# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Norbert Mitzel' _publ_contact_author_email MITZEL@UNI-BIELEFELD.DE _publ_section_title ; Two diamino-substituted lithiocarbanions in one molecule ; _publ_author_name 'Norbert Mitzel' # Attachment 'CIF_files.CIF' #============================================================================== data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 726196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H44 Li4 N8' _chemical_formula_sum 'C22 H44 Li4 N8' _chemical_formula_weight 448.41 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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 11.5563(3) _cell_length_b 11.5563(3) _cell_length_c 9.7046(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1296.03(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4763 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9796 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8704 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.47 _reflns_number_total 861 _reflns_number_gt 785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _chemical_absolute_configuration . _refine_ls_number_reflns 861 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.40418(10) 0.45219(10) 0.22277(13) 0.0147(3) Uani 1 1 d . . . N2 N 0.35460(11) 0.28194(11) 0.08429(13) 0.0167(3) Uani 1 1 d . . . Li1 Li 0.6130(2) 0.4146(2) 0.0695(3) 0.0198(6) Uani 1 1 d . . . C1 C 0.45150(13) 0.34749(13) 0.15009(15) 0.0154(3) Uani 1 1 d . . . H1 H 0.4813(14) 0.2996(15) 0.2243(18) 0.021(4) Uiso 1 1 d . . . C2 C 0.25785(13) 0.25402(13) 0.17796(15) 0.0192(3) Uani 1 1 d . . . H2A H 0.2839 0.1957 0.2460 0.023 Uiso 1 1 calc R . . H2B H 0.1937 0.2197 0.1241 0.023 Uiso 1 1 calc R . . C3 C 0.21392(12) 0.36011(12) 0.25356(17) 0.0206(4) Uani 1 1 d . . . H3A H 0.1757 0.4130 0.1875 0.025 Uiso 1 1 calc R . . H3B H 0.1560 0.3366 0.3233 0.025 Uiso 1 1 calc R . . C4 C 0.31303(12) 0.42226(13) 0.32354(16) 0.0185(3) Uani 1 1 d . . . H4A H 0.2839 0.4937 0.3678 0.022 Uiso 1 1 calc R . . H4B H 0.3461 0.3721 0.3963 0.022 Uiso 1 1 calc R . . C5 C 0.40228(15) 0.17209(14) 0.03547(18) 0.0212(4) Uani 1 1 d . . . H5A H 0.4319(15) 0.1248(15) 0.113(2) 0.029(5) Uiso 1 1 d . . . H5B H 0.4687(17) 0.1854(16) -0.024(2) 0.030(5) Uiso 1 1 d . . . H5C H 0.3426(17) 0.1271(16) -0.018(2) 0.027(5) Uiso 1 1 d . . . C6 C 0.5000 0.5000 0.3040(2) 0.0158(4) Uani 1 2 d S . . H6A H 0.4692 0.5618 0.3643 0.019 Uiso 0.50 1 calc PR . . H6B H 0.5308 0.4382 0.3643 0.019 Uiso 0.50 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 N1 0.0139(5) 0.0157(6) 0.0145(6) -0.0009(5) 0.0010(5) -0.0014(5) N2 0.0168(6) 0.0172(6) 0.0160(6) 0.0005(5) 0.0020(5) -0.0035(5) Li1 0.0186(12) 0.0223(13) 0.0186(13) -0.0001(10) 0.0020(11) -0.0017(11) C1 0.0160(7) 0.0151(7) 0.0151(7) -0.0004(6) -0.0016(6) -0.0011(5) C2 0.0180(7) 0.0209(7) 0.0187(7) 0.0020(6) -0.0002(6) -0.0047(6) C3 0.0153(6) 0.0224(7) 0.0243(8) 0.0031(6) 0.0052(6) -0.0024(6) C4 0.0192(7) 0.0176(7) 0.0187(8) 0.0009(6) 0.0049(6) 0.0008(6) C5 0.0242(8) 0.0183(7) 0.0211(8) -0.0022(6) 0.0020(7) -0.0043(7) C6 0.0184(10) 0.0158(9) 0.0134(10) 0.000 0.000 0.0002(8) _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 C6 1.4673(16) . ? N1 C4 1.4783(18) . ? N1 C1 1.5035(18) . ? N1 Li1 2.149(3) 2_665 ? N2 C5 1.463(2) . ? N2 C2 1.4767(19) . ? N2 C1 1.4952(18) . ? N2 Li1 2.045(3) 8_565 ? Li1 N2 2.045(3) 7_655 ? Li1 N1 2.149(3) 2_665 ? Li1 C1 2.167(3) . ? Li1 C1 2.221(3) 7_655 ? Li1 Li1 2.679(4) 8_565 ? Li1 Li1 2.679(4) 7_655 ? Li1 C5 2.688(3) 7_655 ? Li1 Li1 3.273(5) 2_665 ? C1 Li1 2.221(3) 8_565 ? C1 H1 0.971(18) . ? C2 C3 1.516(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.5129(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 Li1 2.688(3) 8_565 ? C5 H5A 0.995(19) . ? C5 H5B 0.97(2) . ? C5 H5C 1.01(2) . ? C6 N1 1.4672(16) 2_665 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 C6 N1 C4 105.69(11) . . ? C6 N1 C1 106.30(9) . . ? C4 N1 C1 112.41(11) . . ? C6 N1 Li1 99.89(10) . 