Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Roland Fischer' _publ_contact_author_address ; Department of Chemistry Lehrstuhl f\"ur Anorganische Chemie II - Organometallics and Materials Chemistry Ruhr-Universitaet Bochum Universitaetsstrasse 150 44780 Bochum GERMANY ; _publ_contact_author_email ROLAND.FISCHER@RUHR-UNI-BOCHUM.DE _publ_section_title ; Mixed Hydrazido Amido/Imido Complexes of Tantalum, Hafnium and Zirconium: Potential Precursors for Metal Nitride MOCVD ; loop_ _publ_author_name 'Roland Fischer' 'Arne Baunemann' 'Younsoo Kim' 'Manuela Winter' data_cvd3 _database_code_depnum_ccdc_archive 'CCDC 282095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H45 Cl N6 Si3 Zr' _chemical_formula_weight 520.51 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.019(8) _cell_length_b 10.197(6) _cell_length_c 15.690(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.83(4) _cell_angle_gamma 90.00 _cell_volume 2873(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2950 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (mo)x-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '586 images at 1.0 deg. in \w and 30 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31119 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 30.08 _reflns_number_total 8352 _reflns_number_gt 4897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0727P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8352 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.251145(19) 0.38347(3) 0.40388(2) 0.02027(11) Uani 1 1 d . . . Si2 Si 0.26027(8) 0.63162(11) 0.57159(8) 0.0399(3) Uani 1 1 d . . . Cl1 Cl 0.25550(7) 0.24578(10) 0.53506(7) 0.0419(3) Uani 1 1 d . . . Si3 Si 0.07295(7) 0.21211(13) 0.39046(10) 0.0469(4) Uani 1 1 d . . . Si1 Si 0.41786(8) 0.18441(16) 0.39616(11) 0.0618(4) Uani 1 1 d . . . N4 N 0.25818(18) 0.5585(3) 0.4722(2) 0.0288(7) Uani 1 1 d . . . N6 N 0.14511(17) 0.3118(3) 0.3659(2) 0.0303(7) Uani 1 1 d . . . N3 N 0.2164(2) 0.6002(3) 0.3945(2) 0.0403(9) Uani 1 1 d . . . N2 N 0.34744(17) 0.2947(3) 0.3684(2) 0.0306(7) Uani 1 1 d . . . N5 N 0.17717(19) 0.3237(3) 0.2846(2) 0.0362(8) Uani 1 1 d . . . N1 N 0.3525(2) 0.4187(4) 0.3270(2) 0.0417(9) Uani 1 1 d . . . C2 C 0.3537(3) 0.4085(5) 0.2337(3) 0.0463(12) Uani 1 1 d . . . H2A H 0.4039 0.4285 0.2176 0.070 Uiso 1 1 calc R . . H2B H 0.3181 0.4709 0.2059 0.070 Uiso 1 1 calc R . . H2C H 0.3400 0.3192 0.2154 0.070 Uiso 1 1 calc R . . C12 C 0.1383(3) 0.4123(5) 0.2233(3) 0.0501(13) Uani 1 1 d . . . H12A H 0.1107 0.3612 0.1782 0.075 Uiso 1 1 calc R . . H12B H 0.1746 0.4687 0.1978 0.075 Uiso 1 1 calc R . . H12C H 0.1035 0.4668 0.2525 0.075 Uiso 1 1 calc R . . C11 C 0.1898(2) 0.1919(4) 0.2452(3) 0.0433(11) Uani 1 1 d . . . H11A H 0.1544 0.1798 0.1949 0.065 Uiso 1 1 calc R . . H11B H 0.1824 0.1228 0.2871 0.065 Uiso 1 1 calc R . . H11C H 0.2408 0.1874 0.2280 0.065 Uiso 1 1 calc R . . C7 C 0.1388(3) 0.6379(5) 0.4085(3) 0.0539(13) Uani 1 1 d . . . H7A H 0.1330 0.7331 0.4020 0.081 Uiso 1 1 calc R . . H7B H 0.1278 0.6122 0.4663 0.081 Uiso 1 1 calc R . . H7C H 0.1042 0.5934 0.3665 0.081 Uiso 1 1 calc R . . C1 C 0.4155(3) 0.4990(5) 0.3650(4) 0.0609(15) Uani 1 1 d . . . H1A H 0.4539 0.5051 0.3246 0.091 Uiso 1 1 calc R . . H1B H 0.4366 0.4577 0.4181 0.091 Uiso 1 1 calc R . . H1C H 0.3977 0.5871 0.3776 0.091 Uiso 1 1 calc R . . C14 C 0.0431(3) 0.2784(5) 0.4920(3) 0.0545(14) Uani 1 1 d . . . H14A H 0.0851 0.2759 0.5360 0.082 Uiso 1 1 calc R . . H14B H 0.0021 0.2253 0.5105 0.082 Uiso 1 1 calc R . . H14C H 0.0264 0.3693 0.4833 0.082 Uiso 1 1 calc R . . C10 C 0.1745(3) 0.5980(5) 0.6263(3) 0.0593(14) Uani 1 1 d . . . H10A H 0.1317 0.6393 0.5943 0.089 Uiso 1 1 calc R . . H10B H 0.1803 0.6340 0.6845 0.089 Uiso 1 1 calc R . . H10C H 0.1665 0.5031 0.6290 0.089 Uiso 1 1 calc R . . C9 C 0.3405(3) 0.5516(6) 0.6344(3) 0.0662(16) Uani 1 1 d . . . H9A H 0.3863 0.5680 0.6066 0.099 Uiso 1 1 calc R . . H9B H 0.3318 0.4569 0.6372 0.099 Uiso 1 1 calc R . . H9C H 0.3456 0.5878 0.6925 0.099 Uiso 1 1 calc R . . C6 C 0.2519(3) 0.7023(4) 0.3478(3) 0.0532(14) Uani 1 1 d . . . H6A H 0.2259 0.7856 0.3542 0.080 Uiso 1 1 calc R . . H6B H 0.2499 0.6788 0.2871 0.080 Uiso 1 1 calc R . . H6C H 0.3040 0.7114 0.3706 0.080 Uiso 1 1 calc R . . C15 C 0.0982(4) 0.0380(5) 0.4060(4) 0.0758(19) Uani 1 1 d . . . H15A H 0.1399 0.0307 0.4500 0.114 Uiso 1 1 calc R . . H15B H 0.1128 0.0014 0.3521 0.114 Uiso 1 1 calc R . . H15C H 0.0553 -0.0105 0.4242 0.114 Uiso 1 1 calc R . . C13 C -0.0065(3) 0.2177(7) 0.3052(4) 0.082(2) Uani 1 1 d . . . H13A H -0.0224 0.3088 0.2955 0.124 Uiso 1 1 calc R . . H13B H -0.0483 0.1661 0.3234 0.124 Uiso 1 1 calc R . . H13C H 0.0095 0.1810 0.2520 0.124 Uiso 1 1 calc R . . C5 C 0.3691(4) 0.0243(5) 0.4058(5) 0.094(2) Uani 1 1 d . . . H5A H 0.3341 0.0308 0.4501 0.141 Uiso 1 1 calc R . . H5B H 0.4057 -0.0445 0.4213 0.141 Uiso 1 1 calc R . . H5C H 0.3418 0.0024 0.3510 0.141 Uiso 1 1 calc R . . C8 C 0.2772(5) 0.8111(5) 0.5704(4) 0.111(3) Uani 1 1 d . . . H8A H 0.2355 0.8547 0.5377 0.167 Uiso 1 1 calc R . . H8B H 0.3234 0.8289 0.5437 0.167 Uiso 1 1 calc R . . H8C H 0.2816 0.8444 0.6292 0.167 Uiso 1 1 calc R . . C4 C 0.4849(3) 0.1671(7) 0.3122(5) 0.089(2) Uani 1 1 d . . . H4A H 0.5120 0.2497 0.3070 0.133 Uiso 1 1 calc R . . H4B H 0.4576 0.1458 0.2573 0.133 Uiso 1 1 calc R . . H4C H 0.5204 0.0967 0.3283 0.133 Uiso 1 1 calc R . . C3 C 0.4697(4) 0.2310(9) 0.5005(5) 0.118(3) Uani 1 1 d . . . H3A H 0.4957 0.3144 0.4938 0.178 Uiso 1 1 calc R . . H3B H 0.5061 0.1626 0.5178 0.178 Uiso 1 1 calc R . . H3C H 0.4345 0.2404 0.5444 0.178 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 0.02228(17) 0.02188(18) 0.01674(17) 0.00351(14) 0.00210(12) -0.00033(15) Si2 0.0613(8) 0.0323(7) 0.0262(6) -0.0055(5) 