Supplementary Material (ESI) for Dalton Transactions Thsi journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bezombes, Jean Philippe' 'Hitchcock, P. B.' 'Lappert, M.' 'Merle, Philippe G.' _publ_contact_author_name 'Prof M Lappert' _publ_contact_author_address ; Prof M Lappert The Chemistry Laboratory, School of Chemistry, Physics & Environmental Science University of Sussex Brighton East Sussex BN1 9QJ UNITED KINGDOM ; data_nov1699 _database_code_CSD 154172 _audit_creation_date 1999-11-15T13:44:18-00:00 _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 ; C24 H44 Li2 N4 Si2 ; _chemical_name_common nov1699 _chemical_formula_moiety 'C24 H44 Li2 N4 Si2' _chemical_formula_structural 'C24 H44 LI2 N4 SI2' _chemical_formula_sum 'C24 H44 Li2 N4 Si2' _chemical_formula_weight 458.69 _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 9.2590(10) _cell_length_b 18.225(2) _cell_length_c 9.3338(7) _cell_angle_alpha 90 _cell_angle_beta 118.617(6) _cell_angle_gamma 90 _cell_volume 1382.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 35812 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 22.986 _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 0.1 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.146 #----------------------------------------------------------------------------# # 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 11797 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.0614 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.84 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 1900 _reflns_number_gt 1469 _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 was an extremely thin plate giving limited, poor quality, diffraction. 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^)+(0.0407P)^2^+3.7267P] 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 1900 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0815 _refine_ls_wR_factor_ref 0.2 _refine_ls_wR_factor_gt 0.189 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.28 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # 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 Li Li -0.0324(11) 0.0171(5) 0.3642(10) 0.046(2) Uani 1 1 d . . . Si Si -0.28897(18) 0.10921(8) 0.42364(18) 0.0416(5) Uani 1 1 d . . . N1 N -0.0898(5) 0.0779(2) 0.5122(5) 0.0373(11) Uani 1 1 d . . . N2 N -0.0177(6) 0.0567(2) 0.1642(5) 0.0481(12) Uani 1 1 d . . . C1 C 0.0377(6) 0.1215(3) 0.6328(6) 0.0373(13) Uani 1 1 d . . . C2 C 0.1998(7) 0.1124(3) 0.6630(7) 0.0484(14) Uani 1 1 d . . . H2 H 0.2218 0.0794 0.5971 0.058 Uiso 1 1 calc R . . C3 C 0.3287(7) 0.1502(4) 0.7865(8) 0.0620(18) Uani 1 1 d . . . H3 H 0.4376 0.1419 0.8049 0.074 Uiso 1 1 calc R . . C4 C 0.3026(9) 0.1993(3) 0.8829(8) 0.0636(18) Uani 1 1 d . . . H4 H 0.3917 0.2256 0.9664 0.076 Uiso 1 1 calc R . . C5 C 0.1447(8) 0.2095(3) 0.8560(7) 0.0550(17) Uani 1 1 d . . . H5 H 0.1244 0.2428 0.9228 0.066 Uiso 1 1 calc R . . C6 C 0.0153(7) 0.1722(3) 0.7334(6) 0.0453(14) Uani 1 1 d . . . H6 H -0.0929 0.181 0.7165 0.054 Uiso 1 1 calc R . . C7 C -0.3037(7) 0.2073(3) 0.3530(7) 0.0534(16) Uani 1 1 d . . . H7A H -0.2353 0.2387 0.4466 0.08 Uiso 1 1 calc R . . H7B H -0.4183 0.2237 0.3036 0.08 Uiso 1 1 calc R . . H7C H -0.2649 0.2105 0.2722 0.08 Uiso 1 1 calc R . . C8 C -0.3936(7) 0.1054(4) 0.5528(7) 0.0580(16) Uani 1 1 d . . . H8C H -0.5051 0.1254 0.4912 0.087 Uiso 