.124 Uiso 1 1 calc R . . H19C H 0.7778 0.0721 0.0833 0.124 Uiso 1 1 calc R . . C20 C 0.7782(4) 0.0315(3) 0.2205(4) 0.076(2) Uani 1 1 d . . . H20A H 0.7558 0.0741 0.2138 0.114 Uiso 1 1 calc R . . H20B H 0.8090 0.0284 0.2686 0.114 Uiso 1 1 calc R . . H20C H 0.7285 0.0021 0.2190 0.114 Uiso 1 1 calc R . . C21 C 0.8618(4) -0.0534(2) 0.1651(4) 0.0636(16) Uani 1 1 d . . . H21A H 0.8063 -0.0770 0.1608 0.095 Uiso 1 1 calc R . . H21B H 0.8903 -0.0623 0.2132 0.095 Uiso 1 1 calc R . . H21C H 0.9017 -0.0656 0.1250 0.095 Uiso 1 1 calc R . . C51 C 0.3924(2) 0.12210(17) 0.0355(2) 0.0227(7) Uani 1 1 d . . . H51A H 0.3274 0.1211 0.0434 0.027 Uiso 1 1 calc R . . H51B H 0.4094 0.0810 0.0149 0.027 Uiso 1 1 calc R . . C52 C 0.4119(2) 0.17272(17) -0.0241(2) 0.0220(7) Uani 1 1 d . . . C53 C 0.3806(3) 0.23909(18) -0.0008(3) 0.0326(9) Uani 1 1 d . . . H53A H 0.3810 0.2662 -0.0453 0.039 Uiso 1 1 calc R . . H53B H 0.3183 0.2361 0.0158 0.039 Uiso 1 1 calc R . . C54 C 0.3541(2) 0.15468(19) -0.0906(2) 0.0282(8) Uani 1 1 d . . . H54A H 0.3627 0.1849 -0.1307 0.042 Uiso 1 1 calc R . . H54B H 0.2916 0.1546 -0.0761 0.042 Uiso 1 1 calc R . . H54C H 0.3707 0.1129 -0.1077 0.042 Uiso 1 1 calc R . . C55 C 0.5097(2) 0.17509(17) -0.0431(2) 0.0244(8) Uani 1 1 d . . . C56 C 0.5402(3) 0.1699(2) -0.1152(2) 0.0326(9) Uani 1 1 d . . . H56 H 0.4996 0.1637 -0.1553 0.039 Uiso 1 1 calc R . . C57 C 0.6302(3) 0.1738(2) -0.1279(3) 0.0415(11) Uani 1 1 d . . . H57 H 0.6519 0.1714 -0.1771 0.050 Uiso 1 1 calc R . . C58 C 0.6883(3) 0.1812(2) -0.0695(3) 0.0403(11) Uani 1 1 d . . . H58 H 0.7506 0.1825 -0.0774 0.048 Uiso 1 1 calc R . . C59 C 0.6548(3) 0.1867(2) 0.0007(3) 0.0353(10) Uani 1 1 d . . . H59 H 0.6951 0.1914 0.0412 0.042 Uiso 1 1 calc R . . C60 C 0.5171(4) 0.0824(3) 0.2462(3) 0.0659(17) Uani 1 1 d . . . H60A H 0.5736 0.0997 0.2290 0.099 Uiso 1 1 calc R . . H60B H 0.5286 0.0447 0.2756 0.099 Uiso 1 1 calc R . . H60C H 0.4869 0.1134 0.2769 0.099 Uiso 1 1 calc R . . C61 C 0.5032(3) -0.0005(2) 0.1126(3) 0.0472(12) Uani 1 1 d . . . H61A H 0.4683 -0.0115 0.0681 0.071 Uiso 1 1 calc R . . H61B H 0.5096 -0.0374 0.1444 0.071 Uiso 1 1 calc R . . H61C H 0.5620 0.0142 0.0979 0.071 Uiso 1 1 calc R . . C62 C 0.3330(4) 0.0344(3) 0.1952(3) 0.0552(15) Uani 1 1 d . . . C63 C 0.2806(5) 0.0897(3) 0.2230(5) 0.095(3) Uani 1 1 d . . . H63A H 0.2764 0.1214 0.1839 0.142 Uiso 1 1 calc R . . H63B H 0.3106 0.1075 0.2667 0.142 Uiso 1 1 calc R . . H63C H 0.2207 0.0761 0.2365 0.142 Uiso 1 1 calc R . . C64 C 0.2818(4) 0.0023(3) 0.1319(4) 0.075(2) Uani 1 1 d . . . H64A H 0.2269 -0.0158 0.1511 0.113 Uiso 1 1 calc R . . H64B H 0.3186 -0.0308 0.1107 0.113 Uiso 1 1 calc R . . H64C H 0.2672 0.0331 0.0933 0.113 Uiso 1 1 calc R . . C65 C 0.3463(5) -0.0133(4) 0.2582(4) 0.086(2) Uani 1 1 d . . . H65A H 0.3772 0.0067 0.3001 0.129 Uiso 1 1 calc R . . H65B H 0.3818 -0.0484 0.2403 0.129 Uiso 1 1 calc R . . H65C H 0.2883 -0.0285 0.2745 0.129 Uiso 1 1 calc R . . C66 C 0.5007(5) 0.3651(3) -0.0450(4) 0.0710(18) Uani 1 1 d . . . H66A H 0.5529 0.3388 -0.0532 0.107 Uiso 1 1 calc R . . H66B H 0.5177 0.4092 -0.0484 0.107 Uiso 1 1 calc R . . H66C H 0.4552 0.3558 -0.0827 0.107 Uiso 1 1 calc R . . C67 C 0.5421(4) 0.3679(3) 0.1183(4) 0.076(2) Uani 1 1 d . . . H67A H 0.5211 0.3568 0.1679 0.115 Uiso 1 1 calc R . . H67B H 0.5552 0.4127 0.1166 0.115 Uiso 1 1 calc R . . H67C H 0.5961 0.3442 0.1075 0.115 Uiso 1 1 calc R . . C68 C 0.3526(4) 0.3986(3) 0.0648(5) 0.077(2) Uani 1 1 d . . . C69 C 0.2824(4) 0.3864(3) 0.0059(7) 0.127(4) Uani 1 1 d . . . H69A H 0.2559 0.3452 0.0141 0.190 Uiso 1 1 calc R . . H69B H 0.3096 0.3875 -0.0432 0.190 Uiso 1 1 calc R . . H69C H 0.2362 0.4185 0.0087 0.190 Uiso 1 1 calc R . . C70 C 0.3176(7) 0.3841(4) 0.1407(7) 0.159(6) Uani 1 1 d . . . H70A H 0.2671 0.4115 0.1512 0.239 Uiso 1 1 calc R . . H70B H 0.3646 0.3911 0.1780 0.239 Uiso 1 1 calc R . . H70C H 0.2983 0.3405 0.1425 0.239 Uiso 1 1 calc R . . C71 C 0.3805(5) 0.4681(3) 0.0611(5) 0.099(3) Uani 1 1 d . . . H71A H 0.3298 0.4945 0.0740 0.149 Uiso 1 1 calc R . . H71B H 0.3997 0.4781 0.0107 0.149 Uiso 1 1 calc R . . H71C H 0.4295 0.4757 0.0962 0.149 Uiso 1 1 calc R . . Cl1 Cl 1.14274(6) 0.18170(5) 0.03331(6) 0.0329(2) Uani 1 1 d . . . Cl2 Cl 0.92477(7) 0.15607(5) -0.03137(5) 0.0294(2) Uani 1 1 d . . . Cl51 Cl 0.64789(8) 0.22067(8) 0.17896(8) 0.0586(4) Uani 1 1 d . . . Cl52 Cl 0.43177(8) 0.24236(7) 0.24609(8) 0.0581(4) Uani 1 1 d . . . N1 N 0.9326(2) 0.27933(15) 0.09431(17) 0.0236(7) Uani 1 1 d . . . N2 N 0.9336(2) 0.14194(14) 0.15927(17) 0.0223(6) Uani 1 1 d . . . N3 N 1.0664(2) 0.23319(14) 0.19172(17) 0.0224(6) Uani 1 1 d . . . N51 N 0.4365(2) 0.12909(16) 0.10861(17) 0.0257(7) Uani 1 1 d . . . N52 N 0.4331(2) 0.26984(16) 0.0582(2) 0.0347(8) Uani 1 1 d . . . N53 N 0.5668(2) 0.18555(15) 0.01455(19) 0.0270(7) Uani 1 1 d . . . Si1 Si 0.95600(8) 0.34849(5) 0.04806(6) 0.0269(2) Uani 1 1 d . . . Si2 Si 0.94981(7) 0.06133(5) 0.16847(6) 0.0257(2) Uani 1 1 d . . . Si51 Si 0.44522(8) 0.06237(6) 0.16433(6) 0.0333(3) Uani 1 1 d . . . Si52 Si 0.45559(9) 0.34912(6) 0.04885(9) 0.0461(4) Uani 1 1 d . . . Zr1 Zr 0.99290(2) 0.196048(16) 0.083741(19) 0.01944(9) Uani 1 1 d . . . Zr51 Zr 0.49682(2) 0.21103(2) 0.12758(2) 0.03096(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 0.0245(19) 0.031(2) 0.025(2) 0.0008(16) 0.0045(15) 0.0059(16) C2 0.0204(18) 0.0283(19) 0.0183(17) -0.0017(14) 0.0017(14) -0.0006(15) C3 0.0251(19) 0.0294(19) 0.0183(18) -0.0004(15) 0.0033(14) -0.0049(15) C4 0.0231(19) 0.038(2) 0.026(2) -0.0075(17) 0.0075(16) -0.0006(17) C5 0.0226(18) 0.0192(17) 0.0216(18) 0.0004(14) 0.0033(14) 0.0014(14) C6 0.027(2) 0.031(2) 0.0227(19) -0.0062(16) 0.0014(15) -0.0039(16) C7 0.030(2) 0.046(3) 0.028(2) -0.0088(18) -0.0037(17) -0.0061(19) C8 0.021(2) 0.052(3) 0.037(2) -0.008(2) -0.0013(17) -0.0023(19) C9 0.0180(18) 0.041(2) 0.032(2) -0.0050(18) 0.0032(16) 0.0009(16) C10 0.045(3) 0.036(2) 0.042(3) 0.006(2) 0.021(2) 0.002(2) C11 0.057(3) 0.039(3) 0.065(4) -0.014(2) 0.007(3) -0.020(2) C12 0.045(3) 0.033(2) 0.041(3) 0.008(2) 0.008(2) 0.012(2) C13 0.105(6) 0.114(6) 0.139(7) 0.098(6) 0.070(6) 0.062(5) C14 0.063(4) 0.074(4) 0.075(4) 0.018(3) 0.023(3) 0.037(3) C15 0.070(5) 0.107(6) 0.118(7) -0.037(5) -0.051(5) 0.033(4) C16 0.050(3) 0.042(3) 0.035(3) 0.011(2) 0.001(2) 0.005(2) C17 0.038(2) 0.031(2) 0.037(2) -0.0005(18) 0.0051(19) 0.0055(18) C18 0.037(3) 0.031(2) 0.059(3) 0.006(2) -0.002(2) -0.0089(19) C19 0.060(4) 0.093(5) 0.095(5) 0.026(4) -0.036(4) -0.039(4) C20 0.046(3) 0.060(4) 0.122(6) -0.018(4) 0.035(4) -0.023(3) C21 0.064(4) 0.031(3) 0.095(5) -0.006(3) -0.004(3) -0.018(3) C51 0.0180(17) 0.0273(19) 0.0229(18) -0.0009(15) 0.0014(14) -0.0012(14) C52 0.0163(17) 0.0188(17) 0.031(2) 0.0039(15) -0.0029(15) -0.0014(14) C53 0.0204(19) 0.0222(19) 0.055(3) -0.0039(18) -0.0077(18) 0.0027(15) C54 0.0173(18) 0.034(2) 0.033(2) 0.0071(17) -0.0032(15) -0.0012(16) C55 0.0207(18) 0.0177(17) 0.035(2) 0.0050(15) -0.0001(15) 0.0027(14) C56 0.028(2) 0.037(2) 0.032(2) 0.0077(18) 0.0012(17) -0.0022(18) C57 0.033(2) 0.053(3) 0.039(3) 0.009(2) 0.011(2) -0.002(2) C58 0.020(2) 0.056(3) 0.046(3) 0.008(2) 0.0072(19) 0.0016(19) C59 0.0146(18) 0.045(3) 0.047(3) 0.005(2) 0.0001(17) -0.0010(17) C60 0.079(4) 0.086(4) 0.032(3) 0.006(3) -0.016(3) 0.027(4) C61 0.048(3) 0.041(3) 0.052(3) 0.006(2) 0.006(2) 0.017(2) C62 0.048(3) 0.059(3) 0.059(3) 0.033(3) 0.022(3) 0.015(3) C63 0.069(4) 0.090(5) 0.127(7) 0.037(5) 0.066(5) 0.036(4) C64 0.038(3) 0.080(4) 0.108(6) 0.049(4) -0.004(3) -0.012(3) C65 0.074(5) 0.106(6) 0.077(5) 0.063(4) 0.021(4) 0.019(4) C66 0.074(4) 0.047(3) 0.093(5) 0.006(3) 0.020(4) -0.024(3) C67 0.055(4) 0.063(4) 0.111(6) -0.031(4) -0.002(4) -0.027(3) C68 0.054(4) 0.030(3) 0.146(7) -0.008(3) 0.019(4) 0.003(3) C69 0.041(4) 0.059(4) 0.279(13) -0.041(6) -0.029(6) 0.020(3) C70 0.139(9) 0.098(7) 0.244(14) 0.014(8) 0.133(10) 0.055(6) C71 0.080(5) 0.030(3) 0.189(9) -0.021(4) -0.012(5) 0.008(3) Cl1 0.0219(5) 0.0475(6) 0.0293(5) -0.0048(4) 0.0074(4) 0.0038(4) Cl2 0.0305(5) 0.0376(5) 0.0200(4) -0.0009(4) -0.0026(4) -0.0031(4) Cl51 0.0234(5) 0.0979(11) 0.0543(8) -0.0280(7) -0.0112(5) -0.0013(6) Cl52 0.0355(6) 0.0861(10) 0.0527(8) -0.0424(7) 0.0029(5) 0.0008(6) N1 0.0252(16) 0.0254(16) 0.0202(15) 0.0010(12) 0.0038(13) 0.0030(13) N2 0.0205(15) 0.0262(16) 0.0203(15) 0.0001(12) 0.0016(12) -0.0022(12) N3 0.0170(15) 0.0255(16) 0.0248(16) -0.0036(13) 0.0020(12) 0.0001(12) N51 0.0171(15) 0.0376(19) 0.0225(16) -0.0013(14) -0.0005(12) 0.0029(13) N52 0.0193(16) 0.0258(17) 0.059(2) -0.0122(16) -0.0027(16) 0.0001(13) N53 0.0149(15) 0.0286(17) 0.0374(19) -0.0015(14) -0.0039(13) -0.0010(13) Si1 0.0300(6) 0.0207(5) 0.0302(6) -0.0017(4) 0.0090(5) -0.0025(4) Si2 0.0264(5) 0.0251(5) 0.0255(5) 0.0022(4) -0.0005(4) -0.0014(4) Si51 0.0296(6) 0.0431(7) 0.0272(6) 0.0064(5) 0.0014(5) 0.0131(5) Si52 0.0288(7) 0.0271(6) 0.0827(11) -0.0113(6) 0.0072(7) -0.0074(5) Zr1 0.01739(17) 0.02315(18) 0.01783(17) -0.00017(13) 0.00251(13) 0.00078(13) Zr51 0.01705(19) 0.0384(2) 0.0374(2) -0.01463(18) -0.00273(16) 0.00116(16) _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(5) . ? C1 C2 1.557(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.509(5) . ? C2 C4 1.535(5) . ? C2 C3 1.561(5) . ? C3 N2 1.470(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.357(5) . ? C5 C6 1.374(5) . ? C6 C7 1.371(6) . ? C6 H6 0.9500 . ? C7 C8 1.382(6) . ? C7 H7 0.9500 . ? C8 C9 1.381(6) . ? C8 H8 0.9500 . ? C9 N3 1.343(5) . ? C9 H9 0.9500 . ? C10 Si1 1.857(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.867(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.500(8) . ? C12 C14 1.520(7) . ? C12 C13 1.531(7) . ? C12 Si1 1.900(5) . ? 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 1.870(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.861(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.504(8) . ? C18 C19 1.506(8) . ? C18 C21 1.526(7) . ? C18 Si2 1.894(5) . ? 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 . ? C51 N51 1.475(5) . ? C51 C52 1.557(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C55 1.517(5) . ? C52 C54 1.521(5) . ? C52 C53 1.557(5) . ? C53 N52 1.474(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N53 1.358(5) . ? C55 C56 1.388(6) . ? C56 C57 1.379(6) . ? C56 H56 0.9500 . ? C57 C58 1.370(7) . ? C57 H57 0.9500 . ? C58 C59 1.372(6) . ? C58 H58 0.9500 . ? C59 N53 1.351(5) . ? C59 H59 0.9500 . ? C60 Si51 1.869(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 Si51 1.862(5) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.513(8) . ? C62 C64 1.532(9) . ? C62 C65 1.538(7) . ? C62 Si51 1.883(5) . ? 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 1.861(6) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 Si52 1.840(6) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C70 1.505(12) . ? C68 C69 1.511(11) . ? C68 C71 1.549(8) . ? C68 Si52 1.903(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 . ? Cl1 Zr1 2.4614(10) . ? Cl2 Zr1 2.4567(10) . ? Cl51 Zr51 2.4539(12) . ? Cl52 Zr51 2.4533(13) . ? N1 Si1 1.738(3) . ? N1 Zr1 2.012(3) . ? N2 Si2 1.752(3) . ? N2 Zr1 2.006(3) . ? N3 Zr1 2.364(3) . ? N51 Si51 1.751(4) . ? N51 Zr51 2.004(3) . ? N52 Si52 1.740(4) . ? N52 Zr51 2.010(4) . ? N53 Zr51 2.368(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 116.9(3) . . ? N1 C1 H1A 108.1 . . ? C2 C1 H1A 108.1 . . ? N1 C1 H1B 108.1 . . ? C2 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C5 C2 C4 112.6(3) . . ? C5 C2 C1 110.8(3) . . ? C4 C2 C1 104.8(3) . . ? C5 C2 C3 111.0(3) . . ? C4 C2 C3 105.0(3) . . ? C1 C2 C3 112.4(3) . . ? N2 C3 C2 116.5(3) . . ? N2 C3 H3A 108.2 . . ? C2 C3 H3A 108.2 . . ? N2 C3 H3B 108.2 . . ? C2 C3 H3B 108.2 . . ? 