# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Lappert, Michael Franz' 'Hitchcock, Peter B.' 'Liu, Diang-Sheng' 'Sablong, Rafael' _publ_contact_author_name 'Prof Michael Franz Lappert' _publ_contact_author_address ; Chemistry Laboratory University of Sussex CPES, University of Sussex Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'M.F.LAPPERT@SUSSEX.AC.UK' _publ_section_title ; Syntheses and structures of structurally diverse potassium b-diketiminates derived from the ligand [{N(SiMe3)C(Ph)2CH}2]- ; data_mfl-1 _database_code_CSD 187158 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[K(thf)2(Me3SiNCPhCHCPhNSiMe3)]n' _chemical_formula_analytical ? _chemical_formula_sum 'C29 H45 K N2 O2 Si2' _chemical_formula_weight 548.95 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.217(3) _cell_length_b 19.020(3) _cell_length_c 15.526(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.05(2) _cell_angle_gamma 90.00 _cell_volume 3307.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14 _cell_measurement_theta_max 17 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method ? _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 2.289 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6061 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 65.95 _reflns_number_total 5756 _reflns_number_observed 3500 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.8932P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5756 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1211 _refine_ls_R_factor_obs 0.0693 _refine_ls_wR_factor_all 0.2055 _refine_ls_wR_factor_obs 0.1674 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.015 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K K 0.20210(9) 0.27194(6) 0.95067(6) 0.0642(3) Uani 1 d . . Si1 Si 0.15975(13) 0.40806(6) 0.75777(8) 0.0631(4) Uani 1 d . . Si2 Si -0.30406(13) 0.38016(7) 0.62540(8) 0.0635(4) Uani 1 d . . O1 O 0.4153(4) 0.2199(3) 0.8986(3) 0.1058(14) Uani 1 d . . O2 O -0.0057(4) 0.3295(3) 1.0029(3) 0.133(2) Uani 1 d . . N1 N 0.1215(3) 0.3248(2) 0.7877(2) 0.0528(9) Uani 1 d . . N2 N -0.2463(3) 0.2980(2) 0.6094(2) 0.0535(9) Uani 1 d . . C1 C 0.0352(4) 0.2850(2) 0.7528(2) 0.0454(9) Uani 1 d . . C2 C -0.0589(4) 0.3079(2) 0.6962(2) 0.0490(10) Uani 1 d . . H2 H -0.0642(4) 0.3565(2) 0.6909(2) 0.059 Uiso 1 calc R . C3 C -0.1478(4) 0.2707(2) 0.6454(2) 0.0452(9) Uani 1 d . . C4 C 0.0389(4) 0.2101(2) 0.7833(2) 0.0469(10) Uani 1 d . . C5 C -0.0581(4) 0.1761(2) 0.8136(3) 0.0608(12) Uani 1 d . . H5 H -0.1310(4) 0.1993(2) 0.8157(3) 0.073 Uiso 1 calc R . C6 C -0.0467(6) 0.1056(3) 0.8418(4) 0.089(2) Uani 1 d . . H6 H -0.1130(6) 0.0822(3) 0.8611(4) 0.107 Uiso 1 calc R . C7 C 0.0593(7) 0.0720(3) 0.8411(4) 0.098(2) Uani 1 d . . H7 H 0.0657(7) 0.0256(3) 0.8600(4) 0.117 Uiso 1 calc R . C8 C 0.1554(6) 0.1052(3) 0.8132(4) 0.088(2) Uani 1 d . . H8 H 0.2281(6) 0.0818(3) 0.8129(4) 0.105 Uiso 1 calc R . C9 C 0.1472(4) 0.1739(2) 0.7848(3) 0.0613(12) Uani 1 d . . H9 H 0.2149(4) 0.1963(2) 0.7663(3) 0.074 Uiso 1 calc R . C10 C -0.1297(4) 0.1941(2) 0.6246(2) 0.0446(9) Uani 1 d . . C11 C -0.2245(4) 0.1477(2) 0.6299(3) 0.0577(11) Uani 1 d . . H11 H -0.2975(4) 0.1642(2) 0.6472(3) 0.069 Uiso 1 calc R . C12 C -0.2122(5) 0.0768(2) 0.6099(3) 0.0749(14) Uani 1 d . . H12 H -0.2763(5) 0.0463(2) 0.6144(3) 0.090 Uiso 1 calc R . C13 C -0.1062(6) 0.0522(3) 0.5837(3) 0.080(2) Uani 1 d . . H13 H -0.0975(6) 0.0049(3) 0.5706(3) 0.096 Uiso 1 calc R . C14 C -0.0130(5) 0.0971(3) 0.5766(3) 0.078(2) Uani 1 d . . H14 H 0.0593(5) 0.0802(3) 0.5584(3) 0.093 Uiso 1 calc R . C15 C -0.0244(4) 0.1680(2) 0.5962(3) 0.0578(11) Uani 1 d . . H15 H 0.0399(4) 0.1981(2) 0.5900(3) 0.069 Uiso 1 calc R . C16 C 0.2986(6) 0.4307(3) 0.8227(4) 0.110(2) Uani 1 d . . H16A H 0.2837(6) 0.4283(3) 0.8829(4) 0.165 Uiso 1 calc R . H16B H 0.3232(6) 0.4774(3) 0.8086(4) 0.165 Uiso 1 calc R . H16C H 0.3605(6) 0.3980(3) 0.8100(4) 0.165 Uiso 1 calc R . C17 C 0.0487(6) 0.4779(3) 0.7810(5) 0.114(2) Uani 1 d . . H17A H -0.0250(6) 0.4686(3) 0.7489(5) 0.172 Uiso 1 calc R . H17B H 0.0790(6) 0.5229(3) 0.7646(5) 0.172 Uiso 1 calc R . H17C H 0.0352(6) 0.4781(3) 0.8416(5) 0.172 Uiso 1 calc R . C18 C 0.1888(6) 0.4128(3) 0.6409(3) 0.099(2) Uani 1 d . . H18A H 0.1173(6) 0.4011(3) 0.6073(3) 0.148 Uiso 1 calc R . H18B H 0.2508(6) 0.3801(3) 0.6283(3) 0.148 Uiso 1 calc R . H18C H 0.2135(6) 0.4595(3) 0.6268(3) 0.148 Uiso 1 calc R . C19 C -0.3105(5) 0.4064(3) 0.7406(3) 0.084(2) Uani 1 d . . H19A H -0.3511(5) 0.3707(3) 0.7714(3) 0.126 Uiso 1 calc R . H19B H -0.3528(5) 0.4501(3) 0.7442(3) 0.126 Uiso 1 calc R . H19C H -0.2309(5) 0.4120(3) 0.7655(3) 0.126 Uiso 1 calc R . C20 C -0.2253(6) 0.4496(3) 0.5662(4) 0.096(2) Uani 1 d . . H20A H -0.2218(6) 0.4363(3) 0.5068(4) 0.144 Uiso 1 calc R . H20B H -0.1458(6) 0.4551(3) 0.5913(4) 0.144 Uiso 1 calc R . H20C H -0.2677(6) 0.4932(3) 0.5700(4) 0.144 Uiso 1 calc R . C21 C -0.4615(6) 0.3760(3) 0.5806(5) 0.116(2) Uani 1 d . . H21A H -0.5038(6) 0.3404(3) 0.6103(5) 0.174 Uiso 1 calc R . H21B H -0.4623(6) 0.3648(3) 0.5202(5) 0.174 Uiso 1 calc R . H21C H -0.4993(6) 0.4207(3) 0.5880(5) 0.174 Uiso 1 calc R . C22 C 0.4772(8) 0.2461(6) 0.8322(6) 0.183(5) Uani 1 d . . H22A H 0.4975(8) 0.2950(6) 0.8430(6) 0.219 Uiso 1 calc R . H22B H 0.4289(8) 0.2433(6) 0.7786(6) 0.219 Uiso 1 calc R . C23 C 0.5823(9) 0.2057(8) 0.8263(7) 0.215(6) Uani 1 d . . H23A H 0.5769(9) 0.1770(8) 0.7746(7) 0.258 Uiso 1 calc R . H23B H 0.6511(9) 0.2364(8) 0.8235(7) 0.258 Uiso 1 calc R . C24 C 0.5946(9) 0.1625(6) 0.9001(8) 0.189(5) Uani 1 d . . H24A H 0.6592(9) 0.1790(6) 0.9389(8) 0.227 Uiso 1 calc R . H24B H 0.6107(9) 0.1143(6) 0.8840(8) 0.227 Uiso 1 calc R . C25 C 0.4836(7) 0.1674(5) 0.9395(5) 0.135(3) Uani 1 d . . H25A H 0.4418(7) 