2_665 ? C4 N1 Li1 124.02(11) . 2_665 ? C1 N1 Li1 106.57(11) . 2_665 ? C5 N2 C2 107.16(11) . . ? C5 N2 C1 107.21(11) . . ? C2 N2 C1 114.51(11) . . ? C5 N2 Li1 98.69(12) . 8_565 ? C2 N2 Li1 146.69(12) . 8_565 ? C1 N2 Li1 75.93(10) . 8_565 ? N2 Li1 N1 143.37(14) 7_655 2_665 ? N2 Li1 C1 130.78(14) 7_655 . ? N1 Li1 C1 85.83(10) 2_665 . ? N2 Li1 C1 40.77(7) 7_655 7_655 ? N1 Li1 C1 123.06(12) 2_665 7_655 ? C1 Li1 C1 126.30(13) . 7_655 ? N2 Li1 Li1 95.74(15) 7_655 8_565 ? N1 Li1 Li1 110.78(10) 2_665 8_565 ? C1 Li1 Li1 53.29(9) . 8_565 ? C1 Li1 Li1 73.47(12) 7_655 8_565 ? N2 Li1 Li1 89.62(15) 7_655 7_655 ? N1 Li1 Li1 74.03(10) 2_665 7_655 ? C1 Li1 Li1 112.68(9) . 7_655 ? C1 Li1 Li1 51.46(11) 7_655 7_655 ? Li1 Li1 Li1 75.30(9) 8_565 7_655 ? N2 Li1 C5 32.54(6) 7_655 7_655 ? N1 Li1 C5 112.67(11) 2_665 7_655 ? C1 Li1 C5 155.97(13) . 7_655 ? C1 Li1 C5 57.08(8) 7_655 7_655 ? Li1 Li1 C5 126.39(16) 8_565 7_655 ? Li1 Li1 C5 87.97(13) 7_655 7_655 ? N2 Li1 Li1 132.70(8) 7_655 2_665 ? N1 Li1 Li1 59.65(8) 2_665 2_665 ? C1 Li1 Li1 61.89(9) . 2_665 ? C1 Li1 Li1 92.77(8) 7_655 2_665 ? Li1 Li1 Li1 52.35(5) 8_565 2_665 ? Li1 Li1 Li1 52.35(5) 7_655 2_665 ? C5 Li1 Li1 140.27(12) 7_655 2_665 ? N2 C1 N1 109.61(11) . . ? N2 C1 Li1 132.24(12) . . ? N1 C1 Li1 101.21(11) . . ? N2 C1 Li1 63.30(10) . 8_565 ? N1 C1 Li1 102.41(11) . 8_565 ? Li1 C1 Li1 75.25(11) . 8_565 ? N2 C1 H1 107.1(10) . . ? N1 C1 H1 103.9(10) . . ? Li1 C1 H1 99.5(10) . . ? Li1 C1 H1 153.7(10) 8_565 . ? N2 C2 C3 112.00(12) . . ? N2 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 110.34(12) . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 110.70(12) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N2 C5 Li1 48.77(9) . 8_565 ? N2 C5 H5A 111.1(11) . . ? Li1 C5 H5A 141.1(10) 8_565 . ? N2 C5 H5B 110.6(11) . . ? Li1 C5 H5B 65.6(11) 8_565 . ? H5A C5 H5B 105.4(15) . . ? N2 C5 H5C 110.9(9) . . ? Li1 C5 H5C 108.6(11) 8_565 . ? H5A C5 H5C 110.0(14) . . ? H5B C5 H5C 108.6(15) . . ? N1 C6 N1 115.01(17) 2_665 . ? N1 C6 H6A 108.5 2_665 . ? N1 C6 H6A 108.5 . . ? N1 C6 H6B 108.5 2_665 . ? N1 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.153 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.036 #============================================================================== data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 726197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H55 Li3 N8, C5 H12' _chemical_formula_sum 'C31 H67 Li3 N8' _chemical_formula_weight 572.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 14.1087(2) _cell_length_b 16.8082(2) _cell_length_c 16.9787(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.4903(9) _cell_angle_gamma 90.00 _cell_volume 3840.21(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 59880 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9827 _exptl_absorpt_correction_T_max 0.9884 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79398 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8752 _reflns_number_gt 6907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.018 0.427 0.518 1043.7 14.3 _platon_squeeze_details ; ; _refine_special_details ; The electron density of a highly disordered pentane was squeezed. 