data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Richard J. Bowen' 'Manuel Fernandes' 'Peter B. Hitchcock' 'Michael F. Lappert' 'Marcus Layh' _publ_contact_author_name 'Prof Michael Lappert' _publ_contact_author_address ; The Chemistry Laboratory Sussex University Falmer Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.Lappert@sussex.ac.uk _journal_name_full 'Journal of the Chemical Society, Dalton Transactions' _publ_section_title ; Synthesis and crystal structures of novel 1-aza-2-silacyclobut-3-enes ; data_li4rtf_s _database_code_CSD 181494 _chemical_name_systematic ; Bis-{(P,P,P',P'-tetramethylethylenediphosphine)-(1-(2,6-dimethylphenyl)- 2,2-bis(trimethylsilyl)-3-(trimethylsilyl-4-(2,6-dimethylphenyl)amido-1-aza-2- sila-cyclobut-3-ene-N)-lithium} ; _exptl_crystal_preparation 'grown from hexane at -20 C' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H122 Li2 N4 P4 Si8' _chemical_formula_sum 'C66 H122 Li2 N4 P4 Si8' _chemical_formula_weight 1334.16 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1824(16) _cell_length_b 12.756(2) _cell_length_c 18.168(3) _cell_angle_alpha 100.496(3) _cell_angle_beta 100.679(3) _cell_angle_gamma 111.366(3) _cell_volume 2077.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rectangular _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.243 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.9092 _exptl_absorpt_correction_T_max 0.9577 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Siemens Industrial Automation, Inc.: Madison, WI.. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14560 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10016 _reflns_number_gt 7063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10016 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.016 _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 0.13778(5) 0.72682(4) 0.34840(3) 0.02625(12) Uani 1 1 d . . . Si4 Si -0.17323(5) 0.52248(4) 0.22331(3) 0.02639(12) Uani 1 1 d . . . Si2 Si 0.09182(6) 0.77940(5) 0.46935(3) 0.03550(14) Uani 1 1 d . . . Si3 Si 0.31472(6) 0.64753(5) 0.35886(4) 0.04410(16) Uani 1 1 d . . . N1 N 0.00102(16) 0.81578(12) 0.18403(8) 0.0282(3) Uani 1 1 d . . . N2 N 0.16955(16) 0.84357(12) 0.30267(8) 0.0282(3) Uani 1 1 d . . . C2 C -0.01502(18) 0.66162(14) 0.25870(10) 0.0251(4) Uani 1 1 d . . . C1 C 0.03971(18) 0.77045(14) 0.24077(10) 0.0245(3) Uani 1 1 d . . . C11 C 0.2472(2) 0.96566(15) 0.31487(10) 0.0332(4) Uani 1 1 d . . . C12 C 0.1826(3) 1.04332(17) 0.33448(11) 0.0442(5) Uani 1 1 d . . . C3 C -0.1099(2) 0.73831(16) 0.11576(11) 0.0359(5) Uani 1 1 d . . . C8 C -0.0723(3) 0.66906(17) 0.05989(12) 0.0506(6) Uani 1 1 d . . . C19 C 0.2275(3) 0.93251(19) 0.52355(13) 0.0526(6) Uani 1 1 d . . . H19A H 0.2098 0.9543 0.5730 0.079 Uiso 1 1 calc R . . H19B H 0.2170 0.9853 0.4938 0.079 Uiso 1 1 calc R . . H19C H 0.3252 0.9363 0.5317 0.079 Uiso 1 1 calc R . . C16 C 0.3915(2) 1.00836(18) 0.30711(11) 0.0437(5) Uani 1 1 d . . . C26 C -0.1650(3) 0.44171(18) 0.29922(13) 0.0500(6) Uani 1 1 d . . . H26A H -0.0791 0.4257 0.3046 0.075 Uiso 1 1 calc R . . H26B H -0.2508 0.3694 0.2838 0.075 Uiso 1 1 calc R . . H26C H -0.1608 0.4887 0.3481 0.075 Uiso 1 1 calc R . . C27 C -0.1850(3) 0.42223(17) 0.13041(12) 0.0510(6) Uani 1 1 d . . . H27A H -0.2061 0.4535 0.0877 0.076 Uiso 1 1 calc R . . H27B H -0.2616 0.3463 0.1221 0.076 Uiso 1 1 calc R . . H27C H -0.0932 0.4156 0.1340 0.076 Uiso 1 1 calc R . . C4 C -0.2491(2) 0.7366(2) 0.09960(15) 0.0544(6) Uani 1 1 d . . . C18 C 0.4599(2) 0.9261(2) 0.28619(14) 0.0553(6) Uani 1 1 d . . . H18A H 0.5480 0.9663 0.2726 0.083 Uiso 1 1 calc R . . H18B H 0.3926 0.8618 0.2427 0.083 Uiso 1 1 calc R . . H18C H 0.4833 0.8973 0.3298 0.083 Uiso 1 1 calc R . . C14 C 0.4050(4) 1.2054(2) 0.33839(15) 0.0732(9) Uani 1 1 d . . . H14 H 0.4571 1.2852 0.3460 0.088 Uiso 1 1 calc R . . C17 C 0.0321(3) 1.0003(2) 0.34664(14) 0.0562(6) Uani 1 1 d . . . H17A H -0.0360 0.9393 0.3015 0.084 Uiso 1 1 calc R . . H17B H 0.0023 1.0638 0.3547 0.084 Uiso 1 1 calc R . . H17C H 0.0337 0.9703 0.3914 0.084 Uiso 1 1 calc R . . C25 C -0.3547(2) 0.5312(2) 0.21070(19) 0.0663(8) Uani 1 1 d . . . H25A H -0.3550 0.5798 0.2577 0.099 Uiso 1 1 calc R . . H25B H -0.4307 0.4542 0.1996 0.099 Uiso 1 1 calc R . . H25C H -0.3718 0.5643 0.1683 0.099 Uiso 1 1 calc R . . C15 C 0.4677(3) 1.1292(2) 0.32023(14) 0.0631(8) Uani 1 1 d . . . H15 H 0.5636 1.1585 0.3165 0.076 Uiso 1 1 calc R . . C23 C 0.2428(3) 0.5075(2) 0.38816(19) 0.0721(8) Uani 1 1 d . . . H23A H 0.3147 0.4753 0.3920 0.108 Uiso 1 1 calc R . . H23B H 0.1541 0.4525 0.3497 0.108 Uiso 1 1 calc R . . H23C H 0.2229 0.5234 0.4377 0.108 Uiso 1 1 calc R . . C20 C 0.1172(3) 0.6840(2) 0.53270(14) 0.0671(8) Uani 1 1 d . . . H20A H 0.2141 0.6864 0.5395 0.101 Uiso 1 1 calc R . . H20B H 0.0461 0.6050 0.5086 0.101 Uiso 1 1 calc R . . H20C H 0.1043 0.7116 0.5825 0.101 Uiso 1 1 calc R . . C7 C -0.1762(4) 0.6015(2) -0.01027(14) 0.0786(10) Uani 1 1 d . . . H7 H -0.1515 0.5568 -0.0472 0.094 Uiso 1 1 calc R . . C21 C -0.1016(2) 0.7658(2) 0.45425(14) 0.0584(6) Uani 1 1 d . . . H21A H -0.1680 0.6888 0.4223 0.088 Uiso 1 1 calc R . . H21B H -0.1134 0.8229 0.4289 0.088 Uiso 1 1 calc R . . H21C H -0.1224 0.7788 0.5037 0.088 Uiso 1 1 calc R . . C10 C 0.0758(3) 0.6680(2) 0.07735(15) 0.0609(7) Uani 1 1 d . . . H10A H 0.0808 0.6205 0.1122 0.091 Uiso 1 1 calc R . . H10B H 0.1487 0.7465 0.1012 0.091 Uiso 1 1 calc R . . H10C H 0.0934 0.6364 0.0299 0.091 Uiso 1 1 calc R . . C6 C -0.3125(5) 0.5989(3) -0.02628(18) 0.0948(14) Uani 1 1 d . . . H6 H -0.3803 0.5521 -0.0736 0.114 Uiso 1 1 calc R . . C13 C 0.2648(3) 1.1629(2) 0.34523(13) 0.0641(8) Uani 1 1 d . . . H13 H 0.2227 1.2151 0.3574 0.077 Uiso 1 1 calc R . . C24 C 0.4920(3) 0.7445(3) 0.43539(19) 0.0776(9) Uani 1 1 d . . . H24A H 0.4726 0.7623 0.4848 0.116 Uiso 1 1 calc R . . H24B H 0.5378 0.8158 0.4217 0.116 Uiso 1 1 calc R . . H24C H 0.5562 0.7050 0.4387 0.116 Uiso 1 1 calc R . . C5 C -0.3519(3) 0.6654(3) 0.0272(2) 0.0810(11) Uani 1 1 d . . . H5 H -0.4458 0.6635 0.0156 0.097 Uiso 1 1 calc R . . C9 C -0.2903(3) 0.8066(2) 0.1590(2) 0.0750(9) Uani 1 1 d . . . H9A H -0.2744 0.7851 0.2067 0.113 Uiso 1 1 calc R . . H9B H -0.3920 0.7912 0.1405 0.113 Uiso 1 1 calc R . . H9C H -0.2312 0.8883 0.1679 0.113 Uiso 1 1 calc R . . Li1 Li 0.1097(4) 0.9736(3) 0.17921(19) 0.0345(7) Uani 1 1 d . . . C22 C 0.3469(3) 0.6095(2) 0.26106(18) 0.0728(8) Uani 1 1 d . . . H22A H 0.3936 0.5563 0.2606 0.109 Uiso 1 1 calc R . . H22B H 0.4088 0.6795 0.2508 0.109 Uiso 1 1 calc R . . H22C H 0.2547 0.5733 0.2216 0.109 Uiso 1 1 calc R . . P1 P 0.29069(6) 1.01812(5) 0.09018(3) 0.04474(15) Uani 1 1 d . . . P2 P 0.00359(7) 1.12954(5) 0.15519(3) 0.04331(15) Uani 1 1 d . . . C28 C 0.2082(2) 1.00347(18) -0.01232(12) 0.0398(5) Uani 1 1 d . . . H28A H 0.1698 1.0624 -0.0146 0.048 Uiso 1 1 calc R . . H28B H 0.2839 1.0181 -0.0394 0.048 Uiso 1 1 calc R . . C29 C -0.0850(2) 1.11701(18) 0.05408(12) 0.0420(5) Uani 1 1 d . . . H29A H -0.1246 1.1756 0.0541 0.050 Uiso 1 1 calc R . . H29B H -0.0117 1.1332 0.0255 0.050 Uiso 1 1 calc R . . C33 C -0.1317(3) 1.1483(2) 0.20420(15) 0.0686(8) Uani 1 1 d . . . H33A H -0.0912 1.1686 0.2595 0.103 Uiso 1 1 calc R . . H33B H -0.2185 1.0765 0.1881 0.103 Uiso 1 1 calc R . . H33C H -0.1562 1.2095 0.1906 0.103 Uiso 1 1 calc R . . C30 C 0.3998(3) 0.9322(3) 0.07914(17) 0.0724(9) Uani 1 1 d . . . H30A H 0.4670 0.9633 0.0499 0.109 Uiso 1 1 calc R . . H30B H 0.3358 0.8522 0.0521 0.109 Uiso 1 1 calc R . . H30C H 0.4537 0.9361 0.1296 0.109 Uiso 1 1 calc R . . C32 C 0.1439(3) 1.2798(2) 0.18321(16) 0.0725(9) Uani 1 1 d . . . H32A H 0.0980 1.3320 0.1753 0.109 Uiso 1 1 calc R . . H32B H 0.2112 1.2852 0.1519 0.109 Uiso 1 1 calc R . . H32C H 0.1961 1.3008 0.2371 0.109 Uiso 1 1 calc R . . C31 C 0.4351(3) 1.1662(2) 0.11751(16) 0.0783(10) Uani 1 1 d . . . H31A H 0.4973 1.1822 0.1686 0.117 Uiso 1 1 calc R . . H31B H 0.3916 1.2215 0.1176 0.117 Uiso 1 1 calc R . . H31C H 0.4923 1.1725 0.0807 0.117 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 0.0266(2) 0.0234(2) 0.0247(2) 0.00707(19) 0.00371(19) 0.00715(19) Si4 0.0251(2) 0.0217(2) 0.0280(3) 0.00860(19) 0.00459(19) 0.00537(19) Si2 0.0417(3) 0.0328(3) 0.0236(3) 0.0071(2) 0.0066(2) 0.0075(2) Si3 0.0313(3) 0.0375(3) 0.0629(4) 0.0151(3) 0.0071(3) 0.0156(3) N1 0.0312(8) 0.0231(7) 0.0252(8) 0.0087(6) 0.0042(6) 0.0063(6) N2 0.0291(8) 0.0218(7) 0.0255(8) 0.0066(6) 0.0021(6) 0.0041(6) C2 0.0263(8) 0.0234(8) 0.0223(8) 0.0070(7) 0.0044(7) 0.0073(7) C1 0.0244(8) 0.0236(8) 0.0226(8) 0.0049(7) 0.0063(7) 0.0075(7) C11 0.0401(11) 0.0242(9) 0.0201(9) 0.0058(7) -0.0014(8) 0.0013(8) C12 0.0687(15) 0.0301(10) 0.0246(10) 0.0050(8) 0.0027(10) 0.0164(10) C3 0.0392(11) 0.0248(9) 0.0303(10) 0.0147(8) -0.0011(8) 0.0003(8) C8 0.0794(17) 0.0262(10) 0.0251(10) 0.0083(8) 0.0086(10) 0.0008(10) C19 0.0586(15) 0.0384(12) 0.0398(13) -0.0020(10) 0.0035(11) 0.0076(11) C16 0.0401(11) 0.0396(11) 0.0276(10) 0.0128(9) -0.0028(8) -0.0055(9) C26 0.0562(14) 0.0368(11) 0.0404(12) 0.0203(10) 0.0046(10) 0.0002(10) C27 0.0678(15) 0.0270(10) 0.0384(12) 0.0024(9) 0.0153(11) 0.0004(10) C4 0.0401(12) 0.0426(13) 0.0681(16) 0.0319(12) -0.0014(11) 0.0033(10) C18 0.0349(11) 0.0690(16) 0.0531(14) 0.0244(12) 0.0115(10) 0.0083(11) C14 0.094(2) 0.0289(12) 0.0490(15) 0.0128(11) -0.0164(14) -0.0112(14) C17 0.0834(18) 0.0552(15) 0.0436(13) 0.0107(11) 0.0197(12) 0.0438(14) C25 0.0273(11) 0.0451(14) 0.121(2) 0.0285(15) 0.0140(13) 0.0093(10) C15 0.0566(15) 