# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2096 data_liampi _audit_creation_date 99-11-16 _audit_creation_method from_xtal_archive_file_using_CIFIO _audit_update_record ? _chemical_compound_source ? #ActaC _chemical_name_systematic ? #ActaC _chemical_name_common ? #ActaC _chemical_formula_analytical ? #ActaC _chemical_formula_moiety ? #ActaC _chemical_formula_structural C44H62N12O3Li8 #ActaC _chemical_formula_sum ? #ActaC _chemical_formula_weight ? #ActaC _chemical_melting_point ? #ActaC _computing_data_collection ? #ActaC _computing_cell_refinement ? #ActaC _computing_data_reduction xtal_DIFDAT_SORTRF_ADDREF_ABSORB #ActaC _computing_structure_solution xtal_SIMPEL #ActaC _computing_structure_refinement xtal_CRYLSQ #ActaC _computing_molecular_graphics xtal #ActaC _computing_publication_material xtal_BONDLA_CIFIO #ActaC _cell_length_a 10.9177(14) #ActaC _cell_length_b 11.4313(8) #ActaC _cell_length_c 11.7098(15) #ActaC _cell_angle_alpha 71.001(8) #ActaC _cell_angle_beta 71.220(9) #ActaC _cell_angle_gamma 73.495(8) #ActaC _cell_volume 1281.7(3) #ActaC _cell_formula_units_Z 1 #ActaC _cell_measurement_temperature 293 #ActaC _cell_measurement_reflns_used ? #ActaC _cell_measurement_theta_min ? #ActaC _cell_measurement_theta_max ? #ActaC _cell_special_details #ActaC ; ? ; _symmetry_cell_setting triclinic #ActaC _symmetry_space_group_name_H-M p_-1 #ActaC _symmetry_space_group_name_Hall -p_1 #ActaC loop_ _symmetry_equiv_pos_as_xyz #ActaC +x,+y,+z -x,-y,-z _exptl_crystal_description ? #ActaC _exptl_crystal_preparation ? _exptl_crystal_colour ? #ActaC _exptl_crystal_size_max 0.28 #ActaC _exptl_crystal_size_mid 0.36 #ActaC _exptl_crystal_size_min 0.28 #ActaC _exptl_crystal_density_diffrn 1.117 #ActaC _exptl_crystal_density_meas ? #ActaC _exptl_crystal_density_method ? #ActaC _exptl_crystal_F_000 458 #ActaC _exptl_absorpt_process_details ? _exptl_absorpt_coefficient_mu ? #ActaC _exptl_absorpt_correction_type ? #ActaC _exptl_absorpt_correction_A*_min 1.016 #ActaC _exptl_absorpt_correction_A*_max 1.026 #ActaC _exptl_special_details #ActaC ; ? ; _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293 #ActaC _diffrn_radiation_wavelength 0.71073 #ActaC _diffrn_radiation_type xray_tube #ActaC _diffrn_radiation_source ? #ActaC _diffrn_radiation_monochromator ? #ActaC _diffrn_radiation_detector ? #ActaC _diffrn_measurement_device CAD4 #ActaC _diffrn_measurement_method ? #ActaC _diffrn_standards_number ? #ActaC _diffrn_standards_interval_count ? #ActaC _diffrn_standards_interval_time ? #ActaC _diffrn_standards_decay_% ? #ActaC loop_ _diffrn_standard_refln_index_h #ActaC _diffrn_standard_refln_index_k #ActaC _diffrn_standard_refln_index_l #ActaC ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _diffrn_reflns_number 5218 #ActaC _diffrn_reflns_av_R_equivalents .081 #ActaC _diffrn_reflns_av_sigmaI/netI .104 #ActaC _diffrn_reflns_limit_h_min 0 #ActaC _diffrn_reflns_limit_h_max 12 #ActaC _diffrn_reflns_limit_k_min -13 #ActaC _diffrn_reflns_limit_k_max 13 #ActaC _diffrn_reflns_limit_l_min -13 #ActaC _diffrn_reflns_limit_l_max 13 #ActaC _diffrn_reflns_theta_min 1.9 #ActaC _diffrn_reflns_theta_max 24.96 #ActaC _diffrn_reflns_reduction_process perpendicular_monochr_Lp #ActaC loop_ _atom_type_symbol #ActaC _atom_type_description #ActaC _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real #ActaC _atom_type_scat_dispersion_imag #ActaC _atom_type_scat_source #ActaC C ? 0 44 .002 .002 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 H ? 0 62 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 N ? 0 12 .004 .003 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 O ? 0 3 .008 .006 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 Li ? 0 8 0 0 Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 loop_ _atom_site_label #ActaC _atom_site_fract_x #ActaC _atom_site_fract_y #ActaC _atom_site_fract_z #ActaC _atom_site_U_iso_or_equiv #ActaC _atom_site_thermal_displace_type #ActaC _atom_site_calc_flag #ActaC _atom_site_calc_attached_atom #ActaC Li1 .1715(11) .5261(12) .4260(11) .054(14) Uani ? ? Li2 .1849(14) .6272(12) .6032(12) .072(17) Uani ? ? Li3 .0454(11) .4407(12) .6539(10) .058(15) Uani ? ? Li4 -.0420(13) .6607(11) .5264(11) .063(15) Uani ? ? O1 .00000 .50000 .50000 .041(7) Uani ? ? N1 .2084(5) .6773(5) .2823(5) .049(7) Uani ? ? N2 .1075(6) .7570(5) .4545(5) .058(7) Uani ? ? C1 .1721(6) .7802(6) .3337(6) .046(8) Uani ? ? C2 .2032(7) .8978(7) .2575(7) .065(10) Uani ? ? C3 .2701(8) .9049(8) .1325(7) .079(11) Uani ? ? C4 .3058(8) .8026(7) .0850(6) .079(11) Uani ? ? C5 .2763(7) .6917(7) .1610(6) .058(9) Uani ? ? C6 .3098(8) .5737(8) .1162(7) .080(11) Uani ? ? N3 .2037(5) .3076(5) .6903(5) .049(7) Uani ? ? N4 .2929(5) .4700(5) .5387(5) .053(7) Uani ? ? C7 .3108(7) .3513(6) .6177(6) .050(8) Uani ? ? C8 .4393(7) .2785(7) .6266(7) .065(10) Uani ? ? C9 .4463(7) .1633(8) .7089(7) .076(11) Uani ? ? C10 .3348(8) .1207(7) .7872(7) .081(11) Uani ? ? C11 .2104(7) .1940(6) .7758(6) .057(9) Uani ? ? C12 .0840(8) .1548(7) .8584(7) .077(10) Uani ? ? N5 -.1686(5) .7067(5) .6824(5) .056(7) Uani ? ? N6 .0155(6) .5750(5) .7410(5) .066(8) Uani ? ? C13 -.1017(7) .6539(6) .7720(6) .058(9) Uani ? ? C14 -.1630(8) .6787(8) .8901(7) .081(11) Uani ? ? C15 -.2808(9) .7550(7) .9124(7) .088(11) Uani ? ? C16 -.3492(7) .8066(7) .8224(7) .081(11) Uani ? ? C17 -.2884(7) .7814(7) .7057(7) .069(10) Uani ? ? C18 -.3523(8) .8332(8) .6004(8) .094(12) Uani ? ? O1a .2755(6) .7040(5) .6704(5) .101(9) Uani ? ? C1a .3326(16) .6457(13) .7661(10) .19(2) Uani ? ? C2a .3644(11) .5146(10) .7967(9) .133(17) Uani ? ? C3a .2481(12) .8442(13) .6404(11) .16(2) Uani ? ? C4a .1278(11) .8946(11) .6989(12) .16(2) Uani ? ? H2 .17031 .98027 .29487 .03500 Uiso ? ? H3 .29231 .99313 .07500 .03500 Uiso ? ? H4 .36338 .81030 -.01082 .03500 Uiso ? ? H6a .24215 .57952 .06409 .03500 Uiso ? ? H6b .30090 .49140 .18984 .03500 Uiso ? ? H6c .40228 .55973 .05531 .03500 Uiso ? ? H8 .52812 .31502 .56471 .03500 Uiso ? ? H9 .54076 .10261 .71682 .03500 Uiso ? ? H10 .33967 .02760 .85297 .03500 Uiso ? ? H12a .05782 .18488 .94267 .03500 Uiso ? ? H12b .09158 .05880 .88314 .03500 Uiso ? ? H12c .00715 .19993 .81466 .03500 Uiso ? ? H14 -.11105 .63482 .96632 .03500 Uiso ? ? H15 -.32561 .77410 .99984 .03500 Uiso ? ? H16 -.44617 .85996 .84004 .03500 Uiso ? ? H18a -.35929 .93246 .56643 .03500 Uiso ? ? H18b -.45015 .81765 .63029 .03500 Uiso ? ? H18c -.30092 .79163 .52763 .03500 Uiso ? ? H1aa .25655 .67501 .85207 .03500 Uiso ? ? H1ab .40920 .69010 .75749 .03500 Uiso ? ? H2ab .45524 .49183 .73172 .03500 Uiso ? ? H2ac .29238 .48661 .77407 .03500 Uiso ? ? H2aa .37440 .47447 .88614 .03500 Uiso ? ? H3aa .27539 .88585 .54359 .03500 Uiso ? ? H3ab .32188 .87215 .67326 .03500 Uiso ? ? H4ab .06810 .96051 .64285 .03500 Uiso ? ? H4ac .12022 .92855 .77372 .03500 Uiso ? ? H4aa .07052 .81767 .74752 .03500 Uiso ? ? H2n .07307 .82661 .50407 .03500 Uiso ? ? H4n .38797 .46446 .47968 .03500 Uiso ? ? H6n .03217 .51293 .82500 .03500 Uiso ? ? loop_ _atom_site_aniso_label #ActaC _atom_site_aniso_U_11 #ActaC _atom_site_aniso_U_22 #ActaC _atom_site_aniso_U_33 #ActaC _atom_site_aniso_U_12 #ActaC _atom_site_aniso_U_13 #ActaC _atom_site_aniso_U_23 #ActaC Li1 .007(8) .073(9) .063(8) -.001(6) -.007(6) -.001(7) Li2 .083(12) .051(8) .066(9) -.024(7) -.007(8) .003(7) Li3 .035(9) .072(9) .048(7) .010(7) -.020(6) .000(6) Li4 .065(11) .049(8) .059(8) .011(7) -.010(7) -.017(6) O1 .027(4) .047(4) .049(4) -.002(3) -.018(3) -.009(3) N1 .039(4) .055(4) .049(4) -.006(3) -.021(3) -.004(3) N2 .062(5) .066(4) .038(3) -.011(4) -.001(3) -.017(3) C1 .034(5) .047(4) .063(5) -.006(4) -.033(4) -.005(4) C2 .048(6) .068(5) .077(5) -.013(4) -.026(4) -.006(4) C3 .089(7) .078(6) .062(5) -.049(5) -.025(5) .024(5) C4 .101(8) .072(6) .049(5) -.035(5) .000(5) -.001(4) C5 .052(6) .074(6) .047(5) -.029(4) -.006(4) -.006(4) C6 .086(7) .093(7) .052(5) -.027(5) -.006(5) -.008(5) N3 .045(4) .043(4) .053(4) -.004(3) -.016(3) -.007(3) N4 .041(4) .049(4) .056(4) -.011(3) -.007(3) -.000(3) C7 .053(6) .050(5) .049(4) -.001(4) -.028(4) -.009(4) C8 .043(6) .071(6) .075(5) -.004(4) -.020(4) -.012(4) C9 .055(6) .079(6) .085(6) .019(5) -.039(5) -.013(5) C10 .072(7) .070(6) .073(6) -.000(5) -.025(5) .012(5) C11 .072(6) .051(5) .048(5) .003(4) -.030(4) -.012(4) C12 .076(7) .057(6) .071(6) -.010(5) -.015(5) .012(4) N5 .045(5) .049(4) .068(4) -.004(3) -.007(3) -.021(3) N6 .081(5) .059(4) .043(4) -.003(4) -.015(3) -.004(3) C13 .073(6) .038(4) .064(5) -.020(4) -.010(4) -.013(4) C14 .107(8) .072(6) .062(5) -.022(5) .002(5) -.036(5) C15 .125(8) .054(5) .072(6) -.021(5) .012(5) -.033(5) C16 .059(7) .066(6) .098(7) -.005(5) .013(5) -.032(5) C17 .060(6) .061(6) .079(5) -.006(4) -.007(5) -.025(4) C18 .063(7) .076(6) .134(8) .007(5) -.018(6) -.042(6) O1a .116(5) .089(5) .122(5) -.029(4) -.058(4) -.024(4) C1a .318(17) .182(13) .127(9) -.087(12) -.152(11) .000(9) C2a .166(11) .111(8) .129(9) .008(8) -.078(8) -.031(7) C3a .155(12) .208(14) .171(11) -.106(11) -.051(10) -.035(10) C4a .111(10) .163(12) .226(13) .010(8) -.032(9) -.117(11) _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _refine_special_details sfls:_F____sigma_weight_atomblock_matrix _refine_ls_structure_factor_coef F #ActaC _refine_ls_matrix_type atomblock #ActaC _refine_ls_weighting_scheme sigma #ActaC _refine_ls_hydrogen_treatment ? #ActaC _refine_ls_extinction_method none #ActaC _refine_ls_extinction_coef .00000 #ActaC _refine_ls_extinction_expression ? _refine_ls_abs_structure_details none #ActaC _refine_ls_abs_structure_Flack 0 #ActaC _refine_ls_number_reflns 1397 #ActaC _refine_ls_number_parameters 305 #ActaC _refine_ls_number_restraints 0 #ActaC _refine_ls_number_constraints 0 #ActaC _refine_ls_R_factor_all .333 #ActaC _refine_ls_R_factor_obs .088 #ActaC _refine_ls_wR_factor_all .114 #ActaC _refine_ls_wR_factor_obs .11 #ActaC _refine_ls_goodness_of_fit_all 2.684 #ActaC _refine_ls_goodness_of_fit_obs 4.839 #ActaC _refine_ls_shift/esd_max 1.728 #ActaC _refine_ls_shift/esd_mean .359 #ActaC _refine_diff_density_min -.982 #ActaC _refine_diff_density_max .789 #ActaC _geom_special_details ? #ActaC loop_ _geom_bond_atom_site_label_1 #ActaC _geom_bond_atom_site_label_2 #ActaC _geom_bond_distance #ActaC _geom_bond_site_symmetry_1 #ActaC _geom_bond_site_symmetry_2 #ActaC _geom_bond_publ_flag #ActaC Li1 Li3 2.583(14) . . ? Li1 Li4 2.560(15) . . ? Li1 O1 1.857(11) . . ? Li1 N1 2.012(12) . . ? Li1 N4 2.000(15) . . ? Li2 N2 2.122(14) . . ? Li2 N4 2.073(14) . . ? Li2 N6 2.112(14) . . ? Li2 O1a 1.95(2) . . ? Li3 Li4 2.564(15) . . ? Li3 O1 1.882(12) . . ? Li3 N3 2.011(12) . . ? Li3 N6 2.006(16) . . ? Li4 O1 1.865(14) . . ? Li4 N2 2.029(15) . . ? Li4 N5 2.028(13) . . ? N1 C1 1.394(10) . . ? N1 C5 1.354(8) . . ? N2 C1 1.337(7) . . ? N2 H2n 1.049(6) . . ? C1 C2 1.415(10) . . ? C2 C3 1.396(10) . . ? C2 H2 1.089(9) . . ? C3 C4 1.362(13) . . ? C3 H3 1.059(8) . . ? C4 C5 1.347(10) . . ? C4 H4 1.084(7) . . ? C5 C6 1.511(13) . . ? C6 H6a 1.076(10) . . ? C6 H6b 1.053(7) . . ? C6 H6c 1.035(7) . . ? N3 C7 1.325(9) . . ? N3 C11 1.356(7) . . ? N4 C7 1.373(8) . . ? N4 H4n 1.043(5) . . ? C7 C8 1.430(10) . . ? C8 C9 1.354(10) . . ? C8 H8 1.105(7) . . ? C9 C10 1.374(11) . . ? C9 H9 1.080(7) . . ? C10 C11 1.400(11) . . ? C10 H10 1.090(7) . . ? C11 C12 1.501(10) . . ? C12 H12a 1.076(8) . . ? C12 H12b 1.026(8) . . ? C12 H12c 1.044(8) . . ? N5 C13 1.352(10) . . ? N5 C17 1.343(8) . . ? N6 C13 1.357(8) . . ? N6 H6n 1.045(5) . . ? C13 C14 1.411(11) . . ? C14 C15 1.333(11) . . ? C14 H14 1.115(9) . . ? C15 C16 1.367(13) . . ? C15 H15 1.047(8) . . ? C16 C17 1.398(11) . . ? C16 H16 1.054(7) . . ? C17 C18 1.483(13) . . ? C18 H18a 1.063(8) . . ? C18 H18b 1.059(9) . . ? C18 H18c 1.035(9) . . ? O1a C1a 1.347(16) . . ? O1a C3a 1.487(15) . . ? C1a C2a 1.389(18) . . ? C1a H1aa 1.157(12) . . ? C1a H1ab 1.059(19) . . ? C2a H2ab 1.062(10) . . ? C2a H2ac 1.059(14) . . ? C2a H2aa 1.026(11) . . ? C3a C4a 1.332(15) . . ? C3a H3aa 1.054(11) . . ? C3a H3ab 1.152(16) . . ? C4a H4ab 1.047(12) . . ? C4a H4ac 1.041(16) . . ? C4a H4aa 1.115(13) . . ? loop_ _geom_contact_atom_site_label_1 #ActaC _geom_contact_atom_site_label_2 #ActaC _geom_contact_distance #ActaC _geom_contact_site_symmetry_1 #ActaC _geom_contact_site_symmetry_2 #ActaC _geom_contact_publ_flag #ActaC ? ? ? ? ? ? loop_ _geom_angle_atom_site_label_1 #ActaC _geom_angle_atom_site_label_2 #ActaC _geom_angle_atom_site_label_3 #ActaC _geom_angle #ActaC _geom_angle_site_symmetry_1 #ActaC _geom_angle_site_symmetry_2 #ActaC _geom_angle_site_symmetry_3 #ActaC _geom_angle_publ_flag #ActaC Li3 Li1 Li4 59.8(4) . . . ? Li3 Li1 O1 46.7(4) . . . ? Li3 Li1 N1 147.7(7) . . . ? Li3 Li1 N4 69.8(5) . . . ? Li4 Li1 O1 46.7(4) . . . ? Li4 Li1 N1 89.9(5) . . . ? Li4 Li1 N4 108.2(7) . . . ? O1 Li1 N1 120.6(6) . . . ? O1 Li1 N4 116.4(6) . . . ? N1 Li1 N4 114.5(7) . . . ? N2 Li2 N4 106.1(7) . . . ? N2 Li2 N6 103.6(7) . . . ? N2 Li2 O1a 112.5(7) . . . ? N4 Li2 N6 107.5(7) . . . ? N4 Li2 O1a 117.0(8) . . . ? N6 Li2 O1a 109.3(7) . . . ? Li1 Li3 Li4 59.7(4) . . . ? Li1 Li3 O1 45.9(4) . . . ? Li1 Li3 N3 92.2(5) . . . ? Li1 Li3 N6 106.1(6) . . . ? Li4 Li3 O1 46.6(4) . . . ? Li4 Li3 N3 147.3(6) . . . ? Li4 Li3 N6 68.0(5) . . . ? O1 Li3 N3 125.4(6) . . . ? O1 Li3 N6 114.5(6) . . . ? N3 Li3 N6 109.4(7) . . . ? Li1 Li4 Li3 60.5(4) . . . ? Li1 Li4 O1 46.4(4) . . . ? Li1 Li4 N2 69.0(5) . . . ? Li1 Li4 N5 148.9(7) . . . ? Li3 Li4 O1 47.1(4) . . . ? Li3 Li4 N2 107.8(6) . . . ? Li3 Li4 N5 91.4(5) . . . ? O1 Li4 N2 115.3(6) . . . ? O1 Li4 N5 123.9(6) . . . ? N2 Li4 N5 112.2(8) . . . ? Li1 O1 Li3 87.4(5) . . . ? Li1 O1 Li4 86.9(6) . . . ? Li1 O1 Li1 180.0(8) . . 