Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Alexander Steiner' _publ_contact_author_address ; Department of Chemistry University of Liverpool Crown Street Liverpool L69 7ZD UNITED KINGDOM ; _publ_contact_author_email A.STEINER@LIV.AC.UK _publ_section_title ; >From the tetra(amino) phosphonium cation, [P(NHPh)4]+, to the tetra(imino) phosphate trianion, [P(NPh)4]3-, two-faced ligands that bind anions and cations ; loop_ _publ_author_name 'Alexander Steiner' 'Jamie F. Bickley' 'May C. Copsey' 'John C. Jeffery' 'A. P. Leedham' ; C.Russell ; 'Dietmar Stalke' 'Thomas Stey' 'Stefano Zacchini' data_1Cl _database_code_depnum_ccdc_archive 'CCDC 229159' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cl N4 P' _chemical_formula_weight 434.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.332(8) _cell_length_b 10.106(3) _cell_length_c 18.831(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.901(7) _cell_angle_gamma 90.00 _cell_volume 4587(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.254 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _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 4619 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.29 _reflns_number_total 3105 _reflns_number_gt 2404 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0459P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3105 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.17550(10) 0.6192(2) 0.47748(12) 0.0316(6) Uani 1 1 d . . . C12 C 0.14260(11) 0.7258(2) 0.44667(14) 0.0398(7) Uani 1 1 d . . . H12 H 0.1175 0.7204 0.3975 0.048 Uiso 1 1 calc R . . C13 C 0.14625(11) 0.8408(3) 0.48761(14) 0.0437(7) Uani 1 1 d . . . H13 H 0.1237 0.9145 0.4662 0.052 Uiso 1 1 calc R . . C14 C 0.18221(12) 0.8497(3) 0.55897(16) 0.0519(8) Uani 1 1 d . . . H14 H 0.1845 0.9289 0.5869 0.062 Uiso 1 1 calc R . . C15 C 0.21464(13) 0.7429(3) 0.58928(15) 0.0603(9) Uani 1 1 d . . . H15 H 0.2396 0.7485 0.6385 0.072 Uiso 1 1 calc R . . C16 C 0.21146(11) 0.6281(3) 0.54944(14) 0.0454(7) Uani 1 1 d . . . H16 H 0.2340 0.5545 0.5712 0.054 Uiso 1 1 calc R . . C21 C 0.11483(10) 0.1950(2) 0.31025(12) 0.0304(6) Uani 1 1 d . . . C22 C 0.12741(12) 0.0662(3) 0.33021(14) 0.0461(7) Uani 1 1 d . . . H22 H 0.1547 0.0458 0.3762 0.055 Uiso 1 1 calc R . . C23 C 0.10055(13) -0.0340(3) 0.28359(15) 0.0591(9) Uani 1 1 d . . . H23 H 0.1094 -0.1234 0.2979 0.071 Uiso 1 1 calc R . . C24 C 0.06107(12) -0.0070(3) 0.21659(14) 0.0494(7) Uani 1 1 d . . . H24 H 0.0425 -0.0767 0.1849 0.059 Uiso 1 1 calc R . . C25 C 0.04932(14) 0.1202(3) 0.19683(16) 0.0710(10) Uani 1 1 d . . . H25 H 0.0222 0.1403 0.1506 0.085 Uiso 1 1 calc R . . C26 C 0.07634(14) 0.2223(3) 0.24323(16) 0.0689(10) Uani 1 1 d . . . H26 H 0.0680 0.3116 0.2282 0.083 Uiso 1 1 calc R . . C31 C 0.15871(10) 0.5656(2) 0.25854(12) 0.0290(6) Uani 1 1 d . . . C32 C 0.14585(11) 0.6626(2) 0.20396(13) 0.0384(6) Uani 1 1 d . . . H32 H 0.1105 0.7044 0.1901 0.046 Uiso 1 1 calc R . . C33 C 0.18491(12) 0.6981(3) 0.16978(14) 0.0469(7) Uani 1 1 d . . . H33 H 0.1762 0.7642 0.1321 0.056 Uiso 1 1 calc R . . C34 C 0.23601(12) 0.6390(3) 0.18978(14) 0.0457(7) Uani 1 1 d . . . H34 H 0.2629 0.6653 0.1668 0.055 Uiso 1 1 calc R . . C35 C 0.24830(11) 0.5414(3) 0.24325(14) 0.0416(7) Uani 1 1 d . . . H35 H 0.2836 0.4995 0.2565 0.050 Uiso 1 1 calc R . . C36 C 0.20994(10) 0.5037(3) 0.27788(13) 0.0372(6) Uani 1 1 d . . . H36 H 0.2186 0.4359 0.3146 0.045 Uiso 1 1 calc R . . C41 C 0.04038(10) 0.3863(2) 0.42401(12) 0.0332(6) Uani 1 1 d . . . C42 C -0.01473(11) 0.4069(2) 0.41802(13) 0.0368(6) Uani 1 1 d . . . H42 H -0.0360 0.4690 0.3828 0.044 Uiso 1 1 calc R . . C43 C -0.03908(12) 0.3379(3) 0.46299(14) 0.0469(7) Uani 1 1 d . . . H43 H -0.0770 0.3525 0.4588 0.056 Uiso 1 1 calc R . . C44 C -0.00842(12) 0.2477(3) 0.51384(14) 0.0521(8) Uani 1 1 d . . . H44 H -0.0252 0.1988 0.5442 0.063 Uiso 1 1 calc R . . C45 C 0.04656(12) 0.2288(3) 0.52055(14) 0.0515(8) Uani 1 1 d . . . H45 H 0.0678 0.1677 0.5564 0.062 Uiso 1 1 calc R . . C46 C 0.07166(11) 0.2977(3) 0.47574(13) 0.0443(7) Uani 1 1 d . . . H46 H 0.1097 0.2840 0.4806 0.053 Uiso 1 1 calc R . . Cl1 Cl 0.2500 0.2500 0.5000 0.0740(4) Uani 1 2 d S . . Cl2 Cl 0.0000 0.66944(8) 0.2500 0.0352(2) Uani 1 2 d S . . N1 N 0.17344(9) 0.4976(2) 0.43847(11) 0.0329(5) Uani 1 1 d . . . H1 H 0.1975(10) 0.438(2) 0.4598(12) 0.031(7) Uiso 1 1 d . . . N2 N 0.14387(9) 0.2955(2) 0.36018(11) 0.0325(5) Uani 1 1 d . . . H2 H 0.1701(9) 0.268(2) 0.3963(12) 0.025(7) Uiso 1 1 d . . . N3 N 0.11744(9) 0.5322(2) 0.29199(10) 0.0307(5) Uani 1 1 d . . . H3 H 0.0867(9) 0.568(2) 0.2773(10) 0.013(6) Uiso 1 1 d . . . N4 N 0.06297(9) 0.4574(2) 0.37484(11) 0.0340(5) Uani 1 1 d . . . H4 H 0.0445(9) 0.512(2) 0.3487(11) 0.014(6) Uiso 1 1 d . . . P1 P 0.12440(3) 0.44587(6) 0.36664(3) 0.0292(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0325(16) 0.0335(15) 0.0332(13) 0.0011(11) 0.0165(12) -0.0011(13) C12 0.0447(18) 0.0384(16) 0.0372(14) 0.0030(12) 0.0140(13) 0.0029(14) C13 0.0475(19) 0.0358(16) 0.0533(17) 0.0029(13) 0.0236(14) 0.0017(14) C14 0.057(2) 0.0420(18) 0.0577(18) -0.0137(14) 0.0186(16) -0.0014(16) C15 0.068(2) 0.058(2) 0.0444(17) -0.0140(15) 0.0018(15) 0.0018(18) C16 0.0456(19) 0.0429(17) 0.0408(15) -0.0028(13) 0.0031(13) 0.0051(14) C21 0.0301(16) 0.0308(14) 0.0316(13) 0.0018(11) 0.0113(11) 0.0002(12) C22 0.059(2) 0.0371(16) 0.0372(14) 0.0065(12) 0.0084(13) 0.0018(15) C23 0.086(3) 0.0332(17) 0.0537(19) 0.0069(14) 0.0150(17) -0.0045(17) C24 0.063(2) 0.0391(17) 0.0442(16) -0.0055(13) 0.0131(15) -0.0089(15) C25 0.090(3) 0.0449(19) 0.0512(18) -0.0010(15) -0.0189(17) -0.0034(19) C26 0.092(3) 0.0318(16) 0.0542(19) 0.0034(14) -0.0192(17) 0.0015(17) C31 0.0265(16) 0.0331(14) 0.0283(12) -0.0065(11) 0.0098(11) -0.0026(12) C32 0.0377(17) 0.0382(15) 0.0412(14) 0.0075(12) 0.0150(12) 0.0048(13) C33 0.047(2) 0.0493(18) 0.0480(16) 0.0130(13) 0.0204(14) -0.0024(15) C34 0.042(2) 0.0530(18) 0.0500(16) -0.0016(14) 0.0253(14) -0.0086(15) C35 0.0324(17) 0.0492(17) 0.0470(15) -0.0030(13) 0.0177(13) 0.0034(14) C36 0.0333(17) 0.0422(15) 0.0386(14) 0.0042(12) 0.0149(12) 0.0025(13) C41 0.0322(17) 0.0412(15) 0.0277(13) -0.0016(11) 0.0116(11) -0.0056(13) C42 0.0301(17) 0.0467(16) 0.0335(14) -0.0021(12) 0.0097(12) -0.0033(13) C43 0.0351(18) 0.0638(19) 0.0447(16) -0.0011(14) 0.0166(13) -0.0071(15) C44 0.046(2) 0.073(2) 0.0414(16) 0.0073(15) 0.0198(14) -0.0159(17) C45 0.049(2) 0.065(2) 0.0390(15) 0.0178(14) 0.0110(14) -0.0024(16) C46 0.0324(17) 0.0626(19) 0.0384(14) 0.0127(13) 0.0118(13) 0.0036(15) Cl1 0.0775(9) 0.0692(8) 0.0478(6) -0.0189(5) -0.0212(5) 0.0453(7) Cl2 0.0272(6) 0.0305(5) 0.0453(5) 0.000 0.0071(4) 0.000 N1 0.0309(14) 0.0334(12) 0.0323(11) 0.0019(10) 0.0066(9) 0.0079(11) N2 0.0281(14) 0.0354(13) 0.0290(11) 0.0049(10) 0.0012(10) 0.0049(11) N3 0.0179(13) 0.0409(13) 0.0350(11) 0.0063(9) 0.0104(10) 0.0084(11) N4 0.0272(14) 0.0395(14) 0.0368(12) 0.0127(11) 0.0118(10) 0.0076(11) P1 0.0279(4) 0.0326(4) 0.0281(3) 0.0023(3) 0.0099(3) 0.0031(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 C11 C12 1.377(3) . ? C11 C16 1.384(3) . ? C11 N1 1.424(3) . ? C12 C13 1.382(3) . ? C13 C14 1.375(4) . ? C14 C15 1.370(4) . ? C15 C16 1.371(4) . ? C21 C26 1.365(4) . ? C21 C22 1.365(3) . ? C21 N2 1.425(3) . ? C22 C23 1.375(4) . ? C23 C24 1.375(4) . ? C24 C25 1.345(4) . ? C25 C26 1.389(4) . ? C31 C36 1.385(3) . ? C31 C32 1.385(3) . ? C31 N3 1.417(3) . ? C32 C33 1.383(3) . ? C33 C34 1.369(4) . ? C34 C35 1.375(4) . ? C35 C36 1.380(3) . ? C41 C46 1.380(3) . ? C41 C42 1.381(3) . ? C41 N4 1.424(3) . ? C42 C43 1.381(3) . ? C43 C44 1.376(4) . ? C44 C45 1.373(4) . ? C45 C46 1.389(3) . ? N1 P1 1.617(2) . ? N2 P1 1.614(2) . ? N3 P1 1.617(2) . ? N4 P1 1.615(2) . ? 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 C12 C11 C16 119.5(2) . . ? C12 C11 N1 122.5(2) . . ? C16 C11 N1 118.0(2) . . ? C11 C12 C13 119.7(2) . . ? C14 C13 C12 120.7(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 120.8(3) . . ? C15 C16 C11 120.1(3) . . ? C26 C21 C22 119.2(2) . . ? C26 C21 N2 122.9(2) . . ? C22 C21 N2 117.9(2) . . ? C21 C22 C23 119.9(2) . . ? C22 C23 C24 121.2(3) . . ? C25 C24 C23 118.7(3) . . ? C24 C25 C26 120.7(3) . . ? C21 C26 C25 120.3(3) . . ? C36 C31 C32 120.2(2) . . ? C36 C31 N3 122.4(2) . . ? C32 C31 N3 117.5(2) . . ? C33 C32 C31 119.4(2) . . ? C34 C33 C32 120.7(2) . . ? C33 C34 C35 119.8(2) . . ? C34 C35 C36 120.7(3) . . ? C35 C36 C31 119.4(2) . . ? C46 C41 C42 120.2(2) . . ? C46 C41 N4 121.9(2) . . ? C42 C41 N4 117.9(2) . . ? C43 C42 C41 120.3(2) . . ? C44 C43 C42 119.9(3) . . ? C45 C44 C43 119.7(2) . . ? C44 C45 C46 121.0(3) . . ? C41 C46 C45 118.9(3) . . ? C11 N1 P1 127.42(18) . . ? C21 N2 P1 127.80(18) . . ? C31 N3 P1 128.07(18) . . ? C41 N4 P1 128.15(19) . . ? N2 P1 N4 113.62(11) . . ? N2 P1 N1 101.18(12) . . ? N4 P1 N1 114.34(11) . . ? N2 P1 N3 113.35(11) . . ? N4 P1 N3 101.16(11) . . ? N1 P1 N3 113.79(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4 Cl2 0.79(2) 2.45(2) 3.219(2) 167(2) . N3 H3 Cl2 0.83(2) 2.33(2) 3.155(2) 173.4(18) . N2 H2 Cl1 0.84(2) 2.35(2) 3.165(2) 165(2) . N1 H1 Cl1 0.86(2) 2.31(2) 3.160(2) 168(2) . _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.299 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.044 #===END data_2LiClthf2 _database_code_depnum_ccdc_archive 'CCDC 229160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H39 Cl Li N4 O2 P' _chemical_formula_weight 585.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8386(11) _cell_length_b 15.0001(17) _cell_length_c 11.1318(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.660(2) _cell_angle_gamma 90.00 _cell_volume 1589.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _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 8404 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4400 _reflns_number_gt 4151 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0444P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(5) _refine_ls_number_reflns 4400 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.2298(2) 0.13957(15) 0.63758(17) 0.0228(4) Uani 1 1 d . . . C12 C 0.0905(2) 0.11573(15) 0.5878(2) 0.0285(5) Uani 1 1 d . . . H12 H 0.0685 0.0695 0.5277 0.034 Uiso 1 1 calc R . . C13 C -0.0173(2) 0.15889(17) 0.6249(2) 0.0339(6) Uani 1 1 d . . . H13 H -0.1120 0.1416 0.5903 0.041 Uiso 1 1 calc R . . C14 C 0.0123(2) 0.22617(17) 0.7110(2) 0.0336(5) Uani 1 1 d . . . H14 H -0.0615 0.2552 0.7366 0.040 Uiso 1 1 calc R . . C15 C 0.1503(2) 0.25128(16) 0.7602(2) 0.0323(5) Uani 1 1 d . . . H15 H 0.1714 0.2986 0.8187 0.039 Uiso 1 1 calc R . . C16 C 0.2589(2) 0.20749(16) 0.7244(2) 0.0293(5) Uani 1 1 d . . . H16 H 0.3536 0.2245 0.7599 0.035 Uiso 1 1 calc R . . C21 C 0.6198(2) 0.07909(15) 0.40716(19) 0.0239(5) Uani 1 1 d . . . C22 C 0.7057(2) 0.00756(16) 0.39530(19) 0.0274(5) Uani 1 1 d . . . H22 H 0.6962 -0.0479 0.4335 0.033 Uiso 1 1 calc R . . C23 C 0.8050(2) 0.01765(17) 0.3277(2) 0.0315(5) Uani 1 1 d . . . H23 H 0.8637 -0.0312 0.3201 0.038 Uiso 1 1 calc R . . C24 C 0.8200(2) 0.09764(18) 0.2710(2) 0.0340(5) Uani 1 1 d . . . H24 H 0.8882 0.1040 0.2245 0.041 Uiso 1 1 calc R . . C25 C 0.7348(2) 0.16782(16) 0.2829(2) 0.0311(5) Uani 1 1 d . . . H25 H 0.7446 0.2231 0.2442 0.037 Uiso 1 1 calc R . . C26 C 0.6344(2) 0.15958(15) 0.35061(19) 0.0268(5) Uani 1 1 d . . . H26 H 0.5762 0.2088 0.3580 0.032 Uiso 1 1 calc R . . C31 C 0.6105(2) 0.22676(16) 0.70361(19) 0.0261(5) Uani 1 1 d . . . C32 C 0.6526(2) 0.30724(17) 0.7622(2) 0.0304(5) Uani 1 1 d . . . H32 H 0.6212 0.3617 0.7209 0.036 Uiso 1 1 calc R . . C33 C 0.7404(2) 0.30835(19) 0.8810(2) 0.0361(6) Uani 1 1 d . . . H33 H 0.7688 0.3638 0.9206 0.043 Uiso 1 1 calc R . . C34 C 0.7870(2) 0.23012(19) 0.9426(2) 0.0381(6) Uani 1 1 d . . . H34 H 0.8463 0.2313 1.0245 0.046 Uiso 1 1 calc R . . C35 C 0.7465(2) 0.15021(19) 0.8837(2) 0.0392(6) Uani 1 1 d . . . H35 H 0.7787 0.0960 0.9255 0.047 Uiso 1 1 calc R . . C36 C 0.6591(2) 0.14755(18) 0.7642(2) 0.0330(5) Uani 1 1 d . . . H36 H 0.6328 0.0920 0.7241 0.040 Uiso 1 1 calc R . . C41 C 0.24597(19) 0.14390(16) 0.28895(18) 0.0254(5) Uani 1 1 d . . . C42 C 0.2117(2) 0.18653(18) 0.1747(2) 0.0358(6) Uani 1 1 d . . . H42 H 0.2415 0.2461 0.1678 0.043 Uiso 1 1 calc R . . C43 C 0.1332(3) 0.1418(2) 0.0699(2) 0.0443(7) Uani 1 1 d . . . H43 H 0.1097 0.1714 -0.0081 0.053 Uiso 1 1 calc R . . C44 C 0.0897(3) 0.0559(2) 0.0782(2) 0.0447(7) Uani 1 1 d . . . H44 H 0.0369 0.0258 0.0064 0.054 Uiso 1 1 calc R . . C45 C 0.1232(2) 0.01332(19) 0.1916(2) 0.0373(6) Uani 1 1 d . . . H45 H 0.0927 -0.0462 0.1979 0.045 Uiso 1 1 calc R . . C46 C 0.2009(2) 0.05663(17) 0.2967(2) 0.0303(5) Uani 1 1 d . . . H46 H 0.2234 0.0266 0.3744 0.036 Uiso 1 1 calc R . . C51 C 0.1008(2) -0.0810(2) 0.7555(2) 0.0404(6) Uani 1 1 d . . . H51A H 0.1088 -0.0189 0.7864 0.049 Uiso 1 1 calc R . . H51B H 0.1300 -0.1219 0.8272 0.049 Uiso 1 1 calc R . . C52 C -0.0488(3) -0.1010(2) 0.6824(2) 0.0454(7) Uani 1 1 d . . . H52A H -0.1054 -0.1251 0.7369 0.054 Uiso 1 1 calc R . . H52B H -0.0954 -0.0471 0.6398 0.054 Uiso 1 1 calc R . . C53 C -0.0274(3) -0.17023(19) 0.5900(3) 0.0454(7) Uani 1 1 d . . . H53A H -0.1074 -0.1712 0.5153 0.054 Uiso 1 1 calc R . . H53B H -0.0148 -0.2305 0.6275 0.054 Uiso 1 1 calc R . . C54 C 0.1056(2) -0.13795(17) 0.5593(2) 0.0367(6) Uani 1 1 d . . . H54A H 0.1586 -0.1888 0.5371 0.044 Uiso 1 1 calc R . . H54B H 0.0829 -0.0958 0.4885 0.044 Uiso 1 1 calc R . . C61 C 0.4242(3) 0.04646(18) 0.9474(2) 0.0368(6) Uani 1 1 d . . . H61A H 0.3260 0.0674 0.9333 0.044 Uiso 1 1 calc R . . H61B H 0.4833 0.0970 0.9338 0.044 Uiso 1 1 calc R . . C62 C 0.4767(3) 0.01040(19) 1.0775(2) 0.0383(6) Uani 1 1 d . . . H62A H 0.3980 -0.0112 1.1103 0.046 Uiso 1 1 calc R . . H62B H 0.5300 0.0562 1.1344 0.046 Uiso 1 1 calc R . . C63 C 0.5716(3) -0.0662(2) 1.0601(2) 0.0442(7) Uani 1 1 d . . . H63A H 0.6670 -0.0447 1.0610 0.053 Uiso 1 1 calc R . . H63B H 0.5786 -0.1121 1.1252 0.053 Uiso 1 1 calc R . . C64 C 0.4971(3) -0.10174(18) 0.9343(2) 0.0405(6) Uani 1 1 d . . . H64A H 0.5646 -0.1303 0.8938 0.049 Uiso 1 1 calc R . . H64B H 0.4253 -0.1462 0.9416 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.53521(6) -0.11643(3) 0.62240(5) 0.03182(14) Uani 1 1 d . . . Li1 Li 0.3657(4) -0.0315(3) 0.6864(3) 0.0278(8) Uani 1 1 d . . . N1 N 0.33876(17) 0.09002(12) 0.60161(15) 0.0242(4) Uani 1 1 d . . . N2 N 0.52007(19) 0.06581(13) 0.47741(17) 0.0266(4) Uani 1 1 d . . . H2 H 0.520(2) 0.0168(15) 0.507(2) 0.011(5) Uiso 1 1 d . . . N3 N 0.51760(18) 0.22706(14) 0.58344(17) 0.0254(4) Uani 1 1 d . . . H3 H 0.512(3) 0.2723(17) 0.545(2) 0.031(7) Uiso 1 1 d . . . N4 N 0.3244(2) 0.19021(15) 0.39341(17) 0.0255(4) Uani 1 1 d . . . H4 H 0.345(3) 0.237(2) 0.389(2) 0.034(8) Uiso 1 1 d . . . O1 O 0.18649(15) -0.09422(11) 0.66921(14) 0.0325(4) Uani 1 1 d . . . O2 O 0.43249(18) -0.02605(12) 0.86436(14) 0.0377(4) Uani 1 1 d . . . P1 P 0.42106(5) 0.14147(4) 0.51924(5) 0.02182(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0274(10) 0.0213(11) 0.0222(9) 0.0056(10) 0.0110(8) 0.0003(9) C12 0.0281(11) 0.0274(13) 0.0308(11) -0.0007(10) 0.0091(9) -0.0016(9) C13 0.0226(10) 0.0395(15) 0.0407(13) 0.0013(12) 0.0101(9) 0.0003(10) C14 0.0347(12) 0.0338(14) 0.0377(12) 0.0054(11) 0.0190(11) 0.0079(11) C15 0.0373(13) 0.0303(14) 0.0333(12) -0.0065(11) 0.0163(10) -0.0006(10) C16 0.0277(11) 0.0318(13) 0.0299(11) 0.0022(10) 0.0098(10) -0.0005(10) C21 0.0210(10) 0.0293(13) 0.0229(10) -0.0020(9) 0.0083(9) 0.0004(9) C22 0.0268(11) 0.0294(13) 0.0252(10) -0.0013(10) 0.0053(9) 0.0021(10) C23 0.0250(11) 0.0386(14) 0.0310(12) -0.0029(11) 0.0072(10) 0.0088(10) C24 0.0278(12) 0.0454(15) 0.0324(12) -0.0035(12) 0.0145(10) 0.0009(11) C25 0.0312(11) 0.0338(14) 0.0315(11) 0.0001(10) 0.0140(10) -0.0045(10) C26 0.0284(11) 0.0259(13) 0.0283(11) -0.0025(10) 0.0113(9) 0.0003(9) C31 0.0205(10) 0.0333(13) 0.0275(10) 0.0017(10) 0.0115(9) -0.0014(10) C32 0.0308(12) 0.0318(13) 0.0318(12) -0.0041(11) 0.0141(10) -0.0016(10) C33 0.0332(13) 0.0441(15) 0.0329(12) -0.0095(12) 0.0120(11) -0.0045(11) C34 0.0327(12) 0.0526(17) 0.0292(11) -0.0006(13) 0.0081(10) -0.0033(12) C35 0.0312(12) 0.0457(16) 0.0389(13) 0.0125(13) 0.0055(10) 0.0008(12) C36 0.0294(11) 0.0323(13) 0.0360(12) 0.0032(12) 0.0061(10) -0.0028(11) C41 0.0203(10) 0.0317(12) 0.0264(10) 0.0002(11) 0.0100(8) 0.0055(10) C42 0.0352(13) 0.0428(15) 0.0305(12) 0.0045(11) 0.0103(11) 0.0094(11) C43 0.0414(13) 0.067(2) 0.0244(11) 0.0043(14) 0.0076(10) 0.0182(15) C44 0.0309(13) 0.068(2) 0.0352(13) -0.0194(14) 0.0076(11) 0.0082(13) C45 0.0275(12) 0.0420(15) 0.0455(14) -0.0157(13) 0.0146(11) -0.0012(11) C46 0.0254(11) 0.0393(14) 0.0278(11) -0.0033(11) 0.0099(10) 0.0012(10) C51 0.0367(13) 0.0549(17) 0.0334(12) 0.0070(12) 0.0158(11) -0.0018(12) C52 0.0332(13) 0.0533(19) 0.0522(15) 0.0034(14) 0.0154(12) -0.0056(12) C53 0.0350(14) 0.0386(16) 0.0591(17) 0.0011(14) 0.0055(13) -0.0069(12) C54 0.0366(13) 0.0344(15) 0.0364(13) 0.0005(11) 0.0043(11) -0.0044(11) C61 0.0463(14) 0.0355(14) 0.0313(12) -0.0023(11) 0.0148(11) 0.0023(11) C62 0.0437(13) 0.0432(14) 0.0273(11) -0.0062(11) 0.0078(10) -0.0028(11) C63 0.0435(15) 0.0553(18) 0.0321(13) 0.0034(13) 0.0066(12) 0.0069(13) C64 0.0506(15) 0.0397(16) 0.0319(12) 0.0026(12) 0.0120(11) 0.0101(12) Cl1 0.0451(3) 0.0211(3) 0.0348(3) 0.0001(2) 0.0201(2) 0.0042(2) Li1 0.0307(19) 0.025(2) 0.0285(18) -0.0022(16) 0.0095(16) -0.0021(16) N1 0.0232(9) 0.0243(10) 0.0275(9) 0.0020(8) 0.0107(8) 0.0021(7) N2 0.0302(10) 0.0206(11) 0.0328(10) 0.0058(9) 0.0150(8) 0.0020(8) N3 0.0262(9) 0.0221(10) 0.0288(9) 0.0056(9) 0.0087(8) -0.0010(8) N4 0.0276(10) 0.0217(11) 0.0293(10) 0.0022(9) 0.0112(8) -0.0017(8) O1 0.0287(8) 0.0365(10) 0.0350(8) -0.0009(7) 0.0131(7) -0.0061(7) O2 0.0498(10) 0.0358(10) 0.0260(8) -0.0023(8) 0.0071(8) 0.0087(8) P1 0.0224(3) 0.0206(3) 0.0244(2) 0.0009(2) 0.0095(2) 0.0004(2) _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 C11 C16 1.384(3) . ? C11 C12 1.389(3) . ? C11 N1 1.442(3) . ? C12 C13 1.391(3) . ? C13 C14 1.371(3) . ? C14 C15 1.382(3) . ? C15 C16 1.396(3) . ? C21 C26 1.386(3) . ? C21 C22 1.393(3) . ? C21 N2 1.415(2) . ? C22 C23 1.384(3) . ? C23 C24 1.381(3) . ? C24 C25 1.373(3) . ? C25 C26 1.392(3) . ? C31 C32 1.385(3) . ? C31 C36 1.390(3) . ? C31 N3 1.417(3) . ? C32 C33 1.385(3) . ? C33 C34 1.378(4) . ? C34 C35 1.376(4) . ? C35 C36 1.390(3) . ? C41 C42 1.386(3) . ? C41 C46 1.392(3) . ? C41 N4 1.406(3) . ? C42 C43 1.397(4) . ? C43 C44 1.369(4) . ? C44 C45 1.378(4) . ? C45 C46 1.386(3) . ? C51 O1 1.443(3) . ? C51 C52 1.521(4) . ? C52 C53 1.513(4) . ? C53 C54 1.514(3) . ? C54 O1 1.438(3) . ? C61 O2 1.443(3) . ? C61 C62 1.509(3) . ? C62 C63 1.524(4) . ? C63 C64 1.504(3) . ? C64 O2 1.431(3) . ? Cl1 Li1 2.348(4) . ? Li1 O2 1.925(4) . ? Li1 O1 1.964(4) . ? Li1 N1 2.039(4) . ? N1 P1 1.5709(17) . ? N2 P1 1.6381(19) . ? N3 P1 1.649(2) . ? N4 P1 1.651(2) . ? 