0.0469(14) 0.0427(13) 0.0196(11) -0.0119(11) -0.0172(12) C23 0.0667(17) 0.0492(15) 0.114(3) 0.0388(16) 0.0224(17) 0.0320(13) C20 0.098(2) 0.0535(15) 0.0408(13) 0.0249(12) 0.0152(13) 0.0171(14) C7 0.123(3) 0.0397(14) 0.0290(12) 0.0102(10) -0.0051(15) -0.0024(15) C21 0.0483(14) 0.0671(16) 0.0498(14) 0.0001(12) 0.0192(11) 0.0176(12) C10 0.090(2) 0.0450(14) 0.0531(15) 0.0090(11) 0.0395(14) 0.0260(13) C6 0.120(3) 0.0495(17) 0.0492(18) 0.0244(14) -0.0307(19) -0.0162(18) C13 0.108(2) 0.0297(12) 0.0359(13) 0.0044(9) -0.0039(13) 0.0218(14) C24 0.0461(15) 0.0745(19) 0.095(2) 0.0321(17) -0.0141(14) 0.0180(14) C5 0.0498(15) 0.0637(18) 0.092(2) 0.0523(18) -0.0247(16) -0.0114(14) C9 0.0405(14) 0.0696(19) 0.125(3) 0.0489(19) 0.0194(16) 0.0243(13) Li1 0.0401(18) 0.0280(16) 0.0336(17) 0.0129(13) 0.0096(14) 0.0101(14) C22 0.0638(17) 0.0652(18) 0.097(2) 0.0107(16) 0.0405(16) 0.0318(14) P1 0.0359(3) 0.0540(4) 0.0385(3) 0.0220(3) 0.0103(2) 0.0076(3) P2 0.0614(4) 0.0309(3) 0.0365(3) 0.0115(2) 0.0067(3) 0.0200(3) C28 0.0423(11) 0.0414(11) 0.0403(11) 0.0202(9) 0.0142(9) 0.0165(9) C29 0.0503(12) 0.0388(11) 0.0412(12) 0.0186(9) 0.0105(10) 0.0203(10) C33 0.118(2) 0.0688(17) 0.0546(16) 0.0284(14) 0.0406(16) 0.0636(18) C30 0.0504(14) 0.124(3) 0.0791(19) 0.0681(19) 0.0338(14) 0.0487(16) C32 0.100(2) 0.0339(13) 0.0554(16) 0.0127(11) -0.0079(15) 0.0099(13) C31 0.0613(17) 0.0759(19) 0.0521(16) 0.0240(14) 0.0019(13) -0.0184(14) _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 N2 1.7923(15) . ? Si1 C2 1.8417(17) . ? Si1 Si2 2.3600(8) . ? Si1 Si3 2.3613(8) . ? Si4 C2 1.8098(17) . ? Si4 C25 1.866(2) . ? Si4 C26 1.873(2) . ? Si4 C27 1.878(2) . ? Si2 C20 1.871(2) . ? Si2 C21 1.876(2) . ? Si2 C19 1.877(2) . ? Si3 C22 1.875(3) . ? Si3 C24 1.881(3) . ? Si3 C23 1.883(2) . ? N1 C1 1.336(2) . ? N1 C3 1.418(2) . ? N1 Li1 1.939(3) . ? N2 C11 1.418(2) . ? N2 C1 1.432(2) . ? C2 C1 1.419(2) . ? C11 C12 1.405(3) . ? C11 C16 1.413(3) . ? C12 C13 1.403(3) . ? C12 C17 1.502(3) . ? C3 C4 1.385(3) . ? C3 C8 1.422(3) . ? C8 C7 1.386(3) . ? C8 C10 1.487(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C16 C15 1.400(3) . ? C16 C18 1.488(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C4 C5 1.419(4) . ? C4 C9 1.491(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C14 C13 1.368(4) . ? C14 C15 1.369(4) . ? C14 H14 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C15 H15 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C7 C6 1.352(5) . ? C7 H7 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C6 C5 1.384(5) . ? C6 H6 0.9300 . ? C13 H13 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C5 H5 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? Li1 P1 2.648(3) . ? Li1 P2 2.651(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? P1 C31 1.827(2) . ? P1 C30 1.835(3) . ? P1 C28 1.840(2) . ? P2 C32 1.831(2) . ? P2 C33 1.834(3) . ? P2 C29 1.841(2) . ? C28 C29 1.526(3) 2_575 ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C28 1.526(3) 2_575 ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 Si1 C2 77.25(7) . . ? N2 Si1 Si2 110.79(6) . . ? C2 Si1 Si2 119.62(6) . . ? N2 Si1 Si3 116.35(6) . . ? C2 Si1 Si3 116.96(6) . . ? Si2 Si1 Si3 111.61(3) . . ? C2 Si4 C25 115.37(9) . . ? C2 Si4 C26 107.21(9) . . ? C25 Si4 C26 104.56(12) . . ? C2 Si4 C27 116.31(9) . . ? C25 Si4 C27 106.47(13) . . ? C26 Si4 C27 105.91(10) . . ? C20 Si2 C21 107.61(13) . . ? C20 Si2 C19 106.38(11) . . ? C21 Si2 C19 111.37(11) . . ? C20 Si2 Si1 112.12(10) . . ? C21 Si2 Si1 110.30(8) . . ? C19 Si2 Si1 109.02(8) . . ? C22 Si3 C24 111.17(15) . . ? C22 Si3 C23 107.14(14) . . ? C24 Si3 C23 105.46(13) . . ? C22 Si3 Si1 109.14(9) . . ? C24 Si3 Si1 113.96(10) . . ? C23 Si3 Si1 109.69(9) . . ? C1 N1 C3 117.91(14) . . ? C1 N1 Li1 124.46(15) . . ? C3 N1 Li1 116.53(14) . . ? C11 N2 C1 124.58(14) . . ? C11 N2 Si1 144.22(12) . . ? C1 N2 Si1 89.39(10) . . ? C1 C2 Si4 139.44(13) . . ? C1 C2 Si1 87.85(11) . . ? Si4 C2 Si1 132.23(9) . . ? N1 C1 C2 136.67(16) . . ? N1 C1 N2 117.86(14) . . ? C2 C1 N2 105.47(14) . . ? C12 C11 C16 120.29(18) . . ? C12 C11 N2 120.87(18) . . ? C16 C11 N2 118.84(18) . . ? C13 C12 C11 118.1(2) . . ? C13 C12 C17 120.8(2) . . ? C11 C12 C17 121.09(18) . . ? C4 C3 N1 121.4(2) . . ? C4 C3 C8 119.7(2) . . ? N1 C3 C8 118.66(19) . . ? C7 C8 C3 119.1(3) . . ? C7 C8 C10 120.7(3) . . ? C3 C8 C10 120.20(19) . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C16 C11 118.3(2) . . ? C15 C16 C18 121.4(2) . . ? C11 C16 C18 120.31(18) . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H27A 109.5 . . ? Si4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 C9 119.9(2) . . ? C5 C4 C9 121.0(3) . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C14 C15 C16 121.8(3) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 C7 C8 121.5(3) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C6 C5 120.5(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C14 C13 C12 122.1(3) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 Li1 P1 121.84(16) . . ? N1 Li1 P2 127.09(16) . . ? P1 Li1 P2 96.63(10) . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 P1 C30 100.19(15) . . ? C31 P1 C28 100.14(11) . . ? C30 P1 C28 100.94(11) . . ? C31 P1 Li1 116.83(13) . . ? C30 P1 Li1 118.98(10) . . ? C28 P1 Li1 116.58(10) . . ? C32 P2 C33 101.32(14) . . ? C32 P2 C29 100.08(10) . . ? C33 P2 C29 101.04(12) . . ? C32 P2 Li1 113.69(12) . . ? C33 P2 Li1 120.01(11) . . ? C29 P2 Li1 117.63(10) . . ? C29 C28 P1 113.05(13) 2_575 . ? C29 C28 H28A 109.0 2_575 . ? P1 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 2_575 . ? P1 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C28 C29 P2 113.12(14) 2_575 . ? C28 C29 H29A 109.0 2_575 . ? P2 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 2_575 . ? P2 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? P2 C33 H33A 109.5 . . ? P2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P1 C30 H30A 109.5 . . ? P1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P2 C32 H32A 109.5 . . ? P2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P1 C31 H31A 109.5 . . ? P1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 N2 Si1 Si2 C20 -161.80(11) . . . . ? C2 Si1 Si2 C20 111.40(12) . . . . ? Si3 Si1 Si2 C20 -30.42(10) . . . . ? N2 Si1 Si2 C21 78.30(11) . . . . ? C2 Si1 Si2 C21 -8.50(11) . . . . ? Si3 Si1 Si2 C21 -150.32(9) . . . . ? N2 Si1 Si2 C19 -44.27(10) . . . . ? C2 Si1 Si2 C19 -131.07(10) . . . . ? Si3 Si1 Si2 C19 87.11(9) . . . . ? N2 Si1 Si3 C22 -50.89(11) . . . . ? C2 Si1 Si3 C22 37.70(11) . . . . ? Si2 Si1 Si3 C22 -179.37(9) . . . . ? N2 Si1 Si3 C24 74.05(13) . . . . ? C2 Si1 Si3 C24 162.65(13) . . . . ? Si2 Si1 Si3 C24 -54.43(12) . . . . ? N2 Si1 Si3 C23 -167.99(12) . . . . ? C2 Si1 Si3 C23 -79.39(13) . . . . ? Si2 Si1 Si3 C23 63.53(11) . . . . ? C2 Si1 N2 C11 164.3(2) . . . . ? Si2 Si1 N2 C11 47.1(2) . . . . ? Si3 Si1 N2 C11 -81.7(2) . . . . ? C2 Si1 N2 C1 1.33(10) . . . . ? Si2 Si1 N2 C1 -115.80(9) . . . . ? Si3 Si1 N2 C1 115.32(9) . . . . ? C25 Si4 C2 C1 -52.3(2) . . . . ? C26 Si4 C2 C1 -168.3(2) . . . . ? C27 Si4 C2 C1 73.4(2) . . . . ? C25 Si4 C2 Si1 116.99(16) . . . . ? C26 Si4 C2 Si1 1.00(17) . . . . ? C27 Si4 C2 Si1 -117.25(14) . . . . ? N2 Si1 C2 C1 -1.34(10) . . . . ? Si2 Si1 C2 C1 105.51(10) . . . . ? Si3 Si1 C2 C1 -114.63(10) . . . . ? N2 Si1 C2 Si4 -174.42(15) . . . . ? Si2 Si1 C2 Si4 -67.57(14) . . . . ? Si3 Si1 C2 Si4 72.28(14) . . . . ? C3 N1 C1 C2 -11.5(3) . . . . ? Li1 N1 C1 C2 -179.1(2) . . . . ? C3 N1 C1 N2 168.19(16) . . . . ? Li1 N1 C1 N2 0.6(3) . . . . ? Si4 C2 C1 N1 -6.5(4) . . . . ? Si1 C2 C1 N1 -178.6(2) . . . . ? Si4 C2 C1 N2 173.82(16) . . . . ? Si1 C2 C1 N2 1.70(13) . . . . ? C11 N2 C1 N1 10.5(3) . . . . ? Si1 N2 C1 N1 178.47(14) . . . . ? C11 N2 C1 C2 -169.73(16) . . . . ? Si1 N2 C1 C2 -1.75(13) . . . . ? C1 N2 C11 C12 65.1(2) . . . . ? Si1 N2 C11 C12 -94.0(3) . . . . ? C1 N2 C11 C16 -115.0(2) . . . . ? Si1 N2 C11 C16 85.9(3) . . . . ? C16 C11 C12 C13 0.6(3) . . . . ? N2 C11 C12 C13 -179.56(17) . . . . ? C16 C11 C12 C17 -177.13(18) . . . . ? N2 C11 C12 C17 2.8(3) . . . . ? C1 N1 C3 C4 107.9(2) . . . . ? Li1 N1 C3 C4 -83.5(2) . . . . ? C1 N1 C3 C8 -77.9(2) . . . . ? Li1 N1 C3 C8 90.7(2) . . . . ? C4 C3 C8 C7 0.4(3) . . . . ? N1 C3 C8 C7 -173.92(18) . . . . ? C4 C3 C8 C10 -178.58(19) . . . . ? N1 C3 C8 C10 7.1(3) . . . . ? C12 C11 C16 C15 0.7(3) . . . . ? N2 C11 C16 C15 -179.23(17) . . . . ? C12 C11 C16 C18 -179.88(18) . . . . ? N2 C11 C16 C18 0.2(3) . . . . ? N1 C3 C4 C5 174.15(17) . . . . ? C8 C3 C4 C5 0.0(3) . . . . ? N1 C3 C4 C9 -7.5(3) . . . . ? C8 C3 C4 C9 178.28(19) . . . . ? C13 C14 C15 C16 1.1(4) . . . . ? C11 C16 C15 C14 -1.5(3) . . . . ? C18 C16 C15 C14 179.0(2) . . . . ? C3 C8 C7 C6 -0.8(3) . . . . ? C10 C8 C7 C6 178.2(2) . . . . ? C8 C7 C6 C5 0.7(4) . . . . ? C15 C14 C13 C12 0.2(4) . . . . ? C11 C12 C13 C14 -1.0(3) . . . . ? C17 C12 C13 C14 176.7(2) . . . . ? C7 C6 C5 C4 -0.3(4) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C9 C4 C5 C6 -178.3(2) . . . . ? C1 N1 Li1 P1 99.7(2) . . . . ? C3 N1 Li1 P1 -68.0(2) . . . . ? C1 N1 Li1 P2 -130.49(18) . . . . ? C3 N1 Li1 P2 61.8(2) . . . . ? N1 Li1 P1 C31 -156.93(17) . . . . ? P2 Li1 P1 C31 61.17(15) . . . . ? N1 Li1 P1 C30 -36.5(2) . . . . ? P2 Li1 P1 C30 -178.39(12) . . . . ? N1 Li1 P1 C28 84.80(19) . . . . ? P2 Li1 P1 C28 -57.09(13) . . . . ? N1 Li1 P2 C32 162.64(19) . . . . ? P1 Li1 P2 C32 -58.45(15) . . . . ? N1 Li1 P2 C33 42.6(2) . . . . ? P1 Li1 P2 C33 -178.50(12) . . . . ? N1 Li1 P2 C29 -80.9(2) . . . . ? P1 Li1 P2 C29 58.00(13) . . . . ? C31 P1 C28 C29 177.11(18) . . . 