# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1743 data_LiTPP #------------------------------------------------------------------------------ _audit_creation_date 'Tue Sep 7 14:50:08 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'sir 92' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 6.43020(10) _cell_length_b 10.3539(4) _cell_length_c 12.3020(4) _cell_angle_alpha 95.305(2) _cell_angle_beta 99.351(2) _cell_angle_gamma 101.149(2) _cell_volume 786.38(4) _cell_formula_units_Z 1 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'blocklike' _exptl_crystal_colour 'bright purple' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 619.67 _chemical_formula_sum 'C44 H28 Li N4 ' _chemical_formula_moiety 'C44 H28 Li N4 ' _chemical_formula_structural ? _exptl_crystal_F_000 323.00 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'SMART' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 3152 _reflns_number_total 2197 _reflns_number_observed 1719 _reflns_observed_criterion '3.00 sigma' _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.25 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li 0 1 0.000 0.000 'International Tables' C 0 44 0.003 0.002 'International Tables' N 0 4 0.006 0.003 'International Tables' H 0 28 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom N(1) 0.2672(3) 0.1376(2) 0.5771(2) 0.02984 Uij ? ? N(2) 0.1290(3) -0.0140(2) 0.3569(2) 0.03004 Uij ? ? C(1) 0.0242(4) -0.0815(2) 0.2553(2) 0.02866 Uij ? ? C(2) 0.1435(4) -0.0414(3) 0.1698(2) 0.03421 Uij ? ? C(3) 0.3198(4) 0.0509(3) 0.2204(2) 0.03331 Uij ? ? C(4) 0.3097(4) 0.0681(2) 0.3371(2) 0.02781 Uij ? ? C(5) 0.4552(4) 0.1638(2) 0.4177(2) 0.02902 Uij ? ? C(6) 0.4378(4) 0.1903(2) 0.5302(2) 0.02953 Uij ? ? C(7) 0.6002(4) 0.2812(3) 0.6121(2) 0.03511 Uij ? ? C(8) 0.5241(4) 0.2847(2) 0.7077(2) 0.03463 Uij ? ? C(9) 0.3145(4) 0.1948(2) 0.6857(2) 0.02939 Uij ? ? C(10) 0.1795(4) 0.1701(2) 0.7642(2) 0.02983 Uij ? ? C(11) 0.6371(4) 0.2497(2) 0.3799(2) 0.02897 Uij ? ? C(12) 0.7892(4) 0.1959(3) 0.3330(2) 0.03376 Uij ? ? C(13) 0.9559(4) 0.2773(3) 0.2971(2) 0.04024 Uij ? ? C(14) 0.9722(4) 0.4136(3) 0.3082(2) 0.04024 Uij ? ? C(15) 0.8231(5) 0.4682(3) 0.3552(2) 0.04101 Uij ? ? C(16) 0.6553(4) 0.3873(3) 0.3904(2) 0.03500 Uij ? ? C(17) 0.2565(4) 0.2409(2) 0.8793(2) 0.03108 Uij ? ? C(18) 0.4508(4) 0.2286(3) 0.9423(2) 0.03880 Uij ? ? C(19) 0.5215(5) 0.2967(3) 1.0494(2) 0.04746 Uij ? ? C(20) 0.3998(5) 0.3764(3) 1.0931(2) 0.05062 Uij ? ? C(21) 0.2076(5) 0.3892(3) 1.0327(2) 0.04924 Uij ? ? C(22) 0.1355(4) 0.3225(3) 0.9247(2) 0.04065 Uij ? ? Li(1) 0.00000 0.00000 0.50000 0.04477 Uij ? ? H(1) 0.10395 -0.06986 0.08974 0.03770 Uij ? ? H(2) 0.42624 0.09816 0.18524 0.03433 Uij ? ? H(3) 0.73721 0.32868 0.59625 0.05211 Uij ? ? H(4) 0.59020 0.33842 0.77838 0.04598 Uij ? ? H(5) 0.77580 0.10032 0.32339 