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^)+(0.0954P)^2^+0.1661P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8752 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.32812(13) 0.37337(10) 0.12980(11) 0.0258(4) Uani 1 1 d . . . Li2 Li 0.37958(14) 0.38388(11) 0.30404(12) 0.0294(4) Uani 1 1 d . . . Li3 Li 0.18212(14) 0.37203(11) 0.20993(11) 0.0273(4) Uani 1 1 d . . . N1 N 0.11101(7) 0.28297(5) 0.13323(5) 0.0237(2) Uani 1 1 d . . . N2 N 0.22401(7) 0.22753(5) 0.06535(5) 0.0229(2) Uani 1 1 d . . . N3 N 0.34264(6) 0.30930(5) 0.02653(5) 0.0241(2) Uani 1 1 d . . . N4 N 0.28652(7) 0.40837(6) -0.07877(6) 0.0286(2) Uani 1 1 d . . . N5 N 0.46343(6) 0.47261(5) 0.25941(5) 0.02112(19) Uani 1 1 d . . . N6 N 0.51370(6) 0.34167(5) 0.30412(5) 0.0244(2) Uani 1 1 d . . . N7 N 0.31172(6) 0.50387(5) 0.15249(5) 0.02128(19) Uani 1 1 d . . . N8 N 0.15231(6) 0.50123(5) 0.17639(5) 0.0230(2) Uani 1 1 d . . . C1 C 0.21620(8) 0.28244(6) 0.13207(6) 0.0225(2) Uani 1 1 d . . . H1 H 0.2459(9) 0.2531(7) 0.1865(8) 0.026(3) Uiso 1 1 d . . . C2 C 0.07693(9) 0.20233(6) 0.14660(7) 0.0284(2) Uani 1 1 d . . . H2A H 0.0052(11) 0.2063(8) 0.1418(8) 0.030(3) Uiso 1 1 d . . . H2B H 0.1172(10) 0.1843(8) 0.2035(9) 0.032(3) Uiso 1 1 d . . . C3 C 0.09363(9) 0.14150(7) 0.08537(7) 0.0294(3) Uani 1 1 d . . . H3A H 0.0494(10) 0.1533(8) 0.0283(8) 0.030(3) Uiso 1 1 d . . . H3B H 0.0795(10) 0.0875(8) 0.1035(8) 0.029(3) Uiso 1 1 d . . . C4 C 0.20005(8) 0.14544(6) 0.08181(7) 0.0257(2) Uani 1 1 d . . . H4A H 0.2480(9) 0.1264(7) 0.1354(8) 0.024(3) Uiso 1 1 d . . . H4B H 0.2100(9) 0.1091(7) 0.0398(7) 0.022(3) Uiso 1 1 d . . . C5 C 0.04409(9) 0.31846(7) 0.05821(7) 0.0292(3) Uani 1 1 d . . . H5A H -0.0240(12) 0.3169(8) 0.0617(9) 0.041(4) Uiso 1 1 d . . . H5B H 0.0448(10) 0.2913(8) 0.0043(9) 0.035(3) Uiso 1 1 d . . . H5C H 0.0621(10) 0.3767(9) 0.0529(8) 0.035(3) Uiso 1 1 d . . . C6 C 0.32096(8) 0.23014(6) 0.05380(7) 0.0248(2) Uani 1 1 d . . . H6A H 0.3241(9) 0.1887(7) 0.0120(8) 0.027(3) Uiso 1 1 d . . . H6B H 0.3762(9) 0.2168(7) 0.1057(8) 0.024(3) Uiso 1 1 d . . . C7 C 0.26950(8) 0.32879(6) -0.05275(6) 0.0253(2) Uani 1 1 d . . . H7A H 0.2051(10) 0.3275(7) -0.0455(7) 0.022(3) Uiso 1 1 d . . . H7B H 0.2761(10) 0.2879(7) -0.0967(8) 0.029(3) Uiso 1 1 d . . . C8 C 0.44280(9) 0.30968(7) 0.01697(7) 0.0297(2) Uani 1 1 d . . . H8A H 0.4482(9) 0.2669(8) -0.0225(8) 0.029(3) Uiso 1 1 d . . . H8B H 0.4899(10) 0.2957(7) 0.0696(8) 0.028(3) Uiso 1 1 d . . . C9 C 0.46455(9) 0.39081(7) -0.01319(8) 0.0333(3) Uani 1 1 d . . . H9A H 0.5308(11) 0.3904(8) -0.0237(9) 0.039(4) Uiso 1 1 d . . . H9B H 0.4678(10) 0.4326(8) 0.0309(8) 0.033(3) Uiso 1 1 d . . . C10 C 0.38395(9) 0.41360(8) -0.09186(7) 0.0329(3) Uani 1 1 d . . . H10A H 0.3856(11) 0.3767(9) -0.1365(10) 0.043(4) Uiso 1 1 d . . . H10B H 0.3935(10) 0.4684(8) -0.1065(8) 0.032(3) Uiso 1 1 d . . . C11 C 0.20821(11) 0.42932(9) -0.15383(8) 0.0387(3) Uani 1 1 d . . . H11A H 0.2157(11) 0.4841(10) -0.1697(9) 0.048(4) Uiso 1 1 d . . . H11B H 0.2055(11) 0.3929(9) -0.2024(10) 0.046(4) Uiso 1 1 d . . . H11C H 0.1417(13) 0.4259(9) -0.1456(10) 0.049(4) Uiso 1 1 d . . . C12 C 0.47240(8) 0.39034(6) 0.22817(6) 0.0230(2) Uani 1 1 d . . . H12 H 0.5280(10) 0.3942(7) 0.1977(8) 