# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2242 data_kendalt_1 _publ_contact_author ; Alan Kennedy Dept. of P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL Scotland ; _publ_contact_letter ; Dear Debbie, This file is the supplementary cif informatiom for the ms B007038 recently sent to you by Dr Kenneth Henderson. If there are any problems with the construction of the CIF or with its transmission please contact me. Yours Sincerely, Alan Kennedy ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 0141 548 2016' _publ_contact_author_fax '0141 552 5664 ' _publ_contact_author_email ' a.r.kennedy@strath.ac.uk ' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 Li2 N2 O8 P2' _chemical_formula_weight 510.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' 'N' 'N' 0.0061 0.0033 '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' 'Li' 'Li' -0.0003 0.0001 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.926(8) _cell_length_b 11.024(5) _cell_length_c 16.663(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.83(5) _cell_angle_gamma 90.00 _cell_volume 2716(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 17 _cell_measurement_theta_min 5.41 _cell_measurement_theta_max 8.12 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9233 _exptl_absorpt_correction_T_max 0.9606 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S Diffractometer' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.71 _diffrn_reflns_number 4936 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4776 _reflns_number_gt 3534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC diffractometer control' _computing_cell_refinement ' " ' _computing_data_reduction 'texsan' _computing_structure_solution 'SIR92' _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 w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+3.3413P] 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 'see text' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4776 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.15543(6) 0.40886(8) 0.29251(6) 0.0242(2) Uani 1 d . . . P2 P -0.16547(6) 0.68173(8) 0.16787(5) 0.0220(2) Uani 1 d . . . O1 O 0.07404(14) 0.4784(2) 0.25438(15) 0.0261(6) Uani 1 d . . . O2 O 0.12775(16) 0.2898(2) 0.33719(14) 0.0282(6) Uani 1 d . . . O3 O 0.20451(16) 0.4687(2) 0.37328(16) 0.0337(6) Uani 1 d . . . O4 O -0.07876(14) 0.6179(2) 0.19625(14) 0.0257(6) Uani 1 d . . . O5 O -0.15195(16) 0.8164(2) 0.13773(14) 0.0255(5) Uani 1 d . . . O6 O -0.20361(15) 0.6208(2) 0.08372(15) 0.0290(6) Uani 1 d . . . O7 O 0.06806(16) 0.6188(2) 0.07448(15) 0.0321(6) Uani 1 d . . . O8 O -0.04718(17) 0.5507(2) 0.38319(16) 0.0334(6) Uani 1 d . . . N1 N 0.3777(2) 0.2711(3) 0.2694(2) 0.0347(8) Uani 1 d . . . N2 N -0.3597(2) 0.8488(3) 0.2348(2) 0.0376(8) Uani 1 d . . . C1 C 0.2288(2) 0.3812(4) 0.2253(2) 0.0311(9) Uani 1 d . . . C2 C 0.3101(2) 0.3213(4) 0.2488(2) 0.0299(8) Uani 1 d . . . C3 C 0.0775(3) 0.1955(4) 0.2898(2) 0.0375(9) Uani 1 d . . . H3A H 0.1042 0.1805 0.2395 0.045 Uiso 1 calc R . . H3B H 0.0138 0.2210 0.2747 0.045 Uiso 1 calc R . . C4 C 0.0814(3) 0.0841(4) 0.3390(3) 0.0459(11) Uani 1 d . . . H4A H 0.1447 0.0607 0.3549 0.069 Uiso 1 calc R . . H4B H 0.0494 0.0186 0.3072 0.069 Uiso 1 calc R . . H4C H 0.0527 0.0987 0.3876 0.069 Uiso 1 calc R . . C5 C 0.2574(3) 0.5781(4) 0.3693(3) 0.0489(12) Uani 1 d . A 1 H5A H 0.2860 0.5765 0.3191 0.059 Uiso 1 calc R A 1 H5B H 0.2165 0.6491 0.3663 0.059 Uiso 1 calc