0.04807 Uij ? ? H(6) 1.07144 0.23828 0.26636 0.05765 Uij ? ? H(7) 1.09212 0.46793 0.27924 0.06527 Uij ? ? H(8) 0.82919 0.56277 0.36451 0.04920 Uij ? ? H(9) 0.54046 0.42569 0.42173 0.03813 Uij ? ? H(10) 0.53925 0.17181 0.91268 0.04197 Uij ? ? H(11) 0.65608 0.28520 1.08891 0.04436 Uij ? ? H(12) 0.45491 0.42873 1.17100 0.05714 Uij ? ? H(13) 0.11206 0.44513 1.06219 0.04870 Uij ? ? H(14) -0.00925 0.32856 0.87936 0.05380 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(1) 0.034(1) 0.029(1) 0.025(1) 0.0042(10) 0.0061(9) -0.0004(9) N(2) 0.030(1) 0.027(1) 0.029(1) 0.0011(9) 0.0031(9) -0.0009(9) C(1) 0.031(1) 0.028(1) 0.025(1) 0.005(1) 0.005(1) -0.002(1) C(2) 0.038(2) 0.036(2) 0.025(1) 0.002(1) 0.007(1) -0.004(1) C(3) 0.039(2) 0.033(1) 0.027(1) 0.002(1) 0.011(1) 0.002(1) C(4) 0.028(1) 0.026(1) 0.029(1) 0.004(1) 0.008(1) 0.001(1) C(5) 0.031(1) 0.026(1) 0.030(1) 0.006(1) 0.005(1) 0.004(1) C(6) 0.028(1) 0.027(1) 0.032(1) 0.001(1) 0.006(1) 0.002(1) C(7) 0.034(2) 0.033(1) 0.033(1) -0.005(1) 0.007(1) 0.001(1) C(8) 0.036(2) 0.030(1) 0.031(1) -0.004(1) 0.003(1) -0.002(1) C(9) 0.033(1) 0.026(1) 0.027(1) 0.004(1) 0.004(1) -0.001(1) C(10) 0.033(1) 0.027(1) 0.028(1) 0.005(1) 0.005(1) 0.000(1) C(11) 0.028(1) 0.030(1) 0.027(1) 0.003(1) 0.003(1) 0.001(1) C(12) 0.033(1) 0.031(1) 0.037(1) 0.006(1) 0.006(1) 0.004(1) C(13) 0.034(2) 0.044(2) 0.042(2) 0.005(1) 0.009(1) 0.004(1) C(14) 0.037(2) 0.041(2) 0.038(2) -0.004(1) 0.007(1) 0.004(1) C(15) 0.048(2) 0.030(1) 0.041(2) -0.002(1) 0.008(1) 0.006(1) C(16) 0.039(2) 0.030(1) 0.035(1) 0.006(1) 0.009(1) 0.002(1) C(17) 0.036(2) 0.027(1) 0.027(1) 0.001(1) 0.006(1) -0.001(1) C(18) 0.040(2) 0.042(2) 0.030(1) 0.003(1) 0.003(1) 0.004(1) C(19) 0.048(2) 0.050(2) 0.034(2) -0.004(1) -0.008(1) 0.009(1) C(20) 0.074(2) 0.041(2) 0.027(2) -0.002(2) 0.002(2) -0.004(1) C(21) 0.068(2) 0.044(2) 0.033(2) 0.011(2) 0.011(2) -0.008(1) C(22) 0.049(2) 0.040(2) 0.030(2) 0.007(1) 0.005(1) -0.003(1) Li(1) 0.043(4) 0.047(4) 0.036(4) -0.006(3) 0.007(3) -0.002(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1719 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0493 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0534 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.196 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.28 _refine_diff_density_max 0.18 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N(1) C(2) 1.371(3) ? ? yes N(1) C(5) 1.366(3) ? ? yes N(1) Li(1) 2.039(2) ? ? yes N(2) C(7) 1.371(3) ? ? yes N(2) C(10) 1.373(3) ? ? yes N(2) Li(1) 2.069(2) ? ? yes C(1) C(2) 1.408(4) ? ? yes C(1) C(10) 1.417(4) ? ? yes C(1) C(11) 1.492(3) ? ? yes C(2) C(3) 1.452(4) ? ? yes C(3) C(4) 1.345(4) ? ? yes C(4) C(5) 1.447(4) ? ? yes C(5) C(6) 1.413(4) ? ? yes C(6) C(7) 1.414(3) ? ? yes C(6) C(17) 1.492(4) ? ? yes C(7) C(8) 1.443(4) ? ? yes C(8) C(9) 1.351(4) ? ? yes