0.1228(5) 0.9347(5) 0.162 Uiso 1 calc R . H25B H 0.4969(7) 0.1785(5) 1.0002(5) 0.162 Uiso 1 calc R . C26 C -0.0926(10) 0.3555(8) 0.9498(7) 0.263(8) Uani 1 d . . H26A H -0.0642(10) 0.3981(8) 0.9234(7) 0.316 Uiso 1 calc R . H26B H -0.1108(10) 0.3217(8) 0.9041(7) 0.316 Uiso 1 calc R . C27 C -0.1914(10) 0.3698(9) 0.9888(7) 0.267(9) Uani 1 d . . H27A H -0.2607(10) 0.3509(9) 0.9567(7) 0.321 Uiso 1 calc R . H27B H -0.2014(10) 0.4202(9) 0.9953(7) 0.321 Uiso 1 calc R . C28 C -0.1751(9) 0.3372(10) 1.0691(8) 0.258(8) Uani 1 d . . H28A H -0.2044(9) 0.3666(10) 1.1144(8) 0.310 Uiso 1 calc R . H28B H -0.2159(9) 0.2922(10) 1.0695(8) 0.310 Uiso 1 calc R . C29 C -0.0539(9) 0.3285(8) 1.0794(6) 0.244(8) Uani 1 d . . H29A H -0.0198(9) 0.3659(8) 1.1153(6) 0.293 Uiso 1 calc R . H29B H -0.0362(9) 0.2840(8) 1.1079(6) 0.293 Uiso 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 K 0.0614(7) 0.0816(7) 0.0491(5) 0.0061(5) -0.0015(4) 0.0137(6) Si1 0.0782(10) 0.0462(7) 0.0633(8) 0.0037(6) -0.0129(7) -0.0168(6) Si2 0.0693(9) 0.0576(7) 0.0627(8) -0.0059(6) -0.0045(6) 0.0197(7) O1 0.073(3) 0.159(4) 0.087(3) 0.021(3) 0.017(2) 0.025(3) O2 0.081(3) 0.229(6) 0.091(3) 0.010(3) 0.019(3) 0.062(4) N1 0.061(2) 0.043(2) 0.054(2) 0.0023(15) -0.009(2) -0.010(2) N2 0.054(2) 0.053(2) 0.052(2) -0.006(2) -0.009(2) 0.007(2) C1 0.054(3) 0.038(2) 0.044(2) -0.001(2) 0.004(2) 0.001(2) C2 0.058(3) 0.035(2) 0.052(2) 0.000(2) -0.004(2) 0.002(2) C3 0.049(2) 0.044(2) 0.042(2) -0.002(2) 0.002(2) 0.000(2) C4 0.054(3) 0.039(2) 0.047(2) 0.002(2) -0.006(2) -0.002(2) C5 0.065(3) 0.057(3) 0.060(3) 0.010(2) -0.002(2) -0.009(2) C6 0.102(5) 0.072(4) 0.093(4) 0.030(3) -0.005(4) -0.032(3) C7 0.126(6) 0.050(3) 0.114(5) 0.023(3) -0.026(4) -0.001(4) C8 0.100(5) 0.051(3) 0.109(4) -0.005(3) -0.026(4) 0.021(3) C9 0.062(3) 0.048(2) 0.074(3) -0.002(2) -0.006(2) 0.003(2) C10 0.050(3) 0.041(2) 0.042(2) -0.002(2) -0.002(2) -0.003(2) C11 0.056(3) 0.052(2) 0.066(3) -0.003(2) 0.003(2) -0.001(2) C12 0.086(4) 0.052(3) 0.086(4) -0.005(2) -0.008(3) -0.014(3) C13 0.104(5) 0.052(3) 0.082(4) -0.021(3) -0.005(3) 0.002(3) C14 0.081(4) 0.063(3) 0.089(4) -0.025(3) 0.012(3) 0.009(3) C15 0.060(3) 0.055(3) 0.059(3) -0.013(2) 0.009(2) -0.003(2) C16 0.119(5) 0.081(4) 0.126(5) 0.014(4) -0.048(4) -0.044(4) C17 0.131(6) 0.053(3) 0.158(6) -0.015(4) -0.008(5) 0.005(3) C18 0.113(5) 0.105(5) 0.079(4) 0.013(3) 0.002(3) -0.046(4) C19 0.101(4) 0.078(3) 0.075(3) -0.014(3) 0.012(3) 0.017(3) C20 0.127(5) 0.066(3) 0.098(4) 0.018(3) 0.018(4) 0.024(3) C21 0.088(5) 0.112(5) 0.143(6) -0.026(4) -0.033(4) 0.043(4) C22 0.107(6) 0.292(13) 0.153(8) 0.112(8) 0.046(6) 0.036(8) C23 0.147(9) 0.360(18) 0.145(8) 0.072(10) 0.078(7) 0.101(10) C24 0.148(9) 0.215(11) 0.210(11) 0.057(9) 0.061(8) 0.091(8) C25 0.105(6) 0.166(8) 0.137(7) 0.056(6) 0.036(5) 0.036(6) C26 0.166(10) 0.495(23) 0.133(8) 0.096(11) 0.051(7) 0.191(13) C27 0.158(10) 0.511(24) 0.138(8) 0.116(12) 0.062(7) 0.198(13) C28 0.098(8) 0.504(25) 0.177(11) 0.094(14) 0.044(7) 0.016(11) C29 0.123(8) 0.483(23) 0.128(8) 0.063(11) 0.025(7) 0.115(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K O2 2.737(4) . ? K O1 2.749(4) . ? K N1 2.827(3) . ? K N2 2.833(3) 2 ? K C9 3.213(5) . ? K C11 3.243(5) 2 ? K C10 3.275(4) 2 ? K C4 3.314(4) . ? K C3 3.478(4) 2 ? K C1 3.520(4) . ? Si1 N1 1.711(3) . ? Si1 C16 1.860(6) . ? Si1 C18 1.863(5) . ? Si1 C17 1.869(6) . ? Si2 N2 1.715(3) . ? Si2 C20 1.859(6) . ? Si2 C19 1.862(5) . ? Si2 C21 1.865(6) . ? O1 C22 1.367(8) . ? O1 C25 1.391(8) . ? O2 C29 1.331(9) . ? O2 C26 1.336(9) . ? N1 C1 1.322(5) . ? N2 C3 1.317(5) . ? N2 K 2.833(3) 2_454 ? C1 C2 1.406(5) . ? C1 C4 1.502(5) . ? C2 C3 1.426(5) . ? C3 C10 1.509(5) . ? C3 K 3.478(4) 2_454 ? C4 C5 1.371(6) . ? C4 C9 1.395(6) . ? C5 C6 1.415(7) . ? C6 C7 1.352(8) . ? C7 C8 1.341(8) . ? C8 C9 1.379(6) . ? C10 C15 1.375(6) . ? C10 C11 1.389(6) . ? C10 K 3.275(4) 2_454 ? C11 C12 1.392(6) . ? C11 K 3.243(5) 2_454 ? C12 C13 1.359(7) . ? C13 C14 1.359(7) . ? C14 C15 1.389(6) . ? C22 C23 1.414(11) . ? C23 C24 1.410(11) . ? C24 C25 1.419(10) . ? C26 C27 1.319(10) . ? C27 C28 1.396(13) . ? C28 C29 1.370(12) . ? 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 O2 K O1 177.5(2) . . ? O2 K N1 83.43(13) . . ? O1 K N1 96.13(12) . . ? O2 K N2 93.91(13) . 2 ? O1 K N2 86.91(12) . 2 ? N1 K N2 170.65(11) . 2 ? O2 K C9 109.8(2) . . ? O1 K C9 71.82(13) . . ? N1 K C9 56.67(10) . . ? N2 K C9 116.51(11) 2 . ? O2 K C11 74.86(14) . 2 ? O1 K C11 103.70(13) . 2 ? N1 K C11 130.92(11) . 2 ? N2 K C11 56.22(11) 2 2 ? C9 K C11 172.18(11) . 2 ? O2 K C10 98.03(14) . 2 ? O1 K C10 80.86(12) . 2 ? N1 K C10 144.18(10) . 2 ? N2 K C10 45.02(10) 2 2 ? C9 K C10 148.51(11) . 2 ? C11 K C10 24.60(10) 2 2 ? O2 K C4 86.02(14) . . ? O1 K C4 95.41(12) . . ? N1 K C4 44.55(9) . . ? N2 K C4 126.46(10) 2 . ? C9 K C4 24.62(10) . . ? C11 K C4 160.88(11) 2 . ? C10 K C4 170.56(10) 2 . ? O2 K C3 102.50(13) . 2 ? O1 K C3 77.49(11) . 2 ? N1 K C3 168.09(10) . 2 ? N2 K C3 21.08(9) 2 2 ? C9 K C3 128.66(11) . 2 ? C11 K C3 43.51(10) 2 2 ? C10 K C3 25.59(9) 2 2 ? C4 K C3 145.14(10) . 2 ? O2 K C1 78.94(13) . . ? O1 K C1 101.50(11) . . ? N1 K C1 20.55(9) . . ? N2 K C1 150.11(10) 2 . ? C9 K C1 43.21(10) . . ? C11 K C1 144.54(10) 2 . ? C10 K C1 164.13(10) 2 . ? C4 K C1 25.16(9) . . ? C3 K C1 170.27(9) 2 . ? N1 Si1 C16 106.4(2) . . ? N1 Si1 C18 111.6(2) . . ? C16 Si1 C18 109.4(3) . . ? N1 Si1 C17 115.2(3) . . ? C16 Si1 C17 106.1(3) . . ? C18 Si1 C17 107.9(3) . . ? N2 Si2 C20 112.5(2) . . ? N2 Si2 C19 114.7(2) . . ? C20 Si2 C19 109.2(3) . . ? N2 Si2 C21 105.4(2) . . ? C20 Si2 C21 108.1(3) . . ? C19 Si2 C21 106.6(3) . . ? C22 O1 C25 108.4(6) . . ? C22 O1 K 125.1(5) . . ? C25 O1 K 126.2(4) . . ? C29 O2 C26 103.7(6) . . ? C29 O2 K 130.6(5) . . ? C26 O2 K 124.8(5) . . ? C1 N1 Si1 127.4(3) . . ? C1 N1 K 110.8(2) . . ? Si1 N1 K 120.0(2) . . ? C3 N2 Si2 127.7(3) . . ? C3 N2 K 108.2(2) . 