# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Alexander Steiner' 'Mark A. Benson' 'Philip I. Richards' _publ_contact_author_name 'Dr Alexander Steiner' _publ_contact_author_address ; Department of Chemistry Liverpool University Crown Street Liverpool L69 7ZD UNITED KINGDOM ; _publ_contact_author_email A.STEINER@LIV.AC.UK _publ_section_title ; In-situ-complexation of inorganic lithium salts by amphiprotic cyclophosphazenes ; data_3b _database_code_CSD 203806 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H50 Cl2 N9 P3' _chemical_formula_weight 556.48 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0168(17) _cell_length_b 17.140(2) _cell_length_c 13.1283(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.420(2) _cell_angle_gamma 90.00 _cell_volume 3102.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(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 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.387 _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 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 15124 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5471 _reflns_number_gt 3202 _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^)+(0.0522P)^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 5471 _refine_ls_number_parameters 325 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.940 _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 0.4960(3) 0.0977(2) 0.3026(3) 0.0278(10) Uani 1 1 d . . . H11 H 0.4387 0.1188 0.3292 0.033 Uiso 1 1 calc R . . C12 C 0.5307(3) 0.0273(2) 0.3644(3) 0.0345(11) Uani 1 1 d . . . H12A H 0.4777 -0.0106 0.3594 0.052 Uiso 1 1 calc R . . H12B H 0.5522 0.0422 0.4370 0.052 Uiso 1 1 calc R . . H12C H 0.5850 0.0040 0.3376 0.052 Uiso 1 1 calc R . . C13 C 0.5719(3) 0.1601(2) 0.3149(3) 0.0448(12) Uani 1 1 d . . . H13A H 0.6289 0.1412 0.2887 0.067 Uiso 1 1 calc R . . H13B H 0.5906 0.1737 0.3883 0.067 Uiso 1 1 calc R . . H13C H 0.5460 0.2065 0.2756 0.067 Uiso 1 1 calc R . . C21 C 0.2518(3) -0.16261(19) -0.0174(3) 0.0271(10) Uani 1 1 d . . . H21 H 0.1861 -0.1527 -0.0597 0.032 Uiso 1 1 calc R . . C22 C 0.3066(4) -0.2152(2) -0.0788(3) 0.0503(14) Uani 1 1 d . . . H22A H 0.3103 -0.1907 -0.1454 0.075 Uiso 1 1 calc R . . H22B H 0.2728 -0.2654 -0.0910 0.075 Uiso 1 1 calc R . . H22C H 0.3723 -0.2239 -0.0400 0.075 Uiso 1 1 calc R . . C23 C 0.2388(3) -0.1995(2) 0.0833(3) 0.0320(10) Uani 1 1 d . . . H23A H 0.3024 -0.2069 0.1275 0.048 Uiso 1 1 calc R . . H23B H 0.2067 -0.2501 0.0694 0.048 Uiso 1 1 calc R . . H23C H 0.1989 -0.1654 0.1184 0.048 Uiso 1 1 calc R . . C31 C 0.2237(3) 0.0222(2) 0.3451(3) 0.0267(10) Uani 1 1 d . . . H31 H 0.2813 0.0575 0.3610 0.032 Uiso 1 1 calc R . . C32 C 0.1793(3) 0.0164(3) 0.4413(3) 0.0492(13) Uani 1 1 d . . . H32A H 0.1608 0.0686 0.4613 0.074 Uiso 1 1 calc R . . H32B H 0.2265 -0.0061 0.4978 0.074 Uiso 1 1 calc R . . H32C H 0.1216 -0.0169 0.4274 0.074 Uiso 1 1 calc R . . C33 C 0.2593(3) -0.0569(2) 0.3151(3) 0.0373(11) Uani 1 1 d . . . H33A H 0.2041 -0.0927 0.2983 0.056 Uiso 1 1 calc R . . H33B H 0.3060 -0.0781 0.3731 0.056 Uiso 1 1 calc R . . H33C H 0.2906 -0.0510 0.2546 0.056 Uiso 1 1 calc R . . C41 C 0.3431(3) 0.26531(18) 0.0477(3) 0.0216(9) Uani 