#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bott,S.' 'Daniele, S.' 'Drost, C.' 'Gehrhus, B.' 'Hawkins, S.M.' 'Hitchcock, P.B.' 'Lappert, M.' 'Merle, P.G.' _publ_contact_author_name 'Prof M. Lappert' _publ_contact_author_address ; Prof M Lappert School of Chemistry & Molecular Science University of Sussex BRIGHTON BN1 9QJ U.K. ; _publ_contact_author_email 'M.F.LAPPERT@SUSSEX.AC.UK' data_mfl-1-jun800 _database_code_CSD 168078 _audit_creation_date 2000-06-06T14:30:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Li2(C6H4(NSiMe3)2)}2]' _chemical_formula_moiety 'C24 H44 Li4 N4 Si4' _chemical_formula_structural 'C24 H44 LI4 N4 SI4' _chemical_formula_sum 'C24 H44 Li4 N4 Si4' _chemical_formula_weight 528.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm _symmetry_space_group_name_Hall '-C 2c 2c' _symmetry_Int_Tables_number 63 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y, z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.7489(7) _cell_length_b 13.7919(4) _cell_length_c 14.8525(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3226.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5281 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_T_min 0.9512 _exptl_absorpt_correction_T_max 0.9703 #----------------------------------------------------------------------------# # 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 10357 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.82 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2054 _reflns_number_gt 1655 _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^)+(0.0494P)^2^+2.4913P] 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_number_reflns 2054 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.354 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' 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' 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 Li1 Li 0.0848(3) 0.2162(3) 0.75 0.0324(8) Uani 1 2 d S . . Li2 Li 0 0.1096(2) 0.8407(3) 0.0305(8) Uani 1 2 d S . . Si1 Si 0 0.25865(4) 0.53970(4) 0.03160(19) Uani 1 2 d S . . Si2 Si 0.19809(4) 0.06707(5) 0.75 0.0444(2) Uani 1 2 d S . . N1 N 0.08874(11) 0.06492(11) 0.75 0.0254(4) Uani 1 2 d S . . N2 N 0 0.26050(11) 0.65581(11) 0.0280(4) Uani 1 2 d S . . C1 C 0.04574(12) -0.02581(13) 0.75 0.0206(4) Uani 1 2 d S . . C2 C 0.08703(13) -0.11579(14) 0.75 0.0260(4) Uani 1 2 d S . . H2 H 0.1473 -0.1168 0.75 0.031 Uiso 1 2 calc SR . . C3 C 0.04388(14) -0.20338(15) 0.75 0.0297(5) Uani 1 2 d S . . H3 H 0.0743 -0.2628 0.75 0.036 Uiso 1 2 calc SR . . C4 C 0.24762(14) 0.01403(18) 0.64710(19) 0.0769(8) Uani 1 1 d . . . H4A H 0.2214 0.0425 0.5934 0.115 Uiso 1 1 calc R . . H4B H 0.2388 -0.0563 0.6468 0.115 Uiso 1 1 calc R . . H4C H 0.3086 0.028 0.6471 0.115 Uiso 1 1 calc R . . C5 C 0.22780(19) 0.2006(2) 0.75 0.0805(12) Uani 1 2 d S . . H5A H 0.2036 0.232 0.6967 0.121 Uiso 0.5 1 calc PR . . H5B H 0.2898 0.207 0.7488 0.121 Uiso 1 2 calc SR . . H5C H 0.2054 0.2315 0.8044 0.121 Uiso 0.5 1 calc PR . . C6 C 0 0.35132(14) 0.70162(14) 0.0254(4) Uani 1 2 d S . . C7 C 0 0.44127(15) 0.65756(15) 0.0324(5) Uani 1 2 d S . . H7 H 0 0.4422 0.5936 0.039 Uiso 1 2 calc SR . . C8 C 0 0.52907(15) 0.70354(16) 0.0351(5) Uani 1 2 d S . . H8 H 0 0.5886 0.6713 0.042 Uiso 1 2 calc SR . . C9 C -0.09835(13) 0.31100(14) 0.48827(12) 0.0488(5) Uani 1 1 d . . . H10A H -0.1485 0.2821 0.5167 0.073 Uiso 1 1 calc R . . H10B H -0.0991 0.297 0.4236 0.073 Uiso 1 1 calc R . . H10C H -0.099 0.3813 0.4976 0.073 Uiso 1 1 calc R . . C10 C 0 0.12682(18) 0.50646(17) 0.0489(7) Uani 1 2 d S . . H9A H -0.0503 0.0949 0.5315 0.073 Uiso 0.5 1 calc PR . . H9B H 0.0513 0.0954 0.5299 0.073 Uiso 0.5 1 calc PR . . H9C H -0.0009 0.1215 0.4407 0.073 Uiso 1 2 calc SR . . 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 Li1 0.036(2) 0.0270(18) 0.034(2) 0 0 -0.0003(16) Li2 0.036(2) 0.0235(17) 0.0318(19) -0.0011(14) 0 0 Si1 0.0487(4) 0.0242(3) 0.0219(3) 0.0003(2) 0 0 Si2 0.0202(3) 0.0314(4) 0.0815(6) 0 0 -0.0038(3) N1 0.0214(8) 0.0186(8) 0.0362(10) 0 0 -0.0029(7) N2 0.0444(11) 0.0186(8) 0.0209(8) -0.0004(6) 0 0 C1 0.0226(10) 0.0183(9) 0.0210(9) 0 0 -0.0009(7) C2 0.0222(10) 0.0238(10) 0.0320(11) 0 0 0.0022(8) C3 0.0342(12) 0.0187(9) 0.0362(12) 0 0 0.0049(9) C4 0.0506(13) 0.0650(15) 0.115(2) 0.0041(13) 0.0447(14) 0.0025(12) C5 0.0312(15) 0.0418(16) 0.169(4) 0 0 -0.0172(13) C6 0.0302(11) 0.0188(9) 0.0271(10) -0.0012(8) 0 0 C7 0.0476(14) 0.0229(10) 0.0269(11) 0.0034(8) 0 0 C8 0.0477(14) 0.0187(10) 0.0389(12) 0.0044(9) 0 0 C9 0.0591(12) 0.0517(11) 0.0356(10) 0.0043(8) -0.0092(9) 0.0034(9) C10 0.085(2) 0.0321(13) 0.0292(12) -0.0063(10) 0 0 #----------------------------------------------------------------------------# # 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 Li1 N2 2.028(3) . ? Li1 N2 2.028(3) 10_557 ? Li1 N1 2.087(4) . ? Li2 N1 2.036(3) 11 ? Li2 N1 2.036(3) . ? Li2 N2 2.082(4) 10_557 ? Si1 N2 1.7247(18) . ? Si1 C9 1.8719(19) . ? Si1 C9 1.8719(19) 11 ? Si1 C10 1.884(2) . ? Si2 N1 1.7223(19) . ? Si2 C4 1.865(2) 10_557 ? Si2 C4 1.865(2) . ? Si2 C5 1.900(3) . ? N1 C1 1.423(2) . ? N1 Li2 2.036(3) 10_557 ? N2 C6 1.426(2) . ? N2 Li1 2.028(3) 11 ? N2 Li2 2.082(4) 10_557 ? C1 C2 1.401(3) . ? C1 C1 1.441(4) 11 ? C2 C3 1.386(3) . ? C3 C3 1.382(4) 11 ? C6 C7 1.403(3) . ? C6 C6 1.437(4) 10_557 ? C7 C8 1.390(3) . ? C8 C8 1.380(5) 10_557 ? 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 Li1 N2 87.22(17) . 10_557 ? N2 Li1 N1 108.72(15) . . ? N2 Li1 N1 108.72(15) 10_557 . ? N1 Li2 N1 86.68(16) 11 . ? N1 Li2 N2 108.59(14) 11 10_557 ? N1 Li2 N2 108.59(14) . 10_557 ? N2 Si1 C9 113.72(7) . . ? N2 Si1 C9 113.72(7) . 11 ? C9 Si1 C9 111.68(13) . 11 ? N2 Si1 C10 106.03(10) . . ? C9 Si1 C10 105.38(8) . . ? C9 Si1 C10 105.38(8) 11 . ? N1 Si2 C4 114.29(8) . 10_557 ? N1 Si2 C4 114.29(8) . . ? C4 Si2 C4 110.04(17) 10_557 . ? N1 Si2 C5 105.25(11) . . ? C4 Si2 C5 106.08(9) 10_557 . ? C4 Si2 C5 106.08(9) . . ? C1 N1 Si2 119.41(13) . . ? C1 N1 Li2 86.51(12) . . ? Si2 N1 Li2 132.92(9) . . ? C1 N1 Li2 86.51(12) . 10_557 ? Si2 N1 Li2 132.92(9) . 10_557 ? Li2 N1 Li2 82.83(18) . 10_557 ? C1 N1 Li1 149.86(17) . . ? Si2 N1 Li1 90.73(13) . . ? Li2 N1 Li1 71.17(13) . . ? Li2 N1 Li1 71.17(13) 10_557 . ? C6 N2 Si1 119.35(13) . . ? C6 N2 Li1 86.31(13) . 11 ? Si1 N2 Li1 133.25(9) . 11 ? C6 N2 Li1 86.31(13) . . ? Si1 N2 Li1 133.25(9) . . ? Li1 N2 Li1 82.35(19) 11 . ? C6 N2 Li2 150.06(17) . 10_557 ? Si1 N2 Li2 90.58(13) . 10_557 ? Li1 N2 Li2 71.43(13) 11 10_557 ? Li1 N2 Li2 71.43(13) . 10_557 ? C2 C1 N1 123.92(18) . . ? C2 C1 C1 117.66(12) . 11 ? N1 C1 C1 118.43(10) . 11 ? C3 C2 C1 122.98(19) . . ? C3 C3 C2 119.36(12) 11 . ? C7 C6 N2 123.68(19) . . ? C7 C6 C6 117.81(12) . 10_557 ? N2 C6 C6 118.51(11) . 10_557 ? C8 C7 C6 122.8(2) . . ? C8 C8 C7 119.42(13) 10_557 . ? #===END data_mfl-2-feb600 _database_code_CSD 168079 _audit_creation_date 2000-02-07T14:15:26-00:00 _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 '[{Li2(thf)2(C6H4(NSiMe3)2)}2]' _chemical_formula_moiety 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_structural 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_sum 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_weight 817.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7906(7) _cell_length_b 17.7715(9) _cell_length_c 25.8104(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4949.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 48384 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9921 #----------------------------------------------------------------------------# # 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 23361 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2994 _reflns_number_gt 2190 _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 ; The crystal diffracted poorly . The O1 thf group is disordered and modelled as two alternative sets of ring C atoms with bond length constraints applied(SADI). 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^)+(0.1004P)^2^+13.5296P] 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_number_reflns 2994 _refine_ls_number_parameters 249 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.114 _refine_ls_R_factor_gt 0.087 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2168 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.593 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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 Li1 Li 0.4308(10) 0.5756(5) 0.3545(4) 0.067(3) Uani 1 1 d . A . Li2 Li 0.5112(8) 0.5285(4) 0.4443(3) 0.049(2) Uani 1 1 d . . . Si1 Si 0.50626(17) 0.72205(8) 0.41658(7) 0.0614(6) Uani 1 1 d . A . Si2 Si 0.5055(2) 0.40179(8) 0.34077(6) 0.0695(7) Uani 1 1 d . A . O1 O 0.3051(5) 0.6047(3) 0.30724(19) 0.0871(15) Uani 1 1 d D . . O2 O 0.6295(3) 0.50332(17) 0.50589(14) 0.0479(10) Uani 1 1 d . . . N1 N 0.5338(4) 0.6292(2) 0.40514(19) 0.0549(13) Uani 1 1 d . . . N2 N 0.5325(5) 0.4863(2) 0.36979(18) 0.0557(13) Uani 1 1 d . . . C1 C 0.6489(5) 0.5983(3) 0.3924(2) 0.0505(14) Uani 1 1 d . A . C2 C 0.6492(6) 0.5211(3) 0.3733(2) 0.0523(15) Uani 1 1 d . A . C3 C 0.7645(7) 0.4881(3) 0.3618(2) 0.0726(19) Uani 1 1 d . . . H3 H 0.7659 0.4375 0.35 0.087 Uiso 1 1 calc R A . C4 C 0.8753(7) 0.5257(4) 0.3669(3) 0.086(2) Uani 1 1 d . A . H4 H 0.9512 0.5017 0.3584 0.104 Uiso 1 1 calc R . . C5 C 0.8742(6) 0.5984(4) 0.3844(3) 0.078(2) Uani 1 1 d . . . H5 H 0.9502 0.6248 0.3882 0.093 Uiso 1 1 calc R A . C6 C 0.7635(6) 0.6340(3) 0.3969(2) 0.0636(17) Uani 1 1 d . A . H6 H 0.7659 0.6846 0.4088 0.076 Uiso 1 1 calc R . . C7 C 0.3363(8) 0.7349(4) 0.4241(5) 0.165(6) Uani 1 1 d . . . H7A H 0.2938 0.7152 0.3934 0.247 Uiso 1 1 calc R A . H7B H 0.3176 0.7886 0.4279 0.247 Uiso 1 1 calc R . . H7C H 0.3078 0.7078 0.4549 0.247 Uiso 1 1 calc R . . C8 C 0.5569(7) 0.7851(3) 0.3631(3) 0.079(2) Uani 1 1 d . . . H8A H 0.5214 0.7675 0.3303 0.119 Uiso 1 1 calc R A . H8B H 0.6475 0.7846 0.3607 0.119 Uiso 1 1 calc R . . H8C H 0.5284 0.8365 0.37 0.119 Uiso 1 1 calc R . . C9 C 0.5785(12) 0.7607(4) 0.4760(3) 0.148(5) Uani 1 1 d . . . H9A H 0.555 0.7298 0.5058 0.222 Uiso 1 1 calc R A . H9B H 0.5498 0.8125 0.4814 0.222 Uiso 1 1 calc R . . H9C H 0.6688 0.7605 0.4722 0.222 Uiso 1 1 calc R . . C10 C 0.3345(8) 0.3926(4) 0.3321(3) 0.106(3) Uani 1 1 d . . . H10A H 0.3035 0.4353 0.3119 0.158 Uiso 1 1 calc R A . H10B H 0.2941 0.3918 0.3661 0.158 Uiso 1 1 calc R . . H10C H 0.3162 0.3457 0.3136 0.158 Uiso 1 1 calc R . . C11 C 0.5749(13) 0.3932(5) 0.2740(3) 0.164(5) Uani 1 1 d . . . H11A H 0.6653 0.3973 0.2764 0.246 Uiso 1 1 calc R A . H11B H 0.5428 0.4336 0.2519 0.246 Uiso 1 1 calc R . . H11C H 0.5527 0.3444 0.2591 0.246 Uiso 1 1 calc R . . C12 C 0.5572(8) 0.3187(3) 0.3798(3) 0.088(2) Uani 1 1 d . . . H12A H 0.6471 0.3212 0.385 0.132 Uiso 1 1 calc R A . H12B H 0.5363 0.2722 0.3613 0.132 Uiso 1 1 calc R . . H12C H 0.5153 0.3191 0.4135 0.132 Uiso 1 1 calc R . . C17 C 0.7160(5) 0.4413(3) 0.4973(3) 0.0599(16) Uani 1 1 d . . . H17A H 0.6802 0.393 0.5091 0.072 Uiso 1 1 calc R . . H17B H 0.7379 0.4371 0.4601 0.072 Uiso 1 1 calc R . . C18 C 0.8243(7) 0.4616(4) 0.5282(5) 0.136(4) Uani 1 1 d . . . H18A H 0.8213 0.4352 0.562 0.163 Uiso 1 1 calc R . . H18B H 0.9008 0.446 0.51 0.163 Uiso 1 1 calc R . . C19 C 0.8261(6) 0.5402(4) 0.5365(4) 0.095(2) Uani 1 1 d . . . H19A H 0.8881 0.5643 0.5136 0.114 Uiso 1 1 calc R . . H19B H 0.8479 0.5514 0.5729 0.114 Uiso 1 1 calc R . . C20 C 0.7003(5) 0.5685(3) 0.5245(2) 0.0542(15) Uani 1 1 d . . . H20A H 0.6612 0.5899 0.5559 0.065 Uiso 1 1 calc R . . H20B H 0.7041 0.608 0.4975 0.065 Uiso 1 1 calc R . . C13 C 0.1788(14) 0.5715(10) 0.3026(7) 0.119(6) Uiso 0.5 1 d PD A 1 H13C H 0.1859 0.5171 0.2951 0.143 Uiso 0.5 1 calc PR A 1 H13D H 0.1345 0.5772 0.336 0.143 Uiso 0.5 1 calc PR A 1 C14 C 0.1069(15) 0.6083(7) 0.2612(6) 0.088(4) Uiso 0.5 1 d PD A 1 H14C H 0.0169 0.6079 0.2684 0.105 Uiso 0.5 1 calc PR A 1 H14D H 0.123 0.5855 0.2269 0.105 Uiso 0.5 1 calc PR A 1 C15 C 0.1605(12) 0.6849(7) 0.2656(6) 0.073(4) Uiso 0.5 1 d PD A 1 H15C H 0.1402 0.7096 0.2989 0.088 Uiso 0.5 1 calc PR A 1 H15D H 0.137 0.7179 0.2363 0.088 Uiso 0.5 1 calc PR A 1 C16 C 0.2980(17) 0.6584(13) 0.2626(8) 0.148(8) Uiso 0.5 1 d PD A 1 H16C H 0.3158 0.6328 0.2294 0.178 Uiso 0.5 1 calc PR A 1 H16D H 0.356 0.701 0.2671 0.178 Uiso 0.5 1 calc PR A 1 C13B C 0.245(2) 0.5711(12) 0.2635(8) 0.159(9) Uiso 0.5 1 d PD A 2 H13A H 0.1855 0.532 0.2743 0.19 Uiso 0.5 1 calc PR A 2 H13B H 0.3064 0.5488 0.2393 0.19 Uiso 0.5 1 calc PR A 2 C14B C 0.181(2) 0.6380(12) 0.2395(9) 0.142(7) Uiso 0.5 1 d PD A 2 H14A H 0.1907 0.6377 0.2014 0.171 Uiso 0.5 1 calc PR A 2 H14B H 0.0909 0.6371 0.2477 0.171 Uiso 0.5 1 calc PR A 2 C15B C 0.239(4) 0.7046(17) 0.2620(11) 0.231(15) Uiso 0.5 1 d PD A 2 H15A H 0.1897 0.7509 0.257 0.277 Uiso 0.5 1 calc PR A 2 H15B H 0.325 0.7123 0.2496 0.277 Uiso 0.5 1 calc PR A 2 C16B C 0.233(3) 0.6753(12) 0.3164(11) 0.196(11) Uiso 0.5 1 d PD A 2 H16A H 0.2749 0.7092 0.3414 0.235 Uiso 0.5 1 calc PR A 2 H16B H 0.1474 0.6651 0.3278 0.235 Uiso 0.5 1 calc PR A 2 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 Li1 0.074(7) 0.040(5) 0.088(7) 0.003(5) -0.014(6) 0.002(5) Li2 0.053(6) 0.034(4) 0.060(5) -0.003(4) 0.001(4) -0.002(4) Si1 0.0819(13) 0.0282(9) 0.0741(12) -0.0009(7) 0.0132(10) -0.0011(7) Si2 0.1247(17) 0.0345(9) 0.0492(10) -0.0046(7) -0.0009(10) -0.0121(9) O1 0.097(4) 0.072(3) 0.093(3) 0.011(2) -0.026(3) 0.001(3) O2 0.0350(19) 0.0362(19) 0.072(2) -0.0027(16) -0.0028(17) -0.0016(16) N1 0.054(3) 0.028(2) 0.082(3) -0.007(2) 0.012(2) -0.004(2) N2 0.074(4) 0.032(2) 0.060(3) -0.006(2) -0.003(2) -0.001(2) C1 0.057(4) 0.039(3) 0.055(3) 0.000(2) 0.010(3) -0.005(3) C2 0.071(4) 0.037(3) 0.048(3) -0.001(2) 0.006(3) 0.003(3) C3 0.094(5) 0.049(4) 0.075(4) 0.001(3) 0.029(4) 0.014(4) C4 0.074(5) 0.072(5) 0.114(6) 0.022(4) 0.042(4) 0.011(4) C5 0.054(4) 0.080(5) 0.099(5) 0.020(4) 0.022(4) -0.016(4) C6 0.061(4) 0.052(3) 0.078(4) 0.006(3) 0.016(3) -0.012(3) C7 0.102(7) 0.047(4) 0.344(17) 0.036(7) 0.095(9) 0.024(4) C8 0.084(5) 0.062(4) 0.091(5) 0.024(4) -0.008(4) -0.007(4) C9 0.315(15) 0.056(4) 0.074(5) -0.023(4) -0.043(7) 0.047(7) C10 0.154(8) 0.056(4) 0.106(6) 0.006(4) -0.070(6) -0.024(4) C11 0.310(16) 0.118(7) 0.063(5) -0.037(5) 0.057(7) -0.095(9) C12 0.113(6) 0.040(3) 0.111(6) 0.009(3) 0.014(5) 0.008(4) C17 0.050(4) 0.045(3) 0.085(4) 0.003(3) 0.007(3) 0.009(3) C18 0.061(5) 0.083(6) 0.264(13) -0.025(7) -0.069(7) 0.020(4) C19 0.050(5) 0.086(5) 0.149(7) -0.018(5) -0.020(4) 0.000(4) C20 0.044(3) 0.046(3) 0.073(4) -0.001(3) -0.010(3) -0.012(3) #----------------------------------------------------------------------------# # 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 Li1 O1 1.897(11) . ? Li1 N1 1.962(11) . ? Li1 N2 1.968(10) . ? Li1 C1 2.580(12) . ? Li1 C2 2.593(12) . ? Li1 Li2 2.613(14) . ? Li1 Si1 3.163(10) . ? Li2 O2 2.067(9) 5_666 ? Li2 N1 2.070(9) . ? Li2 N2 2.077(10) . ? Li2 O2 2.086(10) . ? Li2 C1 2.354(10) . ? Li2 C2 2.365(11) . ? Li2 Li2 3.056(18) 5_666 ? Si1 N1 1.702(4) . ? Si1 C9 1.853(8) . ? Si1 C7 1.859(8) . ? Si1 C8 1.861(6) . ? Si2 N2 1.704(4) . ? Si2 C10 1.865(9) . ? Si2 C12 1.873(6) . ? Si2 C11 1.884(8) . ? O1 C13B 1.431(15) . ? O1 C13 1.490(14) . ? O1 C16B 1.492(16) . ? O1 C16 1.496(15) . ? O2 C17 1.462(6) . ? O2 C20 1.468(6) . ? O2 Li2 2.067(10) 5_666 ? N1 C1 1.397(7) . ? N2 C2 1.405(7) . ? C1 C6 1.395(8) . ? C1 C2 1.458(7) . ? C2 C3 1.407(9) . ? C3 C4 1.377(10) . ? C4 C5 1.368(10) . ? C5 C6 1.390(9) . ? C17 C18 1.461(9) . ? C18 C19 1.412(10) . ? C19 C20 1.480(8) . ? C13 C14 1.474(15) . ? C14 C15 1.483(14) . ? C15 C16 1.558(15) . ? C13B C14B 1.513(16) . ? C14B C15B 1.461(17) . ? C15B C16B 1.499(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 Li1 N1 134.5(5) . . ? O1 Li1 N2 138.4(6) . . ? N1 Li1 N2 86.7(5) . . ? O1 Li1 C1 148.6(5) . . ? N1 Li1 C1 32.3(2) . . ? N2 Li1 C1 62.7(3) . . ? O1 Li1 C2 150.7(6) . . ? N1 Li1 C2 62.8(3) . . ? N2 Li1 C2 32.4(2) . . ? C1 Li1 C2 32.7(2) . . ? O1 Li1 Li2 153.6(6) . . ? N1 Li1 Li2 51.5(3) . . ? N2 Li1 Li2 51.6(3) . . ? C1 Li1 Li2 53.9(3) . . ? C2 Li1 Li2 54.0(3) . . ? O1 Li1 Si1 106.5(4) . . ? N1 Li1 Si1 28.03(19) . . ? N2 Li1 Si1 114.7(4) . . ? C1 Li1 Si1 56.3(2) . . ? C2 Li1 Si1 88.8(3) . . ? Li2 Li1 Si1 74.3(3) . . ? O2 Li2 N1 128.8(5) 5_666 . ? O2 Li2 N2 123.9(4) 5_666 . ? N1 Li2 N2 81.1(4) . . ? O2 Li2 O2 85.2(4) 5_666 . ? N1 Li2 O2 119.1(4) . . ? N2 Li2 O2 124.1(4) . . ? O2 Li2 C1 164.0(4) 5_666 . ? N1 Li2 C1 36.1(2) . . ? N2 Li2 C1 66.0(3) . . ? O2 Li2 C1 99.2(4) . . ? O2 Li2 C2 158.2(4) 5_666 . ? N1 Li2 C2 66.1(3) . . ? N2 Li2 C2 36.2(2) . . ? O2 Li2 C2 101.2(4) . . ? C1 Li2 C2 36.0(2) . . ? O2 Li2 Li1 113.3(5) 5_666 . ? N1 Li2 Li1 47.8(3) . . ? N2 Li2 Li1 48.0(3) . . ? O2 Li2 Li1 161.3(5) . . ? C1 Li2 Li1 62.3(3) . . ? C2 Li2 Li1 62.6(4) . . ? O2 Li2 Li2 42.9(2) 5_666 5_666 ? N1 Li2 Li2 139.0(5) . 5_666 ? N2 Li2 Li2 139.5(5) . 5_666 ? O2 Li2 Li2 42.4(2) . 5_666 ? C1 Li2 Li2 139.4(5) . 5_666 ? C2 Li2 Li2 139.5(5) . 5_666 ? Li1 Li2 Li2 156.0(6) . 5_666 ? N1 Si1 C9 115.5(3) . . ? N1 Si1 C7 108.0(3) . . ? C9 Si1 C7 106.4(6) . . ? N1 Si1 C8 113.8(3) . . ? C9 Si1 C8 105.5(4) . . ? C7 Si1 C8 107.0(4) . . ? N1 Si1 Li1 32.8(2) . . ? C9 Si1 Li1 146.4(3) . . ? C7 Si1 Li1 84.3(4) . . ? C8 Si1 Li1 101.3(3) . . ? N2 Si2 C10 107.4(3) . . ? N2 Si2 C12 114.1(3) . . ? C10 Si2 C12 106.9(3) . . ? N2 Si2 C11 113.9(3) . . ? C10 Si2 C11 106.0(5) . . ? C12 Si2 C11 108.0(4) . . ? C13B O1 C13 50.2(11) . . ? C13B O1 C16B 104.1(15) . . ? C13 O1 C16B 82.6(14) . . ? C13B O1 C16 68.7(13) . . ? C13 O1 C16 98.3(11) . . ? C16B O1 C16 63.9(14) . . ? C13B O1 Li1 135.7(9) . . ? C13 O1 Li1 126.7(8) . . ? C16B O1 Li1 119.9(12) . . ? C16 O1 Li1 134.9(9) . . ? C17 O2 C20 108.1(4) . . ? C17 O2 Li2 111.0(4) . 5_666 ? C20 O2 Li2 113.2(4) . 5_666 ? C17 O2 Li2 115.9(4) . . ? C20 O2 Li2 113.5(4) . . ? Li2 O2 Li2 94.8(4) 5_666 . ? C1 N1 Si1 125.2(3) . . ? C1 N1 Li1 99.0(4) . . ? Si1 N1 Li1 119.2(4) . . ? C1 N1 Li2 83.1(4) . . ? Si1 N1 Li2 137.1(4) . . ? Li1 N1 Li2 80.7(4) . . ? C2 N2 Si2 124.7(4) . . ? C2 N2 Li1 99.1(4) . . ? Si2 N2 Li1 121.8(4) . . ? C2 N2 Li2 83.1(4) . . ? Si2 N2 Li2 134.9(3) . . ? Li1 N2 Li2 80.4(4) . . ? C6 C1 N1 126.1(5) . . ? C6 C1 C2 117.0(5) . . ? N1 C1 C2 116.8(5) . . ? C6 C1 Li2 138.8(5) . . ? N1 C1 Li2 60.8(3) . . ? C2 C1 Li2 72.4(4) . . ? C6 C1 Li1 155.6(5) . . ? N1 C1 Li1 48.7(3) . . ? C2 C1 Li1 74.1(4) . . ? Li2 C1 Li1 63.8(3) . . ? N2 C2 C3 126.5(5) . . ? N2 C2 C1 115.7(5) . . ? C3 C2 C1 117.7(6) . . ? N2 C2 Li2 60.7(3) . . ? C3 C2 Li2 138.0(5) . . ? C1 C2 Li2 71.6(4) . . ? N2 C2 Li1 48.5(3) . . ? C3 C2 Li1 156.9(5) . . ? C1 C2 Li1 73.2(4) . . ? Li2 C2 Li1 63.4(4) . . ? C4 C3 C2 123.1(6) . . ? C5 C4 C3 118.8(6) . . ? C4 C5 C6 120.9(6) . . ? C5 C6 C1 122.4(6) . . ? C18 C17 O2 104.0(5) . . ? C19 C18 C17 109.7(6) . . ? C18 C19 C20 107.0(6) . . ? O2 C20 C19 106.1(5) . . ? C14 C13 O1 111.3(12) . . ? C13 C14 C15 98.4(12) . . ? C14 C15 C16 95.1(13) . . ? O1 C16 C15 101.8(11) . . ? O1 C13B C14B 101.7(14) . . ? C15B C14B C13B 106(2) . . ? C14B C15B C16B 94(2) . . ? O1 C16B C15B 97(2) . . ? #===END data_mfl-3-jan700 _database_code_CSD 168080 _audit_creation_date 2000-01-13T15:35:53-00:00 _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 '[(Me3SiNC6H4NSiMe3)Li2(thf)3]' _chemical_formula_moiety 'C24 H46 Li2 N2 O3 Si2' _chemical_formula_structural 'C24 H46 N2 LI2 SI2 O3' _chemical_formula_sum 'C24 H46 Li2 N2 O3 Si2' _chemical_formula_weight 480.