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 120.6(3) . . ? N3 C5 C2 116.1(3) . . ? C6 C5 C2 123.3(3) . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 118.2(4) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? N3 C9 C8 122.9(4) . . ? 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 C14 107.7(5) . . ? C15 C12 C13 111.8(6) . . ? C14 C12 C13 106.2(5) . . ? C15 C12 Si1 109.7(4) . . ? C14 C12 Si1 112.9(4) . . ? C13 C12 Si1 108.6(4) . . ? 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 110.0(5) . . ? C20 C18 C21 106.8(5) . . ? C19 C18 C21 108.4(5) . . ? C20 C18 Si2 112.4(4) . . ? C19 C18 Si2 110.1(4) . . ? C21 C18 Si2 109.0(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 . . ? N51 C51 C52 117.3(3) . . ? N51 C51 H51A 108.0 . . ? C52 C51 H51A 108.0 . . ? N51 C51 H51B 108.0 . . ? C52 C51 H51B 108.0 . . ? H51A C51 H51B 107.2 . . ? C55 C52 C54 112.3(3) . . ? C55 C52 C53 109.2(3) . . ? C54 C52 C53 105.8(3) . . ? C55 C52 C51 111.7(3) . . ? C54 C52 C51 104.8(3) . . ? C53 C52 C51 112.9(3) . . ? N52 C53 C52 116.2(3) . . ? N52 C53 H53A 108.2 . . ? C52 C53 H53A 108.2 . . ? N52 C53 H53B 108.2 . . ? C52 C53 H53B 108.2 . . ? H53A C53 H53B 107.4 . . ? 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 121.0(4) . . ? N53 C55 C52 116.2(3) . . ? C56 C55 C52 122.7(4) . . ? C57 C56 C55 119.1(4) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C58 C57 C56 120.0(4) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 118.6(4) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? N53 C59 C58 122.8(4) . . ? N53 C59 H59 118.6 . . ? C58 C59 H59 118.6 . . ? 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 . . ? C63 C62 C64 109.8(6) . . ? C63 C62 C65 109.8(5) . . ? C64 C62 C65 108.2(5) . . ? C63 C62 Si51 108.8(4) . . ? C64 C62 Si51 111.6(4) . . ? C65 C62 Si51 108.7(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 . . ? C70 C68 C69 110.7(8) . . ? C70 C68 C71 109.6(7) . . ? C69 C68 C71 108.9(7) . . ? C70 C68 Si52 108.5(5) . . ? C69 C68 Si52 111.2(5) . . ? C71 C68 Si52 107.9(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 . . ? C1 N1 Si1 115.5(2) . . ? C1 N1 Zr1 113.7(2) . . ? Si1 N1 Zr1 128.05(17) . . ? C3 N2 Si2 117.8(2) . . ? C3 N2 Zr1 116.1(2) . . ? Si2 N2 Zr1 124.82(17) . . ? C9 N3 C5 118.3(3) . . ? C9 N3 Zr1 127.1(3) . . ? C5 N3 Zr1 114.5(2) . . ? C51 N51 Si51 117.3(3) . . ? C51 N51 Zr51 116.1(2) . . ? Si51 N51 Zr51 125.92(18) . . ? C53 N52 Si52 118.0(3) . . ? C53 N52 Zr51 114.6(3) . . ? Si52 N52 Zr51 125.47(19) . . ? C59 N53 C55 118.3(4) . . ? C59 N53 Zr51 127.1(3) . . ? C55 N53 Zr51 114.3(2) . . ? N1 Si1 C10 106.88(18) . . ? N1 Si1 C11 108.3(2) . . ? C10 Si1 C11 108.8(2) . . ? N1 Si1 C12 111.96(19) . . ? C10 Si1 C12 110.1(2) . . ? C11 Si1 C12 110.7(2) . . ? N2 Si2 C17 106.72(18) . . ? N2 Si2 C16 108.95(19) . . ? C17 Si2 C16 108.3(2) . . ? N2 Si2 C18 112.03(18) . . ? C17 Si2 C18 110.2(2) . . ? C16 Si2 C18 110.5(2) . . ? N51 Si51 C61 109.6(2) . . ? N51 Si51 C60 107.7(2) . . ? C61 Si51 C60 106.9(3) . . ? N51 Si51 C62 111.60(19) . . ? C61 Si51 C62 110.2(3) . . ? C60 Si51 C62 110.7(3) . . ? N52 Si52 C67 106.5(3) . . ? N52 Si52 C66 110.0(2) . . ? C67 Si52 C66 108.3(3) . . ? N52 Si52 C68 111.7(2) . . ? C67 Si52 C68 110.3(3) . . ? C66 Si52 C68 110.0(3) . . ? N2 Zr1 N1 104.07(12) . . ? N2 Zr1 N3 81.04(12) . . ? N1 Zr1 N3 80.27(12) . . ? N2 Zr1 Cl2 100.74(9) . . ? N1 Zr1 Cl2 101.81(9) . . ? N3 Zr1 Cl2 176.77(8) . . ? N2 Zr1 Cl1 126.58(9) . . ? N1 Zr1 Cl1 124.21(9) . . ? N3 Zr1 Cl1 85.62(8) . . ? Cl2 Zr1 Cl1 91.15(4) . . ? N51 Zr51 N52 103.37(13) . . ? N51 Zr51 N53 81.77(12) . . ? N52 Zr51 N53 79.87(13) . . ? N51 Zr51 Cl52 101.72(10) . . ? N52 Zr51 Cl52 100.18(11) . . ? N53 Zr51 Cl52 176.35(8) . . ? N51 Zr51 Cl51 123.65(10) . . ? N52 Zr51 Cl51 127.96(11) . . ? N53 Zr51 Cl51 85.63(8) . . ? Cl52 Zr51 Cl51 91.52(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 52.9(4) . . . . ? N1 C1 C2 C4 174.5(3) . . . . ? N1 C1 C2 C3 -72.0(4) . . . . ? C5 C2 C3 N2 -59.1(4) . . . . ? C4 C2 C3 N2 178.9(3) . . . . ? C1 C2 C3 N2 65.6(4) . . . . ? C4 C2 C5 N3 178.5(3) . . . . ? C1 C2 C5 N3 -64.5(4) . . . . ? C3 C2 C5 N3 61.1(4) . . . . ? C4 C2 C5 C6 -0.8(5) . . . . ? C1 C2 C5 C6 116.1(4) . . . . ? C3 C2 C5 C6 -118.2(4) . . . . ? N3 C5 C6 C7 -1.6(6) . . . . ? C2 C5 C6 C7 177.7(4) . . . . ? C5 C6 C7 C8 0.9(7) . . . . ? C6 C7 C8 C9 0.7(7) . . . . ? C7 C8 C9 N3 -1.5(7) . . . . ? N51 C51 C52 C55 61.0(4) . . . . ? N51 C51 C52 C54 -177.2(3) . . . . ? N51 C51 C52 C53 -62.6(4) . . . . ? C55 C52 C53 N52 -52.9(5) . . . . ? C54 C52 C53 N52 -173.9(4) . . . . ? C51 C52 C53 N52 72.1(4) . . . . ? C54 C52 C55 N53 -174.5(3) . . . . ? C53 C52 C55 N53 68.5(4) . . . . ? C51 C52 C55 N53 -57.1(4) . . . . ? C54 C52 C55 C56 8.4(5) . . . . ? C53 C52 C55 C56 -108.6(4) . . . . ? C51 C52 C55 C56 125.8(4) . . . . ? N53 C55 C56 C57 1.7(6) . . . . ? C52 C55 C56 C57 178.6(4) . . . . ? C55 C56 C57 C58 1.6(7) . . . . ? C56 C57 C58 C59 -2.2(7) . . . . ? C57 C58 C59 N53 -0.6(7) . . . . ? C2 C1 N1 Si1 -138.0(3) . . . . ? C2 C1 N1 Zr1 24.9(4) . . . . ? C2 C3 N2 Si2 151.9(3) . . . . ? C2 C3 N2 Zr1 -15.7(4) . . . . ? C8 C9 N3 C5 0.8(6) . . . . ? C8 C9 N3 Zr1 178.9(3) . . . . ? C6 C5 N3 C9 0.8(5) . . . . ? C2 C5 N3 C9 -178.6(3) . . . . ? C6 C5 N3 Zr1 -177.5(3) . . . . ? C2 C5 N3 Zr1 3.1(4) . . . . ? C52 C51 N51 Si51 -159.7(3) . . . . ? C52 C51 N51 Zr51 11.3(4) . . . . ? C52 C53 N52 Si52 139.0(3) . . . . ? C52 C53 N52 Zr51 -26.1(5) . . . . ? C58 C59 N53 C55 3.8(6) . . . . ? C58 C59 N53 Zr51 -168.9(3) . . . . ? C56 C55 N53 C59 -4.3(6) . . . . ? C52 C55 N53 C59 178.5(3) . . . . ? C56 C55 N53 Zr51 169.3(3) . . . . ? C52 C55 N53 Zr51 -7.9(4) . . . . ? C1 N1 Si1 C10 176.5(3) . . . . ? Zr1 N1 Si1 C10 16.4(3) . . . . ? C1 N1 Si1 C11 59.4(3) . . . . ? Zr1 N1 Si1 C11 -100.7(3) . . . . ? C1 N1 Si1 C12 -62.9(3) . . . . ? Zr1 N1 Si1 C12 137.1(2) . . . . ? C15 C12 Si1 N1 -47.0(5) . . . . ? C14 C12 Si1 N1 73.0(4) . . . . ? C13 C12 Si1 N1 -169.5(5) . . . . ? C15 C12 Si1 C10 71.7(5) . . . . ? C14 C12 Si1 C10 -168.2(4) . . . . ? C13 C12 Si1 C10 -50.7(5) . . . . ? C15 C12 Si1 C11 -168.0(5) . . . . ? C14 C12 Si1 C11 -47.9(5) . . . . ? C13 C12 Si1 C11 69.6(5) . . . . ? C3 N2 Si2 C17 -168.3(3) . . . . ? Zr1 N2 Si2 C17 -1.9(3) . . . . ? C3 N2 Si2 C16 -51.5(3) . . . . ? Zr1 N2 Si2 C16 114.8(2) . . . . ? C3 N2 Si2 C18 71.0(3) . . . . ? Zr1 N2 Si2 C18 -122.6(2) . . . . ? C20 C18 Si2 N2 -63.9(5) . . . . ? C19 C18 Si2 N2 59.1(5) . . . . ? C21 C18 Si2 N2 177.9(4) . . . . ? C20 C18 Si2 C17 177.4(4) . . . . ? C19 C18 Si2 C17 -59.6(5) . . . . ? C21 C18 Si2 C17 59.2(4) . . . . ? C20 C18 Si2 C16 57.8(5) . . . . ? C19 C18 Si2 C16 -179.2(4) . . . . ? C21 C18 Si2 C16 -60.4(4) . . . . ? C51 N51 Si51 C61 56.2(3) . . . . ? Zr51 N51 Si51 C61 -113.8(3) . . . . ? C51 N51 Si51 C60 172.1(3) . . . . ? Zr51 N51 Si51 C60 2.1(3) . . . . ? C51 N51 Si51 C62 -66.2(3) . . . . ? Zr51 N51 Si51 C62 123.8(3) . . . . ? C63 C62 Si51 N51 -46.7(5) . . . . ? C64 C62 Si51 N51 74.6(4) . . . . ? C65 C62 Si51 N51 -166.2(4) . . . . ? C63 C62 Si51 C61 -168.7(5) . . . . ? C64 C62 Si51 C61 -47.5(4) . . . . ? C65 C62 Si51 C61 71.7(5) . . . . ? C63 C62 Si51 C60 73.2(5) . . . . ? C64 C62 Si51 C60 -165.5(4) . . . . ? C65 C62 Si51 C60 -46.3(6) . . . . ? C53 N52 Si52 C67 -167.0(4) . . . . ? Zr51 N52 Si52 C67 -3.7(4) . . . . ? C53 N52 Si52 C66 -49.8(4) . . . . ? Zr51 N52 Si52 C66 113.5(3) . . . . ? C53 N52 Si52 C68 72.5(4) . . . . ? Zr51 N52 Si52 C68 -124.2(3) . . . . ? C70 C68 Si52 N52 57.2(7) . . . . ? C69 C68 Si52 N52 -64.7(6) . . . . ? C71 C68 Si52 N52 175.9(5) . . . . ? C70 C68 Si52 C67 -61.0(7) . . . . ? C69 C68 Si52 C67 177.0(6) . . . . ? C71 C68 Si52 C67 57.7(7) . . . . ? C70 C68 Si52 C66 179.6(6) . . . . ? C69 C68 Si52 C66 57.6(6) . . . . ? C71 C68 Si52 C66 -61.8(7) . . . . ? C3 N2 Zr1 N1 -21.1(3) . . . . ? Si2 N2 Zr1 N1 172.31(19) . . . . ? C3 N2 Zr1 N3 56.4(3) . . . . ? Si2 N2 Zr1 N3 -110.2(2) . . . . ? C3 N2 Zr1 Cl2 -126.4(2) . . . . ? Si2 N2 Zr1 Cl2 67.1(2) . . . . ? C3 N2 Zr1 Cl1 134.1(2) . . . . ? Si2 N2 Zr1 Cl1 -32.5(2) . . . . ? C1 N1 Zr1 N2 16.4(3) . . . . ? Si1 N1 Zr1 N2 176.7(2) . . . . ? C1 N1 Zr1 N3 -61.7(3) . . . . ? Si1 N1 Zr1 N3 98.6(2) . . . . ? C1 N1 Zr1 Cl2 120.8(2) . . . . ? Si1 N1 Zr1 Cl2 -78.9(2) . . . . ? C1 N1 Zr1 Cl1 -139.6(2) . . . . ? Si1 N1 Zr1 Cl1 20.7(3) . . . . ? C9 N3 Zr1 N2 127.6(3) . . . . ? C5 N3 Zr1 N2 -54.2(3) . . . . ? C9 N3 Zr1 N1 -126.3(3) . . . . ? C5 N3 Zr1 N1 51.8(3) . . . . ? C9 N3 Zr1 Cl2 4.0(17) . . . . ? C5 N3 Zr1 Cl2 -178(24) . . . . ? C9 N3 Zr1 Cl1 -0.5(3) . . . . ? C5 N3 Zr1 Cl1 177.7(2) . . . . ? C51 N51 Zr51 N52 23.9(3) . . . . ? Si51 N51 Zr51 N52 -166.0(2) . . . . ? C51 N51 Zr51 N53 -53.6(2) . . . . ? Si51 N51 Zr51 N53 116.5(2) . . . . ? C51 N51 Zr51 Cl52 127.5(2) . . . . ? Si51 N51 Zr51 Cl52 -62.4(2) . . . . ? C51 N51 Zr51 Cl51 -132.7(2) . . . . ? Si51 N51 Zr51 Cl51 37.4(2) . . . . ? C53 N52 Zr51 N51 -16.2(3) . . . . ? Si52 N52 Zr51 N51 180.0(2) . . . . ? C53 N52 Zr51 N53 62.7(3) . . . . ? Si52 N52 Zr51 N53 -101.1(2) . . . . ? C53 N52 Zr51 Cl52 -121.0(3) . . . . ? Si52 N52 Zr51 Cl52 75.2(2) . . . . ? C53 N52 Zr51 Cl51 139.0(2) . . . . ? Si52 N52 Zr51 Cl51 -24.8(3) . . . . ? C59 N53 Zr51 N51 -130.5(4) . . . . ? C55 N53 Zr51 N51 56.5(3) . . . . ? C59 N53 Zr51 N52 124.2(4) . . . . ? C55 N53 Zr51 N52 -48.7(3) . . . . ? C59 N53 Zr51 Cl52 33.1(16) . . . . ? C55 N53 Zr51 Cl52 -139.8(13) . . . . ? C59 N53 Zr51 Cl51 -5.6(3) . . . . ? C55 N53 Zr51 Cl51 -178.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.560 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.105 _audit_block_code ga_hh11a _audit_block_refno 413 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 674840' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H48 Cl N5 Si2 Zr' _chemical_formula_weight 577.