Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_category FM loop_ _publ_author_name 'M. F. Lappert' 'P. B. Hitchcock' 'J. D. Farwell' 'X. H. Wei' data_(2)-nov302 _database_code_depnum_ccdc_archive 'CCDC 665648' _audit_creation_date 2002-11-01T11:07:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (O(Li(thf)2(SiMeNCPhC(SiMe3)CPhN))2) _chemical_formula_moiety 'C54 H76 Li2 N4 O5 Si4' _chemical_formula_sum 'C54 H76 Li2 N4 O5 Si4' _chemical_formula_weight 987.43 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/mnm _symmetry_space_group_name_Hall '-P 4n 2n' _symmetry_Int_Tables_number 136 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-y, -x, -z' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-y, -x, z' '-y-1/2, x-1/2, -z-1/2' 'y-1/2, -x-1/2, -z-1/2' 'y, x, z' _cell_length_a 19.9377(1) _cell_length_b 19.9377(1) _cell_length_c 16.6530(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6619.77(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 49032 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.13 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_unetI/netI 0.0171 _diffrn_reflns_number 66549 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 3119 _reflns_number_gt 2788 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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 ; There is very weak diffuse residual density(< 1 e/angstrom cubed) , not associated with the complex. This is probably very disordered thf solvate molecules. Attempts to model this density were not successful and were abandoned. 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^)+(0.1564P)^2^+7.7157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3119 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2961 _refine_ls_wR_factor_gt 0.2847 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.642 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # 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 Li Li 0.8603(4) 0.3188(5) 0 0.055(2) Uani 1 2 d S . . Si1 Si 0.72126(4) 0.27874(4) 0.08986(7) 0.0346(4) Uani 1 2 d S . . Si2 Si 0.79358(7) 0.20642(7) 0.32454(10) 0.0869(8) Uani 1 2 d S . . O1 O 0.69809(14) 0.30191(14) 0 0.0357(9) Uani 1 4 d S . . O2 O 0.94462(19) 0.2696(2) 0 0.0637(11) Uani 1 2 d S . . O3 O 0.8651(2) 0.4186(2) 0 0.0905(16) Uani 1 2 d S . . N4 N 0.80582(14) 0.29134(15) 0.10259(17) 0.0462(7) Uani 1 1 d . . . C1 C 0.7899(2) 0.2101(2) 0.2128(3) 0.0617(15) Uani 1 2 d S . . C2 C 0.82686(18) 0.2600(2) 0.1684(2) 0.0551(10) Uani 1 1 d . . . C3 C 0.8976(2) 0.2745(3) 0.1943(3) 0.0813(16) Uani 1 1 d . . . C4 C 0.9386(3) 0.2223(4) 0.2230(3) 0.111(2) Uani 1 1 d . . . H4 H 0.9218 0.1783 0.2252 0.133 Uiso 1 1 calc R . . C5 C 1.0030(4) 0.2351(7) 0.2477(5) 0.161(5) Uani 1 1 d . . . H5 H 1.0297 0.2004 0.2684 0.194 Uiso 1 1 calc R . . C6 C 1.0284(4) 0.2997(7) 0.2422(5) 0.160(5) Uani 1 1 d . . . H6 H 1.0726 0.3085 0.2586 0.192 Uiso 1 1 calc R . . C7 C 0.9898(3) 0.3500(6) 0.2131(5) 0.151(4) Uani 1 1 d . . . H7 H 1.0073 0.3937 0.2102 0.181 Uiso 1 1 calc R . . C8 C 0.9234(2) 0.3376(4) 0.1873(3) 0.099(2) Uani 1 1 d . . . H8 H 0.8974 0.3724 0.1655 0.119 Uiso 1 1 calc R . . C9 C 0.8541(4) 0.1459(4) 0.3751(5) 0.165(6) Uani 1 2 d S . . H9A H 0.8501 0.15 0.433 0.247 Uiso 1 2 calc SR . . H9B H 0.8997 0.1565 0.359 0.247 Uiso 0.5 1 calc PR . . H9C H 0.8434 0.1003 0.3592 0.247 Uiso 0.5 1 calc PR . . C10 C 0.7070(4) 0.1866(4) 0.3631(3) 0.114(2) Uani 1 1 d . . . H10C H 0.7071 0.1878 0.4214 0.17 Uiso 1 1 calc R . . H10B H 0.6938 0.1422 0.3451 0.17 Uiso 1 1 calc R . . H10A H 0.6754 0.2195 0.3428 0.17 Uiso 1 1 calc R . . C11 C 1.0140(3) 0.2904(4) 0 0.083(2) Uani 1 2 d S . . H11B H 1.0241 0.3172 0.0479 0.1 Uiso 0.5 1 calc PR . . H11A H 1.0241 0.3172 -0.0479 0.1 Uiso 0.5 1 calc PR . . C12 C 1.0536(6) 0.2259(7) 0 0.152(5) Uani 1 2 d S . . H12B H 1.0824 0.2241 -0.0477 0.183 Uiso 0.5 1 calc PR . . H12A H 1.0824 0.2241 0.0477 0.183 Uiso 0.5 1 calc PR . . C13 C 1.0100(6) 0.1711(6) 0 0.161(5) Uani 1 2 d S . . H13B H 1.0174 0.1434 0.0478 0.194 Uiso 0.5 1 calc PR . . H13A H 1.0174 0.1434 -0.0478 0.194 Uiso 0.5 1 calc PR . . C14 C 0.9409(4) 0.1986(4) 0 0.083(2) Uani 1 2 d S . . H14B H 0.9167 0.1831 -0.0477 0.099 Uiso 0.5 1 calc PR . . H14A H 0.9167 0.1831 0.0477 0.099 Uiso 0.5 1 calc PR . . C15 C 0.8024(5) 0.4520(4) 0 0.123(4) Uani 1 2 d S . . H15B H 0.7767 0.4391 -0.0477 0.148 Uiso 0.5 1 calc PR . . H15A H 0.7767 0.4391 0.0477 0.148 Uiso 0.5 1 calc PR . . C16 C 0.8130(6) 0.5220(5) 0 0.155(5) Uani 1 2 d S . . H16B H 0.7931 0.5426 0.0478 0.186 Uiso 0.5 1 calc PR . . H16A H 0.7931 0.5426 -0.0478 0.186 Uiso 0.5 1 calc PR . . C17 C 0.8840(7) 0.5303(6) 0 0.219(10) Uani 1 2 d S . . H17B H 0.8978 0.5556 -0.0477 0.262 Uiso 0.5 1 calc PR . . H17A H 0.8978 0.5556 0.0477 0.262 Uiso 0.5 1 calc PR . . C18 C 0.9146(5) 0.4676(5) 0 0.135(4) Uani 1 2 d S . . H18B H 0.943 0.4628 -0.0477 0.162 Uiso 0.5 1 calc PR . . H18A H 0.943 0.4628 0.0477 0.162 Uiso 0.5 1 calc PR . . C19 C 0.66983(19) 0.33017(19) 0.1595(3) 0.0527(12) Uani 1 2 d S . . H19C H 0.6788 0.3773 0.1502 0.079 Uiso 0.5 1 calc PR . . H19B H 0.6811 0.3189 0.2145 0.079 Uiso 1 2 calc SR . . H19A H 0.6227 0.3212 0.1502 0.079 Uiso 0.5 1 calc PR . . 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 Li 0.041(4) 0.056(5) 0.069(6) 0 0 -0.011(4) Si1 0.0353(5) 0.0353(5) 0.0332(7) -0.0012(3) 0.0012(3) -0.0056(4) Si2 0.1132(11) 0.1132(11) 0.0344(9) 0.0074(5) -0.0074(5) 0.0416(13) O1 0.0355(13) 0.0355(13) 0.036(2) 0 0 -0.0013(16) O2 0.046(2) 0.070(2) 0.075(3) 0 0 -0.0048(17) O3 0.067(3) 0.058(2) 0.147(5) 0 0 -0.025(2) N4 0.0368(14) 0.0611(18) 0.0408(16) -0.0022(13) -0.0020(11) -0.0049(12) C1 0.073(2) 0.073(2) 0.038(3) 0.0050(16) -0.0050(16) 0.022(3) C2 0.0456(19) 0.082(3) 0.0382(18) -0.0088(17) -0.0070(15) 0.0082(17) C3 0.048(2) 0.150(5) 0.046(2) -0.027(3) -0.0147(18) 0.015(3) C4 0.074(3) 0.188(7) 0.070(3) -0.024(4) -0.030(3) 0.051(4) C5 0.082(5) 0.288(13) 0.114(6) -0.068(7) -0.059(4) 0.078(6) C6 0.057(4) 0.303(15) 0.120(6) -0.089(8) -0.038(4) 0.025(6) C7 0.068(4) 0.275(11) 0.109(5) -0.096(6) -0.006(4) -0.025(5) C8 0.054(3) 0.173(6) 0.070(3) -0.042(3) -0.002(2) -0.029(3) C9 0.219(9) 0.219(9) 0.056(5) 0.031(3) -0.031(3) 0.112(11) C10 0.162(6) 0.132(5) 0.047(3) 0.013(3) 0.030(3) 0.014(4) C11 0.049(3) 0.112(6) 0.089(5) 0 0 -0.012(3) C12 0.091(7) 0.162(12) 0.204(14) 0 0 0.054(7) C13 0.108(8) 0.107(8) 0.269(18) 0 0 0.038(7) C14 0.102(5) 0.075(4) 0.071(4) 0 0 -0.006(4) C15 0.090(6) 0.063(5) 0.216(12) 0 0 -0.012(4) C16 0.144(10) 0.069(5) 0.253(16) 0 0 -0.012(6) C17 0.129(10) 0.076(7) 0.45(3) 0 0 -0.041(7) C18 0.104(7) 0.081(6) 