0.027(3) Uiso 1 1 d . . . C13 C 0.55984(8) 0.50671(6) 0.30705(7) 0.0243(2) Uani 1 1 d . . . H13A H 0.6057(9) 0.5140(7) 0.2711(8) 0.025(3) Uiso 1 1 d . . . H13B H 0.5496(9) 0.5603(8) 0.3227(8) 0.027(3) Uiso 1 1 d . . . C14 C 0.60717(8) 0.45424(7) 0.38141(7) 0.0273(2) Uani 1 1 d . . . H14A H 0.6768(10) 0.4748(8) 0.4112(8) 0.031(3) Uiso 1 1 d . . . H14B H 0.5698(10) 0.4582(8) 0.4221(8) 0.032(3) Uiso 1 1 d . . . C15 C 0.61235(8) 0.36820(7) 0.35515(7) 0.0277(2) Uani 1 1 d . . . H15A H 0.6339(11) 0.3333(8) 0.4041(9) 0.037(4) Uiso 1 1 d . . . H15B H 0.6631(9) 0.3634(7) 0.3228(7) 0.023(3) Uiso 1 1 d . . . C16 C 0.51736(9) 0.25830(7) 0.28256(8) 0.0311(3) Uani 1 1 d . . . H16A H 0.5615(11) 0.2500(9) 0.2496(9) 0.039(4) Uiso 1 1 d . . . H16B H 0.5435(10) 0.2273(8) 0.3345(8) 0.028(3) Uiso 1 1 d . . . H16C H 0.4497(10) 0.2395(7) 0.2515(8) 0.027(3) Uiso 1 1 d . . . C17 C 0.41686(8) 0.52411(6) 0.18989(6) 0.0221(2) Uani 1 1 d . . . H17A H 0.4245(9) 0.5801(7) 0.2061(7) 0.021(3) Uiso 1 1 d . . . H17B H 0.4520(9) 0.5202(7) 0.1456(7) 0.019(3) Uiso 1 1 d . . . C18 C 0.25435(8) 0.53108(6) 0.20641(6) 0.0222(2) Uani 1 1 d . . . H18A H 0.2845(9) 0.5101(7) 0.2623(8) 0.022(3) Uiso 1 1 d . . . H18B H 0.2557(9) 0.5911(7) 0.2073(7) 0.020(3) Uiso 1 1 d . . . C19 C 0.27219(8) 0.54307(6) 0.07143(6) 0.0243(2) Uani 1 1 d . . . H19A H 0.3149(9) 0.5253(7) 0.0362(8) 0.023(3) Uiso 1 1 d . . . H19B H 0.2749(9) 0.6014(8) 0.0770(8) 0.028(3) Uiso 1 1 d . . . C20 C 0.16410(8) 0.51889(7) 0.03455(7) 0.0257(2) Uani 1 1 d . . . H20A H 0.1633(9) 0.4620(8) 0.0239(8) 0.030(3) Uiso 1 1 d . . . H20B H 0.1329(10) 0.5472(8) -0.0195(8) 0.030(3) Uiso 1 1 d . . . C21 C 0.10464(8) 0.53604(7) 0.09375(7) 0.0262(2) Uani 1 1 d . . . H21A H 0.0380(10) 0.5138(7) 0.0732(8) 0.028(3) Uiso 1 1 d . . . H21B H 0.0983(9) 0.5963(7) 0.1006(7) 0.023(3) Uiso 1 1 d . . . C22 C 0.09718(8) 0.52819(7) 0.23266(7) 0.0292(2) Uani 1 1 d . . . H22A H 0.0271(12) 0.5028(8) 0.2154(9) 0.042(4) Uiso 1 1 d . . . H22B H 0.0922(10) 0.5878(9) 0.2343(8) 0.035(3) Uiso 1 1 d . . . H22C H 0.1343(10) 0.5078(7) 0.2883(8) 0.026(3) Uiso 1 1 d . . . C23 C 0.25816(8) 0.35406(6) 0.34899(6) 0.0261(2) Uani 1 1 d . . . C24 C 0.15030(10) 0.33795(8) 0.34553(8) 0.0353(3) Uani 1 1 d . . . H24A H 0.1049(12) 0.3904(10) 0.3332(10) 0.052(4) Uiso 1 1 d . . . H24B H 0.1156(12) 0.2941(10) 0.3005(10) 0.052(4) Uiso 1 1 d . . . H24C H 0.1393(12) 0.3172(10) 0.4000(11) 0.055(4) Uiso 1 1 d . . . C25 C 0.29998(10) 0.41450(7) 0.41831(7) 0.0334(3) Uani 1 1 d . . . H25A H 0.2961(11) 0.3944(8) 0.4750(10) 0.045(4) Uiso 1 1 d . . . H25B H 0.2639(11) 0.4645(9) 0.4089(9) 0.037(4) Uiso 1 1 d . . . H25C H 0.3724(12) 0.4280(9) 0.4262(9) 0.044(4) Uiso 1 1 d . . . C26 C 0.31348(10) 0.27551(7) 0.37724(7) 0.0317(3) Uani 1 1 d . . . H26A H 0.3043(10) 0.2562(8) 0.4317(9) 0.034(3) Uiso 1 1 d . . . H26B H 0.2889(11) 0.2317(9) 0.3325(9) 0.039(4) Uiso 1 1 d . . . H26C H 0.3863(12) 0.2813(9) 0.3877(9) 0.046(4) Uiso 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 Li1 0.0250(9) 0.0232(9) 0.0256(9) 0.0000(7) 0.0023(7) -0.0017(7) Li2 0.0265(9) 0.0310(9) 0.0283(9) 0.0026(7) 0.0048(7) 0.0022(7) Li3 0.0272(9) 0.0267(9) 0.0254(9) -0.0002(7) 0.0041(7) -0.0010(7) N1 0.0229(4) 0.0223(4) 0.0234(4) 0.0029(3) 0.0030(4) -0.0030(3) N2 0.0250(5) 0.0207(4) 0.0206(4) -0.0008(3) 0.0032(3) -0.0047(3) N3 0.0228(5) 0.0255(4) 0.0214(4) 0.0009(3) 0.0027(4) -0.0040(3) N4 0.0298(5) 0.0292(5) 0.0250(5) 0.0038(4) 0.0056(4) -0.0048(4) N5 0.0193(4) 0.0198(4) 