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 C16 C11 C12 118.52(19) . . ? C16 C11 N1 122.44(18) . . ? C12 C11 N1 118.97(19) . . ? C11 C12 C13 120.7(2) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 119.4(2) . . ? C14 C15 C16 120.3(2) . . ? C11 C16 C15 120.5(2) . . ? C26 C21 C22 119.55(19) . . ? C26 C21 N2 122.67(19) . . ? C22 C21 N2 117.8(2) . . ? C23 C22 C21 119.7(2) . . ? C24 C23 C22 121.0(2) . . ? C25 C24 C23 119.0(2) . . ? C24 C25 C26 121.2(2) . . ? C21 C26 C25 119.5(2) . . ? C32 C31 C36 119.5(2) . . ? C32 C31 N3 119.1(2) . . ? C36 C31 N3 121.4(2) . . ? C31 C32 C33 120.0(2) . . ? C34 C33 C32 120.9(2) . . ? C35 C34 C33 119.0(2) . . ? C34 C35 C36 121.0(3) . . ? C31 C36 C35 119.6(2) . . ? C42 C41 C46 118.9(2) . . ? C42 C41 N4 119.1(2) . . ? C46 C41 N4 122.0(2) . . ? C41 C42 C43 120.0(3) . . ? C44 C43 C42 120.8(2) . . ? C43 C44 C45 119.5(3) . . ? C44 C45 C46 120.6(3) . . ? C45 C46 C41 120.3(2) . . ? O1 C51 C52 105.43(19) . . ? C53 C52 C51 102.5(2) . . ? C52 C53 C54 102.2(2) . . ? O1 C54 C53 106.11(18) . . ? O2 C61 C62 106.5(2) . . ? C61 C62 C63 102.70(19) . . ? C64 C63 C62 102.4(2) . . ? O2 C64 C63 105.7(2) . . ? O2 Li1 O1 100.65(17) . . ? O2 Li1 N1 114.12(19) . . ? O1 Li1 N1 112.02(19) . . ? O2 Li1 Cl1 104.57(17) . . ? O1 Li1 Cl1 113.57(18) . . ? N1 Li1 Cl1 111.33(16) . . ? C11 N1 P1 115.98(14) . . ? C11 N1 Li1 110.55(15) . . ? P1 N1 Li1 133.13(14) . . ? C21 N2 P1 127.23(17) . . ? C31 N3 P1 124.77(17) . . ? C41 N4 P1 124.10(18) . . ? C54 O1 C51 109.78(16) . . ? C54 O1 Li1 126.21(16) . . ? C51 O1 Li1 122.05(18) . . ? C64 O2 C61 109.82(17) . . ? C64 O2 Li1 120.99(17) . . ? C61 O2 Li1 129.16(18) . . ? N1 P1 N2 104.89(10) . . ? N1 P1 N3 117.07(9) . . ? N2 P1 N3 110.12(10) . . ? N1 P1 N4 116.19(10) . . ? N2 P1 N4 108.78(10) . . ? N3 P1 N4 99.67(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.81(2) 2.36(2) 3.159(2) 172(2) . N3 H3 Cl1 0.80(2) 2.46(3) 3.229(2) 164(2) 2_656 N4 H4 Cl1 0.74(3) 2.51(3) 3.237(2) 169(3) 2_656 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.037 #===END data_3Lithf3 _database_code_depnum_ccdc_archive 'CCDC 229161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Li N4 O3.50 P' _chemical_formula_weight 656.73 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.229(3) _cell_length_b 9.9824(7) _cell_length_c 18.6572(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.5120(10) _cell_angle_gamma 90.00 _cell_volume 7283.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _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 14961 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 22.49 _reflns_number_total 4754 _reflns_number_gt 3991 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0695P)^2^+6.8605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4754 _refine_ls_number_parameters 428 _refine_ls_number_restraints 294 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.140737(17) 0.35212(6) 0.40228(3) 0.0265(2) Uani 1 1 d . . . N1 N 0.10094(5) 0.3772(2) 0.40362(11) 0.0293(5) Uani 1 1 d . . . C11 C 0.14299(7) 0.1362(2) 0.31061(13) 0.0292(6) Uani 1 1 d . . . C12 C 0.16361(7) 0.0330(3) 0.28909(14) 0.0360(7) Uani 1 1 d . . . H12 H 0.1828 0.0054 0.3198 0.043 Uiso 1 1 calc R . . C13 C 0.15661(8) -0.0302(3) 0.22362(16) 0.0426(8) Uani 1 1 d . . . H13 H 0.1708 -0.1014 0.2101 0.051 Uiso 1 1 calc R . . C14 C 0.12922(8) 0.0093(3) 0.17796(16) 0.0434(8) Uani 1 1 d . . . H14 H 0.1244 -0.0341 0.1330 0.052 Uiso 1 1 calc R . . C15 C 0.10887(8) 0.1130(3) 0.19860(15) 0.0429(7) Uani 1 1 d . . . H15 H 0.0901 0.1417 0.1672 0.052 Uiso 1 1 calc R . . C16 C 0.11542(7) 0.1758(3) 0.26432(14) 0.0368(7) Uani 1 1 d . . . H16 H 0.1010 0.2463 0.2778 0.044 Uiso 1 1 calc R . . N2 N 0.15132(5) 0.4701(2) 0.35131(11) 0.0282(5) Uani 1 1 d . . . C21 C 0.16610(6) 0.4493(3) 0.53400(13) 0.0282(6) Uani 1 1 d . . . C22 C 0.15049(7) 0.5735(3) 0.52401(14) 0.0349(7) Uani 1 1 d . . . H22 H 0.1373 0.5928 0.4803 0.042 Uiso 1 1 calc R . . C23 C 0.15411(7) 0.6689(3) 0.57762(15) 0.0398(7) Uani 1 1 d . . . H23 H 0.1430 0.7530 0.5705 0.048 Uiso 1 1 calc R . . C24 C 0.17344(7) 0.6448(3) 0.64129(15) 0.0417(8) Uani 1 1 d . . . H24 H 0.1760 0.7116 0.6776 0.050 Uiso 1 1 calc R . . C25 C 0.18891(7) 0.5221(3) 0.65109(15) 0.0429(8) Uani 1 1 d . . . H25 H 0.2025 0.5044 0.6945 0.051 Uiso 1 1 calc R . . C26 C 0.18505(7) 0.4242(3) 0.59889(13) 0.0356(7) Uani 1 1 d . . . H26 H 0.1954 0.3390 0.6073 0.043 Uiso 1 1 calc R . . N3 N 0.16344(6) 0.3486(2) 0.48132(11) 0.0296(6) Uani 1 1 d . . . H3 H 0.1755(6) 0.287(3) 0.4903(13) 0.018(7) Uiso 1 1 d . . . C31 C 0.07801(7) 0.3087(3) 0.44333(13) 0.0304(6) Uani 1 1 d . . . C32 C 0.04316(7) 0.3259(3) 0.42461(17) 0.0490(8) Uani 1 1 d . . . H32 H 0.0361 0.3814 0.3848 0.059 Uiso 1 1 calc R . . C33 C 0.01870(8) 0.2648(4) 0.46206(19) 0.0666(11) Uani 1 1 d . . . H33 H -0.0048 0.2788 0.4477 0.080 Uiso 1 1 calc R . . C34 C 0.02768(8) 0.1836(3) 0.52005(18) 0.0572(9) Uani 1 1 d . . . H34 H 0.0107 0.1404 0.5454 0.069 Uiso 1 1 calc R . . C35 C 0.06169(8) 0.1668(3) 0.54019(16) 0.0456(8) Uani 1 1 d . . . H35 H 0.0683 0.1124 0.5807 0.055 Uiso 1 1 calc R . . C36 C 0.08659(7) 0.2271(3) 0.50292(14) 0.0371(7) Uani 1 1 d . . . H36 H 0.1100 0.2128 0.5181 0.045 Uiso 1 1 calc R . . N4 N 0.15031(7) 0.1955(2) 0.37807(12) 0.0310(6) Uani 1 1 d . . . H4 H 0.1656(7) 0.166(3) 0.3998(15) 0.028(9) Uiso 1 1 d . . . C41 C 0.18475(7) 0.5039(3) 0.33926(12) 0.0282(6) Uani 1 1 d . . . C42 C 0.19191(7) 0.6380(3) 0.32297(14) 0.0373(7) Uani 1 1 d . . . H42 H 0.1740 0.7020 0.3216 0.045 Uiso 1 1 calc R . . C43 C 0.22423(8) 0.6791(3) 0.30893(16) 0.0449(8) Uani 1 1 d . . . H43 H 0.2282 0.7705 0.2983 0.054 Uiso 1 1 calc R . . C44 C 0.25093(8) 0.5889(3) 0.31019(15) 0.0455(8) Uani 1 1 d . . . H44 H 0.2732 0.6172 0.3003 0.055 Uiso 1 1 calc R . . C45 C 0.24462(7) 0.4569(3) 0.32606(14) 0.0403(7) Uani 1 1 d . . . H45 H 0.2627 0.3936 0.3271 0.048 Uiso 1 1 calc R . . C46 C 0.21225(7) 0.4152(3) 0.34053(13) 0.0337(7) Uani 1 1 d . . . H46 H 0.2087 0.3236 0.3516 0.040 Uiso 1 1 calc R . . Li1 Li 0.10303(12) 0.5382(5) 0.3370(2) 0.0380(11) Uani 1 1 d . A . O1 O 0.08138(5) 0.5549(3) 0.24195(10) 0.0595(7) Uani 1 1 d D . . C101 C 0.09698(17) 0.5587(10) 0.1766(3) 0.050(2) Uiso 0.564(13) 1 d PD A 1 H10A H 0.1189 0.5089 0.1800 0.059 Uiso 0.564(13) 1 calc PR A 1 H10B H 0.1012 0.6520 0.1615 0.059 Uiso 0.564(13) 1 calc PR A 1 C102 C 0.0706(2) 0.4910(11) 0.1256(5) 0.063(4) Uiso 0.564(13) 1 d PD A 1 H10C H 0.0755 0.3941 0.1215 0.075 Uiso 0.564(13) 1 calc PR A 1 H10D H 0.0698 0.5320 0.0772 0.075 Uiso 0.564(13) 1 calc PR A 1 C103 C 0.0364(2) 0.5148(11) 0.1612(5) 0.073(4) Uiso 0.564(13) 1 d PD A 1 H10E H 0.0187 0.5560 0.1272 0.088 Uiso 0.564(13) 1 calc PR A 1 H10F H 0.0273 0.4308 0.1806 0.088 Uiso 0.564(13) 1 calc PR A 1 C104 C 0.04868(15) 0.6121(9) 0.2213(3) 0.048(2) Uiso 0.564(13) 1 d PD A 1 H10G H 0.0507 0.7048 0.2032 0.057 Uiso 0.564(13) 1 calc PR A 1 H10H H 0.0335 0.6111 0.2613 0.057 Uiso 0.564(13) 1 calc PR A 1 C1A1 C 0.09475(19) 0.5155(11) 0.1745(4) 0.034(2) Uiso 0.436(13) 1 d PD A 2 H1A1 H 0.1103 0.4378 0.1820 0.041 Uiso 0.436(13) 1 calc PR A 2 H1A2 H 0.1075 0.5904 0.1544 0.041 Uiso 0.436(13) 1 calc PR A 2 C1A2 C 0.0638(3) 0.4787(14) 0.1243(6) 0.055(4) Uiso 0.436(13) 1 d PD A 2 H1A3 H 0.0668 0.5084 0.0746 0.066 Uiso 0.436(13) 1 calc PR A 2 H1A4 H 0.0599 0.3807 0.1242 0.066 Uiso 0.436(13) 1 calc PR A 2 C1A3 C 0.0346(3) 0.5509(15) 0.1540(5) 0.065(4) Uiso 0.436(13) 1 d PD A 2 H1A5 H 0.0332 0.6449 0.1371 0.079 Uiso 0.436(13) 1 calc PR A 2 H1A6 H 0.0126 0.5054 0.1409 0.079 Uiso 0.436(13) 1 calc PR A 2 C1A4 C 0.04391(18) 0.5436(12) 0.2315(4) 0.047(3) Uiso 0.436(13) 1 d PD A 2 H1A7 H 0.0363 0.4574 0.2510 0.056 Uiso 0.436(13) 1 calc PR A 2 H1A8 H 0.0329 0.6175 0.2567 0.056 Uiso 0.436(13) 1 calc PR A 2 O2 O 0.08692(6) 0.69886(19) 0.38033(11) 0.0558(6) Uani 1 1 d D . . C201 C 0.0619(2) 0.7112(7) 0.4307(4) 0.052(2) Uiso 0.601(13) 1 d PD A 1 H20A H 0.0644 0.6396 0.4675 0.062 Uiso 0.601(13) 1 calc PR A 1 H20B H 0.0385 0.7071 0.4065 0.062 Uiso 0.601(13) 1 calc PR A 1 C202 C 0.0690(2) 0.8487(7) 0.4644(4) 0.050(3) Uiso 0.601(13) 1 d PD A 1 H20C H 0.0489 0.8840 0.4871 0.059 Uiso 0.601(13) 1 calc PR A 1 H20D H 0.0889 0.8465 0.5004 0.059 Uiso 0.601(13) 1 calc PR A 1 C203 C 0.0763(2) 0.9277(5) 0.3997(3) 0.050(2) Uiso 0.601(13) 1 d PD A 1 H20E H 0.0873 1.0145 0.4128 0.061 Uiso 0.601(13) 1 calc PR A 1 H20F H 0.0554 0.9433 0.3676 0.061 Uiso 0.601(13) 1 calc PR A 1 C204 C 0.1012(2) 0.8309(5) 0.3659(3) 0.0421(18) Uiso 0.601(13) 1 d PD A 1 H20G H 0.1016 0.8469 0.3137 0.050 Uiso 0.601(13) 1 calc PR A 1 H20H H 0.1247 0.8402 0.3890 0.050 Uiso 0.601(13) 1 calc PR A 1 C2A1 C 0.0694(3) 0.7051(8) 0.4464(5) 0.029(3) Uiso 0.399(13) 1 d PD A 2 H2A1 H 0.0447 0.6868 0.4361 0.034 Uiso 0.399(13) 1 calc PR A 2 H2A2 H 0.0790 0.6377 0.4813 0.034 Uiso 0.399(13) 1 calc PR A 2 C2A2 C 0.0745(4) 0.8386(11) 0.4753(7) 0.052(5) Uiso 0.399(13) 1 d PD A 2 H2A3 H 0.0891 0.8368 0.5210 0.062 Uiso 0.399(13) 1 calc PR A 2 H2A4 H 0.0524 0.8811 0.4838 0.062 Uiso 0.399(13) 1 calc PR A 2 C2A3 C 0.0922(4) 0.9135(11) 0.4169(6) 0.076(4) Uiso 0.399(13) 1 d PD A 2 H2A5 H 0.1170 0.9220 0.4305 0.091 Uiso 0.399(13) 1 calc PR A 2 H2A6 H 0.0824 1.0043 0.4096 0.091 Uiso 0.399(13) 1 calc PR A 2 C2A4 C 0.0859(3) 0.8291(7) 0.3483(4) 0.047(3) Uiso 0.399(13) 1 d PD A 2 H2A7 H 0.0634 0.8485 0.3226 0.056 Uiso 0.399(13) 1 calc PR A 2 H2A8 H 0.1042 0.8414 0.3152 0.056 Uiso 0.399(13) 1 calc PR A 2 O3 O 0.20342(5) 0.10270(19) 0.48992(12) 0.0493(6) Uani 1 1 d D . . C301 C 0.1884(2) -0.0208(6) 0.5145(4) 0.036(3) Uiso 0.65(2) 1 d PD B 1 H30A H 0.1634 -0.0226 0.5015 0.044 Uiso 0.65(2) 1 calc PR B 1 H30B H 0.1925 -0.0301 0.5673 0.044 Uiso 0.65(2) 1 calc PR B 1 C302 C 0.20574(18) -0.1283(5) 0.4773(5) 0.0458(18) Uiso 0.65(2) 1 d PD B 1 H30C H 0.1964 -0.1379 0.4267 0.055 Uiso 0.65(2) 1 calc PR B 1 H30D H 0.2043 -0.2153 0.5023 0.055 Uiso 0.65(2) 1 calc PR B 1 C303 C 0.24353(13) -0.0720(5) 0.4826(5) 0.034(2) Uiso 0.65(2) 1 d PD B 1 H30E H 0.2557 -0.0929 0.5298 0.041 Uiso 0.65(2) 1 calc PR B 1 H30F H 0.2567 -0.1081 0.4439 0.041 Uiso 0.65(2) 1 calc PR B 1 C304 C 0.23755(14) 0.0757(5) 0.4739(5) 0.039(2) Uiso 0.65(2) 1 d PD B 1 H30G H 0.2538 0.1261 0.5070 0.047 Uiso 0.65(2) 1 calc PR B 1 H30H H 0.2410 0.1033 0.4240 0.047 Uiso 0.65(2) 1 calc PR B 1 C3A1 C 0.1922(4) -0.0101(12) 0.5245(9) 0.044(6) Uiso 0.35(2) 1 d PD B 2 H3A1 H 0.1676 -0.0258 0.5115 0.053 Uiso 0.35(2) 1 calc PR B 2 H3A2 H 0.1959 0.0002 0.5773 0.053 Uiso 0.35(2) 1 calc PR B 2 C3A2 C 0.2137(3) -0.1265(9) 0.4986(8) 0.038(3) Uiso 0.35(2) 1 d PD B 2 H3A3 H 0.2218 -0.1840 0.5397 0.046 Uiso 0.35(2) 1 calc PR B 2 H3A4 H 0.1999 -0.1818 0.4632 0.046 Uiso 0.35(2) 1 calc PR B 2 C3A3 C 0.2419(4) -0.0692(13) 0.4664(12) 0.079(8) Uiso 0.35(2) 1 d PD B 2 H3A5 H 0.2452 -0.1149 0.4204 0.095 Uiso 0.35(2) 1 calc PR B 2 H3A6 H 0.2630 -0.0806 0.4986 0.095 Uiso 0.35(2) 1 calc PR B 2 C3A4 C 0.2354(3) 0.0729(9) 0.4536(9) 0.034(3) Uiso 0.35(2) 1 d PD B 2 H3A7 H 0.2320 0.0917 0.4015 0.041 Uiso 0.35(2) 1 calc PR B 2 H3A8 H 0.2547 0.1277 0.4746 0.041 Uiso 0.35(2) 1 calc PR B 2 O4 O 0.0000 -0.0889(5) 0.2500 0.144(2) Uani 1 2 d S . . C401 C 0.01646(13) 0.1310(5) 0.2379(3) 0.1084(17) Uani 1 1 d . . . H40A H 0.0341 0.1462 0.2781 0.130 Uiso 1 1 calc R . . H40B H 0.0187 0.2004 0.2007 0.130 Uiso 1 1 calc R . . C402 C 0.01927(15) -0.0048(6) 0.2077(3) 0.126(2) Uani 1 1 d . . . H40C H 0.0100 -0.0068 0.1569 0.151 Uiso 1 1 calc R . . H40D H 0.0435 -0.0340 0.2104 0.151 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 P1 0.0275(4) 0.0271(4) 0.0254(4) 0.0015(3) 0.0048(3) 0.0024(3) N1 0.0317(13) 0.0295(12) 0.0274(11) 0.0021(9) 0.0064(10) 0.0015(10) C11 0.0288(15) 0.0289(14) 0.0308(15) 0.0013(12) 0.0088(12) -0.0053(12) C12 0.0374(17) 0.0354(16) 0.0359(16) 0.0004(13) 0.0077(13) 0.0037(13) C13 0.0438(19) 0.0424(17) 0.0434(18) -0.0084(14) 0.0156(15) -0.0005(15) C14 0.0470(19) 0.0491(18) 0.0354(16) -0.0098(14) 0.0116(15) -0.0112(16) C15 0.0372(17) 0.0533(18) 0.0377(17) -0.0029(15) -0.0004(14) -0.0059(15) C16 0.0355(17) 0.0376(16) 0.0377(16) -0.0031(13) 0.0049(13) 0.0013(13) N2 0.0282(12) 0.0290(12) 0.0281(12) 0.0019(9) 0.0058(10) 0.0016(10) C21 0.0250(14) 0.0339(15) 0.0268(14) 0.0010(12) 0.0098(11) -0.0034(12) C22 0.0404(17) 0.0346(16) 0.0300(15) 0.0003(12) 0.0034(13) -0.0015(13) C23 0.0449(18) 0.0371(16) 0.0387(17) -0.0047(13) 0.0107(14) -0.0032(14) C24 0.0389(17) 0.055(2) 0.0329(16) -0.0126(14) 0.0138(14) -0.0132(15) C25 0.0348(17) 0.069(2) 0.0252(15) -0.0013(15) 0.0053(13) -0.0043(16) C26 0.0305(15) 0.0510(17) 0.0258(15) 0.0038(13) 0.0059(12) 0.0044(14) N3 0.0301(13) 0.0276(13) 0.0314(13) 0.0024(11) 0.0031(10) 0.0079(11) C31 0.0324(16) 0.0290(14) 0.0308(14) -0.0024(12) 0.0087(12) 0.0017(12) C32 0.0305(17) 0.066(2) 0.0503(18) 0.0231(16) 0.0060(14) 0.0025(16) C33 0.0287(18) 0.098(3) 0.074(2) 0.035(2) 0.0091(17) 0.0019(19) C34 0.039(2) 0.069(2) 0.066(2) 0.0261(19) 0.0210(17) -0.0016(17) C35 0.044(2) 0.0470(18) 0.0481(18) 0.0144(15) 0.0155(15) 0.0036(15) C36 0.0320(16) 0.0395(16) 0.0407(16) 0.0071(13) 0.0083(13) 0.0027(13) N4 0.0320(14) 0.0318(13) 0.0289(13) 0.0022(10) 0.0001(11) 0.0037(12) C41 0.0324(16) 0.0348(15) 0.0177(13) -0.0013(11) 0.0035(11) 0.0004(13) C42 0.0400(18) 0.0339(16) 0.0393(16) 0.0004(12) 0.0107(13) 0.0001(14) C43 0.050(2) 0.0405(17) 0.0459(18) 0.0008(14) 0.0153(15) -0.0135(16) C44 0.0347(18) 0.064(2) 0.0385(17) -0.0033(15) 0.0091(14) -0.0131(17) C45 0.0304(17) 0.0551(19) 0.0356(16) 0.0007(14) 0.0043(13) 0.0033(15) C46 0.0317(16) 0.0387(15) 0.0313(15) 0.0042(12) 0.0060(12) 0.0023(13) Li1 0.039(3) 0.040(3) 0.035(3) 0.006(2) 0.006(2) 0.007(2) O1 0.0373(12) 0.1100(19) 0.0316(11) 0.0004(12) 0.0046(9) 0.0276(13) O2 0.0797(17) 0.0347(11) 0.0580(14) 0.0076(10) 0.0370(12) 0.0130(11) O3 0.0371(12) 0.0363(11) 0.0752(15) 0.0069(11) 0.0079(11) 0.0128(10) O4 0.086(3) 0.072(3) 0.281(8) 0.000 0.057(4) 0.000 C401 0.097(4) 0.108(4) 0.124(4) 0.015(3) 0.028(3) 0.004(3) C402 0.105(4) 0.161(6) 0.121(4) -0.050(4) 0.062(3) -0.029(4) _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 P1 N1 1.583(2) . ? P1 N2 1.590(2) . ? P1 N3 1.662(2) . ? P1 N4 1.678(2) . ? P1 Li1 2.615(4) . ? N1 C31 1.389(3) . ? N1 Li1 2.037(5) . ? C11 C16 1.387(4) . ? C11 C12 1.389(4) . ? C11 N4 1.400(3) . ? C12 C13 1.383(4) . ? C13 C14 1.375(4) . ? C14 C15 1.380(4) . ? C15 C16 1.383(4) . ? N2 C41 1.390(3) . ? N2 Li1 2.010(5) . ? C21 C22 1.389(4) . ? C21 C26 1.393(4) . ? C21 N3 1.404(3) . ? C22 C23 1.380(4) . ? C23 C24 1.379(4) . ? C24 C25 1.372(4) . ? C25 C26 1.380(4) . ? C31 C32 1.395(4) . ? C31 C36 1.398(4) . ? C32 C33 1.374(4) . ? C33 C34 1.375(5) . ? C34 C35 1.368(4) . ? C35 C36 1.381(4) . ? C41 C46 1.394(4) . ? C41 C42 1.406(4) . ? C42 C43 1.377(4) . ? C43 C44 1.380(4) . ? C44 C45 1.377(4) . ? C45 C46 1.383(4) . ? Li1 O1 1.913(5) . ? Li1 O2 1.925(5) . ? O1 C101 1.408(6) . ? O1 C104 1.429(6) . ? O1 C1A1 1.455(7) . ? O1 C1A4 1.472(7) . ? C101 C102 1.509(10) . ? C102 C103 1.563(10) . ? C103 C104 1.532(9) . ? C1A1 C1A2 1.520(11) . ? C1A2 C1A3 1.493(11) . ? C1A3 C1A4 1.465(10) . ? O2 C201 1.419(6) . ? O2 C2A4 1.431(7) . ? O2 C2A1 1.459(7) . ? O2 C204 1.465(5) . ? C201 C202 1.526(8) . ? C202 C203 1.488(8) . ? C203 C204 1.543(8) . ? C2A1 C2A2 1.446(11) . ? C2A2 C2A3 1.531(12) . ? C2A3 C2A4 1.537(12) . ? O3 C3A1 1.386(11) . ? O3 C304 1.420(6) . ? O3 C301 1.457(6) . ? O3 C3A4 1.500(9) . ? C301 C302 1.474(7) . ? C302 C303 1.581(8) . ? C303 C304 1.499(7) . ? C3A1 C3A2 1.534(12) . ? C3A2 C3A3 1.420(12) . ? C3A3 C3A4 1.458(12) . ? O4 C402 1.411(6) 2 ? O4 C402 1.411(6) . ? C401 C401 1.401(9) 2 ? C401 C402 1.475(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 N2 101.34(11) . . ? N1 P1 N3 116.72(11) . . ? N2 P1 N3 113.56(11) . . ? N1 P1 N4 113.15(12) . . ? N2 P1 N4 117.05(11) . . ? N3 P1 N4 95.94(13) . . ? N1 P1 Li1 51.16(12) . . ? N2 P1 Li1 50.18(12) . . ? N3 P1 Li1 132.24(14) . . ? N4 P1 Li1 131.81(14) . . ? C31 N1 P1 127.68(18) . . ? C31 N1 Li1 140.6(2) . . ? P1 N1 Li1 91.59(16) . . ? C16 C11 C12 118.3(2) . . ? C16 C11 N4 122.3(2) . . ? C12 C11 N4 119.4(2) . . ? C13 C12 C11 120.9(3) . . ? C14 C13 C12 120.5(3) . . ? C13 C14 C15 118.9(3) . . ? C14 C15 C16 121.1(3) . . ? C15 C16 C11 120.3(3) . . ? C41 N2 P1 124.80(18) . . ? C41 N2 Li1 142.0(2) . . ? P1 N2 Li1 92.41(16) . . ? C22 C21 C26 118.5(2) . . ? C22 C21 N3 122.5(2) . . ? C26 C21 N3 119.0(2) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 121.5(3) . . ? C25 C24 C23 118.6(3) . . ? C24 C25 C26 121.0(3) . . ? C25 C26 C21 120.5(3) . . ? C21 N3 P1 127.7(2) . . ? N1 C31 C32 118.0(2) . . ? N1 C31 C36 125.8(2) . . ? C32 C31 C36 116.1(2) . . ? C33 C32 C31 121.9(3) . . ? C32 C33 C34 121.0(3) . . ? C35 C34 C33 118.2(3) . . ? C34 C35 C36 121.4(3) . . ? C35 C36 C31 121.3(3) . . ? C11 N4 P1 127.0(2) . . ? N2 C41 C46 125.6(2) . . ? N2 C41 C42 118.2(2) . . ? C46 C41 C42 116.2(2) . . ? C43 C42 C41 121.8(3) . . ? C42 C43 C44 120.8(3) . . ? C45 C44 C43 118.6(3) . . ? C44 C45 C46 120.9(3) . . ? C45 C46 C41 121.8(3) . . ? O1 Li1 O2 100.4(2) . . ? O1 Li1 N2 119.8(2) . . ? O2 Li1 N2 124.3(3) . . ? O1 Li1 N1 126.8(3) . . ? O2 Li1 N1 111.8(2) . . ? N2 Li1 N1 74.66(17) . . ? O1 Li1 P1 133.5(2) . . ? O2 Li1 P1 126.1(2) . . ? N2 Li1 P1 37.40(10) . . ? N1 Li1 P1 37.25(10) . . ? C101 O1 C104 101.4(4) . . ? C101 O1 C1A1 17.6(4) . . ? C104 O1 C1A1 104.6(4) . . ? C101 O1 C1A4 112.7(4) . . ? C104 O1 C1A4 29.4(3) . . ? C1A1 O1 C1A4 106.8(4) . . ? C101 O1 Li1 127.9(3) . . ? C104 O1 Li1 127.5(3) . . ? C1A1 O1 Li1 127.9(4) . . ? C1A4 O1 Li1 118.8(3) . . ? O1 C101 C102 102.2(6) . . ? C101 C102 C103 103.5(6) . . ? C104 C103 C102 100.1(6) . . ? O1 C104 C103 99.8(6) . . ? O1 C1A1 C1A2 105.8(6) . . ? C1A3 C1A2 C1A1 104.6(7) . . ? C1A4 C1A3 C1A2 101.8(8) . . ? C1A3 C1A4 O1 107.1(6) . . ? C201 O2 C2A4 101.5(5) . . ? C201 O2 C2A1 16.1(5) . . ? C2A4 O2 C2A1 108.3(5) . . ? C201 O2 C204 109.8(3) . . ? C2A4 O2 C204 26.4(4) . . ? C2A1 O2 C204 109.2(4) . . ? C201 O2 Li1 128.2(3) . . ? C2A4 O2 Li1 125.6(3) . . ? C2A1 O2 Li1 125.6(4) . . ? C204 O2 Li1 122.0(3) . . ? O2 C201 C202 103.7(5) . . ? C203 C202 C201 100.6(6) . . ? C202 C203 C204 99.7(5) . . ? O2 C204 C203 103.0(4) . . ? C2A2 C2A1 O2 107.1(6) . . ? C2A1 C2A2 C2A3 104.0(8) . . ? C2A2 C2A3 C2A4 105.8(8) . . ? O2 C2A4 C2A3 98.7(7) . . ? C3A1 O3 C304 106.3(6) . . ? C3A1 O3 C301 9.8(10) . . ? C304 O3 C301 108.5(4) . . ? C3A1 O3 C3A4 110.8(6) . . ? C304 O3 C3A4 14.7(6) . . ? C301 O3 C3A4 110.4(5) . . ? O3 C301 C302 104.7(4) . . ? C301 C302 C303 100.2(5) . . ? C304 C303 C302 101.8(4) . . ? O3 C304 C303 107.8(4) . . ? O3 C3A1 C3A2 105.5(8) . . ? C3A3 C3A2 C3A1 107.1(8) . . ? C3A2 C3A3 C3A4 109.1(10) . . ? C3A3 C3A4 O3 105.2(7) . . ? C402 O4 C402 107.0(5) 2 . ? C401 C401 C402 102.8(3) 2 . ? O4 C402 C401 105.