R A 1 C6A C 0.3243(8) 0.5926(11) 0.4350(7) 0.057(3) Uiso 0.50 d P A 1 H6A1 H 0.2963 0.6024 0.4845 0.085 Uiso 0.50 calc PR A 1 H6A2 H 0.3604 0.6646 0.4268 0.085 Uiso 0.50 calc PR A 1 H6A3 H 0.3635 0.5208 0.4402 0.085 Uiso 0.50 calc PR A 1 C6B C 0.3506(6) 0.5533(10) 0.4150(6) 0.043(2) Uiso 0.50 d P B 2 H6D H 0.3836 0.6462 0.4189 0.06(3) Uiso 0.50 d PR B 2 H6E H 0.3717 0.5040 0.3962 0.006(16) Uiso 0.50 d PR B 2 H6F H 0.3466 0.5483 0.4633 0.03(2) Uiso 0.50 d PR B 2 C7 C -0.2389(2) 0.6852(3) 0.2363(2) 0.0263(8) Uani 1 d . . . C8 C -0.3049(2) 0.7741(4) 0.2353(2) 0.0303(8) Uani 1 d . . . C9 C -0.1119(3) 0.9065(3) 0.1960(2) 0.0344(9) Uani 1 d . . . H9A H -0.0534 0.8766 0.2243 0.041 Uiso 1 calc R . . H9B H -0.1527 0.9226 0.2369 0.041 Uiso 1 calc R . . C10 C -0.0978(3) 1.0198(4) 0.1500(3) 0.0384(10) Uani 1 d . . . H10A H -0.0546 1.0040 0.1120 0.058 Uiso 1 calc R . . H10B H -0.0741 1.0837 0.1880 0.058 Uiso 1 calc R . . H10C H -0.1556 1.0461 0.1200 0.058 Uiso 1 calc R . . C11 C -0.2955(2) 0.6445(4) 0.0466(3) 0.0397(10) Uani 1 d . . . H11A H -0.2964 0.6618 -0.0118 0.048 Uiso 1 calc R . . H11B H -0.3196 0.7164 0.0722 0.048 Uiso 1 calc R . . C12 C -0.3535(3) 0.5361(5) 0.0571(3) 0.0539(13) Uani 1 d . . . H12A H -0.3287 0.4649 0.0327 0.081 Uiso 1 calc R . . H12B H -0.4152 0.5512 0.0306 0.081 Uiso 1 calc R . . H12C H -0.3545 0.5214 0.1150 0.081 Uiso 1 calc R . . C13 C 0.0030(3) 0.6753(4) 0.0149(2) 0.0411(10) Uani 1 d . . . H13A H -0.0074 0.7605 0.0299 0.049 Uiso 1 calc R . . H13B H -0.0553 0.6312 0.0096 0.049 Uiso 1 calc R . . C14 C 0.0432(3) 0.6696(4) -0.0626(2) 0.0376(9) Uani 1 d . . . H14A H 0.0193 0.7350 -0.1002 0.045 Uiso 1 calc R . . H14B H 0.0315 0.5902 -0.0897 0.045 Uiso 1 calc R . . C15 C 0.1428(3) 0.6872(4) -0.0336(3) 0.0401(10) Uani 1 d . . . H15A H 0.1580 0.7744 -0.0270 0.048 Uiso 1 calc R . . H15B H 0.1804 0.6504 -0.0717 0.048 Uiso 1 calc R . . C16 C 0.1560(3) 0.6224(4) 0.0472(2) 0.0385(10) Uani 1 d . . . H16A H 0.1791 0.5392 0.0410 0.046 Uiso 1 calc R . . H16B H 0.1998 0.6668 0.0866 0.046 Uiso 1 calc R . . C17 C 0.0010(3) 0.6637(4) 0.3978(2) 0.0388(10) Uani 1 d . . . H17A H -0.0083 0.7157 0.3489 0.047 Uiso 1 calc R . . H17B H 0.0666 0.6486 0.4122 0.047 Uiso 1 calc R . . C18 C -0.0370(3) 0.7239(5) 0.4673(3) 0.0500(12) Uani 1 d . . . H18A H -0.0359 0.8134 0.4625 0.060 Uiso 1 calc R . . H18B H -0.0034 0.6996 0.5201 0.060 Uiso 1 calc R . . C19 C -0.1339(3) 0.6755(4) 0.4568(3) 0.0457(11) Uani 1 d . . . H19A H -0.1603 0.6798 0.5081 0.055 Uiso 1 calc R . . H19B H -0.1732 0.7201 0.4140 0.055 Uiso 1 calc R . . C20 C -0.1197(3) 0.5476(4) 0.4326(3) 0.0432(11) Uani 1 d . . . H20A H -0.1028 0.4962 0.4810 0.052 Uiso 1 calc R . . H20B H -0.1755 0.5145 0.4014 0.052 Uiso 1 calc R . . Li1 Li 0.0498(4) 0.6253(6) 0.1890(4) 0.0269(13) Uani 1 d . . . Li2 Li -0.0510(4) 0.4852(6) 0.2741(4) 0.0297(14) Uani 1 d . . . H1 H 0.215(3) 0.401(5) 0.174(3) 0.064(16) Uiso 1 d . . . H2 H -0.238(3) 0.628(4) 0.268(3) 0.045(13) Uiso 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 P1 0.0178(4) 0.0248(5) 0.0307(5) 0.0012(4) 0.0054(4) 0.0020(4) P2 0.0155(4) 0.0206(5) 0.0307(5) 0.0000(4) 0.0057(3) 0.0010(3) O1 0.0155(11) 0.0276(13) 0.0355(14) 0.0026(11) 0.0051(10) 0.0052(10) O2 0.0308(13) 0.0237(13) 0.0300(14) -0.0008(11) 0.0032(10) -0.0045(11) O3 0.0273(13) 0.0364(15) 0.0370(15) -0.0018(12) 0.0023(11) -0.0116(12) O4 0.0133(11) 0.0279(13) 0.0361(14) 0.0031(11) 0.0046(10) 0.0019(10) O5 0.0278(12) 0.0185(12) 