# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cun Wang' _publ_contact_author_email 'WANG CUN@ICES.A-STAR.EDU.SG' _publ_section_title ; The Amido-Bridged Zirconocene's Reactivity and Catalytic Behavior for Ethylene Polymerization ; loop_ _publ_author_name 'Cun Wang.' 'Srinivasulu Aitipamula' 'Jacob Chacko' 'He-Kuan Luo.' 'Ludger P. Stubbs' ; Xiang-Jie Tan ; 'Boon Ying Tay.' 'M.van Meurs' 'Pui Kwan Wong.' 'Suming Ye.' # Attachment 'shelxs.cif' data_CUN106 _database_code_depnum_ccdc_archive 'CCDC 707932' _audit_creation_method 'by Crystalclear-SM 1.4.0 rs' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H25 B F15 N Si2 Zr' _chemical_formula_weight 878.75 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.245(2) _cell_length_b 13.098(3) _cell_length_c 13.383(3) _cell_angle_alpha 77.57(3) _cell_angle_beta 67.01(3) _cell_angle_gamma 74.56(3) _cell_volume 1735.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180.1500 _cell_measurement_reflns_used 4608 _cell_measurement_theta_min 2.0089 _cell_measurement_theta_max 31.0675 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9225 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180.1500 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn70 (2*2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24966 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8511 _reflns_number_gt 7731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystalclear (Rigaku Inc., 2007)' _computing_cell_refinement 'Crystalclear (Rigaku Inc., 2007)' _computing_data_reduction 'Crystalclear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.9378P] 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 8511 _refine_ls_number_parameters 570 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.004 _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 F10 F 0.3034(3) -0.06656(17) 0.2328(2) 0.0726(7) Uani 1 1 d . . . Zr1 Zr 0.47042(2) 0.17804(2) 0.23462(2) 0.03250(10) Uani 1 1 d . . . Si1 Si 0.44178(9) 0.42084(7) 0.20181(9) 0.0472(2) Uani 1 1 d . . . Si2 Si 0.36897(10) 0.28153(8) 0.44454(8) 0.0471(2) Uani 1 1 d . . . F6 F -0.07718(18) 0.10000(15) 0.1425(2) 0.0546(5) Uani 1 1 d . . . F11 F -0.07980(18) 0.33532(16) 0.13404(17) 0.0513(5) Uani 1 1 d . . . F15 F 0.33711(18) 0.10794(15) -0.00676(16) 0.0479(4) Uani 1 1 d . . . F1 F 0.0788(2) 0.36639(15) 0.24013(17) 0.0514(5) Uani 1 1 d . . . N1 N 0.3937(2) 0.3199(2) 0.3069(2) 0.0409(5) Uani 1 1 d . . . F5 F -0.0964(2) 0.05255(19) 0.38819(18) 0.0663(6) Uani 1 1 d . . . F7 F -0.10201(19) -0.09039(17) 0.1220(2) 0.0582(5) Uani 1 1 d . . . F12 F -0.0424(2) 0.44495(16) -0.0616(2) 0.0633(6) Uani 1 1 d . . . F2 F -0.0977(3) 0.46074(18) 0.4101(2) 0.0708(6) Uani 1 1 d . . . C21 C 0.0014(3) 0.2045(2) 0.3022(2) 0.0386(6) Uani 1 1 d . . . F14 F 0.3725(2) 0.2214(2) -0.20226(17) 0.0682(6) Uani 1 1 d . . . F8 F 0.0630(2) -0.27024(16) 0.1706(2) 0.0628(6) Uani 1 1 d . . . C27 C 0.1312(3) 0.2199(2) 0.0781(2) 0.0353(6) Uani 1 1 d . . . C32 C 0.0371(3) 0.3052(2) 0.0550(3) 0.0396(6) Uani 1 1 d . . . C15 C 0.1121(3) 0.0289(2) 0.1914(2) 0.0372(6) Uani 1 1 d . . . C28 C 0.2410(3) 0.1949(2) -0.0146(3) 0.0398(6) Uani 1 1 d . . . F9 F 0.2665(3) -0.25348(17) 0.2251(3) 0.0844(9) Uani 1 1 d . . . C33 C 0.2569(3) 0.1489(3) 0.2234(3) 0.0385(6) Uani 1 1 d . . . F13 F 0.1847(3) 0.3931(2) -0.23324(18) 0.0749(7) Uani 1 1 d . . . C11 C 0.3990(3) 0.0622(3) 0.4142(2) 0.0409(6) Uani 1 1 d . . . C10 C 0.4585(3) 0.1397(3) 0.4253(3) 0.0448(7) Uani 1 1 d . . . C2 C 0.4893(3) 0.2739(3) 0.0485(3) 0.0436(7) Uani 1 1 d . . . B1 B 0.1224(3) 0.1497(3) 0.1982(3) 0.0352(6) Uani 1 1 d . . . C5 C 0.6594(3) 0.2524(3) 0.1067(3) 0.0449(7) Uani 1 1 d . . . C19 C -0.0039(3) -0.0836(3) 0.1531(3) 0.0412(6) Uani 1 1 d . . . C20 C 0.0133(3) 0.0141(2) 0.1616(3) 0.0384(6) Uani 1 1 d . . . C30 C 0.1675(4) 0.3375(3) -0.1334(3) 0.0496(8) Uani 1 1 d . . . C12 C 0.4934(3) -0.0082(3) 0.3412(3) 0.0441(7) Uani 1 1 d . . . F3 F -0.2806(3) 0.3572(3) 0.5671(2) 0.0892(9) Uani 1 1 d . . . C18 C 0.0791(3) -0.1749(3) 0.1776(3) 0.0449(7) Uani 1 1 d . . . C4 C 0.6739(3) 0.1580(3) 0.0644(3) 0.0470(7) Uani 1 1 d . . . C1 C 0.5445(3) 0.3264(3) 0.0971(3) 0.0432(7) Uani 1 1 d . . . C29 C 0.2619(3) 0.2515(3) -0.1174(3) 0.0480(7) Uani 1 1 d . . . C3 C 0.5678(3) 0.1710(3) 0.0293(3) 0.0460(7) Uani 1 1 d . . . C14 C 0.5936(3) 0.1139(3) 0.3576(3) 0.0469(7) Uani 1 1 d . . . C26 C -0.0064(3) 0.3079(3) 0.3160(3) 0.0437(7) Uani 1 1 d . . . C25 C -0.0988(4) 0.3604(3) 0.4032(3) 0.0515(8) Uani 1 1 d . . . C16 C 0.1954(3) -0.0658(3) 0.2104(3) 0.0466(7) Uani 1 1 d . . . C22 C -0.0920(3) 0.1554(3) 0.3866(3) 0.0495(8) Uani 1 1 d . . . C31 C 0.0541(4) 0.3635(2) -0.0473(3) 0.0481(8) Uani 1 1 d . . . F4 F -0.2751(3) 0.1517(3) 0.5516(2) 0.0995(10) Uani 1 1 d . . . C13 C 0.6150(3) 0.0234(3) 0.3073(3) 0.0477(7) Uani 1 1 d . . . C17 C 0.1805(4) -0.1658(3) 0.2054(3) 0.0524(8) Uani 1 1 d . . . C23 C -0.1864(4) 0.2045(4) 0.4745(3) 0.0627(10) Uani 1 1 d . . . C6 C 0.3029(5) 0.5092(3) 0.1657(5) 0.0669(12) Uani 1 1 d . . . C9 C 0.1933(5) 0.2849(5) 0.5308(4) 0.0689(12) Uani 1 1 d . . . C7 C 0.5466(5) 0.4967(4) 0.2223(5) 0.0717(12) Uani 1 1 d . . . C8 C 0.4485(6) 0.3529(5) 0.4987(5) 0.0735(13) Uani 1 1 d . . . C24 C -0.1896(4) 0.3073(4) 0.4833(3) 0.0621(10) Uani 1 1 d . . . H10 H 0.482(4) -0.070(3) 0.311(3) 0.053(10) Uiso 1 1 d . . . H7 H 0.718(4) 0.271(3) 0.135(3) 0.050(10) Uiso 1 1 d . . . H5 H 0.561(4) 0.119(3) -0.003(3) 0.049(10) Uiso 1 1 d . . . H11 H 0.314(3) 0.062(3) 0.443(3) 0.040(9) Uiso 1 1 d . . . H6 H 0.745(4) 0.098(3) 0.058(3) 0.046(9) Uiso 1 1 d . . . H1 H 0.243(4) 0.113(3) 0.300(3) 0.052(10) Uiso 1 1 d . . . H4 H 0.410(4) 0.301(3) 0.035(3) 0.058(11) Uiso 1 1 d . . . H9 H 0.700(4) -0.016(3) 0.252(4) 0.069(12) Uiso 1 1 d . . . H2 H 0.260(3) 0.220(3) 0.222(3) 0.044(9) Uiso 1 1 d . . . H3 H 0.335(3) 0.115(3) 0.172(3) 0.041(9) Uiso 1 1 d . . . H8 H 0.667(4) 0.161(3) 0.335(3) 0.060(11) Uiso 1 1 d . . . H17 H 0.338(5) 0.560(4) 0.113(4) 0.093(16) Uiso 1 1 d . . . H16 H 0.251(6) 0.467(4) 0.149(5) 0.102(18) Uiso 1 1 d . . . H15 H 0.246(6) 0.544(4) 0.233(5) 0.101(19) Uiso 1 1 d . . . H13 H 0.146(5) 0.237(4) 0.507(4) 0.099(17) Uiso 1 1 d . . . H14 H 0.151(7) 0.343(6) 0.521(6) 0.13(3) Uiso 1 1 d . . . H12 H 0.176(7) 0.264(5) 0.607(6) 0.14(3) Uiso 1 1 d . . . H21 H 0.623(4) 0.448(3) 0.239(3) 0.058(12) Uiso 1 1 d . . . H23 H 0.565(5) 0.551(4) 0.165(4) 0.076(14) Uiso 1 1 d . . . H22 H 0.513(6) 0.530(5) 0.281(5) 0.12(2) Uiso 1 1 d . . . H18 H 0.542(6) 0.341(4) 0.455(4) 0.088(17) Uiso 1 1 d . . . H20 H 0.413(6) 0.428(5) 0.495(5) 