2_575 ? C30 P1 C28 C29 74.55(18) . . . 2_575 ? Li1 P1 C28 C29 -55.87(19) . . . 2_575 ? C32 P2 C29 C28 178.35(18) . . . 2_575 ? C33 P2 C29 C28 -77.90(18) . . . 2_575 ? Li1 P2 C29 C28 54.73(19) . . . 2_575 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.369 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.054 data_d:\wits\marcus\li4rt\work\soln\li4rt_s _database_code_CSD 181495 _chemical_name_systematic ; (N,N,N',N'-Tetramethylethylenediamine)-(1-(2,6-dimethylphenyl)- 2,2-bis(trimethylsilyl)-3-(trimethylsilyl-4-(2,6-dimethylphenyl)amido- 1-aza-2-sila-cyclobut-3-ene-N)-lithium ; _exptl_crystal_preparation 'grown from hexane at -20 C' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '124 C (dec.)' _chemical_formula_moiety 'C33 H61 Li N4 Si4' _chemical_formula_sum 'C33 H61 Li N4 Si4' _chemical_formula_weight 633.16 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 P21/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 17.600(3) _cell_length_b 18.995(4) _cell_length_c 24.897(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.285(4) _cell_angle_gamma 90.00 _cell_volume 8029(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description spherical _exptl_crystal_colour 'brown light' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9371 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Siemens Industrial Automation, Inc.: Madison, WI.. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55808 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 28.31 _reflns_number_total 19843 _reflns_number_gt 12833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0643P)^2^+0.9845P] 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 19843 _refine_ls_number_parameters 791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Si1A Si 0.24873(3) 0.15669(2) 0.038212(19) 0.02616(10) Uani 1 1 d . . . Si4A Si 0.27502(3) 0.31160(3) 0.10205(2) 0.03355(12) Uani 1 1 d . . . Si2A Si 0.26972(3) 0.17582(3) -0.05066(2) 0.03766(13) Uani 1 1 d . . . Si3A Si 0.12009(3) 0.11258(3) 0.02496(2) 0.03485(12) Uani 1 1 d . . . N2A N 0.32230(8) 0.10504(7) 0.08501(6) 0.0280(3) Uani 1 1 d . . . N1A N 0.39481(8) 0.15557(7) 0.17011(6) 0.0293(3) Uani 1 1 d . . . C1A C 0.33922(9) 0.16356(8) 0.12253(7) 0.0257(3) Uani 1 1 d . . . C2A C 0.28642(10) 0.21749(8) 0.09680(7) 0.0276(3) Uani 1 1 d . . . C12A C 0.35075(11) -0.02024(9) 0.09828(7) 0.0364(4) Uani 1 1 d . . . C11A C 0.37383(10) 0.04768(9) 0.08592(7) 0.0314(4) Uani 1 1 d . . . C3A C 0.39905(11) 0.20560(9) 0.21329(7) 0.0319(4) Uani 1 1 d . . . C8A C 0.34013(12) 0.20785(10) 0.24217(8) 0.0416(5) Uani 1 1 d . . . C16A C 0.44606(11) 0.05739(11) 0.07292(7) 0.0388(4) Uani 1 1 d . . . C4A C 0.46672(12) 0.24751(10) 0.23152(8) 0.0423(5) Uani 1 1 d . . . C15A C 0.49235(13) -0.00128(13) 0.07021(8) 0.0513(6) Uani 1 1 d . . . H15A H 0.5397 0.0046 0.0608 0.062 Uiso 1 1 calc R . . C14A C 0.46919(14) -0.06787(13) 0.08123(9) 0.0569(6) Uani 1 1 d . . . H14A H 0.5005 -0.1065 0.0787 0.068 Uiso 1 1 calc R . . C13A C 0.40004(14) -0.07712(11) 0.09585(8) 0.0492(5) Uani 1 1 d . . . H13A H 0.3857 -0.1221 0.1043 0.059 Uiso 1 1 calc R . . C5A C 0.47573(16) 0.28718(11) 0.28042(9) 0.0598(6) Uani 1 1 d . . . H5A H 0.5212 0.3138 0.2936 0.072 Uiso 1 1 calc R . . C23A C 0.10209(12) 0.08832(12) 0.09349(9) 0.0503(5) Uani 1 1 d . . . H23A H 0.1099 0.1289 0.1173 0.075 Uiso 1 1 calc R . . H23B H 0.1382 0.0519 0.1107 0.075 Uiso 1 1 calc R . . H23C H 0.0490 0.0717 0.0876 0.075 Uiso 1 1 calc R . . C24A C 0.10236(14) 0.03420(13) -0.02281(10) 0.0601(6) Uani 1 1 d . . . H24A H 0.0484 0.0197 -0.0298 0.090 Uiso 1 1 calc R . . H24B H 0.1362 -0.0037 -0.0057 0.090 Uiso 1 1 calc R . . H24C H 0.1135 0.0466 -0.0573 0.090 Uiso 1 1 calc R . . C7A C 0.35202(16) 0.24894(12) 0.28984(9) 0.0598(6) Uani 1 1 d . . . H7A H 0.3133 0.2501 0.3091 0.072 Uiso 1 1 calc R . . C27A C 0.25721(18) 0.34812(12) 0.16742(11) 0.0728(8) Uani 1 1 d . . . H27A H 0.2131 0.3245 0.1752 0.109 Uiso 1 1 calc R . . H27B H 0.2463 0.3976 0.1628 0.109 Uiso 1 1 calc R . . H27C H 0.3032 0.3410 0.1978 0.109 Uiso 1 1 calc R . . C33A C 0.64217(14) 0.10330(14) 0.24715(11) 0.0662(7) Uani 1 1 d . . . H33A H 0.6925 0.0856 0.2677 0.099 Uiso 1 1 calc R . . H33B H 0.6260 0.1405 0.2679 0.099 Uiso 1 1 calc R . . H33C H 0.6461 0.1212 0.2119 0.099 Uiso 1 1 calc R . . C25A C 0.36115(16) 0.36264(12) 0.09285(12) 0.0698(8) Uani 1 1 d . . . H25A H 0.4066 0.3520 0.1228 0.105 Uiso 1 1 calc R . . H25B H 0.3499 0.4121 0.0930 0.105 Uiso 1 1 calc R . . H25C H 0.3713 0.3502 0.0580 0.105 Uiso 1 1 calc R . . C22A C 0.04435(13) 0.18043(14) -0.00684(11) 0.0658(7) Uani 1 1 d . . . H22A H -0.0074 0.1610 -0.0116 0.099 Uiso 1 1 calc R . . H22B H 0.0510 0.1944 -0.0424 0.099 Uiso 1 1 calc R . . H22C H 0.0506 0.2207 0.0172 0.099 Uiso 1 1 calc R . . C6A C 0.41929(18) 0.28773(13) 0.30923(10) 0.0682(7) Uani 1 1 d . . . H6A H 0.4266 0.3142 0.3416 0.082 Uiso 1 1 calc R . . C26A C 0.18812(18) 0.33756(13) 0.04500(13) 0.0991(12) Uani 1 1 d . . . H26A H 0.1966 0.3243 0.0098 0.149 Uiso 1 1 calc R . . H26B H 0.1809 0.3876 0.0458 0.149 Uiso 1 1 calc R . . H26C H 0.1420 0.3142 0.0499 0.149 Uiso 1 1 calc R . . Li1A Li 0.45959(19) 0.07271(17) 0.20157(13) 0.0407(7) Uani 1 1 d . . . Si1 Si 0.24861(3) 0.84325(3) 0.47376(2) 0.03047(11) Uani 1 1 d . . . Si4 Si 0.20503(3) 0.68477(3) 0.41564(2) 0.03731(13) Uani 1 1 d . . . Si2 Si 0.21813(3) 0.84201(3) 0.56068(2) 0.04424(14) Uani 1 1 d . . . N1 N 0.10665(8) 0.84411(7) 0.34019(6) 0.0310(3) Uani 1 1 d . . . N2 N 0.18487(8) 0.89755(7) 0.42270(6) 0.0317(3) Uani 1 1 d . . . C2 C 0.20367(10) 0.77973(9) 0.41885(7) 0.0319(4) Uani 1 1 d . . . C1 C 0.16006(10) 0.83660(9) 0.38871(7) 0.0288(4) Uani 1 1 d . . . C3 C 0.09660(11) 0.78968(9) 0.30014(7) 0.0325(4) Uani 1 1 d . . . C11 C 0.14633(11) 0.96333(10) 0.41651(7) 0.0383(4) Uani 1 1 d . . . C4 C 0.15693(12) 0.77298(10) 0.27413(8) 0.0389(4) Uani 1 1 d . . . C8 C 0.02208(12) 0.75835(10) 0.28093(9) 0.0428(5) Uani 1 1 d . . . C16 C 0.18631(14) 1.02299(10) 0.40357(9) 0.0523(6) Uani 1 1 d . . . C26 C 0.10567(14) 0.64325(11) 0.39341(10) 0.0564(6) Uani 1 1 d . . . H26D H 0.0730 0.6615 0.4156 0.085 Uiso 1 1 calc R . . H26E H 0.1107 0.5932 0.3983 0.085 Uiso 1 1 calc R . . H26F H 0.0821 0.6537 0.3549 0.085 Uiso 1 1 calc R . . C5 C 0.14006(15) 0.72656(11) 0.22919(9) 0.0536(6) Uani 1 1 d . . . H5 H 0.1795 0.7150 0.2122 0.064 Uiso 1 1 calc R . . C7 C 0.00812(15) 0.71323(11) 0.23479(10) 0.0577(6) Uani 1 1 d . . . H7 H -0.0416 0.6935 0.2211 0.069 Uiso 1 1 calc R . . C12 C 0.07143(13) 0.97110(12) 0.42477(9) 0.0506(5) Uani 1 1 d . . . C13 C 0.03818(15) 1.03918(16) 0.42121(10) 0.0700(8) Uani 1 1 d . . . H13 H -0.0114 1.0453 0.4271 0.084 Uiso 1 1 calc R . . C27 C 0.25108(18) 0.65237(12) 0.48782(10) 0.0776(9) Uani 1 1 d . . . H27D H 0.3022 0.6733 0.5015 0.116 Uiso 1 1 calc R . . H27E H 0.2562 0.6021 0.4873 0.116 Uiso 1 1 calc R . . H27F H 0.2185 0.6651 0.5117 0.116 Uiso 1 1 calc R . . C20 C 0.29880(15) 0.79740(14) 0.61493(9) 0.0660(7) Uani 1 1 d . . . H20A H 0.2852 0.7968 0.6498 0.099 Uiso 1 1 calc R . . H20B H 0.3472 0.8227 0.6192 0.099 Uiso 1 1 calc R . . H20C H 0.3051 0.7500 0.6035 0.099 Uiso 1 1 calc R . . C25 C 0.26417(16) 0.64457(13) 0.37084(11) 0.0694(7) Uani 1 1 d . . . H25D H 0.2395 0.6548 0.3324 0.104 Uiso 1 1 calc R . . H25E H 0.2668 0.5945 0.3763 0.104 Uiso 1 1 calc R . . H25F H 0.3164 0.6638 0.3809 0.104 Uiso 1 1 calc R . . C19 C 0.20928(15) 0.93463(14) 0.58378(10) 0.0675(7) Uani 1 1 d . . . H19A H 0.1673 0.9579 0.5572 0.101 Uiso 1 1 calc R . . H19B H 0.2578 0.9592 0.5864 0.101 Uiso 1 1 calc R . . H19C H 0.1982 0.9343 0.6195 0.101 Uiso 1 1 calc R . . C15 C 0.14990(19) 1.08865(12) 0.39992(11) 0.0742(8) Uani 1 1 d . . . H15 H 0.1756 1.1280 0.3910 0.089 Uiso 1 1 calc R . . C6 C 0.06671(17) 0.69764(12) 0.20943(9) 0.0612(7) Uani 1 1 d . . . H6 H 0.0565 0.6675 0.1789 0.073 Uiso 1 1 calc R . . C21 C 0.12540(16) 0.79288(17) 0.55954(11) 0.0788(9) Uani 1 1 d . . . H21A H 0.1177 0.7923 0.5963 0.118 Uiso 1 1 calc R . . H21B H 0.1295 0.7455 0.5473 0.118 Uiso 1 1 calc R . . H21C H 0.0815 0.8158 0.5345 0.118 Uiso 1 1 calc R . . C14 C 0.07811(19) 1.09629(15) 0.40914(11) 0.0788(9) Uani 1 1 d . . . H14 H 0.0556 1.1408 0.4073 0.095 Uiso 1 1 calc R . . Si3 Si 0.38460(3) 0.86336(3) 0.48907(2) 0.04638(15) Uani 1 1 d . . . N4A N 0.58374(9) 0.04617(9) 0.23785(7) 0.0427(4) Uani 1 1 d . . . N3A N 0.43821(10) 0.01182(9) 0.26926(7) 0.0478(4) Uani 1 1 d . . . C20A C 0.17515(13) 0.20201(11) -0.10194(8) 0.0476(5) Uani 1 1 d . . . H20D H 0.1852 0.2128 -0.1371 0.071 Uiso 1 1 calc R . . H20E H 0.1538 0.2427 -0.0884 0.071 Uiso 1 1 calc R . . H20F H 0.1382 0.1639 -0.1066 0.071 Uiso 1 1 calc R . . C9 C 0.23647(12) 0.80656(11) 0.29264(9) 0.0479(5) Uani 1 1 d . . . H9A H 0.2657 0.7853 0.3268 0.072 Uiso 1 1 calc R . . H9B H 0.2305 0.8560 0.2984 0.072 Uiso 1 1 calc R . . H9C H 0.2642 0.7999 0.2646 0.072 Uiso 1 1 calc R . . C10A C 0.26600(13) 0.16573(12) 0.22276(9) 0.0498(5) Uani 1 1 d . . . H10A H 0.2395 0.1637 0.2519 0.075 Uiso 1 1 calc R . . H10B H 0.2787 0.1189 0.2135 0.075 Uiso 1 1 calc R . . H10C H 0.2322 0.1876 0.1905 0.075 Uiso 1 1 calc R . . C17A C 0.27368(12) -0.03124(10) 0.11179(9) 0.0482(5) Uani 1 1 d . . . H17A H 0.2316 -0.0279 0.0783 0.072 Uiso 1 1 calc R . . H17B H 0.2670 0.0041 0.1377 0.072 Uiso 1 1 calc R . . H17C H 0.2730 -0.0770 0.1280 0.072 Uiso 1 1 calc R . . C10 