1 1 calc R . . H8B H -0.3309 0.1346 0.6519 0.087 Uiso 1 1 calc R . . H8A H -0.3993 0.0544 0.5827 0.087 Uiso 1 1 calc R . . C9 C -0.4214(7) 0.0520(3) 0.2402(7) 0.0543(16) Uani 1 1 d . . . H9C H -0.4268 0.0018 0.2748 0.081 Uiso 1 1 calc R . . H9B H -0.3741 0.0515 0.166 0.081 Uiso 1 1 calc R . . H9A H -0.5324 0.0729 0.1839 0.081 Uiso 1 1 calc R . . C10 C -0.0161(7) -0.0072(3) 0.0719(6) 0.0484(15) Uani 1 1 d . . . H10B H -0.1236 -0.0323 0.0298 0.058 Uiso 1 1 calc R . . H10A H 0.0692 -0.0415 0.1478 0.058 Uiso 1 1 calc R . . C11 C 0.1430(9) 0.0946(4) 0.2399(9) 0.074(2) Uani 1 1 d . . . H11C H 0.2285 0.061 0.3147 0.111 Uiso 1 1 calc R . . H11B H 0.1379 0.1375 0.3005 0.111 Uiso 1 1 calc R . . H11A H 0.1691 0.1104 0.1546 0.111 Uiso 1 1 calc R . . C12 C -0.1493(10) 0.1094(4) 0.0623(9) 0.090(3) Uani 1 1 d . . . H12C H -0.1324 0.1262 -0.0284 0.135 Uiso 1 1 calc R . . H12B H -0.1457 0.1516 0.129 0.135 Uiso 1 1 calc R . . H12A H -0.2567 0.0853 0.0189 0.135 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 Li 0.053(6) 0.046(5) 0.037(5) 0.002(4) 0.021(4) 0.010(4) Si 0.0384(9) 0.0378(9) 0.0415(9) 0.0003(7) 0.0133(7) 0.0019(7) N1 0.038(2) 0.035(2) 0.037(2) -0.0011(19) 0.017(2) -0.0009(19) N2 0.059(3) 0.045(3) 0.039(3) 0.004(2) 0.022(2) 0.011(2) C1 0.044(3) 0.029(3) 0.033(3) 0.007(2) 0.014(2) 0.002(2) C2 0.044(3) 0.046(3) 0.048(3) -0.003(3) 0.016(3) -0.005(3) C3 0.041(4) 0.060(4) 0.068(4) -0.002(3) 0.013(3) -0.001(3) C4 0.058(4) 0.052(4) 0.053(4) -0.006(3) 0.004(3) -0.011(3) C5 0.069(5) 0.039(3) 0.046(3) -0.004(3) 0.019(3) -0.007(3) C6 0.047(3) 0.041(3) 0.041(3) -0.002(3) 0.015(3) -0.006(3) C7 0.056(4) 0.044(3) 0.052(4) 0.004(3) 0.019(3) 0.010(3) C8 0.047(3) 0.059(4) 0.062(4) 0.000(3) 0.021(3) -0.001(3) C9 0.046(3) 0.050(4) 0.049(3) -0.003(3) 0.008(3) 0.001(3) C10 0.062(4) 0.040(3) 0.044(3) 0.007(3) 0.026(3) 0.001(3) C11 0.097(5) 0.065(5) 0.072(5) -0.017(4) 0.051(4) -0.018(4) C12 0.127(7) 0.091(5) 0.073(5) 0.035(4) 0.066(5) 0.060(5) #----------------------------------------------------------------------------# # 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 N1 2.030(10) . ? Li N2 2.065(10) . ? Li N1 2.088(10) 3_556 ? Li Li 2.392(17) 3_556 ? Li C1 2.527(10) 3_556 ? Li C2 2.767(11) 3_556 ? Li C11 2.790(12) . ? Li Si 3.168(9) . ? Si N1 1.717(4) . ? Si C9 1.874(6) . ? Si C8 1.874(6) . ? Si C7 1.888(6) . ? N1 C1 1.422(6) . ? N1 Li 2.088(10) 3_556 ? N2 C10 1.453(7) . ? N2 C11 1.477(8) . ? N2 C12 1.485(7) . ? C1 C2 1.398(7) . ? C1 C6 1.401(7) . ? C1 Li 2.527(10) 3_556 ? C2 C3 1.382(8) . ? C2 Li 2.767(11) 3_556 ? C3 C4 1.370(9) . ? C4 C5 1.373(9) . ? C5 C6 1.377(7) . ? C10 C10 1.530(10) 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 Li N2 125.2(5) . . ? N1 Li N1 109.0(4) . 3_556 ? N2 Li N1 122.4(5) . 3_556 ? N1 Li Li 55.6(4) . 3_556 ? N2 Li Li 163.2(7) . 3_556 ? N1 Li Li 53.4(4) 3_556 3_556 ? N1 Li C1 121.7(4) . 3_556 ? N2 Li C1 111.7(4) . 3_556 ? N1 Li C1 34.2(2) 3_556 3_556 ? Li Li C1 74.0(4) 3_556 3_556 ? N1 Li C2 102.1(4) . 3_556 ? N2 Li C2 119.4(4) . 