Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Beswick, Michael A.' 'Elvidge, Benjamin L.' 'Feeder, Neil' 'Kidd, Sara J.' 'Wright, Dominic S.' _publ_contact_author_name 'Dr Dominic S Wright' _publ_contact_author_address ; Dr Dominic S Wright University of Cambridge Lensfiedl Road Cambridge CB2 1EW UNITED KINGDOM ; data_dw0028 _database_code_CSD 150926 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 N4 P2' _chemical_formula_weight 292.34 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 11.3660(4) _cell_length_b 15.4720(4) _cell_length_c 9.9800(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1755.03(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13503 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.240 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2914 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.04 _reflns_number_total 1603 _reflns_number_gt 1320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; "Collect" data collection software, Nonius B.V., 1998. ; _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; "Collect" data collection software, Nonius B.V., 1998. ; _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^)+(0.0357P)^2^+0.8363P] 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 1603 _refine_ls_number_parameters 102 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 1.205 _refine_ls_shift/su_mean 0.018 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 0.32038(5) 0.2500 0.84367(6) 0.02634(19) Uani 1 2 d S . . P2 P 0.37345(6) 0.2500 0.59038(6) 0.0329(2) Uani 1 2 d S . . N1 N 0.36501(12) 0.17760(9) 0.72195(13) 0.0287(3) Uani 1 1 d . . . N2 N 0.42691(18) 0.2500 0.9578(2) 0.0329(5) Uani 1 2 d SD . . H2A H 0.4958(16) 0.2500 0.928(3) 0.039 Uiso 1 2 d SD . . N3 N 0.5135(2) 0.2500 0.5422(2) 0.0449(6) Uani 1 2 d SD . . H3A H 0.571(2) 0.2500 0.600(3) 0.054 Uiso 1 2 d SD . . H3B H 0.528(3) 0.2500 0.4589(19) 0.054 Uiso 1 2 d SD . . C11 C 0.18995(16) 0.08808(14) 0.6664(2) 0.0513(6) Uani 1 1 d . . . H11A H 0.1426 0.1184 0.7337 0.077 Uiso 1 1 calc R . . H11B H 0.1622 0.0284 0.6579 0.077 Uiso 1 1 calc R . . H11C H 0.1824 0.1175 0.5799 0.077 Uiso 1 1 calc R . . C12 C 0.39302(16) 0.04080(13) 0.6051(2) 0.0478(5) Uani 1 1 d . . . H12A H 0.3836 0.0691 0.5180 0.072 Uiso 1 1 calc R . . H12B H 0.3668 -0.0194 0.5987 0.072 Uiso 1 1 calc R . . H12C H 0.4760 0.0423 0.6315 0.072 Uiso 1 1 calc R . . C13 C 0.33280(19) 0.04390(12) 0.8448(2) 0.0498(5) Uani 1 1 d . . . H13A H 0.4156 0.0452 0.8720 0.075 Uiso 1 1 calc R . . H13B H 0.3065 -0.0162 0.8378 0.075 Uiso 1 1 calc R . . H13C H 0.2850 0.0742 0.9117 0.075 Uiso 1 1 calc R . . C14 C 0.31931(15) 0.08808(11) 0.70979(18) 0.0348(4) Uani 1 1 d . . . C22 C 0.4808(2) 0.33003(13) 1.1592(2) 0.0635(7) Uani 1 1 d . . . H22A H 0.5636 0.3287 1.1322 0.095 Uiso 1 1 calc R . . H22B H 0.4754 0.3310 1.2572 0.095 Uiso 1 1 calc R . . H22C H 0.4432 0.3819 1.1224 0.095 Uiso 1 1 calc R . . C23 C 0.2909(3) 0.2500 1.1497(3) 0.0780(12) Uani 1 2 d S . . H23A H 0.2867 0.2416 1.2470 0.117 Uiso 0.50 1 calc PR A -1 H23B H 0.2489 0.2030 1.1046 0.117 Uiso 0.50 1 calc PR A -1 H23C H 0.2546 0.3054 1.1261 0.117 Uiso 0.50 1 calc PR A -1 C24 C 0.4185(2) 0.2500 1.1058(2) 0.0347(6) Uani 1 2 d S . . 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 0.0267(3) 0.0291(3) 0.0232(3) 0.000 0.0014(3) 0.000 P2 0.0298(4) 0.0464(4) 0.0227(3) 0.000 0.0004(3) 0.000 N1 0.0303(7) 0.0310(7) 0.0249(8) -0.0036(6) 0.0019(6) -0.0018(6) N2 0.0273(11) 0.0484(13) 0.0230(11) 0.000 -0.0002(9) 0.000 N3 0.0337(13) 0.0751(16) 0.0260(12) 0.000 0.0058(10) 0.000 C11 0.0341(11) 0.0500(12) 0.0699(15) -0.0185(11) -0.0003(10) -0.0058(9) C12 0.0423(11) 0.0449(11) 0.0562(13) -0.0218(10) 0.0035(10) 0.0010(9) C13 0.0668(14) 0.0308(10) 0.0518(13) 0.0009(9) 0.0044(11) -0.0059(9) C14 0.0324(9) 0.0317(9) 0.0402(10) -0.0093(8) 0.0020(8) -0.0028(7) C22 0.105(2) 0.0461(12) 0.0396(12) -0.0038(10) -0.0172(12) -0.0095(12) C23 