2_454 ? Si2 N2 K 119.5(2) . 2_454 ? N1 C1 C2 126.0(4) . . ? N1 C1 C4 114.0(4) . . ? C2 C1 C4 119.9(4) . . ? N1 C1 K 48.6(2) . . ? C2 C1 K 156.1(3) . . ? C4 C1 K 69.7(2) . . ? C1 C2 C3 132.2(4) . . ? N2 C3 C2 125.9(4) . . ? N2 C3 C10 114.1(3) . . ? C2 C3 C10 119.9(4) . . ? N2 C3 K 50.7(2) . 2_454 ? C2 C3 K 152.7(3) . 2_454 ? C10 C3 K 69.7(2) . 2_454 ? C5 C4 C9 118.0(4) . . ? C5 C4 C1 123.1(4) . . ? C9 C4 C1 118.9(4) . . ? C5 C4 K 108.3(3) . . ? C9 C4 K 73.7(2) . . ? C1 C4 K 85.1(2) . . ? C4 C5 C6 119.5(5) . . ? C7 C6 C5 120.8(5) . . ? C8 C7 C6 120.1(5) . . ? C7 C8 C9 120.6(6) . . ? C8 C9 C4 121.0(5) . . ? C8 C9 K 106.7(3) . . ? C4 C9 K 81.7(2) . . ? C15 C10 C11 117.5(4) . . ? C15 C10 C3 123.1(4) . . ? C11 C10 C3 119.3(4) . . ? C15 C10 K 105.9(3) . 2_454 ? C11 C10 K 76.4(2) . 2_454 ? C3 C10 K 84.7(2) . 2_454 ? C10 C11 C12 121.2(4) . . ? C10 C11 K 79.0(2) . 2_454 ? C12 C11 K 106.7(3) . 2_454 ? C13 C12 C11 119.9(5) . . ? C14 C13 C12 119.8(5) . . ? C13 C14 C15 120.8(5) . . ? C10 C15 C14 120.8(4) . . ? O1 C22 C23 108.0(8) . . ? C24 C23 C22 108.0(7) . . ? C23 C24 C25 105.2(8) . . ? O1 C25 C24 109.0(7) . . ? C27 C26 O2 113.4(8) . . ? C26 C27 C28 104.1(9) . . ? C29 C28 C27 103.9(9) . . ? O2 C29 C28 110.0(9) . . ? _refine_diff_density_max 0.463 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.053 #===END data_mfl-2 _database_code_CSD 187159 _audit_creation_date 2000-03-06T17:26:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{K(thf)2(Me3SiNCPhCHCPhNH)}2].2(thf)' _chemical_formula_moiety '(C52 H74 K2 N4 O4 Si2).2(C4 H8 O)' _chemical_formula_sum 'C60 H90 K2 N4 O6 Si2' _chemical_formula_weight 1097.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8158(3) _cell_length_b 10.7658(3) _cell_length_c 15.2080(5) _cell_angle_alpha 83.771(2) _cell_angle_beta 88.730(2) _cell_angle_gamma 89.386(2) _cell_volume 1597.17(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16822 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_T_min 0.9122 _exptl_absorpt_correction_T_max 0.9331 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18737 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 5491 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; H atoms on C2 and N2 were 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^)+(0.0817P)^2^+1.0209P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5491 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.574 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 K K 0.17253(5) -0.10156(5) 0.08003(3) 0.03964(18) Uani 1 1 d . . . Si Si 0.01189(7) -0.06310(6) 0.32681(4) 0.0405(2) Uani 1 1 d . . . O1 O 0.2639(3) -0.2754(2) -0.02647(16) 0.0846(8) Uani 1 1 d . . . O2 O 0.4165(2) -0.1596(2) 0.16253(15) 0.0651(6) Uani 1 1 d . . . N1 N -0.0150(2) -0.12663(17) 0.23025(12) 0.0374(4) Uani 1 1 d . . . N2 N -0.1544(2) -0.07269(18) 0.06519(14) 0.0376(4) Uani 1 1 d . . . H2A H -0.129(3) -0.056(3) 0.114(2) 0.046(8) Uiso 1 1 d . . . C1 C -0.0273(2) -0.2437(2) 0.21245(14) 0.0337(5) Uani 1 1 d . . . C2 C -0.0776(2) -0.2774(2) 0.13300(15) 0.0347(5) Uani 1 1 d . . . H2 H -0.078(2) -0.359(3) 0.1253(16) 0.037(6) Uiso 1 1 d . . . C3 C -0.1351(2) -0.1924(2) 0.06421(14) 0.0325(5) Uani 1 1 d . . . C4 C 0.0204(2) -0.3508(2) 0.27717(14) 0.0363(5) Uani 1 1 d . . . C5 C -0.0661(3) -0.4460(2) 0.31090(17) 0.0466(6) Uani 1 1 d . . . H5 H -0.1579 -0.4457 0.2924 0.056 Uiso 1 1 calc R . . C6 C -0.0194(4) -0.5423(3) 0.3717(2) 0.0616(8) Uani 1 1 d . . . H6 H -0.0801 -0.6059 0.3956 0.074 Uiso 1 1 calc R . . C7 C 0.1131(4) -0.5458(3) 0.3972(2) 0.0637(8) Uani 1 1 d . . . H7 H 0.1443 -0.6115 0.4388 0.076 Uiso 1 1 calc R . . C8 C 0.2009(3) -0.4547(3) 0.3628(2) 0.0620(8) Uani 1 1 d . . . H8 H 0.2937 -0.4585 0.3793 0.074 Uiso 1 1 calc R . . C9 C 0.1550(3) -0.3567(3) 0.30370(18) 0.0495(6) Uani 1 1 d . . . H9 H 0.2164 -0.2928 0.2811 0.059 Uiso 1 1 calc R . . C10 C -0.1778(2) -0.2463(2) -0.01791(14) 0.0351(5) Uani 1 1 d . . . C11 C -0.1013(3) -0.3383(3) -0.05433(17) 0.0474(6) Uani 1 1 d . . . H11 H -0.0211 -0.3701 -0.0258 0.057 Uiso 1 1 calc R . . C12 C -0.1402(3) -0.3843(3) -0.13156(19) 0.0585(7) Uani 1 1 d . . . H12 H -0.0862 -0.4466 -0.1557 0.07 Uiso 1 1 calc R . . C13 C -0.2570(3) -0.3399(3) -0.17356(18) 0.0574(7) Uani 1 1 d . . . H13 H -0.2838 -0.3714 -0.2265 0.069 Uiso 1 1 calc R . . C14 C -0.3342(3) -0.2498(3) -0.13812(18) 0.0524(6) Uani 1 1 d . . . H14 H -0.415 -0.2195 -0.1666 0.063 Uiso 1 1 calc R . . C15 C -0.2955(2) -0.2025(2) -0.06132(16) 0.0424(5) Uani 1 1 d . . . H15 H -0.3496 -0.1396 -0.038 0.051 Uiso 1 1 calc R . . C16 C -0.0791(5) 0.0907(3) 0.3179(3) 0.0859(12) Uani 1 1 d . . . H16A H -0.0467 0.1425 0.2648 0.129 Uiso 1 1 calc R . . H16B H -0.0612 0.1331 0.3703 0.129 Uiso 1 1 calc R . . H16C H -0.1773 0.0774 0.3141 0.129 Uiso 1 1 calc R . . C17 C -0.0542(4) -0.1575(3) 0.42825(19) 0.0714(9) Uani 1 1 d . . . H17A H -0.0082 -0.2391 0.4346 0.107 Uiso 1 1 calc R . . H17B H -0.1525 -0.1692 0.4235 0.107 Uiso 1 1 calc R . . H17C H -0.0366 -0.1138 0.4801 0.107 Uiso 1 1 calc R . . C18 C 0.1952(4) -0.0264(4) 0.3414(3) 0.0819(11) Uani 1 1 d . . . H18A H 0.2304 0.0229 0.2879 0.123 Uiso 1 1 calc R . . H18B H 0.2476 -0.1043 0.3518 0.123 Uiso 1 1 calc R . . H18C H 0.2035 0.0216 0.3922 0.123 Uiso 1 1 calc R . . C19 C 0.2468(4) -0.2322(3) -0.1163(2) 0.0652(8) Uani 1 1 d . . . H19A H 0.3186 -0.1716 -0.1372 0.078 Uiso 1 1 calc R . . H19B H 0.1567 -0.1911 -0.1253 0.078 Uiso 1 1 calc R . . C20 C 0.2571(5) -0.3446(4) -0.1646(3) 0.0867(11) Uani 1 1 d . . . H20A H 0.1654 -0.3783 -0.1733 0.104 Uiso 1 1 calc R . . H20B H 0.3019 -0.324 -0.2233 0.104 Uiso 1 1 calc R . . C21 C 