3_556 ? N1 Li C2 58.3(3) 3_556 3_556 ? Li Li C2 73.8(5) 3_556 3_556 ? C1 Li C2 30.2(2) 3_556 3_556 ? N1 Li C11 113.6(4) . . ? N2 Li C11 31.1(2) . . ? N1 Li C11 112.4(4) 3_556 . ? Li Li C11 132.2(6) 3_556 . ? C1 Li C11 121.9(4) 3_556 . ? C2 Li C11 143.7(4) 3_556 . ? N1 Li Si 29.40(18) . . ? N2 Li Si 110.7(4) . . ? N1 Li Si 126.6(4) 3_556 . ? Li Li Si 77.3(4) 3_556 . ? C1 Li Si 120.5(4) 3_556 . ? C2 Li Si 91.9(3) 3_556 . ? C11 Li Si 116.1(3) . . ? N1 Si C9 109.7(2) . . ? N1 Si C8 116.4(2) . . ? C9 Si C8 104.7(3) . . ? N1 Si C7 111.3(2) . . ? C9 Si C7 107.6(3) . . ? C8 Si C7 106.6(3) . . ? N1 Si Li 35.5(2) . . ? C9 Si Li 76.3(3) . . ? C8 Si Li 139.0(3) . . ? C7 Si Li 112.1(3) . . ? C1 N1 Si 119.2(3) . . ? C1 N1 Li 117.1(4) . . ? Si N1 Li 115.1(3) . . ? C1 N1 Li 90.1(4) . 3_556 ? Si N1 Li 135.6(4) . 3_556 ? Li N1 Li 71.0(4) . 3_556 ? C10 N2 C11 111.4(5) . . ? C10 N2 C12 112.2(5) . . ? C11 N2 C12 109.4(5) . . ? C10 N2 Li 106.3(4) . . ? C11 N2 Li 102.6(4) . . ? C12 N2 Li 114.6(4) . . ? C2 C1 C6 115.7(5) . . ? C2 C1 N1 119.8(5) . . ? C6 C1 N1 124.4(5) . . ? C2 C1 Li 84.4(4) . 3_556 ? C6 C1 Li 129.9(4) . 3_556 ? N1 C1 Li 55.7(3) . 3_556 ? C3 C2 C1 121.6(6) . . ? C3 C2 Li 136.4(4) . 3_556 ? C1 C2 Li 65.4(3) . 3_556 ? C4 C3 C2 121.3(6) . . ? C3 C4 C5 118.5(6) . . ? C4 C5 C6 120.7(6) . . ? C5 C6 C1 122.2(6) . . ? N2 C10 C10 116.4(6) . 3 ? N2 C11 Li 46.2(3) . . ? #===END data_nov499 _database_code_CSD 154173 _audit_creation_date 1999-11-02T16:32:05-00:00 _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 '[Li(tmeda)(N(Ph)CH2tBu)]' _chemical_formula_moiety 'C14 H24 Li N2' _chemical_formula_sum 'C14 H24 Li N2' _chemical_formula_weight 227.29 _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 8.0808(6) _cell_length_b 19.835(2) _cell_length_c 9.4817(6) _cell_angle_alpha 90 _cell_angle_beta 106.504(5) _cell_angle_gamma 90 _cell_volume 1457.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19400 _cell_measurement_theta_min 4.246 _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 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.06 #----------------------------------------------------------------------------# # 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 6759 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.36 _diffrn_reflns_theta_max 25.1 _diffrn_reflns_theta_full 25.1 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 2536 _reflns_number_gt 2005 _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^)+(0.0861P)^2^+0.6372P] 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 2536 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1819 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.323 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.035 #----------------------------------------------------------------------------# # 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' 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 N1 N 0.0370(2) 0.57776(10) 0.4658(2) 0.0493(5) Uani 1 1 d . . . N2 N -0.3214(2) 0.54994(10) 0.6323(2) 0.0504(5) Uani 1 1 d . . . C1 C 0.1281(3) 0.61556(12) 0.5858(3) 0.0476(6) Uani 1 1 d . . . C2 C 0.1569(3) 0.58667(14) 0.7264(3) 0.0568(6) Uani 1 1 d . . . H2 H 0.1121 0.543 0.7339 0.068 Uiso 1 1 calc R . . C3 C 0.2480(4) 0.61932(16) 0.8544(3) 0.0694(8) Uani 1 1 d . . . H3 H 0.2625 0.5982 0.947 0.083 Uiso 1 1 calc R . . C4 C 0.3172(4) 0.68200(16) 0.8478(3) 0.0683(8) Uani 1 1 d . . . H4 H 0.3813 0.7043 0.9349 0.082 Uiso 1 1 calc R . . C5 C 0.2913(3) 0.71201(14) 0.7108(3) 0.0669(8) Uani 1 1 d . . . H5 H 0.3382 0.7555 0.7047 0.08 Uiso 1 1 calc R . . C6 C 0.1990(3) 0.68016(13) 0.5834(3) 0.0563(6) Uani 1 1 d . . . H6 H 0.1829 0.7024 0.4918 0.068 Uiso 1 1 calc R . . C7 C 0.0202(3) 