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O3 0.79(3) 2.14(3) 2.911(3) 166(2) . N4 H4 O3 0.76(3) 2.24(3) 2.978(3) 164(3) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.381 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.045 #===END data_3Li2Clthf4 _database_code_depnum_ccdc_archive 'CCDC 229162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H112 Cl2 Li4 N8 O8.50 P2' _chemical_formula_weight 1506.40 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 19.1591(10) _cell_length_b 19.8041(10) _cell_length_c 44.318(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16815.4(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6432 _exptl_absorpt_coefficient_mu 0.173 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _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 35682 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 22.49 _reflns_number_total 10953 _reflns_number_gt 8220 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0791P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(9) _refine_ls_number_reflns 10953 _refine_ls_number_parameters 879 _refine_ls_number_restraints 2854 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.29431(7) 0.19711(7) 0.94279(3) 0.0352(3) Uani 1 1 d . . . N1 N 0.3299(2) 0.2372(2) 0.91339(9) 0.0422(11) Uani 1 1 d . . . H1 H 0.3118 0.2278 0.8956 0.051 Uiso 1 1 calc R . . C11 C 0.3847(3) 0.2836(3) 0.91350(14) 0.0427(14) Uani 1 1 d U . . C12 C 0.4184(3) 0.3039(3) 0.93948(15) 0.0594(17) Uani 1 1 d U . . H12 H 0.4043 0.2860 0.9584 0.071 Uiso 1 1 calc R . . C13 C 0.4721(3) 0.3495(4) 0.93817(19) 0.075(2) Uani 1 1 d U . . H13 H 0.4952 0.3630 0.9562 0.091 Uiso 1 1 calc R . . C14 C 0.4925(3) 0.3757(3) 0.9109(2) 0.074(2) Uani 1 1 d U . . H14 H 0.5300 0.4070 0.9100 0.089 Uiso 1 1 calc R . . C15 C 0.4596(4) 0.3573(3) 0.88545(18) 0.0655(18) Uani 1 1 d U . . H15 H 0.4733 0.3764 0.8667 0.079 Uiso 1 1 calc R . . C16 C 0.4060(3) 0.3108(3) 0.88636(14) 0.0527(16) Uani 1 1 d U . . H16 H 0.3837 0.2974 0.8682 0.063 Uiso 1 1 calc R . . N2 N 0.2283(2) 0.1618(2) 0.92385(9) 0.0398(11) Uani 1 1 d . . . H2 H 0.2274 0.1692 0.9043 0.048 Uiso 1 1 calc R . . C21 C 0.1748(3) 0.1222(3) 0.93527(12) 0.0387(13) Uani 1 1 d U . . C22 C 0.1280(3) 0.0927(3) 0.91505(13) 0.0450(14) Uani 1 1 d U . . H22 H 0.1331 0.0997 0.8940 0.054 Uiso 1 1 calc R . . C23 C 0.0747(4) 0.0535(3) 0.92594(16) 0.068(2) Uani 1 1 d U . . H23 H 0.0428 0.0339 0.9120 0.081 Uiso 1 1 calc R . . C24 C 0.0658(4) 0.0414(3) 0.95619(17) 0.074(2) Uani 1 1 d U . . H24 H 0.0292 0.0131 0.9632 0.089 Uiso 1 1 calc R . . C25 C 0.1110(3) 0.0713(3) 0.97602(15) 0.0646(19) Uani 1 1 d U . . H25 H 0.1049 0.0647 0.9971 0.078 Uiso 1 1 calc R . . C26 C 0.1658(3) 0.1113(3) 0.96578(13) 0.0485(15) Uani 1 1 d U . . H26 H 0.1972 0.1310 0.9798 0.058 Uiso 1 1 calc R . . N3 N 0.2727(2) 0.2456(2) 0.96963(9) 0.0379(11) Uani 1 1 d . . . C31 C 0.2310(3) 0.3029(3) 0.96678(13) 0.0441(14) Uani 1 1 d U . . C32 C 0.1922(3) 0.3208(3) 0.94121(15) 0.0534(16) Uani 1 1 d U . . H32 H 0.1933 0.2924 0.9240 0.064 Uiso 1 1 calc R . . C33 C 0.1521(3) 0.3792(3) 0.9406(2) 0.074(2) Uani 1 1 d U . . H33 H 0.1277 0.3910 0.9227 0.088 Uiso 1 1 calc R . . C34 C 0.1472(4) 0.4200(4) 0.9654(2) 0.077(2) Uani 1 1 d U . . H34 H 0.1183 0.4589 0.9652 0.092 Uiso 1 1 calc R . . C35 C 0.1845(4) 0.4036(3) 0.99023(18) 0.076(2) Uani 1 1 d U . . H35 H 0.1823 0.4323 1.0074 0.091 Uiso 1 1 calc R . . C36 C 0.2263(3) 0.3458(3) 0.99150(14) 0.0581(16) Uani 1 1 d U . . H36 H 0.2515 0.3357 1.0094 0.070 Uiso 1 1 calc R . . N4 N 0.3430(2) 0.1448(2) 0.95968(9) 0.0389(11) Uani 1 1 d . . . C41 C 0.3784(3) 0.0905(3) 0.94654(13) 0.0413(14) Uani 1 1 d U . . C42 C 0.4217(3) 0.0518(3) 0.96554(14) 0.0471(15) Uani 1 1 d U . . H42 H 0.4243 0.0620 0.9865 0.057 Uiso 1 1 calc R . . C43 C 0.4604(3) -0.0010(3) 0.95383(16) 0.0588(17) Uani 1 1 d U . . H43 H 0.4896 -0.0263 0.9670 0.071 Uiso 1 1 calc R . . C44 C 0.4582(4) -0.0179(3) 0.92433(17) 0.0635(18) Uani 1 1 d U . . H44 H 0.4852 -0.0543 0.9167 0.076 Uiso 1 1 calc R . . C45 C 0.4158(4) 0.0191(3) 0.90572(17) 0.072(2) Uani 1 1 d U . . H45 H 0.4135 0.0079 0.8849 0.086 Uiso 1 1 calc R . . C46 C 0.3767(3) 0.0719(3) 0.91632(13) 0.0537(16) Uani 1 1 d U . . H46 H 0.3479 0.0963 0.9027 0.064 Uiso 1 1 calc R . . Li1 Li 0.3295(5) 0.1894(4) 0.9997(2) 0.045(2) Uiso 1 1 d . A . O1 O 0.2766(2) 0.1474(2) 1.03116(8) 0.0599(11) Uani 1 1 d DU . . C101 C 0.2209(3) 0.1775(3) 1.04704(15) 0.0694(19) Uiso 1 1 d DU . . H10A H 0.1859 0.1958 1.0328 0.083 Uiso 1 1 calc R . . H10B H 0.2382 0.2149 1.0598 0.083 Uiso 1 1 calc R . . C102 C 0.1894(4) 0.1238(4) 1.0660(2) 0.113(3) Uiso 1 1 d DU . . H10C H 0.1806 0.1409 1.0866 0.135 Uiso 1 1 calc R . . H10D H 0.1445 0.1087 1.0572 0.135 Uiso 1 1 calc R . . C103 C 0.2386(4) 0.0683(4) 1.06683(17) 0.090(2) Uiso 1 1 d DU . . H10E H 0.2141 0.0243 1.0665 0.108 Uiso 1 1 calc R . . H10F H 0.2682 0.0707 1.0851 0.108 Uiso 1 1 calc R . . C104 C 0.2813(4) 0.0776(3) 1.03896(15) 0.074(2) Uiso 1 1 d DU . . H10G H 0.3305 0.0648 1.0428 0.089 Uiso 1 1 calc R . . H10H H 0.2630 0.0491 1.0224 0.089 Uiso 1 1 calc R . . O2 O 0.4169(2) 0.2192(2) 1.01726(9) 0.0725(13) Uani 1 1 d DU . . C201 C 0.4834(5) 0.2001(5) 1.0027(3) 0.060(3) Uiso 0.613(16) 1 d PDU A 1 H20A H 0.4787 0.2006 0.9804 0.072 Uiso 0.613(16) 1 calc PR A 1 H20B H 0.4983 0.1545 1.0091 0.072 Uiso 0.613(16) 1 calc PR A 1 C202 C 0.5340(6) 0.2517(6) 1.0128(3) 0.066(4) Uiso 0.613(16) 1 d PDU A 1 H20C H 0.5819 0.2330 1.0139 0.079 Uiso 0.613(16) 1 calc PR A 1 H20D H 0.5340 0.2914 0.9992 0.079 Uiso 0.613(16) 1 calc PR A 1 C203 C 0.5075(6) 0.2692(8) 1.0429(3) 0.085(5) Uiso 0.613(16) 1 d PDU A 1 H20E H 0.5282 0.3117 1.0505 0.102 Uiso 0.613(16) 1 calc PR A 1 H20F H 0.5159 0.2325 1.0576 0.102 Uiso 0.613(16) 1 calc PR A 1 C204 C 0.4254(6) 0.2778(7) 1.0355(3) 0.089(5) Uiso 0.613(16) 1 d PDU A 1 H20G H 0.3963 0.2761 1.0539 0.107 Uiso 0.613(16) 1 calc PR A 1 H20H H 0.4155 0.3199 1.0242 0.107 Uiso 0.613(16) 1 calc PR A 1 C2A1 C 0.4875(8) 0.1954(10) 1.0160(6) 0.093(8) Uiso 0.387(16) 1 d PDU A 2 H2A1 H 0.4997 0.1806 0.9954 0.112 Uiso 0.387(16) 1 calc PR A 2 H2A2 H 0.4944 0.1571 1.0301 0.112 Uiso 0.387(16) 1 calc PR A 2 C2A2 C 0.5310(10) 0.2547(12) 1.0253(7) 0.108(9) Uiso 0.387(16) 1 d PDU A 2 H2A3 H 0.5466 0.2808 1.0074 0.130 Uiso 0.387(16) 1 calc PR A 2 H2A4 H 0.5724 0.2400 1.0369 0.130 Uiso 0.387(16) 1 calc PR A 2 C2A3 C 0.4819(12) 0.2960(10) 1.0447(5) 0.102(8) Uiso 0.387(16) 1 d PDU A 2 H2A5 H 0.4611 0.3350 1.0341 0.122 Uiso 0.387(16) 1 calc PR A 2 H2A6 H 0.5027 0.3102 1.0642 0.122 Uiso 0.387(16) 1 calc PR A 2 C2A4 C 0.4323(9) 0.2354(10) 1.0476(3) 0.076(7) Uiso 0.387(16) 1 d PDU A 2 H2A7 H 0.4553 0.1971 1.0579 0.091 Uiso 0.387(16) 1 calc PR A 2 H2A8 H 0.3895 0.2478 1.0588 0.091 Uiso 0.387(16) 1 calc PR A 2 P2 P 0.24033(7) 0.14591(7) 0.68125(3) 0.0354(3) Uani 1 1 d . B . N5 N 0.2763(2) 0.1942(2) 0.70791(9) 0.0393(11) Uani 1 1 d . . . H5 H 0.2569 0.1924 0.7259 0.047 Uiso 1 1 calc R . . C51 C 0.3332(3) 0.2370(2) 0.70489(12) 0.0392(13) Uani 1 1 d DU . . C52 C 0.3622(3) 0.2663(3) 0.73022(13) 0.0520(16) Uani 1 1 d DU . . H52 H 0.3428 0.2568 0.7495 0.062 Uiso 1 1 calc R . . C53 C 0.4193(3) 0.3093(3) 0.72817(18) 0.070(2) Uani 1 1 d DU . . H53 H 0.4382 0.3290 0.7460 0.084 Uiso 1 1 calc R . . C54 C 0.4484(4) 0.3236(3) 0.7010(2) 0.078(2) Uani 1 1 d DU . . H54 H 0.4878 0.3525 0.6996 0.093 Uiso 1 1 calc R . . C55 C 0.4193(4) 0.2949(4) 0.67566(18) 0.081(2) Uani 1 1 d DU . . H55 H 0.4389 0.3047 0.6565 0.097 Uiso 1 1 calc R . . C56 C 0.3627(3) 0.2524(3) 0.67743(14) 0.0603(17) Uani 1 1 d DU . . H56 H 0.3438 0.2335 0.6595 0.072 Uiso 1 1 calc R . . N6 N 0.1758(2) 0.1151(2) 0.70271(9) 0.0386(11) Uani 1 1 d . . . H6 H 0.1777 0.1250 0.7220 0.046 Uiso 1 1 calc R . . C61 C 0.1189(3) 0.0751(2) 0.69343(12) 0.0371(13) Uani 1 1 d DU . . C62 C 0.1052(3) 0.0623(3) 0.66312(12) 0.0431(14) Uani 1 1 d DU . . H62 H 0.1353 0.0800 0.6480 0.052 Uiso 1 1 calc R . . C63 C 0.0483(3) 0.0242(3) 0.65490(14) 0.0546(16) Uani 1 1 d DU . . H63 H 0.0395 0.0158 0.6341 0.065 Uiso 1 1 calc R . . C64 C 0.0038(3) -0.0022(3) 0.67632(14) 0.0524(16) Uani 1 1 d DU . . H64 H -0.0358 -0.0279 0.6705 0.063 Uiso 1 1 calc R . . C65 C 0.0181(3) 0.0097(3) 0.70631(14) 0.0531(16) Uani 1 1 d DU . . H65 H -0.0114 -0.0090 0.7214 0.064 Uiso 1 1 calc R . . C66 C 0.0744(3) 0.0482(3) 0.71478(13) 0.0464(15) Uani 1 1 d DU . . H66 H 0.0828 0.0563 0.7356 0.056 Uiso 1 1 calc R . . N7 N 0.2151(2) 0.1853(2) 0.65228(9) 0.0450(12) Uani 1 1 d . . . C71 C 0.1732(6) 0.2519(7) 0.6546(3) 0.036(3) Uiso 0.543(17) 1 d PDU B 1 C72 C 0.1462(6) 0.2797(6) 0.6811(3) 0.040(4) Uiso 0.543(17) 1 d PDU B 1 H72 H 0.1537 0.2582 0.7000 0.048 Uiso 0.543(17) 1 calc PR B 1 C73 C 0.1084(6) 0.3390(6) 0.6795(3) 0.054(4) Uiso 0.543(17) 1 d PDU B 1 H73 H 0.0900 0.3578 0.6975 0.064 Uiso 0.543(17) 1 calc PR B 1 C74 C 0.0966(6) 0.3715(6) 0.6527(3) 0.059(4) Uiso 0.543(17) 1 d PDU B 1 H74 H 0.0720 0.4131 0.6525 0.071 Uiso 0.543(17) 1 calc PR B 1 C75 C 0.1204(6) 0.3441(6) 0.6260(3) 0.049(4) Uiso 0.543(17) 1 d PDU B 1 H75 H 0.1103 0.3652 0.6073 0.059 Uiso 0.543(17) 1 calc PR B 1 C76 C 0.1594(6) 0.2849(6) 0.6272(3) 0.044(3) Uiso 0.543(17) 1 d PDU B 1 H76 H 0.1772 0.2663 0.6090 0.053 Uiso 0.543(17) 1 calc PR B 1 C71' C 0.1791(7) 0.2331(8) 0.6479(3) 0.029(4) Uiso 0.457(17) 1 d PDU B 2 C72' C 0.1454(7) 0.2694(7) 0.6711(4) 0.040(4) Uiso 0.457(17) 1 d PDU B 2 H72' H 0.1505 0.2543 0.6914 0.048 Uiso 0.457(17) 1 calc PR B 2 C73' C 0.1052(7) 0.3258(7) 0.6656(4) 0.053(4) Uiso 0.457(17) 1 d PDU B 2 H73' H 0.0832 0.3483 0.6820 0.064 Uiso 0.457(17) 1 calc PR B 2 C74' C 0.0965(8) 0.3501(7) 0.6371(4) 0.053(5) Uiso 0.457(17) 1 d PDU B 2 H74' H 0.0691 0.3892 0.6334 0.064 Uiso 0.457(17) 1 calc PR B 2 C75' C 0.1289(6) 0.3161(7) 0.6133(3) 0.054(5) Uiso 0.457(17) 1 d PDU B 2 H75' H 0.1243 0.3328 0.5933 0.064 Uiso 0.457(17) 1 calc PR B 2 C76' C 0.1679(7) 0.2578(7) 0.6187(3) 0.047(4) Uiso 0.457(17) 1 d PDU B 2 H76' H 0.1874 0.2342 0.6020 0.057 Uiso 0.457(17) 1 calc PR B 2 N8 N 0.2898(2) 0.0914(2) 0.66691(12) 0.0630(15) Uani 1 1 d . . . C81 C 0.3385(5) 0.0536(5) 0.6737(2) 0.039(3) Uiso 0.543(9) 1 d PDU B 1 C82 C 0.3522(6) 0.0425(6) 0.7042(3) 0.049(3) Uiso 0.543(9) 1 d PDU B 1 H82 H 0.3259 0.0656 0.7191 0.059 Uiso 0.543(9) 1 calc PR B 1 C83 C 0.4048(7) -0.0027(7) 0.7129(3) 0.078(4) Uiso 0.543(9) 1 d PDU B 1 H83 H 0.4141 -0.0099 0.7337 0.094 Uiso 0.543(9) 1 calc PR B 1 C84 C 0.4427(10) -0.0363(9) 0.6917(3) 0.067(6) Uiso 0.543(9) 1 d PDU B 1 H84 H 0.4788 -0.0661 0.6979 0.080 Uiso 0.543(9) 1 calc PR B 1 C85 C 0.4299(7) -0.0281(6) 0.6619(3) 0.077(4) Uiso 0.543(9) 1 d PDU B 1 H85 H 0.4557 -0.0524 0.6471 0.092 Uiso 0.543(9) 1 calc PR B 1 C86 C 0.3778(5) 0.0170(5) 0.6536(3) 0.052(3) Uiso 0.543(9) 1 d PDU B 1 H86 H 0.3686 0.0228 0.6326 0.062 Uiso 0.543(9) 1 calc PR B 1 C81' C 0.3340(6) 0.0452(6) 0.6906(3) 0.034(3) Uiso 0.457(9) 1 d PDU B 2 C82' C 0.3333(6) 0.0476(6) 0.7218(3) 0.042(3) Uiso 0.457(9) 1 d PDU B 2 H82' H 0.3000 0.0750 0.7319 0.051 Uiso 0.457(9) 1 calc PR B 2 C83' C 0.3817(7) 0.0096(6) 0.7389(3) 0.059(4) Uiso 0.457(9) 1 d PDU B 2 H83' H 0.3813 0.0114 0.7604 0.071 Uiso 0.457(9) 1 calc PR B 2 C84' C 0.4295(8) -0.0301(8) 0.7239(3) 0.083(5) Uiso 0.457(9) 1 d PDU B 2 H84' H 0.4649 -0.0529 0.7349 0.099 Uiso 0.457(9) 1 calc PR B 2 C85' C 0.4266(12) -0.0369(12) 0.6940(4) 0.079(9) Uiso 0.457(9) 1 d PDU B 2 H85' H 0.4569 -0.0682 0.6845 0.095 Uiso 0.457(9) 1 calc PR B 2 C86' C 0.3801(6) 0.0009(6) 0.6761(3) 0.047(4) Uiso 0.457(9) 1 d PDU B 2 H86' H 0.3799 -0.0037 0.6547 0.057 Uiso 0.457(9) 1 calc PR B 2 Li2 Li 0.2678(8) 0.1246(7) 0.6243(3) 0.099(4) Uiso 1 1 d . B . O3 O 0.3421(3) 0.1524(4) 0.59828(14) 0.144(3) Uani 1 1 d DU . . C301 C 0.4042(6) 0.1856(7) 0.6070(3) 0.105(5) Uiso 0.657(9) 1 d PDU B 1 H30A H 0.4178 0.1714 0.6276 0.127 Uiso 0.657(9) 1 calc PR B 1 H30B H 0.3970 0.2351 0.6071 0.127 Uiso 0.657(9) 1 calc PR B 1 C302 C 0.4571(5) 0.1679(6) 0.5861(2) 0.077(4) Uiso 0.657(9) 1 d PDU B 1 H30C H 0.4816 0.1262 0.5923 0.093 Uiso 0.657(9) 1 calc PR B 1 H30D H 0.4915 0.2048 0.5838 0.093 Uiso 0.657(9) 1 calc PR B 1 C303 C 0.4160(7) 0.1570(9) 0.5571(3) 0.111(5) Uiso 0.657(9) 1 d PDU B 1 H30E H 0.4093 0.2000 0.5461 0.133 Uiso 0.657(9) 1 calc PR B 1 H30F H 0.4399 0.1244 0.5437 0.133 Uiso 0.657(9) 1 calc PR B 1 C304 C 0.3486(6) 0.1297(6) 0.5678(2) 0.089(4) Uiso 0.657(9) 1 d PDU B 1 H30G H 0.3096 0.1470 0.5554 0.107 Uiso 0.657(9) 1 calc PR B 1 H30H H 0.3486 0.0798 0.5669 0.107 Uiso 0.657(9) 1 calc PR B 1 C3A1 C 0.3693(16) 0.2164(9) 0.5948(7) 0.147(11) Uiso 0.343(9) 1 d PDU B 2 H3A1 H 0.3948 0.2312 0.6130 0.177 Uiso 0.343(9) 1 calc PR B 2 H3A2 H 0.3325 0.2497 0.5899 0.177 Uiso 0.343(9) 1 calc PR B 2 C3A2 C 0.4173(11) 0.2060(9) 0.5689(5) 0.077(7) Uiso 0.343(9) 1 d PDU B 2 H3A3 H 0.4576 0.2371 0.5701 0.092 Uiso 0.343(9) 1 calc PR B 2 H3A4 H 0.3927 0.2137 0.5495 0.092 Uiso 0.343(9) 1 calc PR B 2 C3A3 C 0.4407(15) 0.1341(11) 0.5713(7) 0.121(10) Uiso 0.343(9) 1 d PDU B 2 H3A5 H 0.4251 0.1075 0.5537 0.145 Uiso 0.343(9) 1 calc PR B 2 H3A6 H 0.4921 0.1313 0.5729 0.145 Uiso 0.343(9) 1 calc PR B 2 C3A4 C 0.4067(12) 0.1097(12) 0.5994(6) 0.128(10) Uiso 0.343(9) 1 d PDU B 2 H3A7 H 0.4353 0.1194 0.6176 0.154 Uiso 0.343(9) 1 calc PR B 2 H3A8 H 0.3959 0.0609 0.5985 0.154 Uiso 0.343(9) 1 calc PR B 2 O4 O 0.2124(2) 0.0639(2) 0.59831(10) 0.0803(14) Uani 1 1 d DU . . C401 C 0.2313(16) -0.0036(9) 0.5955(8) 0.114(12) Uiso 0.37(3) 1 d PDU B 1 H40A H 0.2354 -0.0251 0.6156 0.137 Uiso 0.37(3) 1 calc PR B 1 H40B H 0.2766 -0.0078 0.5849 0.137 Uiso 0.37(3) 1 calc PR B 1 C402 C 0.1741(10) -0.0362(8) 0.5775(7) 0.060(7) Uiso 0.37(3) 1 d PDU B 1 H40C H 0.1941 -0.0640 0.5611 0.072 Uiso 0.37(3) 1 calc PR B 1 H40D H 0.1454 -0.0657 0.5906 0.072 Uiso 0.37(3) 1 calc PR B 1 C403 C 0.1316(13) 0.0179(10) 0.5650(6) 0.072(8) Uiso 0.37(3) 1 d PDU B 1 H40E H 0.0815 0.0091 0.5688 0.086 Uiso 0.37(3) 1 calc PR B 1 H40F H 0.1391 0.0215 0.5429 0.086 Uiso 0.37(3) 1 calc PR B 1 C404 C 0.1534(17) 0.0803(11) 0.5800(8) 0.109(13) Uiso 0.37(3) 1 d PDU B 1 H40G H 0.1661 0.1150 0.5649 0.130 Uiso 0.37(3) 1 calc PR B 1 H40H H 0.1150 0.0981 0.5927 0.130 Uiso 0.37(3) 1 calc PR B 1 C4A1 C 0.2115(10) -0.0083(5) 0.5980(3) 0.076(5) Uiso 0.63(3) 1 d PDU B 2 H4A1 H 0.1810 -0.0263 0.6141 0.091 Uiso 0.63(3) 1 calc PR B 2 H4A2 H 0.2591 -0.0268 0.6006 0.091 Uiso 0.63(3) 1 calc PR B 2 C4A2 C 0.1825(9) -0.0253(7) 0.5667(4) 0.089(5) Uiso 0.63(3) 1 d PDU B 2 H4A3 H 0.2197 -0.0447 0.5539 0.106 Uiso 0.63(3) 1 calc PR B 2 H4A4 H 0.1444 -0.0589 0.5685 0.106 Uiso 0.63(3) 1 calc PR B 2 C4A3 C 0.1573(10) 0.0340(7) 0.5540(4) 0.087(5) Uiso 0.63(3) 1 d PDU B 2 H4A5 H 0.1072 0.0289 0.5489 0.104 Uiso 0.63(3) 1 calc PR B 2 H4A6 H 0.1832 0.0443 0.5352 0.104 Uiso 0.63(3) 1 calc PR B 2 C4A4 C 0.1664(9) 0.0881(7) 0.5756(4) 0.081(6) Uiso 0.63(3) 1 d PDU B 2 H4A7 H 0.1865 0.1284 0.5656 0.097 Uiso 0.63(3) 1 calc PR B 2 H4A8 H 0.1209 0.1008 0.5846 0.097 Uiso 0.63(3) 1 calc PR B 2 Li3 Li 0.2718(6) 0.1163(5) 0.8144(2) 0.069(3) Uiso 1 1 d . . . O5 O 0.2485(5) 0.0269(2) 0.82411(10) 0.141(3) Uani 1 1 d DU C . C501 C 0.2527(9) -0.0079(6) 0.8510(3) 0.068(4) Uiso 0.526(15) 1 d PDU C 1 H50A H 0.2365 0.0201 0.8682 0.082 Uiso 0.526(15) 1 calc PR C 1 H50B H 0.3009 -0.0235 0.8550 0.082 Uiso 0.526(15) 1 calc PR C 1 C502 C 0.2027(10) -0.0680(9) 0.8451(3) 0.085(6) Uiso 0.526(15) 1 d PDU C 1 H50C H 0.2201 -0.1100 0.8547 0.102 Uiso 0.526(15) 1 calc PR C 1 H50D H 0.1550 -0.0583 0.8525 0.102 Uiso 0.526(15) 1 calc PR C 1 C503 C 0.2046(9) -0.0729(8) 0.8109(3) 0.085(6) Uiso 0.526(15) 1 d PDU C 1 H50E H 0.1596 -0.0583 0.8021 0.102 Uiso 0.526(15) 1 calc PR C 1 H50F H 0.2144 -0.1198 0.8044 0.102 Uiso 0.526(15) 1 calc PR C 1 C504 C 0.2636(8) -0.0256(6) 0.8016(3) 0.077(5) Uiso 0.526(15) 1 d PDU C 1 H50G H 0.3102 -0.0461 0.8043 0.092 Uiso 0.526(15) 1 calc PR C 1 H50H H 0.2583 -0.0090 0.7806 0.092 Uiso 0.526(15) 1 calc PR C 1 C5A1 C 0.2171(11) -0.0037(6) 0.8499(3) 0.071(5) Uiso 0.474(15) 1 d PDU C 2 H5A1 H 0.1675 0.0097 0.8518 0.086 Uiso 0.474(15) 1 calc PR C 2 H5A2 H 0.2421 0.0091 0.8686 0.086 Uiso 0.474(15) 1 calc PR C 2 C5A2 C 0.2239(13) -0.0794(7) 0.8438(4) 0.084(7) Uiso 0.474(15) 1 d PDU C 2 H5A3 H 0.2650 -0.0985 0.8543 0.101 Uiso 0.474(15) 1 calc PR C 2 H5A4 H 0.1816 -0.1039 0.8504 0.101 Uiso 0.474(15) 1 calc PR C 2 C5A3 C 0.2327(12) -0.0832(7) 0.8099(4) 0.094(7) Uiso 0.474(15) 1 d PDU C 2 H5A5 H 0.2820 -0.0907 0.8042 0.112 Uiso 0.474(15) 1 calc PR C 2 H5A6 H 0.2034 -0.1193 0.8011 0.112 Uiso 0.474(15) 1 calc PR C 2 C5A4 C 0.2085(8) -0.0159(6) 0.8007(3) 0.062(5) Uiso 0.474(15) 1 d PDU C 2 H5A7 H 0.1573 -0.0110 0.8028 0.075 Uiso 0.474(15) 1 calc PR C 2 H5A8 H 0.2225 -0.0049 0.7798 0.075 Uiso 0.474(15) 1 calc PR C 2 O6 O 0.3692(3) 0.1144(4) 0.80596(12) 0.128(2) Uani 1 1 d DU D . C601 C 0.4163(9) 0.1157(11) 0.7815(3) 0.133(7) Uiso 0.584(15) 1 d PDU D 1 H60A H 0.3976 0.1421 0.7643 0.160 Uiso 0.584(15) 1 calc PR D 1 H60B H 0.4282 0.0696 0.7746 0.160 Uiso 0.584(15) 1 calc PR D 1 C602 C 0.4798(9) 0.1512(12) 0.7962(4) 0.120(9) Uiso 0.584(15) 1 d PDU D 1 H60C H 0.5244 0.1315 0.7891 0.144 Uiso 0.584(15) 1 calc PR D 1 H60D H 0.4797 0.2003 0.7920 0.144 Uiso 0.584(15) 1 calc PR D 1 C603 C 0.4685(12) 0.1372(14) 0.8291(4) 0.167(11) Uiso 0.584(15) 1 d PDU D 1 H60E H 0.5113 0.1187 0.8384 0.200 Uiso 0.584(15) 1 calc PR D 1 H60F H 0.4550 0.1789 0.8399 0.200 Uiso 0.584(15) 1 calc PR D 1 C604 C 0.4112(6) 0.0870(7) 0.8297(3) 0.077(5) Uiso 0.584(15) 1 d PDU D 1 H60G H 0.4279 0.0409 0.8250 0.093 Uiso 0.584(15) 1 calc PR D 1 H60H H 0.3863 0.0869 0.8493 0.093 Uiso 0.584(15) 1 calc PR D 1 C6A1 C 0.4030(6) 0.1600(7) 0.7871(3) 0.047(5) Uiso 0.416(15) 1 d PDU D 2 H6A1 H 0.3967 0.2069 0.7943 0.056 Uiso 0.416(15) 1 calc PR D 2 H6A2 H 0.3855 0.1564 0.7661 0.056 Uiso 0.416(15) 1 calc PR D 2 C6A2 C 0.4807(8) 0.1381(16) 0.7891(5) 0.102(10) Uiso 0.416(15) 1 d PDU D 2 H6A3 H 0.4895 0.0947 0.7788 0.122 Uiso 0.416(15) 1 calc PR D 2 H6A4 H 0.5127 0.1731 0.7812 0.122 Uiso 0.416(15) 1 calc PR D 2 C6A3 C 0.4849(9) 0.1317(12) 0.8230(4) 0.079(7) Uiso 0.416(15) 1 d PDU D 2 H6A5 H 0.5001 0.0860 0.8291 0.094 Uiso 0.416(15) 1 calc PR D 2 H6A6 H 0.5168 0.1657 0.8318 0.094 Uiso 0.416(15) 1 calc PR D 2 C6A4 C 0.4116(10) 0.1446(18) 0.8316(5) 0.189(12) Uiso 0.416(15) 1 d PDU D 2 H6A7 H 0.4026 0.1937 0.8334 0.226 Uiso 0.416(15) 1 calc PR D 2 H6A8 H 0.4002 0.1225 0.8510 0.226 Uiso 0.416(15) 1 calc PR D 2 Cl1 Cl 0.24957(9) 0.19155(8) 0.85256(3) 0.0601(4) Uani 1 1 d . F . Cl2 Cl 0.20899(8) 0.15472(9) 0.77354(3) 0.0619(5) Uani 1 1 d . F . O7 O 0.2182(3) 0.3297(2) 0.79887(15) 0.110(2) Uani 1 1 d DU . . C701 C 0.2277(4) 0.3649(4) 0.77145(16) 0.088(2) Uiso 1 1 d DU . . H70A H 0.1859 0.3923 0.7666 0.106 Uiso 1 1 calc R . . H70B H 0.2362 0.3329 0.7547 0.106 Uiso 1 1 calc R . . C702 C 0.2912(4) 0.4106(3) 0.77612(15) 0.0724(19) Uiso 1 1 d DU . . H70C H 0.3266 0.4032 0.7602 0.087 Uiso 1 1 calc R F . H70D H 0.2776 0.4588 0.7763 0.087 Uiso 1 1 calc R . . C703 C 0.3180(4) 0.3891(4) 0.80617(18) 0.101(3) Uiso 1 1 d DU F . H70E H 0.3536 0.3531 0.8040 0.121 Uiso 1 1 calc R . . H70F H 0.3389 0.4277 0.8171 0.121 Uiso 1 1 calc R . . C704 C 0.2557(5) 0.3637(5) 0.8219(2) 0.128(3) Uiso 1 1 d DU F . H70G H 0.2687 0.3323 0.8384 0.153 Uiso 1 1 calc R E 1 H70H H 0.2280 0.4013 0.8304 0.153 Uiso 1 1 calc R E 1 O8 O 0.0911(2) 0.2405(2) 0.82558(9) 0.0605(11) Uani 1 1 d DU . . C801 C 0.0933(15) 0.2886(7) 0.8506(4) 0.056(6) Uiso 0.50(6) 1 d PDU F 1 H80A H 0.0644 0.3286 0.8459 0.068 Uiso 0.50(6) 1 calc PR F 1 H80B H 0.1418 0.3036 0.8542 0.068 Uiso 0.50(6) 1 calc PR F 1 C802 C 0.0655(12) 0.2537(10) 0.8781(4) 0.056(7) Uiso 0.50(6) 1 d PDU F 1 H80C H 0.1031 0.2307 0.8894 0.067 Uiso 0.50(6) 1 calc PR F 1 H80D H 0.0412 0.2858 0.8917 0.067 Uiso 0.50(6) 1 calc PR F 1 C803 C 0.0161(9) 0.2045(15) 0.8646(4) 0.052(6) Uiso 0.50(6) 1 d PDU F 1 H80E H -0.0297 0.2258 0.8604 0.062 Uiso 0.50(6) 1 calc PR F 1 H80F H 0.0090 0.1652 0.8781 0.062 Uiso 0.50(6) 1 calc PR F 1 C804 C 0.0518(15) 0.1838(11) 0.8359(4) 0.072(8) Uiso 0.50(6) 1 d PDU F 1 H80G H 0.0831 0.1450 0.8397 0.086 Uiso 0.50(6) 1 calc PR F 1 H80H H 0.0168 0.1705 0.8206 0.086 Uiso 0.50(6) 1 calc PR F 1 C8A1 C 0.0747(18) 0.2900(7) 0.8470(4) 0.073(7) Uiso 0.50(6) 1 d PDU F 2 H8A1 H 0.0357 0.3187 0.8399 0.087 Uiso 0.50(6) 1 calc PR F 2 H8A2 H 0.1157 0.3190 0.8512 0.087 Uiso 0.50(6) 1 calc PR F 2 C8A2 C 0.0540(16) 0.2498(10) 0.8747(4) 0.067(8) Uiso 0.50(6) 1 d PDU F 2 H8A3 H 0.0954 0.2375 0.8868 0.081 Uiso 0.50(6) 1 calc PR F 2 H8A4 H 0.0210 0.2755 0.8874 0.081 Uiso 0.50(6) 1 calc PR F 2 C8A3 C 0.0195(8) 0.1877(12) 0.8615(4) 0.048(5) Uiso 0.50(6) 1 d PDU F 2 H8A5 H 0.0213 0.1492 0.8758 0.058 Uiso 0.50(6) 1 calc PR F 2 H8A6 H -0.0296 0.1967 0.8559 0.058 Uiso 0.50(6) 1 calc PR F 2 C8A4 C 0.0639(12) 0.1752(8) 0.8343(4) 0.045(6) Uiso 0.50(6) 1 d PDU F 2 H8A7 H 0.1025 0.1437 0.8391 0.054 Uiso 0.50(6) 1 calc PR F 2 H8A8 H 0.0357 0.1555 0.8178 0.054 Uiso 0.50(6) 1 calc PR F 2 Li4 Li 0.1867(10) 0.2424(9) 0.8121(4) 0.051(5) Uiso 0.50 1 d P F 1 Li4' Li 0.1533(11) 0.2483(10) 0.7897(5) 0.062(6) Uiso 0.50 1 d P F -2 O9 O 0.0835(4) 0.2599(3) 0.75741(18) 0.054(2) Uani 