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.583(3) _cell_length_b 15.613(4) _cell_length_c 20.578(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.439(6) _cell_angle_gamma 90.00 _cell_volume 3073.5(14) _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 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.8923 _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 77762 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 32.10 _reflns_number_total 10414 _reflns_number_gt 7730 _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^)+(0.0446P)^2^+1.1419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10414 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.31678(19) 0.26159(12) 0.13441(10) 0.0231(4) Uani 1 1 d . . . H1A H 0.3703 0.2668 0.0949 0.028 Uiso 1 1 calc R . . H1B H 0.3815 0.2757 0.1722 0.028 Uiso 1 1 calc R . . C2 C 0.19771(19) 0.33136(11) 0.13021(10) 0.0226(4) Uani 1 1 d . . . C3 C 0.1196(2) 0.33637(12) 0.06097(10) 0.0260(4) Uani 1 1 d . . . H3A H 0.0694 0.3918 0.0577 0.031 Uiso 1 1 calc R . . H3B H 0.1910 0.3371 0.0281 0.031 Uiso 1 1 calc R . . C4 C 0.2748(2) 0.41703(13) 0.13875(13) 0.0355(5) Uani 1 1 d . . . H4A H 0.2069 0.4640 0.1369 0.053 Uiso 1 1 calc R . . H4B H 0.3391 0.4241 0.1038 0.053 Uiso 1 1 calc R . . H4C H 0.3279 0.4178 0.1810 0.053 Uiso 1 1 calc R . . C5 C 0.09512(19) 0.31735(12) 0.18169(10) 0.0217(4) Uani 1 1 d . . . C6 C 0.0720(2) 0.37550(14) 0.23146(11) 0.0317(5) Uani 1 1 d . . . H6 H 0.1242 0.4272 0.2346 0.038 Uiso 1 1 calc R . . C7 C -0.0260(2) 0.35838(15) 0.27610(11) 0.0351(5) Uani 1 1 d . . . H7 H -0.0412 0.3978 0.3101 0.042 Uiso 1 1 calc R . . C8 C -0.1017(2) 0.28325(14) 0.27074(10) 0.0299(4) Uani 1 1 d . . . H8 H -0.1715 0.2706 0.3002 0.036 Uiso 1 1 calc R . . C9 C -0.07337(19) 0.22675(12) 0.22123(9) 0.0220(4) Uani 1 1 d . . . H9 H -0.1240 0.1744 0.2180 0.026 Uiso 1 1 calc R . . C10 C 0.5666(2) 0.11805(15) 0.17351(12) 0.0330(5) Uani 1 1 d . . . H10A H 0.5795 0.1131 0.1268 0.050 Uiso 1 1 calc R . . H10B H 0.6221 0.0740 0.1971 0.050 Uiso 1 1 calc R . . H10C H 0.5972 0.1749 0.1888 0.050 Uiso 1 1 calc R . . C11 C 0.3252(3) -0.00861(14) 0.16638(15) 0.0440(6) Uani 1 1 d . . . H11A H 0.2231 -0.0122 0.1613 0.066 Uiso 1 1 calc R . . H11B H 0.3598 -0.0479 0.2008 0.066 Uiso 1 1 calc R . . H11C H 0.3651 -0.0245 0.1253 0.066 Uiso 1 1 calc R . . C12 C 0.3573(3) 0.11878(19) 0.27859(12) 0.0437(7) Uani 1 1 d . . . C13 C 0.2091(3) 0.0925(3) 0.29515(16) 0.1000(18) Uani 1 1 d . . . H13A H 0.1950 0.1069 0.3406 0.150 Uiso 1 1 calc R . . H13B H 0.1974 0.0306 0.2887 0.150 Uiso 1 1 calc R . . H13C H 0.1404 0.1231 0.2667 0.150 Uiso 1 1 calc R . . C14 C 0.3878(5) 0.2110(2) 0.29950(15) 0.0930(16) Uani 1 1 d . . . H14A H 0.3144 0.2487 0.2805 0.139 Uiso 1 1 calc R . . H14B H 0.4785 0.2286 0.2843 0.139 Uiso 1 1 calc R . . H14C H 0.3902 0.2149 0.3471 0.139 Uiso 1 1 calc R . . C15 C 0.4599(3) 0.05976(17) 0.31758(12) 0.0399(6) Uani 1 1 d . . . H15A H 0.5560 0.0769 0.3102 0.060 Uiso 1 1 calc R . . H15B H 0.4450 0.0004 0.3033 0.060 Uiso 1 1 calc R . . H15C H 0.4440 0.0644 0.3641 0.060 Uiso 1 1 calc R . . C16 C -0.0798(2) 0.34996(13) -0.08136(10) 0.0300(4) Uani 1 1 d . . . H16A H -0.0326 0.4038 -0.0691 0.045 Uiso 1 1 calc R . . H16B H -0.1646 0.3623 -0.1088 0.045 Uiso 1 1 calc R . . H16C H -0.0170 0.3140 -0.1055 0.045 Uiso 1 1 calc R . . C17 C -0.2145(2) 0.18748(14) -0.02768(12) 0.0348(5) Uani 1 1 d . . . H17A H -0.1465 0.1490 -0.0461 0.052 Uiso 1 1 calc R . . H17B H -0.2926 0.1973 -0.0598 0.052 Uiso 1 1 calc R . . H17C H -0.2497 0.1614 0.0115 0.052 Uiso 1 1 calc R . . C18 C -0.2606(2) 0.36341(13) 0.03438(10) 0.0243(4) Uani 1 1 d . . . C19 C -0.2920(3) 0.3298(2) 0.10120(13) 0.0508(8) Uani 1 1 d . . . H19A H -0.3665 0.3642 0.1188 0.076 Uiso 1 1 calc R . . H19B H -0.2076 0.3336 0.1304 0.076 Uiso 1 1 calc R . . H19C H -0.3221 0.2699 0.0975 0.076 Uiso 1 1 calc R . . C20 C -0.2087(3) 0.45539(17) 0.04234(18) 0.0634(10) Uani 1 1 d . . . H20A H -0.2833 0.4911 0.0585 0.095 Uiso 1 1 calc R . . H20B H -0.1823 0.4773 0.0002 0.095 Uiso 1 1 calc R . . H20C H -0.1273 0.4568 0.0735 0.095 Uiso 1 1 calc R . . C21 C -0.3949(3) 0.3665(2) -0.00852(15) 0.0629(9) Uani 1 1 d . . . H21A H -0.4328 0.3085 -0.0140 0.094 Uiso 1 1 calc R . . H21B H -0.3755 0.3902 -0.0512 0.094 Uiso 1 1 calc R . . H21C H -0.4631 0.4029 0.0119 0.094 Uiso 1 1 calc R . . C22 C 0.3630(2) 0.09718(17) -0.00045(12) 0.0375(5) Uani 1 1 d . . . H22A H 0.3844 0.0711 0.0423 0.056 Uiso 1 1 calc R . . H22B H 0.4282 0.1444 -0.0069 0.056 Uiso 1 1 calc R . . H22C H 0.3724 0.0540 -0.0345 0.056 Uiso 1 1 calc R . . C23 C 0.1855(3) 0.16796(14) -0.06810(11) 0.0338(5) Uani 1 1 d . . . H23A H 0.2018 0.1256 -0.1020 0.051 Uiso 1 1 calc R . . H23B H 0.2449 0.2181 -0.0740 0.051 Uiso 1 1 calc R . . H23C H 0.0871 0.1854 -0.0713 0.051 Uiso 1 1 calc R . . Cl1 Cl -0.08122(5) 0.05340(3) 0.12982(2) 0.02137(9) Uani 1 1 d . . . H1 H 0.110(3) 0.0273(18) -0.0101(13) 0.037(7) Uiso 1 1 d . . . N1 N 0.27473(15) 0.17168(9) 0.14056(8) 0.0183(3) Uani 1 1 d . . . N2 N 0.01884(16) 0.26811(9) 0.04306(8) 0.0186(3) Uani 1 1 d . . . N3 N 0.02230(15) 0.24253(9) 0.17763(7) 0.0176(3) Uani 1 1 d . . . N4 N 0.12027(17) 0.06773(10) 0.01482(8) 0.0224(3) Uani 1 1 d . . . N5 N 0.21956(17) 0.13013(11) -0.00383(8) 0.0231(3) Uani 1 1 d . . . Si1 Si 0.37789(5) 0.10323(3) 0.18853(3) 0.02049(11) Uani 1 1 d . . . Si2 Si -0.12825(5) 0.29203(3) -0.00587(3) 0.01991(10) Uani 1 1 d . . . Zr1 Zr 0.089081(16) 0.155093(10) 0.086443(8) 0.01447(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 0.0145(8) 0.0200(8) 0.0345(10) 0.0023(7) -0.0006(7) -0.0033(6) C2 0.0185(8) 0.0152(8) 0.0331(10) 0.0019(7) -0.0073(7) -0.0038(6) C3 0.0239(9) 0.0196(8) 0.0335(11) 0.0094(7) -0.0074(8) -0.0080(7) C4 0.0297(11) 0.0182(9) 0.0566(15) 0.0027(9) -0.0136(10) -0.0089(8) C5 0.0198(8) 0.0159(7) 0.0281(10) -0.0034(7) -0.0093(7) 0.0036(6) C6 0.0319(11) 0.0226(9) 0.0389(12) -0.0110(8) -0.0130(9) 0.0067(8) C7 0.0371(12) 0.0363(12) 0.0306(11) -0.0150(9) -0.0088(9) 0.0170(9) C8 0.0308(10) 0.0383(11) 0.0203(9) -0.0044(8) -0.0004(8) 0.0140(9) C9 0.0208(8) 0.0247(9) 0.0203(8) -0.0002(7) -0.0005(7) 0.0070(7) C10 0.0150(8) 0.0378(12) 0.0464(13) 0.0104(10) 0.0043(8) 0.0035(8) C11 0.0363(13) 0.0237(10) 0.0702(18) 0.0123(11) -0.0130(12) -0.0050(9) C12 0.0387(13) 0.0644(17) 0.0287(11) 0.0139(11) 0.0073(10) 0.0333(12) C13 0.0402(16) 0.212(5) 0.0508(18) 0.075(3) 0.0257(14) 0.062(2) C14 0.178(4) 0.069(2) 0.0308(15) -0.0091(14) -0.007(2) 0.075(3) C15 0.0333(12) 0.0513(15) 0.0344(12) 0.0116(11) -0.0046(9) 0.0150(11) C16 0.0420(12) 0.0279(10) 0.0196(9) 0.0044(8) -0.0017(8) 0.0017(9) C17 0.0317(11) 0.0239(10) 0.0468(13) 0.0014(9) -0.0135(10) -0.0060(8) C18 0.0206(9) 0.0244(9) 0.0277(10) 0.0070(7) -0.0005(7) 0.0008(7) C19 0.0426(14) 0.0671(18) 0.0447(14) 0.0314(13) 0.0212(12) 0.0288(13) C20 0.066(2) 0.0316(13) 0.098(3) -0.0190(15) 0.0466(19) -0.0066(13) C21 0.0383(15) 0.095(2) 0.0531(18) -0.0123(17) -0.0167(13) 0.0342(16) C22 0.0230(10) 0.0515(14) 0.0391(13) -0.0101(11) 0.0119(9) 0.0007(9) C23 0.0481(13) 0.0292(11) 0.0254(10) 0.0032(8) 0.0137(9) -0.0017(9) Cl1 0.0207(2) 0.01809(19) 0.0261(2) -0.00141(16) 0.00752(16) -0.00584(15) N1 0.0140(6) 0.0161(7) 0.0248(8) 0.0026(6) 0.0006(6) -0.0009(5) N2 0.0178(7) 0.0151(6) 0.0226(7) 0.0020(5) -0.0009(6) -0.0031(5) N3 0.0156(6) 0.0167(6) 0.0199(7) -0.0008(5) -0.0032(5) 0.0025(5) N4 0.0250(8) 0.0180(7) 0.0249(8) -0.0037(6) 0.0086(6) -0.0057(6) N5 0.0222(8) 0.0234(7) 0.0247(8) -0.0006(6) 0.0086(6) -0.0051(6) Si1 0.0129(2) 0.0202(2) 0.0285(3) 0.0046(2) 0.00233(19) 0.00202(17) Si2 0.0213(2) 0.0163(2) 0.0215(2) 0.00299(18) -0.00407(19) -0.00277(18) Zr1 0.01315(8) 0.01229(7) 0.01809(8) 0.00028(6) 0.00190(5) -0.00132(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 1.468(2) . ? C1 C2 1.576(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.504(3) . ? C2 C4 1.533(3) . ? C2 C3 1.571(3) . ? C3 N2 1.470(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.361(2) . ? C5 C6 1.396(3) . ? C6 C7 1.379(4) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 N3 1.344(2) . ? C9 H9 0.9500 . ? C10 Si1 1.867(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.867(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.526(5) . ? C12 C13 1.536(4) . ? C12 C15 1.538(3) . ? C12 Si1 1.891(3) . ? 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 1.880(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.872(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.518(3) . ? C18 C19 1.519(3) . ? C18 C20 1.525(3) . ? C18 Si2 1.914(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 N5 1.466(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N5 1.467(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Cl1 Zr1 2.4812(6) . ? N1 Si1 1.7254(16) . ? N1 Zr1 2.0579(16) . ? N2 Si2 1.7234(16) . ? N2 Zr1 2.0716(15) . ? N3 Zr1 2.4369(16) . ? N4 N5 1.430(2) . ? N4 Zr1 2.0434(17) . ? N4 H1 0.82(3) . ? N5 Zr1 2.3336(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 117.65(14) . . ? 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 112.16(18) . . ? C5 C2 C3 110.48(15) . . ? C4 C2 C3 105.13(16) . . ? C5 C2 C1 111.25(15) . . ? C4 C2 C1 104.72(15) . . ? C3 C2 C1 112.85(17) . . ? N2 C3 C2 117.48(15) . . ? 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 120.00(19) . . ? N3 C5 C2 115.86(16) . . ? C6 C5 C2 124.14(18) . . ? C7 C6 C5 120.5(2) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.17(19) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C7 C8 C9 118.3(2) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? N3 C9 C8 123.05(19) . . ? 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 . . ? C14 C12 C13 110.7(3) . . ? C14 C12 C15 108.2(2) . . ? C13 C12 C15 107.1(2) . . ? C14 C12 Si1 111.6(2) . . ? C13 C12 Si1 109.6(2) . . ? C15 C12 Si1 109.46(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 . . ? C21 C18 C19 109.3(2) . . ? C21 C18 C20 107.0(2) . . ? C19 C18 C20 108.0(2) . . ? C21 C18 Si2 109.14(17) . . ? C19 C18 Si2 111.31(15) . . ? C20 C18 Si2 112.01(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 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 N1 Si1 119.39(12) . . ? C1 N1 Zr1 107.85(11) . . ? Si1 N1 Zr1 132.75(8) . . ? C3 N2 Si2 119.41(12) . . ? C3 N2 Zr1 108.54(11) . . ? Si2 N2 Zr1 132.04(8) . . ? C9 N3 C5 118.98(16) . . ? C9 N3 Zr1 129.25(12) . . ? C5 N3 Zr1 111.77(12) . . ? N5 N4 Zr1 82.37(10) . . ? N5 N4 H1 114.8(18) . . ? Zr1 N4 H1 162.1(18) . . ? N4 N5 C22 112.66(17) . . ? N4 N5 C23 113.62(16) . . ? C22 N5 C23 109.95(17) . . ? N4 N5 Zr1 60.22(9) . . ? C22 N5 Zr1 124.52(14) . . ? C23 N5 Zr1 123.35(13) . . ? N1 Si1 C11 107.60(10) . . ? N1 Si1 C10 110.85(9) . . ? C11 Si1 C10 109.02(12) . . ? N1 Si1 C12 113.03(9) . . ? C11 Si1 C12 108.47(14) . . ? C10 Si1 C12 107.79(12) . . ? N2 Si2 C17 106.57(9) . . ? N2 Si2 C16 110.69(9) . . ? C17 Si2 C16 110.41(11) . . ? N2 Si2 C18 114.42(9) . . ? C17 Si2 C18 108.47(10) . . ? C16 Si2 C18 106.28(9) . . ? N4 Zr1 N1 108.37(7) . . ? N4 Zr1 N2 108.39(7) . . ? N1 Zr1 N2 111.97(6) . . ? N4 Zr1 N5 37.41(6) . . ? N1 Zr1 N5 87.98(6) . . ? N2 Zr1 N5 88.56(6) . . ? N4 Zr1 N3 170.38(6) . . ? N1 Zr1 N3 76.78(6) . . ? N2 Zr1 N3 76.18(6) . . ? N5 Zr1 N3 152.20(5) . . ? N4 Zr1 Cl1 87.72(5) . . ? N1 Zr1 Cl1 116.86(5) . . ? N2 Zr1 Cl1 119.76(5) . . ? N5 Zr1 Cl1 125.10(4) . . ? N3 Zr1 Cl1 82.68(4) . . ? 