0.3397(4) -0.4362(3) -0.1087(3) 0.0857(12) Uani 1 1 d . . . H21A H 0.4319 -0.4451 -0.135 0.103 Uiso 1 1 calc R . . H21B H 0.2955 -0.519 -0.1012 0.103 Uiso 1 1 calc R . . C22 C 0.3470(4) -0.3830(3) -0.0215(3) 0.0814(10) Uani 1 1 d . . . H22A H 0.3145 -0.445 0.027 0.098 Uiso 1 1 calc R . . H22B H 0.4422 -0.3614 -0.0099 0.098 Uiso 1 1 calc R . . C23 C 0.5119(3) -0.0722(3) 0.1877(3) 0.0729(9) Uani 1 1 d . . . H23A H 0.464 0.0012 0.2081 0.087 Uiso 1 1 calc R . . H23B H 0.5729 -0.0432 0.1371 0.087 Uiso 1 1 calc R . . C24 C 0.5914(4) -0.1385(5) 0.2605(3) 0.0953(14) Uani 1 1 d . . . H24A H 0.5631 -0.1111 0.3183 0.114 Uiso 1 1 calc R . . H24B H 0.6902 -0.1235 0.2508 0.114 Uiso 1 1 calc R . . C25 C 0.5584(5) -0.2742(5) 0.2568(3) 0.1075(16) Uani 1 1 d . . . H25A H 0.6427 -0.3254 0.2553 0.129 Uiso 1 1 calc R . . H25B H 0.5014 -0.3069 0.3085 0.129 Uiso 1 1 calc R . . C26 C 0.4827(4) -0.2753(3) 0.1734(3) 0.0774(10) Uani 1 1 d . . . H26A H 0.5459 -0.285 0.1229 0.093 Uiso 1 1 calc R . . H26B H 0.4161 -0.3443 0.1784 0.093 Uiso 1 1 calc R . . C27 C 0.5894(10) -0.6246(7) 0.4118(6) 0.170(3) Uani 1 1 d . . . C28 C 0.590(2) -0.7163(14) 0.4783(8) 0.380(14) Uani 1 1 d . . . C29 C 0.5002(16) -0.8166(10) 0.4631(7) 0.272(8) Uani 1 1 d . . . C30 C 0.4650(16) -0.7823(11) 0.3795(8) 0.271(8) Uani 1 1 d . . . C31 C 0.4993(7) -0.6575(7) 0.3544(5) 0.142(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K 0.0398(3) 0.0408(3) 0.0369(3) 0.0022(2) -0.0019(2) 0.0008(2) Si 0.0535(4) 0.0391(4) 0.0301(3) -0.0078(3) -0.0049(3) -0.0027(3) O1 0.110(2) 0.0829(16) 0.0647(15) -0.0251(12) -0.0250(13) 0.0400(15) O2 0.0501(11) 0.0668(13) 0.0796(15) -0.0113(11) -0.0167(10) 0.0054(10) N1 0.0501(11) 0.0334(10) 0.0290(9) -0.0041(7) -0.0033(8) -0.0021(8) N2 0.0443(11) 0.0356(10) 0.0332(11) -0.0037(8) -0.0051(8) 0.0011(8) C1 0.0377(11) 0.0328(11) 0.0301(11) -0.0015(8) 0.0013(9) -0.0016(9) C2 0.0427(12) 0.0282(11) 0.0335(11) -0.0041(9) -0.0033(9) -0.0007(9) C3 0.0324(11) 0.0351(11) 0.0302(11) -0.0040(9) 0.0020(8) -0.0019(9) C4 0.0481(13) 0.0335(11) 0.0276(11) -0.0051(9) -0.0011(9) 0.0013(9) C5 0.0551(15) 0.0402(13) 0.0434(14) 0.0008(10) -0.0005(11) -0.0012(11) C6 0.081(2) 0.0435(15) 0.0568(17) 0.0109(13) 0.0088(15) -0.0051(14) C7 0.088(2) 0.0539(17) 0.0459(15) 0.0110(13) -0.0107(15) 0.0137(15) C8 0.0656(18) 0.0592(17) 0.0593(18) 0.0043(14) -0.0204(14) 0.0112(14) C9 0.0522(15) 0.0470(14) 0.0482(15) 0.0020(11) -0.0090(11) -0.0011(11) C10 0.0382(11) 0.0360(11) 0.0308(11) -0.0016(9) -0.0010(9) -0.0057(9) C11 0.0483(14) 0.0553(15) 0.0402(13) -0.0128(11) -0.0043(11) 0.0083(11) C12 0.0675(18) 0.0632(17) 0.0490(16) -0.0249(13) -0.0021(13) 0.0081(14) C13 0.0745(19) 0.0605(17) 0.0400(14) -0.0144(12) -0.0144(13) -0.0072(14) C14 0.0537(15) 0.0557(16) 0.0487(15) -0.0055(12) -0.0197(12) -0.0040(12) C15 0.0432(13) 0.0412(13) 0.0433(13) -0.0056(10) -0.0074(10) -0.0029(10) C16 0.137(3) 0.0559(19) 0.071(2) -0.0304(17) -0.039(2) 0.028(2) C17 0.109(3) 0.069(2) 0.0374(15) -0.0125(14) 0.0139(16) -0.0175(18) C18 0.071(2) 0.103(3) 0.080(2) -0.042(2) -0.0051(18) -0.0237(19) C19 0.082(2) 0.0503(16) 0.0636(19) -0.0073(14) -0.0020(16) 0.0024(15) C20 0.106(3) 0.082(2) 0.078(2) -0.035(2) 0.001(2) 0.017(2) C21 0.073(2) 0.0490(18) 0.139(4) -0.028(2) 0.009(2) -0.0067(16) C22 0.077(2) 0.067(2) 0.096(3) 0.0146(19) -0.009(2) 0.0046(17) C23 0.0611(19) 0.0630(19) 0.096(3) -0.0133(18) 0.0023(17) -0.0035(15) C24 0.062(2) 0.155(4) 0.071(2) -0.020(3) -0.0110(18) -0.011(2) C25 0.084(3) 0.122(4) 0.105(3) 0.037(3) -0.005(2) 0.030(3) C26 0.073(2) 0.062(2) 0.098(3) -0.0168(18) 0.0157(19) 0.0064(16) C27 0.190(7) 0.138(6) 0.175(7) 0.029(5) -0.037(6) -0.057(5) C28 0.69(3) 0.279(14) 0.173(9) 0.046(9) -0.190(15) -0.30(2) C29 0.436(19) 0.207(9) 0.160(8) 0.078(7) -0.116(10) -0.186(11) C30 0.404(19) 0.215(10) 0.191(10) 0.031(8) -0.140(11) -0.152(12) C31 0.116(4) 0.157(6) 0.143(5) 0.045(4) -0.037(4) -0.015(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K O1 2.736(2) . ? K N2 2.746(2) 2 ? K O2 2.762(2) . ? K N1 2.893(2) . ? K C1 3.077(2) . ? K C2 3.153(2) . ? K C3 3.207(2) . ? K N2 3.231(2) . ? K C15 3.481(2) 2 ? K C19 3.495(3) . ? K K 4.6077(10) 2 ? Si N1 1.7126(19) . ? Si C17 1.861(3) . ? Si C16 1.867(3) . ? Si C18 1.869(3) . ? O1 C22 1.406(4) . ? O1 C19 1.408(4) . ? O2 C26 1.394(4) . ? O2 C23 1.422(4) . ? N1 C1 1.325(3) . ? N2 C3 1.302(3) . ? N2 K 2.746(2) 2 ? C1 C2 1.400(3) . ? C1 C4 1.510(3) . ? C2 C3 1.435(3) . ? C3 C10 1.502(3) . ? C4 C5 1.386(3) . ? C4 C9 1.388(4) . ? C5 C6 1.393(4) . ? C6 C7 1.364(5) . ? C7 C8 1.365(5) . ? C8 C9 1.388(4) . ? C10 C11 1.392(3) . ? C10 C15 1.396(3) . ? C11 C12 1.386(4) . ? C12 C13 1.380(4) . ? C13 C14 1.373(4) . ? C14 C15 1.386(4) . ? C15 K 3.481(2) 2 ? C19 C20 1.483(5) . ? C20 C21 1.479(6) . ? C21 C22 1.503(6) . ? C23 C24 1.482(6) . ? C24 C25 1.508(7) . ? C25 C26 1.485(6) . ? C27 C31 1.334(9) . ? C27 C28 1.334(12) . ? C28 C29 1.444(12) . ? C29 C30 1.338(11) . ? C30 C31 1.399(11) . ? 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 O1 K N2 89.93(7) . 2 ? O1 K O2 82.22(7) . . ? N2 K O2 122.16(7) 2 . ? O1 K N1 130.26(8) . . ? N2 K N1 125.82(6) 2 . ? O2 K N1 100.74(6) . . ? O1 K C1 104.88(8) . . ? N2 K C1 136.63(6) 2 . ? O2 K C1 100.39(7) . . ? N1 K C1 25.41(5) . . ? O1 K C2 87.74(8) . . ? N2 K C2 119.05(6) 2 . ? O2 K C2 117.75(6) . . ? N1 K C2 46.62(5) . . ? C1 K C2 25.94(6) . . ? O1 K C3 90.74(7) . . ? N2 K C3 93.19(6) 2 . ? O2 K C3 143.73(6) . . ? N1 K C3 57.94(5) . . ? C1 K C3 47.16(6) . . ? C2 K C3 26.06(6) . . ? O1 K N2 109.31(7) . . ? N2 K N2 79.44(6) 2 . ? O2 K N2 156.35(6) . . ? N1 K N2 55.90(5) . . ? C1 K N2 57.22(5) . . ? C2 K N2 45.08(5) . . ? C3 K N2 23.34(5) . . ? O1 K C15 122.67(8) . 2 ? N2 K C15 53.60(6) 2 2 ? O2 K C15 83.75(6) . 