0.50 1 d PDU F -2 C901 C 0.0439(7) 0.2017(6) 0.7482(4) 0.049(4) Uiso 0.50 1 d PDU F -2 H90A H 0.0579 0.1616 0.7601 0.059 Uiso 0.50 1 calc PR F -2 H90B H 0.0515 0.1921 0.7266 0.059 Uiso 0.50 1 calc PR F -2 C902 C -0.0306(7) 0.2191(6) 0.7540(4) 0.057(5) Uiso 0.50 1 d PDU F -2 H90C H -0.0437 0.2089 0.7752 0.069 Uiso 0.50 1 calc PR F -2 H90D H -0.0620 0.1941 0.7403 0.069 Uiso 0.50 1 calc PR F -2 C903 C -0.0331(7) 0.2931(7) 0.7480(4) 0.066(5) Uiso 0.50 1 d PDU F -2 H90E H -0.0356 0.3031 0.7261 0.079 Uiso 0.50 1 calc PR F -2 H90F H -0.0726 0.3152 0.7585 0.079 Uiso 0.50 1 calc PR F -2 C904 C 0.0350(7) 0.3127(6) 0.7611(4) 0.071(5) Uiso 0.50 1 d PDU F -2 H90G H 0.0525 0.3539 0.7510 0.085 Uiso 0.50 1 calc PR F -2 H90H H 0.0293 0.3228 0.7828 0.085 Uiso 0.50 1 calc PR F -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0357(8) 0.0370(7) 0.0328(8) -0.0003(7) -0.0013(7) -0.0042(7) N1 0.045(3) 0.049(3) 0.033(3) 0.001(2) -0.006(2) -0.014(2) C11 0.036(3) 0.035(3) 0.057(4) 0.002(3) 0.007(3) 0.005(3) C12 0.055(4) 0.060(4) 0.064(4) 0.018(4) -0.015(3) -0.022(4) C13 0.058(4) 0.075(5) 0.093(6) 0.015(5) -0.026(4) -0.027(4) C14 0.042(4) 0.054(4) 0.126(7) 0.015(5) 0.007(5) -0.011(3) C15 0.056(4) 0.056(4) 0.084(5) 0.017(4) 0.024(4) -0.001(4) C16 0.058(4) 0.043(3) 0.057(4) 0.001(3) 0.019(3) 0.000(3) N2 0.049(3) 0.041(2) 0.029(2) 0.006(2) -0.007(2) -0.005(2) C21 0.038(3) 0.037(3) 0.041(3) 0.006(3) -0.011(3) 0.000(3) C22 0.045(3) 0.041(3) 0.049(4) 0.009(3) -0.015(3) -0.007(3) C23 0.064(5) 0.069(4) 0.070(5) 0.012(4) -0.035(4) -0.020(4) C24 0.067(5) 0.076(5) 0.078(5) 0.031(4) -0.021(4) -0.035(4) C25 0.061(4) 0.074(4) 0.059(4) 0.021(4) -0.008(4) -0.015(4) C26 0.045(4) 0.055(4) 0.046(4) 0.011(3) -0.009(3) -0.020(3) N3 0.039(3) 0.038(2) 0.037(2) -0.002(2) -0.001(2) 0.000(2) C31 0.035(3) 0.043(3) 0.054(4) -0.003(3) 0.005(3) -0.007(3) C32 0.045(4) 0.045(4) 0.071(4) -0.004(3) -0.013(3) 0.005(3) C33 0.046(4) 0.056(4) 0.118(6) 0.005(5) -0.019(4) -0.007(4) C34 0.051(4) 0.057(5) 0.123(7) -0.003(5) 0.007(5) 0.015(4) C35 0.090(6) 0.060(4) 0.077(5) -0.019(4) 0.013(4) 0.009(4) C36 0.067(4) 0.048(4) 0.059(4) -0.013(3) 0.008(3) 0.012(3) N4 0.042(3) 0.040(2) 0.035(2) 0.001(2) 0.003(2) 0.004(2) C41 0.038(3) 0.038(3) 0.048(4) 0.000(3) 0.001(3) -0.003(3) C42 0.044(3) 0.045(3) 0.053(4) 0.003(3) 0.005(3) 0.006(3) C43 0.047(4) 0.056(4) 0.074(5) 0.010(4) 0.005(3) 0.005(3) C44 0.059(4) 0.052(4) 0.080(5) -0.013(4) 0.012(4) 0.006(3) C45 0.090(5) 0.061(4) 0.065(5) -0.025(4) 0.006(4) 0.009(4) C46 0.061(4) 0.057(4) 0.043(4) -0.010(3) 0.002(3) 0.012(3) O1 0.054(3) 0.071(3) 0.054(2) 0.015(2) 0.020(2) 0.015(2) O2 0.058(3) 0.101(4) 0.058(3) -0.020(3) -0.010(2) -0.016(3) P2 0.0339(8) 0.0380(7) 0.0343(7) -0.0040(7) 0.0011(6) -0.0020(6) N5 0.041(3) 0.042(2) 0.035(2) 0.000(2) 0.003(2) -0.009(2) C51 0.034(3) 0.036(3) 0.048(4) 0.005(3) 0.001(3) 0.002(3) C52 0.040(4) 0.059(4) 0.057(4) -0.005(3) -0.008(3) -0.004(3) C53 0.045(4) 0.067(4) 0.098(6) -0.022(4) -0.015(4) -0.010(4) C54 0.048(4) 0.063(5) 0.122(7) 0.004(5) -0.006(5) -0.019(4) C55 0.063(5) 0.087(5) 0.092(6) 0.017(5) 0.010(4) -0.023(4) C56 0.052(4) 0.077(4) 0.052(4) 0.004(4) 0.002(3) -0.024(4) N6 0.042(3) 0.041(2) 0.033(3) 0.004(2) -0.007(2) -0.011(2) C61 0.040(3) 0.030(3) 0.041(3) -0.002(3) -0.010(3) 0.001(3) C62 0.044(3) 0.046(3) 0.040(4) 0.001(3) 0.002(3) -0.007(3) C63 0.052(4) 0.058(4) 0.053(4) -0.012(3) -0.015(3) -0.008(3) C64 0.048(4) 0.052(4) 0.057(4) -0.006(3) -0.005(3) -0.017(3) C65 0.048(4) 0.048(4) 0.063(4) 0.000(3) 0.015(3) -0.009(3) C66 0.051(4) 0.044(3) 0.044(4) -0.001(3) 0.006(3) -0.017(3) N7 0.039(3) 0.068(3) 0.028(2) 0.008(2) 0.002(2) -0.007(3) N8 0.034(3) 0.062(3) 0.093(4) -0.035(3) -0.003(3) 0.003(3) O3 0.069(4) 0.245(7) 0.117(5) -0.099(5) 0.059(3) -0.052(5) O4 0.077(3) 0.108(4) 0.056(3) -0.024(3) -0.001(3) -0.026(3) O5 0.322(9) 0.056(3) 0.046(3) -0.004(2) 0.011(5) -0.009(4) O6 0.067(3) 0.247(8) 0.070(4) 0.001(4) -0.009(3) 0.045(4) Cl1 0.0789(11) 0.0672(9) 0.0343(7) -0.0045(7) -0.0083(8) -0.0062(9) Cl2 0.0533(9) 0.1023(12) 0.0302(7) 0.0038(8) -0.0049(7) -0.0056(9) O7 0.106(4) 0.062(3) 0.162(5) 0.019(3) 0.055(4) -0.006(3) O8 0.066(3) 0.061(3) 0.054(3) 0.016(2) 0.009(2) -0.001(2) O9 0.055(5) 0.036(4) 0.069(5) -0.011(4) -0.009(4) 0.004(4) _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 P1 N4 1.582(4) . ? P1 N3 1.585(4) . ? P1 N1 1.671(4) . ? P1 N2 1.671(4) . ? P1 Li1 2.616(9) . ? N1 C11 1.396(6) . ? C11 C16 1.379(8) . ? C11 C12 1.380(8) . ? C12 C13 1.371(8) . ? C13 C14 1.371(10) . ? C14 C15 1.342(9) . ? C15 C16 1.380(9) . ? N2 C21 1.386(6) . ? C21 C26 1.380(7) . ? C21 C22 1.396(7) . ? C22 C23 1.372(8) . ? C23 C24 1.372(9) . ? C24 C25 1.369(9) . ? C25 C26 1.390(8) . ? N3 C31 1.393(7) . ? N3 Li1 2.050(10) . ? C31 C36 1.388(7) . ? C31 C32 1.401(8) . ? C32 C33 1.389(8) . ? C33 C34 1.370(10) . ? C34 C35 1.351(10) . ? C35 C36 1.398(9) . ? N4 C41 1.398(6) . ? N4 Li1 1.999(10) . ? C41 C46 1.390(8) . ? C41 C42 1.409(7) . ? C42 C43 1.384(8) . ? C43 C44 1.350(8) . ? C44 C45 1.369(9) . ? C45 C46 1.369(8) . ? Li1 O1 1.915(10) . ? Li1 O2 1.938(10) . ? O1 C101 1.411(7) . ? O1 C104 1.428(7) . ? C101 C102 1.484(9) . ? C102 C103 1.449(9) . ? C103 C104 1.493(9) . ? O2 C2A4 1.413(13) . ? O2 C204 1.422(11) . ? O2 C2A1 1.434(15) . ? O2 C201 1.479(10) . ? C201 C202 1.479(11) . ? C202 C203 1.467(14) . ? C203 C204 1.616(14) . ? C2A1 C2A2 1.496(16) . ? C2A1 C2A4 1.92(2) . ? C2A2 C2A3 1.515(17) . ? C2A3 C2A4 1.536(16) . ? P2 N8 1.571(5) . ? P2 N7 1.578(4) . ? P2 N5 1.669(4) . ? P2 N6 1.675(4) . ? P2 Li2 2.611(14) . ? N5 C51 1.387(6) . ? C51 C56 1.377(7) . ? C51 C52 1.381(7) . ? C52 C53 1.390(8) . ? C53 C54 1.354(9) . ? C54 C55 1.377(9) . ? C55 C56 1.375(8) . ? N6 C61 1.408(6) . ? C61 C66 1.381(7) . ? C61 C62 1.392(7) . ? C62 C63 1.375(7) . ? C63 C64 1.378(7) . ? C64 C65 1.377(7) . ? C65 C66 1.373(7) . ? N7 C71' 1.188(13) . ? N7 C71 1.548(14) . ? N7 Li2 2.000(15) . ? C71 C72 1.399(13) . ? C71 C76 1.402(11) . ? C72 C73 1.380(11) . ? C73 C74 1.370(12) . ? C74 C75 1.377(14) . ? C75 C76 1.393(13) . ? C71' C76' 1.402(12) . ? C71' C72' 1.410(14) . ? C72' C73' 1.380(13) . ? C73' C74' 1.363(14) . ? C74' C75' 1.393(15) . ? C75' C76' 1.395(14) . ? N8 C81 1.233(10) . ? N8 C81' 1.627(15) . ? N8 Li2 2.043(15) . ? C81 C86 1.376(11) . ? C81 C82 1.393(13) . ? C82 C83 1.401(13) . ? C83 C84 1.363(14) . ? C84 C85 1.353(14) . ? C85 C86 1.389(12) . ? C81' C82' 1.387(14) . ? C81' C86' 1.402(13) . ? C82' C83' 1.414(13) . ? C83' C84' 1.380(14) . ? C84' C85' 1.329(15) . ? C85' C86' 1.410(15) . ? Li2 O3 1.914(15) . ? Li2 O4 1.975(15) . ? O3 C3A1 1.380(16) . ? O3 C301 1.413(11) . ? O3 C304 1.428(10) . ? O3 C3A4 1.499(16) . ? C301 C302 1.418(12) . ? C302 C303 1.524(13) . ? C303 C304 1.477(12) . ? C3A1 C3A2 1.483(16) . ? C3A2 C3A3 1.495(17) . ? C3A3 C3A4 1.486(17) . ? O4 C401 1.391(16) . ? O4 C4A4 1.421(11) . ? O4 C404 1.427(16) . ? O4 C4A1 1.429(11) . ? C401 C402 1.502(16) . ? C402 C403 1.454(16) . ? C403 C404 1.465(16) . ? C4A1 C4A2 1.532(13) . ? C4A2 C4A3 1.389(12) . ? C4A3 C4A4 1.450(13) . ? Li3 O5 1.875(12) . ? Li3 O6 1.905(13) . ? Li3 Cl1 2.293(11) . ? Li3 Cl2 2.303(11) . ? Li3 Li4 2.98(2) . ? O5 C501 1.380(11) . ? O5 C5A1 1.427(12) . ? O5 C504 1.470(11) . ? O5 C5A4 1.544(12) . ? C501 C502 1.550(14) . ? C502 C503 1.518(14) . ? C503 C504 1.526(14) . ? C5A1 C5A2 1.529(15) . ? C5A2 C5A3 1.513(15) . ? C5A3 C5A4 1.470(15) . ? O6 C6A1 1.389(11) . ? O6 C601 1.411(13) . ? O6 C604 1.432(10) . ? O6 C6A4 1.517(17) . ? C601 C602 1.549(15) . ? C602 C603 1.497(16) . ? C603 C604 1.482(16) . ? C6A1 C6A2 1.553(16) . ? C6A1 C6A4 2.00(2) . ? C6A2 C6A3 1.506(16) . ? C6A3 C6A4 1.478(17) . ? Cl1 Li4 2.38(2) . ? Cl2 Li4' 2.26(2) . ? Cl2 Li4 2.472(19) . ? O7 C701 1.414(8) . ? O7 C704 1.419(9) . ? O7 Li4 1.92(2) . ? O7 Li4' 2.08(2) . ? C701 C702 1.529(8) . ? C702 C703 1.490(9) . ? C703 C704 1.472(10) . ? C704 Li4 2.78(2) . ? O8 C8A1 1.399(13) . ? O8 C804 1.427(13) . ? O8 C8A4 1.448(11) . ? O8 C801 1.462(12) . ? O8 Li4 1.93(2) . ? O8 Li4' 1.99(2) . ? C801 C802 1.497(13) . ? C801 Li4 2.64(3) . ? C802 C803 1.484(15) . ? C803 C804 1.501(15) . ? C8A1 C8A2 1.517(14) . ? C8A2 C8A3 1.511(15) . ? C8A3 C8A4 1.498(14) . ? Li4' O9 1.97(2) . ? O9 C904 1.408(13) . ? O9 C901 1.437(12) . ? C901 C902 1.490(12) . ? C902 C903 1.492(14) . ? C903 C904 1.480(12) . ? 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 N4 P1 N3 101.3(2) . . ? N4 P1 N1 116.1(2) . . ? N3 P1 N1 113.8(2) . . ? N4 P1 N2 114.2(2) . . ? N3 P1 N2 115.7(2) . . ? N1 P1 N2 96.7(2) . . ? N4 P1 Li1 49.7(2) . . ? N3 P1 Li1 51.6(2) . . ? N1 P1 Li1 132.4(3) . . ? N2 P1 Li1 130.9(3) . . ? C11 N1 P1 128.1(4) . . ? C16 C11 C12 118.4(5) . . ? C16 C11 N1 118.5(5) . . ? C12 C11 N1 123.1(5) . . ? C13 C12 C11 120.5(6) . . ? C12 C13 C14 120.0(7) . . ? C15 C14 C13 120.3(6) . . ? C14 C15 C16 120.4(7) . . ? C11 C16 C15 120.4(6) . . ? C21 N2 P1 127.8(3) . . ? C26 C21 N2 122.6(5) . . ? C26 C21 C22 118.9(5) . . ? N2 C21 C22 118.5(5) . . ? C23 C22 C21 119.3(6) . . ? C22 C23 C24 122.3(6) . . ? C25 C24 C23 118.3(6) . . ? C24 C25 C26 121.0(6) . . ? C21 C26 C25 120.2(6) . . ? C31 N3 P1 125.1(4) . . ? C31 N3 Li1 143.7(4) . . ? P1 N3 Li1 91.2(3) . . ? C36 C31 N3 117.6(5) . . ? C36 C31 C32 116.7(5) . . ? N3 C31 C32 125.7(5) . . ? C33 C32 C31 121.4(6) . . ? C34 C33 C32 120.8(7) . . ? C35 C34 C33 118.5(7) . . ? C34 C35 C36 122.2(7) . . ? C31 C36 C35 120.4(6) . . ? C41 N4 P1 126.3(4) . . ? C41 N4 Li1 140.6(4) . . ? P1 N4 Li1 93.1(3) . . ? C46 C41 N4 126.5(5) . . ? C46 C41 C42 116.4(5) . . ? N4 C41 C42 117.1(5) . . ? C43 C42 C41 120.2(6) . . ? C44 C43 C42 122.2(6) . . ? C43 C44 C45 118.0(6) . . ? C46 C45 C44 121.7(7) . . ? C45 C46 C41 121.4(6) . . ? O1 Li1 O2 107.3(5) . . ? O1 Li1 N4 121.5(5) . . ? O2 Li1 N4 112.3(5) . . ? O1 Li1 N3 115.4(4) . . ? O2 Li1 N3 123.7(5) . . ? N4 Li1 N3 74.4(3) . . ? O1 Li1 P1 126.2(4) . . ? O2 Li1 P1 126.3(4) . . ? N4 Li1 P1 37.2(2) . . ? N3 Li1 P1 37.28(19) . . ? C101 O1 C104 109.7(4) . . ? C101 O1 Li1 125.4(4) . . ? C104 O1 Li1 124.3(4) . . ? O1 C101 C102 106.6(5) . . ? C103 C102 C101 107.1(6) . . ? C102 C103 C104 104.0(6) . . ? O1 C104 C103 106.5(5) . . ? C2A4 O2 C204 41.5(8) . . ? C2A4 O2 C2A1 85.0(13) . . ? C204 O2 C2A1 100.5(10) . . ? C2A4 O2 C201 107.1(9) . . ? C204 O2 C201 111.0(7) . . ? C2A1 O2 C201 23.9(11) . . ? C2A4 O2 Li1 129.1(8) . . ? C204 O2 Li1 125.1(6) . . ? C2A1 O2 Li1 134.4(9) . . ? C201 O2 Li1 119.4(6) . . ? O2 C201 C202 104.8(8) . . ? C203 C202 C201 102.2(9) . . ? C202 C203 C204 100.3(9) . . ? O2 C204 C203 98.1(9) . . ? O2 C2A1 C2A2 104.9(13) . . ? O2 C2A1 C2A4 47.0(8) . . ? C2A2 C2A1 C2A4 77.6(11) . . ? C2A1 C2A2 C2A3 103.5(13) . . ? C2A2 C2A3 C2A4 90.5(13) . . ? O2 C2A4 C2A3 103.2(13) . . ? O2 C2A4 C2A1 48.0(8) . . ? C2A3 C2A4 C2A1 85.5(10) . . ? N8 P2 N7 101.3(3) . . ? N8 P2 N5 115.5(2) . . ? N7 P2 N5 114.8(2) . . ? N8 P2 N6 115.1(2) . . ? N7 P2 N6 114.6(2) . . ? N5 P2 N6 96.4(2) . . ? N8 P2 Li2 51.4(4) . . ? N7 P2 Li2 49.9(4) . . ? N5 P2 Li2 133.9(4) . . ? N6 P2 Li2 129.7(4) . . ? C51 N5 P2 127.3(4) . . ? C56 C51 C52 117.3(5) . . ? C56 C51 N5 123.0(5) . . ? C52 C51 N5 119.7(5) . . ? C51 C52 C53 121.5(6) . . ? C54 C53 C52 120.6(6) . . ? C53 C54 C55 118.2(6) . . ? C56 C55 C54 121.6(7) . . ? C55 C56 C51 120.7(6) . . ? C61 N6 P2 127.6(4) . . ? C66 C61 C62 118.3(5) . . ? C66 C61 N6 119.7(5) . . ? C62 C61 N6 122.0(5) . . ? C63 C62 C61 120.4(5) . . ? C62 C63 C64 121.0(5) . . ? C65 C64 C63 118.5(5) . . ? C66 C65 C64 121.0(5) . . ? C65 C66 C61 120.8(5) . . ? C71' N7 C71 13.9(8) . . ? C71' N7 P2 134.7(7) . . ? C71 N7 P2 121.8(5) . . ? C71' N7 Li2 132.3(8) . . ? C71 N7 Li2 144.6(6) . . ? P2 N7 Li2 93.0(5) . . ? C72 C71 C76 118.3(11) . . ? C72 C71 N7 125.7(8) . . ? C76 C71 N7 116.0(10) . . ? C73 C72 C71 119.0(11) . . ? C74 C73 C72 122.1(11) . . ? C73 C74 C75 120.3(11) . . ? C74 C75 C76 118.4(10) . . ? C75 C76 C71 121.8(11) . . ? N7 C71' C76' 121.1(12) . . ? N7 C71' C72' 123.7(10) . . ? C76' C71' C72' 115.2(12) . . ? C73' C72' C71' 122.6(13) . . ? C74' C73' C72' 121.3(13) . . ? C73' C74' C75' 118.4(12) . . ? C74' C75' C76' 120.6(12) . . ? C75' C76' C71' 121.9(12) . . ? C81 N8 P2 140.7(6) . . ? C81 N8 C81' 26.9(6) . . ? P2 N8 C81' 116.1(5) . . ? C81 N8 Li2 125.3(7) . . ? P2 N8 Li2 91.6(5) . . ? C81' N8 Li2 152.0(6) . . ? N8 C81 C86 125.0(10) . . ? N8 C81 C82 118.5(9) . . ? C86 C81 C82 116.3(9) . . ? C81 C82 C83 120.2(10) . . ? C84 C83 C82 120.3(13) . . ? C85 C84 C83 121.3(14) . . ? C84 C85 C86 117.8(12) . . ? C81 C86 C85 124.0(11) . . ? C82' C81' C86' 119.0(12) . . ? C82' C81' N8 128.3(9) . . ? C86' C81' N8 112.6(10) . . ? C81' C82' C83' 120.9(11) . . ? C84' C83' C82' 118.6(12) . . ? C85' C84' C83' 120.7(16) . . ? C84' C85' C86' 122.4(16) . . ? C81' C86' C85' 118.1(12) . . ? O3 Li2 O4 102.9(7) . . ? O3 Li2 N7 125.2(8) . . ? O4 Li2 N7 117.1(7) . . ? O3 Li2 N8 119.7(8) . . ? O4 Li2 N8 117.0(7) . . ? N7 Li2 N8 74.0(5) . . ? O3 Li2 P2 133.3(7) . . ? O4 Li2 P2 123.6(7) . . ? N7 Li2 P2 37.1(3) . . ? N8 Li2 P2 37.0(3) . . ? C3A1 O3 C301 44.4(14) . . ? C3A1 O3 C304 98.5(14) . . ? C301 O3 C304 109.4(7) . . ? C3A1 O3 C3A4 102.1(15) . . ? C301 O3 C3A4 63.8(12) . . ? C304 O3 C3A4 77.5(11) . . ? C3A1 O3 Li2 127.9(10) . . ? C301 O3 Li2 126.5(7) . . ? C304 O3 Li2 123.0(7) . . ? C3A4 O3 Li2 115.6(11) . . ? O3 C301 C302 107.9(9) . . ? C301 C302 C303 102.6(9) . . ? C304 C303 C302 103.4(9) . . ? O3 C304 C303 105.5(9) . . ? O3 C3A1 C3A2 101.2(14) . . ? C3A1 C3A2 C3A3 105.2(14) . . ? C3A4 C3A3 C3A2 103.8(14) . . ? C3A3 C3A4 O3 98.6(13) . . ? C401 O4 C4A4 115.0(11) . . ? C401 O4 C404 112.0(12) . . ? C4A4 O4 C404 14(2) . . ? C401 O4 C4A1 16.5(18) . . ? C4A4 O4 C4A1 108.9(8) . . ? C404 O4 C4A1 102.3(11) . . ? C401 O4 Li2 119.8(9) . . ? C4A4 O4 Li2 122.8(8) . . ? C404 O4 Li2 128.2(10) . . ? C4A1 O4 Li2 128.3(8) . . ? O4 C401 C402 105.6(12) . . ? C403 C402 C401 107.1(12) . . ? C402 C403 C404 106.8(13) . . ? O4 C404 C403 107.0(13) . . ? O4 C4A1 C4A2 103.5(9) . . ? C4A3 C4A2 C4A1 108.0(9) . . ? C4A2 C4A3 C4A4 108.3(10) . . ? O4 C4A4 C4A3 107.1(9) . . ? O5 Li3 O6 105.0(6) . . ? O5 Li3 Cl1 113.6(5) . . ? O6 Li3 Cl1 109.8(6) . . ? O5 Li3 Cl2 111.6(6) . . ? O6 Li3 Cl2 111.3(5) . . ? Cl1 Li3 Cl2 105.6(4) . . ? O5 Li3 Li4 131.9(7) . . ? O6 Li3 Li4 123.0(6) . . ? Cl1 Li3 Li4 51.7(4) . . ? Cl2 Li3 Li4 53.9(4) . . ? C501 O5 C5A1 28.3(8) . . ? C501 O5 C504 102.9(8) . . ? C5A1 O5 C504 109.1(8) . . ? C501 O5 C5A4 109.6(8) . . ? C5A1 O5 C5A4 95.5(10) . . ? C504 O5 C5A4 41.6(6) . . ? C501 O5 Li3 131.0(7) . . ? C5A1 O5 Li3 133.2(7) . . ? C504 O5 Li3 117.7(6) . . ? C5A4 O5 Li3 118.8(6) . . ? O5 C501 C502 101.6(10) . . ? C503 C502 C501 101.8(10) . . ? C502 C503 C504 104.4(10) . . ? O5 C504 C503 96.0(9) . . ? O5 C5A1 C5A2 103.8(10) . . ? C5A3 C5A2 C5A1 103.5(11) . . ? C5A4 C5A3 C5A2 101.3(11) . . ? C5A3 C5A4 O5 98.9(10) . . ? C6A1 O6 C601 39.5(8) . . ? C6A1 O6 C604 115.3(8) . . ? C601 O6 C604 102.3(9) . . ? C6A1 O6 C6A4 86.8(13) . . ? C601 O6 C6A4 103.0(11) . . ? C604 O6 C6A4 45.5(13) . . ? C6A1 O6 Li3 124.2(7) . . ? C601 O6 Li3 141.0(8) . . ? C604 O6 Li3 114.4(7) . . ? C6A4 O6 Li3 111.7(9) . . ? O6 C601 C602 100.8(11) . . ? C603 C602 C601 102.3(12) . . ? C604 C603 C602 104.5(13) . . ? O6 C604 C603 98.5(11) . . ? O6 C6A1 C6A2 103.3(12) . . ? O6 C6A1 C6A4 49.2(9) . . ? C6A2 C6A1 C6A4 79.7(9) . . ? C6A3 C6A2 C6A1 97.7(12) . . ? C6A4 C6A3 C6A2 101.0(13) . . ? C6A3 C6A4 O6 104.3(14) . . ? C6A3 C6A4 C6A1 81.4(11) . . ? O6 C6A4 C6A1 43.9(7) . . ? Li3 Cl1 Li4 79.2(5) . . ? Li4' Cl2 Li3 105.6(6) . . ? Li4' Cl2 Li4 28.5(6) . . ? Li3 Cl2 Li4 77.2(5) . . ? C701 O7 C704 108.6(6) . . ? C701 O7 Li4 138.3(8) . . ? C704 O7 Li4 111.5(8) . . ? C701 O7 Li4' 107.1(8) . . ? C704 O7 Li4' 144.4(8) . . ? Li4 O7 Li4' 34.2(7) . . ? O7 C701 C702 106.2(6) . . ? C703 C702 C701 103.1(6) . . ? C704 C703 C702 104.0(7) . . ? O7 C704 C703 103.4(7) . . ? O7 C704 Li4 40.1(5) . . ? C703 C704 Li4 127.4(8) . . ? C8A1 O8 C804 102.4(10) . . ? C8A1 O8 C8A4 111.5(9) . . ? C804 O8 C8A4 11.9(13) . . ? C8A1 O8 C801 15.5(13) . . ? C804 O8 C801 106.4(10) . . ? C8A4 O8 C801 113.0(9) . . ? C8A1 O8 Li4 114.2(15) . . ? C804 O8 Li4 128.0(14) . . ? C8A4 O8 Li4 116.2(12) . . ? C801 O8 Li4 101.3(12) . . ? C8A1 O8 Li4' 128.3(10) . . ? C804 O8 Li4' 129.3(12) . . ? C8A4 O8 Li4' 119.8(10) . . ? C801 O8 Li4' 122.5(10) . . ? Li4 O8 Li4' 35.1(8) . . ? O8 C801 C802 107.9(10) . . ? O8 C801 Li4 45.8(8) . . ? C802 C801 Li4 127.5(15) . . ? C803 C802 C801 101.7(11) . . ? C802 C803 C804 103.2(12) . . ? O8 C804 C803 107.4(11) . . ? O8 C8A1 C8A2 103.8(11) . . ? C8A3 C8A2 C8A1 103.3(11) . . ? C8A4 C8A3 C8A2 101.4(11) . . ? O8 C8A4 C8A3 105.7(10) . . ? O7 Li4 O8 114.2(10) . . ? O7 Li4 Cl1 116.8(9) . . ? O8 Li4 Cl1 103.8(8) . . ? O7 Li4 Cl2 111.6(9) . . ? O8 Li4 Cl2 111.4(9) . . ? Cl1 Li4 Cl2 97.8(7) . . ? O7 Li4 C801 95.6(8) . . ? O8 Li4 C801 32.9(6) . . ? Cl1 Li4 C801 90.1(9) . . ? Cl2 Li4 C801 143.9(9) . . ? O7 Li4 C704 28.4(4) . . ? O8 Li4 C704 114.8(8) . . ? Cl1 Li4 C704 90.4(7) . . ? Cl2 Li4 C704 129.4(8) . . ? C801 Li4 C704 85.5(7) . . ? O7 Li4 Li3 126.3(9) . . ? O8 Li4 Li3 119.5(8) . . ? Cl1 Li4 Li3 49.0(4) . . ? Cl2 Li4 Li3 48.8(4) . . ? C801 Li4 Li3 129.6(9) . . ? C704 Li4 Li3 117.3(7) . . ? O9 Li4' O8 100.5(10) . . ? O9 Li4' O7 117.3(10) . . ? O8 Li4' O7 105.3(10) . . ? O9 Li4' Cl2 100.7(9) . . ? O8 Li4' Cl2 118.2(10) . . ? O7 Li4' Cl2 114.6(10) . . ? C904 O9 C901 106.3(9) . . ? C904 O9 Li4' 116.7(10) . . ? C901 O9 Li4' 118.0(9) . . ? O9 C901 C902 105.8(10) . . ? C901 C902 C903 103.1(10) . . ? C904 C903 C902 99.1(10) . . ? O9 C904 C903 110.0(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Cl1 0.88 2.36 3.233(4) 170.2 . N2 H2 Cl1 0.88 2.37 3.240(4) 168.5 . N5 H5 Cl2 0.88 2.42 3.276(4) 164.4 . N6 H6 Cl2 0.88 2.43 3.297(4) 168.0 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.333 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.044 #===END data_3Li2Clthf6 _database_code_depnum_ccdc_archive 'CCDC 229163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H140 Cl2 Li4 N8 O12 P2' _chemical_formula_weight 1758.76 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.135(7) _cell_length_b 13.475(7) _cell_length_c 15.345(8) _cell_angle_alpha 107.012(9) _cell_angle_beta 105.860(9) _cell_angle_gamma 90.125(9) _cell_volume 2488(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.158 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART 1000' _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 16519 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 22.49 _reflns_number_total 12350 _reflns_number_gt 8772 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1651P)^2^+3.7687P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.63(14) _refine_ls_number_reflns 12350 _refine_ls_number_parameters 1117 _refine_ls_number_restraints 1599 _refine_ls_R_factor_all 0.1332 _refine_ls_R_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.2791 _refine_ls_wR_factor_gt 0.2457 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.65354(17) 0.59634(17) 1.35399(15) 0.0405(6) Uani 1 1 d . . . N1 N 0.7527(6) 0.6571(5) 1.4383(4) 0.0443(18) Uani 1 1 d . . . C11 C 0.8542(7) 0.6731(7) 1.4350(6) 0.048(2) Uani 1 1 d . . . C12 C 0.8943(8) 0.6332(8) 1.3560(8) 0.060(3) Uani 1 1 d . . . H12 H 0.8477 0.5911 1.2975 0.072 Uiso 1 1 calc R . . C13 C 0.9984(10) 0.6538(9) 1.3618(10) 0.082(4) Uani 1 1 d . . . H13 H 1.0230 0.6268 1.3074 0.098 Uiso 1 1 calc R . . C14 C 1.0669(9) 0.7128(10) 1.4454(11) 0.092(4) Uani 1 1 d . . . H14 H 1.1390 0.7270 1.4488 0.110 Uiso 1 1 calc R . . C15 C 1.0328(9) 0.7524(10) 1.5257(9) 0.077(3) Uani 1 1 d . . . H15 H 1.0814 0.7920 1.5841 0.092 Uiso 1 1 calc R . . C16 C 0.9311(8) 0.7345(7) 1.5203(7) 0.061(3) Uani 1 1 d . . . H16 H 0.9084 0.7637 1.5754 0.074 Uiso 1 1 calc R . . N2 N 0.5636(6) 0.6085(6) 1.4093(5) 0.0453(18) Uani 1 1 d . . . C21 C 0.4595(7) 0.5736(7) 1.3744(6) 0.046(2) Uani 1 1 d . . . C22 C 0.4058(7) 0.5215(7) 1.2756(6) 0.051(2) Uani 1 1 d . . . H22 H 0.4434 0.5070 1.2291 0.061 Uiso 1 1 calc R . . C23 C 0.2983(8) 0.4934(8) 1.2507(8) 0.059(3) Uani 1 1 d . . . H23 H 0.2628 0.4606 1.1853 0.070 Uiso 1 1 calc R . . C24 C 0.2392(8) 0.5099(9) 1.3142(8) 0.067(3) Uani 1 1 d . . . H24 H 0.1655 0.4878 1.2935 0.081 Uiso 1 1 calc R . . C25 C 0.2898(8) 0.5592(9) 1.4083(8) 0.063(3) Uani 1 1 d . . . H25 H 0.2497 0.5726 1.4529 0.075 Uiso 1 1 calc R . . C26 C 0.3953(9) 0.5891(8) 1.4394(7) 0.060(3) Uani 1 1 d . . . H26 H 0.4279 0.6210 1.5055 0.072 Uiso 1 1 calc R . . N3 N 0.6247(5) 0.6383(5) 1.2574(5) 0.0447(17) Uani 1 1 d . . . H3 H 0.6257 0.5921 1.2037 0.054 Uiso 1 1 calc R . . C31 C 0.6000(6) 0.7349(6) 1.2524(6) 0.040(2) Uani 1 1 d . . . C32 C 0.6288(8) 0.8232(7) 1.3329(7) 0.058(3) Uani 1 1 d . . . H32 H 0.6647 0.8173 1.3938 0.070 Uiso 1 1 calc R . . C33 C 0.6034(9) 0.9191(9) 1.3214(9) 0.076(3) Uani 1 1 d . . . H33 H 0.6248 0.9790 1.3757 0.091 Uiso 1 1 calc R . . C34 C 0.5497(9) 0.9324(8) 1.2369(9) 0.074(3) Uani 1 1 d . . . H34 H 0.5321 0.9991 1.2317 0.089 Uiso 1 1 calc R . . C35 C 0.5225(9) 0.8451(10) 1.1600(10) 0.083(4) Uani 1 1 d . . . H35 H 0.4862 0.8517 1.0996 0.099 Uiso 1 1 calc R . . C36 C 0.5453(8) 0.7498(8) 1.1669(8) 0.062(3) Uani 1 1 d . . . H36 H 0.5232 0.6912 1.1116 0.074 Uiso 1 1 calc R . . N4 N 0.6684(6) 0.4733(6) 1.2978(5) 0.0505(19) Uani 1 1 d . . . H4 H 0.6618 0.4583 1.2366 0.061 Uiso 1 1 calc R . . C41 C 0.6901(6) 0.3911(7) 1.3368(6) 0.040(2) Uani 1 1 d . . . C42 C 0.6835(7) 0.2902(6) 1.2769(7) 0.044(2) Uani 1 1 d . . . H42 H 0.6643 0.2779 1.2101 0.053 Uiso 1 1 calc R . . C43 C 0.7037(10) 0.2102(9) 1.3116(10) 0.075(3) Uani 1 1 d . . . H43 H 0.6969 0.1418 1.2688 0.090 Uiso 1 1 calc R . . C44 C 0.7346(12) 0.2243(9) 1.4096(10) 0.089(4) Uani 1 1 d . . . H44 H 0.7491 0.1666 1.4334 0.107 Uiso 1 1 calc R . . C45 C 0.7439(10) 0.3273(9) 1.4727(8) 0.075(3) Uani 1 1 d . . . H45 H 0.7643 0.3397 1.5396 0.090 Uiso 1 1 calc R . . C46 C 0.7230(9) 0.4081(8) 1.4356(7) 0.064(3) Uani 1 1 d . . . H46 H 0.7308 0.4772 1.4774 0.077 Uiso 1 1 calc R . . P2 P 0.41019(16) 0.34497(17) 0.78491(14) 0.0385(6) Uani 1 1 d . . . N5 N 0.3456(5) 0.2447(5) 0.7023(4) 0.0422(18) Uani 1 1 d . . . C51 C 0.3323(6) 0.1443(7) 0.7081(6) 0.044(2) Uani 1 1 d . . . C52 C 0.2724(8) 0.0687(8) 0.6234(7) 0.064(3) Uani 1 1 d . . . H52 H 0.2427 0.0873 0.5671 0.077 Uiso 1 1 calc R . . C53 C 0.2579(10) -0.0337(9) 0.6243(11) 0.081(4) Uani 1 1 d . . . H53 H 0.2210 -0.0850 0.5667 0.097 Uiso 1 1 calc R . . C54 C 0.2938(10) -0.0626(9) 0.7031(10) 0.077(3) Uani 1 1 d . . . H54 H 0.2793 -0.1319 0.7026 0.093 Uiso 1 1 calc R . . C55 C 0.3534(8) 0.0127(9) 0.7860(9) 0.067(3) Uani 1 1 d . . . H55 H 0.3815 -0.0065 0.8422 0.080 Uiso 1 1 calc R . . C56 C 0.3721(7) 0.1139(7) 0.7879(7) 0.052(2) Uani 1 1 d . . . H56 H 0.4131 0.1634 0.8451 0.062 Uiso 1 1 calc R . . N6 N 0.3938(5) 0.4291(5) 0.7307(5) 0.0460(18) Uani 1 1 d . . . C61 C 0.4265(7) 0.5349(7) 0.7668(6) 0.045(2) Uani 1 1 d . . . C62 C 0.4002(9) 0.5946(7) 0.7038(7) 0.062(3) Uani 1 1 d . . . H62 H 0.3615 0.5614 0.6393 0.075 Uiso 1 1 calc R . . C63 C 0.4286(13) 0.6982(11) 0.7327(11) 0.096(4) Uani 1 1 d . . . H63 H 0.4108 0.7364 0.6882 0.115 Uiso 1 1 calc R . . C64 C 0.4835(14) 0.7490(10) 0.8263(12) 0.105(5) Uani 1 1 d . . . H64 H 0.5013 0.8221 0.8462 0.126 Uiso 1 1 calc R . . C65 C 0.5119(9) 0.6956(8) 0.8894(7) 0.070(3) Uani 1 1 d . . . H65 H 0.5507 0.7317 0.9532 0.084 Uiso 1 1 calc R . . C66 C 0.4858(8) 0.5884(7) 0.8636(7) 0.057(3) Uani 1 1 d . . . H66 H 0.5068 0.5516 0.9089 0.068 Uiso 1 1 calc R . . N7 N 0.5378(5) 0.3288(5) 0.8359(5) 0.0419(17) Uani 1 1 d . . . H7 H 0.5568 0.3410 0.8980 0.050 Uiso 1 1 calc R . . C71 C 0.6148(7) 0.2988(7) 0.7912(6) 0.043(2) Uani 1 1 d . . . C72 C 0.5919(8) 0.2614(8) 0.6922(7) 0.059(3) Uani 1 1 d . . . H72 H 0.5210 0.2571 0.6534 0.070 Uiso 1 1 calc R . . C73 C 0.6729(8) 0.2303(9) 0.6503(8) 0.066(3) Uani 1 1 d . . . H73 H 0.6558 0.2008 0.5832 0.080 Uiso 1 1 calc R . . C74 C 0.7764(9) 0.2414(11) 0.7037(9) 0.082(4) Uani 1 1 d . . . H74 H 0.8315 0.2269 0.6737 0.099 Uiso 1 1 calc R . . C75 C 0.7999(9) 0.2729(10) 0.7989(10) 0.081(4) Uani 1 1 d . . . H75 H 0.8710 0.2742 0.8362 0.098 Uiso 1 1 calc R . . C76 C 0.7201(7) 0.3040(8) 0.8440(7) 0.058(3) Uani 1 1 d . . . H76 H 0.7386 0.3290 0.9115 0.070 Uiso 1 1 calc R . . N8 N 0.3706(6) 0.3749(5) 0.8837(5) 0.0453(18) Uani 1 1 d . . . H8 H 0.4186 0.3759 0.9368 0.054 Uiso 1 1 calc R . . C81 C 0.2665(7) 0.3990(7) 0.8901(6) 0.044(2) Uani 1 1 d . . . C82 C 0.2561(7) 0.4551(8) 0.9784(6) 0.053(2) Uani 1 1 d . . . H82 H 0.3167 0.4753 1.0326 0.063 Uiso 1 1 calc R . . C83 C 0.1575(9) 0.4810(9) 0.9867(8) 0.072(3) Uani 1 1 d . . . H83 H 0.1504 0.5226 1.0462 0.087 Uiso 1 1 calc R . . C84 C 0.0654(9) 0.4459(10) 0.9066(8) 0.075(3) Uani 1 1 d . . . H84 H -0.0036 0.4600 0.9127 0.090 Uiso 1 1 calc R . . C85 C 0.0791(8) 0.3933(10) 0.8239(8) 0.076(3) Uani 1 1 d . . . H85 H 0.0186 0.3718 0.7698 0.091 Uiso 1 1 calc R . . C86 C 0.1790(7) 0.3679(8) 0.8122(7) 0.059(3) Uani 1 1 d . . . H86 H 0.1859 0.3298 0.7516 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.5874(2) 0.4348(2) 1.06648(16) 0.0671(8) Uani 1 1 d . . . Cl2 Cl 0.0237(4) 0.9772(3) 0.0816(4) 0.1219(14) Uani 1 1 d . . . Li1 Li 0.6642(13) 0.6850(13) 1.5340(11) 0.067(5) Uani 1 1 d . . . Li2 Li 0.3097(12) 0.3286(12) 0.6066(11) 0.061(5) Uani 1 1 d . . . Li3 Li 0.081(2) 1.107(2) 0.0432(16) 0.105(7) Uani 1 1 d . . . Li4 Li 0.093(3) 0.830(3) 0.090(3) 0.169(17) Uani 1 1 d . . . O1 O 0.6136(7) 0.8158(6) 1.5921(5) 0.094(3) Uani 1 1 d DU . . C101 C 0.5217(9) 0.8566(8) 1.5453(8) 0.094(4) Uani 1 1 d DU . . H10A H 0.4572 0.8301 1.5559 0.112 Uiso 1 1 calc R . . H10B H 0.5127 0.8362 1.4760 0.112 Uiso 1 1 calc R . . C102 C 0.5396(12) 0.9703(9) 1.5868(9) 0.104(4) Uani 1 1 d DU . . H10C H 0.4715 1.0022 1.5848 0.125 Uiso 1 1 calc R . . H10D H 0.5790 1.0012 1.5531 0.125 Uiso 1 1 calc R . . C103 C 0.6034(14) 0.9844(9) 1.6857(9) 0.120(6) Uani 1 1 d DU . . H10E H 0.6578 1.0442 1.7078 0.144 Uiso 1 1 calc R . . H10F H 0.5575 0.9970 1.7287 0.144 Uiso 1 1 calc R . . C104 C 0.6535(11) 0.8875(9) 1.6838(7) 0.103(5) Uani 1 1 d DU . . H10G H 0.7316 0.9009 1.6994 0.124 Uiso 1 1 calc R . . H10H H 0.6379 0.8587 1.7316 0.124 Uiso 1 1 calc R . . O2 O 0.7214(5) 0.6322(6) 1.6396(5) 0.071(2) Uani 1 1 d DU . . C201 C 0.6567(10) 0.5740(13) 1.6694(10) 0.112(5) Uani 1 1 d DU . . H20A H 0.6196 0.5128 1.6156 0.135 Uiso 1 1 calc R . . H20B H 0.6024 0.6173 1.6915 0.135 Uiso 1 1 calc R . . C202 C 0.7214(13) 0.5402(16) 1.7455(13) 0.146(7) Uani 1 1 d DU . . H20C H 0.6991 0.4674 1.7384 0.175 Uiso 1 1 calc R . . H20D H 0.7179 0.5856 1.8081 0.175 Uiso 1 1 calc R . . C203 C 0.8283(12) 0.5492(17) 1.7349(16) 0.164(7) Uani 1 1 d DU . . H20E H 0.8432 0.4835 1.6925 0.197 Uiso 1 1 calc R . . H20F H 0.8827 0.5662 1.7975 0.197 Uiso 1 1 calc R . . C204 C 0.8273(8) 0.6347(14) 1.6928(11) 0.118(5) Uani 1 1 d DU . . H20G H 0.8503 0.7025 1.7431 0.142 Uiso 1 1 calc R . . H20H H 0.8750 0.6234 1.6514 0.142 Uiso 1 1 calc R . . O3 O 0.3656(5) 0.2788(5) 0.5005(4) 0.0600(18) Uani 1 1 d DU . . C301 C 0.3474(13) 0.1758(8) 0.4331(8) 0.099(4) Uani 1 1 d DU . . H30A H 0.2712 0.1505 0.4126 0.119 Uiso 1 1 calc R . . H30B H 0.3893 0.1264 0.4618 0.119 Uiso 1 1 calc R . . C302 C 0.3810(18) 0.1852(11) 0.3527(10) 0.145(7) Uani 1 1 d DU . . H30C H 0.4315 0.1327 0.3380 0.175 Uiso 1 1 calc R . . H30D H 0.3187 0.1721 0.2960 0.175 Uiso 1 1 calc R . . C303 C 0.4312(12) 0.2879(9) 0.3754(7) 0.092(4) Uani 1 1 d DU . . H30E H 0.3881 0.3273 0.3355 0.111 Uiso 1 1 calc R . . H30F H 0.5029 0.2847 0.3660 0.111 Uiso 1 1 calc R . . C304 C 0.4379(9) 0.3366(8) 0.4767(6) 0.072(3) Uani 1 1 d DU . . H30G H 0.5111 0.3367 0.5169 0.086 Uiso 1 1 calc R . . H30H H 0.4198 0.4097 0.4875 0.086 Uiso 1 1 calc R . . O4 O 0.1741(6) 0.3781(7) 0.5559(4) 0.097(3) Uani 1 1 d DU . . C401 C 0.1170(8) 0.3526(11) 0.4567(6) 0.087(4) Uani 1 1 d DU . . H40A H 0.0976 0.2766 0.4289 0.104 Uiso 1 1 calc R . . H40B H 0.1608 0.3747 0.4213 0.104 Uiso 1 1 calc R . . C402 C 0.0210(11) 0.4094(15) 0.4526(9) 0.139(7) Uani 1 1 d DU . . H40C H -0.0438 0.3603 0.4225 0.166 Uiso 1 1 calc R . . H40D H 0.0196 0.4587 0.4156 0.166 Uiso 1 1 calc R . . C403 C 0.0272(12) 0.4669(18) 0.5536(9) 0.155(8) Uani 1 1 d DU . . H40E H 0.0107 0.5399 0.5601 0.186 Uiso 1 1 calc R . . H40F H -0.0237 0.4329 0.5755 0.186 Uiso 1 1 calc R . . C404 C 0.1302(12) 0.4634(14) 0.6056(8) 0.145(7) Uani 1 1 d DU . . H40G H 0.1309 0.4566 0.6683 0.174 Uiso 1 1 calc R . . H40H H 0.1730 0.5287 0.6164 0.174 Uiso 1 1 calc R . . O5 O 0.0415(6) 1.0906(7) -0.0936(5) 0.092(3) Uani 1 1 d DU . . C501 C -0.0487(10) 1.0297(12) -0.1663(8) 0.106(5) Uani 1 1 d DU . . H50A H -0.1118 1.0700 -0.1696 0.127 Uiso 1 1 calc R . . H50B H -0.0646 0.9654 -0.1519 0.127 Uiso 1 1 calc R . . C502 C -0.0231(14) 1.0031(13) -0.2572(9) 0.131(6) Uani 1 1 d DU . . H50C H -0.0875 0.9967 -0.3109 0.158 Uiso 1 1 calc R . . H50D H 0.0116 0.9373 -0.2686 0.158 Uiso 1 1 calc R . . C503 C 0.0502(11) 1.0922(12) -0.2438(8) 0.106(4) Uani 1 1 d DU . . H50E H 0.0110 1.1498 -0.2607 0.127 Uiso 1 1 calc R . . H50F H 0.1000 1.0718 -0.2828 0.127 Uiso 1 1 calc R . . C504 C 0.1076(9) 1.1228(13) -0.1401(7) 0.098(4) Uani 1 1 d DU . . H50G H 0.1749 1.0891 -0.1297 0.118 Uiso 1 1 calc R . . H50H H 0.1246 1.1993 -0.1147 0.118 Uiso 1 1 calc R . . O6 O 0.2334(6) 1.1371(6) 0.0781(6) 0.089(2) Uani 1 1 d DU . . C601 C 0.2881(10) 1.2354(8) 0.0971(10) 0.095(4) Uani 1 1 d DU . . H60A H 0.2969 1.2778 0.1639 0.114 Uiso 1 1 calc R . . H60B H 0.2472 1.2734 0.0547 0.114 Uiso 1 1 calc R . . C602 C 0.3907(11) 1.2173(13) 0.0809(14) 0.132(6) Uani 1 1 d DU . . H60C H 0.4457 1.2727 0.1261 0.158 Uiso 1 1 calc R . . H60D H 0.3884 1.2141 0.0151 0.158 Uiso 1 1 calc R . . C603 C 0.4118(9) 1.1161(13) 0.0972(12) 0.124(5) Uani 1 1 d DU . . H60E H 0.4478 1.1252 0.1652 0.149 Uiso 1 1 calc R . . H60F H 0.4566 1.0780 0.0584 0.149 Uiso 1 1 calc R . . C604 C 0.3053(9) 1.0600(8) 0.0677(11) 0.094(4) Uani 1 1 d DU . . H60G H 0.2878 1.0153 0.0007 0.113 Uiso 1 1 calc R . . H60H H 0.3025 1.0156 0.1084 0.113 Uiso 1 1 calc R . . O7 O 0.0275(7) 1.2389(7) 0.1062(6) 0.097(3) Uani 1 1 d DU . . C701 C -0.0280(14) 1.3054(11) 0.0606(10) 0.118(5) Uani 1 1 d DU . . H70A H -0.0805 1.2647 0.0006 0.142 Uiso 1 1 calc R . . H70B H 0.0215 1.3485 0.0451 0.142 Uiso 1 1 calc R . . C702 C -0.0823(18) 1.3722(14) 0.1245(15) 0.196(11) Uani 1 1 d DU . . H70C H -0.0465 1.4437 0.1519 0.235 Uiso 1 1 calc R . . H70D H -0.1573 1.3753 0.0902 0.235 Uiso 1 1 calc R . . C703 C -0.0758(16) 1.3239(18) 0.1980(14) 0.174(9) Uani 1 1 d DU . . H70E H -0.1443 1.2845 0.1869 0.209 Uiso 1 1 calc R . . H70F H -0.0588 1.3774 0.2612 0.209 Uiso 1 1 calc R . . C704 C 0.0076(14) 1.2546(12) 0.1938(8) 0.117(5) Uani 1 1 d DU . . H70G H 0.0727 1.2858 0.2463 0.140 Uiso 1 1 calc R . . H70H H -0.0148 1.1873 0.1999 0.140 Uiso 1 1 calc R . . O8 O 0.1973(9) 0.8293(7) 0.1876(6) 0.130(4) Uani 1 1 d DU . . C801 C 0.2436(15) 0.9229(9) 0.2645(10) 0.138(6) Uani 1 1 d DU . . H80A H 0.1884 0.9712 0.2751 0.165 Uiso 1 1 calc R . . H80B H 0.2992 0.9586 0.2492 0.165 Uiso 1 1 calc R . . C802 C 0.2893(17) 0.8919(10) 0.3486(9) 0.137(6) Uani 1 1 d DU . . H80C H 0.3547 0.9371 0.3891 0.165 Uiso 1 1 calc R . . H80D H 0.2382 0.8966 0.3863 0.165 Uiso 1 1 calc R . . C803 C 0.3132(12) 0.7853(9) 0.3142(9) 0.115(5) Uani 1 1 d DU . . H80E H 0.3000 0.7442 0.3546 0.138 Uiso 1 1 calc R . . H80F H 0.3883 0.7824 0.3134 0.138 Uiso 1 1 calc R . . C804 C 0.2406(16) 0.7457(9) 0.2168(11) 0.157(8) Uani 1 1 d DU . . H80G H 0.2800 0.7070 0.1729 0.188 Uiso 1 1 calc R . . H80H H 0.1830 0.6973 0.2156 0.188 Uiso 1 1 calc R . . O9 O 0.1335(9) 0.7654(11) -0.0327(7) 0.151(5) Uani 1 1 d DU . . C901 C 0.0762(12) 0.774(2) -0.1205(9) 0.174(8) Uani 1 1 d DU . . H90A H 0.0642 0.8485 -0.1139 0.208 Uiso 1 1 calc R . . H90B H 0.0060 0.7343 -0.1417 0.208 Uiso 1 1 calc R . . C902 C 0.1325(15) 0.7360(19) -0.1919(10) 0.160(7) Uani 1 1 d DU . . H90C H 0.0847 0.6892 -0.2518 0.193 Uiso 1 1 calc R . . H90D H 0.1648 0.7940 -0.2056 0.193 Uiso 1 1 calc R . . C903 C 0.2125(15) 0.6802(16) -0.1459(10) 0.147(7) Uani 1 1 d DU . . H90E H 0.2775 0.6822 -0.1664 0.176 Uiso 1 1 calc R . . H90F H 0.1860 0.6066 -0.1607 0.176 Uiso 1 1 calc R . . C904 C 0.2343(11) 0.7360(15) -0.0423(11) 0.148(7) Uani 1 1 d DU . . H90G H 0.2629 0.6896 -0.0037 0.177 Uiso 1 1 calc R . . H90H H 0.2855 0.7980 -0.0225 0.177 Uiso 1 1 calc R . . O10 O -0.0366(11) 0.7289(12) 0.0773(12) 0.159(5) Uani 1 1 d DU . . C911 C -0.0944(18) 0.7784(15) 0.1419(18) 0.206(9) Uani 1 1 d DU . . H91A H -0.0964 0.8530 0.1462 0.247 Uiso 1 1 calc R . . H91B H -0.0585 0.7734 0.2060 0.247 Uiso 1 1 calc R . . C912 C -0.2024(17) 0.728(2) 0.109(2) 0.241(11) Uani 1 1 d DU . . H91C H -0.2289 0.7281 0.1637 0.289 Uiso 1 1 calc R . . H91D H -0.2514 0.7643 0.0694 0.289 Uiso 1 1 calc R . . C913 C -0.192(2) 0.625(2) 0.055(3) 0.275(14) Uani 1 1 d DU . . H91E H -0.2512 0.6023 -0.0044 0.330 Uiso 1 1 calc R . . H91F H -0.1929 0.5762 0.0921 0.330 Uiso 1 1 calc R . . C914 C -0.091(2) 0.6289(17) 0.034(3) 0.264(13) Uani 1 1 d DU . . H91G H -0.0464 0.5776 0.0576 0.317 Uiso 1 1 calc R . . H91H H -0.1034 0.6098 -0.0355 0.317 Uiso 1 1 calc R . . O11 O 0.6581(13) 0.0821(14) 0.0670(11) 0.177(5) Uani 1 1 d DU . . C921 C 0.7118(17) -0.0103(14) 0.0528(12) 0.144(6) Uani 1 1 d DU . . H92A H 0.6661 -0.0698 0.0511 0.173 Uiso 1 1 calc R . . H92B H 0.7781 -0.0013 0.1053 0.173 Uiso 1 1 calc R . . C922 C 0.7363(16) -0.0297(14) -0.0388(13) 0.148(7) Uani 1 1 d DU . . H92C H 0.8066 -0.0573 -0.0356 0.178 Uiso 1 1 calc R . . H92D H 0.6814 -0.0795 -0.0911 0.178 Uiso 1 1 calc R . . C923 C 0.7362(16) 0.0723(17) -0.0513(13) 0.163(8) Uani 1 1 d DU . . H92E H 0.7175 0.0673 -0.1196 0.196 Uiso 1 1 calc R . . H92F H 0.8064 0.1123 -0.0184 0.196 Uiso 1 1 calc R . . C924 C 0.6557(16) 0.1202(15) -0.0088(15) 0.145(6) Uani 1 1 d DU . . H92G H 0.6706 0.1970 0.0142 0.174 Uiso 1 1 calc R . . H92H H 0.5848 0.1024 -0.0562 0.174 Uiso 1 1 calc R . . O12 O 0.9092(17) -0.0476(14) 0.3825(15) 0.214(7) Uani 1 1 d DU . . C931 C 0.932(2) 0.015(2) 0.4782(15) 0.224(11) Uani 1 1 d DU . . H93A H 0.9780 -0.0195 0.5210 0.268 Uiso 1 1 calc R . . H93B H 0.8658 0.0293 0.4968 0.268 Uiso 1 1 calc R . . C932 C 0.987(2) 0.1122(18) 0.4829(18) 0.243(12) Uani 1 1 d DU . . H93C H 0.9363 0.1636 0.4695 0.292 Uiso 1 1 calc R . . H93D H 1.0391 0.1433 0.5461 0.292 Uiso 1 1 calc R . . C933 C 1.041(2) 0.079(2) 0.409(2) 0.208(10) Uani 1 1 d DU . . H93E H 1.1058 0.0451 0.4308 0.249 Uiso 1 1 calc R . . H93F H 1.0594 0.1377 0.3886 0.249 Uiso 1 1 calc R . . C934 C 0.960(3) 0.004(3) 0.3337(16) 0.267(13) Uani 1 1 d DU . . H93G H 0.9079 0.0405 0.2965 0.320 Uiso 1 1 calc R . . H93H H 0.9922 -0.0460 0.2902 0.320 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 P1 0.0458(13) 0.0371(13) 0.0261(11) -0.0009(10) 0.0014(10) 0.0070(10) N1 0.047(5) 0.043(4) 0.020(3) -0.010(3) -0.007(3) 0.006(3) C11 0.054(6) 0.032(5) 0.040(5) -0.003(4) 0.004(4) 0.001(4) C12 0.061(7) 0.050(6) 0.062(7) 0.004(5) 0.019(5) 0.002(5) C13 0.077(9) 0.060(7) 0.100(10) -0.009(7) 0.048(8) -0.002(6) C14 0.049(7) 0.081(9) 0.121(12) 0.018(9) 0.000(8) -0.013(6) C15 0.046(7) 0.084(8) 0.067(8) -0.003(6) -0.008(6) -0.007(6) C16 0.066(7) 0.048(6) 0.048(6) -0.005(5) 0.001(5) -0.013(5) N2 0.042(4) 0.048(4) 0.032(4) -0.007(3) 0.010(3) 0.000(3) C21 0.048(6) 0.041(5) 0.046(5) 0.007(4) 0.013(4) 0.017(4) C22 0.051(6) 0.055(6) 0.030(5) 0.000(4) 0.000(4) -0.006(4) C23 0.048(6) 0.059(6) 0.057(6) 0.016(5) 0.000(5) 0.000(5) C24 0.050(6) 0.077(8) 0.064(7) 0.025(6) -0.005(6) -0.013(5) C25 0.054(7) 0.079(7) 0.060(7) 0.019(6) 0.026(5) 0.016(5) C26 0.076(8) 0.067(7) 0.037(5) 0.007(5) 0.025(5) 0.008(5) N3 0.047(4) 0.040(4) 0.039(4) 0.003(3) 0.010(3) 0.011(3) C31 0.033(4) 0.040(5) 0.039(5) 0.009(4) -0.003(4) 0.011(4) C32 0.069(6) 0.035(6) 0.053(6) 0.006(5) -0.002(5) 0.011(5) C33 0.086(8) 0.055(7) 0.065(8) 0.004(6) 0.002(6) -0.003(6) C34 0.081(8) 0.041(6) 0.091(9) 0.017(6) 0.013(7) 0.018(5) C35 0.077(8) 0.075(9) 0.102(10) 0.041(8) 0.019(7) 0.017(6) C36 0.067(7) 0.054(6) 0.065(7) 0.017(5) 0.020(5) 0.021(5) N4 0.074(5) 0.043(4) 0.019(4) -0.009(3) 0.008(3) 0.000(4) C41 0.038(5) 0.047(6) 0.030(5) 0.004(4) 0.010(4) -0.003(4) C42 0.051(5) 0.034(5) 0.048(5) 0.004(4) 0.024(4) 0.005(4) C43 0.088(8) 0.047(7) 0.092(9) 0.016(7) 0.035(7) -0.005(6) C44 0.138(12) 0.045(7) 0.105(11) 0.022(7) 0.070(9) 0.031(7) C45 0.100(9) 0.060(7) 0.059(7) 0.011(6) 0.019(6) 0.007(6) C46 0.093(8) 0.046(6) 0.055(7) 0.012(5) 0.028(6) 0.009(5) P2 0.0384(12) 0.0403(13) 0.0240(11) -0.0020(10) 0.0013(9) 0.0048(10) N5 0.046(4) 0.034(4) 0.024(4) -0.013(3) -0.003(3) 0.000(3) C51 0.034(5) 0.047(6) 0.036(5) -0.007(4) 0.006(4) -0.001(4) C52 0.060(6) 0.065(7) 0.054(6) -0.007(5) 0.021(5) -0.012(5) C53 0.093(9) 0.045(7) 0.099(10) -0.009(7) 0.051(8) -0.008(6) C54 0.089(9) 0.053(7) 0.095(10) 0.022(7) 0.036(8) 0.006(6) C55 0.053(6) 0.061(7) 0.086(8) 0.022(6) 0.018(6) 0.004(5) C56 0.048(5) 0.042(6) 0.048(6) -0.001(5) 0.004(4) 0.005(4) N6 0.047(4) 0.044(5) 0.028(4) -0.010(3) 0.002(3) 0.002(3) C61 0.051(5) 0.049(6) 0.027(5) 0.000(4) 0.007(4) 0.008(4) C62 0.102(8) 0.034(6) 0.054(6) 0.012(5) 0.028(6) 0.017(5) C63 0.145(13) 0.070(9) 0.088(10) 0.038(8) 0.043(9) 0.033(8) C64 0.165(15) 0.043(7) 0.119(13) 0.014(8) 0.072(12) 0.006(8) C65 0.096(8) 0.053(7) 0.040(6) 0.005(5) -0.005(5) -0.002(6) C66 0.067(6) 0.044(6) 0.046(6) 0.000(5) 0.009(5) 0.005(5) N7 0.041(4) 0.051(4) 0.022(4) 0.000(3) 0.001(3) -0.004(3) C71 0.036(5) 0.057(6) 0.044(5) 0.023(5) 0.014(4) 0.008(4) C72 0.057(6) 0.068(7) 0.047(6) 0.019(5) 0.009(5) 0.009(5) C73 0.048(6) 0.112(9) 0.055(6) 0.043(6) 0.020(5) 0.020(6) C74 0.061(8) 0.135(12) 0.074(9) 0.059(8) 0.027(6) 0.017(7) C75 0.054(7) 0.101(9) 0.106(11) 0.046(8) 0.034(7) 0.005(6) C76 0.048(6) 0.082(7) 0.039(5) 0.018(5) 0.002(5) -0.001(5) N8 0.053(5) 0.047(4) 0.024(4) -0.005(3) 0.009(3) 0.006(3) C81 0.042(5) 0.041(5) 0.041(5) 0.003(4) 0.007(4) 0.012(4) C82 0.049(6) 0.070(6) 0.027(5) -0.001(4) 0.009(4) 0.009(5) C83 0.084(8) 0.081(8) 0.045(6) 0.001(6) 0.026(6) 0.020(6) C84 0.066(7) 0.097(9) 0.068(8) 0.020(7) 0.034(6) 0.037(6) C85 0.052(7) 0.105(9) 0.058(7) 0.015(7) 0.003(5) 0.002(6) C86 0.040(6) 0.075(7) 0.056(6) 0.012(5) 0.012(5) 0.006(5) Cl1 0.0826(18) 0.0652(17) 0.0286(12) -0.0058(11) -0.0026(11) 0.0077(13) Cl2 0.117(3) 0.097(3) 0.180(4) 0.060(3) 0.068(3) 0.024(2) Li1 0.062(10) 0.059(10) 0.049(10) -0.021(8) 0.008(8) 0.027(8) Li2 0.056(9) 0.052(9) 0.039(9) -0.016(7) -0.012(7) 0.020(8) Li3 0.104(17) 0.14(2) 0.068(14) 0.028(14) 0.021(12) -0.001(14) Li4 0.20(4) 0.16(3) 0.24(4) 0.12(3) 0.15(4) 0.09(3) O1 0.112(6) 0.067(5) 0.053(4) -0.025(4) -0.009(4) 0.047(4) C101 0.089(9) 0.083(8) 0.067(8) -0.007(7) -0.013(7) 0.017(7) C102 0.106(10) 0.076(8) 0.095(10) -0.001(7) -0.001(8) 0.006(7) C103 0.152(13) 0.066(8) 0.096(10) -0.004(7) -0.009(9) 0.031(8) C104 0.122(11) 0.075(9) 0.061(8) -0.030(7) -0.001(7) 0.012(8) O2 0.070(5) 0.087(5) 0.043(4) 0.006(4) 0.007(3) 0.012(4) C201 0.106(10) 0.146(13) 0.083(9) 0.031(9) 0.027(8) -0.025(10) C202 0.169(16) 0.179(16) 0.127(13) 0.101(12) 0.042(12) -0.020(13) C203 0.111(12) 0.219(18) 0.186(16) 0.146(14) -0.008(12) 0.006(13) C204 0.054(7) 0.189(15) 0.118(11) 