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8015(7) _cell_length_b 27.9629(9) _cell_length_c 23.7088(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11801.8(6) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23421 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.145 #----------------------------------------------------------------------------# # 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 36417 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 21.94 _diffrn_reflns_theta_full 21.94 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 7079 _reflns_number_gt 5069 _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^)+(0.0605P)^2^+16.2025P] 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_number_reflns 7079 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.158 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.406 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # 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' 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' 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 Si1 Si 0.31264(6) 0.24031(4) 0.12301(5) 0.0410(3) Uani 1 1 d . . . Si2 Si 0.27991(7) 0.27399(4) -0.12452(5) 0.0472(3) Uani 1 1 d . . . O1 O 0.22608(16) 0.13808(10) -0.01261(12) 0.0516(8) Uani 1 1 d . . . O2 O 0.12839(16) 0.22752(10) 0.00462(12) 0.0534(8) Uani 1 1 d . . . O3 O 0.25587(18) 0.35555(10) 0.02012(13) 0.0608(9) Uani 1 1 d . . . N1 N 0.30986(17) 0.23637(11) 0.05173(12) 0.0367(8) Uani 1 1 d . . . N2 N 0.29385(19) 0.25048(11) -0.05969(13) 0.0424(8) Uani 1 1 d . . . C1 C 0.3643(2) 0.21497(13) 0.01688(16) 0.0367(9) Uani 1 1 d . . . C2 C 0.3552(2) 0.22254(13) -0.04280(16) 0.0389(10) Uani 1 1 d . . . C3 C 0.4061(2) 0.20043(15) -0.07919(17) 0.0483(11) Uani 1 1 d . . . H3 H 0.4003 0.2048 -0.1187 0.058 Uiso 1 1 calc R . . C4 C 0.4652(3) 0.17226(16) -0.0597(2) 0.0568(12) Uani 1 1 d . . . H4 H 0.4992 0.1581 -0.0857 0.068 Uiso 1 1 calc R . . C5 C 0.4741(2) 0.16501(15) -0.0027(2) 0.0534(12) Uani 1 1 d . . . H5 H 0.5143 0.1458 0.0109 0.064 Uiso 1 1 calc R . . C6 C 0.4235(2) 0.18618(14) 0.03517(18) 0.0457(11) Uani 1 1 d . . . H6 H 0.4297 0.1807 0.0744 0.055 Uiso 1 1 calc R . . C7 C 0.2349(2) 0.28222(15) 0.14416(16) 0.0485(11) Uani 1 1 d . . . H7A H 0.1869 0.2702 0.1296 0.073 Uiso 1 1 calc R . . H7B H 0.2447 0.314 0.1284 0.073 Uiso 1 1 calc R . . H7C H 0.2325 0.2843 0.1854 0.073 Uiso 1 1 calc R . . C8 C 0.2968(3) 0.18202(16) 0.16061(18) 0.0585(12) Uani 1 1 d . . . H8A H 0.3366 0.1594 0.1504 0.088 Uiso 1 1 calc R . . H8B H 0.248 0.1688 0.1496 0.088 Uiso 1 1 calc R . . H8C H 0.2976 0.1874 0.2014 0.088 Uiso 1 1 calc R . . C9 C 0.4010(3) 0.26702(18) 0.15276(18) 0.0649(13) Uani 1 1 d . . . H9A H 0.4439 0.2466 0.1431 0.097 Uiso 1 1 calc R . . H9B H 0.3967 0.2694 0.1939 0.097 Uiso 1 1 calc R . . H9C H 0.4086 0.299 0.1368 0.097 Uiso 1 1 calc R . . C10 C 0.2008(3) 0.31795(17) -0.11844(19) 0.0651(13) Uani 1 1 d . . . H10A H 0.2128 0.3416 -0.0893 0.098 Uiso 1 1 calc R . . H10B H 0.1546 0.301 -0.1082 0.098 Uiso 1 1 calc R . . H10C H 0.1938 0.3342 -0.1547 0.098 Uiso 1 1 calc R . . C11 C 0.2525(3) 0.23057(17) -0.18080(18) 0.0677(14) Uani 1 1 d . . . H11A H 0.2925 0.2068 -0.1856 0.102 Uiso 1 1 calc R . . H11B H 0.2447 0.2477 -0.2164 0.102 Uiso 1 1 calc R . . H11C H 0.2058 0.2144 -0.1699 0.102 Uiso 1 1 calc R . . C12 C 0.3632(3) 0.30770(18) -0.1526(2) 0.0698(14) Uani 1 1 d . . . H12A H 0.38 0.331 -0.1244 0.105 Uiso 1 1 calc R . . H12B H 0.3491 0.3244 -0.1873 0.105 Uiso 1 1 calc R . . H12C H 0.4041 0.2852 -0.1606 0.105 Uiso 1 1 calc R . . C13 C 0.2690(3) 0.10522(16) 0.02131(19) 0.0582(12) Uani 1 1 d . . . H13A H 0.2362 0.0887 0.0488 0.07 Uiso 1 1 calc R . . H13B H 0.3091 0.1222 0.0421 0.07 Uiso 1 1 calc R . . C14 C 0.3019(3) 0.07040(19) -0.0197(2) 0.0823(17) Uani 1 1 d . . . H14A H 0.3515 0.0815 -0.0333 0.099 Uiso 1 1 calc R . . H14B H 0.3077 0.0384 -0.0022 0.099 Uiso 1 1 calc R . . C15 C 0.2462(3) 0.06903(18) -0.0664(2) 0.0689(14) Uani 1 1 d . . . H15A H 0.2698 0.0589 -0.1023 0.083 Uiso 1 1 calc R . . H15B H 0.2038 0.0474 -0.0576 0.083 Uiso 1 1 calc R . . C16 C 0.2215(3) 0.11963(17) -0.0688(2) 0.0742(15) Uani 1 1 d . . . H16A H 0.2545 0.1382 -0.0944 0.089 Uiso 1 1 calc R . . H16B H 0.1693 0.1217 -0.083 0.089 Uiso 1 1 calc R . . C17 C 0.0887(3) 0.2108(2) 0.0533(2) 0.0750(15) Uani 1 1 d . . . H17A H 0.0635 0.2377 0.0728 0.09 Uiso 1 1 calc R . . H17B H 0.1234 0.195 0.08 0.09 Uiso 1 1 calc R . . C18 C 0.0322(4) 0.1760(3) 0.0314(3) 0.114(2) Uani 1 1 d . . . H18A H 0.0522 0.143 0.0338 0.137 Uiso 1 1 calc R . . H18B H -0.0146 0.1777 0.0538 0.137 Uiso 1 1 calc R . . C19 C 0.0177(3) 0.1884(2) -0.0258(2) 0.0818(17) Uani 1 1 d . . . H19A H -0.0327 0.2032 -0.0295 0.098 Uiso 1 1 calc R . . H19B H 0.0196 0.1596 -0.0501 0.098 Uiso 1 1 calc R . . C20 C 0.0781(3) 0.22366(17) -0.04294(19) 0.0630(13) Uani 1 1 d . . . H20A H 0.1054 0.212 -0.0766 0.076 Uiso 1 1 calc R . . H20B H 0.0557 0.2552 -0.0518 0.076 Uiso 1 1 calc R . . C21 C 0.1933(3) 0.38419(16) 0.0380(2) 0.0603(13) Uani 1 1 d . . . H21A H 0.1709 0.3712 0.073 0.072 Uiso 1 1 calc R . . H21B H 0.1541 0.3854 0.0084 0.072 Uiso 1 1 calc R . . C22 C 0.2261(3) 0.43304(19) 0.0481(3) 0.0831(17) Uani 1 1 d . . . H22A H 0.1886 0.4585 0.0412 0.1 Uiso 1 1 calc R . . H22B H 0.2457 0.4361 0.0871 0.1 Uiso 1 1 calc R . . C23 C 0.2884(3) 0.4348(2) 0.0057(3) 0.0934(19) Uani 1 1 d . . . H23A H 0.2691 0.4433 -0.0322 0.112 Uiso 1 1 calc R . . H23B H 0.3273 0.4583 0.0169 0.112 Uiso 1 1 calc R . . C24 C 0.3182(3) 0.38607(19) 0.0065(3) 0.0949(19) Uani 1 1 d . . . H24A H 0.3393 0.3775 -0.0309 0.114 Uiso 1 1 calc R . . H24B H 0.3583 0.383 0.0352 0.114 Uiso 1 1 calc R . . Li1 Li 0.2328(4) 0.2068(2) -0.0043(3) 0.0452(17) Uani 1 1 d . . . Li2 Li 0.2688(5) 0.2891(2) 0.0073(3) 0.060(2) Uani 1 1 d . . . Si1B Si 0.00854(7) 0.01445(4) 0.37567(4) 0.0414(3) Uani 1 1 d . . . Si2B Si 0.01628(7) 0.00617(4) 0.12082(5) 0.0460(3) Uani 1 1 d . . . O1B O -0.10386(16) -0.08347(9) 0.25470(12) 0.0526(8) Uani 1 1 d . . . O2B O -0.16087(15) 0.01977(9) 0.24546(12) 0.0501(7) Uani 1 1 d . . . O3B O 0.03620(16) 0.11934(9) 0.24281(11) 0.0505(7) Uani 1 1 d . . . N1B N 0.01446(17) 0.00181(10) 0.30565(12) 0.0363(8) Uani 1 1 d . . . N2B N 0.01826(17) -0.00153(11) 0.19183(12) 0.0353(8) Uani 1 1 d . . . C1B C 0.0622(2) -0.03265(13) 0.28135(16) 0.0359(9) Uani 1 1 d . . . C2B C 0.0636(2) -0.03435(13) 0.22067(16) 0.0362(9) Uani 1 1 d . . . C3B C 0.1106(2) -0.06853(14) 0.19540(17) 0.0441(10) Uani 1 1 d . . . H3B H 0.1134 -0.0697 0.1554 0.053 Uiso 1 1 calc R . . C4B C 0.1534(2) -0.10075(14) 0.2268(2) 0.0525(12) Uani 1 1 d . . . H4B H 0.1843 -0.1236 0.2082 0.063 Uiso 1 1 calc R . . C5B C 0.1505(2) -0.09930(15) 0.2843(2) 0.0556(12) Uani 1 1 d . . . H5B H 0.179 -0.1214 0.306 0.067 Uiso 1 1 calc R . . C6B C 0.1059(2) -0.06542(14) 0.31117(17) 0.0459(10) Uani 1 1 d . . . H6B H 0.1052 -0.0646 0.3512 0.055 Uiso 1 1 calc R . . C7B C -0.0679(3) 0.05941(17) 0.38513(19) 0.0639(13) Uani 1 1 d . . . H7B1 H -0.0578 0.0873 0.3613 0.096 Uiso 1 1 calc R . . H7B2 H -0.0699 0.0694 0.4247 0.096 Uiso 1 1 calc R . . H7B3 H -0.1161 0.0452 0.3743 0.096 Uiso 1 1 calc R . . C8B C -0.0178(3) -0.03634(16) 0.42355(17) 0.0602(13) Uani 1 1 d . . . H8B1 H 0.0202 -0.0615 0.421 0.09 Uiso 1 1 calc R . . H8B2 H -0.0667 -0.0492 0.4122 0.09 Uiso 1 1 calc R . . H8B3 H -0.0208 -0.0248 0.4625 0.09 Uiso 1 1 calc R . . C9B C 0.0969(3) 0.04141(16) 0.40465(18) 0.0593(13) Uani 1 1 d . . . H9B1 H 0.1383 0.0186 0.4005 0.089 Uiso 1 1 calc R . . H9B2 H 0.0898 0.049 0.4447 0.089 Uiso 1 1 calc R . . H9B3 H 0.1087 0.0708 0.3839 0.089 Uiso 1 1 calc R . . C10B C -0.0578(3) 0.05148(19) 0.10418(19) 0.0716(15) Uani 1 1 d . . . H10D H -0.1063 0.0404 0.1187 0.107 Uiso 1 1 calc R . . H10E H -0.061 0.0557 0.0632 0.107 Uiso 1 1 calc R . . H10F H -0.0447 0.082 0.1219 0.107 Uiso 1 1 calc R . . C11B C -0.0088(3) -0.04817(18) 0.07747(18) 0.0664(14) Uani 1 1 d . . . H11D H 0.0281 -0.0735 0.0843 0.1 Uiso 1 1 calc R . . H11E H -0.0086 -0.0397 0.0374 0.1 Uiso 1 1 calc R . . H11F H -0.0589 -0.0595 0.0882 0.1 Uiso 1 1 calc R . . C12B C 0.1068(3) 0.03059(17) 0.09156(19) 0.0669(14) Uani 1 1 d . . . H12D H 0.1476 0.0079 0.099 0.1 Uiso 1 1 calc R . . H12E H 0.1182 0.0612 0.1097 0.1 Uiso 1 1 calc R . . H12F H 0.1017 0.0353 0.0508 0.1 Uiso 1 1 calc R . . C13B C -0.0841(4) -0.11709(19) 0.2987(2) 0.0824(18) Uani 1 1 d . . . H13C H -0.1292 -0.1271 0.3201 0.099 Uiso 1 1 calc R . . H13D H -0.0475 -0.1028 0.3252 0.099 Uiso 1 1 calc R . . C14B C -0.0502(5) -0.1586(2) 0.2683(3) 0.116(3) Uani 1 1 d . . . H14C H 0.0045 -0.1604 0.2758 0.14 Uiso 1 1 calc R . . H14D H -0.0737 -0.1889 0.2807 0.14 Uiso 1 1 calc R . . C15B C -0.0638(4) -0.1508(3) 0.2094(4) 0.118(3) Uani 1 1 d . . . H15C H -0.0161 -0.1441 0.1894 0.141 Uiso 1 1 calc R . . H15D H -0.0875 -0.1793 0.1922 0.141 Uiso 1 1 calc R . . C16B C -0.1126(4) -0.1109(2) 0.2058(2) 0.098(2) Uani 1 1 d . . . H16C H -0.1002 -0.0915 0.1722 0.118 Uiso 1 1 calc R . . H16D H -0.1653 -0.1218 0.2025 0.118 Uiso 1 1 calc R . . C17B C -0.1674(3) 0.06963(19) 0.2385(3) 0.099(2) Uani 1 1 d . . . H17C H -0.1376 0.0805 0.2057 0.119 Uiso 1 1 calc R . . H17D H -0.1492 0.0865 0.2726 0.119 Uiso 1 1 calc R . . C18B C -0.2478(4) 0.0792(3) 0.2295(3) 0.125(3) Uani 1 1 d . . . H18C H -0.2622 0.1106 0.2455 0.15 Uiso 1 1 calc R . . H18D H -0.2602 0.0789 0.1888 0.15 Uiso 1 1 calc R . . C19B C -0.2827(4) 0.0430(2) 0.2569(6) 0.230(7) Uani 1 1 d . . . H19C H -0.3288 0.0336 0.2364 0.276 Uiso 1 1 calc R . . H19D H -0.2972 0.0534 0.2954 0.276 Uiso 1 1 calc R . . C20B C -0.2296(3) 0.0017(2) 0.2603(5) 0.183(5) Uani 1 1 d . . . H20C H -0.2282 -0.0115 0.299 0.219 Uiso 1 1 calc R . . H20D H -0.245 -0.024 0.2339 0.219 Uiso 1 1 calc R . . C21B C 0.0201(3) 0.15365(16) 0.2858(2) 0.0720(15) Uani 1 1 d . . . H21C H 0.0472 0.1455 0.321 0.086 Uiso 1 1 calc R . . H21D H -0.0344 0.1543 0.294 0.086 Uiso 1 1 calc R . . C22B C 0.0456(3) 0.20158(17) 0.2640(2) 0.0772(16) Uani 1 1 d . . . H22C H 0.0023 0.2207 0.2507 0.093 Uiso 1 1 calc R . . H22D H 0.0723 0.2197 0.2938 0.093 Uiso 1 1 calc R . . C23B C 0.0948(4) 0.19066(18) 0.2187(3) 0.097(2) Uani 1 1 d . . . H23C H 0.1473 0.1882 0.2322 0.117 Uiso 1 1 calc R . . H23D H 0.0922 0.2158 0.1893 0.117 Uiso 1 1 calc R . . C24B C 0.0686(3) 0.14365(15) 0.19566(19) 0.0619(13) Uani 1 1 d . . . H24C H 0.0308 0.1485 0.1656 0.074 Uiso 1 1 calc R . . H24D H 0.1113 0.1252 0.18 0.074 Uiso 1 1 calc R . . Li1B Li -0.0687(4) -0.0179(2) 0.2491(3) 0.0425(16) Uani 1 1 d . . . Li2B Li 0.0238(4) 0.0514(2) 0.2472(3) 0.0428(16) 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 Si1 0.0463(7) 0.0429(7) 0.0338(6) 0.0015(5) -0.0038(5) 0.0014(5) Si2 0.0651(8) 0.0424(7) 0.0342(7) 0.0060(5) -0.0001(6) -0.0015(6) O1 0.0515(19) 0.0440(17) 0.0593(19) -0.0076(14) -0.0060(14) 0.0048(15) O2 0.0458(18) 0.0633(19) 0.0511(18) 0.0014(15) -0.0011(14) 0.0097(15) O3 0.072(2) 0.0383(17) 0.072(2) 0.0003(15) 0.0175(17) 0.0137(17) N1 0.0393(19) 0.0355(18) 0.0354(18) 0.0002(14) -0.0022(15) 0.0019(15) N2 0.050(2) 0.0402(19) 0.0367(19) 0.0023(15) 0.0025(16) 0.0072(17) C1 0.037(2) 0.029(2) 0.044(2) 0.0005(17) 0.0019(19) -0.0032(19) C2 0.045(3) 0.032(2) 0.040(2) 0.0012(18) 0.0050(19) -0.001(2) C3 0.053(3) 0.050(3) 0.042(2) 0.000(2) 0.011(2) 0.003(2) C4 0.050(3) 0.050(3) 0.069(3) -0.001(2) 0.021(2) 0.002(2) C5 0.036(3) 0.050(3) 0.074(4) 0.005(2) 0.004(2) 0.007(2) C6 0.040(3) 0.047(3) 0.050(3) 0.006(2) -0.001(2) -0.001(2) C7 0.063(3) 0.048(3) 0.035(2) -0.0056(19) 0.002(2) 0.006(2) C8 0.073(3) 0.057(3) 0.046(3) 0.010(2) 0.006(2) 0.009(3) C9 0.066(3) 0.079(3) 0.050(3) -0.010(2) -0.012(2) -0.012(3) C10 0.082(4) 0.061(3) 0.052(3) 0.012(2) -0.008(3) 0.013(3) C11 0.099(4) 0.057(3) 0.047(3) 0.000(2) -0.013(3) 0.000(3) C12 0.083(4) 0.063(3) 0.063(3) 0.015(2) 0.011(3) -0.009(3) C13 0.073(3) 0.048(3) 0.054(3) 0.011(2) -0.002(2) -0.008(3) C14 0.085(4) 0.068(4) 0.094(4) -0.014(3) -0.022(3) 0.024(3) C15 0.071(3) 0.060(3) 0.076(4) -0.013(3) 0.004(3) 0.001(3) C16 0.107(4) 0.052(3) 0.064(3) -0.014(2) -0.022(3) 0.008(3) C17 0.060(3) 0.110(4) 0.055(3) 0.001(3) 0.009(3) 0.006(3) C18 0.103(5) 0.159(7) 0.079(4) 0.027(4) -0.001(4) -0.053(5) C19 0.076(4) 0.074(4) 0.095(4) 0.012(3) -0.016(3) -0.018(3) C20 0.065(3) 0.064(3) 0.059(3) 0.006(2) -0.008(2) 0.014(3) C21 0.061(3) 0.053(3) 0.068(3) 0.007(2) 0.004(2) 0.006(3) C22 0.067(4) 0.063(3) 0.119(5) -0.032(3) 0.017(3) 0.005(3) C23 0.079(4) 0.063(4) 0.139(5) -0.026(4) 0.025(4) -0.019(3) C24 0.067(4) 0.065(4) 0.153(6) -0.018(4) 0.021(4) -0.003(3) Li1 0.049(4) 0.044(4) 0.043(4) -0.002(3) -0.007(3) -0.001(3) Li2 0.095(6) 0.039(4) 0.046(4) 0.005(3) 0.001(4) 0.021(4) Si1B 0.0507(7) 0.0396(6) 0.0339(6) -0.0019(5) 0.0016(5) -0.0030(5) Si2B 0.0490(7) 0.0536(7) 0.0355(7) -0.0036(5) 0.0016(5) -0.0006(6) O1B 0.0527(19) 0.0372(15) 0.068(2) -0.0064(15) -0.0016(15) -0.0044(14) O2B 0.0339(16) 0.0373(16) 0.079(2) 0.0031(14) 0.0058(14) 0.0020(13) O3B 0.0624(19) 0.0349(15) 0.0543(18) 0.0001(14) 0.0090(15) -0.0085(14) N1B 0.0395(19) 0.0349(18) 0.0344(18) -0.0026(14) 0.0022(14) 0.0063(15) N2B 0.0326(18) 0.0401(18) 0.0333(18) -0.0010(14) 0.0016(14) 0.0022(15) C1B 0.034(2) 0.035(2) 0.039(2) -0.0041(18) -0.0032(18) -0.0007(19) C2B 0.029(2) 0.030(2) 0.050(3) -0.0066(18) 0.0031(18) -0.0058(18) C3B 0.039(2) 0.044(2) 0.050(3) -0.011(2) 0.006(2) 0.000(2) C4B 0.043(3) 0.037(2) 0.078(4) -0.014(2) 0.002(2) 0.009(2) C5B 0.048(3) 0.042(3) 0.077(4) -0.001(2) -0.013(2) 0.013(2) C6B 0.046(3) 0.042(2) 0.050(3) 0.001(2) -0.007(2) 0.008(2) C7B 0.074(3) 0.064(3) 0.053(3) -0.012(2) 0.016(2) 0.010(3) C8B 0.077(3) 0.060(3) 0.043(3) 0.002(2) 0.008(2) -0.015(3) C9B 0.073(3) 0.058(3) 0.047(3) -0.008(2) -0.008(2) -0.015(3) C10B 0.082(4) 0.084(4) 0.049(3) 0.008(3) -0.007(3) 0.020(3) C11B 0.069(3) 0.085(4) 0.046(3) -0.014(2) -0.007(2) -0.007(3) C12B 0.078(4) 0.069(3) 0.054(3) -0.007(2) 0.023(3) -0.007(3) C13B 0.120(5) 0.072(4) 0.055(3) 0.003(3) 0.010(3) -0.044(4) C14B 0.148(7) 0.046(3) 0.155(7) 0.001(4) -0.038(6) 0.017(4) C15B 0.088(5) 0.110(6) 0.155(7) -0.070(5) 0.008(5) 0.002(4) C16B 0.162(7) 0.060(3) 0.072(4) -0.005(3) -0.033(4) -0.039(4) C17B 0.079(4) 0.056(3) 0.164(6) 0.023(4) 0.045(4) 0.013(3) C18B 0.120(6) 0.089(5) 0.167(7) -0.006(5) -0.064(5) 0.042(5) C19B 0.059(5) 0.058(4) 0.57(2) 0.055(8) 0.102(8) 0.012(4) C20B 0.045(4) 0.055(4) 0.448(16) 0.029(6) 0.049(6) 0.000(3) C21B 0.096(4) 0.053(3) 0.068(3) -0.017(3) 0.023(3) -0.022(3) C22B 0.104(4) 0.043(3) 0.085(4) -0.008(3) 0.017(3) -0.011(3) C23B 0.134(6) 0.049(3) 0.109(5) -0.011(3) 0.057(4) -0.030(3) C24B 0.081(4) 0.048(3) 0.057(3) 0.001(2) 0.013(3) -0.008(3) Li1B 0.035(4) 0.040(4) 0.053(4) -0.003(3) 0.002(3) 0.000(3) Li2B 0.051(4) 0.034(3) 0.043(4) 0.001(3) -0.002(3) -0.003(3) #----------------------------------------------------------------------------# # 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 Si1 N1 1.694(3) . ? Si1 C8 1.879(4) . ? Si1 C9 1.879(4) . ? Si1 C7 1.882(4) . ? Si1 Li2 3.162(7) . ? Si2 N2 1.690(3) . ? Si2 C11 1.869(4) . ? Si2 C10 1.875(5) . ? Si2 C12 1.879(5) . ? Si2 Li2 3.160(7) . ? O1 C16 1.432(5) . ? O1 C13 1.440(5) . ? O1 Li1 1.934(7) . ? O2 C17 1.432(5) . ? O2 C20 1.444(5) . ? O2 Li1 1.959(7) . ? O3 C21 1.436(5) . ? O3 C24 1.438(6) . ? O3 Li2 1.897(7) . ? N1 C1 1.407(5) . ? N1 Li2 1.954(7) . ? N1 Li1 2.081(7) . ? N2 C2 1.401(5) . ? N2 Li2 1.971(8) . ? N2 Li1 2.098(7) . ? C1 C6 1.395(5) . ? C1 C2 1.440(5) . ? C1 Li1 2.405(8) . ? C1 Li2 2.690(8) . ? C2 C3 1.396(5) . ? C2 Li1 2.402(8) . ? C2 Li2 2.690(8) . ? C3 C4 1.393(6) . ? C4 C5 1.376(6) . ? C5 C6 1.403(6) . ? C13 C14 1.495(6) . ? C14 C15 1.488(7) . ? C15 C16 1.483(6) . ? C17 C18 1.493(8) . ? C18 C19 1.425(7) . ? C19 C20 1.514(7) . ? C21 C22 1.505(7) . ? C22 C23 1.498(7) . ? C23 C24 1.464(7) . ? Li1 Li2 2.405(10) . ? Si1B N1B 1.701(3) . ? Si1B C7B 1.865(5) . ? Si1B C9B 1.875(4) . ? Si1B C8B 1.878(4) . ? Si2B N2B 1.698(3) . ? Si2B C10B 1.870(5) . ? Si2B C12B 1.883(5) . ? Si2B C11B 1.888(5) . ? O1B C16B 1.398(6) . ? O1B C13B 1.448(6) . ? O1B Li1B 1.941(7) . ? O2B C20B 1.370(6) . ? O2B C17B 1.409(6) . ? O2B Li1B 1.953(7) . ? O3B C21B 1.429(5) . ? O3B C24B 1.430(5) . ? O3B Li2B 1.915(7) . ? N1B C1B 1.408(5) . ? N1B Li2B 1.968(7) . ? N1B Li1B 2.072(7) . ? N2B C2B 1.401(5) . ? N2B Li2B 1.980(7) . ? N2B Li1B 2.109(7) . ? C1B C6B 1.395(5) . ? C1B C2B 1.440(5) . ? C1B Li1B 2.486(7) . ? C1B Li2B 2.578(7) . ? C2B C3B 1.405(5) . ? C2B Li1B 2.492(7) . ? C2B Li2B 2.578(7) . ? C3B C4B 1.395(6) . ? C4B C5B 1.366(6) . ? C5B C6B 1.390(6) . ? C13B C14B 1.494(8) . ? C14B C15B 1.433(9) . ? C15B C16B 1.416(8) . ? C17B C18B 1.471(9) . ? C18B C19B 1.355(10) . ? C19B C20B 1.497(9) . ? C21B C22B 1.507(6) . ? C22B C23B 1.419(7) . ? C23B C24B 1.497(6) . ? Li1B Li2B 2.544(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C8 114.35(18) . . ? N1 Si1 C9 115.13(19) . . ? C8 Si1 C9 107.0(2) . . ? N1 Si1 C7 106.54(17) . . ? C8 Si1 C7 107.7(2) . . ? C9 Si1 C7 105.6(2) . . ? N1 Si1 Li2 32.36(16) . . ? C8 Si1 Li2 138.5(2) . . ? C9 Si1 Li2 111.1(2) . . ? C7 Si1 Li2 77.35(19) . . ? N2 Si2 C11 115.79(19) . . ? N2 Si2 C10 107.17(18) . . ? C11 Si2 C10 106.5(2) . . ? N2 Si2 C12 113.7(2) . . ? C11 Si2 C12 106.2(2) . . ? C10 Si2 C12 106.9(2) . . ? N2 Si2 Li2 33.02(16) . . ? C11 Si2 Li2 141.0(2) . . ? C10 Si2 Li2 77.8(2) . . ? C12 Si2 Li2 109.4(2) . . ? C16 O1 C13 108.7(3) . . ? C16 O1 Li1 117.2(3) . . ? C13 O1 Li1 122.9(3) . . ? C17 O2 C20 107.4(3) . . ? C17 O2 Li1 117.3(3) . . ? C20 O2 Li1 118.8(3) . . ? C21 O3 C24 109.5(3) . . ? C21 O3 Li2 133.5(4) . . ? C24 O3 Li2 116.8(4) . . ? C1 N1 Si1 126.4(3) . . ? C1 N1 Li2 105.2(3) . . ? Si1 N1 Li2 120.0(3) . . ? C1 N1 Li1 84.8(3) . . ? Si1 N1 Li1 133.0(3) . . ? Li2 N1 Li1 73.1(3) . . ? C2 N2 Si2 126.2(3) . . ? C2 N2 Li2 104.5(3) . . ? Si2 N2 Li2 119.1(3) . . ? C2 N2 Li1 84.2(3) . . ? Si2 N2 Li1 136.1(3) . . ? Li2 N2 Li1 72.4(3) . . ? C6 C1 N1 125.7(3) . . ? C6 C1 C2 118.4(4) . . ? N1 C1 C2 115.9(3) . . ? C6 C1 Li1 138.1(3) . . ? N1 C1 Li1 59.5(2) . . ? C2 C1 Li1 72.5(3) . . ? C6 C1 Li2 161.5(3) . . ? N1 C1 Li2 44.5(2) . . ? C2 C1 Li2 74.5(3) . . ? Li1 C1 Li2 56.0(3) . . ? C3 C2 N2 125.2(4) . . ? C3 C2 C1 117.9(4) . . ? N2 C2 C1 116.8(3) . . ? C3 C2 Li1 138.0(3) . . ? N2 C2 Li1 60.3(2) . . ? C1 C2 Li1 72.7(3) . . ? C3 C2 Li2 161.9(3) . . ? N2 C2 Li2 45.2(2) . . ? C1 C2 Li2 74.5(3) . . ? Li1 C2 Li2 56.0(3) . . ? C4 C3 C2 122.4(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 119.4(4) . . ? C1 C6 C5 122.0(4) . . ? O1 C13 C14 105.1(4) . . ? C15 C14 C13 103.9(4) . . ? C16 C15 C14 101.6(4) . . ? O1 C16 C15 106.9(4) . . ? O2 C17 C18 105.4(4) . . ? C19 C18 C17 107.1(5) . . ? C18 C19 C20 106.5(5) . . ? O2 C20 C19 106.3(4) . . ? O3 C21 C22 104.6(4) . . ? C23 C22 C21 102.2(4) . . ? C24 C23 C22 103.2(5) . . ? O3 C24 C23 106.0(4) . . ? O1 Li1 O2 104.3(3) . . ? O1 Li1 N1 120.1(3) . . ? O2 Li1 N1 116.0(3) . . ? O1 Li1 N2 123.2(4) . . ? O2 Li1 N2 112.7(3) . . ? N1 Li1 N2 80.0(3) . . ? O1 Li1 C2 101.5(3) . . ? O2 Li1 C2 147.9(4) . . ? N1 Li1 C2 