C -0.04003(13) 0.77076(12) 0.31145(11) 0.0617(6) Uani 1 1 d . . . H10D H -0.0881 0.7481 0.2919 0.093 Uiso 1 1 calc R . . H10E H -0.0490 0.8204 0.3136 0.093 Uiso 1 1 calc R . . H10F H -0.0226 0.7517 0.3484 0.093 Uiso 1 1 calc R . . C28A C 0.51289(13) -0.02647(13) 0.29094(10) 0.0604(6) Uani 1 1 d . . . H28A H 0.5139 -0.0671 0.2675 0.072 Uiso 1 1 calc R . . H28B H 0.5156 -0.0434 0.3282 0.072 Uiso 1 1 calc R . . C29A C 0.58294(13) 0.01839(13) 0.29277(9) 0.0571(6) Uani 1 1 d . . . H29A H 0.5836 0.0575 0.3180 0.069 Uiso 1 1 calc R . . H29B H 0.6303 -0.0091 0.3075 0.069 Uiso 1 1 calc R . . C18A C 0.47322(12) 0.12923(12) 0.06038(9) 0.0506(5) Uani 1 1 d . . . H18A H 0.4974 0.1531 0.0946 0.076 Uiso 1 1 calc R . . H18B H 0.4288 0.1560 0.0397 0.076 Uiso 1 1 calc R . . H18C H 0.5108 0.1244 0.0388 0.076 Uiso 1 1 calc R . . C21A C 0.30367(15) 0.09219(14) -0.07686(10) 0.0665(7) Uani 1 1 d . . . H21D H 0.3107 0.0999 -0.1134 0.100 Uiso 1 1 calc R . . H21E H 0.2649 0.0561 -0.0786 0.100 Uiso 1 1 calc R . . H21F H 0.3528 0.0778 -0.0521 0.100 Uiso 1 1 calc R . . C24 C 0.42132(15) 0.94056(15) 0.53553(11) 0.0758(8) Uani 1 1 d . . . H24D H 0.4773 0.9445 0.5418 0.114 Uiso 1 1 calc R . . H24E H 0.4089 0.9339 0.5705 0.114 Uiso 1 1 calc R . . H24F H 0.3965 0.9828 0.5181 0.114 Uiso 1 1 calc R . . C30A C 0.37413(15) -0.03975(14) 0.25636(11) 0.0698(7) Uani 1 1 d . . . H30A H 0.3750 -0.0669 0.2891 0.105 Uiso 1 1 calc R . . H30B H 0.3807 -0.0705 0.2273 0.105 Uiso 1 1 calc R . . H30C H 0.3246 -0.0157 0.2442 0.105 Uiso 1 1 calc R . . C9A C 0.52627(13) 0.25139(13) 0.19835(11) 0.0609(6) Uani 1 1 d . . . H9A1 H 0.5357 0.2050 0.1862 0.091 Uiso 1 1 calc R . . H9A2 H 0.5746 0.2705 0.2211 0.091 Uiso 1 1 calc R . . H9A3 H 0.5067 0.2811 0.1665 0.091 Uiso 1 1 calc R . . C31A C 0.42495(16) 0.06077(14) 0.31151(10) 0.0654(7) Uani 1 1 d . . . H31A H 0.3732 0.0807 0.2990 0.098 Uiso 1 1 calc R . . H31B H 0.4635 0.0977 0.3174 0.098 Uiso 1 1 calc R . . H31C H 0.4295 0.0359 0.3458 0.098 Uiso 1 1 calc R . . C22 C 0.41433(15) 0.87371(17) 0.42270(11) 0.0759(8) Uani 1 1 d . . . H22D H 0.3897 0.9149 0.4034 0.114 Uiso 1 1 calc R . . H22E H 0.3981 0.8330 0.3997 0.114 Uiso 1 1 calc R . . H22F H 0.4705 0.8786 0.4310 0.114 Uiso 1 1 calc R . . C23 C 0.43672(17) 0.78265(17) 0.52466(14) 0.0949(10) Uani 1 1 d . . . H23D H 0.4242 0.7431 0.4999 0.142 Uiso 1 1 calc R . . H23E H 0.4199 0.7732 0.5576 0.142 Uiso 1 1 calc R . . H23F H 0.4926 0.7905 0.5346 0.142 Uiso 1 1 calc R . . N4 N 0.07058(11) 0.96293(10) 0.22760(8) 0.0535(5) Uani 1 1 d . . . C17 C 0.02767(14) 0.90865(15) 0.43856(11) 0.0723(8) Uani 1 1 d . . . H17D H 0.0000 0.8855 0.4048 0.108 Uiso 1 1 calc R . . H17E H -0.0093 0.9241 0.4583 0.108 Uiso 1 1 calc R . . H17F H 0.0644 0.8764 0.4614 0.108 Uiso 1 1 calc R . . C19A C 0.34138(14) 0.24896(14) -0.05035(10) 0.0664(7) Uani 1 1 d . . . H19D H 0.3892 0.2403 -0.0219 0.100 Uiso 1 1 calc R . . H19E H 0.3189 0.2928 -0.0430 0.100 Uiso 1 1 calc R . . H19F H 0.3527 0.2513 -0.0860 0.100 Uiso 1 1 calc R . . C32A C 0.60840(16) -0.00750(15) 0.20424(10) 0.0737(8) Uani 1 1 d . . . H32A H 0.6577 -0.0273 0.2247 0.111 Uiso 1 1 calc R . . H32B H 0.6145 0.0133 0.1705 0.111 Uiso 1 1 calc R . . H32C H 0.5693 -0.0439 0.1953 0.111 Uiso 1 1 calc R . . C18 C 0.26631(16) 1.01644(13) 0.39428(12) 0.0738(8) Uani 1 1 d . . . H18D H 0.2773 1.0574 0.3750 0.111 Uiso 1 1 calc R . . H18E H 0.2683 0.9752 0.3724 0.111 Uiso 1 1 calc R . . H18F H 0.3048 1.0125 0.4295 0.111 Uiso 1 1 calc R . . C32 C 0.13479(17) 1.01150(16) 0.24993(12) 0.0817(8) Uani 1 1 d . . . H32D H 0.1478 1.0361 0.2199 0.123 Uiso 1 1 calc R . . H32E H 0.1800 0.9858 0.2707 0.123 Uiso 1 1 calc R . . H32F H 0.1190 1.0447 0.2740 0.123 Uiso 1 1 calc R . . C33 C 0.09345(19) 0.91490(15) 0.18819(11) 0.0799(9) Uani 1 1 d . . . H33D H 0.1000 0.9412 0.1568 0.120 Uiso 1 1 calc R . . H33E H 0.0531 0.8801 0.1757 0.120 Uiso 1 1 calc R . . H33F H 0.1421 0.8921 0.2063 0.120 Uiso 1 1 calc R . . Li1 Li 0.0417(2) 0.91879(17) 0.29712(14) 0.0432(8) Uani 1 1 d . . . N3 N -0.07334(10) 0.96220(9) 0.26423(7) 0.0440(4) Uani 1 1 d . . . C30 C -0.11257(14) 0.99290(14) 0.30368(10) 0.0631(6) Uani 1 1 d . . . H30D H -0.1596 1.0168 0.2836 0.095 Uiso 1 1 calc R . . H30E H -0.0778 1.0258 0.3273 0.095 Uiso 1 1 calc R . . H30F H -0.1261 0.9562 0.3260 0.095 Uiso 1 1 calc R . . C29 C -0.00052(16) 1.00140(15) 0.19812(12) 0.0754(8) Uani 1 1 d . . . H29C H 0.0150 1.0437 0.1820 0.090 Uiso 1 1 calc R . . H29D H -0.0305 0.9724 0.1678 0.090 Uiso 1 1 calc R . . C28 C -0.05034(16) 1.02074(14) 0.23330(13) 0.0771(9) Uani 1 1 d . . . H28C H -0.0977 1.0425 0.2104 0.093 Uiso 1 1 calc R . . H28D H -0.0231 1.0558 0.2598 0.093 Uiso 1 1 calc R . . C31 C -0.12890(17) 0.91410(15) 0.22834(11) 0.0768(8) Uani 1 1 d . . . H31D H -0.1473 0.8805 0.2509 0.115 Uiso 1 1 calc R . . H31E H -0.1032 0.8898 0.2042 0.115 Uiso 1 1 calc R . . H31F H -0.1728 0.9403 0.2063 0.115 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 Si1A 0.0232(2) 0.0291(2) 0.0253(2) -0.00121(18) 0.00486(18) 0.00205(18) Si4A 0.0360(3) 0.0254(2) 0.0366(3) -0.0009(2) 0.0049(2) 0.0040(2) Si2A 0.0343(3) 0.0528(3) 0.0257(3) -0.0015(2) 0.0074(2) 0.0009(2) Si3A 0.0246(2) 0.0401(3) 0.0384(3) -0.0012(2) 0.0057(2) -0.0014(2) N2A 0.0272(7) 0.0274(7) 0.0267(7) -0.0043(6) 0.0026(6) 0.0064(6) N1A 0.0290(8) 0.0298(7) 0.0260(7) -0.0018(6) 0.0020(6) 0.0029(6) C1A 0.0249(8) 0.0270(8) 0.0258(8) -0.0030(6) 0.0076(7) -0.0011(6) C2A 0.0280(9) 0.0269(8) 0.0262(9) -0.0016(7) 0.0043(7) 0.0013(7) C12A 0.0419(11) 0.0306(9) 0.0308(10) -0.0062(7) -0.0007(8) 0.0046(8) C11A 0.0329(9) 0.0336(9) 0.0244(9) -0.0053(7) 0.0018(7) 0.0075(7) C3A 0.0368(10) 0.0294(9) 0.0258(9) 0.0008(7) 0.0020(7) 0.0010(7) C8A 0.0536(12) 0.0389(10) 0.0321(10) -0.0055(8) 0.0108(9) -0.0015(9) C16A 0.0346(10) 0.0527(12) 0.0285(9) -0.0012(8) 0.0071(8) 0.0132(9) C4A 0.0460(12) 0.0340(10) 0.0387(11) 0.0032(8) -0.0031(9) -0.0053(9) C15A 0.0441(12) 0.0714(16) 0.0371(11) -0.0048(10) 0.0082(9) 0.0252(11) C14A 0.0610(15) 0.0582(15) 0.0429(12) -0.0131(10) -0.0017(10) 0.0360(12) C13A 0.0629(15) 0.0323(10) 0.0416(12) -0.0061(9) -0.0050(10) 0.0135(10) C5A 0.0749(17) 0.0417(12) 0.0473(13) -0.0056(10) -0.0113(12) -0.0191(11) C23A 0.0370(11) 0.0637(14) 0.0549(13) 0.0037(11) 0.0203(10) -0.0044(10) C24A 0.0550(14) 0.0623(15) 0.0590(15) -0.0180(12) 0.0081(11) -0.0195(12) C7A 0.0843(18) 0.0587(14) 0.0403(13) -0.0131(11) 0.0233(12) -0.0037(13) C27A 0.111(2) 0.0388(13) 0.0877(19) -0.0085(12) 0.0598(18) 0.0106(13) C33A 0.0510(15) 0.0745(17) 0.0710(17) -0.0019(13) 0.0123(12) -0.0073(13) C25A 0.0817(19) 0.0424(13) 0.097(2) -0.0143(13) 0.0443(16) -0.0186(12) C22A 0.0358(12) 0.0831(18) 0.0767(18) 0.0192(14) 0.0117(11) 0.0179(12) C6A 0.108(2) 0.0550(15) 0.0387(13) -0.0171(11) 0.0152(14) -0.0133(15) C26A 0.099(2) 0.0421(14) 0.112(3) -0.0029(15) -0.0513(19) 0.0208(14) Li1A 0.0349(17) 0.0452(18) 0.0414(18) 0.0102(14) 0.0090(14) 0.0087(14) Si1 0.0287(2) 0.0335(3) 0.0289(3) -0.0037(2) 0.00707(19) -0.0006(2) Si4 0.0474(3) 0.0287(3) 0.0323(3) 0.0007(2) 0.0041(2) 0.0036(2) Si2 0.0425(3) 0.0608(4) 0.0304(3) -0.0086(3) 0.0113(2) -0.0113(3) N1 0.0315(8) 0.0307(8) 0.0299(8) -0.0005(6) 0.0063(6) 0.0010(6) N2 0.0309(8) 0.0282(7) 0.0341(8) -0.0048(6) 0.0054(6) 0.0014(6) C2 0.0342(9) 0.0308(9) 0.0290(9) -0.0021(7) 0.0055(7) -0.0009(7) C1 0.0274(9) 0.0292(9) 0.0316(9) -0.0026(7) 0.0111(7) -0.0016(7) C3 0.0398(10) 0.0262(8) 0.0281(9) 0.0042(7) 0.0029(7) -0.0002(7) C11 0.0429(11) 0.0370(10) 0.0303(10) -0.0098(8) 0.0014(8) 0.0085(8) C4 0.0509(12) 0.0352(10) 0.0307(10) 0.0022(8) 0.0111(9) 0.0026(9) C8 0.0425(11) 0.0320(10) 0.0475(12) 0.0058(8) 0.0010(9) -0.0044(8) C16 0.0692(16) 0.0309(10) 0.0500(13) -0.0059(9) 0.0036(11) 0.0007(10) C26 0.0678(16) 0.0361(11) 0.0605(15) 0.0052(10) 0.0086(12) -0.0134(11) C5 0.0794(17) 0.0452(12) 0.0373(12) -0.0051(9) 0.0171(11) 0.0047(12) C7 0.0632(15) 0.0401(12) 0.0543(14) 0.0020(10) -0.0120(12) -0.0162(11) C12 0.0432(12) 0.0656(14) 0.0399(12) -0.0157(10) 0.0056(9) 0.0128(11) C13 0.0494(14) 0.093(2) 0.0555(15) -0.0334(14) -0.0071(11) 0.0290(14) C27 0.115(2) 0.0443(14) 0.0507(15) 0.0087(11) -0.0188(14) 0.0007(14) C20 0.0737(17) 0.0795(18) 0.0384(13) -0.0019(12) 0.0033(12) -0.0023(14) C25 0.0802(19) 0.0497(14) 0.0854(19) 0.0001(13) 0.0342(15) 0.0264(13) C19 0.0620(16) 0.0852(19) 0.0564(15) -0.0277(13) 0.0175(12) 0.0044(14) C15 0.093(2) 0.0365(13) 0.0751(18) -0.0086(12) -0.0089(15) 0.0060(13) C6 0.093(2) 0.0420(13) 0.0398(13) -0.0089(10) 0.0010(13) -0.0043(13) C21 0.0685(18) 0.120(2) 0.0513(15) -0.0008(15) 0.0214(13) -0.0395(17) C14 0.085(2) 0.0549(16) 0.0727(19) -0.0280(14) -0.0210(15) 0.0237(15) Si3 0.0277(3) 0.0657(4) 0.0455(3) -0.0091(3) 0.0094(2) -0.0003(3) N4A 0.0359(9) 0.0500(10) 0.0392(9) 0.0044(8) 0.0048(7) 0.0062(8) N3A 0.0420(10) 0.0550(11) 0.0441(10) 0.0149(8) 0.0074(8) 0.0018(8) C20A 0.0525(13) 0.0532(13) 0.0320(11) 0.0009(9) 0.0020(9) 0.0029(10) C9 0.0450(12) 0.0557(13) 0.0487(12) -0.0016(10) 0.0224(10) 0.0000(10) C10A 0.0485(13) 0.0596(14) 0.0473(13) -0.0064(10) 0.0229(10) -0.0034(10) C17A 0.0510(13) 0.0353(11) 0.0544(13) 0.0026(9) 0.0068(10) -0.0054(9) C10 0.0386(12) 0.0535(14) 0.0902(19) 0.0076(13) 0.0117(12) -0.0091(10) C28A 0.0522(14) 0.0606(15) 0.0617(15) 0.0271(12) 0.0032(11) 0.0072(11) C29A 0.0429(12) 0.0735(16) 0.0479(13) 0.0163(11) -0.0004(10) 0.0069(11) C18A 0.0394(12) 0.0665(15) 0.0492(13) 0.0053(11) 0.0176(10) 0.0023(10) C21A 0.0657(16) 0.0886(19) 0.0466(13) -0.0129(13) 0.0174(12) 0.0271(14) C24 