0.095(11) -0.016(7) -0.013(8) O3 0.080(5) 0.050(4) 0.039(4) -0.007(3) 0.021(3) 0.000(3) C301 0.163(12) 0.063(8) 0.085(9) 0.004(7) 0.077(9) -0.011(8) C302 0.252(18) 0.107(11) 0.088(10) -0.006(9) 0.104(11) -0.054(12) C303 0.130(11) 0.089(9) 0.061(7) 0.013(7) 0.043(7) -0.026(8) C304 0.093(8) 0.063(7) 0.052(6) 0.019(5) 0.009(6) -0.003(6) O4 0.084(5) 0.139(7) 0.036(4) 0.001(4) -0.009(4) 0.067(5) C401 0.060(7) 0.120(10) 0.048(6) 0.002(6) -0.012(5) -0.003(7) C402 0.085(10) 0.183(15) 0.098(11) 0.019(11) -0.029(8) 0.052(10) C403 0.139(13) 0.187(16) 0.080(10) -0.017(11) -0.002(10) 0.078(12) C404 0.104(10) 0.208(16) 0.061(8) -0.016(9) -0.013(8) 0.094(11) O5 0.082(6) 0.113(7) 0.070(5) 0.011(5) 0.024(4) -0.017(5) C501 0.082(9) 0.128(11) 0.096(10) 0.012(9) 0.031(8) -0.018(8) C502 0.139(13) 0.135(13) 0.090(11) -0.013(10) 0.035(10) 0.001(11) C503 0.092(9) 0.126(12) 0.082(9) 0.006(8) 0.026(8) 0.011(8) C504 0.083(8) 0.141(12) 0.074(8) 0.042(8) 0.020(7) -0.027(8) O6 0.089(6) 0.076(6) 0.101(6) 0.025(5) 0.028(5) -0.004(4) C601 0.096(10) 0.081(9) 0.092(9) 0.018(7) 0.009(8) -0.004(7) C602 0.102(11) 0.161(15) 0.143(13) 0.067(12) 0.032(10) -0.027(11) C603 0.075(9) 0.178(16) 0.118(12) 0.066(11) 0.003(8) 0.024(10) C604 0.100(10) 0.075(8) 0.123(11) 0.035(8) 0.052(8) 0.040(7) O7 0.109(7) 0.111(7) 0.093(6) 0.041(6) 0.054(5) 0.020(5) C701 0.181(15) 0.082(9) 0.114(11) 0.048(9) 0.059(11) 0.015(10) C702 0.179(16) 0.112(13) 0.20(2) -0.027(14) -0.013(16) 0.086(12) C703 0.121(13) 0.23(2) 0.152(16) -0.017(15) 0.081(13) 0.040(13) C704 0.174(15) 0.100(10) 0.069(9) 0.002(8) 0.049(9) 0.000(10) O8 0.150(9) 0.088(7) 0.084(6) -0.010(5) -0.036(6) 0.032(6) C801 0.166(15) 0.085(10) 0.109(12) -0.006(9) -0.009(11) 0.001(10) C802 0.194(16) 0.092(11) 0.101(11) 0.032(9) -0.002(11) 0.030(10) C803 0.120(11) 0.073(9) 0.108(11) 0.000(8) -0.007(9) 0.004(8) C804 0.206(16) 0.045(8) 0.141(13) -0.013(8) -0.030(12) 0.039(9) O9 0.120(8) 0.199(12) 0.091(8) -0.013(8) 0.024(6) 0.053(8) C901 0.093(10) 0.32(2) 0.057(9) 0.007(12) -0.009(8) 0.069(12) C902 0.151(15) 0.24(2) 0.077(10) 0.020(12) 0.035(11) 0.043(14) C903 0.142(13) 0.189(17) 0.095(11) 0.006(11) 0.051(10) 0.079(12) C904 0.101(11) 0.137(14) 0.165(15) -0.013(12) 0.038(11) 0.033(10) O10 0.142(10) 0.138(10) 0.219(15) 0.062(11) 0.080(10) 0.012(8) C911 0.22(2) 0.139(16) 0.32(2) 0.050(17) 0.185(18) -0.013(15) C912 0.22(2) 0.21(2) 0.35(3) 0.07(2) 0.19(2) -0.024(19) C913 0.22(2) 0.22(2) 0.36(3) 0.01(2) 0.12(2) -0.07(2) C914 0.19(2) 0.22(2) 0.34(3) 0.00(2) 0.10(2) 0.00(2) O11 0.189(13) 0.201(14) 0.164(12) 0.061(11) 0.083(10) 0.085(11) C921 0.167(16) 0.161(16) 0.121(13) 0.061(12) 0.045(12) 0.020(13) C922 0.116(12) 0.159(16) 0.164(17) 0.028(14) 0.055(12) 0.009(12) C923 0.169(16) 0.23(2) 0.092(11) 0.027(14) 0.058(11) -0.018(16) C924 0.148(15) 0.173(16) 0.140(14) 0.079(13) 0.050(12) 0.043(12) O12 0.245(18) 0.205(17) 0.192(16) 0.032(13) 0.095(14) 0.004(13) C931 0.28(3) 0.20(2) 0.149(18) 0.021(19) 0.04(2) 0.02(2) C932 0.23(3) 0.27(3) 0.21(2) 0.08(2) 0.03(2) 0.05(2) C933 0.22(2) 0.26(3) 0.20(2) 0.10(2) 0.125(18) 0.010(19) C934 0.23(3) 0.32(3) 0.26(3) 0.05(2) 0.11(2) 0.02(2) _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 P1 N1 1.579(7) . ? P1 N2 1.616(7) . ? P1 N4 1.670(7) . ? P1 N3 1.686(8) . ? P1 Li1 2.633(16) . ? N1 C11 1.367(12) . ? N1 Li1 2.064(19) . ? C11 C12 1.416(14) . ? C11 C16 1.434(13) . ? C12 C13 1.369(15) . ? C13 C14 1.363(18) . ? C14 C15 1.386(18) . ? C15 C16 1.333(15) . ? N2 C21 1.352(12) . ? N2 Li1 1.981(17) . ? C21 C22 1.442(12) . ? C21 C26 1.444(13) . ? C22 C23 1.378(13) . ? C23 C24 1.375(15) . ? C24 C25 1.371(15) . ? C25 C26 1.355(14) . ? N3 C31 1.360(11) . ? C31 C36 1.385(13) . ? C31 C32 1.403(12) . ? C32 C33 1.384(15) . ? C33 C34 1.359(16) . ? C34 C35 1.364(17) . ? C35 C36 1.346(15) . ? N4 C41 1.400(11) . ? C41 C42 1.388(12) . ? C41 C46 1.406(13) . ? C42 C43 1.333(14) . ? C43 C44 1.400(18) . ? C44 C45 1.425(16) . ? C45 C46 1.365(15) . ? P2 N6 1.575(8) . ? P2 N5 1.599(7) . ? P2 N8 1.674(7) . ? P2 N7 1.689(7) . ? P2 Li2 2.636(15) . ? N5 C51 1.396(12) . ? N5 Li2 2.062(19) . ? C51 C56 1.373(13) . ? C51 C52 1.417(13) . ? C52 C53 1.397(16) . ? C53 C54 1.342(18) . ? C54 C55 1.399(17) . ? C55 C56 1.376(14) . ? N6 C61 1.389(11) . ? N6 Li2 2.005(15) . ? C61 C62 1.406(13) . ? C61 C66 1.439(13) . ? C62 C63 1.353(17) . ? C63 C64 1.38(2) . ? C64 C65 1.344(18) . ? C65 C66 1.396(14) . ? N7 C71 1.370(10) . ? C71 C76 1.389(13) . ? C71 C72 1.398(13) . ? C72 C73 1.392(14) . ? C73 C74 1.364(15) . ? C74 C75 1.341(17) . ? C75 C76 1.409(15) . ? N8 C81 1.429(11) . ? C81 C86 1.372(12) . ? C81 C82 1.389(12) . ? C82 C83 1.371(14) . ? C83 C84 1.429(16) . ? C84 C85 1.321(15) . ? C85 C86 1.402(15) . ? Cl2 Li3 2.19(3) . ? Cl2 Li4 2.22(3) . ? Li1 O2 1.93(2) . ? Li1 O1 1.937(15) . ? Li2 O3 1.912(18) . ? Li2 O4 1.942(15) . ? Li3 O6 1.94(3) . ? Li3 O5 1.96(2) . ? Li3 O7 1.99(3) . ? Li4 O8 1.72(5) . ? Li4 O9 2.04(4) . ? Li4 O10 2.11(4) . ? Li4 C801 2.78(6) . ? O1 C104 1.410(10) . ? O1 C101 1.427(10) . ? C101 C102 1.468(12) . ? C102 C103 1.475(13) . ? C103 C104 1.460(12) . ? O2 C204 1.402(10) . ? O2 C201 1.403(11) . ? C201 C202 1.437(13) . ? C202 C203 1.466(14) . ? C203 C204 1.475(13) . ? O3 C304 1.413(10) . ? O3 C301 1.441(10) . ? C301 C302 1.457(11) . ? C302 C303 1.435(12) . ? C303 C304 1.476(11) . ? O4 C404 1.402(11) . ? O4 C401 1.438(10) . ? C401 C402 1.473(12) . ? C402 C403 1.495(13) . ? C403 C404 1.379(12) . ? O5 C504 1.403(10) . ? O5 C501 1.435(11) . ? C501 C502 1.466(12) . ? C502 C503 1.467(13) . ? C503 C504 1.494(12) . ? O6 C604 1.410(10) . ? O6 C601 1.417(11) . ? C601 C602 1.445(13) . ? C602 C603 1.471(13) . ? C603 C604 1.477(12) . ? O7 C701 1.383(11) . ? O7 C704 1.394(11) . ? C701 C702 1.466(13) . ? C702 C703 1.442(15) . ? C703 C704 1.444(13) . ? O8 C804 1.398(11) . ? O8 C801 1.445(11) . ? C801 C802 1.447(13) . ? C802 C803 1.445(13) . ? C803 C804 1.476(12) . ? O9 C901 1.392(12) . ? O9 C904 1.416(12) . ? C901 C902 1.458(13) . ? C902 C903 1.441(14) . ? C903 C904 1.492(13) . ? O10 C914 1.406(13) . ? O10 C911 1.424(13) . ? C911 C912 1.458(14) . ? C912 C913 1.424(15) . ? C913 C914 1.455(14) . ? O11 C924 1.396(12) . ? O11 C921 1.423(12) . ? C921 C922 1.477(13) . ? C922 C923 1.443(14) . ? C923 C924 1.447(13) . ? O12 C931 1.412(13) . ? O12 C934 1.437(14) . ? C931 C932 1.467(15) . ? C932 C933 1.453(15) . ? C933 C934 1.457(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 N2 100.2(4) . . ? N1 P1 N4 115.7(4) . . ? N2 P1 N4 114.3(4) . . ? N1 P1 N3 115.5(4) . . ? N2 P1 N3 115.6(4) . . ? N4 P1 N3 96.6(4) . . ? N1 P1 Li1 51.6(5) . . ? N2 P1 Li1 48.7(5) . . ? N4 P1 Li1 129.7(5) . . ? N3 P1 Li1 133.6(5) . . ? C11 N1 P1 127.7(6) . . ? C11 N1 Li1 140.6(7) . . ? P1 N1 Li1 91.6(6) . . ? N1 C11 C12 127.1(8) . . ? N1 C11 C16 118.1(8) . . ? C12 C11 C16 114.9(9) . . ? C13 C12 C11 121.7(10) . . ? C14 C13 C12 120.1(12) . . ? C13 C14 C15 120.8(11) . . ? C16 C15 C14 119.5(10) . . ? C15 C16 C11 123.0(10) . . ? C21 N2 P1 128.8(6) . . ? C21 N2 Li1 137.7(8) . . ? P1 N2 Li1 93.5(6) . . ? N2 C21 C22 124.9(8) . . ? N2 C21 C26 118.7(8) . . ? C22 C21 C26 116.4(9) . . ? C23 C22 C21 118.0(9) . . ? C24 C23 C22 124.2(10) . . ? C25 C24 C23 118.1(10) . . ? C26 C25 C24 121.7(10) . . ? C25 C26 C21 121.5(9) . . ? C31 N3 P1 128.0(6) . . ? N3 C31 C36 121.0(8) . . ? N3 C31 C32 121.7(7) . . ? C36 C31 C32 117.2(8) . . ? C33 C32 C31 118.2(9) . . ? C34 C33 C32 123.8(10) . . ? C33 C34 C35 116.7(10) . . ? C36 C35 C34 122.2(12) . . ? C35 C36 C31 121.9(11) . . ? C41 N4 P1 127.5(6) . . ? C42 C41 N4 119.5(7) . . ? C42 C41 C46 118.5(9) . . ? N4 C41 C46 121.9(8) . . ? C43 C42 C41 121.1(9) . . ? C42 C43 C44 121.7(11) . . ? C43 C44 C45 118.3(11) . . ? C46 C45 C44 119.0(11) . . ? C45 C46 C41 121.3(10) . . ? N6 P2 N5 100.7(4) . . ? N6 P2 N8 115.2(4) . . ? N5 P2 N8 114.4(4) . . ? N6 P2 N7 115.6(4) . . ? N5 P2 N7 114.6(4) . . ? N8 P2 N7 97.2(3) . . ? N6 P2 Li2 49.3(4) . . ? N5 P2 Li2 51.4(5) . . ? N8 P2 Li2 132.3(5) . . ? N7 P2 Li2 130.5(4) . . ? C51 N5 P2 127.3(6) . . ? C51 N5 Li2 141.4(6) . . ? P2 N5 Li2 91.2(5) . . ? C56 C51 N5 125.6(7) . . ? C56 C51 C52 118.5(9) . . ? N5 C51 C52 115.9(8) . . ? C53 C52 C51 118.6(11) . . ? C54 C53 C52 122.9(12) . . ? C53 C54 C55 117.8(11) . . ? C56 C55 C54 121.4(11) . . ? C51 C56 C55 120.8(9) . . ? C61 N6 P2 128.3(6) . . ? C61 N6 Li2 137.5(8) . . ? P2 N6 Li2 94.1(6) . . ? N6 C61 C62 117.5(8) . . ? N6 C61 C66 125.2(8) . . ? C62 C61 C66 117.2(9) . . ? C63 C62 C61 121.6(11) . . ? C62 C63 C64 120.5(12) . . ? C65 C64 C63 120.5(12) . . ? C64 C65 C66 121.6(11) . . ? C65 C66 C61 118.5(9) . . ? C71 N7 P2 127.1(6) . . ? N7 C71 C76 120.4(8) . . ? N7 C71 C72 122.4(8) . . ? C76 C71 C72 117.3(8) . . ? C73 C72 C71 120.1(9) . . ? C74 C73 C72 121.3(10) . . ? C75 C74 C73 119.5(11) . . ? C74 C75 C76 120.6(11) . . ? C71 C76 C75 120.9(10) . . ? C81 N8 P2 126.3(6) . . ? C86 C81 C82 120.5(8) . . ? C86 C81 N8 121.6(8) . . ? C82 C81 N8 117.9(7) . . ? C83 C82 C81 119.4(8) . . ? C82 C83 C84 120.5(9) . . ? C85 C84 C83 118.0(10) . . ? C84 C85 C86 123.0(10) . . ? C81 C86 C85 118.6(9) . . ? Li3 Cl2 Li4 130.5(12) . . ? O2 Li1 O1 103.2(8) . . ? O2 Li1 N2 126.9(10) . . ? O1 Li1 N2 111.6(8) . . ? O2 Li1 N1 113.4(8) . . ? O1 Li1 N1 127.7(11) . . ? N2 Li1 N1 74.6(6) . . ? O2 Li1 P1 127.8(7) . . ? O1 Li1 P1 129.0(9) . . ? N2 Li1 P1 37.8(3) . . ? N1 Li1 P1 36.8(3) . . ? O3 Li2 O4 105.1(8) . . ? O3 Li2 N6 122.7(9) . . ? O4 Li2 N6 111.7(7) . . ? O3 Li2 N5 114.2(7) . . ? O4 Li2 N5 128.1(11) . . ? N6 Li2 N5 73.9(6) . . ? O3 Li2 P2 125.8(7) . . ? O4 Li2 P2 128.7(8) . . ? N6 Li2 P2 36.6(3) . . ? N5 Li2 P2 37.3(3) . . ? O6 Li3 O5 101.3(11) . . ? O6 Li3 O7 104.9(13) . . ? O5 Li3 O7 107.3(13) . . ? O6 Li3 Cl2 116.6(13) . . ? O5 Li3 Cl2 115.4(13) . . ? O7 Li3 Cl2 110.2(11) . . ? O8 Li4 O9 110.4(17) . . ? O8 Li4 O10 110.2(18) . . ? O9 Li4 O10 103(2) . . ? O8 Li4 Cl2 120(3) . . ? O9 Li4 Cl2 107.2(16) . . ? O10 Li4 Cl2 104.2(16) . . ? O8 Li4 C801 25.9(9) . . ? O9 Li4 C801 122.9(18) . . ? O10 Li4 C801 122.0(17) . . ? Cl2 Li4 C801 94.0(17) . . ? C104 O1 C101 106.4(7) . . ? C104 O1 Li1 130.1(8) . . ? C101 O1 Li1 123.5(7) . . ? O1 C101 C102 106.1(8) . . ? C101 C102 C103 103.2(9) . . ? C104 C103 C102 105.5(9) . . ? O1 C104 C103 108.7(8) . . ? C204 O2 C201 108.8(9) . . ? C204 O2 Li1 129.5(9) . . ? C201 O2 Li1 121.4(9) . . ? O2 C201 C202 109.2(10) . . ? C201 C202 C203 103.1(10) . . ? C202 C203 C204 104.7(10) . . ? O2 C204 C203 104.9(9) . . ? C304 O3 C301 107.0(7) . . ? C304 O3 Li2 125.4(7) . . ? C301 O3 Li2 127.5(8) . . ? O3 C301 C302 105.9(8) . . ? C303 C302 C301 109.6(9) . . ? C302 C303 C304 104.3(8) . . ? O3 C304 C303 108.2(8) . . ? C404 O4 C401 107.8(8) . . ? C404 O4 Li2 125.2(7) . . ? C401 O4 Li2 125.1(7) . . ? O4 C401 C402 105.8(8) . . ? C401 C402 C403 105.7(8) . . ? C404 C403 C402 105.7(10) . . ? C403 C404 O4 109.4(10) . . ? C504 O5 C501 106.8(8) . . ? C504 O5 Li3 124.8(10) . . ? C501 O5 Li3 127.6(11) . . ? O5 C501 C502 108.0(9) . . ? C501 C502 C503 102.5(10) . . ? C502 C503 C504 103.2(10) . . ? O5 C504 C503 108.1(9) . . ? C604 O6 C601 108.7(8) . . ? C604 O6 Li3 123.8(11) . . ? C601 O6 Li3 126.2(11) . . ? O6 C601 C602 107.8(9) . . ? C601 C602 C603 103.4(10) . . ? C602 C603 C604 104.2(9) . . ? O6 C604 C603 106.2(9) . . ? C701 O7 C704 109.8(9) . . ? C701 O7 Li3 125.6(10) . . ? C704 O7 Li3 120.9(11) . . ? O7 C701 C702 108.0(10) . . ? C703 C702 C701 105.0(10) . . ? C702 C703 C704 106.4(11) . . ? O7 C704 C703 107.5(10) . . ? C804 O8 C801 106.7(9) . . ? C804 O8 Li4 129.9(15) . . ? C801 O8 Li4 122.7(15) . . ? O8 C801 C802 107.3(10) . . ? O8 C801 Li4 31.4(8) . . ? C802 C801 Li4 134.5(12) . . ? C803 C802 C801 105.6(10) . . ? C802 C803 C804 104.5(9) . . ? O8 C804 C803 109.4(9) . . ? C901 O9 C904 105.9(10) . . ? C901 O9 Li4 123.6(14) . . ? C904 O9 Li4 127.6(15) . . ? O9 C901 C902 111.3(10) . . ? C903 C902 C901 101.9(11) . . ? C902 C903 C904 104.5(11) . . ? O9 C904 C903 103.7(10) . . ? C914 O10 C911 102.7(12) . . ? C914 O10 Li4 146.8(17) . . ? C911 O10 Li4 110.4(15) . . ? O10 C911 C912 109.9(13) . . ? C913 C912 C911 103.4(13) . . ? C912 C913 C914 106.2(13) . . ? O10 C914 C913 111.1(13) . . ? C924 O11 C921 106.9(11) . . ? O11 C921 C922 107.2(11) . . ? C923 C922 C921 102.9(11) . . ? C922 C923 C924 103.5(12) . . ? O11 C924 C923 107.3(11) . . ? C931 O12 C934 108.0(13) . . ? O12 C931 C932 105.5(13) . . ? C933 C932 C931 103.2(14) . . ? C932 C933 C934 101.6(15) . . ? O12 C934 C933 104.6(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.769 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.077 #===END data_5Li4Clthf4 _database_code_depnum_ccdc_archive 'CCDC 229164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Cl Li4 N4 O4 P' _chemical_formula_weight 747.04 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.554(3) _cell_length_b 16.624(4) _cell_length_c 21.304(5) _cell_angle_alpha 85.131(4) _cell_angle_beta 80.666(4) _cell_angle_gamma 80.165(5) _cell_volume 3971.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.181 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _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 16440 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.2091 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 22.49 _reflns_number_total 10299 _reflns_number_gt 4001 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0452P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10299 _refine_ls_number_parameters 936 _refine_ls_number_restraints 3202 _refine_ls_R_factor_all 0.1743 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.65444(16) 0.39408(11) 0.28495(10) 0.0453(6) Uani 1 1 d . . . N1 N 0.7552(4) 0.3409(3) 0.2353(2) 0.0422(15) Uani 1 1 d . . . C11 C 0.8319(6) 0.3789(4) 0.1894(4) 0.0419(18) Uani 1 1 d U . . C12 C 0.8776(6) 0.4487(4) 0.2007(3) 0.051(2) Uani 1 1 d U A . H12 H 0.8552 0.4725 0.2408 0.061 Uiso 1 1 calc R . . C13 C 0.9559(6) 0.4830(4) 0.1531(4) 0.059(2) Uani 1 1 d U . . H13 H 0.9841 0.5312 0.1607 0.070 Uiso 1 1 calc R . . C14 C 0.9918(7) 0.4493(5) 0.0969(4) 0.065(2) Uani 1 1 d U . . H14 H 1.0453 0.4730 0.0649 0.078 Uiso 1 1 calc R . . C15 C 0.9506(8) 0.3803(5) 0.0864(4) 0.080(3) Uani 1 1 d U . . H15 H 0.9771 0.3554 0.0470 0.095 Uiso 1 1 calc R . . C16 C 0.8711(7) 0.3459(5) 0.1318(4) 0.059(2) Uani 1 1 d U . . H16 H 0.8432 0.2983 0.1228 0.071 Uiso 1 1 calc R . . N2 N 0.5806(5) 0.3211(3) 0.3107(3) 0.0448(15) Uani 1 1 d . . . C21 C 0.4854(7) 0.3272(5) 0.3584(4) 0.047(2) Uani 1 1 d U . . C22 C 0.4556(7) 0.2555(5) 0.3920(4) 0.063(2) Uani 1 1 d U . . H22 H 0.5036 0.2047 0.3815 0.076 Uiso 1 1 calc R . . C23 C 0.3612(8) 0.2562(6) 0.4388(4) 0.075(3) Uani 1 1 d U . . H23 H 0.3438 0.2059 0.4596 0.090 Uiso 1 1 calc R . . C24 C 0.2894(7) 0.3282(7) 0.4570(4) 0.080(3) Uani 1 1 d U . . H24 H 0.2232 0.3286 0.4899 0.097 Uiso 1 1 calc R . . C25 C 0.3178(7) 0.3986(5) 0.4258(4) 0.070(2) Uani 1 1 d U . . H25 H 0.2705 0.4492 0.4375 0.084 Uiso 1 1 calc R . . C26 C 0.4126(6) 0.3988(5) 0.3778(3) 0.052(2) Uani 1 1 d U . . H26 H 0.4288 0.4495 0.3573 0.062 Uiso 1 1 calc R . . N3 N 0.7051(5) 0.4382(3) 0.3368(3) 0.0472(16) Uani 1 1 d . . . C31 C 0.7795(6) 0.3952(5) 0.3764(4) 0.055(2) Uani 1 1 d U . . C32 C 0.7970(6) 0.3111(5) 0.3899(3) 0.053(2) Uani 1 1 d U . . H32 H 0.7544 0.2781 0.3709 0.064 Uiso 1 1 calc R . . C33 C 0.8752(7) 0.2747(5) 0.4303(4) 0.069(2) Uani 1 1 d U . . H33 H 0.8862 0.2169 0.4377 0.082 Uiso 1 1 calc R . . C34 C 0.9371(7) 0.3188(7) 0.4599(4) 0.079(3) Uani 1 1 d U . . H34 H 0.9913 0.2925 0.4871 0.095 Uiso 1 1 calc R . . C35 C 0.9193(8) 0.4020(7) 0.4495(4) 0.092(3) Uani 1 1 d U . . H35 H 0.9607 0.4342 0.4702 0.110 Uiso 1 1 calc R . . C36 C 0.8417(7) 0.4391(5) 0.4093(4) 0.074(3) Uani 1 1 d U . . H36 H 0.8297 0.4971 0.4035 0.088 Uiso 1 1 calc R . . N4 N 0.5888(4) 0.4779(3) 0.2505(3) 0.0474(16) Uani 1 1 d . . . C41 C 0.4918(6) 0.4837(4) 0.2201(3) 0.0479(19) Uani 1 1 d U . . C42 C 0.4393(6) 0.5626(4) 0.2003(4) 0.071(2) Uani 1 1 d U . . H42 H 0.4714 0.6083 0.2099 0.085 Uiso 1 1 calc R . . C43 C 0.3452(7) 0.5762(5) 0.1681(4) 0.080(3) Uani 1 1 d U . . H43 H 0.3123 0.6308 0.1566 0.096 Uiso 1 1 calc R . . C44 C 0.2966(6) 0.5130(5) 0.1519(4) 0.067(2) Uani 1 1 d U . . H44 H 0.2320 0.5225 0.1283 0.081 Uiso 1 1 calc R . . C45 C 0.3440(6) 0.4361(4) 0.1707(3) 0.053(2) Uani 1 1 d U . . H45 H 0.3102 0.3913 0.1608 0.063 Uiso 1 1 calc R . . C46 C 0.4398(6) 0.4205(4) 0.2038(3) 0.050(2) Uani 1 1 d U . . H46 H 0.4707 0.3656 0.2155 0.061 Uiso 1 1 calc R . . P2 P 0.87540(17) -0.12365(11) 0.22109(9) 0.0441(5) Uani 1 1 d . . . N5 N 0.9491(5) -0.2074(3) 0.1931(3) 0.0445(15) Uani 1 1 d D . . C51 C 1.0335(7) -0.2131(5) 0.1402(4) 0.061(2) Uani 1 1 d DU . . C52 C 1.0868(7) -0.1494(5) 0.1093(4) 0.075(3) Uani 1 1 d DU . . H52 H 1.0666 -0.0964 0.1253 0.090 Uiso 1 1 calc R . . C53 C 1.1684(9) -0.1624(7) 0.0557(5) 0.117(4) Uani 1 1 d DU . . H53 H 1.2023 -0.1176 0.0343 0.140 Uiso 1 1 calc R . . C54 C 1.2024(10) -0.2374(8) 0.0320(5) 0.139(5) Uani 1 1 d DU . . H54 H 1.2620 -0.2454 -0.0042 0.166 Uiso 1 1 calc R . . C55 C 1.1505(10) -0.3003(7) 0.0607(5) 0.118(4) Uani 1 1 d DU . . H55 H 1.1727 -0.3531 0.0443 0.141 Uiso 1 1 calc R . . C56 C 1.0665(8) -0.2883(5) 0.1128(4) 0.083(3) Uani 1 1 d DU . . H56 H 1.0287 -0.3329 0.1313 0.100 Uiso 1 1 calc R . . N6 N 0.7755(5) -0.1653(3) 0.2717(3) 0.0418(15) Uani 1 1 d D . . C61 C 0.6966(6) -0.1212(4) 0.3158(3) 0.0428(19) Uani 1 1 d DU . . C62 C 0.6553(6) -0.0378(4) 0.3090(4) 0.055(2) Uani 1 1 d DU . . H62 H 0.6858 -0.0076 0.2719 0.066 Uiso 1 1 calc R . . C63 C 0.5718(7) 0.0025(5) 0.3542(4) 0.069(2) Uani 1 1 d DU . . H63 H 0.5467 0.0597 0.3482 0.083 Uiso 1 1 calc R . . C64 C 0.5250(7) -0.0389(6) 0.4071(4) 0.070(2) Uani 1 1 d DU . . H64 H 0.4673 -0.0113 0.4383 0.084 Uiso 1 1 calc R . . C65 C 0.5621(7) -0.1206(5) 0.4149(4) 0.070(2) Uani 1 1 d DU . . H65 H 0.5287 -0.1502 0.4515 0.084 Uiso 1 1 calc R . . C66 C 0.6463(7) -0.1609(4) 0.3711(3) 0.055(2) Uani 1 1 d DU . . H66 H 0.6715 -0.2179 0.3786 0.065 Uiso 1 1 calc R . . N7 N 0.9299(12) -0.0602(9) 0.2623(7) 0.035(6) Uiso 0.503(6) 1 d PDU . 1 C71 C 1.0149(13) -0.0871(8) 0.2993(7) 0.042(5) Uiso 0.503(6) 1 d PDU . 1 C72 C 1.0335(12) -0.1642(7) 0.3314(6) 0.055(4) Uiso 0.503(6) 1 d PDU . 1 H72 H 0.9880 -0.2039 0.3238 0.066 Uiso 0.503(6) 1 calc PR . 1 C73 C 1.1134(12) -0.1856(8) 0.3733(6) 0.068(5) Uiso 0.503(6) 1 d PDU . 1 H73 H 1.1229 -0.2391 0.3933 0.081 Uiso 0.503(6) 1 calc PR . 1 C74 C 1.1797(13) -0.1299(9) 0.3863(7) 0.079(5) Uiso 0.503(6) 1 d PDU . 1 H74 H 1.2321 -0.1433 0.4170 0.095 Uiso 0.503(6) 1 calc PR . 1 C75 C 1.1691(14) -0.0539(9) 0.3542(8) 0.078(5) Uiso 0.503(6) 1 d PDU . 1 H75 H 1.2193 -0.0162 0.3598 0.093 Uiso 0.503(6) 1 calc PR . 1 C76 C 1.0853(13) -0.0333(9) 0.3140(8) 0.054(6) Uiso 0.503(6) 1 d PDU . 1 H76 H 1.0748 0.0208 0.2952 0.065 Uiso 0.503(6) 1 calc PR . 1 N7' N 0.9519(11) -0.0693(8) 0.2497(6) 0.022(5) Uiso 0.497(6) 1 d PDU . 2 C71' C 1.0534(11) -0.0922(7) 0.2749(7) 0.027(4) Uiso 0.497(6) 1 d PDU . 2 C72' C 1.1096(11) -0.1719(7) 0.2859(6) 0.046(4) Uiso 0.497(6) 1 d PDU . 2 H72' H 1.0739 -0.2165 0.2774 0.055 Uiso 0.497(6) 1 calc PR . 2 C73' C 1.2171(11) -0.1872(8) 0.3093(6) 0.063(5) Uiso 0.497(6) 1 d PDU . 2 H73' H 1.2563 -0.2420 0.3140 0.075 Uiso 0.497(6) 1 calc PR . 2 C74' C 1.2683(11) -0.1245(7) 0.3259(6) 0.058(5) Uiso 0.497(6) 1 d PDU . 2 H74' H 1.3393 -0.1359 0.3444 0.069 Uiso 0.497(6) 1 calc PR . 2 C75' C 1.2150(11) -0.0454(7) 0.3152(7) 0.047(4) Uiso 0.497(6) 1 d PDU . 2 H75' H 1.2497 -0.0010 0.3249 0.056 Uiso 0.497(6) 1 calc PR . 2 C76' C 1.1121(12) -0.0316(8) 0.2906(7) 0.033(4) Uiso 0.497(6) 1 d PDU . 