0.221(13) 0 0 -0.048(5) C19 0.0541(17) 0.0541(17) 0.050(3) -0.0088(16) 0.0088(16) -0.004(2) #----------------------------------------------------------------------------# # 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 Li O2 1.947(10) . ? Li O3 1.992(10) . ? Li N4 2.097(5) 11 ? Li N4 2.097(5) . ? Si1 O1 1.633(2) . ? Si1 N4 1.718(3) . ? Si1 N4 1.718(3) 13_665 ? Si1 C19 1.857(5) . ? Si2 C1 1.863(6) . ? Si2 C10 1.884(7) 13_665 ? Si2 C10 1.884(7) . ? Si2 C9 1.904(9) . ? O1 Si1 1.633(2) 11 ? O2 C14 1.416(8) . ? O2 C11 1.444(7) . ? O3 C18 1.390(8) . ? O3 C15 1.416(10) . ? N4 C2 1.330(5) . ? C1 C2 1.442(5) 13_665 ? C1 C2 1.442(5) . ? C2 C3 1.503(5) . ? C3 C8 1.364(8) . ? C3 C4 1.408(8) . ? C4 C5 1.372(10) . ? C5 C6 1.386(14) . ? C6 C7 1.355(14) . ? C7 C8 1.412(8) . ? C11 C12 1.510(13) . ? C12 C13 1.395(16) . ? C13 C14 1.483(13) . ? C15 C16 1.412(12) . ? C16 C17 1.426(16) . ? C17 C18 1.392(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li O3 117.5(4) . . ? O2 Li N4 108.4(3) . 11 ? O3 Li N4 106.6(3) . 11 ? O2 Li N4 108.4(3) . . ? O3 Li N4 106.6(3) . . ? N4 Li N4 109.1(4) 11 . ? O1 Si1 N4 110.46(13) . . ? O1 Si1 N4 110.46(13) . 13_665 ? N4 Si1 N4 105.8(2) . 13_665 ? O1 Si1 C19 105.1(2) . . ? N4 Si1 C19 112.59(14) . . ? N4 Si1 C19 112.59(14) 13_665 . ? C1 Si2 C10 108.2(2) . 13_665 ? C1 Si2 C10 108.2(2) . . ? C10 Si2 C10 105.6(5) 13_665 . ? C1 Si2 C9 119.5(4) . . ? C10 Si2 C9 107.3(3) 13_665 . ? C10 Si2 C9 107.3(3) . . ? Si1 O1 Si1 132.8(3) . 11 ? C14 O2 C11 109.7(5) . . ? C14 O2 Li 117.3(5) . . ? C11 O2 Li 133.0(5) . . ? C18 O3 C15 107.3(7) . . ? C18 O3 Li 137.4(6) . . ? C15 O3 Li 115.3(5) . . ? C2 N4 Si1 110.0(2) . . ? C2 N4 Li 129.1(3) . . ? Si1 N4 Li 116.5(2) . . ? C2 C1 C2 116.2(5) 13_665 . ? C2 C1 Si2 121.3(2) 13_665 . ? C2 C1 Si2 121.3(2) . . ? N4 C2 C1 125.9(3) . . ? N4 C2 C3 116.2(4) . . ? C1 C2 C3 117.7(4) . . ? C8 C3 C4 119.4(5) . . ? C8 C3 C2 120.5(5) . . ? C4 C3 C2 120.0(6) . . ? C5 C4 C3 120.5(9) . . ? C4 C5 C6 119.7(9) . . ? C7 C6 C5 120.2(7) . . ? C6 C7 C8 120.7(9) . . ? C3 C8 C7 119.3(7) . . ? O2 C11 C12 104.8(8) . . ? C13 C12 C11 110.0(9) . . ? C12 C13 C14 106.8(9) . . ? O2 C14 C13 108.7(7) . . ? C16 C15 O3 109.5(8) . . ? C15 C16 C17 105.3(10) . . ? C18 C17 C16 109.4(9) . . ? O3 C18 C17 108.6(9) . . ? #===END data_(3)-may502 _database_code_depnum_ccdc_archive 'CCDC 665649' _audit_creation_date 2002-05-02T14:34:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (O(SiMeNCPhCHCPhNLi(thf)2)2).(thf) _chemical_formula_moiety 'C48 H60 Li2 N4 O5 Si2, C4 H8 O1' _chemical_formula_sum 'C52 H68 Li2 N4 O6 Si2' _chemical_formula_weight 915.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 20.4546(5) _cell_length_b 14.9128(4) _cell_length_c 17.1049(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5217.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15438 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_number 21730 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 3756 _reflns_number_gt 2792 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0912P)^2^+4.1191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3756 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.179 _refine_ls_wR_factor_gt 0.1611 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.06 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.332 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # 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 Li1 Li 0.2009(3) 0.25 0.2417(4) 0.0415(17) Uani 1 2 d S . . Li2 Li 0.2072(3) 0.25 0.5384(4) 0.0444(18) Uani 1 2 d S . . Si Si 0.27071(4) 0.14975(6) 0.38782(4) 0.0374(3) Uani 1 1 d . . . O1 O 0.30270(12) 0.25 0.38688(14) 0.0389(7) Uani 1 2 d S . . O2 O 0.26413(16) 0.25 0.63274(18) 0.0610(10) Uani 1 2 d S . . O3 O 0.11344(14) 0.25 0.57108(16) 0.0529(9) Uani 1 2 d S . . O4 O 0.24770(14) 0.25 0.14146(17) 0.0555(9) Uani 1 2 d S . . O5 O 0.10501(13) 0.25 0.22764(16) 0.0490(8) Uani 1 2 d S . . N1 N 0.22156(11) 0.13400(17) 0.30683(13) 0.0394(6) Uani 1 1 d . . . N2 N 0.22260(11) 0.13511(17) 0.46947(13) 0.0388(6) Uani 1 1 d . . . C1 C 0.17860(14) 0.0678(2) 0.31649(17) 0.0424(8) Uani 1 1 d . . . C2 C 0.16317(16) 0.0272(2) 0.38903(17) 0.0468(8) Uani 1 1 d . . . H2 H 0.1407 -0.0286 0.3894 0.056 Uiso 1 1 calc R . . C3 C 0.18049(14) 0.0678(2) 0.46101(16) 0.0426(8) Uani 1 1 d . . . C4 C 0.14219(15) 0.0373(2) 0.24515(17) 0.0458(8) Uani 1 1 d . . . C5 C 0.07971(17) 0.0014(3) 0.2476(2) 0.0652(11) Uani 1 1 d . . . H5 H 0.0587 -0.006 0.2967 0.078 Uiso 1 1 calc R . . C6 C 0.04713(19) -0.0241(3) 0.1799(2) 0.0804(13) Uani 1 1 d . . . H6 H 0.004 -0.0476 0.1829 0.096 Uiso 1 1 calc R . . C7 C 0.0772(2) -0.0153(3) 0.1085(2) 0.0773(13) Uani 1 1 d . . . H7 H 0.0552 -0.0333 0.0622 0.093 Uiso 1 1 calc R . . C8 C 0.1393(2) 0.0197(3) 0.1044(2) 0.0672(11) Uani 1 1 d . . . H8 H 0.1603 0.0257 0.0551 0.081 Uiso 1 1 calc R . . C9 C 0.17154(16) 0.0463(2) 0.17196(18) 0.0522(9) Uani 1 1 d . . . H9 H 0.2142 0.071 0.1683 0.063 Uiso 1 1 calc R . . C10 C 0.14765(14) 0.0346(2) 0.53415(17) 0.0443(8) Uani 1 1 d . . . C11 C 0.08680(16) -0.0077(3) 0.53393(19) 0.0576(10) Uani 1 1 d . . . H11 H 0.0644 -0.0162 0.4859 0.069 Uiso 1 1 calc R . . C12 C 0.05872(18) -0.0376(3) 0.6030(2) 0.0668(11) Uani 1 1 d . . . H12 H 0.0171 -0.0658 0.6019 0.08 Uiso 1 1 calc R . . C13 C 0.09077(18) -0.0265(3) 0.6731(2) 0.0669(11) Uani 1 1 d . . . H13 H 0.0713 -0.0467 0.7204 0.08 Uiso 1 1 calc R . . C14 C 0.15128(17) 0.0141(3) 0.67411(19) 0.0619(10) Uani 1 1 d . . . H14 H 0.1741 0.0208 0.7221 0.074 Uiso 1 1 calc R . . C15 C 0.17895(16) 0.0452(2) 0.60545(17) 0.0518(9) Uani 1 1 d . . . H15 H 0.2202 0.0743 0.6072 0.062 Uiso 1 1 calc R . . C16 C 0.34174(15) 0.0718(3) 0.38847(18) 0.0537(9) Uani 1 1 d . . . H16A H 0.326 0.0097 0.3891 0.081 Uiso 1 1 calc R . . H16B H 0.3684 0.0829 0.4351 0.081 Uiso 1 1 calc R . . H16C H 0.3683 0.0816 0.3415 0.081 Uiso 1 1 calc R . . C17 C 0.3314(3) 0.25 0.6187(3) 0.0773(17) Uani 1 2 d S . . H17A H 0.3441 0.3039 0.5885 0.093 Uiso 0.5 1 calc PR . . H17B H 0.3441 0.1961 0.5885 0.093 Uiso 0.5 1 calc PR . . C18 C 0.3641(4) 0.25 0.6963(4) 0.114(3) Uani 1 2 d S . . H18A H 0.3919 0.1961 0.7021 0.136 Uiso 0.5 1 calc PR . . H18B H 0.3919 0.3039 0.7021 0.136 Uiso 0.5 1 calc PR . . C19 C 0.3135(4) 0.25 0.7538(4) 0.145(4) Uani 1 2 d S . . H19A H 0.3169 0.1961 0.7873 0.174 Uiso 0.5 1 calc PR . . H19B H 0.3169 0.3039 0.7873 0.174 Uiso 0.5 1 calc PR . . C20 C 0.2537(3) 0.25 0.7136(3) 0.126(3) Uani 1 2 d S . . H20A H 0.2282 0.1963 0.7284 0.152 Uiso 0.5 1 calc PR . . H20B H 0.2282 0.3037 0.7284 0.152 Uiso 0.5 1 calc PR . . C21 C 0.0830(2) 0.25 0.6469(3) 