0.0028(6) -0.0095(6) Cl1 0.0613(7) 0.0415(6) 0.0238(5) 0.0123(4) 0.0095(5) 0.0063(5) Si3 0.0312(6) 0.0493(8) 0.0624(9) -0.0228(7) 0.0171(6) -0.0168(6) Si1 0.0414(8) 0.0724(10) 0.0716(11) -0.0054(9) 0.0045(7) 0.0298(7) N4 0.0361(18) 0.0258(16) 0.0237(17) 0.0068(13) -0.0024(14) -0.0020(14) N6 0.0262(16) 0.0376(19) 0.0275(18) -0.0095(14) 0.0047(14) -0.0048(14) N3 0.060(2) 0.0311(19) 0.0286(19) 0.0041(15) -0.0043(17) 0.0024(17) N2 0.0276(16) 0.0367(19) 0.0284(18) 0.0023(15) 0.0077(14) 0.0001(14) N5 0.0386(19) 0.043(2) 0.0273(19) -0.0018(16) 0.0017(15) -0.0014(16) N1 0.037(2) 0.056(2) 0.032(2) 0.0031(17) 0.0105(16) -0.0105(17) C2 0.048(3) 0.065(3) 0.029(2) 0.001(2) 0.018(2) -0.014(2) C12 0.050(3) 0.062(3) 0.035(3) 0.002(2) -0.019(2) 0.014(2) C11 0.040(2) 0.048(3) 0.042(3) -0.018(2) 0.007(2) -0.008(2) C7 0.057(3) 0.053(3) 0.049(3) -0.003(2) -0.008(3) 0.025(2) C1 0.044(3) 0.072(4) 0.068(4) -0.010(3) 0.016(3) -0.027(3) C14 0.041(3) 0.062(3) 0.065(4) -0.017(3) 0.028(2) -0.012(2) C10 0.070(4) 0.067(3) 0.042(3) 0.007(3) 0.017(3) 0.017(3) C9 0.045(3) 0.110(5) 0.040(3) -0.005(3) -0.010(2) -0.009(3) C6 0.093(4) 0.030(2) 0.038(3) 0.008(2) 0.012(3) -0.004(2) C15 0.093(5) 0.039(3) 0.103(5) -0.008(3) 0.051(4) -0.020(3) C13 0.032(3) 0.122(5) 0.093(5) -0.056(4) 0.007(3) -0.019(3) C5 0.123(6) 0.048(3) 0.117(6) 0.026(4) 0.041(5) 0.044(4) C8 0.237(10) 0.048(4) 0.047(4) -0.014(3) 0.006(5) -0.038(5) C4 0.048(3) 0.105(5) 0.117(6) -0.034(5) 0.021(4) 0.022(3) C3 0.080(5) 0.171(8) 0.095(6) -0.002(5) -0.044(4) 0.062(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N2 2.074(3) . ? Zr1 N4 2.081(3) . ? Zr1 N6 2.085(3) . ? Zr1 N5 2.287(4) . ? Zr1 N3 2.298(4) . ? Zr1 N1 2.300(4) . ? Zr1 Cl1 2.4872(13) . ? Si2 N4 1.725(3) . ? Si2 C8 1.855(6) . ? Si2 C10 1.862(5) . ? Si2 C9 1.868(5) . ? Si3 N6 1.720(3) . ? Si3 C15 1.844(5) . ? Si3 C14 1.851(5) . ? Si3 C13 1.877(6) . ? Si1 N2 1.724(3) . ? Si1 C5 1.867(7) . ? Si1 C4 1.870(6) . ? Si1 C3 1.877(7) . ? N4 N3 1.443(4) . ? N6 N5 1.449(5) . ? N3 C6 1.453(6) . ? N3 C7 1.485(6) . ? N2 N1 1.428(5) . ? N5 C12 1.455(5) . ? N5 C11 1.504(5) . ? N1 C2 1.470(5) . ? N1 C1 1.483(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zr1 N4 119.77(13) . . ? N2 Zr1 N6 122.53(13) . . ? N4 Zr1 N6 117.54(12) . . ? N2 Zr1 N5 96.18(13) . . ? N4 Zr1 N5 131.03(12) . . ? N6 Zr1 N5 38.36(12) . . ? N2 Zr1 N3 129.20(13) . . ? N4 Zr1 N3 38.06(12) . . ? N6 Zr1 N3 94.60(14) . . ? N5 Zr1 N3 93.83(13) . . ? N2 Zr1 N1 37.66(13) . . ? N4 Zr1 N1 96.87(13) . . ? N6 Zr1 N1 130.85(13) . . ? N5 Zr1 N1 92.67(13) . . ? N3 Zr1 N1 92.32(14) . . ? N2 Zr1 Cl1 90.38(10) . . ? N4 Zr1 Cl1 93.51(9) . . ? N6 Zr1 Cl1 90.18(10) . . ? N5 Zr1 Cl1 120.16(10) . . ? N3 Zr1 Cl1 125.82(10) . . ? N1 Zr1 Cl1 123.42(10) . . ? N4 Si2 C8 114.1(2) . . ? N4 Si2 C10 112.4(2) . . ? C8 Si2 C10 109.2(3) . . ? N4 Si2 C9 104.2(2) . . ? C8 Si2 C9 108.4(3) . . ? C10 Si2 C9 108.2(3) . . ? N6 Si3 C15 114.6(2) . . ? N6 Si3 C14 104.86(19) . . ? C15 Si3 C14 108.9(3) . . ? N6 Si3 C13 111.6(3) . . ? C15 Si3 C13 106.8(3) . . ? C14 Si3 C13 110.1(3) . . ? N2 Si1 C5 104.4(2) . . ? N2 Si1 C4 112.9(3) . . ? C5 Si1 C4 108.1(3) . . ? N2 Si1 C3 110.9(3) . . ? C5 Si1 C3 110.8(4) . . ? C4 Si1 C3 109.5(3) . . ? N3 N4 Si2 127.4(3) . . ? N3 N4 Zr1 79.16(19) . . ? Si2 N4 Zr1 146.32(18) . . ? N5 N6 Si3 127.7(2) . . ? N5 N6 Zr1 78.38(19) . . ? Si3 N6 Zr1 146.6(2) . . ? N4 N3 C6 114.6(4) . . ? N4 N3 C7 112.5(3) . . ? C6 N3 C7 110.5(4) . . ? N4 N3 Zr1 62.78(17) . . ? C6 N3 Zr1 126.3(3) . . ? C7 N3 Zr1 119.7(3) . . ? N1 N2 Si1 128.2(3) . . ? N1 N2 Zr1 79.8(2) . . ? Si1 N2 Zr1 146.3(2) . . ? N6 N5 C12 115.4(3) . . ? N6 N5 C11 111.9(3) . . ? C12 N5 C11 111.3(4) . . ? N6 N5 Zr1 63.26(17) . . ? C12 N5 Zr1 126.2(3) . . ? C11 N5 Zr1 118.4(3) . . ? N2 N1 C2 113.4(4) . . ? N2 N1 C1 112.5(4) . . ? C2 N1 C1 111.4(4) . . ? N2 N1 Zr1 62.55(17) . . ? C2 N1 Zr1 126.2(3) . . ? C1 N1 Zr1 119.4(3) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N5 C12 H12A 109.5 . . ? N5 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N5 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si3 C14 H14A 109.5 . . ? Si3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C13 H13A 109.5 . . ? Si3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? 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 C8 Si2 N4 N3 -49.4(5) . . . . ? C10 Si2 N4 N3 75.7(4) . . . . ? C9 Si2 N4 N3 -167.4(3) . . . . ? C8 Si2 N4 Zr1 174.6(4) . . . . ? C10 Si2 N4 Zr1 -60.3(4) . . . . ? C9 Si2 N4 Zr1 56.6(4) . . . . ? N2 Zr1 N4 N3 116.8(2) . . . . ? N6 Zr1 N4 N3 -58.7(2) . . . . ? N5 Zr1 N4 N3 -14.7(3) . . . . ? N1 Zr1 N4 N3 85.0(2) . . . . ? Cl1 Zr1 N4 N3 -150.8(2) . . . . ? N2 Zr1 N4 Si2 -97.5(4) . . . . ? N6 Zr1 N4 Si2 87.0(4) . . . . ? N5 Zr1 N4 Si2 131.1(3) . . . . ? N3 Zr1 N4 Si2 145.8(5) . . . . ? N1 Zr1 N4 Si2 -129.3(3) . . . . ? Cl1 Zr1 N4 Si2 -5.0(3) . . . . ? C15 Si3 N6 N5 76.4(4) . . . . ? C14 Si3 N6 N5 -164.3(3) . . . . ? C13 Si3 N6 N5 -45.2(4) . . . . ? C15 Si3 N6 Zr1 -58.9(4) . . . . ? C14 Si3 N6 Zr1 60.4(4) . . . . ? C13 Si3 N6 Zr1 179.5(3) . . . . ? N2 Zr1 N6 N5 -53.1(2) . . . . ? N4 Zr1 N6 N5 122.3(2) . . . . ? N3 Zr1 N6 N5 90.4(2) . . . . ? N1 Zr1 N6 N5 -6.7(3) . . . . ? Cl1 Zr1 N6 N5 -143.67(19) . . . . ? N2 Zr1 N6 Si3 92.3(3) . . . . ? N4 Zr1 N6 Si3 -92.3(3) . . . . ? N5 Zr1 N6 Si3 145.4(4) . . . . ? N3 Zr1 N6 Si3 -124.3(3) . . . . ? N1 Zr1 N6 Si3 138.7(3) . . . . ? Cl1 Zr1 N6 Si3 1.7(3) . . . . ? Si2 N4 N3 C6 83.3(4) . . . . ? Zr1 N4 N3 C6 -119.8(3) . . . . ? Si2 N4 N3 C7 -44.0(5) . . . . ? Zr1 N4 N3 C7 112.9(3) . . . . ? Si2 N4 N3 Zr1 -156.9(3) . . . . ? N2 Zr1 N3 N4 -89.9(2) . . . . ? N6 Zr1 N3 N4 130.5(2) . . . . ? N5 Zr1 N3 N4 169.0(2) . . . . ? N1 Zr1 N3 N4 -98.2(2) . . . . ? Cl1 Zr1 N3 N4 37.0(2) . . . . ? N2 Zr1 N3 