2 H76' H 1.0770 0.0237 0.2834 0.040 Uiso 0.497(6) 1 calc PR . 2 N8 N 0.8223(4) -0.0541(3) 0.1702(2) 0.0468(15) Uani 1 1 d D . . C81 C 0.7719(12) -0.0621(7) 0.1194(6) 0.038(4) Uiso 0.541(12) 1 d PDU . 1 C82 C 0.7501(12) -0.1364(8) 0.1026(7) 0.049(4) Uiso 0.541(12) 1 d PDU . 1 H82 H 0.7808 -0.1852 0.1250 0.058 Uiso 0.541(12) 1 calc PR . 1 C83 C 0.6854(12) -0.1417(8) 0.0544(7) 0.058(5) Uiso 0.541(12) 1 d PDU . 1 H83 H 0.6718 -0.1936 0.0443 0.070 Uiso 0.541(12) 1 calc PR . 1 C84 C 0.6405(12) -0.0718(7) 0.0211(7) 0.056(5) Uiso 0.541(12) 1 d PDU . 1 H84 H 0.5967 -0.0751 -0.0124 0.067 Uiso 0.541(12) 1 calc PR . 1 C85 C 0.6596(12) 0.0017(7) 0.0365(6) 0.057(4) Uiso 0.541(12) 1 d PDU . 1 H85 H 0.6287 0.0501 0.0137 0.068 Uiso 0.541(12) 1 calc PR . 1 C86 C 0.7221(11) 0.0068(7) 0.0839(6) 0.043(4) Uiso 0.541(12) 1 d PDU . 1 H86 H 0.7330 0.0594 0.0939 0.052 Uiso 0.541(12) 1 calc PR . 1 C81' C 0.7413(14) -0.0769(8) 0.1355(8) 0.038(5) Uiso 0.459(12) 1 d PDU . 2 C82' C 0.7176(13) -0.1545(8) 0.1275(7) 0.041(5) Uiso 0.459(12) 1 d PDU . 2 H82' H 0.7580 -0.2002 0.1494 0.049 Uiso 0.459(12) 1 calc PR . 2 C83' C 0.6379(13) -0.1681(8) 0.0891(7) 0.046(5) Uiso 0.459(12) 1 d PDU . 2 H83' H 0.6242 -0.2221 0.0855 0.056 Uiso 0.459(12) 1 calc PR . 2 C84' C 0.5791(15) -0.1045(9) 0.0565(8) 0.064(6) Uiso 0.459(12) 1 d PDU . 2 H84' H 0.5223 -0.1136 0.0313 0.077 Uiso 0.459(12) 1 calc PR . 2 C85' C 0.6021(16) -0.0277(9) 0.0602(8) 0.068(6) Uiso 0.459(12) 1 d PDU . 2 H85' H 0.5657 0.0164 0.0350 0.081 Uiso 0.459(12) 1 calc PR . 2 C86' C 0.6777(15) -0.0135(9) 0.1001(8) 0.059(6) Uiso 0.459(12) 1 d PDU . 2 H86' H 0.6877 0.0413 0.1041 0.071 Uiso 0.459(12) 1 calc PR . 2 Cl1 Cl 0.81857(16) 0.13630(10) 0.26977(9) 0.0586(6) Uani 1 1 d . . . Cl2 Cl 0.71747(15) 0.65096(9) 0.23751(9) 0.0544(6) Uani 1 1 d . . . Li1 Li 0.8784(11) 0.2629(7) 0.2768(6) 0.060(4) Uani 1 1 d . . . O1 O 1.0413(4) 0.2553(2) 0.2767(2) 0.0567(13) Uani 1 1 d DU . . C101 C 1.1099(10) 0.1853(6) 0.3029(6) 0.059(4) Uiso 0.716(14) 1 d PDU . 1 H10A H 1.1556 0.1507 0.2688 0.071 Uiso 0.716(14) 1 calc PR . 1 H10B H 1.0583 0.1523 0.3323 0.071 Uiso 0.716(14) 1 calc PR . 1 C102 C 1.1909(10) 0.2186(6) 0.3378(6) 0.058(4) Uiso 0.716(14) 1 d PDU . 1 H10C H 1.2664 0.1803 0.3387 0.070 Uiso 0.716(14) 1 calc PR . 1 H10D H 1.1533 0.2295 0.3820 0.070 Uiso 0.716(14) 1 calc PR . 1 C103 C 1.2113(9) 0.2962(6) 0.2999(6) 0.060(4) Uiso 0.716(14) 1 d PDU . 1 H10E H 1.2344 0.3354 0.3263 0.072 Uiso 0.716(14) 1 calc PR . 1 H10F H 1.2736 0.2856 0.2624 0.072 Uiso 0.716(14) 1 calc PR . 1 C104 C 1.0952(9) 0.3267(5) 0.2805(6) 0.049(3) Uiso 0.716(14) 1 d PDU . 1 H10G H 1.0456 0.3633 0.3122 0.059 Uiso 0.716(14) 1 calc PR . 1 H10H H 1.1043 0.3575 0.2386 0.059 Uiso 0.716(14) 1 calc PR . 1 C1A1 C 1.0931(15) 0.1990(14) 0.3255(11) 0.040(9) Uiso 0.284(14) 1 d PDU . 2 H1A1 H 1.0614 0.1467 0.3302 0.048 Uiso 0.284(14) 1 calc PR . 2 H1A2 H 1.0782 0.2237 0.3673 0.048 Uiso 0.284(14) 1 calc PR . 2 C1A2 C 1.2223(15) 0.1868(13) 0.2989(14) 0.055(9) Uiso 0.284(14) 1 d PDU . 2 H1A3 H 1.2721 0.1703 0.3329 0.066 Uiso 0.284(14) 1 calc PR . 2 H1A4 H 1.2416 0.1450 0.2667 0.066 Uiso 0.284(14) 1 calc PR . 2 C1A3 C 1.2386(16) 0.2695(13) 0.2692(13) 0.043(8) Uiso 0.284(14) 1 d PDU . 2 H1A5 H 1.2638 0.3023 0.2998 0.052 Uiso 0.284(14) 1 calc PR . 2 H1A6 H 1.2999 0.2647 0.2309 0.052 Uiso 0.284(14) 1 calc PR . 2 C1A4 C 1.1217(16) 0.3086(13) 0.2518(14) 0.044(8) Uiso 0.284(14) 1 d PDU . 2 H1A7 H 1.0964 0.3626 0.2704 0.053 Uiso 0.284(14) 1 calc PR . 2 H1A8 H 1.1263 0.3164 0.2050 0.053 Uiso 0.284(14) 1 calc PR . 2 Li2 Li 0.6615(11) 0.2483(7) 0.2464(6) 0.065(4) Uani 1 1 d . . . O2 O 0.5750(4) 0.2080(3) 0.1901(2) 0.0669(15) Uani 1 1 d DU . . C201 C 0.5264(18) 0.1346(10) 0.1955(10) 0.053(6) Uiso 0.48(3) 1 d PDU . 1 H20A H 0.4771 0.1279 0.2376 0.064 Uiso 0.48(3) 1 calc PR . 1 H20B H 0.5900 0.0865 0.1897 0.064 Uiso 0.48(3) 1 calc PR . 1 C202 C 0.4516(18) 0.1449(11) 0.1426(10) 0.071(7) Uiso 0.48(3) 1 d PDU . 1 H20C H 0.4556 0.0925 0.1230 0.085 Uiso 0.48(3) 1 calc PR . 1 H20D H 0.3676 0.1665 0.1585 0.085 Uiso 0.48(3) 1 calc PR . 1 C203 C 0.507(2) 0.2052(9) 0.0965(9) 0.067(7) Uiso 0.48(3) 1 d PDU . 1 H20E H 0.5385 0.1807 0.0551 0.080 Uiso 0.48(3) 1 calc PR . 1 H20F H 0.4485 0.2544 0.0893 0.080 Uiso 0.48(3) 1 calc PR . 1 C204 C 0.606(2) 0.2270(12) 0.1254(6) 0.067(6) Uiso 0.48(3) 1 d PDU . 1 H20G H 0.6832 0.1945 0.1084 0.081 Uiso 0.48(3) 1 calc PR . 1 H20H H 0.6113 0.2859 0.1171 0.081 Uiso 0.48(3) 1 calc PR . 1 C2A1 C 0.5004(16) 0.1500(11) 0.2136(9) 0.055(6) Uiso 0.52(3) 1 d PDU . 2 H2A1 H 0.4504 0.1678 0.2539 0.066 Uiso 0.52(3) 1 calc PR . 2 H2A2 H 0.5492 0.0966 0.2227 0.066 Uiso 0.52(3) 1 calc PR . 2 C2A2 C 0.4236(16) 0.1414(9) 0.1661(10) 0.068(6) Uiso 0.52(3) 1 d PDU . 2 H2A3 H 0.3393 0.1454 0.1859 0.081 Uiso 0.52(3) 1 calc PR . 2 H2A4 H 0.4487 0.0886 0.1457 0.081 Uiso 0.52(3) 1 calc PR . 2 C2A3 C 0.442(2) 0.2114(9) 0.1190(10) 0.072(6) Uiso 0.52(3) 1 d PDU . 2 H2A5 H 0.4426 0.1955 0.0751 0.086 Uiso 0.52(3) 1 calc PR . 2 H2A6 H 0.3774 0.2585 0.1281 0.086 Uiso 0.52(3) 1 calc PR . 2 C2A4 C 0.557(2) 0.2322(11) 0.1264(6) 0.067(6) Uiso 0.52(3) 1 d PDU . 2 H2A7 H 0.6209 0.2029 0.0960 0.081 Uiso 0.52(3) 1 calc PR . 2 H2A8 H 0.5564 0.2917 0.1181 0.081 Uiso 0.52(3) 1 calc PR . 2 Li3 Li 0.6275(11) 0.5493(7) 0.3148(6) 0.059(4) Uani 1 1 d . . . O3 O 0.5319(4) 0.6098(3) 0.3787(2) 0.0727(16) Uani 1 1 d DU . . C301 C 0.5284(11) 0.5743(8) 0.4415(5) 0.074(4) Uiso 0.684(13) 1 d PDU A 1 H30A H 0.5994 0.5822 0.4593 0.088 Uiso 0.684(13) 1 calc PR A 1 H30B H 0.5269 0.5149 0.4418 0.088 Uiso 0.684(13) 1 calc PR A 1 C302 C 0.4202(12) 0.6150(8) 0.4794(5) 0.084(5) Uiso 0.684(13) 1 d PDU A 1 H30C H 0.4355 0.6256 0.5221 0.100 Uiso 0.684(13) 1 calc PR A 1 H30D H 0.3561 0.5812 0.4845 0.100 Uiso 0.684(13) 1 calc PR A 1 C303 C 0.3870(11) 0.6948(6) 0.4410(5) 0.066(4) Uiso 0.684(13) 1 d PDU A 1 H30E H 0.2997 0.7100 0.4441 0.080 Uiso 0.684(13) 1 calc PR A 1 H30F H 0.4195 0.7399 0.4560 0.080 Uiso 0.684(13) 1 calc PR A 1 C304 C 0.4413(10) 0.6767(7) 0.3760(5) 0.064(4) Uiso 0.684(13) 1 d PDU A 1 H30G H 0.3810 0.6639 0.3518 0.076 Uiso 0.684(13) 1 calc PR A 1 H30H H 0.4742 0.7247 0.3541 0.076 Uiso 0.684(13) 1 calc PR A 1 C3A1 C 0.5599(17) 0.6178(18) 0.4389(8) 0.070(8) Uiso 0.316(13) 1 d PDU A 2 H3A1 H 0.6258 0.6496 0.4357 0.084 Uiso 0.316(13) 1 calc PR A 2 H3A2 H 0.5837 0.5633 0.4599 0.084 Uiso 0.316(13) 1 calc PR A 2 C3A2 C 0.4495(17) 0.6616(16) 0.4757(9) 0.055(8) Uiso 0.316(13) 1 d PDU A 2 H3A3 H 0.4508 0.7211 0.4739 0.066 Uiso 0.316(13) 1 calc PR A 2 H3A4 H 0.4395 0.6406 0.5208 0.066 Uiso 0.316(13) 1 calc PR A 2 C3A3 C 0.3518(17) 0.643(2) 0.4425(12) 0.126(12) Uiso 0.316(13) 1 d PDU A 2 H3A5 H 0.3257 0.5910 0.4599 0.152 Uiso 0.316(13) 1 calc PR A 2 H3A6 H 0.2826 0.6875 0.4470 0.152 Uiso 0.316(13) 1 calc PR A 2 C3A4 C 0.4074(15) 0.637(2) 0.3759(11) 0.101(10) Uiso 0.316(13) 1 d PDU A 2 H3A7 H 0.3739 0.5980 0.3546 0.121 Uiso 0.316(13) 1 calc PR A 2 H3A8 H 0.3953 0.6915 0.3523 0.121 Uiso 0.316(13) 1 calc PR A 2 Li4 Li 0.6946(10) 0.5387(7) 0.1849(6) 0.060(4) Uani 1 1 d . . . O4 O 0.6919(4) 0.5572(3) 0.0977(2) 0.0653(14) Uani 1 1 d DU A . C401 C 0.619(2) 0.5245(11) 0.0605(7) 0.065(5) Uiso 0.65(5) 1 d PDU A 1 H40A H 0.5466 0.5102 0.0873 0.078 Uiso 0.65(5) 1 calc PR A 1 H40B H 0.6637 0.4755 0.0391 0.078 Uiso 0.65(5) 1 calc PR A 1 C402 C 0.5894(14) 0.5947(16) 0.0122(8) 0.081(6) Uiso 0.65(5) 1 d PDU A 1 H40C H 0.5226 0.6356 0.0307 0.097 Uiso 0.65(5) 1 calc PR A 1 H40D H 0.5690 0.5747 -0.0265 0.097 Uiso 0.65(5) 1 calc PR A 1 C403 C 0.7044(17) 0.6301(10) -0.0025(7) 0.062(5) Uiso 0.65(5) 1 d PDU A 1 H40E H 0.7554 0.6058 -0.0404 0.075 Uiso 0.65(5) 1 calc PR A 1 H40F H 0.6879 0.6902 -0.0106 0.075 Uiso 0.65(5) 1 calc PR A 1 C404 C 0.7622(16) 0.6085(11) 0.0548(7) 0.060(6) Uiso 0.65(5) 1 d PDU A 1 H40G H 0.8438 0.5790 0.0431 0.072 Uiso 0.65(5) 1 calc PR A 1 H40H H 0.7669 0.6587 0.0756 0.072 Uiso 0.65(5) 1 calc PR A 1 C4A1 C 0.660(4) 0.5081(15) 0.0534(11) 0.066(9) Uiso 0.35(5) 1 d PDU A 2 H4A1 H 0.6010 0.4740 0.0747 0.080 Uiso 0.35(5) 1 calc PR A 2 H4A2 H 0.7306 0.4721 0.0328 0.080 Uiso 0.35(5) 1 calc PR A 2 C4A2 C 0.608(3) 0.568(2) 0.0061(13) 0.082(11) Uiso 0.35(5) 1 d PDU A 2 H4A3 H 0.5212 0.5826 0.0183 0.098 Uiso 0.35(5) 1 calc PR A 2 H4A4 H 0.6252 0.5466 -0.0368 0.098 Uiso 0.35(5) 1 calc PR A 2 C4A3 C 0.668(5) 0.6410(16) 0.0076(16) 0.084(11) Uiso 0.35(5) 1 d PDU A 2 H4A5 H 0.6079 0.6912 0.0132 0.101 Uiso 0.35(5) 1 calc PR A 2 H4A6 H 0.7222 0.6483 -0.0327 0.101 Uiso 0.35(5) 1 calc PR A 2 C4A4 C 0.736(4) 0.625(2) 0.0627(13) 0.080(12) Uiso 0.35(5) 1 d PDU A 2 H4A7 H 0.8220 0.6117 0.0478 0.096 Uiso 0.35(5) 1 calc PR A 2 H4A8 H 0.7206 0.6731 0.0890 0.096 Uiso 0.35(5) 1 calc PR A 2 Li5 Li 0.8483(12) 0.0076(8) 0.3215(6) 0.070(4) Uani 1 1 d . . . O5 O 0.8162(11) 0.0169(7) 0.4111(5) 0.060(3) Uiso 0.490(8) 1 d PDU . 1 C501 C 0.8563(16) -0.0475(9) 0.4540(7) 0.088(6) Uiso 0.490(8) 1 d PDU . 1 H50A H 0.9431 -0.0647 0.4430 0.106 Uiso 0.490(8) 1 calc PR . 1 H50B H 0.8166 -0.0952 0.4514 0.106 Uiso 0.490(8) 1 calc PR . 1 C502 C 0.8276(15) -0.0179(9) 0.5192(6) 0.072(5) Uiso 0.490(8) 1 d PDU . 1 H50C H 0.8998 -0.0255 0.5399 0.086 Uiso 0.490(8) 1 calc PR . 1 H50D H 0.7680 -0.0477 0.5457 0.086 Uiso 0.490(8) 1 calc PR . 1 C503 C 0.7785(13) 0.0712(8) 0.5107(6) 0.067(5) Uiso 0.490(8) 1 d PDU . 1 H50E H 0.7106 0.0875 0.5443 0.080 Uiso 0.490(8) 1 calc PR . 1 H50F H 0.8402 0.1056 0.5116 0.080 Uiso 0.490(8) 1 calc PR . 1 C504 C 0.7401(12) 0.0779(8) 0.4471(6) 0.056(5) Uiso 0.490(8) 1 d PDU . 1 H50G H 0.6566 0.0690 0.4512 0.067 Uiso 0.490(8) 1 calc PR . 1 H50H H 0.7465 0.1328 0.4262 0.067 Uiso 0.490(8) 1 calc PR . 1 O5A O 0.8830(10) -0.0179(7) 0.4062(5) 0.069(3) Uiso 0.510(8) 1 d PDU . 2 C5A1 C 0.9260(12) -0.1019(8) 0.4249(6) 0.069(5) Uiso 0.510(8) 1 d PDU . 2 H5A1 H 1.0139 -0.1133 0.4162 0.083 Uiso 0.510(8) 1 calc PR . 2 H5A2 H 0.8938 -0.1398 0.4015 0.083 Uiso 0.510(8) 1 calc PR . 2 C5A2 C 0.8832(12) -0.1112(9) 0.4949(6) 0.088(6) Uiso 0.510(8) 1 d PDU . 2 H5A3 H 0.8633 -0.1666 0.5071 0.105 Uiso 0.510(8) 1 calc PR . 2 H5A4 H 0.9437 -0.1012 0.5200 0.105 Uiso 0.510(8) 1 calc PR . 2 C5A3 C 0.7756(12) -0.0479(8) 0.5045(7) 0.068(5) Uiso 0.510(8) 1 d PDU . 2 H5A5 H 0.7586 -0.0309 0.5489 0.082 Uiso 0.510(8) 1 calc PR . 2 H5A6 H 0.7054 -0.0679 0.4941 0.082 Uiso 0.510(8) 1 calc PR . 2 C5A4 C 0.8086(13) 0.0207(9) 0.4589(7) 0.071(5) Uiso 0.510(8) 1 d PDU . 2 H5A7 H 0.7369 0.0546 0.4452 0.085 Uiso 0.510(8) 1 calc PR . 2 H5A8 H 0.8518 0.0559 0.4787 0.085 Uiso 0.510(8) 1 calc PR . 2 Li6 Li 0.9077(11) 0.0300(7) 0.1909(6) 0.067(4) Uani 1 1 d . . . O6 O 1.0162(5) 0.0768(3) 0.1293(2) 0.0830(17) Uani 1 1 d DU . . C601 C 1.0295(19) 0.0739(8) 0.0610(6) 0.064(6) Uiso 0.540(19) 1 d PDU . 1 H60A H 0.9587 0.0591 0.0469 0.077 Uiso 0.540(19) 1 calc PR . 1 H60B H 1.1016 0.0363 0.0438 0.077 Uiso 0.540(19) 1 calc PR . 1 C602 C 1.0413(18) 0.1649(9) 0.0443(8) 0.076(6) Uiso 0.540(19) 1 d PDU . 1 H60C H 1.0771 0.1737 -0.0007 0.091 Uiso 0.540(19) 1 calc PR . 1 H60D H 0.9633 0.2007 0.0523 0.091 Uiso 0.540(19) 1 calc PR . 1 C603 C 1.1205(17) 0.1790(9) 0.0881(7) 0.063(5) Uiso 0.540(19) 1 d PDU . 1 H60E H 1.0915 0.2318 0.1081 0.075 Uiso 0.540(19) 1 calc PR . 1 H60F H 1.2021 0.1798 0.0653 0.075 Uiso 0.540(19) 1 calc PR . 1 C604 C 1.1185(15) 0.1086(10) 0.1378(7) 0.062(6) Uiso 0.540(19) 1 d PDU . 1 H60G H 1.1911 0.0672 0.1300 0.075 Uiso 0.540(19) 1 calc PR . 1 H60H H 1.1108 0.1277 0.1813 0.075 Uiso 0.540(19) 1 calc PR . 1 C6A1 C 0.9842(17) 0.0974(15) 0.0674(7) 0.076(7) Uiso 0.460(19) 1 d PDU . 2 H6A1 H 0.9142 0.1412 0.0685 0.092 Uiso 0.460(19) 1 calc PR . 2 H6A2 H 0.9671 0.0491 0.0485 0.092 Uiso 0.460(19) 1 calc PR . 2 C6A2 C 1.0953(19) 0.1269(18) 0.0308(7) 0.097(8) Uiso 0.460(19) 1 d PDU . 2 H6A3 H 1.1417 0.0843 0.0029 0.117 Uiso 0.460(19) 1 calc PR . 2 H6A4 H 1.0733 0.1769 0.0038 0.117 Uiso 0.460(19) 1 calc PR . 2 C6A3 C 1.1664(19) 0.1445(19) 0.0788(9) 0.120(9) Uiso 0.460(19) 1 d PDU . 2 H6A5 H 1.1866 0.2004 0.0710 0.144 Uiso 0.460(19) 1 calc PR . 2 H6A6 H 1.2408 0.1046 0.0779 0.144 Uiso 0.460(19) 1 calc PR . 2 C6A4 C 1.0839(19) 0.1361(15) 0.1428(8) 0.085(8) Uiso 0.460(19) 1 d PDU . 2 H6A7 H 1.1298 0.1161 0.1780 0.102 Uiso 0.460(19) 1 calc PR . 2 H6A8 H 1.0325 0.1887 0.1536 0.102 Uiso 0.460(19) 1 calc PR . 2 Li7 Li 0.8731(10) -0.2796(7) 0.2592(6) 0.059(4) Uani 1 1 d . . . O7 O 0.9723(4) -0.3546(3) 0.3075(3) 0.0848(18) Uani 1 1 d DU . . C701 C 0.9873(9) -0.3533(7) 0.3755(5) 0.068(4) Uiso 0.627(8) 1 d PDU . 1 H70A H 0.9299 -0.3829 0.4041 0.082 Uiso 0.627(8) 1 calc PR . 1 H70B H 0.9786 -0.2967 0.3888 0.082 Uiso 0.627(8) 1 calc PR . 1 C702 C 1.1126(11) -0.3973(8) 0.3744(6) 0.093(5) Uiso 0.627(8) 1 d PDU . 1 H70C H 1.1224 -0.4276 0.4157 0.112 Uiso 0.627(8) 1 calc PR . 1 H70D H 1.1696 -0.3580 0.3656 0.112 Uiso 0.627(8) 1 calc PR . 1 C703 C 1.1328(14) -0.4569(9) 0.3202(7) 0.084(5) Uiso 0.627(8) 1 d PDU . 1 H70E H 1.2134 -0.4591 0.2954 0.100 Uiso 0.627(8) 1 calc PR . 1 H70F H 1.1212 -0.5128 0.3371 0.100 Uiso 0.627(8) 1 calc PR . 1 C704 C 1.0442(11) -0.4213(8) 0.2831(6) 0.086(5) Uiso 0.627(8) 1 d PDU . 1 H70G H 1.0833 -0.4056 0.2400 0.103 Uiso 0.627(8) 1 calc PR . 1 H70H H 0.9947 -0.4629 0.2784 0.103 Uiso 0.627(8) 1 calc PR . 1 C7A1 C 0.9630(15) -0.4189(12) 0.3447(10) 0.088(8) Uiso 0.373(8) 1 d PDU . 2 H7A1 H 0.9245 -0.4569 0.3247 0.106 Uiso 0.373(8) 1 calc PR . 2 H7A2 H 0.9124 -0.4035 0.3854 0.106 Uiso 0.373(8) 1 calc PR . 2 C7A2 C 1.0806(15) -0.4600(12) 0.3573(10) 0.066(7) Uiso 0.373(8) 1 d PDU . 2 H7A3 H 1.0906 -0.5191 0.3506 0.079 Uiso 0.373(8) 1 calc PR . 2 H7A4 H 1.0902 -0.4535 0.4019 0.079 Uiso 0.373(8) 1 calc PR . 2 C7A3 C 1.1692(14) -0.4211(14) 0.3124(10) 0.085(9) Uiso 0.373(8) 1 d PDU . 2 H7A5 H 1.2170 -0.3935 0.3358 0.103 Uiso 0.373(8) 1 calc PR . 2 H7A6 H 1.2233 -0.4624 0.2862 0.103 Uiso 0.373(8) 1 calc PR . 2 C7A4 C 1.1031(11) -0.3634(9) 0.2734(7) 0.036(5) Uiso 0.373(8) 1 d PDU . 2 H7A7 H 1.1098 -0.3832 0.2303 0.043 Uiso 0.373(8) 1 calc PR . 2 H7A8 H 1.1321 -0.3102 0.2696 0.043 Uiso 0.373(8) 1 calc PR . 2 Li8 Li 0.6558(11) -0.2098(7) 0.2336(6) 0.064(4) Uani 1 1 d . . . O8 O 0.5118(7) -0.1712(5) 0.2049(5) 0.046(3) Uiso 0.514(8) 1 d PDU . 1 C801 C 0.4508(12) -0.2239(7) 0.1763(7) 0.051(4) Uiso 0.514(8) 1 d PDU . 1 H80A H 0.3909 -0.2461 0.2087 0.062 Uiso 0.514(8) 1 calc PR . 1 H80B H 0.5080 -0.2703 0.1578 0.062 Uiso 0.514(8) 1 calc PR . 1 C802 C 0.3926(13) -0.1748(8) 0.1263(6) 0.075(5) Uiso 0.514(8) 1 d PDU . 1 H80C H 0.3215 -0.1964 0.1191 0.090 Uiso 0.514(8) 1 calc PR . 1 H80D H 0.4478 -0.1724 0.0857 0.090 Uiso 0.514(8) 1 calc PR . 1 C803 C 0.3603(11) -0.0943(7) 0.1540(7) 0.050(4) Uiso 0.514(8) 1 d PDU . 1 H80E H 0.2859 -0.0918 0.1848 0.060 Uiso 0.514(8) 1 calc PR . 1 H80F H 0.3498 -0.0500 0.1203 0.060 Uiso 0.514(8) 1 calc PR . 1 C804 C 0.4633(11) -0.0875(7) 0.1868(7) 0.050(4) Uiso 0.514(8) 1 d PDU . 1 H80G H 0.5236 -0.0611 0.1576 0.060 Uiso 0.514(8) 1 calc PR . 1 H80H H 0.4367 -0.0550 0.2248 0.060 Uiso 0.514(8) 1 calc PR . 1 O8A O 0.4880(8) -0.1710(6) 0.2438(6) 0.053(3) Uiso 0.486(8) 1 d PDU . 2 C8A1 C 0.4120(15) -0.2226(9) 0.2282(11) 0.112(7) Uiso 0.486(8) 1 d PDU . 2 H8A1 H 0.3841 -0.2561 0.2665 0.135 Uiso 0.486(8) 1 calc PR . 2 H8A2 H 0.4560 -0.2600 0.1955 0.135 Uiso 0.486(8) 1 calc PR . 2 C8A2 C 0.3126(14) -0.1734(9) 0.2044(9) 0.105(7) Uiso 0.486(8) 1 d PDU . 2 H8A3 H 0.2389 -0.1760 0.2351 0.126 Uiso 0.486(8) 1 calc PR . 2 H8A4 H 0.3020 -0.1925 0.1632 0.126 Uiso 0.486(8) 1 calc PR . 2 C8A3 C 0.3399(14) -0.0884(9) 0.1959(9) 0.088(6) Uiso 0.486(8) 1 d PDU . 2 H8A5 H 0.2693 -0.0490 0.2124 0.106 Uiso 0.486(8) 1 calc PR . 2 H8A6 H 0.3642 -0.0735 0.1503 0.106 Uiso 0.486(8) 1 calc PR . 2 C8A4 C 0.4390(13) -0.0877(7) 0.2328(8) 0.067(5) Uiso 0.486(8) 1 d PDU . 2 H8A7 H 0.4996 -0.0572 0.2081 0.080 Uiso 0.486(8) 1 calc PR . 2 H8A8 H 0.4088 -0.0617 0.2736 0.080 Uiso 0.486(8) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0380(12) 0.0335(11) 0.0656(15) 0.0043(11) -0.0114(11) -0.0092(10) N1 0.038(4) 0.032(3) 0.054(4) -0.001(3) -0.003(3) -0.003(3) C11 0.039(5) 0.036(5) 0.052(5) 0.005(4) -0.017(4) -0.005(4) C12 0.042(5) 0.045(5) 0.065(5) 0.006(4) -0.015(4) -0.005(4) C13 0.044(5) 0.048(5) 0.082(6) 0.013(5) -0.006(5) -0.014(4) C14 0.057(6) 0.060(6) 0.069(6) 0.016(5) 0.008(5) -0.011(5) C15 0.092(7) 0.068(6) 0.075(7) -0.008(5) 0.005(6) -0.018(6) C16 0.066(6) 0.055(5) 0.058(6) -0.001(5) -0.010(5) -0.014(5) N2 0.040(4) 0.033(3) 0.063(4) 0.006(3) -0.012(3) -0.010(3) C21 0.042(5) 0.044(5) 0.060(6) 0.013(5) -0.026(5) -0.013(5) C22 0.051(5) 0.058(5) 0.080(6) 0.024(5) -0.016(5) -0.014(5) C23 0.065(6) 0.087(7) 0.078(7) 0.036(6) -0.015(6) -0.039(6) C24 0.058(6) 0.108(8) 0.071(6) 0.026(7) -0.008(5) -0.018(6) C25 0.058(6) 0.084(7) 0.062(6) 0.006(5) -0.009(5) 0.004(5) C26 0.040(5) 0.058(6) 0.051(5) 0.018(4) -0.006(4) -0.005(5) N3 0.046(4) 0.034(3) 0.065(4) 0.000(3) -0.016(3) -0.009(3) C31 0.041(5) 0.056(5) 0.073(6) -0.011(5) -0.008(5) -0.016(4) C32 0.047(5) 0.061(6) 0.052(5) 0.001(4) -0.014(4) -0.009(4) C33 0.059(6) 0.075(6) 0.069(6) 0.009(5) -0.019(5) -0.002(5) C34 0.052(6) 0.119(8) 0.072(6) 0.000(7) -0.031(5) -0.011(6) C35 0.060(7) 0.131(9) 0.097(8) -0.025(8) -0.022(6) -0.031(7) C36 0.056(6) 0.066(6) 0.106(7) -0.024(6) -0.023(5) -0.012(5) N4 0.035(4) 0.032(3) 0.077(4) 0.008(3) -0.017(3) -0.006(3) C41 0.038(5) 0.040(5) 0.065(5) 0.008(4) -0.011(4) -0.009(4) C42 0.052(5) 0.031(5) 0.137(8) 0.003(5) -0.038(5) -0.010(4) C43 0.052(6) 0.046(5) 0.148(8) 0.009(5) -0.044(6) -0.005(5) C44 0.044(5) 0.059(6) 0.102(7) 0.009(5) -0.028(5) -0.009(5) C45 0.050(5) 0.051(5) 0.063(5) 0.005(4) -0.016(4) -0.022(4) C46 0.051(5) 0.042(5) 0.059(5) 0.011(4) -0.006(4) -0.015(4) P2 0.0430(12) 0.0416(12) 0.0497(13) 0.0044(11) -0.0152(11) -0.0078(11) N5 0.047(4) 0.036(4) 0.046(4) -0.006(3) -0.008(3) 0.008(3) C51 0.065(6) 0.070(6) 0.046(6) -0.009(6) -0.026(5) 0.016(6) C52 0.061(6) 0.087(7) 0.068(6) 0.020(6) -0.011(5) 0.004(6) C53 0.102(8) 0.137(10) 0.072(8) 0.033(7) 0.030(7) 0.031(8) C54 0.121(10) 0.181(13) 0.063(8) 0.034(9) 0.010(7) 0.076(10) C55 0.150(11) 0.125(10) 0.048(7) -0.004(7) -0.021(7) 0.069(9) C56 0.105(8) 0.082(7) 0.050(6) -0.008(5) -0.017(6) 0.026(6) N6 0.038(4) 0.032(3) 0.054(4) -0.007(3) -0.003(3) -0.001(3) C61 0.035(5) 0.040(5) 0.057(5) 0.007(4) -0.015(4) -0.012(4) C62 0.052(5) 0.039(5) 0.068(6) -0.007(5) 0.006(5) -0.004(4) C63 0.067(6) 0.052(6) 0.085(7) -0.008(6) -0.007(5) 0.002(5) C64 0.055(6) 0.088(7) 0.063(6) -0.017(6) 0.005(5) -0.005(6) C65 0.076(7) 0.071(7) 0.062(6) 0.007(5) -0.005(5) -0.020(6) C66 0.063(6) 0.045(5) 0.056(6) 0.000(5) -0.008(5) -0.011(5) N8 0.055(4) 0.046(4) 0.042(4) 0.000(3) -0.023(3) -0.001(3) Cl1 0.0616(13) 0.0338(11) 0.0842(15) 0.0052(11) -0.0235(12) -0.0102(10) Cl2 0.0533(12) 0.0339(11) 0.0804(14) 0.0065(10) -0.0203(11) -0.0145(9) Li1 0.058(9) 0.048(8) 0.079(10) -0.010(7) -0.022(8) -0.011(7) O1 0.045(3) 0.042(3) 0.087(4) 0.006(3) -0.024(3) -0.010(2) Li2 0.059(9) 0.054(8) 0.085(10) 0.004(8) -0.017(8) -0.016(7) O2 0.085(4) 0.052(3) 0.075(4) 0.011(3) -0.034(3) -0.030(3) Li3 0.061(9) 0.040(7) 0.074(9) 0.002(7) -0.007(8) -0.009(7) O3 0.076(4) 0.061(4) 0.065(4) 0.000(3) 0.010(3) 0.014(3) Li4 0.054(8) 0.055(8) 0.072(9) -0.003(7) -0.017(7) -0.005(7) O4 0.078(4) 0.059(3) 0.066(3) 0.019(3) -0.027(3) -0.025(3) Li5 0.092(11) 0.058(9) 0.071(10) -0.014(8) -0.017(8) -0.028(8) Li6 0.070(9) 0.071(9) 0.067(9) 0.033(8) -0.034(8) -0.022(8) O6 0.113(5) 0.093(4) 0.054(4) 0.024(3) -0.025(3) -0.051(4) Li7 0.052(8) 0.050(8) 0.075(9) -0.006(7) -0.018(7) -0.001(7) O7 0.074(4) 0.059(3) 0.131(5) -0.031(4) -0.059(4) 0.018(3) Li8 