0.0302(13) -0.0001(10) 0.0037(10) -0.0010(10) O6 0.0189(12) 0.0309(14) 0.0366(14) -0.0082(12) 0.0021(10) -0.0014(10) O7 0.0229(13) 0.0422(16) 0.0319(14) 0.0047(12) 0.0069(10) 0.0010(11) O8 0.0303(13) 0.0343(15) 0.0387(15) -0.0013(12) 0.0155(11) -0.0002(12) N1 0.0237(16) 0.0363(19) 0.045(2) 0.0007(16) 0.0094(14) 0.0069(14) N2 0.0298(17) 0.0362(19) 0.050(2) -0.0016(16) 0.0168(15) 0.0074(16) C1 0.0214(18) 0.041(2) 0.033(2) 0.0053(18) 0.0092(15) 0.0104(16) C2 0.0211(18) 0.031(2) 0.040(2) 0.0026(17) 0.0098(15) 0.0008(16) C3 0.045(2) 0.027(2) 0.039(2) -0.0033(17) -0.0005(18) -0.0082(18) C4 0.052(3) 0.035(2) 0.049(3) 0.000(2) 0.003(2) -0.008(2) C5 0.039(2) 0.039(3) 0.068(3) 0.005(2) 0.001(2) -0.015(2) C7 0.0233(17) 0.0250(19) 0.033(2) 0.0038(17) 0.0124(15) 0.0019(15) C8 0.0237(18) 0.032(2) 0.037(2) -0.0035(17) 0.0109(15) -0.0011(17) C9 0.040(2) 0.023(2) 0.037(2) -0.0070(17) -0.0050(17) -0.0037(17) C10 0.039(2) 0.028(2) 0.048(2) 0.0003(19) 0.0082(19) -0.0060(17) C11 0.0259(19) 0.042(2) 0.048(2) -0.005(2) -0.0078(17) 0.0041(18) C12 0.028(2) 0.059(3) 0.071(3) -0.010(3) -0.005(2) -0.007(2) C13 0.0232(18) 0.062(3) 0.039(2) 0.010(2) 0.0056(16) 0.0048(19) C14 0.037(2) 0.040(2) 0.036(2) 0.0059(19) 0.0056(17) -0.0034(18) C15 0.032(2) 0.044(2) 0.047(2) 0.011(2) 0.0158(18) 0.0025(18) C16 0.0255(19) 0.052(3) 0.040(2) 0.000(2) 0.0114(16) 0.0042(18) C17 0.039(2) 0.040(2) 0.037(2) -0.0014(19) 0.0054(18) -0.0027(18) C18 0.046(2) 0.058(3) 0.044(3) -0.014(2) 0.000(2) 0.013(2) C19 0.040(2) 0.063(3) 0.035(2) -0.002(2) 0.0078(18) 0.022(2) C20 0.037(2) 0.057(3) 0.040(2) 0.013(2) 0.0194(19) 0.011(2) Li1 0.021(3) 0.031(3) 0.030(3) -0.002(3) 0.009(2) -0.003(2) Li2 0.019(3) 0.029(3) 0.043(4) 0.004(3) 0.012(3) 0.002(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 O1 1.502(2) . ? P1 O3 1.586(3) . ? P1 O2 1.591(3) . ? P1 C1 1.697(4) . ? P2 O4 1.492(2) . ? P2 O6 1.589(3) . ? P2 O5 1.589(3) . ? P2 C7 1.687(4) . ? O1 Li2 1.941(6) . ? O1 Li1 1.958(7) . ? O2 C3 1.451(4) . ? O3 C5 1.448(5) . ? O4 Li1 1.940(6) . ? O4 Li2 1.962(7) . ? O5 C9 1.459(4) . ? O6 C11 1.450(4) . ? O7 C13 1.433(5) . ? O7 C16 1.447(4) . ? O7 Li1 1.965(6) . ? O8 C17 1.442(5) . ? O8 C20 1.447(4) . ? O8 Li2 1.950(7) . ? N1 C2 1.160(5) . ? N1 Li1 2.009(7) 2_545 ? N2 C8 1.160(5) . ? N2 Li2 2.001(7) 2_455 ? C1 C2 1.391(5) . ? C1 H1 0.87(5) . ? C3 C4 1.473(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6A 1.386(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C6A H6D 1.1267 . ? C6A H6E 1.4129 . ? C6A H6F 0.7260 . ? C6B H6D 1.1338 . ? C6B H6E 0.7210 . ? C6B H6F 0.8160 . ? C7 C8 1.388(5) . ? C7 H2 0.82(5) . ? C9 C10 1.495(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.500(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.497(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.512(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.512(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.511(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.529(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.490(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? Li1 N1 2.008(7) 2 ? Li1 Li2 2.691(8) . ? Li2 N2 2.001(7) 2_445 ? 