64.7(2) . . ? N2 Li1 C2 35.46(16) . . ? O1 Li1 C1 100.2(3) . . ? O2 Li1 C1 150.8(4) . . ? N1 Li1 C1 35.65(16) . . ? N2 Li1 C1 64.6(2) . . ? C2 Li1 C1 34.86(16) . . ? O1 Li1 Li2 168.1(4) . . ? O2 Li1 Li2 87.5(3) . . ? N1 Li1 Li2 51.0(2) . . ? N2 Li1 Li2 51.4(2) . . ? C2 Li1 Li2 68.0(3) . . ? C1 Li1 Li2 68.0(3) . . ? O3 Li2 N1 134.3(4) . . ? O3 Li2 N2 133.9(4) . . ? N1 Li2 N2 86.4(3) . . ? O3 Li2 Li1 157.4(5) . . ? N1 Li2 Li1 55.9(3) . . ? N2 Li2 Li1 56.2(3) . . ? O3 Li2 C2 144.9(4) . . ? N1 Li2 C2 60.2(2) . . ? N2 Li2 C2 30.27(16) . . ? Li1 Li2 C2 55.9(2) . . ? O3 Li2 C1 144.9(5) . . ? N1 Li2 C1 30.33(16) . . ? N2 Li2 C1 60.2(2) . . ? Li1 Li2 C1 56.0(2) . . ? C2 Li2 C1 31.05(14) . . ? O3 Li2 Si2 107.3(3) . . ? N1 Li2 Si2 114.2(3) . . ? N2 Li2 Si2 27.86(14) . . ? Li1 Li2 Si2 77.0(2) . . ? C2 Li2 Si2 55.61(16) . . ? C1 Li2 Si2 86.6(2) . . ? O3 Li2 Si1 108.3(3) . . ? N1 Li2 Si1 27.65(14) . . ? N2 Li2 Si1 114.0(3) . . ? Li1 Li2 Si1 75.6(2) . . ? C2 Li2 Si1 86.8(2) . . ? C1 Li2 Si1 55.84(15) . . ? Si2 Li2 Si1 141.7(2) . . ? N1B Si1B C7B 107.61(18) . . ? N1B Si1B C9B 112.91(18) . . ? C7B Si1B C9B 107.2(2) . . ? N1B Si1B C8B 116.64(18) . . ? C7B Si1B C8B 104.8(2) . . ? C9B Si1B C8B 107.0(2) . . ? N2B Si2B C10B 108.05(18) . . ? N2B Si2B C12B 113.18(19) . . ? C10B Si2B C12B 106.2(2) . . ? N2B Si2B C11B 116.28(19) . . ? C10B Si2B C11B 105.3(2) . . ? C12B Si2B C11B 107.1(2) . . ? C16B O1B C13B 105.5(4) . . ? C16B O1B Li1B 119.8(4) . . ? C13B O1B Li1B 125.7(3) . . ? C20B O2B C17B 108.8(4) . . ? C20B O2B Li1B 122.7(4) . . ? C17B O2B Li1B 127.5(4) . . ? C21B O3B C24B 108.6(3) . . ? C21B O3B Li2B 127.2(3) . . ? C24B O3B Li2B 124.1(3) . . ? C1B N1B Si1B 125.4(2) . . ? C1B N1B Li2B 98.2(3) . . ? Si1B N1B Li2B 123.1(2) . . ? C1B N1B Li1B 89.0(3) . . ? Si1B N1B Li1B 130.0(3) . . ? Li2B N1B Li1B 78.0(3) . . ? C2B N2B Si2B 125.4(3) . . ? C2B N2B Li2B 97.9(3) . . ? Si2B N2B Li2B 124.3(2) . . ? C2B N2B Li1B 88.1(3) . . ? Si2B N2B Li1B 130.6(2) . . ? Li2B N2B Li1B 76.9(3) . . ? C6B C1B N1B 125.4(3) . . ? C6B C1B C2B 118.3(3) . . ? N1B C1B C2B 116.3(3) . . ? C6B C1B Li1B 142.0(3) . . ? N1B C1B Li1B 56.5(2) . . ? C2B C1B Li1B 73.4(3) . . ? C6B C1B Li2B 154.9(3) . . ? N1B C1B Li2B 49.1(2) . . ? C2B C1B Li2B 73.8(3) . . ? Li1B C1B Li2B 60.3(2) . . ? N2B C2B C3B 125.5(4) . . ? N2B C2B C1B 117.1(3) . . ? C3B C2B C1B 117.4(4) . . ? N2B C2B Li1B 57.8(2) . . ? C3B C2B Li1B 143.5(3) . . ? C1B C2B Li1B 73.0(3) . . ? N2B C2B Li2B 49.5(2) . . ? C3B C2B Li2B 154.2(3) . . ? C1B C2B Li2B 73.8(3) . . ? Li1B C2B Li2B 60.2(2) . . ? C4B C3B C2B 122.5(4) . . ? C5B C4B C3B 119.6(4) . . ? C4B C5B C6B 119.9(4) . . ? C5B C6B C1B 122.3(4) . . ? O1B C13B C14B 104.8(4) . . ? C15B C14B C13B 106.5(5) . . ? C16B C15B C14B 106.4(5) . . ? O1B C16B C15B 108.3(5) . . ? O2B C17B C18B 106.1(5) . . ? C19B C18B C17B 103.9(6) . . ? C18B C19B C20B 108.2(6) . . ? O2B C20B C19B 105.4(5) . . ? O3B C21B C22B 107.0(4) . . ? C23B C22B C21B 104.7(4) . . ? C22B C23B C24B 105.8(4) . . ? O3B C24B C23B 105.0(4) . . ? O1B Li1B O2B 104.0(3) . . ? O1B Li1B N1B 116.0(3) . . ? O2B Li1B N1B 119.0(3) . . ? O1B Li1B N2B 119.1(3) . . ? O2B Li1B N2B 118.1(3) . . ? N1B Li1B N2B 80.5(3) . . ? O1B Li1B C1B 97.2(3) . . ? O2B Li1B C1B 152.9(3) . . ? N1B Li1B C1B 34.49(15) . . ? N2B Li1B C1B 63.0(2) . . ? O1B Li1B C2B 98.6(3) . . ? O2B Li1B C2B 151.9(4) . . ? N1B Li1B C2B 63.2(2) . . ? N2B Li1B C2B 34.17(15) . . ? C1B Li1B C2B 33.63(15) . . ? O1B Li1B Li2B 158.4(4) . . ? O2B Li1B Li2B 97.6(3) . . ? N1B Li1B Li2B 49.2(2) . . ? N2B Li1B Li2B 49.3(2) . . ? C1B Li1B Li2B 61.7(2) . . ? C2B Li1B Li2B 61.6(2) . . ? O3B Li2B N1B 138.3(4) . . ? O3B Li2B N2B 135.3(4) . . ? N1B Li2B N2B 86.3(3) . . ? O3B Li2B Li1B 146.2(4) . . ? N1B Li2B Li1B 52.8(2) . . ? N2B Li2B Li1B 53.8(2) . . ? O3B Li2B C1B 153.0(4) . . ? N1B Li2B C1B 32.71(15) . . ? N2B Li2B C1B 62.6(2) . . ? Li1B Li2B C1B 58.1(2) . . ? O3B Li2B C2B 151.4(4) . . ? N1B Li2B C2B 62.6(2) . . ? N2B Li2B C2B 32.55(15) . . ? Li1B Li2B C2B 58.2(2) . . ? C1B Li2B C2B 32.43(14) . . ? #===END data_mfl-4-dec798 _database_code_CSD 168081 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4{N(SiMe3)Li(tmeda)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Li2 N6 Si2' _chemical_formula_weight 496.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.813(5) _cell_length_b 16.812(3) _cell_length_c 10.872(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.20(3) _cell_angle_gamma 90.00 _cell_volume 1609.3(9) _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 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.131 _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 ? _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 3098 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2931 _reflns_number_gt 2519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.6117P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(19) _refine_ls_number_reflns 2931 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Si1 Si 0.40161(12) 0.40365(6) 0.16412(11) 0.0251(3) Uani 1 1 d . . . Si2 Si 0.10350(13) 0.67432(6) 0.32949(11) 0.0300(3) Uani 1 1 d . . . N1 N 0.2947(3) 0.46994(19) 0.2012(3) 0.0211(7) Uani 1 1 d . . . N2 N 0.1608(3) 0.59519(19) 0.2663(3) 0.0229(7) Uani 1 1 d . . . N3 N 0.4351(4) 0.6649(2) 0.1209(4) 0.0450(10) Uani 1 1 d . . . N4 N 0.1281(4) 0.6239(2) -0.0777(4) 0.0384(9) Uani 1 1 d . . . N5 N 0.4862(4) 0.5088(2) 0.5972(3) 0.0401(9) Uani 1 1 d . . . N6 N 0.2001(4) 0.4159(2) 0.4689(3) 0.0344(8) Uani 1 1 d . . . C1 C 0.1362(4) 0.4702(2) 0.1447(4) 0.0213(8) Uani 1 1 d . . . C2 C 0.0655(4) 0.5363(2) 0.1816(3) 0.0202(7) Uani 1 1 d . . . C3 C -0.0937(4) 0.5350(3) 0.1281(4) 0.0281(9) Uani 1 1 d . . . H3 H -0.1423 0.5765 0.1532 0.034 Uiso 1 1 calc R . . C4 C -0.1834(4) 0.4758(3) 0.0402(4) 0.0333(10) Uani 1 1 d . . . H4 H -0.2907 0.4780 0.0055 0.040 Uiso 1 1 calc R . . C5 C -0.1173(4) 0.4148(3) 0.0037(4) 0.0340(10) Uani 1 1 d . . . H5 H -0.1781 0.3743 -0.0563 0.041 Uiso 1 1 calc R . . C6 C 0.0400(4) 0.4126(2) 0.0555(4) 0.0274(8) Uani 1 1 d . . . H6 H 0.0845 0.3698 0.0289 0.033 Uiso 1 1 calc R . . C7 C 0.3728(5) 0.4082(3) -0.0195(4) 0.0382(10) Uani 1 1 d . . . H7A H 0.2662 0.3971 -0.0813 0.057 Uiso 1 1 calc R . . H7B H 0.4376 0.3684 -0.0336 0.057 Uiso 1 1 calc R . . H7C H 0.3998 0.4613 -0.0387 0.057 Uiso 1 1 calc R . . C8 C 0.6065(5) 0.4256(3) 0.2766(5) 0.0440(12) Uani 1 1 d . . . H8A H 0.6254 0.4237 0.3729 0.066 Uiso 1 1 calc R . . H8B H 0.6315 0.4786 0.2552 0.066 Uiso 1 1 calc R . . H8C H 0.6700 0.3858 0.2605 0.066 Uiso 1 1 calc R . . C9 C 0.3783(5) 0.2939(3) 0.1924(5) 0.0416(11) Uani 1 1 d . . . H9A H 0.2726 0.2780 0.1364 0.062 Uiso 1 1 calc R . . H9B H 0.4052 0.2846 0.2894 0.062 Uiso 1 1 calc R . . H9C H 0.4453 0.2624 0.1660 0.062 Uiso 1 1 calc R . . C10 C 0.0220(8) 0.6467(3) 0.4516(6) 0.0638(17) Uani 1 1 d . . . H10A H -0.0667 0.6123 0.4045 0.096 Uiso 1 1 calc R . . H10B H -0.0086 0.6950 0.4832 0.096 Uiso 1 1 calc R . . H10C H 0.0990 0.6184 0.5304 0.096 Uiso 1 1 calc R . . C11 C -0.0419(6) 0.7442(3) 0.2058(5) 0.0469(12) Uani 1 1 d . . . H11A H -0.1355 0.7148 0.1506 0.070 Uiso 1 1 calc R . . H11B H -0.0026 0.7678 0.1454 0.070 Uiso 1 1 calc R . . H11C H -0.0635 0.7864 0.2568 0.070 Uiso 1 1 calc R . . C12 C 0.2708(6) 0.7395(3) 0.4257(6) 0.0647(16) Uani 1 1 d . . . H12A H 0.3533 0.7078 0.4940 0.097 Uiso 1 1 calc R . . H12B H 0.2422 0.7817 0.4720 0.097 Uiso 1 1 calc R . . H12C H 0.3048 0.7633 0.3618 0.097 Uiso 1 1 calc R . . C13 C 0.3437(7) 0.7137(4) 0.0012(8) 0.087(2) Uani 1 1 d . . . H13A H 0.2917 0.7552 0.0295 0.104 Uiso 1 1 calc R . . H13B H 0.4129 0.7411 -0.0292 0.104 Uiso 1 1 calc R . . C14 C 0.2311(7) 0.6712(5) -0.1138(6) 0.074(2) Uani 1 1 d . . . H14A H 0.2832 0.6354 -0.1519 0.088 Uiso 1 1 calc R . . H14B H 0.1707 0.7098 -0.1862 0.088 Uiso 1 1 calc R . . C15 C 0.5484(7) 0.6224(4) 0.0936(8) 0.081(2) Uani 1 1 d . . . H15A H 0.4973 0.5857 0.0167 0.121 Uiso 1 1 calc R . . H15B H 0.6152 0.5923 0.1753 0.121 Uiso 1 1 calc R . . H15C H 0.6087 0.6606 0.0703 0.121 Uiso 1 1 calc R . . C16 C 0.5126(12) 0.7170(6) 0.2365(9) 0.140(4) Uani 1 1 d . . . H16A H 0.4378 0.7454 0.2569 0.211 Uiso 1 1 calc R . . H16B H 0.5738 0.7554 0.2147 0.211 Uiso 1 1 calc R . . H16C H 0.5789 0.6854 0.3165 0.211 Uiso 1 1 calc R . . C17 C 0.0656(7) 0.5601(4) -0.1745(5) 0.0634(16) Uani 1 1 d . . . H17A H -0.0028 0.5283 -0.1504 0.095 Uiso 1 1 calc R . . H17B H 0.1481 0.5263 -0.1722 0.095 Uiso 1 1 calc R . . H17C H 0.0090 0.5821 -0.2668 0.095 Uiso 1 1 calc R . . C18 C 0.0027(7) 0.6731(4) -0.0845(6) 0.0645(16) Uani 1 1 d . . . H18A H 0.0428 0.7177 -0.0204 0.097 Uiso 1 1 calc R . . H18B H -0.0649 0.6410 -0.0597 0.097 Uiso 1 1 calc R . . H18C H -0.0540 0.6936 -0.1778 0.097 Uiso 1 1 calc R . . C19 C 0.4529(6) 0.4372(3) 0.6589(5) 0.0557(14) Uani 1 1 d . . . H19A H 0.4965 0.3901 0.6345 0.067 Uiso 1 1 calc R . . H19B H 0.5044 0.4427 0.7599 0.067 Uiso 1 1 calc R . . C20 C 0.2929(6) 0.4231(4) 0.6164(5) 0.0523(14) Uani 1 1 d . . . H20A H 0.2524 0.4673 0.6507 0.063 Uiso 1 1 calc R . . H20B H 0.2822 0.3737 0.6608 0.063 Uiso 1 1 calc R . . C21 C 0.6387(6) 0.5013(5) 0.6102(6) 0.083(2) Uani 1 1 d . . . H21A H 0.6454 0.4536 0.5612 0.124 Uiso 1 1 calc R . . H21B H 0.7105 0.4967 0.7073 0.124 Uiso 1 1 calc R . . H21C H 0.6637 0.5483 0.5710 0.124 Uiso 1 1 calc R . . C22 C 0.4760(8) 0.5794(4) 0.6699(6) 0.082(2) Uani 1 1 d . . . H22A H 0.3729 0.5840 0.6619 0.123 Uiso 1 1 calc R . . H22B H 0.4997 0.6265 0.6300 0.123 Uiso 1 1 calc R . . H22C H 0.5487 0.5751 0.7668 0.123 Uiso 1 1 calc R . . C23 C 0.2248(7) 0.3383(3) 0.4210(5) 0.0580(15) Uani 1 1 d . . . H23A H 0.3326 0.3323 0.4437 0.087 Uiso 1 1 calc R . . H23B H 0.1642 0.3347 0.3215 0.087 Uiso 1 1 calc R . . H23C H 0.1941 0.2961 0.4657 0.087 Uiso 1 1 calc R . . C24 C 0.0402(6) 0.4224(4) 0.4358(6) 0.0659(17) Uani 1 1 d . . . H24A H 0.0206 0.4745 0.4652 0.099 Uiso 1 1 calc R . . H24B H 0.0126 0.3804 0.4831 0.099 Uiso 1 1 calc R . . H24C H -0.0207 0.4168 0.3365 0.099 Uiso 1 1 calc R . . Li1 Li 0.2732(7) 0.5887(4) 0.1434(7) 0.0283(14) Uani 1 1 d . . . Li2 Li 0.3037(8) 0.5065(4) 0.3851(6) 0.0286(15) 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 Si1 0.0275(5) 0.0231(6) 0.0279(5) 0.0016(5) 0.0153(4) 0.0053(5) Si2 0.0382(6) 0.0263(6) 0.0268(6) -0.0014(5) 0.0154(5) 0.0096(5) N1 0.0210(16) 0.0191(15) 0.0232(16) -0.0010(13) 0.0098(13) 0.0010(13) N2 0.0218(16) 0.0214(17) 0.0251(16) -0.0015(14) 0.0099(13) 0.0012(14) N3 0.044(2) 0.036(2) 0.065(3) -0.004(2) 0.034(2) -0.0090(19) N4 0.044(2) 0.043(2) 0.037(2) 0.0122(18) 0.0250(18) 0.0081(18) N5 0.038(2) 0.046(2) 0.0278(18) -0.0014(17) 0.0075(16) 0.0000(18) N6 0.041(2) 0.035(2) 0.0292(17) 0.0071(16) 0.0171(16) 0.0033(17) C1 0.0263(19) 0.0208(18) 0.0189(17) 0.0014(15) 0.0119(15) -0.0015(16) C2 0.0253(19) 0.0199(18) 0.0161(16) 0.0038(14) 0.0099(15) 0.0018(15) C3 0.0227(19) 0.032(2) 0.030(2) 0.0046(17) 0.0125(17) 0.0067(17) C4 0.021(2) 0.042(3) 0.035(2) 0.005(2) 0.0096(18) -0.0038(19) C5 0.030(2) 0.032(2) 0.032(2) -0.0004(19) 0.0060(17) -0.0117(19) C6 0.034(2) 0.021(2) 0.0280(18) -0.0007(17) 0.0143(17) -0.0024(18) C7 0.053(3) 0.034(2) 0.037(2) 0.004(2) 0.028(2) 0.009(2) C8 0.032(2) 0.049(3) 0.053(3) 0.009(2) 0.020(2) 0.009(2) C9 0.053(3) 0.027(2) 0.052(3) 0.007(2) 0.029(2) 0.010(2) C10 0.109(5) 0.053(3) 0.056(3) 0.010(3) 0.061(3) 0.030(3) C11 0.053(3) 0.033(3) 0.055(3) 0.004(2) 0.023(2) 0.016(2) C12 0.071(4) 0.039(3) 0.066(4) -0.024(3) 0.014(3) -0.001(3) C13 0.061(4) 0.061(4) 0.146(7) 0.041(5) 0.053(4) -0.006(3) C14 0.057(3) 0.100(5) 0.068(4) 0.049(4) 0.031(3) 0.004(4) C15 0.054(4) 0.060(4) 0.144(7) 0.026(4) 0.058(4) 0.011(3) C16 0.209(11) 0.125(8) 0.121(7) -0.067(6) 0.103(8) -0.117(8) C17 0.072(4) 0.073(4) 0.036(3) 0.007(3) 0.015(3) 0.022(3) C18 0.076(4) 0.067(4) 0.069(3) 0.027(3) 0.050(3) 0.038(3) C19 0.059(3) 0.060(3) 0.034(3) 0.010(2) 0.008(2) -0.001(3) C20 0.059(3) 0.067(4) 0.030(2) 0.012(2) 0.019(2) -0.003(3) C21 0.049(3) 0.132(7) 0.058(4) 0.009(4) 0.015(3) 0.003(4) C22 0.107(5) 0.055(4) 0.049(3) -0.013(3) 0.002(3) 0.013(4) C23 0.093(4) 0.038(3) 0.054(3) -0.001(2) 0.042(3) -0.009(3) C24 0.041(3) 0.076(4) 0.083(4) 0.033(3) 0.029(3) 0.002(3) Li1 0.029(4) 0.027(3) 0.033(3) 0.001(3) 0.018(3) 0.001(3) Li2 0.032(4) 0.031(4) 0.023(3) 0.003(3) 0.012(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.697(3) . ? Si1 C8 1.872(5) . ? Si1 C7 1.890(4) . ? Si1 C9 1.901(5) . ? Si2 N2 1.703(3) . ? Si2 C12 1.864(5) . ? Si2 C11 1.879(5) . ? Si2 C10 1.885(5) . ? N1 C1 1.397(5) . ? N1 Li2 2.056(7) . ? N1 Li1 2.076(7) . ? N2 C2 1.394(5) . ? N2 Li2 2.063(7) . ? N2 Li1 2.078(7) . ? N3 C16 1.442(8) . ? N3 C15 1.459(7) . ? N3 C13 1.463(8) . ? N3 Li1 2.136(8) . ? N4 C17 1.437(7) . ? N4 C18 1.457(6) . ? N4 C14 1.470(6) . ? N4 Li1 2.265(8) . ? N5 C21 1.446(7) . ? N5 C22 1.453(7) . ? N5 C19 1.483(6) . ? N5 Li2 2.209(7) . ? N6 C24 1.451(6) . ? N6 C20 1.458(6) . ? N6 C23 1.463(6) . ? N6 Li2 2.238(8) . ? C1 C6 1.401(5) . ? C1 C2 1.457(5) . ? C1 Li1 2.408(8) . ? C1 Li2 2.472(7) . ? C2 C3 1.406(5) . ? C2 Li1 2.420(7) . ? C2 Li2 2.458(7) . ? C3 C4 1.391(6) . ? C4 C5 1.362(6) . ? C5 C6 1.391(5) . ? C13 C14 1.441(9) . ? C19 C20 1.447(7) . ? Li1 Li2 2.866(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C8 108.31(19) . . ? N1 Si1 C7 113.88(18) . . ? C8 Si1 C7 107.4(2) . . ? N1 Si1 C9 117.92(18) . . ? C8 Si1 C9 104.9(2) . . ? C7 Si1 C9 103.7(2) . . ? N2 Si2 C12 108.7(2) . . ? N2 Si2 C11 118.78(19) . . ? C12 Si2 C11 103.7(3) . . ? N2 Si2 C10 114.2(2) . . ? C12 Si2 C10 107.0(3) . . ? C11 Si2 C10 103.5(2) . . ? C1 N1 Si1 125.6(3) . . ? C1 N1 Li2 89.3(3) . . ? Si1 N1 Li2 131.4(3) . . ? C1 N1 Li1 85.4(3) . . ? Si1 N1 Li1 123.4(2) . . ? Li2 N1 Li1 87.8(3) . . ? C2 N2 Si2 125.2(3) . . ? C2 N2 Li2 88.4(3) . . ? Si2 N2 Li2 124.5(2) . . ? C2 N2 Li1 86.0(3) . . ? Si2 N2 Li1 131.6(3) . . ? Li2 N2 Li1 87.6(3) . . ? C16 N3 C15 108.6(6) . . ? C16 N3 C13 108.4(6) . . ? C15 N3 C13 108.4(5) . . ? C16 N3 Li1 113.4(4) . . ? C15 N3 Li1 113.7(4) . . ? C13 N3 Li1 104.1(4) . . ? C17 N4 C18 108.0(4) . . ? C17 N4 C14 109.3(5) . . ? C18 N4 C14 110.2(4) . . ? C17 N4 Li1 116.5(4) . . ? C18 N4 Li1 108.9(3) . . ? C14 N4 Li1 103.9(3) . . ? C21 N5 C22 109.6(5) . . ? C21 N5 C19 108.0(5) . . ? C22 N5 C19 109.6(4) . . ? C21 N5 Li2 115.3(4) . . ? C22 N5 Li2 111.3(4) . . ? C19 N5 Li2 102.7(3) . . ? C24 N6 C20 110.4(4) . . ? C24 N6 C23 108.1(4) . . ? C20 N6 C23 110.2(4) . . ? C24 N6 Li2 118.9(3) . . ? C20 N6 Li2 102.4(3) . . ? C23 N6 Li2 106.6(3) . . ? N1 C1 C6 125.5(3) . . ? N1 C1 C2 117.0(3) . . ? C6 C1 C2 117.5(3) . . ? N1 C1 Li1 59.3(2) . . ? C6 C1 Li1 140.8(3) . . ? C2 C1 Li1 72.9(3) . . ? N1 C1 Li2 56.3(2) . . ? C6 C1 Li2 146.5(3) . . ? C2 C1 Li2 72.3(2) . . ? Li1 C1 Li2 71.9(2) . . ? N2 C2 C3 125.7(3) . . ? N2 C2 C1 117.5(3) . . ? C3 C2 C1 116.9(3) . . ? N2 C2 Li1 58.9(2) . . ? C3 C2 Li1 143.2(3) . . ? C1 C2 Li1 72.0(2) . . ? N2 C2 Li2 57.0(2) . . ? C3 C2 Li2 144.1(3) . . ? C1 C2 Li2 73.3(2) . . ? Li1 C2 Li2 72.0(2) . . ? C4 C3 C2 123.0(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 119.3(4) . . ? C5 C6 C1 123.3(4) . . ? C14 C13 N3 115.3(5) . . ? C13 C14 N4 113.0(5) . . ? C20 C19 N5 114.4(4) . . ? C19 C20 N6 115.3(4) . . ? N1 Li1 N2 82.4(3) . . ? N1 Li1 N3 129.1(4) . . ? N2 Li1 N3 132.4(4) . . ? N1 Li1 N4 120.3(3) . . ? N2 Li1 N4 113.9(3) . . ? N3 Li1 N4 82.7(3) . . ? N1 Li1 C1 35.35(16) . . ? N2 Li1 C1 65.3(2) . . ? N3 Li1 C1 160.4(4) . . ? N4 Li1 C1 97.5(3) . . ? N1 Li1 C2 65.0(2) . . ? N2 Li1 C2 35.08(16) . . ? N3 Li1 C2 164.4(4) . . ? N4 Li1 C2 95.4(3) . . ? C1 Li1 C2 35.13(15) . . ? N1 Li1 Li2 45.8(2) . . ? N2 Li1 Li2 46.0(2) . . ? N3 Li1 Li2 127.7(3) . . ? N4 Li1 Li2 149.4(4) . . ? C1 Li1 Li2 55.1(2) . . ? C2 Li1 Li2 54.6(2) . . ? N1 Li2 N2 83.2(3) . . ? N1 Li2 N5 133.4(4) . . ? N2 Li2 N5 130.9(4) . . ? N1 Li2 N6 111.1(3) . . ? N2 Li2 N6 116.2(3) . . ? N5 Li2 N6 83.8(3) . . ? N1 Li2 C2 64.5(2) . . ? N2 Li2 C2 34.53(16) . . ? N5 Li2 C2 161.2(3) . . ? N6 Li2 C2 94.7(3) . . ? N1 Li2 C1 34.42(15) . . ? N2 Li2 C1 64.3(2) . . ? N5 Li2 C1 164.2(4) . . ? N6 Li2 C1 93.0(3) . . ? C2 Li2 C1 34.37(15) . . ? N1 Li2 Li1 46.4(2) . . ? N2 Li2 Li1 46.4(2) . . ? N5 Li2 Li1 131.1(3) . . ? N6 Li2 Li1 145.1(3) . . ? C2 Li2 Li1 53.4(2) . . ? C1 Li2 Li1 53.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.292 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.043 #===END data_mfl-6-jul1297 _database_code_CSD 168083 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H54 Li2 N6 Si2' _chemical_formula_weight 520.81 _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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' '-x, y, z' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 36.532(11) _cell_length_b 16.972(10) _cell_length_c 16.030(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9938.9(73) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method ? _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6301 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6301 _reflns_number_observed 4508 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1255P)^2^+16.9497P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(22) _refine_ls_number_reflns 6301 _refine_ls_number_parameters 502 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_obs 0.0743 _refine_ls_wR_factor_all 0.2234 _refine_ls_wR_factor_obs 0.1902 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_goodness_of_fit_obs 0.998 _refine_ls_restrained_S_all 0.982 _refine_ls_restrained_S_obs 0.998 _refine_ls_shift/esd_max -0.003 _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 Si1 Si 0.34430(4) 0.14283(9) -0.07400(11) 0.0392(4) Uani 1 d . . Si2 Si 0.32594(4) 0.38902(8) 0.20144(10) 0.0343(3) Uani 1 d . . Si3 Si 0.08434(4) 0.23982(10) 0.06543(11) 0.0377(4) Uani 1 d . . N1 N 0.34217(12) 0.2194(3) -0.0057(3) 0.0300(9) Uani 1 d . . N2 N 0.33464(11) 0.3283(2) 0.1191(3) 0.0262(8) Uani 1 d . . N3 N 0.36441(14) 0.1242(3) 0.2108(4) 0.0468(13) Uani 1 d . . N4 N 0.41943(12) 0.2254(3) 0.1305(3) 0.0398(11) Uani 1 d . . N5 N 0.24060(13) 0.2414(3) 0.0553(4) 0.0478(13) Uani 1 d . . N6 N 0.27127(14) 0.3636(3) -0.0550(3) 0.0428(12) Uani 1 d . . N7 N 0.03781(10) 0.2443(2) 0.0578(3) 0.0281(9) Uani 1 d . . N8 N 0.0000 0.2626(5) 0.2842(5) 0.047(2) Uani 1 d S . N9 N 0.0000 0.4030(4) 0.1787(5) 0.047(2) Uani 1 d S . N10 N 0.0000 0.0303(4) 0.0813(5) 0.049(2) Uani 1 d S . N11 N 0.0000 0.1012(4) -0.0843(5) 0.042(2) Uani 1 d S . C1 C 0.35805(14) 0.2932(3) -0.0181(3) 0.0281(10) Uani 1 d . . C2 C 0.35421(13) 0.3516(3) 0.0477(3) 0.0272(10) Uani 1 d . . C3 C 0.36947(15) 0.4258(3) 0.0342(4) 0.0356(12) Uani 1 d . . H3 H 0.36691(15) 0.4637(3) 0.0756(4) 0.043 Uiso 1 calc R . C4 C 0.3882(2) 0.4459(4) -0.0376(4) 0.0443(14) Uani 1 d . . H4 H 0.3981(2) 0.4961(4) -0.0432(4) 0.053 Uiso 1 calc R . C5 C 0.3922(2) 0.3919(4) -0.1005(4) 0.0479(15) Uani 1 d . . H5 H 0.4045(2) 0.4051(4) -0.1494(4) 0.057 Uiso 1 calc R . C6 C 0.3774(2) 0.3164(4) -0.0897(4) 0.0396(13) Uani 1 d . . H6 H 0.3805(2) 0.2798(4) -0.1322(4) 0.048 Uiso 1 calc R . C7 C 0.3912(2) 0.1078(4) -0.0981(6) 0.063(2) Uani 1 d . . H7 H 0.4060(2) 0.1419(4) -0.1286(6) 0.076 Uiso 1 calc R . C8 C 0.4059(2) 0.0396(5) -0.0766(8) 0.086(3) Uani 1 d . . H8B H 0.3923(2) 0.0033(5) -0.0461(8) 