2_566 ? Li1 O1 Li3 92.6(5) . . 2_566 ? Li1 O1 Li4 93.1(6) . . 2_566 ? Li3 O1 Li4 86.3(6) . . . ? Li3 O1 Li1 92.6(5) . . 2_566 ? Li3 O1 Li3 180.0(7) . . 2_566 ? Li3 O1 Li4 93.7(6) . . 2_566 ? Li4 O1 Li1 93.1(6) . . 2_566 ? Li4 O1 Li3 93.7(6) . . 2_566 ? Li4 O1 Li4 180.0(6) . . 2_566 ? Li1 O1 Li3 87.4(5) 2_566 . 2_566 ? Li1 O1 Li4 86.9(6) 2_566 . 2_566 ? Li3 O1 Li4 86.3(6) 2_566 . 2_566 ? Li1 N1 C1 106.3(5) . . . ? Li1 N1 C5 133.7(6) . . . ? C1 N1 C5 118.9(6) . . . ? Li2 N2 Li4 84.3(6) . . . ? Li2 N2 C1 125.5(5) . . . ? Li2 N2 H2n 90.5(5) . . . ? Li4 N2 C1 122.6(7) . . . ? Li4 N2 H2n 101.4(5) . . . ? C1 N2 H2n 122.7(6) . . . ? N1 C1 N2 115.0(6) . . . ? N1 C1 C2 119.5(6) . . . ? N2 C1 C2 125.5(7) . . . ? C1 C2 C3 117.6(8) . . . ? C1 C2 H2 120.3(6) . . . ? C3 C2 H2 122.0(7) . . . ? C2 C3 C4 121.7(7) . . . ? C2 C3 H3 117.7(8) . . . ? C4 C3 H3 120.6(6) . . . ? C3 C4 C5 119.0(6) . . . ? C3 C4 H4 119.4(7) . . . ? C5 C4 H4 121.5(8) . . . ? N1 C5 C4 123.2(7) . . . ? N1 C5 C6 114.0(6) . . . ? C4 C5 C6 122.7(6) . . . ? C5 C6 H6a 110.1(6) . . . ? C5 C6 H6b 113.0(7) . . . ? C5 C6 H6c 114.2(8) . . . ? H6a C6 H6b 105.4(9) . . . ? H6a C6 H6c 104.6(7) . . . ? H6b C6 H6c 108.9(7) . . . ? Li3 N3 C7 107.8(5) . . . ? Li3 N3 C11 129.9(6) . . . ? C7 N3 C11 122.1(6) . . . ? Li1 N4 Li2 84.6(6) . . . ? Li1 N4 C7 123.3(7) . . . ? Li1 N4 H4n 105.5(5) . . . ? Li2 N4 C7 122.1(5) . . . ? Li2 N4 H4n 124.2(6) . . . ? C7 N4 H4n 98.1(4) . . . ? N3 C7 N4 117.5(6) . . . ? N3 C7 C8 120.5(5) . . . ? N4 C7 C8 122.0(6) . . . ? C7 C8 C9 117.5(6) . . . ? C7 C8 H8 120.0(6) . . . ? C9 C8 H8 122.5(6) . . . ? C8 C9 C10 121.6(7) . . . ? C8 C9 H9 120.7(7) . . . ? C10 C9 H9 117.7(6) . . . ? C9 C10 C11 119.3(6) . . . ? C9 C10 H10 122.0(7) . . . ? C11 C10 H10 118.4(7) . . . ? N3 C11 C10 118.8(6) . . . ? N3 C11 C12 118.5(6) . . . ? C10 C11 C12 122.6(6) . . . ? C11 C12 H12a 109.3(8) . . . ? C11 C12 H12b 112.4(6) . . . ? C11 C12 H12c 110.1(6) . . . ? H12a C12 H12b 107.8(6) . . . ? H12a C12 H12c 106.7(6) . . . ? H12b C12 H12c 110.3(9) . . . ? Li4 N5 C13 105.2(5) . . . ? Li4 N5 C17 133.9(6) . . . ? C13 N5 C17 120.5(6) . . . ? Li2 N6 Li3 84.4(6) . . . ? Li2 N6 C13 125.9(5) . . . ? Li2 N6 H6n 115.8(6) . . . ? Li3 N6 C13 124.8(7) . . . ? Li3 N6 H6n 95.8(5) . . . ? C13 N6 H6n 106.0(5) . . . ? N5 C13 N6 115.9(6) . . . ? N5 C13 C14 117.8(6) . . . ? N6 C13 C14 126.2(7) . . . ? C13 C14 C15 121.7(8) . . . ? C13 C14 H14 119.3(7) . . . ? C15 C14 H14 119.0(7) . . . ? C14 C15 C16 120.4(8) . . . ? C14 C15 H15 121.6(9) . . . ? C16 C15 H15 118.0(7) . . . ? C15 C16 C17 117.7(7) . . . ? C15 C16 H16 122.1(8) . . . ? C17 C16 H16 120.1(8) . . . ? N5 C17 C16 121.8(7) . . . ? N5 C17 C18 115.6(7) . . . ? C16 C17 C18 122.6(6) . . . ? C17 C18 H18a 111.0(10) . . . ? C17 C18 H18b 110.4(7) . . . ? C17 C18 H18c 111.5(7) . . . ? H18a C18 H18b 106.4(6) . . . ? H18a C18 H18c 108.9(7) . . . ? H18b C18 H18c 108.4(10) . . . ? Li2 O1a C1a 126.0(9) . . . ? Li2 O1a C3a 117.3(8) . . . ? C1a O1a C3a 114.3(11) . . . ? O1a C1a C2a 117.3(14) . . . ? O1a C1a H1aa 105.3(11) . . . ? O1a C1a H1ab 110.1(10) . . . ? C2a C1a H1aa 107.3(9) . . . ? C2a C1a H1ab 114.9(13) . . . ? H1aa C1a H1ab 100.0(14) . . . ? C1a C2a H2ab 105.1(9) . . . ? C1a C2a H2ac 105.2(11) . . . ? C1a C2a H2aa 113.8(12) . . . ? H2ab C2a H2ac 106.4(11) . . . ? H2ab C2a H2aa 110.1(10) . . . ? H2ac C2a H2aa 115.5(10) . . . ? O1a C3a C4a 113.9(10) . . . ? O1a C3a H3aa 112.4(11) . . . ? O1a C3a H3ab 107.4(9) . . . ? C4a C3a H3aa 114.6(11) . . . ? C4a C3a H3ab 106.7(13) . . . ? H3aa C3a H3ab 100.6(11) . . . ? C3a C4a H4ab 116.9(11) . . . ? C3a C4a H4ac 117.3(14) . . . ? C3a C4a H4aa 108.2(11) . . . ? H4ab C4a H4ac 108.8(11) . . . ? H4ab C4a H4aa 102.9(12) . . . ? H4ac C4a H4aa 100.4(9) . . . ? loop_ _geom_torsion_atom_site_label_1 #ActaC _geom_torsion_atom_site_label_2 #ActaC _geom_torsion_atom_site_label_3 #ActaC _geom_torsion_atom_site_label_4 #ActaC _geom_torsion #ActaC _geom_torsion_site_symmetry_1 #ActaC _geom_torsion_site_symmetry_2 #ActaC _geom_torsion_site_symmetry_3 #ActaC _geom_torsion_site_symmetry_4 #ActaC _geom_torsion_publ_flag #ActaC ? ? ? ? ? ? ? ? ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min -12 _reflns_limit_l_max 13 _reflns_number_total 4490 #ActaC _reflns_number_observed 1492 #ActaC _reflns_observed_criterion refl_observed_if_F____>_.000_sigma(F___) _reflns_d_resolution_high .842 _reflns_d_resolution_low 10.711 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? 1.4563 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_meas _refln_F_calc _refln_F_sigma _refln_observed_status _refln_scale_group_code ? ? ? ? ? ? ? ? _publ_requested_journal ? #ActaC _publ_requested_coeditor_name ? #ActaC _publ_contact_author #ActaC ; ? name ? institute ? department ? address ? city ? country ; _publ_contact_letter #ActaC ; ? letter to co-editor ; _publ_contact_author_phone ? #ActaC _publ_contact_author_fax ? #ActaC _publ_contact_author_email ? #ActaC loop_ _publ_author_name #ActaC _publ_author_address #ActaC '? surname, initials' ; ? institute ? department ? address ? city ? country ; _publ_section_title #ActaC ; ? ; _publ_section_abstract #ActaC ; ? ; _publ_section_comment #ActaC ; ? ; _publ_section_experimental #ActaC ; ? ; _publ_section_references #ActaC ; ? ; _publ_section_figure_captions #ActaC ; ? ; _publ_section_acknowledgements #ActaC ; ? ; #============================================================================== # (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #===END data_pj103 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H37 Li4 N8 O0.50' _chemical_formula_weight 473.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4923(17) _cell_length_b 13.4905(19) _cell_length_c 19.326(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.137(3) _cell_angle_gamma 90.00 _cell_volume 2917.