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 O1 P1 O3 113.59(15) . . ? O1 P1 O2 111.85(14) . . ? O3 P1 O2 93.74(14) . . ? O1 P1 C1 111.69(17) . . ? O3 P1 C1 111.73(18) . . ? O2 P1 C1 113.12(18) . . ? O4 P2 O6 105.73(14) . . ? O4 P2 O5 113.50(14) . . ? O6 P2 O5 99.33(14) . . ? O4 P2 C7 114.31(17) . . ? O6 P2 C7 114.77(17) . . ? O5 P2 C7 108.35(16) . . ? P1 O1 Li2 133.6(2) . . ? P1 O1 Li1 137.3(2) . . ? Li2 O1 Li1 87.3(3) . . ? C3 O2 P1 119.0(2) . . ? C5 O3 P1 120.0(3) . . ? P2 O4 Li1 141.5(2) . . ? P2 O4 Li2 131.1(2) . . ? Li1 O4 Li2 87.2(3) . . ? C9 O5 P2 118.9(2) . . ? C11 O6 P2 120.3(2) . . ? C13 O7 C16 109.2(3) . . ? C13 O7 Li1 119.1(3) . . ? C16 O7 Li1 123.8(3) . . ? C17 O8 C20 108.6(3) . . ? C17 O8 Li2 115.3(3) . . ? C20 O8 Li2 126.3(3) . . ? C2 N1 Li1 152.8(4) . 2_545 ? C8 N2 Li2 174.8(4) . 2_455 ? C2 C1 P1 121.1(3) . . ? C2 C1 H1 118(3) . . ? P1 C1 H1 121(3) . . ? N1 C2 C1 179.1(4) . . ? O2 C3 C4 108.5(3) . . ? O2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6A C5 O3 113.5(6) . . ? C6A C5 H5A 108.9 . . ? O3 C5 H5A 108.9 . . ? C6A C5 H5B 108.9 . . ? O3 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C8 C7 P2 122.2(3) . . ? C8 C7 H2 120(3) . . ? P2 C7 H2 118(3) . . ? N2 C8 C7 179.6(4) . . ? O5 C9 C10 107.5(3) . . ? O5 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O5 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 109.5(3) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 C14 105.4(3) . . ? O7 C13 H13A 110.7 . . ? C14 C13 H13A 110.7 . . ? O7 C13 H13B 110.7 . . ? C14 C13 H13B 110.7 . . ? H13A C13 H13B 108.8 . . ? C13 C14 C15 102.2(3) . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14B 111.3 . . ? C15 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C14 C15 C16 103.1(3) . . ? C14 C15 H15A 111.1 . . ? C16 C15 H15A 111.1 . . ? C14 C15 H15B 111.1 . . ? C16 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? O7 C16 C15 106.2(3) . . ? O7 C16 H16A 110.5 . . ? C15 C16 H16A 110.5 . . ? O7 C16 H16B 110.5 . . ? C15 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? O8 C17 C18 106.1(3) . . ? O8 C17 H17A 110.5 . . ? C18 C17 H17A 110.5 . . ? O8 C17 H17B 110.5 . . ? C18 C17 H17B 110.5 . . ? H17A C17 H17B 108.7 . . ? C17 C18 C19 102.0(4) . . ? C17 C18 H18A 111.4 . . ? C19 C18 H18A 111.4 . . ? C17 C18 H18B 111.4 . . ? C19 C18 H18B 111.4 . . ? H18A C18 H18B 109.2 . . ? C20 C19 C18 101.2(3) . . ? C20 C19 H19A 111.5 . . ? C18 C19 H19A 111.5 . . ? C20 C19 H19B 111.5 . . ? C18 C19 H19B 111.5 . . ? H19A C19 H19B 109.4 . . ? O8 C20 C19 106.1(4) . . ? O8 C20 H20A 110.5 . . ? C19 C20 H20A 110.5 . . ? O8 C20 H20B 110.5 . . ? C19 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? O4 Li1 O1 92.3(3) . . ? O4 Li1 O7 109.2(3) . . ? O1 Li1 O7 118.1(3) . . ? O4 Li1 N1 120.2(3) . 2 ? O1 Li1 N1 114.8(3) . 2 ? O7 Li1 N1 103.0(3) . 2 ? O4 Li1 Li2 46.73(19) . . ? O1 Li1 Li2 46.09(19) . . ? O7 Li1 Li2 130.7(3) . . ? N1 Li1 Li2 126.2(3) 2 . ? O1 Li2 O8 105.4(3) . . ? O1 Li2 O4 92.2(3) . . ? O8 Li2 O4 108.5(3) . . ? O1 Li2 N2 127.2(3) . 2_445 ? O8 Li2 N2 106.4(3) . 2_445 ? O4 Li2 N2 115.7(3) . 2_445 ? O1 Li2 Li1 46.61(19) . . ? O8 Li2 Li1 109.3(3) . . ? O4 Li2 Li1 46.06(19) . . ? N2 Li2 Li1 143.8(3) 2_445 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Li2 -82.1(4) . . . . ? O2 P1 O1 Li2 22.5(4) . . . . ? C1 P1 O1 Li2 150.5(3) . . . . ? O3 P1 O1 Li1 77.3(4) . . . . ? O2 P1 O1 Li1 -178.1(3) . . . . ? C1 P1 O1 Li1 -50.2(4) . . . . ? O1 P1 O2 C3 62.6(3) . . . . ? O3 P1 O2 C3 179.9(3) . . . . ? C1 P1 O2 C3 -64.5(3) . . . . ? O1 P1 O3 C5 -73.2(3) . . . . ? O2 P1 O3 C5 171.0(3) . . . . ? C1 P1 O3 C5 54.3(3) . . . . ? O6 P2 O4 Li1 88.9(4) . . . . ? O5 P2 O4 Li1 -18.9(4) . . . . ? C7 P2 O4 Li1 -143.8(4) . . . . ? O6 P2 O4 Li2 -98.5(3) . . . . ? O5 P2 O4 Li2 153.6(3) . . . . ? C7 