2 ? N1 K C15 106.91(6) . 2 ? C1 K C15 132.31(6) . 2 ? C2 K C15 146.17(6) . 2 ? C3 K C15 128.43(6) . 2 ? N2 K C15 105.33(5) . 2 ? O1 K C19 22.09(7) . . ? N2 K C19 68.31(7) 2 . ? O2 K C19 97.68(8) . . ? N1 K C19 141.01(7) . . ? C1 K C19 117.23(7) . . ? C2 K C19 94.39(7) . . ? C3 K C19 87.55(7) . . ? N2 K C19 99.73(7) . . ? C15 K C19 109.04(7) 2 . ? O1 K K 103.37(5) . 2 ? N2 K K 43.58(4) 2 2 ? O2 K K 163.65(5) . 2 ? N1 K K 87.45(4) . 2 ? C1 K K 93.07(4) . 2 ? C2 K K 78.13(4) . 2 ? C3 K K 52.36(4) . 2 ? N2 K K 35.86(4) . 2 ? C15 K K 80.32(4) 2 2 ? C19 K K 84.16(6) . 2 ? N1 Si C17 114.71(12) . . ? N1 Si C16 106.74(13) . . ? C17 Si C16 107.59(19) . . ? N1 Si C18 112.51(14) . . ? C17 Si C18 109.27(19) . . ? C16 Si C18 105.4(2) . . ? C22 O1 C19 108.3(3) . . ? C22 O1 K 139.2(2) . . ? C19 O1 K 110.92(17) . . ? C26 O2 C23 105.6(3) . . ? C26 O2 K 127.6(2) . . ? C23 O2 K 125.90(19) . . ? C1 N1 Si 132.13(16) . . ? C1 N1 K 85.05(12) . . ? Si N1 K 123.70(10) . . ? C3 N2 K 126.28(15) . 2 ? C3 N2 K 77.27(13) . . ? K N2 K 100.56(6) 2 . ? N1 C1 C2 123.8(2) . . ? N1 C1 C4 120.63(19) . . ? C2 C1 C4 115.47(19) . . ? N1 C1 K 69.54(12) . . ? C2 C1 K 80.08(13) . . ? C4 C1 K 121.20(14) . . ? C1 C2 C3 125.1(2) . . ? C1 C2 K 73.98(12) . . ? C3 C2 K 79.05(12) . . ? N2 C3 C2 126.8(2) . . ? N2 C3 C10 116.16(19) . . ? C2 C3 C10 116.99(19) . . ? N2 C3 K 79.39(13) . . ? C2 C3 K 74.89(12) . . ? C10 C3 K 119.72(13) . . ? C5 C4 C9 118.0(2) . . ? C5 C4 C1 121.9(2) . . ? C9 C4 C1 120.0(2) . . ? C4 C5 C6 120.5(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C8 119.9(3) . . ? C7 C8 C9 120.3(3) . . ? C8 C9 C4 120.8(3) . . ? C11 C10 C15 117.9(2) . . ? C11 C10 C3 121.9(2) . . ? C15 C10 C3 120.2(2) . . ? C12 C11 C10 121.1(2) . . ? C13 C12 C11 120.3(3) . . ? C14 C13 C12 119.4(2) . . ? C13 C14 C15 120.7(3) . . ? C14 C15 C10 120.7(2) . . ? C14 C15 K 117.67(17) . 2 ? C10 C15 K 90.53(14) . 2 ? O1 C19 C20 105.8(3) . . ? O1 C19 K 46.98(13) . . ? C20 C19 K 149.0(3) . . ? C21 C20 C19 105.7(3) . . ? C20 C21 C22 104.6(3) . . ? O1 C22 C21 107.6(3) . . ? O2 C23 C24 106.5(3) . . ? C23 C24 C25 103.9(3) . . ? C26 C25 C24 104.3(3) . . ? O2 C26 C25 104.5(3) . . ? C31 C27 C28 106.2(7) . . ? C27 C28 C29 112.0(9) . . ? C30 C29 C28 101.0(8) . . ? C29 C30 C31 110.4(8) . . ? C27 C31 C30 107.7(7) . . ? #===END data_mfl-3 _database_code_CSD 187160 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{(Me2NCH2CH2NMe2)K(Me3SiNCPhCHCPhNH)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C48 H74 K2 N8 Si2' _chemical_formula_weight 897.53 _chemical_melting_point ? _chemical_compound_source ? 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 12.361(3) _cell_length_b 16.470(4) _cell_length_c 13.088(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.54(2) _cell_angle_gamma 90.00 _cell_volume 2656.2(11) _cell_formula_units_Z 2 _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 ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method ? _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.262 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3420 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0993 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 21.98 _reflns_number_total 3249 _reflns_number_observed 2030 _reflns_observed_criterion >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-93 (Sheldrick, 1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+2.3196P] 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 'H on N2 was refined others were riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3248 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_obs 0.0604 _refine_ls_wR_factor_all 0.1431 _refine_ls_wR_factor_obs 0.1194 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.126 _refine_ls_restrained_S_all 1.041 _refine_ls_restrained_S_obs 1.126 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K K -0.05613(9) 0.11377(7) 0.06934(9) 0.0320(3) Uani 1 d . . Si Si -0.29339(11) 0.03218(9) 0.23267(11) 0.0314(4) Uani 1 d . . N1 N -0.2613(3) 0.0411(2) 0.1091(3) 0.0303(11) Uani 1 d . . N2 N -0.1361(3) -0.0361(3) -0.0418(4) 0.0302(11) Uani 1 d . . H1 H -0.1547(32) -0.0334(25) 0.0154(31) 0.006(13) Uiso 1 d . . N3 N 0.0508(4) 0.2428(3) 0.1788(4) 0.0496(13) Uani 1 d . . N4 N -0.0321(5) 0.2553(3) -0.0418(4) 0.072(2) Uani 1 d . . C1 C -0.3119(4) 0.0752(3) 0.0268(4) 0.0253(12) Uani 1 d . . C2 C -0.2824(4) 0.0639(3) -0.0718(4) 0.0264(12) Uani 1 d . . H2 H -0.3214(4) 0.0937(3) -0.1248(4) 0.032 Uiso 1 calc R . C3 C -0.1979(4) 0.0110(3) -0.1013(4) 0.0256(12) Uani 1 d . . C4 C -0.4048(4) 0.1335(3) 0.0379(4) 0.0284(13) Uani 1 d . . C5 C -0.3861(5) 0.2081(4) 0.0849(4) 0.045(2) Uani 1 d . . H5 H -0.3146(5) 0.2215(4) 0.1115(4) 0.054 Uiso 1 calc R . C6 C -0.4687(5) 0.2632(4) 0.0941(5) 0.056(2) Uani 1 d . . H6 H -0.4537(5) 0.3146(4) 0.1250(5) 0.067 Uiso 1 calc R . C7 C -0.5733(5) 0.2432(4) 0.0581(5) 0.052(2) Uani 1 d . . H7 H -0.6309(5) 0.2805(4) 0.0650(5) 0.063 Uiso 1 calc R . C8 C -0.5937(5) 0.1695(4) 0.0127(4) 0.048(2) Uani 1 d . . H8 H -0.6658(5) 0.1551(4) -0.0110(4) 0.058 Uiso 1 calc R . C9 C -0.5093(4) 0.1159(3) 0.0011(4) 0.0354(13) Uani 1 d . . H9 H -0.5241(4) 0.0657(3) -0.0331(4) 0.042 Uiso 1 calc R . C10 C -0.1794(4) 0.0093(3) -0.2124(4) 0.0258(12) Uani 1 d . . C11 C -0.0740(4) 0.0161(3) -0.2429(4) 0.0343(14) Uani 1 d . . H11 H -0.0145(4) 0.0229(3) -0.1931(4) 0.041 Uiso 1 calc R . C12 C -0.0565(5) 0.0128(3) -0.3458(4) 0.045(2) Uani 1 d . . H12 H 0.0153(5) 0.0172(3) -0.3661(4) 0.053 Uiso 1 calc R . C13 C -0.1409(5) 0.0033(4) -0.4188(4) 0.054(2) Uani 1 d . . H13 H -0.1278(5) 0.0013(4) -0.4892(4) 0.065 Uiso 1 calc R . C14 C -0.2447(5) -0.0033(4) -0.3897(4) 0.051(2) Uani 1 d . . H14 H -0.3036(5) -0.0107(4) -0.4400(4) 0.062 Uiso 1 calc R . C15 C -0.2633(4) 