0.11(2) Uiso 1 1 d . . . H19 H 0.442(6) 0.322(4) 0.571(5) 0.106(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F10 0.0852(16) 0.0465(12) 0.121(2) 0.0048(12) -0.0806(16) -0.0148(11) Zr1 0.03026(15) 0.03416(17) 0.03501(15) -0.00319(11) -0.01330(11) -0.00787(11) Si1 0.0439(5) 0.0355(5) 0.0638(6) -0.0001(4) -0.0190(4) -0.0158(4) Si2 0.0513(5) 0.0508(5) 0.0437(5) -0.0152(4) -0.0148(4) -0.0133(4) F6 0.0376(9) 0.0434(10) 0.0945(16) -0.0188(10) -0.0345(10) -0.0021(8) F11 0.0398(9) 0.0559(12) 0.0598(11) -0.0116(9) -0.0227(8) -0.0012(8) F15 0.0440(10) 0.0489(11) 0.0511(10) -0.0157(8) -0.0177(8) -0.0009(8) F1 0.0543(11) 0.0421(10) 0.0580(11) -0.0079(9) -0.0156(9) -0.0152(9) N1 0.0386(12) 0.0381(13) 0.0492(14) -0.0084(11) -0.0166(11) -0.0088(10) F5 0.0803(15) 0.0715(15) 0.0512(11) -0.0066(10) -0.0058(10) -0.0498(13) F7 0.0435(10) 0.0564(12) 0.0915(16) -0.0286(11) -0.0316(10) -0.0101(9) F12 0.0847(16) 0.0449(11) 0.0759(14) -0.0036(10) -0.0553(13) -0.0002(11) F2 0.0870(17) 0.0552(13) 0.0708(15) -0.0298(11) -0.0256(13) -0.0013(12) C21 0.0359(14) 0.0443(16) 0.0404(14) -0.0080(12) -0.0142(11) -0.0126(12) F14 0.0735(15) 0.0816(16) 0.0401(10) -0.0143(10) -0.0053(10) -0.0180(12) F8 0.0719(14) 0.0380(10) 0.0934(17) -0.0141(11) -0.0384(13) -0.0167(10) C27 0.0364(13) 0.0347(14) 0.0417(14) -0.0073(11) -0.0183(11) -0.0096(11) C32 0.0401(14) 0.0391(15) 0.0465(15) -0.0088(12) -0.0208(12) -0.0080(12) C15 0.0391(14) 0.0381(15) 0.0400(14) -0.0030(11) -0.0160(11) -0.0153(12) C28 0.0436(15) 0.0395(15) 0.0440(15) -0.0080(12) -0.0205(12) -0.0114(12) F9 0.112(2) 0.0372(11) 0.140(3) 0.0073(13) -0.093(2) -0.0125(12) C33 0.0378(14) 0.0380(16) 0.0443(15) -0.0048(13) -0.0177(12) -0.0103(12) F13 0.117(2) 0.0670(15) 0.0475(11) 0.0118(10) -0.0393(13) -0.0289(14) C11 0.0417(15) 0.0401(16) 0.0382(14) 0.0015(12) -0.0164(12) -0.0055(13) C10 0.0508(17) 0.0497(18) 0.0374(14) -0.0014(13) -0.0211(13) -0.0107(14) C2 0.0431(16) 0.0515(18) 0.0392(15) 0.0063(13) -0.0184(12) -0.0180(14) B1 0.0357(15) 0.0364(16) 0.0391(15) -0.0024(12) -0.0164(12) -0.0132(13) C5 0.0357(14) 0.059(2) 0.0430(15) -0.0016(14) -0.0128(12) -0.0196(14) C19 0.0343(14) 0.0441(16) 0.0515(16) -0.0151(13) -0.0139(12) -0.0126(12) C20 0.0321(13) 0.0397(15) 0.0466(15) -0.0099(12) -0.0150(11) -0.0072(11) C30 0.073(2) 0.0461(18) 0.0407(16) 0.0013(13) -0.0281(15) -0.0216(16) C12 0.0451(16) 0.0380(16) 0.0470(16) 0.0017(13) -0.0205(13) -0.0041(13) F3 0.0815(17) 0.119(2) 0.0582(14) -0.0463(15) -0.0002(12) -0.0157(16) C18 0.0522(17) 0.0382(16) 0.0505(17) -0.0071(13) -0.0180(14) -0.0185(14) C4 0.0326(14) 0.062(2) 0.0433(16) -0.0095(15) -0.0079(12) -0.0109(14) C1 0.0391(15) 0.0464(17) 0.0451(16) 0.0069(13) -0.0152(12) -0.0200(13) C29 0.0565(19) 0.054(2) 0.0394(15) -0.0099(14) -0.0155(14) -0.0205(16) C3 0.0409(15) 0.061(2) 0.0369(15) -0.0102(14) -0.0095(12) -0.0157(15) C14 0.0433(16) 0.0563(19) 0.0475(17) 0.0011(14) -0.0263(13) -0.0108(14) C26 0.0409(15) 0.0486(18) 0.0433(16) -0.0055(13) -0.0158(12) -0.0109(13) C25 0.0538(19) 0.055(2) 0.0514(18) -0.0168(16) -0.0225(15) -0.0054(16) C16 0.0516(18) 0.0426(17) 0.0582(19) 0.0029(14) -0.0335(15) -0.0159(14) C22 0.0487(17) 0.064(2) 0.0424(16) -0.0094(15) -0.0104(13) -0.0277(16) C31 0.068(2) 0.0337(15) 0.0581(19) -0.0040(14) -0.0411(17) -0.0080(15) F4 0.103(2) 0.136(3) 0.0535(14) -0.0266(15) 0.0188(13) -0.074(2) C13 0.0428(16) 0.0474(18) 0.0491(17) -0.0002(14) -0.0206(13) -0.0011(14) C17 0.067(2) 0.0355(16) 0.065(2) 0.0023(15) -0.0383(18) -0.0112(15) C23 0.059(2) 0.089(3) 0.0408(17) -0.0120(18) -0.0023(15) -0.036(2) C6 0.061(2) 0.0376(19) 0.093(3) 0.016(2) -0.027(2) -0.0148(18) C9 0.064(3) 0.071(3) 0.061(2) -0.025(2) 0.0012(19) -0.017(2) C7 0.070(3) 0.061(3) 0.093(4) -0.013(3) -0.022(3) -0.035(2) C8 0.091(4) 0.083(3) 0.069(3) -0.028(3) -0.036(3) -0.027(3) C24 0.057(2) 0.087(3) 0.0441(18) -0.0272(19) -0.0110(15) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F10 C16 1.357(3) . ? Zr1 N1 2.098(3) . ? Zr1 C14 2.429(3) . ? Zr1 C5 2.437(3) . ? Zr1 C1 2.446(3) . ? Zr1 C10 2.450(3) . ? Zr1 C2 2.492(3) . ? Zr1 C11 2.509(3) . ? Zr1 C13 2.515(3) . ? Zr1 C4 2.522(3) . ? Zr1 C3 2.542(3) . ? Zr1 C33 2.594(3) . ? Zr1 Si2 3.0567(13) . ? Si1 N1 1.733(3) . ? Si1 C6 1.843(4) . ? Si1 C7 1.856(4) . ? Si1 C1 1.885(4) . ? Si2 N1 1.732(3) . ? Si2 C9 1.852(5) . ? Si2 C8 1.856(4) . ? Si2 C10 1.881(4) . ? F6 C20 1.355(3) . ? F11 C32 1.349(4) . ? F15 C28 1.363(4) . ? F1 C26 1.354(4) . ? F5 C22 1.356(4) . ? F7 C19 1.351(3) . ? F12 C31 1.346(4) . ? F2 C25 1.340(4) . ? C21 C26 1.381(4) . ? C21 C22 1.383(4) . ? C21 B1 1.654(4) . ? F14 C29 1.349(4) . ? F8 C18 1.336(4) . ? C27 C28 1.391(4) . ? C27 C32 1.393(4) . ? C27 B1 1.652(4) . ? C32 C31 1.385(5) . ? C15 C16 1.382(4) . ? C15 C20 1.388(4) . ? C15 B1 1.641(4) . ? C28 C29 1.378(4) . ? F9 C17 1.342(4) . ? C33 B1 1.670(4) . ? F13 C30 1.344(4) . ? C11 C12 1.410(5) . ? C11 C10 1.415(5) . ? C10 C14 1.424(5) . ? C2 C3 1.415(5) . ? C2 C1 1.418(4) . ? C5 C4 1.413(5) . ? C5 C1 1.427(5) . ? C19 C18 1.373(5) . ? C19 C20 1.378(4) . ? C30 C31 1.364(5) . ? C30 C29 1.371(5) . ? C12 C13 1.408(5) . ? F3 C24 1.340(4) . ? C18 C17 1.369(5) . ? C4 C3 1.404(4) . ? C14 C13 1.407(5) . ? C26 C25 1.391(5) . ? C25 C24 1.370(6) . ? C16 C17 1.384(5) . ? C22 C23 1.382(5) . ? F4 C23 1.339(4) . ? C23 C24 1.367(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C14 88.13(11) . . ? N1 Zr1 C5 89.49(11) . . ? C14 Zr1 C5 87.23(11) . . ? N1 Zr1 C1 70.88(11) . . ? C14 Zr1 C1 114.03(11) . . ? C5 Zr1 C1 33.99(11) . . ? N1 Zr1 C10 70.63(11) . . ? C14 Zr1 C10 33.93(11) . . ? C5 Zr1 C10 115.13(11) . . ? C1 Zr1 C10 129.06(11) . . ? N1 Zr1 C2 92.81(11) . . ? C14 Zr1 C2 141.86(11) . . ? C5 Zr1 C2 54.68(11) . . ? C1 Zr1 C2 33.37(10) . . ? C10 Zr1 C2 161.50(12) . . ? N1 Zr1 C11 93.48(11) . . ? C14 Zr1 C11 54.36(11) . . ? C5 Zr1 C11 141.29(11) . . ? C1 Zr1 C11 161.76(11) . . ? C10 Zr1 C11 33.14(11) . . ? C2 Zr1 C11 162.85(11) . . ? N1 Zr1 C13 120.80(11) . . ? C14 Zr1 C13 33.02(12) . . ? C5 Zr1 C13 92.21(12) . . ? C1 Zr1 C13 126.10(11) . . ? C10 Zr1 C13 55.50(12) . . ? C2 Zr1 C13 133.89(12) . . ? C11 Zr1 C13 53.67(11) . . ? N1 Zr1 C4 122.02(12) . . ? C14 Zr1 C4 93.84(12) . . ? C5 Zr1 C4 33.04(12) . . ? C1 Zr1 C4 55.65(12) . . ? C10 Zr1 C4 127.76(11) . . ? C2 Zr1 C4 54.03(12) . . ? C11 Zr1 C4 132.96(11) . . ? C13 Zr1 C4 80.48(12) . . ? N1 Zr1 C3 124.10(12) . . ? C14 Zr1 C3 124.82(11) . . ? C5 Zr1 C3 54.27(11) . . ? C1 Zr1 C3 55.26(12) . . ? C10 Zr1 C3 158.01(11) . . ? C2 Zr1 C3 32.63(12) . . ? C11 Zr1 C3 142.00(11) . . ? C13 Zr1 C3 103.44(12) . . ? C4 Zr1 C3 32.18(10) . . ? N1 