P2 O4 Li2 28.7(4) . . . . ? O4 P2 O5 C9 -64.8(3) . . . . ? O6 P2 O5 C9 -176.6(2) . . . . ? C7 P2 O5 C9 63.3(3) . . . . ? O4 P2 O6 C11 168.0(3) . . . . ? O5 P2 O6 C11 -74.2(3) . . . . ? C7 P2 O6 C11 41.1(3) . . . . ? O1 P1 C1 C2 177.9(3) . . . . ? O3 P1 C1 C2 49.4(4) . . . . ? O2 P1 C1 C2 -54.8(4) . . . . ? Li1 N1 C2 C1 62(28) 2_545 . . . ? P1 C1 C2 N1 3(28) . . . . ? P1 O2 C3 C4 165.0(3) . . . . ? P1 O3 C5 C6A -154.7(6) . . . . ? O4 P2 C7 C8 155.4(3) . . . . ? O6 P2 C7 C8 -82.2(4) . . . . ? O5 P2 C7 C8 27.7(4) . . . . ? Li2 N2 C8 C7 76(64) 2_455 . . . ? P2 C7 C8 N2 -83(63) . . . . ? P2 O5 C9 C10 173.8(2) . . . . ? P2 O6 C11 C12 -104.9(4) . . . . ? C16 O7 C13 C14 22.0(4) . . . . ? Li1 O7 C13 C14 172.1(3) . . . . ? O7 C13 C14 C15 -35.6(4) . . . . ? C13 C14 C15 C16 35.3(4) . . . . ? C13 O7 C16 C15 0.9(4) . . . . ? Li1 O7 C16 C15 -147.5(3) . . . . ? C14 C15 C16 O7 -23.0(4) . . . . ? C20 O8 C17 C18 7.4(4) . . . . ? Li2 O8 C17 C18 155.8(3) . . . . ? O8 C17 C18 C19 -29.1(4) . . . . ? C17 C18 C19 C20 39.0(4) . . . . ? C17 O8 C20 C19 18.2(4) . . . . ? Li2 O8 C20 C19 -125.7(4) . . . . ? C18 C19 C20 O8 -35.6(4) . . . . ? P2 O4 Li1 O1 -178.1(3) . . . . ? Li2 O4 Li1 O1 7.6(3) . . . . ? P2 O4 Li1 O7 -57.2(5) . . . . ? Li2 O4 Li1 O7 128.4(3) . . . . ? P2 O4 Li1 N1 61.3(5) . . . 2 ? Li2 O4 Li1 N1 -113.0(4) . . . 2 ? P2 O4 Li1 Li2 174.4(4) . . . . ? P1 O1 Li1 O4 -172.8(2) . . . . ? Li2 O1 Li1 O4 -7.6(3) . . . . ? P1 O1 Li1 O7 73.9(5) . . . . ? Li2 O1 Li1 O7 -120.9(4) . . . . ? P1 O1 Li1 N1 -47.9(5) . . . 2 ? Li2 O1 Li1 N1 117.3(3) . . . 2 ? P1 O1 Li1 Li2 -165.2(4) . . . . ? C13 O7 Li1 O4 34.5(5) . . . . ? C16 O7 Li1 O4 180.0(3) . . . . ? C13 O7 Li1 O1 138.0(3) . . . . ? C16 O7 Li1 O1 -76.5(4) . . . . ? C13 O7 Li1 N1 -94.4(4) . . . 2 ? C16 O7 Li1 N1 51.1(4) . . . 2 ? C13 O7 Li1 Li2 83.3(5) . . . . ? C16 O7 Li1 Li2 -131.2(4) . . . . ? P1 O1 Li2 O8 63.9(4) . . . . ? Li1 O1 Li2 O8 -102.3(3) . . . . ? P1 O1 Li2 O4 173.7(2) . . . . ? Li1 O1 Li2 O4 7.6(3) . . . . ? P1 O1 Li2 N2 -61.3(6) . . . 2_445 ? Li1 O1 Li2 N2 132.5(4) . . . 2_445 ? P1 O1 Li2 Li1 166.2(4) . . . . ? C17 O8 Li2 O1 53.3(4) . . . . ? C20 O8 Li2 O1 -164.8(3) . . . . ? C17 O8 Li2 O4 -44.4(4) . . . . ? C20 O8 Li2 O4 97.5(4) . . . . ? C17 O8 Li2 N2 -169.5(3) . . . 2_445 ? C20 O8 Li2 N2 -27.6(5) . . . 2_445 ? C17 O8 Li2 Li1 4.5(4) . . . . ? C20 O8 Li2 Li1 146.4(3) . . . . ? P2 O4 Li2 O1 177.0(2) . . . . ? Li1 O4 Li2 O1 -7.6(3) . . . . ? P2 O4 Li2 O8 -76.0(4) . . . . ? Li1 O4 Li2 O8 99.4(3) . . . . ? P2 O4 Li2 N2 43.4(5) . . . 2_445 ? Li1 O4 Li2 N2 -141.2(4) . . . 2_445 ? P2 O4 Li2 Li1 -175.3(4) . . . . ? O4 Li1 Li2 O1 169.5(4) . . . . ? O7 Li1 Li2 O1 91.9(4) . . . . ? N1 Li1 Li2 O1 -90.9(4) 2 . . . ? O4 Li1 Li2 O8 -97.4(3) . . . . ? O1 Li1 Li2 O8 93.2(3) . . . . ? O7 Li1 Li2 O8 -175.0(3) . . . . ? N1 Li1 Li2 O8 2.2(5) 2 . . . ? O1 Li1 Li2 O4 -169.5(4) . . . . ? O7 Li1 Li2 O4 -77.6(4) . . . . ? N1 Li1 Li2 O4 99.6(4) 2 . . . ? O4 Li1 Li2 N2 72.7(5) . . . 2_445 ? O1 Li1 Li2 N2 -96.8(6) . . . 2_445 ? O7 Li1 Li2 N2 -4.9(8) . . . 2_445 ? N1 Li1 Li2 N2 172.3(4) 2 . . 2_445 ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.499 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.075 #===END data_ak61 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H46 Li2 N2 O8 P2' _chemical_formula_weight 566.