0.0009(3) -0.2873(4) 0.0369(14) Uani 1 d . . H15 H -0.3357(4) -0.0021(3) -0.2681(4) 0.044 Uiso 1 calc R . C16 C -0.4411(4) 0.0342(4) 0.2540(4) 0.0422(15) Uani 1 d . . H16A H -0.4717(4) 0.0870(4) 0.2329(4) 0.063 Uiso 1 calc R . H16B H -0.4504(4) 0.0253(4) 0.3268(4) 0.063 Uiso 1 calc R . H16C H -0.4787(4) -0.0088(4) 0.2133(4) 0.063 Uiso 1 calc R . C17 C -0.2416(4) -0.0702(3) 0.2745(4) 0.0413(15) Uani 1 d . . H17A H -0.1640(4) -0.0740(3) 0.2647(4) 0.062 Uiso 1 calc R . H17B H -0.2810(4) -0.1123(3) 0.2337(4) 0.062 Uiso 1 calc R . H17C H -0.2527(4) -0.0782(3) 0.3472(4) 0.062 Uiso 1 calc R . C18 C -0.2226(4) 0.1110(3) 0.3164(4) 0.049(2) Uani 1 d . . H18A H -0.1449(4) 0.1107(3) 0.3060(4) 0.074 Uiso 1 calc R . H18B H -0.2328(4) 0.0990(3) 0.3883(4) 0.074 Uiso 1 calc R . H18C H -0.2530(4) 0.1646(3) 0.2986(4) 0.074 Uiso 1 calc R . C19 C 0.0590(12) 0.3088(6) 0.1137(8) 0.218(8) Uani 1 d . . H19A H 0.0197(12) 0.3532(6) 0.1459(8) 0.262 Uiso 1 calc R . H19B H 0.1366(12) 0.3242(6) 0.1215(8) 0.262 Uiso 1 calc R . C20 C 0.0311(8) 0.3159(5) 0.0146(6) 0.099(3) Uani 1 d . . H20A H 0.0992(8) 0.3223(5) -0.0197(6) 0.119 Uiso 1 calc R . H20B H -0.0090(8) 0.3678(5) 0.0051(6) 0.119 Uiso 1 calc R . C21 C 0.0008(9) 0.2667(6) 0.2665(8) 0.189(7) Uani 1 d . . H21A H -0.0047(9) 0.2199(6) 0.3121(8) 0.284 Uiso 1 calc R . H21B H -0.0720(9) 0.2877(6) 0.2464(8) 0.284 Uiso 1 calc R . H21C H 0.0443(9) 0.3093(6) 0.3024(8) 0.284 Uiso 1 calc R . C22 C 0.1555(7) 0.2147(5) 0.2088(9) 0.160(5) Uani 1 d . . H22A H 0.1509(7) 0.1681(5) 0.2547(9) 0.240 Uiso 1 calc R . H22B H 0.1973(7) 0.2582(5) 0.2445(9) 0.240 Uiso 1 calc R . H22C H 0.1915(7) 0.1982(5) 0.1480(9) 0.240 Uiso 1 calc R . C23 C -0.1344(9) 0.2865(6) -0.0792(10) 0.203(7) Uani 1 d . . H23A H -0.1759(9) 0.2440(6) -0.1173(10) 0.305 Uiso 1 calc R . H23B H -0.1238(9) 0.3326(6) -0.1247(10) 0.305 Uiso 1 calc R . H23C H -0.1743(9) 0.3045(6) -0.0215(10) 0.305 Uiso 1 calc R . C24 C 0.0245(11) 0.2248(6) -0.1263(7) 0.166(6) Uani 1 d . . H24A H 0.0952(11) 0.2032(6) -0.1003(7) 0.249 Uiso 1 calc R . H24B H 0.0350(11) 0.2690(6) -0.1746(7) 0.249 Uiso 1 calc R . H24C H -0.0184(11) 0.1816(6) -0.1613(7) 0.249 Uiso 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 K 0.0269(6) 0.0290(7) 0.0408(7) -0.0030(6) 0.0065(5) 0.0002(6) Si 0.0265(8) 0.0392(9) 0.0292(9) -0.0001(7) 0.0058(6) -0.0012(7) N1 0.026(2) 0.037(3) 0.029(3) 0.006(2) 0.007(2) 0.003(2) N2 0.027(3) 0.038(3) 0.026(3) 0.000(2) 0.005(2) -0.001(2) N3 0.054(3) 0.042(3) 0.052(3) -0.010(3) -0.006(3) -0.008(3) N4 0.108(5) 0.045(4) 0.062(4) 0.013(3) -0.005(4) -0.028(4) C1 0.020(3) 0.025(3) 0.032(3) -0.003(3) 0.010(2) -0.003(2) C2 0.023(3) 0.027(3) 0.029(3) 0.007(2) 0.005(2) 0.007(2) C3 0.021(3) 0.024(3) 0.032(3) -0.003(3) 0.004(2) -0.005(2) C4 0.029(3) 0.034(4) 0.023(3) 0.000(3) 0.010(2) 0.004(3) C5 0.038(3) 0.046(4) 0.052(4) -0.007(3) 0.002(3) 0.001(3) C6 0.061(5) 0.040(4) 0.067(5) -0.021(3) 0.004(4) 0.013(4) C7 0.042(4) 0.058(5) 0.060(4) -0.007(4) 0.014(3) 0.027(3) C8 0.031(3) 0.056(4) 0.059(4) -0.010(4) 0.007(3) 0.012(3) C9 0.029(3) 0.034(3) 0.044(3) -0.008(3) 0.007(3) 0.006(3) C10 0.023(3) 0.026(3) 0.030(3) 0.000(2) 0.009(2) 0.003(2) C11 0.030(3) 0.038(3) 0.034(3) 0.005(3) 0.001(3) 0.004(3) C12 0.036(3) 0.062(4) 0.038(4) 0.008(3) 0.013(3) 0.006(3) C13 0.060(4) 0.073(5) 0.033(4) 0.004(3) 0.021(3) 0.014(4) C14 0.048(4) 0.083(5) 0.023(3) -0.010(3) 0.000(3) 0.015(4) C15 0.027(3) 0.049(4) 0.035(4) -0.005(3) 0.006(3) 0.007(3) C16 0.036(3) 0.054(4) 0.038(3) 0.004(3) 0.013(3) -0.001(3) C17 0.038(3) 0.048(4) 0.038(3) 0.007(3) 0.001(3) -0.002(3) C18 0.047(4) 0.052(4) 0.048(4) -0.004(3) 0.003(3) -0.009(3) C19 0.394(21) 0.107(8) 0.129(9) 0.062(7) -0.131(12) -0.170(11) C20 0.157(9) 0.063(5) 0.077(6) 0.014(5) 0.003(6) -0.055(6) C21 0.196(12) 0.178(11) 0.213(12) -0.152(10) 0.141(10) -0.125(10) C22 0.088(7) 0.089(7) 0.289(15) -0.067(8) -0.071(8) 0.001(6) C23 0.163(11) 0.106(9) 0.318(18) 0.087(10) -0.129(12) -0.024(8) C24 0.317(17) 0.101(8) 0.090(7) -0.012(6) 0.082(9) -0.078(10) _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 K N2 2.747(4) 3 ? K N4 2.775(5) . ? K N3 2.831(5) . ? K N1 2.889(4) . ? K N2 2.993(5) . ? Si N1 1.702(4) . ? Si C16 1.869(5) . ? Si C17 1.871(5) . ? Si C18 1.871(5) . ? N1 C1 1.326(6) . ? N2 C3 1.303(6) . ? N2 K 2.747(4) 3 ? N3 C19 1.391(9) . ? N3 C22 1.401(9) . ? N3 C21 1.403(9) . ? N4 C23 1.416(10) . ? N4 C20 1.436(8) . ? N4 C24 1.444(10) . ? C1 C2 1.381(6) . ? C1 C4 1.512(6) . ? C2 C3 1.436(6) . ? C3 C10 1.489(7) . ? C4 C9 1.375(7) . ? C4 C5 1.385(7) . ? C5 C6 1.378(7) . ? C6 C7 1.381(8) . ? C7 C8 1.366(8) . ? C8 C9 1.384(7) . ? C10 C15 1.378(6) . ? C10 C11 1.397(6) . ? C11 C12 1.381(7) . ? C12 C13 1.367(7) . ? C13 C14 1.370(8) . ? C14 C15 1.379(7) . ? C19 C20 1.320(10) . ? 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 K N4 101.1(2) 3 . ? N2 K N3 92.39(14) 3 . ? N4 K N3 64.5(2) . . ? N2 K N1 127.71(13) 3 . ? N4 K N1 125.0(2) . . ? N3 K N1 126.96(14) . . ? N2 K N2 78.93(13) 3 . ? N4 K N2 118.9(2) . . ? N3 K N2 171.09(14) . . ? N1 K N2 59.01(12) . . ? N1 Si C16 116.3(2) . . ? N1 Si C17 104.9(2) . . ? C16 Si C17 106.7(3) . . ? N1 Si C18 111.3(2) . . ? C16 Si C18 108.5(3) . . ? C17 Si C18 108.7(3) . . ? C1 N1 Si 132.7(3) . . ? C1 N1 K 92.4(3) . . ? Si N1 K 118.7(2) . . ? C3 N2 K 132.2(4) . 