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9678 _exptl_absorpt_correction_T_max 0.9678 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13241 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.32 _reflns_number_total 4211 _reflns_number_gt 2547 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0942P)^2^+0.3583P] 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 SHELXL _refine_ls_extinction_coef 0.0039(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4211 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.216 _refine_ls_shift/su_mean 0.014 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 O1 O 0.5000 0.0000 0.0000 0.0474(6) Uani 1 2 d S . . Li1 Li 0.3603(4) 0.0620(3) 0.0113(3) 0.0605(12) Uani 1 1 d . . . Li2 Li 0.6010(4) 0.0746(3) 0.0714(2) 0.0634(12) Uani 1 1 d . . . Li3 Li 0.4926(4) -0.0934(3) 0.0702(2) 0.0594(11) Uani 1 1 d . . . Li4 Li 0.2699(4) 0.0821(3) -0.1317(2) 0.0619(12) Uani 1 1 d . . . N1A N 0.33804(18) 0.20693(15) 0.02602(12) 0.0539(6) Uani 1 1 d . . . N2A N 0.3800(2) 0.19815(18) -0.08431(14) 0.0599(7) Uani 1 1 d . . . H2NA H 0.384(2) 0.2341(19) -0.1187(15) 0.056(9) Uiso 1 1 d . . . C1A C 0.3445(2) 0.25411(19) -0.03506(15) 0.0536(7) Uani 1 1 d . . . C2A C 0.3144(3) 0.3560(2) -0.04362(18) 0.0747(9) Uani 1 1 d . . . H2A H 0.3196 0.3897 -0.0848 0.144(3) Uiso 1 1 calc R . . C3A C 0.2777(3) 0.4033(2) 0.0098(2) 0.0912(11) Uani 1 1 d . . . H3A H 0.2580 0.4702 0.0050 0.144(3) Uiso 1 1 calc R . . C4A C 0.2692(3) 0.3542(2) 0.0709(2) 0.0830(10) Uani 1 1 d . . . H4A H 0.2427 0.3868 0.1069 0.144(3) Uiso 1 1 calc R . . C5A C 0.3004(2) 0.2570(2) 0.07729(16) 0.0612(8) Uani 1 1 d . . . C6A C 0.2935(3) 0.1971(2) 0.14182(17) 0.0819(10) Uani 1 1 d . . . H6A1 H 0.3185 0.1303 0.1360 0.144(3) Uiso 1 1 calc R . . H6A2 H 0.2127 0.1968 0.1476 0.144(3) Uiso 1 1 calc R . . H6A3 H 0.3449 0.2259 0.1831 0.144(3) Uiso 1 1 calc R . . N1B N 0.7341(2) 0.15574(17) 0.05013(11) 0.0593(6) Uani 1 1 d . . . N2B N 0.7915(2) -0.00733(18) 0.05067(13) 0.0612(7) Uani 1 1 d . . . H2NB H 0.856(3) -0.050(2) 0.0492(16) 0.082(10) Uiso 1 1 d . . . C1B C 0.8221(3) 0.0891(2) 0.04819(14) 0.0592(7) Uani 1 1 d . . . C2B C 0.9371(3) 0.1233(3) 0.04375(18) 0.0827(10) Uani 1 1 d . . . H2B H 0.9986 0.0786 0.0436 0.144(3) Uiso 1 1 calc R . . C3B C 0.9560(3) 0.2226(3) 0.0398(2) 0.1036(13) Uani 1 1 d . . . H3B H 1.0305 0.2457 0.0360 0.144(3) Uiso 1 1 calc R . . C4B C 0.8647(4) 0.2898(3) 0.0413(2) 0.1007(13) Uani 1 1 d . . . H4B H 0.8775 0.3576 0.0388 0.144(3) Uiso 1 1 calc R . . C5B C 0.7561(3) 0.2540(2) 0.04661(16) 0.0720(9) Uani 1 1 d . . . C6B C 0.6534(3) 0.3211(2) 0.04923(19) 0.0900(11) Uani 1 1 d . . . H6B1 H 0.5851 0.2821 0.0526 0.144(3) Uiso 1 1 calc R . . H6B2 H 0.6346 0.3606 0.0068 0.144(3) Uiso 1 1 calc R . . H6B3 H 0.6748 0.3637 0.0899 0.144(3) Uiso 1 1 calc R . . N1C N 0.4444(2) -0.05115(16) 0.16055(12) 0.0593(6) Uani 1 1 d . . . N2C N 0.6278(2) 0.02133(19) 0.17041(14) 0.0622(7) Uani 1 1 d . . . H2NC H 0.675(3) 0.051(2) 0.1985(16) 0.066(10) Uiso 1 1 d . . . C1C C 0.5380(3) -0.0022(2) 0.20141(15) 0.0588(7) Uani 1 1 d . . . C2C C 0.5367(3) 0.0202(2) 0.27306(17) 0.0840(10) Uani 1 1 d . . . H2C H 0.6015 0.0518 0.3023 0.144(3) Uiso 1 1 calc R . . C3C C 0.4399(4) -0.0048(3) 0.2984(2) 0.1053(13) Uani 1 1 d . . . H3C H 0.4382 0.0100 0.3451 0.144(3) Uiso 1 1 calc R . . C4C C 0.3441(4) -0.0522(3) 0.2553(2) 0.0955(12) Uani 1 1 d . . . H4C H 0.2769 -0.0680 0.2722 0.144(3) Uiso 1 1 calc R . . C5C C 0.3491(3) -0.0756(2) 0.18707(17) 0.0739(9) Uani 1 1 d . . . C6C C 0.2512(3) -0.1290(3) 0.1383(2) 0.1071(13) Uani 1 1 d . . . H6C1 H 0.2713 -0.1378 0.0931 0.144(3) Uiso 1 1 calc R . . H6C2 H 0.1787 -0.0913 0.1321 0.144(3) Uiso 1 1 calc R . . H6C3 H 0.2400 -0.1926 0.1581 0.144(3) Uiso 1 1 calc R . . N1 N 0.3651(2) 0.64072(18) -0.28485(14) 0.0720(7) Uani 1 1 d . . . N2 N 0.4711(2) 0.3890(2) -0.21803(14) 0.0777(8) Uani 1 1 d . . . C1 C 0.4527(3) 0.6856(3) -0.3199(2) 0.1006(12) Uani 1 1 d . . . H1A H 0.4136 0.7334 -0.3541 0.144(3) Uiso 1 1 calc R . . H1B H 0.4879 0.6350 -0.3434 0.144(3) Uiso 1 1 calc R . . H1C H 0.5139 0.7177 -0.2850 0.144(3) Uiso 1 1 calc R . . C2 C 0.3118(3) 0.7184(3) -0.2491(2) 0.0999(12) Uani 1 1 d . . . H2D H 0.2766 0.7680 -0.2831 0.144(3) Uiso 1 1 calc R . . H2E H 0.3726 0.7482 -0.2127 0.144(3) Uiso 1 1 calc R . . H2F H 0.2514 0.6900 -0.2282 0.144(3) Uiso 1 1 calc R . . C3 C 0.4174(3) 0.5658(3) -0.23143(17) 0.0853(10) Uani 1 1 d . . . H3D H 0.3577 0.5452 -0.2061 0.144(3) Uiso 1 1 calc R . . H3E H 0.4833 0.5953 -0.1973 0.144(3) Uiso 1 1 calc R . . C4 C 0.4620(3) 0.4759(2) -0.26403(18) 0.0769(9) Uani 1 1 d . . . H4D H 0.4079 0.4614 -0.3092 0.144(3) Uiso 1 1 calc R . . H4E H 0.5399 0.4903 -0.2731 0.144(3) Uiso 1 1 calc R . . C5 C 0.4949(4) 0.3020(3) -0.2567(2) 0.0985(12) Uani 1 1 d . . . H5A H 0.4326 0.2943 -0.2989 0.144(3) Uiso 1 1 calc R . . H5B H 0.4975 0.2444 -0.2272 0.144(3) Uiso 1 1 calc R . . H5C H 0.5702 0.3097 -0.2696 0.144(3) Uiso 1 1 calc R . . C6 C 0.5649(4) 0.4020(3) -0.1535(2) 0.1140(14) Uani 1 1 d . . . H6A H 0.5481 0.4598 -0.1285 0.144(3) Uiso 1 1 calc R . . H6B H 0.6406 0.4100 -0.1661 0.144(3) Uiso 1 1 calc R . . H6C H 0.5677 0.3447 -0.1237 0.144(3) 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 O1 0.0500(14) 0.0503(14) 0.0439(14) 0.0005(11) 0.0147(11) -0.0026(11) Li1 0.064(3) 0.057(3) 0.064(3) -0.005(2) 0.021(2) -0.001(2) Li2 0.074(3) 0.062(3) 0.057(3) -0.001(2) 0.020(2) -0.010(2) Li3 0.063(3) 0.068(3) 0.052(3) 0.008(2) 0.024(2) 0.002(2) Li4 0.063(3) 0.065(3) 0.058(3) 0.005(2) 0.014(2) 0.000(2) N1A 0.0574(14) 0.0524(13) 0.0533(14) -0.0066(11) 0.0150(11) -0.0024(10) N2A 0.0718(16) 0.0585(15) 0.0518(15) 0.0038(13) 0.0190(12) -0.0009(12) C1A 0.0531(16) 0.0515(16) 0.0557(18) -0.0054(14) 0.0111(13) -0.0013(12) C2A 0.093(2) 0.0498(18) 0.083(2) 0.0032(17) 0.0245(18) 0.0038(16) C3A 0.119(3) 0.0541(19) 0.106(3) -0.010(2) 0.037(2) 0.0113(19) C4A 0.106(3) 0.062(2) 0.089(3) -0.0151(19) 0.038(2) 0.0036(18) C5A 0.0622(18) 0.0599(18) 0.0631(19) -0.0092(15) 0.0173(14) -0.0041(14) C6A 0.101(3) 0.087(2) 0.063(2) -0.0059(18) 0.0310(18) 0.0005(18) N1B 0.0699(16) 0.0559(15) 0.0515(14) 0.0026(11) 0.0125(11) -0.0122(12) N2B 0.0599(15) 0.0622(16) 0.0632(16) 0.0010(12) 0.0178(12) -0.0044(13) C1B 0.0599(18) 0.070(2) 0.0468(16) 0.0052(14) 0.0112(13) -0.0146(16) C2B 0.063(2) 0.104(3) 0.080(2) 0.0109(19) 0.0144(16) -0.0235(18) C3B 0.075(3) 0.113(3) 0.119(3) 0.023(3) 0.014(2) -0.042(2) C4B 0.099(3) 0.083(3) 0.112(3) 0.018(2) 0.006(2) -0.035(2) C5B 0.082(2) 0.069(2) 0.060(2) 0.0087(16) 0.0054(16) -0.0191(18) C6B 0.116(3) 0.065(2) 0.085(3) 0.0073(18) 0.015(2) -0.006(2) N1C 0.0635(15) 0.0672(15) 0.0532(14) 0.0087(12) 0.0255(12) 0.0055(12) N2C 0.0673(17) 0.0682(16) 0.0529(16) -0.0070(13) 0.0174(13) -0.0049(13) C1C 0.075(2) 0.0555(17) 0.0501(17) 0.0063(14) 0.0222(15) 0.0100(14) C2C 0.117(3) 0.089(2) 0.0508(19) -0.0055(17) 0.0307(19) -0.001(2) C3C 0.138(4) 0.130(3) 0.063(2) 0.002(2) 0.054(3) 0.004(3) C4C 0.102(3) 0.128(3) 0.071(3) 0.016(2) 0.052(2) 0.013(2) C5C 0.073(2) 0.091(2) 0.067(2) 0.0199(18) 0.0340(17) 0.0115(17) C6C 0.073(2) 0.166(4) 0.089(3) 0.017(3) 0.034(2) -0.024(2) N1 0.0688(16) 0.0718(16) 0.0705(17) -0.0100(14) 0.0059(13) 0.0001(13) N2 0.0763(18) 0.0831(19) 0.0736(18) 0.0004(15) 0.0169(14) -0.0030(14) C1 0.082(2) 0.094(3) 0.123(3) -0.004(2) 0.016(2) -0.021(2) C2 0.108(3) 0.095(3) 0.089(3) -0.034(2) 0.005(2) 0.017(2) C3 0.090(2) 0.092(2) 0.065(2) -0.0123(19) -0.0024(18) 0.0089(19) C4 0.075(2) 0.085(2) 0.069(2) -0.0015(18) 0.0113(17) 0.0084(17) C5 0.116(3) 0.086(2) 0.101(3) 0.011(2) 0.040(2) 0.013(2) C6 0.123(3) 0.120(3) 0.083(3) 0.027(2) -0.009(2) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 Li1 1.866(5) . ? O1 Li1 1.866(5) 3_655 ? O1 Li3 1.867(4) . ? O1 Li3 1.867(4) 3_655 ? O1 Li2 1.881(5) . ? O1 Li2 1.881(5) 3_655 ? Li1 