# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1618 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Chris Russell School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287599' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email Chris.Russell@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the crystal structure in the paper 'Model for a Superbase: Synthesis and Crystal Structure of the Mixed-Metal/Mixed-Anion Aggregate [NaLi2{N(H)R}2(OR')]2' by Rebecca Holland et al., submitted to Dalton Transactions for publication. ; #================================================================= data_nap _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H82 Li4 N4 Na2 O10' _chemical_formula_weight 996.96 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.169(4) _cell_length_b 13.666(5) _cell_length_c 22.173(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.05(3) _cell_angle_gamma 90.00 _cell_volume 2774.2(20) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.093 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11443 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3624 _reflns_number_observed 2505 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material XCIF _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+28.2094P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3624 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_obs 0.1347 _refine_ls_wR_factor_all 0.3471 _refine_ls_wR_factor_obs 0.3322 _refine_ls_goodness_of_fit_all 1.236 _refine_ls_goodness_of_fit_obs 1.442 _refine_ls_restrained_S_all 1.236 _refine_ls_restrained_S_obs 1.442 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Na Na 0.1007(4) 0.3834(3) 0.1118(2) 0.0283(10) Uani 1 d . . N1 N 0.1438(9) 0.3593(5) -0.0011(3) 0.025(2) Uani 1 d . . Li1 Li -0.0818(17) 0.3726(11) 0.0039(7) 0.024(4) Uani 1 d . . N2 N 0.1588(8) 0.5604(5) 0.0781(3) 0.022(2) Uani 1 d . . Li2 Li -0.0655(18) 0.5567(10) 0.0769(7) 0.025(4) Uani 1 d . . C11 C 0.1800(11) 0.2636(7) -0.0205(4) 0.027(2) Uani 1 d . . C12 C 0.3199(11) 0.2338(7) -0.0338(4) 0.026(2) Uani 1 d . . H12A H 0.3987(11) 0.2787(7) -0.0289(4) 0.032 Uiso 1 calc R . C13 C 0.3464(12) 0.1394(8) -0.0540(5) 0.038(3) Uani 1 d . . H13A H 0.4427(12) 0.1206(8) -0.0629(5) 0.046 Uiso 1 calc R . C14 C 0.2344(12) 0.0735(7) -0.0612(4) 0.034(3) Uani 1 d . . H14A H 0.2527(12) 0.0091(7) -0.0751(4) 0.041 Uiso 1 calc R . C15 C 0.0959(12) 0.1009(7) -0.0481(4) 0.030(2) Uani 1 d . . H15A H 0.0184(12) 0.0551(7) -0.0538(4) 0.036 Uiso 1 calc R . C16 C 0.0657(10) 0.1939(7) -0.0269(4) 0.023(2) Uani 1 d . . O17 O -0.0707(7) 0.2277(4) -0.0124(3) 