0.0576(16) 0.103(2) 0.0643(17) -0.0249(15) 0.0123(13) -0.0356(15) C30A 0.0585(16) 0.0808(18) 0.0662(17) 0.0149(14) 0.0096(13) -0.0169(14) C9A 0.0439(13) 0.0597(15) 0.0761(17) 0.0053(12) 0.0103(12) -0.0142(11) C31A 0.0691(17) 0.0768(18) 0.0518(14) 0.0151(13) 0.0186(12) 0.0049(14) C22 0.0491(15) 0.121(2) 0.0673(17) -0.0177(16) 0.0330(13) -0.0071(15) C23 0.0546(17) 0.113(3) 0.113(3) 0.014(2) 0.0137(16) 0.0385(17) N4 0.0471(11) 0.0600(12) 0.0580(12) 0.0261(9) 0.0220(9) 0.0114(9) C17 0.0443(14) 0.114(2) 0.0633(16) -0.0068(15) 0.0229(12) 0.0078(14) C19A 0.0574(15) 0.100(2) 0.0412(13) 0.0130(12) 0.0127(11) -0.0262(14) C32A 0.0722(18) 0.0824(19) 0.0573(16) -0.0177(14) 0.0008(13) 0.0222(15) C18 0.0711(18) 0.0522(15) 0.099(2) 0.0074(14) 0.0239(15) -0.0184(13) C32 0.0754(19) 0.097(2) 0.0760(19) 0.0134(16) 0.0259(15) -0.0151(17) C33 0.105(2) 0.0757(19) 0.0710(18) 0.0239(15) 0.0445(17) 0.0216(17) Li1 0.0421(19) 0.0435(18) 0.0461(19) 0.0132(15) 0.0153(15) 0.0100(15) N3 0.0382(9) 0.0475(10) 0.0472(10) 0.0077(8) 0.0128(8) 0.0026(8) C30 0.0482(14) 0.0740(17) 0.0652(16) -0.0114(13) 0.0114(12) 0.0083(12) C29 0.0674(17) 0.090(2) 0.0759(18) 0.0488(15) 0.0320(14) 0.0312(15) C28 0.0700(18) 0.0702(17) 0.102(2) 0.0434(16) 0.0412(16) 0.0298(14) C31 0.0740(18) 0.0806(19) 0.0630(17) -0.0203(14) -0.0048(14) 0.0029(15) _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 Si1A N2A 1.7892(14) . ? Si1A C2A 1.8415(17) . ? Si1A Si3A 2.3544(8) . ? Si1A Si2A 2.3655(8) . ? Si4A C2A 1.8075(17) . ? Si4A C26A 1.859(2) . ? Si4A C25A 1.864(2) . ? Si4A C27A 1.870(2) . ? Si2A C21A 1.874(2) . ? Si2A C19A 1.875(2) . ? Si2A C20A 1.878(2) . ? Si3A C22A 1.873(2) . ? Si3A C23A 1.873(2) . ? Si3A C24A 1.880(2) . ? N2A C11A 1.414(2) . ? N2A C1A 1.432(2) . ? N1A C1A 1.331(2) . ? N1A C3A 1.422(2) . ? N1A Li1A 1.980(3) . ? C1A C2A 1.417(2) . ? C12A C13A 1.397(3) . ? C12A C11A 1.411(3) . ? C12A C17A 1.496(3) . ? C11A C16A 1.404(3) . ? C3A C4A 1.405(3) . ? C3A C8A 1.410(3) . ? C8A C7A 1.390(3) . ? C8A C10A 1.498(3) . ? C16A C15A 1.393(3) . ? C16A C18A 1.506(3) . ? C4A C5A 1.405(3) . ? C4A C9A 1.497(3) . ? C15A C14A 1.378(3) . ? C15A H15A 0.9300 . ? C14A C13A 1.371(3) . ? C14A H14A 0.9300 . ? C13A H13A 0.9300 . ? C5A C6A 1.370(4) . ? C5A H5A 0.9300 . ? C23A H23A 0.9600 . ? C23A H23B 0.9600 . ? C23A H23C 0.9600 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C7A C6A 1.370(4) . ? C7A H7A 0.9300 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? C33A N4A 1.471(3) . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C6A H6A 0.9300 . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? Li1A N3A 2.157(4) . ? Li1A N4A 2.192(3) . ? Si1 N2 1.7849(15) . ? Si1 C2 1.8385(18) . ? Si1 Si3 2.3536(8) . ? Si1 Si2 2.3629(8) . ? Si4 C2 1.8060(18) . ? Si4 C26 1.865(2) . ? Si4 C27 1.870(2) . ? Si4 C25 1.877(2) . ? Si2 C19 1.870(2) . ? Si2 C21 1.874(2) . ? Si2 C20 1.883(2) . ? N1 C1 1.328(2) . ? N1 C3 1.415(2) . ? N1 Li1 1.955(3) . ? N2 C11 1.411(2) . ? N2 C1 1.433(2) . ? C2 C1 1.420(2) . ? C3 C8 1.404(3) . ? C3 C4 1.418(3) . ? C11 C12 1.395(3) . ? C11 C16 1.415(3) . ? C4 C5 1.394(3) . ? C4 C9 1.496(3) . ? C8 C7 1.402(3) . ? C8 C10 1.505(3) . ? C16 C15 1.394(3) . ? C16 C18 1.491(3) . ? C26 H26D 0.9600 . ? C26 H26E 0.9600 . ? C26 H26F 0.9600 . ? C5 C6 1.370(3) . ? C5 H5 0.9300 . ? C7 C6 1.376(4) . ? C7 H7 0.9300 . ? C12 C13 1.413(3) . ? C12 C17 1.503(3) . ? C13 C14 1.368(4) . ? C13 H13 0.9300 . ? C27 H27D 0.9600 . ? C27 H27E 0.9600 . ? C27 H27F 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C25 H25D 0.9600 . ? C25 H25E 0.9600 . ? C25 H25F 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C15 C14 1.350(4) . ? C15 H15 0.9300 . ? C6 H6 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C14 H14 0.9300 . ? Si3 C22 1.870(2) . ? Si3 C24 1.874(3) . ? Si3 C23 1.884(3) . ? N4A C32A 1.456(3) . ? N4A C29A 1.469(3) . ? N3A C30A 1.464(3) . ? N3A C31A 1.468(3) . ? N3A C28A 1.474(3) . ? C20A H20D 0.9600 . ? C20A H20E 0.9600 . ? C20A H20F 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C10 H10D 0.9600 . ? C10 H10E 0.9600 . ? C10 H10F 0.9600 . ? C28A C29A 1.490(3) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C29A H29A 0.9700 . ? C29A H29B 0.9700 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C21A H21D 0.9600 . ? C21A H21E 0.9600 . ? C21A H21F 0.9600 . ? C24 H24D 0.9600 . ? C24 H24E 0.9600 . ? C24 H24F 0.9600 . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C22 H22D 0.9600 . ? C22 H22E 0.9600 . ? C22 H22F 0.9600 . ? C23 H23D 0.9600 . ? C23 H23E 0.9600 . ? C23 H23F 0.9600 . ? N4 C32 1.451(3) . ? N4 C29 1.468(3) . ? N4 C33 1.471(3) . ? N4 Li1 2.102(4) . ? C17 H17D 0.9600 . ? C17 H17E 0.9600 . ? C17 H17F 0.9600 . ? C19A H19D 0.9600 . ? C19A H19E 0.9600 . ? C19A H19F 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C18 H18D 0.9600 . ? C18 H18E 0.9600 . ? C18 H18F 0.9600 . ? C32 H32D 0.9600 . ? C32 H32E 0.9600 . ? C32 H32F 0.9600 . ? C33 H33D 0.9600 . ? C33 H33E 0.9600 . ? C33 H33F 0.9600 . ? Li1 N3 2.140(4) . ? N3 C31 1.459(3) . ? N3 C30 1.463(3) . ? N3 C28 1.469(3) . ? C30 H30D 0.9600 . ? C30 H30E 0.9600 . ? C30 H30F 0.9600 . ? C29 C28 1.441(3) . ? C29 H29C 0.9700 . ? C29 H29D 0.9700 . ? C28 H28C 0.9700 . ? C28 H28D 0.9700 . ? C31 H31D 0.9600 . ? C31 H31E 0.9600 . ? C31 H31F 0.9600 . ? 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 N2A Si1A C2A 77.31(7) . . ? N2A Si1A Si3A 113.59(5) . . ? C2A Si1A Si3A 117.81(6) . . ? N2A Si1A Si2A 115.38(5) . . ? C2A Si1A Si2A 122.15(6) . . ? Si3A Si1A Si2A 107.76(3) . . ? C2A Si4A C26A 106.96(10) . . ? C2A Si4A C25A 113.34(10) . . ? C26A Si4A C25A 107.46(15) . . ? C2A Si4A C27A 118.50(9) . . ? C26A Si4A C27A 105.89(15) . . ? C25A Si4A C27A 104.03(12) . . ? C21A Si2A C19A 110.72(12) . . ? C21A Si2A C20A 107.14(10) . . ? C19A Si2A C20A 106.33(11) . . ? C21A Si2A Si1A 109.76(8) . . ? C19A Si2A Si1A 112.38(8) . . ? C20A Si2A Si1A 110.34(7) . . ? C22A Si3A C23A 106.37(11) . . ? C22A Si3A C24A 107.26(12) . . ? C23A Si3A C24A 109.98(11) . . ? C22A Si3A Si1A 111.43(8) . . ? C23A Si3A Si1A 110.31(7) . . ? C24A Si3A Si1A 111.33(8) . . ? C11A N2A C1A 124.44(14) . . ? C11A N2A Si1A 141.64(11) . . ? C1A N2A Si1A 89.39(10) . . ? C1A N1A C3A 118.44(14) . . ? C1A N1A Li1A 130.85(15) . . ? C3A N1A Li1A 108.79(14) . . ? N1A C1A C2A 136.46(15) . . ? N1A C1A N2A 118.01(14) . . ? C2A C1A N2A 105.51(14) . . ? C1A C2A Si4A 138.95(13) . . ? C1A C2A Si1A 87.77(10) . . ? Si4A C2A Si1A 130.84(10) . . ? C13A C12A C11A 118.69(19) . . ? C13A C12A C17A 120.80(18) . . ? C11A C12A C17A 120.47(16) . . ? C16A C11A C12A 120.04(16) . . ? C16A C11A N2A 120.72(16) . . ? C12A C11A N2A 119.20(16) . . ? C4A C3A C8A 119.54(17) . . ? C4A C3A N1A 119.61(17) . . ? C8A C3A N1A 120.45(16) . . ? C7A C8A C3A 119.2(2) . . ? C7A C8A C10A 119.85(19) . . ? C3A C8A C10A 120.98(17) . . ? C15A C16A C11A 118.87(19) . . ? C15A C16A C18A 119.57(18) . . ? C11A C16A C18A 121.53(17) . . ? C3A C4A C5A 118.5(2) . . ? C3A C4A C9A 120.45(18) . . ? C5A C4A C9A 121.1(2) . . ? C14A C15A C16A 121.2(2) . . ? C14A C15A H15A 119.4 . . ? C16A C15A H15A 119.4 . . ? C13A C14A C15A 120.02(19) . . ? C13A C14A H14A 120.0 . . ? C15A C14A H14A 120.0 . . ? C14A C13A C12A 121.2(2) . . ? C14A C13A H13A 119.4 . . ? C12A C13A H13A 119.4 . . ? C6A C5A C4A 121.7(2) . . ? C6A C5A H5A 119.1 . . ? C4A C5A H5A 119.1 . . ? Si3A C23A H23A 109.5 . . ? Si3A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? Si3A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? Si3A C24A H24A 109.5 . . ? Si3A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? Si3A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C6A C7A C8A 121.6(2) . . ? C6A C7A H7A 119.2 . . ? C8A C7A H7A 119.2 . . ? Si4A C27A H27A 109.5 . . ? Si4A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? Si4A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? N4A C33A H33A 109.5 . . ? N4A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? N4A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? Si4A C25A H25A 109.5 . . ? Si4A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? Si4A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? Si3A C22A H22A 109.5 . . ? Si3A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? Si3A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C7A C6A C5A 119.3(2) . . ? C7A C6A H6A 120.3 . . ? C5A C6A H6A 120.3 . . ? Si4A C26A H26A 109.5 . . ? Si4A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? Si4A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? N1A Li1A N3A 122.31(17) . . ? N1A Li1A N4A 138.89(18) . . ? N3A Li1A N4A 85.12(13) . . ? N2 Si1 C2 77.48(7) . . ? N2 Si1 Si3 116.30(5) . . ? C2 Si1 Si3 116.53(6) . . ? N2 Si1 Si2 113.97(5) . . ? C2 Si1 Si2 121.16(6) . . ? Si3 Si1 Si2 108.66(3) . . ? C2 Si4 C26 114.41(10) . . ? C2 Si4 C27 107.08(10) . . ? C26 Si4 C27 106.32(12) . . ? C2 Si4 C25 116.65(10) . . ? C26 Si4 C25 105.97(12) . . ? C27 Si4 C25 105.63(13) . . ? C19 Si2 C21 109.29(13) . . ? C19 Si2 C20 108.11(12) . . ? C21 Si2 C20 106.01(13) . . ? C19 Si2 Si1 109.25(9) . . ? C21 Si2 Si1 113.47(8) . . ? C20 Si2 Si1 110.55(8) . . ? C1 N1 C3 119.30(14) . . ? C1 N1 Li1 138.41(16) . . ? C3 N1 Li1 101.38(15) . . ? C11 N2 C1 126.04(15) . . ? C11 N2 Si1 141.57(12) . . ? C1 N2 Si1 89.44(10) . . ? C1 C2 Si4 138.44(14) . . ? C1 C2 Si1 87.72(11) . . ? Si4 C2 Si1 132.86(10) . . ? N1 C1 C2 135.79(16) . . ? N1 C1 N2 118.87(15) . . ? C2 C1 N2 105.34(14) . . ? C8 C3 N1 118.80(17) . . ? C8 C3 C4 119.62(17) . . ? N1 C3 C4 