0.059(2) 0.149(4) 0.0264(16) 0.000 0.0090(15) 0.000 C24 0.0438(15) 0.0380(14) 0.0224(12) 0.000 -0.0041(11) 0.000 _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 1.663(2) . ? P1 N1 1.7285(14) . ? P1 N1 1.7285(14) 8_565 ? P1 P2 2.5988(9) . ? P2 N3 1.663(2) . ? P2 N1 1.7287(14) 8_565 ? P2 N1 1.7287(14) . ? N1 C14 1.484(2) . ? N2 C24 1.480(3) . ? N2 H2A 0.838(17) . ? N3 H3A 0.874(17) . ? N3 H3B 0.848(17) . ? C11 C14 1.533(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.526(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.519(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C22 C24 1.522(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.515(4) . ? C23 H23A 0.9802 . ? C23 H23B 0.9802 . ? C23 H23C 0.9802 . ? C24 C22 1.522(2) 8_565 ? 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 N1 105.54(7) . . ? N2 P1 N1 105.54(7) . 8_565 ? N1 P1 N1 80.79(9) . 8_565 ? N2 P1 P2 119.84(8) . . ? N1 P1 P2 41.26(5) . . ? N1 P1 P2 41.26(5) 8_565 . ? N3 P2 N1 105.81(8) . 8_565 ? N3 P2 N1 105.81(8) . . ? N1 P2 N1 80.78(9) 8_565 . ? N3 P2 P1 120.21(9) . . ? N1 P2 P1 41.26(5) 8_565 . ? N1 P2 P1 41.26(5) . . ? C14 N1 P1 124.02(11) . . ? C14 N1 P2 124.20(11) . . ? P1 N1 P2 97.48(7) . . ? C24 N2 P1 129.58(18) . . ? C24 N2 H2A 114.6(19) . . ? P1 N2 H2A 115.8(19) . . ? P2 N3 H3A 122(2) . . ? P2 N3 H3B 118(2) . . ? H3A N3 H3B 120(3) . . ? C14 C11 H11A 109.5 . . ? C14 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C14 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 H12A 109.5 . . ? C14 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C14 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C13 108.19(14) . . ? N1 C14 C12 108.13(14) . . ? C13 C14 C12 109.64(16) . . ? N1 C14 C11 111.03(14) . . ? C13 C14 C11 110.34(16) . . ? C12 C14 C11 109.47(15) . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? N2 C24 C23 110.5(2) . . ? N2 C24 C22 108.62(15) . . ? C23 C24 C22 110.08(17) . . ? N2 C24 C22 108.62(15) . 8_565 ? C23 C24 C22 110.08(17) . 8_565 ? C22 C24 C22 108.9(2) . 8_565 ? 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 N2 P1 P2 N3 0.0 . . . . ? N1 P1 P2 N3 -79.31(7) . . . . ? N1 P1 P2 N3 79.31(7) 8_565 . . . ? N2 P1 P2 N1 -79.31(7) . . . 8_565 ? N1 P1 P2 N1 -158.62(14) . . . 8_565 ? N2 P1 P2 N1 79.31(7) . . . . ? N1 P1 P2 N1 158.62(14) 8_565 . . . ? N2 P1 N1 C14 101.63(14) . . . . ? N1 P1 N1 C14 -154.68(10) 8_565 . . . ? P2 P1 N1 C14 -140.58(16) . . . . ? N2 P1 N1 P2 -117.79(7) . . . . ? N1 P1 N1 P2 -14.10(9) 8_565 . . . ? N3 P2 N1 C14 -101.48(14) . . . . ? N1 P2 N1 C14 154.58(10) 8_565 . . . ? P1 P2 N1 C14 140.48(16) . . . . ? N3 P2 N1 P1 118.04(8) . . . . ? N1 P2 N1 P1 14.10(9) 8_565 . . . ? N1 P1 N2 C24 -137.73(5) . . . . ? N1 P1 N2 C24 137.73(5) 8_565 . . . ? P2 P1 N2 C24 180.0 . . . . ? P1 N1 C14 C13 -52.73(18) . . . . ? P2 N1 C14 C13 176.84(12) . . . . ? P1 N1 C14 C12 -171.41(12) . . . . ? P2 N1 C14 C12 58.16(18) . . . . ? P1 N1 C14 C11 68.49(19) . . . . ? P2 N1 C14 C11 -61.94(19) . . . . ? P1 N2 C24 C23 0.0 . . . . ? P1 N2 C24 C22 -120.86(16) . . . . ? P1 N2 C24 C22 120.86(16) . . . 8_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.310 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.037 data_dw0030 _database_code_CSD 150927 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H34 N5 P2 Sb' _chemical_formula_weight 456.15 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' 'Sb' 'Sb' -0.5866 1.5461 '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)/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 9.560(2) _cell_length_b 14.260(3) _cell_length_c 16.030(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.53(3) _cell_angle_gamma 90.00 _cell_volume 2184.