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 47.1(2) . . . . ? N1 C1 C2 C4 168.43(18) . . . . ? N1 C1 C2 C3 -77.8(2) . . . . ? C5 C2 C3 N2 -49.7(2) . . . . ? C4 C2 C3 N2 -170.92(18) . . . . ? C1 C2 C3 N2 75.5(2) . . . . ? C4 C2 C5 N3 -179.89(16) . . . . ? C3 C2 C5 N3 63.2(2) . . . . ? C1 C2 C5 N3 -63.0(2) . . . . ? C4 C2 C5 C6 0.2(3) . . . . ? C3 C2 C5 C6 -116.7(2) . . . . ? C1 C2 C5 C6 117.1(2) . . . . ? N3 C5 C6 C7 -1.1(3) . . . . ? C2 C5 C6 C7 178.81(18) . . . . ? C5 C6 C7 C8 -0.4(3) . . . . ? C6 C7 C8 C9 1.6(3) . . . . ? C7 C8 C9 N3 -1.3(3) . . . . ? C2 C1 N1 Si1 -143.43(15) . . . . ? C2 C1 N1 Zr1 35.7(2) . . . . ? C2 C3 N2 Si2 146.25(15) . . . . ? C2 C3 N2 Zr1 -33.1(2) . . . . ? C8 C9 N3 C5 -0.2(3) . . . . ? C8 C9 N3 Zr1 -179.35(14) . . . . ? C6 C5 N3 C9 1.4(3) . . . . ? C2 C5 N3 C9 -178.53(15) . . . . ? C6 C5 N3 Zr1 -179.32(14) . . . . ? C2 C5 N3 Zr1 0.78(18) . . . . ? Zr1 N4 N5 C22 117.95(15) . . . . ? Zr1 N4 N5 C23 -116.17(15) . . . . ? C1 N1 Si1 C11 -163.59(16) . . . . ? Zr1 N1 Si1 C11 17.51(16) . . . . ? C1 N1 Si1 C10 -44.47(18) . . . . ? Zr1 N1 Si1 C10 136.63(13) . . . . ? C1 N1 Si1 C12 76.67(18) . . . . ? Zr1 N1 Si1 C12 -102.23(15) . . . . ? C14 C12 Si1 N1 -56.4(2) . . . . ? C13 C12 Si1 N1 66.6(2) . . . . ? C15 C12 Si1 N1 -176.16(17) . . . . ? C14 C12 Si1 C11 -175.7(2) . . . . ? C13 C12 Si1 C11 -52.6(2) . . . . ? C15 C12 Si1 C11 64.6(2) . . . . ? C14 C12 Si1 C10 66.4(2) . . . . ? C13 C12 Si1 C10 -170.5(2) . . . . ? C15 C12 Si1 C10 -53.3(2) . . . . ? C3 N2 Si2 C17 171.70(16) . . . . ? Zr1 N2 Si2 C17 -9.15(15) . . . . ? C3 N2 Si2 C16 51.61(17) . . . . ? Zr1 N2 Si2 C16 -129.24(12) . . . . ? C3 N2 Si2 C18 -68.43(17) . . . . ? Zr1 N2 Si2 C18 110.72(12) . . . . ? C21 C18 Si2 N2 -169.92(18) . . . . ? C19 C18 Si2 N2 -49.2(2) . . . . ? C20 C18 Si2 N2 71.8(2) . . . . ? C21 C18 Si2 C17 -51.1(2) . . . . ? C19 C18 Si2 C17 69.6(2) . . . . ? C20 C18 Si2 C17 -169.4(2) . . . . ? C21 C18 Si2 C16 67.6(2) . . . . ? C19 C18 Si2 C16 -171.66(18) . . . . ? C20 C18 Si2 C16 -50.6(2) . . . . ? N5 N4 Zr1 N1 -60.30(11) . . . . ? N5 N4 Zr1 N2 61.43(11) . . . . ? N5 N4 Zr1 N3 178.5(3) . . . . ? N5 N4 Zr1 Cl1 -177.89(10) . . . . ? C1 N1 Zr1 N4 118.19(12) . . . . ? Si1 N1 Zr1 N4 -62.82(13) . . . . ? C1 N1 Zr1 N2 -1.32(14) . . . . ? Si1 N1 Zr1 N2 177.68(11) . . . . ? C1 N1 Zr1 N5 86.32(12) . . . . ? Si1 N1 Zr1 N5 -94.69(12) . . . . ? C1 N1 Zr1 N3 -70.26(12) . . . . ? Si1 N1 Zr1 N3 108.74(12) . . . . ? C1 N1 Zr1 Cl1 -144.85(11) . . . . ? Si1 N1 Zr1 Cl1 34.15(13) . . . . ? C3 N2 Zr1 N4 -119.45(13) . . . . ? Si2 N2 Zr1 N4 61.33(13) . . . . ? C3 N2 Zr1 N1 0.04(14) . . . . ? Si2 N2 Zr1 N1 -179.18(10) . . . . ? C3 N2 Zr1 N5 -87.19(13) . . . . ? Si2 N2 Zr1 N5 93.59(12) . . . . ? C3 N2 Zr1 N3 69.36(13) . . . . ? Si2 N2 Zr1 N3 -109.86(12) . . . . ? C3 N2 Zr1 Cl1 142.40(11) . . . . ? Si2 N2 Zr1 Cl1 -36.82(13) . . . . ? C22 N5 Zr1 N4 -98.3(2) . . . . ? C23 N5 Zr1 N4 100.14(19) . . . . ? N4 N5 Zr1 N1 124.43(11) . . . . ? C22 N5 Zr1 N1 26.08(17) . . . . ? C23 N5 Zr1 N1 -135.43(16) . . . . ? N4 N5 Zr1 N2 -123.53(11) . . . . ? C22 N5 Zr1 N2 138.13(17) . . . . ? C23 N5 Zr1 N2 -23.39(16) . . . . ? N4 N5 Zr1 N3 -179.48(11) . . . . ? C22 N5 Zr1 N3 82.2(2) . . . . ? C23 N5 Zr1 N3 -79.34(19) . . . . ? N4 N5 Zr1 Cl1 2.58(12) . . . . ? C22 N5 Zr1 Cl1 -95.77(16) . . . . ? C23 N5 Zr1 Cl1 102.72(15) . . . . ? C9 N3 Zr1 N4 0.6(4) . . . . ? C5 N3 Zr1 N4 -178.6(3) . . . . ? C9 N3 Zr1 N1 -122.85(15) . . . . ? C5 N3 Zr1 N1 57.93(12) . . . . ? C9 N3 Zr1 N2 120.18(15) . . . . ? C5 N3 Zr1 N2 -59.04(12) . . . . ? C9 N3 Zr1 N5 178.72(14) . . . . ? C5 N3 Zr1 N5 -0.50(19) . . . . ? C9 N3 Zr1 Cl1 -2.98(14) . . . . ? C5 N3 Zr1 Cl1 177.81(12) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 32.10 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.622 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.091 _audit_block_code ga_hh7 _audit_block_refno 316 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 674841' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H59 N5 Si3 Zr' _chemical_formula_weight 629.28 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.7739(9) _cell_length_b 12.2454(7) _cell_length_c 18.3510(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.5670(10) _cell_angle_gamma 90.00 _cell_volume 3505.5(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 needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8982 _exptl_absorpt_correction_T_max 0.9574 _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 24978 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7742 _reflns_number_gt 5499 _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^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7742 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.19181(18) -0.1256(2) 0.51200(17) 0.0191(6) Uani 1 1 d . . . H1A H 0.1341 -0.1102 0.5124 0.023 Uiso 1 1 calc R . . H1B H 0.2171 -0.1844 0.5507 0.023 Uiso 1 1 calc R . . C2 C 0.18036(17) -0.1714(2) 0.42896(17) 0.0179(6) Uani 1 1 d . . . C3 C 0.11328(17) -0.1063(2) 0.35905(17) 0.0200(6) Uani 1 1 d . . . H3A H 0.0980 -0.1524 0.3115 0.024 Uiso 1 1 calc R . . H3B H 0.0606 -0.0974 0.3709 0.024 Uiso 1 1 calc R . . C4 C 0.14121(19) -0.2846(2) 0.42501(19) 0.0258(7) Uani 1 1 d . . . H4A H 0.1341 -0.3187 0.3747 0.039 Uiso 1 1 calc R . . H4B H 0.0852 -0.2782 0.4300 0.039 Uiso 1 1 calc R . . H4C H 0.1792 -0.3298 0.4678 0.039 Uiso 1 1 calc R . . C5 C 0.26604(17) -0.1750(2) 0.41908(16) 0.0166(6) Uani 1 1 d . . . C6 C 0.30534(19) -0.2711(2) 0.40938(18) 0.0232(7) Uani 1 1 d . . . H6 H 0.2793 -0.3395 0.4110 0.028 Uiso 1 1 calc R . . C7 C 0.38188(19) -0.2677(3) 0.39750(18) 0.0253(7) Uani 1 1 d . . . H7 H 0.4090 -0.3331 0.3910 0.030 Uiso 1 1 calc R . . C8 C 0.41803(19) -0.1680(3) 0.39528(18) 0.0245(7) Uani 1 1 d . . . H8 H 0.4702 -0.1629 0.3864 0.029 Uiso 1 1 calc R . . C9 C 0.37726(17) -0.0754(2) 0.40618(17) 0.0188(6) Uani 1 1 d . . . H9 H 0.4031 -0.0067 0.4053 0.023 Uiso 1 1 calc R . . C10 C 0.3438(2) 0.1273(3) 0.65533(19) 0.0288(7) Uani 1 1 d . . . H10A H 0.3819 0.1443 0.6272 0.043 Uiso 1 1 calc R . . H10B H 0.3745 0.1389 0.7116 0.043 Uiso 1 1 calc R . . H10C H 0.2935 0.1752 0.6366 0.043 Uiso 1 1 calc R . . C11 C 0.2463(2) -0.0568(3) 0.70015(19) 0.0295(8) Uani 1 1 d . . . H11A H 0.2023 -0.0014 0.6948 0.044 Uiso 1 1 calc R . . H11B H 0.2852 -0.0612 0.7550 0.044 Uiso 1 1 calc R . . H11C H 0.2188 -0.1279 0.6834 0.044 Uiso 1 1 calc R . . C12 C 0.40849(18) -0.1089(3) 0.66796(18) 0.0223(7) Uani 1 1 d . . . C13 C 0.4728(2) -0.0687(4) 0.7476(2) 0.0470(10) Uani 1 1 d . . . H13A H 0.4447 -0.0666 0.7858 0.071 Uiso 1 1 calc R . . H13B H 0.4929 0.0046 0.7414 0.071 Uiso 1 1 calc R . . H13C H 0.5218 -0.1188 0.7660 0.071 Uiso 1 1 calc R . . C14 C 0.3887(2) -0.2286(3) 0.6773(2) 0.0405(9) Uani 1 1 d . . . H14A H 0.3517 -0.2580 0.6265 0.061 Uiso 1 1 calc R . . H14B H 0.3594 -0.2343 0.7146 0.061 Uiso 1 1 calc R . . H14C H 0.4423 -0.2702 0.6970 0.061 Uiso 1 1 calc R . . C15 C 0.4517(2) -0.1019(3) 0.6082(2) 0.0315(8) Uani 1 1 d . . . H15A H 0.5071 -0.1395 0.6287 0.047 Uiso 1 1 calc R . . H15B H 0.4607 -0.0251 0.5984 0.047 Uiso 1 1 calc R . . H15C H 0.4151 -0.1365 0.5592 0.047 Uiso 1 1 calc R . . C16 C 0.0979(2) 0.1923(2) 0.23688(19) 0.0276(7) Uani 1 1 d . . . H16A H 0.0510 0.2208 0.2511 0.041 Uiso 1 1 calc R . . H16B H 0.0897 0.2153 0.1835 0.041 Uiso 1 1 calc R . . H16C H 0.1526 0.2208 0.2734 0.041 Uiso 1 1 calc R . . C17 C -0.01315(19) -0.0144(3) 0.19312(19) 0.0288(7) Uani 1 1 d . . . H17A H -0.0116 -0.0944 0.1925 0.043 Uiso 1 1 calc R . . H17B H -0.0375 0.0130 0.1392 0.043 Uiso 1 1 calc R . . H17C H -0.0487 0.0099 0.2221 0.043 Uiso 1 1 calc R . . C18 C 0.1651(2) -0.0117(3) 0.18426(17) 0.0238(7) Uani 1 1 d . . . C19 C 0.1838(2) -0.1341(3) 0.19762(19) 0.0291(7) Uani 1 1 d . . . H19A H 0.1298 -0.1738 0.1863 0.044 Uiso 1 1 calc R . . H19B H 0.2212 -0.1466 0.2522 0.044 Uiso 1 1 calc R . . H19C H 0.2122 -0.1601 0.1628 0.044 Uiso 1 1 calc R . . C20 C 0.1168(2) 0.0068(3) 0.09577(19) 0.0373(9) Uani 1 1 d . . . H20A H 0.1543 -0.0119 0.0674 0.056 Uiso 1 1 calc R . . H20B H 0.0998 0.0837 0.0863 0.056 Uiso 1 1 calc R . . H20C H 0.0656 -0.0394 0.0773 0.056 Uiso 1 1 calc R . . C21 C 0.2513(2) 0.0491(3) 0.2093(2) 0.0340(8) Uani 1 1 d . . . H21A H 0.2815 0.0417 0.2660 0.051 Uiso 1 1 calc R . . H21B H 0.2410 0.1266 0.1957 0.051 Uiso 1 1 calc R . . H21C H 0.2865 0.0178 0.1820 0.051 Uiso 1 1 calc R . . C22 C 0.0883(2) 0.1368(3) 0.54171(19) 0.0272(7) Uani 1 1 d . . . H22A H 0.1449 0.1259 0.5828 0.041 Uiso 1 1 calc R . . H22B H 0.0499 0.0776 0.5437 0.041 Uiso 1 1 calc R . . H22C H 0.0647 0.2069 0.5500 0.041 Uiso 1 1 calc R . . C23 C 0.01308(19) 0.1552(3) 0.40288(19) 0.0292(8) Uani 1 1 d . . . H23A H -0.0095 0.2263 0.4104 0.044 Uiso 1 1 calc R . . H23B H -0.0267 0.0975 0.4046 0.044 Uiso 1 1 calc R . . H23C H 0.0195 0.1538 0.3519 0.044 Uiso 1 1 calc R . . C24 C 0.32931(17) 0.1800(2) 0.43492(16) 0.0162(6) Uani 1 1 d . . . H24A H 0.3821 0.1504 0.4751 0.019 Uiso 1 1 calc R . . H24B H 0.3330 0.1619 0.3837 0.019 Uiso 1 1 calc R . . C25 C 0.2449(2) 0.4014(3) 0.3739(2) 0.0343(8) Uani 1 1 d . . . H25A H 0.2345 0.3769 0.3203 0.051 Uiso 1 1 calc R . . H25B H 0.2550 0.4804 0.3775 0.051 Uiso 1 1 calc R . . H25C H 0.1948 0.3846 0.3872 0.051 Uiso 1 1 calc R . . C26 C 0.4344(2) 0.3791(3) 0.4198(2) 0.0288(7) Uani 1 1 d . . . H26A H 0.4865 0.3411 0.4530 0.043 Uiso 1 1 calc R . . H26B H 0.4416 0.4579 0.4294 0.043 Uiso 1 1 calc R . . H26C H 0.4240 0.3642 0.3646 0.043 Uiso 1 1 calc R . . C27 C 0.3581(2) 0.3784(3) 0.5449(2) 0.0326(8) Uani 1 1 d . . . H27A H 0.3095 0.3559 0.5590 0.049 Uiso 1 1 calc R . . H27B H 0.3626 0.4582 0.5467 0.049 Uiso 1 1 calc R . . H27C H 0.4110 0.3466 0.5820 0.049 Uiso 1 1 calc R . . H4 H 0.147(2) 0.273(3) 0.4643(19) 0.023(9) Uiso 1 1 d . . . N1 N 0.24431(14) -0.02717(19) 0.53950(13) 0.0153(5) Uani 1 1 d . . . N2 N 0.13787(14) 0.00232(19) 0.33955(14) 0.0164(5) Uani 1 1 d . . . N3 N 0.30289(14) -0.07693(19) 0.41804(13) 0.0154(5) Uani 1 1 d . . . N4 N 0.16051(16) 0.2125(2) 0.46137(16) 0.0232(6) Uani 1 1 d . . . N5 N 0.09660(14) 0.1372(2) 0.46513(15) 0.0205(5) Uani 1 1 d . . . Si1 Si 0.30866(5) -0.01852(7) 0.63728(5) 0.01824(18) Uani 1 1 d . . . Si2 Si 0.09872(5) 0.03983(6) 0.24204(5) 0.01793(18) Uani 1 1 d . . . Si3 Si 0.34098(5) 0.32967(7) 0.44360(5) 0.01828(18) Uani 1 1 d . . . Zr1 Zr 0.220067(16) 0.07406(2) 0.442596(16) 0.01281(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0185(14) 0.0187(15) 0.0202(15) 0.0022(12) 0.0074(12) -0.0053(12) C2 0.0184(14) 0.0112(14) 0.0213(15) 0.0010(12) 0.0040(12) -0.0011(11) C3 0.0148(14) 0.0184(15) 0.0217(16) 0.0024(12) 0.0005(12) -0.0028(11) C4 0.0266(17) 0.0174(16) 0.0300(18) 0.0018(13) 0.0062(14) -0.0077(13) C5 0.0177(14) 0.0153(14) 0.0120(14) 0.0004(11) 0.0000(11) -0.0003(11) C6 0.0300(17) 0.0123(15) 0.0237(17) -0.0027(12) 0.0057(13) 0.0005(12) C7 0.0259(17) 0.0209(16) 0.0252(17) -0.0053(13) 0.0046(13) 0.0098(13) C8 0.0195(15) 0.0317(18) 0.0228(16) -0.0038(14) 0.0085(13) 0.0036(13) C9 0.0197(14) 0.0185(15) 0.0183(15) -0.0007(12) 0.0070(12) -0.0009(12) C10 0.0367(19) 0.0232(17) 0.0228(17) -0.0038(14) 0.0065(14) -0.0028(14) C11 0.0344(18) 0.032(2) 0.0276(18) 0.0001(15) 0.0178(15) 0.0031(14) C12 0.0219(15) 0.0250(16) 0.0176(15) 0.0067(13) 0.0045(13) 0.0018(12) C13 0.036(2) 0.069(3) 0.0229(19) -0.0056(19) -0.0042(16) 0.014(2) C14 0.0298(19) 0.030(2) 0.064(3) 0.0177(19) 0.0204(19) 0.0098(15) C15 0.0237(17) 0.039(2) 0.034(2) 0.0112(16) 0.0127(15) 0.0085(14) C16 0.0407(19) 0.0174(17) 0.0227(17) 0.0016(13) 0.0094(15) 0.0045(14) C17 0.0227(16) 0.0230(17) 0.0294(18) 0.0000(14) -0.0037(13) 0.0000(13) C18 0.0300(17) 0.0227(17) 0.0156(15) -0.0020(13) 0.0047(13) 0.0026(13) C19 0.0347(19) 0.0256(18) 0.0247(17) -0.0024(14) 0.0081(14) 0.0051(14) C20 0.054(2) 0.032(2) 0.0204(17) 0.0016(15) 0.0080(16) 0.0120(17) C21 0.0365(19) 0.040(2) 0.0310(19) -0.0010(16) 0.0191(16) -0.0018(16) C22 0.0291(17) 0.0279(18) 0.0296(18) -0.0029(14) 0.0164(14) 0.0024(14) C23 0.0207(16) 0.0337(19) 0.0329(19) 0.0045(15) 0.0098(14) 0.0058(14) C24 0.0174(14) 0.0165(14) 0.0142(14) -0.0005(11) 0.0052(11) -0.0017(11) C25 0.0309(18) 0.0162(17) 0.046(2) 0.0072(15) 0.0028(16) -0.0028(13) C26 0.0325(18) 0.0226(17) 0.0302(18) -0.0013(14) 0.0101(15) -0.0122(14) C27 0.046(2) 0.0217(17) 0.0333(19) -0.0073(15) 0.0175(16) -0.0089(15) N1 0.0141(11) 0.0155(12) 0.0150(12) 0.0005(10) 0.0039(9) -0.0003(9) N2 0.0152(12) 0.0133(12) 0.0193(13) -0.0001(10) 0.0045(10) -0.0007(9) N3 0.0143(11) 0.0149(12) 0.0129(12) -0.0016(10) 0.0002(9) -0.0019(9) N4 0.0248(14) 0.0120(13) 0.0358(16) 0.0002(12) 0.0148(12) 0.0011(11) N5 0.0173(12) 0.0192(13) 0.0262(14) 0.0021(11) 0.0094(11) 0.0012(10) Si1 0.0210(4) 0.0185(4) 0.0158(4) 0.0006(3) 0.0075(3) -0.0010(3) Si2 0.0178(4) 0.0132(4) 0.0178(4) -0.0003(3) 0.0006(3) 0.0010(3) Si3 0.0218(4) 0.0130(4) 0.0188(4) -0.0009(3) 0.0061(3) -0.0039(3) Zr1 0.01271(14) 0.01050(13) 0.01496(14) -0.00009(11) 0.00478(10) -0.00060(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.469(3) . ? C1 C2 1.568(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C5 1.514(4) . ? C2 C4 1.525(4) . ? C2 C3 1.577(4) . ? 