Zr1 C33 99.30(10) . . ? C14 Zr1 C33 136.76(11) . . ? C5 Zr1 C33 134.95(11) . . ? C1 Zr1 C33 108.60(10) . . ? C10 Zr1 C33 109.43(11) . . ? C2 Zr1 C33 80.67(11) . . ? C11 Zr1 C33 82.57(11) . . ? C13 Zr1 C33 119.07(11) . . ? C4 Zr1 C33 116.51(11) . . ? C3 Zr1 C33 85.57(11) . . ? N1 Zr1 Si2 33.10(8) . . ? C14 Zr1 Si2 62.58(9) . . ? C5 Zr1 Si2 107.65(9) . . ? C1 Zr1 Si2 100.85(9) . . ? C10 Zr1 Si2 37.97(8) . . ? C2 Zr1 Si2 125.91(9) . . ? C11 Zr1 Si2 61.88(8) . . ? C13 Zr1 Si2 91.90(9) . . ? C4 Zr1 Si2 138.31(8) . . ? C3 Zr1 Si2 156.07(9) . . ? C33 Zr1 Si2 103.08(8) . . ? N1 Si1 C6 113.03(17) . . ? N1 Si1 C7 114.1(2) . . ? C6 Si1 C7 112.3(2) . . ? N1 Si1 C1 94.11(13) . . ? C6 Si1 C1 111.5(2) . . ? C7 Si1 C1 110.6(2) . . ? N1 Si1 Zr1 41.27(9) . . ? C6 Si1 Zr1 120.48(15) . . ? C7 Si1 Zr1 127.15(19) . . ? C1 Si1 Zr1 53.00(10) . . ? N1 Si2 C9 113.1(2) . . ? N1 Si2 C8 113.6(2) . . ? C9 Si2 C8 112.0(2) . . ? N1 Si2 C10 94.00(14) . . ? C9 Si2 C10 110.0(2) . . ? C8 Si2 C10 113.0(2) . . ? N1 Si2 Zr1 41.41(9) . . ? C9 Si2 Zr1 116.32(17) . . ? C8 Si2 Zr1 131.49(19) . . ? C10 Si2 Zr1 53.25(10) . . ? Si2 N1 Si1 141.78(16) . . ? Si2 N1 Zr1 105.50(13) . . ? Si1 N1 Zr1 105.71(13) . . ? C26 C21 C22 113.0(3) . . ? C26 C21 B1 119.6(3) . . ? C22 C21 B1 127.2(3) . . ? C28 C27 C32 112.6(3) . . ? C28 C27 B1 120.1(3) . . ? C32 C27 B1 127.3(3) . . ? F11 C32 C31 115.6(3) . . ? F11 C32 C27 120.5(3) . . ? C31 C32 C27 124.0(3) . . ? C16 C15 C20 112.8(3) . . ? C16 C15 B1 127.1(3) . . ? C20 C15 B1 120.1(3) . . ? F15 C28 C29 115.5(3) . . ? F15 C28 C27 119.5(3) . . ? C29 C28 C27 125.0(3) . . ? B1 C33 Zr1 169.4(2) . . ? C12 C11 C10 110.1(3) . . ? C12 C11 Zr1 75.48(18) . . ? C10 C11 Zr1 71.12(17) . . ? C11 C10 C14 105.3(3) . . ? C11 C10 Si2 122.6(2) . . ? C14 C10 Si2 122.0(3) . . ? C11 C10 Zr1 75.74(17) . . ? C14 C10 Zr1 72.24(17) . . ? Si2 C10 Zr1 88.78(13) . . ? C3 C2 C1 109.6(3) . . ? C3 C2 Zr1 75.66(18) . . ? C1 C2 Zr1 71.54(17) . . ? C15 B1 C27 107.0(2) . . ? C15 B1 C21 112.9(2) . . ? C27 B1 C21 113.6(2) . . ? C15 B1 C33 111.6(2) . . ? C27 B1 C33 109.0(2) . . ? C21 B1 C33 102.8(2) . . ? C4 C5 C1 109.5(3) . . ? C4 C5 Zr1 76.77(18) . . ? C1 C5 Zr1 73.33(17) . . ? F7 C19 C18 119.8(3) . . ? F7 C19 C20 120.8(3) . . ? C18 C19 C20 119.4(3) . . ? F6 C20 C19 116.0(2) . . ? F6 C20 C15 119.2(3) . . ? C19 C20 C15 124.8(3) . . ? F13 C30 C31 120.6(3) . . ? F13 C30 C29 120.5(3) . . ? C31 C30 C29 118.9(3) . . ? C13 C12 C11 107.2(3) . . ? F8 C18 C17 121.1(3) . . ? F8 C18 C19 120.1(3) . . ? C17 C18 C19 118.8(3) . . ? C3 C4 C5 107.6(3) . . ? C3 C4 Zr1 74.72(18) . . ? C5 C4 Zr1 70.19(18) . . ? C2 C1 C5 105.4(3) . . ? C2 C1 Si1 123.2(2) . . ? C5 C1 Si1 121.3(2) . . ? C2 C1 Zr1 75.09(17) . . ? C5 C1 Zr1 72.68(18) . . ? Si1 C1 Zr1 89.01(12) . . ? F14 C29 C30 120.0(3) . . ? F14 C29 C28 120.6(3) . . ? C30 C29 C28 119.3(3) . . ? C4 C3 C2 107.8(3) . . ? C4 C3 Zr1 73.10(18) . . ? C2 C3 Zr1 71.71(18) . . ? C13 C14 C10 109.5(3) . . ? C13 C14 Zr1 76.85(18) . . ? C10 C14 Zr1 73.83(17) . . ? F1 C26 C21 119.9(3) . . ? F1 C26 C25 115.1(3) . . ? C21 C26 C25 125.0(3) . . ? F2 C25 C24 120.4(3) . . ? F2 C25 C26 120.6(3) . . ? C24 C25 C26 118.9(3) . . ? F10 C16 C15 121.2(3) . . ? F10 C16 C17 114.2(3) . . ? C15 C16 C17 124.5(3) . . ? F5 C22 C23 114.8(3) . . ? F5 C22 C21 121.0(3) . . ? C23 C22 C21 124.2(3) . . ? F12 C31 C30 120.2(3) . . ? F12 C31 C32 119.7(3) . . ? C30 C31 C32 120.1(3) . . ? C14 C13 C12 107.9(3) . . ? C14 C13 Zr1 70.13(18) . . ? C12 C13 Zr1 75.28(18) . . ? F9 C17 C18 120.0(3) . . ? F9 C17 C16 120.3(3) . . ? C18 C17 C16 119.6(3) . . ? F4 C23 C24 119.6(4) . . ? F4 C23 C22 120.3(4) . . ? C24 C23 C22 120.1(3) . . ? F3 C24 C23 121.4(4) . . ? F3 C24 C25 119.8(4) . . ? C23 C24 C25 118.8(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.695 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.081 #===END data_cun115 _database_code_depnum_ccdc_archive 'CCDC 707933' _audit_creation_method 'by Crystalclear-SM 1.4.0 r3' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 F5 N Si2 Zr' _chemical_formula_weight 516.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.491(2) _cell_length_b 10.952(2) _cell_length_c 17.244(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.20(3) _cell_angle_gamma 90.00 _cell_volume 2135.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180.1500 _cell_measurement_reflns_used 6367 _cell_measurement_theta_min 1.8006 _cell_measurement_theta_max 31.2288 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180.1500 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn70 (2x2 bin mode)' _diffrn_measurement_method '\W scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16465 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5269 _reflns_number_gt 4949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+5.3088P] 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 5269 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr -0.00613(3) 0.17156(3) 0.23500(2) 0.03299(11) Uani 1 1 d . . . Si2 Si -0.08678(11) 0.22000(11) 0.39184(7) 0.0407(3) Uani 1 1 d . . . Si1 Si 0.19081(10) 0.22554(11) 0.37422(6) 0.0388(2) Uani 1 1 d . . . F4 F 0.0221(2) -0.3350(2) 0.31885(16) 0.0547(7) Uani 1 1 d . . . F1 F -0.0682(2) -0.0142(2) 0.07587(13) 0.0500(6) Uani 1 1 d . . . F5 F 0.0389(3) -0.0953(2) 0.34875(14) 0.0549(7) Uani 1 1 d . . . N1 N 0.0427(3) 0.1900(3) 0.35806(18) 0.0353(7) Uani 1 1 d . . . F2 F -0.0827(3) -0.2549(2) 0.04751(15) 0.0570(7) Uani 1 1 d . . . F3 F -0.0391(2) -0.4168(2) 0.16871(17) 0.0554(7) Uani 1 1 d . . . C10 C 0.1356(4) 0.3329(4) 0.2200(2) 0.0432(9) Uani 1 1 d . . . H10 H 0.1294 0.4179 0.2365 0.052 Uiso 1 1 calc R . . C1 C -0.0135(3) -0.0422(3) 0.2141(2) 0.0351(8) Uani 1 1 d . . . C3 C 0.0003(4) -0.2538(4) 0.2593(3) 0.0410(9) Uani 1 1 d . . . C17 C -0.1788(3) 0.2349(4) 0.2910(2) 0.0392(8) Uani 1 1 d . . . C6 C -0.0434(4) -0.0913(4) 0.1394(2) 0.0374(8) Uani 1 1 d . . . C2 C 0.0088(3) -0.1299(4) 0.2724(2) 0.0372(8) Uani 1 1 d . . . C18 C -0.2176(4) 0.1327(4) 0.2437(3) 0.0441(9) Uani 1 1 d . . . H18 H -0.2483 0.0570 0.2627 0.053 Uiso 1 1 calc R . . C9 C 0.2012(4) 0.2394(4) 0.2672(2) 0.0403(9) Uani 1 1 d . . . C7 C 0.1417(4) 0.1691(4) 0.1397(3) 0.0459(10) Uani 1 1 d . . . H7 H 0.1361 0.1180 0.0925 0.055 Uiso 1 1 calc R . . C8 C 0.2023(4) 0.1384(4) 0.2158(2) 0.0422(9) Uani 1 1 d . . . H8 H 0.2475 0.0632 0.2292 0.051 Uiso 1 1 calc R . . C5 C -0.0530(4) -0.2136(4) 0.1225(2) 0.0398(8) Uani 1 1 d . . . C16 C -0.1561(4) 0.3289(4) 0.2381(3) 0.0509(11) Uani 1 1 d . . . H16 H -0.1400 0.4147 0.2522 0.061 Uiso 1 1 calc R . . C4 