0.60514(13) 0.3183(3) 0.0543(6) Uani 1 1 d . . . H7B H 0.0338 0.5672 0.2546 0.065 Uiso 1 1 calc R . . H7A H 0.1184 0.6362 0.3261 0.065 Uiso 1 1 calc R . . C8 C -0.1467(3) 0.64313(12) 0.2379(3) 0.0569(7) Uani 1 1 d . . . C9 C -0.1668(4) 0.70766(13) 0.3200(3) 0.0715(8) Uani 1 1 d . . . H9A H -0.0663 0.7368 0.3293 0.107 Uiso 1 1 calc R . . H9B H -0.1753 0.6961 0.4182 0.107 Uiso 1 1 calc R . . H9C H -0.2716 0.7314 0.2652 0.107 Uiso 1 1 calc R . . C10 C -0.3034(4) 0.59857(14) 0.2242(3) 0.0697(8) Uani 1 1 d . . . H10A H -0.2917 0.5571 0.1717 0.105 Uiso 1 1 calc R . . H10B H -0.4078 0.6226 0.1696 0.105 Uiso 1 1 calc R . . H10C H -0.3117 0.5872 0.3226 0.105 Uiso 1 1 calc R . . C11 C -0.1359(5) 0.66152(18) 0.0844(3) 0.0867(10) Uani 1 1 d . . . H11A H -0.0352 0.6904 0.0929 0.13 Uiso 1 1 calc R . . H11B H -0.2408 0.6856 0.0311 0.13 Uiso 1 1 calc R . . H11C H -0.1247 0.6203 0.0309 0.13 Uiso 1 1 calc R . . C12 C -0.3058(3) 0.62300(13) 0.6598(3) 0.0630(7) Uani 1 1 d . . . H12A H -0.1913 0.6332 0.7259 0.094 Uiso 1 1 calc R . . H12B H -0.3945 0.6376 0.7054 0.094 Uiso 1 1 calc R . . H12C H -0.3214 0.6469 0.5664 0.094 Uiso 1 1 calc R . . C13 C -0.2986(4) 0.51613(15) 0.7749(3) 0.0650(7) Uani 1 1 d . . . H13A H -0.3081 0.4672 0.76 0.097 Uiso 1 1 calc R . . H13B H -0.3881 0.5315 0.8188 0.097 Uiso 1 1 calc R . . H13C H -0.1845 0.5271 0.8408 0.097 Uiso 1 1 calc R . . C14 C -0.4953(3) 0.53516(12) 0.5332(3) 0.0541(6) Uani 1 1 d . . . H14A H -0.5246 0.569 0.4531 0.065 Uiso 1 1 calc R . . H14B H -0.5814 0.5389 0.589 0.065 Uiso 1 1 calc R . . Li Li -0.1299(5) 0.52001(19) 0.5316(4) 0.0474(9) 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 N1 0.0457(10) 0.0527(12) 0.0501(11) 0.0018(9) 0.0146(8) 0.0016(8) N2 0.0410(10) 0.0496(11) 0.0652(12) -0.0167(9) 0.0223(9) -0.0042(8) C1 0.0389(11) 0.0463(13) 0.0617(14) 0.0006(11) 0.0212(10) 0.0045(9) C2 0.0478(13) 0.0653(16) 0.0571(14) 0.0050(12) 0.0145(11) 0.0032(11) C3 0.0611(16) 0.086(2) 0.0601(16) 0.0044(14) 0.0156(13) 0.0135(15) C4 0.0615(16) 0.077(2) 0.0595(16) -0.0153(14) 0.0057(12) 0.0136(14) C5 0.0527(15) 0.0560(16) 0.086(2) -0.0086(14) 0.0103(13) 0.0026(12) C6 0.0487(13) 0.0540(15) 0.0632(15) 0.0013(12) 0.0114(11) 0.0023(11) C7 0.0625(15) 0.0481(14) 0.0547(14) -0.0001(11) 0.0203(11) -0.0041(11) C8 0.0671(16) 0.0443(13) 0.0536(14) 0.0071(10) 0.0080(12) -0.0029(11) C9 0.0711(18) 0.0486(15) 0.0817(19) -0.0031(13) 0.0002(14) 0.0082(13) C10 0.0689(17) 0.0528(16) 0.0779(18) 0.0043(13) 0.0052(14) -0.0060(13) C11 0.112(3) 0.084(2) 0.0543(16) 0.0126(15) 0.0075(16) -0.0275(19) C12 0.0568(14) 0.0533(15) 0.0827(19) -0.0221(13) 0.0262(13) -0.0038(12) C13 0.0623(16) 0.0746(19) 0.0630(16) -0.0091(13) 0.0261(12) -0.0057(13) C14 0.0391(12) 0.0547(14) 0.0713(16) -0.0174(12) 0.0203(11) -0.0021(10) Li 0.047(2) 0.044(2) 0.054(2) -0.0012(16) 0.0186(16) 0.0048(16) #----------------------------------------------------------------------------# # 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 N1 C1 1.386(3) . ? N1 C7 1.471(3) . ? N1 Li 1.999(4) . ? N1 Li 2.077(4) 3_566 ? N2 C12 1.472(3) . ? N2 C13 1.473(3) . ? N2 C14 1.481(3) . ? N2 Li 2.121(4) . ? C1 C6 1.406(3) . ? C1 C2 1.408(3) . ? C1 Li 2.755(4) . ? C2 C3 1.388(4) . ? C3 C4 1.372(4) . ? C4 C5 1.390(4) . ? C5 C6 1.379(4) . ? C7 C8 1.544(3) . ? C8 C10 1.519(4) . ? C8 C11 1.527(4) . ? C8 C9 1.531(4) . ? C14 C14 1.523(4) 3_466 ? Li N1 2.077(4) 3_566 ? Li Li 2.472(7) 3_566 ? 