0.103 Uiso 1 calc R . H8A H 0.4298(2) 0.0278(5) -0.0921(8) 0.103 Uiso 1 calc R . C9 C 0.3243(3) 0.1594(6) -0.1810(6) 0.102(4) Uani 1 d . . H9C H 0.2996(3) 0.1780(6) -0.1757(6) 0.153 Uiso 1 calc R . H9B H 0.3244(3) 0.1107(6) -0.2116(6) 0.153 Uiso 1 calc R . H9A H 0.3386(3) 0.1979(6) -0.2102(6) 0.153 Uiso 1 calc R . C10 C 0.3193(3) 0.0568(5) -0.0306(8) 0.097(4) Uani 1 d . . H10C H 0.2947(3) 0.0720(5) -0.0171(8) 0.146 Uiso 1 calc R . H10B H 0.3315(3) 0.0387(5) 0.0188(8) 0.146 Uiso 1 calc R . H10A H 0.3188(3) 0.0153(5) -0.0713(8) 0.146 Uiso 1 calc R . C11 C 0.2945(2) 0.4733(4) 0.1746(4) 0.055(2) Uani 1 d . . H11 H 0.3038(2) 0.5122(4) 0.1397(4) 0.065 Uiso 1 calc R . C12 C 0.2601(3) 0.4823(6) 0.2011(6) 0.084(3) Uani 1 d . . H12B H 0.2497(3) 0.4448(6) 0.2361(6) 0.101 Uiso 1 calc R . H12A H 0.2466(3) 0.5260(6) 0.1845(6) 0.101 Uiso 1 calc R . C13 C 0.3658(2) 0.4353(5) 0.2558(5) 0.063(2) Uani 1 d . . H13C H 0.3796(2) 0.4662(5) 0.2167(5) 0.094 Uiso 1 calc R . H13B H 0.3812(2) 0.3948(5) 0.2787(5) 0.094 Uiso 1 calc R . H13A H 0.3571(2) 0.4686(5) 0.2999(5) 0.094 Uiso 1 calc R . C14 C 0.3024(2) 0.3319(5) 0.2849(4) 0.058(2) Uani 1 d . . H14C H 0.2813(2) 0.3060(5) 0.2619(4) 0.087 Uiso 1 calc R . H14B H 0.2948(2) 0.3670(5) 0.3285(4) 0.087 Uiso 1 calc R . H14A H 0.3188(2) 0.2932(5) 0.3073(4) 0.087 Uiso 1 calc R . C15 C 0.4016(2) 0.1249(6) 0.2341(7) 0.088(3) Uani 1 d . . H15B H 0.4088(2) 0.0706(6) 0.2433(7) 0.106 Uiso 1 calc R . H15A H 0.4031(2) 0.1513(6) 0.2877(7) 0.106 Uiso 1 calc R . C16 C 0.4286(2) 0.1594(6) 0.1818(8) 0.099(4) Uani 1 d . . H16B H 0.4377(2) 0.1183(6) 0.1454(8) 0.119 Uiso 1 calc R . H16A H 0.4488(2) 0.1753(6) 0.2173(8) 0.119 Uiso 1 calc R . C17 C 0.3576(5) 0.0470(6) 0.1666(10) 0.133(5) Uani 1 d . . H17C H 0.3733(5) 0.0433(6) 0.1187(10) 0.200 Uiso 1 calc R . H17B H 0.3325(5) 0.0444(6) 0.1491(10) 0.200 Uiso 1 calc R . H17A H 0.3628(5) 0.0041(6) 0.2039(10) 0.200 Uiso 1 calc R . C18 C 0.3417(5) 0.1277(11) 0.2789(9) 0.198(11) Uani 1 d . . H18C H 0.3166(5) 0.1271(11) 0.2607(9) 0.298 Uiso 1 calc R . H18B H 0.3463(5) 0.1753(11) 0.3094(9) 0.298 Uiso 1 calc R . H18A H 0.3461(5) 0.0830(11) 0.3143(9) 0.298 Uiso 1 calc R . C19 C 0.4291(3) 0.2964(5) 0.1754(11) 0.132(6) Uani 1 d . . H19C H 0.4232(3) 0.3416(5) 0.1421(11) 0.198 Uiso 1 calc R . H19B H 0.4548(3) 0.2962(5) 0.1872(11) 0.198 Uiso 1 calc R . H19A H 0.4156(3) 0.2985(5) 0.2268(11) 0.198 Uiso 1 calc R . C20 C 0.4395(2) 0.2259(11) 0.0537(7) 0.132(6) Uani 1 d . . H20C H 0.4326(2) 0.2711(11) 0.0213(7) 0.198 Uiso 1 calc R . H20B H 0.4343(2) 0.1788(11) 0.0229(7) 0.198 Uiso 1 calc R . H20A H 0.4653(2) 0.2283(11) 0.0655(7) 0.198 Uiso 1 calc R . C21 C 0.2189(2) 0.2870(7) -0.0048(8) 0.090(3) Uani 1 d . . H21B H 0.2143(2) 0.2534(7) -0.0526(8) 0.109 Uiso 1 calc R . H21A H 0.1954(2) 0.2977(7) 0.0208(8) 0.109 Uiso 1 calc R . C22 C 0.2322(2) 0.3567(7) -0.0341(8) 0.108(4) Uani 1 d . . H22B H 0.2268(2) 0.3968(7) 0.0073(8) 0.130 Uiso 1 calc R . H22A H 0.2184(2) 0.3701(7) -0.0838(8) 0.130 Uiso 1 calc R . C23 C 0.2334(3) 0.1602(6) 0.0321(8) 0.086(3) Uani 1 d . . H23C H 0.2412(3) 0.1516(6) -0.0244(8) 0.129 Uiso 1 calc R . H23B H 0.2077(3) 0.1498(6) 0.0367(8) 0.129 Uiso 1 calc R . H23A H 0.2466(3) 0.1256(6) 0.0686(8) 0.129 Uiso 1 calc R . C24 C 0.2297(3) 0.2591(8) 0.1390(6) 0.106(4) Uani 1 d . . H24C H 0.2351(3) 0.3133(8) 0.1511(6) 0.159 Uiso 1 calc R . H24B H 0.2429(3) 0.2258(8) 0.1770(6) 0.159 Uiso 1 calc R . H24A H 0.2039(3) 0.2500(8) 0.1451(6) 0.159 Uiso 1 calc R . C25 C 0.2783(3) 0.3394(6) -0.1375(5) 0.086(3) Uani 1 d . . H25C H 0.2718(3) 0.2849(6) -0.1437(5) 0.128 Uiso 1 calc R . H25B H 0.3038(3) 0.3461(6) -0.1498(5) 0.128 Uiso 1 calc R . H25A H 0.2640(3) 0.3706(6) -0.1754(5) 0.128 Uiso 1 calc R . C26 C 0.2811(3) 0.4449(5) -0.0474(6) 0.084(3) Uani 1 d . . H26C H 0.2765(3) 0.4623(5) 0.0086(6) 0.126 Uiso 1 calc R . H26B H 0.2668(3) 0.4756(5) -0.0856(6) 0.126 Uiso 1 calc R . H26A H 0.3066(3) 0.4512(5) -0.0601(6) 0.126 Uiso 1 calc R . C27 C 0.01988(13) 0.2917(3) -0.0004(3) 0.0272(10) Uani 1 d . . C28 C 0.03772(14) 0.3400(3) -0.0593(3) 0.0339(11) Uani 1 d . . H28 H 0.06317(14) 0.3408(3) -0.0601(3) 0.041 Uiso 1 calc R . C29 C 0.0187(2) 0.3867(3) -0.1165(4) 0.0379(12) Uani 1 d . . H29 H 0.0315(2) 0.4177(3) -0.1544(4) 0.045 Uiso 1 calc R . C30 C 0.0973(2) 0.1679(10) 0.1466(10) 0.158(8) Uani 1 d . . H30 H 0.0776(2) 0.1447(10) 0.1739(10) 0.190 Uiso 1 calc R . C31 C 0.1265(4) 0.1461(9) 0.1700(13) 0.159(7) Uani 1 d . . H31B H 0.1477(4) 0.1664(9) 0.1460(13) 0.190 Uiso 1 calc R . H31A H 0.1282(4) 0.1088(9) 0.2124(13) 0.190 Uiso 1 calc R . C32 C 0.1085(2) 0.3340(5) 0.0936(8) 0.083(3) Uani 1 d . . H32C H 0.1028(2) 0.3739(5) 0.0532(8) 0.124 Uiso 1 calc R . H32B H 0.1345(2) 0.3252(5) 0.0942(8) 0.124 Uiso 1 calc R . H32A H 0.1007(2) 0.3511(5) 0.1478(8) 0.124 Uiso 1 calc R . C33 C 0.1088(2) 0.2028(5) -0.0298(6) 0.068(2) Uani 1 d . . H33C H 0.1037(2) 0.2369(5) -0.0761(6) 0.101 Uiso 1 calc R . H33B H 0.1006(2) 0.1504(5) -0.0425(6) 0.101 Uiso 1 calc R . H33A H 0.1347(2) 0.2020(5) -0.0195(6) 0.101 Uiso 1 calc R . C34 C 0.0000 0.3419(7) 0.3189(7) 0.065(3) Uani 1 d S . H34A H -0.0214 0.3470(7) 0.3544(7) 0.077 Uiso 0.50 calc PR . H34B H 0.0214 0.3470(7) 0.3544(7) 0.077 Uiso 0.50 calc PR . C35 C 0.0000 0.4013(11) 0.2663(11) 0.301(28) Uani 1 d S . H35A H 0.0212 0.4325(11) 0.2821(11) 0.361 Uiso 0.50 calc PR . H35B H -0.0212 0.4325(11) 0.2821(11) 0.361 Uiso 0.50 calc PR . C36 C 0.0315(4) 0.2216(7) 0.3117(9) 0.143(7) Uani 1 d . . H36A H 0.0531(4) 0.2489(7) 0.2934(9) 0.215 Uiso 1 calc R . H36B H 0.0314(4) 0.1693(7) 0.2889(9) 0.215 Uiso 1 calc R . H36C H 0.0314(4) 0.2187(7) 0.3715(9) 0.215 Uiso 1 calc R . C37 C 0.0300(4) 0.4422(7) 0.1524(14) 0.205(12) Uani 1 d . . H37A H 0.0516(4) 0.4149(7) 0.1707(14) 0.308 Uiso 1 calc R . H37B H 0.0299(4) 0.4945(7) 0.1752(14) 0.308 Uiso 1 calc R . H37C H 0.0299(4) 0.4451(7) 0.0926(14) 0.308 Uiso 1 calc R . C38 C 0.0000 -0.0140(7) 0.0031(9) 0.089(4) Uani 1 d S . H38A H 0.0213 -0.0481(7) 0.0049(9) 0.107 Uiso 0.50 calc PR . H38B H -0.0213 -0.0481(7) 0.0049(9) 0.107 Uiso 0.50 calc PR . C39 C 0.0000 0.0181(12) -0.0697(11) 0.251(21) Uani 1 d S . H39A H -0.0213 -0.0026(12) -0.0985(11) 0.301 Uiso 0.50 calc PR . H39B H 0.0213 -0.0026(12) -0.0985(11) 0.301 Uiso 0.50 calc PR . C40 C 0.0318(5) 0.0135(9) 0.1266(11) 0.206(10) Uani 1 d . . H40A H 0.0529(5) 0.0259(9) 0.0934(11) 0.309 Uiso 1 calc R . H40B H 0.0322(5) -0.0415(9) 0.1409(11) 0.309 Uiso 1 calc R . H40C H 0.0322(5) 0.0445(9) 0.1767(11) 0.309 Uiso 1 calc R . C41 C -0.0318(3) 0.1197(9) -0.1264(9) 0.159(8) Uani 1 d . . H41A H -0.0525(3) 0.1050(9) -0.0930(9) 0.238 Uiso 1 calc R . H41B H -0.0325(3) 0.0916(9) -0.1783(9) 0.238 Uiso 1 calc R . H41C H -0.0325(3) 0.1753(9) -0.1370(9) 0.238 Uiso 1 calc R . Li1 Li 0.3600(2) 0.2192(5) 0.1174(6) 0.032(2) Uani 1 d . . Li2 Li 0.2971(2) 0.2812(5) 0.0355(6) 0.031(2) Uani 1 d . . Li3 Li 0.0000 0.2784(8) 0.1470(9) 0.037(3) Uani 1 d S . Li4 Li 0.0000 0.1557(7) 0.0388(8) 0.031(3) Uani 1 d S . 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 0.0392(8) 0.0365(7) 0.0419(9) -0.0158(7) -0.0057(7) 0.0084(6) Si2 0.0460(8) 0.0306(7) 0.0264(6) -0.0050(6) -0.0012(7) -0.0008(6) Si3 0.0197(6) 0.0461(8) 0.0474(9) 0.0061(8) -0.0005(6) 0.0010(6) N1 0.030(2) 0.028(2) 0.031(2) -0.009(2) 0.001(2) 0.001(2) N2 0.032(2) 0.025(2) 0.022(2) -0.003(2) -0.001(2) 0.001(2) N3 0.041(3) 0.042(3) 0.057(3) 0.018(3) 0.001(3) 0.003(2) N4 0.031(2) 0.047(3) 0.041(3) 0.012(2) -0.010(2) -0.004(2) N5 0.036(2) 0.055(3) 0.052(3) -0.004(3) 0.003(2) -0.004(2) N6 0.042(3) 0.040(2) 0.046(3) 0.000(2) -0.007(2) 0.010(2) N7 0.017(2) 0.030(2) 0.037(2) 0.003(2) 0.002(2) -0.001(2) N8 0.050(4) 0.056(4) 0.035(4) -0.013(4) 0.000 0.000 N9 0.060(5) 0.029(3) 0.054(5) -0.010(3) 0.000 0.000 N10 0.060(5) 0.032(3) 0.056(5) 0.011(3) 0.000 0.000 N11 0.043(4) 0.046(4) 0.036(4) -0.006(3) 0.000 0.000 C1 0.029(2) 0.029(2) 0.027(2) 0.003(2) -0.003(2) 0.002(2) C2 0.027(2) 0.027(2) 0.027(2) 0.001(2) -0.004(2) 0.002(2) C3 0.033(3) 0.031(3) 0.043(3) 0.000(2) -0.004(2) -0.002(2) C4 0.045(3) 0.037(3) 0.051(4) 0.011(3) 0.001(3) -0.003(2) C5 0.049(3) 0.053(4) 0.042(3) 0.017(3) 0.009(3) 0.006(3) C6 0.042(3) 0.046(3) 0.031(3) 0.003(2) 0.006(2) 0.008(3) C7 0.057(4) 0.045(4) 0.087(6) -0.010(4) 0.018(4) 0.010(3) C8 0.070(5) 0.068(5) 0.120(8) -0.025(6) -0.003(6) 0.030(4) C9 0.146(9) 0.091(6) 0.069(6) -0.046(5) -0.065(6) 0.061(6) C10 0.103(7) 0.056(5) 0.134(9) -0.045(6) 0.039(7) -0.036(5) C11 0.077(5) 0.047(4) 0.039(3) -0.005(3) 0.009(3) 0.020(3) C12 0.091(6) 0.091(7) 0.071(5) -0.022(5) 0.011(5) 0.028(5) C13 0.066(5) 0.075(5) 0.047(4) -0.022(4) -0.015(3) -0.014(4) C14 0.074(5) 0.064(4) 0.035(3) -0.001(3) 0.016(3) -0.006(4) C15 0.055(4) 0.113(7) 0.097(7) 0.075(6) -0.019(4) 0.001(5) C16 0.039(3) 0.095(6) 0.163(11) 0.087(7) -0.010(5) 0.003(4) C17 0.188(13) 0.068(6) 0.143(12) 0.000(8) -0.009(11) -0.050(8) C18 0.231(17) 0.246(19) 0.119(11) 0.134(13) 0.109(12) 0.170(16) C19 0.092(7) 0.062(5) 0.243(18) -0.042(8) -0.085(10) 0.000(5) C20 0.041(4) 0.286(19) 0.069(6) 0.020(9) 0.008(4) 0.041(7) C21 0.031(3) 0.115(8) 0.125(9) 0.046(7) -0.010(5) 0.002(4) C22 0.034(4) 0.143(10) 0.147(11) 0.078(9) -0.007(5) 0.022(5) C23 0.060(5) 0.083(6) 0.115(8) -0.020(6) 0.006(5) -0.014(4) C24 0.068(6) 0.187(12) 0.064(6) -0.042(7) 0.027(5) -0.036(7) C25 0.119(8) 0.091(7) 0.046(4) -0.013(4) -0.025(5) 0.056(6) C26 0.111(7) 0.052(4) 0.089(7) -0.002(4) -0.046(6) 0.021(5) C27 0.025(2) 0.029(2) 0.028(2) 0.003(2) -0.001(2) -0.002(2) C28 0.029(2) 0.035(3) 0.038(3) 0.008(2) 0.001(2) -0.001(2) C29 0.039(3) 0.035(3) 0.039(3) 0.010(2) 0.009(2) -0.004(2) C30 0.033(4) 0.253(17) 0.188(14) 0.161(14) -0.002(6) 0.023(7) C31 0.101(9) 0.161(13) 0.214(18) 0.081(13) 0.014(12) -0.009(9) C32 0.042(4) 0.070(5) 0.137(9) -0.039(6) -0.019(5) 0.002(3) C33 0.033(3) 0.083(5) 0.086(6) -0.035(5) 0.007(4) 0.005(3) C34 0.063(6) 0.088(8) 0.042(5) -0.026(6) 0.000 0.000 C35 0.797(89) 0.061(10) 0.044(9) -0.028(8) 0.000 0.000 C36 0.168(12) 0.113(9) 0.148(12) -0.057(9) -0.117(10) 0.077(9) C37 0.129(10) 0.099(8) 0.389(30) -0.140(14) 0.151(15) -0.072(8) C38 0.147(13) 0.037(6) 0.083(10) 0.005(6) 0.000 0.000 C39 0.615(68) 0.084(13) 0.054(10) -0.046(10) 0.000 0.000 C40 0.266(18) 0.143(12) 0.208(17) -0.058(12) -0.169(16) 0.139(13) C41 0.098(8) 0.214(15) 0.163(13) -0.129(12) -0.088(9) 0.085(9) Li1 0.029(4) 0.031(4) 0.036(5) 0.000(4) -0.003(4) -0.004(3) Li2 0.025(4) 0.042(5) 0.028(4) -0.005(4) 0.000(3) 0.000(3) Li3 0.026(6) 0.041(7) 0.043(8) -0.001(6) 0.000 0.000 Li4 0.039(6) 0.026(6) 0.027(6) 0.000(5) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.701(4) . ? Si1 C7 1.855(7) . ? Si1 C10 1.856(9) . ? Si1 C9 1.886(8) . ? Si2 N2 1.704(4) . ? Si2 C14 1.863(7) . ? Si2 C13 1.869(7) . ? Si2 C11 1.883(7) . ? Si3 N7 1.706(4) . ? Si3 C30 1.845(10) . ? Si3 C33 1.877(8) . ? Si3 C32 1.882(8) . ? N1 C1 1.395(7) . ? N1 Li2 2.062(9) . ? N1 Li1 2.078(11) . ? N2 C2 1.406(6) . ? N2 Li1 2.072(10) . ? N2 Li2 2.078(9) . ? N3 C18 1.374(12) . ? N3 C15 1.408(9) . ? N3 C17 1.511(12) . ? N3 Li1 2.206(10) . ? N4 C16 1.429(9) . ? N4 C20 1.433(11) . ? N4 C19 1.449(11) . ? N4 Li1 2.183(9) . ? N5 C24 1.431(11) . ? N5 C23 1.452(11) . ? N5 C21 1.468(11) . ? N5 Li2 2.193(10) . ? N6 C25 1.409(10) . ? N6 C26 1.430(10) . ? N6 C22 1.470(10) . ? N6 Li2 2.225(11) . ? N7 C27 1.396(6) . ? N7 Li4 2.064(10) . ? N7 Li3 2.070(11) . ? N8 C36 1.417(10) 3 ? N8 C36 1.417(10) . ? N8 C34 1.456(13) . ? N8 Li3 2.22(2) . ? N9 C37 1.350(11) . ? N9 C37 1.350(11) 3 ? N9 C35 1.40(2) . ? N9 Li3 2.18(2) . ? N10 C40 1.401(12) . ? N10 C40 1.401(12) 3 ? N10 C38 1.46(2) . ? N10 Li4 2.235(14) . ? N11 C41 1.379(10) . ? N11 C41 1.379(10) 3 ? N11 C39 1.43(2) . ? N11 Li4 2.179(14) . ? C1 C6 1.403(7) . ? C1 C2 1.454(7) . ? C1 Li2 2.397(10) . ? C1 Li1 2.511(10) . ? C2 C3 1.394(7) . ? C2 Li2 2.413(10) . ? C2 Li1 2.518(10) . ? C3 C4 1.381(9) . ? C4 C5 1.370(10) . ? C5 C6 1.402(9) . ? C7 C8 1.322(11) . ? C11 C12 1.335(11) . ? C15 C16 1.420(12) . ? C21 C22 1.363(13) . ? C27 C28 1.410(7) . ? C27 C27 1.452(9) 3 ? C27 Li3 2.482(15) . ? C27 Li4 2.499(13) . ? C28 C29 1.396(8) . ? C29 C29 1.369(11) 3 ? C30 C31 1.19(2) . ? C34 C35 1.31(2) . ? C38 C39 1.29(2) . ? Li1 Li2 2.850(12) . ? Li3 N7 2.070(11) 3 ? Li3 C27 2.482(15) 3 ? Li3 Li4 2.71(2) . ? Li4 N7 2.064(10) 3 ? Li4 C27 2.499(13) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C7 114.9(3) . . ? N1 Si1 C10 109.7(4) . . ? C7 Si1 C10 106.3(4) . . ? N1 Si1 C9 117.0(3) . . ? C7 Si1 C9 102.5(5) . . ? C10 Si1 C9 105.5(6) . . ? N2 Si2 C14 109.1(3) . . ? N2 Si2 C13 118.0(3) . . ? C14 Si2 C13 104.1(4) . . ? N2 Si2 C11 113.3(3) . . ? C14 Si2 C11 106.1(4) . . ? C13 Si2 C11 105.2(4) . . ? N7 Si3 C30 109.6(3) . . ? N7 Si3 C33 115.5(3) . . ? C30 Si3 C33 103.3(6) . . ? N7 Si3 C32 116.6(3) . . ? C30 Si3 C32 105.8(7) . . ? C33 Si3 C32 104.9(4) . . ? C1 N1 Si1 125.1(4) . . ? C1 N1 Li2 85.5(4) . . ? Si1 N1 Li2 129.1(3) . . ? C1 N1 Li1 90.4(4) . . ? Si1 N1 Li1 126.5(3) . . ? Li2 N1 Li1 87.0(4) . . ? C2 N2 Si2 123.8(3) . . ? C2 N2 Li1 90.7(4) . . ? Si2 N2 Li1 129.4(4) . . ? C2 N2 Li2 85.4(4) . . ? Si2 N2 Li2 127.5(3) . . ? Li1 N2 Li2 86.7(4) . . ? C18 N3 C15 111.9(10) . . ? C18 N3 C17 108.1(12) . . ? C15 N3 C17 106.9(9) . . ? C18 N3 Li1 117.7(6) . . ? C15 N3 Li1 104.1(5) . . ? C17 N3 Li1 107.7(7) . . ? C16 N4 C20 112.3(8) . . ? C16 N4 C19 107.9(8) . . ? C20 N4 C19 107.3(10) . . ? C16 N4 Li1 104.5(5) . . ? C20 N4 Li1 115.3(5) . . ? C19 N4 Li1 109.3(6) . . ? C24 N5 C23 112.9(8) . . ? C24 N5 C21 110.8(8) . . ? C23 N5 C21 103.6(8) . . ? C24 N5 Li2 109.4(5) . . ? C23 N5 Li2 115.2(5) . . ? C21 N5 Li2 104.5(5) . . ? C25 N6 C26 108.4(8) . . ? C25 N6 C22 111.5(8) . . ? C26 N6 C22 107.5(8) . . ? C25 N6 Li2 110.6(5) . . ? C26 N6 Li2 116.4(5) . . ? C22 N6 Li2 102.2(5) . . ? C27 N7 Si3 122.8(3) . . ? C27 N7 Li4 90.4(4) . . ? Si3 N7 Li4 130.2(3) . . ? C27 N7 Li3 89.3(4) . . ? Si3 N7 Li3 128.9(4) . . ? Li4 N7 Li3 81.9(4) . . ? C36 N8 C36 108.8(16) 3 . ? C36 N8 C34 109.6(6) 3 . ? C36 N8 C34 109.6(6) . . ? C36 N8 Li3 111.6(8) 3 . ? C36 N8 Li3 111.6(8) . . ? C34 N8 Li3 105.6(7) . . ? C37 N9 C37 108.6(19) . 3 ? C37 N9 C35 108.8(11) . . ? C37 N9 C35 108.8(11) 3 . ? C37 N9 Li3 114.0(6) . . ? C37 N9 Li3 114.0(6) 3 . ? C35 N9 Li3 102.4(9) . . ? C40 N10 C40 112.3(19) . 3 ? C40 N10 C38 109.9(8) . . ? C40 N10 C38 109.9(8) 3 . ? C40 N10 Li4 110.7(8) . . ? C40 N10 Li4 110.7(8) 3 . ? C38 N10 Li4 103.2(7) . . ? C41 N11 C41 114.7(17) . 3 ? C41 N11 C39 107.7(8) . . ? C41 N11 C39 107.7(8) 3 . ? C41 N11 Li4 110.2(6) . . ? C41 N11 Li4 110.2(6) 3 . ? C39 N11 Li4 105.7(9) . . ? N1 C1 C6 125.3(5) . . ? N1 C1 C2 117.9(4) . . ? C6 C1 C2 116.8(5) . . ? N1 C1 Li2 59.1(3) . . ? C6 C1 Li2 141.7(4) . . ? C2 C1 Li2 73.0(3) . . ? N1 C1 Li1 55.9(3) . . ? C6 C1 Li1 146.4(4) . . ? C2 C1 Li1 73.5(3) . . ? Li2 C1 Li1 71.0(3) . . ? C3 C2 N2 125.7(5) . . ? C3 C2 C1 117.6(5) . . ? N2 C2 C1 116.7(4) . . ? C3 C2 Li2 141.3(4) . . ? N2 C2 Li2 59.1(3) . . ? C1 C2 Li2 71.8(3) . . ? C3 C2 Li1 147.3(4) . . ? N2 C2 Li1 55.4(3) . . ? C1 C2 Li1 72.9(3) . . ? Li2 C2 Li1 70.6(3) . . ? C4 C3 C2 123.4(5) . . ? C5 C4 C3 120.1(5) . . ? C4 C5 C6 118.6(6) . . ? C5 C6 C1 123.5(6) . . ? C8 C7 Si1 127.0(7) . . ? C12 C11 Si2 126.0(7) . . ? N3 C15 C16 121.2(7) . . ? C15 C16 N4 120.0(6) . . ? C22 C21 N5 119.4(7) . . ? C21 C22 N6 119.6(8) . . ? N7 C27 C28 124.5(4) . . ? N7 C27 C27 118.0(2) . 3 ? C28 C27 C27 117.5(3) . 3 ? N7 C27 Li3 56.5(3) . . ? C28 C27 Li3 145.6(5) . . ? C27 C27 Li3 72.99(15) 3 . ? N7 C27 Li4 55.7(3) . . ? C28 C27 Li4 147.1(5) . . ? C27 C27 Li4 73.10(13) 3 . ? Li3 C27 Li4 65.9(4) . . ? C29 C28 C27 122.7(5) . . ? C29 C29 C28 119.8(3) 3 . ? C31 C30 Si3 131.1(11) . . ? C35 C34 N8 117.6(10) . . ? C34 C35 N9 131.1(13) . . ? C39 C38 N10 124.1(11) . . ? C38 C39 N11 124.5(12) . . ? N2 Li1 N1 82.6(4) . . ? N2 Li1 N4 113.6(4) . . ? N1 Li1 N4 113.8(4) . . ? N2 Li1 N3 132.6(5) . . ? N1 Li1 N3 132.0(5) . . ? N4 Li1 N3 84.1(4) . . ? N2 Li1 C1 63.3(3) . . ? N1 Li1 C1 33.7(2) . . ? N4 Li1 C1 95.0(4) . . ? N3 Li1 C1 162.8(5) . . ? N2 Li1 C2 33.9(2) . . ? N1 Li1 C2 63.3(3) . . ? N4 Li1 C2 94.8(3) . . ? N3 Li1 C2 163.5(5) . . ? C1 Li1 C2 33.6(2) . . ? N2 Li1 Li2 46.7(3) . . ? N1 Li1 Li2 46.3(3) . . ? N4 Li1 Li2 146.0(5) . . ? N3 Li1 Li2 129.9(4) . . ? C1 Li1 Li2 52.7(3) . . ? C2 Li1 Li2 53.0(3) . . ? N1 Li2 N2 82.8(3) . . ? N1 Li2 N5 129.9(5) . . ? N2 Li2 N5 130.3(5) . . ? N1 Li2 N6 116.7(4) . . ? N2 Li2 N6 117.3(5) . . ? N5 Li2 N6 83.7(4) . . ? N1 Li2 C1 35.5(2) . . ? N2 Li2 C1 65.4(3) . . ? N5 Li2 C1 162.2(5) . . ? N6 Li2 C1 96.1(4) . . ? N1 Li2 C2 65.6(3) . . ? N2 Li2 C2 35.5(2) . . ? N5 Li2 C2 162.6(5) . . ? N6 Li2 C2 96.2(4) . . ? C1 Li2 C2 35.2(2) . . ? N1 Li2 Li1 46.7(3) . . ? N2 Li2 Li1 46.5(3) . . ? N5 Li2 Li1 125.4(5) . . ? N6 Li2 Li1 151.0(4) . . ? C1 Li2 Li1 56.4(3) . . ? C2 Li2 Li1 56.4(3) . . ? N7 Li3 N7 83.7(6) . 3 ? N7 Li3 N9 115.7(5) . . ? N7 Li3 N9 115.7(5) 3 . ? N7 Li3 N8 130.7(5) . . ? N7 Li3 N8 130.7(5) 3 . ? N9 Li3 N8 83.4(6) . . ? N7 Li3 C27 64.1(4) . 3 ? N7 Li3 C27 34.2(3) 3 3 ? N9 Li3 C27 97.7(6) . 3 ? N8 Li3 C27 162.9(2) . 3 ? N7 Li3 C27 34.2(3) . . ? N7 Li3 C27 64.1(4) 3 . ? N9 Li3 C27 97.7(6) . . ? N8 Li3 C27 162.9(2) . . ? C27 Li3 C27 34.0(3) 3 . ? N7 Li3 Li4 49.0(3) . . ? N7 Li3 Li4 49.0(3) 3 . ? N9 Li3 Li4 153.7(7) . . ? N8 Li3 Li4 122.9(7) . . ? C27 Li3 Li4 57.3(4) 3 . ? C27 Li3 Li4 57.3(4) . . ? N7 Li4 N7 84.0(5) . 3 ? N7 Li4 N11 116.3(5) . . ? N7 Li4 N11 116.3(5) 3 . ? N7 Li4 N10 130.4(4) . . ? N7 Li4 N10 130.4(4) 3 . ? N11 Li4 N10 82.6(5) . . ? N7 Li4 C27 34.0(2) . . ? N7 Li4 C27 63.9(4) 3 . ? N11 Li4 C27 99.5(5) . . ? N10 Li4 C27 162.9(2) . . ? N7 Li4 C27 63.9(4) . 3 ? N7 Li4 C27 34.0(2) 3 3 ? N11 Li4 C27 99.5(5) . 3 ? N10 Li4 C27 162.9(2) . 3 ? C27 Li4 C27 33.8(3) . 3 ? N7 Li4 Li3 49.2(3) . . ? N7 Li4 Li3 49.2(3) 3 . ? N11 Li4 Li3 155.0(7) . . ? N10 Li4 Li3 122.4(6) . . ? C27 Li4 Li3 56.8(4) . . ? C27 Li4 Li3 56.8(4) 3 . ? _refine_diff_density_max 0.708 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.066 #===END The following crystal structures have been deposited at the Cambridge Crystallographic Data Centre and allocated the deposition numbers CCDC 168078 - 168083 If we have any queries relating to these data then we will contact you later. Summary of Data CCDC 168078 --------------- Authors: S.Bott,S.Daniele,C.Drost,B.Gehrhus,S.M.Hawkins,P.B.Hitchcock, M.Lappert,P.G.Merle Journal: J.Chem.Soc.,Dalton Trans. (0186) Compound: ((Li2(C6H4(NSiMe3)2))2) Unit cell parameters: a 15.7489(7) b 13.7919(4) c 14.8525(5) space group Cmcm Summary of Data CCDC 168079 --------------- Authors: S.Bott,S.Daniele,C.Drost,B.Gehrhus,S.M.Hawkins,P.B.Hitchcock, M.Lappert,P.G.Merle Journal: J.Chem.Soc.,Dalton Trans. (0186) Compound: ((Li2(thf)2(C6H4(NSiMe3)2))2) Unit cell parameters: a 10.7906(7) b 17.7715(9) c 25.8104(14) space group Pbca Summary of Data CCDC 168080 --------------- Authors: S.Bott,S.Daniele,C.Drost,B.Gehrhus,S.M.Hawkins,P.B.Hitchcock, M.Lappert,P.G.Merle Journal: J.Chem.Soc.,Dalton Trans. (0186) Compound: ((Me3SiNC6H4NSiMe3)Li2(thf)3) Unit cell parameters: a 17.8015(7) b 27.9629(9) c 23.7088(5) space group Pbca Summary of Data CCDC 168081 --------------- Authors: S.Bott,S.Daniele,C.Drost,B.Gehrhus,S.M.Hawkins,P.B.Hitchcock, M.Lappert,P.G.Merle Journal: J.Chem.Soc.,Dalton Trans. (0186) Compound: (C6H4(N(SiMe3)Li(tmeda))2) Unit cell parameters: a 9.813(5) b 16.812(3) c 10.872(2) beta 116.20(3) space group P21 Summary of Data CCDC 168083 --------------- Authors: S.Bott,S.Daniele,C.Drost,B.Gehrhus,S.M.Hawkins,P.B.Hitchcock, M.Lappert,P.G.Merle Journal: J.Chem.Soc.,Dalton Trans. (0186) Compound: C26 H54 Li2 N6 Si2 Unit cell parameters: a 36.532(11) b 16.972(10) c 16.030(5) alpha 90.00 beta 90.00 gamma 90.00 space group Cmc21 Any publication carrying these CCDC numbers will refer to the most recent set of deposited data; previous depositions carrying these numbers will not be retained. Best wishes Jenny Field CCDC field@ccdc.cam.ac.uk 12 Union Road Tel +44 (0)1223 762093 Cambridge CB2 1EZ Fax +44 (0)1223 336033 UK http://www.ccdc.cam.ac.uk/ data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bott,S.' 