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 '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' 'N' 'N' 0.0061 0.0033 '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' 'Li' 'Li' -0.0003 0.0001 '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' _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 22.243(3) _cell_length_b 9.837(2) _cell_length_c 15.585(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.131(8) _cell_angle_gamma 90.00 _cell_volume 3258.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18810 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sortav, Blessing 1997' _exptl_absorpt_correction_T_min 0.9493 _exptl_absorpt_correction_T_max 0.9982 _exptl_special_details ; From Southhampton EPSRC service ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi & omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4671 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1111 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 24.00 _reflns_number_total 2432 _reflns_number_gt 1353 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Denzo & Collect (Otwinowski & Minor, 1997; Hooft & Nonius 1988) ; _computing_cell_refinement 'Denzo & Collect' _computing_data_reduction 'Denzo & Collect' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97' _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 w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+10.2437P] 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 2432 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1486 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.1744 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.69036(7) 0.09991(17) 0.60950(9) 0.0463(5) Uani 1 d . . . O1 O 0.63658(17) 0.2043(4) 0.6117(2) 0.0580(11) Uani 1 d . . . O2 O 0.64748(16) -0.0282(4) 0.5737(3) 0.0542(11) Uani 1 d . . . O3 O 0.72081(16) 0.1569(4) 0.5442(2) 0.0482(10) Uani 1 d . . . O4 O 0.63234(18) 0.3025(5) 0.3783(3) 0.0667(12) Uani 1 d . . . N1 N 0.7197(2) -0.0792(6) 0.8310(3) 0.0623(14) Uani 1 d . . . C1 C 0.7433(3) 0.0647(7) 0.7095(4) 0.0568(17) Uani 1 d . . . H1 H 0.784(3) 0.102(8) 0.721(5) 0.10(2) Uiso 1 d . . . C2 C 0.7303(3) -0.0138(6) 0.7752(4) 0.0515(15) Uani 1 d . . . C3 C 0.6044(4) 0.1992(9) 0.6813(5) 0.089(3) Uani 1 d . A 1 H3 H 0.6256 0.1377 0.7324 0.106 Uiso 1 calc R A 1 C4 C 0.5332(7) 0.1489(16) 0.6259(12) 0.095(6) Uiso 0.63(3) d P A 1 H4A H 0.5142 0.2146 0.5783 0.143 Uiso 0.63(3) calc PR A 1 H4B H 0.5075 0.1425 0.6671 0.143 Uiso 0.63(3) calc PR A 1 H4C H 0.5353 0.0596 0.5991 0.143 Uiso 0.63(3) calc PR A 1 C4A C 0.5593(14) 0.101(3) 0.677(2) 0.104(11) Uiso 0.37(3) d P A 2 C5 C 0.5980(4) 0.3396(11) 0.7100(7) 0.122(4) Uani 1 d . A 1 H5A H 0.6394 0.3833 0.7285 0.184 Uiso 1 calc R A 1 H5B H 0.5803 0.3386 0.7606 0.184 Uiso 1 calc R A 1 H5C H 0.5699 0.3904 0.6599 0.184 Uiso 1 calc R A 1 C6 C 0.6743(3) -0.1592(7) 0.5625(5) 0.0702(19) Uani 1 d . . . H6 H 0.7201 -0.1613 0.5967 0.084 Uiso 1 calc R . . C7 C 0.6398(4) -0.2670(8) 0.5969(5) 0.086(2) Uani 1 d . . . H7A H 0.6417 -0.2466 0.6592 0.129 Uiso 1 calc R . . H7B H 0.6594 -0.3555 0.5943 0.129 Uiso 1 calc R . . H7C H 0.5958 -0.2694 0.5597 0.129 Uiso 1 calc R . . C8 C 0.6656(4) -0.1775(8) 0.4615(5) 0.096(3) Uani 1 d . . . H8A H 0.6206 -0.1768 0.4288 0.144 Uiso 1 calc R . . H8B H 0.6840 -0.2643 0.4514 0.144 Uiso 1 calc R . . H8C H 0.6866 -0.1029 0.4400 0.144 Uiso 1 calc R . . C9 C 0.5744(5) 0.2333(14) 0.3651(9) 0.085(4) Uiso 0.734(18) d P B 1 H9A H 0.5805 0.1483 0.4007 0.103 Uiso 0.734(18) calc PR B 1 H9B H 0.5552 0.2107 0.3009 0.103 Uiso 0.734(18) calc PR B 1 C10 C 0.5338(6) 