3 ? C3 N2 K 87.5(3) . . ? K N2 K 101.07(13) 3 . ? C19 N3 C22 108.6(8) . . ? C19 N3 C21 109.9(9) . . ? C22 N3 C21 108.7(8) . . ? C19 N3 K 109.3(4) . . ? C22 N3 K 106.2(4) . . ? C21 N3 K 114.0(4) . . ? C23 N4 C20 111.1(8) . . ? C23 N4 C24 109.5(9) . . ? C20 N4 C24 111.0(7) . . ? C23 N4 K 110.9(5) . . ? C20 N4 K 113.1(4) . . ? C24 N4 K 100.8(5) . . ? N1 C1 C2 124.0(4) . . ? N1 C1 C4 120.2(4) . . ? C2 C1 C4 115.8(4) . . ? C1 C2 C3 125.8(4) . . ? N2 C3 C2 127.2(5) . . ? N2 C3 C10 116.3(4) . . ? C2 C3 C10 116.5(4) . . ? C9 C4 C5 117.5(5) . . ? C9 C4 C1 122.2(5) . . ? C5 C4 C1 120.3(5) . . ? C6 C5 C4 121.6(5) . . ? C5 C6 C7 119.6(6) . . ? C8 C7 C6 119.7(5) . . ? C7 C8 C9 120.0(5) . . ? C4 C9 C8 121.5(5) . . ? C15 C10 C11 118.1(5) . . ? C15 C10 C3 122.1(4) . . ? C11 C10 C3 119.8(4) . . ? C12 C11 C10 119.8(5) . . ? C13 C12 C11 121.1(5) . . ? C12 C13 C14 119.7(5) . . ? C13 C14 C15 119.8(5) . . ? C10 C15 C14 121.5(5) . . ? C20 C19 N3 130.2(8) . . ? C19 C20 N4 122.1(7) . . ? _refine_diff_density_max 0.321 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.055 #===END data_mfl-4 _database_code_CSD 187161 _audit_creation_date 2000-01-31T16:23:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{K(thf)3(C3HPh2N2SiMe2)}2]' _chemical_formula_moiety 'C58 H82 K2 N4 O6 Si2' _chemical_formula_structural 'C58 H82 K2 N4 O6 Si2' _chemical_formula_sum 'C58 H82 K2 N4 O6 Si2' _chemical_formula_weight 1065.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5035(4) _cell_length_b 18.0757(7) _cell_length_c 14.5585(6) _cell_angle_alpha 90 _cell_angle_beta 100.978(2) _cell_angle_gamma 90 _cell_volume 2971.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13337 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.25 _exptl_absorpt_correction_T_min 0.9517 _exptl_absorpt_correction_T_max 0.9876 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 29045 _diffrn_reflns_av_R_equivalents 0.1145 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5226 _reflns_number_gt 3421 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0830P)^2^+6.2106P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5226 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1262 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.177 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.677 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 K K 0.03412(9) 0.07793(5) 0.82153(7) 0.0391(3) Uani 1 1 d . . . Si Si 0.02811(9) 0.11774(6) 1.08072(8) 0.0300(3) Uani 1 1 d . . . O1 O -0.0837(3) 0.20845(19) 0.8209(3) 0.0604(10) Uani 1 1 d . . . O2 O 0.1900(3) -0.0121(2) 0.7556(3) 0.0641(11) Uani 1 1 d . . . O3 O 0.0850(10) 0.1629(6) 0.6721(5) 0.241(6) Uani 1 1 d . . . N1 N 0.1270(3) 0.12478(18) 1.0050(2) 0.0309(8) Uani 1 1 d . . . N2 N 0.0858(3) 0.05649(19) 1.1691(2) 0.0323(8) Uani 1 1 d . . . C1 C 0.2393(3) 0.1109(2) 1.0422(3) 0.0293(9) Uani 1 1 d . . . C2 C 0.2802(3) 0.0802(2) 1.1314(3) 0.0322(9) Uani 1 1 d . . . H2 H 0.363 0.0796 1.1554 0.039 Uiso 1 1 calc R . . C3 C 0.2032(3) 0.0502(2) 1.1868(3) 0.0290(9) Uani 1 1 d . . . C4 C 0.3292(3) 0.1270(2) 0.9813(3) 0.0318(9) Uani 1 1 d . . . C5 C 0.3005(4) 0.1761(3) 0.9065(3) 0.0432(11) Uani 1 1 d . . . H5 H 0.2251 0.1994 0.8953 0.052 Uiso 1 1 calc R . . C6 C 0.3796(4) 0.1915(3) 0.8484(4) 0.0516(13) Uani 1 1 d . . . H6 H 0.3579 0.2248 0.7975 0.062 Uiso 1 1 calc R . . C7 C 0.4896(4) 0.1588(3) 0.8640(4) 0.0487(13) Uani 1 1 d . . . H7 H 0.5439 0.1695 0.8241 0.058 Uiso 1 1 calc R . . C8 C 0.5204(4) 0.1108(3) 0.9376(3) 0.0452(12) Uani 1 1 d . . . H8 H 0.5965 0.0883 0.9489 0.054 Uiso 1 1 calc R . . C9 C 0.4409(3) 0.0947(2) 0.9957(3) 0.0365(10) Uani 1 1 d . . . H9 H 0.4633 0.0611 1.0461 0.044 Uiso 1 1 calc R . . C10 C 0.2571(3) 0.0056(2) 1.2717(3) 0.0313(9) Uani 1 1 d . . . C11 C 0.1999(4) 0.0009(3) 1.3465(3) 0.0435(11) Uani 1 1 d . . . H11 H 0.1253 0.0244 1.3427 0.052 Uiso 1 1 calc R . . C12 C 0.2486(5) -0.0372(3) 1.4270(4) 0.0596(15) Uani 1 1 d . . . H12 H 0.2088 -0.0383 1.4785 0.072 Uiso 1 1 calc R . . C13 C 0.3558(5) -0.0740(3) 1.4326(4) 0.0621(15) Uani 1 1 d . . . H13 H 0.3893 -0.1007 1.4875 0.075 Uiso 1 1 calc R . . C14 C 0.4128(4) -0.0712(3) 1.3578(4) 0.0525(13) Uani 1 1 d . . . H14 H 0.4861 -0.0963 1.3611 0.063 Uiso 1 1 calc R . . C15 C 0.3648(4) -0.0322(2) 1.2781(3) 0.0402(11) Uani 1 1 d . . . H15 H 0.4051 -0.0311 1.2269 0.048 Uiso 1 1 calc R . . C16 C 0.0039(4) 0.2107(3) 1.1316(3) 0.0428(11) Uani 1 1 d . . . H16A H -0.0523 0.2058 1.174 0.064 Uiso 1 1 calc R . . H16B H -0.028 0.2451 1.081 0.064 Uiso 1 1 calc R . . H16C H 0.0794 0.2297 1.1662 0.064 Uiso 1 1 calc R . . C17 C -0.1201(4) 0.0867(3) 1.0179(3) 0.0384(10) Uani 1 1 d . . . H17A H -0.1743 0.0834 1.0622 0.058 Uiso 1 1 calc R . . H17B H -0.113 0.038 0.99 0.058 Uiso 1 1 calc R . . H17C H -0.1511 0.1223 0.9686 0.058 Uiso 1 1 calc R . . C18 C -0.0265(4) 0.2720(3) 0.8684(4) 0.0588(14) Uani 1 1 d . . . H18A H 0.0207 0.298 0.8281 0.071 Uiso 1 1 calc R . . H18B H 0.0273 0.2569 0.9268 0.071 Uiso 1 1 calc R . . C19 C -0.1223(5) 0.3219(3) 0.8902(5) 0.0649(16) Uani 1 1 d . . . H19A H -0.1164 0.3718 0.8635 0.078 Uiso 1 1 calc R . . H19B H -0.117 0.3265 0.9587 0.078 Uiso 1 1 calc R . . C20 C -0.2366(5) 0.2846(3) 0.8453(4) 0.0626(15) Uani 1 1 d . . . H20A H -0.2725 0.2583 0.8926 0.075 Uiso 1 1 calc R . . H20B H -0.2942 0.3211 0.8127 0.075 Uiso 1 1 calc R . . C21 C -0.2002(5) 0.2315(3) 0.7774(4) 0.0662(16) Uani 1 1 d . . . H21A H -0.2549 0.1887 0.7668 0.079 Uiso 1 1 calc R . . H21B H -0.1993 0.2559 0.7167 0.079 Uiso 1 1 calc R . . C22 C 0.1511(4) -0.0740(3) 0.6970(4) 0.0593(15) Uani 1 1 d . . . H22A H 0.1179 -0.0575 0.6325 0.071 Uiso 1 1 calc R . . H22B H 0.0896 -0.1021 0.7214 0.071 Uiso 1 1 calc R . . C23 C 0.2573(5) -0.1201(4) 0.6982(6) 0.087(2) Uani 1 1 d . . . H23A H 0.2587 -0.1621 0.7421 0.104 Uiso 1 1 calc R . . H23B H 0.2587 -0.14 0.635 0.104 Uiso 1 1 calc R . . C24 C 0.3578(5) -0.0713(4) 0.7289(7) 0.119(4) Uani 1 1 d . . . H24A H 0.4242 -0.0986 0.7674 0.143 Uiso 1 1 calc R . . H24B H 0.3854 -0.0494 0.6745 0.143 Uiso 1 1 calc R . . C25 C 0.3152(5) -0.0146(4) 0.7833(6) 0.085(2) Uani 1 1 d . . . H25A H 0.3375 -0.0262 0.8508 0.102 Uiso 1 1 calc R . . H25B H 0.3501 0.0338 0.7719 0.102 Uiso 1 