N1A 2.001(5) . ? Li1 N2B 2.018(5) 3_655 ? Li1 Li2 2.544(6) 3_655 ? Li1 Li3 2.593(6) 3_655 ? Li1 N2A 2.652(5) . ? Li1 Li3 2.685(6) . ? Li1 Li4 2.737(7) . ? Li1 C1A 2.735(5) . ? Li1 Li2 2.751(7) . ? Li2 N1B 1.999(5) . ? Li2 N2C 2.001(5) . ? Li2 Li1 2.544(6) 3_655 ? Li2 N2B 2.565(5) . ? Li2 Li3 2.584(6) . ? Li2 C1B 2.687(5) . ? Li2 Li4 2.691(7) 3_655 ? Li2 Li3 2.715(6) 3_655 ? Li3 N2A 2.008(5) 3_655 ? Li3 N1C 2.030(5) . ? Li3 Li1 2.593(6) 3_655 ? Li3 N2C 2.682(6) . ? Li3 Li2 2.715(6) 3_655 ? Li3 Li4 2.723(6) 3_655 ? Li3 C1C 2.760(5) . ? Li4 N2C 2.070(5) 3_655 ? Li4 N2A 2.090(5) . ? Li4 N2B 2.115(5) 3_655 ? Li4 N1 2.120(5) 2_544 ? Li4 Li2 2.691(7) 3_655 ? Li4 Li3 2.723(6) 3_655 ? N1A C5A 1.349(3) . ? N1A C1A 1.358(3) . ? N2A C1A 1.349(3) . ? N2A Li3 2.008(5) 3_655 ? C1A C2A 1.418(4) . ? C2A C3A 1.360(4) . ? C3A C4A 1.376(5) . ? C4A C5A 1.359(4) . ? C5A C6A 1.503(4) . ? N1B C5B 1.353(4) . ? N1B C1B 1.360(4) . ? N2B C1B 1.351(3) . ? N2B Li1 2.018(5) 3_655 ? N2B Li4 2.115(5) 3_655 ? C1B C2B 1.421(4) . ? C2B C3B 1.361(5) . ? C3B C4B 1.392(5) . ? C4B C5B 1.363(5) . ? C5B C6B 1.498(5) . ? N1C C5C 1.351(4) . ? N1C C1C 1.353(3) . ? N2C C1C 1.344(4) . ? N2C Li4 2.070(5) 3_655 ? C1C C2C 1.421(4) . ? C2C C3C 1.355(5) . ? C3C C4C 1.378(5) . ? C4C C5C 1.369(5) . ? C5C C6C 1.481(5) . ? N1 C2 1.463(4) . ? N1 C1 1.465(4) . ? N1 C3 1.472(4) . ? N1 Li4 2.120(5) 2_554 ? N2 C5 1.451(4) . ? N2 C4 1.460(4) . ? N2 C6 1.462(4) . ? C3 C4 1.509(4) . ? 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 Li1 O1 Li1 180.0(4) . 3_655 ? Li1 O1 Li3 92.0(2) . . ? Li1 O1 Li3 88.0(2) 3_655 . ? Li1 O1 Li3 88.0(2) . 3_655 ? Li1 O1 Li3 92.0(2) 3_655 3_655 ? Li3 O1 Li3 180.0(3) . 3_655 ? Li1 O1 Li2 94.5(2) . . ? Li1 O1 Li2 85.5(2) 3_655 . ? Li3 O1 Li2 87.2(2) . . ? Li3 O1 Li2 92.8(2) 3_655 . ? Li1 O1 Li2 85.5(2) . 3_655 ? Li1 O1 Li2 94.5(2) 3_655 3_655 ? Li3 O1 Li2 92.8(2) . 3_655 ? Li3 O1 Li2 87.2(2) 3_655 3_655 ? Li2 O1 Li2 180.0(2) . 3_655 ? O1 Li1 N1A 126.6(2) . . ? O1 Li1 N2B 114.7(2) . 3_655 ? N1A Li1 N2B 108.7(2) . 3_655 ? O1 Li1 Li2 47.48(15) . 3_655 ? N1A Li1 Li2 147.5(3) . 3_655 ? N2B Li1 Li2 67.27(18) 3_655 3_655 ? O1 Li1 Li3 46.02(14) . 3_655 ? N1A Li1 Li3 92.8(2) . 3_655 ? N2B Li1 Li3 107.1(2) 3_655 3_655 ? Li2 Li1 Li3 60.38(18) 3_655 3_655 ? O1 Li1 N2A 90.97(18) . . ? N1A Li1 N2A 57.03(14) . . ? N2B Li1 N2A 92.2(2) 3_655 . ? Li2 Li1 N2A 90.53(19) 3_655 . ? Li3 Li1 N2A 45.01(14) 3_655 . ? O1 Li1 Li3 44.02(13) . . ? N1A Li1 Li3 141.4(2) . . ? N2B Li1 Li3 107.2(2) 3_655 . ? Li2 Li1 Li3 62.48(18) 3_655 . ? Li3 Li1 Li3 90.03(19) 3_655 . ? N2A Li1 Li3 134.9(2) . . ? O1 Li1 Li4 93.8(2) . . ? N1A Li1 Li4 90.9(2) . . ? N2B Li1 Li4 50.06(16) 3_655 . ? Li2 Li1 Li4 61.15(18) 3_655 . ? Li3 Li1 Li4 61.37(18) 3_655 . ? N2A Li1 Li4 45.61(14) . . ? Li3 Li1 Li4 123.6(2) . . ? O1 Li1 C1A 112.4(2) . . ? N1A Li1 C1A 28.26(11) . . ? N2B Li1 C1A 99.6(2) 3_655 . ? Li2 Li1 C1A 119.3(2) 3_655 . ? Li3 Li1 C1A 69.52(16) 3_655 . ? N2A Li1 C1A 28.94(9) . . ? Li3 Li1 C1A 150.2(2) . . ? Li4 Li1 C1A 66.02(16) . . ? O1 Li1 Li2 42.98(14) . . ? N1A Li1 Li2 91.6(2) . . ? N2B Li1 Li2 157.5(3) 3_655 . ? Li2 Li1 Li2 90.5(2) 3_655 . ? Li3 Li1 Li2 60.98(17) 3_655 . ? N2A Li1 Li2 90.83(17) . . ? Li3 Li1 Li2 56.75(16) . . ? Li4 Li1 Li2 122.4(2) . . ? C1A Li1 Li2 93.73(17) . . ? O1 Li2 N1B 121.0(2) . . ? O1 Li2 N2C 116.4(2) . . ? N1B Li2 N2C 115.8(2) . . ? O1 Li2 Li1 46.99(15) . 3_655 ? N1B Li2 Li1 90.9(2) . 3_655 ? N2C Li2 Li1 109.2(2) . 3_655 ? O1 Li2 N2B 93.48(19) . . ? N1B Li2 N2B 58.87(15) . . ? N2C Li2 N2B 92.5(2) . . ? Li1 Li2 N2B 46.54(14) 3_655 . ? O1 Li2 Li3 46.19(14) . . ? N1B Li2 Li3 150.3(3) . . ? N2C Li2 Li3 70.30(19) . . ? Li1 Li2 Li3 60.75(18) 3_655 . ? N2B Li2 Li3 92.70(19) . . ? O1 Li2 C1B 111.4(2) . . ? N1B Li2 C1B 29.33(11) . . ? N2C Li2 C1B 103.9(2) . . ? Li1 Li2 C1B 68.93(17) 3_655 . ? N2B Li2 C1B 29.71(9) . . ? Li3 Li2 C1B 122.3(2) . . ? O1 Li2 Li4 94.9(2) . 3_655 ? N1B Li2 Li4 98.4(2) . 3_655 ? N2C Li2 Li4 49.73(16) . 3_655 ? Li1 Li2 Li4 62.96(18) 3_655 3_655 ? N2B Li2 Li4 47.37(14) . 3_655 ? Li3 Li2 Li4 62.11(17) . 3_655 ? C1B Li2 Li4 71.33(17) . 3_655 ? O1 Li2 Li3 43.38(14) . 3_655 ? N1B Li2 Li3 83.56(19) . 3_655 ? N2C Li2 Li3 159.5(3) . 3_655 ? Li1 Li2 Li3 61.31(18) 3_655 3_655 ? N2B Li2 Li3 92.25(18) . 3_655 ? Li3 Li2 Li3 89.6(2) . 3_655 ? C1B Li2 Li3 89.88(17) . 3_655 ? Li4 Li2 Li3 124.3(2) 3_655 3_655 ? O1 Li2 Li1 42.55(14) . . ? N1B Li2 Li1 133.7(2) . . ? N2C Li2 Li1 107.6(2) . . ? Li1 Li2 Li1 89.5(2) 3_655 . ? N2B Li2 Li1 136.0(2) . . ? Li3 Li2 Li1 60.35(17) . . ? C1B Li2 Li1 146.3(2) . . ? Li4 Li2 Li1 122.5(2) 3_655 . ? Li3 Li2 Li1 56.64(17) 3_655 . ? O1 Li3 N2A 114.9(2) . 3_655 ? O1 Li3 N1C 120.1(2) . . ? N2A Li3 N1C 114.4(2) 3_655 . ? O1 Li3 Li2 46.64(15) . . ? N2A Li3 Li2 106.3(2) 3_655 . ? N1C Li3 Li2 88.3(2) . . ? O1 Li3 Li1 45.98(14) . 3_655 ? N2A Li3 Li1 69.03(18) 3_655 3_655 ? N1C Li3 Li1 145.0(3) . 3_655 ? Li2 Li3 Li1 58.87(17) . 3_655 ? O1 Li3 Li1 43.98(14) . . ? N2A Li3 Li1 158.7(2) 3_655 . ? N1C Li3 Li1 84.64(19) . . ? Li2 Li3 Li1 62.90(18) . . ? Li1 Li3 Li1 89.97(19) 3_655 . ? O1 Li3 N2C 91.18(19) . . ? N2A Li3 N2C 91.32(19) 3_655 . ? N1C Li3 N2C 56.16(14) . . ? Li2 Li3 N2C 44.61(14) . . ? Li1 Li3 N2C 89.64(18) 3_655 . ? Li1 Li3 N2C 92.00(18) . . ? O1 Li3 Li2 43.78(13) . 3_655 ? N2A Li3 Li2 108.2(2) 3_655 3_655 ? N1C Li3 Li2 135.9(2) . 3_655 ? Li2 Li3 Li2 90.42(19) . 3_655 ? Li1 Li3 Li2 62.38(17) 3_655 3_655 ? Li1 Li3 Li2 56.21(16) . 3_655 ? N2C Li3 Li2 134.9(2) . 3_655 ? O1 Li3 Li4 94.2(2) . 3_655 ? N2A Li3 Li4 49.67(16) 3_655 3_655 ? N1C Li3 Li4 92.9(2) . 3_655 ? Li2 Li3 Li4 60.88(18) . 3_655 ? Li1 Li3 Li4 61.91(17) 3_655 3_655 ? Li1 Li3 Li4 123.8(2) . 3_655 ? N2C Li3 Li4 45.03(14) . 3_655 ? Li2 Li3 Li4 124.3(2) 3_655 3_655 ? O1 Li3 C1C 109.6(2) . . ? N2A Li3 C1C 102.1(2) 3_655 . ? N1C Li3 C1C 27.85(11) . . ? Li2 Li3 C1C 67.05(16) . . ? Li1 Li3 C1C 118.2(2) 3_655 . ? Li1 Li3 C1C 90.68(18) . . ? N2C Li3 C1C 28.54(9) . . ? Li2 Li3 C1C 146.5(2) 3_655 . ? Li4 Li3 C1C 67.17(16) 3_655 . ? N2C Li4 N2A 109.0(2) 3_655 . ? N2C Li4 N2B 105.0(2) 3_655 3_655 ? N2A Li4 N2B 107.6(2) . 3_655 ? N2C Li4 N1 110.8(2) 3_655 2_544 ? N2A Li4 N1 108.6(2) . 2_544 ? N2B Li4 N1 115.6(2) 3_655 2_544 ? N2C Li4 Li2 47.52(15) 3_655 3_655 ? N2A Li4 Li2 100.3(2) . 3_655 ? N2B Li4 Li2 63.17(17) 3_655 3_655 ? N1 Li4 Li2 149.2(2) 2_544 3_655 ? N2C Li4 Li3 66.44(18) 3_655 3_655 ? N2A Li4 Li3 47.08(15) . 3_655 ? N2B Li4 Li3 100.0(2) 3_655 3_655 ? N1 Li4 Li3 143.0(2) 2_544 3_655 ? Li2 Li4 Li3 57.01(16) 3_655 3_655 ? N2C Li4 Li1 100.4(2) 3_655 . ? N2A Li4 Li1 65.04(17) . . ? N2B Li4 Li1 47.04(15) 3_655 . ? N1 Li4 Li1 148.2(2) 2_544 . ? Li2 Li4 Li1 55.89(16) 3_655 . ? Li3 Li4 Li1 56.71(16) 3_655 . ? C5A N1A C1A 119.6(2) . . ? C5A N1A Li1 131.8(2) . . ? C1A N1A Li1 107.5(2) . . ? C1A N2A Li3 128.8(2) . 