1 1 d . . . H41 H 0.2905 0.2701 0.0897 0.026 Uiso 1 1 calc R . . C42 C 0.4032(3) 0.33918(19) 0.0615(3) 0.0298(10) Uani 1 1 d . . . H42A H 0.4285 0.3475 0.1353 0.045 Uiso 1 1 calc R . . H42B H 0.3626 0.3836 0.0339 0.045 Uiso 1 1 calc R . . H42C H 0.4574 0.3342 0.0241 0.045 Uiso 1 1 calc R . . C43 C 0.2966(3) 0.2524(2) -0.0640(3) 0.0321(10) Uani 1 1 d . . . H43A H 0.3472 0.2438 -0.1054 0.048 Uiso 1 1 calc R . . H43B H 0.2583 0.2983 -0.0900 0.048 Uiso 1 1 calc R . . H43C H 0.2542 0.2065 -0.0691 0.048 Uiso 1 1 calc R . . C51 C 0.2196(3) -0.00400(19) -0.2188(3) 0.0224(9) Uani 1 1 d . . . H51 H 0.2871 -0.0254 -0.2051 0.027 Uiso 1 1 calc R . . C52 C 0.1553(3) -0.0606(2) -0.2880(3) 0.0456(13) Uani 1 1 d . . . H52A H 0.1552 -0.1110 -0.2528 0.068 Uiso 1 1 calc R . . H52B H 0.1800 -0.0675 -0.3527 0.068 Uiso 1 1 calc R . . H52C H 0.0891 -0.0400 -0.3035 0.068 Uiso 1 1 calc R . . C53 C 0.2221(3) 0.0755(2) -0.2677(3) 0.0280(10) Uani 1 1 d . . . H53A H 0.1569 0.0983 -0.2793 0.042 Uiso 1 1 calc R . . H53B H 0.2442 0.0704 -0.3341 0.042 Uiso 1 1 calc R . . H53C H 0.2668 0.1094 -0.2215 0.042 Uiso 1 1 calc R . . C61 C 0.0754(3) 0.22359(19) 0.1378(3) 0.0279(10) Uani 1 1 d . . . H61 H 0.1384 0.2434 0.1774 0.033 Uiso 1 1 calc R . . C62 C 0.0457(3) 0.2757(2) 0.0446(3) 0.0424(12) Uani 1 1 d . . . H62A H 0.0970 0.2761 0.0028 0.064 Uiso 1 1 calc R . . H62B H 0.0352 0.3289 0.0677 0.064 Uiso 1 1 calc R . . H62C H -0.0145 0.2560 0.0027 0.064 Uiso 1 1 calc R . . C63 C 0.0034(3) 0.2244(2) 0.2083(4) 0.0421(12) Uani 1 1 d . . . H63A H -0.0606 0.2100 0.1694 0.063 Uiso 1 1 calc R . . H63B H 0.0003 0.2768 0.2374 0.063 Uiso 1 1 calc R . . H63C H 0.0230 0.1869 0.2646 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.48140(6) 0.10100(5) -0.12864(7) 0.0230(2) Uani 1 1 d . . . Cl2 Cl 0.01672(6) -0.08941(5) 0.13171(7) 0.0236(2) Uani 1 1 d . . . N1 N 0.3404(2) 0.05967(16) 0.0201(2) 0.0176(7) Uani 1 1 d D . . H1 H 0.378(2) 0.061(2) -0.019(2) 0.021 Uiso 1 1 d D . . N2 N 0.1807(2) 0.01445(15) 0.0746(2) 0.0166(7) Uani 1 1 d D . . H2 H 0.1334(18) -0.0121(17) 0.075(3) 0.020 Uiso 1 1 d D . . N3 N 0.2813(2) 0.12891(15) 0.1778(2) 0.0192(7) Uani 1 1 d . . . N10 N 0.4633(2) 0.07589(16) 0.1926(2) 0.0235(8) Uani 1 1 d D . . H10 H 0.476(3) 0.0321(12) 0.180(3) 0.028 Uiso 1 1 d D . . N20 N 0.3028(2) -0.08750(16) 0.0002(2) 0.0202(7) Uani 1 1 d D . . H20 H 0.3552(17) -0.092(2) 0.038(2) 0.024 Uiso 1 1 d D . . N30 N 0.1531(2) 0.05906(17) 0.2633(2) 0.0216(7) Uani 1 1 d D . . H30 H 0.0990(15) 0.043(2) 0.254(3) 0.026 Uiso 1 1 d D . . N40 N 0.4073(2) 0.20074(16) 0.0898(2) 0.0195(7) Uani 1 1 d D . . H40 H 0.4607(16) 0.200(2) 0.076(3) 0.023 Uiso 1 1 d D . . N50 N 0.1859(2) 0.00338(16) -0.1190(2) 0.0199(7) Uani 1 1 d D . . H50 H 0.1348(17) 0.0276(18) -0.124(3) 0.024 Uiso 1 1 d D . . N60 N 0.0917(2) 0.14369(16) 0.1010(2) 0.0229(8) Uani 1 1 d D . . H60 H 0.065(2) 0.138(2) 0.0428(17) 0.027 Uiso 1 1 d D . . P1 P 0.37039(7) 0.11649(5) 0.12344(7) 0.0182(2) Uani 1 1 d . . . P2 P 0.25204(7) -0.00368(5) -0.00751(7) 0.0171(2) Uani 1 1 d . . . P3 P 0.17951(7) 0.08941(5) 0.15457(7) 0.0185(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 0.036(2) 0.020(2) 0.024(2) -0.0043(17) -0.0026(18) 0.0013(18) C12 0.053(3) 