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 1.354(4) . ? C5 C6 1.392(4) . ? C6 C7 1.380(4) . ? C6 H6 0.9500 . ? C7 C8 1.370(4) . ? C7 H7 0.9500 . ? C8 C9 1.376(4) . ? C8 H8 0.9500 . ? C9 N3 1.343(3) . ? C9 H9 0.9500 . ? C10 Si1 1.872(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Si1 1.880(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.522(4) . ? C12 C14 1.527(4) . ? C12 C13 1.543(4) . ? C12 Si1 1.911(3) . ? 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 1.869(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Si2 1.879(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.532(4) . ? C18 C21 1.539(4) . ? C18 C20 1.542(4) . ? C18 Si2 1.906(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 N5 1.462(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N5 1.463(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Si3 1.844(3) . ? C24 Zr1 2.291(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 Si3 1.868(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 Si3 1.875(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si3 1.871(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N1 Si1 1.724(2) . ? N1 Zr1 2.081(2) . ? N2 Si2 1.726(2) . ? N2 Zr1 2.081(2) . ? N3 Zr1 2.452(2) . ? N4 N5 1.435(3) . ? N4 Zr1 2.060(3) . ? N4 H4 0.79(3) . ? N5 Zr1 2.385(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 118.1(2) . . ? 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 112.3(2) . . ? C5 C2 C1 110.1(2) . . ? C4 C2 C1 105.5(2) . . ? C5 C2 C3 110.0(2) . . ? C4 C2 C3 104.8(2) . . ? C1 C2 C3 114.0(2) . . ? N2 C3 C2 118.3(2) . . ? 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 120.5(3) . . ? N3 C5 C2 115.7(2) . . ? C6 C5 C2 123.7(3) . . ? C7 C6 C5 120.5(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 118.6(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 118.7(3) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? N3 C9 C8 123.6(3) . . ? N3 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? 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 108.4(3) . . ? C15 C12 C13 108.1(3) . . ? C14 C12 C13 107.7(3) . . ? C15 C12 Si1 110.7(2) . . ? C14 C12 Si1 112.7(2) . . ? C13 C12 Si1 109.1(2) . . ? 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 . . ? C19 C18 C21 108.2(3) . . ? C19 C18 C20 108.0(3) . . ? C21 C18 C20 108.4(3) . . ? C19 C18 Si2 111.2(2) . . ? C21 C18 Si2 110.6(2) . . ? C20 C18 Si2 110.4(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 . . ? N5 C22 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 Zr1 128.28(14) . . ? Si3 C24 H24A 105.2 . . ? Zr1 C24 H24A 105.2 . . ? Si3 C24 H24B 105.2 . . ? Zr1 C24 H24B 105.2 . . ? H24A C24 H24B 105.9 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C1 N1 Si1 118.36(18) . . ? C1 N1 Zr1 106.93(16) . . ? Si1 N1 Zr1 134.72(13) . . ? C3 N2 Si2 117.23(18) . . ? C3 N2 Zr1 108.12(17) . . ? Si2 N2 Zr1 134.59(13) . . ? C9 N3 C5 118.1(2) . . ? C9 N3 Zr1 129.96(19) . . ? C5 N3 Zr1 111.95(17) . . ? N5 N4 Zr1 84.02(15) . . ? N5 N4 H4 111(2) . . ? Zr1 N4 H4 164(2) . . ? N4 N5 C22 112.6(2) . . ? N4 N5 C23 112.5(2) . . ? C22 N5 C23 110.4(2) . . ? N4 N5 Zr1 59.22(13) . . ? C22 N5 Zr1 124.12(18) . . ? C23 N5 Zr1 123.84(19) . . ? N1 Si1 C10 106.19(13) . . ? N1 Si1 C11 110.29(13) . . ? C10 Si1 C11 109.88(15) . . ? N1 Si1 C12 114.62(13) . . ? C10 Si1 C12 108.37(14) . . ? C11 Si1 C12 107.44(14) . . ? N2 Si2 C16 108.13(13) . . ? N2 Si2 C17 109.50(14) . . ? C16 Si2 C17 109.96(15) . . ? N2 Si2 C18 114.29(12) . . ? C16 Si2 C18 107.30(15) . . ? C17 Si2 C18 107.61(14) . . ? C24 Si3 C25 111.76(14) . . ? C24 Si3 C27 112.05(14) . . ? C25 Si3 C27 108.00(17) . . ? C24 Si3 C26 111.85(14) . . ? C25 Si3 C26 105.85(16) . . ? C27 Si3 C26 107.00(15) . . ? N4 Zr1 N2 107.41(10) . . ? N4 Zr1 N1 107.56(10) . . ? N2 Zr1 N1 112.39(9) . . ? N4 Zr1 C24 89.56(10) . . ? N2 Zr1 C24 117.44(9) . . ? N1 Zr1 C24 118.70(9) . . ? N4 Zr1 N5 36.76(9) . . ? N2 Zr1 N5 88.10(9) . . ? N1 Zr1 N5 87.38(9) . . ? C24 Zr1 N5 126.32(9) . . ? N4 Zr1 N3 173.55(9) . . ? N2 Zr1 N3 75.26(8) . . ? N1 Zr1 N3 76.23(8) . . ? C24 Zr1 N3 84.02(9) . . ? N5 Zr1 N3 149.66(8) . . ? 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 46.2(3) . . . . ? N1 C1 C2 C4 167.7(2) . . . . ? N1 C1 C2 C3 -78.0(3) . . . . ? C5 C2 C3 N2 -50.4(3) . . . . ? C4 C2 C3 N2 -171.3(2) . . . . ? C1 C2 C3 N2 73.8(3) . . . . ? C4 C2 C5 N3 176.9(2) . . . . ? C1 C2 C5 N3 -65.8(3) . . . . ? C3 C2 C5 N3 60.6(3) . . . . ? C4 C2 C5 C6 -1.4(4) . . . . ? C1 C2 C5 C6 115.9(3) . . . . ? C3 C2 C5 C6 -117.7(3) . . . . ? N3 C5 C6 C7 -0.9(4) . . . . ? C2 C5 C6 C7 177.3(3) . . . . ? C5 C6 C7 C8 -0.2(5) . . . . ? C6 C7 C8 C9 1.0(5) . . . . ? C7 C8 C9 N3 -0.8(5) . . . . ? C2 C1 N1 Si1 -142.5(2) . . . . ? C2 C1 N1 Zr1 37.4(3) . . . . ? C2 C3 N2 Si2 145.7(2) . . . . ? C2 C3 N2 Zr1 -32.0(3) . . . . ? C8 C9 N3 C5 -0.2(4) . . . . ? C8 C9 N3 Zr1 178.0(2) . . . . ? C6 C5 N3 C9 1.0(4) . . . . ? C2 C5 N3 C9 -177.3(2) . . . . ? C6 C5 N3 Zr1 -177.5(2) . . . . ? C2 C5 N3 Zr1 4.2(3) . . . . ? Zr1 N4 N5 C22 117.3(2) . . . . ? Zr1 N4 N5 C23 -117.0(2) . . . . ? C1 N1 Si1 C10 -166.5(2) . . . . ? Zr1 N1 Si1 C10 13.6(2) . . . . ? C1 N1 Si1 C11 -47.5(2) . . . . ? Zr1 N1 Si1 C11 132.59(18) . . . . ? C1 N1 Si1 C12 73.9(2) . . . . ? Zr1 N1 Si1 C12 -106.01(19) . . . . ? C15 C12 Si1 N1 44.0(3) . . . . ? C14 C12 Si1 N1 -77.5(3) . . . . ? C13 C12 Si1 N1 162.9(2) . . . . ? C15 C12 Si1 C10 -74.3(3) . . . . ? C14 C12 Si1 C10 164.1(2) . . . . ? C13 C12 Si1 C10 44.5(3) . . . . ? C15 C12 Si1 C11 167.0(2) . . . . ? C14 C12 Si1 C11 45.4(3) . . . . ? C13 C12 Si1 C11 -74.2(3) . . . . ? C3 N2 Si2 C16 156.2(2) . . . . ? Zr1 N2 Si2 C16 -26.8(2) . . . . ? C3 N2 Si2 C17 36.4(2) . . . . ? Zr1 N2 Si2 C17 -146.65(17) . . . . ? C3 N2 Si2 C18 -84.4(2) . . . . ? Zr1 N2 Si2 C18 92.6(2) . . . . ? C19 C18 Si2 N2 49.5(2) . . . . ? C21 C18 Si2 N2 -70.7(3) . . . . ? C20 C18 Si2 N2 169.4(2) . . . . ? C19 C18 Si2 C16 169.4(2) . . . . ? C21 C18 Si2 C16 49.2(3) . . . . ? C20 C18 Si2 C16 -70.7(3) . . . . ? C19 C18 Si2 C17 -72.3(2) . . . . ? C21 C18 Si2 C17 167.5(2) . . . . ? C20 C18 Si2 C17 47.6(3) . . . . ? Zr1 C24 Si3 C25 -53.9(2) . . . . ? Zr1 C24 Si3 C27 67.4(2) . . . . ? Zr1 C24 Si3 C26 -172.40(17) . . . . ? N5 N4 Zr1 N2 61.45(17) . . . . ? N5 N4 Zr1 N1 -59.75(17) . . . . ? N5 N4 Zr1 C24 -179.83(16) . . . . ? N5 N4 Zr1 N3 175.1(8) . . . . ? C3 N2 Zr1 N4 -117.05(18) . . . . ? Si2 N2 Zr1 N4 65.79(19) . . . . ? C3 N2 Zr1 N1 1.06(19) . . . . ? Si2 N2 Zr1 N1 -176.10(16) . . . . ? C3 N2 Zr1 C24 144.11(17) . . . . ? Si2 N2 Zr1 C24 -33.1(2) . . . . ? C3 N2 Zr1 N5 -85.32(17) . . . . ? Si2 N2 Zr1 N5 97.52(18) . . . . ? C3 N2 Zr1 N3 69.06(17) . . . . ? Si2 N2 Zr1 N3 -108.10(18) . . . . ? C1 N1 Zr1 N4 114.54(17) . . . . ? Si1 N1 Zr1 N4 -65.56(19) . . . . ? C1 N1 Zr1 N2 -3.48(19) . . . . ? Si1 N1 Zr1 N2 176.42(16) . . . . ? C1 N1 Zr1 C24 -146.02(17) . . . . ? Si1 N1 Zr1 C24 33.9(2) . . . . ? C1 N1 Zr1 N5 83.37(17) . . . . ? Si1 N1 Zr1 N5 -96.73(18) . . . . ? C1 N1 Zr1 N3 -70.88(17) . . . . ? Si1 N1 Zr1 N3 109.02(18) . . . . ? Si3 C24 Zr1 N4 -0.49(19) . . . . ? Si3 C24 Zr1 N2 108.97(18) . . . . ? Si3 C24 Zr1 N1 -110.35(18) . . . . ? Si3 C24 Zr1 N5 -0.6(2) . . . . ? Si3 C24 Zr1 N3 178.93(18) . . . . ? C22 N5 Zr1 N4 -97.9(3) . . . . ? C23 N5 Zr1 N4 97.9(3) . . . . ? N4 N5 Zr1 N2 -123.01(17) . . . . ? C22 N5 Zr1 N2 139.1(2) . . . . ? C23 N5 Zr1 N2 -25.1(2) . . . . ? N4 N5 Zr1 N1 124.46(17) . . . . ? C22 N5 Zr1 N1 26.6(2) . . . . ? C23 N5 Zr1 N1 -137.6(2) . . . . ? N4 N5 Zr1 C24 0.2(2) . . . . ? C22 N5 Zr1 C24 -97.6(2) . . . . ? C23 N5 Zr1 C24 98.1(2) . . . . ? N4 N5 Zr1 N3 -178.90(17) . . . . ? C22 N5 Zr1 N3 83.2(3) . . . . ? C23 N5 Zr1 N3 -81.0(3) . . . . ? C9 N3 Zr1 N4 4.3(10) . . . . ? C5 N3 Zr1 N4 -177.4(8) . . . . ? C9 N3 Zr1 N2 119.6(2) . . . . ? C5 N3 Zr1 N2 -62.09(18) . . . . ? C9 N3 Zr1 N1 -122.3(2) . . . . ? C5 N3 Zr1 N1 55.95(18) . . . . ? C9 N3 Zr1 C24 -0.8(2) . . . . ? C5 N3 Zr1 C24 177.47(19) . . . . ? C9 N3 Zr1 N5 178.5(2) . . . . ? C5 N3 Zr1 N5 -3.3(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.669 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.097 _audit_block_code ga_hh9 _audit_block_refno 336 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_4a _database_code_depnum_ccdc_archive 'CCDC 674842' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H50 Cl N5 Si2 Zr' _chemical_formula_weight 639.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.360(3) _cell_length_b 15.968(3) _cell_length_c 16.930(3) _cell_angle_alpha 70.93(3) _cell_angle_beta 85.85(3) _cell_angle_gamma 74.74(3) _cell_volume 3292.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 170(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 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004-2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 (Nonius Kappa CCD)' _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 61069 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.76 _reflns_number_total 15160 _reflns_number_gt 13082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0376P)^2^+1.2874P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15160 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.15508(13) 0.27155(11) 0.07161(11) 0.0189(3) Uani 1 1 d . . . H1A H 0.1601 0.2406 0.1315 0.023 Uiso 1 1 calc R . . H1B H 0.0830 0.3043 0.0583 0.023 Uiso 1 1 calc R . . C2 C 0.22104(13) 0.34406(11) 0.05020(10) 0.0177(3) Uani 1 1 d . . . C3 C 0.33570(13) 0.30266(12) 0.08636(10) 0.0192(3) Uani 1 1 d . . . H3A H 0.3613 0.3526 0.0903 0.023 Uiso 1 1 calc R . . H3B H 0.3328 0.2618 0.1428 0.023 Uiso 1 1 calc R . . C4 C 0.16990(14) 0.41153(13) 0.09697(12) 0.0252(4) Uani 1 1 d . . . H4A H 0.2049 0.4597 0.0841 0.038 Uiso 1 1 calc R . . H4B H 0.1745 0.3799 0.1560 0.038 Uiso 1 1 calc R . . H4C H 0.0983 0.4373 0.0801 0.038 Uiso 1 1 calc R . . C5 C 0.22119(13) 0.39011(11) -0.04356(10) 0.0177(3) Uani 1 1 d . . . C6 C 0.17837(14) 0.48305(12) -0.08256(12) 0.0242(4) Uani 1 1 d . . . H6 H 0.1480 0.5207 -0.0509 0.029 Uiso 1 1 calc R . . C7 C 0.18109(15) 0.51933(13) -0.16884(12) 0.0282(4) Uani 1 1 d . . . H7 H 0.1527 0.5814 -0.1955 0.034 Uiso 1 1 calc R . . C8 C 0.22622(14) 0.46253(13) -0.21451(11) 0.0258(4) Uani 1 1 d . . . H8 H 0.2287 0.4853 -0.2725 0.031 Uiso 1 1 calc R . . C9 C 0.26781(13) 0.37079(12) -0.17237(11) 0.0215(4) Uani 1 1 d . . . H9 H 0.2984 0.3324 -0.2033 0.026 Uiso 1 1 calc R . . C10 C 0.14975(16) 0.05051(13) -0.01844(13) 0.0314(4) Uani 1 1 d . . . H10A