3_655 ? C1A N2A Li4 118.6(2) . . ? Li3 N2A Li4 83.3(2) 3_655 . ? C1A N2A Li1 78.97(19) . . ? Li3 N2A Li1 65.96(17) 3_655 . ? Li4 N2A Li1 69.35(18) . . ? N2A C1A N1A 115.9(2) . . ? N2A C1A C2A 124.4(3) . . ? N1A C1A C2A 119.7(3) . . ? N2A C1A Li1 72.09(18) . . ? N1A C1A Li1 44.25(16) . . ? C2A C1A Li1 162.4(2) . . ? C3A C2A C1A 118.4(3) . . ? C2A C3A C4A 121.4(3) . . ? C5A C4A C3A 118.2(3) . . ? N1A C5A C4A 122.6(3) . . ? N1A C5A C6A 115.3(2) . . ? C4A C5A C6A 122.1(3) . . ? C5B N1B C1B 119.8(3) . . ? C5B N1B Li2 135.0(3) . . ? C1B N1B Li2 104.6(2) . . ? C1B N2B Li1 121.8(2) . 3_655 ? C1B N2B Li4 128.2(2) . 3_655 ? Li1 N2B Li4 82.9(2) 3_655 3_655 ? C1B N2B Li2 80.1(2) . . ? Li1 N2B Li2 66.19(18) 3_655 . ? Li4 N2B Li2 69.46(17) 3_655 . ? N2B C1B N1B 115.7(2) . . ? N2B C1B C2B 124.6(3) . . ? N1B C1B C2B 119.6(3) . . ? N2B C1B Li2 70.15(19) . . ? N1B C1B Li2 46.03(16) . . ? C2B C1B Li2 164.1(3) . . ? C3B C2B C1B 119.0(3) . . ? C2B C3B C4B 120.6(3) . . ? C5B C4B C3B 118.5(3) . . ? N1B C5B C4B 122.4(3) . . ? N1B C5B C6B 115.7(3) . . ? C4B C5B C6B 122.0(3) . . ? C5C N1C C1C 120.2(3) . . ? C5C N1C Li3 131.4(3) . . ? C1C N1C Li3 107.6(2) . . ? C1C N2C Li2 123.0(2) . . ? C1C N2C Li4 124.0(2) . 3_655 ? Li2 N2C Li4 82.8(2) . 3_655 ? C1C N2C Li3 79.0(2) . . ? Li2 N2C Li3 65.09(18) . . ? Li4 N2C Li3 68.53(17) 3_655 . ? N2C C1C N1C 116.4(3) . . ? N2C C1C C2C 124.3(3) . . ? N1C C1C C2C 119.3(3) . . ? N2C C1C Li3 72.5(2) . . ? N1C C1C Li3 44.50(15) . . ? C2C C1C Li3 161.6(3) . . ? C3C C2C C1C 119.4(4) . . ? C2C C3C C4C 120.4(4) . . ? C5C C4C C3C 119.1(3) . . ? N1C C5C C4C 121.6(3) . . ? N1C C5C C6C 116.2(3) . . ? C4C C5C C6C 122.2(3) . . ? C2 N1 C1 109.1(3) . . ? C2 N1 C3 108.0(3) . . ? C1 N1 C3 113.2(3) . . ? C2 N1 Li4 108.3(2) . 2_554 ? C1 N1 Li4 105.3(2) . 2_554 ? C3 N1 Li4 112.9(2) . 2_554 ? C5 N2 C4 109.4(3) . . ? C5 N2 C6 110.3(3) . . ? C4 N2 C6 111.1(3) . . ? N1 C3 C4 112.5(3) . . ? N2 C4 C3 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.221 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.041 #===END data_pj021 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H52 Li4 N8 O4 Si4' _chemical_formula_weight 752.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.766(2) _cell_length_b 11.486(2) _cell_length_c 18.049(4) _cell_angle_alpha 93.880(4) _cell_angle_beta 97.690(5) _cell_angle_gamma 102.459(4) _cell_volume 2148.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9513 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9728 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.35 _reflns_number_total 6152 _reflns_number_gt 3075 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1053P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0040(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6152 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1361 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2068 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.008 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 0.8004(8) 0.3110(8) 0.1659(5) 0.055(2) Uani 1 1 d . . . Li2 Li 0.6349(8) 0.1600(8) 0.2175(5) 0.052(2) Uani 1 1 d . . . Li3 Li 0.8575(8) 0.2320(8) 0.2917(5) 0.053(2) Uani 1 1 d . . . Li4 Li 0.7022(8) 0.3745(7) 0.2790(5) 0.048(2) Uani 1 1 d . . . N1A N 0.8083(4) 0.3352(4) 0.0538(2) 0.0565(12) Uani 1 1 d . . . N2A N 0.5867(5) 0.2988(5) 0.0253(3) 0.0678(15) Uani 1 1 d . . . C1A C 0.7026(6) 0.3028(5) 0.0014(3) 0.0615(16) Uani 1 1 d . . . C2A C 0.7111(7) 0.2693(6) -0.0739(3) 0.085(2) Uani 1 1 d . . . H2A H 0.6375 0.2463 -0.1097 0.142(4) Uiso 1 1 calc R . . C3A C 0.8290(8) 0.2714(7) -0.0931(4) 0.105(3) Uani 1 1 d . . . H3A H 0.8363 0.2488 -0.1425 0.142(4) Uiso 1 1 calc R . . C4A C 0.9376(7) 0.3064(6) -0.0404(4) 0.092(2) Uani 1 1 d . . . H4A H 1.0185 0.3088 -0.0539 0.142(4) Uiso 1 1 calc R . . C5A C 0.9249(6) 0.3379(6) 0.0326(3) 0.0693(17) Uani 1 1 d . . . C6A C 1.0378(6) 0.3762(7) 0.0933(4) 0.093(2) Uani 1 1 d . . . H6A1 H 1.0088 0.3937 0.1400 0.142(4) Uiso 1 1 calc R . . H6A2 H 1.0944 0.4466 0.0810 0.142(4) Uiso 1 1 calc R . . H6A3 H 1.0831 0.3130 0.0980 0.142(4) Uiso 1 1 calc R . . Si1A Si 0.55303(15) 0.36145(15) 0.10887(9) 0.0614(5) Uani 1 1 d . . . O1A O 0.6222(3) 0.3125(3) 0.17893(18) 0.0509(9) Uani 1 1 d . . . C7A C 0.6044(7) 0.5249(6) 0.1101(4) 0.101(2) Uani 1 1 d . . . H7A1 H 0.5597 0.5506 0.0668 0.142(4) Uiso 1 1 calc R . . H7A2 H 0.6954 0.5469 0.1094 0.142(4) Uiso 1 1 calc R . . H7A3 H 0.5848 0.5627 0.1548 0.142(4) Uiso 1 1 calc R . . C8A C 0.3753(6) 0.3204(7) 0.0963(4) 0.093(2) Uani 1 1 d . . . H8A1 H 0.3411 0.3539 0.0529 0.142(4) Uiso 1 1 calc R . . H8A2 H 0.3462 0.3514 0.1400 0.142(4) Uiso 1 1 calc R . . H8A3 H 0.3463 0.2348 0.0896 0.142(4) Uiso 1 1 calc R . . N1B N 0.5455(4) -0.0268(4) 0.2136(3) 0.0589(12) Uani 1 1 d . . . N2B N 0.7351(5) -0.0855(5) 0.2068(3) 0.0700(16) Uani 1 1 d . . . C1B C 0.6189(6) -0.1053(5) 0.2319(3) 0.0596(15) Uani 1 1 d . . . C2B C 0.5761(6) -0.2012(5) 0.2730(4) 0.0778(19) Uani 1 1 d . . . H2B H 0.6281 -0.2542 0.2854 0.142(4) Uiso 1 1 calc R . . C3B C 0.4579(7) -0.2163(6) 0.2947(4) 0.087(2) Uani 1 1 d . . . H3B H 0.4296 -0.2777 0.3237 0.142(4) Uiso 1 1 calc R . . C4B C 0.3800(6) -0.1392(6) 0.2730(4) 0.0738(18) Uani 1 1 d . . . H4B H 0.2974 -0.1499 0.2853 0.142(4) Uiso 1 1 calc R . . C5B C 0.4276(6) -0.0470(5) 0.2332(3) 0.0643(16) Uani 1 1 d . . . C6B C 0.3487(6) 0.0421(6) 0.2069(4) 0.087(2) Uani 1 1 d . . . H6B1 H 0.3989 0.1003 0.1805 0.142(4) Uiso 1 1 calc R . . H6B2 H 0.3252 0.0819 0.2496 0.142(4) Uiso 1 1 calc R . . H6B3 H 0.2722 0.0002 0.1740 0.142(4) Uiso 1 1 calc R . . Si1B Si 0.80176(16) 0.02465(14) 0.15311(10) 0.0625(5) Uani 1 1 d . . . O1B O 0.8046(3) 0.1526(3) 0.19194(17) 0.0487(9) Uani 1 1 d . . . C7B C 0.9618(6) -0.0067(6) 0.1470(4) 0.096(2) Uani 1 1 d . . . H7B1 H 0.9513 -0.0860 0.1228 0.142(4) Uiso 1 1 calc R . . H7B2 H 1.0091 -0.0009 0.1967 0.142(4) Uiso 1 1 calc R . . H7B3 H 1.0082 0.0506 0.1184 0.142(4) Uiso 1 1 calc R . . C8B C 0.7058(7) -0.0057(6) 0.0585(4) 0.098(2) Uani 1 1 d . . . H8B1 H 0.7068 -0.0844 0.0374 0.142(4) Uiso 1 1 calc R . . H8B2 H 0.7418 0.0526 0.0270 0.142(4) Uiso 1 1 calc R . . H8B3 H 0.6187 -0.0011 0.0619 0.142(4) Uiso 1 1 calc R . . N1C N 0.9362(4) 0.1258(4) 0.3668(2) 0.0575(12) Uani 1 1 d . . . N2C N 0.7439(5) 0.0508(4) 0.4081(3) 0.0669(14) Uani 1 1 d . . . C1C C 0.8614(6) 0.0360(5) 0.3949(3) 0.0622(16) Uani 1 1 d . . . C2C C 0.8990(8) -0.0705(6) 0.4111(4) 0.091(2) Uani 1 1 d . . . H2C H 0.8440 -0.1332 0.4285 0.142(4) Uiso 1 1 calc R . . C3C C 1.0213(9) -0.0774(7) 0.3999(4) 0.102(3) Uani 1 1 d . . . H3C H 1.0502 -0.1459 0.4105 0.142(4) Uiso 1 1 calc R . . C4C C 1.1004(7) 0.0140(8) 0.3736(4) 0.096(2) Uani 1 1 d . . . H4C H 1.1837 0.0093 0.3676 0.142(4) Uiso 1 1 calc R . . C5C C 1.0553(6) 0.1137(6) 0.3559(3) 0.0692(17) Uani 1 1 d . . . C6C C 1.1308(6) 0.2152(6) 0.3217(4) 