0.3310(19) 0.3967(12) 0.117(5) Uiso 0.734(18) d P B 1 H10A H 0.4945 0.3463 0.3476 0.141 Uiso 0.734(18) calc PR B 1 H10B H 0.5224 0.2899 0.4477 0.141 Uiso 0.734(18) calc PR B 1 C11 C 0.5613(5) 0.4489(12) 0.4221(8) 0.086(4) Uiso 0.734(18) d P B 1 H11A H 0.5555 0.4769 0.4802 0.103 Uiso 0.734(18) calc PR B 1 H11B H 0.5428 0.5196 0.3768 0.103 Uiso 0.734(18) calc PR B 1 C12 C 0.6311(6) 0.4315(13) 0.4316(9) 0.072(4) Uiso 0.734(18) d P B 1 H12A H 0.6476 0.5101 0.4059 0.087 Uiso 0.734(18) calc PR B 1 H12B H 0.6560 0.4204 0.4953 0.087 Uiso 0.734(18) calc PR B 1 C9A C 0.5820(13) 0.183(3) 0.333(2) 0.077(10) Uiso 0.266(18) d P B 2 C10A C 0.5345(12) 0.229(3) 0.3963(18) 0.072(10) Uiso 0.266(18) d P B 2 C11A C 0.5330(13) 0.390(4) 0.359(2) 0.078(10) Uiso 0.266(18) d P B 2 C12A C 0.6151(14) 0.402(4) 0.418(2) 0.053(9) Uiso 0.266(18) d P B 2 Li1 Li 0.7130(4) 0.2096(9) 0.4225(6) 0.047(2) Uani 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 P1 0.0543(8) 0.0527(10) 0.0355(8) 0.0056(7) 0.0189(6) 0.0016(8) O1 0.063(2) 0.072(3) 0.047(2) 0.007(2) 0.0293(19) 0.012(2) O2 0.051(2) 0.055(3) 0.057(2) 0.006(2) 0.0154(19) 0.001(2) O3 0.061(2) 0.055(2) 0.0335(19) 0.0038(17) 0.0213(17) 0.0002(19) O4 0.058(2) 0.076(3) 0.063(3) 0.009(2) 0.014(2) 0.004(2) N1 0.081(3) 0.068(4) 0.042(3) 0.009(3) 0.025(3) 0.003(3) C1 0.058(4) 0.079(5) 0.034(3) 0.020(3) 0.013(3) -0.007(3) C2 0.061(4) 0.058(4) 0.036(3) 0.001(3) 0.015(3) 0.003(3) C3 0.107(6) 0.111(7) 0.064(4) 0.014(4) 0.049(4) 0.042(5) C5 0.109(7) 0.146(9) 0.121(8) -0.049(7) 0.049(6) 0.022(6) C6 0.065(4) 0.055(4) 0.088(5) -0.008(4) 0.019(4) -0.002(3) C7 0.119(6) 0.070(5) 0.064(4) 0.012(4) 0.018(4) -0.014(5) C8 0.135(7) 0.079(6) 0.102(6) -0.019(5) 0.079(5) -0.018(5) Li1 0.055(5) 0.045(6) 0.039(5) 0.004(4) 0.014(4) 0.002(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 O3 1.488(4) . ? P1 O2 1.580(4) . ? P1 O1 1.585(4) . ? P1 C1 1.689(6) . ? P1 Li1 3.002(9) 7_656 ? O1 C3 1.465(7) . ? O2 C6 1.452(7) . ? O3 Li1 1.925(9) . ? O3 Li1 1.926(10) 7_656 ? O4 C12A 1.27(3) . ? O4 C9 1.419(12) . ? O4 C12 1.522(13) . ? O4 C9A 1.63(3) . ? O4 Li1 1.949(9) . ? N1 C2 1.160(7) . ? N1 Li1 1.957(10) 6_556 ? C1 C2 1.379(8) . ? C3 C5 1.471(12) . ? C3 C4 1.643(17) . ? C6 C7 1.497(9) . ? C6 C8 1.539(10) . ? C9 C10 1.497(18) . ? C10 C11 1.317(18) . ? C11 C12 1.525(15) . ? C9A C10A 1.70(4) . ? C10A C11A 1.68(5) . ? C11A C12A 1.79(4) . ? Li1 O3 1.926(10) 7_656 ? Li1 N1 1.957(10) 6 ? Li1 Li1 2.615(17) 7_656 ? Li1 P1 3.002(9) 7_656 ? 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 O3 P1 O2 114.1(2) . . ? O3 P1 O1 105.6(2) . . ? O2 P1 O1 98.3(2) . . ? O3 P1 C1 112.0(3) . . ? O2 P1 C1 110.2(3) . . ? O1 P1 C1 116.0(3) . . ? O3 P1 Li1 32.7(2) . 7_656 ? O2 P1 Li1 145.8(2) . 7_656 ? O1 P1 Li1 100.5(2) . 7_656 ? C1 P1 Li1 86.7(3) . 7_656 ? C3 O1 P1 122.0(4) . . ? C6 O2 P1 121.6(3) . . ? P1 O3 Li1 148.0(4) . . ? P1 O3 Li1 122.6(3) . 7_656 ? Li1 O3 Li1 85.5(4) . 7_656 ? C12A O4 C9 92.8(16) . . ? C12A O4 C12 16.0(15) . . ? C9 O4 C12 108.5(8) . . ? C12A O4 C9A 119.6(19) . . ? C9 O4 C9A 27.5(11) . . ? C12 O4 C9A 135.5(13) . . ? C12A O4 Li1 124.6(15) . . ? C9 O4 Li1 122.0(6) . . ? C12 O4 Li1 111.1(6) . . ? C9A O4 Li1 105.0(12) . . ? C2 N1 Li1 170.3(6) . 6_556 ? C2 C1 P1 124.0(5) . . ? N1 C2 C1 179.5(6) . . ? O1 C3 C5 107.8(7) . . ? O1 C3 C4 103.1(7) . . ? C5 C3 C4 106.1(8) . . ? O2 C6 C7 108.3(5) . . ? O2 C6 C8 107.1(6) . . ? C7 C6 C8 111.1(6) . . ? O4 C9 C10 104.8(11) . . ? C11 C10 C9 113.2(12) . . ? C10 C11 C12 107.4(11) . . ? O4 C12 C11 102.8(9) . . ? O4 C9A C10A 92(2) . . ? C11A C10A C9A 90(2) . . ? C10A C11A C12A 88(2) . . ? O4 C12A C11A 97(2) . . ? O3 Li1 O3 94.5(4) . 