0.0736(17) Uani 1 2 d S . . H21A H 0.0962 0.1961 0.6768 0.088 Uiso 0.5 1 calc PR . . H21B H 0.0962 0.3039 0.6768 0.088 Uiso 0.5 1 calc PR . . C22 C 0.0140(3) 0.25 0.6345(5) 0.154(4) Uani 1 2 d S . . H22A H -0.0056 0.1962 0.6589 0.185 Uiso 0.5 1 calc PR . . H22B H -0.0056 0.3038 0.6589 0.185 Uiso 0.5 1 calc PR . . C23 C 0.0015(3) 0.25 0.5545(5) 0.137(4) Uani 1 2 d S . . H23A H -0.0242 0.3038 0.5402 0.164 Uiso 0.5 1 calc PR . . H23B H -0.0242 0.1962 0.5402 0.164 Uiso 0.5 1 calc PR . . C24 C 0.0639(2) 0.25 0.5124(3) 0.0675(15) Uani 1 2 d S . . H24A H 0.0677 0.196 0.479 0.081 Uiso 0.5 1 calc PR . . H24B H 0.0677 0.304 0.479 0.081 Uiso 0.5 1 calc PR . . C25 C 0.3162(2) 0.25 0.1489(3) 0.0753(17) Uani 1 2 d S . . H25A H 0.331 0.1961 0.1777 0.09 Uiso 0.5 1 calc PR . . H25B H 0.331 0.3039 0.1777 0.09 Uiso 0.5 1 calc PR . . C26 C 0.3426(4) 0.25 0.0683(5) 0.116(3) Uani 1 2 d S . . H26A H 0.3698 0.3039 0.0594 0.14 Uiso 0.5 1 calc PR . . H26B H 0.3698 0.1961 0.0594 0.14 Uiso 0.5 1 calc PR . . C27 C 0.2889(4) 0.25 0.0180(4) 0.187(6) Uani 1 2 d S . . H27A H 0.2905 0.1963 -0.0159 0.225 Uiso 0.5 1 calc PR . . H27B H 0.2905 0.3037 -0.0159 0.225 Uiso 0.5 1 calc PR . . C28 C 0.2295(3) 0.25 0.0617(3) 0.097(2) Uani 1 2 d S . . H28A H 0.2032 0.3039 0.0493 0.116 Uiso 0.5 1 calc PR . . H28B H 0.2032 0.1961 0.0493 0.116 Uiso 0.5 1 calc PR . . C29 C 0.0647(2) 0.25 0.1590(3) 0.0633(14) Uani 1 2 d S . . H29A H 0.0733 0.196 0.1269 0.076 Uiso 0.5 1 calc PR . . H29B H 0.0733 0.304 0.1269 0.076 Uiso 0.5 1 calc PR . . C30 C -0.0032(3) 0.25 0.1874(5) 0.150(4) Uani 1 2 d S . . H30A H -0.0263 0.3038 0.1678 0.18 Uiso 0.5 1 calc PR . . H30B H -0.0263 0.1962 0.1678 0.18 Uiso 0.5 1 calc PR . . C31 C -0.0036(3) 0.25 0.2678(5) 0.099(2) Uani 1 2 d S . . H31A H -0.0266 0.1962 0.2875 0.119 Uiso 0.5 1 calc PR . . H31B H -0.0266 0.3038 0.2875 0.119 Uiso 0.5 1 calc PR . . C32 C 0.0654(2) 0.25 0.2960(3) 0.0640(15) Uani 1 2 d S . . H32A H 0.0742 0.3039 0.328 0.077 Uiso 0.5 1 calc PR . . H32B H 0.0742 0.1961 0.328 0.077 Uiso 0.5 1 calc PR . . O6 O 0.0321(8) 0.25 -0.0706(12) 0.380(13) Uani 1 2 d S . . C33 C 0.1206(5) 0.2984(5) -0.1278(4) 0.185(4) Uani 1 1 d . . . H33A H 0.1646 0.3216 -0.1152 0.222 Uiso 1 1 calc R . . H33B H 0.1073 0.3216 -0.1796 0.222 Uiso 1 1 calc R . . C34 C 0.0748(6) 0.3247(7) -0.0695(6) 0.191(5) Uani 1 1 d . . . H34A H 0.0519 0.3808 -0.084 0.229 Uiso 1 1 calc R . . H34B H 0.0959 0.3322 -0.0178 0.229 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.036(4) 0.062(5) 0.026(3) 0 -0.002(3) 0 Li2 0.038(4) 0.069(5) 0.027(4) 0 0.002(3) 0 Si 0.0328(5) 0.0545(6) 0.0249(5) 0.0008(4) 0.0012(3) 0.0042(4) O1 0.0299(15) 0.0573(19) 0.0294(15) 0 0.0011(11) 0 O2 0.053(2) 0.093(3) 0.0361(18) 0 -0.0104(14) 0 O3 0.0432(17) 0.081(2) 0.0345(17) 0 0.0045(13) 0 O4 0.0454(18) 0.088(3) 0.0328(17) 0 0.0064(14) 0 O5 0.0347(16) 0.076(2) 0.0360(17) 0 0.0029(13) 0 N1 0.0360(13) 0.0549(17) 0.0272(13) -0.0016(11) 0.0011(10) 0.0011(13) N2 0.0360(13) 0.0516(17) 0.0288(13) 0.0038(11) 0.0003(10) 0.0021(13) C1 0.0415(17) 0.051(2) 0.0351(17) -0.0064(15) -0.0008(13) 0.0057(16) C2 0.053(2) 0.047(2) 0.0407(19) -0.0010(15) 0.0026(14) -0.0049(16) C3 0.0408(17) 0.053(2) 0.0336(17) 0.0083(15) 0.0021(13) 0.0093(16) C4 0.0459(18) 0.049(2) 0.0428(18) -0.0091(15) -0.0023(14) 0.0030(16) C5 0.060(2) 0.083(3) 0.053(2) -0.020(2) 0.0033(17) -0.010(2) C6 0.063(3) 0.104(4) 0.074(3) -0.036(3) -0.005(2) -0.021(2) C7 0.079(3) 0.097(3) 0.056(3) -0.034(2) -0.015(2) -0.004(3) C8 0.074(3) 0.083(3) 0.044(2) -0.0210(19) -0.0043(17) -0.004(2) C9 0.055(2) 0.062(2) 0.0400(18) -0.0139(16) -0.0015(15) 0.0013(17) C10 0.0431(18) 0.050(2) 0.0397(18) 0.0130(15) 0.0027(13) 0.0047(15) C11 0.052(2) 0.076(3) 0.044(2) 0.0156(18) -0.0032(15) -0.0049(19) C12 0.052(2) 0.089(3) 0.059(2) 0.024(2) 0.0019(17) -0.014(2) C13 0.059(2) 0.092(3) 0.050(2) 0.028(2) 0.0053(17) -0.001(2) C14 0.057(2) 0.091(3) 0.0384(19) 0.0209(19) -0.0039(15) -0.002(2) C15 0.0445(18) 0.070(2) 0.0412(19) 0.0147(17) 0.0004(14) -0.0017(17) C16 0.0469(19) 0.074(2) 0.0398(18) -0.0010(17) 0.0011(14) 0.0167(18) C17 0.053(3) 0.107(5) 0.072(4) 0 -0.007(3) 0 C18 0.091(5) 0.153(7) 0.097(6) 0 -0.048(5) 0 C19 0.101(6) 0.275(13) 0.058(4) 0 -0.030(4) 0 C20 0.093(5) 0.250(11) 0.037(4) 0 -0.016(3) 0 C21 0.056(3) 0.117(5) 0.047(3) 0 0.020(2) 0 C22 0.052(4) 0.305(14) 0.107(6) 0 0.028(4) 0 C23 0.047(4) 0.253(11) 0.111(6) 0 -0.015(4) 0 C24 0.065(3) 0.080(4) 0.058(3) 0 -0.022(3) 0 C25 0.042(3) 0.100(5) 0.084(4) 0 0.013(3) 0 C26 0.084(5) 0.156(8) 0.110(6) 0 0.052(5) 0 C27 0.114(7) 0.399(19) 0.049(5) 0 0.032(5) 0 C28 0.086(4) 0.167(7) 0.036(3) 0 0.009(3) 0 C29 0.049(3) 0.083(4) 0.058(3) 0 -0.016(2) 0 C30 0.040(4) 0.287(13) 0.122(7) 0 -0.015(4) 0 C31 0.054(4) 0.116(6) 0.128(6) 0 0.038(4) 0 C32 0.056(3) 0.081(4) 0.056(3) 0 0.022(2) 0 O6 0.220(14) 0.51(4) 0.41(2) 0 -0.131(15) 0 C33 0.322(12) 0.130(6) 0.104(5) 0.011(4) 0.038(6) -0.066(7) C34 0.273(13) 0.149(8) 0.150(8) -0.038(6) -0.103(8) 0.088(8) #----------------------------------------------------------------------------# # 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 O4 1.964(7) . ? Li1 O5 1.977(7) . ? Li1 N1 2.100(4) . ? Li2 O2 1.990(7) . ? Li2 O3 1.998(7) . ? Li2 N2 2.103(4) . ? Si O1 1.6320(14) . ? Si N2 1.722(2) . ? Si N1 1.728(2) . ? Si C16 1.861(3) . ? O2 C17 1.398(6) . ? O2 C20 1.399(6) . ? O3 C24 1.426(5) . ? O3 C21 1.439(5) . ? O4 C25 1.407(6) . ? O4 C28 1.415(6) . ? O5 C32 1.423(5) . ? O5 C29 1.435(5) . ? N1 C1 1.332(4) . ? N2 C3 1.331(4) . ? C1 C2 1.417(4) . ? C1 C4 1.501(4) . ? C2 C3 1.417(4) . ? C3 C10 1.503(4) . ? C4 C5 1.386(5) . ? C4 C9 1.395(4) . ? C5 C6 1.390(5) . ? C6 C7 1.374(5) . ? C7 C8 1.375(6) . ? C8 C9 1.388(4) . ? C10 C15 1.386(4) . ? C10 C11 1.396(4) . ? C11 C12 1.387(4) . ? C12 C13 1.377(5) . ? C13 C14 1.378(5) . ? C14 C15 1.383(4) . ? C17 C18 1.487(8) . ? C18 C19 1.428(10) . ? C19 C20 1.402(9) . ? C21 C22 1.427(8) . ? C22 C23 1.392(10) . ? C23 C24 1.466(8) . ? C25 C26 1.482(9) . ? C26 C27 1.395(10) . ? C27 C28 1.426(9) . ? C29 C30 1.472(8) . ? C30 C31 1.375(10) . ? C31 C32 1.490(8) . ? O6 C34 1.415(14) . ? C33 C34 1.423(12) . ? C33 C33 1.442(15) 8_565 ? 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 O4 Li1 O5 112.2(3) . . ? O4 Li1 N1 111.4(2) . . ? O5 Li1 N1 105.3(2) . . ? N1 Li1 N1 110.9(3) 8_565 . ? O2 Li2 O3 109.6(3) . . ? O2 Li2 N2 111.5(2) . . ? O3 Li2 N2 107.5(2) . . ? N2 Li2 N2 109.1(3) . 