1 calc R . . C26 C 0.0318(13) 0.2159(7) 0.6251(8) 0.160(5) Uani 1 1 d . . . H26A H 0.084 0.259 0.622 0.192 Uiso 1 1 calc R . . H26B H -0.0401 0.2316 0.648 0.192 Uiso 1 1 calc R . . C27 C 0.0045(15) 0.1755(11) 0.5371(11) 0.231(8) Uani 1 1 d . . . H27A H -0.0733 0.1505 0.5302 0.277 Uiso 1 1 calc R . . H27B H 0.0036 0.209 0.4832 0.277 Uiso 1 1 calc R . . C28 C 0.0958(16) 0.1240(8) 0.5438(11) 0.220(8) Uani 1 1 d . . . H28A H 0.124 0.1174 0.4842 0.264 Uiso 1 1 calc R . . H28B H 0.0752 0.0755 0.568 0.264 Uiso 1 1 calc R . . C29 C 0.1752(9) 0.1647(15) 0.6101(11) 0.325(15) Uani 1 1 d . . . H29A H 0.192 0.215 0.5889 0.39 Uiso 1 1 calc R . . H29B H 0.2494 0.138 0.6359 0.39 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 K 0.0429(5) 0.0377(6) 0.0387(6) 0.0014(4) 0.0127(4) 0.0022(4) Si 0.0242(5) 0.0340(7) 0.0324(6) 0.0003(5) 0.0067(4) 0.0028(5) O1 0.054(2) 0.046(2) 0.080(3) 0.0018(19) 0.0080(19) 0.0110(17) O2 0.047(2) 0.064(2) 0.087(3) -0.022(2) 0.0259(19) 0.0036(18) O3 0.323(12) 0.312(12) 0.126(6) 0.138(7) 0.143(7) 0.202(10) N1 0.0273(17) 0.0299(19) 0.036(2) 0.0038(15) 0.0081(15) 0.0043(14) N2 0.0279(17) 0.037(2) 0.0323(19) 0.0009(15) 0.0074(15) 0.0032(15) C1 0.028(2) 0.027(2) 0.034(2) -0.0034(18) 0.0076(17) 0.0003(17) C2 0.0221(19) 0.036(2) 0.037(2) -0.0011(19) 0.0027(17) -0.0051(18) C3 0.027(2) 0.030(2) 0.029(2) -0.0057(18) 0.0038(17) 0.0015(17) C4 0.028(2) 0.030(2) 0.038(2) -0.0029(19) 0.0083(18) -0.0015(18) C5 0.039(2) 0.041(3) 0.053(3) 0.013(2) 0.018(2) 0.010(2) C6 0.050(3) 0.044(3) 0.069(4) 0.016(3) 0.032(3) 0.007(2) C7 0.047(3) 0.043(3) 0.063(3) 0.003(3) 0.031(3) -0.004(2) C8 0.027(2) 0.052(3) 0.059(3) -0.008(3) 0.014(2) -0.001(2) C9 0.030(2) 0.042(3) 0.037(2) 0.003(2) 0.0061(19) 0.0033(19) C10 0.031(2) 0.030(2) 0.032(2) -0.0018(18) 0.0044(17) -0.0031(18) C11 0.040(2) 0.052(3) 0.040(3) 0.008(2) 0.011(2) 0.006(2) C12 0.062(3) 0.083(4) 0.036(3) 0.020(3) 0.016(2) 0.014(3) C13 0.061(3) 0.075(4) 0.047(3) 0.024(3) 0.003(3) 0.016(3) C14 0.046(3) 0.054(3) 0.057(3) 0.013(3) 0.008(2) 0.011(2) C15 0.041(2) 0.040(3) 0.040(3) 0.002(2) 0.008(2) 0.008(2) C16 0.041(2) 0.041(3) 0.046(3) -0.002(2) 0.008(2) 0.004(2) C17 0.030(2) 0.047(3) 0.039(3) -0.001(2) 0.0078(19) -0.001(2) C18 0.047(3) 0.047(3) 0.081(4) 0.011(3) 0.010(3) -0.007(2) C19 0.057(3) 0.052(3) 0.079(4) -0.002(3) -0.004(3) 0.009(3) C20 0.047(3) 0.059(4) 0.082(4) 0.001(3) 0.012(3) 0.000(3) C21 0.055(3) 0.058(4) 0.080(4) -0.003(3) -0.002(3) 0.007(3) C22 0.043(3) 0.082(4) 0.054(3) -0.018(3) 0.012(2) -0.007(3) C23 0.048(3) 0.065(4) 0.143(7) -0.038(4) 0.005(4) 0.000(3) C24 0.041(3) 0.102(6) 0.206(10) -0.087(6) 0.003(4) -0.001(3) C25 0.047(3) 0.090(5) 0.120(6) -0.043(4) 0.019(3) -0.011(3) C26 0.250(14) 0.147(9) 0.097(7) 0.022(7) 0.068(9) 0.097(10) C27 0.221(16) 0.26(2) 0.169(15) -0.048(14) -0.068(12) 0.012(15) C28 0.278(18) 0.160(12) 0.191(14) -0.105(10) -0.035(13) 0.112(12) C29 0.078(7) 0.70(4) 0.217(15) -0.22(2) 0.075(9) -0.098(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K O1 2.720(3) . ? K O2 2.727(3) . ? K N2 2.810(4) 3_557 ? K N1 2.811(4) . ? K O3 2.814(7) . ? Si N2 1.732(4) . ? Si N1 1.733(3) . ? Si C17 1.861(4) . ? Si C16 1.878(5) . ? O1 C21 1.431(6) . ? O1 C18 1.435(6) . ? O2 C25 1.420(6) . ? O2 C22 1.427(6) . ? O3 C26 1.265(11) . ? O3 C29 1.499(12) . ? N1 C1 1.326(5) . ? N2 C3 1.330(5) . ? N2 K 2.810(4) 3_557 ? C1 C2 1.408(6) . ? C1 C4 1.514(5) . ? C2 C3 1.415(6) . ? C3 C10 1.506(6) . ? C4 C9 1.391(6) . ? C4 C5 1.394(6) . ? C5 C6 1.384(6) . ? C6 C7 1.375(6) . ? C7 C8 1.372(7) . ? C8 C9 1.389(6) . ? C10 C11 1.379(6) . ? C10 C15 1.402(6) . ? C11 C12 1.382(7) . ? C12 C13 1.389(7) . ? C13 C14 1.375(7) . ? C14 C15 1.380(7) . ? C18 C19 1.505(7) . ? C19 C20 1.511(7) . ? C20 C21 1.494(8) . ? C22 C23 1.476(7) . ? C23 C24 1.456(8) . ? C24 C25 1.436(9) . ? C26 C27 1.456(16) . ? C26 C29 1.940(19) . ? C27 C28 1.393(17) . ? C28 C29 1.404(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K O2 151.25(12) . . ? O1 K N2 120.08(11) . 3_557 ? O2 K N2 82.14(11) . 3_557 ? O1 K N1 80.84(11) . . ? O2 K N1 110.96(11) . . ? N2 K N1 108.41(10) 3_557 . ? O1 K O3 72.60(19) . . ? O2 K O3 78.81(19) . . ? N2 K O3 133.3(3) 3_557 . ? N1 K O3 118.2(3) . . ? N2 Si N1 108.34(16) . . ? N2 Si C17 111.00(19) . . ? N1 Si C17 111.13(19) . . ? N2 Si C16 110.1(2) . . ? N1 Si C16 110.46(19) . . ? C17 Si C16 105.8(2) . . ? C21 O1 C18 106.6(4) . . ? C21 O1 K 132.7(3) . . ? C18 O1 K 120.7(3) . . ? C25 O2 C22 109.2(4) . . ? C25 O2 K 128.2(3) . . ? C22 O2 K 121.8(3) . . ? C26 O3 C29 88.7(12) . . ? C26 O3 K 132.9(7) . . ? C29 O3 K 138.3(11) . . ? C1 N1 Si 115.6(3) . . ? C1 N1 K 119.7(2) . . ? Si N1 K 113.93(15) . . ? C3 N2 Si 115.5(3) . . ? C3 N2 K 114.0(3) . 3_557 ? Si N2 K 117.79(16) . 3_557 ? N1 C1 C2 125.5(4) . . ? N1 C1 C4 116.4(4) . . ? C2 C1 C4 118.1(3) . . ? C1 C2 C3 122.8(4) . . ? N2 C3 C2 125.4(4) . . ? N2 C3 C10 116.7(3) . . ? C2 C3 C10 117.9(3) . . ? C9 C4 C5 117.3(4) . . ? C9 C4 C1 123.1(4) . . ? C5 C4 C1 119.6(4) . . ? C6 C5 C4 121.4(4) . . ? C7 C6 C5 120.2(5) . . ? C8 C7 C6 119.6(4) . . ? C7 C8 C9 120.4(4) . . ? C8 C9 C4 121.1(4) . . ? C11 C10 C15 117.8(4) . . ? C11 C10 C3 119.8(4) . . ? C15 C10 C3 122.5(4) . . ? C10 C11 C12 121.5(4) . . ? C11 C12 C13 120.1(5) . . ? C14 C13 C12 119.2(5) . . ? C13 C14 C15 120.6(5) . . ? C14 C15 C10 120.8(4) . . ? O1 C18 C19 107.1(4) . . ? C18 C19 C20 104.7(5) . . ? C21 C20 C19 104.1(4) . . ? O1 C21 C20 104.5(5) . . ? O2 C22 C23 105.8(4) . . ? C24 C23 C22 105.5(5) . . ? C25 C24 C23 105.5(5) . . ? O2 C25 C24 107.5(5) . . ? O3 C26 C27 95.6(11) . . ? O3 C26 C29 50.6(8) . . ? C27 C26 C29 73.0(9) . . ? C28 C27 C26 103.9(11) . . ? C27 C28 C29 94.7(12) . . ? C28 C29 O3 88.2(11) . . ? C28 C29 C26 82.6(9) . . ? O3 C29 C26 40.7(5) . . ? #===END