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 C1 N1 C7 117.71(19) . . ? C1 N1 Li 107.56(17) . . ? C7 N1 Li 128.32(18) . . ? C1 N1 Li 112.93(18) . 3_566 ? C7 N1 Li 106.93(17) . 3_566 ? Li N1 Li 74.62(17) . 3_566 ? C12 N2 C13 107.7(2) . . ? C12 N2 C14 108.96(19) . . ? C13 N2 C14 109.92(19) . . ? C12 N2 Li 108.60(18) . . ? C13 N2 Li 111.66(18) . . ? C14 N2 Li 109.95(16) . . ? N1 C1 C6 127.1(2) . . ? N1 C1 C2 117.6(2) . . ? C6 C1 C2 115.3(2) . . ? N1 C1 Li 43.77(13) . . ? C6 C1 Li 156.02(18) . . ? C2 C1 Li 79.02(16) . . ? C3 C2 C1 122.8(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 118.4(3) . . ? C6 C5 C4 121.5(3) . . ? C5 C6 C1 121.6(3) . . ? N1 C7 C8 118.8(2) . . ? C10 C8 C11 109.2(2) . . ? C10 C8 C9 108.9(2) . . ? C11 C8 C9 109.2(2) . . ? C10 C8 C7 110.4(2) . . ? C11 C8 C7 108.0(2) . . ? C9 C8 C7 111.2(2) . . ? N2 C14 C14 111.7(2) . 3_466 ? N1 Li N1 105.38(17) . 3_566 ? N1 Li N2 128.5(2) . . ? N1 Li N2 124.29(19) 3_566 . ? N1 Li Li 54.12(15) . 3_566 ? N1 Li Li 51.26(14) 3_566 3_566 ? N2 Li Li 167.8(3) . 3_566 ? N1 Li C1 28.66(9) . . ? N1 Li C1 112.87(16) 3_566 . ? N2 Li C1 109.48(16) . . ? Li Li C1 67.46(17) 3_566 . ? #===END data_nov1399 _database_code_CSD 154174 _audit_creation_date 1999-11-09T15:43:02-00:00 _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 '[{Li(OEt2)(PhNCH2tBu)}2]' _chemical_formula_moiety 'C30 H52 Li2 N2 O2' _chemical_formula_structural 'C30 H52 LI2 N2 O2' _chemical_formula_sum 'C30 H52 Li2 N2 O2' _chemical_formula_weight 486.62 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9810(2) _cell_length_b 16.1914(4) _cell_length_c 19.2524(4) _cell_angle_alpha 90 _cell_angle_beta 95.7960(10) _cell_angle_gamma 90 _cell_volume 3095.40(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14770 _cell_measurement_theta_min 4.246 _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 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.063 #----------------------------------------------------------------------------# # 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 25409 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 7257 _reflns_number_gt 5366 _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^)+(0.0897P)^2^+1.3997P] 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 7257 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1795 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.003 _refine_diff_density_max 0.628 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' 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 1.0439(2) 0.58555(18) 0.19470(14) 0.0368(6) Uani 1 1 d . A . Li2 Li 0.9554(2) 0.64271(18) 0.30203(13) 0.0361(6) Uani 1 1 d . A . O1 O 1.14403(11) 0.50840(7) 0.13884(6) 0.0402(3) Uani 1 1 d . . . O2 O 0.85138(11) 0.71632(8) 0.35587(6) 0.0450(3) Uani 1 1 d . . . N1 N 0.84995(11) 0.59386(8) 0.21366(6) 0.0292(3) Uani 1 1 d . . . N2 N 1.14995(11) 0.63424(8) 0.28298(6) 0.0296(3) Uani 1 1 d . . . C1 C 0.79091(13) 0.53541(9) 0.25231(7) 0.0280(3) Uani 1 1 d . A . C2 C 0.65055(14) 0.52244(10) 0.25600(8) 0.0319(3) Uani 1 1 d . . . H2 H 0.5875 0.5544 0.2271 0.038 Uiso 1 1 calc R A . C3 C 0.60374(15) 0.46451(11) 0.30062(8) 0.0364(4) Uani 1 1 d . A . H3 H 0.5094 0.4581 0.3017 0.044 Uiso 1 1 calc R . . C4 C 0.69042(16) 0.41567(11) 0.34381(8) 0.0392(4) Uani 1 1 d . . . H4 H 0.6569 0.3766 