0.0204(4) -0.0009(3) 0.0001(3) -0.0003(3) N6 0.0230(5) 0.0217(4) 0.0226(4) -0.0002(3) -0.0022(4) 0.0026(3) N7 0.0189(4) 0.0218(4) 0.0197(4) 0.0021(3) 0.0006(3) 0.0003(3) N8 0.0195(4) 0.0241(4) 0.0223(4) 0.0010(3) 0.0017(3) 0.0010(3) C1 0.0220(5) 0.0230(5) 0.0192(5) -0.0004(4) 0.0013(4) -0.0020(4) C2 0.0276(6) 0.0250(5) 0.0312(6) 0.0035(4) 0.0068(5) -0.0045(4) C3 0.0318(6) 0.0230(5) 0.0298(6) 0.0020(4) 0.0038(5) -0.0076(4) C4 0.0314(6) 0.0207(5) 0.0218(5) 0.0008(4) 0.0031(4) -0.0025(4) C5 0.0238(6) 0.0279(6) 0.0305(6) 0.0057(4) 0.0002(5) -0.0023(4) C6 0.0254(5) 0.0241(5) 0.0226(5) -0.0004(4) 0.0036(4) -0.0014(4) C7 0.0260(6) 0.0275(5) 0.0197(5) -0.0007(4) 0.0031(4) -0.0059(4) C8 0.0246(6) 0.0340(6) 0.0296(6) -0.0013(5) 0.0068(5) -0.0032(5) C9 0.0283(6) 0.0393(7) 0.0333(6) -0.0017(5) 0.0106(5) -0.0090(5) C10 0.0370(7) 0.0339(6) 0.0299(6) 0.0017(5) 0.0132(5) -0.0077(5) C11 0.0408(8) 0.0408(7) 0.0301(6) 0.0112(5) 0.0041(5) -0.0018(6) C12 0.0236(5) 0.0215(5) 0.0209(5) -0.0010(4) 0.0020(4) 0.0014(4) C13 0.0215(5) 0.0245(5) 0.0234(5) -0.0036(4) 0.0013(4) -0.0019(4) C14 0.0243(5) 0.0286(5) 0.0233(5) -0.0030(4) -0.0016(4) -0.0006(4) C15 0.0226(5) 0.0287(6) 0.0253(5) -0.0009(4) -0.0027(4) 0.0043(4) C16 0.0319(6) 0.0241(5) 0.0303(6) -0.0014(5) -0.0014(5) 0.0049(5) C17 0.0204(5) 0.0209(5) 0.0220(5) 0.0014(4) 0.0021(4) -0.0010(4) C18 0.0210(5) 0.0206(5) 0.0220(5) 0.0006(4) 0.0021(4) 0.0004(4) C19 0.0243(5) 0.0232(5) 0.0218(5) 0.0037(4) 0.0017(4) -0.0009(4) C20 0.0244(5) 0.0260(5) 0.0215(5) 0.0035(4) -0.0013(4) -0.0005(4) C21 0.0198(5) 0.0262(5) 0.0264(5) 0.0028(4) -0.0025(4) 0.0013(4) C22 0.0238(6) 0.0323(6) 0.0305(6) -0.0004(5) 0.0067(5) 0.0041(4) C23 0.0292(6) 0.0248(5) 0.0223(5) 0.0006(4) 0.0048(4) 0.0004(4) C24 0.0347(6) 0.0399(7) 0.0325(6) 0.0038(5) 0.0119(5) -0.0034(5) C25 0.0437(7) 0.0290(6) 0.0251(6) -0.0020(5) 0.0066(5) -0.0014(5) C26 0.0386(7) 0.0262(6) 0.0283(6) 0.0047(5) 0.0069(5) 0.0017(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 Li1 N3 2.119(2) . ? Li1 C1 2.206(2) . ? Li1 C12 2.2296(19) . ? Li1 N7 2.2509(19) . ? Li1 C6 2.719(2) . ? Li1 Li3 2.789(3) . ? Li1 Li2 2.832(3) . ? Li2 N6 2.020(2) . ? Li2 C12 2.098(2) . ? Li2 C23 2.134(2) . ? Li2 N5 2.176(2) . ? Li2 C26 2.536(2) . ? Li2 C25 2.569(2) . ? Li2 Li3 2.771(3) . ? Li2 H25C 2.234(15) . ? Li2 H26C 2.217(15) . ? Li3 N1 2.039(2) . ? Li3 C1 2.151(2) . ? Li3 N8 2.252(2) . ? Li3 C23 2.301(2) . ? Li3 C24 2.540(2) . ? Li3 H1 2.276(12) . ? N1 C5 1.4653(13) . ? N1 C2 1.4783(13) . ? N1 C1 1.4902(14) . ? N2 C6 1.4396(14) . ? N2 C4 1.4673(13) . ? N2 C1 1.4908(13) . ? N3 C7 1.4660(13) . ? N3 C8 1.4700(15) . ? N3 C6 1.4709(13) . ? N4 C7 1.4511(14) . ? N4 C11 1.4569(15) . ? N4 C10 1.4595(16) . ? N5 C17 1.4520(13) . ? N5 C13 1.4736(13) . ? N5 C12 1.4999(13) . ? N6 C16 1.4533(14) . ? N6 C15 1.4703(13) . ? N6 C12 1.4900(13) . ? N7 C18 1.4656(14) . ? N7 C17 1.4674(13) . ? N7 C19 1.4759(13) . ? N8 C18 1.4639(13) . ? N8 C22 1.4729(15) . ? N8 C21 1.4820(13) . ? C1 H1 1.020(13) . ? C2 C3 1.5260(17) . ? C2 H2A 0.993(14) . ? C2 H2B 1.008(14) . ? C3 C4 1.5222(16) . ? C3 H3A 1.002(13) . ? C3 H3B 0.998(13) . ? C4 H4A 1.009(13) . ? C4 H4B 0.981(12) . ? C5 H5A 0.980(16) . ? C5 H5B 1.026(14) . ? C5 H5C 1.021(14) . ? C6 H6A 1.004(13) . ? C6 H6B 1.011(13) . ? C7 H7A 0.954(13) . ? C7 H7B 1.040(13) . ? C8 C9 1.5201(16) . ? C8 H8A 1.001(14) . ? C8 H8B 0.969(14) . ? C9 C10 1.5202(17) . ? C9 H9A 1.003(15) . ? C9 H9B 1.017(14) . ? C10 H10A 0.985(16) . ? C10 