C6 11.9(4) . . . . ? N4 Zr1 N3 C6 101.7(4) . . . . ? N6 Zr1 N3 C6 -127.8(4) . . . . ? N5 Zr1 N3 C6 -89.3(4) . . . . ? N1 Zr1 N3 C6 3.5(4) . . . . ? Cl1 Zr1 N3 C6 138.7(3) . . . . ? N2 Zr1 N3 C7 168.5(3) . . . . ? N4 Zr1 N3 C7 -101.6(4) . . . . ? N6 Zr1 N3 C7 28.9(3) . . . . ? N5 Zr1 N3 C7 67.3(3) . . . . ? N1 Zr1 N3 C7 160.2(3) . . . . ? Cl1 Zr1 N3 C7 -64.7(3) . . . . ? C5 Si1 N2 N1 -158.0(4) . . . . ? C4 Si1 N2 N1 -40.8(4) . . . . ? C3 Si1 N2 N1 82.6(5) . . . . ? C5 Si1 N2 Zr1 61.3(4) . . . . ? C4 Si1 N2 Zr1 178.6(4) . . . . ? C3 Si1 N2 Zr1 -58.0(5) . . . . ? N4 Zr1 N2 N1 -59.0(2) . . . . ? N6 Zr1 N2 N1 116.3(2) . . . . ? N5 Zr1 N2 N1 86.4(2) . . . . ? N3 Zr1 N2 N1 -13.7(3) . . . . ? Cl1 Zr1 N2 N1 -153.2(2) . . . . ? N4 Zr1 N2 Si1 90.6(4) . . . . ? N6 Zr1 N2 Si1 -94.1(4) . . . . ? N5 Zr1 N2 Si1 -124.1(3) . . . . ? N3 Zr1 N2 Si1 135.9(3) . . . . ? N1 Zr1 N2 Si1 149.6(5) . . . . ? Cl1 Zr1 N2 Si1 -3.7(3) . . . . ? Si3 N6 N5 C12 83.8(4) . . . . ? Zr1 N6 N5 C12 -119.5(3) . . . . ? Si3 N6 N5 C11 -44.8(4) . . . . ? Zr1 N6 N5 C11 111.9(3) . . . . ? Si3 N6 N5 Zr1 -156.7(3) . . . . ? N2 Zr1 N5 N6 137.3(2) . . . . ? N4 Zr1 N5 N6 -83.6(2) . . . . ? N3 Zr1 N5 N6 -92.6(2) . . . . ? N1 Zr1 N5 N6 174.9(2) . . . . ? Cl1 Zr1 N5 N6 43.3(2) . . . . ? N2 Zr1 N5 C12 -119.6(4) . . . . ? N4 Zr1 N5 C12 19.5(4) . . . . ? N6 Zr1 N5 C12 103.1(4) . . . . ? N3 Zr1 N5 C12 10.5(4) . . . . ? N1 Zr1 N5 C12 -82.0(4) . . . . ? Cl1 Zr1 N5 C12 146.3(3) . . . . ? N2 Zr1 N5 C11 35.7(3) . . . . ? N4 Zr1 N5 C11 174.8(3) . . . . ? N6 Zr1 N5 C11 -101.6(3) . . . . ? N3 Zr1 N5 C11 165.8(3) . . . . ? N1 Zr1 N5 C11 73.3(3) . . . . ? Cl1 Zr1 N5 C11 -58.4(3) . . . . ? Si1 N2 N1 C2 81.0(4) . . . . ? Zr1 N2 N1 C2 -120.0(3) . . . . ? Si1 N2 N1 C1 -46.5(5) . . . . ? Zr1 N2 N1 C1 112.5(3) . . . . ? Si1 N2 N1 Zr1 -159.0(3) . . . . ? N4 Zr1 N1 N2 131.5(2) . . . . ? N6 Zr1 N1 N2 -92.5(2) . . . . ? N5 Zr1 N1 N2 -96.6(2) . . . . ? N3 Zr1 N1 N2 169.4(2) . . . . ? Cl1 Zr1 N1 N2 32.7(2) . . . . ? N2 Zr1 N1 C2 100.1(4) . . . . ? N4 Zr1 N1 C2 -128.4(4) . . . . ? N6 Zr1 N1 C2 7.6(4) . . . . ? N5 Zr1 N1 C2 3.4(4) . . . . ? N3 Zr1 N1 C2 -90.5(4) . . . . ? Cl1 Zr1 N1 C2 132.7(3) . . . . ? N2 Zr1 N1 C1 -101.6(4) . . . . ? N4 Zr1 N1 C1 29.8(4) . . . . ? N6 Zr1 N1 C1 165.9(3) . . . . ? N5 Zr1 N1 C1 161.7(4) . . . . ? N3 Zr1 N1 C1 67.8(4) . . . . ? Cl1 Zr1 N1 C1 -69.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.944 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.103 # Attachment 'Compound 5.cif' data_70scale _database_code_depnum_ccdc_archive 'CCDC 282096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H72 N10 Si2 Ta2' _chemical_formula_weight 943.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3189(7) _cell_length_b 33.5381(18) _cell_length_c 13.6538(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.595(6) _cell_angle_gamma 90.00 _cell_volume 4164.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 4724 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour prism _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 5.336 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.320 _exptl_absorpt_correction_T_max 0.682 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (mo)x-ray source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1102 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32885 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9121 _reflns_number_gt 6980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0303P)^2^+55.9900P] 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 9121 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Ta1 Ta 0.81941(4) 0.222537(9) 0.04693(3) 0.01423(9) Uani 1 1 d . . . Ta2 Ta 1.34028(4) -0.041619(10) 0.23738(3) 0.01854(10) Uani 1 1 d . . . Si1 Si 1.1974(3) 0.19818(7) 0.05185(18) 0.0187(5) Uani 1 1 d . . . Si2 Si 1.2227(3) 0.03621(7) 0.37556(19) 0.0259(6) Uani 1 1 d . . . N15 N 0.6823(8) 0.2005(2) -0.0739(5) 0.0204(16) Uani 1 1 d . . . N11 N 1.0302(8) 0.2232(2) 0.0314(5) 0.0161(14) Uani 1 1 d . . . N14 N 0.7557(8) 0.27563(19) 0.0916(5) 0.0166(15) Uani 1 1 d . . . N13 N 0.8043(8) 0.1889(2) 0.1455(5) 0.0160(14) Uani 1 1 d . . . N21 N 1.3231(9) 0.0123(2) 0.2990(5) 0.0221(16) Uani 1 1 d . . . N22 N 1.3838(9) 0.0275(2) 0.2180(6) 0.0269(18) Uani 1 1 d . . . N12 N 0.9753(8) 0.2518(2) -0.0468(5) 0.0187(15) Uani 1 1 d . . . N24 N 1.2143(10) -0.0460(2) 0.0987(6) 0.0301(19) Uani 1 1 d . . . N25 N 1.5478(8) -0.0597(2) 0.2447(6) 0.0251(17) Uani 1 1 d . . . N23 N 1.2648(8) -0.0773(2) 0.3093(5) 0.0207(16) Uani 1 1 d . . . C131 C 0.7917(10) 0.1613(2) 0.2252(7) 0.0199(18) Uani 1 1 d . . . C142 C 0.7184(11) 0.2838(3) 0.1872(7) 0.024(2) Uani 1 1 d . . . H14A H 0.7767 0.3064 0.2195 0.036 Uiso 1 1 calc R . . H14B H 0.7396 0.2602 0.2304 0.036 Uiso 1 1 calc R . . H14C H 0.6135 0.2903 0.1763 0.036 Uiso 1 1 calc R . . C231 C 1.2022(11) -0.1046(3) 0.3691(7) 0.024(2) Uani 1 1 d . . . C134 C 0.8353(11) 0.1190(3) 0.1995(8) 0.028(2) Uani 1 1 d . . . H13A H 0.7681 0.1098 0.1381 0.042 Uiso 1 1 calc R . . H13B H 0.8296 0.1009 0.2549 0.042 Uiso 1 1 calc R . . H13C H 0.9361 0.1193 0.1891 0.042 Uiso 1 1 calc R . . C252 C 1.6192(11) -0.0947(3) 0.2982(8) 0.032(2) Uani 1 1 d . . . H25A H 1.6491 -0.1130 0.2503 0.048 Uiso 1 1 calc R . . H25B H 1.5503 -0.1082 0.3319 0.048 Uiso 1 1 calc R . . H25C H 1.7061 -0.0862 0.3482 0.048 Uiso 1 1 calc R . . C133 C 0.6318(10) 0.1613(3) 0.2353(7) 0.023(2) Uani 1 1 d . . . H13D H 0.6049 0.1880 0.2543 0.035 Uiso 1 1 calc R . . H13E H 0.6197 0.1421 0.2871 0.035 Uiso 1 1 calc R . . H13F H 0.5679 0.1537 0.1711 0.035 Uiso 1 1 calc R . . C122 C 1.0421(10) 0.2912(3) -0.0261(7) 0.024(2) Uani 1 1 d . . . H12A H 1.0400 0.2991 0.0427 0.035 Uiso 1 1 calc R . . H12B H 0.9869 0.3106 -0.0733 0.035 Uiso 