0.029(2) 0.020(2) -0.0017(18) 0.001(2) 0.002(2) C13 0.064(3) 0.036(3) 0.030(3) -0.001(2) -0.001(2) -0.017(2) C21 0.036(3) 0.0109(18) 0.032(3) -0.0040(17) 0.0007(19) -0.0036(17) C22 0.100(4) 0.015(2) 0.045(3) -0.006(2) 0.038(3) 0.002(2) C23 0.037(3) 0.0135(19) 0.048(3) 0.0020(19) 0.016(2) 0.0032(18) C31 0.040(3) 0.023(2) 0.016(2) -0.0002(16) 0.0015(19) -0.0120(18) C32 0.079(4) 0.048(3) 0.021(3) 0.006(2) 0.012(2) -0.012(3) C33 0.055(3) 0.025(2) 0.027(3) 0.0064(19) -0.005(2) -0.001(2) C41 0.029(2) 0.0111(18) 0.024(2) 0.0019(16) 0.0053(18) 0.0033(16) C42 0.048(3) 0.0110(18) 0.030(2) 0.0013(17) 0.008(2) -0.0001(18) C43 0.048(3) 0.018(2) 0.029(2) 0.0026(17) 0.004(2) -0.0002(19) C51 0.033(2) 0.0211(19) 0.014(2) -0.0002(16) 0.0090(17) -0.0014(17) C52 0.090(4) 0.032(2) 0.018(2) -0.0074(19) 0.017(2) -0.027(2) C53 0.041(3) 0.030(2) 0.014(2) -0.0022(17) 0.0050(18) -0.0065(18) C61 0.028(2) 0.015(2) 0.039(3) -0.0121(18) 0.004(2) 0.0001(17) C62 0.053(3) 0.016(2) 0.056(3) 0.004(2) 0.005(2) 0.007(2) C63 0.043(3) 0.030(2) 0.054(3) -0.017(2) 0.010(2) 0.001(2) Cl1 0.0287(6) 0.0180(5) 0.0235(5) 0.0015(4) 0.0079(4) 0.0023(4) Cl2 0.0270(6) 0.0191(5) 0.0251(5) 0.0038(4) 0.0055(4) -0.0019(4) N1 0.025(2) 0.0130(15) 0.0172(18) -0.0013(13) 0.0094(14) -0.0013(13) N2 0.0225(18) 0.0087(15) 0.0202(17) 0.0006(13) 0.0084(15) -0.0047(12) N3 0.0244(18) 0.0158(15) 0.0181(17) 0.0000(13) 0.0062(14) -0.0024(13) N10 0.036(2) 0.0122(16) 0.0203(18) -0.0047(14) 0.0009(15) 0.0024(15) N20 0.0274(19) 0.0092(15) 0.0230(19) 0.0003(13) 0.0016(14) 0.0012(14) N30 0.027(2) 0.0219(17) 0.0172(18) -0.0028(14) 0.0063(16) -0.0060(15) N40 0.0230(19) 0.0083(15) 0.0282(19) 0.0033(13) 0.0069(16) -0.0016(14) N50 0.0246(19) 0.0204(17) 0.0153(17) -0.0007(14) 0.0051(14) 0.0029(14) N60 0.030(2) 0.0156(16) 0.0209(19) -0.0047(14) -0.0016(15) 0.0031(14) P1 0.0275(6) 0.0093(5) 0.0176(5) -0.0008(4) 0.0036(4) -0.0016(4) P2 0.0249(5) 0.0112(5) 0.0156(5) -0.0004(4) 0.0042(4) -0.0007(4) P3 0.0286(6) 0.0124(5) 0.0154(5) -0.0012(4) 0.0065(4) -0.0005(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 C11 N10 1.482(4) . ? C11 C12 1.486(5) . ? C11 C13 1.496(5) . ? C21 N20 1.470(4) . ? C21 C23 1.506(5) . ? C21 C22 1.509(5) . ? C31 N30 1.465(5) . ? C31 C32 1.510(5) . ? C31 C33 1.521(5) . ? C41 N40 1.470(4) . ? C41 C43 1.510(5) . ? C41 C42 1.514(5) . ? C51 N50 1.477(5) . ? C51 C53 1.509(5) . ? C51 C52 1.510(5) . ? C61 N60 1.484(4) . ? C61 C63 1.488(5) . ? C61 C62 1.512(5) . ? N1 P2 1.637(3) . ? N1 P1 1.661(3) . ? N2 P2 1.627(3) . ? N2 P3 1.662(3) . ? N3 P3 1.559(3) . ? N3 P1 1.561(3) . ? N10 P1 1.605(3) . ? N20 P2 1.598(3) . ? N30 P3 1.624(3) . ? N40 P1 1.622(3) . ? N50 P2 1.589(3) . ? N60 P3 1.601(3) . ? 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 N10 C11 C12 109.9(3) . . ? N10 C11 C13 112.0(3) . . ? C12 C11 C13 111.4(3) . . ? N20 C21 C23 111.2(3) . . ? N20 C21 C22 109.1(3) . . ? C23 C21 C22 111.9(3) . . ? N30 C31 C32 108.4(3) . . ? N30 C31 C33 113.8(3) . . ? C32 C31 C33 111.2(3) . . ? N40 C41 C43 112.4(3) . . ? N40 C41 C42 107.2(3) . . ? C43 C41 C42 111.8(3) . . ? N50 C51 C53 109.6(3) . . ? N50 C51 C52 109.7(3) . . ? C53 C51 C52 112.4(3) . . ? N60 C61 C63 111.9(3) . . ? N60 C61 C62 108.5(3) . . ? C63 C61 