121.06(16) . . ? C12 C11 N2 121.57(19) . . ? C12 C11 C16 119.67(19) . . ? N2 C11 C16 118.72(18) . . ? C5 C4 C3 118.79(19) . . ? C5 C4 C9 120.07(19) . . ? C3 C4 C9 121.09(17) . . ? C7 C8 C3 119.0(2) . . ? C7 C8 C10 121.0(2) . . ? C3 C8 C10 119.93(19) . . ? C15 C16 C11 118.9(2) . . ? C15 C16 C18 120.1(2) . . ? C11 C16 C18 121.01(19) . . ? Si4 C26 H26D 109.5 . . ? Si4 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? Si4 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C6 C7 C8 121.1(2) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C11 C12 C13 118.7(2) . . ? C11 C12 C17 120.8(2) . . ? C13 C12 C17 120.6(2) . . ? C14 C13 C12 120.8(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? Si4 C27 H27D 109.5 . . ? Si4 C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? Si4 C27 H27F 109.5 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si4 C25 H25D 109.5 . . ? Si4 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? Si4 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C15 C16 121.3(3) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C5 C6 C7 119.9(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C22 Si3 C24 109.38(13) . . ? C22 Si3 C23 106.63(14) . . ? C24 Si3 C23 107.50(15) . . ? C22 Si3 Si1 112.54(8) . . ? C24 Si3 Si1 113.41(9) . . ? C23 Si3 Si1 107.00(10) . . ? C32A N4A C29A 111.16(19) . . ? C32A N4A C33A 107.76(19) . . ? C29A N4A C33A 107.24(17) . . ? C32A N4A Li1A 109.89(16) . . ? C29A N4A Li1A 102.30(15) . . ? C33A N4A Li1A 118.35(16) . . ? C30A N3A C31A 108.79(19) . . ? C30A N3A C28A 108.11(19) . . ? C31A N3A C28A 110.18(19) . . ? C30A N3A Li1A 118.05(17) . . ? C31A N3A Li1A 108.28(16) . . ? C28A N3A Li1A 103.20(15) . . ? Si2A C20A H20D 109.5 . . ? Si2A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? Si2A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8A C10A H10A 109.5 . . ? C8A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C8A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C12A C17A H17A 109.5 . . ? C12A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C12A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C8 C10 H10D 109.5 . . ? C8 C10 H10E 109.5 . . ? H10D C10 H10E 109.5 . . ? C8 C10 H10F 109.5 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? N3A C28A C29A 112.31(19) . . ? N3A C28A H28A 109.1 . . ? C29A C28A H28A 109.1 . . ? N3A C28A H28B 109.1 . . ? C29A C28A H28B 109.1 . . ? H28A C28A H28B 107.9 . . ? N4A C29A C28A 112.82(18) . . ? N4A C29A H29A 109.0 . . ? C28A C29A H29A 109.0 . . ? N4A C29A H29B 109.0 . . ? C28A C29A H29B 109.0 . . ? H29A C29A H29B 107.8 . . ? C16A C18A H18A 109.5 . . ? C16A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C16A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? Si2A C21A H21D 109.5 . . ? Si2A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? Si2A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? Si3 C24 H24D 109.5 . . ? Si3 C24 H24E 109.5 . . ? H24D C24 H24E 109.5 . . ? Si3 C24 H24F 109.5 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? N3A C30A H30A 109.5 . . ? N3A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? N3A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? N3A C31A H31A 109.5 . . ? N3A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? N3A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? Si3 C22 H22D 109.5 . . ? Si3 C22 H22E 109.5 . . ? H22D C22 H22E 109.5 . . ? Si3 C22 H22F 109.5 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.5 . . ? Si3 C23 H23D 109.5 . . ? Si3 C23 H23E 109.5 . . ? H23D C23 H23E 109.5 . . ? Si3 C23 H23F 109.5 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C32 N4 C29 110.5(2) . . ? C32 N4 C33 109.1(2) . . ? C29 N4 C33 108.8(2) . . ? C32 N4 Li1 105.71(18) . . ? C29 N4 Li1 104.54(16) . . ? C33 N4 Li1 118.01(17) . . ? C12 C17 H17D 109.5 . . ? C12 C17 H17E 109.5 . . ? H17D C17 H17E 109.5 . . ? C12 C17 H17F 109.5 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? Si2A C19A H19D 109.5 . . ? Si2A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? Si2A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? N4A C32A H32A 109.5 . . ? N4A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? N4A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C16 C18 H18D 109.5 . . ? C16 C18 H18E 109.5 . . ? H18D C18 H18E 109.5 . . ? C16 C18 H18F 109.5 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? N4 C32 H32D 109.5 . . ? N4 C32 H32E 109.5 . . ? H32D C32 H32E 109.5 . . ? N4 C32 H32F 109.5 . . ? H32D C32 H32F 109.5 . . ? H32E C32 H32F 109.5 . . ? N4 C33 H33D 109.5 . . ? N4 C33 H33E 109.5 . . ? H33D C33 H33E 109.5 . . ? N4 C33 H33F 109.5 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? N1 Li1 N4 120.52(17) . . ? N1 Li1 N3 147.89(19) . . ? N4 Li1 N3 86.61(13) . . ? C31 N3 C30 107.58(19) . . ? C31 N3 C28 112.7(2) . . ? C30 N3 C28 107.12(19) . . ? C31 N3 Li1 114.02(18) . . ? C30 N3 Li1 117.61(17) . . ? C28 N3 Li1 97.39(16) . . ? N3 C30 H30D 109.5 . . ? N3 C30 H30E 109.5 . . ? H30D C30 H30E 109.5 . . ? N3 C30 H30F 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? C28 C29 N4 113.5(2) . . ? C28 C29 H29C 108.9 . . ? N4 C29 H29C 108.9 . . ? C28 C29 H29D 108.9 . . ? N4 C29 H29D 108.9 . . ? H29C C29 H29D 107.7 . . ? C29 C28 N3 114.9(2) . . ? C29 C28 H28C 108.5 . . ? N3 C28 H28C 108.5 . . ? C29 C28 H28D 108.5 . . ? N3 C28 H28D 108.5 . . ? H28C C28 H28D 107.5 . . ? N3 C31 H31D 109.5 . . ? N3 C31 H31E 109.5 . . ? H31D C31 H31E 109.5 . . ? N3 C31 H31F 109.5 . . ? H31D C31 H31F 109.5 . . ? H31E C31 H31F 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 N2A Si1A Si2A C21A 42.63(11) . . . . ? C2A Si1A Si2A C21A 133.27(11) . . . . ? Si3A Si1A Si2A C21A -85.48(9) . . . . ? N2A Si1A Si2A C19A -81.04(11) . . . . ? C2A Si1A Si2A C19A 9.60(12) . . . . ? Si3A Si1A Si2A C19A 150.85(10) . . . . ? N2A Si1A Si2A C20A 160.48(9) . . . . ? C2A Si1A Si2A C20A -108.89(10) . . . . ? Si3A Si1A Si2A C20A 32.36(8) . . . . ? N2A Si1A Si3A C22A 163.65(10) . . . . ? C2A Si1A Si3A C22A 75.97(11) . . . . ? Si2A Si1A Si3A C22A -67.22(10) . . . . ? N2A Si1A Si3A C23A 45.74(9) . . . . ? C2A Si1A Si3A C23A -41.93(10) . . . . ? Si2A Si1A Si3A C23A 174.87(8) . . . . ? N2A Si1A Si3A C24A -76.66(10) . . . . ? C2A Si1A Si3A C24A -164.33(10) . . . . ? Si2A Si1A Si3A C24A 52.48(9) . . . . ? C2A Si1A N2A C11A -154.6(2) . . . . ? Si3A Si1A N2A C11A 90.32(19) . . . . ? Si2A Si1A N2A C11A -34.8(2) . . . . ? C2A Si1A N2A C1A -0.75(9) . . . . ? Si3A Si1A N2A C1A -115.80(8) . . . . ? Si2A Si1A N2A C1A 119.05(8) . . . . ? C3A N1A C1A C2A 13.5(3) . . . . ? Li1A N1A C1A C2A 175.79(19) . . . . ? C3A N1A C1A N2A -164.71(14) . . . . ? Li1A N1A C1A N2A -2.4(3) . . . . ? C11A N2A C1A N1A -19.7(2) . . . . ? Si1A N2A C1A N1A 179.67(13) . . . . ? C11A N2A C1A C2A 161.64(15) . . . . ? Si1A N2A C1A C2A 0.98(12) . . . . ? N1A C1A C2A Si4A 18.6(3) . . . . ? N2A C1A C2A Si4A -163.06(15) . . . . ? N1A C1A C2A Si1A -179.27(19) . . . . ? N2A C1A C2A Si1A -0.95(12) . . . . ? C26A Si4A C2A C1A 175.7(2) . . . . ? C25A Si4A C2A C1A 57.4(2) . . . . ? C27A Si4A C2A C1A -64.9(2) . . . . ? C26A Si4A C2A Si1A 19.59(19) . . . . ? C25A Si4A C2A Si1A -98.66(15) . . . . ? C27A Si4A C2A Si1A 139.02(14) . . . . ? N2A Si1A C2A C1A 0.75(9) . . . . ? Si3A Si1A C2A C1A 110.94(9) . . . . ? Si2A Si1A C2A C1A -111.42(9) . . . . ? N2A Si1A C2A Si4A 165.29(13) . . . . ? Si3A Si1A C2A Si4A -84.52(12) . . . . ? Si2A Si1A C2A Si4A 53.11(14) . . . . ? C13A C12A C11A C16A -1.6(3) . . . . ? C17A C12A C11A C16A -179.57(17) . . . . ? C13A C12A C11A N2A 176.27(16) . . . . ? C17A C12A C11A N2A -1.7(2) . . . . ? C1A N2A C11A C16A -66.2(2) . . . . ? Si1A N2A C11A C16A 81.5(2) . . . . ? C1A N2A C11A C12A 115.87(18) . . . . ? Si1A N2A C11A C12A -96.4(2) . . . . ? C1A N1A C3A C4A -117.19(18) . . . . ? Li1A N1A C3A C4A 76.9(2) . . . . ? C1A N1A C3A C8A 70.1(2) . . . . ? Li1A N1A C3A C8A -95.9(2) . . . . ? C4A C3A C8A C7A -3.2(3) . . . . ? N1A C3A C8A C7A 169.54(18) . . . . ? C4A C3A C8A C10A 177.92(18) . . . . ? N1A C3A C8A C10A -9.4(3) . . . . ? C12A C11A C16A C15A 2.7(3) . . . . ? N2A C11A C16A C15A -175.19(16) . . . . ? C12A C11A C16A C18A -179.05(17) . . . . ? N2A C11A C16A C18A 3.1(3) . . . . ? C8A C3A C4A C5A 4.0(3) . . . . ? N1A C3A C4A C5A -168.75(17) . . . . ? C8A C3A C4A C9A -173.98(19) . . . . ? N1A C3A C4A C9A 13.2(3) . . . . ? C11A C16A C15A C14A -1.5(3) . . . . ? C18A C16A C15A C14A -179.76(19) . . . . ? C16A C15A C14A C13A -0.8(3) . . . . ? C15A C14A C13A C12A 1.9(3) . . . . ? C11A C12A C13A C14A -0.7(3) . . . . ? C17A C12A C13A C14A 177.25(19) . . . . ? C3A C4A C5A C6A -2.3(3) . . . . ? C9A C4A C5A C6A 175.7(2) . . . . ? C3A C8A C7A C6A 0.5(3) . . . . ? C10A C8A C7A C6A 179.4(2) . . . . ? C8A C7A C6A C5A 1.3(4) . . . . ? C4A C5A C6A C7A -0.3(4) . . . . ? C1A N1A Li1A N3A -105.2(2) . . . . ? C3A N1A Li1A N3A 58.4(2) . . . . ? C1A N1A Li1A N4A 129.9(2) . . . . ? C3A N1A Li1A N4A -66.5(3) . . . . ? N2 Si1 Si2 C19 -50.73(10) . . . . ? C2 Si1 Si2 C19 -140.25(11) . . . . ? Si3 Si1 Si2 C19 80.71(9) . . . . ? N2 Si1 Si2 C21 71.48(13) . . . . ? C2 Si1 Si2 C21 -18.04(14) . . . . ? Si3 Si1 Si2 C21 -157.08(12) . . . . ? N2 Si1 Si2 C20 -169.58(10) . . . . ? C2 Si1 Si2 C20 100.90(11) . . . . ? Si3 Si1 Si2 C20 -38.14(10) . . . . ? C2 Si1 N2 C11 159.9(2) . . . . ? Si3 Si1 N2 C11 -86.5(2) . . . . ? Si2 Si1 N2 C11 41.1(2) . . . . ? C2 Si1 N2 C1 0.74(10) . . . . ? Si3 Si1 N2 C1 114.36(9) . . . . ? Si2 Si1 N2 C1 -118.03(9) . . . . ? C26 Si4 C2 C1 -37.6(2) . . . . ? C27 Si4 C2 C1 -155.2(2) . . . . ? C25 Si4 C2 C1 86.8(2) . . . . ? C26 Si4 C2 Si1 127.16(14) . . . . ? C27 Si4 C2 Si1 9.62(19) . . . . ? C25 Si4 C2 Si1 -108.38(16) . . . . ? N2 Si1 C2 C1 -0.75(10) . . . . ? Si3 Si1 C2 C1 -114.10(10) . . . . ? Si2 Si1 C2 C1 109.86(10) . . . . ? N2 Si1 C2 Si4 -170.72(15) . . . . ? Si3 Si1 C2 Si4 75.93(14) . . . . ? Si2 Si1 C2 Si4 -60.11(15) . . . . ? C3 N1 C1 C2 -15.9(3) . . . . ? Li1 N1 C1 C2 177.3(2) . . . . ? C3 N1 C1 N2 163.61(15) . . . . ? Li1 N1 C1 N2 -3.1(3) . . . . ? Si4 C2 C1 N1 -10.6(4) . . . . ? Si1 C2 C1 N1 -179.5(2) . . . . ? Si4 C2 C1 N2 169.85(16) . . . . ? Si1 C2 C1 N2 0.94(13) . . . . ? C11 N2 C1 N1 15.3(3) . . . . ? Si1 N2 C1 N1 179.37(14) . . . . ? C11 N2 C1 C2 -165.08(16) . . . . ? Si1 N2 C1 C2 -0.97(13) . . . . ? C1 N1 C3 C8 121.71(18) . . . . ? Li1 N1 C3 C8 -67.22(19) . . . . ? C1 N1 C3 C4 -66.6(2) . . . . ? Li1 N1 C3 C4 104.47(18) . . . . ? C1 N2 C11 C12 65.3(2) . . . . ? Si1 N2 C11 C12 -88.6(2) . . . . ? C1 N2 C11 C16 -117.0(2) . . . . ? Si1 N2 C11 C16 89.1(2) . . . . ? C8 C3 C4 C5 1.2(3) . . . . ? N1 C3 C4 C5 -170.43(17) . . . . ? C8 C3 C4 C9 178.62(17) . . . . ? N1 C3 C4 C9 7.0(3) . . . . ? N1 C3 C8 C7 169.25(17) . . . . ? C4 C3 C8 C7 -2.6(3) . . . . ? N1 C3 C8 C10 -13.6(3) . . . . ? C4 C3 C8 C10 174.59(18) . . . . ? C12 C11 C16 C15 0.6(3) . . . . ? N2 C11 C16 C15 -177.09(19) . . . . ? C12 C11 C16 C18 -179.8(2) . . . . ? N2 C11 C16 C18 2.5(3) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C9 C4 C5 C6 -176.7(2) . . . . ? C3 C8 C7 C6 2.1(3) . . . . ? C10 C8 C7 C6 -175.0(2) . . . . ? N2 C11 C12 C13 176.21(18) . . . . ? C16 C11 C12 C13 -1.5(3) . . . . ? N2 C11 C12 C17 -2.3(3) . . . . ? C16 C11 C12 C17 180.0(2) . . . . ? C11 C12 C13 C14 0.9(3) . . . . ? C17 C12 C13 C14 179.4(2) . . . . ? C11 C16 C15 C14 0.8(4) . . . . ? C18 C16 C15 C14 -178.8(2) . . . . ? C4 C5 C6 C7 -1.3(3) . . . . ? C8 C7 C6 C5 -0.2(3) . . . . ? C16 C15 C14 C13 -1.4(4) . . . . ? C12 C13 C14 C15 0.5(4) . . . . ? N2 Si1 Si3 C22 -44.55(12) . . . . ? C2 Si1 Si3 C22 44.10(13) . . . . ? Si2 Si1 Si3 C22 -174.73(11) . . . . ? N2 Si1 Si3 C24 80.28(12) . . . . ? C2 Si1 Si3 C24 168.93(12) . . . . ? Si2 Si1 Si3 C24 -49.90(11) . . . . ? N2 Si1 Si3 C23 -161.36(12) . . . . ? C2 Si1 Si3 C23 -72.71(13) . . . . ? Si2 Si1 Si3 C23 68.46(11) . . . . ? N1A Li1A N4A C32A -119.1(3) . . . . ? N3A Li1A N4A C32A 104.99(18) . . . . ? N1A Li1A N4A C29A 122.7(3) . . . . ? N3A Li1A N4A C29A -13.16(17) . . . . ? N1A Li1A N4A C33A 5.2(3) . . . . ? N3A Li1A N4A C33A -130.69(17) . . . . ? N1A Li1A N3A C30A 79.5(3) . . . . ? N4A Li1A N3A C30A -133.30(19) . . . . ? N1A Li1A N3A C31A -44.6(3) . . . . ? N4A Li1A N3A C31A 102.62(17) . . . . ? N1A Li1A N3A C28A -161.4(2) . . . . ? N4A Li1A N3A C28A -14.17(18) . . . . ? C30A N3A C28A C29A 166.5(2) . . . . ? C31A N3A C28A C29A -74.7(2) . . . . ? Li1A N3A C28A C29A 40.7(2) . . . . ? C32A N4A C29A C28A -77.3(3) . . . . ? C33A N4A C29A C28A 165.1(2) . . . . ? Li1A N4A C29A C28A 39.9(2) . . . . ? N3A C28A C29A N4A -59.0(3) . . . . ? C1 N1 Li1 N4 104.7(3) . . . . ? C3 N1 Li1 N4 -63.5(2) . . . . ? C1 N1 Li1 N3 -111.2(4) . . . . ? C3 N1 Li1 N3 80.6(4) . . . . ? C32 N4 Li1 N1 -78.2(3) . . . . ? C29 N4 Li1 N1 165.2(2) . . . . ? C33 N4 Li1 N1 44.2(3) . . . . ? C32 N4 Li1 N3 120.00(19) . . . . ? C29 N4 Li1 N3 3.3(2) . . . . ? C33 N4 Li1 N3 -117.7(2) . . . . ? N1 Li1 N3 C31 -57.2(4) . . . . ? N4 Li1 N3 C31 92.4(2) . . . . ? N1 Li1 N3 C30 70.1(4) . . . . ? N4 Li1 N3 C30 -140.30(18) . . . . ? N1 Li1 N3 C28 -176.2(4) . . . . ? N4 Li1 N3 C28 -26.54(19) . . . . ? C32 N4 C29 C28 -90.2(3) . . . . ? C33 N4 C29 C28 150.0(3) . . . . ? Li1 N4 C29 C28 23.1(3) . . . . ? N4 C29 C28 N3 -53.9(4) . . . . ? C31 N3 C28 C29 -70.6(3) . . . . ? C30 N3 C28 C29 171.2(2) . . . . ? Li1 N3 C28 C29 49.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.596 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.045 data_f:\marcus\updates\sep988 _database_code_CSD 181496 _chemical_name_systematic ; 1-(2,6-dimethylphenyl)-2,2-bis(trimethylsilyl)-3-(trimethylsilyl-4- (2,6-dimethylphenyl)amine ; _exptl_crystal_preparation 'grown from pentane at -20 C' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 190 _chemical_formula_moiety 'C27 H46 N2 Si4' _chemical_formula_sum 'C27 H46 N2 Si4' _chemical_formula_weight 511.02 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.179(2) _cell_length_b 20.683(7) _cell_length_c 16.748(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.05(3) _cell_angle_gamma 90.00 _cell_volume 3148.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.206 _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 173(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 'Enraf Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8019 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7577 _reflns_number_gt 5222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Cameron (Watkin and Pearce, 1993)' _computing_publication_material SHELXL-97 _refine_special_details ; The H atom on N1 was freely refined; others were in riding mode. 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^)+(0.0483P)^2^+1.7786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7577 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.08752(7) 0.12123(3) 0.33252(3) 0.02537(14) Uani 1 1 d . . . Si2 Si -0.08341(8) 0.19648(4) 0.36956(5) 0.0433(2) Uani 1 1 d . . . Si3 Si 0.26531(8) 0.09401(4) 0.44160(4) 0.0423(2) Uani 1 1 d . . . Si4 Si 0.25091(7) 0.19686(3) 0.19334(4) 0.03170(16) Uani 1 1 d . . . N2 N 0.0075(2) 0.05333(9) 0.27579(10) 0.0259(4) Uani 1 1 d . . . N1 N 0.0500(3) 0.04122(11) 0.14069(12) 0.0371(5) Uani 1 1 d . . . H1 H 0.004(3) 0.0101(14) 0.1391(17) 0.042(9) Uiso 1 1 d . . . C1 C 0.0714(2) 0.07600(10) 0.21005(12) 0.0259(5) Uani 1 1 d . . . C2 C 0.1464(2) 0.13206(11) 0.23194(12) 0.0273(5) Uani 1 1 d . . . C3 C -0.2240(4) 0.21739(19) 0.2818(3) 0.0857(13) Uani 1 1 d . . . H3A H -0.1746 0.2287 0.2355 0.129 Uiso 1 1 calc R . . H3B H -0.2825 0.2542 0.2959 0.129 Uiso 1 1 calc R . . H3C H -0.2887 0.1802 0.2680 0.129 Uiso 1 1 calc R . . C4 C 0.0107(5) 0.27453(18) 0.3997(3) 0.1020(16) Uani 1 1 d . . . H4A H 0.0595 0.2907 0.3552 0.153 Uiso 1 1 calc R . . H4B H 0.0841 0.2676 0.4473 0.153 Uiso 1 1 calc R . . H4C H -0.0620 0.3062 0.4123 0.153 Uiso 1 1 calc R . . C5 C -0.1751(4) 0.16501(19) 0.4534(2) 0.0727(10) Uani 1 1 d . . . H5A H -0.2203 0.1231 0.4381 0.109 Uiso 1 1 calc R . . H5B H -0.2512 0.1955 0.4649 0.109 Uiso 1 1 calc R . . H5C H -0.1022 0.1598 0.5017 0.109 Uiso 1 1 calc R . . C6 C 0.3101(5) 0.16740(19) 0.50568(19) 0.0917(15) Uani 1 1 d . . . H6A H 0.2219 0.1818 0.5274 0.138 Uiso 1 1 calc R . . H6B H 0.3446 0.2020 0.4730 0.138 Uiso 1 1 calc R . . H6C H 0.3874 0.1568 0.5503 0.138 Uiso 1 1 calc R . . C7 C 0.4387(4) 0.0658(3) 0.4076(3) 0.1038(18) Uani 1 1 d . . . H7A H 0.5162 0.0630 0.4541 0.156 Uiso 1 1 calc R . . H7B H 0.4683 0.0964 0.3682 0.156 Uiso 1 1 calc R . . H7C H 0.4229 0.0231 0.3826 0.156 Uiso 1 1 calc R . . C8 C 0.1930(3) 0.03052(13) 0.50495(15) 0.0426(6) Uani 1 1 d . . . H8A H 0.1634 -0.0075 0.4717 0.064 Uiso 1 1 calc R . . H8B H 0.1077 0.0475 0.5275 0.064 Uiso 1 1 calc R . . H8C H 0.2699 0.0183 0.5490 0.064 Uiso 1 1 calc R . . C9 C 0.3498(3) 0.23772(14) 0.28503(16) 0.0493(7) Uani 1 1 d . . . H9A H 0.4019 0.2758 0.2687 0.074 Uiso 1 1 calc R . . H9B H 0.4207 0.2076 0.3142 0.074 Uiso 1 1 calc R . . H9C H 0.2785 0.2511 0.3202 0.074 Uiso 1 1 calc R . . C10 C 0.1313(4) 0.25902(15) 0.1361(2) 0.0600(9) Uani 1 1 d . . . H10A H 0.1922 0.2949 0.1215 0.090 Uiso 1 1 calc R . . H10B H 0.0600 0.2753 0.1697 0.090 Uiso 1 1 calc R . . H10C H 0.0787 0.2396 0.0870 0.090 Uiso 1 1 calc R . . C11 C 0.3907(3) 0.17255(17) 0.12901(19) 0.0581(8) Uani 1 1 d . . . H11A H 0.4531 0.2097 0.1208 0.087 Uiso 1 1 calc R . . H11B H 0.3412 0.1574 0.0767 0.087 Uiso 1 1 calc R . . H11C H 0.4516 0.1377 0.1555 0.087 Uiso 1 1 calc R . . C12 C -0.0624(3) -0.00714(12) 0.28212(14) 0.0425(7) Uani 1 1 d . . . C13 C -0.2137(4) -0.01054(19) 0.27082(19) 0.0701(12) Uani 1 1 d . . . C14 C -0.2801(7) -0.0701(3) 0.2822(3) 0.138(3) Uani 1 1 d . . . H14 H -0.3844 -0.0730 0.2756 0.166 Uiso 1 1 calc R . . C15 C -0.1999(13) -0.1229(3) 0.3020(4) 0.195(6) Uani 1 1 d . . . H15 H -0.2478 -0.1627 0.3097 0.234 Uiso 1 1 calc R . . C16 C -0.0519(10) -0.12071(19) 0.3113(3) 0.145(3) Uani 1 1 d . . . H16 H 0.0027 -0.1591 0.3254 0.173 Uiso 1 1 calc R . . C17 C 0.0244(6) -0.06245(14) 0.30048(17) 0.0821(15) Uani 1 1 d . . . C18 C -0.3040(4) 0.0474(3) 0.2480(3) 0.0923(15) Uani 1 1 d . . . H18A H -0.3041 0.0752 0.2953 0.138 Uiso 1 1 calc R . . H18B H -0.4050 0.0342 0.2279 0.138 Uiso 1 1 calc R . . H18C H -0.2627 0.0711 0.2058 0.138 Uiso 1 1 calc R . . C19 C 0.1875(7) -0.0604(2) 0.3064(2) 0.118(2) Uani 1 1 d . . . H19A H 0.2187 -0.0166 0.2943 0.177 Uiso 1 1 calc R . . H19B H 0.2199 -0.0909 0.2677 0.177 Uiso 1 1 calc R . . H19C H 0.2313 -0.0724 0.3612 0.177 Uiso 1 1 calc R . . C20 C 0.0862(3) 0.06347(12) 0.06553(13) 0.0342(5) Uani 1 1 d . . . C21 C -0.0050(3) 0.10805(13) 0.02166(15) 0.0424(6) Uani 1 1 d . . . C22 C 0.0318(4) 0.12729(16) -0.05280(16) 0.0614(9) Uani 1 1 d . . . H22 H -0.0274 0.1585 -0.0838 0.074 Uiso 1 1 calc R . . C23 C 0.1511(4) 0.10213(19) -0.08183(18) 0.0697(11) Uani 1 1 d . . . H23 H 0.1734 0.1156 -0.1330 0.084 Uiso 1 1 calc R . . C24 C 0.2388(4) 0.05770(19) -0.03804(19) 0.0655(10) Uani 1 1 d . . . H24 H 0.3211 0.0402 -0.0592 0.079 Uiso 1 1 calc R . . C25 C 