0.026(2) Uani 1 d . . C18 C -0.1945(12) 0.1667(7) -0.0272(5) 0.036(3) Uani 1 d . . H18A H -0.2834(12) 0.1990(7) -0.0147(5) 0.053 Uiso 1 calc R . H18B H -0.1825(12) 0.1039(7) -0.0063(5) 0.053 Uiso 1 calc R . H18C H -0.2023(12) 0.1556(7) -0.0710(5) 0.053 Uiso 1 calc R . C21 C 0.2162(10) 0.6330(6) 0.1180(4) 0.019(2) Uani 1 d . . C22 C 0.3652(10) 0.6554(7) 0.1268(4) 0.025(2) Uani 1 d . . H22A H 0.4347(10) 0.6183(7) 0.1063(4) 0.030 Uiso 1 calc R . C23 C 0.4124(11) 0.7292(7) 0.1643(4) 0.031(2) Uani 1 d . . H23A H 0.5140(11) 0.7430(7) 0.1688(4) 0.037 Uiso 1 calc R . C24 C 0.3171(11) 0.7838(7) 0.1956(4) 0.030(2) Uani 1 d . . H24A H 0.3516(11) 0.8359(7) 0.2209(4) 0.036 Uiso 1 calc R . C25 C 0.1688(11) 0.7620(7) 0.1898(4) 0.028(2) Uani 1 d . . H25A H 0.1014(11) 0.7982(7) 0.2121(4) 0.034 Uiso 1 calc R . C26 C 0.1194(9) 0.6874(7) 0.1517(4) 0.019(2) Uani 1 d . . O27 O -0.0267(7) 0.6594(4) 0.1441(3) 0.025(2) Uani 1 d . . C28 C -0.1302(11) 0.7187(7) 0.1740(5) 0.033(3) Uani 1 d . . H28A H -0.2288(11) 0.6926(7) 0.1657(5) 0.050 Uiso 1 calc R . H28B H -0.1257(11) 0.7860(7) 0.1591(5) 0.050 Uiso 1 calc R . H28C H -0.1067(11) 0.7178(7) 0.2177(5) 0.050 Uiso 1 calc R . O31 O 0.1933(8) 0.2219(5) 0.1350(3) 0.041(2) Uani 1 d . . C32 C 0.3359(13) 0.1873(9) 0.1248(6) 0.050(3) Uani 1 d . . H32A H 0.4023(13) 0.1995(9) 0.1607(6) 0.060 Uiso 1 calc R . H32B H 0.3755(13) 0.2210(9) 0.0897(6) 0.060 Uiso 1 calc R . C33 C 0.3223(13) 0.0788(8) 0.1128(5) 0.043(3) Uani 1 d . . H33A H 0.4137(13) 0.0435(8) 0.1245(5) 0.051 Uiso 1 calc R . H33B H 0.2942(13) 0.0651(8) 0.0699(5) 0.051 Uiso 1 calc R . C34 C 0.2003(13) 0.0531(8) 0.1539(5) 0.043(3) Uani 1 d . . H34A H 0.2365(13) 0.0489(8) 0.1966(5) 0.052 Uiso 1 calc R . H34B H 0.1521(13) -0.0092(8) 0.1418(5) 0.052 Uiso 1 calc R . C35 C 0.0983(12) 0.1400(7) 0.1431(5) 0.037(3) Uani 1 d . . H35A H 0.0330(12) 0.1295(7) 0.1067(5) 0.045 Uiso 1 calc R . H35B H 0.0379(12) 0.1505(7) 0.1782(5) 0.045 Uiso 1 calc R . O41 O 0.1665(8) 0.4139(5) 0.2164(3) 0.038(2) Uani 1 d . . C42 C 0.1180(12) 0.4897(7) 0.2569(5) 0.037(3) Uani 1 d . . H42A H 0.0689(12) 0.4602(7) 0.2912(5) 0.044 Uiso 1 calc R . H42B H 0.0489(12) 0.5348(7) 0.2352(5) 0.044 Uiso 1 calc R . C43 C 0.2542(12) 0.5434(8) 0.2789(5) 0.040(3) Uani 1 d . . H43A H 0.2445(12) 0.5693(8) 0.3202(5) 0.048 Uiso 1 calc R . H43B H 0.2760(12) 0.5981(8) 0.2516(5) 0.048 Uiso 1 calc R . C44 C 0.3722(13) 0.4645(9) 0.2782(6) 0.053(3) Uani 1 d . . H44A H 0.4697(13) 0.4932(9) 0.2727(6) 0.064 Uiso 1 calc R . H44B H 0.3757(13) 0.4251(9) 0.3158(6) 0.064 Uiso 1 calc R . C45 C 0.3213(12) 0.4046(9) 0.2247(5) 0.046(3) Uani 1 d . . H45A H 0.3686(12) 