C -0.0305(4) -0.2964(4) 0.1830(3) 0.0406(9) Uani 1 1 d . . . C12 C 0.2866(4) 0.1014(5) 0.4230(3) 0.0513(11) Uani 1 1 d . . . H12A H 0.2703 0.0886 0.4751 0.077 Uiso 1 1 calc R . . H12B H 0.3681 0.1238 0.4262 0.077 Uiso 1 1 calc R . . H12C H 0.2710 0.0276 0.3929 0.077 Uiso 1 1 calc R . . C14 C -0.1405(4) 0.0913(5) 0.4453(3) 0.0554(12) Uani 1 1 d . . . H14A H -0.1378 0.0173 0.4158 0.083 Uiso 1 1 calc R . . H14B H -0.2205 0.1069 0.4518 0.083 Uiso 1 1 calc R . . H14C H -0.0912 0.0828 0.4961 0.083 Uiso 1 1 calc R . . C19 C -0.2214(4) 0.1633(5) 0.1639(3) 0.0581(12) Uani 1 1 d . . . H19 H -0.2520 0.1112 0.1187 0.070 Uiso 1 1 calc R . . C11 C 0.1012(4) 0.2894(4) 0.1417(3) 0.0478(10) Uani 1 1 d . . . H11 H 0.0640 0.3378 0.0962 0.057 Uiso 1 1 calc R . . C13 C 0.2262(5) 0.3728(5) 0.4271(3) 0.0595(13) Uani 1 1 d . . . H13A H 0.1836 0.4378 0.3973 0.089 Uiso 1 1 calc R . . H13B H 0.3096 0.3882 0.4334 0.089 Uiso 1 1 calc R . . H13C H 0.2035 0.3684 0.4780 0.089 Uiso 1 1 calc R . . C15 C -0.0843(5) 0.3641(5) 0.4496(3) 0.0710(16) Uani 1 1 d . . . H15A H -0.0316 0.3549 0.4990 0.106 Uiso 1 1 calc R . . H15B H -0.1625 0.3816 0.4590 0.106 Uiso 1 1 calc R . . H15C H -0.0576 0.4300 0.4205 0.106 Uiso 1 1 calc R . . C20 C -0.1845(5) 0.2826(5) 0.1598(3) 0.0625(14) Uani 1 1 d . . . H20 H -0.1865 0.3301 0.1114 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0360(2) 0.02884(19) 0.03460(19) 0.00085(13) 0.00741(14) 0.00118(14) Si2 0.0407(6) 0.0412(6) 0.0429(6) -0.0065(5) 0.0147(5) -0.0034(5) Si1 0.0370(6) 0.0414(6) 0.0382(5) -0.0016(4) 0.0073(4) -0.0079(5) F4 0.0625(17) 0.0430(14) 0.0583(15) 0.0208(12) 0.0105(13) 0.0045(12) F1 0.0693(17) 0.0438(13) 0.0350(12) 0.0070(10) 0.0040(11) 0.0005(12) F5 0.0757(19) 0.0504(15) 0.0357(12) 0.0035(11) 0.0020(12) -0.0003(13) N1 0.0355(16) 0.0393(17) 0.0318(15) -0.0048(12) 0.0076(12) -0.0034(13) F2 0.0730(19) 0.0530(15) 0.0447(14) -0.0135(12) 0.0097(13) -0.0056(14) F3 0.0623(17) 0.0289(12) 0.0779(19) -0.0051(12) 0.0205(14) -0.0005(11) C10 0.054(2) 0.0326(19) 0.046(2) 0.0013(16) 0.0153(19) -0.0112(18) C1 0.039(2) 0.0286(17) 0.0381(18) 0.0008(14) 0.0076(15) 0.0004(15) C3 0.042(2) 0.0330(19) 0.049(2) 0.0107(16) 0.0105(18) 0.0032(16) C17 0.0325(19) 0.0340(19) 0.052(2) -0.0022(16) 0.0103(17) 0.0030(15) C6 0.040(2) 0.0338(18) 0.0393(19) 0.0044(15) 0.0081(16) 0.0025(16) C2 0.038(2) 0.0358(19) 0.0382(19) -0.0004(15) 0.0084(16) 0.0021(15) C18 0.031(2) 0.046(2) 0.054(2) -0.0026(19) 0.0043(17) -0.0014(17) C9 0.034(2) 0.043(2) 0.045(2) 0.0024(17) 0.0121(16) -0.0059(16) C7 0.053(3) 0.048(2) 0.041(2) -0.0005(18) 0.0189(19) -0.004(2) C8 0.039(2) 0.045(2) 0.046(2) 0.0019(18) 0.0167(17) 0.0022(17) C5 0.045(2) 0.037(2) 0.0379(19) -0.0076(16) 0.0088(16) -0.0007(17) C16 0.054(3) 0.035(2) 0.066(3) 0.0086(19) 0.017(2) 0.0154(19) C4 0.040(2) 0.0297(18) 0.054(2) -0.0034(16) 0.0148(18) -0.0015(16) C12 0.042(2) 0.064(3) 0.048(2) 0.009(2) 0.0078(19) -0.003(2) C14 0.042(2) 0.075(3) 0.053(3) 0.009(2) 0.018(2) -0.003(2) C19 0.044(2) 0.071(3) 0.056(3) -0.007(2) -0.003(2) 0.015(2) C11 0.059(3) 0.045(2) 0.042(2) 0.0085(18) 0.0148(19) -0.002(2) C13 0.064(3) 0.060(3) 0.054(3) -0.012(2) 0.008(2) -0.023(3) C15 0.072(4) 0.068(3) 0.077(4) -0.034(3) 0.024(3) 0.000(3) C20 0.057(3) 0.078(4) 0.053(3) 0.021(3) 0.012(2) 0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.106(3) . ? Zr1 C1 2.367(4) . ? Zr1 C16 2.445(4) . ? Zr1 C10 2.448(4) . ? Zr1 C17 2.456(4) . ? Zr1 C9 2.463(4) . ? Zr1 C18 2.498(4) . ? Zr1 C8 2.501(4) . ? Zr1 C20 2.535(5) . ? Zr1 C11 2.545(4) . ? Zr1 C19 2.560(5) . ? Zr1 C7 2.564(4) . ? Si2 N1 1.723(3) . ? Si2 C14 1.850(5) . ? Si2 C15 1.863(5) . ? Si2 C17 1.875(4) . ? Si1 N1 1.719(3) . ? Si1 C12 1.855(5) . ? Si1 C13 1.862(5) . ? Si1 C9 1.876(4) . ? F4 C3 1.348(4) . ? F1 C6 1.372(4) . ? F5 C2 1.355(4) . ? F2 C5 1.354(4) . ? F3 C4 1.341(4) . ? C10 C11 1.420(6) . ? C10 C9 1.436(6) . ? C1 C6 1.381(5) . ? C1 C2 1.382(5) . ? C3 C2 1.377(6) . ? C3 C4 1.382(6) . ? C17 C18 1.410(6) . ? C17 C16 1.431(6) . ? C6 C5 1.372(5) . ? C18 C19 1.411(7) . ? C9 C8 1.418(6) . ? C7 C11 1.400(6) . ? C7 C8 1.413(6) . ? C5 C4 1.372(6) . ? C16 C20 1.425(7) . ? C19 C20 1.379(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C1 104.13(13) . . ? N1 Zr1 C16 88.50(15) . . ? C1 Zr1 C16 133.95(15) . . ? N1 Zr1 C10 88.49(13) . . ? C1 Zr1 C10 134.75(14) . . ? C16 Zr1 C10 88.76(16) . . ? N1 Zr1 C17 70.51(13) . . ? C1 Zr1 C17 109.25(13) . . ? C16 Zr1 C17 33.94(14) . . ? C10 Zr1 C17 115.91(14) . . ? N1 Zr1 C9 70.68(13) . . ? C1 Zr1 C9 109.85(14) . . ? C16 Zr1 C9 116.11(16) . . ? C10 Zr1 C9 34.01(14) . . ? C17 Zr1 C9 129.99(14) . . ? N1 Zr1 C18 92.53(14) . . ? C1 Zr1 C18 80.33(14) . . ? C16 Zr1 C18 54.65(15) . . ? C10 Zr1 C18 143.33(15) . . ? C17 Zr1 C18 33.05(13) . . ? C9 Zr1 C18 161.84(14) . . ? N1 Zr1 C8 93.23(13) . . ? C1 Zr1 C8 81.13(14) . . ? C16 Zr1 C8 143.16(15) . . ? C10 Zr1 C8 54.55(14) . . ? C17 Zr1 C8 162.20(14) . . ? C9 Zr1 C8 33.19(13) . . ? C18 Zr1 C8 161.41(15) . . ? N1 Zr1 C20 121.11(15) . . ? C1 Zr1 C20 113.12(17) . . ? C16 Zr1 C20 33.19(16) . . ? C10 Zr1 C20 95.32(18) . . ? C17 Zr1 C20 55.17(15) . . ? C9 Zr1 C20 129.29(17) . . ? C18 Zr1 C20 53.49(16) . . ? C8 Zr1 C20 135.13(15) . . ? N1 Zr1 C11 121.04(14) . . ? C1 Zr1 C11 114.42(14) . . ? C16 Zr1 C11 94.50(15) . . ? C10 Zr1 C11 32.98(14) . . ? C17 Zr1 C11 128.39(14) . . ? C9 Zr1 C11 55.41(15) . . ? C18 Zr1 C11 135.23(15) . . ? C8 Zr1 C11 53.68(15) . . ? C20 Zr1 C11 82.63(17) . . ? N1 Zr1 C19 123.27(15) . . ? C1 Zr1 C19 83.50(16) . . ? C16 Zr1 C19 53.86(17) . . ? C10 Zr1 C19 125.40(17) . . ? C17 Zr1 C19 54.50(15) . . ? C9 Zr1 C19 158.81(16) . . ? C18 Zr1 C19 32.37(15) . . ? C8 Zr1 C19 142.92(15) . . ? C20 Zr1 C19 31.40(17) . . ? C11 Zr1 C19 104.47(17) . . ? N1 Zr1 C7 123.91(14) . . ? C1 Zr1 C7 84.37(13) . . ? C16 Zr1 C7 124.81(15) . . ? C10 Zr1 C7 53.91(14) . . ? C17 Zr1 C7 158.15(14) . . ? C9 Zr1 C7 54.81(14) . . ? C18 Zr1 C7 143.03(15) . . ? C8 Zr1 C7 32.37(14) . . ? C20 Zr1 C7 104.17(15) . . ? C11 Zr1 C7 31.80(14) . . ? C19 Zr1 C7 112.70(16) . . ? N1 Si2 C14 114.1(2) . . ? N1 Si2 C15 114.2(2) . . ? C14 Si2 C15 110.7(3) . . ? N1 Si2 C17 94.73(17) . . ? C14 Si2 C17 110.2(2) . . ? C15 Si2 C17 112.0(2) . . ? N1 Si2 Zr1 41.62(11) . . ? C14 Si2 Zr1 119.30(17) . . ? C15 Si2 Zr1 129.9(2) . . ? C17 Si2 Zr1 53.45(12) . . ? N1 Si1 C12 113.48(19) . . ? N1 Si1 C13 113.5(2) . . ? C12 Si1 C13 110.6(2) . . ? N1 Si1 C9 95.30(17) . . ? C12 Si1 C9 111.7(2) . . ? C13 Si1 C9 111.4(2) . . ? N1 Si1 Zr1 41.74(10) . . ? C12 Si1 Zr1 120.85(16) . . ? C13 Si1 Zr1 128.34(18) . . ? C9 Si1 Zr1 