C(9) C(10) 1.445(4) ? ? yes C(11) C(12) 1.393(4) ? ? yes C(11) C(16) 1.393(4) ? ? yes C(12) C(13) 1.401(4) ? ? yes C(13) C(14) 1.371(5) ? ? yes C(14) C(15) 1.374(5) ? ? yes C(15) C(16) 1.397(4) ? ? yes C(17) C(18) 1.399(4) ? ? yes C(17) C(22) 1.391(4) ? ? yes C(18) C(19) 1.386(4) ? ? yes C(19) C(20) 1.379(4) ? ? yes C(20) C(21) 1.387(4) ? ? yes C(21) C(22) 1.388(4) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) N(1) C(5) 106.0(2) ? ? ? yes C(2) N(1) Li(1) 127.6(2) ? ? ? yes C(5) N(1) Li(1) 126.4(2) ? ? ? yes C(7) N(2) C(10) 105.8(2) ? ? ? yes C(7) N(2) Li(1) 125.9(2) ? ? ? yes C(10) N(2) Li(1) 126.2(2) ? ? ? yes C(2) C(1) C(10) 125.8(2) ? ? ? yes C(2) C(1) C(11) 118.0(2) ? ? ? yes C(10) C(1) C(11) 116.1(2) ? ? ? yes N(1) C(2) C(1) 125.1(2) ? ? ? yes N(1) C(2) C(3) 109.9(2) ? ? ? yes C(1) C(2) C(3) 125.1(2) ? ? ? yes C(2) C(3) C(4) 106.9(2) ? ? ? yes C(3) C(4) C(5) 106.8(2) ? ? ? yes N(1) C(5) C(4) 110.3(2) ? ? ? yes N(1) C(5) C(6) 125.9(2) ? ? ? yes C(4) C(5) C(6) 123.8(2) ? ? ? yes C(5) C(6) C(7) 125.8(2) ? ? ? yes C(5) C(6) C(17) 116.7(2) ? ? ? yes C(7) C(6) C(17) 117.5(2) ? ? ? yes N(2) C(7) C(6) 124.8(2) ? ? ? yes N(2) C(7) C(8) 110.3(2) ? ? ? yes C(6) C(7) C(8) 124.8(2) ? ? ? yes C(7) C(8) C(9) 106.9(2) ? ? ? yes C(8) C(9) C(10) 106.8(2) ? ? ? yes N(2) C(10) C(1) 124.9(2) ? ? ? yes N(2) C(10) C(9) 110.2(2) ? ? ? yes C(1) C(10) C(9) 124.7(2) ? ? ? yes C(1) C(11) C(12) 120.0(2) ? ? ? yes C(1) C(11) C(16) 121.0(2) ? ? ? yes C(12) C(11) C(16) 119.0(2) ? ? ? yes C(11) C(12) C(13) 120.1(3) ? ? ? yes C(12) C(13) C(14) 120.0(3) ? ? ? yes C(13) C(14) C(15) 120.6(3) ? ? ? yes C(14) C(15) C(16) 120.1(3) ? ? ? yes C(11) C(16) C(15) 120.3(3) ? ? ? yes C(6) C(17) C(18) 119.8(2) ? ? ? yes C(6) C(17) C(22) 121.4(2) ? ? ? yes C(18) C(17) C(22) 118.8(2) ? ? ? yes C(17) C(18) C(19) 120.4(3) ? ? ? yes C(18) C(19) C(20) 120.3(3) ? ? ? yes C(19) C(20) C(21) 119.9(3) ? ? ? yes C(20) C(21) C(22) 120.0(3) ? ? ? yes C(17) C(22) C(21) 120.6(3) ? ? ? yes N(1) Li(1) N(1) 180.0 ? ? ? yes N(1) Li(1) N(2) 90.33(8) ? ? ? yes N(1) Li(1) N(2) 89.67(8) ? ? ? yes N(1) Li(1) N(2) 89.67(8) ? ? ? yes N(1) Li(1) N(2) 90.33(8) ? ? ? yes N(2) Li(1) N(2) 180.0 ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'Chemical Communications' _publ_contact_author ; John Arnold Department of Chemistry, University of California, Berkeley, CA 94720 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 510-643-5181 ' _publ_contact_author_fax ' 510-643-5482 ' _publ_contact_author_email ' arnold@socrates.berkeley.edu ' loop_ _publ_author_name _publ_author_address 'Andreas Gebauer' ; Department of Chemistry, University of California, Berkeley, CA 94720 ; 'Denisha Y. Dawson' ; Department of Chemistry, University of California, Berkeley, CA 94720 ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;