H 0.2005 0.0628 -0.0609 0.047 Uiso 1 1 calc R . . H10B H 0.0983 0.0298 -0.0384 0.047 Uiso 1 1 calc R . . H10C H 0.1831 0.0040 0.0309 0.047 Uiso 1 1 calc R . . C11 C 0.00152(15) 0.13069(14) 0.10001(12) 0.0305(4) Uani 1 1 d . . . H11A H 0.0439 0.0935 0.1486 0.046 Uiso 1 1 calc R . . H11B H -0.0451 0.0982 0.0906 0.046 Uiso 1 1 calc R . . H11C H -0.0377 0.1867 0.1085 0.046 Uiso 1 1 calc R . . C12 C 0.00251(14) 0.24050(12) -0.08704(11) 0.0237(4) Uani 1 1 d . . . C13 C -0.03715(16) 0.33672(13) -0.07899(13) 0.0326(4) Uani 1 1 d . . . H13A H -0.0823 0.3756 -0.1255 0.049 Uiso 1 1 calc R . . H13B H 0.0207 0.3617 -0.0785 0.049 Uiso 1 1 calc R . . H13C H -0.0746 0.3330 -0.0279 0.049 Uiso 1 1 calc R . . C14 C -0.09167(15) 0.20474(14) -0.09497(13) 0.0343(5) Uani 1 1 d . . . H14A H -0.1317 0.2449 -0.1440 0.051 Uiso 1 1 calc R . . H14B H -0.1340 0.2028 -0.0464 0.051 Uiso 1 1 calc R . . H14C H -0.0679 0.1443 -0.0994 0.051 Uiso 1 1 calc R . . C15 C 0.06509(16) 0.24810(15) -0.16723(12) 0.0351(5) Uani 1 1 d . . . H15A H 0.0848 0.1896 -0.1762 0.053 Uiso 1 1 calc R . . H15B H 0.1262 0.2669 -0.1621 0.053 Uiso 1 1 calc R . . H15C H 0.0235 0.2925 -0.2137 0.053 Uiso 1 1 calc R . . C16 C 0.47434(15) 0.41940(12) -0.05730(12) 0.0282(4) Uani 1 1 d . . . H16A H 0.4234 0.4306 -0.0992 0.042 Uiso 1 1 calc R . . H16B H 0.5326 0.4418 -0.0834 0.042 Uiso 1 1 calc R . . H16C H 0.4444 0.4504 -0.0180 0.042 Uiso 1 1 calc R . . C17 C 0.57864(16) 0.23317(15) -0.07726(14) 0.0345(5) Uani 1 1 d . . . H17A H 0.5899 0.1682 -0.0509 0.052 Uiso 1 1 calc R . . H17B H 0.6438 0.2474 -0.0951 0.052 Uiso 1 1 calc R . . H17C H 0.5332 0.2527 -0.1248 0.052 Uiso 1 1 calc R . . C18 C 0.62262(14) 0.27486(13) 0.07829(12) 0.0266(4) Uani 1 1 d . . . C19 C 0.69054(16) 0.17638(15) 0.10388(17) 0.0467(6) Uani 1 1 d . . . H19A H 0.7187 0.1617 0.0548 0.070 Uiso 1 1 calc R . . H19B H 0.6493 0.1351 0.1331 0.070 Uiso 1 1 calc R . . H19C H 0.7462 0.1707 0.1397 0.070 Uiso 1 1 calc R . . C20 C 0.57408(18) 0.2960(2) 0.15613(14) 0.0534(7) Uani 1 1 d . . . H20A H 0.5348 0.2527 0.1843 0.080 Uiso 1 1 calc R . . H20B H 0.5290 0.3568 0.1402 0.080 Uiso 1 1 calc R . . H20C H 0.6278 0.2920 0.1929 0.080 Uiso 1 1 calc R . . C21 C 0.69476(15) 0.33806(14) 0.03976(14) 0.0343(5) Uani 1 1 d . . . H21A H 0.7511 0.3241 0.0779 0.052 Uiso 1 1 calc R . . H21B H 0.6565 0.4007 0.0290 0.052 Uiso 1 1 calc R . . H21C H 0.7218 0.3288 -0.0117 0.052 Uiso 1 1 calc R . . C22 C 0.47113(13) 0.05533(12) 0.17859(11) 0.0225(4) Uani 1 1 d . . . H22A H 0.5035 -0.0084 0.2048 0.034 Uiso 1 1 calc R . . H22B H 0.4516 0.0848 0.2206 0.034 Uiso 1 1 calc R . . H22C H 0.5189 0.0836 0.1410 0.034 Uiso 1 1 calc R . . C23 C 0.30438(13) 0.02224(11) 0.18687(10) 0.0187(3) Uani 1 1 d . . . C24 C 0.28752(15) -0.05953(12) 0.18626(12) 0.0258(4) Uani 1 1 d . . . H24 H 0.3208 -0.0872 0.1476 0.031 Uiso 1 1 calc R . . C25 C 0.22032(16) -0.10004(14) 0.24403(13) 0.0343(5) Uani 1 1 d . . . H25 H 0.2089 -0.1549 0.2436 0.041 Uiso 1 1 calc R . . C26 C 0.17075(15) -0.06000(15) 0.30166(12) 0.0328(5) Uani 1 1 d . . . H26 H 0.1266 -0.0878 0.3403 0.039 Uiso 1 1 calc R . . C27 C 0.18715(14) 0.02194(14) 0.30152(11) 0.0294(4) Uani 1 1 d . . . H27 H 0.1532 0.0498 0.3399 0.035 Uiso 1 1 calc R . . C28 C 0.25368(14) 0.06281(12) 0.24472(11) 0.0232(4) Uani 1 1 d . . . H28 H 0.2645 0.1178 0.2453 0.028 Uiso 1 1 calc R . . C51 C 0.26430(13) 0.16940(12) 0.44540(11) 0.0200(3) Uani 1 1 d . . . H51A H 0.2280 0.1781 0.3946 0.024 Uiso 1 1 calc R . . H51B H 0.2861 0.1040 0.4741 0.024 Uiso 1 1 calc R . . C52 C 0.36410(13) 0.20554(12) 0.42000(11) 0.0194(3) Uani 1 1 d . . . C53 C 0.34062(14) 0.30397(12) 0.35422(11) 0.0228(4) Uani 1 1 d . . . H53A H 0.4051 0.3128 0.3267 0.027 Uiso 1 1 calc R . . H53B H 0.2940 0.3058 0.3120 0.027 Uiso 1 1 calc R . . C54 C 0.43106(15) 0.14308(13) 0.37383(13) 0.0293(4) Uani 1 1 d . . . H54A H 0.4949 0.1605 0.3579 0.044 Uiso 1 1 calc R . . H54B H 0.3945 0.1489 0.3248 0.044 Uiso 1 1 calc R . . H54C H 0.4458 0.0807 0.4099 0.044 Uiso 1 1 calc R . . C55 C 0.41789(13) 0.20154(11) 0.49740(11) 0.0197(3) Uani 1 1 d . . . C56 C 0.51638(14) 0.14566(13) 0.52428(13) 0.0296(4) Uani 1 1 d . . . H56 H 0.5532 0.1093 0.4934 0.035 Uiso 1 1 calc R . . C57 C 0.55964(15) 0.14400(14) 0.59664(14) 0.0346(5) Uani 1 1 d . . . H57 H 0.6254 0.1067 0.6147 0.041 Uiso 1 1 calc R . . C58 C 0.50412(15) 0.19833(13) 0.64150(12) 0.0306(4) Uani 1 1 d . . . H58 H 0.5314 0.1985 0.6904 0.037 Uiso 1 1 calc R . . C59 C 0.40685(14) 0.25253(12) 0.61217(11) 0.0226(4) Uani 1 1 d . . . H59 H 0.3692 0.2892 0.6425 0.027 Uiso 1 1 calc R . . C60 C 0.05020(15) 0.09075(13) 0.51497(12) 0.0282(4) Uani 1 1 d . . . H60A H 0.0037 0.1375 0.4729 0.042 Uiso 1 1 calc R . . H60B H 0.0115 0.0538 0.5548 0.042 Uiso 1 1 calc R . . H60C H 0.1005 0.0530 0.4892 0.042 Uiso 1 1 calc R . . C61 C 0.02278(14) 0.22502(13) 0.61518(12) 0.0266(4) Uani 1 1 d . . . H61A H 0.0592 0.2555 0.6392 0.040 Uiso 1 1 calc R . . H61B H -0.0158 0.1908 0.6578 0.040 Uiso 1 1 calc R . . H61C H -0.0240 0.2697 0.5721 0.040 Uiso 1 1 calc R . . C62 C 0.19824(14) 0.04922(13) 0.65868(11) 0.0260(4) Uani 1 1 d . . . C63 C 0.12271(17) 0.00401(17) 0.71987(15) 0.0506(7) Uani 1 1 d . . . H63A H 0.0845 -0.0213 0.6918 0.076 Uiso 1 1 calc R . . H63B H 0.0754 0.0490 0.7400 0.076 Uiso 1 1 calc R . . H63C H 0.1610 -0.0439 0.7661 0.076 Uiso 1 1 calc R . . C64 C 0.2737(2) -0.02462(16) 0.62996(16) 0.0535(7) Uani 1 1 d . . . H64A H 0.3041 -0.0752 0.6779 0.080 Uiso 1 1 calc R . . H64B H 0.3273 0.0002 0.5976 0.080 Uiso 1 1 calc R . . H64C H 0.2372 -0.0454 0.5963 0.080 Uiso 1 1 calc R . . C65 C 0.25942(19) 0.08734(17) 0.70567(14) 0.0460(6) Uani 1 1 d . . . H65A H 0.2883 0.0404 0.7563 0.069 Uiso 1 1 calc R . . H65B H 0.2139 0.1383 0.7190 0.069 Uiso 1 1 calc R . . H65C H 0.3144 0.1072 0.6712 0.069 Uiso 1 1 calc R . . C66 C 0.25618(16) 0.56607(13) 0.39090(15) 0.0362(5) Uani 1 1 d . . . H66A H 0.1845 0.5655 0.3912 0.054 Uiso 1 1 calc R . . H66B H 0.2634 0.6264 0.3603 0.054 Uiso 1 1 calc R . . H66C H 0.2806 0.5492 0.4473 0.054 Uiso 1 1 calc R . . C67 C 0.30930(16) 0.52786(15) 0.22399(12) 0.0343(5) Uani 1 1 d . . . H67A H 0.3419 0.4811 0.1996 0.051 Uiso 1 1 calc R . . H67B H 0.3373 0.5801 0.2000 0.051 Uiso 1 1 calc R . . H67C H 0.2359 0.5456 0.2131 0.051 Uiso 1 1 calc R . . C68 C 0.47816(14) 0.46938(12) 0.35639(11) 0.0230(4) Uani 1 1 d . . . C69 C 0.49622(17) 0.56577(14) 0.33514(13) 0.0336(5) Uani 1 1 d . . . H69A H 0.5680 0.5604 0.3443 0.050 Uiso 1 1 calc R . . H69B H 0.4541 0.5973 0.3703 0.050 Uiso 1 1 calc R . . H69C H 0.4778 0.5996 0.2776 0.050 Uiso 1 1 calc R . . C70 C 0.51025(15) 0.41473(14) 0.44771(12) 0.0296(4) Uani 1 1 d . . . H70A H 0.5097 0.3520 0.4586 0.044 Uiso 1 1 calc R . . H70B H 0.4623 0.4402 0.4840 0.044 Uiso 1 1 calc R . . H70C H 0.5788 0.4179 0.4577 0.044 Uiso 1 1 calc R . . C71 C 0.54950(15) 0.42101(15) 0.30039(13) 0.0319(4) Uani 1 1 d . . . H71A H 0.6198 0.4222 0.3073 0.048 Uiso 1 1 calc R . . H71B H 0.5281 0.4520 0.2430 0.048 Uiso 1 1 calc R . . H71C H 0.5452 0.3586 0.3159 0.048 Uiso 1 1 calc R . . C72 C 0.05619(14) 0.47564(12) 0.30031(11) 0.0241(4) Uani 1 1 d . . . H72A H -0.0131 0.5145 0.2911 0.036 Uiso 1 1 calc R . . H72B H 0.0765 0.4541 0.2534 0.036 Uiso 1 1 calc R . . H72C H 0.1029 0.5096 0.3067 0.036 Uiso 1 1 calc R . . C73 C -0.00716(13) 0.34217(11) 0.36701(11) 0.0203(3) Uani 1 1 d . . . C74 C -0.10183(14) 0.34356(13) 0.40595(12) 0.0265(4) Uani 1 1 d . . . H74 H -0.1230 0.3776 0.4422 0.032 Uiso 1 1 calc R . . C75 C -0.16528(16) 0.29389(14) 0.39075(14) 0.0376(5) Uani 1 1 d . . . H75 H -0.2288 0.2946 0.4172 0.045 Uiso 1 1 calc R . . C76 C -0.13443(18) 0.24339(14) 0.33648(15) 0.0423(6) Uani 1 1 d . . . H76 H -0.1775 0.2109 0.3259 0.051 Uiso 1 1 calc R . . C77 C -0.03996(19) 0.24154(14) 0.29835(14) 0.0382(5) Uani 1 1 d . . . H77 H -0.0189 0.2073 0.2622 0.046 Uiso 1 1 calc R . . C78 C 0.02395(16) 0.29036(12) 0.31335(12) 0.0277(4) Uani 1 1 d . . . H78 H 0.0880 0.2886 0.2875 0.033 Uiso 1 1 calc R . . Cl1 Cl 0.37884(4) 0.15046(3) -0.13661(3) 0.02558(10) Uani 1 1 d . . . Cl51 Cl 0.18602(4) 0.40397(3) 0.59873(3) 0.02813(10) Uani 1 1 d . . . H4 H 0.4474(17) -0.0095(16) 0.0642(14) 0.032(6) Uiso 1 1 d . . . H54 H -0.0036(18) 0.4625(16) 0.4476(14) 0.032(6) Uiso 1 1 d . . . N1 N 0.18232(10) 0.20135(9) 0.02991(9) 0.0173(3) Uani 1 1 d . . . N2 N 0.41246(10) 0.25213(9) 0.04055(8) 0.0173(3) Uani 1 1 d . . . N3 N 0.26612(10) 0.33444(9) -0.08872(8) 0.0174(3) Uani 1 1 d . . . N4 N 0.40175(12) 0.03885(10) 0.05711(9) 0.0198(3) Uani 1 1 d . . . N5 N 0.37787(11) 0.06468(9) 0.13152(8) 0.0175(3) Uani 1 1 d . . . N51 N 0.19027(10) 0.21099(9) 0.49857(8) 0.0165(3) Uani 1 1 d . . . N52 N 0.29511(11) 0.38239(9) 0.38422(9) 0.0184(3) Uani 1 1 d . . . N53 N 0.36373(11) 0.25489(9) 0.54170(8) 0.0173(3) Uani 1 1 d . . . N54 N 0.04518(12) 0.42287(10) 0.45099(9) 0.0200(3) Uani 1 1 d . . . N55 N 0.05963(11) 0.39665(9) 0.37689(8) 0.0179(3) Uani 1 1 d . . . Si1 Si 0.08622(4) 0.15738(3) 0.00704(3) 0.01875(10) Uani 1 1 d . . . Si2 Si 0.51854(4) 0.29351(3) -0.00151(3) 0.01758(10) Uani 1 1 d . . . Si51 Si 0.11802(3) 0.14527(3) 0.56926(3) 0.01715(9) Uani 1 1 d . . . Si52 Si 0.33437(4) 0.48233(3) 0.34003(3) 0.02034(10) Uani 1 1 d . . . Zr1 Zr 0.336160(12) 0.176352(10) -0.000739(9) 0.01483(5) Uani 1 1 d . . . Zr51 Zr 0.194314(11) 0.344016(10) 0.479472(9) 0.01428(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0168(8) 0.0214(8) 0.0190(8) -0.0076(7) 0.0027(6) -0.0051(7) C2 0.0169(8) 0.0172(8) 0.0184(8) -0.0069(7) 0.0002(6) -0.0017(6) C3 0.0177(8) 0.0236(9) 0.0178(8) -0.0090(7) 0.0005(6) -0.0049(7) C4 0.0252(9) 0.0257(9) 0.0276(9) -0.0150(8) 0.0035(7) -0.0040(7) C5 0.0159(8) 0.0179(8) 0.0200(8) -0.0059(7) -0.0016(6) -0.0051(6) C6 0.0230(9) 0.0179(8) 0.0300(10) -0.0079(7) -0.0017(7) -0.0016(7) C7 0.0280(10) 0.0191(9) 0.0312(10) 0.0013(8) -0.0080(8) -0.0050(7) C8 0.0274(9) 0.0270(9) 0.0201(9) -0.0007(7) -0.0056(7) -0.0094(8) C9 0.0228(9) 0.0246(9) 0.0174(8) -0.0060(7) 0.0004(7) -0.0078(7) C10 0.0321(11) 0.0243(10) 0.0407(12) -0.0140(9) -0.0060(9) -0.0054(8) C11 0.0271(10) 0.0401(11) 0.0242(9) -0.0039(8) 0.0012(8) -0.0165(9) C12 0.0200(9) 0.0261(9) 0.0251(9) -0.0071(7) -0.0030(7) -0.0064(7) C13 0.0304(10) 0.0265(10) 0.0365(11) -0.0058(9) -0.0128(9) -0.0020(8) C14 0.0275(10) 0.0365(11) 0.0389(11) -0.0076(9) -0.0106(9) -0.0108(9) C15 0.0372(11) 0.0454(12) 0.0216(9) -0.0069(9) -0.0028(8) -0.0127(10) C16 0.0259(10) 0.0217(9) 0.0328(10) -0.0005(8) -0.0025(8) -0.0090(8) C17 0.0336(11) 0.0403(12) 0.0395(12) -0.0233(10) 0.0161(9) -0.0167(9) C18 0.0184(9) 0.0295(10) 0.0295(10) -0.0049(8) -0.0022(7) -0.0071(7) C19 0.0231(10) 0.0327(11) 0.0657(16) 0.0127(11) -0.0120(10) -0.0089(9) C20 0.0320(12) 0.105(2) 0.0316(12) -0.0283(14) -0.0046(9) -0.0209(13) C21 0.0225(10) 0.0299(10) 0.0507(13) -0.0102(9) -0.0065(9) -0.0084(8) C22 0.0194(8) 0.0240(9) 0.0225(9) -0.0052(7) -0.0028(7) -0.0045(7) C23 0.0172(8) 0.0189(8) 0.0164(8) -0.0023(7) -0.0016(6) -0.0025(6) C24 0.0286(10) 0.0240(9) 0.0259(9) -0.0082(8) 0.0014(7) -0.0082(8) C25 0.0379(11) 0.0322(11) 0.0345(11) -0.0045(9) -0.0016(9) -0.0191(9) C26 0.0223(9) 0.0444(12) 0.0248(10) 0.0010(9) 0.0014(8) -0.0129(9) C27 0.0228(9) 0.0388(11) 0.0194(9) -0.0058(8) 0.0007(7) -0.0002(8) C28 0.0232(9) 0.0236(9) 0.0205(9) -0.0069(7) -0.0017(7) -0.0015(7) C51 