'Daniele, S.' 'Drost, C.' 'Gehrhus, B.' 'Hawkins, S.M.' 'Hitchcock, P.B.' 'Lappert, M.' 'Merle, P.G.' _publ_contact_author_name 'Prof M. Lappert' _publ_contact_author_address ; Prof M Lappert School of Chemistry & Molecular Science University of Sussex BRIGHTON BN1 9QJ U.K. ; _publ_contact_author_email 'M.F.LAPPERT@SUSSEX.AC.UK' data_mfl-1-jun800 _database_code_CSD 168078 _audit_creation_date 2000-06-06T14:30:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{Li2(C6H4(NSiMe3)2)}2]' _chemical_formula_moiety 'C24 H44 Li4 N4 Si4' _chemical_formula_structural 'C24 H44 LI4 N4 SI4' _chemical_formula_sum 'C24 H44 Li4 N4 Si4' _chemical_formula_weight 528.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmcm _symmetry_space_group_name_Hall '-C 2c 2c' _symmetry_Int_Tables_number 63 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y, z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.7489(7) _cell_length_b 13.7919(4) _cell_length_c 14.8525(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3226.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5281 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_T_min 0.9512 _exptl_absorpt_correction_T_max 0.9703 #----------------------------------------------------------------------------# # 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 10357 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.82 _diffrn_reflns_theta_full 27.82 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2054 _reflns_number_gt 1655 _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^)+(0.0494P)^2^+2.4913P] 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_number_reflns 2054 _refine_ls_number_parameters 103 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.354 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' 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' 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 Li1 Li 0.0848(3) 0.2162(3) 0.75 0.0324(8) Uani 1 2 d S . . Li2 Li 0 0.1096(2) 0.8407(3) 0.0305(8) Uani 1 2 d S . . Si1 Si 0 0.25865(4) 0.53970(4) 0.03160(19) Uani 1 2 d S . . Si2 Si 0.19809(4) 0.06707(5) 0.75 0.0444(2) Uani 1 2 d S . . N1 N 0.08874(11) 0.06492(11) 0.75 0.0254(4) Uani 1 2 d S . . N2 N 0 0.26050(11) 0.65581(11) 0.0280(4) Uani 1 2 d S . . C1 C 0.04574(12) -0.02581(13) 0.75 0.0206(4) Uani 1 2 d S . . C2 C 0.08703(13) -0.11579(14) 0.75 0.0260(4) Uani 1 2 d S . . H2 H 0.1473 -0.1168 0.75 0.031 Uiso 1 2 calc SR . . C3 C 0.04388(14) -0.20338(15) 0.75 0.0297(5) Uani 1 2 d S . . H3 H 0.0743 -0.2628 0.75 0.036 Uiso 1 2 calc SR . . C4 C 0.24762(14) 0.01403(18) 0.64710(19) 0.0769(8) Uani 1 1 d . . . H4A H 0.2214 0.0425 0.5934 0.115 Uiso 1 1 calc R . . H4B H 0.2388 -0.0563 0.6468 0.115 Uiso 1 1 calc R . . H4C H 0.3086 0.028 0.6471 0.115 Uiso 1 1 calc R . . C5 C 0.22780(19) 0.2006(2) 0.75 0.0805(12) Uani 1 2 d S . . H5A H 0.2036 0.232 0.6967 0.121 Uiso 0.5 1 calc PR . . H5B H 0.2898 0.207 0.7488 0.121 Uiso 1 2 calc SR . . H5C H 0.2054 0.2315 0.8044 0.121 Uiso 0.5 1 calc PR . . C6 C 0 0.35132(14) 0.70162(14) 0.0254(4) Uani 1 2 d S . . C7 C 0 0.44127(15) 0.65756(15) 0.0324(5) Uani 1 2 d S . . H7 H 0 0.4422 0.5936 0.039 Uiso 1 2 calc SR . . C8 C 0 0.52907(15) 0.70354(16) 0.0351(5) Uani 1 2 d S . . H8 H 0 0.5886 0.6713 0.042 Uiso 1 2 calc SR . . C9 C -0.09835(13) 0.31100(14) 0.48827(12) 0.0488(5) Uani 1 1 d . . . H10A H -0.1485 0.2821 0.5167 0.073 Uiso 1 1 calc R . . H10B H -0.0991 0.297 0.4236 0.073 Uiso 1 1 calc R . . H10C H -0.099 0.3813 0.4976 0.073 Uiso 1 1 calc R . . C10 C 0 0.12682(18) 0.50646(17) 0.0489(7) Uani 1 2 d S . . H9A H -0.0503 0.0949 0.5315 0.073 Uiso 0.5 1 calc PR . . H9B H 0.0513 0.0954 0.5299 0.073 Uiso 0.5 1 calc PR . . H9C H -0.0009 0.1215 0.4407 0.073 Uiso 1 2 calc SR . . 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 Li1 0.036(2) 0.0270(18) 0.034(2) 0 0 -0.0003(16) Li2 0.036(2) 0.0235(17) 0.0318(19) -0.0011(14) 0 0 Si1 0.0487(4) 0.0242(3) 0.0219(3) 0.0003(2) 0 0 Si2 0.0202(3) 0.0314(4) 0.0815(6) 0 0 -0.0038(3) N1 0.0214(8) 0.0186(8) 0.0362(10) 0 0 -0.0029(7) N2 0.0444(11) 0.0186(8) 0.0209(8) -0.0004(6) 0 0 C1 0.0226(10) 0.0183(9) 0.0210(9) 0 0 -0.0009(7) C2 0.0222(10) 0.0238(10) 0.0320(11) 0 0 0.0022(8) C3 0.0342(12) 0.0187(9) 0.0362(12) 0 0 0.0049(9) C4 0.0506(13) 0.0650(15) 0.115(2) 0.0041(13) 0.0447(14) 0.0025(12) C5 0.0312(15) 0.0418(16) 0.169(4) 0 0 -0.0172(13) C6 0.0302(11) 0.0188(9) 0.0271(10) -0.0012(8) 0 0 C7 0.0476(14) 0.0229(10) 0.0269(11) 0.0034(8) 0 0 C8 0.0477(14) 0.0187(10) 0.0389(12) 0.0044(9) 0 0 C9 0.0591(12) 0.0517(11) 0.0356(10) 0.0043(8) -0.0092(9) 0.0034(9) C10 0.085(2) 0.0321(13) 0.0292(12) -0.0063(10) 0 0 #----------------------------------------------------------------------------# # 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 Li1 N2 2.028(3) . ? Li1 N2 2.028(3) 10_557 ? Li1 N1 2.087(4) . ? Li2 N1 2.036(3) 11 ? Li2 N1 2.036(3) . ? Li2 N2 2.082(4) 10_557 ? Si1 N2 1.7247(18) . ? Si1 C9 1.8719(19) . ? Si1 C9 1.8719(19) 11 ? Si1 C10 1.884(2) . ? Si2 N1 1.7223(19) . ? Si2 C4 1.865(2) 10_557 ? Si2 C4 1.865(2) . ? Si2 C5 1.900(3) . ? N1 C1 1.423(2) . ? N1 Li2 2.036(3) 10_557 ? N2 C6 1.426(2) . ? N2 Li1 2.028(3) 11 ? N2 Li2 2.082(4) 10_557 ? C1 C2 1.401(3) . ? C1 C1 1.441(4) 11 ? C2 C3 1.386(3) . ? C3 C3 1.382(4) 11 ? C6 C7 1.403(3) . ? C6 C6 1.437(4) 10_557 ? C7 C8 1.390(3) . ? C8 C8 1.380(5) 10_557 ? 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 Li1 N2 87.22(17) . 10_557 ? N2 Li1 N1 108.72(15) . . ? N2 Li1 N1 108.72(15) 10_557 . ? N1 Li2 N1 86.68(16) 11 . ? N1 Li2 N2 108.59(14) 11 10_557 ? N1 Li2 N2 108.59(14) . 10_557 ? N2 Si1 C9 113.72(7) . . ? N2 Si1 C9 113.72(7) . 11 ? C9 Si1 C9 111.68(13) . 11 ? N2 Si1 C10 106.03(10) . . ? C9 Si1 C10 105.38(8) . . ? C9 Si1 C10 105.38(8) 11 . ? N1 Si2 C4 114.29(8) . 10_557 ? N1 Si2 C4 114.29(8) . . ? C4 Si2 C4 110.04(17) 10_557 . ? N1 Si2 C5 105.25(11) . . ? C4 Si2 C5 106.08(9) 10_557 . ? C4 Si2 C5 106.08(9) . . ? C1 N1 Si2 119.41(13) . . ? C1 N1 Li2 86.51(12) . . ? Si2 N1 Li2 132.92(9) . . ? C1 N1 Li2 86.51(12) . 10_557 ? Si2 N1 Li2 132.92(9) . 10_557 ? Li2 N1 Li2 82.83(18) . 10_557 ? C1 N1 Li1 149.86(17) . . ? Si2 N1 Li1 90.73(13) . . ? Li2 N1 Li1 71.17(13) . . ? Li2 N1 Li1 71.17(13) 10_557 . ? C6 N2 Si1 119.35(13) . . ? C6 N2 Li1 86.31(13) . 11 ? Si1 N2 Li1 133.25(9) . 11 ? C6 N2 Li1 86.31(13) . . ? Si1 N2 Li1 133.25(9) . . ? Li1 N2 Li1 82.35(19) 11 . ? C6 N2 Li2 150.06(17) . 10_557 ? Si1 N2 Li2 90.58(13) . 10_557 ? Li1 N2 Li2 71.43(13) 11 10_557 ? Li1 N2 Li2 71.43(13) . 10_557 ? C2 C1 N1 123.92(18) . . ? C2 C1 C1 117.66(12) . 11 ? N1 C1 C1 118.43(10) . 11 ? C3 C2 C1 122.98(19) . . ? C3 C3 C2 119.36(12) 11 . ? C7 C6 N2 123.68(19) . . ? C7 C6 C6 117.81(12) . 10_557 ? N2 C6 C6 118.51(11) . 10_557 ? C8 C7 C6 122.8(2) . . ? C8 C8 C7 119.42(13) 10_557 . ? #===END data_mfl-2-feb600 _database_code_CSD 168079 _audit_creation_date 2000-02-07T14:15:26-00:00 _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 '[{Li2(thf)2(C6H4(NSiMe3)2)}2]' _chemical_formula_moiety 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_structural 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_sum 'C40 H76 Li4 N4 O4 Si4' _chemical_formula_weight 817.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7906(7) _cell_length_b 17.7715(9) _cell_length_c 25.8104(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4949.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 48384 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9921 #----------------------------------------------------------------------------# # 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 23361 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2994 _reflns_number_gt 2190 _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 ; The crystal diffracted poorly . The O1 thf group is disordered and modelled as two alternative sets of ring C atoms with bond length constraints applied(SADI). 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^)+(0.1004P)^2^+13.5296P] 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_number_reflns 2994 _refine_ls_number_parameters 249 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.114 _refine_ls_R_factor_gt 0.087 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2168 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.593 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # 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' 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' O O 0.0106 0.006 '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 Li1 Li 0.4308(10) 0.5756(5) 0.3545(4) 0.067(3) Uani 1 1 d . A . Li2 Li 0.5112(8) 0.5285(4) 0.4443(3) 0.049(2) Uani 1 1 d . . . Si1 Si 0.50626(17) 0.72205(8) 0.41658(7) 0.0614(6) Uani 1 1 d . A . Si2 Si 0.5055(2) 0.40179(8) 0.34077(6) 0.0695(7) Uani 1 1 d . A . O1 O 0.3051(5) 0.6047(3) 0.30724(19) 0.0871(15) Uani 1 1 d D . . O2 O 0.6295(3) 0.50332(17) 0.50589(14) 0.0479(10) Uani 1 1 d . . . N1 N 0.5338(4) 0.6292(2) 0.40514(19) 0.0549(13) Uani 1 1 d . . . N2 N 0.5325(5) 0.4863(2) 0.36979(18) 0.0557(13) Uani 1 1 d . . . C1 C 0.6489(5) 0.5983(3) 0.3924(2) 0.0505(14) Uani 1 1 d . A . C2 C 0.6492(6) 0.5211(3) 0.3733(2) 0.0523(15) Uani 1 1 d . A . C3 C 0.7645(7) 0.4881(3) 0.3618(2) 0.0726(19) Uani 1 1 d . . . H3 H 0.7659 0.4375 0.35 0.087 Uiso 1 1 calc R A . C4 C 0.8753(7) 0.5257(4) 0.3669(3) 0.086(2) Uani 1 1 d . A . H4 H 0.9512 0.5017 0.3584 0.104 Uiso 1 1 calc R . . C5 C 0.8742(6) 0.5984(4) 0.3844(3) 0.078(2) Uani 1 1 d . . . H5 H 0.9502 0.6248 0.3882 0.093 Uiso 1 1 calc R A . C6 C 0.7635(6) 0.6340(3) 0.3969(2) 0.0636(17) Uani 1 1 d . A . H6 H 0.7659 0.6846 0.4088 0.076 Uiso 1 1 calc R . . C7 C 0.3363(8) 0.7349(4) 0.4241(5) 0.165(6) Uani 1 1 d . . . H7A H 0.2938 0.7152 0.3934 0.247 Uiso 1 1 calc R A . H7B H 0.3176 0.7886 0.4279 0.247 Uiso 1 1 calc R . . H7C H 0.3078 0.7078 0.4549 0.247 Uiso 1 1 calc R . . C8 C 0.5569(7) 0.7851(3) 0.3631(3) 0.079(2) Uani 1 1 d . . . H8A H 0.5214 0.7675 0.3303 0.119 Uiso 1 1 calc R A . H8B H 0.6475 0.7846 0.3607 0.119 Uiso 1 1 calc R . . H8C H 0.5284 0.8365 0.37 0.119 Uiso 1 1 calc R . . C9 C 0.5785(12) 0.7607(4) 0.4760(3) 0.148(5) Uani 1 1 d . . . H9A H 0.555 0.7298 0.5058 0.222 Uiso 1 1 calc R A . H9B H 0.5498 0.8125 0.4814 0.222 Uiso 1 1 calc R . . H9C H 0.6688 0.7605 0.4722 0.222 Uiso 1 1 calc R . . C10 C 0.3345(8) 0.3926(4) 0.3321(3) 0.106(3) Uani 1 1 d . . . H10A H 0.3035 0.4353 0.3119 0.158 Uiso 1 1 calc R A . H10B H 0.2941 0.3918 0.3661 0.158 Uiso 1 1 calc R . . H10C H 0.3162 0.3457 0.3136 0.158 Uiso 1 1 calc R . . C11 C 0.5749(13) 0.3932(5) 0.2740(3) 0.164(5) Uani 1 1 d . . . H11A H 0.6653 0.3973 0.2764 0.246 Uiso 1 1 calc R A . H11B H 0.5428 0.4336 0.2519 0.246 Uiso 1 1 calc R . . H11C H 0.5527 0.3444 0.2591 0.246 Uiso 1 1 calc R . . C12 C 0.5572(8) 0.3187(3) 0.3798(3) 0.088(2) Uani 1 1 d . . . H12A H 0.6471 0.3212 0.385 0.132 Uiso 1 1 calc R A . H12B H 0.5363 0.2722 0.3613 0.132 Uiso 1 1 calc R . . H12C H 0.5153 0.3191 0.4135 0.132 Uiso 1 1 calc R . . C17 C 0.7160(5) 0.4413(3) 0.4973(3) 0.0599(16) Uani 1 1 d . . . H17A H 0.6802 0.393 0.5091 0.072 Uiso 1 1 calc R . . H17B H 0.7379 0.4371 0.4601 0.072 Uiso 1 1 calc R . . C18 C 0.8243(7) 0.4616(4) 0.5282(5) 0.136(4) Uani 1 1 d . . . H18A H 0.8213 0.4352 0.562 0.163 Uiso 1 1 calc R . . H18B H 0.9008 0.446 0.51 0.163 Uiso 1 1 calc R . . C19 C 0.8261(6) 0.5402(4) 0.5365(4) 0.095(2) Uani 1 1 d . . . H19A H 0.8881 0.5643 0.5136 0.114 Uiso 1 1 calc R . . H19B H 0.8479 0.5514 0.5729 0.114 Uiso 1 1 calc R . . C20 C 0.7003(5) 0.5685(3) 0.5245(2) 0.0542(15) Uani 1 1 d . . . H20A H 0.6612 0.5899 0.5559 0.065 Uiso 1 1 calc R . . H20B H 0.7041 0.608 0.4975 0.065 Uiso 1 1 calc R . . C13 C 0.1788(14) 0.5715(10) 0.3026(7) 0.119(6) Uiso 0.5 1 d PD A 1 H13C H 0.1859 0.5171 0.2951 0.143 Uiso 0.5 1 calc PR A 1 H13D H 0.1345 0.5772 0.336 0.143 Uiso 0.5 1 calc PR A 1 C14 C 0.1069(15) 0.6083(7) 0.2612(6) 0.088(4) Uiso 0.5 1 d PD A 1 H14C H 0.0169 0.6079 0.2684 0.105 Uiso 0.5 1 calc PR A 1 H14D H 0.123 0.5855 0.2269 0.105 Uiso 0.5 1 calc PR A 1 C15 C 0.1605(12) 0.6849(7) 0.2656(6) 0.073(4) Uiso 0.5 1 d PD A 1 H15C H 0.1402 0.7096 0.2989 0.088 Uiso 0.5 1 calc PR A 1 H15D H 0.137 0.7179 0.2363 0.088 Uiso 0.5 1 calc PR A 1 C16 C 0.2980(17) 0.6584(13) 0.2626(8) 0.148(8) Uiso 0.5 1 d PD A 1 H16C H 0.3158 0.6328 0.2294 0.178 Uiso 0.5 1 calc PR A 1 H16D H 0.356 0.701 0.2671 0.178 Uiso 0.5 1 calc PR A 1 C13B C 0.245(2) 0.5711(12) 0.2635(8) 0.159(9) Uiso 0.5 1 d PD A 2 H13A H 0.1855 0.532 0.2743 0.19 Uiso 0.5 1 calc PR A 2 H13B H 0.3064 0.5488 0.2393 0.19 Uiso 0.5 1 calc PR A 2 C14B C 0.181(2) 0.6380(12) 0.2395(9) 0.142(7) Uiso 0.5 1 d PD A 2 H14A H 0.1907 0.6377 0.2014 0.171 Uiso 0.5 1 calc PR A 2 H14B H 0.0909 0.6371 0.2477 0.171 Uiso 0.5 1 calc PR A 2 C15B C 0.239(4) 0.7046(17) 0.2620(11) 0.231(15) Uiso 0.5 1 d PD A 2 H15A H 0.1897 0.7509 0.257 0.277 Uiso 0.5 1 calc PR A 2 H15B H 0.325 0.7123 0.2496 0.277 Uiso 0.5 1 calc PR A 2 C16B C 0.233(3) 0.6753(12) 0.3164(11) 0.196(11) Uiso 0.5 1 d PD A 2 H16A H 0.2749 0.7092 0.3414 0.235 Uiso 0.5 1 calc PR A 2 H16B H 0.1474 0.6651 0.3278 0.235 Uiso 0.5 1 calc PR A 2 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 Li1 0.074(7) 0.040(5) 0.088(7) 0.003(5) -0.014(6) 0.002(5) Li2 0.053(6) 0.034(4) 0.060(5) -0.003(4) 0.001(4) -0.002(4) Si1 0.0819(13) 0.0282(9) 0.0741(12) -0.0009(7) 0.0132(10) -0.0011(7) Si2 0.1247(17) 0.0345(9) 0.0492(10) -0.0046(7) -0.0009(10) -0.0121(9) O1 0.097(4) 0.072(3) 0.093(3) 0.011(2) -0.026(3) 0.001(3) O2 0.0350(19) 0.0362(19) 0.072(2) -0.0027(16) -0.0028(17) -0.0016(16) N1 0.054(3) 0.028(2) 0.082(3) -0.007(2) 0.012(2) -0.004(2) N2 0.074(4) 0.032(2) 0.060(3) -0.006(2) -0.003(2) -0.001(2) C1 0.057(4) 0.039(3) 0.055(3) 0.000(2) 0.010(3) -0.005(3) C2 0.071(4) 0.037(3) 0.048(3) -0.001(2) 0.006(3) 0.003(3) C3 0.094(5) 0.049(4) 0.075(4) 0.001(3) 0.029(4) 0.014(4) C4 0.074(5) 0.072(5) 0.114(6) 0.022(4) 0.042(4) 0.011(4) C5 0.054(4) 0.080(5) 0.099(5) 0.020(4) 0.022(4) -0.016(4) C6 0.061(4) 0.052(3) 0.078(4) 0.006(3) 0.016(3) -0.012(3) C7 0.102(7) 0.047(4) 0.344(17) 0.036(7) 0.095(9) 0.024(4) C8 0.084(5) 0.062(4) 0.091(5) 0.024(4) -0.008(4) -0.007(4) C9 0.315(15) 0.056(4) 0.074(5) -0.023(4) -0.043(7) 0.047(7) C10 0.154(8) 0.056(4) 0.106(6) 0.006(4) -0.070(6) -0.024(4) C11 0.310(16) 0.118(7) 0.063(5) -0.037(5) 0.057(7) -0.095(9) C12 0.113(6) 0.040(3) 0.111(6) 0.009(3) 0.014(5) 0.008(4) C17 0.050(4) 0.045(3) 0.085(4) 0.003(3) 0.007(3) 0.009(3) C18 0.061(5) 0.083(6) 0.264(13) -0.025(7) -0.069(7) 0.020(4) C19 0.050(5) 0.086(5) 0.149(7) -0.018(5) -0.020(4) 0.000(4) C20 0.044(3) 0.046(3) 0.073(4) -0.001(3) -0.010(3) -0.012(3) #----------------------------------------------------------------------------# # 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 Li1 O1 1.897(11) . ? Li1 N1 1.962(11) . ? Li1 N2 1.968(10) . ? Li1 C1 2.580(12) . ? Li1 C2 2.593(12) . ? Li1 Li2 2.613(14) . ? Li1 Si1 3.163(10) . ? Li2 O2 2.067(9) 5_666 ? Li2 N1 2.070(9) . ? Li2 N2 2.077(10) . ? Li2 O2 2.086(10) . ? Li2 C1 2.354(10) . ? Li2 C2 2.365(11) . ? Li2 Li2 3.056(18) 5_666 ? Si1 N1 1.702(4) . ? Si1 C9 1.853(8) . ? Si1 C7 1.859(8) . ? Si1 C8 1.861(6) . ? Si2 N2 1.704(4) . ? Si2 C10 1.865(9) . ? Si2 C12 1.873(6) . ? Si2 C11 1.884(8) . ? O1 C13B 1.431(15) . ? O1 C13 1.490(14) . ? O1 C16B 1.492(16) . ? O1 C16 1.496(15) . ? O2 C17 1.462(6) . ? O2 C20 1.468(6) . ? O2 Li2 2.067(10) 5_666 ? N1 C1 1.397(7) . ? N2 C2 1.405(7) . ? C1 C6 1.395(8) . ? C1 C2 1.458(7) . ? C2 C3 1.407(9) . ? C3 C4 1.377(10) . ? C4 C5 1.368(10) . ? C5 C6 1.390(9) . ? C17 C18 1.461(9) . ? C18 C19 1.412(10) . ? C19 C20 1.480(8) . ? C13 C14 1.474(15) . ? C14 C15 1.483(14) . ? C15 C16 1.558(15) . ? C13B C14B 1.513(16) . ? C14B C15B 1.461(17) . ? C15B C16B 1.499(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 Li1 N1 134.5(5) . . ? O1 Li1 N2 138.4(6) . . ? N1 Li1 N2 86.7(5) . . ? O1 Li1 C1 148.6(5) . . ? N1 Li1 C1 32.3(2) . . ? N2 Li1 C1 62.7(3) . . ? O1 Li1 C2 150.7(6) . . ? N1 Li1 C2 62.8(3) . . ? N2 Li1 C2 32.4(2) . . ? C1 Li1 C2 32.7(2) . . ? O1 Li1 Li2 153.6(6) . . ? N1 Li1 Li2 51.5(3) . . ? N2 Li1 Li2 51.6(3) . . ? C1 Li1 Li2 53.9(3) . . ? C2 Li1 Li2 54.0(3) . . ? O1 Li1 Si1 106.5(4) . . ? N1 Li1 Si1 28.03(19) . . ? N2 Li1 Si1 114.7(4) . . ? C1 Li1 Si1 56.3(2) . . ? C2 Li1 Si1 88.8(3) . . ? Li2 Li1 Si1 74.3(3) . . ? O2 Li2 N1 128.8(5) 5_666 . ? O2 Li2 N2 123.9(4) 5_666 . ? N1 Li2 N2 81.1(4) . . ? O2 Li2 O2 85.2(4) 5_666 . ? N1 Li2 O2 119.1(4) . . ? N2 Li2 O2 124.1(4) . . ? O2 Li2 C1 164.0(4) 5_666 . ? N1 Li2 C1 36.1(2) . . ? N2 Li2 C1 66.0(3) . . ? O2 Li2 C1 99.2(4) . . ? O2 Li2 C2 158.2(4) 5_666 . ? N1 Li2 C2 66.1(3) . . ? N2 Li2 C2 36.2(2) . . ? O2 Li2 C2 101.2(4) . . ? C1 Li2 C2 36.0(2) . . ? O2 Li2 Li1 113.3(5) 5_666 . ? N1 Li2 Li1 47.8(3) . . ? N2 Li2 Li1 48.0(3) . . ? O2 Li2 Li1 161.3(5) . . ? C1 Li2 Li1 62.3(3) . . ? C2 Li2 Li1 62.6(4) . . ? O2 Li2 Li2 42.9(2) 5_666 5_666 ? N1 Li2 Li2 139.0(5) . 5_666 ? N2 Li2 Li2 139.5(5) . 5_666 ? O2 Li2 Li2 42.4(2) . 5_666 ? C1 Li2 Li2 139.4(5) . 5_666 ? C2 Li2 Li2 139.5(5) . 5_666 ? Li1 Li2 Li2 156.0(6) . 5_666 ? N1 Si1 C9 115.5(3) . . ? N1 Si1 C7 108.0(3) . . ? C9 Si1 C7 106.4(6) . . ? N1 Si1 C8 113.8(3) . . ? C9 Si1 C8 105.5(4) . . ? C7 Si1 C8 107.0(4) . . ? N1 Si1 Li1 32.8(2) . . ? C9 Si1 Li1 146.4(3) . . ? C7 Si1 Li1 84.3(4) . . ? C8 Si1 Li1 101.3(3) . . ? N2 Si2 C10 107.4(3) . . ? N2 Si2 C12 114.1(3) . . ? C10 Si2 C12 106.9(3) . . ? N2 Si2 C11 113.9(3) . . ? C10 Si2 C11 106.0(5) . . ? C12 Si2 C11 108.0(4) . . ? C13B O1 C13 50.2(11) . . ? C13B O1 C16B 104.1(15) . . ? C13 O1 C16B 82.6(14) . . ? C13B O1 C16 68.7(13) . . ? C13 O1 C16 98.3(11) . . ? C16B O1 C16 63.9(14) . . ? C13B O1 Li1 135.7(9) . . ? C13 O1 Li1 126.7(8) . . ? C16B O1 Li1 119.9(12) . . ? C16 O1 Li1 134.9(9) . . ? C17 O2 C20 108.1(4) . . ? C17 O2 Li2 111.0(4) . 5_666 ? C20 O2 Li2 113.2(4) . 