53.80(13) . . ? Si1 N1 Si2 142.3(2) . . ? Si1 N1 Zr1 105.34(15) . . ? Si2 N1 Zr1 105.47(16) . . ? C11 C10 C9 109.3(4) . . ? C11 C10 Zr1 77.3(2) . . ? C9 C10 Zr1 73.6(2) . . ? C6 C1 C2 113.0(3) . . ? C6 C1 Zr1 121.5(3) . . ? C2 C1 Zr1 125.4(3) . . ? F4 C3 C2 121.8(4) . . ? F4 C3 C4 119.0(4) . . ? C2 C3 C4 119.2(4) . . ? C18 C17 C16 106.1(4) . . ? C18 C17 Si2 122.4(3) . . ? C16 C17 Si2 121.2(3) . . ? C18 C17 Zr1 75.1(2) . . ? C16 C17 Zr1 72.6(2) . . ? Si2 C17 Zr1 88.72(15) . . ? F1 C6 C5 115.6(3) . . ? F1 C6 C1 119.2(3) . . ? C5 C6 C1 125.2(4) . . ? F5 C2 C3 115.7(4) . . ? F5 C2 C1 119.7(4) . . ? C3 C2 C1 124.6(4) . . ? C17 C18 C19 109.1(4) . . ? C17 C18 Zr1 71.8(2) . . ? C19 C18 Zr1 76.2(3) . . ? C8 C9 C10 105.2(4) . . ? C8 C9 Si1 124.1(3) . . ? C10 C9 Si1 119.8(3) . . ? C8 C9 Zr1 74.9(2) . . ? C10 C9 Zr1 72.4(2) . . ? Si1 C9 Zr1 88.29(15) . . ? C11 C7 C8 108.2(4) . . ? C11 C7 Zr1 73.3(2) . . ? C8 C7 Zr1 71.4(2) . . ? C7 C8 C9 109.8(4) . . ? C7 C8 Zr1 76.3(2) . . ? C9 C8 Zr1 71.9(2) . . ? F2 C5 C6 121.8(4) . . ? F2 C5 C4 119.2(4) . . ? C6 C5 C4 119.1(4) . . ? C20 C16 C17 108.2(4) . . ? C20 C16 Zr1 76.9(3) . . ? C17 C16 Zr1 73.5(2) . . ? F3 C4 C5 120.8(4) . . ? F3 C4 C3 120.3(4) . . ? C5 C4 C3 118.9(4) . . ? C20 C19 C18 108.5(5) . . ? C20 C19 Zr1 73.3(3) . . ? C18 C19 Zr1 71.4(3) . . ? C7 C11 C10 107.5(4) . . ? C7 C11 Zr1 74.9(2) . . ? C10 C11 Zr1 69.7(2) . . ? C19 C20 C16 108.1(4) . . ? C19 C20 Zr1 75.3(3) . . ? C16 C20 Zr1 69.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.799 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.089 #===END data_cun155 _database_code_depnum_ccdc_archive 'CCDC 707934' _audit_creation_method 'by Crystalclear-SM 1.4.0 r3' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H43 B F20 N2 Si4 Zr2' _chemical_formula_weight 1393.50 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.554(3) _cell_length_b 15.672(3) _cell_length_c 16.284(3) _cell_angle_alpha 100.12(3) _cell_angle_beta 103.26(3) _cell_angle_gamma 111.69(3) _cell_volume 2774.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110.15(2) _cell_measurement_reflns_used 8375 _cell_measurement_theta_min 1.7969 _cell_measurement_theta_max 31.3735 _exptl_crystal_description Prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110.15(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn70 (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18307 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.28 _reflns_number_total 13522 _reflns_number_gt 12146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1835P)^2^+3.0145P] 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 13522 _refine_ls_number_parameters 752 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.2743 _refine_ls_wR_factor_gt 0.2200 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group H1C H 0.033(6) 0.714(4) 0.215(4) 0.032(9) Uiso 1 1 d . . . Zr1 Zr 0.23497(5) 0.80234(4) 0.17615(3) 0.02204(19) Uani 1 1 d . . . Zr2 Zr -0.02742(5) 0.69153(4) 0.34998(3) 0.02236(19) Uani 1 1 d . . . Si3 Si 0.05506(17) 0.86938(12) 0.50364(10) 0.0278(4) Uani 1 1 d . . . Si4 Si 0.10866(17) 0.68619(13) 0.52930(9) 0.0298(4) Uani 1 1 d . . . Si1 Si 0.44824(16) 0.99510(12) 0.28334(10) 0.0276(4) Uani 1 1 d . . . Si2 Si 0.47670(16) 0.79608(13) 0.25873(11) 0.0301(4) Uani 1 1 d . . . F6 F 0.0911(3) 0.3877(3) 0.1688(2) 0.0281(7) Uani 1 1 d . . . F20 F 0.3192(4) 0.2250(3) 0.2998(2) 0.0338(9) Uani 1 1 d . . . F16 F 0.3252(4) 0.5238(3) 0.2760(2) 0.0317(8) Uani 1 1 d . . . F15 F 0.5022(3) 0.4959(3) 0.2045(2) 0.0328(8) Uani 1 1 d . . . F14 F 0.5524(4) 0.6118(3) 0.1039(2) 0.0354(8) Uani 1 1 d . . . F19 F 0.3487(4) 0.2788(3) 0.4700(2) 0.0415(10) Uani 1 1 d . . . F13 F 0.3815(4) 0.5830(3) -0.0499(2) 0.0366(9) Uani 1 1 d . . . F1 F 0.5358(3) 0.3551(3) 0.2727(2) 0.0327(8) Uani 1 1 d . . . F12 F 0.1548(3) 0.4351(3) -0.0974(2) 0.0319(8) Uani 1 1 d . . . F11 F 0.1024(3) 0.3191(3) 0.0005(2) 0.0288(7) Uani 1 1 d . . . F2 F 0.6646(3) 0.2732(3) 0.2143(2) 0.0373(9) Uani 1 1 d . . . F10 F 0.1571(4) 0.1056(3) 0.1367(2) 0.0360(8) Uani 1 1 d . . . N1 N 0.4107(4) 0.8746(4) 0.2693(3) 0.0255(10) Uani 1 1 d . . . F9 F -0.0609(4) 0.0100(3) 0.1472(3) 0.0464(11) Uani 1 1 d . . . F7 F -0.1340(4) 0.2851(3) 0.1679(2) 0.0345(9) Uani 1 1 d . . . F3 F 0.5684(4) 0.1378(4) 0.0537(3) 0.0492(12) Uani 1 1 d . . . F17 F 0.3563(4) 0.5764(3) 0.4464(2) 0.0385(9) Uani 1 1 d . . . C42 C 0.2988(5) 0.4018(4) 0.1108(3) 0.0258(12) Uani 1 1 d . . . C45 C 0.3551(6) 0.5256(4) 0.0017(3) 0.0279(13) Uani 1 1 d . . . C31 C 0.4800(5) 0.2900(4) 0.1910(3) 0.0253(11) Uani 1 1 d . . . F18 F 0.3664(4) 0.4560(4) 0.5469(2) 0.0465(12) Uani 1 1 d . . . F8 F -0.2098(4) 0.0982(3) 0.1634(3) 0.0429(9) Uani 1 1 d . . . N2 N 0.0854(5) 0.7713(4) 0.4811(3) 0.0274(11) Uani 1 1 d . . . C25 C -0.0781(6) 0.8260(4) 0.3998(3) 0.0265(12) Uani 1 1 d . . . F5 F 0.2106(4) 0.1822(3) 0.0022(2) 0.0449(11) Uani 1 1 d . . . C35 C 0.3227(5) 0.2049(4) 0.0591(3) 0.0254(11) Uani 1 1 d . . . F4 F 0.3380(5) 0.0912(4) -0.0501(2) 0.0548(13) Uani 1 1 d . . . C6 C 0.1926(6) 0.9464(4) 0.2170(4) 0.0284(12) Uani 1 1 d . . . H6 H 0.1827 0.9700 0.2733 0.034 Uiso 1 1 calc R . . C37 C 0.0537(5) 0.2914(4) 0.1603(3) 0.0257(12) Uani 1 1 d . . . C44 C 0.2408(6) 0.4507(4) -0.0211(3) 0.0267(12) Uani 1 1 d . . . C18 C -0.0497(7) 0.5232(5) 0.2764(3) 0.0345(15) Uani 1 1 d . . . H18 H -0.0482 0.5010 0.2167 0.041 Uiso 1 1 calc R . . C27 C -0.1592(6) 0.7488(5) 0.2494(4) 0.0373(16) Uani 1 1 d . . . H27 H -0.1752 0.7374 0.1857 0.045 Uiso 1 1 calc R . . C2 C 0.3051(6) 0.9767(4) 0.1992(3) 0.0273(12) Uani 1 1 d . . . C12 C 0.2361(5) 0.6398(4) 0.1626(3) 0.0232(10) Uani 1 1 d . . . H12 H 0.2270 0.6054 0.2072 0.028 Uiso 1 1 calc R . . C4 C 0.1469(7) 0.8787(5) 0.0706(4) 0.0396(18) Uani 1 1 d . . . H4 H 0.1002 0.8478 0.0080 0.047 Uiso 1 1 calc R . . C48 C 0.3205(5) 0.3701(4) 0.2769(3) 0.0232(11) Uani 1 1 d . . . C43 C 0.2150(5) 0.3912(4) 0.0316(3) 0.0252(11) Uani 1 1 d . . . C16 C 0.0128(5) 0.5807(4) 0.4291(3) 0.0211(10) Uani 1 1 d . . . C46 C 0.4413(5) 0.5400(4) 0.0798(3) 0.0223(10) Uani 1 1 d . . . C1 C 0.1110(5) 0.7447(4) 0.2689(3) 0.0226(11) Uani 1 1 d . . . H1A H 0.1224 0.6863 0.2618 0.027 Uiso 1 1 calc R . . H1B H 0.1762 0.7876 0.3224 0.027 Uiso 1 1 calc R . . C14 C 0.1934(7) 0.6790(6) 0.0347(4) 0.0415(18) Uani 1 1 d . . . H14 H 0.1520 0.6773 -0.0248 0.050 Uiso 1 1 calc R . . C36 C 0.1365(5) 0.2513(4) 0.1516(3) 0.0249(11) Uani 1 1 d . . . H36 H 0.1140 0.2395 0.0875 0.030 Uiso 1 1 calc R . . C30 C 0.3627(6) 0.2695(4) 0.1412(3) 0.0266(12) Uani 1 1 d . . . C38 C -0.0607(6) 0.2411(5) 