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.099 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995); _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13136 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.66 _reflns_number_total 4947 _reflns_number_gt 3891 _reflns_threshold_expression >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _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^)+(0.1000P)^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 4947 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1400 _refine_ls_R_factor_gt 0.1156 _refine_ls_wR_factor_ref 0.3267 _refine_ls_wR_factor_gt 0.3163 _refine_ls_goodness_of_fit_ref 2.134 _refine_ls_restrained_S_all 2.134 _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 Sb1 Sb 0.10902(7) 0.03564(5) 0.43220(5) 0.0284(3) Uani 1 1 d . . . N1 N 0.2549(9) -0.1378(7) 0.6470(6) 0.030(2) Uani 1 1 d . . . N2 N 0.0624(11) -0.1544(7) 0.7630(6) 0.039(2) Uani 1 1 d . . . H2A H 0.0447 -0.0977 0.7437 0.047 Uiso 1 1 calc R . . N3 N 0.0693(9) -0.2272(6) 0.6034(6) 0.0286(19) Uani 1 1 d . . . N4 N 0.0821(10) -0.0681(7) 0.5208(6) 0.0298(19) Uani 1 1 d . . . N5 N 0.0435(11) -0.0326(6) 0.3250(7) 0.037(2) Uani 1 1 d . . . P1 P 0.1593(3) -0.2202(2) 0.70167(17) 0.0284(6) Uani 1 1 d . . . P2 P 0.1848(3) -0.15916(19) 0.54841(17) 0.0268(6) Uani 1 1 d . . . C1 C 0.4171(16) -0.0847(15) 0.7539(10) 0.068(5) Uani 1 1 d . . . H1A H 0.5146 -0.0685 0.7678 0.102 Uiso 1 1 calc R . . H1B H 0.3870 -0.1360 0.7900 0.102 Uiso 1 1 calc R . . H1C H 0.3575 -0.0298 0.7624 0.102 Uiso 1 1 calc R . . C2 C 0.4438(16) -0.0359(10) 0.6075(12) 0.058(4) Uani 1 1 d . . . H2B H 0.4357 -0.0572 0.5494 0.088 Uiso 1 1 calc R . . H2C H 0.5404 -0.0163 0.6200 0.088 Uiso 1 1 calc R . . H2D H 0.3806 0.0172 0.6157 0.088 Uiso 1 1 calc R . . C3 C 0.4051(11) -0.1149(9) 0.6649(7) 0.035(3) Uani 1 1 d . . . C4 C 0.4988(14) -0.1992(12) 0.6490(10) 0.056(4) Uani 1 1 d . . . H4B H 0.4913 -0.2167 0.5900 0.084 Uiso 1 1 calc R . . H4C H 0.4691 -0.2521 0.6834 0.084 Uiso 1 1 calc R . . H4D H 0.5960 -0.1831 0.6636 0.084 Uiso 1 1 calc R . . C5 C 0.1284(15) -0.3916(10) 0.5657(8) 0.050(3) Uani 1 1 d . . . H5A H 0.1723 -0.4024 0.6208 0.074 Uiso 1 1 calc R . . H5B H 0.1992 -0.3695 0.5272 0.074 Uiso 1 1 calc R . . H5C H 0.0876 -0.4503 0.5446 0.074 Uiso 1 1 calc R . . C6 C -0.0989(17) -0.3524(11) 0.6319(11) 0.059(4) Uani 1 1 d . . . H6A H -0.0569 -0.3618 0.6877 0.088 Uiso 1 1 calc R . . H6B H -0.1375 -0.4119 0.6111 0.088 Uiso 1 1 calc R . . H6C H -0.1739 -0.3058 0.6347 0.088 Uiso 1 1 calc R . . C7 C -0.0540(18) -0.3014(10) 0.4844(9) 0.055(4) Uani 1 1 d . . . H7A H 0.0175 -0.2792 0.4464 0.083 Uiso 1 1 calc R . . H7B H -0.1285 -0.2544 0.4878 0.083 Uiso 1 1 calc R . . H7C H -0.0936 -0.3605 0.4633 0.083 Uiso 1 1 calc R . . C8 C 0.0133(13) -0.3175(8) 0.5726(7) 0.036(3) Uani 1 1 d . . . C9 C -0.1576(15) -0.1744(12) 0.8314(10) 0.058(4) Uani 1 1 d . . . H9A H -0.1858 -0.2235 0.7917 0.086 Uiso 1 1 calc R . . H9B H -0.1884 -0.1132 0.8100 0.086 Uiso 1 1 calc R . . H9C H -0.2008 -0.1863 0.8852 0.086 Uiso 1 1 calc R . . C10 C 0.047(2) -0.1001(13) 0.9053(10) 0.071(5) Uani 1 1 d . . . H10A H 0.1486 -0.1013 0.9131 0.106 Uiso 1 1 calc R . . H10B H 0.0027 -0.1122 0.9588 0.106 Uiso 1 1 calc R . . H10C H 0.0174 -0.0384 0.8844 0.106 Uiso 1 1 calc R . . C11 C 0.054(2) -0.2735(12) 0.8737(10) 0.065(5) Uani 1 1 d . . . H11A H 0.0245 -0.3212 0.8328 0.098 Uiso 1 1 calc R . . H11B H 0.0127 -0.2878 0.9277 0.098 Uiso 1 1 calc R . . H11C H 0.1559 -0.2733 0.8798 0.098 Uiso 1 1 calc R . . C12 C 0.0021(14) -0.1746(9) 0.8432(8) 0.043(3) Uani 1 1 d . . . C13 C 0.1543(16) -0.0718(11) 0.2752(9) 0.052(3) Uani 1 1 d . . . H13A H 0.1131 -0.1024 0.2256 0.078 Uiso 1 1 calc R . . H13B H 0.2075 -0.1179 0.3084 0.078 Uiso 1 1 calc R . . H13C H 0.2170 -0.0214 0.2579 0.078 Uiso 1 1 calc R . . C14 C -0.0818(14) -0.0883(11) 0.3235(8) 0.049(3) Uani 1 1 d . . . H14A H -0.0959 -0.1161 0.2680 0.074 Uiso 1 1 calc R . . H14B H -0.1620 -0.0486 0.3362 0.074 Uiso 1 1 calc R . . H14C H -0.0728 -0.1383 0.3653 0.074 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 Sb1 0.0253(5) 0.0291(5) 0.0308(5) 0.0055(3) 0.0018(3) -0.0011(3) N1 