H10B 0.974(14) . ? C11 H11A 0.974(17) . ? C11 H11B 1.018(16) . ? C11 H11C 0.991(17) . ? C12 H12 1.064(13) . ? C13 C14 1.5202(15) . ? C13 H13A 1.022(13) . ? C13 H13B 0.962(13) . ? C14 C15 1.5216(16) . ? C14 H14A 1.021(14) . ? C14 H14B 0.989(14) . ? C15 H15A 0.987(15) . ? C15 H15B 1.028(13) . ? C16 H16A 0.964(15) . ? C16 H16B 0.995(13) . ? C16 H16C 0.993(13) . ? C17 H17A 0.977(12) . ? C17 H17B 1.019(12) . ? C18 H18A 0.982(12) . ? C18 H18B 1.009(12) . ? C19 C20 1.5195(15) . ? C19 H19A 1.013(13) . ? C19 H19B 0.985(13) . ? C20 C21 1.5179(16) . ? C20 H20A 0.973(13) . ? C20 H20B 1.010(13) . ? C21 H21A 0.974(14) . ? C21 H21B 1.027(12) . ? C22 H22A 1.035(16) . ? C22 H22B 1.005(14) . ? C22 H22C 0.993(13) . ? C23 C24 1.5293(17) . ? C23 C25 1.5324(15) . ? C23 C26 1.5352(16) . ? C24 H24A 1.073(17) . ? C24 H24B 1.069(17) . ? C24 H24C 1.042(17) . ? C25 H25A 1.037(16) . ? C25 H25B 0.971(15) . ? C25 H25C 1.015(16) . ? C26 H26A 1.025(14) . ? C26 H26B 1.040(15) . ? C26 H26C 0.994(16) . ? 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 N3 Li1 C1 84.84(7) . . ? N3 Li1 C12 113.03(9) . . ? C1 Li1 C12 124.94(9) . . ? N3 Li1 N7 132.62(9) . . ? C1 Li1 N7 124.14(9) . . ? C12 Li1 N7 82.23(7) . . ? N3 Li1 C6 32.49(4) . . ? C1 Li1 C6 58.01(5) . . ? C12 Li1 C6 111.36(8) . . ? N7 Li1 C6 162.35(9) . . ? N3 Li1 Li3 131.97(9) . . ? C1 Li1 Li3 49.35(6) . . ? C12 Li1 Li3 106.11(8) . . ? N7 Li1 Li3 78.20(7) . . ? C6 Li1 Li3 107.27(7) . . ? N3 Li1 Li2 146.91(9) . . ? C1 Li1 Li2 89.15(8) . . ? C12 Li1 Li2 47.14(6) . . ? N7 Li1 Li2 76.57(7) . . ? C6 Li1 Li2 120.82(8) . . ? Li3 Li1 Li2 59.07(6) . . ? N6 Li2 C12 42.37(5) . . ? N6 Li2 C23 140.31(10) . . ? C12 Li2 C23 161.47(11) . . ? N6 Li2 N5 68.52(7) . . ? C12 Li2 N5 41.04(5) . . ? C23 Li2 N5 149.80(10) . . ? N6 Li2 C26 103.28(8) . . ? C12 Li2 C26 136.69(10) . . ? C23 Li2 C26 37.15(5) . . ? N5 Li2 C26 168.94(10) . . ? N6 Li2 C25 133.76(9) . . ? C12 Li2 C25 161.57(10) . . ? C23 Li2 C25 36.57(5) . . ? N5 Li2 C25 122.17(9) . . ? C26 Li2 C25 57.66(6) . . ? N6 Li2 Li3 138.96(10) . . ? C12 Li2 Li3 110.77(9) . . ? C23 Li2 Li3 54.08(6) . . ? N5 Li2 Li3 113.95(8) . . ? C26 Li2 Li3 77.11(7) . . ? C25 Li2 Li3 81.83(7) . . ? N6 Li2 Li1 85.69(8) . . ? C12 Li2 Li1 51.18(6) . . ? C23 Li2 Li1 112.19(8) . . ? N5 Li2 Li1 71.01(7) . . ? C26 Li2 Li1 116.78(8) . . ? C25 Li2 Li1 140.21(9) . . ? Li3 Li2 Li1 59.70(6) . . ? N6 Li2 H25C 114.8(4) . . ? C12 Li2 H25C 139.8(4) . . ? C23 Li2 H25C 58.7(4) . . ? N5 Li2 H25C 106.1(4) . . ? C26 Li2 H25C 69.9(4) . . ? C25 Li2 H25C 23.1(4) . . ? Li3 Li2 H25C 103.9(4) . . ? Li1 Li2 H25C 157.2(4) . . ? N6 Li2 H26C 82.3(4) . . ? C12 Li2 H26C 121.3(4) . . ? C23 Li2 H26C 58.2(4) . . ? N5 Li2 H26C 146.4(4) . . ? C26 Li2 H26C 22.9(4) . . ? C25 Li2 H26C 67.5(4) . . ? Li3 Li2 H26C 99.0(4) . . ? Li1 Li2 H26C 124.7(4) . . ? H25C Li2 H26C 70.6(6) . . ? N1 Li3 C1 41.55(5) . . ? N1 Li3 N8 121.85(9) . . ? C1 Li3 N8 125.36(9) . . ? N1 Li3 C23 123.17(9) . . ? C1 Li3 C23 114.66(9) . . ? N8 Li3 C23 112.34(8) . . ? N1 Li3 C24 103.07(8) . . ? C1 Li3 C24 122.15(9) . . ? N8 Li3 C24 112.10(8) . . ? C23 Li3 C24 36.41(5) . . ? N1 Li3 Li2 129.60(9) . . ? C1 Li3 Li2 91.89(8) . . ? N8 Li3 Li2 98.94(8) . . ? C23 Li3 Li2 48.69(6) . . ? C24 Li3 Li2 85.10(7) . . ? N1 Li3 Li1 89.32(8) . . ? C1 Li3 Li1 51.07(6) . . ? N8 Li3 Li1 88.74(7) . . ? C23 Li3 Li1 108.46(8) . . ? C24 Li3 Li1 143.28(9) . . ? Li2 Li3 Li1 61.23(7) . . ? N1 Li3 H1 52.3(3) . . ? C1 Li3 H1 26.4(3) . . ? N8 Li3 H1 148.9(3) . . ? C23 