C62 112.3(3) . . ? P2 N1 P1 129.72(19) . . ? P2 N2 P3 130.12(17) . . ? P3 N3 P1 129.11(19) . . ? C11 N10 P1 121.2(2) . . ? C21 N20 P2 125.4(2) . . ? C31 N30 P3 123.5(3) . . ? C41 N40 P1 124.7(2) . . ? C51 N50 P2 125.7(3) . . ? C61 N60 P3 123.0(3) . . ? N3 P1 N10 115.78(17) . . ? N3 P1 N40 108.89(15) . . ? N10 P1 N40 105.90(16) . . ? N3 P1 N1 110.37(15) . . ? N10 P1 N1 105.50(15) . . ? N40 P1 N1 110.23(15) . . ? N50 P2 N20 107.81(15) . . ? N50 P2 N2 105.63(16) . . ? N20 P2 N2 116.70(16) . . ? N50 P2 N1 116.43(16) . . ? N20 P2 N1 105.78(16) . . ? N2 P2 N1 104.92(15) . . ? N3 P3 N60 115.96(16) . . ? N3 P3 N30 108.23(16) . . ? N60 P3 N30 107.05(17) . . ? N3 P3 N2 110.23(15) . . ? N60 P3 N2 105.46(15) . . ? N30 P3 N2 109.76(15) . . ? 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 0.797(17) 2.33(2) 3.101(3) 164(3) . N2 H2 Cl2 0.806(17) 2.33(2) 3.105(3) 162(3) . N10 H10 Cl1 0.797(18) 2.480(18) 3.276(3) 176(4) 3_655 N20 H20 Cl1 0.813(17) 2.386(19) 3.194(3) 172(4) 3_655 N50 H50 Cl2 0.820(17) 2.359(18) 3.177(3) 175(4) 3 N60 H60 Cl2 0.796(18) 2.507(19) 3.290(3) 168(4) 3 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.669 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.073 #===END data_4a _database_code_CSD 203807 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 Cl2 Li2 N9 O6 P3' _chemical_formula_weight 748.50 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 11.0489(14) _cell_length_b 11.7087(16) _cell_length_c 16.158(2) _cell_angle_alpha 70.746(2) _cell_angle_beta 85.124(2) _cell_angle_gamma 80.226(2) _cell_volume 1943.9(4) _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 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.279 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.337 _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 153(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 8541 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5529 _reflns_number_gt 3684 _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^)+(0.0369P)^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 5529 _refine_ls_number_parameters 433 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _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 Cl1 Cl 1.09158(7) -0.05342(6) 0.41300(5) 0.0270(2) Uani 1 1 d . . . Cl2 Cl 1.05368(8) 0.34669(7) 0.00355(5) 0.0359(2) Uani 1 1 d . . . P1 P 0.95774(7) 0.37415(7) 0.42669(5) 0.0205(2) Uani 1 1 d . . . P2 P 0.98517(7) 0.27584(7) 0.28590(5) 0.0205(2) Uani 1 1 d . . . P3 P 0.92240(7) 0.53231(7) 0.25244(5) 0.0198(2) Uani 1 1 d . . . N1 N 0.9981(2) 0.2638(2) 0.38633(14) 0.0199(6) Uani 1 1 d . . . N2 N 0.9480(2) 0.4123(2) 0.22122(14) 0.0211(6) Uani 1 1 d . . . N3 N 0.9401(2) 0.5065(2) 0.35460(14) 0.0193(6) Uani 1 1 d . . . N10 N 1.0624(2) 0.3528(2) 0.49835(15) 0.0223(6) Uani 1 1 d D . . H10 H 1.043(3) 0.381(3) 0.5358(15) 0.027 Uiso 1 1 d D . . N20 N 1.1115(3) 0.2149(2) 0.24575(16) 0.0244(6) Uani 1 1 d D . . H20 H 1.128(3) 0.1469(17) 0.2745(17) 0.029 Uiso 1 1 d D . . N30 N 1.0069(2) 0.6375(2) 0.19993(15) 0.0224(6) Uani 1 1 d D . . H30 H 0.999(3) 0.656(3) 0.1475(11) 0.027 Uiso 1 1 d D . . N40 N 0.8339(2) 0.3639(2) 0.49184(15) 0.0236(6) Uani 1 1 d D . . H40 H 0.840(3) 0.3014(19) 0.5288(15) 