0.066(9) 0.034(7) 0.096(11) -0.003(7) -0.027(8) -0.005(7) _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 P1 N2 1.609(5) . ? P1 N3 1.611(5) . ? P1 N1 1.632(5) . ? P1 N4 1.644(5) . ? P1 Li2 2.608(12) . ? P1 Li3 2.665(11) . ? P1 Li1 3.078(12) . ? P1 Li4 3.120(12) . ? N1 C11 1.396(7) . ? N1 Li2 2.005(13) . ? N1 Li1 2.017(13) . ? C11 C16 1.363(8) . ? C11 C12 1.408(8) . ? C11 Li1 2.615(14) . ? C12 C13 1.398(8) . ? C12 Li4 2.426(13) . ? C13 C14 1.339(9) . ? C14 C15 1.362(9) . ? C15 C16 1.379(9) . ? N2 C21 1.368(8) . ? N2 Li2 1.923(14) . ? C21 C26 1.386(9) . ? C21 C22 1.402(9) . ? C22 C23 1.352(9) . ? C23 C24 1.382(10) . ? C24 C25 1.359(10) . ? C25 C26 1.372(9) . ? N3 C31 1.374(8) . ? N3 Li3 1.964(12) . ? C31 C32 1.391(9) . ? C31 C36 1.404(9) . ? C32 C33 1.379(9) . ? C32 Li1 2.582(14) . ? C33 C34 1.361(9) . ? C34 C35 1.367(10) . ? C35 C36 1.374(10) . ? N4 C41 1.369(7) . ? N4 Li4 2.024(13) . ? N4 Li3 2.035(13) . ? C41 C46 1.388(8) . ? C41 C42 1.410(9) . ? C41 Li4 2.634(13) . ? C42 C43 1.355(9) . ? C43 C44 1.366(9) . ? C44 C45 1.356(9) . ? C45 C46 1.383(8) . ? P2 N7' 1.585(12) . ? P2 N5 1.610(5) . ? P2 N8 1.628(5) . ? P2 N6 1.648(5) . ? P2 N7 1.687(14) . ? P2 Li7 2.654(12) . ? P2 Li6 2.654(12) . ? P2 Li8 3.085(12) . ? N5 C51 1.364(8) . ? N5 Li7 1.967(13) . ? C51 C52 1.381(9) . ? C51 C56 1.391(8) . ? C52 C53 1.365(9) . ? C53 C54 1.355(10) . ? C54 C55 1.347(11) . ? C55 C56 1.355(9) . ? N6 C61 1.365(7) . ? N6 Li8 1.985(12) . ? N6 Li7 2.052(12) . ? C61 C66 1.392(7) . ? C61 C62 1.392(8) . ? C61 Li8 2.531(14) . ? C62 C63 1.376(8) . ? C62 Li5 2.532(14) . ? C63 C64 1.355(8) . ? C64 C65 1.356(8) . ? C65 C66 1.361(8) . ? N7 C71 1.351(12) . ? N7 Li5 1.800(19) . ? N7 Li6 2.058(17) . ? C71 C76 1.392(12) . ? C71 C72 1.401(12) . ? C71 Li5 2.28(2) . ? C72 C73 1.370(12) . ? C73 C74 1.370(12) . ? C74 C75 1.381(13) . ? C75 C76 1.377(12) . ? C76 Li5 2.69(2) . ? N7' C71' 1.351(11) . ? N7' Li6 2.031(17) . ? N7' Li5 2.15(2) . ? C71' C72' 1.392(11) . ? C71' C76' 1.397(11) . ? C71' Li5 2.743(19) . ? C72' C73' 1.388(12) . ? C73' C74' 1.380(12) . ? C74' C75' 1.370(12) . ? C75' C76' 1.352(11) . ? N8 C81 1.335(10) . ? N8 C81' 1.399(11) . ? N8 Li6 1.960(13) . ? C81 C82 1.388(12) . ? C81 C86 1.408(11) . ? C82 C83 1.382(11) . ? C83 C84 1.378(12) . ? C84 C85 1.353(12) . ? C85 C86 1.351(11) . ? C81' C82' 1.393(12) . ? C81' C86' 1.414(13) . ? C82' C83' 1.383(12) . ? C82' Li8 2.41(2) . ? C83' C84' 1.358(13) . ? C84' C85' 1.359(13) . ? C85' C86' 1.375(13) . ? Cl1 Li5 2.320(13) . ? Cl1 Li1 2.348(11) . ? Cl1 Li2 2.447(12) . ? Cl1 Li6 2.516(14) . ? Cl2 Li8 2.301(11) 1_565 ? Cl2 Li4 2.331(12) . ? Cl2 Li7 2.418(12) 1_565 ? Cl2 Li3 2.494(11) . ? Li1 O1 1.865(12) . ? Li1 Li2 2.742(16) . ? O1 C1A4 1.403(13) . ? O1 C101 1.419(9) . ? O1 C104 1.445(8) . ? O1 C1A1 1.471(14) . ? C101 C102 1.485(11) . ? C102 C103 1.496(10) . ? C103 C104 1.463(10) . ? C1A1 C1A2 1.494(16) . ? C1A2 C1A3 1.492(15) . ? C1A3 C1A4 1.486(15) . ? Li2 O2 1.909(13) . ? O2 C204 1.391(12) . ? O2 C2A1 1.408(11) . ? O2 C201 1.416(12) . ? O2 C2A4 1.421(12) . ? C201 C202 1.509(13) . ? C202 C203 1.495(14) . ? C203 C204 1.489(14) . ? C2A1 C2A2 1.482(12) . ? C2A2 C2A3 1.490(14) . ? C2A3 C2A4 1.466(13) . ? Li3 O3 1.857(13) . ? Li3 Li4 2.763(17) . ? O3 C3A1 1.396(14) . ? O3 C304 1.395(9) . ? O3 C301 1.414(9) . ? O3 C3A4 1.442(15) . ? C301 C302 1.465(10) . ? C302 C303 1.523(12) . ? C303 C304 1.460(10) . ? C3A1 C3A2 1.492(15) . ? C3A2 C3A3 1.510(16) . ? C3A3 C3A4 1.464(15) . ? Li4 O4 1.861(13) . ? O4 C4A4 1.417(14) . ? O4 C4A1 1.429(14) . ? O4 C401 1.440(10) . ? O4 C404 1.444(10) . ? C401 C402 1.520(12) . ? C402 C403 1.520(12) . ? C403 C404 1.475(11) . ? C4A1 C4A2 1.480(15) . ? C4A2 C4A3 1.493(16) . ? C4A3 C4A4 1.497(15) . ? Li5 O5 1.899(16) . ? Li5 O5A 1.909(16) . ? Li5 Li6 2.765(18) . ? O5 C501 1.414(13) . ? O5 C504 1.413(11) . ? C501 C502 1.482(13) . ? C502 C503 1.499(13) . ? C503 C504 1.483(12) . ? O5A C5A4 1.425(12) . ? O5A C5A1 1.445(12) . ? C5A1 C5A2 1.496(12) . ? C5A2 C5A3 1.484(13) . ? C5A3 C5A4 1.493(13) . ? Li6 O6 1.877(13) . ? O6 C604 1.417(11) . ? O6 C6A1 1.426(12) . ? O6 C6A4 1.434(13) . ? O6 C601 1.442(11) . ? C601 C602 1.549(13) . ? C602 C603 1.467(12) . ? C603 C604 1.511(13) . ? C6A1 C6A2 1.524(14) . ? C6A2 C6A3 1.487(14) . ? C6A3 C6A4 1.543(15) . ? Li7 O7 1.899(12) . ? Li7 Cl2 2.418(12) 1_545 ? Li7 Li8 2.700(17) . ? O7 C7A1 1.284(13) . ? O7 C704 1.355(10) . ? O7 C701 1.488(10) . ? O7 C7A4 1.556(11) . ? C701 C702 1.504(11) . ? C702 C703 1.549(12) . ? C703 C704 1.415(11) . ? C7A1 C7A2 1.469(14) . ? C7A2 C7A3 1.478(15) . ? C7A3 C7A4 1.419(14) . ? Li8 O8 1.858(14) . ? Li8 O8A 1.918(15) . ? Li8 Cl2 2.301(11) 1_545 ? O8 C801 1.442(10) . ? O8 C804 1.454(11) . ? C801 C802 1.466(12) . ? C802 C803 1.472(12) . ? C803 C804 1.500(12) . ? O8A C8A4 1.419(11) . ? O8A C8A1 1.421(12) . ? C8A1 C8A2 1.430(13) . ? C8A2 C8A3 1.490(13) . ? C8A3 C8A4 1.492(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 N2 P1 N3 117.4(3) . . ? N2 P1 N1 96.5(3) . . ? N3 P1 N1 115.2(3) . . ? N2 P1 N4 119.9(3) . . ? N3 P1 N4 96.7(3) . . ? N1 P1 N4 112.5(3) . . ? N2 P1 Li2 47.3(3) . . ? N3 P1 Li2 139.9(3) . . ? N1 P1 Li2 50.2(3) . . ? N4 P1 Li2 123.4(4) . . ? N2 P1 Li3 132.3(3) . . ? N3 P1 Li3 47.1(3) . . ? N1 P1 Li3 131.2(3) . . ? N4 P1 Li3 49.7(3) . . ? Li2 P1 Li3 173.0(4) . . ? N2 P1 Li1 86.6(3) . . ? N3 P1 Li1 89.3(3) . . ? N1 P1 Li1 36.6(3) . . ? N4 P1 Li1 145.0(3) . . ? Li2 P1 Li1 56.9(3) . . ? Li3 P1 Li1 129.0(3) . . ? N2 P1 Li4 148.1(3) . . ? N3 P1 Li4 90.5(3) . . ? N1 P1 Li4 83.9(3) . . ? N4 P1 Li4 35.6(3) . . ? Li2 P1 Li4 119.6(4) . . ? Li3 P1 Li4 56.4(3) . . ? Li1 P1 Li4 110.3(3) . . ? C11 N1 P1 121.2(4) . . ? C11 N1 Li2 140.7(6) . . ? P1 N1 Li2 91.0(4) . . ? C11 N1 Li1 98.4(5) . . ? P1 N1 Li1 114.6(5) . . ? Li2 N1 Li1 86.0(5) . . ? C16 C11 N1 120.0(7) . . ? C16 C11 C12 117.1(7) . . ? N1 C11 C12 122.8(7) . . ? C16 C11 Li1 106.9(5) . . ? N1 C11 Li1 49.7(4) . . ? C12 C11 Li1 109.8(5) . . ? C13 C12 C11 120.0(7) . . ? C13 C12 Li4 99.1(5) . . ? C11 C12 Li4 92.3(5) . . ? C14 C13 C12 121.2(7) . . ? C13 C14 C15 118.9(8) . . ? C14 C15 C16 121.3(8) . . ? C11 C16 C15 121.4(7) . . ? C21 N2 P1 124.6(5) . . ? C21 N2 Li2 140.1(6) . . ? P1 N2 Li2 94.8(5) . . ? N2 C21 C26 126.3(7) . . ? N2 C21 C22 118.7(7) . . ? C26 C21 C22 115.0(7) . . ? C23 C22 C21 122.3(8) . . ? C22 C23 C24 121.6(8) . . ? C25 C24 C23 117.0(8) . . ? C24 C25 C26 122.0(8) . . ? C25 C26 C21 122.0(7) . . ? C31 N3 P1 121.8(5) . . ? C31 N3 Li3 142.3(6) . . ? P1 N3 Li3 95.9(5) . . ? N3 C31 C32 126.5(7) . . ? N3 C31 C36 118.3(7) . . ? C32 C31 C36 115.2(7) . . ? C33 C32 C31 121.2(7) . . ? C33 C32 Li1 108.3(6) . . ? C31 C32 Li1 99.6(5) . . ? C34 C33 C32 122.1(8) . . ? C33 C34 C35 118.4(8) . . ? C34 C35 C36 120.1(8) . . ? C35 C36 C31 122.9(8) . . ? C41 N4 P1 125.6(4) . . ? C41 N4 Li4 100.1(5) . . ? P1 N4 Li4 116.2(4) . . ? C41 N4 Li3 131.5(5) . . ? P1 N4 Li3 92.2(4) . . ? Li4 N4 Li3 85.8(5) . . ? N4 C41 C46 128.0(6) . . ? N4 C41 C42 117.2(6) . . ? C46 C41 C42 114.7(7) . . ? N4 C41 Li4 49.2(4) . . ? C46 C41 Li4 136.2(6) . . ? C42 C41 Li4 85.0(5) . . ? C43 C42 C41 122.8(7) . . ? C42 C43 C44 121.3(7) . . ? C45 C44 C43 117.6(7) . . ? C44 C45 C46 122.2(7) . . ? C45 C46 C41 121.3(7) . . ? N7' P2 N5 114.8(5) . . ? N7' P2 N8 97.1(5) . . ? N5 P2 N8 117.0(3) . . ? N7' P2 N6 116.9(5) . . ? N5 P2 N6 96.9(3) . . ? N8 P2 N6 115.4(3) . . ? N7' P2 N7 12.2(8) . . ? N5 P2 N7 124.8(5) . . ? N8 P2 N7 96.6(5) . . ? N6 P2 N7 106.8(5) . . ? N7' P2 Li7 122.0(5) . . ? N5 P2 Li7 47.6(3) . . ? N8 P2 Li7 140.9(3) . . ? N6 P2 Li7 50.6(3) . . ? N7 P2 Li7 121.9(5) . . ? N7' P2 Li6 49.8(5) . . ? N5 P2 Li6 130.1(4) . . ? N8 P2 Li6 47.3(3) . . ? N6 P2 Li6 133.0(4) . . ? N7 P2 Li6 50.9(5) . . ? Li7 P2 Li6 171.3(4) . . ? N7' P2 Li8 150.3(6) . . ? N5 P2 Li8 85.5(3) . . ? N8 P2 Li8 91.8(3) . . ? N6 P2 Li8 35.3(3) . . ? N7 P2 Li8 138.6(6) . . ? Li7 P2 Li8 55.5(3) . . ? Li6 P2 Li8 132.7(3) . . ? C51 N5 P2 125.6(5) . . ? C51 N5 Li7 139.1(6) . . ? P2 N5 Li7 95.3(4) . . ? N5 C51 C52 125.6(8) . . ? N5 C51 C56 118.2(8) . . ? C52 C51 C56 116.2(8) . . ? C53 C52 C51 120.1(9) . . ? C54 C53 C52 122.0(10) . . ? C55 C54 C53 119.1(11) . . ? C54 C55 C56 119.9(10) . . ? C55 C56 C51 122.6(9) . . ? C61 N6 P2 122.2(4) . . ? C61 N6 Li8 96.4(5) . . ? P2 N6 Li8 116.0(5) . . ? C61 N6 Li7 141.5(6) . . ? P2 N6 Li7 91.0(4) . . ? Li8 N6 Li7 84.0(5) . . ? N6 C61 C66 119.7(6) . . ? N6 C61 C62 125.0(7) . . ? C66 C61 C62 115.2(7) . . ? N6 C61 Li8 51.2(4) . . ? C66 C61 Li8 99.7(5) . . ? C62 C61 Li8 116.9(5) . . ? C63 C62 C61 122.2(7) . . ? C63 C62 Li5 104.6(5) . . ? C61 C62 Li5 95.8(5) . . ? C64 C63 C62 120.5(7) . . ? C63 C64 C65 118.9(8) . . ? C64 C65 C66 121.3(8) . . ? C65 C66 C61 122.0(7) . . ? C71 N7 P2 122.5(11) . . ? C71 N7 Li5 91.6(11) . . ? P2 N7 Li5 127.4(9) . . ? C71 N7 Li6 135.1(11) . . ? P2 N7 Li6 89.7(7) . . ? Li5 N7 Li6 91.3(8) . . ? N7 C71 C76 119.8(12) . . ? N7 C71 C72 126.2(12) . . ? C76 C71 C72 113.7(11) . . ? N7 C71 Li5 52.1(9) . . ? C76 C71 Li5 90.8(10) . . ? C72 C71 Li5 123.9(12) . . ? C73 C72 C71 123.7(12) . . ? C74 C73 C72 120.0(12) . . ? C73 C74 C75 119.0(13) . . ? C76 C75 C74 119.4(14) . . ? C75 C76 C71 123.9(13) . . ? C75 C76 Li5 138.8(13) . . ? C71 C76 Li5 58.0(8) . . ? C71' N7' P2 129.3(11) . . ? C71' N7' Li6 128.4(11) . . ? P2 N7' Li6 93.6(6) . . ? C71' N7' Li5 100.8(10) . . ? P2 N7' Li5 112.8(8) . . ? Li6 N7' Li5 82.8(7) . . ? N7' C71' C72' 126.5(11) . . ? N7' C71' C76' 118.7(11) . . ? C72' C71' C76' 114.7(10) . . ? N7' C71' Li5 50.3(8) . . ? C72' C71' Li5 138.3(10) . . ? C76' C71' Li5 85.6(8) . . ? C73' C72' C71' 120.9(11) . . ? C74' C73' C72' 121.3(12) . . ? C75' C74' C73' 118.9(12) . . ? C76' C75' C74' 118.9(11) . . ? C75' C76' C71' 125.2(11) . . ? C81 N8 C81' 22.2(9) . . ? C81 N8 P2 129.9(6) . . ? C81' N8 P2 115.8(7) . . ? C81 N8 Li6 131.9(8) . . ? C81' N8 Li6 149.1(8) . . ? P2 N8 Li6 95.0(4) . . ? N8 C81 C82 123.4(10) . . ? N8 C81 C86 121.3(10) . . ? C82 C81 C86 114.8(10) . . ? C83 C82 C81 122.2(11) . . ? C84 C83 C82 119.9(12) . . ? C85 C84 C83 119.4(11) . . ? C86 C85 C84 120.6(11) . . ? C85 C86 C81 123.1(11) . . ? C82' C81' N8 129.5(11) . . ? C82' C81' C86' 113.8(11) . . ? N8 C81' C86' 116.5(11) . . ? C83' C82' C81' 123.0(12) . . ? C83' C82' Li8 108.1(10) . . ? C81' C82' Li8 105.2(10) . . ? C84' C83' C82' 120.4(12) . . ? C83' C84' C85' 119.5(13) . . ? C84' C85' C86' 120.3(14) . . ? C85' C86' C81' 122.8(13) . . ? Li5 Cl1 Li1 136.2(4) . . ? Li5 Cl1 Li2 142.0(5) . . ? Li1 Cl1 Li2 69.7(4) . . ? Li5 Cl1 Li6 69.6(4) . . ? Li1 Cl1 Li6 127.3(4) . . ? Li2 Cl1 Li6 121.6(4) . . ? Li8 Cl2 Li4 138.0(4) 1_565 . ? Li8 Cl2 Li7 69.7(4) 1_565 1_565 ? Li4 Cl2 Li7 139.8(4) . 1_565 ? Li8 Cl2 Li3 125.8(4) 1_565 . ? Li4 Cl2 Li3 69.8(4) . . ? Li7 Cl2 Li3 123.0(4) 1_565 . ? O1 Li1 N1 134.9(7) . . ? O1 Li1 Cl1 113.4(6) . . ? N1 Li1 Cl1 101.9(5) . . ? O1 Li1 C32 100.6(5) . . ? N1 Li1 C32 94.1(5) . . ? Cl1 Li1 C32 107.6(5) . . ? O1 Li1 C11 103.9(5) . . ? N1 Li1 C11 31.9(3) . . ? Cl1 Li1 C11 118.3(5) . . ? C32 Li1 C11 111.5(5) . . ? O1 Li1 Li2 163.4(7) . . ? N1 Li1 Li2 46.8(4) . . ? Cl1 Li1 Li2 56.8(3) . . ? C32 Li1 Li2 95.5(5) . . ? C11 Li1 Li2 73.6(4) . . ? O1 Li1 P1 139.1(5) . . ? N1 Li1 P1 28.8(2) . . ? Cl1 Li1 P1 107.5(4) . . ? C32 Li1 P1 65.3(3) . . ? C11 Li1 P1 54.5(3) . . ? Li2 Li1 P1 52.9(3) . . ? C1A4 O1 C101 105.9(9) . . ? C1A4 O1 C104 28.6(12) . . ? C101 O1 C104 109.7(6) . . ? C1A4 O1 C1A1 108.6(11) . . ? C101 O1 C1A1 21.6(12) . . ? C104 O1 C1A1 101.5(11) . . ? C1A4 O1 Li1 131.8(9) . . ? C101 O1 Li1 122.2(6) . . ? C104 O1 Li1 121.6(6) . . ? C1A1 O1 Li1 116.8(8) . . ? O1 C101 C102 104.7(7) . . ? C101 C102 C103 103.4(7) . . ? C104 C103 C102 102.5(7) . . ? O1 C104 C103 106.0(7) . . ? O1 C1A1 C1A2 102.0(12) . . ? C1A3 C1A2 C1A1 102.4(13) . . ? C1A4 C1A3 C1A2 106.4(12) . . ? O1 C1A4 C1A3 106.1(11) . . ? O2 Li2 N2 120.5(7) . . ? O2 Li2 N1 131.5(7) . . ? N2 Li2 N1 75.9(5) . . ? O2 Li2 Cl1 106.5(5) . . ? N2 Li2 Cl1 121.1(6) . . ? N1 Li2 Cl1 99.0(5) . . ? O2 Li2 P1 132.2(6) . . ? N2 Li2 P1 37.9(3) . . ? N1 Li2 P1 38.7(3) . . ? Cl1 Li2 P1 120.8(5) . . ? O2 Li2 Li1 147.8(7) . . ? N2 Li2 Li1 91.4(5) . . ? N1 Li2 Li1 47.2(4) . . ? Cl1 Li2 Li1 53.4(3) . . ? P1 Li2 Li1 70.2(4) . . ? C204 O2 C2A1 122.9(9) . . ? C204 O2 C201 107.0(10) . . ? C2A1 O2 C201 20.7(12) . . ? C204 O2 C2A4 22.9(10) . . ? C2A1 O2 C2A4 107.8(9) . . ? C201 O2 C2A4 97.4(9) . . ? C204 O2 Li2 116.5(9) . . ? C2A1 O2 Li2 119.5(8) . . ? C201 O2 Li2 129.6(8) . . ? C2A4 O2 Li2 132.2(9) . . ? O2 C201 C202 103.9(10) . . ? C203 C202 C201 102.9(11) . . ? C204 C203 C202 106.5(10) . . ? O2 C204 C203 103.5(10) . . ? O2 C2A1 C2A2 109.8(10) . . ? C2A1 C2A2 C2A3 103.3(10) . . ? C2A4 C2A3 C2A2 105.2(10) . . ? O2 C2A4 C2A3 107.0(10) . . ? O3 Li3 N3 119.0(7) . . ? O3 Li3 N4 131.9(7) . . ? N3 Li3 N4 74.9(4) . . ? O3 Li3 Cl2 105.7(5) . . ? N3 Li3 Cl2 125.8(6) . . ? N4 Li3 Cl2 97.9(5) . . ? O3 Li3 P1 133.9(6) . . ? N3 Li3 P1 37.0(3) . . ? N4 Li3 P1 38.0(2) . . ? Cl2 Li3 P1 119.6(5) . . ? O3 Li3 Li4 145.4(6) . . ? N3 Li3 Li4 94.9(5) . . ? N4 Li3 Li4 46.9(4) . . ? Cl2 Li3 Li4 52.3(3) . . ? P1 Li3 Li4 70.1(4) . . ? C3A1 O3 C304 99.7(10) . . ? C3A1 O3 C301 35.5(11) . . ? C304 O3 C301 110.5(7) . . ? C3A1 O3 C3A4 111.6(12) . . ? C304 O3 C3A4 33.4(13) . . ? C301 O3 C3A4 101.6(12) . . ? C3A1 O3 Li3 125.9(9) . . ? C304 O3 Li3 131.3(7) . . ? C301 O3 Li3 116.6(6) . . ? C3A4 O3 Li3 121.0(11) . . ? O3 C301 C302 107.2(8) . . ? C301 C302 C303 104.3(8) . . ? C304 C303 C302 103.6(8) . . ? O3 C304 C303 108.3(8) . . ? O3 C3A1 C3A2 105.7(12) . . ? C3A1 C3A2 C3A3 103.5(13) . . ? C3A4 C3A3 C3A2 103.6(15) . . ? O3 C3A4 C3A3 104.8(14) . . ? O4 Li4 N4 129.0(6) . . ? O4 Li4 Cl2 115.4(6) . . ? N4 Li4 Cl2 103.6(5) . . ? O4 Li4 C12 108.5(6) . . ? N4 Li4 C12 95.2(5) . . ? Cl2 Li4 C12 99.5(5) . . ? O4 Li4 C41 100.1(5) . . ? N4 Li4 C41 30.8(3) . . ? Cl2 Li4 C41 115.4(5) . . ? C12 Li4 C41 118.6(5) . . ? O4 Li4 Li3 160.3(7) . . ? N4 Li4 Li3 47.3(4) . . ? Cl2 Li4 Li3 57.9(4) . . ? C12 Li4 Li3 91.2(5) . . ? C41 Li4 Li3 70.5(4) . . ? O4 Li4 P1 135.4(5) . . ? N4 Li4 P1 28.2(2) . . ? Cl2 Li4 P1 108.9(4) . . ? C12 Li4 P1 67.0(3) . . ? C41 Li4 P1 54.8(3) . . ? Li3 Li4 P1 53.5(3) . . ? C4A4 O4 C4A1 107.7(13) . . ? C4A4 O4 C401 108.8(11) . . ? C4A1 O4 C401 20.4(16) . . ? C4A4 O4 C404 16(2) . . ? C4A1 O4 C404 100.5(12) . . ? C401 O4 C404 107.2(8) . . ? C4A4 O4 Li4 121.8(11) . . ? C4A1 O4 Li4 130.3(10) . . ? C401 O4 Li4 127.0(7) . . ? C404 O4 Li4 125.8(7) . . ? O4 C401 C402 102.9(8) . . ? C401 C402 C403 102.3(9) . . ? C404 C403 C402 105.0(9) . . ? O4 C404 C403 107.9(8) . . ? O4 C4A1 C4A2 104.1(13) . . ? C4A1 C4A2 C4A3 104.3(13) . . ? C4A2 C4A3 C4A4 106.6(13) . . ? O4 C4A4 C4A3 104.2(13) . . ? N7 Li5 O5 141.3(10) . . ? N7 Li5 O5A 115.9(9) . . ? O5 Li5 O5A 26.7(4) . . ? N7 Li5 N7' 2.8(7) . . ? O5 Li5 N7' 141.9(9) . . ? O5A Li5 N7' 116.1(8) . . ? N7 Li5 C71 36.3(5) . . ? O5 Li5 C71 108.1(8) . . ? O5A Li5 C71 81.5(7) . . ? N7' Li5 C71 35.7(5) . . ? N7 Li5 Cl1 106.1(7) . . ? O5 Li5 Cl1 109.8(7) . . ? O5A Li5 Cl1 127.0(6) . . ? N7' Li5 Cl1 104.3(6) . . ? C71 Li5 Cl1 124.1(7) . . ? N7 Li5 C62 91.1(6) . . ? O5 Li5 C62 97.3(6) . . ? O5A Li5 C62 110.8(7) . . ? N7' Li5 C62 93.6(6) . . ? C71 Li5 C62 115.4(6) . . ? Cl1 Li5 C62 98.7(5) . . ? N7 Li5 C76 60.0(6) . . ? O5 Li5 C76 96.4(7) . . ? O5A Li5 C76 72.5(6) . . ? N7' Li5 C76 58.2(6) . . ? C71 Li5 C76 31.2(4) . . ? Cl1 Li5 C76 105.1(6) . . ? C62 Li5 C76 146.6(6) . . ? N7 Li5 C71' 30.2(6) . . ? O5 Li5 C71' 116.8(8) . . ? O5A Li5 C71' 90.2(7) . . ? N7' Li5 C71' 28.9(4) . . ? C71 Li5 C71' 9.7(4) . . ? Cl1 Li5 C71' 115.1(6) . . ? C62 Li5 C71' 116.4(5) . . ? C76 Li5 C71' 31.3(4) . . ? N7 Li5 Li6 48.1(6) . . ? O5 Li5 Li6 166.7(7) . . ? O5A Li5 Li6 154.2(8) . . ? N7' Li5 Li6 46.8(5) . . ? C71 Li5 Li6 77.0(6) . . ? Cl1 Li5 Li6 58.5(4) . . ? C62 Li5 Li6 91.3(5) . . ? C76 Li5 Li6 81.8(6) . . ? C71' Li5 Li6 67.5(5) . . ? C501 O5 C504 107.9(10) . . ? C501 O5 Li5 121.8(10) . . ? C504 O5 Li5 129.8(9) . . ? O5 C501 C502 108.3(11) . . ? C501 C502 C503 105.2(10) . . ? C504 C503 C502 103.1(10) . . ? O5 C504 C503 106.7(9) . . ? C5A4 O5A C5A1 109.7(9) . . ? C5A4 O5A Li5 120.9(10) . . ? C5A1 O5A Li5 118.6(9) . . ? O5A C5A1 C5A2 105.5(10) . . ? C5A3 C5A2 C5A1 103.3(10) . . ? C5A2 C5A3 C5A4 103.0(10) . . ? O5A C5A4 C5A3 105.0(10) . . ? O6 Li6 N8 121.6(7) . . ? O6 Li6 N7' 124.5(8) . . ? N8 Li6 N7' 74.2(6) . . ? O6 Li6 N7 132.4(8) . . ? N8 Li6 N7 76.0(6) . . ? N7' Li6 N7 10.1(7) . . ? O6 Li6 Cl1 107.3(6) . . ? N8 Li6 Cl1 123.3(6) . . ? N7' Li6 Cl1 101.4(7) . . ? N7 Li6 Cl1 92.0(6) . . ? O6 Li6 P2 132.4(7) . . ? N8 Li6 P2 37.7(3) . . ? N7' Li6 P2 36.6(4) . . ? N7 Li6 P2 39.5(4) . . ? Cl1 Li6 P2 118.5(5) . . ? O6 Li6 Li5 141.0(7) . . ? N8 Li6 Li5 95.5(5) . . ? N7' Li6 Li5 50.4(6) . . ? N7 Li6 Li5 40.6(5) . . ? Cl1 Li6 Li5 51.9(4) . . ? P2 Li6 Li5 70.4(4) . . ? C604 O6 C6A1 112.6(9) . . ? C604 O6 C6A4 22.6(12) . . ? C6A1 O6 C6A4 108.1(12) . . ? C604 O6 C601 102.6(11) . . ? C6A1 O6 C601 24.2(11) . . ? C6A4 O6 C601 107.7(9) . . ? C604 O6 Li6 128.7(8) . . ? C6A1 O6 Li6 117.7(8) . . ? C6A4 O6 Li6 123.6(8) . . ? C601 O6 Li6 127.6(8) . . ? O6 C601 C602 97.1(10) . . ? C603 C602 C601 102.0(10) . . ? C602 C603 C604 105.4(9) . . ? O6 C604 C603 102.4(9) . . ? O6 C6A1 C6A2 102.3(11) . . ? C6A3 C6A2 C6A1 107.1(11) . . ? C6A2 C6A3 C6A4 103.9(11) . . ? O6 C6A4 C6A3 101.2(12) . . ? O7 Li7 N5 118.0(6) . . ? O7 Li7 N6 135.4(7) . . ? N5 Li7 N6 74.7(5) . . ? O7 Li7 Cl2 107.5(5) . 1_545 ? N5 Li7 Cl2 120.6(6) . 1_545 ? N6 Li7 Cl2 98.6(5) . 1_545 ? O7 Li7 P2 132.0(6) . . ? N5 Li7 P2 37.2(3) . . ? N6 Li7 P2 38.4(3) . . ? Cl2 Li7 P2 120.5(5) 1_545 . ? O7 Li7 Li8 151.1(7) . . ? N5 Li7 Li8 90.9(5) . . ? N6 Li7 Li8 47.0(4) . . ? Cl2 Li7 Li8 53.1(3) 1_545 . ? P2 Li7 Li8 70.4(4) . . ? C7A1 O7 C704 68.4(10) . . ? C7A1 O7 C701 60.6(11) . . ? C704 O7 C701 108.0(7) . . ? C7A1 O7 C7A4 107.3(10) . . ? C704 O7 C7A4 50.6(7) . . ? C701 O7 C7A4 101.9(8) . . ? C7A1 O7 Li7 137.2(10) . . ? C704 O7 Li7 123.1(7) . . ? C701 O7 Li7 129.0(6) . . ? C7A4 O7 Li7 109.7(7) . . ? O7 C701 C702 101.2(8) . . ? C701 C702 C703 105.3(9) . . ? C704 C703 C702 102.0(9) . . ? O7 C704 C703 114.2(9) . . ? O7 C7A1 C7A2 110.5(12) . . ? C7A1 C7A2 C7A3 106.7(12) . . ? C7A4 C7A3 C7A2 105.9(12) . . ? C7A3 C7A4 O7 105.4(10) . . ? O8 Li8 O8A 25.3(4) . . ? O8 Li8 N6 137.8(7) . . ? O8A Li8 N6 126.6(7) . . ? O8 Li8 Cl2 117.2(6) . 1_545 ? O8A Li8 Cl2 117.7(6) . 1_545 ? N6 Li8 Cl2 104.7(5) . 1_545 ? O8 Li8 C82' 77.5(6) . . ? O8A Li8 C82' 101.0(7) . . ? N6 Li8 C82' 94.2(6) . . ? Cl2 Li8 C82' 108.7(6) 1_545 . ? O8 Li8 C61 112.2(6) . . ? O8A Li8 C61 95.1(6) . . ? N6 Li8 C61 32.4(2) . . ? Cl2 Li8 C61 121.6(5) 1_545 . ? C82' Li8 C61 110.5(5) . . ? O8 Li8 Li7 171.2(8) . . ? O8A Li8 Li7 161.4(8) . . ? N6 Li8 Li7 49.1(4) . . ? Cl2 Li8 Li7 57.2(4) 1_545 . ? C82' Li8 Li7 97.5(6) . . ? C61 Li8 Li7 76.3(4) . . ? O8 Li8 P2 128.1(6) . . ? O8A Li8 P2 133.3(6) . . ? N6 Li8 P2 28.7(2) . . ? Cl2 Li8 P2 108.8(4) 1_545 . ? C82' Li8 P2 65.8(4) . . ? C61 Li8 P2 55.0(3) . . ? Li7 Li8 P2 54.1(3) . . ? C801 O8 C804 107.1(8) . . ? C801 O8 Li8 121.6(8) . . ? C804 O8 Li8 128.2(8) . . ? O8 C801 C802 107.5(9) . . ? C801 C802 C803 101.5(9) . . ? C802 C803 C804 104.2(9) . . ? O8 C804 C803 105.0(8) . . ? C8A4 O8A C8A1 110.2(10) . . ? C8A4 O8A Li8 123.1(9) . . ? C8A1 O8A Li8 118.6(10) . . ? O8A C8A1 C8A2 109.2(11) . . ? C8A1 C8A2 C8A3 106.0(11) . . ? C8A2 C8A3 C8A4 106.0(11) . . ? O8A C8A4 C8A3 105.7(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.264 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.049 #===END