0.4279(9) 0.1882(5) 0.056 Uiso 1 calc R . H45B H 0.3481(12) 0.3352(9) 0.2314(5) 0.056 Uiso 1 calc R . O50 O -0.1336(6) 0.4250(4) 0.0789(3) 0.0204(14) Uani 1 d . . C50 C -0.2630(10) 0.3988(6) 0.1063(4) 0.023(2) Uani 1 d . . C51 C -0.2876(12) 0.4688(8) 0.1587(5) 0.047(3) Uani 1 d . . H51A H -0.2043(12) 0.4652(8) 0.1881(5) 0.071 Uiso 1 calc R . H51B H -0.3770(12) 0.4502(8) 0.1782(5) 0.071 Uiso 1 calc R . H51C H -0.2973(12) 0.5358(8) 0.1432(5) 0.071 Uiso 1 calc R . C52 C -0.3915(11) 0.4064(7) 0.0627(5) 0.033(3) Uani 1 d . . H52A H -0.3785(11) 0.3622(7) 0.0286(5) 0.049 Uiso 1 calc R . H52B H -0.4005(11) 0.4738(7) 0.0479(5) 0.049 Uiso 1 calc R . H52C H -0.4802(11) 0.3883(7) 0.0829(5) 0.049 Uiso 1 calc R . C53 C -0.2459(12) 0.2943(7) 0.1310(5) 0.039(3) Uani 1 d . . H53A H -0.1607(12) 0.2913(7) 0.1596(5) 0.059 Uiso 1 calc R . H53B H -0.2322(12) 0.2490(7) 0.0975(5) 0.059 Uiso 1 calc R . H53C H -0.3337(12) 0.2760(7) 0.1516(5) 0.059 Uiso 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 Na 0.033(2) 0.024(2) 0.028(2) 0.000(2) -0.003(2) 0.000(2) N1 0.041(5) 0.013(4) 0.019(4) -0.002(3) 0.002(4) 0.003(4) Li1 0.033(9) 0.018(8) 0.022(9) 0.000(7) 0.007(7) -0.010(7) N2 0.036(5) 0.018(4) 0.012(4) -0.004(3) -0.005(3) -0.006(4) Li2 0.049(10) 0.011(7) 0.015(8) -0.002(6) 0.002(7) -0.002(7) C11 0.036(6) 0.023(5) 0.022(5) -0.003(4) -0.001(4) -0.001(5) C12 0.031(6) 0.034(6) 0.014(5) 0.003(4) 0.007(4) 0.004(5) C13 0.046(7) 0.040(7) 0.029(6) 0.004(5) 0.013(5) 0.008(6) C14 0.057(8) 0.024(6) 0.022(6) 0.001(5) 0.008(5) 0.006(6) C15 0.047(7) 0.026(6) 0.017(5) 0.001(4) -0.002(5) -0.006(5) C16 0.027(6) 0.026(6) 0.015(5) 0.001(4) -0.004(4) 0.000(4) O17 0.032(4) 0.020(4) 0.027(4) -0.001(3) 0.001(3) -0.005(3) C18 0.048(7) 0.028(6) 0.030(6) 0.005(5) -0.008(5) -0.019(5) C21 0.029(6) 0.012(5) 0.017(5) 0.006(4) 0.003(4) -0.006(4) C22 0.032(6) 0.019(5) 0.026(6) 0.009(4) 0.002(4) 0.005(4) C23 0.034(6) 0.036(6) 0.023(6) 0.004(5) 0.006(5) -0.005(5) C24 0.039(7) 0.022(5) 0.027(6) -0.001(4) -0.009(5) -0.003(5) C25 0.038(6) 0.027(6) 0.020(5) 0.006(5) 0.003(4) 0.008(5) C26 0.019(5) 0.026(5) 0.012(5) 0.007(4) -0.002(4) -0.002(4) O27 0.030(4) 0.020(4) 0.027(4) 0.000(3) 0.007(3) 0.002(3) C28 0.034(6) 0.031(6) 0.035(6) 0.004(5) 0.006(5) 0.006(5) O31 0.055(5) 0.024(4) 0.044(5) 0.002(3) 0.003(4) 0.004(4) C32 0.054(8) 0.051(8) 0.045(8) 0.001(6) 0.002(6) -0.011(6) C33 0.056(7) 0.038(7) 0.035(6) -0.007(5) 0.008(5) 0.006(6) C34 0.071(8) 0.025(6) 0.033(7) -0.003(5) -0.006(6) 0.002(6) C35 0.042(7) 0.035(6) 0.035(6) 0.002(5) 0.002(5) -0.005(5) O41 0.039(4) 0.040(4) 0.035(4) 0.000(3) -0.004(3) 0.004(3) C42 0.046(7) 0.024(6) 