8_565 ? O1 Si N2 110.68(13) . . ? O1 Si N1 110.49(13) . . ? N2 Si N1 107.49(12) . . ? O1 Si C16 105.04(15) . . ? N2 Si C16 111.22(13) . . ? N1 Si C16 111.97(13) . . ? Si O1 Si 132.71(17) 8_565 . ? C17 O2 C20 108.7(4) . . ? C17 O2 Li2 115.9(3) . . ? C20 O2 Li2 135.5(4) . . ? C24 O3 C21 109.1(4) . . ? C24 O3 Li2 119.0(3) . . ? C21 O3 Li2 131.9(3) . . ? C25 O4 C28 110.5(4) . . ? C25 O4 Li1 113.9(3) . . ? C28 O4 Li1 135.6(4) . . ? C32 O5 C29 110.2(3) . . ? C32 O5 Li1 117.7(3) . . ? C29 O5 Li1 132.1(3) . . ? C1 N1 Si 112.66(19) . . ? C1 N1 Li1 122.9(2) . . ? Si N1 Li1 115.5(2) . . ? C3 N2 Si 112.16(19) . . ? C3 N2 Li2 125.4(3) . . ? Si N2 Li2 115.9(2) . . ? N1 C1 C2 124.9(3) . . ? N1 C1 C4 116.9(3) . . ? C2 C1 C4 118.1(3) . . ? C1 C2 C3 121.5(3) . . ? N2 C3 C2 125.3(3) . . ? N2 C3 C10 116.5(3) . . ? C2 C3 C10 118.1(3) . . ? C5 C4 C9 117.5(3) . . ? C5 C4 C1 123.4(3) . . ? C9 C4 C1 119.1(3) . . ? C4 C5 C6 121.5(3) . . ? C7 C6 C5 120.0(4) . . ? C6 C7 C8 119.7(3) . . ? C7 C8 C9 120.3(3) . . ? C8 C9 C4 121.0(3) . . ? C15 C10 C11 117.7(3) . . ? C15 C10 C3 119.2(3) . . ? C11 C10 C3 123.0(3) . . ? C12 C11 C10 120.8(3) . . ? C13 C12 C11 120.4(3) . . ? C12 C13 C14 119.4(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C10 121.3(3) . . ? O2 C17 C18 106.8(5) . . ? C19 C18 C17 106.8(6) . . ? C20 C19 C18 107.1(6) . . ? O2 C20 C19 110.7(6) . . ? C22 C21 O3 107.1(5) . . ? C23 C22 C21 109.2(6) . . ? C22 C23 C24 108.8(5) . . ? O3 C24 C23 105.8(5) . . ? O4 C25 C26 106.1(5) . . ? C27 C26 C25 106.7(5) . . ? C26 C27 C28 110.4(6) . . ? O4 C28 C27 106.3(6) . . ? O5 C29 C30 105.8(5) . . ? C31 C30 C29 109.6(6) . . ? C30 C31 C32 108.6(5) . . ? O5 C32 C31 105.9(5) . . ? C34 O6 C34 103.8(13) . 8_565 ? C34 C33 C33 106.0(6) . 8_565 ? C33 C34 O6 100.4(11) . . ? #===END data_(5)-dec2201 _database_code_depnum_ccdc_archive 'CCDC 665650' _audit_creation_date 2002-01-02T11:02:37-00:00 _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 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety 'C48 H84 Li2 N6 O2 Si4' _chemical_formula_sum 'C48 H84 Li2 N6 O2 Si4' _chemical_formula_weight 903.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7827(9) _cell_length_b 9.7621(4) _cell_length_c 21.3079(12) _cell_angle_alpha 90 _cell_angle_beta 96.894(2) _cell_angle_gamma 90 _cell_volume 2846.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9565 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 21.967 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 11437 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.18 _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 3443 _reflns_number_gt 2753 _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 H atom on N1 was refined. The C11 tBu group is disordered and the lower occupancy methyl C positions were left isotropic. The ether ligand is very poorly defined and diffuse. It was included with disordered, isotropic, C atoms restrained to an idealised geometry using DFIX restraints . 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^)+(0.1190P)^2^+3.4045P] 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 3443 _refine_ls_number_parameters 294 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.425 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.045 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 Li Li 0.9330(5) 0.4244(8) 0.0213(3) 0.0645(19) Uani 1 1 d . . . Si1 Si 0.72522(9) 0.93007(13) 0.19258(6) 0.0605(4) Uani 1 1 d . . . Si2 Si 0.87155(11) 0.53581(14) 0.19068(5) 0.0758(5) Uani 1 1 d . B . O O 0.8505(3) 0.2721(4) -0.0070(2) 0.1037(12) Uani 1 1 d D . . N1 N 0.9231(3) 0.6037(4) -0.04545(19) 0.0644(11) Uani 1 1 d . . . H1 H 0.904(3) 0.631(4) -0.080(2) 0.064(14) Uiso 1 1 d . . . N2 N 0.8586(2) 0.5885(3) 0.04962(14) 0.0467(8) Uani 1 1 d . . . N3 N 0.6642(3) 0.7764(4) 0.18791(16) 0.0649(10) Uani 1 1 d . . . C1 C 0.8534(3) 0.6337(4) -0.00981(18) 0.0477(10) Uani 1 1 d . B . C2 C 0.7626(3) 0.7129(4) -0.02663(17) 0.0485(10) Uani 1 1 d . . . C3 C 0.7255(3) 0.7795(5) -0.08135(19) 0.0672(13) Uani 1 1 d . B . H3 H 0.7602 0.7807 -0.1173 0.081 Uiso 1 1 calc R . . C4 C 0.6360(3) 0.8444(5) -0.0823(2) 0.0780(15) Uani 1 1 d . . . H4 H 0.6082 0.8893 -0.1197 0.094 Uiso 1 1 calc R B . C5 C 0.5868(3) 0.8450(5) -0.0297(2) 0.0692(13) Uani 1 1 d . B . H5 H 0.5253 0.8897 -0.0317 0.083 Uiso 1 1 calc R . . C6 C 0.6253(3) 0.7817(4) 0.02571(19) 0.0562(11) Uani 1 1 d . . . H6 H 0.5918 0.7852 0.0622 0.067 Uiso 1 1 calc R B . C7 C 0.7137(2) 0.7128(4) 0.02720(16) 0.0449(9) Uani 1 1 d . B . C8 C 0.7769(2) 0.6353(4) 0.07650(17) 0.0455(9) Uani 1 1 d . B . C9 C 0.7659(3) 0.6127(4) 0.13817(18) 0.0554(11) Uani 1 1 d . . . C10 C 0.6746(3) 0.6599(5) 0.1657(2) 0.0652(12) Uani 1 1 d . A . C11 C 0.5879(4) 0.5536(5) 0.1681(3) 0.095(2) Uani 1 1 d . . . C15 C 0.7526(4) 0.9699(7) 0.2776(3) 0.103(2) Uani 1 1 d . . . H15A H 0.7790 1.0629 0.2827 0.155 Uiso 1 1 calc R . . H15B H 0.8008 0.9044 0.2974 0.155 Uiso 1 1 calc R . . H15C H 0.6926 0.9633 0.2978 0.155 Uiso 1 1 calc R . . C16 C 0.8384(4) 0.9461(5) 0.1547(3) 0.0819(15) Uani 1 1 d . . . H16A H 0.8241 0.9261 0.1094 0.123 Uiso 1 1 calc R . . H16B H 0.8872 0.8811 0.1741 0.123 Uiso 1 1 calc R . . H16C H 0.8638 1.0396 0.1603 0.123 Uiso 1 1 calc R . . C17 C 0.6342(4) 1.0522(6) 0.1557(3) 0.0962(18) Uani 1 1 d . . . H17A H 0.5743 1.0452 0.1760 0.144 Uiso 1 1 calc R . . H17B H 0.6195 1.0312 0.1106 0.144 Uiso 1 1 calc R . . H17C H 0.6602 1.1455 0.1608 0.144 Uiso 1 1 calc R . . C18 C 0.8545(6) 0.5694(8) 0.2752(2) 0.143(3) Uani 1 1 d . . . H18A H 0.9079 0.5267 0.3030 0.215 Uiso 1 1 calc R B . H18B H 0.7920 0.5306 0.2841 0.215 Uiso 1 1 calc R . . H18C H 0.8546 0.6684 0.2828 0.215 Uiso 1 1 calc R . . C19 C 0.9918(4) 0.6140(6) 0.1792(3) 0.0922(17) Uani 1 1 d . . . H19A H 0.9900 0.7125 0.1879 0.138 Uiso 1 1 calc R B . H19B H 1.0049 0.5996 0.1355 0.138 Uiso 1 1 calc R . . H19C H 1.0436 0.5711 0.2082 0.138 Uiso 1 1 calc R . . C20 C 0.8809(5) 0.3461(6) 0.1769(3) 0.116(2) Uani 1 1 d . . . H20A H 0.9366 0.3090 0.2047 0.174 Uiso 1 1 calc R B . H20B H 0.8904 0.3293 0.1327 0.174 Uiso 1 1 calc R . . H20C H 0.8207 0.3012 0.1862 0.174 Uiso 1 1 calc R . . C12 C 0.4982(6) 0.6332(9) 0.1782(7) 0.184(6) Uani 0.922(9) 1 d P A 1 H12A H 0.5168 0.7134 0.2046 0.276 Uiso 0.922(9) 1 calc PR A 1 H12B H 0.4541 0.5750 0.1994 0.276 Uiso 0.922(9) 1 calc PR A 1 H12C H 0.4649 0.6632 0.1373 0.276 Uiso 0.922(9) 1 calc PR A 1 C13 C 0.6150(8) 0.4603(9) 0.2254(5) 0.170(5) Uani 0.922(9) 1 d P A 1 H13A H 0.5711 0.3809 0.2227 0.254 Uiso 0.922(9) 1 calc PR A 1 H13B H 0.6084 0.5113 0.2643 0.254 Uiso 0.922(9) 1 calc PR A 1 H13C H 0.6826 0.4290 0.2259 0.254 Uiso 0.922(9) 1 calc PR A 1 C14 C 0.5762(6) 0.4700(8) 0.1111(4) 0.133(4) Uani 0.922(9) 1 d P A 1 H14A H 0.5454 0.3828 0.1199 0.200 Uiso 0.922(9) 1 calc PR A 1 H14B H 0.6405 0.4524 0.0974 0.200 Uiso 0.922(9) 1 calc PR