0.0227(9) 0.0186(8) 0.0209(8) -0.0084(7) 0.0027(7) -0.0069(7) C52 0.0180(8) 0.0209(8) 0.0206(8) -0.0095(7) 0.0035(7) -0.0046(7) C53 0.0289(9) 0.0240(9) 0.0183(8) -0.0082(7) 0.0052(7) -0.0110(7) C54 0.0266(10) 0.0318(10) 0.0337(10) -0.0192(9) 0.0083(8) -0.0056(8) C55 0.0178(8) 0.0178(8) 0.0220(9) -0.0048(7) 0.0013(7) -0.0043(6) C56 0.0216(9) 0.0258(10) 0.0376(11) -0.0110(8) -0.0010(8) 0.0017(7) C57 0.0218(10) 0.0304(10) 0.0435(12) -0.0054(9) -0.0128(9) 0.0021(8) C58 0.0288(10) 0.0302(10) 0.0285(10) -0.0023(8) -0.0127(8) -0.0057(8) C59 0.0240(9) 0.0228(9) 0.0201(8) -0.0041(7) -0.0027(7) -0.0073(7) C60 0.0322(10) 0.0278(10) 0.0270(10) -0.0054(8) -0.0009(8) -0.0157(8) C61 0.0261(9) 0.0268(9) 0.0239(9) -0.0059(8) 0.0058(7) -0.0061(8) C62 0.0212(9) 0.0258(9) 0.0238(9) 0.0017(8) 0.0004(7) -0.0061(7) C63 0.0308(11) 0.0526(15) 0.0411(13) 0.0239(11) -0.0039(10) -0.0129(10) C64 0.0545(15) 0.0328(12) 0.0462(14) 0.0026(11) -0.0021(12) 0.0155(11) C65 0.0471(14) 0.0498(14) 0.0338(12) 0.0029(10) -0.0196(10) -0.0153(11) C66 0.0323(11) 0.0233(10) 0.0539(14) -0.0145(10) 0.0073(10) -0.0077(8) C67 0.0288(10) 0.0409(12) 0.0251(10) 0.0069(9) -0.0053(8) -0.0156(9) C68 0.0233(9) 0.0270(9) 0.0212(9) -0.0058(7) -0.0009(7) -0.0125(7) C69 0.0368(11) 0.0344(11) 0.0331(11) -0.0055(9) -0.0012(9) -0.0213(9) C70 0.0297(10) 0.0352(11) 0.0259(10) -0.0058(8) -0.0034(8) -0.0157(8) C71 0.0237(10) 0.0425(12) 0.0322(11) -0.0135(9) 0.0029(8) -0.0118(9) C72 0.0248(9) 0.0228(9) 0.0218(9) -0.0024(7) -0.0016(7) -0.0066(7) C73 0.0215(8) 0.0163(8) 0.0198(8) -0.0017(7) -0.0073(7) -0.0023(7) C74 0.0215(9) 0.0236(9) 0.0310(10) -0.0041(8) -0.0042(7) -0.0045(7) C75 0.0259(10) 0.0303(11) 0.0487(13) 0.0031(10) -0.0119(9) -0.0103(8) C76 0.0465(13) 0.0260(10) 0.0533(14) -0.0006(10) -0.0290(11) -0.0146(10) C77 0.0561(14) 0.0235(10) 0.0352(11) -0.0088(9) -0.0214(10) -0.0055(9) C78 0.0354(11) 0.0222(9) 0.0237(9) -0.0073(8) -0.0076(8) -0.0022(8) Cl1 0.0311(2) 0.0256(2) 0.0190(2) -0.01134(17) -0.00007(17) -0.00007(18) Cl51 0.0269(2) 0.0322(2) 0.0274(2) -0.01946(19) -0.00565(18) 0.00316(18) N1 0.0171(7) 0.0164(7) 0.0181(7) -0.0053(6) 0.0003(5) -0.0039(5) N2 0.0171(7) 0.0174(7) 0.0174(7) -0.0063(6) 0.0008(5) -0.0036(5) N3 0.0170(7) 0.0184(7) 0.0169(7) -0.0054(6) 0.0002(5) -0.0052(5) N4 0.0221(7) 0.0161(7) 0.0183(7) -0.0072(6) 0.0020(6) 0.0015(6) N5 0.0190(7) 0.0171(7) 0.0154(7) -0.0050(6) 0.0008(5) -0.0035(5) N51 0.0162(7) 0.0162(7) 0.0160(7) -0.0041(5) 0.0010(5) -0.0040(5) N52 0.0186(7) 0.0174(7) 0.0182(7) -0.0046(6) -0.0004(5) -0.0042(6) N53 0.0178(7) 0.0159(7) 0.0177(7) -0.0037(6) -0.0005(5) -0.0052(5) N54 0.0192(7) 0.0202(7) 0.0193(7) -0.0094(6) -0.0017(6) 0.0017(6) N55 0.0185(7) 0.0178(7) 0.0163(7) -0.0052(6) -0.0014(5) -0.0028(6) Si1 0.0177(2) 0.0185(2) 0.0199(2) -0.00479(19) -0.00085(18) -0.00594(18) Si2 0.0172(2) 0.0164(2) 0.0188(2) -0.00534(18) 0.00179(17) -0.00454(18) Si51 0.0161(2) 0.0169(2) 0.0172(2) -0.00301(18) -0.00018(17) -0.00499(17) Si52 0.0202(2) 0.0186(2) 0.0206(2) -0.00220(19) -0.00040(18) -0.00720(18) Zr1 0.01505(8) 0.01430(8) 0.01474(8) -0.00530(6) 0.00056(6) -0.00232(6) Zr51 0.01427(8) 0.01388(8) 0.01443(8) -0.00482(6) -0.00038(6) -0.00258(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 1.467(2) . ? C1 C2 1.570(2) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C5 1.516(2) . ? C2 C4 1.532(2) . ? C2 C3 1.580(2) . ? C3 N2 1.471(2) . ? C3 Zr1 2.8597(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N3 1.354(2) . ? C5 C6 1.390(2) . ? C6 C7 1.386(3) . ? C6 H6 0.9300 . ? C7 C8 1.374(3) . ? C7 H7 0.9300 . ? C8 C9 1.382(3) . ? C8 H8 0.9300 . ? C9 N3 1.345(2) . ? C9 H9 0.9300 . ? C10 Si1 1.867(2) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 Si1 1.870(2) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C15 1.529(3) . ? C12 C13 1.536(3) . ? C12 C14 1.543(3) . ? C12 Si1 1.909(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 Si2 1.870(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 Si2 1.862(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.524(3) . ? C18 C19 1.531(3) . ? C18 C21 1.537(3) . ? C18 Si2 1.907(2) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N5 1.476(2) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.386(2) . ? C23 C28 1.387(2) . ? C23 N5 1.450(2) . ? C24 C25 1.395(3) . ? C24 H24 0.9300 . ? C25 C26 1.375(3) . ? C25 H25 0.9300 . ? C26 C27 1.382(3) . ? C26 H26 0.9300 . ? C27 C28 1.383(3) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C51 N51 1.465(2) . ? C51 C52 1.567(2) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C55 1.515(2) . ? C52 C54 1.531(2) . ? C52 C53 1.567(2) . ? C53 N52 1.472(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N53 1.351(2) . ? C55 C56 1.392(3) . ? C56 C57 1.382(3) . ? C56 H56 0.9300 . ? C57 C58 1.375(3) . ? C57 H57 0.9300 . ? C58 C59 1.380(3) . ? C58 H58 0.9300 . ? C59 N53 1.347(2) . ? C59 H59 0.9300 . ? C60 Si51 1.8661(19) . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 Si51 1.870(2) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C64 1.524(3) . ? C62 C65 1.531(3) . ? C62 C63 1.535(3) . ? C62 Si51 1.909(2) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 Si52 1.873(2) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 Si52 1.880(2) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C70 1.534(3) . ? C68 C71 1.538(3) . ? C68 C69 1.542(3) . ? C68 Si52 1.9079(18) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 N55 1.478(2) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.382(3) . ? C73 C78 1.392(3) . ? C73 N55 1.451(2) . ? C74 C75 1.390(3) . ? C74 H74 0.9300 . ? C75 C76 1.385(3) . ? C75 H75 0.9300 . ? C76 C77 1.373(3) . ? C76 H76 0.9300 . ? C77 C78 1.383(3) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? Cl1 Zr1 2.4687(7) . ? Cl51 Zr51 2.4859(7) . ? N1 Si1 1.7364(15) . ? N1 Zr1 2.0499(15) . ? N2 Si2 1.7297(15) . ? N2 Zr1 2.0730(14) . ? N3 Zr1 2.4429(17) . ? N4 N5 1.439(2) . ? N4 Zr1 2.0626(17) . ? N4 H4 0.83(2) . ? N5 Zr1 2.3564(17) . ? N51 Si51 1.7350(15) . ? N51 Zr51 2.0564(14) . ? N52 Si52 1.7278(15) . ? N52 Zr51 2.0648(16) . ? N53 Zr51 2.4348(17) . ? N54 N55 1.432(2) . ? N54 Zr51 2.0517(17) . ? N54 H54 0.77(2) . ? N55 Zr51 2.3796(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 117.38(13) . . ? 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 112.47(14) . . ? C5 C2 C1 109.92(13) . . ? C4 C2 C1 105.45(13) . . ? C5 C2 C3 110.65(14) . . ? C4 C2 C3 104.81(13) . . ? C1 C2 C3 113.39(14) . . ? N2 C3 C2 118.02(13) . . ? N2 C3 Zr1 44.07(7) . . ? C2 C3 Zr1 82.08(9) . . ? N2 C3 H3A 107.8 . . ? C2 C3 H3A 107.8 . . ? Zr1 C3 H3A 148.0 . . ? N2 C3 H3B 107.8 . . ? C2 C3 H3B 107.8 . . ? Zr1 C3 H3B 98.0 . . ? 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 120.86(16) . . ? N3 C5 C2 115.56(14) . . ? C6 C5 C2 123.57(16) . . ? C7 C6 C5 119.74(17) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 119.23(17) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 118.50(17) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? N3 C9 C8 123.09(17) . . ? 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 108.27(17) . . ? C15 C12 C14 108.32(16) . . ? C13 C12 C14 108.67(16) . . ? C15 C12 Si1 110.17(13) . . ? C13 C12 Si1 111.76(13) . . ? C14 C12 Si1 109.57(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 109.1(2) . . ? C20 C18 C21 108.53(18) . . ? C19 C18 C21 106.98(16) . . ? C20 C18 Si2 111.02(13) . . ? C19 C18 Si2 111.39(15) . . ? C21 C18 Si2 109.72(13) . . ? 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 H22A 109.5 . . ? N5 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N5 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 119.42(16) . . ? C24 C23 N5 121.90(16) . . ? C28 C23 N5 118.60(15) . . ? C23 C24 C25 119.56(18) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 120.88(19) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.32(18) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 120.43(18) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 120.38(18) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? N51 C51 C52 117.10(13) . . ? N51 C51 H51A 108.0 . . ? C52 C51 H51A 108.0 . . ? N51 C51 H51B 108.0 . . ? C52 C51 H51B 108.0 . . ? H51A C51 H51B 107.3 . . ? C55 C52 C54 112.50(15) . . ? C55 C52 C51 109.82(14) . . ? C54 C52 C51 105.19(14) . . ? C55 C52 C53 111.60(14) . . ? C54 C52 C53 104.92(14) . . ? C51 C52 C53 112.58(14) . . ? N52 C53 C52 117.95(14) . . ? 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 120.35(16) . . ? N53 C55 C52 116.11(14) . . ? C56 C55 C52 123.53(16) . . ? C57 C56 C55 120.34(18) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C58 C57 C56 119.06(18) . . ? C58 C57 H57 120.5 . . ? C56 C57 H57 120.5 . . ? C57 C58 C59 118.35(18) . . ? C57 C58 H58 120.8 . . ? C59 C58 H58 120.8 . . ? N53 C59 C58 123.23(18) . . ? 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 . . ? C64 C62 C65 108.66(19) . . ? C64 C62 C63 107.97(19) . . ? C65 C62 C63 108.24(19) . . ? C64 C62 Si51 113.21(14) . . ? C65 C62 Si51 110.89(14) . . ? C63 C62 Si51 107.71(13) . . ? 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 . . ? C70 C68 C71 108.07(16) . . ? C70 C68 C69 109.30(15) . . ? C71 C68 C69 107.37(16) . . ? C70 C68 Si52 110.14(13) . . ? C71 C68 Si52 113.44(12) . . ? C69 C68 Si52 108.41(13) . . ? 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 . . ? N55 C72 H72A 109.5 . . ? N55 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N55 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 119.49(17) . . ? C74 C73 N55 122.16(16) . . ? C78 C73 N55 118.27(16) . . ? C73 C74 C75 119.79(19) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C76 C75 C74 120.4(2) . . ? C76 C75 H75 119.8 . . ? C74 C75 H75 119.8 . . ? C77 C76 C75 119.69(19) . . ? C77 C76 H76 120.2 . . ? C75 C76 H76 120.2 . . ? C76 C77 C78 120.3(2) . . ? C76 C77 H77 119.8 . . ? C78 C77 H77 119.8 . . ? C77 C78 C73 120.3(2) . . ? C77 C78 H78 119.9 . . ? C73 C78 H78 119.9 . . ? C1 N1 Si1 119.74(11) . . ? C1 N1 Zr1 111.05(10) . . ? Si1 N1 Zr1 129.05(8) . . ? C3 N2 Si2 119.13(11) . . ? C3 N2 Zr1 106.37(10) . . ? Si2 N2 Zr1 129.15(8) . . ? C9 N3 C5 118.57(15) . . ? C9 N3 Zr1 129.03(12) . . ? C5 N3 Zr1 112.39(11) . . ? N5 N4 Zr1 82.52(9) . . ? N5 N4 H4 113.8(15) . . ? Zr1 N4 H4 154.0(15) . . ? N4 N5 C23 115.57(13) . . ? N4 N5 C22 113.11(13) . . ? C23 N5 C22 110.61(13) . . ? N4 N5 Zr1 60.21(8) . . ? C23 N5 Zr1 124.95(10) . . ? C22 N5 Zr1 121.15(11) . . ? C51 N51 Si51 119.26(11) . . ? C51 N51 Zr51 111.50(10) . . ? Si51 N51 Zr51 129.18(8) . . ? C53 N52 Si52 118.87(11) . . ? C53 N52 Zr51 108.46(10) . . ? Si52 N52 Zr51 132.63(8) . . ? C59 N53 C55 118.68(15) . . ? C59 N53 Zr51 128.62(12) . . ? C55 N53 Zr51 112.70(11) . . ? N55 N54 Zr51 84.16(9) . . ? N55 N54 H54 111.7(17) . . ? Zr51 N54 H54 159.8(17) . . ? N54 N55 C73 116.08(13) . . ? N54 N55 C72 112.36(13) . . ? C73 N55 C72 110.22(13) . . ? N54 N55 Zr51 59.06(8) . . ? C73 N55 Zr51 124.60(10) . . ? C72 N55 Zr51 122.51(11) . . ? N1 Si1 C10 108.46(8) . . ? N1 Si1 C11 109.32(8) . . ? C10 Si1 C11 109.84(10) . . ? N1 Si1 C12 112.26(8) . . ? C10 Si1 C12 107.81(9) . . ? C11 Si1 C12 109.12(9) . . ? N2 Si2 C17 107.51(8) . . ? N2 Si2 C16 109.37(8) . . ? C17 Si2 C16 109.63(10) . . ? N2 Si2 C18 114.54(8) . . ? C17 Si2 C18 107.97(10) . . ? C16 Si2 C18 107.76(9) . . ? N51 Si51 C60 110.24(8) . . ? N51 Si51 C61 106.42(8) . . ? C60 Si51 C61 111.03(9) . . ? N51 Si51 C62 114.03(8) . . ? C60 Si51 C62 107.10(9) . . ? C61 Si51 C62 108.04(9) . . ? N52 Si52 C66 106.13(9) . . ? N52 Si52 C67 110.84(9) . . ? C66 Si52 C67 110.17(11) . . ? N52 Si52 C68 114.18(8) . . ? C66 Si52 C68 108.77(9) . . ? C67 Si52 C68 106.74(9) . . ? N1 Zr1 N4 107.15(7) . . ? N1 Zr1 N2 111.63(6) . . ? N4 Zr1 N2 108.92(6) . . ? N1 Zr1 N5 89.93(6) . . ? N4 Zr1 N5 37.27(6) . . ? N2 Zr1 N5 85.94(6) . . ? N1 Zr1 N3 77.15(6) . . ? N4 Zr1 N3 171.46(5) . . ? N2 Zr1 N3 75.49(5) . . ? N5 Zr1 N3 151.23(5) . . ? N1 Zr1 Cl1 116.44(5) . . ? N4 Zr1 Cl1 88.40(5) . . ? N2 Zr1 Cl1 120.55(5) . . ? N5 Zr1 Cl1 125.60(4) . . ? N3 Zr1 Cl1 83.06(4) . . ? N1 Zr1 C3 82.10(6) . . ? N4 Zr1 C3 118.78(6) . . ? N2 Zr1 C3 29.56(5) . . ? N5 Zr1 C3 84.25(5) . . ? N3 Zr1 C3 68.72(5) . . ? Cl1 Zr1 C3 142.21(4) . . ? N54 Zr51 N51 106.58(6) . . ? N54 Zr51 N52 111.95(6) . . ? N51 Zr51 N52 109.76(6) . . ? N54 Zr51 N55 36.78(6) . . ? N51 Zr51 N55 89.96(6) . . ? N52 Zr51 N55 88.25(5) . . ? N54 Zr51 N53 168.02(5) . . ? N51 Zr51 N53 76.56(6) . . ? N52 Zr51 N53 76.93(6) . . ? N55 Zr51 N53 154.94(5) . . ? N54 Zr51 Cl51 86.56(5) . . ? N51 Zr51 Cl51 121.05(5) . . ? N52 Zr51 Cl51 117.72(4) . . ? N55 Zr51 Cl51 122.95(4) . . ? N53 Zr51 Cl51 82.04(4) . . ? 