0.084(2) Uani 1 1 d . . . H6C1 H 1.0809 0.2743 0.3133 0.142(4) Uiso 1 1 calc R . . H6C2 H 1.1510 0.1860 0.2747 0.142(4) Uiso 1 1 calc R . . H6C3 H 1.2091 0.2506 0.3551 0.142(4) Uiso 1 1 calc R . . Si1C Si 0.68009(15) 0.17850(14) 0.40150(9) 0.0574(5) Uani 1 1 d . . . O1C O 0.6853(3) 0.2251(3) 0.32178(17) 0.0468(9) Uani 1 1 d . . . C7C C 0.5165(6) 0.1292(6) 0.4247(4) 0.086(2) Uani 1 1 d . . . H7C1 H 0.5216 0.1020 0.4739 0.142(4) Uiso 1 1 calc R . . H7C2 H 0.4681 0.0650 0.3885 0.142(4) Uiso 1 1 calc R . . H7C3 H 0.4747 0.1951 0.4238 0.142(4) Uiso 1 1 calc R . . C8C C 0.7745(6) 0.2915(5) 0.4766(3) 0.0780(19) Uani 1 1 d . . . H8C1 H 0.7694 0.2601 0.5243 0.142(4) Uiso 1 1 calc R . . H8C2 H 0.7408 0.3624 0.4760 0.142(4) Uiso 1 1 calc R . . H8C3 H 0.8628 0.3111 0.4687 0.142(4) Uiso 1 1 calc R . . N1D N 0.7082(4) 0.5199(4) 0.3563(2) 0.0491(11) Uani 1 1 d . . . N2D N 0.9292(5) 0.5654(4) 0.3856(3) 0.0622(15) Uani 1 1 d . . . C1D C 0.8126(5) 0.5742(4) 0.4056(3) 0.0519(14) Uani 1 1 d . . . C2D C 0.8045(7) 0.6378(5) 0.4736(3) 0.0699(17) Uani 1 1 d . . . H2D H 0.8782 0.6750 0.5068 0.142(4) Uiso 1 1 calc R . . C3D C 0.6852(7) 0.6433(6) 0.4891(4) 0.081(2) Uani 1 1 d . . . H3D H 0.6770 0.6836 0.5339 0.142(4) Uiso 1 1 calc R . . C4D C 0.5765(7) 0.5892(6) 0.4386(4) 0.0738(18) Uani 1 1 d . . . H4D H 0.4952 0.5950 0.4482 0.142(4) Uiso 1 1 calc R . . C5D C 0.5914(6) 0.5266(5) 0.3738(3) 0.0602(15) Uani 1 1 d . . . C6D C 0.4784(5) 0.4611(6) 0.3184(4) 0.0788(19) Uani 1 1 d . . . H6D1 H 0.5078 0.4234 0.2771 0.142(4) Uiso 1 1 calc R . . H6D2 H 0.4292 0.5166 0.3002 0.142(4) Uiso 1 1 calc R . . H6D3 H 0.4254 0.4012 0.3423 0.142(4) Uiso 1 1 calc R . . Si1D Si 0.96406(14) 0.52763(13) 0.29633(9) 0.0530(5) Uani 1 1 d . . . O1D O 0.8871(3) 0.3977(3) 0.26389(18) 0.0485(9) Uani 1 1 d . . . C7D C 1.1424(5) 0.5494(6) 0.3134(4) 0.0792(19) Uani 1 1 d . . . H7D1 H 1.1809 0.6309 0.3331 0.142(4) Uiso 1 1 calc R . . H7D2 H 1.1723 0.5322 0.2670 0.142(4) Uiso 1 1 calc R . . H7D3 H 1.1659 0.4964 0.3489 0.142(4) Uiso 1 1 calc R . . C8D C 0.9238(6) 0.6445(5) 0.2375(3) 0.0802(19) Uani 1 1 d . . . H8D1 H 0.9732 0.7218 0.2595 0.142(4) Uiso 1 1 calc R . . H8D2 H 0.8337 0.6428 0.2344 0.142(4) Uiso 1 1 calc R . . H8D3 H 0.9438 0.6294 0.1879 0.142(4) Uiso 1 1 calc R . . H1A H 0.530(5) 0.278(5) -0.008(3) 0.061(19) Uiso 1 1 d . . . H1B H 0.773(5) -0.131(5) 0.218(3) 0.06(2) Uiso 1 1 d . . . H1C H 0.693(6) -0.004(6) 0.427(3) 0.10(2) Uiso 1 1 d . . . H1D H 0.984(5) 0.599(5) 0.416(3) 0.056(19) 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 0.052(5) 0.064(6) 0.054(5) 0.009(4) 0.008(4) 0.026(4) Li2 0.044(5) 0.051(5) 0.059(6) 0.001(4) 0.002(4) 0.012(4) Li3 0.046(5) 0.058(6) 0.053(5) -0.001(4) 0.001(4) 0.013(4) Li4 0.044(5) 0.052(5) 0.051(5) 0.005(4) 0.007(4) 0.018(4) N1A 0.052(3) 0.070(3) 0.052(3) 0.004(2) 0.008(2) 0.022(2) N2A 0.052(3) 0.094(4) 0.054(3) -0.004(3) -0.005(3) 0.020(3) C1A 0.066(4) 0.066(4) 0.054(4) 0.007(3) 0.011(3) 0.017(3) C2A 0.083(5) 0.114(6) 0.054(4) -0.001(4) 0.011(4) 0.015(4) C3A 0.105(6) 0.146(7) 0.063(5) -0.008(4) 0.031(5) 0.018(5) C4A 0.086(5) 0.119(6) 0.076(5) 0.006(4) 0.037(5) 0.025(4) C5A 0.069(4) 0.084(5) 0.060(4) 0.006(3) 0.018(4) 0.024(3) C6A 0.060(4) 0.132(6) 0.087(5) 0.002(4) 0.023(4) 0.020(4) Si1A 0.0581(10) 0.0742(12) 0.0567(10) 0.0078(8) -0.0001(8) 0.0302(8) O1A 0.0430(19) 0.061(2) 0.051(2) 0.0072(17) -0.0002(17) 0.0216(16) C7A 0.132(6) 0.081(5) 0.096(5) 0.018(4) -0.004(5) 0.044(4) C8A 0.064(4) 0.139(7) 0.083(5) 0.020(4) -0.003(4) 0.043(4) N1B 0.055(3) 0.044(3) 0.075(3) 0.000(2) 0.005(3) 0.010(2) N2B 0.064(4) 0.051(3) 0.102(5) 0.013(3) 0.012(3) 0.027(3) C1B 0.057(4) 0.040(3) 0.080(4) 0.004(3) 0.005(3) 0.011(3) C2B 0.070(4) 0.056(4) 0.108(5) 0.014(4) 0.007(4) 0.018(3) C3B 0.094(5) 0.060(5) 0.108(6) 0.020(4) 0.016(5) 0.013(4) C4B 0.062(4) 0.059(4) 0.097(5) -0.001(4) 0.023(4) 0.003(3) C5B 0.055(4) 0.060(4) 0.073(4) -0.005(3) 0.007(3) 0.008(3) C6B 0.066(4) 0.081(5) 0.114(6) 0.009(4) 0.009(4) 0.021(4) Si1B 0.0594(10) 0.0551(11) 0.0738(12) -0.0073(8) 0.0092(9) 0.0197(8) O1B 0.046(2) 0.048(2) 0.053(2) -0.0028(16) 0.0020(17) 0.0174(16) C7B 0.073(4) 0.090(5) 0.128(6) -0.016(4) 0.027(4) 0.024(4) C8B 0.113(6) 0.081(5) 0.088(5) -0.021(4) -0.010(4) 0.018(4) N1C 0.055(3) 0.057(3) 0.063(3) 0.004(2) 0.001(2) 0.025(2) N2C 0.073(4) 0.054(3) 0.080(4) 0.024(3) 0.018(3) 0.018(3) C1C 0.073(4) 0.052(4) 0.061(4) 0.001(3) -0.005(3) 0.023(3) C2C 0.117(6) 0.064(5) 0.098(5) 0.021(4) -0.002(5) 0.042(4) C3C 0.138(7) 0.080(6) 0.103(6) 0.010(4) -0.006(6) 0.073(5) C4C 0.091(5) 0.111(7) 0.099(6) 0.004(5) -0.001(5) 0.063(5) C5C 0.073(4) 0.070(4) 0.070(4) 0.002(3) 0.005(3) 0.032(3) C6C 0.055(4) 0.096(5) 0.104(5) -0.003(4) 0.007(4) 0.032(4) Si1C 0.0589(10) 0.0552(10) 0.0599(10) 0.0084(8) 0.0060(8) 0.0177(7) O1C 0.050(2) 0.046(2) 0.046(2) 0.0059(15) 0.0053(17) 0.0163(16) C7C 0.088(5) 0.090(5) 0.085(5) 0.012(4) 0.025(4) 0.019(4) C8C 0.087(5) 0.070(4) 0.072(4) 0.005(3) -0.007(4) 0.019(3) N1D 0.048(3) 0.045(3) 0.058(3) 0.008(2) 0.013(2) 0.015(2) N2D 0.056(3) 0.062(3) 0.061(3) -0.008(3) 0.008(3) 0.002(3) C1D 0.059(4) 0.046(3) 0.054(3) 0.007(3) 0.016(3) 0.012(3) C2D 0.093(5) 0.061(4) 0.058(4) -0.003(3) 0.025(4) 0.017(3) C3D 0.096(5) 0.093(5) 0.064(4) -0.002(4) 0.033(4) 0.037(4) C4D 0.082(5) 0.087(5) 0.069(4) 0.014(4) 0.033(4) 0.039(4) C5D 0.070(4) 0.051(3) 0.071(4) 0.016(3) 0.029(3) 0.024(3) C6D 0.053(4) 0.087(5) 0.098(5) 0.003(4) 0.013(4) 0.020(3) Si1D 0.0462(9) 0.0511(10) 0.0613(10) 0.0008(7) 0.0117(8) 0.0096(7) O1D 0.0422(19) 0.045(2) 0.058(2) 0.0007(16) 0.0065(17) 0.0110(15) C7D 0.056(4) 0.078(5) 0.097(5) -0.003(4) 0.015(4) 0.004(3) C8D 0.092(5) 0.066(4) 0.084(5) 0.012(3) 0.019(4) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1B 1.918(10) . ? Li1 O1A 1.968(9) . ? Li1 O1D 1.977(9) . ? Li1 N1A 2.071(10) . ? Li1 Li2 2.526(12) . ? Li1 Li3 2.549(12) . ? Li1 Li4 2.555(12) . ? Li1 Si1A 2.916(9) . ? Li2 O1C 1.938(9) . ? Li2 O1A 1.952(9) . ? Li2 O1B 1.961(9) . ? Li2 N1B 2.146(9) . ? Li2 Li3 2.521(11) . ? Li2 Li4 2.543(12) . ? Li2 Si1B 2.918(9) . ? Li3 O1B 1.917(9) . ? Li3 O1D 1.971(9) . ? Li3 O1C 1.988(9) . ? Li3 N1C 2.098(10) . ? Li3 Li4 2.580(12) . ? Li3 Si1C 2.938(9) . ? Li4 O1C 1.911(9) . ? Li4 O1A 1.912(9) . ? Li4 O1D 2.009(8) . ? Li4 N1D 2.087(9) . ? Li4 Si1D 2.948(8) . ? N1A C1A 1.345(6) . ? N1A C5A 1.355(7) . ? N2A C1A 1.366(7) . ? N2A Si1A 1.743(5) . ? C1A C2A 1.408(8) . ? C2A C3A 1.356(9) . ? C3A C4A 1.371(9) . ? C4A C5A 1.376(8) . ? C5A C6A 1.490(8) . ? Si1A O1A 1.580(4) . ? Si1A C7A 1.837(7) . ? Si1A C8A 1.848(6) . ? N1B C5B 1.340(6) . ? N1B C1B 1.351(7) . ? N2B C1B 1.366(7) . ? N2B Si1B 1.736(6) . ? C1B C2B 1.400(8) . ? C2B C3B 1.360(8) . ? C3B C4B 1.385(9) . ? C4B C5B 1.366(8) . ? C5B C6B 1.526(8) . ? Si1B O1B 1.577(3) . ? Si1B C8B 1.843(7) . ? Si1B C7B 1.851(6) . ? N1C C1C 1.339(7) . ? N1C C5C 1.358(7) . ? N2C C1C 1.362(7) . ? N2C Si1C 1.753(5) . ? C1C C2C 1.406(8) . ? C2C C3C 1.376(10) . ? C3C C4C 1.357(10) . ? C4C C5C 1.378(9) . ? C5C C6C 1.491(8) . ? Si1C O1C 1.573(3) . ? Si1C C8C 1.838(6) . ? Si1C C7C 1.843(6) . ? N1D C1D 1.341(6) . ? N1D C5D 1.353(6) . ? N2D C1D 1.375(7) . ? N2D Si1D 1.749(5) . ? C1D C2D 1.407(7) . ? C2D C3D 1.364(8) . ? C3D C4D 1.382(8) . ? C4D C5D 1.377(8) . ? C5D C6D 1.490(8) . ? Si1D O1D 1.573(3) . ? Si1D C8D 1.854(6) . ? Si1D C7D 1.862(6) . ? 