5_666 ? C17 O2 Li2 115.9(4) . . ? C20 O2 Li2 113.5(4) . . ? Li2 O2 Li2 94.8(4) 5_666 . ? C1 N1 Si1 125.2(3) . . ? C1 N1 Li1 99.0(4) . . ? Si1 N1 Li1 119.2(4) . . ? C1 N1 Li2 83.1(4) . . ? Si1 N1 Li2 137.1(4) . . ? Li1 N1 Li2 80.7(4) . . ? C2 N2 Si2 124.7(4) . . ? C2 N2 Li1 99.1(4) . . ? Si2 N2 Li1 121.8(4) . . ? C2 N2 Li2 83.1(4) . . ? Si2 N2 Li2 134.9(3) . . ? Li1 N2 Li2 80.4(4) . . ? C6 C1 N1 126.1(5) . . ? C6 C1 C2 117.0(5) . . ? N1 C1 C2 116.8(5) . . ? C6 C1 Li2 138.8(5) . . ? N1 C1 Li2 60.8(3) . . ? C2 C1 Li2 72.4(4) . . ? C6 C1 Li1 155.6(5) . . ? N1 C1 Li1 48.7(3) . . ? C2 C1 Li1 74.1(4) . . ? Li2 C1 Li1 63.8(3) . . ? N2 C2 C3 126.5(5) . . ? N2 C2 C1 115.7(5) . . ? C3 C2 C1 117.7(6) . . ? N2 C2 Li2 60.7(3) . . ? C3 C2 Li2 138.0(5) . . ? C1 C2 Li2 71.6(4) . . ? N2 C2 Li1 48.5(3) . . ? C3 C2 Li1 156.9(5) . . ? C1 C2 Li1 73.2(4) . . ? Li2 C2 Li1 63.4(4) . . ? C4 C3 C2 123.1(6) . . ? C5 C4 C3 118.8(6) . . ? C4 C5 C6 120.9(6) . . ? C5 C6 C1 122.4(6) . . ? C18 C17 O2 104.0(5) . . ? C19 C18 C17 109.7(6) . . ? C18 C19 C20 107.0(6) . . ? O2 C20 C19 106.1(5) . . ? C14 C13 O1 111.3(12) . . ? C13 C14 C15 98.4(12) . . ? C14 C15 C16 95.1(13) . . ? O1 C16 C15 101.8(11) . . ? O1 C13B C14B 101.7(14) . . ? C15B C14B C13B 106(2) . . ? C14B C15B C16B 94(2) . . ? O1 C16B C15B 97(2) . . ? #===END data_mfl-3-jan700 _database_code_CSD 168080 _audit_creation_date 2000-01-13T15:35:53-00:00 _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 '[(Me3SiNC6H4NSiMe3)Li2(thf)3]' _chemical_formula_moiety 'C24 H46 Li2 N2 O3 Si2' _chemical_formula_structural 'C24 H46 N2 LI2 SI2 O3' _chemical_formula_sum 'C24 H46 Li2 N2 O3 Si2' _chemical_formula_weight 480.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2bc 2ac' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8015(7) _cell_length_b 27.9629(9) _cell_length_c 23.7088(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 11801.8(6) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23421 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.145 #----------------------------------------------------------------------------# # 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 36417 _diffrn_reflns_av_R_equivalents 0.0939 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 21.94 _diffrn_reflns_theta_full 21.94 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 7079 _reflns_number_gt 5069 _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^)+(0.0605P)^2^+16.2025P] 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_number_reflns 7079 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.158 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.406 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # 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' 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' 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 Si1 Si 0.31264(6) 0.24031(4) 0.12301(5) 0.0410(3) Uani 1 1 d . . . Si2 Si 0.27991(7) 0.27399(4) -0.12452(5) 0.0472(3) Uani 1 1 d . . . O1 O 0.22608(16) 0.13808(10) -0.01261(12) 0.0516(8) Uani 1 1 d . . . O2 O 0.12839(16) 0.22752(10) 0.00462(12) 0.0534(8) Uani 1 1 d . . . O3 O 0.25587(18) 0.35555(10) 0.02012(13) 0.0608(9) Uani 1 1 d . . . N1 N 0.30986(17) 0.23637(11) 0.05173(12) 0.0367(8) Uani 1 1 d . . . N2 N 0.29385(19) 0.25048(11) -0.05969(13) 0.0424(8) Uani 1 1 d . . . C1 C 0.3643(2) 0.21497(13) 0.01688(16) 0.0367(9) Uani 1 1 d . . . C2 C 0.3552(2) 0.22254(13) -0.04280(16) 0.0389(10) Uani 1 1 d . . . C3 C 0.4061(2) 0.20043(15) -0.07919(17) 0.0483(11) Uani 1 1 d . . . H3 H 0.4003 0.2048 -0.1187 0.058 Uiso 1 1 calc R . . C4 C 0.4652(3) 0.17226(16) -0.0597(2) 0.0568(12) Uani 1 1 d . . . H4 H 0.4992 0.1581 -0.0857 0.068 Uiso 1 1 calc R . . C5 C 0.4741(2) 0.16501(15) -0.0027(2) 0.0534(12) Uani 1 1 d . . . H5 H 0.5143 0.1458 0.0109 0.064 Uiso 1 1 calc R . . C6 C 0.4235(2) 0.18618(14) 0.03517(18) 0.0457(11) Uani 1 1 d . . . H6 H 0.4297 0.1807 0.0744 0.055 Uiso 1 1 calc R . . C7 C 0.2349(2) 0.28222(15) 0.14416(16) 0.0485(11) Uani 1 1 d . . . H7A H 0.1869 0.2702 0.1296 0.073 Uiso 1 1 calc R . . H7B H 0.2447 0.314 0.1284 0.073 Uiso 1 1 calc R . . H7C H 0.2325 0.2843 0.1854 0.073 Uiso 1 1 calc R . . C8 C 0.2968(3) 0.18202(16) 0.16061(18) 0.0585(12) Uani 1 1 d . . . H8A H 0.3366 0.1594 0.1504 0.088 Uiso 1 1 calc R . . H8B H 0.248 0.1688 0.1496 0.088 Uiso 1 1 calc R . . H8C H 0.2976 0.1874 0.2014 0.088 Uiso 1 1 calc R . . C9 C 0.4010(3) 0.26702(18) 0.15276(18) 0.0649(13) Uani 1 1 d . . . H9A H 0.4439 0.2466 0.1431 0.097 Uiso 1 1 calc R . . H9B H 0.3967 0.2694 0.1939 0.097 Uiso 1 1 calc R . . H9C H 0.4086 0.299 0.1368 0.097 Uiso 1 1 calc R . . C10 C 0.2008(3) 0.31795(17) -0.11844(19) 0.0651(13) Uani 1 1 d . . . H10A H 0.2128 0.3416 -0.0893 0.098 Uiso 1 1 calc R . . H10B H 0.1546 0.301 -0.1082 0.098 Uiso 1 1 calc R . . H10C H 0.1938 0.3342 -0.1547 0.098 Uiso 1 1 calc R . . C11 C 0.2525(3) 0.23057(17) -0.18080(18) 0.0677(14) Uani 1 1 d . . . H11A H 0.2925 0.2068 -0.1856 0.102 Uiso 1 1 calc R . . H11B H 0.2447 0.2477 -0.2164 0.102 Uiso 1 1 calc R . . H11C H 0.2058 0.2144 -0.1699 0.102 Uiso 1 1 calc R . . C12 C 0.3632(3) 0.30770(18) -0.1526(2) 0.0698(14) Uani 1 1 d . . . H12A H 0.38 0.331 -0.1244 0.105 Uiso 1 1 calc R . . H12B H 0.3491 0.3244 -0.1873 0.105 Uiso 1 1 calc R . . H12C H 0.4041 0.2852 -0.1606 0.105 Uiso 1 1 calc R . . C13 C 0.2690(3) 0.10522(16) 0.02131(19) 0.0582(12) Uani 1 1 d . . . H13A H 0.2362 0.0887 0.0488 0.07 Uiso 1 1 calc R . . H13B H 0.3091 0.1222 0.0421 0.07 Uiso 1 1 calc R . . C14 C 0.3019(3) 0.07040(19) -0.0197(2) 0.0823(17) Uani 1 1 d . . . H14A H 0.3515 0.0815 -0.0333 0.099 Uiso 1 1 calc R . . H14B H 0.3077 0.0384 -0.0022 0.099 Uiso 1 1 calc R . . C15 C 0.2462(3) 0.06903(18) -0.0664(2) 0.0689(14) Uani 1 1 d . . . H15A H 0.2698 0.0589 -0.1023 0.083 Uiso 1 1 calc R . . H15B H 0.2038 0.0474 -0.0576 0.083 Uiso 1 1 calc R . . C16 C 0.2215(3) 0.11963(17) -0.0688(2) 0.0742(15) Uani 1 1 d . . . H16A H 0.2545 0.1382 -0.0944 0.089 Uiso 1 1 calc R . . H16B H 0.1693 0.1217 -0.083 0.089 Uiso 1 1 calc R . . C17 C 0.0887(3) 0.2108(2) 0.0533(2) 0.0750(15) Uani 1 1 d . . . H17A H 0.0635 0.2377 0.0728 0.09 Uiso 1 1 calc R . . H17B H 0.1234 0.195 0.08 0.09 Uiso 1 1 calc R . . C18 C 0.0322(4) 0.1760(3) 0.0314(3) 0.114(2) Uani 1 1 d . . . H18A H 0.0522 0.143 0.0338 0.137 Uiso 1 1 calc R . . H18B H -0.0146 0.1777 0.0538 0.137 Uiso 1 1 calc R . . C19 C 0.0177(3) 0.1884(2) -0.0258(2) 0.0818(17) Uani 1 1 d . . . H19A H -0.0327 0.2032 -0.0295 0.098 Uiso 1 1 calc R . . H19B H 0.0196 0.1596 -0.0501 0.098 Uiso 1 1 calc R . . C20 C 0.0781(3) 0.22366(17) -0.04294(19) 0.0630(13) Uani 1 1 d . . . H20A H 0.1054 0.212 -0.0766 0.076 Uiso 1 1 calc R . . H20B H 0.0557 0.2552 -0.0518 0.076 Uiso 1 1 calc R . . C21 C 0.1933(3) 0.38419(16) 0.0380(2) 0.0603(13) Uani 1 1 d . . . H21A H 0.1709 0.3712 0.073 0.072 Uiso 1 1 calc R . . H21B H 0.1541 0.3854 0.0084 0.072 Uiso 1 1 calc R . . C22 C 0.2261(3) 0.43304(19) 0.0481(3) 0.0831(17) Uani 1 1 d . . . H22A H 0.1886 0.4585 0.0412 0.1 Uiso 1 1 calc R . . H22B H 0.2457 0.4361 0.0871 0.1 Uiso 1 1 calc R . . C23 C 0.2884(3) 0.4348(2) 0.0057(3) 0.0934(19) Uani 1 1 d . . . H23A H 0.2691 0.4433 -0.0322 0.112 Uiso 1 1 calc R . . H23B H 0.3273 0.4583 0.0169 0.112 Uiso 1 1 calc R . . C24 C 0.3182(3) 0.38607(19) 0.0065(3) 0.0949(19) Uani 1 1 d . . . H24A H 0.3393 0.3775 -0.0309 0.114 Uiso 1 1 calc R . . H24B H 0.3583 0.383 0.0352 0.114 Uiso 1 1 calc R . . Li1 Li 0.2328(4) 0.2068(2) -0.0043(3) 0.0452(17) Uani 1 1 d . . . Li2 Li 0.2688(5) 0.2891(2) 0.0073(3) 0.060(2) Uani 1 1 d . . . Si1B Si 0.00854(7) 0.01445(4) 0.37567(4) 0.0414(3) Uani 1 1 d . . . Si2B Si 0.01628(7) 0.00617(4) 0.12082(5) 0.0460(3) Uani 1 1 d . . . O1B O -0.10386(16) -0.08347(9) 0.25470(12) 0.0526(8) Uani 1 1 d . . . O2B O -0.16087(15) 0.01977(9) 0.24546(12) 0.0501(7) Uani 1 1 d . . . O3B O 0.03620(16) 0.11934(9) 0.24281(11) 0.0505(7) Uani 1 1 d . . . N1B N 0.01446(17) 0.00181(10) 0.30565(12) 0.0363(8) Uani 1 1 d . . . N2B N 0.01826(17) -0.00153(11) 0.19183(12) 0.0353(8) Uani 1 1 d . . . C1B C 0.0622(2) -0.03265(13) 0.28135(16) 0.0359(9) Uani 1 1 d . . . C2B C 0.0636(2) -0.03435(13) 0.22067(16) 0.0362(9) Uani 1 1 d . . . C3B C 0.1106(2) -0.06853(14) 0.19540(17) 0.0441(10) Uani 1 1 d . . . H3B H 0.1134 -0.0697 0.1554 0.053 Uiso 1 1 calc R . . C4B C 0.1534(2) -0.10075(14) 0.2268(2) 0.0525(12) Uani 1 1 d . . . H4B H 0.1843 -0.1236 0.2082 0.063 Uiso 1 1 calc R . . C5B C 0.1505(2) -0.09930(15) 0.2843(2) 0.0556(12) Uani 1 1 d . . . H5B H 0.179 -0.1214 0.306 0.067 Uiso 1 1 calc R . . C6B C 0.1059(2) -0.06542(14) 0.31117(17) 0.0459(10) Uani 1 1 d . . . H6B H 0.1052 -0.0646 0.3512 0.055 Uiso 1 1 calc R . . C7B C -0.0679(3) 0.05941(17) 0.38513(19) 0.0639(13) Uani 1 1 d . . . H7B1 H -0.0578 0.0873 0.3613 0.096 Uiso 1 1 calc R . . H7B2 H -0.0699 0.0694 0.4247 0.096 Uiso 1 1 calc R . . H7B3 H -0.1161 0.0452 0.3743 0.096 Uiso 1 1 calc R . . C8B C -0.0178(3) -0.03634(16) 0.42355(17) 0.0602(13) Uani 1 1 d . . . H8B1 H 0.0202 -0.0615 0.421 0.09 Uiso 1 1 calc R . . H8B2 H -0.0667 -0.0492 0.4122 0.09 Uiso 1 1 calc R . . H8B3 H -0.0208 -0.0248 0.4625 0.09 Uiso 1 1 calc R . . C9B C 0.0969(3) 0.04141(16) 0.40465(18) 0.0593(13) Uani 1 1 d . . . H9B1 H 0.1383 0.0186 0.4005 0.089 Uiso 1 1 calc R . . H9B2 H 0.0898 0.049 0.4447 0.089 Uiso 1 1 calc R . . H9B3 H 0.1087 0.0708 0.3839 0.089 Uiso 1 1 calc R . . C10B C -0.0578(3) 0.05148(19) 0.10418(19) 0.0716(15) Uani 1 1 d . . . H10D H -0.1063 0.0404 0.1187 0.107 Uiso 1 1 calc R . . H10E H -0.061 0.0557 0.0632 0.107 Uiso 1 1 calc R . . H10F H -0.0447 0.082 0.1219 0.107 Uiso 1 1 calc R . . C11B C -0.0088(3) -0.04817(18) 0.07747(18) 0.0664(14) Uani 1 1 d . . . H11D H 0.0281 -0.0735 0.0843 0.1 Uiso 1 1 calc R . . H11E H -0.0086 -0.0397 0.0374 0.1 Uiso 1 1 calc R . . H11F H -0.0589 -0.0595 0.0882 0.1 Uiso 1 1 calc R . . C12B C 0.1068(3) 0.03059(17) 0.09156(19) 0.0669(14) Uani 1 1 d . . . H12D H 0.1476 0.0079 0.099 0.1 Uiso 1 1 calc R . . H12E H 0.1182 0.0612 0.1097 0.1 Uiso 1 1 calc R . . H12F H 0.1017 0.0353 0.0508 0.1 Uiso 1 1 calc R . . C13B C -0.0841(4) -0.11709(19) 0.2987(2) 0.0824(18) Uani 1 1 d . . . H13C H -0.1292 -0.1271 0.3201 0.099 Uiso 1 1 calc R . . H13D H -0.0475 -0.1028 0.3252 0.099 Uiso 1 1 calc R . . C14B C -0.0502(5) -0.1586(2) 0.2683(3) 0.116(3) Uani 1 1 d . . . H14C H 0.0045 -0.1604 0.2758 0.14 Uiso 1 1 calc R . . H14D H -0.0737 -0.1889 0.2807 0.14 Uiso 1 1 calc R . . C15B C -0.0638(4) -0.1508(3) 0.2094(4) 0.118(3) Uani 1 1 d . . . H15C H -0.0161 -0.1441 0.1894 0.141 Uiso 1 1 calc R . . H15D H -0.0875 -0.1793 0.1922 0.141 Uiso 1 1 calc R . . C16B C -0.1126(4) -0.1109(2) 0.2058(2) 0.098(2) Uani 1 1 d . . . H16C H -0.1002 -0.0915 0.1722 0.118 Uiso 1 1 calc R . . H16D H -0.1653 -0.1218 0.2025 0.118 Uiso 1 1 calc R . . C17B C -0.1674(3) 0.06963(19) 0.2385(3) 0.099(2) Uani 1 1 d . . . H17C H -0.1376 0.0805 0.2057 0.119 Uiso 1 1 calc R . . H17D H -0.1492 0.0865 0.2726 0.119 Uiso 1 1 calc R . . C18B C -0.2478(4) 0.0792(3) 0.2295(3) 0.125(3) Uani 1 1 d . . . H18C H -0.2622 0.1106 0.2455 0.15 Uiso 1 1 calc R . . H18D H -0.2602 0.0789 0.1888 0.15 Uiso 1 1 calc R . . C19B C -0.2827(4) 0.0430(2) 0.2569(6) 0.230(7) Uani 1 1 d . . . H19C H -0.3288 0.0336 0.2364 0.276 Uiso 1 1 calc R . . H19D H -0.2972 0.0534 0.2954 0.276 Uiso 1 1 calc R . . C20B C -0.2296(3) 0.0017(2) 0.2603(5) 0.183(5) Uani 1 1 d . . . H20C H -0.2282 -0.0115 0.299 0.219 Uiso 1 1 calc R . . H20D H -0.245 -0.024 0.2339 0.219 Uiso 1 1 calc R . . C21B C 0.0201(3) 0.15365(16) 0.2858(2) 0.0720(15) Uani 1 1 d . . . H21C H 0.0472 0.1455 0.321 0.086 Uiso 1 1 calc R . . H21D H -0.0344 0.1543 0.294 0.086 Uiso 1 1 calc R . . C22B C 0.0456(3) 0.20158(17) 0.2640(2) 0.0772(16) Uani 1 1 d . . . H22C H 0.0023 0.2207 0.2507 0.093 Uiso 1 1 calc R . . H22D H 0.0723 0.2197 0.2938 0.093 Uiso 1 1 calc R . . C23B C 0.0948(4) 0.19066(18) 0.2187(3) 0.097(2) Uani 1 1 d . . . H23C H 0.1473 0.1882 0.2322 0.117 Uiso 1 1 calc R . . H23D H 0.0922 0.2158 0.1893 0.117 Uiso 1 1 calc R . . C24B C 0.0686(3) 0.14365(15) 0.19566(19) 0.0619(13) Uani 1 1 d . . . H24C H 0.0308 0.1485 0.1656 0.074 Uiso 1 1 calc R . . H24D H 0.1113 0.1252 0.18 0.074 Uiso 1 1 calc R . . Li1B Li -0.0687(4) -0.0179(2) 0.2491(3) 0.0425(16) Uani 1 1 d . . . Li2B Li 0.0238(4) 0.0514(2) 0.2472(3) 0.0428(16) 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 Si1 0.0463(7) 0.0429(7) 0.0338(6) 0.0015(5) -0.0038(5) 0.0014(5) Si2 0.0651(8) 0.0424(7) 0.0342(7) 0.0060(5) -0.0001(6) -0.0015(6) O1 0.0515(19) 0.0440(17) 0.0593(19) -0.0076(14) -0.0060(14) 0.0048(15) O2 0.0458(18) 0.0633(19) 0.0511(18) 0.0014(15) -0.0011(14) 0.0097(15) O3 0.072(2) 0.0383(17) 0.072(2) 0.0003(15) 0.0175(17) 0.0137(17) N1 0.0393(19) 0.0355(18) 0.0354(18) 0.0002(14) -0.0022(15) 0.0019(15) N2 0.050(2) 0.0402(19) 0.0367(19) 0.0023(15) 0.0025(16) 0.0072(17) C1 0.037(2) 0.029(2) 0.044(2) 0.0005(17) 0.0019(19) -0.0032(19) C2 0.045(3) 0.032(2) 0.040(2) 0.0012(18) 0.0050(19) -0.001(2) C3 0.053(3) 0.050(3) 0.042(2) 0.000(2) 0.011(2) 0.003(2) C4 0.050(3) 0.050(3) 0.069(3) -0.001(2) 0.021(2) 0.002(2) C5 0.036(3) 0.050(3) 0.074(4) 0.005(2) 0.004(2) 0.007(2) C6 0.040(3) 0.047(3) 0.050(3) 0.006(2) -0.001(2) -0.001(2) C7 0.063(3) 0.048(3) 0.035(2) -0.0056(19) 0.002(2) 0.006(2) C8 0.073(3) 0.057(3) 0.046(3) 0.010(2) 0.006(2) 0.009(3) C9 0.066(3) 0.079(3) 0.050(3) -0.010(2) -0.012(2) -0.012(3) C10 0.082(4) 0.061(3) 0.052(3) 0.012(2) -0.008(3) 0.013(3) C11 0.099(4) 0.057(3) 0.047(3) 0.000(2) -0.013(3) 0.000(3) C12 0.083(4) 0.063(3) 0.063(3) 0.015(2) 0.011(3) -0.009(3) C13 0.073(3) 0.048(3) 0.054(3) 0.011(2) -0.002(2) -0.008(3) C14 0.085(4) 0.068(4) 0.094(4) -0.014(3) -0.022(3) 0.024(3) C15 0.071(3) 0.060(3) 0.076(4) -0.013(3) 0.004(3) 0.001(3) C16 0.107(4) 0.052(3) 0.064(3) -0.014(2) -0.022(3) 0.008(3) C17 0.060(3) 0.110(4) 0.055(3) 0.001(3) 0.009(3) 0.006(3) C18 0.103(5) 0.159(7) 0.079(4) 0.027(4) -0.001(4) -0.053(5) C19 0.076(4) 0.074(4) 0.095(4) 0.012(3) -0.016(3) -0.018(3) C20 0.065(3) 0.064(3) 0.059(3) 0.006(2) -0.008(2) 0.014(3) C21 0.061(3) 0.053(3) 0.068(3) 0.007(2) 0.004(2) 0.006(3) C22 0.067(4) 0.063(3) 0.119(5) -0.032(3) 0.017(3) 0.005(3) C23 0.079(4) 0.063(4) 0.139(5) -0.026(4) 0.025(4) -0.019(3) C24 0.067(4) 0.065(4) 0.153(6) -0.018(4) 0.021(4) -0.003(3) Li1 0.049(4) 0.044(4) 0.043(4) -0.002(3) -0.007(3) -0.001(3) Li2 0.095(6) 0.039(4) 0.046(4) 0.005(3) 0.001(4) 0.021(4) Si1B 0.0507(7) 0.0396(6) 0.0339(6) -0.0019(5) 0.0016(5) -0.0030(5) Si2B 0.0490(7) 0.0536(7) 0.0355(7) -0.0036(5) 0.0016(5) -0.0006(6) O1B 0.0527(19) 0.0372(15) 0.068(2) -0.0064(15) -0.0016(15) -0.0044(14) O2B 0.0339(16) 0.0373(16) 0.079(2) 0.0031(14) 0.0058(14) 0.0020(13) O3B 0.0624(19) 0.0349(15) 0.0543(18) 0.0001(14) 0.0090(15) -0.0085(14) N1B 0.0395(19) 0.0349(18) 0.0344(18) -0.0026(14) 0.0022(14) 0.0063(15) N2B 0.0326(18) 0.0401(18) 0.0333(18) -0.0010(14) 0.0016(14) 0.0022(15) C1B 0.034(2) 0.035(2) 0.039(2) -0.0041(18) -0.0032(18) -0.0007(19) C2B 0.029(2) 0.030(2) 0.050(3) -0.0066(18) 0.0031(18) -0.0058(18) C3B 0.039(2) 0.044(2) 0.050(3) -0.011(2) 0.006(2) 0.000(2) C4B 0.043(3) 0.037(2) 0.078(4) -0.014(2) 0.002(2) 0.009(2) C5B 0.048(3) 0.042(3) 0.077(4) -0.001(2) -0.013(2) 0.013(2) C6B 0.046(3) 0.042(2) 0.050(3) 0.001(2) -0.007(2) 0.008(2) C7B 0.074(3) 0.064(3) 0.053(3) -0.012(2) 0.016(2) 0.010(3) C8B 0.077(3) 0.060(3) 0.043(3) 0.002(2) 0.008(2) -0.015(3) C9B 0.073(3) 0.058(3) 0.047(3) -0.008(2) -0.008(2) -0.015(3) C10B 0.082(4) 0.084(4) 0.049(3) 0.008(3) -0.007(3) 0.020(3) C11B 0.069(3) 0.085(4) 0.046(3) -0.014(2) -0.007(2) -0.007(3) C12B 0.078(4) 0.069(3) 0.054(3) -0.007(2) 0.023(3) -0.007(3) C13B 0.120(5) 0.072(4) 0.055(3) 0.003(3) 0.010(3) -0.044(4) C14B 0.148(7) 0.046(3) 0.155(7) 0.001(4) -0.038(6) 0.017(4) C15B 0.088(5) 0.110(6) 0.155(7) -0.070(5) 0.008(5) 0.002(4) C16B 0.162(7) 0.060(3) 0.072(4) -0.005(3) -0.033(4) -0.039(4) C17B 0.079(4) 0.056(3) 0.164(6) 0.023(4) 0.045(4) 0.013(3) C18B 0.120(6) 0.089(5) 0.167(7) -0.006(5) -0.064(5) 0.042(5) C19B 0.059(5) 0.058(4) 0.57(2) 0.055(8) 0.102(8) 0.012(4) C20B 0.045(4) 0.055(4) 0.448(16) 0.029(6) 0.049(6) 0.000(3) C21B 0.096(4) 0.053(3) 0.068(3) -0.017(3) 0.023(3) -0.022(3) C22B 0.104(4) 0.043(3) 0.085(4) -0.008(3) 0.017(3) -0.011(3) C23B 0.134(6) 0.049(3) 0.109(5) -0.011(3) 0.057(4) -0.030(3) C24B 0.081(4) 0.048(3) 0.057(3) 0.001(2) 0.013(3) -0.008(3) Li1B 0.035(4) 0.040(4) 0.053(4) -0.003(3) 0.002(3) 0.000(3) Li2B 0.051(4) 0.034(3) 0.043(4) 0.001(3) -0.002(3) -0.003(3) #----------------------------------------------------------------------------# # 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 Si1 N1 1.694(3) . ? Si1 C8 1.879(4) . ? Si1 C9 1.879(4) . ? Si1 C7 1.882(4) . ? Si1 Li2 3.162(7) . ? Si2 N2 1.690(3) . ? Si2 C11 1.869(4) . ? Si2 C10 1.875(5) . ? Si2 C12 1.879(5) . ? Si2 Li2 3.160(7) . ? O1 C16 1.432(5) . ? O1 C13 1.440(5) . ? O1 Li1 1.934(7) . ? O2 C17 1.432(5) . ? O2 C20 1.444(5) . ? O2 Li1 1.959(7) . ? O3 C21 1.436(5) . ? O3 C24 1.438(6) . ? O3 Li2 1.897(7) . ? N1 C1 1.407(5) . ? N1 Li2 1.954(7) . ? N1 Li1 2.081(7) . ? N2 C2 1.401(5) . ? N2 Li2 1.971(8) . ? N2 Li1 2.098(7) . ? C1 C6 1.395(5) . ? C1 C2 1.440(5) . ? C1 Li1 2.405(8) . ? C1 Li2 2.690(8) . ? C2 C3 1.396(5) . ? C2 Li1 2.402(8) . ? C2 Li2 2.690(8) . ? C3 C4 1.393(6) . ? C4 C5 1.376(6) . ? C5 C6 1.403(6) . ? C13 C14 1.495(6) . ? C14 C15 1.488(7) . ? C15 C16 1.483(6) . ? C17 C18 1.493(8) . ? C18 C19 1.425(7) . ? C19 C20 1.514(7) . ? C21 C22 1.505(7) . ? C22 C23 1.498(7) . ? C23 C24 1.464(7) . ? Li1 Li2 2.405(10) . ? Si1B N1B 1.701(3) . ? Si1B C7B 1.865(5) . ? Si1B C9B 1.875(4) . ? Si1B C8B 1.878(4) . ? Si2B N2B 1.698(3) . ? Si2B C10B 1.870(5) . ? Si2B C12B 1.883(5) . ? Si2B C11B 1.888(5) . ? O1B C16B 1.398(6) . ? O1B C13B 1.448(6) . ? O1B Li1B 1.941(7) . ? O2B C20B 1.370(6) . ? O2B C17B 1.409(6) . ? O2B Li1B 1.953(7) . ? O3B C21B 1.429(5) . ? O3B C24B 1.430(5) . ? O3B Li2B 1.915(7) . ? N1B C1B 1.408(5) . ? N1B Li2B 1.968(7) . ? N1B Li1B 2.072(7) . ? N2B C2B 1.401(5) . ? N2B Li2B 1.980(7) . ? N2B Li1B 2.109(7) . ? C1B C6B 1.395(5) . ? C1B C2B 1.440(5) . ? C1B Li1B 2.486(7) . ? C1B Li2B 2.578(7) . ? C2B C3B 1.405(5) . ? C2B Li1B 2.492(7) . ? C2B Li2B 2.578(7) . ? C3B C4B 1.395(6) . ? C4B C5B 1.366(6) . ? C5B C6B 1.390(6) . ? C13B C14B 1.494(8) . ? C14B C15B 1.433(9) . ? C15B C16B 1.416(8) . ? C17B C18B 1.471(9) . ? C18B C19B 1.355(10) . ? C19B C20B 1.497(9) . ? C21B C22B 1.507(6) . ? C22B C23B 1.419(7) . ? C23B C24B 1.497(6) . ? Li1B Li2B 2.544(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C8 114.35(18) . . ? N1 Si1 C9 115.13(19) . . ? C8 Si1 C9 107.0(2) . . ? N1 Si1 C7 106.54(17) . . ? C8 Si1 C7 107.7(2) . . ? C9 Si1 C7 105.6(2) . . ? N1 Si1 Li2 32.36(16) . . ? C8 Si1 Li2 138.5(2) . . ? C9 Si1 Li2 111.1(2) . . ? C7 Si1 Li2 77.35(19) . . ? N2 Si2 C11 115.79(19) . . ? N2 Si2 C10 107.17(18) . . ? C11 Si2 C10 106.5(2) . . ? N2 Si2 C12 113.7(2) . . ? C11 Si2 C12 106.2(2) . . ? C10 Si2 C12 106.9(2) . . ? N2 Si2 Li2 33.02(16) . . ? C11 Si2 Li2 141.0(2) . . ? C10 Si2 Li2 77.8(2) . . ? C12 Si2 Li2 109.4(2) . . ? C16 O1 C13 108.7(3) . . ? C16 O1 Li1 117.2(3) . . ? C13 O1 Li1 122.9(3) . . ? C17 O2 C20 107.4(3) . . ? C17 O2 Li1 117.3(3) . . ? C20 O2 Li1 118.8(3) . . ? C21 O3 C24 109.5(3) . . ? C21 O3 Li2 133.5(4) . . ? C24 O3 Li2 116.8(4) . . ? C1 N1 Si1 126.4(3) . . ? C1 N1 Li2 105.2(3) . . ? Si1 N1 Li2 120.0(3) . . ? C1 N1 Li1 84.8(3) . . ? Si1 N1 Li1 133.0(3) . . ? Li2 N1 Li1 73.1(3) . . ? C2 N2 Si2 126.2(3) . . ? C2 N2 Li2 104.5(3) . . ? Si2 N2 Li2 119.1(3) . . ? C2 N2 Li1 84.2(3) . . ? Si2 N2 Li1 136.1(3) . . ? Li2 N2 Li1 