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 54.23(19) . . . . ? N1 C1 C2 C4 175.69(14) . . . . ? N1 C1 C2 C3 -70.19(18) . . . . ? C5 C2 C3 N2 -44.15(19) . . . . ? C4 C2 C3 N2 -165.63(14) . . . . ? C1 C2 C3 N2 79.88(18) . . . . ? C5 C2 C3 Zr1 -70.55(12) . . . . ? C4 C2 C3 Zr1 167.97(12) . . . . ? C1 C2 C3 Zr1 53.48(12) . . . . ? C4 C2 C5 N3 179.44(14) . . . . ? C1 C2 C5 N3 -63.40(18) . . . . ? C3 C2 C5 N3 62.60(18) . . . . ? C4 C2 C5 C6 -0.8(2) . . . . ? C1 C2 C5 C6 116.38(17) . . . . ? C3 C2 C5 C6 -117.63(18) . . . . ? N3 C5 C6 C7 0.4(3) . . . . ? C2 C5 C6 C7 -179.41(16) . . . . ? C5 C6 C7 C8 0.0(3) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C7 C8 C9 N3 0.1(3) . . . . ? C28 C23 C24 C25 -0.3(3) . . . . ? N5 C23 C24 C25 176.39(16) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 C27 0.7(3) . . . . ? C25 C26 C27 C28 -0.8(3) . . . . ? C26 C27 C28 C23 0.3(3) . . . . ? C24 C23 C28 C27 0.2(3) . . . . ? N5 C23 C28 C27 -176.61(15) . . . . ? N51 C51 C52 C55 52.56(19) . . . . ? N51 C51 C52 C54 173.85(15) . . . . ? N51 C51 C52 C53 -72.45(19) . . . . ? C55 C52 C53 N52 -45.9(2) . . . . ? C54 C52 C53 N52 -168.00(15) . . . . ? C51 C52 C53 N52 78.14(19) . . . . ? C54 C52 C55 N53 179.99(14) . . . . ? C51 C52 C55 N53 -63.22(19) . . . . ? C53 C52 C55 N53 62.35(19) . . . . ? C54 C52 C55 C56 -1.3(2) . . . . ? C51 C52 C55 C56 115.48(19) . . . . ? C53 C52 C55 C56 -118.95(19) . . . . ? N53 C55 C56 C57 0.2(3) . . . . ? C52 C55 C56 C57 -178.49(17) . . . . ? C55 C56 C57 C58 -0.1(3) . . . . ? C56 C57 C58 C59 0.0(3) . . . . ? C57 C58 C59 N53 -0.1(3) . . . . ? C78 C73 C74 C75 -0.5(3) . . . . ? N55 C73 C74 C75 176.50(16) . . . . ? C73 C74 C75 C76 -0.3(3) . . . . ? C74 C75 C76 C77 0.8(3) . . . . ? C75 C76 C77 C78 -0.5(3) . . . . ? C76 C77 C78 C73 -0.3(3) . . . . ? C74 C73 C78 C77 0.8(3) . . . . ? N55 C73 C78 C77 -176.31(16) . . . . ? C2 C1 N1 Si1 -148.40(12) . . . . ? C2 C1 N1 Zr1 27.47(17) . . . . ? C2 C3 N2 Si2 117.19(14) . . . . ? Zr1 C3 N2 Si2 156.47(14) . . . . ? C2 C3 N2 Zr1 -39.28(16) . . . . ? C8 C9 N3 C5 0.3(2) . . . . ? C8 C9 N3 Zr1 -179.00(12) . . . . ? C6 C5 N3 C9 -0.5(2) . . . . ? C2 C5 N3 C9 179.26(14) . . . . ? C6 C5 N3 Zr1 178.91(13) . . . . ? C2 C5 N3 Zr1 -1.31(17) . . . . ? Zr1 N4 N5 C23 117.25(12) . . . . ? Zr1 N4 N5 C22 -113.81(12) . . . . ? C24 C23 N5 N4 22.7(2) . . . . ? C28 C23 N5 N4 -160.52(14) . . . . ? C24 C23 N5 C22 -107.42(18) . . . . ? C28 C23 N5 C22 69.33(19) . . . . ? C24 C23 N5 Zr1 93.01(18) . . . . ? C28 C23 N5 Zr1 -90.24(17) . . . . ? C52 C51 N51 Si51 -148.38(12) . . . . ? C52 C51 N51 Zr51 28.92(17) . . . . ? C52 C53 N52 Si52 142.38(13) . . . . ? C52 C53 N52 Zr51 -35.76(17) . . . . ? C58 C59 N53 C55 0.2(3) . . . . ? C58 C59 N53 Zr51 179.61(13) . . . . ? C56 C55 N53 C59 -0.2(2) . . . . ? C52 C55 N53 C59 178.54(14) . . . . ? C56 C55 N53 Zr51 -179.73(13) . . . . ? C52 C55 N53 Zr51 -0.99(17) . . . . ? Zr51 N54 N55 C73 116.34(12) . . . . ? Zr51 N54 N55 C72 -115.53(12) . . . . ? C74 C73 N55 N54 23.6(2) . . . . ? C78 C73 N55 N54 -159.36(15) . . . . ? C74 C73 N55 C72 -105.53(18) . . . . ? C78 C73 N55 C72 71.47(19) . . . . ? C74 C73 N55 Zr51 92.68(18) . . . . ? C78 C73 N55 Zr51 -90.32(17) . . . . ? C1 N1 Si1 C10 -165.05(13) . . . . ? Zr1 N1 Si1 C10 19.92(13) . . . . ? C1 N1 Si1 C11 -45.30(15) . . . . ? Zr1 N1 Si1 C11 139.67(10) . . . . ? C1 N1 Si1 C12 75.93(14) . . . . ? Zr1 N1 Si1 C12 -99.10(11) . . . . ? C15 C12 Si1 N1 70.33(15) . . . . ? C13 C12 Si1 N1 -50.09(15) . . . . ? C14 C12 Si1 N1 -170.59(13) . . . . ? C15 C12 Si1 C10 -49.07(15) . . . . ? C13 C12 Si1 C10 -169.48(14) . . . . ? C14 C12 Si1 C10 70.01(15) . . . . ? C15 C12 Si1 C11 -168.33(13) . . . . ? C13 C12 Si1 C11 71.26(15) . . . . ? C14 C12 Si1 C11 -49.25(16) . . . . ? C3 N2 Si2 C17 -165.18(13) . . . . ? Zr1 N2 Si2 C17 -14.77(13) . . . . ? C3 N2 Si2 C16 -46.21(14) . . . . ? Zr1 N2 Si2 C16 104.20(11) . . . . ? C3 N2 Si2 C18 74.85(14) . . . . ? Zr1 N2 Si2 C18 -134.74(10) . . . . ? C20 C18 Si2 N2 -42.93(18) . . . . ? C19 C18 Si2 N2 78.84(16) . . . . ? C21 C18 Si2 N2 -162.90(13) . . . . ? C20 C18 Si2 C17 -162.64(17) . . . . ? C19 C18 Si2 C17 -40.87(17) . . . . ? C21 C18 Si2 C17 77.39(16) . . . . ? C20 C18 Si2 C16 79.02(18) . . . . ? C19 C18 Si2 C16 -159.22(14) . . . . ? C21 C18 Si2 C16 -40.95(16) . . . . ? C51 N51 Si51 C60 -52.82(15) . . . . ? Zr51 N51 Si51 C60 130.42(10) . . . . ? C51 N51 Si51 C61 -173.32(12) . . . . ? Zr51 N51 Si51 C61 9.92(12) . . . . ? C51 N51 Si51 C62 67.67(14) . . . . ? Zr51 N51 Si51 C62 -109.08(11) . . . . ? C64 C62 Si51 N51 -66.24(18) . . . . ? C65 C62 Si51 N51 56.19(17) . . . . ? C63 C62 Si51 N51 174.46(15) . . . . ? C64 C62 Si51 C60 55.99(18) . . . . ? C65 C62 Si51 C60 178.43(15) . . . . ? C63 C62 Si51 C60 -63.30(18) . . . . ? C64 C62 Si51 C61 175.67(16) . . . . ? C65 C62 Si51 C61 -61.89(16) . . . . ? C63 C62 Si51 C61 56.37(18) . . . . ? C53 N52 Si52 C66 177.75(13) . . . . ? Zr51 N52 Si52 C66 -4.64(13) . . . . ? C53 N52 Si52 C67 58.14(15) . . . . ? Zr51 N52 Si52 C67 -124.25(12) . . . . ? C53 N52 Si52 C68 -62.44(14) . . . . ? Zr51 N52 Si52 C68 115.17(11) . . . . ? C70 C68 Si52 N52 -45.75(15) . . . . ? C71 C68 Si52 N52 75.53(15) . . . . ? C69 C68 Si52 N52 -165.30(12) . . . . ? C70 C68 Si52 C66 72.55(15) . . . . ? C71 C68 Si52 C66 -166.16(14) . . . . ? C69 C68 Si52 C66 -46.99(15) . . . . ? C70 C68 Si52 C67 -168.60(14) . . . . ? C71 C68 Si52 C67 -47.31(16) . . . . ? C69 C68 Si52 C67 71.86(15) . . . . ? C1 N1 Zr1 N4 121.95(11) . . . . ? Si1 N1 Zr1 N4 -62.67(11) . . . . ? C1 N1 Zr1 N2 2.78(12) . . . . ? Si1 N1 Zr1 N2 178.16(9) . . . . ? C1 N1 Zr1 N5 88.38(11) . . . . ? Si1 N1 Zr1 N5 -96.24(10) . . . . ? C1 N1 Zr1 N3 -65.69(11) . . . . ? Si1 N1 Zr1 N3 109.69(10) . . . . ? C1 N1 Zr1 Cl1 -141.11(9) . . . . ? Si1 N1 Zr1 Cl1 34.27(11) . . . . ? C1 N1 Zr1 C3 4.18(10) . . . . ? Si1 N1 Zr1 C3 179.56(10) . . . . ? N5 N4 Zr1 N1 -65.95(10) . . . . ? N5 N4 Zr1 N2 54.96(10) . . . . ? N5 N4 Zr1 N3 174.9(3) . . . . ? N5 N4 Zr1 Cl1 176.82(8) . . . . ? N5 N4 Zr1 C3 24.36(10) . . . . ? C3 N2 Zr1 N1 2.82(11) . . . . ? Si2 N2 Zr1 N1 -150.46(9) . . . . ? C3 N2 Zr1 N4 -115.30(11) . . . . ? Si2 N2 Zr1 N4 91.42(10) . . . . ? C3 N2 Zr1 N5 -85.50(11) . . . . ? Si2 N2 Zr1 N5 121.22(10) . . . . ? C3 N2 Zr1 N3 72.34(10) . . . . ? Si2 N2 Zr1 N3 -80.94(10) . . . . ? C3 N2 Zr1 Cl1 145.03(9) . . . . ? Si2 N2 Zr1 Cl1 -8.25(11) . . . . ? Si2 N2 Zr1 C3 -153.28(17) . . . . ? N4 N5 Zr1 N1 119.24(9) . . . . ? C23 N5 Zr1 N1 17.31(13) . . . . ? C22 N5 Zr1 N1 -140.24(12) . . . . ? C23 N5 Zr1 N4 -101.93(15) . . . . ? C22 N5 Zr1 N4 100.52(15) . . . . ? N4 N5 Zr1 N2 -129.07(9) . . . . ? C23 N5 Zr1 N2 129.00(13) . . . . ? C22 N5 Zr1 N2 -28.55(12) . . . . ? N4 N5 Zr1 N3 -178.43(10) . . . . ? C23 N5 Zr1 N3 79.65(16) . . . . ? C22 N5 Zr1 N3 -77.91(16) . . . . ? N4 N5 Zr1 Cl1 -3.91(10) . . . . ? C23 N5 Zr1 Cl1 -105.84(12) . . . . ? C22 N5 Zr1 Cl1 96.61(12) . . . . ? N4 N5 Zr1 C3 -158.69(9) . . . . ? C23 N5 Zr1 C3 99.38(13) . . . . ? C22 N5 Zr1 C3 -58.17(12) . . . . ? C9 N3 Zr1 N1 -122.52(15) . . . . ? C5 N3 Zr1 N1 58.13(11) . . . . ? C9 N3 Zr1 N4 -1.4(4) . . . . ? C5 N3 Zr1 N4 179(17) . . . . ? C9 N3 Zr1 N2 120.76(15) . . . . ? C5 N3 Zr1 N2 -58.59(11) . . . . ? C9 N3 Zr1 N5 172.19(12) . . . . ? C5 N3 Zr1 N5 -7.16(17) . . . . ? C9 N3 Zr1 Cl1 -3.32(13) . . . . ? C5 N3 Zr1 Cl1 177.33(11) . . . . ? C9 N3 Zr1 C3 151.06(15) . . . . ? C5 N3 Zr1 C3 -28.29(10) . . . . ? N2 C3 Zr1 N1 -177.35(11) . . . . ? C2 C3 Zr1 N1 -31.71(9) . . . . ? N2 C3 Zr1 N4 77.37(12) . . . . ? C2 C3 Zr1 N4 -136.98(9) . . . . ? C2 C3 Zr1 N2 145.64(15) . . . . ? N2 C3 Zr1 N5 91.91(11) . . . . ? C2 C3 Zr1 N5 -122.45(10) . . . . ? N2 C3 Zr1 N3 -98.13(11) . . . . ? C2 C3 Zr1 N3 47.51(9) . . . . ? N2 C3 Zr1 Cl1 -53.67(12) . . . . ? C2 C3 Zr1 Cl1 91.98(10) . . . . ? N55 N54 Zr51 N51 -66.47(10) . . . . ? N55 N54 Zr51 N52 53.55(10) . . . . ? N55 N54 Zr51 N53 -170.0(2) . . . . ? N55 N54 Zr51 Cl51 172.12(8) . . . . ? C51 N51 Zr51 N54 125.41(11) . . . . ? Si51 N51 Zr51 N54 -57.63(11) . . . . ? C51 N51 Zr51 N52 3.99(12) . . . . ? Si51 N51 Zr51 N52 -179.06(9) . . . . ? C51 N51 Zr51 N55 92.11(11) . . . . ? Si51 N51 Zr51 N55 -90.93(10) . . . . ? C51 N51 Zr51 N53 -66.57(11) . . . . ? Si51 N51 Zr51 N53 110.39(10) . . . . ? C51 N51 Zr51 Cl51 -138.50(10) . . . . ? Si51 N51 Zr51 Cl51 38.46(11) . . . . ? C53 N52 Zr51 N54 -118.98(11) . . . . ? Si52 N52 Zr51 N54 63.23(12) . . . . ? C53 N52 Zr51 N51 -0.84(12) . . . . ? Si52 N52 Zr51 N51 -178.63(9) . . . . ? C53 N52 Zr51 N55 -90.17(11) . . . . ? Si52 N52 Zr51 N55 92.04(11) . . . . ? C53 N52 Zr51 N53 69.47(11) . . . . ? Si52 N52 Zr51 N53 -108.32(11) . . . . ? C53 N52 Zr51 Cl51 143.05(10) . . . . ? Si52 N52 Zr51 Cl51 -34.74(12) . . . . ? C73 N55 Zr51 N54 -102.08(16) . . . . ? C72 N55 Zr51 N54 98.28(15) . . . . ? N54 N55 Zr51 N51 118.51(9) . . . . ? C73 N55 Zr51 N51 16.43(13) . . . . ? C72 N55 Zr51 N51 -143.21(13) . . . . ? N54 N55 Zr51 N52 -131.71(9) . . . . ? C73 N55 Zr51 N52 126.21(13) . . . . ? C72 N55 Zr51 N52 -33.44(13) . . . . ? N54 N55 Zr51 N53 175.14(11) . . . . ? C73 N55 Zr51 N53 73.06(17) . . . . ? C72 N55 Zr51 N53 -86.59(16) . . . . ? N54 N55 Zr51 Cl51 -9.39(10) . . . . ? C73 N55 Zr51 Cl51 -111.47(12) . . . . ? C72 N55 Zr51 Cl51 88.89(13) . . . . ? C59 N53 Zr51 N54 -15.2(3) . . . . ? C55 N53 Zr51 N54 164.3(2) . . . . ? C59 N53 Zr51 N51 -121.89(15) . . . . ? C55 N53 Zr51 N51 57.59(11) . . . . ? C59 N53 Zr51 N52 123.76(14) . . . . ? C55 N53 Zr51 N52 -56.77(11) . . . . ? C59 N53 Zr51 N55 178.95(13) . . . . ? C55 N53 Zr51 N55 -1.57(18) . . . . ? C59 N53 Zr51 Cl51 2.79(13) . . . . ? C55 N53 Zr51 Cl51 -177.74(11) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.76 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.365 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.114 _audit_block_code ga_hh27 _audit_block_refno 636 _chemical_absolute_configuration ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'