0.1617(3) 0.0309(14) Uani 1 1 d . . . C49 C 0.3323(5) 0.4601(4) 0.3203(3) 0.0258(11) Uani 1 1 d . . . C47 C 0.4094(5) 0.4762(4) 0.1299(3) 0.0234(10) Uani 1 1 d . . . C5 C 0.0985(6) 0.8888(5) 0.1401(4) 0.0321(14) Uani 1 1 d . . . H5 H 0.0122 0.8635 0.1339 0.039 Uiso 1 1 calc R . . C40 C -0.0261(5) 0.1005(4) 0.1495(4) 0.0285(12) Uani 1 1 d . . . C20 C -0.1174(6) 0.5451(4) 0.3936(4) 0.0282(12) Uani 1 1 d . . . H20 H -0.1724 0.5357 0.4287 0.034 Uiso 1 1 calc R . . C51 C 0.3529(6) 0.4284(6) 0.4604(4) 0.0358(15) Uani 1 1 d . . . C3 C 0.2747(7) 0.9321(5) 0.1065(4) 0.0351(15) Uani 1 1 d . . . H3 H 0.3303 0.9470 0.0721 0.042 Uiso 1 1 calc R . . C8 C 0.4611(6) 1.0601(5) 0.3955(4) 0.0335(13) Uani 1 1 d . . . H8A H 0.4041 1.0178 0.4171 0.050 Uiso 1 1 calc R . . H8B H 0.4441 1.1146 0.3924 0.050 Uiso 1 1 calc R . . H8C H 0.5417 1.0813 0.4347 0.050 Uiso 1 1 calc R . . C17 C 0.0532(6) 0.5670(4) 0.3549(3) 0.0287(13) Uani 1 1 d . . . H17 H 0.1360 0.5770 0.3578 0.034 Uiso 1 1 calc R . . C19 C -0.1541(7) 0.5103(5) 0.3003(4) 0.0394(15) Uani 1 1 d . . . H19 H -0.2378 0.4762 0.2605 0.047 Uiso 1 1 calc R . . C10 C 0.4996(7) 0.7524(5) 0.3568(4) 0.0431(16) Uani 1 1 d . . . H10A H 0.5509 0.8058 0.4081 0.065 Uiso 1 1 calc R . . H10B H 0.5370 0.7094 0.3490 0.065 Uiso 1 1 calc R . . H10C H 0.4228 0.7192 0.3644 0.065 Uiso 1 1 calc R . . C29 C -0.1823(6) 0.7395(5) 0.3838(4) 0.0329(14) Uani 1 1 d . . . H29 H -0.2207 0.7217 0.4280 0.040 Uiso 1 1 calc R . . C41 C 0.0912(6) 0.1559(5) 0.1465(4) 0.0317(14) Uani 1 1 d . . . C50 C 0.3467(6) 0.4895(5) 0.4091(4) 0.0339(15) Uani 1 1 d . . . C13 C 0.1395(7) 0.6240(5) 0.0865(4) 0.0347(14) Uani 1 1 d . . . H13 H 0.0545 0.5781 0.0701 0.042 Uiso 1 1 calc R . . C22 C 0.0446(9) 0.6759(6) 0.6213(4) 0.050(2) Uani 1 1 d . . . H22A H 0.0869 0.7354 0.6676 0.074 Uiso 1 1 calc R . . H22B H 0.0537 0.6253 0.6435 0.074 Uiso 1 1 calc R . . H22C H -0.0397 0.6619 0.6003 0.074 Uiso 1 1 calc R . . C52 C 0.3446(6) 0.3405(5) 0.4220(3) 0.0301(13) Uani 1 1 d . . . C23 C 0.1811(7) 0.9797(6) 0.5083(4) 0.0434(17) Uani 1 1 d . . . H23A H 0.2546 0.9869 0.5492 0.065 Uiso 1 1 calc R . . H23B H 0.1649 1.0339 0.5273 0.065 Uiso 1 1 calc R . . H23C H 0.1897 0.9761 0.4509 0.065 Uiso 1 1 calc R . . C15 C 0.3197(6) 0.7285(5) 0.0791(4) 0.0326(14) Uani 1 1 d . . . H15 H 0.3800 0.7632 0.0537 0.039 Uiso 1 1 calc R . . C24 C 0.0101(8) 0.8875(5) 0.6044(4) 0.0403(17) Uani 1 1 d . . . H24A H -0.0518 0.8283 0.6035 0.060 Uiso 1 1 calc R . . H24B H -0.0204 0.9354 0.6059 0.060 Uiso 1 1 calc R . . H24C H 0.0792 0.9081 0.6558 0.060 Uiso 1 1 calc R . . C34 C 0.3862(7) 0.1576(5) 0.0285(4) 0.0354(14) Uani 1 1 d . . . C26 C -0.0662(6) 0.8308(5) 0.3154(3) 0.0325(15) Uani 1 1 d . . . H26 H -0.0080 0.8858 0.3043 0.039 Uiso 1 1 calc R . . C11 C 0.3464(6) 0.7034(4) 0.1596(3) 0.0268(12) Uani 1 1 d . . . B1 B 0.2789(6) 0.3232(5) 0.1691(4) 0.0254(13) Uani 1 1 d . . . C28 C -0.2339(5) 0.6904(5) 0.2913(4) 0.0309(12) Uani 1 1 d . . . H28 H -0.3113 0.6338 0.2619 0.037 Uiso 1 1 calc R . . C53 C 0.3284(6) 0.3122(5) 0.3321(4) 0.0342(15) Uani 1 1 d . . . C9 C 0.6206(7) 0.8453(6) 0.2317(6) 0.0495(19) Uani 1 1 d . . . H9A H 0.6064 0.8670 0.1805 0.074 Uiso 1 1 calc R . . H9B H 0.6479 0.7961 0.2204 0.074 Uiso 1 1 calc R . . H9C H 0.6812 0.8981 0.2806 0.074 Uiso 1 1 calc R . . C39 C -0.0996(6) 0.1473(5) 0.1594(4) 0.0319(13) Uani 1 1 d . . . C32 C 0.5477(6) 0.2463(5) 0.1619(4) 0.0323(14) Uani 1 1 d . . . C33 C 0.5037(7) 0.1821(5) 0.0822(4) 0.0349(15) Uani 1 1 d . . . C7 C 0.5852(7) 1.0560(5) 0.2525(4) 0.0410(16) Uani 1 1 d . . . H7A H 0.6540 1.0543 0.2915 0.061 Uiso 1 1 calc R . . H7B H 0.5991 1.1214 0.2572 0.061 Uiso 1 1 calc R . . H7C H 0.5729 1.0236 0.1930 0.061 Uiso 1 1 calc R . . C21 C 0.2683(6) 0.7043(5) 0.5619(4) 0.0355(14) Uani 1 1 d . . . H21A H 0.2907 0.6917 0.5101 0.053 Uiso 1 1 calc R . . H21B H 0.2776 0.6613 0.5953 0.053 Uiso 1 1 calc R . . H21C H 0.3194 0.7693 0.5972 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0282(4) 0.0263(3) 0.0191(3) 0.0088(2) 0.0076(2) 0.0186(3) Zr2 0.0264(4) 0.0263(3) 0.0205(3) 0.0081(2) 0.0072(2) 0.0173(3) Si3 0.0376(10) 0.0290(8) 0.0250(7) 0.0085(7) 0.0108(7) 0.0222(8) Si4 0.0451(11) 0.0357(9) 0.0195(6) 0.0102(7) 0.0094(7) 0.0285(9) Si1 0.0343(10) 0.0294(8) 0.0258(7) 0.0098(7) 0.0108(7) 0.0193(8) Si2 0.0289(10) 0.0322(8) 0.0366(8) 0.0133(7) 0.0085(7) 0.0208(8) F6 0.031(2) 0.0281(17) 0.0331(16) 0.0117(15) 0.0114(15) 0.0188(17) F20 0.045(2) 0.035(2) 0.0352(17) 0.0204(17) 0.0162(17) 0.026(2) F16 0.045(2) 0.0307(18) 0.0239(14) 0.0066(15) 0.0065(15) 0.0240(19) F15 0.030(2) 0.042(2) 0.0268(15) 0.0135(16) 0.0026(15) 0.0176(19) F14 0.041(2) 0.0329(19) 0.0322(17) 0.0092(16) 0.0110(17) 0.0164(19) F19 0.053(3) 0.052(2) 0.0351(18) 0.028(2) 0.0192(19) 0.030(2) F13 0.051(3) 0.039(2) 0.0331(17) 0.0217(17) 0.0199(18) 0.024(2) F1 0.027(2) 0.042(2) 0.0306(16) 0.0080(16) 0.0037(15) 0.021(2) F12 0.032(2) 0.041(2) 0.0218(14) 0.0126(15) 0.0026(14) 0.0168(19) F11 0.0175(18) 0.0331(18) 0.0282(15) 0.0104(15) 0.0010(13) 0.0056(16) F2 0.026(2) 0.048(2) 0.051(2) 0.022(2) 0.0155(18) 0.024(2) F10 0.035(2) 0.0303(19) 0.0478(19) 0.0113(17) 0.0092(17) 0.0217(19) N1 0.025(3) 0.029(2) 0.027(2) 0.013(2) 0.0063(19) 0.015(2) F9 0.041(3) 0.031(2) 0.074(3) 0.023(2) 0.022(2) 0.017(2) F7 0.037(2) 0.053(2) 0.0296(15) 0.0126(17) 0.0150(16) 0.034(2) F3 0.060(3) 0.066(3) 0.057(2) 0.026(2) 0.035(2) 0.051(3) F17 0.047(3) 0.034(2) 0.0309(17) 0.0023(17) 0.0107(17) 0.018(2) C42 0.032(3) 0.031(3) 0.021(2) 0.005(2) 0.007(2) 0.023(3) C45 0.040(4) 0.034(3) 0.023(2) 0.013(2) 0.013(2) 0.025(3) C31 0.026(3) 0.026(3) 0.029(2) 0.010(2) 0.007(2) 0.016(3) F18 0.052(3) 0.076(3) 0.0238(16) 0.014(2) 0.0183(18) 0.036(3) F8 0.024(2) 0.043(2) 0.065(3) 0.022(2) 0.023(2) 0.010(2) N2 0.039(3) 0.030(2) 0.0182(18) 0.0042(19) 0.0034(19) 0.025(3) C25 0.031(3) 0.034(3) 0.026(2) 0.007(2) 0.010(2) 0.026(3) F5 0.054(3) 0.064(3) 0.0277(16) 0.0078(19) 0.0066(17) 0.043(3) C35 0.023(3) 0.027(3) 0.026(2) 0.010(2) 0.007(2) 0.009(3) F4 0.070(4) 0.069(3) 0.0315(18) -0.003(2) 0.012(2) 0.046(3) C6 0.040(4) 0.025(3) 0.030(2) 0.011(2) 0.010(2) 0.023(3) C37 0.030(3) 0.031(3) 0.022(2) 0.009(2) 0.009(2) 0.018(3) C44 0.030(3) 0.033(3) 0.019(2) 0.005(2) 0.004(2) 0.020(3) C18 0.060(5) 0.034(3) 0.021(2) 0.009(2) 0.009(3) 0.033(4) C27 0.046(4) 0.056(4) 0.029(3) 0.018(3) 0.009(3) 0.041(4) C2 0.035(3) 0.025(3) 0.028(2) 0.009(2) 0.007(2) 0.021(3) C12 0.023(3) 0.011(2) 0.032(2) 0.003(2) 0.006(2) 0.007(2) C4 0.060(5) 0.053(4) 0.025(2) 0.021(3) 0.011(3) 0.043(4) C48 0.027(3) 0.025(3) 0.019(2) 0.005(2) 0.003(2) 0.016(3) C43 