0.041(7) -0.001(5) 0.016(5) 0.004(5) C43 0.059(8) 0.032(6) 0.027(6) 0.001(5) -0.005(5) 0.012(5) C44 0.048(8) 0.064(8) 0.048(8) -0.018(7) -0.005(6) 0.014(6) C45 0.047(7) 0.055(8) 0.036(7) -0.021(6) -0.007(5) 0.007(6) O50 0.017(3) 0.022(3) 0.022(3) -0.001(3) 0.001(3) -0.001(3) C50 0.040(6) 0.013(5) 0.015(5) -0.002(4) 0.001(4) -0.005(4) C51 0.043(7) 0.046(7) 0.055(8) -0.009(6) 0.024(6) -0.007(6) C52 0.032(6) 0.031(6) 0.034(6) 0.007(5) -0.006(5) -0.007(5) C53 0.044(7) 0.028(6) 0.046(7) 0.013(5) 0.011(5) -0.006(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 Na O50 2.303(7) . ? Na O41 2.402(8) . ? Na O31 2.409(8) . ? Na N1 2.576(8) . ? Na N2 2.595(8) . ? Na Li1 2.85(2) . ? Na Li2 2.90(2) . ? N1 C11 1.422(12) . ? N1 Li1 2.08(2) . ? N1 Li2 2.13(2) 3_565 ? Li1 O50 1.90(2) . ? Li1 O17 2.02(2) . ? Li1 N2 2.12(2) 3_565 ? Li1 Li2 2.49(2) 3_565 ? Li1 Li2 2.99(2) . ? N2 C21 1.412(11) . ? N2 Li2 2.06(2) . ? N2 Li1 2.12(2) 3_565 ? Li2 O50 1.91(2) . ? Li2 O27 2.06(2) . ? Li2 N1 2.13(2) 3_565 ? Li2 Li1 2.49(2) 3_565 ? C11 C12 1.392(13) . ? C11 C16 1.418(13) . ? C12 C13 1.391(14) . ? C13 C14 1.369(15) . ? C14 C15 1.370(14) . ? C15 C16 1.388(13) . ? C16 O17 1.387(11) . ? O17 C18 1.433(11) . ? C21 C26 1.404(12) . ? C21 C22 1.404(13) . ? C22 C23 1.362(14) . ? C23 C24 1.366(14) . ? C24 C25 1.392(14) . ? C25 C26 1.384(13) . ? C26 O27 1.395(10) . ? O27 C28 1.437(11) . ? O31 C32 1.420(14) . ? O31 C35 1.436(12) . ? C32 C33 1.51(2) . ? C33 C34 1.52(2) . ? C34 C35 1.522(15) . ? O41 C45 1.428(13) . ? O41 C42 1.457(12) . ? C42 C43 1.507(15) . ? C43 C44 1.529(15) . ? C44 C45 1.50(2) . ? O50 C50 1.408(11) . ? C50 C52 1.488(13) . ? C50 C51 1.529(14) . ? C50 C53 1.534(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O50 Na O41 116.4(3) . . ? O50 Na O31 127.3(3) . . ? O41 Na O31 83.4(3) . . ? O50 Na N1 85.0(3) . . ? O41 Na N1 156.5(3) . . ? O31 Na N1 91.2(3) . . ? O50 Na N2 83.2(2) . . ? O41 Na N2 94.1(3) . . ? O31 Na N2 147.1(3) . . ? N1 Na N2 78.2(2) . . ? O50 Na Li1 41.5(3) . . ? O41 Na Li1 157.8(4) . . ? O31 Na Li1 108.5(4) . . ? N1 Na Li1 44.8(3) . . ? N2 Na Li1 85.8(3) . . ? O50 Na Li2 41.0(3) . . ? O41 Na Li2 102.5(4) . . ? O31 Na Li2 168.3(4) . . ? N1 Na Li2 87.2(3) . . ? N2 Na Li2 43.5(4) . . ? Li1 Na Li2 62.7(4) . . ? C11 N1 Li1 110.2(7) . . ? C11 N1 Li2 109.4(7) . 3_565 ? Li1 N1 Li2 72.6(6) . 3_565 ? C11 N1 Na 117.5(6) . . ? Li1 N1 Na 74.5(5) . . ? Li2 N1 Na 129.5(5) 3_565 . ? O50 Li1 O17 123.0(8) . . ? O50 Li1 N1 112.1(8) . . ? O17 Li1 N1 81.1(6) . . ? O50 Li1 N2 120.1(8) . 3_565 ? O17 Li1 N2 106.8(7) . 3_565 ? N1 Li1 N2 106.1(7) . 3_565 ? O50 Li1 Li2 130.9(8) . 3_565 ? O17 Li1 Li2 102.6(7) . 