0.3745 0.047 Uiso 1 1 calc R A . C5 C 0.82818(16) 0.42571(11) 0.34080(8) 0.0376(4) Uani 1 1 d . A . H5 H 0.8897 0.3927 0.3697 0.045 Uiso 1 1 calc R . . C6 C 0.87677(14) 0.48304(10) 0.29638(7) 0.0323(3) Uani 1 1 d . . . H6 H 0.9714 0.4877 0.2952 0.039 Uiso 1 1 calc R A . C7 C 0.76122(14) 0.65147(10) 0.17285(7) 0.0306(3) Uani 1 1 d . A . H7A H 0.802 0.7072 0.1777 0.037 Uiso 1 1 calc R . . H7B H 0.6747 0.6536 0.1938 0.037 Uiso 1 1 calc R . . C8 C 0.73015(14) 0.63292(11) 0.09400(8) 0.0342(3) Uani 1 1 d . . . C9 C 0.64117(17) 0.70280(12) 0.06211(9) 0.0445(4) Uani 1 1 d . A . H9A H 0.6882 0.7556 0.0701 0.067 Uiso 1 1 calc R . . H9B H 0.5567 0.7041 0.084 0.067 Uiso 1 1 calc R . . H9C H 0.6215 0.6935 0.0118 0.067 Uiso 1 1 calc R . . C10 C 0.86159(17) 0.63040(13) 0.05932(9) 0.0472(4) Uani 1 1 d . A . H10A H 0.9187 0.5857 0.0798 0.071 Uiso 1 1 calc R . . H10B H 0.9089 0.6832 0.0668 0.071 Uiso 1 1 calc R . . H10C H 0.8413 0.6207 0.0091 0.071 Uiso 1 1 calc R . . C11 C 0.65711(17) 0.55020(12) 0.08225(9) 0.0426(4) Uani 1 1 d . A . H11A H 0.7145 0.5057 0.103 0.064 Uiso 1 1 calc R . . H11B H 0.6373 0.5404 0.032 0.064 Uiso 1 1 calc R . . H11C H 0.5727 0.5516 0.1042 0.064 Uiso 1 1 calc R . . C12 C 1.13870(17) 0.42332(12) 0.15934(10) 0.0466(4) Uani 1 1 d . . . H12A H 1.1638 0.4183 0.2102 0.056 Uiso 1 1 calc R . . H12B H 1.2036 0.3907 0.135 0.056 Uiso 1 1 calc R . . C13 C 1.00010(18) 0.39066(12) 0.14136(10) 0.0473(4) Uani 1 1 d . . . H13A H 0.9968 0.3326 0.1554 0.071 Uiso 1 1 calc R . . H13B H 0.976 0.3951 0.0909 0.071 Uiso 1 1 calc R . . H13C H 0.9363 0.4227 0.1659 0.071 Uiso 1 1 calc R . . C14 C 1.27031(18) 0.53382(13) 0.11789(11) 0.0500(5) Uani 1 1 d . . . H14A H 1.3117 0.4876 0.094 0.06 Uiso 1 1 calc R . . H14B H 1.3317 0.5491 0.1595 0.06 Uiso 1 1 calc R . . C15 C 1.25120(18) 0.60603(12) 0.06982(10) 0.0480(4) Uani 1 1 d . . . H15A H 1.3386 0.6234 0.0559 0.072 Uiso 1 1 calc R . . H15B H 1.2107 0.6517 0.0937 0.072 Uiso 1 1 calc R . . H15C H 1.1917 0.5904 0.0283 0.072 Uiso 1 1 calc R . . C16 C 1.20915(13) 0.69429(9) 0.24617(7) 0.0285(3) Uani 1 1 d . A . C17 C 1.34970(14) 0.70897(10) 0.24424(8) 0.0334(3) Uani 1 1 d . . . H17 H 1.4126 0.6767 0.273 0.04 Uiso 1 1 calc R A . C18 C 1.39674(15) 0.76895(11) 0.20164(8) 0.0373(4) Uani 1 1 d . A . H18 H 1.4912 0.7764 0.2017 0.045 Uiso 1 1 calc R . . C19 C 1.31030(17) 0.81865(11) 0.15879(9) 0.0404(4) Uani 1 1 d . . . H19 H 1.3441 0.8593 0.1295 0.048 Uiso 1 1 calc R A . C20 C 1.17262(16) 0.80691(10) 0.16016(8) 0.0372(4) Uani 1 1 d . A . H20 H 1.1112 0.8403 0.1316 0.045 Uiso 1 1 calc R . . C21 C 1.12378(14) 0.74744(10) 0.20243(8) 0.0324(3) Uani 1 1 d . . . H21 H 1.029 0.7417 0.2023 0.039 Uiso 1 1 calc R A . C22 C 1.23916(14) 0.57811(10) 0.32563(7) 0.0297(3) Uani 1 1 d . A . H22A H 1.3275 0.5774 0.3064 0.036 Uiso 1 1 calc R . . H22B H 1.2012 0.5217 0.3204 0.036 Uiso 1 1 calc R . . C23 C 1.26378(14) 0.59784(10) 0.40466(8) 0.0320(3) Uani 1 1 d . . . C24 C 1.13058(17) 0.59559(13) 0.43764(9) 0.0447(4) Uani 1 1 d . A . H24A H 1.0884 0.5413 0.4296 0.067 Uiso 1 1 calc R . . H24B H 1.0702 0.6384 0.4164 0.067 Uiso 1 1 calc R . . H24C H 1.1478 0.6056 0.488 0.067 Uiso 1 1 calc R . . C25 C 1.35736(19) 0.53148(12) 0.43844(9) 0.0487(5) Uani 1 1 d . A . H25A H 1.3158 0.4771 0.4302 0.073 Uiso 1 1 calc R . . H25B H 1.373 0.5416 0.4888 0.073 Uiso 1 1 calc R . . H25C H 1.4434 0.5331 0.418 