1 1 calc R . . H12C H 1.1441 0.2902 -0.0337 0.035 Uiso 1 1 calc R . . C141 C 0.7214(11) 0.3101(3) 0.0274(7) 0.025(2) Uani 1 1 d . . . H14D H 0.6197 0.3184 0.0246 0.037 Uiso 1 1 calc R . . H14E H 0.7331 0.3034 -0.0403 0.037 Uiso 1 1 calc R . . H14F H 0.7882 0.3320 0.0543 0.037 Uiso 1 1 calc R . . C112 C 1.2185(11) 0.1770(3) 0.1800(7) 0.026(2) Uani 1 1 d . . . H11A H 1.2180 0.1987 0.2281 0.038 Uiso 1 1 calc R . . H11B H 1.3117 0.1625 0.1980 0.038 Uiso 1 1 calc R . . H11C H 1.1368 0.1588 0.1813 0.038 Uiso 1 1 calc R . . C152 C 0.6265(11) 0.2246(3) -0.1620(7) 0.025(2) Uani 1 1 d . . . H15A H 0.6379 0.2101 -0.2222 0.038 Uiso 1 1 calc R . . H15B H 0.6816 0.2497 -0.1571 0.038 Uiso 1 1 calc R . . H15C H 0.5221 0.2304 -0.1665 0.038 Uiso 1 1 calc R . . C151 C 0.6071(12) 0.1618(3) -0.0833(7) 0.030(2) Uani 1 1 d . . . H15D H 0.5011 0.1660 -0.0911 0.045 Uiso 1 1 calc R . . H15E H 0.6443 0.1459 -0.0228 0.045 Uiso 1 1 calc R . . H15F H 0.6256 0.1477 -0.1421 0.045 Uiso 1 1 calc R . . C121 C 0.9856(11) 0.2381(3) -0.1470(7) 0.025(2) Uani 1 1 d . . . H12D H 1.0892 0.2351 -0.1497 0.038 Uiso 1 1 calc R . . H12E H 0.9390 0.2577 -0.1971 0.038 Uiso 1 1 calc R . . H12F H 0.9354 0.2124 -0.1611 0.038 Uiso 1 1 calc R . . C213 C 1.2750(14) 0.0123(3) 0.5014(7) 0.037(3) Uani 1 1 d . . . H21A H 1.2734 -0.0167 0.4937 0.056 Uiso 1 1 calc R . . H21B H 1.2051 0.0202 0.5420 0.056 Uiso 1 1 calc R . . H21C H 1.3742 0.0209 0.5348 0.056 Uiso 1 1 calc R . . C132 C 0.8918(11) 0.1756(3) 0.3238(7) 0.027(2) Uani 1 1 d . . . H13G H 0.9933 0.1775 0.3152 0.041 Uiso 1 1 calc R . . H13H H 0.8871 0.1566 0.3774 0.041 Uiso 1 1 calc R . . H13I H 0.8588 0.2019 0.3414 0.041 Uiso 1 1 calc R . . C111 C 1.1952(12) 0.1555(3) -0.0378(8) 0.035(2) Uani 1 1 d . . . H11D H 1.1065 0.1395 -0.0407 0.053 Uiso 1 1 calc R . . H11E H 1.2825 0.1389 -0.0146 0.053 Uiso 1 1 calc R . . H11F H 1.1957 0.1660 -0.1047 0.053 Uiso 1 1 calc R . . C212 C 1.2595(14) 0.0912(3) 0.3908(8) 0.040(3) Uani 1 1 d . . . H21X H 1.3654 0.0957 0.4135 0.060 Uiso 1 1 calc R . . H21Y H 1.2083 0.1019 0.4405 0.060 Uiso 1 1 calc R . . H21Z H 1.2239 0.1046 0.3263 0.060 Uiso 1 1 calc R . . C234 C 1.3057(12) -0.1096(3) 0.4710(7) 0.032(2) Uani 1 1 d . . . H23A H 1.3996 -0.1205 0.4620 0.048 Uiso 1 1 calc R . . H23B H 1.2618 -0.1280 0.5121 0.048 Uiso 1 1 calc R . . H23C H 1.3225 -0.0837 0.5045 0.048 Uiso 1 1 calc R . . C222 C 1.2805(15) 0.0521(3) 0.1466(8) 0.042(3) Uani 1 1 d . . . H22A H 1.1861 0.0382 0.1270 0.064 Uiso 1 1 calc R . . H22B H 1.3205 0.0570 0.0870 0.064 Uiso 1 1 calc R . . H22C H 1.2660 0.0776 0.1782 0.064 Uiso 1 1 calc R . . C233 C 1.1822(13) -0.1450(3) 0.3156(8) 0.035(3) Uani 1 1 d . . . H23D H 1.1146 -0.1421 0.2502 0.053 Uiso 1 1 calc R . . H23E H 1.1417 -0.1643 0.3564 0.053 Uiso 1 1 calc R . . H23F H 1.2776 -0.1546 0.3061 0.053 Uiso 1 1 calc R . . C221 C 1.5226(14) 0.0486(3) 0.2552(9) 0.044(3) Uani 1 1 d . . . H22D H 1.5033 0.0734 0.2877 0.066 Uiso 1 1 calc R . . H22E H 1.5688 0.0546 0.1990 0.066 Uiso 1 1 calc R . . H22F H 1.5885 0.0317 0.3039 0.066 Uiso 1 1 calc R . . C251 C 1.6427(13) -0.0412(4) 0.1875(9) 0.044(3) Uani 1 1 d . . . H25D H 1.7309 -0.0309 0.2334 0.067 Uiso 1 1 calc R . . H25E H 1.5905 -0.0191 0.1480 0.067 Uiso 1 1 calc R . . H25F H 1.6714 -0.0609 0.1424 0.067 Uiso 1 1 calc R . . C211 C 1.0199(13) 0.0293(3) 0.3238(8) 0.038(3) Uani 1 1 d . . . H21D H 0.9927 0.0415 0.2571 0.057 Uiso 1 1 calc R . . H21E H 0.9646 0.0421 0.3686 0.057 Uiso 1 1 calc R . . H21F H 0.9969 0.0008 0.3187 0.057 Uiso 1 1 calc R . . C241 C 1.2608(16) -0.0296(4) 0.0116(8) 0.048(3) Uani 1 1 d . . . H24A H 1.2768 -0.0513 -0.0327 0.072 Uiso 1 1 calc R . . H24B H 1.3525 -0.0146 0.0339 0.072 Uiso 1 1 calc R . . H24C H 1.1844 -0.0117 -0.0249 0.072 Uiso 1 1 calc R . . C232 C 1.0533(12) -0.0891(3) 0.3828(10) 0.043(3) Uani 1 1 d . . . H23G H 1.0685 -0.0655 0.4261 0.065 Uiso 1 1 calc R . . H23H H 1.0041 -0.1099 0.4139 0.065 Uiso 1 1 calc R . . H23I H 0.9920 -0.0820 0.3173 0.065 Uiso 1 1 calc R . . C242 C 1.0824(13) -0.0701(4) 0.0684(9) 0.045(3) Uani 1 1 d . . . H24D H 1.0008 -0.0531 0.0348 0.068 Uiso 1 1 calc R . . H24E H 1.0578 -0.0824 0.1278 0.068 Uiso 1 1 calc R . . H24F H 1.0997 -0.0910 0.0222 0.068 Uiso 1 1 calc R . . C110 C 1.3538(11) 0.2317(3) 0.0444(8) 0.029(2) Uani 1 1 d . . . H11X H 1.3439 0.2410 -0.0248 0.044 Uiso 1 1 calc R . . H11Y H 1.4466 0.2172 0.0655 0.044 Uiso 1 1 calc R . . H11Z H 1.3533 0.2547 0.0886 0.044 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 Ta1 0.01412(19) 0.01505(16) 0.01449(17) 0.00030(12) 0.00527(12) -0.00041(13) Ta2 0.0211(2) 0.01563(17) 0.01846(18) 0.00044(13) 0.00331(13) -0.00298(15) Si1 0.0158(13) 0.0194(11) 0.0225(12) -0.0001(9) 0.0076(9) -0.0010(10) Si2 0.0338(16) 0.0168(12) 0.0250(13) -0.0013(10) 0.0016(11) 0.0028(11) N15 0.019(4) 0.020(4) 0.021(4) 0.000(3) 0.003(3) 0.000(3) N11 0.011(4) 0.015(3) 0.024(4) 0.002(3) 0.008(3) -0.001(3) N14 0.019(4) 0.011(3) 0.021(4) 0.001(3) 0.007(3) 0.003(3) N13 0.010(4) 0.018(3) 0.020(4) -0.003(3) 0.004(3) -0.006(3) N21 0.030(5) 0.013(3) 0.022(4) 0.003(3) 0.003(3) -0.003(3) N22 0.038(5) 0.017(4) 0.022(4) 0.010(3) -0.002(3) -0.005(3) N12 0.025(4) 0.016(3) 0.017(4) 0.003(3) 0.008(3) -0.005(3) N24 0.040(5) 0.028(4) 0.019(4) -0.003(3) 0.000(3) -0.010(4) N25 0.016(4) 0.025(4) 0.034(5) -0.002(3) 0.004(3) -0.005(3) N23 0.018(4) 0.020(4) 0.023(4) 0.001(3) 0.002(3) 0.001(3) C131 0.017(5) 0.016(4) 0.027(5) 0.004(3) 0.006(4) 0.000(3) C142 0.029(6) 0.023(4) 0.023(5) -0.002(4) 0.011(4) 0.005(4) C231 0.026(6) 0.019(4) 0.028(5) 0.006(4) 0.010(4) -0.005(4) C134 0.025(6) 0.019(4) 0.046(6) 0.006(4) 0.019(4) 0.004(4) C252 0.020(6) 0.033(5) 0.043(6) -0.002(4) 0.007(4) 0.003(4) C133 0.026(6) 0.019(4) 0.028(5) 0.000(4) 0.013(4) -0.001(4) C122 0.021(5) 0.031(5) 