0.018(4) 0.045(5) 0.028(5) 0.006(4) -0.001(3) 0.000(4) N2 0.045(6) 0.037(5) 0.035(5) 0.009(4) 0.010(4) 0.006(4) N3 0.030(5) 0.028(5) 0.028(5) 0.004(4) 0.000(3) 0.000(4) N4 0.031(5) 0.028(4) 0.031(5) 0.008(4) 0.004(4) 0.003(4) N5 0.038(6) 0.039(6) 0.035(6) 0.000(4) 0.007(4) 0.010(4) P1 0.0298(15) 0.0293(14) 0.0262(14) 0.0040(12) 0.0018(10) 0.0020(11) P2 0.0252(14) 0.0261(13) 0.0292(14) 0.0031(11) 0.0017(10) 0.0027(10) C1 0.042(9) 0.101(14) 0.060(9) -0.009(10) -0.013(7) -0.020(9) C2 0.033(7) 0.064(10) 0.078(11) 0.025(8) -0.005(7) -0.008(6) C3 0.021(5) 0.046(7) 0.038(6) 0.003(5) -0.003(4) -0.004(5) C4 0.034(7) 0.070(10) 0.066(9) 0.023(8) 0.003(6) 0.007(7) C5 0.072(10) 0.033(7) 0.044(8) -0.001(6) 0.001(6) 0.003(6) C6 0.058(9) 0.044(8) 0.075(10) -0.017(7) 0.015(7) -0.016(7) C7 0.078(11) 0.038(7) 0.049(8) -0.006(7) -0.014(7) -0.010(7) C8 0.047(7) 0.026(5) 0.033(6) -0.002(5) -0.001(5) -0.009(5) C9 0.049(9) 0.071(10) 0.054(9) 0.008(8) 0.015(6) -0.013(7) C10 0.080(12) 0.075(11) 0.058(10) -0.031(9) 0.001(8) 0.000(9) C11 0.093(13) 0.062(10) 0.042(8) 0.031(7) 0.015(8) 0.015(9) C12 0.050(8) 0.048(7) 0.033(6) 0.010(6) 0.014(5) 0.005(6) C13 0.059(9) 0.058(8) 0.039(7) -0.018(7) 0.011(6) 0.013(7) C14 0.043(8) 0.069(10) 0.035(6) -0.026(7) -0.003(5) -0.006(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 Sb1 N4 2.048(9) 3_556 ? Sb1 N5 2.057(11) . ? Sb1 N4 2.071(9) . ? Sb1 Sb1 3.2165(16) 3_556 ? N1 C3 1.493(14) . ? N1 P2 1.726(9) . ? N1 P1 1.739(9) . ? N2 C12 1.451(15) . ? N2 P1 1.660(10) . ? N3 C8 1.474(14) . ? N3 P2 1.729(9) . ? N3 P1 1.778(9) . ? N4 P2 1.680(9) . ? N4 Sb1 2.048(9) 3_556 ? N5 C14 1.437(18) . ? N5 C13 1.456(16) . ? P1 P2 2.624(4) . ? C1 C3 1.49(2) . ? C2 C3 1.507(19) . ? C3 C4 1.525(19) . ? C5 C8 1.532(19) . ? C6 C8 1.534(19) . ? C7 C8 1.556(18) . ? C9 C12 1.53(2) . ? C10 C12 1.51(2) . ? C11 C12 1.567(19) . ? 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 Sb1 N5 99.2(4) 3_556 . ? N4 Sb1 N4 77.3(4) 3_556 . ? N5 Sb1 N4 101.2(4) . . ? N4 Sb1 Sb1 38.9(2) 3_556 3_556 ? N5 Sb1 Sb1 103.1(3) . 3_556 ? N4 Sb1 Sb1 38.4(3) . 3_556 ? C3 N1 P2 124.2(7) . . ? C3 N1 P1 124.5(7) . . ? P2 N1 P1 98.4(5) . . ? C12 N2 P1 130.8(9) . . ? C8 N3 P2 123.5(7) . . ? C8 N3 P1 120.6(7) . . ? P2 N3 P1 96.8(5) . . ? P2 N4 Sb1 126.8(5) . 3_556 ? P2 N4 Sb1 130.5(5) . . ? Sb1 N4 Sb1 102.7(4) 3_556 . ? C14 N5 C13 113.4(11) . . ? C14 N5 Sb1 120.7(8) . . ? C13 N5 Sb1 115.5(9) . . ? N2 P1 N1 103.1(5) . . ? N2 P1 N3 107.0(5) . . ? N1 P1 N3 80.8(4) . . ? N2 P1 P2 115.8(4) . . ? N1 P1 P2 40.6(3) . . ? N3 P1 P2 40.9(3) . . ? N4 P2 N1 108.3(5) . . ? N4 P2 N3 101.0(4) . . ? N1 P2 N3 82.5(4) . . ? N4 P2 P1 115.8(3) . . ? N1 P2 P1 41.0(3) . . ? N3 P2 P1 42.3(3) . . ? C1 C3 N1 107.2(10) . . ? C1 C3 C2 110.8(13) . . ? N1 C3 C2 107.3(10) . . ? C1 C3 C4 110.9(12) . . ? N1 C3 C4 111.2(10) . . ? C2 C3 C4 109.4(11) . . ? N3 C8 C5 111.8(10) . . ? N3 C8 C6 109.3(10) . . ? C5 C8 C6 109.7(11) . . ? N3 C8 C7 108.2(9) . . ? C5 C8 C7 108.4(11) . . ? C6 C8 C7 109.4(12) . . ? N2 C12 C10 109.4(12) . . ? N2 C12 C9 108.0(11) . . ? C10 C12 C9 110.0(12) . . ? N2 C12 C11 109.1(10) . . ? C10 C12 C11 110.2(13) . . ? C9 C12 C11 110.1(13) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 4.392 _refine_diff_density_min -2.164 _refine_diff_density_rms 0.394 data_dw0031 _database_code_CSD 150928 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H72 Li5 N7 P4' _chemical_formula_weight 713.55 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 9.7314(4) _cell_length_b 10.3230(2) _cell_length_c 21.8906(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.5070(10) _cell_angle_gamma 90.00 _cell_volume 2184.90(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.026 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995); _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13694 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6809 _reflns_number_observed 6116 _reflns_observed_criterion >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+0.5664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(8) _refine_ls_number_reflns 6792 _refine_ls_number_parameters 467 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_obs 0.0423 _refine_ls_wR_factor_all 0.1289 _refine_ls_wR_factor_obs 0.1043 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.023 _refine_ls_restrained_S_all 1.196 _refine_ls_restrained_S_obs 1.023 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.80710(7) 0.19309(7) 0.51717(4) 0.0270(2) Uani 1 d . . P2 P 0.87302(7) 0.21560(7) 0.40240(4) 0.0246(2) Uani 1 d . . P3 P 0.77379(8) 0.25469(7) 0.27828(4) 0.0250(2) Uani 1 d . . P4 P 0.52601(7) 0.28757(7) 0.21653(4) 0.0257(2) Uani 1 d . . Li1 Li 0.3950(6) 0.2620(6) 0.3667(3) 0.0432(14) Uani 1 d . . Li2 Li 0.5410(6) 0.1211(5) 0.3148(3) 0.0385(13) Uani 1 d . . Li3 Li 0.5739(6) 0.3890(5) 0.3320(3) 0.0402(13) Uani 1 d . . Li4 Li 0.6301(6) 0.3581(6) 0.4561(3) 0.0387(13) Uani 1 d . . Li5 Li 0.6048(6) 0.1009(6) 0.4388(3) 0.0433(14) Uani 1 d . . N1 N 0.7341(3) 0.2406(2) 0.35114(12) 0.0251(5) Uani 1 d . . C1 C 0.4164(4) 0.0476(3) 0.3862(2) 0.0380(8) Uani 1 d D . H1A H 0.3263(34) 0.0817(37) 0.3958(18) 0.066(7) Uiso 1 d D . H1B H 0.4517(39) -0.0071(38) 0.4210(16) 0.066(7) Uiso 1 d D . C2 C 0.3776(4) -0.0514(4) 0.3351(2) 0.0505(9) Uani 1 d . . H2A H 0.4511(4) -0.1180(4) 0.3369(2) 0.061 Uiso 1 calc R . H2B H 0.3756(4) -0.0068(4) 0.2949(2) 0.061 Uiso 1 calc R . C3 C 0.2377(5) -0.1201(5) 0.3375(2) 0.0679(12) Uani 1 d . . H3A H 0.2375(5) -0.1623(5) 0.3781(2) 0.082 Uiso 1 calc R . H3B H 0.1630(5) -0.0545(5) 0.3335(2) 0.082 Uiso 1 calc R . C4 C 0.2084(8) -0.2186(7) 0.2887(3) 0.122(3) Uani 1 d . . H4A H 0.1209(30) -0.2622(38) 0.2938(16) 0.183 Uiso 1 calc R . H4B H 0.2834(29) -0.2824(30) 0.2917(16) 0.183 Uiso 1 calc R . H4C H 0.2014(58) -0.1765(9) 0.2484(4) 0.183 Uiso 1 calc R . C5 C 0.4607(4) 0.4584(4) 0.4056(2) 0.0420(8) Uani 1 d D . H5B H 0.4321(40) 0.5199(38) 0.3743(17) 0.066(7) Uiso 1 d D . H5A H 0.3705(36) 0.4252(37) 0.4204(19) 0.066(7) Uiso 1 d D . C6 C 0.5013(5) 0.5492(4) 0.4587(2) 0.0554(11) Uani 1 d . . H6A H 0.5223(5) 0.4947(4) 0.4958(2) 0.066 Uiso 1 calc R . H6B H 0.5893(5) 0.5908(4) 0.4509(2) 0.066 Uiso 1 calc R . C7 C 0.4092(7) 0.6526(6) 0.4749(3) 0.103(2) Uani 1 d . . H7A H 0.3975(7) 0.7136(6) 0.4398(3) 0.124 Uiso 1 calc R . H7B H 0.3176(7) 0.6129(6) 0.4780(3) 0.124 Uiso 1 calc R . C8 C 0.4443(8) 0.7292(6) 0.5303(3) 0.114(3) Uani 1 d . . H8A H 0.3640(20) 0.7811(39) 0.5385(14) 0.171 Uiso 1 calc R . H8B H 0.5218(38) 0.7867(38) 0.5245(10) 0.171 Uiso 1 calc R . H8C H 0.4705(53) 0.6714(6) 0.5652(6) 0.171 Uiso 1 calc R . N2 N 0.8432(3) 0.3182(2) 0.46455(12) 0.0255(5) Uani 1 d . . C21 C 0.9477(3) 0.4203(3) 0.48519(15) 0.0333(7) Uani 1 d . . C22 C 1.0901(4) 0.3628(4) 0.5039(2) 0.0482(9) Uani 1 d . . H22A H 1.0850(7) 0.3017(20) 0.5379(8) 0.072 Uiso 1 calc R . H22B H 1.1552(7) 0.4324(5) 0.5172(12) 0.072 Uiso 1 calc R . H22C H 1.1217(12) 0.3172(22) 0.4688(4) 0.072 Uiso 1 calc R . C23 C 0.8983(4) 0.4907(4) 0.5401(2) 0.0442(9) Uani 1 d . . H23A H 0.8076(13) 0.5297(21) 0.5278(4) 0.066 Uiso 1 calc R . H23B H 0.9647(14) 0.5587(17) 0.5541(8) 0.066 Uiso 1 calc R . H23C H 0.8910(25) 0.4288(6) 0.5735(5) 0.066 Uiso 1 calc R . C24 C 0.9541(4) 0.5152(4) 0.4323(2) 0.0476(9) Uani 1 d . . H24A H 0.8625(7) 0.5534(19) 0.4212(8) 0.071 Uiso 1 calc R . H24B H 0.9832(26) 0.4693(6) 0.3967(4) 0.071 Uiso 1 calc R . H24C H 1.0208(20) 0.5839(14) 0.4450(4) 0.071 Uiso 1 calc R . N3 N 0.8174(3) 0.0947(2) 0.45085(11) 0.0274(5) Uani 1 d . . C31 C 0.8869(4) -0.0348(3) 0.4554(2) 0.0369(8) Uani 1 d . . C32 C 0.8150(5) -0.1179(4) 0.4996(2) 0.0549(11) Uani 1 d . . H32A H 0.7170(8) -0.1272(24) 0.4841(7) 0.082 Uiso 1 calc R . H32B H 0.8232(27) -0.0764(15) 0.5402(4) 0.082 Uiso 1 calc R . H32C H 0.8585(20) -0.2036(10) 0.5032(11) 0.082 Uiso 1 calc R . C33 C 1.0403(4) -0.0225(4) 0.4785(2) 0.0514(10) Uani 1 