Li3 H1 88.7(3) . . ? C24 Li3 H1 98.5(3) . . ? Li2 Li3 H1 77.4(3) . . ? Li1 Li3 H1 62.2(3) . . ? C5 N1 C2 110.64(8) . . ? C5 N1 C1 112.02(8) . . ? C2 N1 C1 111.57(8) . . ? C5 N1 Li3 108.73(8) . . ? C2 N1 Li3 134.06(9) . . ? C1 N1 Li3 73.26(7) . . ? C6 N2 C4 109.72(8) . . ? C6 N2 C1 112.02(8) . . ? C4 N2 C1 111.32(8) . . ? C7 N3 C8 109.41(9) . . ? C7 N3 C6 109.61(8) . . ? C8 N3 C6 109.66(8) . . ? C7 N3 Li1 115.45(8) . . ? C8 N3 Li1 115.11(8) . . ? C6 N3 Li1 96.79(8) . . ? C7 N4 C11 109.73(9) . . ? C7 N4 C10 110.57(9) . . ? C11 N4 C10 110.71(10) . . ? C17 N5 C13 109.38(8) . . ? C17 N5 C12 109.13(8) . . ? C13 N5 C12 112.99(8) . . ? C17 N5 Li2 122.08(8) . . ? C13 N5 Li2 125.74(8) . . ? C12 N5 Li2 66.67(7) . . ? C16 N6 C15 109.99(8) . . ? C16 N6 C12 110.22(8) . . ? C15 N6 C12 113.47(8) . . ? C16 N6 Li2 116.27(9) . . ? C15 N6 Li2 127.91(9) . . ? C12 N6 Li2 71.59(8) . . ? C18 N7 C17 109.49(8) . . ? C18 N7 C19 108.56(8) . . ? C17 N7 C19 110.46(8) . . ? C18 N7 Li1 121.03(8) . . ? C17 N7 Li1 99.06(7) . . ? C19 N7 Li1 107.76(8) . . ? C18 N8 C22 108.94(8) . . ? C18 N8 C21 108.25(8) . . ? C22 N8 C21 108.35(8) . . ? C18 N8 Li3 98.80(7) . . ? C22 N8 Li3 103.15(8) . . ? C21 N8 Li3 128.11(8) . . ? N1 C1 N2 108.37(8) . . ? N1 C1 Li3 65.18(7) . . ? N2 C1 Li3 168.97(9) . . ? N1 C1 Li1 135.81(8) . . ? N2 C1 Li1 101.47(8) . . ? Li3 C1 Li1 79.58(8) . . ? N1 C1 H1 97.5(7) . . ? N2 C1 H1 106.5(7) . . ? Li3 C1 H1 83.6(7) . . ? Li1 C1 H1 104.5(7) . . ? N1 C2 C3 112.70(9) . . ? N1 C2 H2A 107.2(7) . . ? C3 C2 H2A 110.6(7) . . ? N1 C2 H2B 107.9(7) . . ? C3 C2 H2B 107.1(8) . . ? H2A C2 H2B 111.5(11) . . ? C4 C3 C2 110.73(9) . . ? C4 C3 H3A 106.7(7) . . ? C2 C3 H3A 110.4(7) . . ? C4 C3 H3B 110.0(7) . . ? C2 C3 H3B 108.3(7) . . ? H3A C3 H3B 110.8(10) . . ? N2 C4 C3 109.57(9) . . ? N2 C4 H4A 109.9(7) . . ? C3 C4 H4A 110.6(7) . . ? N2 C4 H4B 110.8(7) . . ? C3 C4 H4B 111.1(7) . . ? H4A C4 H4B 104.7(10) . . ? N1 C5 H5A 108.9(9) . . ? N1 C5 H5B 114.7(8) . . ? H5A C5 H5B 108.3(12) . . ? N1 C5 H5C 110.8(8) . . ? H5A C5 H5C 107.7(11) . . ? H5B C5 H5C 106.2(11) . . ? N2 C6 N3 111.50(8) . . ? N2 C6 Li1 82.16(7) . . ? N3 C6 Li1 50.72(6) . . ? N2 C6 H6A 108.7(7) . . ? N3 C6 H6A 110.3(7) . . ? Li1 C6 H6A 161.0(7) . . ? N2 C6 H6B 112.9(7) . . ? N3 C6 H6B 107.3(7) . . ? Li1 C6 H6B 82.8(7) . . ? H6A C6 H6B 106.0(10) . . ? N4 C7 N3 110.51(8) . . ? N4 C7 H7A 108.1(7) . . ? N3 C7 H7A 108.1(7) . . ? N4 C7 H7B 109.4(7) . . ? N3 C7 H7B 108.7(7) . . ? H7A C7 H7B 111.9(10) . . ? N3 C8 C9 109.82(9) . . ? N3 C8 H8A 109.9(7) . . ? C9 C8 H8A 110.8(7) . . ? N3 C8 H8B 108.2(8) . . ? C9 C8 H8B 112.2(8) . . ? H8A C8 H8B 105.9(11) . . ? C8 C9 C10 110.40(10) . . ? C8 C9 H9A 110.3(8) . . ? C10 C9 H9A 109.7(8) . . ? C8 C9 H9B 109.9(7) . . ? C10 C9 H9B 109.2(7) . . ? H9A C9 H9B 107.3(11) . . ? N4 C10 C9 109.94(9) . . ? N4 C10 H10A 108.7(9) . . ? C9 C10 H10A 109.5(9) . . ? N4 C10 H10B 107.8(8) . . ? C9 C10 H10B 109.7(8) . . ? H10A C10 H10B 111.2(11) . . ? N4 C11 H11A 110.7(9) . . ? N4 C11 H11B 113.4(9) . . ? H11A C11 H11B 108.9(12) . . ? N4 C11 H11C 111.4(9) . . ? H11A C11 H11C 106.3(13) . . ? H11B C11 H11C 105.8(13) . . ? N6 C12 N5 104.63(7) . . ? N6 C12 Li2 66.04(7) . . ? N5 C12 Li2 72.30(8) . . ? N6 C12 Li1 127.56(8) . . ? N5 C12 Li1 103.17(7) . . ? Li2 C12 Li1 81.69(8) . . ? N6 C12 H12 107.5(7) . . ? N5 C12 H12 105.6(6) . . ? Li2 C12 H12 171.8(7) . . ? Li1 C12 H12 106.5(7) . . ? N5 C13 C14 109.44(9) . . ? N5 C13 H13A 111.4(7) . . ? C14 C13 