0.027(3) 0.029(3) 0.022(2) 0.007(2) 0.006(2) 0.016(3) C16 0.023(3) 0.013(2) 0.024(2) 0.004(2) 0.007(2) 0.005(2) C46 0.014(3) 0.020(2) 0.024(2) 0.001(2) 0.001(2) 0.004(2) C1 0.019(3) 0.023(3) 0.027(2) 0.007(2) 0.008(2) 0.009(2) C14 0.068(5) 0.052(4) 0.020(2) 0.011(3) 0.012(3) 0.044(4) C36 0.026(3) 0.033(3) 0.018(2) 0.008(2) 0.004(2) 0.017(3) C30 0.032(3) 0.031(3) 0.025(2) 0.012(2) 0.008(2) 0.020(3) C38 0.036(4) 0.050(4) 0.020(2) 0.012(3) 0.012(2) 0.030(4) C49 0.025(3) 0.025(3) 0.025(2) 0.004(2) 0.001(2) 0.015(3) C47 0.019(3) 0.026(3) 0.024(2) 0.006(2) 0.004(2) 0.010(2) C5 0.042(4) 0.034(3) 0.033(3) 0.015(3) 0.010(3) 0.028(3) C40 0.019(3) 0.022(3) 0.037(3) 0.010(3) 0.005(2) 0.002(3) C20 0.026(3) 0.019(2) 0.039(3) 0.012(2) 0.014(3) 0.006(3) C51 0.037(4) 0.060(4) 0.024(2) 0.017(3) 0.014(3) 0.030(4) C3 0.059(5) 0.038(3) 0.029(3) 0.020(3) 0.020(3) 0.035(4) C8 0.022(3) 0.036(3) 0.032(3) 0.001(3) 0.006(3) 0.006(3) C17 0.038(4) 0.034(3) 0.025(2) 0.009(2) 0.011(2) 0.026(3) C19 0.045(4) 0.035(3) 0.037(3) 0.008(3) 0.001(3) 0.024(4) C10 0.043(4) 0.038(4) 0.042(3) 0.019(3) -0.002(3) 0.017(4) C29 0.030(4) 0.039(3) 0.038(3) 0.014(3) 0.014(3) 0.022(3) C41 0.036(4) 0.040(3) 0.031(3) 0.015(3) 0.012(3) 0.027(3) C50 0.036(4) 0.046(4) 0.030(3) 0.007(3) 0.010(3) 0.030(4) C13 0.049(4) 0.032(3) 0.031(3) 0.006(3) 0.010(3) 0.028(3) C22 0.100(7) 0.049(4) 0.027(3) 0.021(3) 0.031(4) 0.049(5) C52 0.030(3) 0.049(4) 0.025(2) 0.022(3) 0.012(2) 0.023(3) C23 0.058(5) 0.048(4) 0.040(3) 0.017(3) 0.015(3) 0.037(4) C15 0.047(4) 0.038(3) 0.034(3) 0.018(3) 0.023(3) 0.031(3) C24 0.063(5) 0.040(4) 0.033(3) 0.009(3) 0.023(3) 0.034(4) C34 0.049(4) 0.034(3) 0.028(3) 0.008(3) 0.015(3) 0.021(3) C26 0.049(4) 0.044(3) 0.027(2) 0.016(3) 0.016(3) 0.038(4) C11 0.032(3) 0.029(3) 0.027(2) 0.008(2) 0.011(2) 0.020(3) B1 0.031(4) 0.029(3) 0.023(2) 0.008(2) 0.006(2) 0.023(3) C28 0.010(3) 0.033(3) 0.047(3) 0.010(3) 0.006(2) 0.009(3) C53 0.040(4) 0.056(4) 0.028(3) 0.023(3) 0.016(3) 0.036(4) C9 0.043(5) 0.056(5) 0.070(5) 0.022(4) 0.026(4) 0.037(4) C39 0.027(3) 0.039(3) 0.034(3) 0.014(3) 0.009(3) 0.018(3) C32 0.030(3) 0.044(3) 0.043(3) 0.028(3) 0.018(3) 0.026(3) C33 0.045(4) 0.041(4) 0.037(3) 0.016(3) 0.021(3) 0.032(4) C7 0.053(5) 0.039(4) 0.048(3) 0.021(3) 0.025(3) 0.029(4) C21 0.032(4) 0.030(3) 0.038(3) 0.005(3) 0.000(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.113(5) . ? Zr1 C3 2.448(5) . ? Zr1 C15 2.450(5) . ? Zr1 C1 2.458(5) . ? Zr1 C11 2.462(4) . ? Zr1 C2 2.468(6) . ? Zr1 C6 2.519(5) . ? Zr1 C12 2.523(4) . ? Zr1 C4 2.537(5) . ? Zr1 C14 2.540(6) . ? Zr1 C5 2.579(5) . ? Zr1 C13 2.582(7) . ? Zr2 N2 2.119(5) . ? Zr2 C1 2.413(5) . ? Zr2 C16 2.464(4) . ? Zr2 C20 2.465(5) . ? Zr2 C29 2.465(5) . ? Zr2 C25 2.476(5) . ? Zr2 C17 2.514(5) . ? Zr2 C26 2.532(5) . ? Zr2 C28 2.541(5) . ? Zr2 C19 2.552(8) . ? Zr2 C27 2.568(5) . ? Zr2 C18 2.582(6) . ? Si3 N2 1.715(4) . ? Si3 C23 1.838(9) . ? Si3 C24 1.864(6) . ? Si3 C25 1.891(6) . ? Si4 N2 1.741(4) . ? Si4 C21 1.849(6) . ? Si4 C22 1.860(6) . ? Si4 C16 1.877(6) . ? Si1 N1 1.727(5) . ? Si1 C7 1.862(7) . ? Si1 C8 1.868(6) . ? Si1 C2 1.881(6) . ? Si2 N1 1.724(4) . ? Si2 C10 1.850(6) . ? Si2 C9 1.872(8) . ? Si2 C11 1.898(7) . ? F6 C37 1.375(7) . ? F20 C53 1.326(7) . ? F16 C49 1.347(6) . ? F15 C47 1.371(6) . ? F14 C46 1.342(7) . ? F19 C52 1.355(6) . ? F13 C45 1.341(6) . ? F1 C31 1.368(7) . ? F12 C44 1.362(6) . ? F11 C43 1.350(7) . ? F2 C32 1.379(7) . ? F10 C41 1.353(5) . ? F9 C40 1.311(7) . ? F7 C38 1.349(5) . ? F3 C33 1.354(6) . ? F17 C50 1.339(7) . ? C42 C47 1.365(9) . ? C42 C43 1.404(7) . ? C42 B1 1.666(8) . ? C45 C46 1.388(7) . ? C45 C44 1.390(9) . ? C31 C32 1.383(7) . ? C31 C30 1.393(8) . ? F18 C51 1.350(6) . ? F8 C39 1.335(8) . ? C25 C29 1.423(10) . ? C25 C26 1.427(7) . ? F5 C35 1.372(7) . ? C35 C30 1.381(8) . ? C35 C34 1.385(7) . ? F4 C34 1.342(8) . ? C6 C5 1.384(9) . ? C6 C2 1.430(9) . ? C37 C38 1.368(9) . ? C37 C36 1.419(6) . ? C44 C43 1.377(8) . ? C18 C19 1.406(10) . ? C18 C17 1.433(9) . ? C27 C26 1.414(10) . ? C27 C28 1.436(9) . ? C2 C3 1.441(8) . ? C12 C11 1.393(9) . ? C12 C13 1.431(8) . ? C4 C5 1.414(8) . ? C4 C3 1.422(11) . ? C48 C53 1.398(7) . ? C48 C49 1.399(7) . ? C48 B1 1.655(7) . ? C16 C17 1.427(7) . ? C16 C20 1.448(8) . ? C46 C47 1.401(7) . ? C14 C13 1.414(10) . ? C14 C15 1.416(11) . ? C36 C41 1.368(9) . ? C36 B1 1.647(10) . ? C30 B1 1.661(7) . ? C38 C39 1.358(9) . ? C49 C50 1.386(7) . ? C40 C39 1.393(7) . ? C40 C41 1.424(9) . ? C20 C19 1.422(9) . ? C51 C52 1.364(9) . ? C51 C50 1.388(8) . ? C29 C28 1.434(9) . ? C52 C53 1.396(7) . ? C15 C11 1.436(7) . ? C34 C33 1.401(10) . ? C32 C33 1.343(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zr1 C3 91.1(2) . . ? N1 Zr1 C15 87.9(2) . . ? C3 Zr1 C15 88.34(18) . . ? N1 Zr1 C1 101.78(18) . . ? C3 Zr1 C1 135.45(17) . . ? C15 Zr1 C1 134.01(19) . . ? N1 Zr1 C11 70.73(19) . . ? C3 Zr1 C11 116.99(19) . . ? C15 Zr1 C11 34.00(16) . . ? C1 Zr1 C11 107.50(17) . . ? N1 Zr1 C2 70.86(18) . . ? C3 Zr1 C2 34.10(18) . . ? C15 Zr1 C2 113.9(2) . . ? C1 Zr1 C2 111.71(17) . . ? C11 Zr1 C2 129.3(2) . . ? N1 Zr1 C6 91.21(19) . . ? C3 Zr1 C6 54.79(18) . . ? C15 Zr1 C6 143.10(19) . . ? C1 Zr1 C6 82.19(17) . . ? C11 Zr1 C6 160.7(2) . . ? C2 Zr1 C6 33.3(2) . . ? N1 Zr1 C12 93.08(18) . . ? C3 Zr1 C12 141.96(18) . . ? C15 Zr1 C12 54.11(18) . . ? C1 Zr1 C12 80.33(17) . . ? C11 Zr1 C12 32.4(2) . . ? C2 Zr1 C12 161.27(19) . . ? C6 Zr1 C12 162.50(19) . . ? N1 Zr1 C4 123.1(2) . . ? C3 Zr1 C4 33.1(2) . . ? C15 Zr1 C4 97.27(18) . . ? C1 Zr1 C4 113.21(19) . . ? C11 Zr1 C4 131.27(18) . . ? C2 Zr1 C4 55.3(2) . . ? C6 Zr1 C4 53.45(18) . . ? C12 Zr1 C4 134.7(2) . . ? N1 Zr1 C14 120.4(2) . . ? C3 Zr1 C14 92.4(2) . . ? C15 Zr1 C14 32.9(2) . . ? C1 Zr1 C14 115.7(2) . . ? C11 Zr1 C14 55.13(19) . . ? C2 Zr1 C14 126.2(2) . . ? C6 Zr1 C14 136.28(17) . . ? C12 Zr1 C14 53.44(17) . . ? C4 Zr1 C14 83.09(19) . . ? N1 Zr1 C5 121.9(2) . . ? C3 Zr1 C5 54.1(2) . . ? C15 Zr1 C5 128.68(17) . . ? C1 Zr1 C5 83.70(17) . . ? C11 Zr1 C5 161.90(18) . . ? C2 Zr1 C5 54.2(2) . . ? C6 Zr1 C5 31.5(2) . . ? C12 Zr1 C5 143.9(2) . . ? C4 Zr1 C5 32.07(18) . . ? C14 Zr1 C5 107.43(18) . . ? N1 Zr1 C13 124.00(18) . . ? C3 Zr1 C13 122.45(19) . . ? C15 Zr1 C13 54.2(2) . . ? C1 Zr1 C13 84.75(19) . . ? C11 Zr1 C13 54.7(2) . . ? C2 Zr1 C13 156.33(17) . . ? C6 Zr1 C13 144.3(2) . . ? C12 Zr1 C13 32.53(17) . . ? C4 Zr1 C13 103.3(2) . . ? C14 Zr1 C13 32.0(2) . . ? C5 Zr1 C13 114.1(2) . . ? N2 Zr2 C1 101.3(2) . . ? N2 Zr2 C16 71.30(17) . . ? C1 Zr2 C16 112.38(16) . . ? N2 Zr2 C20 92.2(2) . . ? C1 Zr2 C20 135.66(16) . . ? C16 