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 O1B Li1 O1A 99.3(4) . . ? O1B Li1 O1D 97.0(4) . . ? O1A Li1 O1D 98.0(4) . . ? O1B Li1 N1A 114.9(5) . . ? O1A Li1 N1A 104.8(4) . . ? O1D Li1 N1A 136.3(5) . . ? O1B Li1 Li2 50.1(3) . . ? O1A Li1 Li2 49.6(3) . . ? O1D Li1 Li2 96.4(4) . . ? N1A Li1 Li2 126.7(4) . . ? O1B Li1 Li3 48.3(3) . . ? O1A Li1 Li3 95.3(4) . . ? O1D Li1 Li3 49.7(3) . . ? N1A Li1 Li3 156.4(5) . . ? Li2 Li1 Li3 59.6(3) . . ? O1B Li1 Li4 96.5(4) . . ? O1A Li1 Li4 47.9(3) . . ? O1D Li1 Li4 50.7(3) . . ? N1A Li1 Li4 142.8(5) . . ? Li2 Li1 Li4 60.1(3) . . ? Li3 Li1 Li4 60.7(3) . . ? O1B Li1 Si1A 118.6(4) . . ? O1A Li1 Si1A 30.58(17) . . ? O1D Li1 Si1A 115.8(4) . . ? N1A Li1 Si1A 75.1(3) . . ? Li2 Li1 Si1A 74.7(3) . . ? Li3 Li1 Si1A 125.9(4) . . ? Li4 Li1 Si1A 72.5(3) . . ? O1C Li2 O1A 95.5(4) . . ? O1C Li2 O1B 99.3(4) . . ? O1A Li2 O1B 98.4(4) . . ? O1C Li2 N1B 108.6(4) . . ? O1A Li2 N1B 145.7(5) . . ? O1B Li2 N1B 101.3(4) . . ? O1C Li2 Li1 96.3(4) . . ? O1A Li2 Li1 50.2(3) . . ? O1B Li2 Li1 48.6(3) . . ? N1B Li2 Li1 144.6(5) . . ? O1C Li2 Li3 50.9(3) . . ? O1A Li2 Li3 96.6(4) . . ? O1B Li2 Li3 48.7(3) . . ? N1B Li2 Li3 117.5(4) . . ? Li1 Li2 Li3 60.7(3) . . ? O1C Li2 Li4 48.2(3) . . ? O1A Li2 Li4 48.2(3) . . ? O1B Li2 Li4 95.8(4) . . ? N1B Li2 Li4 153.6(5) . . ? Li1 Li2 Li4 60.5(3) . . ? Li3 Li2 Li4 61.3(3) . . ? O1C Li2 Si1B 117.3(4) . . ? O1A Li2 Si1B 118.0(4) . . ? O1B Li2 Si1B 30.37(17) . . ? N1B Li2 Si1B 72.4(3) . . ? Li1 Li2 Si1B 73.8(3) . . ? Li3 Li2 Si1B 72.5(3) . . ? Li4 Li2 Si1B 126.1(3) . . ? O1B Li3 O1D 97.3(4) . . ? O1B Li3 O1C 99.1(4) . . ? O1D Li3 O1C 96.8(4) . . ? O1B Li3 N1C 112.7(5) . . ? O1D Li3 N1C 140.9(4) . . ? O1C Li3 N1C 102.2(4) . . ? O1B Li3 Li2 50.2(3) . . ? O1D Li3 Li2 96.7(4) . . ? O1C Li3 Li2 49.2(3) . . ? N1C Li3 Li2 121.5(4) . . ? O1B Li3 Li1 48.4(3) . . ? O1D Li3 Li1 49.9(3) . . ? O1C Li3 Li1 94.3(4) . . ? N1C Li3 Li1 157.2(5) . . ? Li2 Li3 Li1 59.7(3) . . ? O1B Li3 Li4 95.7(4) . . ? O1D Li3 Li4 50.2(3) . . ? O1C Li3 Li4 47.3(3) . . ? N1C Li3 Li4 142.6(5) . . ? Li2 Li3 Li4 59.8(3) . . ? Li1 Li3 Li4 59.7(3) . . ? O1B Li3 Si1C 117.9(4) . . ? O1D Li3 Si1C 114.8(4) . . ? O1C Li3 Si1C 30.06(16) . . ? N1C Li3 Si1C 73.3(3) . . ? Li2 Li3 Si1C 73.3(3) . . ? Li1 Li3 Si1C 124.3(4) . . ? Li4 Li3 Si1C 72.0(3) . . ? O1C Li4 O1A 97.7(4) . . ? O1C Li4 O1D 98.1(4) . . ? O1A Li4 O1D 98.8(4) . . ? O1C Li4 N1D 113.8(4) . . ? O1A Li4 N1D 138.7(5) . . ? O1D Li4 N1D 102.3(4) . . ? O1C Li4 Li1 96.0(4) . . ? O1A Li4 Li1 49.8(3) . . ? O1D Li4 Li1 49.6(3) . . ? N1D Li4 Li1 142.8(4) . . ? O1C Li4 Li2 49.1(3) . . ? O1A Li4 Li2 49.5(3) . . ? O1D Li4 Li2 95.1(4) . . ? N1D Li4 Li2 157.7(4) . . ? Li1 Li4 Li2 59.4(3) . . ? O1C Li4 Li3 49.8(3) . . ? O1A Li4 Li3 95.7(4) . . ? O1D Li4 Li3 48.9(3) . . ? N1D Li4 Li3 124.8(4) . . ? Li1 Li4 Li3 59.5(3) . . ? Li2 Li4 Li3 59.0(3) . . ? O1C Li4 Si1D 116.5(4) . . ? O1A Li4 Si1D 116.8(4) . . ? O1D Li4 Si1D 30.06(15) . . ? N1D Li4 Si1D 73.1(3) . . ? Li1 Li4 Si1D 73.9(3) . . ? Li2 Li4 Si1D 125.1(4) . . ? Li3 Li4 Si1D 73.8(3) . . ? C1A N1A C5A 118.8(5) . . ? C1A N1A Li1 121.5(4) . . ? C5A N1A Li1 114.6(5) . . ? C1A N2A Si1A 129.5(5) . . ? N1A C1A N2A 117.0(5) . . ? N1A C1A C2A 121.3(6) . . ? N2A C1A C2A 121.7(6) . . ? C3A C2A C1A 118.5(7) . . ? C2A C3A C4A 120.7(6) . . ? C5A C4A C3A 118.9(7) . . ? N1A C5A C4A 121.8(6) . . ? N1A C5A C6A 115.9(5) . . ? C4A C5A C6A 122.3(6) . . ? O1A Si1A N2A 110.9(2) . . ? O1A Si1A C7A 112.4(3) . . ? N2A Si1A C7A 107.1(3) . . ? O1A Si1A C8A 114.8(3) . . ? N2A Si1A C8A 102.7(3) . . ? C7A Si1A C8A 108.3(3) . . ? O1A Si1A Li1 39.3(2) . . ? N2A Si1A Li1 81.3(3) . . ? C7A Si1A Li1 98.8(3) . . ? C8A Si1A Li1 149.8(3) . . ? Si1A O1A Li4 136.7(3) . . ? Si1A O1A Li2 139.6(3) . . ? Li4 O1A Li2 82.3(4) . . ? Si1A O1A Li1 110.1(3) . . ? Li4 O1A Li1 82.4(4) . . ? Li2 O1A Li1 80.2(4) . . ? C5B N1B C1B 117.6(5) . . ? C5B N1B Li2 113.4(4) . . ? C1B N1B Li2 119.4(4) . . ? C1B N2B Si1B 129.5(5) . . ? N1B C1B N2B 115.7(5) . . ? N1B C1B C2B 121.3(6) . . ? N2B C1B C2B 123.0(6) . . ? C3B C2B C1B 119.4(6) . . ? C2B C3B C4B 119.3(6) . . ? C5B C4B C3B 118.4(6) . . ? N1B C5B C4B 123.8(6) . . ? N1B C5B C6B 114.2(5) . . ? C4B C5B C6B 122.0(6) . . ? O1B Si1B N2B 110.1(2) . . ? O1B Si1B C8B 112.7(3) . . ? N2B Si1B C8B 107.5(3) . . ? O1B Si1B C7B 114.9(3) . . ? N2B Si1B C7B 102.4(3) . . ? C8B Si1B C7B 108.5(3) . . ? O1B Si1B Li2 39.0(2) . . ? N2B Si1B Li2 83.9(3) . . ? C8B Si1B Li2 95.3(3) . . ? C7B Si1B Li2 151.7(3) . . ? Si1B O1B Li3 135.3(3) . . ? Si1B O1B Li1 139.8(3) . . ? Li3 O1B Li1 83.3(4) . . ? Si1B O1B Li2 110.7(3) . . ? Li3 O1B Li2 81.1(4) . . ? Li1 O1B Li2 81.2(4) . . ? C1C N1C C5C 117.7(5) . . ? C1C N1C Li3 121.5(4) . . ? C5C N1C Li3 113.6(5) . . ? C1C N2C Si1C 128.8(4) . . ? N1C C1C N2C 117.2(5) . . ? N1C C1C C2C 123.1(6) . . ? N2C C1C C2C 119.7(6) . . ? C3C C2C C1C 116.7(7) . . ? C4C C3C C2C 121.3(7) . . ? C3C C4C C5C 118.9(7) . . ? N1C C5C C4C 122.2(6) . . ? N1C C5C C6C 114.5(5) . . ? C4C C5C C6C 123.3(7) . . ? O1C Si1C N2C 111.2(2) . . ? O1C Si1C C8C 111.7(2) . . ? N2C Si1C C8C 106.8(3) . . ? O1C Si1C C7C 114.6(3) . . ? N2C Si1C C7C 103.7(3) . . ? C8C Si1C C7C 108.3(3) . . ? O1C Si1C Li3 39.3(2) . . ? N2C Si1C Li3 82.9(3) . . ? C8C Si1C Li3 96.1(3) . . ? C7C Si1C Li3 151.2(3) . . ? Si1C O1C Li4 138.0(3) . . ? Si1C O1C Li2 137.7(3) . . ? Li4 O1C Li2 82.7(4) . . ? Si1C O1C Li3 110.7(3) . . ? Li4 O1C Li3 82.8(4) . . ? Li2 O1C Li3 79.9(4) . . ? C1D N1D C5D 118.0(5) . . ? C1D N1D Li4 124.0(4) . . ? C5D N1D Li4 113.5(4) . . ? C1D N2D Si1D 128.3(5) . . ? N1D C1D N2D 116.0(5) . . ? N1D C1D C2D 122.5(5) . . ? N2D C1D C2D 121.5(6) . . ? C3D C2D C1D 117.9(6) . . ? C2D C3D C4D 120.5(6) . . ? C5D C4D C3D 118.5(6) . . ? N1D C5D C4D 122.6(6) . . ? N1D C5D C6D 115.8(5) . . ? C4D C5D C6D 121.6(6) . . ? O1D Si1D N2D 111.2(2) . . ? O1D Si1D C8D 112.7(2) . . ? N2D Si1D C8D 106.0(3) . . ? O1D Si1D C7D 115.4(2) . . ? N2D Si1D C7D 102.6(3) . . ? C8D Si1D C7D 108.1(3) . . ? O1D Si1D Li4 39.7(2) . . ? N2D Si1D Li4 82.2(2) . . ? C8D Si1D Li4 97.1(3) . . ? C7D Si1D Li4 151.6(3) . . ? Si1D O1D Li1 138.5(3) . . ? Si1D O1D Li3 139.9(3) . . ? Li1 O1D Li3 80.4(4) . . ? Si1D O1D Li4 110.2(3) . . ? Li1 O1D Li4 79.7(4) . . ? Li3 O1D Li4 80.8(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.283 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.074