72.4(3) . . ? C6 C1 N1 125.7(3) . . ? C6 C1 C2 118.4(4) . . ? N1 C1 C2 115.9(3) . . ? C6 C1 Li1 138.1(3) . . ? N1 C1 Li1 59.5(2) . . ? C2 C1 Li1 72.5(3) . . ? C6 C1 Li2 161.5(3) . . ? N1 C1 Li2 44.5(2) . . ? C2 C1 Li2 74.5(3) . . ? Li1 C1 Li2 56.0(3) . . ? C3 C2 N2 125.2(4) . . ? C3 C2 C1 117.9(4) . . ? N2 C2 C1 116.8(3) . . ? C3 C2 Li1 138.0(3) . . ? N2 C2 Li1 60.3(2) . . ? C1 C2 Li1 72.7(3) . . ? C3 C2 Li2 161.9(3) . . ? N2 C2 Li2 45.2(2) . . ? C1 C2 Li2 74.5(3) . . ? Li1 C2 Li2 56.0(3) . . ? C4 C3 C2 122.4(4) . . ? C5 C4 C3 119.8(4) . . ? C4 C5 C6 119.4(4) . . ? C1 C6 C5 122.0(4) . . ? O1 C13 C14 105.1(4) . . ? C15 C14 C13 103.9(4) . . ? C16 C15 C14 101.6(4) . . ? O1 C16 C15 106.9(4) . . ? O2 C17 C18 105.4(4) . . ? C19 C18 C17 107.1(5) . . ? C18 C19 C20 106.5(5) . . ? O2 C20 C19 106.3(4) . . ? O3 C21 C22 104.6(4) . . ? C23 C22 C21 102.2(4) . . ? C24 C23 C22 103.2(5) . . ? O3 C24 C23 106.0(4) . . ? O1 Li1 O2 104.3(3) . . ? O1 Li1 N1 120.1(3) . . ? O2 Li1 N1 116.0(3) . . ? O1 Li1 N2 123.2(4) . . ? O2 Li1 N2 112.7(3) . . ? N1 Li1 N2 80.0(3) . . ? O1 Li1 C2 101.5(3) . . ? O2 Li1 C2 147.9(4) . . ? N1 Li1 C2 64.7(2) . . ? N2 Li1 C2 35.46(16) . . ? O1 Li1 C1 100.2(3) . . ? O2 Li1 C1 150.8(4) . . ? N1 Li1 C1 35.65(16) . . ? N2 Li1 C1 64.6(2) . . ? C2 Li1 C1 34.86(16) . . ? O1 Li1 Li2 168.1(4) . . ? O2 Li1 Li2 87.5(3) . . ? N1 Li1 Li2 51.0(2) . . ? N2 Li1 Li2 51.4(2) . . ? C2 Li1 Li2 68.0(3) . . ? C1 Li1 Li2 68.0(3) . . ? O3 Li2 N1 134.3(4) . . ? O3 Li2 N2 133.9(4) . . ? N1 Li2 N2 86.4(3) . . ? O3 Li2 Li1 157.4(5) . . ? N1 Li2 Li1 55.9(3) . . ? N2 Li2 Li1 56.2(3) . . ? O3 Li2 C2 144.9(4) . . ? N1 Li2 C2 60.2(2) . . ? N2 Li2 C2 30.27(16) . . ? Li1 Li2 C2 55.9(2) . . ? O3 Li2 C1 144.9(5) . . ? N1 Li2 C1 30.33(16) . . ? N2 Li2 C1 60.2(2) . . ? Li1 Li2 C1 56.0(2) . . ? C2 Li2 C1 31.05(14) . . ? O3 Li2 Si2 107.3(3) . . ? N1 Li2 Si2 114.2(3) . . ? N2 Li2 Si2 27.86(14) . . ? Li1 Li2 Si2 77.0(2) . . ? C2 Li2 Si2 55.61(16) . . ? C1 Li2 Si2 86.6(2) . . ? O3 Li2 Si1 108.3(3) . . ? N1 Li2 Si1 27.65(14) . . ? N2 Li2 Si1 114.0(3) . . ? Li1 Li2 Si1 75.6(2) . . ? C2 Li2 Si1 86.8(2) . . ? C1 Li2 Si1 55.84(15) . . ? Si2 Li2 Si1 141.7(2) . . ? N1B Si1B C7B 107.61(18) . . ? N1B Si1B C9B 112.91(18) . . ? C7B Si1B C9B 107.2(2) . . ? N1B Si1B C8B 116.64(18) . . ? C7B Si1B C8B 104.8(2) . . ? C9B Si1B C8B 107.0(2) . . ? N2B Si2B C10B 108.05(18) . . ? N2B Si2B C12B 113.18(19) . . ? C10B Si2B C12B 106.2(2) . . ? N2B Si2B C11B 116.28(19) . . ? C10B Si2B C11B 105.3(2) . . ? C12B Si2B C11B 107.1(2) . . ? C16B O1B C13B 105.5(4) . . ? C16B O1B Li1B 119.8(4) . . ? C13B O1B Li1B 125.7(3) . . ? C20B O2B C17B 108.8(4) . . ? C20B O2B Li1B 122.7(4) . . ? C17B O2B Li1B 127.5(4) . . ? C21B O3B C24B 108.6(3) . . ? C21B O3B Li2B 127.2(3) . . ? C24B O3B Li2B 124.1(3) . . ? C1B N1B Si1B 125.4(2) . . ? C1B N1B Li2B 98.2(3) . . ? Si1B N1B Li2B 123.1(2) . . ? C1B N1B Li1B 89.0(3) . . ? Si1B N1B Li1B 130.0(3) . . ? Li2B N1B Li1B 78.0(3) . . ? C2B N2B Si2B 125.4(3) . . ? C2B N2B Li2B 97.9(3) . . ? Si2B N2B Li2B 124.3(2) . . ? C2B N2B Li1B 88.1(3) . . ? Si2B N2B Li1B 130.6(2) . . ? Li2B N2B Li1B 76.9(3) . . ? C6B C1B N1B 125.4(3) . . ? C6B C1B C2B 118.3(3) . . ? N1B C1B C2B 116.3(3) . . ? C6B C1B Li1B 142.0(3) . . ? N1B C1B Li1B 56.5(2) . . ? C2B C1B Li1B 73.4(3) . . ? C6B C1B Li2B 154.9(3) . . ? N1B C1B Li2B 49.1(2) . . ? C2B C1B Li2B 73.8(3) . . ? Li1B C1B Li2B 60.3(2) . . ? N2B C2B C3B 125.5(4) . . ? N2B C2B C1B 117.1(3) . . ? C3B C2B C1B 117.4(4) . . ? N2B C2B Li1B 57.8(2) . . ? C3B C2B Li1B 143.5(3) . . ? C1B C2B Li1B 73.0(3) . . ? N2B C2B Li2B 49.5(2) . . ? C3B C2B Li2B 154.2(3) . . ? C1B C2B Li2B 73.8(3) . . ? Li1B C2B Li2B 60.2(2) . . ? C4B C3B C2B 122.5(4) . . ? C5B C4B C3B 119.6(4) . . ? C4B C5B C6B 119.9(4) . . ? C5B C6B C1B 122.3(4) . . ? O1B C13B C14B 104.8(4) . . ? C15B C14B C13B 106.5(5) . . ? C16B C15B C14B 106.4(5) . . ? O1B C16B C15B 108.3(5) . . ? O2B C17B C18B 106.1(5) . . ? C19B C18B C17B 103.9(6) . . ? C18B C19B C20B 108.2(6) . . ? O2B C20B C19B 105.4(5) . . ? O3B C21B C22B 107.0(4) . . ? C23B C22B C21B 104.7(4) . . ? C22B C23B C24B 105.8(4) . . ? O3B C24B C23B 105.0(4) . . ? O1B Li1B O2B 104.0(3) . . ? O1B Li1B N1B 116.0(3) . . ? O2B Li1B N1B 119.0(3) . . ? O1B Li1B N2B 119.1(3) . . ? O2B Li1B N2B 118.1(3) . . ? N1B Li1B N2B 80.5(3) . . ? O1B Li1B C1B 97.2(3) . . ? O2B Li1B C1B 152.9(3) . . ? N1B Li1B C1B 34.49(15) . . ? N2B Li1B C1B 63.0(2) . . ? O1B Li1B C2B 98.6(3) . . ? O2B Li1B C2B 151.9(4) . . ? N1B Li1B C2B 63.2(2) . . ? N2B Li1B C2B 34.17(15) . . ? C1B Li1B C2B 33.63(15) . . ? O1B Li1B Li2B 158.4(4) . . ? O2B Li1B Li2B 97.6(3) . . ? N1B Li1B Li2B 49.2(2) . . ? N2B Li1B Li2B 49.3(2) . . ? C1B Li1B Li2B 61.7(2) . . ? C2B Li1B Li2B 61.6(2) . . ? O3B Li2B N1B 138.3(4) . . ? O3B Li2B N2B 135.3(4) . . ? N1B Li2B N2B 86.3(3) . . ? O3B Li2B Li1B 146.2(4) . . ? N1B Li2B Li1B 52.8(2) . . ? N2B Li2B Li1B 53.8(2) . . ? O3B Li2B C1B 153.0(4) . . ? N1B Li2B C1B 32.71(15) . . ? N2B Li2B C1B 62.6(2) . . ? Li1B Li2B C1B 58.1(2) . . ? O3B Li2B C2B 151.4(4) . . ? N1B Li2B C2B 62.6(2) . . ? N2B Li2B C2B 32.55(15) . . ? Li1B Li2B C2B 58.2(2) . . ? C1B Li2B C2B 32.43(14) . . ? #===END data_mfl-4-dec798 _database_code_CSD 168081 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4{N(SiMe3)Li(tmeda)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Li2 N6 Si2' _chemical_formula_weight 496.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.813(5) _cell_length_b 16.812(3) _cell_length_c 10.872(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.20(3) _cell_angle_gamma 90.00 _cell_volume 1609.3(9) _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 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.131 _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 ? _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 3098 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2931 _reflns_number_gt 2519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.6117P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(19) _refine_ls_number_reflns 2931 _refine_ls_number_parameters 307 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Si1 Si 0.40161(12) 0.40365(6) 0.16412(11) 0.0251(3) Uani 1 1 d . . . Si2 Si 0.10350(13) 0.67432(6) 0.32949(11) 0.0300(3) Uani 1 1 d . . . N1 N 0.2947(3) 0.46994(19) 0.2012(3) 0.0211(7) Uani 1 1 d . . . N2 N 0.1608(3) 0.59519(19) 0.2663(3) 0.0229(7) Uani 1 1 d . . . N3 N 0.4351(4) 0.6649(2) 0.1209(4) 0.0450(10) Uani 1 1 d . . . N4 N 0.1281(4) 0.6239(2) -0.0777(4) 0.0384(9) Uani 1 1 d . . . N5 N 0.4862(4) 0.5088(2) 0.5972(3) 0.0401(9) Uani 1 1 d . . . N6 N 0.2001(4) 0.4159(2) 0.4689(3) 0.0344(8) Uani 1 1 d . . . C1 C 0.1362(4) 0.4702(2) 0.1447(4) 0.0213(8) Uani 1 1 d . . . C2 C 0.0655(4) 0.5363(2) 0.1816(3) 0.0202(7) Uani 1 1 d . . . C3 C -0.0937(4) 0.5350(3) 0.1281(4) 0.0281(9) Uani 1 1 d . . . H3 H -0.1423 0.5765 0.1532 0.034 Uiso 1 1 calc R . . C4 C -0.1834(4) 0.4758(3) 0.0402(4) 0.0333(10) Uani 1 1 d . . . H4 H -0.2907 0.4780 0.0055 0.040 Uiso 1 1 calc R . . C5 C -0.1173(4) 0.4148(3) 0.0037(4) 0.0340(10) Uani 1 1 d . . . H5 H -0.1781 0.3743 -0.0563 0.041 Uiso 1 1 calc R . . C6 C 0.0400(4) 0.4126(2) 0.0555(4) 0.0274(8) Uani 1 1 d . . . H6 H 0.0845 0.3698 0.0289 0.033 Uiso 1 1 calc R . . C7 C 0.3728(5) 0.4082(3) -0.0195(4) 0.0382(10) Uani 1 1 d . . . H7A H 0.2662 0.3971 -0.0813 0.057 Uiso 1 1 calc R . . H7B H 0.4376 0.3684 -0.0336 0.057 Uiso 1 1 calc R . . H7C H 0.3998 0.4613 -0.0387 0.057 Uiso 1 1 calc R . . C8 C 0.6065(5) 0.4256(3) 0.2766(5) 0.0440(12) Uani 1 1 d . . . H8A H 0.6254 0.4237 0.3729 0.066 Uiso 1 1 calc R . . H8B H 0.6315 0.4786 0.2552 0.066 Uiso 1 1 calc R . . H8C H 0.6700 0.3858 0.2605 0.066 Uiso 1 1 calc R . . C9 C 0.3783(5) 0.2939(3) 0.1924(5) 0.0416(11) Uani 1 1 d . . . H9A H 0.2726 0.2780 0.1364 0.062 Uiso 1 1 calc R . . H9B H 0.4052 0.2846 0.2894 0.062 Uiso 1 1 calc R . . H9C H 0.4453 0.2624 0.1660 0.062 Uiso 1 1 calc R . . C10 C 0.0220(8) 0.6467(3) 0.4516(6) 0.0638(17) Uani 1 1 d . . . H10A H -0.0667 0.6123 0.4045 0.096 Uiso 1 1 calc R . . H10B H -0.0086 0.6950 0.4832 0.096 Uiso 1 1 calc R . . H10C H 0.0990 0.6184 0.5304 0.096 Uiso 1 1 calc R . . C11 C -0.0419(6) 0.7442(3) 0.2058(5) 0.0469(12) Uani 1 1 d . . . H11A H -0.1355 0.7148 0.1506 0.070 Uiso 1 1 calc R . . H11B H -0.0026 0.7678 0.1454 0.070 Uiso 1 1 calc R . . H11C H -0.0635 0.7864 0.2568 0.070 Uiso 1 1 calc R . . C12 C 0.2708(6) 0.7395(3) 0.4257(6) 0.0647(16) Uani 1 1 d . . . H12A H 0.3533 0.7078 0.4940 0.097 Uiso 1 1 calc R . . H12B H 0.2422 0.7817 0.4720 0.097 Uiso 1 1 calc R . . H12C H 0.3048 0.7633 0.3618 0.097 Uiso 1 1 calc R . . C13 C 0.3437(7) 0.7137(4) 0.0012(8) 0.087(2) Uani 1 1 d . . . H13A H 0.2917 0.7552 0.0295 0.104 Uiso 1 1 calc R . . H13B H 0.4129 0.7411 -0.0292 0.104 Uiso 1 1 calc R . . C14 C 0.2311(7) 0.6712(5) -0.1138(6) 0.074(2) Uani 1 1 d . . . H14A H 0.2832 0.6354 -0.1519 0.088 Uiso 1 1 calc R . . H14B H 0.1707 0.7098 -0.1862 0.088 Uiso 1 1 calc R . . C15 C 0.5484(7) 0.6224(4) 0.0936(8) 0.081(2) Uani 1 1 d . . . H15A H 0.4973 0.5857 0.0167 0.121 Uiso 1 1 calc R . . H15B H 0.6152 0.5923 0.1753 0.121 Uiso 1 1 calc R . . H15C H 0.6087 0.6606 0.0703 0.121 Uiso 1 1 calc R . . C16 C 0.5126(12) 0.7170(6) 0.2365(9) 0.140(4) Uani 1 1 d . . . H16A H 0.4378 0.7454 0.2569 0.211 Uiso 1 1 calc R . . H16B H 0.5738 0.7554 0.2147 0.211 Uiso 1 1 calc R . . H16C H 0.5789 0.6854 0.3165 0.211 Uiso 1 1 calc R . . C17 C 0.0656(7) 0.5601(4) -0.1745(5) 0.0634(16) Uani 1 1 d . . . H17A H -0.0028 0.5283 -0.1504 0.095 Uiso 1 1 calc R . . H17B H 0.1481 0.5263 -0.1722 0.095 Uiso 1 1 calc R . . H17C H 0.0090 0.5821 -0.2668 0.095 Uiso 1 1 calc R . . C18 C 0.0027(7) 0.6731(4) -0.0845(6) 0.0645(16) Uani 1 1 d . . . H18A H 0.0428 0.7177 -0.0204 0.097 Uiso 1 1 calc R . . H18B H -0.0649 0.6410 -0.0597 0.097 Uiso 1 1 calc R . . H18C H -0.0540 0.6936 -0.1778 0.097 Uiso 1 1 calc R . . C19 C 0.4529(6) 0.4372(3) 0.6589(5) 0.0557(14) Uani 1 1 d . . . H19A H 0.4965 0.3901 0.6345 0.067 Uiso 1 1 calc R . . H19B H 0.5044 0.4427 0.7599 0.067 Uiso 1 1 calc R . . C20 C 0.2929(6) 0.4231(4) 0.6164(5) 0.0523(14) Uani 1 1 d . . . H20A H 0.2524 0.4673 0.6507 0.063 Uiso 1 1 calc R . . H20B H 0.2822 0.3737 0.6608 0.063 Uiso 1 1 calc R . . C21 C 0.6387(6) 0.5013(5) 0.6102(6) 0.083(2) Uani 1 1 d . . . H21A H 0.6454 0.4536 0.5612 0.124 Uiso 1 1 calc R . . H21B H 0.7105 0.4967 0.7073 0.124 Uiso 1 1 calc R . . H21C H 0.6637 0.5483 0.5710 0.124 Uiso 1 1 calc R . . C22 C 0.4760(8) 0.5794(4) 0.6699(6) 0.082(2) Uani 1 1 d . . . H22A H 0.3729 0.5840 0.6619 0.123 Uiso 1 1 calc R . . H22B H 0.4997 0.6265 0.6300 0.123 Uiso 1 1 calc R . . H22C H 0.5487 0.5751 0.7668 0.123 Uiso 1 1 calc R . . C23 C 0.2248(7) 0.3383(3) 0.4210(5) 0.0580(15) Uani 1 1 d . . . H23A H 0.3326 0.3323 0.4437 0.087 Uiso 1 1 calc R . . H23B H 0.1642 0.3347 0.3215 0.087 Uiso 1 1 calc R . . H23C H 0.1941 0.2961 0.4657 0.087 Uiso 1 1 calc R . . C24 C 0.0402(6) 0.4224(4) 0.4358(6) 0.0659(17) Uani 1 1 d . . . H24A H 0.0206 0.4745 0.4652 0.099 Uiso 1 1 calc R . . H24B H 0.0126 0.3804 0.4831 0.099 Uiso 1 1 calc R . . H24C H -0.0207 0.4168 0.3365 0.099 Uiso 1 1 calc R . . Li1 Li 0.2732(7) 0.5887(4) 0.1434(7) 0.0283(14) Uani 1 1 d . . . Li2 Li 0.3037(8) 0.5065(4) 0.3851(6) 0.0286(15) 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 Si1 0.0275(5) 0.0231(6) 0.0279(5) 0.0016(5) 0.0153(4) 0.0053(5) Si2 0.0382(6) 0.0263(6) 0.0268(6) -0.0014(5) 0.0154(5) 0.0096(5) N1 0.0210(16) 0.0191(15) 0.0232(16) -0.0010(13) 0.0098(13) 0.0010(13) N2 0.0218(16) 0.0214(17) 0.0251(16) -0.0015(14) 0.0099(13) 0.0012(14) N3 0.044(2) 0.036(2) 0.065(3) -0.004(2) 0.034(2) -0.0090(19) N4 0.044(2) 0.043(2) 0.037(2) 0.0122(18) 0.0250(18) 0.0081(18) N5 0.038(2) 0.046(2) 0.0278(18) -0.0014(17) 0.0075(16) 0.0000(18) N6 0.041(2) 0.035(2) 0.0292(17) 0.0071(16) 0.0171(16) 0.0033(17) C1 0.0263(19) 0.0208(18) 0.0189(17) 0.0014(15) 0.0119(15) -0.0015(16) C2 0.0253(19) 0.0199(18) 0.0161(16) 0.0038(14) 0.0099(15) 0.0018(15) C3 0.0227(19) 0.032(2) 0.030(2) 0.0046(17) 0.0125(17) 0.0067(17) C4 0.021(2) 0.042(3) 0.035(2) 0.005(2) 0.0096(18) -0.0038(19) C5 0.030(2) 0.032(2) 0.032(2) -0.0004(19) 0.0060(17) -0.0117(19) C6 0.034(2) 0.021(2) 0.0280(18) -0.0007(17) 0.0143(17) -0.0024(18) C7 0.053(3) 0.034(2) 0.037(2) 0.004(2) 0.028(2) 0.009(2) C8 0.032(2) 0.049(3) 0.053(3) 0.009(2) 0.020(2) 0.009(2) C9 0.053(3) 0.027(2) 0.052(3) 0.007(2) 0.029(2) 0.010(2) C10 0.109(5) 0.053(3) 0.056(3) 0.010(3) 0.061(3) 0.030(3) C11 0.053(3) 0.033(3) 0.055(3) 0.004(2) 0.023(2) 0.016(2) C12 0.071(4) 0.039(3) 0.066(4) -0.024(3) 0.014(3) -0.001(3) C13 0.061(4) 0.061(4) 0.146(7) 0.041(5) 0.053(4) -0.006(3) C14 0.057(3) 0.100(5) 0.068(4) 0.049(4) 0.031(3) 0.004(4) C15 0.054(4) 0.060(4) 0.144(7) 0.026(4) 0.058(4) 0.011(3) C16 0.209(11) 0.125(8) 0.121(7) -0.067(6) 0.103(8) -0.117(8) C17 0.072(4) 0.073(4) 0.036(3) 0.007(3) 0.015(3) 0.022(3) C18 0.076(4) 0.067(4) 0.069(3) 0.027(3) 0.050(3) 0.038(3) C19 0.059(3) 0.060(3) 0.034(3) 0.010(2) 0.008(2) -0.001(3) C20 0.059(3) 0.067(4) 0.030(2) 0.012(2) 0.019(2) -0.003(3) C21 0.049(3) 0.132(7) 0.058(4) 0.009(4) 0.015(3) 0.003(4) C22 0.107(5) 0.055(4) 0.049(3) -0.013(3) 0.002(3) 0.013(4) C23 0.093(4) 0.038(3) 0.054(3) -0.001(2) 0.042(3) -0.009(3) C24 0.041(3) 0.076(4) 0.083(4) 0.033(3) 0.029(3) 0.002(3) Li1 0.029(4) 0.027(3) 0.033(3) 0.001(3) 0.018(3) 0.001(3) Li2 0.032(4) 0.031(4) 0.023(3) 0.003(3) 0.012(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.697(3) . ? Si1 C8 1.872(5) . ? Si1 C7 1.890(4) . ? Si1 C9 1.901(5) . ? Si2 N2 1.703(3) . ? Si2 C12 1.864(5) . ? Si2 C11 1.879(5) . ? Si2 C10 1.885(5) . ? N1 C1 1.397(5) . ? N1 Li2 2.056(7) . ? N1 Li1 2.076(7) . ? N2 C2 1.394(5) . ? N2 Li2 2.063(7) . ? N2 Li1 2.078(7) . ? N3 C16 1.442(8) . ? N3 C15 1.459(7) . ? N3 C13 1.463(8) . ? N3 Li1 2.136(8) . ? N4 C17 1.437(7) . ? N4 C18 1.457(6) . ? N4 C14 1.470(6) . ? N4 Li1 2.265(8) . ? N5 C21 1.446(7) . ? N5 C22 1.453(7) . ? N5 C19 1.483(6) . ? N5 Li2 2.209(7) . ? N6 C24 1.451(6) . ? N6 C20 1.458(6) . ? N6 C23 1.463(6) . ? N6 Li2 2.238(8) . ? C1 C6 1.401(5) . ? C1 C2 1.457(5) . ? C1 Li1 2.408(8) . ? C1 Li2 2.472(7) . ? C2 C3 1.406(5) . ? C2 Li1 2.420(7) . ? C2 Li2 2.458(7) . ? C3 C4 1.391(6) . ? C4 C5 1.362(6) . ? C5 C6 1.391(5) . ? C13 C14 1.441(9) . ? C19 C20 1.447(7) . ? Li1 Li2 2.866(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C8 108.31(19) . . ? N1 Si1 C7 113.88(18) . . ? C8 Si1 C7 107.4(2) . . ? N1 Si1 C9 117.92(18) . . ? C8 Si1 C9 104.9(2) . . ? C7 Si1 C9 103.7(2) . . ? N2 Si2 C12 108.7(2) . . ? N2 Si2 C11 118.78(19) . . ? C12 Si2 C11 103.7(3) . . ? N2 Si2 C10 114.2(2) . . ? C12 Si2 C10 107.0(3) . . ? C11 Si2 C10 103.5(2) . . ? C1 N1 Si1 125.6(3) . . ? C1 N1 Li2 89.3(3) . . ? Si1 N1 Li2 131.4(3) . . ? C1 N1 Li1 85.4(3) . . ? Si1 N1 Li1 123.4(2) . . ? Li2 N1 Li1 87.8(3) . . ? C2 N2 Si2 125.2(3) . . ? C2 N2 Li2 88.4(3) . . ? Si2 N2 Li2 124.5(2) . . ? C2 N2 Li1 86.0(3) . . ? Si2 N2 Li1 131.6(3) . . ? Li2 N2 Li1 87.6(3) . . ? C16 N3 C15 108.6(6) . . ? C16 N3 C13 108.4(6) . . ? C15 N3 C13 108.4(5) . . ? C16 N3 Li1 113.4(4) . . ? C15 N3 Li1 113.7(4) . . ? C13 N3 Li1 104.1(4) . . ? C17 N4 C18 108.0(4) . . ? C17 N4 C14 109.3(5) . . ? C18 N4 C14 110.2(4) . . ? C17 N4 Li1 116.5(4) . . ? C18 N4 Li1 108.9(3) . . ? C14 N4 Li1 103.9(3) . . ? C21 N5 C22 109.6(5) . . ? C21 N5 C19 108.0(5) . . ? C22 N5 C19 109.6(4) . . ? C21 N5 Li2 115.3(4) . . ? C22 N5 Li2 111.3(4) . . ? C19 N5 Li2 102.7(3) . . ? C24 N6 C20 110.4(4) . . ? C24 N6 C23 108.1(4) . . ? C20 N6 C23 110.2(4) . . ? C24 N6 Li2 118.9(3) . . ? C20 N6 Li2 102.4(3) . . ? C23 N6 Li2 106.6(3) . . ? N1 C1 C6 125.5(3) . . ? N1 C1 C2 117.0(3) . . ? C6 C1 C2 117.5(3) . . ? N1 C1 Li1 59.3(2) . . ? C6 C1 Li1 140.8(3) . . ? C2 C1 Li1 72.9(3) . . ? N1 C1 Li2 56.3(2) . . ? C6 C1 Li2 146.5(3) . . ? C2 C1 Li2 72.3(2) . . ? Li1 C1 Li2 71.9(2) . . ? N2 C2 C3 125.7(3) . . ? N2 C2 C1 117.5(3) . . ? C3 C2 C1 116.9(3) . . ? N2 C2 Li1 58.9(2) . . ? C3 C2 Li1 143.2(3) . . ? C1 C2 Li1 72.0(2) . . ? N2 C2 Li2 57.0(2) . . ? C3 C2 Li2 144.1(3) . . ? C1 C2 Li2 73.3(2) . . ? Li1 C2 Li2 72.0(2) . . ? C4 C3 C2 123.0(4) . . ? C5 C4 C3 120.1(4) . . ? C4 C5 C6 119.3(4) . . ? C5 C6 C1 123.3(4) . . ? C14 C13 N3 115.3(5) . . ? C13 C14 N4 113.0(5) . . ? C20 C19 N5 114.4(4) . . ? C19 C20 N6 115.3(4) . . ? N1 Li1 N2 82.4(3) . . ? N1 Li1 N3 129.1(4) . . ? N2 Li1 N3 132.4(4) . . ? N1 Li1 N4 120.3(3) . . ? N2 Li1 N4 113.9(3) . . ? N3 Li1 N4 82.7(3) . . ? N1 Li1 C1 35.35(16) . . ? N2 Li1 C1 65.3(2) . . ? N3 Li1 C1 160.4(4) . . ? N4 Li1 C1 97.5(3) . . ? N1 Li1 C2 65.0(2) . . ? N2 Li1 C2 35.08(16) . . ? N3 Li1 C2 164.4(4) . . ? N4 Li1 C2 95.4(3) . . ? C1 Li1 C2 35.13(15) . . ? N1 Li1 Li2 45.8(2) . . ? N2 Li1 Li2 46.0(2) . . ? N3 Li1 Li2 127.7(3) . . ? N4 Li1 Li2 149.4(4) . . ? C1 Li1 Li2 55.1(2) . . ? C2 Li1 Li2 54.6(2) . . ? N1 Li2 N2 83.2(3) . . ? N1 Li2 N5 133.4(4) . . ? N2 Li2 N5 130.9(4) . . ? N1 Li2 N6 111.1(3) . . ? N2 Li2 N6 116.2(3) . . ? N5 Li2 N6 83.8(3) . . ? N1 Li2 C2 64.5(2) . . ? N2 Li2 C2 34.53(16) . . ? N5 Li2 C2 161.2(3) . . ? N6 Li2 C2 94.7(3) . . ? N1 Li2 C1 34.42(15) . . ? N2 Li2 C1 64.3(2) . . ? N5 Li2 C1 164.2(4) . . ? N6 Li2 C1 93.0(3) . . ? C2 Li2 C1 34.37(15) . . ? N1 Li2 Li1 46.4(2) . . ? N2 Li2 Li1 46.4(2) . . ? N5 Li2 Li1 131.1(3) . . ? N6 Li2 Li1 145.1(3) . . ? C2 Li2 Li1 53.4(2) . . ? C1 Li2 Li1 53.0(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.292 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.043 #===END data_mfl-6-jul1297 _database_code_CSD 168083 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H54 Li2 N6 Si2' _chemical_formula_weight 520.81 _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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Cmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' '-x, y, z' '-x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' _cell_length_a 36.532(11) _cell_length_b 16.972(10) _cell_length_c 16.030(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9938.9(73) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method ? _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6301 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6301 _reflns_number_observed 4508 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1255P)^2^+16.9497P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(22) _refine_ls_number_reflns 6301 _refine_ls_number_parameters 502 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_obs 0.0743 _refine_ls_wR_factor_all 0.2234 _refine_ls_wR_factor_obs 0.1902 _refine_ls_goodness_of_fit_all 0.982 _refine_ls_goodness_of_fit_obs 0.998 _refine_ls_restrained_S_all 0.982 _refine_ls_restrained_S_obs 0.998 _refine_ls_shift/esd_max -0.003 _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 Si1 Si 0.34430(4) 0.14283(9) -0.07400(11) 0.0392(4) Uani 1 d . . Si2 Si 0.32594(4) 0.38902(8) 0.20144(10) 0.0343(3) Uani 1 d . . Si3 Si 0.08434(4) 0.23982(10) 0.06543(11) 0.0377(4) Uani 1 d . . N1 N 0.34217(12) 0.2194(3) -0.0057(3) 0.0300(9) Uani 1 d . . N2 N 0.33464(11) 0.3283(2) 0.1191(3) 0.0262(8) Uani 1 d . . N3 N 0.36441(14) 0.1242(3) 0.2108(4) 0.0468(13) Uani 1 d . . N4 N 0.41943(12) 0.2254(3) 0.1305(3) 0.0398(11) Uani 