H13A 111.5(7) . . ? N5 C13 H13B 109.0(8) . . ? C14 C13 H13B 112.3(7) . . ? H13A C13 H13B 103.2(10) . . ? C13 C14 C15 110.85(9) . . ? C13 C14 H14A 109.4(7) . . ? C15 C14 H14A 110.1(7) . . ? C13 C14 H14B 110.3(8) . . ? C15 C14 H14B 110.5(8) . . ? H14A C14 H14B 105.5(11) . . ? N6 C15 C14 109.91(9) . . ? N6 C15 H15A 108.3(8) . . ? C14 C15 H15A 110.4(8) . . ? N6 C15 H15B 110.5(7) . . ? C14 C15 H15B 109.5(7) . . ? H15A C15 H15B 108.3(11) . . ? N6 C16 H16A 111.4(9) . . ? N6 C16 H16B 108.3(7) . . ? H16A C16 H16B 107.9(11) . . ? N6 C16 H16C 109.8(7) . . ? H16A C16 H16C 109.3(12) . . ? H16B C16 H16C 110.1(10) . . ? N5 C17 N7 111.41(8) . . ? N5 C17 H17A 111.1(7) . . ? N7 C17 H17A 110.9(7) . . ? N5 C17 H17B 111.0(6) . . ? N7 C17 H17B 108.6(6) . . ? H17A C17 H17B 103.5(9) . . ? N8 C18 N7 110.22(8) . . ? N8 C18 H18A 108.0(7) . . ? N7 C18 H18A 109.4(7) . . ? N8 C18 H18B 111.1(7) . . ? N7 C18 H18B 108.1(7) . . ? H18A C18 H18B 110.1(10) . . ? N7 C19 C20 108.42(9) . . ? N7 C19 H19A 107.0(7) . . ? C20 C19 H19A 112.3(7) . . ? N7 C19 H19B 111.2(7) . . ? C20 C19 H19B 108.1(7) . . ? H19A C19 H19B 109.8(10) . . ? C21 C20 C19 111.24(9) . . ? C21 C20 H20A 109.4(8) . . ? C19 C20 H20A 107.1(8) . . ? C21 C20 H20B 109.6(7) . . ? C19 C20 H20B 111.0(7) . . ? H20A C20 H20B 108.5(10) . . ? N8 C21 C20 111.60(8) . . ? N8 C21 H21A 107.6(8) . . ? C20 C21 H21A 110.9(8) . . ? N8 C21 H21B 108.2(7) . . ? C20 C21 H21B 110.3(7) . . ? H21A C21 H21B 108.1(10) . . ? N8 C22 H22A 109.6(8) . . ? N8 C22 H22B 112.3(8) . . ? H22A C22 H22B 110.4(11) . . ? N8 C22 H22C 106.3(7) . . ? H22A C22 H22C 108.2(11) . . ? H22B C22 H22C 109.8(10) . . ? C24 C23 C25 107.21(10) . . ? C24 C23 C26 105.45(10) . . ? C25 C23 C26 106.73(9) . . ? C24 C23 Li2 157.56(9) . . ? C25 C23 Li2 87.35(9) . . ? C26 C23 Li2 85.78(9) . . ? C24 C23 Li3 80.33(8) . . ? C25 C23 Li3 130.86(9) . . ? C26 C23 Li3 118.03(9) . . ? Li2 C23 Li3 77.23(8) . . ? C23 C24 Li3 63.26(7) . . ? C23 C24 H24A 113.0(9) . . ? Li3 C24 H24A 84.0(9) . . ? C23 C24 H24B 112.7(9) . . ? Li3 C24 H24B 71.0(9) . . ? H24A C24 H24B 108.0(12) . . ? C23 C24 H24C 115.9(9) . . ? Li3 C24 H24C 173.4(9) . . ? H24A C24 H24C 102.0(13) . . ? H24B C24 H24C 104.3(12) . . ? C23 C25 Li2 56.08(7) . . ? C23 C25 H25A 112.5(8) . . ? Li2 C25 H25A 142.4(8) . . ? C23 C25 H25B 112.7(8) . . ? Li2 C25 H25B 112.1(8) . . ? H25A C25 H25B 105.2(12) . . ? C23 C25 H25C 112.9(9) . . ? Li2 C25 H25C 59.6(8) . . ? H25A C25 H25C 106.3(12) . . ? H25B C25 H25C 106.6(12) . . ? C23 C26 Li2 57.07(7) . . ? C23 C26 H26A 111.4(8) . . ? Li2 C26 H26A 146.6(8) . . ? C23 C26 H26B 110.8(8) . . ? Li2 C26 H26B 104.0(8) . . ? H26A C26 H26B 109.2(11) . . ? C23 C26 H26C 111.9(9) . . ? Li2 C26 H26C 60.2(9) . . ? H26A C26 H26C 106.0(12) . . ? H26B C26 H26C 107.4(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.212 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.049 _vrf_CHEMW03_compound_3 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The electron density of a highly disordered pentane was squeezed, but the sum formular contains the solvent. ; _vrf_PLAT043_compound_3 ; PROBLEM: Check Reported Molecular Weight ................ 572.75 RESPONSE: The electron density of a highly disordered pentane was squeezed, but the sum formular contains the solvent. ; _vrf_PLAT044_compound_3 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: The electron density of a highly disordered pentane was squeezed, but the sum formular contains the solvent. ; #===END