0.028 Uiso 1 1 d D . . N50 N 0.8802(3) 0.1914(2) 0.28345(16) 0.0302(7) Uani 1 1 d D . . H50 H 0.882(3) 0.135(2) 0.3264(14) 0.036 Uiso 1 1 d D . . N60 N 0.7863(2) 0.6014(2) 0.21673(16) 0.0224(6) Uani 1 1 d D . . H60 H 0.733(2) 0.563(2) 0.2226(19) 0.027 Uiso 1 1 d D . . Li1 Li 1.0626(5) 0.1015(4) 0.4784(3) 0.0254(12) Uani 1 1 d . . . Li2 Li 0.9266(5) 0.4533(5) 0.0865(3) 0.0286(13) Uani 1 1 d . . . O1 O 1.21774(18) 0.07558(17) 0.53924(13) 0.0282(5) Uani 1 1 d . . . O2 O 1.4126(2) 0.0450(2) 0.28093(14) 0.0421(6) Uani 1 1 d . . . O3 O 1.1476(2) 0.89393(19) 0.13451(14) 0.0419(6) Uani 1 1 d . . . O4 O 0.55432(19) 0.4845(2) 0.30526(14) 0.0439(6) Uani 1 1 d . . . O5 O 0.7590(2) 0.4141(2) 0.08182(14) 0.0411(6) Uani 1 1 d . . . O6 O 0.5228(2) 0.8262(2) 0.10543(13) 0.0399(6) Uani 1 1 d . . . C11 C 1.1929(3) 0.3428(3) 0.47428(18) 0.0235(7) Uani 1 1 d . . . H11A H 1.2169 0.4256 0.4518 0.028 Uiso 1 1 calc R . . H11B H 1.2089 0.3055 0.4269 0.028 Uiso 1 1 calc R . . C12 C 1.2699(3) 0.2652(3) 0.55250(18) 0.0254(8) Uani 1 1 d . . . H12A H 1.2653 0.3103 0.5952 0.030 Uiso 1 1 calc R . . H12B H 1.3568 0.2521 0.5325 0.030 Uiso 1 1 calc R . . C13 C 1.2282(3) 0.1411(3) 0.59832(18) 0.0264(8) Uani 1 1 d . . . H13A H 1.2878 0.0911 0.6436 0.032 Uiso 1 1 calc R . . H13B H 1.1476 0.1537 0.6283 0.032 Uiso 1 1 calc R . . C14 C 1.3337(3) 0.0300(3) 0.5071(2) 0.0443(10) Uani 1 1 d . . . H14A H 1.3208 -0.0139 0.4671 0.067 Uiso 1 1 calc R . . H14B H 1.3822 -0.0260 0.5564 0.067 Uiso 1 1 calc R . . H14C H 1.3778 0.0985 0.4756 0.067 Uiso 1 1 calc R . . C21 C 1.2247(3) 0.2671(3) 0.2341(2) 0.0334(8) Uani 1 1 d . . . H21A H 1.2630 0.2444 0.2916 0.040 Uiso 1 1 calc R . . H21B H 1.2052 0.3575 0.2113 0.040 Uiso 1 1 calc R . . C22 C 1.3151(3) 0.2227(3) 0.1710(2) 0.0427(9) Uani 1 1 d . . . H22A H 1.2776 0.2491 0.1129 0.051 Uiso 1 1 calc R . . H22B H 1.3894 0.2623 0.1640 0.051 Uiso 1 1 calc R . . C23 C 1.3534(3) 0.0853(3) 0.2001(2) 0.0409(9) Uani 1 1 d . . . H23A H 1.2800 0.0446 0.2062 0.049 Uiso 1 1 calc R . . H23B H 1.4098 0.0626 0.1551 0.049 Uiso 1 1 calc R . . C24 C 1.4341(3) -0.0843(3) 0.3140(2) 0.0522(11) Uani 1 1 d . . . H24A H 1.4754 -0.1107 0.3700 0.078 Uiso 1 1 calc R . . H24B H 1.4862 -0.1162 0.2720 0.078 Uiso 1 1 calc R . . H24C H 1.3555 -0.1157 0.3230 0.078 Uiso 1 1 calc R . . C31 C 1.1285(3) 0.6400(3) 0.2284(2) 0.0280(8) Uani 1 1 d . . . H31A H 1.1865 0.6554 0.1771 0.034 Uiso 1 1 calc R . . H31B H 1.1589 0.5593 0.2708 0.034 Uiso 1 1 calc R . . C32 C 1.1246(3) 0.7383(3) 0.27078(19) 0.0305(8) Uani 1 1 d . . . H32A H 1.0730 0.7178 0.3253 0.037 Uiso 1 1 calc R . . H32B H 1.2088 0.7386 0.2873 0.037 Uiso 1 1 calc R . . C33 C 1.0749(3) 0.8642(3) 0.21274(19) 0.0295(8) Uani 1 1 d . . . H33A H 0.9887 0.8669 0.1989 0.035 Uiso 1 1 calc R . . H33B H 1.0765 0.9246 0.2434 0.035 Uiso 1 1 calc R . . C34 C 1.1066(4) 1.0149(3) 0.0793(2) 0.0550(11) Uani 1 1 d . . . H34A H 1.1583 1.0335 0.0256 0.083 Uiso 1 1 calc R . . H34B H 1.1122 1.0732 0.1101 0.083 Uiso 1 1 calc R . . H34C H 1.0211 1.0215 0.0642 0.083 Uiso 1 1 calc R . . C41 C 0.7110(3) 0.4097(3) 0.45761(19) 0.0277(8) Uani 1 1 d . . . H41A H 0.7132 0.4890 0.4105 0.033 Uiso 1 1 calc R . . H41B H 0.6551 0.4255 0.5052 0.033 Uiso 1 1 calc R . . C42 C 0.6574(3) 0.3256(3) 0.4213(2) 0.0301(8) Uani 1 1 d . . . H42A H 0.7160 0.3039 0.3771 0.036 Uiso 1 1 calc R . . H42B H 0.6473 0.2491 0.4695 0.036 Uiso 1 1 calc R . . C43 C 0.5354(3) 0.3820(3) 0.3798(2) 0.0367(9) Uani 1 1 d . . . H43A H 0.5007 0.3215 0.3618 0.044 Uiso 1 1 calc R . . H43B H 0.4769 0.4085 0.4222 0.044 Uiso 1 1 calc R . . C44 C 0.4425(3) 0.5442(4) 0.2630(3) 0.0666(13) Uani 1 1 d . . . H44A H 0.4587 0.6142 0.2121 0.100 Uiso 1 1 calc R . . H44B H 0.3851 0.5729 0.3041 0.100 Uiso 1 1 calc R . . H44C H 0.4065 0.4867 0.2436 0.100 Uiso 1 1 calc R . . C51 C 0.8560(3) 0.1668(3) 0.2047(2) 0.0367(9) Uani 1 1 d . . . H51A H 0.8775 0.0777 0.2148 0.044 Uiso 1 1 calc R . . H51B H 0.9106 0.2087 0.1565 0.044 Uiso 1 1 calc R . . C52 C 0.7255(3) 0.2066(3) 0.1760(2) 0.0392(9) Uani 1 1 d . . . H52A H 0.6704 0.1638 0.2234 0.047 Uiso 1 1 calc R . . H52B H 0.7163 0.1824 0.1239 0.047 Uiso 1 1 calc R . . C53 C 0.6859(3) 0.3467(3) 0.1532(2) 0.0440(10) Uani 1 1 d . . . H53A H 0.5985 0.3678 0.1373 0.053 Uiso 1 1 calc R . . H53B H 0.6939 0.3707 0.2055 0.053 Uiso 1 1 calc R . . C54 C 0.7233(4) 0.4210(4) -0.0005(2) 0.0648(12) Uani 1 1 d . . . H54A H 0.7769 0.4679 -0.0459 0.097 Uiso 1 1 calc R . . H54B H 0.6381 0.4617 -0.0095 0.097 Uiso 1 1 calc R . . H54C H 0.7298 0.3383 -0.0042 0.097 Uiso 1 1 calc R . . C61 C 0.7369(3) 0.7238(3) 0.22177(19) 0.0265(8) Uani 1 1 d . . . H61A H 0.7890 0.7447 0.2600 0.032 Uiso 1 1 calc R . . H61B H 0.6531 0.7227 0.2488 0.032 Uiso 1 1 calc R . . C62 C 0.7321(3) 0.8214(3) 0.13219(18) 0.0285(8) Uani 1 1 d . . . H62A H 0.7081 0.9026 0.1400 0.034 Uiso 1 1 calc R . . H62B H 0.8154 0.8193 0.1044 0.034 Uiso 1 1 calc R . . C63 C 0.6445(3) 0.8072(3) 0.07168(19) 0.0322(8) Uani 1 1 d . . . H63A H 0.6530 0.8673 0.0126 0.039 Uiso 1 1 calc R . . H63B H 0.6634 0.7240 0.0665 0.039 Uiso 1 1 calc R . . C64 C 0.4346(3) 0.8240(4) 0.0483(2) 0.0577(11) Uani 1 1 d . . . H64A H 0.3522 0.8378 0.0742 0.087 Uiso 1 1 calc R . . H64B H 0.4481 0.7442 0.0389 0.087 Uiso 1 1 calc R . . H64C H 0.4422 0.8886 -0.0080 0.087 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 Cl1 0.0397(5) 0.0148(4) 0.0258(4) -0.0058(4) 0.0042(4) -0.0064(4) Cl2 0.0597(6) 0.0199(4) 0.0239(5) -0.0040(4) 0.0068(4) -0.0043(4) P1 0.0289(5) 0.0124(4) 0.0205(4) -0.0053(4) -0.0001(4) -0.0041(4) P2 0.0284(5) 0.0123(4) 0.0216(5) -0.0056(4) -0.0014(4) -0.0045(4) P3 0.0270(5) 0.0120(4) 0.0200(4) -0.0042(4) 0.0020(4) -0.0051(4) N1 0.0273(15) 0.0121(13) 0.0225(14) -0.0079(11) -0.0002(11) -0.0038(12) N2 0.0319(16) 0.0130(13) 0.0198(14) -0.0069(11) 0.0017(12) -0.0055(12) N3 0.0257(15) 0.0110(13) 0.0216(14) -0.0061(11) 0.0022(11) -0.0038(11) N10 0.0339(17) 0.0154(14) 0.0198(15) -0.0083(12) 0.0024(13) -0.0054(12) N20 0.0345(17) 0.0145(14) 0.0222(15) -0.0048(12) 0.0006(13) -0.0011(14) N30 0.0296(16) 0.0171(14) 0.0208(14) -0.0042(13) 0.0015(13) -0.0095(12) N40 0.0320(17) 0.0133(14) 0.0212(15) -0.0001(11) -0.0014(13) -0.0026(13) N50 0.0449(18) 0.0147(15) 0.0303(17) -0.0017(12) -0.0068(15) -0.0109(14) N60 0.0234(16) 0.0166(15) 0.0267(15) -0.0046(12) 0.0010(13) -0.0069(12) Li1 0.034(3) 0.017(3) 0.027(3) -0.007(2) 0.001(2) -0.009(2) Li2 0.039(3) 0.026(3) 0.021(3) -0.007(2) 0.000(2) -0.006(3) O1 