Zr2 C20 34.17(18) . . ? N2 Zr2 C29 87.42(19) . . ? C1 Zr2 C29 133.24(18) . . ? C16 Zr2 C29 113.90(18) . . ? C20 Zr2 C29 88.9(2) . . ? N2 Zr2 C25 70.70(16) . . ? C1 Zr2 C25 106.75(18) . . ? C16 Zr2 C25 129.42(16) . . ? C20 Zr2 C25 117.56(19) . . ? C29 Zr2 C25 33.5(2) . . ? N2 Zr2 C17 90.94(17) . . ? C1 Zr2 C17 82.63(17) . . ? C16 Zr2 C17 33.29(16) . . ? C20 Zr2 C17 54.84(19) . . ? C29 Zr2 C17 143.7(2) . . ? C25 Zr2 C17 160.51(17) . . ? N2 Zr2 C26 93.79(18) . . ? C1 Zr2 C26 79.35(17) . . ? C16 Zr2 C26 162.22(16) . . ? C20 Zr2 C26 142.1(2) . . ? C29 Zr2 C26 54.1(2) . . ? C25 Zr2 C26 33.10(16) . . ? C17 Zr2 C26 161.93(19) . . ? N2 Zr2 C28 120.46(18) . . ? C1 Zr2 C28 116.30(18) . . ? C16 Zr2 C28 124.9(2) . . ? C20 Zr2 C28 91.1(2) . . ? C29 Zr2 C28 33.2(2) . . ? C25 Zr2 C28 55.6(2) . . ? C17 Zr2 C28 135.9(2) . . ? C26 Zr2 C28 54.1(2) . . ? N2 Zr2 C19 123.98(19) . . ? C1 Zr2 C19 113.4(2) . . ? C16 Zr2 C19 55.55(18) . . ? C20 Zr2 C19 32.9(2) . . ? C29 Zr2 C19 97.9(2) . . ? C25 Zr2 C19 131.4(2) . . ? C17 Zr2 C19 54.1(2) . . ? C26 Zr2 C19 133.7(2) . . ? C28 Zr2 C19 82.0(2) . . ? N2 Zr2 C27 124.20(19) . . ? C1 Zr2 C27 84.73(19) . . ? C16 Zr2 C27 155.5(2) . . ? C20 Zr2 C27 121.5(2) . . ? C29 Zr2 C27 54.20(18) . . ? C25 Zr2 C27 54.86(18) . . ? C17 Zr2 C27 144.4(2) . . ? C26 Zr2 C27 32.2(2) . . ? C28 Zr2 C27 32.6(2) . . ? C19 Zr2 C27 102.3(2) . . ? N2 Zr2 C18 122.76(16) . . ? C1 Zr2 C18 84.17(19) . . ? C16 Zr2 C18 54.82(16) . . ? C20 Zr2 C18 53.75(19) . . ? C29 Zr2 C18 129.0(2) . . ? C25 Zr2 C18 161.5(2) . . ? C17 Zr2 C18 32.62(19) . . ? C26 Zr2 C18 142.27(17) . . ? C28 Zr2 C18 106.2(2) . . ? C19 Zr2 C18 31.8(2) . . ? C27 Zr2 C18 113.0(2) . . ? N2 Si3 C23 111.8(3) . . ? N2 Si3 C24 114.9(2) . . ? C23 Si3 C24 110.0(3) . . ? N2 Si3 C25 95.6(2) . . ? C23 Si3 C25 112.3(3) . . ? C24 Si3 C25 111.7(3) . . ? N2 Si4 C21 113.2(3) . . ? N2 Si4 C22 111.7(2) . . ? C21 Si4 C22 112.4(3) . . ? N2 Si4 C16 95.8(2) . . ? C21 Si4 C16 111.4(3) . . ? C22 Si4 C16 111.4(3) . . ? N1 Si1 C7 112.4(2) . . ? N1 Si1 C8 113.3(3) . . ? C7 Si1 C8 111.8(3) . . ? N1 Si1 C2 95.5(2) . . ? C7 Si1 C2 112.2(3) . . ? C8 Si1 C2 110.9(3) . . ? N1 Si2 C10 111.7(3) . . ? N1 Si2 C9 113.6(3) . . ? C10 Si2 C9 111.0(3) . . ? N1 Si2 C11 94.6(2) . . ? C10 Si2 C11 113.4(3) . . ? C9 Si2 C11 111.8(3) . . ? Si2 N1 Si1 139.2(3) . . ? Si2 N1 Zr1 105.8(3) . . ? Si1 N1 Zr1 105.22(19) . . ? C47 C42 C43 113.3(5) . . ? C47 C42 B1 120.7(4) . . ? C43 C42 B1 125.2(6) . . ? F13 C45 C46 120.7(6) . . ? F13 C45 C44 121.0(5) . . ? C46 C45 C44 118.2(5) . . ? F1 C31 C32 115.5(5) . . ? F1 C31 C30 121.6(4) . . ? C32 C31 C30 122.8(5) . . ? Si3 N2 Si4 140.6(3) . . ? Si3 N2 Zr2 105.11(19) . . ? Si4 N2 Zr2 104.4(2) . . ? C29 C25 C26 105.8(5) . . ? C29 C25 Si3 119.9(4) . . ? C26 C25 Si3 123.7(5) . . ? C29 C25 Zr2 72.9(3) . . ? C26 C25 Zr2 75.6(3) . . ? Si3 C25 Zr2 87.70(17) . . ? F5 C35 C30 119.3(4) . . ? F5 C35 C34 115.6(5) . . ? C30 C35 C34 125.2(5) . . ? C5 C6 C2 109.8(5) . . ? C5 C6 Zr1 76.6(3) . . ? C2 C6 Zr1 71.4(3) . . ? C38 C37 F6 117.4(4) . . ? C38 C37 C36 124.6(6) . . ? F6 C37 C36 118.0(5) . . ? F12 C44 C43 119.9(6) . . ? F12 C44 C45 119.3(5) . . ? C43 C44 C45 120.7(5) . . ? C19 C18 C17 108.5(5) . . ? C19 C18 Zr2 72.9(3) . . ? C17 C18 Zr2 71.1(3) . . ? C26 C27 C28 108.0(5) . . ? C26 C27 Zr2 72.5(3) . . ? C28 C27 Zr2 72.7(3) . . ? C6 C2 C3 105.5(6) . . ? C6 C2 Si1 121.0(4) . . ? C3 C2 Si1 122.7(4) . . ? C6 C2 Zr1 75.3(3) . . ? C3 C2 Zr1 72.2(3) . . ? Si1 C2 Zr1 88.37(17) . . ? C11 C12 C13 110.5(5) . . ? C11 C12 Zr1 71.4(3) . . ? C13 C12 Zr1 76.0(3) . . ? C5 C4 C3 107.5(6) . . ? C5 C4 Zr1 75.6(3) . . ? C3 C4 Zr1 70.0(3) . . ? C53 C48 C49 113.8(5) . . ? C53 C48 B1 119.1(5) . . ? C49 C48 B1 126.3(4) . . ? F11 C43 C44 114.9(5) . . ? F11 C43 C42 121.5(5) . . ? C44 C43 C42 123.5(6) . . ? C17 C16 C20 105.8(5) . . ? C17 C16 Si4 120.9(5) . . ? C20 C16 Si4 123.1(4) . . ? C17 C16 Zr2 75.3(3) . . ? C20 C16 Zr2 73.0(3) . . ? Si4 C16 Zr2 88.52(18) . . ? F14 C46 C45 119.7(5) . . ? F14 C46 C47 122.1(4) . . ? C45 C46 C47 118.2(5) . . ? Zr2 C1 Zr1 173.8(2) . . ? C13 C14 C15 108.4(5) . . ? C13 C14 Zr1 75.6(3) . . ? C15 C14 Zr1 70.1(3) . . ? C41 C36 C37 112.9(5) . . ? C41 C36 B1 126.5(4) . . ? C37 C36 B1 119.3(5) . . ? C35 C30 C31 113.7(5) . . ? C35 C30 B1 120.4(5) . . ? C31 C30 B1 125.6(5) . . ? F7 C38 C39 119.9(6) . . ? F7 C38 C37 120.2(6) . . ? C39 C38 C37 119.9(5) . . ? F16 C49 C50 114.9(5) . . ? F16 C49 C48 121.0(4) . . ? C50 C49 C48 124.0(5) . . ? C42 C47 F15 120.8(4) . . ? C42 C47 C46 126.0(5) . . ? F15 C47 C46 113.2(5) . . ? C6 C5 C4 108.7(6) . . ? C6 C5 Zr1 71.9(3) . . ? C4 C5 Zr1 72.3(3) . . ? F9 C40 C39 121.6(6) . . ? F9 C40 C41 120.9(5) . . ? C39 C40 C41 117.4(5) . . ? C19 C20 C16 109.2(5) . . ? C19 C20 Zr2 76.9(4) . . ? C16 C20 Zr2 72.9(3) . . ? F18 C51 C52 120.9(5) . . ? F18 C51 C50 120.1(6) . . ? C52 C51 C50 119.0(5) . . ? C4 C3 C2 108.4(5) . . ? C4 C3 Zr1 76.9(3) . . ? C2 C3 Zr1 73.7(3) . . ? C16 C17 C18 108.8(5) . . ? C16 C17 Zr2 71.4(2) . . ? C18 C17 Zr2 76.3(3) . . ? C18 C19 C20 107.7(6) . . ? C18 C19 Zr2 75.3(4) . . ? C20 C19 Zr2 70.2(4) . . ? C25 C29 C28 110.2(5) . . ? C25 C29 Zr2 73.7(3) . . ? C28 C29 Zr2 76.3(3) . . ? F10 C41 C36 121.0(6) . . ? F10 C41 C40 114.1(5) . . ? C36 C41 C40 124.9(5) . . ? F17 C50 C49 121.0(5) . . ? F17 C50 C51 119.5(5) . . ? C49 C50 C51 119.5(5) . . ? C14 C13 C12 106.3(6) . . ? C14 C13 Zr1 72.3(4) . . ? C12 C13 Zr1 71.5(3) . . ? F19 C52 C51 120.5(5) . . ? F19 C52 C53 119.2(6) . . ? C51 C52 C53 120.3(5) . . ? C14 C15 C11 108.6(6) . . ? C14 C15 Zr1 77.0(3) . . ? C11 C15 Zr1 73.5(3) . . ? F4 C34 C35 121.6(6) . . ? F4 C34 C33 120.6(5) . . ? C35 C34 C33 117.7(6) . . ? C27 C26 C25 109.8(6) . . ? C27 C26 Zr2 75.3(3) . . ? C25 C26 Zr2 71.3(3) . . ? C12 C11 C15 106.2(5) . . ? C12 C11 Si2 125.2(4) . . ? C15 C11 Si2 118.7(5) . . ? C12 C11 Zr1 76.2(3) . . ? C15 C11 Zr1 72.5(3) . . ? Si2 C11 Zr1 88.5(2) . . ? C36 B1 C48 98.8(4) . . ? C36 B1 C30 115.3(5) . . ? C48 B1 C30 112.3(4) . . ? C36 B1 C42 114.7(4) . . ? C48 B1 C42 115.4(5) . . ? C30 B1 C42 101.1(4) . . ? C29 C28 C27 106.2(6) . . ? C29 C28 Zr2 70.5(3) . . ? C27 C28 Zr2 74.7(3) . . ? F20 C53 C52 116.4(5) . . ? F20 C53 C48 120.3(5) . . ? C52 C53 C48 123.3(6) . . ? F8 C39 C38 120.5(5) . . ? F8 C39 C40 119.4(6) . . ? C38 C39 C40 120.1(6) . . ? C33 C32 F2 119.7(5) . . ? C33 C32 C31 121.3(6) . . ? F2 C32 C31 119.0(6) . . ? C32 C33 F3 121.7(6) . . ? C32 C33 C34 119.1(5) . . ? F3 C33 C34 119.1(6) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.471 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.182