d . . H33A H 1.0869(6) 0.0279(22) 0.4490(6) 0.077 Uiso 1 calc R . H33B H 1.0817(7) -0.1090(4) 0.4830(12) 0.077 Uiso 1 calc R . H33C H 1.0507(4) 0.0215(23) 0.5185(6) 0.077 Uiso 1 calc R . C34 C 0.8674(4) -0.0957(3) 0.3915(2) 0.0469(9) Uani 1 d . . H34A H 0.7685(5) -0.1019(23) 0.3773(5) 0.070 Uiso 1 calc R . H34B H 0.9083(24) -0.1826(10) 0.3933(3) 0.070 Uiso 1 calc R . H34C H 0.9130(23) -0.0419(13) 0.3629(3) 0.070 Uiso 1 calc R . N4 N 0.6626(2) 0.3842(2) 0.25325(11) 0.0259(5) Uani 1 d . . C41 C 0.7132(4) 0.5026(3) 0.2239(2) 0.0372(8) Uani 1 d . . C42 C 0.5913(4) 0.5950(3) 0.2105(2) 0.0507(10) Uani 1 d . . H42A H 0.5578(18) 0.6209(20) 0.2492(2) 0.076 Uiso 1 calc R . H42B H 0.5168(11) 0.5516(9) 0.1844(10) 0.076 Uiso 1 calc R . H42C H 0.6211(8) 0.6720(12) 0.1893(11) 0.076 Uiso 1 calc R . C43 C 0.8246(4) 0.5665(4) 0.2696(2) 0.0503(10) Uani 1 d . . H43A H 0.7852(8) 0.5876(23) 0.3076(5) 0.075 Uiso 1 calc R . H43B H 0.8573(20) 0.6460(14) 0.2515(5) 0.075 Uiso 1 calc R . H43C H 0.9023(13) 0.5065(11) 0.2788(9) 0.075 Uiso 1 calc R . C44 C 0.7734(4) 0.4729(4) 0.1646(2) 0.0530(10) Uani 1 d . . H44A H 0.8515(18) 0.4130(21) 0.1731(3) 0.079 Uiso 1 calc R . H44B H 0.8056(26) 0.5534(5) 0.1472(7) 0.079 Uiso 1 calc R . H44C H 0.7023(9) 0.4330(24) 0.1353(5) 0.079 Uiso 1 calc R . N5 N 0.6414(2) 0.1577(2) 0.23973(11) 0.0255(5) Uani 1 d . . C51 C 0.6742(3) 0.0576(3) 0.19412(15) 0.0325(7) Uani 1 d . . C52 C 0.5401(4) -0.0108(4) 0.1693(2) 0.0446(9) Uani 1 d . . H52A H 0.4987(14) -0.0510(20) 0.2035(2) 0.067 Uiso 1 calc R . H52B H 0.5602(5) -0.0777(16) 0.1399(9) 0.067 Uiso 1 calc R . H52C H 0.4754(10) 0.0524(6) 0.1488(10) 0.067 Uiso 1 calc R . C53 C 0.7717(4) -0.0409(3) 0.2275(2) 0.0433(8) Uani 1 d . . H53A H 0.8584(10) 0.0020(6) 0.2432(10) 0.065 Uiso 1 calc R . H53B H 0.7909(21) -0.1099(13) 0.1989(3) 0.065 Uiso 1 calc R . H53C H 0.7287(11) -0.0782(17) 0.2618(7) 0.065 Uiso 1 calc R . C54 C 0.7406(4) 0.1165(4) 0.1407(2) 0.0432(8) Uani 1 d . . H54A H 0.8273(14) 0.1594(21) 0.1564(2) 0.065 Uiso 1 calc R . H54B H 0.6774(11) 0.1801(18) 0.1194(7) 0.065 Uiso 1 calc R . H54C H 0.7598(24) 0.0480(5) 0.1119(6) 0.065 Uiso 1 calc R . N6 N 0.6373(3) 0.2095(2) 0.51407(12) 0.0303(6) Uani 1 d . . C61 C 0.5684(3) 0.2001(3) 0.5710(2) 0.0346(7) Uani 1 d . . C62 C 0.5980(4) 0.0707(4) 0.6040(2) 0.0506(10) Uani 1 d . . H62A H 0.5671(25) -0.0005(4) 0.5762(4) 0.076 Uiso 1 calc R . H62B H 0.5484(23) 0.0672(11) 0.6405(7) 0.076 Uiso 1 calc R . H62C H 0.6976(6) 0.0626(12) 0.6165(11) 0.076 Uiso 1 calc R . C63 C 0.4124(4) 0.2089(4) 0.5513(2) 0.0538(10) Uani 1 d . . H63A H 0.3835(6) 0.1365(16) 0.5239(10) 0.081 Uiso 1 calc R . H63B H 0.3915(5) 0.2909(13) 0.5296(11) 0.081 Uiso 1 calc R . H63C H 0.3626(4) 0.2052(28) 0.5877(2) 0.081 Uiso 1 calc R . C64 C 0.6113(5) 0.3099(4) 0.6158(2) 0.0512(10) Uani 1 d . . H64A H 0.7096(8) 0.3012(15) 0.6308(10) 0.077 Uiso 1 calc R . H64B H 0.5564(20) 0.3057(16) 0.6506(6) 0.077 Uiso 1 calc R . H64C H 0.5955(26) 0.3932(4) 0.5948(4) 0.077 Uiso 1 calc R . N7 N 0.4190(2) 0.2800(2) 0.27082(12) 0.0287(6) Uani 1 d . . C71 C 0.2692(3) 0.3005(3) 0.2475(2) 0.0336(7) Uani 1 d . . C72 C 0.2152(4) 0.1976(4) 0.1995(2) 0.0565(11) Uani 1 d . . H72A H 0.2657(21) 0.2050(19) 0.1633(6) 0.085 Uiso 1 calc R . H72B H 0.1163(8) 0.2115(18) 0.1872(10) 0.085 Uiso 1 calc R . H72C H 0.2295(28) 0.1110(4) 0.2174(5) 0.085 Uiso 1 calc R . C73 C 0.2442(4) 0.4345(4) 0.2185(2) 0.0595(11) Uani 1 d . . H73A H 0.2997(25) 0.4439(12) 0.1841(9) 0.089 Uiso 1 calc R . H73B H 0.2710(30) 0.5013(4) 0.2494(4) 0.089 Uiso 1 calc R . H73C H 0.1460(7) 0.4440(12) 0.2035(13) 0.089 Uiso 1 calc R . C74 C 0.1822(4) 0.2890(5) 0.3007(2) 0.0552(11) Uani 1 d . . H74A H 0.2092(18) 0.3569(16) 0.3310(6) 0.066 Uiso 1 calc R . H74B H 0.1971(20) 0.2038(10) 0.3201(8) 0.066 Uiso 1 calc R . H74C H 0.0842(4) 0.2990(25) 0.2853(3) 0.066 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0281(4) 0.0318(4) 0.0200(4) 0.0015(3) -0.0017(3) 