A 1 H14C H 0.5351 0.5186 0.0776 0.200 Uiso 0.922(9) 1 calc PR A 1 C21 C 0.7604(8) 0.303(2) -0.0485(7) 0.179(9) Uiso 0.474(13) 1 d PD B 1 H21A H 0.7579 0.2562 -0.0898 0.214 Uiso 0.474(13) 1 calc PR B 1 H21B H 0.7516 0.4032 -0.0554 0.214 Uiso 0.474(13) 1 calc PR B 1 C22 C 0.6860(6) 0.244(3) -0.0075(11) 0.198(10) Uiso 0.474(13) 1 d PD B 1 H22A H 0.6196 0.2614 -0.0281 0.297 Uiso 0.474(13) 1 calc PR B 1 H22B H 0.6945 0.2885 0.0341 0.297 Uiso 0.474(13) 1 calc PR B 1 H22C H 0.6964 0.1455 -0.0025 0.297 Uiso 0.474(13) 1 calc PR B 1 C23 C 0.8791(13) 0.1276(8) -0.0076(8) 0.151(7) Uiso 0.474(13) 1 d PD B 1 H23A H 0.8218 0.0662 -0.0156 0.181 Uiso 0.474(13) 1 calc PR B 1 H23B H 0.9192 0.1004 0.0321 0.181 Uiso 0.474(13) 1 calc PR B 1 C24 C 0.9391(15) 0.1317(16) -0.0638(9) 0.161(8) Uiso 0.474(13) 1 d PD B 1 H24A H 0.9645 0.0399 -0.0710 0.241 Uiso 0.474(13) 1 calc PR B 1 H24B H 0.9938 0.1956 -0.0546 0.241 Uiso 0.474(13) 1 calc PR B 1 H24C H 0.8975 0.1621 -0.1017 0.241 Uiso 0.474(13) 1 calc PR B 1 C13A C 0.628(4) 0.388(5) 0.170(3) 0.054(17) Uiso 0.078(9) 1 d P A 2 H13D H 0.6445 0.3624 0.1282 0.081 Uiso 0.078(9) 1 calc PR A 2 H13E H 0.5759 0.3278 0.1816 0.081 Uiso 0.078(9) 1 calc PR A 2 H13F H 0.6856 0.3793 0.2013 0.081 Uiso 0.078(9) 1 calc PR A 2 C12A C 0.547(4) 0.555(6) 0.237(2) 0.052(16) Uiso 0.078(9) 1 d P A 2 H12D H 0.5040 0.4768 0.2399 0.078 Uiso 0.078(9) 1 calc PR A 2 H12E H 0.5110 0.6404 0.2412 0.078 Uiso 0.078(9) 1 calc PR A 2 H12F H 0.6025 0.5502 0.2701 0.078 Uiso 0.078(9) 1 calc PR A 2 C14A C 0.501(6) 0.565(8) 0.123(4) 0.08(2) Uiso 0.078(9) 1 d P A 2 H14D H 0.5183 0.5531 0.0802 0.125 Uiso 0.078(9) 1 calc PR A 2 H14E H 0.4716 0.6559 0.1268 0.125 Uiso 0.078(9) 1 calc PR A 2 H14F H 0.4539 0.4944 0.1318 0.125 Uiso 0.078(9) 1 calc PR A 2 C21A C 0.7543(6) 0.2534(18) 0.0154(7) 0.154(7) Uiso 0.526(13) 1 d PD B 2 H21C H 0.7510 0.2978 0.0568 0.184 Uiso 0.526(13) 1 calc PR B 2 H21D H 0.7367 0.1554 0.0180 0.184 Uiso 0.526(13) 1 calc PR B 2 C22A C 0.6907(7) 0.327(2) -0.0379(9) 0.201(9) Uiso 0.526(13) 1 d PD B 2 H22D H 0.6224 0.3258 -0.0293 0.302 Uiso 0.526(13) 1 calc PR B 2 H22E H 0.6961 0.2804 -0.0781 0.302 Uiso 0.526(13) 1 calc PR B 2 H22F H 0.7127 0.4221 -0.0405 0.302 Uiso 0.526(13) 1 calc PR B 2 C23A C 0.8594(16) 0.1738(19) -0.0584(7) 0.198(9) Uiso 0.526(13) 1 d PD B 2 H23C H 0.8694 0.2201 -0.0985 0.238 Uiso 0.526(13) 1 calc PR B 2 H23D H 0.8024 0.1117 -0.0655 0.238 Uiso 0.526(13) 1 calc PR B 2 C24A C 0.952(2) 0.099(3) -0.0286(17) 0.38(3) Uiso 0.526(13) 1 d PD B 2 H24D H 0.9712 0.0301 -0.0583 0.576 Uiso 0.526(13) 1 calc PR B 2 H24E H 0.9389 0.0541 0.0106 0.576 Uiso 0.526(13) 1 calc PR B 2 H24F H 1.0052 0.1654 -0.0193 0.576 Uiso 0.526(13) 1 calc PR B 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 Li 0.055(4) 0.078(5) 0.063(4) 0.005(4) 0.018(3) 0.017(4) Si1 0.0567(8) 0.0690(8) 0.0566(8) -0.0013(6) 0.0105(6) 0.0187(6) Si2 0.1056(11) 0.0830(10) 0.0398(7) 0.0089(6) 0.0123(7) 0.0481(8) O 0.107(3) 0.089(3) 0.117(3) -0.034(2) 0.022(2) -0.001(2) N1 0.057(2) 0.098(3) 0.041(2) 0.008(2) 0.0167(18) 0.030(2) N2 0.0409(17) 0.062(2) 0.0375(19) -0.0017(15) 0.0072(14) 0.0122(15) N3 0.069(2) 0.073(3) 0.056(2) 0.0034(19) 0.0231(18) 0.020(2) C1 0.040(2) 0.061(2) 0.042(2) -0.0026(18) 0.0075(17) 0.0085(19) C2 0.040(2) 0.066(2) 0.039(2) -0.0038(18) 0.0018(17) 0.0159(19) C3 0.068(3) 0.088(3) 0.045(3) 0.004(2) 0.008(2) 0.028(3) C4 0.076(3) 0.100(4) 0.055(3) 0.006(2) -0.007(2) 0.042(3) C5 0.052(2) 0.092(3) 0.062(3) -0.010(2) -0.001(2) 0.032(2) C6 0.041(2) 0.076(3) 0.050(3) -0.011(2) 0.0008(18) 0.012(2) C7 0.0328(19) 0.060(2) 0.041(2) -0.0083(18) 0.0015(16) 0.0082(18) C8 0.039(2) 0.057(2) 0.042(2) -0.0063(17) 0.0096(17) 0.0088(18) C9 0.059(2) 0.064(3) 0.047(3) -0.0001(19) 0.0178(19) 0.015(2) C10 0.076(3) 0.071(3) 0.053(3) 0.007(2) 0.024(2) 0.009(2) C11 0.109(4) 0.066(3) 0.128(5) -0.013(3) 0.086(4) -0.015(3) C15 0.068(3) 0.165(6) 0.076(4) -0.010(4) 0.004(3) 0.006(4) C16 0.087(3) 0.060(3) 0.106(4) -0.003(3) 0.039(3) 0.000(3) C17 0.086(4) 0.085(4) 0.112(5) -0.002(3) -0.012(3) 0.015(3) C18 0.191(7) 0.196(8) 0.046(3) 0.021(4) 0.024(4) 0.116(6) C19 0.072(3) 0.117(4) 0.080(4) -0.017(3) -0.021(3) 0.036(3) C20 0.163(6) 0.075(4) 0.115(5) 0.026(3) 0.038(4) 0.041(4) C12 0.122(7) 0.119(7) 0.338(17) -0.025(8) 0.141(9) -0.033(6) C13 0.246(11) 0.120(7) 0.164(8) 0.041(6) 0.112(8) -0.036(7) C14 0.106(6) 0.111(6) 0.185(9) 0.010(6) 0.027(5) -0.058(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li O 1.925(9) . ? Li N1 2.007(8) 3_765 ? Li N2 2.032(7) . ? Li N1 2.249(8) . ? Si1 N3 1.716(4) . ? Si1 C17 1.838(5) . ? Si1 C15 1.846(5) . ? Si1 C16 1.847(5) . ? Si2 C19 1.868(6) . ? Si2 C18 1.874(5) . ? Si2 C20 1.882(6) . ? Si2 C9 1.883(4) . ? O C23 1.465(5) . ? O C21 1.468(5) . ? O C23A 1.472(5) . ? O C21A 1.473(5) . ? N1 C1 1.326(5) . ? N1 Li 2.007(8) 3_765 ? N2 C1 1.335(5) . ? N2 C8 1.400(4) . ? N3 C10 1.246(5) . ? C1 C2 1.478(5) . ? C2 C3 1.378(5) . ? C2 C7 1.398(5) . ? C3 C4 1.385(6) . ? C4 C5 1.376(6) . ? C5 C6 1.381(6) . ? C6 C7 1.389(5) . ? C7 C8 1.489(5) . ? C8 C9 1.359(5) . ? C9 C10 1.523(6) . ? C10 C11 1.589(7) . ? C11 C14A 1.45(7) . ? C11 C14 1.456(10) . ? C11 C12 1.497(10) . ? C11 C13 1.533(11) . ? C11 C12A 1.62(5) . ? C11 C13A 1.70(5) . ? C21 C22 1.538(5) . ? C23 C24 1.536(5) . ? C21A C22A 1.529(5) . ? C23A C24A 1.540(5) . ? 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 O Li N1 120.2(4) . 3_765 ? O Li N2 113.7(4) . . ? N1 Li N2 123.4(4) 3_765 . ? O Li N1 114.4(4) . . ? N1 Li N1 104.6(3) 3_765 . ? N2 Li N1 65.1(2) . . ? N3 Si1 C17 103.8(2) . . ? N3 Si1 C15 106.4(3) . . ? C17 Si1 C15 109.4(3) . . ? N3 Si1 C16 118.81(19) . . ? C17 Si1 C16 109.1(3) . . ? C15 Si1 C16 109.1(3) . . ? C19 Si2 C18 105.7(3) . . ? C19 Si2 C20 107.7(3) . . ? C18 Si2 C20 109.9(3) . . ? C19 Si2 C9 113.3(2) . . ? C18 Si2 C9 108.9(2) . . ? C20 Si2 C9 111.3(3) . . ? C23 O C21 113.9(13) . . ? C23 O C23A 47.1(9) . . ? C21 O C23A 80.1(12) . . ? C23 O C21A 97.9(9) . . ? C21 O C21A 59.5(7) . . ? C23A O C21A 108.6(12) . . ? C23 O Li 126.6(8) . . ? C21 O Li 116.9(9) . . ? C23A O Li 129.6(10) . . ? C21A O Li 121.0(8) . . ? C1 N1 Li 130.1(4) . 