0.022(5) 0.001(4) 0.013(4) 0.001(4) C141 0.028(6) 0.020(4) 0.028(5) 0.003(4) 0.010(4) 0.004(4) C112 0.016(5) 0.026(5) 0.037(5) 0.009(4) 0.010(4) 0.004(4) C152 0.020(5) 0.031(5) 0.018(4) -0.002(4) -0.008(4) 0.003(4) C151 0.038(6) 0.024(5) 0.028(5) -0.005(4) 0.005(4) -0.014(4) C121 0.024(6) 0.031(5) 0.024(5) 0.008(4) 0.013(4) 0.001(4) C213 0.059(8) 0.031(5) 0.022(5) -0.001(4) 0.010(5) 0.003(5) C132 0.023(5) 0.035(5) 0.024(5) 0.008(4) 0.002(4) -0.010(4) C111 0.027(6) 0.040(6) 0.038(6) -0.003(5) 0.006(4) 0.002(5) C212 0.059(8) 0.020(5) 0.039(6) -0.004(4) 0.004(5) 0.005(5) C234 0.042(7) 0.030(5) 0.025(5) 0.005(4) 0.008(4) 0.001(5) C222 0.073(9) 0.022(5) 0.028(6) 0.012(4) 0.002(5) 0.011(5) C233 0.051(7) 0.018(5) 0.039(6) 0.000(4) 0.015(5) -0.010(5) C221 0.060(8) 0.033(6) 0.039(6) -0.005(5) 0.011(5) -0.022(6) C251 0.034(7) 0.051(7) 0.058(8) 0.006(6) 0.031(6) -0.003(6) C211 0.043(7) 0.030(5) 0.036(6) 0.005(4) -0.002(5) -0.011(5) C241 0.075(10) 0.043(6) 0.022(5) 0.000(5) 0.003(5) -0.016(6) C232 0.029(7) 0.043(6) 0.066(8) 0.019(6) 0.029(6) 0.006(5) C242 0.043(8) 0.050(7) 0.037(6) -0.005(5) -0.005(5) -0.015(6) C110 0.026(6) 0.026(5) 0.035(6) 0.005(4) 0.006(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N13 1.786(7) . ? Ta1 N15 1.995(7) . ? Ta1 N14 2.013(7) . ? Ta1 N11 2.021(7) . ? Ta1 N12 2.350(7) . ? Ta2 N23 1.787(7) . ? Ta2 N24 2.003(8) . ? Ta2 N25 2.008(8) . ? Ta2 N21 2.015(7) . ? Ta2 N22 2.378(7) . ? Si1 N11 1.738(7) . ? Si1 C112 1.858(9) . ? Si1 C110 1.862(10) . ? Si1 C111 1.880(11) . ? Si2 N21 1.743(8) . ? Si2 C213 1.862(10) . ? Si2 C212 1.878(10) . ? Si2 C211 1.882(11) . ? N15 C152 1.449(11) . ? N15 C151 1.467(11) . ? N11 N12 1.443(10) . ? N14 C141 1.444(11) . ? N14 C142 1.448(11) . ? N13 C131 1.452(11) . ? N21 N22 1.441(11) . ? N22 C221 1.464(14) . ? N22 C222 1.465(12) . ? N12 C122 1.460(11) . ? N12 C121 1.466(11) . ? N24 C242 1.453(13) . ? N24 C241 1.461(14) . ? N25 C251 1.442(13) . ? N25 C252 1.462(12) . ? N23 C231 1.432(11) . ? C131 C133 1.526(13) . ? C131 C132 1.538(12) . ? C131 C134 1.539(12) . ? C142 H14A 0.9800 . ? C142 H14B 0.9800 . ? C142 H14C 0.9800 . ? C231 C234 1.520(13) . ? C231 C232 1.532(14) . ? C231 C233 1.532(13) . ? C134 H13A 0.9800 . ? C134 H13B 0.9800 . ? C134 H13C 0.9800 . ? C252 H25A 0.9800 . ? C252 H25B 0.9800 . ? C252 H25C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C133 H13F 0.9800 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C141 H14D 0.9800 . ? C141 H14E 0.9800 . ? C141 H14F 0.9800 . ? C112 H11A 0.9800 . ? C112 H11B 0.9800 . ? C112 H11C 0.9800 . ? C152 H15A 0.9800 . ? C152 H15B 0.9800 . ? C152 H15C 0.9800 . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C151 H15F 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C213 H21A 0.9800 . ? C213 H21B 0.9800 . ? C213 H21C 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C132 H13I 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C212 H21X 0.9800 . ? C212 H21Y 0.9800 . ? C212 H21Z 0.9800 . ? C234 H23A 0.9800 . ? C234 H23B 0.9800 . ? C234 H23C 0.9800 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C233 H23D 0.9800 . ? C233 H23E 0.9800 . ? C233 H23F 0.9800 . ? C221 H22D 0.9800 . ? C221 H22E 0.9800 . ? C221 H22F 0.9800 . ? C251 H25D 0.9800 . ? C251 H25E 0.9800 . ? C251 H25F 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C211 H21F 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C232 H23G 0.9800 . ? C232 H23H 0.9800 . ? C232 H23I 0.9800 . ? C242 H24D 0.9800 . ? C242 H24E 0.9800 . ? C242 H24F 0.9800 . ? C110 H11X 0.9800 . ? C110 H11Y 0.9800 . ? C110 H11Z 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Ta1 N15 104.3(3) . . ? N13 Ta1 N14 104.7(3) . . ? N15 Ta1 N14 113.6(3) . . ? N13 Ta1 N11 108.9(3) . . ? N15 Ta1 N11 112.3(3) . . ? N14 Ta1 N11 112.3(3) . . ? N13 Ta1 N12 146.6(3) . . ? N15 Ta1 N12 93.7(3) . . ? N14 Ta1 N12 93.1(3) . . ? N11 Ta1 N12 37.6(3) . . ? N23 Ta2 N24 104.5(3) . . ? N23 Ta2 N25 105.1(3) . . ? N24 Ta2 N25 112.6(3) . . ? N23 Ta2 N21 107.2(3) . . ? N24 Ta2 N21 112.2(3) . . ? N25 Ta2 N21 114.4(3) . . ? N23 Ta2 N22 144.2(3) . . ? N24 Ta2 N22 92.6(3) . . ? N25 Ta2 N22 96.6(3) . . ? N21 Ta2 N22 37.2(3) . . ? N11 Si1 C112 104.0(4) . . ? N11 Si1 C110 112.6(4) . . ? C112 Si1 C110 111.0(4) . . ? N11 Si1 C111 112.4(4) . . ? C112 Si1 C111 107.8(5) . . ? C110 Si1 C111 108.8(5) . . ? N21 Si2 C213 106.8(4) . . ? N21 Si2 C212 114.2(5) . . ? C213 Si2 C212 108.4(5) . . ? N21 Si2 C211 110.1(5) . . ? C213 Si2 C211 109.5(5) . . ? C212 Si2 C211 107.8(5) . . ? C152 N15 C151 110.1(7) . . ? C152 N15 Ta1 122.0(6) . . ? C151 N15 Ta1 127.4(6) . . ? N12 N11 Si1 126.9(5) . . ? N12 N11 Ta1 83.6(4) . . ? Si1 N11 Ta1 146.7(4) . . ? C141 N14 C142 109.3(7) . . ? C141 N14 Ta1 124.4(6) . . ? C142 N14 Ta1 125.8(5) . . ? C131 N13 Ta1 179.6(6) . . ? N22 N21 Si2 130.5(6) . . ? N22 N21 Ta2 85.2(5) . . ? Si2 N21 Ta2 139.9(4) . . ? N21 N22 C221 111.6(7) . . ? N21 N22 C222 113.5(8) . . ? C221 N22 C222 111.2(8) . . ? N21 N22 Ta2 57.6(4) . . ? C221 N22 Ta2 126.2(7) . . ? C222 N22 Ta2 121.4(6) . . ? N11 N12 C122 113.0(7) . . ? N11 N12 C121 113.4(7) . . ? C122 N12 C121 110.6(7) . . ? N11 N12 Ta1 58.8(4) . . ? C122 N12 Ta1 124.1(5) . . ? C121 N12 Ta1 123.5(5) . . ? C242 N24 C241 111.1(8) . . ? C242 N24 Ta2 126.5(7) . . ? C241 N24 Ta2 121.7(7) . . ? C251 N25 C252 110.5(8) . . ? C251 N25 Ta2 122.7(7) . . ? C252 N25 Ta2 126.6(6) . . ? C231 N23 Ta2 177.6(7) . . ? N13 C131 C133 108.0(7) . . ? N13 C131 C132 108.9(7) . . ? C133 C131 C132 109.8(8) . . ? N13 C131 C134 110.4(7) . . ? C133 C131 C134 109.4(7) . . ? C132 C131 C134 110.4(8) . . ? N14 C142 H14A 109.5 . . ? N14 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? N14 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? N23 C231 C234 109.6(8) . . ? N23 C231 C232 