3_565 ? N1 Li1 Li2 54.5(5) . 3_565 ? N2 Li1 Li2 52.1(5) 3_565 3_565 ? O50 Li1 Na 53.6(4) . . ? O17 Li1 Na 99.7(6) . . ? N1 Li1 Na 60.6(4) . . ? N2 Li1 Na 148.3(7) 3_565 . ? Li2 Li1 Na 105.5(6) 3_565 . ? O50 Li1 Li2 38.2(4) . . ? O17 Li1 Li2 157.1(8) . . ? N1 Li1 Li2 94.6(6) . . ? N2 Li1 Li2 96.1(6) 3_565 . ? Li2 Li1 Li2 92.8(6) 3_565 . ? Na Li1 Li2 59.5(4) . . ? C21 N2 Li2 111.4(7) . . ? C21 N2 Li1 109.2(7) . 3_565 ? Li2 N2 Li1 73.3(6) . 3_565 ? C21 N2 Na 123.5(5) . . ? Li2 N2 Na 76.2(5) . . ? Li1 N2 Na 125.8(5) 3_565 . ? O50 Li2 N2 110.6(8) . . ? O50 Li2 O27 132.0(8) . . ? N2 Li2 O27 80.8(6) . . ? O50 Li2 N1 115.5(8) . 3_565 ? N2 Li2 N1 107.0(7) . 3_565 ? O27 Li2 N1 104.0(7) . 3_565 ? O50 Li2 Li1 125.0(8) . 3_565 ? N2 Li2 Li1 54.6(6) . 3_565 ? O27 Li2 Li1 100.1(7) . 3_565 ? N1 Li2 Li1 52.9(5) 3_565 3_565 ? O50 Li2 Na 52.5(4) . . ? N2 Li2 Na 60.3(4) . . ? O27 Li2 Na 107.1(6) . . ? N1 Li2 Na 143.3(7) 3_565 . ? Li1 Li2 Na 102.2(6) 3_565 . ? O50 Li2 Li1 38.0(4) . . ? N2 Li2 Li1 92.8(6) . . ? O27 Li2 Li1 164.6(8) . . ? N1 Li2 Li1 91.2(6) 3_565 . ? Li1 Li2 Li1 87.2(6) 3_565 . ? Na Li2 Li1 57.8(4) . . ? C12 C11 C16 117.8(9) . . ? C12 C11 N1 124.5(9) . . ? C16 C11 N1 117.7(8) . . ? C13 C12 C11 121.2(10) . . ? C14 C13 C12 120.3(10) . . ? C13 C14 C15 119.6(10) . . ? C14 C15 C16 121.7(10) . . ? C15 C16 O17 125.6(8) . . ? C15 C16 C11 119.3(9) . . ? O17 C16 C11 115.1(8) . . ? C16 O17 C18 117.7(7) . . ? C16 O17 Li1 115.1(7) . . ? C18 O17 Li1 124.5(7) . . ? C26 C21 C22 116.6(8) . . ? C26 C21 N2 118.7(8) . . ? C22 C21 N2 124.7(8) . . ? C23 C22 C21 121.5(9) . . ? C22 C23 C24 121.5(10) . . ? C23 C24 C25 119.0(9) . . ? C26 C25 C24 120.0(9) . . ? C25 C26 O27 123.8(8) . . ? C25 C26 C21 121.3(8) . . ? O27 C26 C21 114.8(8) . . ? C26 O27 C28 116.3(7) . . ? C26 O27 Li2 113.7(7) . . ? C28 O27 Li2 128.6(8) . . ? C32 O31 C35 109.3(8) . . ? C32 O31 Na 126.0(6) . . ? C35 O31 Na 122.1(6) . . ? O31 C32 C33 106.7(9) . . ? C32 C33 C34 100.2(9) . . ? C33 C34 C35 101.0(9) . . ? O31 C35 C34 104.8(8) . . ? C45 O41 C42 108.5(8) . . ? C45 O41 Na 107.8(6) . . ? C42 O41 Na 130.6(6) . . ? O41 C42 C43 105.8(8) . . ? C42 C43 C44 103.2(9) . . ? C45 C44 C43 101.7(9) . . ? O41 C45 C44 108.7(9) . . ? C50 O50 Li1 122.6(7) . . ? C50 O50 Li2 122.4(7) . . ? Li1 O50 Li2 103.8(7) . . ? C50 O50 Na 126.4(5) . . ? Li1 O50 Na 84.9(5) . . ? Li2 O50 Na 86.5(5) . . ? O50 C50 C52 111.0(7) . . ? O50 C50 C51 109.2(7) . . ? C52 C50 C51 107.8(9) . . ? O50 C50 C53 108.6(8) . . ? C52 C50 C53 111.1(8) . . ? C51 C50 C53 109.2(8) . . ? _refine_diff_density_max 0.833 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.117