0.0046(3) P2 0.0223(4) 0.0296(4) 0.0212(4) 0.0016(3) -0.0007(3) 0.0022(3) P3 0.0214(3) 0.0315(4) 0.0215(4) 0.0020(3) -0.0001(3) -0.0023(3) P4 0.0245(4) 0.0313(4) 0.0200(4) 0.0019(3) -0.0033(3) -0.0021(3) Li1 0.033(3) 0.054(4) 0.042(3) -0.001(3) 0.001(3) 0.001(3) Li2 0.045(3) 0.033(3) 0.039(3) 0.003(2) 0.011(3) 0.001(2) Li3 0.052(4) 0.036(3) 0.033(3) 0.000(2) 0.009(3) -0.007(2) Li4 0.031(3) 0.040(3) 0.045(3) 0.007(3) 0.002(3) 0.005(2) Li5 0.036(3) 0.049(4) 0.043(3) -0.009(3) -0.003(3) 0.005(2) N1 0.0235(12) 0.0301(13) 0.0211(12) 0.0032(10) -0.0001(10) 0.0000(10) C1 0.038(2) 0.046(2) 0.030(2) 0.0043(14) 0.0015(15) -0.0062(15) C2 0.058(2) 0.046(2) 0.046(2) 0.001(2) -0.001(2) -0.012(2) C3 0.072(3) 0.064(3) 0.067(3) 0.001(2) 0.005(2) -0.024(2) C4 0.141(6) 0.102(5) 0.118(6) -0.035(4) -0.004(5) -0.066(4) C5 0.047(2) 0.045(2) 0.032(2) -0.0019(15) -0.001(2) 0.009(2) C6 0.075(3) 0.047(2) 0.043(2) -0.006(2) 0.001(2) 0.014(2) C7 0.111(4) 0.085(4) 0.111(5) -0.056(4) 0.001(4) 0.036(3) C8 0.166(7) 0.077(4) 0.112(5) -0.041(4) 0.077(5) -0.026(4) N2 0.0257(12) 0.0280(13) 0.0214(12) 0.0007(10) -0.0028(9) -0.0003(10) C21 0.032(2) 0.036(2) 0.030(2) -0.0046(13) -0.0059(14) -0.0063(13) C22 0.033(2) 0.056(2) 0.052(2) -0.007(2) -0.009(2) -0.007(2) C23 0.047(2) 0.046(2) 0.038(2) -0.010(2) -0.006(2) -0.008(2) C24 0.055(2) 0.044(2) 0.042(2) 0.003(2) -0.004(2) -0.019(2) N3 0.0311(14) 0.0299(13) 0.0207(13) 0.0014(10) -0.0001(11) 0.0064(10) C31 0.053(2) 0.028(2) 0.030(2) 0.0033(13) 0.006(2) 0.0156(14) C32 0.085(3) 0.033(2) 0.050(2) 0.013(2) 0.021(2) 0.015(2) C33 0.055(2) 0.056(2) 0.042(2) 0.002(2) -0.002(2) 0.030(2) C34 0.067(3) 0.031(2) 0.042(2) -0.004(2) 0.004(2) 0.012(2) N4 0.0253(12) 0.0269(13) 0.0242(13) 0.0056(10) -0.0030(10) -0.0030(10) C41 0.038(2) 0.036(2) 0.035(2) 0.0155(14) -0.0067(15) -0.0114(13) C42 0.058(2) 0.031(2) 0.059(3) 0.016(2) -0.007(2) -0.004(2) C43 0.052(2) 0.042(2) 0.052(2) 0.012(2) -0.013(2) -0.020(2) C44 0.055(2) 0.061(3) 0.044(2) 0.016(2) 0.009(2) -0.018(2) N5 0.0239(12) 0.0306(13) 0.0213(13) -0.0022(10) -0.0008(10) 0.0018(10) C51 0.038(2) 0.033(2) 0.026(2) -0.0049(13) 0.0036(14) 0.0013(13) C52 0.051(2) 0.046(2) 0.035(2) -0.013(2) -0.001(2) -0.009(2) C53 0.052(2) 0.041(2) 0.035(2) -0.0108(15) 0.001(2) 0.011(2) C54 0.051(2) 0.048(2) 0.033(2) -0.004(2) 0.014(2) 0.002(2) N6 0.0325(14) 0.0365(15) 0.0217(13) 0.0029(10) 0.0020(11) 0.0034(11) C61 0.035(2) 0.041(2) 0.029(2) 0.0061(13) 0.0082(14) 0.0068(13) C62 0.056(2) 0.052(2) 0.047(2) 0.018(2) 0.021(2) 0.013(2) C63 0.037(2) 0.078(3) 0.049(2) 0.009(2) 0.016(2) 0.007(2) C64 0.065(3) 0.053(2) 0.038(2) -0.008(2) 0.017(2) 0.005(2) N7 0.0215(12) 0.0353(14) 0.0282(14) 0.0012(11) -0.0023(11) -0.0010(10) C71 0.0219(15) 0.044(2) 0.033(2) 0.0016(14) -0.0050(13) -0.0007(13) C72 0.034(2) 0.065(3) 0.067(3) -0.013(2) -0.014(2) -0.004(2) C73 0.033(2) 0.056(2) 0.088(3) 0.019(2) -0.003(2) 0.012(2) C74 0.023(2) 0.095(3) 0.047(2) 0.006(2) 0.000(2) 0.005(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 N6 1.655(3) . ? P1 N3 1.784(3) . ? P1 N2 1.792(3) . ? P1 Li5 2.638(6) . ? P1 Li4 2.672(5) . ? P1 P2 2.6725(10) . ? P2 N1 1.676(3) . ? P2 N3 1.762(3) . ? P2 N2 1.774(3) . ? P2 Li5 3.053(6) . ? P3 N1 1.689(3) . ? P3 N4 1.768(2) . ? P3 N5 1.768(2) . ? P3 P4 2.6491(11) . ? P3 Li3 2.758(6) . ? P3 Li2 2.843(6) . ? P4 N7 1.668(3) . ? P4 N4 1.779(2) . ? P4 N5 1.785(2) . ? P4 Li3 2.727(6) . ? P4 Li2 2.744(6) . ? Li1 N7 2.147(7) . ? Li1 C1 2.259(7) . ? Li1 C5 2.263(7) . ? Li1 Li3 2.373(8) . ? Li1 Li2 2.407(8) . ? Li1 C71 2.783(7) . ? Li1 Li5 2.948(9) . ? Li1 Li4 3.005(8) . ? Li2 N5 2.040(6) . ? Li2 N7 2.184(6) . ? Li2 C1 2.218(6) . ? Li2 N1 2.313(6) . ? Li2 Li5 2.723(8) . ? Li2 Li3 2.805(7) . ? Li3 N4 2.014(6) . ? Li3 C5 2.173(7) . ? Li3 N1 2.193(7) . ? Li3 N7 2.208(6) . ? Li3 Li4 2.728(8) . ? Li4 N6 1.987(6) . ? Li4 N2 2.102(6) . ? Li4 C5 2.144(6) . ? Li4 Li5 2.690(8) . ? Li5 N6 1.989(6) . ? Li5 N3 2.057(6) . ? Li5 C1 