0.0310(14) 0.0197(12) 0.0360(13) -0.0126(11) 0.0002(10) -0.0030(10) O2 0.0430(15) 0.0447(16) 0.0415(15) -0.0175(13) -0.0063(12) -0.0046(13) O3 0.0576(17) 0.0249(13) 0.0375(14) -0.0019(12) 0.0165(12) -0.0159(12) O4 0.0288(14) 0.0464(15) 0.0426(15) 0.0067(13) -0.0043(12) -0.0091(12) O5 0.0455(16) 0.0450(15) 0.0290(14) 0.0011(12) -0.0096(12) -0.0191(13) O6 0.0344(15) 0.0491(16) 0.0327(13) -0.0091(12) -0.0042(12) -0.0032(12) C11 0.029(2) 0.0208(17) 0.0228(18) -0.0091(15) 0.0043(15) -0.0079(15) C12 0.031(2) 0.0216(17) 0.0257(18) -0.0080(15) -0.0014(15) -0.0079(15) C13 0.038(2) 0.0188(17) 0.0210(17) -0.0041(15) -0.0033(15) -0.0041(16) C14 0.041(2) 0.038(2) 0.062(3) -0.029(2) 0.0018(19) -0.0021(19) C21 0.036(2) 0.0249(19) 0.041(2) -0.0124(17) 0.0071(17) -0.0085(17) C22 0.041(2) 0.042(2) 0.041(2) -0.0124(19) 0.0101(18) -0.0052(19) C23 0.040(2) 0.047(2) 0.037(2) -0.0216(19) -0.0007(18) 0.0084(19) C24 0.055(3) 0.047(3) 0.044(2) -0.010(2) -0.006(2) 0.013(2) C31 0.030(2) 0.0173(17) 0.0343(19) -0.0031(15) 0.0026(16) -0.0084(15) C32 0.034(2) 0.0281(19) 0.0307(19) -0.0087(16) 0.0013(16) -0.0122(17) C33 0.039(2) 0.0231(18) 0.033(2) -0.0155(16) 0.0029(17) -0.0123(17) C34 0.075(3) 0.039(2) 0.041(2) 0.007(2) -0.004(2) -0.020(2) C41 0.030(2) 0.0225(18) 0.0273(18) -0.0057(15) 0.0045(15) -0.0035(16) C42 0.034(2) 0.0226(18) 0.0316(19) -0.0049(16) -0.0003(16) -0.0077(16) C43 0.035(2) 0.031(2) 0.045(2) -0.0111(18) 0.0040(17) -0.0125(17) C44 0.039(3) 0.066(3) 0.072(3) 0.009(2) -0.019(2) -0.005(2) C51 0.058(3) 0.0218(19) 0.031(2) -0.0051(16) -0.0102(18) -0.0101(18) C52 0.042(2) 0.035(2) 0.041(2) -0.0034(18) -0.0115(18) -0.0172(19) C53 0.040(2) 0.044(2) 0.045(2) -0.008(2) -0.0014(19) -0.010(2) C54 0.075(3) 0.072(3) 0.048(3) -0.006(2) -0.023(2) -0.029(3) C61 0.030(2) 0.0184(17) 0.0279(18) -0.0074(15) 0.0009(15) 0.0034(15) C62 0.036(2) 0.0172(17) 0.0275(19) -0.0035(15) 0.0006(16) -0.0005(16) C63 0.039(2) 0.0267(19) 0.0251(19) -0.0031(16) 0.0032(17) -0.0029(17) C64 0.048(3) 0.064(3) 0.058(3) -0.012(2) -0.008(2) -0.012(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 Cl1 Li1 2.337(5) 2_756 ? Cl1 Li1 2.349(5) . ? Cl2 Li2 2.349(5) . ? Cl2 Li2 2.350(5) 2_765 ? P1 N3 1.594(2) . ? P1 N1 1.614(2) . ? P1 N10 1.637(3) . ? P1 N40 1.650(3) . ? P1 Li1 3.063(5) . ? P2 N1 1.598(2) . ? P2 N2 1.601(2) . ? P2 N20 1.641(3) . ? P2 N50 1.657(3) . ? P3 N3 1.600(2) . ? P3 N2 1.617(2) . ? P3 N30 1.635(2) . ? P3 N60 1.635(3) . ? P3 Li2 3.105(5) . ? N1 Li1 2.047(5) . ? N2 Li2 2.094(5) . ? N10 C11 1.456(4) . ? N20 C21 1.455(4) . ? N30 C31 1.464(4) . ? N40 C41 1.457(4) . ? N50 C51 1.449(4) . ? N60 C61 1.470(4) . ? Li1 O1 1.978(5) . ? Li1 Cl1 2.337(5) 2_756 ? Li1 Li1 2.811(10) 2_756 ? Li2 O5 1.995(6) . ? Li2 Cl2 2.350(5) 2_765 ? Li2 Li2 3.076(10) 2_765 ? O1 C14 1.426(3) . ? O1 C13 1.431(3) . ? O2 C23 1.411(4) . ? O2 C24 1.414(4) . ? O3 C33 1.412(3) . ? O3 C34 1.423(4) . ? O4 C44 1.420(4) . ? O4 C43 1.422(4) . ? O5 C54 1.393(4) . ? O5 C53 1.436(4) . ? O6 C64 1.407(4) . ? O6 C63 1.417(3) . ? C11 C12 1.520(4) . ? C12 C13 1.527(4) . ? C21 C22 1.520(4) . ? C22 C23 1.515(4) . ? C31 C32 1.515(4) . ? C32 C33 1.502(4) . ? C41 C42 1.517(4) . ? C42 C43 1.505(4) . ? C51 C52 1.502(4) . ? C52 C53 1.550(4) . ? C61 C62 1.518(4) . ? C62 C63 1.498(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Li1 Cl1 Li1 73.71(19) 2_756 . ? Li2 Cl2 Li2 81.80(18) . 