1 d . . N5 N 0.24060(13) 0.2414(3) 0.0553(4) 0.0478(13) Uani 1 d . . N6 N 0.27127(14) 0.3636(3) -0.0550(3) 0.0428(12) Uani 1 d . . N7 N 0.03781(10) 0.2443(2) 0.0578(3) 0.0281(9) Uani 1 d . . N8 N 0.0000 0.2626(5) 0.2842(5) 0.047(2) Uani 1 d S . N9 N 0.0000 0.4030(4) 0.1787(5) 0.047(2) Uani 1 d S . N10 N 0.0000 0.0303(4) 0.0813(5) 0.049(2) Uani 1 d S . N11 N 0.0000 0.1012(4) -0.0843(5) 0.042(2) Uani 1 d S . C1 C 0.35805(14) 0.2932(3) -0.0181(3) 0.0281(10) Uani 1 d . . C2 C 0.35421(13) 0.3516(3) 0.0477(3) 0.0272(10) Uani 1 d . . C3 C 0.36947(15) 0.4258(3) 0.0342(4) 0.0356(12) Uani 1 d . . H3 H 0.36691(15) 0.4637(3) 0.0756(4) 0.043 Uiso 1 calc R . C4 C 0.3882(2) 0.4459(4) -0.0376(4) 0.0443(14) Uani 1 d . . H4 H 0.3981(2) 0.4961(4) -0.0432(4) 0.053 Uiso 1 calc R . C5 C 0.3922(2) 0.3919(4) -0.1005(4) 0.0479(15) Uani 1 d . . H5 H 0.4045(2) 0.4051(4) -0.1494(4) 0.057 Uiso 1 calc R . C6 C 0.3774(2) 0.3164(4) -0.0897(4) 0.0396(13) Uani 1 d . . H6 H 0.3805(2) 0.2798(4) -0.1322(4) 0.048 Uiso 1 calc R . C7 C 0.3912(2) 0.1078(4) -0.0981(6) 0.063(2) Uani 1 d . . H7 H 0.4060(2) 0.1419(4) -0.1286(6) 0.076 Uiso 1 calc R . C8 C 0.4059(2) 0.0396(5) -0.0766(8) 0.086(3) Uani 1 d . . H8B H 0.3923(2) 0.0033(5) -0.0461(8) 0.103 Uiso 1 calc R . H8A H 0.4298(2) 0.0278(5) -0.0921(8) 0.103 Uiso 1 calc R . C9 C 0.3243(3) 0.1594(6) -0.1810(6) 0.102(4) Uani 1 d . . H9C H 0.2996(3) 0.1780(6) -0.1757(6) 0.153 Uiso 1 calc R . H9B H 0.3244(3) 0.1107(6) -0.2116(6) 0.153 Uiso 1 calc R . H9A H 0.3386(3) 0.1979(6) -0.2102(6) 0.153 Uiso 1 calc R . C10 C 0.3193(3) 0.0568(5) -0.0306(8) 0.097(4) Uani 1 d . . H10C H 0.2947(3) 0.0720(5) -0.0171(8) 0.146 Uiso 1 calc R . H10B H 0.3315(3) 0.0387(5) 0.0188(8) 0.146 Uiso 1 calc R . H10A H 0.3188(3) 0.0153(5) -0.0713(8) 0.146 Uiso 1 calc R . C11 C 0.2945(2) 0.4733(4) 0.1746(4) 0.055(2) Uani 1 d . . H11 H 0.3038(2) 0.5122(4) 0.1397(4) 0.065 Uiso 1 calc R . C12 C 0.2601(3) 0.4823(6) 0.2011(6) 0.084(3) Uani 1 d . . H12B H 0.2497(3) 0.4448(6) 0.2361(6) 0.101 Uiso 1 calc R . H12A H 0.2466(3) 0.5260(6) 0.1845(6) 0.101 Uiso 1 calc R . C13 C 0.3658(2) 0.4353(5) 0.2558(5) 0.063(2) Uani 1 d . . H13C H 0.3796(2) 0.4662(5) 0.2167(5) 0.094 Uiso 1 calc R . H13B H 0.3812(2) 0.3948(5) 0.2787(5) 0.094 Uiso 1 calc R . H13A H 0.3571(2) 0.4686(5) 0.2999(5) 0.094 Uiso 1 calc R . C14 C 0.3024(2) 0.3319(5) 0.2849(4) 0.058(2) Uani 1 d . . H14C H 0.2813(2) 0.3060(5) 0.2619(4) 0.087 Uiso 1 calc R . H14B H 0.2948(2) 0.3670(5) 0.3285(4) 0.087 Uiso 1 calc R . H14A H 0.3188(2) 0.2932(5) 0.3073(4) 0.087 Uiso 1 calc R . C15 C 0.4016(2) 0.1249(6) 0.2341(7) 0.088(3) Uani 1 d . . H15B H 0.4088(2) 0.0706(6) 0.2433(7) 0.106 Uiso 1 calc R . H15A H 0.4031(2) 0.1513(6) 0.2877(7) 0.106 Uiso 1 calc R . C16 C 0.4286(2) 0.1594(6) 0.1818(8) 0.099(4) Uani 1 d . . H16B H 0.4377(2) 0.1183(6) 0.1454(8) 0.119 Uiso 1 calc R . H16A H 0.4488(2) 0.1753(6) 0.2173(8) 0.119 Uiso 1 calc R . C17 C 0.3576(5) 0.0470(6) 0.1666(10) 0.133(5) Uani 1 d . . H17C H 0.3733(5) 0.0433(6) 0.1187(10) 0.200 Uiso 1 calc R . H17B H 0.3325(5) 0.0444(6) 0.1491(10) 0.200 Uiso 1 calc R . H17A H 0.3628(5) 0.0041(6) 0.2039(10) 0.200 Uiso 1 calc R . C18 C 0.3417(5) 0.1277(11) 0.2789(9) 0.198(11) Uani 1 d . . H18C H 0.3166(5) 0.1271(11) 0.2607(9) 0.298 Uiso 1 calc R . H18B H 0.3463(5) 0.1753(11) 0.3094(9) 0.298 Uiso 1 calc R . H18A H 0.3461(5) 0.0830(11) 0.3143(9) 0.298 Uiso 1 calc R . C19 C 0.4291(3) 0.2964(5) 0.1754(11) 0.132(6) Uani 1 d . . H19C H 0.4232(3) 0.3416(5) 0.1421(11) 0.198 Uiso 1 calc R . H19B H 0.4548(3) 0.2962(5) 0.1872(11) 0.198 Uiso 1 calc R . H19A H 0.4156(3) 0.2985(5) 0.2268(11) 0.198 Uiso 1 calc R . C20 C 0.4395(2) 0.2259(11) 0.0537(7) 0.132(6) Uani 1 d . . H20C H 0.4326(2) 0.2711(11) 0.0213(7) 0.198 Uiso 1 calc R . H20B H 0.4343(2) 0.1788(11) 0.0229(7) 0.198 Uiso 1 calc R . H20A H 0.4653(2) 0.2283(11) 0.0655(7) 0.198 Uiso 1 calc R . C21 C 0.2189(2) 0.2870(7) -0.0048(8) 0.090(3) Uani 1 d . . H21B H 0.2143(2) 0.2534(7) -0.0526(8) 0.109 Uiso 1 calc R . H21A H 0.1954(2) 0.2977(7) 0.0208(8) 0.109 Uiso 1 calc R . C22 C 0.2322(2) 0.3567(7) -0.0341(8) 0.108(4) Uani 1 d . . H22B H 0.2268(2) 0.3968(7) 0.0073(8) 0.130 Uiso 1 calc R . H22A H 0.2184(2) 0.3701(7) -0.0838(8) 0.130 Uiso 1 calc R . C23 C 0.2334(3) 0.1602(6) 0.0321(8) 0.086(3) Uani 1 d . . H23C H 0.2412(3) 0.1516(6) -0.0244(8) 0.129 Uiso 1 calc R . H23B H 0.2077(3) 0.1498(6) 0.0367(8) 0.129 Uiso 1 calc R . H23A H 0.2466(3) 0.1256(6) 0.0686(8) 0.129 Uiso 1 calc R . C24 C 0.2297(3) 0.2591(8) 0.1390(6) 0.106(4) Uani 1 d . . H24C H 0.2351(3) 0.3133(8) 0.1511(6) 0.159 Uiso 1 calc R . H24B H 0.2429(3) 0.2258(8) 0.1770(6) 0.159 Uiso 1 calc R . H24A H 0.2039(3) 0.2500(8) 0.1451(6) 0.159 Uiso 1 calc R . C25 C 0.2783(3) 0.3394(6) -0.1375(5) 0.086(3) Uani 1 d . . H25C H 0.2718(3) 0.2849(6) -0.1437(5) 0.128 Uiso 1 calc R . H25B H 0.3038(3) 0.3461(6) -0.1498(5) 0.128 Uiso 1 calc R . H25A H 0.2640(3) 0.3706(6) -0.1754(5) 0.128 Uiso 1 calc R . C26 C 0.2811(3) 0.4449(5) -0.0474(6) 0.084(3) Uani 1 d . . H26C H 0.2765(3) 0.4623(5) 0.0086(6) 0.126 Uiso 1 calc R . H26B H 0.2668(3) 0.4756(5) -0.0856(6) 0.126 Uiso 1 calc R . H26A H 0.3066(3) 0.4512(5) -0.0601(6) 0.126 Uiso 1 calc R . C27 C 0.01988(13) 0.2917(3) -0.0004(3) 0.0272(10) Uani 1 d . . C28 C 0.03772(14) 0.3400(3) -0.0593(3) 0.0339(11) Uani 1 d . . H28 H 0.06317(14) 0.3408(3) -0.0601(3) 0.041 Uiso 1 calc R . C29 C 0.0187(2) 0.3867(3) -0.1165(4) 0.0379(12) Uani 1 d . . H29 H 0.0315(2) 0.4177(3) -0.1544(4) 0.045 Uiso 1 calc R . C30 C 0.0973(2) 0.1679(10) 0.1466(10) 0.158(8) Uani 1 d . . H30 H 0.0776(2) 0.1447(10) 0.1739(10) 0.190 Uiso 1 calc R . C31 C 0.1265(4) 0.1461(9) 0.1700(13) 0.159(7) Uani 1 d . . H31B H 0.1477(4) 0.1664(9) 0.1460(13) 0.190 Uiso 1 calc R . H31A H 0.1282(4) 0.1088(9) 0.2124(13) 0.190 Uiso 1 calc R . C32 C 0.1085(2) 0.3340(5) 0.0936(8) 0.083(3) Uani 1 d . . H32C H 0.1028(2) 0.3739(5) 0.0532(8) 0.124 Uiso 1 calc R . H32B H 0.1345(2) 0.3252(5) 0.0942(8) 0.124 Uiso 1 calc R . H32A H 0.1007(2) 0.3511(5) 0.1478(8) 0.124 Uiso 1 calc R . C33 C 0.1088(2) 0.2028(5) -0.0298(6) 0.068(2) Uani 1 d . . H33C H 0.1037(2) 0.2369(5) -0.0761(6) 0.101 Uiso 1 calc R . H33B H 0.1006(2) 0.1504(5) -0.0425(6) 0.101 Uiso 1 calc R . H33A H 0.1347(2) 0.2020(5) -0.0195(6) 0.101 Uiso 1 calc R . C34 C 0.0000 0.3419(7) 0.3189(7) 0.065(3) Uani 1 d S . H34A H -0.0214 0.3470(7) 0.3544(7) 0.077 Uiso 0.50 calc PR . H34B H 0.0214 0.3470(7) 0.3544(7) 0.077 Uiso 0.50 calc PR . C35 C 0.0000 0.4013(11) 0.2663(11) 0.301(28) Uani 1 d S . H35A H 0.0212 0.4325(11) 0.2821(11) 0.361 Uiso 0.50 calc PR . H35B H -0.0212 0.4325(11) 0.2821(11) 0.361 Uiso 0.50 calc PR . C36 C 0.0315(4) 0.2216(7) 0.3117(9) 0.143(7) Uani 1 d . . H36A H 0.0531(4) 0.2489(7) 0.2934(9) 0.215 Uiso 1 calc R . H36B H 0.0314(4) 0.1693(7) 0.2889(9) 0.215 Uiso 1 calc R . H36C H 0.0314(4) 0.2187(7) 0.3715(9) 0.215 Uiso 1 calc R . C37 C 0.0300(4) 0.4422(7) 0.1524(14) 0.205(12) Uani 1 d . . H37A H 0.0516(4) 0.4149(7) 0.1707(14) 0.308 Uiso 1 calc R . H37B H 0.0299(4) 0.4945(7) 0.1752(14) 0.308 Uiso 1 calc R . H37C H 0.0299(4) 0.4451(7) 0.0926(14) 0.308 Uiso 1 calc R . C38 C 0.0000 -0.0140(7) 0.0031(9) 0.089(4) Uani 1 d S . H38A H 0.0213 -0.0481(7) 0.0049(9) 0.107 Uiso 0.50 calc PR . H38B H -0.0213 -0.0481(7) 0.0049(9) 0.107 Uiso 0.50 calc PR . C39 C 0.0000 0.0181(12) -0.0697(11) 0.251(21) Uani 1 d S . H39A H -0.0213 -0.0026(12) -0.0985(11) 0.301 Uiso 0.50 calc PR . H39B H 0.0213 -0.0026(12) -0.0985(11) 0.301 Uiso 0.50 calc PR . C40 C 0.0318(5) 0.0135(9) 0.1266(11) 0.206(10) Uani 1 d . . H40A H 0.0529(5) 0.0259(9) 0.0934(11) 0.309 Uiso 1 calc R . H40B H 0.0322(5) -0.0415(9) 0.1409(11) 0.309 Uiso 1 calc R . H40C H 0.0322(5) 0.0445(9) 0.1767(11) 0.309 Uiso 1 calc R . C41 C -0.0318(3) 0.1197(9) -0.1264(9) 0.159(8) Uani 1 d . . H41A H -0.0525(3) 0.1050(9) -0.0930(9) 0.238 Uiso 1 calc R . H41B H -0.0325(3) 0.0916(9) -0.1783(9) 0.238 Uiso 1 calc R . H41C H -0.0325(3) 0.1753(9) -0.1370(9) 0.238 Uiso 1 calc R . Li1 Li 0.3600(2) 0.2192(5) 0.1174(6) 0.032(2) Uani 1 d . . Li2 Li 0.2971(2) 0.2812(5) 0.0355(6) 0.031(2) Uani 1 d . . Li3 Li 0.0000 0.2784(8) 0.1470(9) 0.037(3) Uani 1 d S . Li4 Li 0.0000 0.1557(7) 0.0388(8) 0.031(3) Uani 1 d S . 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 0.0392(8) 0.0365(7) 0.0419(9) -0.0158(7) -0.0057(7) 0.0084(6) Si2 0.0460(8) 0.0306(7) 0.0264(6) -0.0050(6) -0.0012(7) -0.0008(6) Si3 0.0197(6) 0.0461(8) 0.0474(9) 0.0061(8) -0.0005(6) 0.0010(6) N1 0.030(2) 0.028(2) 0.031(2) -0.009(2) 0.001(2) 0.001(2) N2 0.032(2) 0.025(2) 0.022(2) -0.003(2) -0.001(2) 0.001(2) N3 0.041(3) 0.042(3) 0.057(3) 0.018(3) 0.001(3) 0.003(2) N4 0.031(2) 0.047(3) 0.041(3) 0.012(2) -0.010(2) -0.004(2) N5 0.036(2) 0.055(3) 0.052(3) -0.004(3) 0.003(2) -0.004(2) N6 0.042(3) 0.040(2) 0.046(3) 0.000(2) -0.007(2) 0.010(2) N7 0.017(2) 0.030(2) 0.037(2) 0.003(2) 0.002(2) -0.001(2) N8 0.050(4) 0.056(4) 0.035(4) -0.013(4) 0.000 0.000 N9 0.060(5) 0.029(3) 0.054(5) -0.010(3) 0.000 0.000 N10 0.060(5) 0.032(3) 0.056(5) 0.011(3) 0.000 0.000 N11 0.043(4) 0.046(4) 0.036(4) -0.006(3) 0.000 0.000 C1 0.029(2) 0.029(2) 0.027(2) 0.003(2) -0.003(2) 0.002(2) C2 0.027(2) 0.027(2) 0.027(2) 0.001(2) -0.004(2) 0.002(2) C3 0.033(3) 0.031(3) 0.043(3) 0.000(2) -0.004(2) -0.002(2) C4 0.045(3) 0.037(3) 0.051(4) 0.011(3) 0.001(3) -0.003(2) C5 0.049(3) 0.053(4) 0.042(3) 0.017(3) 0.009(3) 0.006(3) C6 0.042(3) 0.046(3) 0.031(3) 0.003(2) 0.006(2) 0.008(3) C7 0.057(4) 0.045(4) 0.087(6) -0.010(4) 0.018(4) 0.010(3) C8 0.070(5) 0.068(5) 0.120(8) -0.025(6) -0.003(6) 0.030(4) C9 0.146(9) 0.091(6) 0.069(6) -0.046(5) -0.065(6) 0.061(6) C10 0.103(7) 0.056(5) 0.134(9) -0.045(6) 0.039(7) -0.036(5) C11 0.077(5) 0.047(4) 0.039(3) -0.005(3) 0.009(3) 0.020(3) C12 0.091(6) 0.091(7) 0.071(5) -0.022(5) 0.011(5) 0.028(5) C13 0.066(5) 0.075(5) 0.047(4) -0.022(4) -0.015(3) -0.014(4) C14 0.074(5) 0.064(4) 0.035(3) -0.001(3) 0.016(3) -0.006(4) C15 0.055(4) 0.113(7) 0.097(7) 0.075(6) -0.019(4) 0.001(5) C16 0.039(3) 0.095(6) 0.163(11) 0.087(7) -0.010(5) 0.003(4) C17 0.188(13) 0.068(6) 0.143(12) 0.000(8) -0.009(11) -0.050(8) C18 0.231(17) 0.246(19) 0.119(11) 0.134(13) 0.109(12) 0.170(16) C19 0.092(7) 0.062(5) 0.243(18) -0.042(8) -0.085(10) 0.000(5) C20 0.041(4) 0.286(19) 0.069(6) 0.020(9) 0.008(4) 0.041(7) C21 0.031(3) 0.115(8) 0.125(9) 0.046(7) -0.010(5) 0.002(4) C22 0.034(4) 0.143(10) 0.147(11) 0.078(9) -0.007(5) 0.022(5) C23 0.060(5) 0.083(6) 0.115(8) -0.020(6) 0.006(5) -0.014(4) C24 0.068(6) 0.187(12) 0.064(6) -0.042(7) 0.027(5) -0.036(7) C25 0.119(8) 0.091(7) 0.046(4) -0.013(4) -0.025(5) 0.056(6) C26 0.111(7) 0.052(4) 0.089(7) -0.002(4) -0.046(6) 0.021(5) C27 0.025(2) 0.029(2) 0.028(2) 0.003(2) -0.001(2) -0.002(2) C28 0.029(2) 0.035(3) 0.038(3) 0.008(2) 0.001(2) -0.001(2) C29 0.039(3) 0.035(3) 0.039(3) 0.010(2) 0.009(2) -0.004(2) C30 0.033(4) 0.253(17) 0.188(14) 0.161(14) -0.002(6) 0.023(7) C31 0.101(9) 0.161(13) 0.214(18) 0.081(13) 0.014(12) -0.009(9) C32 0.042(4) 0.070(5) 0.137(9) -0.039(6) -0.019(5) 0.002(3) C33 0.033(3) 0.083(5) 0.086(6) -0.035(5) 0.007(4) 0.005(3) C34 0.063(6) 0.088(8) 0.042(5) -0.026(6) 0.000 0.000 C35 0.797(89) 0.061(10) 0.044(9) -0.028(8) 0.000 0.000 C36 0.168(12) 0.113(9) 0.148(12) -0.057(9) -0.117(10) 0.077(9) C37 0.129(10) 0.099(8) 0.389(30) -0.140(14) 0.151(15) -0.072(8) C38 0.147(13) 0.037(6) 0.083(10) 0.005(6) 0.000 0.000 C39 0.615(68) 0.084(13) 0.054(10) -0.046(10) 0.000 0.000 C40 0.266(18) 0.143(12) 0.208(17) -0.058(12) -0.169(16) 0.139(13) C41 0.098(8) 0.214(15) 0.163(13) -0.129(12) -0.088(9) 0.085(9) Li1 0.029(4) 0.031(4) 0.036(5) 0.000(4) -0.003(4) -0.004(3) Li2 0.025(4) 0.042(5) 0.028(4) -0.005(4) 0.000(3) 0.000(3) Li3 0.026(6) 0.041(7) 0.043(8) -0.001(6) 0.000 0.000 Li4 0.039(6) 0.026(6) 0.027(6) 0.000(5) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.701(4) . ? Si1 C7 1.855(7) . ? Si1 C10 1.856(9) . ? Si1 C9 1.886(8) . ? Si2 N2 1.704(4) . ? Si2 C14 1.863(7) . ? Si2 C13 1.869(7) . ? Si2 C11 1.883(7) . ? Si3 N7 1.706(4) . ? Si3 C30 1.845(10) . ? Si3 C33 1.877(8) . ? Si3 C32 1.882(8) . ? N1 C1 1.395(7) . ? N1 Li2 2.062(9) . ? N1 Li1 2.078(11) . ? N2 C2 1.406(6) . ? N2 Li1 2.072(10) . ? N2 Li2 2.078(9) . ? N3 C18 1.374(12) . ? N3 C15 1.408(9) . ? N3 C17 1.511(12) . ? N3 Li1 2.206(10) . ? N4 C16 1.429(9) . ? N4 C20 1.433(11) . ? N4 C19 1.449(11) . ? N4 Li1 2.183(9) . ? N5 C24 1.431(11) . ? N5 C23 1.452(11) . ? N5 C21 1.468(11) . ? N5 Li2 2.193(10) . ? N6 C25 1.409(10) . ? N6 C26 1.430(10) . ? N6 C22 1.470(10) . ? N6 Li2 2.225(11) . ? N7 C27 1.396(6) . ? N7 Li4 2.064(10) . ? N7 Li3 2.070(11) . ? N8 C36 1.417(10) 3 ? N8 C36 1.417(10) . ? N8 C34 1.456(13) . ? N8 Li3 2.22(2) . ? N9 C37 1.350(11) . ? N9 C37 1.350(11) 3 ? N9 C35 1.40(2) . ? N9 Li3 2.18(2) . ? N10 C40 1.401(12) . ? N10 C40 1.401(12) 3 ? N10 C38 1.46(2) . ? N10 Li4 2.235(14) . ? N11 C41 1.379(10) . ? N11 C41 1.379(10) 3 ? N11 C39 1.43(2) . ? N11 Li4 2.179(14) . ? C1 C6 1.403(7) . ? C1 C2 1.454(7) . ? C1 Li2 2.397(10) . ? C1 Li1 2.511(10) . ? C2 C3 1.394(7) . ? C2 Li2 2.413(10) . ? C2 Li1 2.518(10) . ? C3 C4 1.381(9) . ? C4 C5 1.370(10) . ? C5 C6 1.402(9) . ? C7 C8 1.322(11) . ? C11 C12 1.335(11) . ? C15 C16 1.420(12) . ? C21 C22 1.363(13) . ? C27 C28 1.410(7) . ? C27 C27 1.452(9) 3 ? C27 Li3 2.482(15) . ? C27 Li4 2.499(13) . ? C28 C29 1.396(8) . ? C29 C29 1.369(11) 3 ? C30 C31 1.19(2) . ? C34 C35 1.31(2) . ? C38 C39 1.29(2) . ? Li1 Li2 2.850(12) . ? Li3 N7 2.070(11) 3 ? Li3 C27 2.482(15) 3 ? Li3 Li4 2.71(2) . ? Li4 N7 2.064(10) 3 ? Li4 C27 2.499(13) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C7 114.9(3) . . ? N1 Si1 C10 109.7(4) . . ? C7 Si1 C10 106.3(4) . . ? N1 Si1 C9 117.0(3) . . ? C7 Si1 C9 102.5(5) . . ? C10 Si1 C9 105.5(6) . . ? N2 Si2 C14 109.1(3) . . ? N2 Si2 C13 118.0(3) . . ? C14 Si2 C13 104.1(4) . . ? N2 Si2 C11 113.3(3) . . ? C14 Si2 C11 106.1(4) . . ? C13 Si2 C11 105.2(4) . . ? N7 Si3 C30 109.6(3) . . ? N7 Si3 C33 115.5(3) . . ? C30 Si3 C33 103.3(6) . . ? N7 Si3 C32 116.6(3) . . ? C30 Si3 C32 105.8(7) . . ? C33 Si3 C32 104.9(4) . . ? C1 N1 Si1 125.1(4) . . ? C1 N1 Li2 85.5(4) . . ? Si1 N1 Li2 129.1(3) . . ? C1 N1 Li1 90.4(4) . . ? Si1 N1 Li1 126.5(3) . . ? Li2 N1 Li1 87.0(4) . . ? C2 N2 Si2 123.8(3) . . ? C2 N2 Li1 90.7(4) . . ? Si2 N2 Li1 129.4(4) . . ? C2 N2 Li2 85.4(4) . . ? Si2 N2 Li2 127.5(3) . . ? Li1 N2 Li2 86.7(4) . . ? C18 N3 C15 111.9(10) . . ? C18 N3 C17 108.1(12) . . ? C15 N3 C17 106.9(9) . . ? C18 N3 Li1 117.7(6) . . ? C15 N3 Li1 104.1(5) . . ? C17 N3 Li1 107.7(7) . . ? C16 N4 C20 112.3(8) . . ? C16 N4 C19 107.9(8) . . ? C20 N4 C19 107.3(10) . . ? C16 N4 Li1 104.5(5) . . ? C20 N4 Li1 115.3(5) . . ? C19 N4 Li1 109.3(6) . . ? C24 N5 C23 112.9(8) . . ? C24 N5 C21 110.8(8) . . ? C23 N5 C21 103.6(8) . . ? C24 N5 Li2 109.4(5) . . ? C23 N5 Li2 115.2(5) . . ? C21 N5 Li2 104.5(5) . . ? C25 N6 C26 108.4(8) . . ? C25 N6 C22 111.5(8) . . ? C26 N6 C22 107.5(8) . . ? C25 N6 Li2 110.6(5) . . ? C26 N6 Li2 116.4(5) . . ? C22 N6 Li2 102.2(5) . . ? C27 N7 Si3 122.8(3) . . ? C27 N7 Li4 90.4(4) . . ? Si3 N7 Li4 130.2(3) . . ? C27 N7 Li3 89.3(4) . . ? Si3 N7 Li3 128.9(4) . . ? Li4 N7 Li3 81.9(4) . . ? C36 N8 C36 108.8(16) 3 . ? C36 N8 C34 109.6(6) 3 . ? C36 N8 C34 109.6(6) . . ? C36 N8 Li3 111.6(8) 3 . ? C36 N8 Li3 111.6(8) . . ? C34 N8 Li3 105.6(7) . . ? C37 N9 C37 108.6(19) . 3 ? C37 N9 C35 108.8(11) . . ? C37 N9 C35 108.8(11) 3 . ? C37 N9 Li3 114.0(6) . . ? C37 N9 Li3 114.0(6) 3 . ? C35 N9 Li3 102.4(9) . . ? C40 N10 C40 112.3(19) . 3 ? C40 N10 C38 109.9(8) . . ? C40 N10 C38 109.9(8) 3 . ? C40 N10 Li4 110.7(8) . . ? C40 N10 Li4 110.7(8) 3 . ? C38 N10 Li4 103.2(7) . . ? C41 N11 C41 114.7(17) . 3 ? C41 N11 C39 107.7(8) . . ? C41 N11 C39 107.7(8) 3 . ? C41 N11 Li4 110.2(6) . . ? C41 N11 Li4 110.2(6) 3 . ? C39 N11 Li4 105.7(9) . . ? N1 C1 C6 125.3(5) . . ? N1 C1 C2 117.9(4) . . ? C6 C1 C2 116.8(5) . . ? N1 C1 Li2 59.1(3) . . ? C6 C1 Li2 141.7(4) . . ? C2 C1 Li2 73.0(3) . . ? N1 C1 Li1 55.9(3) . . ? C6 C1 Li1 146.4(4) . . ? C2 C1 Li1 73.5(3) . . ? Li2 C1 Li1 71.0(3) . . ? C3 C2 N2 125.7(5) . . ? C3 C2 C1 117.6(5) . . ? N2 C2 C1 116.7(4) . . ? C3 C2 Li2 141.3(4) . . ? N2 C2 Li2 59.1(3) . . ? C1 C2 Li2 71.8(3) . . ? C3 C2 Li1 147.3(4) . . ? N2 C2 Li1 55.4(3) . . ? C1 C2 Li1 72.9(3) . . ? Li2 C2 Li1 70.6(3) . . ? C4 C3 C2 123.4(5) . . ? C5 C4 C3 120.1(5) . . ? C4 C5 C6 118.6(6) . . ? C5 C6 C1 123.5(6) . . ? C8 C7 Si1 127.0(7) . . ? C12 C11 Si2 126.0(7) . . ? N3 C15 C16 121.2(7) . . ? C15 C16 N4 120.0(6) . . ? C22 C21 N5 119.4(7) . . ? C21 C22 N6 119.6(8) . . ? N7 C27 C28 124.5(4) . . ? N7 C27 C27 118.0(2) . 3 ? C28 C27 C27 117.5(3) . 3 ? N7 C27 Li3 56.5(3) . . ? C28 C27 Li3 145.6(5) . . ? C27 C27 Li3 72.99(15) 3 . ? N7 C27 Li4 55.7(3) . . ? C28 C27 Li4 147.1(5) . . ? C27 C27 Li4 73.10(13) 3 . ? Li3 C27 Li4 65.9(4) . . ? C29 C28 C27 122.7(5) . . ? C29 C29 C28 119.8(3) 3 . ? C31 C30 Si3 131.1(11) . . ? C35 C34 N8 117.6(10) . . ? C34 C35 N9 131.1(13) . . ? C39 C38 N10 124.1(11) . . ? C38 C39 N11 124.5(12) . . ? N2 Li1 N1 82.6(4) . . ? N2 Li1 N4 113.6(4) . . ? N1 Li1 N4 113.8(4) . . ? N2 Li1 N3 132.6(5) . . ? N1 Li1 N3 132.0(5) . . ? N4 Li1 N3 84.1(4) . . ? N2 Li1 C1 63.3(3) . . ? N1 Li1 C1 33.7(2) . . ? N4 Li1 C1 95.0(4) . . ? N3 Li1 C1 162.8(5) . . ? N2 Li1 C2 33.9(2) . . ? N1 Li1 C2 63.3(3) . . ? N4 Li1 C2 94.8(3) . . ? N3 Li1 C2 163.5(5) . . ? C1 Li1 C2 33.6(2) . . ? N2 Li1 Li2 46.7(3) . . ? N1 Li1 Li2 46.3(3) . . ? N4 Li1 Li2 146.0(5) . . ? N3 Li1 Li2 129.9(4) . . ? C1 Li1 Li2 52.7(3) . . ? C2 Li1 Li2 53.0(3) . . ? N1 Li2 N2 82.8(3) . . ? N1 Li2 N5 129.9(5) . . ? N2 Li2 N5 130.3(5) . . ? N1 Li2 N6 116.7(4) . . ? N2 Li2 N6 117.3(5) . . ? N5 Li2 N6 83.7(4) . . ? N1 Li2 C1 35.5(2) . . ? N2 Li2 C1 65.4(3) . . ? N5 Li2 C1 162.2(5) . . ? N6 Li2 C1 96.1(4) . . ? N1 Li2 C2 65.6(3) . . ? N2 Li2 C2 35.5(2) . . ? N5 Li2 C2 162.6(5) . . ? N6 Li2 C2 96.2(4) . . ? C1 Li2 C2 35.2(2) . . ? N1 Li2 Li1 46.7(3) . . ? N2 Li2 Li1 46.5(3) . . ? N5 Li2 Li1 125.4(5) . . ? N6 Li2 Li1 151.0(4) . . ? C1 Li2 Li1 56.4(3) . . ? C2 Li2 Li1 56.4(3) . . ? N7 Li3 N7 83.7(6) . 3 ? N7 Li3 N9 115.7(5) . . ? N7 Li3 N9 115.7(5) 3 . ? N7 Li3 N8 130.7(5) . . ? N7 Li3 N8 130.7(5) 3 . ? N9 Li3 N8 83.4(6) . . ? N7 Li3 C27 64.1(4) . 3 ? N7 Li3 C27 34.2(3) 3 3 ? N9 Li3 C27 97.7(6) . 3 ? N8 Li3 C27 162.9(2) . 3 ? N7 Li3 C27 34.2(3) . . ? N7 Li3 C27 64.1(4) 3 . ? N9 Li3 C27 97.7(6) . . ? N8 Li3 C27 162.9(2) . . ? C27 Li3 C27 34.0(3) 3 . ? N7 Li3 Li4 49.0(3) . . ? N7 Li3 Li4 49.0(3) 3 . ? N9 Li3 Li4 153.7(7) . . ? N8 Li3 Li4 122.9(7) . . ? C27 Li3 Li4 57.3(4) 3 . ? C27 Li3 Li4 57.3(4) . . ? N7 Li4 N7 84.0(5) . 3 ? N7 Li4 N11 116.3(5) . . ? N7 Li4 N11 116.3(5) 3 . ? N7 Li4 N10 130.4(4) . . ? N7 Li4 N10 130.4(4) 3 . ? N11 Li4 N10 82.6(5) . . ? N7 Li4 C27 34.0(2) . . ? N7 Li4 C27 63.9(4) 3 . ? N11 Li4 C27 99.5(5) . . ? N10 Li4 C27 162.9(2) . . ? N7 Li4 C27 63.9(4) . 3 ? N7 Li4 C27 34.0(2) 3 3 ? N11 Li4 C27 99.5(5) . 3 ? N10 Li4 C27 162.9(2) . 3 ? C27 Li4 C27 33.8(3) . 3 ? N7 Li4 Li3 49.2(3) . . ? N7 Li4 Li3 49.2(3) 3 . ? N11 Li4 Li3 155.0(7) . . ? N10 Li4 Li3 122.4(6) . . ? C27 Li4 Li3 56.8(4) . . ? C27 Li4 Li3 56.8(4) 3 . ? _refine_diff_density_max 0.708 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.066 #===END