3_765 ? C1 N1 Li 78.6(3) . . ? Li N1 Li 75.4(3) 3_765 . ? C1 N2 C8 109.0(3) . . ? C1 N2 Li 87.2(3) . . ? C8 N2 Li 146.9(3) . . ? C10 N3 Si1 137.9(3) . . ? N1 C1 N2 120.7(3) . . ? N1 C1 C2 128.8(4) . . ? N2 C1 C2 110.5(3) . . ? C3 C2 C7 121.9(3) . . ? C3 C2 C1 132.0(3) . . ? C7 C2 C1 106.1(3) . . ? C2 C3 C4 117.9(4) . . ? C5 C4 C3 121.0(4) . . ? C4 C5 C6 121.2(4) . . ? C5 C6 C7 118.8(4) . . ? C6 C7 C2 119.3(3) . . ? C6 C7 C8 134.4(3) . . ? C2 C7 C8 106.3(3) . . ? C9 C8 N2 122.1(3) . . ? C9 C8 C7 129.9(3) . . ? N2 C8 C7 108.0(3) . . ? C8 C9 C10 121.2(4) . . ? C8 C9 Si2 118.1(3) . . ? C10 C9 Si2 120.5(3) . . ? N3 C10 C9 124.1(4) . . ? N3 C10 C11 117.6(4) . . ? C9 C10 C11 118.3(4) . . ? C14A C11 C14 59(3) . . ? C14A C11 C12 55(3) . . ? C14 C11 C12 113.6(8) . . ? C14A C11 C13 133(3) . . ? C14 C11 C13 108.9(6) . . ? C12 C11 C13 108.7(7) . . ? C14A C11 C10 120(3) . . ? C14 C11 C10 110.3(4) . . ? C12 C11 C10 107.6(5) . . ? C13 C11 C10 107.6(6) . . ? C14A C11 C12A 104(4) . . ? C14 C11 C12A 137.8(19) . . ? C12 C11 C12A 59(2) . . ? C13 C11 C12A 51(2) . . ? C10 C11 C12A 111.3(19) . . ? C14A C11 C13A 109(4) . . ? C14 C11 C13A 59.4(18) . . ? C12 C11 C13A 139.3(18) . . ? C13 C11 C13A 51.1(18) . . ? C10 C11 C13A 112.2(18) . . ? C12A C11 C13A 98(3) . . ? O C21 C22 98.8(4) . . ? O C23 C24 98.8(4) . . ? O C21A C22A 99.2(4) . . ? O C23A C24A 98.1(4) . . ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-08-17 at 12:01:15 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : dec102 data_(9)-dec102 _database_code_depnum_ccdc_archive 'CCDC 665651' _audit_creation_date 2007-08-17T12:01:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ;'((tmeda)Li(Me3SiNCPhCHC(NSiMe3)C6H4C(NSiMe3)NCPhCHSiMe3)Li(tm eda))' ; _chemical_formula_moiety 'C48 H84 Li2 N8 Si4' _chemical_formula_sum 'C48 H84 Li2 N8 Si4' _chemical_formula_weight 899.47 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5001(3) _cell_length_b 14.7798(3) _cell_length_c 21.7209(5) _cell_angle_alpha 90 _cell_angle_beta 98.2150(10) _cell_angle_gamma 90 _cell_volume 5878.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17921 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.136 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_number 27808 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 23.03 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 8053 _reflns_number_gt 6243 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _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^)+(0.0592P)^2^+6.7885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8053 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.462 _refine_diff_density_min -0.334 _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' 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 0.1183(3) 0.3810(3) 0.1549(2) 0.0424(12) Uani 1 1 d . . . Li2 Li 0.4746(3) 0.8823(4) 0.1791(3) 0.0542(15) Uani 1 1 d . . . Si1 Si 0.17682(5) 0.31055(6) 0.29992(4) 0.0436(3) Uani 1 1 d . . . Si2 Si 0.23955(5) 0.37924(7) 0.05735(4) 0.0494(3) Uani 1 1 d . . . Si3 Si 0.50720(5) 0.71423(8) 0.07476(5) 0.0586(3) Uani 1 1 d . . . Si4 Si 0.14574(5) 0.86688(7) 0.15711(5) 0.0520(3) Uani 1 1 d . . . N1 N 0.16482(13) 0.39422(15) 0.24410(11) 0.0361(6) Uani 1 1 d . . . N2 N 0.20120(13) 0.43294(16) 0.11534(11) 0.0368(6) Uani 1 1 d . . . N3 N 0.45544(14) 0.7775(2) 0.11750(12) 0.0507(7) Uani 1 1 d . . . N4 N 0.37362(13) 0.83184(18) 0.17676(11) 0.0402(6) Uani 1 1 d . . . N5 N 0.01963(14) 0.46967(18) 0.13861(13) 0.0483(7) Uani 1 1 d . . . N6 N 0.03790(17) 0.2773(2) 0.10930(15) 0.0612(8) Uani 1 1 d . . . N7 N 0.4781(2) 1.0231(4) 0.1639(3) 0.132(2) Uani 1 1 d . . . N8 N 0.54758(17) 0.9071(3) 0.25889(16) 0.0706(10) Uani 1 1 d . . . C1 C 0.18393(15) 0.48092(19) 0.24970(13) 0.0323(7) Uani 1 1 d . . . C2 C 0.20051(15) 0.53763(19) 0.20143(13) 0.0332(7) Uani 1 1 d . . . H2 H 0.2023 0.6006 0.2104 0.04 Uiso 1 1 calc R . . C3 C 0.21488(15) 0.51327(19) 0.14139(13) 0.0319(7) Uani 1 1 d . . . C4 C 0.18905(17) 0.5255(2) 0.31266(14) 0.0387(7) Uani 1 1 d . . . C5 C 0.13303(19) 0.5142(2) 0.34819(15) 0.0466(8) Uani 1 1 d . . . H5 H 0.0906 0.4812 0.3317 0.056 Uiso 1 1 calc R . . C6 C 0.1383(2) 0.5507(3) 0.40753(17) 0.0648(11) Uani 1 1 d . . . H6 H 0.0992 0.5434 0.4311 0.078 Uiso 1 1 calc R . . C7 C 0.1993(3) 0.5971(3) 0.43223(19) 0.0869(15) Uani 1 1 d . . . H7 H 0.2035 0.6204 0.4734 0.104 Uiso 1 1 calc R . . C8 C 0.2547(3) 0.6100(4) 0.39711(19) 0.0973(18) Uani 1 1 d . . . H8 H 0.2971 0.6428 0.414 0.117 Uiso 1 1 calc R . . C9 C 0.2494(2) 0.5757(3) 0.33769(16) 0.0640(11) Uani 1 1 d . . . H9 H 0.2875 0.5866 0.3136 0.077 Uiso 1 1 calc R . . C10 C 0.24759(19) 0.3330(3) 0.36888(17) 0.0586(10) Uani 1 1 d . . . H10A H 0.2545 0.2786 0.3948 0.088 Uiso 1 1 calc R . . H10B H 0.2315 0.3831 0.3932 0.088 Uiso 1 1 calc R . . H10C H 0.2939 0.3492 0.3547 0.088 Uiso 1 1 calc R . . C11 C 0.2080(2) 0.2094(2) 0.2598(2) 0.0710(12) Uani 1 1 d . . . H11A H 0.2124 0.1577 0.2883 0.106 Uiso 1 1 calc R . . H11B H 0.2556 0.222 0.2468 0.106 Uiso 1 1 calc R . . H11C H 0.1725 0.1953 0.2232 0.106 Uiso 1 1 calc R . . C12 C 0.0908(2) 0.2795(3) 0.3307(2) 0.0710(12) Uani 1 1 d . . . H12A H 0.0758 0.3296 0.3556 0.107 Uiso 1 1 calc R . . H12B H 0.0992 0.2253 0.3567 0.107 Uiso 1 1 calc R . . H12C H 0.0521 0.2673 0.2959 0.107 Uiso 1 1 calc R . . C13 C 0.3288(2) 0.4248(3) 0.04028(18) 0.0707(12) Uani 1 1 d . . . H13A H 0.3461 0.3883 0.0077 0.106 Uiso 1 1 calc R . . H13B H 0.3647 0.4225 0.0781 0.106 Uiso 1 1 calc R . . H13C H 0.3223 0.4877 0.0261 0.106 Uiso 1 1 calc R . . C14 C 0.2570(3) 0.2598(3) 0.0838(2) 0.0754(13) Uani 1 1 d . . . H14A H 0.2937 0.2591 0.1211 0.113 Uiso 1 1 calc R . . H14B H 0.275 0.2249 0.0507 0.113 Uiso 1 1 calc R . . H14C H 0.2115 0.2328 0.0934 0.113 Uiso 1 1 calc R . . C15 C 0.1754(2) 0.3780(3) -0.01829(17) 0.0731(12) Uani 1 1 d . . . H15A H 0.1294 0.349 -0.012 0.11 Uiso 1 1 calc R . . H15B H 0.1977 0.3441 -0.0495 0.11 Uiso 1 1 calc R . . H15C H 0.1657 0.4402 -0.0327 0.11 Uiso 1 1 calc R . . C16 C 0.24632(15) 0.58832(19) 0.10626(13) 0.0314(7) Uani 1 1 d . . . C17 C 0.30195(15) 0.64518(19) 0.13340(13) 0.0319(7) Uani 1 1 d . . . H17 H 0.3206 0.6373 0.1761 0.038 Uiso 1 1 calc R . . C18 C 0.33093(15) 0.7128(2) 0.10024(13) 0.0335(7) Uani 1 1 d . . . C19 C 0.30266(16) 0.7244(2) 0.03775(13) 0.0392(7) Uani 1 1 d . . . H19 H 0.3231 0.7689 0.0138 0.047 Uiso 1 1 calc R . . C20 C 0.24536(16) 0.6718(2) 0.01050(13) 0.0399(8) Uani 1 1 d . . . H20 H 0.2247 0.6824 -0.0315 0.048 Uiso 1 1 calc R . . C21 C 0.21780(16) 0.6038(2) 0.04414(13) 0.0360(7) Uani 1 1 d . . . H21 H 0.1789 0.5671 0.0247 0.043 Uiso 1 1 calc R . . C22 C 0.38845(16) 0.7761(2) 0.13139(13) 0.0381(7) Uani 1 1 d . . . C23 C 0.30337(16) 0.8533(2) 0.18769(14) 0.0376(7) Uani 1 1 d . . . C24 C 0.24276(17) 0.8632(2) 0.14602(15) 0.0448(8) Uani 1 1 d . . . H24 H 0.2512 0.8692 0.1041 0.059(10) Uiso 1 1 calc R . . C25 C 0.5853(2) 0.6683(3) 0.1282(2) 0.0840(13) Uani 1 1 d . . . H25A H 0.6112 0.7179 0.1518 0.126 Uiso 1 1 calc R . . H25B H 0.6187 0.6371 0.1041 0.126 Uiso 1 1 calc R . . H25C H 0.5674 0.6255 0.157 0.126 Uiso 1 1 calc R . . C26 C 0.5453(4) 0.7927(5) 0.0219(3) 0.174(4) Uani 1 1 d . . . H26A H 0.5061 0.8142 -0.0099 0.262 Uiso 1 1 calc R . . H26B H 0.5824 0.7613 0.0019 0.262 Uiso 1 1 calc R . . H26C H 0.5677 0.8444 0.0457 0.262 Uiso 1 1 calc R . . C27 C 0.4647(3) 0.6155(5) 0.0319(3) 0.172(4) Uani 1 1 d . . . H27A H 0.5014 0.5836 0.0118 0.258 Uiso 1 1 calc R . . H27B H 0.425 0.636 0.0002 0.258 Uiso 1 1 calc R . . H27C H 0.4451 0.5746 0.061 0.258 Uiso 1 1 calc R . . C28 C 0.30267(17) 0.8736(2) 0.25507(14) 0.0395(7) Uani 1 1 d . . . C29 C 0.3314(2) 0.8135(2) 0.30085(16) 0.0613(10) Uani 1 1 d . . . H29 H 0.3494 0.7567 0.2894 0.074 Uiso 1 1 calc R . . C30 C 0.3344(3) 0.8349(3) 0.36326(18) 0.0882(15) Uani 1 1 d . . . H30 H 0.3546 0.7931 0.3943 0.106 Uiso 1 1 calc R . . C31 C 0.3082(3) 0.9166(3) 0.38000(19) 0.0822(14) Uani 1 1 d . . . H31 H 0.3099 0.9315 0.4227 0.099 Uiso 1 1 calc R . . C32 C 0.2799(2) 0.9759(3) 0.33595(18) 0.0691(11) Uani 1 1 d . . . H32 H 0.2619 1.0325 0.3479 0.083 Uiso 1 1 calc R . . C33 C 0.2767(2) 0.9554(2) 0.27360(16) 0.0534(9) Uani 1 1 d . . . H33 H 0.2564 0.998 0.2431 0.064 Uiso 1 1 calc R . . C34 C 0.0954(2) 0.8061(4) 0.0887(2) 0.0900(15) Uani 1 1 d . . . H34A H 0.1018 0.8384 0.0505 0.135 Uiso 1 1 calc R . . H34B H 0.0433 0.8035 0.0928 0.135 Uiso 1 1 calc R . . H34C H 0.1146 0.7445 0.0871 0.135 Uiso 1 1 calc R . . C35 C 0.1279(2) 0.8068(3) 0.2291(2) 0.0780(13) Uani 1 1 d . . . H35A H 0.0752 0.8038 0.23 0.117 Uiso 1 1 calc R . . H35B H 0.1514 0.8397 0.2657 0.117 Uiso 1 1 calc R . . H35C H 0.1478 0.7453 0.2293 0.117 Uiso 1 1 calc R . . C36 C 0.1070(3) 0.9826(3) 0.1578(3) 0.0958(16) Uani 1 1 d . . . H36A H 0.1303 1.0151 0.1948 0.144 Uiso 1 1 calc R . . H36B H 0.0543 0.9787 0.1588 0.144 Uiso 1 1 calc R . . H36C H 0.1159 1.0151 0.1203 0.144 Uiso 1 1 calc R . . C37 C -0.0418(2) 0.4098(3) 0.1150(2) 0.0685(11) Uani 1 1 d . . . H37A H -0.0804 0.446 0.0901 0.082 Uiso 1 1 calc R . . H37B H -0.0627 0.3841 0.1508 0.082 Uiso 1 1 calc R . . C38 C -0.0199(2) 0.3332(3) 0.0755(2) 0.0825(14) Uani 1 1 d . . . H38A H -0.0631 0.2949 0.0617 0.099 Uiso 1 1 calc R . . H38B H -0.0027 0.3585 0.0379 0.099 Uiso 1 1 calc R . . C39 C 0.0334(2) 0.5348(3) 0.09086(19) 0.0659(11) Uani 1 1 d . . . H39A H 0.0749 0.5734 0.1072 0.099 Uiso 1 1 calc R . . H39B H -0.01 0.5724 0.0793 0.099 Uiso 1 1 calc R . . H39C H 0.0448 0.5022 0.0541 0.099 Uiso 1 1 calc R . . C40 C 0.0029(2) 0.5188(3) 0.19337(19) 0.0679(11) Uani 1 1 d . . . H40A H -0.0404 0.5566 0.1817 0.102 Uiso 1 1 calc R . . H40B H 0.0445 0.5572 0.2096 0.102 Uiso 1 1 calc R . . H40C H -0.0065 0.4755 0.2254 0.102 Uiso 1 1 calc R . . C41 C 0.0577(3) 0.2092(3) 0.0645(2) 0.0959(16) Uani 1 1 d . . . H41A H 0.0149 0.1719 0.0497 0.144 Uiso 1 1 calc R . . H41B H 0.0969 0.1705 0.085 0.144 Uiso 1 1 calc R . . H41C H 0.0742 0.24 0.0291 0.144 Uiso 1 1 calc R . . C42 C 0.0138(3) 0.2281(3) 0.1608(2) 0.0807(13) Uani 1 1 d . . . H42A H -0.0266 0.1877 0.1448 0.121 Uiso 1 1 calc R . . H42B H -0.0027 0.2712 0.1901 0.121 Uiso 1 1 calc R . . H42C H 0.0545 0.1924 0.1821 0.121 Uiso 1 1 calc R . . C43 C 0.5232(7) 1.0520(4) 0.2264(5) 0.166(4) Uani 1 1 d . . . H43A H 0.5677 1.0825 0.2162 0.2 Uiso 1 1 calc R . . H43B H 0.4943 1.0985 0.2448 0.2 Uiso 1 1 calc R . . C44 C 0.5442(5) 0.9941(7) 0.2694(6) 0.234(7) Uani 1 1 d . . . H44A H 0.5117 1.0018 0.3016 0.28 Uiso 1 1 calc R . . H44B H 0.5936 1.0129 0.2888 0.28 Uiso 1 1 calc R . . C45 C 0.5212(5) 1.0455(7) 0.1152(4) 0.224(5) Uani 1 1 d . . . H45A H 0.5178 1.1106 0.1068 0.337 Uiso 1 1 calc R . . H45B H 0.5026 1.012 0.0773 0.337 Uiso 1 1 calc R . . H45C H 0.5723 1.0289 0.1287 0.337 Uiso 1 1 calc R . . C46 C 0.4034(5) 1.0511(6) 0.1465(9) 0.379(12) Uani 1 1 d . . . H46A H 0.3821 1.0185 0.1089 0.569 Uiso 1 1 calc R . . H46B H 0.4017 1.1163 0.1382 0.569 Uiso 1 1 calc R . . H46C H 0.3754 1.0375 0.1804 0.569 Uiso 1 1 calc R . . C47 C 0.6208(2) 0.8787(5) 0.2626(3) 0.121(2) Uani 1 1 d . . . H47A H 0.6458 0.8882 0.305 0.181 Uiso 1 1 calc R . . H47B H 0.6452 0.9139 0.2334 0.181 Uiso 1 1 calc R . . H47C H 0.6223 0.8144 0.2521 0.181 Uiso 1 1 calc R . . C48 C 0.5140(4) 0.8689(9) 0.3095(3) 0.232(6) Uani 1 1 d . . . H48A H 0.4637 0.891 0.307 0.348 Uiso 1 1 calc R . . H48B H 0.5419 0.8873 0.3494 0.348 Uiso 1 1 calc R . . H48C H 0.5138 0.8028 0.3064 0.348 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.044(3) 0.036(3) 0.044(3) 0.000(2) -0.005(2) -0.002(2) Li2 0.042(3) 0.062(4) 0.056(4) 0.000(3) -0.003(3) -0.009(3) Si1 0.0413(5) 0.0363(5) 0.0511(6) 0.0129(4) -0.0005(4) 0.0012(4) Si2 0.0554(6) 0.0538(6) 0.0364(5) -0.0105(4) -0.0022(4) 0.0238(5) Si3 0.0370(5) 0.0925(8) 0.0486(6) -0.0032(6) 0.0142(4) 0.0053(5) Si4 0.0381(5) 0.0559(6) 0.0615(6) -0.0148(5) 0.0050(4) 0.0084(4) N1 0.0373(14) 0.0295(13) 0.0403(14) 0.0035(11) 0.0017(11) 0.0011(11) N2 0.0412(14) 0.0341(14) 0.0336(14) -0.0029(11) -0.0002(11) 0.0056(11) N3 0.0322(15) 0.077(2) 0.0439(16) -0.0073(14) 0.0082(12) -0.0088(14) N4 0.0326(14) 0.0556(16) 0.0330(14) -0.0053(13) 0.0072(11) -0.0061(12) N5 0.0397(15) 0.0518(17) 0.0521(17) 0.0092(14) 0.0025(13) 0.0032(13) N6 0.066(2) 0.0470(17) 0.065(2) 0.0028(16) -0.0108(16) -0.0089(15) N7 0.076(3) 0.105(4) 0.217(6) 0.100(4) 0.023(3) -0.001(3) N8 0.0506(19) 0.089(3) 0.069(2) -0.0225(19) -0.0038(16) -0.0120(18) C1 0.0311(15) 0.0315(16) 0.0338(16) 0.0007(13) 0.0030(13) 0.0052(13) C2 0.0386(17) 0.0277(15) 0.0335(16) 0.0000(13) 0.0063(13) 0.0037(13) C3 0.0277(15) 0.0329(16) 0.0336(16) 0.0015(13) -0.0013(12) 0.0071(13) C4 0.0487(19) 0.0341(16) 0.0352(17) 0.0031(14) 0.0127(15) 0.0011(15) C5 0.053(2) 0.0474(19) 0.0419(19) 0.0046(16) 0.0152(16) 0.0072(16) C6 0.082(3) 0.070(3) 0.050(2) 0.001(2) 0.035(2) 0.007(2) C7 0.134(4) 0.088(3) 0.046(2) -0.023(2) 0.036(3) -0.032(3) C8 0.129(4) 0.118(4) 0.051(3) -0.037(3) 0.035(3) -0.070(3) C9 0.079(3) 0.076(3) 0.043(2) -0.0143(19) 0.0250(19) -0.034(2) C10 0.050(2) 0.069(2) 0.054(2) 0.0200(19) -0.0013(17) 0.0073(19) C11 0.086(3) 0.036(2) 0.087(3) 0.0065(19) -0.002(2) 0.012(2) C12 0.058(2) 0.073(3) 0.080(3) 0.029(2) 0.002(2) -0.017(2) C13 0.061(2) 0.100(3) 0.053(2) 0.002(2) 0.0165(19) 0.036(2) C14 0.096(3) 0.051(2) 0.074(3) -0.017(2) -0.007(2) 0.032(2) C15 0.086(3) 0.080(3) 0.047(2) -0.023(2) -0.013(2) 0.033(2) C16 0.0312(15) 0.0350(16) 0.0289(16) -0.0027(13) 0.0074(12) 0.0072(13) C17 0.0299(15) 0.0409(17) 0.0247(15) 0.0007(13) 0.0034(12) 0.0087(13) C18 0.0289(15) 0.0441(17) 0.0291(16) -0.0010(14) 0.0094(13) 0.0025(14) C19 0.0385(17) 0.0519(19) 0.0284(16) 0.0039(14) 0.0090(14) -0.0028(15) C20 0.0389(17) 0.058(2) 0.0222(15) 0.0023(14) 0.0021(13) 0.0015(16) C21 0.0328(16) 0.0461(18) 0.0283(16) -0.0032(14) 