0.073 Uiso 1 1 calc R . . C26 C 1.32855(18) 0.68244(12) 0.41730(9) 0.0435(4) Uani 1 1 d . A . H26A H 1.414 0.6842 0.3963 0.065 Uiso 1 1 calc R . . H26B H 1.3454 0.6924 0.4676 0.065 Uiso 1 1 calc R . . H26C H 1.268 0.7251 0.3961 0.065 Uiso 1 1 calc R . . C27 C 0.8531(2) 0.80264(15) 0.34026(18) 0.0812(8) Uani 1 1 d . A . H27A H 0.7885 0.8313 0.3678 0.097 Uiso 1 1 calc R . . H27B H 0.8224 0.8107 0.2902 0.097 Uiso 1 1 calc R . . C28 C 0.9848(2) 0.83994(14) 0.35523(12) 0.0591(5) Uani 1 1 d . . . H28A H 0.9794 0.8989 0.344 0.089 Uiso 1 1 calc R A . H28B H 1.0487 0.8131 0.327 0.089 Uiso 1 1 calc R . . H28C H 1.0155 0.833 0.4049 0.089 Uiso 1 1 calc R . . C29 C 0.7377(4) 0.6771(3) 0.3837(3) 0.0492(14) Uani 0.572(8) 1 d P A 1 H29A H 0.7369 0.6177 0.3716 0.059 Uiso 0.572(8) 1 calc PR A 1 H29B H 0.6533 0.7019 0.3615 0.059 Uiso 0.572(8) 1 calc PR A 1 C30 C 0.7423(5) 0.6863(4) 0.4623(2) 0.084(2) Uani 0.572(8) 1 d P A 1 H30A H 0.665 0.6578 0.4788 0.125 Uiso 0.572(8) 1 calc PR A 1 H30B H 0.739 0.745 0.4743 0.125 Uiso 0.572(8) 1 calc PR A 1 H30C H 0.8259 0.6621 0.4844 0.125 Uiso 0.572(8) 1 calc PR A 1 C29A C 0.7643(15) 0.7086(8) 0.4054(7) 0.149(6) Uani 0.428(8) 1 d P A 2 H29C H 0.7916 0.7482 0.4434 0.179 Uiso 0.428(8) 1 calc PR A 2 H29D H 0.6737 0.7253 0.3844 0.179 Uiso 0.428(8) 1 calc PR A 2 C30A C 0.7537(5) 0.6316(4) 0.4347(3) 0.0545(18) Uani 0.428(8) 1 d P A 2 H30D H 0.6827 0.6324 0.4663 0.082 Uiso 0.428(8) 1 calc PR A 2 H30E H 0.8396 0.6168 0.4609 0.082 Uiso 0.428(8) 1 calc PR A 2 H30F H 0.7312 0.5909 0.3977 0.082 Uiso 0.428(8) 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 0.0273(12) 0.0467(16) 0.0368(13) -0.0025(12) 0.0046(10) 0.0019(11) Li2 0.0283(12) 0.0467(16) 0.0335(12) -0.0025(11) 0.0041(10) 0.0023(11) O1 0.0314(6) 0.0393(7) 0.0517(7) 0.0011(5) 0.0133(5) 0.0027(5) O2 0.0377(6) 0.0497(8) 0.0494(7) -0.0052(6) 0.0141(5) 0.0032(5) N1 0.0223(5) 0.0348(7) 0.0303(6) 0.0025(5) 0.0020(4) -0.0001(5) N2 0.0233(5) 0.0341(7) 0.0309(6) 0.0025(5) 0.0005(4) 0.0001(5) C1 0.0253(6) 0.0330(8) 0.0259(6) -0.0035(6) 0.0036(5) -0.0001(5) C2 0.0255(7) 0.0379(9) 0.0323(7) -0.0008(6) 0.0038(5) 0.0008(6) C3 0.0284(7) 0.0425(9) 0.0398(8) -0.0026(7) 0.0104(6) -0.0025(6) C4 0.0414(8) 0.0405(9) 0.0375(8) 0.0050(7) 0.0133(6) -0.0017(7) C5 0.0370(8) 0.0411(9) 0.0352(8) 0.0050(7) 0.0061(6) 0.0062(7) C6 0.0254(7) 0.0392(9) 0.0326(7) 0.0006(6) 0.0043(5) 0.0017(6) C7 0.0259(7) 0.0331(8) 0.0322(7) 0.0016(6) 0.0008(5) -0.0006(6) C8 0.0289(7) 0.0434(9) 0.0300(7) 0.0025(6) 0.0021(5) 0.0000(6) C9 0.0411(9) 0.0513(11) 0.0393(8) 0.0083(8) -0.0054(7) 0.0027(8) C10 0.0376(8) 0.0688(13) 0.0362(8) 0.0077(8) 0.0088(7) 0.0018(8) C11 0.0431(9) 0.0481(11) 0.0359(8) -0.0056(7) 0.0003(7) -0.0039(7) C12 0.0404(9) 0.0420(10) 0.0566(11) 0.0069(8) 0.0005(8) 0.0010(7) C13 0.0442(9) 0.0422(10) 0.0554(11) -0.0036(8) 0.0044(8) -0.0048(8) C14 0.0380(9) 0.0570(12) 0.0573(11) -0.0038(9) 0.0161(8) 0.0018(8) C15 0.0422(9) 0.0508(11) 0.0534(10) -0.0008(9) 0.0168(8) -0.0027(8) C16 0.0249(6) 0.0318(8) 0.0289(7) -0.0032(6) 0.0032(5) 0.0007(5) C17 0.0249(7) 0.0388(9) 0.0368(8) -0.0014(7) 0.0035(5) 0.0013(6) C18 0.0294(7) 0.0412(9) 0.0428(8) -0.0044(7) 0.0105(6) -0.0038(6) C19 0.0446(9) 0.0361(9) 0.0426(9) 0.0021(7) 0.0154(7) -0.0029(7) C20 0.0389(8) 0.0362(9) 0.0370(8) 0.0030(7) 0.0056(6) 0.0050(7) C21 0.0269(7) 0.0360(8) 0.0344(7) 0.0006(6) 0.0036(5) 