2_765 ? N3 P1 N1 113.85(12) . . ? N3 P1 N10 114.81(13) . . ? N1 P1 N10 104.23(12) . . ? N3 P1 N40 107.69(12) . . ? N1 P1 N40 115.75(13) . . ? N10 P1 N40 99.86(13) . . ? N3 P1 Li1 149.60(13) . . ? N1 P1 Li1 37.93(12) . . ? N10 P1 Li1 74.53(13) . . ? N40 P1 Li1 98.40(13) . . ? N1 P2 N2 115.39(12) . . ? N1 P2 N20 111.73(13) . . ? N2 P2 N20 107.85(13) . . ? N1 P2 N50 106.97(13) . . ? N2 P2 N50 109.45(13) . . ? N20 P2 N50 104.94(14) . . ? N3 P3 N2 115.08(12) . . ? N3 P3 N30 106.11(12) . . ? N2 P3 N30 113.95(12) . . ? N3 P3 N60 115.08(13) . . ? N2 P3 N60 105.13(13) . . ? N30 P3 N60 100.80(13) . . ? N3 P3 Li2 153.43(13) . . ? N2 P3 Li2 38.36(12) . . ? N30 P3 Li2 90.05(13) . . ? N60 P3 Li2 81.25(13) . . ? P2 N1 P1 124.51(14) . . ? P2 N1 Li1 122.39(18) . . ? P1 N1 Li1 113.07(18) . . ? P2 N2 P3 124.02(14) . . ? P2 N2 Li2 122.99(18) . . ? P3 N2 Li2 112.99(18) . . ? P1 N3 P3 124.78(14) . . ? C11 N10 P1 121.72(18) . . ? C21 N20 P2 121.5(2) . . ? C31 N30 P3 123.0(2) . . ? C41 N40 P1 121.8(2) . . ? C51 N50 P2 122.6(2) . . ? C61 N60 P3 121.5(2) . . ? O1 Li1 N1 122.6(3) . . ? O1 Li1 Cl1 106.9(2) . 2_756 ? N1 Li1 Cl1 107.8(2) . 2_756 ? O1 Li1 Cl1 103.6(2) . . ? N1 Li1 Cl1 108.5(2) . . ? Cl1 Li1 Cl1 106.29(19) 2_756 . ? O1 Li1 Li1 116.0(3) . 2_756 ? N1 Li1 Li1 121.3(3) . 2_756 ? Cl1 Li1 Li1 53.34(16) 2_756 2_756 ? Cl1 Li1 Li1 52.94(16) . 2_756 ? O1 Li1 P1 108.14(19) . . ? N1 Li1 P1 29.00(9) . . ? Cl1 Li1 P1 91.22(15) 2_756 . ? Cl1 Li1 P1 137.19(19) . . ? Li1 Li1 P1 129.1(3) 2_756 . ? O5 Li2 N2 102.6(2) . . ? O5 Li2 Cl2 104.9(2) . . ? N2 Li2 Cl2 121.9(2) . . ? O5 Li2 Cl2 111.7(2) . 2_765 ? N2 Li2 Cl2 117.1(2) . 2_765 ? Cl2 Li2 Cl2 98.20(18) . 2_765 ? O5 Li2 Li2 118.6(3) . 2_765 ? N2 Li2 Li2 138.8(3) . 2_765 ? Cl2 Li2 Li2 49.11(14) . 2_765 ? Cl2 Li2 Li2 49.09(14) 2_765 2_765 ? O5 Li2 P3 105.8(2) . . ? N2 Li2 P3 28.64(9) . . ? Cl2 Li2 P3 142.3(2) . . ? Cl2 Li2 P3 90.39(15) 2_765 . ? Li2 Li2 P3 127.5(3) 2_765 . ? C14 O1 C13 113.1(2) . . ? C14 O1 Li1 123.0(2) . . ? C13 O1 Li1 120.2(2) . . ? C23 O2 C24 110.6(3) . . ? C33 O3 C34 110.9(3) . . ? C44 O4 C43 111.5(3) . . ? C54 O5 C53 113.8(3) . . ? C54 O5 Li2 115.8(2) . . ? C53 O5 Li2 127.6(2) . . ? C64 O6 C63 112.3(2) . . ? N10 C11 C12 111.1(2) . . ? C11 C12 C13 112.9(2) . . ? O1 C13 C12 112.9(2) . . ? N20 C21 C22 111.8(3) . . ? C23 C22 C21 113.9(3) . . ? O2 C23 C22 110.4(3) . . ? N30 C31 C32 111.5(2) . . ? C33 C32 C31 113.5(3) . . ? O3 C33 C32 109.2(3) . . ? N40 C41 C42 115.3(2) . . ? C43 C42 C41 113.0(3) . . ? O4 C43 C42 108.1(3) . . ? N50 C51 C52 114.6(3) . . ? C51 C52 C53 112.3(3) . . ? O5 C53 C52 111.9(3) . . ? N60 C61 C62 112.2(2) . . ? C63 C62 C61 114.0(3) . . ? O6 C63 C62 109.2(2) . . ? 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 N10 H10 N3 0.776(17) 2.568(19) 3.304(3) 159(3) 2_766 N30 H30 Cl2 0.811(16) 2.567(18) 3.350(2) 163(3) 2_765 N40 H40 Cl1 0.774(17) 2.73(2) 3.431(2) 151(3) 2_756 N60 H60 O4 0.780(17) 2.43(2) 3.126(3) 150(3) . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.534 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.056 #===END