0.0016(13) 0.0023(14) C22 0.0328(17) 0.0518(19) 0.0291(16) 0.0043(15) 0.0025(13) -0.0037(14) C23 0.0403(18) 0.0381(17) 0.0356(17) -0.0028(14) 0.0093(14) -0.0052(14) C24 0.0434(19) 0.050(2) 0.0411(19) -0.0049(15) 0.0067(15) 0.0022(16) C25 0.077(3) 0.079(3) 0.096(3) 0.005(3) 0.010(3) 0.018(2) C26 0.196(7) 0.192(7) 0.172(6) 0.129(6) 0.150(6) 0.127(6) C27 0.059(3) 0.260(9) 0.195(7) -0.176(7) 0.016(4) 0.003(4) C28 0.0417(18) 0.0399(18) 0.0386(18) -0.0027(15) 0.0115(14) -0.0103(14) C29 0.098(3) 0.046(2) 0.043(2) 0.0032(17) 0.021(2) -0.003(2) C30 0.161(5) 0.068(3) 0.040(2) 0.013(2) 0.026(3) 0.001(3) C31 0.140(4) 0.071(3) 0.042(2) -0.013(2) 0.035(3) -0.022(3) C32 0.098(3) 0.055(2) 0.057(3) -0.019(2) 0.022(2) -0.007(2) C33 0.066(2) 0.048(2) 0.046(2) -0.0120(17) 0.0077(17) -0.0033(18) C34 0.046(2) 0.127(4) 0.094(3) -0.044(3) 0.000(2) -0.001(3) C35 0.050(2) 0.092(3) 0.096(3) -0.001(3) 0.026(2) -0.005(2) C36 0.075(3) 0.075(3) 0.137(5) -0.004(3) 0.014(3) 0.030(3) C37 0.043(2) 0.076(3) 0.082(3) 0.011(2) -0.007(2) -0.001(2) C38 0.072(3) 0.077(3) 0.087(3) 0.006(3) -0.027(2) -0.012(2) C39 0.045(2) 0.075(3) 0.074(3) 0.035(2) -0.0011(18) 0.0101(19) C40 0.055(2) 0.075(3) 0.074(3) 0.004(2) 0.011(2) 0.019(2) C41 0.124(4) 0.077(3) 0.084(3) -0.022(3) 0.003(3) -0.021(3) C42 0.085(3) 0.069(3) 0.082(3) 0.004(2) -0.007(2) -0.019(2) C43 0.274(12) 0.058(4) 0.183(8) -0.020(5) 0.089(8) -0.045(5) C44 0.187(9) 0.126(7) 0.331(15) -0.098(9) -0.158(9) 0.042(7) C45 0.202(9) 0.271(11) 0.188(8) 0.150(8) -0.014(7) -0.097(8) C46 0.104(6) 0.113(6) 0.91(4) 0.210(13) 0.050(12) 0.031(5) C47 0.052(3) 0.175(6) 0.128(5) -0.040(4) -0.015(3) 0.018(3) C48 0.174(7) 0.454(17) 0.065(4) -0.020(6) 0.007(4) -0.193(10) #----------------------------------------------------------------------------# # 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 2.014(6) . ? Li1 N1 2.015(6) . ? Li1 N5 2.235(6) . ? Li1 N6 2.263(6) . ? Li2 N4 2.005(6) . ? Li2 N3 2.046(7) . ? Li2 N8 2.071(6) . ? Li2 N7 2.110(8) . ? Si1 N1 1.724(2) . ? Si1 C11 1.863(4) . ? Si1 C12 1.870(4) . ? Si1 C10 1.873(4) . ? Si2 N2 1.725(2) . ? Si2 C13 1.868(4) . ? Si2 C14 1.870(4) . ? Si2 C15 1.885(4) . ? Si3 N3 1.705(3) . ? Si3 C26 1.841(5) . ? Si3 C27 1.845(6) . ? Si3 C25 1.848(4) . ? Si4 C24 1.846(3) . ? Si4 C36 1.855(4) . ? Si4 C34 1.866(4) . ? Si4 C35 1.868(4) . ? N1 C1 1.330(4) . ? N2 C3 1.324(4) . ? N3 C22 1.317(4) . ? N4 C22 1.342(4) . ? N4 C23 1.391(4) . ? N5 C40 1.464(5) . ? N5 C39 1.464(4) . ? N5 C37 1.474(5) . ? N6 C42 1.457(5) . ? N6 C38 1.463(5) . ? N6 C41 1.483(5) . ? N7 C46 1.441(9) . ? N7 C45 1.450(9) . ? N7 C43 1.548(10) . ? N8 C44 1.310(9) . ? N8 C47 1.409(5) . ? N8 C48 1.452(7) . ? C1 C2 1.410(4) . ? C1 C4 1.509(4) . ? C2 C3 1.414(4) . ? C3 C16 1.509(4) . ? C4 C9 1.385(5) . ? C4 C5 1.388(4) . ? C5 C6 1.388(5) . ? C6 C7 1.363(6) . ? C7 C8 1.376(6) . ? C8 C9 1.377(5) . ? C16 C17 1.393(4) . ? C16 C21 1.396(4) . ? C17 C18 1.384(4) . ? C18 C19 1.394(4) . ? C18 C22 1.504(4) . ? C19 C20 1.378(4) . ? C20 C21 1.383(4) . ? C23 C24 1.344(4) . ? C23 C28 1.496(4) . ? C28 C29 1.382(5) . ? C28 C33 1.382(5) . ? C29 C30 1.385(5) . ? C30 C31 1.370(6) . ? C31 C32 1.346(6) . ? C32 C33 1.381(5) . ? C37 C38 1.511(6) . ? C43 C44 1.286(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Li1 N1 97.3(2) . . ? N2 Li1 N5 111.3(2) . . ? N1 Li1 N5 108.8(3) . . ? N2 Li1 N6 124.4(3) . . ? N1 Li1 N6 130.6(3) . . ? N5 Li1 N6 81.8(2) . . ? N4 Li2 N3 68.1(2) . . ? N4 Li2 N8 125.5(3) . . ? N3 Li2 N8 135.4(3) . . ? N4 Li2 N7 114.4(3) . . ? N3 Li2 N7 130.6(4) . . ? N8 Li2 N7 85.8(3) . . ? N1 Si1 C11 105.31(16) . . ? N1 Si1 C12 113.38(15) . . ? C11 Si1 C12 107.9(2) . . ? N1 Si1 C10 116.11(15) . . ? C11 Si1 C10 106.76(18) . . ? C12 Si1 C10 106.93(18) . . ? N2 Si2 C13 116.50(16) . . ? N2 Si2 C14 106.34(16) . . ? C13 Si2 C14 106.4(2) . . ? N2 Si2 C15 111.56(15) . . ? C13 Si2 C15 107.1(2) . . ? C14 Si2 C15 108.55(19) . . ? N3 Si3 C26 106.8(2) . . ? N3 Si3 C27 118.43(19) . . ? C26 Si3 C27 110.9(4) . . ? N3 Si3 C25 107.99(18) . . ? C26 Si3 C25 106.8(3) . . ? C27 Si3 C25 105.3(3) . . ? C24 Si4 C36 114.37(19) . . ? C24 Si4 C34 105.42(17) . . ? C36 Si4 C34 107.5(2) . . ? C24 Si4 C35 112.72(17) . . ? C36 Si4 C35 108.5(2) . . ? C34 Si4 C35 108.0(2) . . ? C1 N1 Si1 128.4(2) . . ? C1 N1 Li1 104.7(2) . . ? Si1 N1 Li1 126.96(19) . . ? C3 N2 Si2 130.6(2) . . ? C3 N2 Li1 105.7(2) . . ? Si2 N2 Li1 123.6(2) . . ? C22 N3 Si3 137.5(2) . . ? C22 N3 Li2 86.7(3) . . ? Si3 N3 Li2 135.5(2) . . ? C22 N4 C23 124.0(2) . . ? C22 N4 Li2 87.7(2) . . ? C23 N4 Li2 143.2(3) . . ? C40 N5 C39 109.2(3) . . ? C40 N5 C37 109.8(3) . . ? C39 N5 C37 110.7(3) . . ? C40 N5 Li1 115.2(2) . . ? C39 N5 Li1 106.0(2) . . ? C37 N5 Li1 105.9(2) . . ? C42 N6 C38 112.7(4) . . ? C42 N6 C41 107.3(3) . . ? C38 N6 C41 106.5(3) . . ? C42 N6 Li1 104.8(3) . . ? C38 N6 Li1 103.0(3) . . ? C41 N6 Li1 122.6(3) . . ? C46 N7 C45 110.5(8) . . ? C46 N7 C43 121.9(11) . . ? C45 N7 C43 107.0(6) . . ? C46 N7 Li2 105.9(4) . . ? C45 N7 Li2 111.8(6) . . ? C43 N7 Li2 99.1(4) . . ? C44 N8 C47 110.6(6) . . ? C44 N8 C48 102.3(9) . . ? C47 N8 C48 110.6(6) . . ? C44 N8 Li2 106.1(5) . . ? C47 N8 Li2 120.2(4) . . ? C48 N8 Li2 105.5(3) . . ? N1 C1 C2 126.0(3) . . ? N1 C1 C4 119.0(3) . . ? C2 C1 C4 115.0(2) . . ? N1 C1 Li1 46.65(18) . . ? C2 C1 Li1 83.1(2) . . ? C4 C1 Li1 154.2(2) . . ? C1 C2 C3 128.6(3) . . ? N2 C3 C2 124.9(3) . . ? N2 C3 C16 120.5(2) . . ? C2 C3 C16 114.6(2) . . ? N2 C3 Li1 46.05(18) . . ? C2 C3 Li1 82.5(2) . . ? C16 C3 Li1 153.9(2) . . ? C9 C4 C5 118.1(3) . . ? C9 C4 C1 122.1(3) . . ? C5 C4 C1 119.8(3) . . ? C4 C5 C6 120.7(3) . . ? C7 C6 C5 120.4(4) . . ? C6 C7 C8 119.4(4) . . ? C7 C8 C9 120.7(4) . . ? C8 C9 C4 120.7(4) . . ? C17 C16 C21 117.7(3) . . ? C17 C16 C3 123.0(2) . . ? C21 C16 C3 119.3(3) . . ? C18 C17 C16 122.2(3) . . ? C17 C18 C19 118.5(3) . . ? C17 C18 C22 121.2(2) . . ? C19 C18 C22 120.3(3) . . ? C20 C19 C18 120.5(3) . . ? C19 C20 C21 120.2(3) . . ? C20 C21 C16 120.9(3) . . ? N3 C22 N4 117.2(3) . . ? N3 C22 C18 122.3(3) . . ? N4 C22 C18 120.4(2) . . ? N3 C22 Li2 59.6(2) . . ? N4 C22 Li2 57.8(2) . . ? C18 C22 Li2 177.0(3) . . ? C24 C23 N4 128.3(3) . . ? C24 C23 C28 120.9(3) . . ? N4 C23 C28 110.6(3) . . ? C23 C24 Si4 130.4(3) . . ? C29 C28 C33 117.8(3) . . ? C29 C28 C23 121.3(3) . . ? C33 C28 C23 120.8(3) . . ? C28 C29 C30 121.0(4) . . ? C31 C30 C29 119.6(4) . . ? C32 C31 C30 120.1(4) . . ? C31 C32 C33 120.8(4) . . ? C32 C33 C28 120.6(4) . . ? N5 C37 C38 113.0(3) . . ? N6 C38 C37 111.9(3) . . ? C44 C43 N7 121.6(6) . . ? C43 C44 N8 122.9(9) . . ? C43 C44 Li2 79.5(5) . . ? N8 C44 Li2 46.5(3) . . ? #===END