0.0026(6) C22 0.0261(6) 0.0310(8) 0.0313(7) -0.0005(6) -0.0003(5) 0.0018(5) C23 0.0291(7) 0.0354(8) 0.0308(7) -0.0004(6) -0.0010(5) 0.0042(6) C24 0.0380(8) 0.0621(12) 0.0344(8) 0.0029(8) 0.0061(6) -0.0005(8) C25 0.0540(10) 0.0526(11) 0.0367(8) -0.0006(8) -0.0094(7) 0.0178(9) C26 0.0448(9) 0.0459(10) 0.0390(9) -0.0101(7) 0.0000(7) -0.0039(8) C27 0.0575(13) 0.0535(14) 0.130(2) 0.0043(15) -0.0048(14) 0.0191(11) C28 0.0656(13) 0.0495(12) 0.0603(12) 0.0073(10) -0.0035(10) 0.0019(10) C29 0.0300(16) 0.072(3) 0.047(2) -0.030(2) 0.0114(14) -0.0100(18) C30 0.087(3) 0.114(5) 0.053(3) -0.014(3) 0.027(2) -0.026(3) C29A 0.199(12) 0.114(9) 0.161(11) 0.077(8) 0.149(10) 0.099(8) C30A 0.051(3) 0.063(4) 0.052(3) 0.003(3) 0.017(2) -0.005(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 Li1 O1 1.983(3) . ? Li1 N1 2.011(3) . ? Li1 N2 2.065(3) . ? Li2 O2 1.947(3) . ? Li2 N2 2.017(3) . ? Li2 N1 2.065(3) . ? O1 C14 1.422(2) . ? O1 C12 1.436(2) . ? O2 C29A 1.360(8) . ? O2 C27 1.430(3) . ? O2 C29 1.448(5) . ? N1 C1 1.3730(19) . ? N1 C7 1.4598(18) . ? N2 C16 1.3717(19) . ? N2 C22 1.4646(18) . ? C1 C6 1.424(2) . ? C1 C2 1.4254(19) . ? C2 C3 1.385(2) . ? C3 C4 1.386(2) . ? C4 C5 1.391(2) . ? C5 C6 1.383(2) . ? C7 C8 1.548(2) . ? C8 C9 1.528(2) . ? C8 C11 1.531(2) . ? C8 C10 1.532(2) . ? C12 C13 1.489(2) . ? C14 C15 1.491(3) . ? C16 C21 1.425(2) . ? C16 C17 1.4271(19) . ? C17 C18 1.383(2) . ? C18 C19 1.389(2) . ? C19 C20 1.390(2) . ? C20 C21 1.381(2) . ? C22 C23 1.550(2) . ? C23 C25 1.526(2) . ? C23 C26 1.524(2) . ? C23 C24 1.530(2) . ? C27 C28 1.449(3) . ? C29 C30 1.517(7) . ? C29A C30A 1.376(13) . ? 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 133.45(15) . . ? O1 Li1 N2 116.27(13) . . ? N1 Li1 N2 104.34(12) . . ? O2 Li2 N2 135.52(15) . . ? O2 Li2 N1 114.72(13) . . ? N2 Li2 N1 104.13(12) . . ? C14 O1 C12 114.46(13) . . ? C14 O1 Li1 118.74(13) . . ? C12 O1 Li1 114.88(13) . . ? C29A O2 C27 105.0(5) . . ? C29A O2 C29 28.4(8) . . ? C27 O2 C29 122.2(3) . . ? C29A O2 Li2 136.9(6) . . ? C27 O2 Li2 117.91(17) . . ? C29 O2 Li2 114.1(2) . . ? C1 N1 C7 117.50(11) . . ? C1 N1 Li1 121.74(12) . . ? C7 N1 Li1 119.21(12) . . ? C1 N1 Li2 91.63(11) . . ? C7 N1 Li2 115.45(12) . . ? Li1 N1 Li2 75.83(11) . . ? C16 N2 C22 117.40(11) . . ? C16 N2 Li2 121.24(12) . . ? C22 N2 Li2 118.83(12) . . ? C16 N2 Li1 93.27(11) . . ? C22 N2 Li1 117.15(12) . . ? Li2 N2 Li1 75.70(11) . . ? N1 C1 C6 117.91(12) . . ? N1 C1 C2 127.33(13) . . ? C6 C1 C2 114.71(13) . . ? C3 C2 C1 121.71(14) . . ? C2 C3 C4 121.97(14) . . ? C3 C4 C5 117.91(15) . . ? C6 C5 C4 120.92(15) . . ? C5 C6 C1 122.74(13) . . ? N1 C7 C8 117.04(13) . . ? C9 C8 C11 109.85(13) . . ? C9 C8 C10 109.46(14) . . ? C11 C8 C10 109.17(14) . . ? C9 C8 C7 107.53(13) . . ? C11 C8 C7 111.09(13) . . ? C10 C8 C7 109.70(12) . . ? O1 C12 C13 109.65(14) . . ? O1 C14 C15 109.95(15) . . ? N2 C16 C21 118.06(12) . . ? N2 C16 C17 127.40(13) . . ? C21 C16 C17 114.50(13) . . ? C18 C17 C16 121.72(14) . . ? C17 C18 C19 122.09(14) . . ? C18 C19 C20 117.75(15) . . ? C21 C20 C19 120.99(15) . . ? C20 C21 C16 122.94(14) . . ? N2 C22 C23 116.72(12) . . ? C25 C23 C26 109.49(14) . . ? C25 C23 C24 109.06(14) . . ? C26 C23 C24 109.12(14) . . ? C25 C23 C22 107.63(13) . . ? C26 C23 C22 111.39(13) . . ? C24 C23 C22 110.12(12) . . ? O2 C27 C28 113.27(18) . . ? O2 C29 C30 112.3(3) . . ? C30A C29A O2 116.8(8) . . ? #===END