7_656 ? O3 Li1 O4 106.3(4) . . ? O3 Li1 O4 109.1(5) 7_656 . ? O3 Li1 N1 122.5(5) . 6 ? O3 Li1 N1 115.3(5) 7_656 6 ? O4 Li1 N1 108.0(4) . 6 ? O3 Li1 Li1 47.3(3) . 7_656 ? O3 Li1 Li1 47.2(3) 7_656 7_656 ? O4 Li1 Li1 116.6(6) . 7_656 ? N1 Li1 Li1 135.3(6) 6 7_656 ? O3 Li1 P1 118.1(4) . 7_656 ? O3 Li1 P1 24.69(16) 7_656 7_656 ? O4 Li1 P1 106.2(4) . 7_656 ? N1 Li1 P1 94.4(3) 6 7_656 ? Li1 Li1 P1 71.2(4) 7_656 7_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C3 -167.0(5) . . . . ? O2 P1 O1 C3 75.0(5) . . . . ? C1 P1 O1 C3 -42.4(6) . . . . ? Li1 P1 O1 C3 -133.8(5) 7_656 . . . ? O3 P1 O2 C6 71.4(5) . . . . ? O1 P1 O2 C6 -177.3(4) . . . . ? C1 P1 O2 C6 -55.6(5) . . . . ? Li1 P1 O2 C6 60.1(6) 7_656 . . . ? O2 P1 O3 Li1 43.7(7) . . . . ? O1 P1 O3 Li1 -63.1(7) . . . . ? C1 P1 O3 Li1 169.8(7) . . . . ? Li1 P1 O3 Li1 -148.1(7) 7_656 . . . ? O2 P1 O3 Li1 -168.2(4) . . . 7_656 ? O1 P1 O3 Li1 85.0(4) . . . 7_656 ? C1 P1 O3 Li1 -42.1(5) . . . 7_656 ? O3 P1 C1 C2 -166.1(5) . . . . ? O2 P1 C1 C2 -37.9(7) . . . . ? O1 P1 C1 C2 72.6(7) . . . . ? Li1 P1 C1 C2 172.6(6) 7_656 . . . ? Li1 N1 C2 C1 -97(78) 6_556 . . . ? P1 C1 C2 N1 -143(77) . . . . ? P1 O1 C3 C5 137.5(6) . . . . ? P1 O1 C3 C4 -110.6(8) . . . . ? P1 O2 C6 C7 137.3(4) . . . . ? P1 O2 C6 C8 -102.9(5) . . . . ? C12A O4 C9 C10 5.8(17) . . . . ? C12 O4 C9 C10 9.2(12) . . . . ? C9A O4 C9 C10 -162(3) . . . . ? Li1 O4 C9 C10 140.2(9) . . . . ? O4 C9 C10 C11 2.9(18) . . . . ? C9 C10 C11 C12 -13.6(18) . . . . ? C12A O4 C12 C11 -4(5) . . . . ? C9 O4 C12 C11 -16.5(10) . . . . ? C9A O4 C12 C11 -10.9(19) . . . . ? Li1 O4 C12 C11 -153.2(7) . . . . ? C10 C11 C12 O4 18.1(14) . . . . ? C12A O4 C9A C10A -19(2) . . . . ? C9 O4 C9A C10A -6(2) . . . . ? C12 O4 C9A C10A -17(2) . . . . ? Li1 O4 C9A C10A 126.7(13) . . . . ? O4 C9A C10A C11A 54.0(17) . . . . ? C9A C10A C11A C12A -66.0(19) . . . . ? C9 O4 C12A C11A -30.0(18) . . . . ? C12 O4 C12A C11A 162(7) . . . . ? C9A O4 C12A C11A -24(3) . . . . ? Li1 O4 C12A C11A -162.5(13) . . . . ? C10A C11A C12A O4 57(2) . . . . ? P1 O3 Li1 O3 153.5(6) . . . 7_656 ? Li1 O3 Li1 O3 0.0 7_656 . . 7_656 ? P1 O3 Li1 O4 42.1(9) . . . . ? Li1 O3 Li1 O4 -111.4(6) 7_656 . . . ? P1 O3 Li1 N1 -82.6(8) . . . 6 ? Li1 O3 Li1 N1 123.9(7) 7_656 . . 6 ? P1 O3 Li1 Li1 153.5(6) . . . 7_656 ? P1 O3 Li1 P1 161.1(4) . . . 7_656 ? Li1 O3 Li1 P1 7.64(17) 7_656 . . 7_656 ? C12A O4 Li1 O3 53.2(18) . . . . ? C9 O4 Li1 O3 -66.8(9) . . . . ? C12 O4 Li1 O3 63.1(7) . . . . ? C9A O4 Li1 O3 -90.5(13) . . . . ? C12A O4 Li1 O3 -47.6(18) . . . 7_656 ? C9 O4 Li1 O3 -167.6(7) . . . 7_656 ? C12 O4 Li1 O3 -37.7(7) . . . 7_656 ? C9A O4 Li1 O3 168.7(13) . . . 7_656 ? C12A O4 Li1 N1 -173.6(17) . . . 6 ? C9 O4 Li1 N1 66.4(9) . . . 6 ? C12 O4 Li1 N1 -163.7(6) . . . 6 ? C9A O4 Li1 N1 42.7(13) . . . 6 ? C12A O4 Li1 Li1 3.3(19) . . . 7_656 ? C9 O4 Li1 Li1 -116.6(9) . . . 7_656 ? C12 O4 Li1 Li1 13.3(9) . . . 7_656 ? C9A O4 Li1 Li1 -140.4(13) . . . 7_656 ? C12A O4 Li1 P1 -73.4(17) . . . 7_656 ? C9 O4 Li1 P1 166.7(7) . . . 7_656 ? C12 O4 Li1 P1 -63.4(6) . . . 7_656 ? C9A O4 Li1 P1 143.0(12) . . . 7_656 ? _diffrn_measured_fraction_theta_max 0.446 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.446 _refine_diff_density_max 0.326 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.060 #===END