0.2085(3) 0.03780(15) 0.03753(16) 0.0471(7) Uani 1 1 d . . . C26 C -0.1380(4) 0.13338(15) 0.0526(2) 0.0579(8) Uani 1 1 d . . . H26A H -0.1882 0.1644 0.0139 0.087 Uiso 1 1 calc R . . H26B H -0.1087 0.1549 0.1045 0.087 Uiso 1 1 calc R . . H26C H -0.2046 0.0975 0.0599 0.087 Uiso 1 1 calc R . . C27 C 0.3069(4) -0.00970(18) 0.0873(2) 0.0721(10) Uani 1 1 d . . . H27A H 0.3886 -0.0217 0.0584 0.108 Uiso 1 1 calc R . . H27B H 0.2503 -0.0484 0.0970 0.108 Uiso 1 1 calc R . . H27C H 0.3460 0.0101 0.1391 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0264(3) 0.0282(3) 0.0216(3) -0.0020(2) 0.0035(2) -0.0015(2) Si2 0.0410(4) 0.0338(4) 0.0586(5) -0.0119(3) 0.0189(3) 0.0007(3) Si3 0.0301(4) 0.0678(5) 0.0271(3) 0.0142(3) -0.0023(3) -0.0134(3) Si4 0.0334(3) 0.0360(4) 0.0252(3) 0.0052(3) 0.0027(2) -0.0076(3) N2 0.0330(10) 0.0257(9) 0.0198(8) -0.0012(7) 0.0063(7) -0.0030(8) N1 0.0594(14) 0.0319(11) 0.0215(9) -0.0026(8) 0.0108(9) -0.0117(11) C1 0.0299(11) 0.0276(11) 0.0201(10) 0.0029(8) 0.0032(8) 0.0055(9) C2 0.0299(11) 0.0308(12) 0.0210(10) 0.0020(8) 0.0035(8) -0.0011(9) C3 0.080(3) 0.075(3) 0.103(3) 0.028(2) 0.017(2) 0.042(2) C4 0.089(3) 0.055(2) 0.173(5) -0.056(3) 0.054(3) -0.016(2) C5 0.066(2) 0.090(3) 0.070(2) -0.002(2) 0.0375(18) 0.012(2) C6 0.130(4) 0.098(3) 0.0384(17) 0.0112(18) -0.019(2) -0.075(3) C7 0.0329(17) 0.174(5) 0.109(3) 0.082(3) 0.0245(19) 0.029(2) C8 0.0447(15) 0.0536(17) 0.0295(12) 0.0065(12) 0.0048(11) -0.0068(13) C9 0.0556(17) 0.0559(18) 0.0362(14) 0.0004(12) 0.0054(12) -0.0277(14) C10 0.0622(19) 0.0439(17) 0.070(2) 0.0238(15) -0.0052(16) -0.0104(15) C11 0.0551(18) 0.071(2) 0.0539(18) -0.0078(16) 0.0261(15) -0.0212(16) C12 0.084(2) 0.0257(12) 0.0211(11) -0.0036(9) 0.0202(12) -0.0119(13) C13 0.088(3) 0.086(3) 0.0462(17) -0.0329(17) 0.0430(18) -0.060(2) C14 0.220(6) 0.142(5) 0.077(3) -0.077(3) 0.106(4) -0.143(5) C15 0.443(15) 0.095(4) 0.079(4) -0.064(3) 0.151(7) -0.157(7) C16 0.380(11) 0.0236(18) 0.044(2) -0.0005(15) 0.079(5) 0.002(4) C17 0.199(5) 0.0279(15) 0.0243(14) -0.0017(11) 0.032(2) 0.017(2) C18 0.0378(18) 0.155(4) 0.086(3) -0.045(3) 0.0134(18) -0.022(2) C19 0.196(6) 0.098(3) 0.055(2) -0.003(2) 0.002(3) 0.106(4) C20 0.0432(14) 0.0407(13) 0.0191(10) -0.0038(9) 0.0061(9) -0.0114(11) C21 0.0536(16) 0.0439(15) 0.0280(12) 0.0015(11) 0.0001(11) -0.0126(13) C22 0.093(3) 0.060(2) 0.0290(14) 0.0091(13) -0.0009(15) -0.0263(18) C23 0.098(3) 0.087(3) 0.0267(14) -0.0077(16) 0.0205(17) -0.050(2) C24 0.066(2) 0.088(3) 0.0479(18) -0.0336(18) 0.0302(16) -0.0355(19) C25 0.0437(15) 0.0613(19) 0.0369(14) -0.0151(13) 0.0073(12) -0.0144(13) C26 0.0599(19) 0.0501(18) 0.0608(19) 0.0030(15) -0.0016(15) 0.0048(15) C27 0.052(2) 0.084(3) 0.078(2) -0.024(2) 0.0003(17) 0.0095(18) _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 N2 1.7942(19) . ? Si1 C2 1.853(2) . ? Si1 C1 2.240(2) . ? Si1 Si3 2.3415(12) . ? Si1 Si2 2.3541(10) . ? Si2 C5 1.854(3) . ? Si2 C3 1.865(4) . ? Si2 C4 1.867(4) . ? Si3 C7 1.857(4) . ? Si3 C8 1.868(3) . ? Si3 C6 1.871(4) . ? Si4 C2 1.819(2) . ? Si4 C11 1.857(3) . ? Si4 C10 1.866(3) . ? Si4 C9 1.872(3) . ? N2 C1 1.399(3) . ? N2 C12 1.416(3) . ? N1 C1 1.357(3) . ? N1 C20 1.423(3) . ? N1 H1 0.77(3) . ? C1 C2 1.372(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.376(5) . ? C12 C17 1.403(5) . ? C13 C14 1.400(5) . ? C13 C18 1.476(6) . ? C14 C15 1.333(12) . ? C14 H14 0.9500 . ? C15 C16 1.346(12) . ? C15 H15 0.9500 . ? C16 C17 1.418(7) . ? C16 H16 0.9500 . ? C17 C19 1.487(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.381(4) . ? C20 C21 1.385(4) . ? C21 C22 1.395(4) . ? C21 C26 1.487(4) . ? C22 C23 1.362(5) . ? C22 H22 0.9500 . ? C23 C24 1.366(5) . ? C23 H23 0.9500 . ? C24 C25 1.396(4) . ? C24 H24 0.9500 . ? C25 C27 1.505(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 Si1 C2 76.30(9) . . ? N2 Si1 C1 38.61(8) . . ? C2 Si1 C1 37.69(9) . . ? N2 Si1 Si3 114.46(7) . . ? C2 Si1 Si3 118.56(8) . . ? C1 Si1 Si3 124.30(7) . . ? N2 Si1 Si2 114.74(7) . . ? C2 Si1 Si2 116.71(8) . . ? C1 Si1 Si2 123.80(7) . . ? Si3 Si1 Si2 111.76(4) . . ? C5 Si2 C3 109.94(19) . . ? C5 Si2 C4 109.9(2) . . ? C3 Si2 C4 104.8(2) . . ? C5 Si2 Si1 110.94(12) . . ? C3 Si2 Si1 111.02(13) . . ? C4 Si2 Si1 110.03(13) . . ? C7 Si3 C8 109.94(17) . . ? C7 Si3 C6 107.6(2) . . ? C8 Si3 C6 108.16(14) . . ? C7 Si3 Si1 111.70(13) . . ? C8 Si3 Si1 110.36(9) . . ? C6 Si3 Si1 109.01(14) . . ? C2 Si4 C11 116.64(13) . . ? C2 Si4 C10 112.86(12) . . ? C11 Si4 C10 107.05(16) . . ? C2 Si4 C9 105.09(11) . . ? C11 Si4 C9 107.65(14) . . ? C10 Si4 C9 107.05(15) . . ? C1 N2 C12 126.81(18) . . ? C1 N2 Si1 88.21(13) . . ? C12 N2 Si1 143.87(15) . . ? C1 N1 C20 124.2(2) . . ? C1 N1 H1 119(2) . . ? C20 N1 H1 116(2) . . ? N1 C1 C2 133.1(2) . . ? N1 C1 N2 118.0(2) . . ? C2 C1 N2 108.85(18) . . ? N1 C1 Si1 171.18(18) . . ? C2 C1 Si1 55.68(11) . . ? N2 C1 Si1 53.18(10) . . ? C1 C2 Si4 142.93(17) . . ? C1 C2 Si1 86.63(14) . . ? Si4 C2 Si1 130.36(13) . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si4 C9 H9A 109.5 . . ? Si4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C10 H10A 109.5 . . ? Si4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 121.3(3) . . ? C13 C12 N2 119.6(3) . . ? C17 C12 N2 119.2(3) . . ? C12 C13 C14 118.5(5) . . ? C12 C13 C18 120.9(3) . . ? C14 C13 C18 120.6(5) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 120.9(5) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 121.5(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C12 C17 C16 116.5(5) . . ? C12 C17 C19 121.8(3) . . ? C16 C17 C19 121.7(5) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 122.4(2) . . ? C25 C20 N1 118.5(2) . . ? C21 C20 N1 119.1(2) . . ? C20 C21 C22 117.4(3) . . ? C20 C21 C26 120.9(2) . . ? C22 C21 C26 121.7(3) . . ? C23 C22 C21 121.2(3) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C20 C25 C24 118.0(3) . . ? C20 C25 C27 121.1(3) . . ? C24 C25 C27 121.0(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 N2 Si1 Si2 C5 75.06(16) . . . . ? C2 Si1 Si2 C5 161.62(16) . . . . ? C1 Si1 Si2 C5 118.43(16) . . . . ? Si3 Si1 Si2 C5 -57.38(15) . . . . ? N2 Si1 Si2 C3 -47.51(17) . . . . ? C2 Si1 Si2 C3 39.05(17) . . . . ? C1 Si1 Si2 C3 -4.14(17) . . . . ? Si3 Si1 Si2 C3 -179.95(15) . . . . ? N2 Si1 Si2 C4 -163.1(2) . . . . ? C2 Si1 Si2 C4 -76.5(2) . . . . ? C1 Si1 Si2 C4 -119.7(2) . . . . ? Si3 Si1 Si2 C4 64.50(19) . . . . ? N2 Si1 Si3 C7 72.34(19) . . . . ? C2 Si1 Si3 C7 -14.9(2) . . . . ? C1 Si1 Si3 C7 29.1(2) . . . . ? Si2 Si1 Si3 C7 -155.08(18) . . . . ? N2 Si1 Si3 C8 -50.29(12) . . . . ? C2 Si1 Si3 C8 -137.50(13) . . . . ? C1 Si1 Si3 C8 -93.50(13) . . . . ? Si2 Si1 Si3 C8 82.29(11) . . . . ? N2 Si1 Si3 C6 -168.93(15) . . . . ? C2 Si1 Si3 C6 103.85(16) . . . . ? C1 Si1 Si3 C6 147.86(15) . . . . ? Si2 Si1 Si3 C6 -36.36(14) . . . . ? C2 Si1 N2 C1 0.46(13) . . . . ? Si3 Si1 N2 C1 -114.99(11) . . . . ? Si2 Si1 N2 C1 113.86(12) . . . . ? C2 Si1 N2 C12 167.3(3) . . . . ? C1 Si1 N2 C12 166.8(4) . . . . ? Si3 Si1 N2 C12 51.8(3) . . . . ? Si2 Si1 N2 C12 -79.3(3) . . . . ? C20 N1 C1 C2 -11.1(4) . . . . ? C20 N1 C1 N2 168.9(2) . . . . ? C20 N1 C1 Si1 172.4(10) . . . . ? C12 N2 C1 N1 9.0(3) . . . . ? Si1 N2 C1 N1 179.33(19) . . . . ? C12 N2 C1 C2 -171.0(2) . . . . ? Si1 N2 C1 C2 -0.64(18) . . . . ? C12 N2 C1 Si1 -170.3(3) . . . . ? N2 Si1 C1 N1 -3.8(11) . . . . ? C2 Si1 C1 N1 176.9(12) . . . . ? Si3 Si1 C1 N1 83.2(12) . . . . ? Si2 Si1 C1 N1 -92.1(12) . . . . ? N2 Si1 C1 C2 179.3(2) . . . . ? Si3 Si1 C1 C2 -93.65(14) . . . . ? Si2 Si1 C1 C2 91.06(14) . . . . ? C2 Si1 C1 N2 -179.3(2) . . . . ? Si3 Si1 C1 N2 87.08(13) . . . . ? Si2 Si1 C1 N2 -88.21(13) . . . . ? N1 C1 C2 Si4 4.2(5) . . . . ? N2 C1 C2 Si4 -175.8(2) . . . . ? Si1 C1 C2 Si4 -176.5(3) . . . . ? N1 C1 C2 Si1 -179.3(3) . . . . ? N2 C1 C2 Si1 0.62(17) . . . . ? C11 Si4 C2 C1 -45.2(3) . . . . ? C10 Si4 C2 C1 79.4(3) . . . . ? C9 Si4 C2 C1 -164.3(3) . . . . ? C11 Si4 C2 Si1 139.46(18) . . . . ? C10 Si4 C2 Si1 -96.0(2) . . . . ? C9 Si4 C2 Si1 20.3(2) . . . . ? N2 Si1 C2 C1 -0.47(13) . . . . ? Si3 Si1 C2 C1 110.17(13) . . . . ? Si2 Si1 C2 C1 -111.54(13) . . . . ? N2 Si1 C2 Si4 176.72(18) . . . . ? C1 Si1 C2 Si4 177.2(3) . . . . ? Si3 Si1 C2 Si4 -72.63(17) . . . . ? Si2 Si1 C2 Si4 65.66(17) . . . . ? C1 N2 C12 C13 -101.5(3) . . . . ? Si1 N2 C12 C13 95.0(3) . . . . ? C1 N2 C12 C17 79.0(3) . . . . ? Si1 N2 C12 C17 -84.5(3) . . . . ? C17 C12 C13 C14 3.3(4) . . . . ? N2 C12 C13 C14 -176.2(2) . . . . ? C17 C12 C13 C18 -177.3(3) . . . . ? N2 C12 C13 C18 3.2(4) . . . . ? C12 C13 C14 C15 -1.2(6) . . . . ? C18 C13 C14 C15 179.4(4) . . . . ? C13 C14 C15 C16 -0.5(8) . . . . ? C14 C15 C16 C17 0.1(8) . . . . ? C13 C12 C17 C16 -3.6(4) . . . . ? N2 C12 C17 C16 175.9(3) . . . . ? C13 C12 C17 C19 175.1(3) . . . . ? N2 C12 C17 C19 -5.4(4) . . . . ? C15 C16 C17 C12 1.9(6) . . . . ? C15 C16 C17 C19 -176.8(4) . . . . ? C1 N1 C20 C25 105.9(3) . . . . ? C1 N1 C20 C21 -76.6(3) . . . . ? C25 C20 C21 C22 -0.8(4) . . . . ? N1 C20 C21 C22 -178.2(2) . . . . ? C25 C20 C21 C26 178.3(3) . . . . ? N1 C20 C21 C26 0.9(4) . . . . ? C20 C21 C22 C23 1.3(4) . . . . ? C26 C21 C22 C23 -177.7(3) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C21 C20 C25 C24 -0.5(4) . . . . ? N1 C20 C25 C24 177.0(2) . . . . ? C21 C20 C25 C27 178.9(3) . . . . ? N1 C20 C25 C27 -3.7(4) . . . . ? C23 C24 C25 C20 1.2(4) . . . . ? C23 C24 C25 C27 -178.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.402 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.054