110.2(8) . . ? C234 C231 C232 109.7(9) . . ? N23 C231 C233 108.5(8) . . ? C234 C231 C233 108.9(8) . . ? C232 C231 C233 109.9(9) . . ? C131 C134 H13A 109.5 . . ? C131 C134 H13B 109.5 . . ? H13A C134 H13B 109.5 . . ? C131 C134 H13C 109.5 . . ? H13A C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? N25 C252 H25A 109.5 . . ? N25 C252 H25B 109.5 . . ? H25A C252 H25B 109.5 . . ? N25 C252 H25C 109.5 . . ? H25A C252 H25C 109.5 . . ? H25B C252 H25C 109.5 . . ? C131 C133 H13D 109.5 . . ? C131 C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? H13D C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? N12 C122 H12A 109.5 . . ? N12 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? N12 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? N14 C141 H14D 109.5 . . ? N14 C141 H14E 109.5 . . ? H14D C141 H14E 109.5 . . ? N14 C141 H14F 109.5 . . ? H14D C141 H14F 109.5 . . ? H14E C141 H14F 109.5 . . ? Si1 C112 H11A 109.5 . . ? Si1 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? Si1 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? N15 C152 H15A 109.5 . . ? N15 C152 H15B 109.5 . . ? H15A C152 H15B 109.5 . . ? N15 C152 H15C 109.5 . . ? H15A C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? N15 C151 H15D 109.5 . . ? N15 C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? N15 C151 H15F 109.5 . . ? H15D C151 H15F 109.5 . . ? H15E C151 H15F 109.5 . . ? N12 C121 H12D 109.5 . . ? N12 C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? N12 C121 H12F 109.5 . . ? H12D C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? Si2 C213 H21A 109.5 . . ? Si2 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? Si2 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C131 C132 H13G 109.5 . . ? C131 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? C131 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? Si1 C111 H11D 109.5 . . ? Si1 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? Si1 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? Si2 C212 H21X 109.5 . . ? Si2 C212 H21Y 109.5 . . ? H21X C212 H21Y 109.5 . . ? Si2 C212 H21Z 109.5 . . ? H21X C212 H21Z 109.5 . . ? H21Y C212 H21Z 109.5 . . ? C231 C234 H23A 109.5 . . ? C231 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C231 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? N22 C222 H22A 109.5 . . ? N22 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? N22 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C231 C233 H23D 109.5 . . ? C231 C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? H23D C233 H23F 109.5 . . ? H23E C233 H23F 109.5 . . ? N22 C221 H22D 109.5 . . ? N22 C221 H22E 109.5 . . ? H22D C221 H22E 109.5 . . ? N22 C221 H22F 109.5 . . ? H22D C221 H22F 109.5 . . ? H22E C221 H22F 109.5 . . ? N25 C251 H25D 109.5 . . ? N25 C251 H25E 109.5 . . ? H25D C251 H25E 109.5 . . ? N25 C251 H25F 109.5 . . ? H25D C251 H25F 109.5 . . ? H25E C251 H25F 109.5 . . ? Si2 C211 H21D 109.5 . . ? Si2 C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? Si2 C211 H21F 109.5 . . ? H21D C211 H21F 109.5 . . ? H21E C211 H21F 109.5 . . ? N24 C241 H24A 109.5 . . ? N24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? N24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C231 C232 H23G 109.5 . . ? C231 C232 H23H 109.5 . . ? H23G C232 H23H 109.5 . . ? C231 C232 H23I 109.5 . . ? H23G C232 H23I 109.5 . . ? H23H C232 H23I 109.5 . . ? N24 C242 H24D 109.5 . . ? N24 C242 H24E 109.5 . . ? H24D C242 H24E 109.5 . . ? N24 C242 H24F 109.5 . . ? H24D C242 H24F 109.5 . . ? H24E C242 H24F 109.5 . . ? Si1 C110 H11X 109.5 . . ? Si1 C110 H11Y 109.5 . . ? H11X C110 H11Y 109.5 . . ? Si1 C110 H11Z 109.5 . . ? H11X C110 H11Z 109.5 . . ? H11Y C110 H11Z 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N13 Ta1 N15 C152 160.4(7) . . . . ? N14 Ta1 N15 C152 47.0(8) . . . . ? N11 Ta1 N15 C152 -81.8(7) . . . . ? N12 Ta1 N15 C152 -48.0(7) . . . . ? N13 Ta1 N15 C151 -9.8(8) . . . . ? N14 Ta1 N15 C151 -123.2(8) . . . . ? N11 Ta1 N15 C151 108.0(8) . . . . ? N12 Ta1 N15 C151 141.8(8) . . . . ? C112 Si1 N11 N12 165.8(7) . . . . ? C110 Si1 N11 N12 45.5(8) . . . . ? C111 Si1 N11 N12 -77.8(8) . . . . ? C112 Si1 N11 Ta1 -41.4(8) . . . . ? C110 Si1 N11 Ta1 -161.7(7) . . . . ? C111 Si1 N11 Ta1 75.0(9) . . . . ? N13 Ta1 N11 N12 -179.6(4) . . . . ? N15 Ta1 N11 N12 65.4(5) . . . . ? N14 Ta1 N11 N12 -64.1(5) . . . . ? N13 Ta1 N11 Si1 22.0(8) . . . . ? N15 Ta1 N11 Si1 -93.0(8) . . . . ? N14 Ta1 N11 Si1 137.5(7) . . . . ? N12 Ta1 N11 Si1 -158.4(10) . . . . ? N13 Ta1 N14 C141 -166.8(7) . . . . ? N15 Ta1 N14 C141 -53.6(8) . . . . ? N11 Ta1 N14 C141 75.2(8) . . . . ? N12 Ta1 N14 C141 41.8(7) . . . . ? N13 Ta1 N14 C142 4.4(8) . . . . ? N15 Ta1 N14 C142 117.6(7) . . . . ? N11 Ta1 N14 C142 -113.6(7) . . . . ? N12 Ta1 N14 C142 -147.0(7) . . . . ? N15 Ta1 N13 C131 24(100) . . . . ? N14 Ta1 N13 C131 144(100) . . . . ? N11 Ta1 N13 C131 -96(100) . . . . ? N12 Ta1 N13 C131 -96(100) . . . . ? C213 Si2 N21 N22 -146.3(8) . . . . ? C212 Si2 N21 N22 -26.5(9) . . . . ? C211 Si2 N21 N22 95.0(8) . . . . ? C213 Si2 N21 Ta2 66.0(8) . . . . ? C212 Si2 N21 Ta2 -174.2(6) . . . . ? C211 Si2 N21 Ta2 -52.7(8) . . . . ? N23 Ta2 N21 N22 -177.0(5) . . . . ? N24 Ta2 N21 N22 -62.9(6) . . . . ? N25 Ta2 N21 N22 67.0(5) . . . . ? N23 Ta2 N21 Si2 -21.1(7) . . . . ? N24 Ta2 N21 Si2 93.1(7) . . . . ? N25 Ta2 N21 Si2 -137.1(6) . . . . ? N22 Ta2 N21 Si2 155.9(10) . . . . ? Si2 N21 N22 C221 80.1(10) . . . . ? Ta2 N21 N22 C221 -120.0(7) . . . . ? Si2 N21 N22 C222 -46.5(11) . . . . ? Ta2 N21 N22 C222 113.3(7) . . . . ? Si2 N21 N22 Ta2 -159.8(8) . . . . ? N23 Ta2 N22 N21 4.9(8) . . . . ? N24 Ta2 N22 N21 124.4(5) . . . . ? N25 Ta2 N22 N21 -122.5(5) . . . . ? N23 Ta2 N22 C221 99.3(9) . . . . ? N24 Ta2 N22 C221 -141.2(8) . . . . ? N25 Ta2 N22 C221 -28.1(8) . . . . ? N21 Ta2 N22 C221 94.4(9) . . . . ? N23 Ta2 N22 C222 -94.7(9) . . . . ? N24 Ta2 N22 C222 24.8(8) . . . . ? N25 Ta2 N22 C222 137.9(8) . . . . ? N21 Ta2 N22 C222 -99.6(9) . . . . ? Si1 N11 N12 C122 -77.6(9) . . . . ? Ta1 N11 N12 C122 117.1(6) . . . . ? Si1 N11 N12 C121 49.2(9) . . . . ? Ta1 N11 N12 C121 -116.1(6) . . . . ? Si1 N11 N12 Ta1 165.3(7) . . . . ? N13 Ta1 N12 N11 0.7(7) . . . . ? N15 Ta1 N12 N11 -122.5(4) . . . . ? N14 Ta1 N12 N11 123.6(4) . . . . ? N13 Ta1 N12 C122 -97.3(8) . . . . ? N15 Ta1 N12 C122 139.4(7) . . . . ? N14 Ta1 N12 C122 25.5(7) . . . . ? N11 Ta1 N12 C122 -98.1(8) . . . . ? N13 Ta1 N12 C121 99.7(8) . . . . ? N15 Ta1 N12 C121 -23.6(7) . . . . ? N14 Ta1 N12 C121 -137.5(7) . . . . ? N11 Ta1 N12 C121 99.0(8) . . . . ? N23 Ta2 N24 C242 5.8(10) . . . . ? N25 Ta2 N24 C242 119.3(9) . . . . ? N21 Ta2 N24 C242 -109.9(9) . . . . ? N22 Ta2 N24 C242 -142.5(9) . . . . ? N23 Ta2 N24 C241 -163.9(8) . . . . ? N25 Ta2 N24 C241 -50.5(9) . . . . ? N21 Ta2 N24 C241 80.3(9) . . . . ? N22 Ta2 N24 C241 47.8(9) . . . . ? N23 Ta2 N25 C251 173.4(8) . . . . ? N24 Ta2 N25 C251 60.3(9) . . . . ? N21 Ta2 N25 C251 -69.3(9) . . . . ? N22 Ta2 N25 C251 -35.3(8) . . . . ? N23 Ta2 N25 C252 -0.2(8) . . . . ? N24 Ta2 N25 C252 -113.3(8) . . . . ? N21 Ta2 N25 C252 117.1(7) . . . . ? N22 Ta2 N25 C252 151.1(7) . . . . ? N24 Ta2 N23 C231 -110(16) . . . . ? N25 Ta2 N23 C231 132(16) . . . . ? N21 Ta2 N23 C231 9(16) . . . . ? N22 Ta2 N23 C231 6(17) . . . . ? Ta1 N13 C131 C133 -84(100) . . . . ? Ta1 N13 C131 C132 156(100) . . . . ? Ta1 N13 C131 C134 35(100) . . . . ? Ta2 N23 C231 C234 -82(16) . . . . ? Ta2 N23 C231 C232 39(17) . . . . ? Ta2 N23 C231 C233 160(16) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 3.819 _refine_diff_density_min -2.136 _refine_diff_density_rms 0.235 # Attachment 'Compound 8.cif' data_raf73a _database_code_depnum_ccdc_archive 'CCDC 282097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 Li2 N6 Si2' _chemical_formula_weight 434.64 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' Li Li -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.063(4) _cell_length_b 19.277(8) _cell_length_c 8.088(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.113(10) _cell_angle_gamma 90.00 _cell_volume 1364.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 150 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Bruker axs ccd1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7796 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2408 _reflns_number_gt 1426 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker axs SHELXTL-PLUS' _computing_publication_material SHELXL-97 _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^)+(0.0600P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2408 _refine_ls_number_parameters 155 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.096 _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 Si1 Si 0.22150(10) 0.40032(4) 0.37653(11) 0.0380(3) Uani 1 1 d . . . N1 N 0.3780(3) 0.45033(11) 0.3798(2) 0.0308(6) Uani 1 1 d D . . C1 C 0.0324(4) 0.4293(2) 0.2341(5) 0.0617(11) Uani 1 1 d . . . H1C H -0.0476 0.3982 0.2484 0.102(15) Uiso 1 1 calc R . . H1B H 0.0370 0.4284 0.1156 0.110(17) Uiso 1 1 calc R . . H1A H 0.0105 0.4761 0.2648 0.120(18) Uiso 1 1 calc R . . Li1 Li 0.4732(6) 0.5431(2) 0.3852(6) 0.0358(12) Uani 1 1 d . . . N2 N 0.4483(3) 0.45680(12) 0.2421(3) 0.0348(6) Uani 1 1 d D . . C2 C 0.2389(5) 0.30539(18) 0.3274(6) 0.0644(11) Uani 1 1 d . . . H2C H 0.1488 0.2808 0.3392 0.094(14) Uiso 1 1 calc R . . H2B H 0.3289 0.2862 0.4067 0.090(15) Uiso 1 1 calc R . . H2A H 0.2480 0.3004 0.2111 0.095(15) Uiso 1 1 calc R . . N3 N 0.3476(3) 0.62613(13) 0.2514(3) 0.0406(7) Uani 1 1 d . . . C3 C 0.1978(5) 0.4049(2) 0.5992(5) 0.0593(10) Uani 1 1 d . . . H3A H 0.1897 0.4530 0.6307 0.071 Uiso 1 1 calc R . . H3C H 0.2856 0.3838 0.6781 0.14(2) Uiso 1 1 calc R . . H3B H 0.1058 0.3802 0.6043 0.16(2) Uiso 1 1 calc R . . C4 C 0.3426(4) 0.45286(18) 0.0719(4) 0.0489(9) Uani 1 1 d . . . H4C H 0.2936 0.4077 0.0566 0.048(9) Uiso 1 1 calc R . . H4B H 0.3984 0.4595 -0.0142 0.084(13) Uiso 1 1 calc R . . H4A H 0.2656 0.4888 0.0602 0.044(9) Uiso 1 1 calc R . . C5 C 0.5695(4) 0.40453(18) 0.2544(5) 0.0498(9) Uani 1 1 d . . . H5C H 0.5247 0.3585 0.2421 0.047(10) Uiso 1 1 calc R . . H5B H 0.6434 0.4083 0.3649 0.067(11) Uiso 1 1 calc R . . H5A H 0.6202 0.4124 0.1641 0.060(10) Uiso 1 1 calc R . . C6 C 0.1991(4) 0.62533(16) 0.2442(4) 0.0439(9) Uani 1 1 d . . . H1 H 0.1623 0.5894 0.3013 0.031(8) Uiso 1 1 calc R . . C7 C 0.0972(4) 0.67355(17) 0.1587(4) 0.0492(9) Uani 1 1 d . . . H2 H -0.0064 0.6711 0.1589 0.060(11) Uiso 1 1 calc R . . C8 C 0.1483(5) 0.72568(18) 0.0724(4) 0.0540(10) Uani 1 1 d . . . H3 H 0.0808 0.7595 0.0120 0.057(10) Uiso 1 1 calc R . . C9 C 0.3010(5) 0.72717(17) 0.0766(4) 0.0533(10) Uani 1 1 d . . . H4 H 0.3399 0.7620 0.0184 0.063(10) Uiso 1 1 calc R . . C10 C 0.3952(4) 0.67701(16) 0.1671(4) 0.0463(9) Uani 1 1 d . . . H5 H 0.4994 0.6786 0.1697 0.051(10) 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 Si1 0.0370(6) 0.0348(5) 0.0433(5) -0.0065(4) 0.0123(4) -0.0064(4) N1 0.0321(15) 0.0343(15) 0.0282(13) -0.0008(11) 0.0116(11) -0.0032(11) C1 0.037(2) 0.069(3) 0.074(3) -0.013(2) 0.006(2) -0.005(2) Li1 0.036(3) 0.028(3) 0.040(3) 0.001(2) 0.005(2) -0.003(2) N2 0.0409(16) 0.0391(16) 0.0266(13) 0.0012(11) 0.0125(12) -0.0004(12) C2 0.067(3) 0.044(2) 0.093(3) -0.011(2) 0.040(3) -0.015(2) N3 0.0473(18) 0.0306(15) 0.0425(15) 0.0046(12) 0.0094(13) 0.0022(13) C3 0.060(3) 0.065(3) 0.061(2) -0.005(2) 0.029(2) -0.005(2) C4 0.060(2) 0.051(2) 0.0348(19) -0.0017(15) 0.0106(18) -0.006(2) C5 0.052(2) 0.049(2) 0.054(2) 0.0005(17) 0.024(2) 0.0075(19) C6 0.055(2) 0.034(2) 0.0437(19) 0.0069(15) 0.0158(18) -0.0024(17) C7 0.048(2) 0.050(2) 0.050(2) 0.0063(17) 0.0131(18) 0.0081(18) C8 0.063(3) 0.049(2) 0.048(2) 0.0088(18) 0.010(2) 0.019(2) C9 0.075(3) 0.035(2) 0.054(2) 0.0146(17) 0.025(2) -0.0019(19) C10 0.050(2) 0.037(2) 0.053(2) 0.0058(17) 0.0161(18) -0.0015(17) _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 Si1 N1 1.709(2) . ? Si1 C3 1.871(3) . ? Si1 C1 1.883(4) . ? Si1 C2 1.888(4) . ? Si1 Li1 3.127(5) 3_666 ? N1 N2 1.4259(11) . ? N1 Li1 1.981(5) . ? N1 Li1 2.027(5) 3_666 ? C1 H1C 0.9700 . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? Li1 N2 2.005(5) . ? Li1 N1 2.027(5) 3_666 ? Li1 N3 2.095(5) . ? Li1 Li1 2.444(9) 3_666 ? Li1 Si1 3.127(5) 3_666 ? N2 C4 1.460(4) . ? N2 C5 1.475(4) . ? C2 H2C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? N3 C6 1.332(4) . ? N3 C10 1.329(4) . ? C3 H3A 0.9700 . ? C3 H3C 0.9700 . ? C3 H3B 0.9700 . ? C4 H4C 0.9700 . ? C4 H4B 0.9700 . ? C4 H4A 0.9700 . ? C5 H5C 0.9700 . ? C5 H5B 0.9700 . ? C5 H5A 0.9700 . ? C6 C7 1.365(4) . ? C6 H1 0.9400 . ? C7 C8 1.371(5) . ? C7 H2 0.9400 . ? C8 C9 1.376(5) . ? C8 H3 0.9400 . ? C9 C10 1.368(4) . ? C9 H4 0.9400 . ? C10 H5 0.9400 . ? 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 Si1 C3 105.16(14) . . ? N1 Si1 C1 117.47(16) . . ? C3 Si1 C1 105.12(19) . . ? N1 Si1 C2 115.81(15) . . ? C3 Si1 C2 106.56(18) . . ? C1 Si1 C2 105.73(19) . . ? N1 Si1 Li1 36.53(11) . 3_666 ? C3 Si1 Li1 72.27(16) . 3_666 ? C1 Si1 Li1 142.32(16) . 3_666 ? C2 Si1 Li1 111.02(16) . 3_666 ? N2 N1 Si1 125.13(18) . . ? N2 N1 Li1 69.95(19) . . ? Si1 N1 Li1 149.8(2) . . ? N2 N1 Li1 113.8(2) . 3_666 ? Si1 N1 Li1 113.35(17) . 3_666 ? Li1 N1 Li1 75.1(2) . 3_666 ? Si1 C1 H1C 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? Si1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? H1B C1 H1A 109.5 . . ? N1 Li1 N2 41.91(10) . . ? N1 Li1 N1 104.9(2) . 3_666 ? N2 Li1 N1 122.7(3) . 3_666 ? N1 Li1 N3 120.2(3) . . ? N2 Li1 N3 111.8(2) . . ? N1 Li1 N3 125.1(2) 3_666 . ? N1 Li1 Li1 53.29(19) . 3_666 ? N2 Li1 Li1 81.1(2) . 3_666 ? N1 Li1 Li1 51.58(19) 3_666 3_666 ? N3 Li1 Li1 152.3(4) . 3_666 ? N1 Li1 Si1 129.7(2) . 3_666 ? N2 Li1 Si1 126.4(2) . 3_666 ? N1 Li1 Si1 30.12(9) 3_666 3_666 ? N3 Li1 Si1 109.04(19) . 3_666 ? Li1 Li1 Si1 78.5(2) 3_666 3_666 ? C4 N2 C5 108.8(2) . . ? C4 N2 N1 114.5(2) . . ? C5 N2 N1 111.4(2) . . ? C4 N2 Li1 122.3(2) . . ? C5 N2 Li1 123.9(3) . . ? N1 N2 Li1 68.14(18) . . ? Si1 C2 H2C 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2C C2 H2B 109.5 . . ? Si1 C2 H2A 109.5 . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? C6 N3 C10 116.4(3) . . ? C6 N3 Li1 114.9(3) . . ? C10 N3 Li1 128.6(3) . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? N2 C4 H4C 109.5 . . ? N2 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N2 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? N2 C5 H5C 109.5 . . ? N2 C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? N2 C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? N3 C6 C7 123.9(3) . . ? N3 C6 H1 118.1 . . ? C7 C6 H1 118.1 . . ? C6 C7 C8 118.9(4) . . ? C6 C7 H2 120.6 . . ? C8 C7 H2 120.6 . . ? C7 C8 C9 118.3(3) . . ? C7 C8 H3 120.8 . . ? C9 C8 H3 120.8 . . ? C10 C9 C8 118.8(3) . . ? C10 C9 H4 120.6 . . ? C8 C9 H4 120.6 . . ? N3 C10 C9 123.7(3) . . ? N3 C10 H5 118.1 . . ? C9 C10 H5 118.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Si1 N1 N2 173.6(2) . . . . ? C1 Si1 N1 N2 -70.0(3) . . . . ? C2 Si1 N1 N2 56.2(3) . . . . ? Li1 Si1 N1 N2 147.2(3) 3_666 . . . ? C3 Si1 N1 Li1 -74.4(4) . . . . ? C1 Si1 N1 Li1 42.1(4) . . . . ? C2 Si1 N1 Li1 168.3(4) . . . . ? Li1 Si1 N1 Li1 -100.7(4) 3_666 . . . ? C3 Si1 N1 Li1 26.4(2) . . . 3_666 ? C1 Si1 N1 Li1 142.8(2) . . . 3_666 ? C2 Si1 N1 Li1 -90.9(2) . . . 3_666 ? Si1 N1 Li1 N2 -126.2(4) . . . . ? Li1 N1 Li1 N2 122.7(3) 3_666 . . . ? N2 N1 Li1 N1 -122.7(3) . . . 3_666 ? Si1 N1 Li1 N1 111.0(4) . . . 3_666 ? Li1 N1 Li1 N1 0.0 3_666 . . 3_666 ? N2 N1 Li1 N3 89.7(3) . . . . ? Si1 N1 Li1 N3 -36.5(5) . . . . ? Li1 N1 Li1 N3 -147.6(4) 3_666 . . . ? N2 N1 Li1 Li1 -122.7(3) . . . 3_666 ? Si1 N1 Li1 Li1 111.0(4) . . . 3_666 ? N2 N1 Li1 Si1 -103.3(3) . . . 3_666 ? Si1 N1 Li1 Si1 130.5(3) . . . 3_666 ? Li1 N1 Li1 Si1 19.47(12) 3_666 . . 3_666 ? Si1 N1 N2 C4 33.5(3) . . . . ? Li1 N1 N2 C4 -116.8(3) . . . . ? Li1 N1 N2 C4 -179.4(2) 3_666 . . . ? Si1 N1 N2 C5 -90.5(3) . . . . ? Li1 N1 N2 C5 119.3(3) . . . . ? Li1 N1 N2 C5 56.6(3) 3_666 . . . ? Si1 N1 N2 Li1 150.3(3) . . . . ? Li1 N1 N2 Li1 -62.7(3) 3_666 . . . ? N1 Li1 N2 C4 106.0(3) . . . . ? N1 Li1 N2 C4 -179.0(3) 3_666 . . . ? N3 Li1 N2 C4 -5.5(4) . . . . ? Li1 Li1 N2 C4 149.0(3) 3_666 . . . ? Si1 Li1 N2 C4 -142.5(2) 3_666 . . . ? N1 Li1 N2 C5 -101.8(3) . . . . ? N1 Li1 N2 C5 -26.7(4) 3_666 . . . ? N3 Li1 N2 C5 146.8(2) . . . . ? Li1 Li1 N2 C5 -58.7(3) 3_666 . . . ? Si1 Li1 N2 C5 9.8(4) 3_666 . . . ? N1 Li1 N2 N1 75.0(3) 3_666 . . . ? N3 Li1 N2 N1 -111.4(3) . . . . ? Li1 Li1 N2 N1 43.0(2) 3_666 . . . ? Si1 Li1 N2 N1 111.5(3) 3_666 . . . ? N1 Li1 N3 C6 33.6(4) . . . . ? N2 Li1 N3 C6 79.6(3) . . . . ? N1 Li1 N3 C6 -107.0(3) 3_666 . . . ? Li1 Li1 N3 C6 -34.1(8) 3_666 . . . ? Si1 Li1 N3 C6 -135.9(2) 3_666 . . . ? N1 Li1 N3 C10 -142.9(3) . . . . ? N2 Li1 N3 C10 -96.9(3) . . . . ? N1 Li1 N3 C10 76.5(4) 3_666 . . . ? Li1 Li1 N3 C10 149.4(7) 3_666 . . . ? Si1 Li1 N3 C10 47.6(4) 3_666 . . . ? C10 N3 C6 C7 -1.0(5) . . . . ? Li1 N3 C6 C7 -177.9(3) . . . . ? N3 C6 C7 C8 1.0(5) . . . . ? C6 C7 C8 C9 -0.3(5) . . . . ? C7 C8 C9 C10 -0.4(5) . . . . ? C6 N3 C10 C9 0.3(5) . . . . ? Li1 N3 C10 C9 176.7(3) . . . . ? C8 C9 C10 N3 0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.447 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.052