2.124(7) . ? C1 C2 1.531(5) . ? C2 C3 1.541(6) . ? C3 C4 1.479(7) . ? C5 C6 1.511(5) . ? C6 C7 1.463(6) . ? C7 C8 1.455(8) . ? N2 C21 1.498(4) . ? C21 C22 1.520(5) . ? C21 C24 1.523(5) . ? C21 C23 1.527(5) . ? N3 C31 1.496(4) . ? C31 C32 1.523(5) . ? C31 C34 1.525(5) . ? C31 C33 1.526(5) . ? N4 C41 1.491(4) . ? C41 C44 1.513(5) . ? C41 C42 1.524(5) . ? C41 C43 1.538(5) . ? N5 C51 1.497(4) . ? C51 C53 1.519(5) . ? C51 C54 1.526(5) . ? C51 C52 1.528(5) . ? N6 C61 1.485(4) . ? C61 C64 1.526(5) . ? C61 C62 1.530(5) . ? C61 C63 1.533(5) . ? N7 C71 1.504(4) . ? C71 C74 1.520(5) . ? C71 C73 1.529(5) . ? C71 C72 1.544(5) . ? 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 N6 P1 N3 99.96(12) . . ? N6 P1 N2 99.64(12) . . ? N3 P1 N2 81.59(12) . . ? N6 P1 Li5 48.9(2) . . ? N3 P1 Li5 51.10(15) . . ? N2 P1 Li5 91.6(2) . . ? N6 P1 Li4 47.92(15) . . ? N3 P1 Li4 92.8(2) . . ? N2 P1 Li4 51.74(14) . . ? Li5 P1 Li4 60.9(2) . . ? N6 P1 P2 107.31(9) . . ? N3 P1 P2 40.78(8) . . ? N2 P1 P2 41.19(8) . . ? Li5 P1 P2 70.19(14) . . ? Li4 P1 P2 71.57(13) . . ? N1 P2 N3 103.45(12) . . ? N1 P2 N2 103.42(12) . . ? N3 P2 N2 82.71(12) . . ? N1 P2 P1 112.43(9) . . ? N3 P2 P1 41.39(8) . . ? N2 P2 P1 41.70(8) . . ? N1 P2 Li5 65.54(14) . . ? N3 P2 Li5 40.38(14) . . ? N2 P2 Li5 79.20(14) . . ? P1 P2 Li5 54.38(11) . . ? N1 P3 N4 99.24(12) . . ? N1 P3 N5 99.78(12) . . ? N4 P3 N5 83.86(12) . . ? N1 P3 P4 101.58(9) . . ? N4 P3 P4 41.85(8) . . ? N5 P3 P4 42.04(8) . . ? N1 P3 Li3 52.64(15) . . ? N4 P3 Li3 46.79(14) . . ? N5 P3 Li3 88.70(15) . . ? P4 P3 Li3 60.53(13) . . ? N1 P3 Li2 54.43(15) . . ? N4 P3 Li2 88.56(14) . . ? N5 P3 Li2 45.50(14) . . ? P4 P3 Li2 59.84(12) . . ? Li3 P3 Li2 60.1(2) . . ? N7 P4 N4 101.49(12) . . ? N7 P4 N5 100.68(12) . . ? N4 P4 N5 83.04(12) . . ? N7 P4 P3 103.65(9) . . ? N4 P4 P3 41.52(8) . . ? N5 P4 P3 41.55(8) . . ? N7 P4 Li3 54.03(15) . . ? N4 P4 Li3 47.58(15) . . ? N5 P4 Li3 89.4(2) . . ? P3 P4 Li3 61.72(13) . . ? N7 P4 Li2 52.72(14) . . ? N4 P4 Li2 91.51(15) . . ? N5 P4 Li2 47.99(14) . . ? P3 P4 Li2 63.59(12) . . ? Li3 P4 Li2 61.7(2) . . ? N7 Li1 C1 104.5(3) . . ? N7 Li1 C5 103.4(3) . . ? C1 Li1 C5 142.3(3) . . ? N7 Li1 Li3 58.2(2) . . ? C1 Li1 Li3 123.1(3) . . ? C5 Li1 Li3 55.9(2) . . ? N7 Li1 Li2 57.0(2) . . ? C1 Li1 Li2 56.6(2) . . ? C5 Li1 Li2 124.2(3) . . ? Li3 Li1 Li2 71.9(3) . . ? N7 Li1 C71 32.38(13) . . ? C1 Li1 C71 109.8(3) . . ? C5 Li1 C71 107.4(3) . . ? Li3 Li1 C71 83.2(2) . . ? Li2 Li1 C71 82.2(2) . . ? N7 Li1 Li5 115.3(3) . . ? C1 Li1 Li5 45.8(2) . . ? C5 Li1 Li5 98.9(3) . . ? Li3 Li1 Li5 89.7(3) . . ? Li2 Li1 Li5 60.1(2) . . ? C71 Li1 Li5 141.9(3) . . ? N7 Li1 Li4 116.7(3) . . ? C1 Li1 Li4 98.9(3) . . ? C5 Li1 Li4 45.4(2) . . ? Li3 Li1 Li4 59.6(2) . . ? Li2 Li1 Li4 93.5(3) . . ? C71 Li1 Li4 141.7(3) . . ? Li5 Li1 Li4 53.7(2) . . ? N5 Li2 N7 78.0(2) . . ? N5 Li2 C1 168.9(3) . . ? N7 Li2 C1 104.7(3) . . ? N5 Li2 N1 74.5(2) . . ? N7 Li2 N1 97.5(2) . . ? C1 Li2 N1 115.3(3) . . ? N5 Li2 Li1 129.1(3) . . ? N7 Li2 Li1 55.5(2) . . ? C1 Li2 Li1 58.3(2) . . ? N1 Li2 Li1 90.9(3) . . ? N5 Li2 Li5 137.9(3) . . ? N7 Li2 Li5 123.2(3) . . ? C1 Li2 Li5 49.6(2) . . ? N1 Li2 Li5 67.3(2) . . ? Li1 Li2 Li5 69.8(2) . . ? N5 Li2 P4 40.56(12) . . ? N7 Li2 P4 37.44(11) . . ? C1 Li2 P4 141.4(3) . . ? N1 Li2 P4 84.5(2) . . ? Li1 Li2 P4 90.6(2) . . ? Li5 Li2 P4 144.6(3) . . ? N5 Li2 Li3 82.4(2) . . ? N7 Li2 Li3 50.7(2) . . ? C1 Li2 Li3 107.8(2) . . ? N1 Li2 Li3 49.6(2) . . ? Li1 Li2 Li3 53.5(2) . . ? Li5 Li2 Li3 86.1(2) . . ? P4 Li2 Li3 58.8(2) . . ? N5 Li2 P3 38.19(12) . . ? N7 Li2 P3 85.5(2) . . ? C1 Li2 P3 151.7(3) . . ? N1 Li2 P3 36.45(10) . . ? Li1 Li2 P3 111.8(2) . . ? Li5 Li2 P3 102.6(2) . . ? P4 Li2 P3 56.57(11) . . ? Li3 Li2 P3 58.5(2) . . ? N4 Li3 C5 160.9(3) . . ? N4 Li3 N1 77.4(2) . . ? C5 Li3 N1 119.9(3) . . ? N4 Li3 N7 78.3(2) . . ? C5 Li3 N7 104.4(3) . . ? N1 Li3 N7 100.5(2) . . ? N4 Li3 Li1 131.4(3) . . ? C5 Li3 Li1 59.5(2) . . ? N1 Li3 Li1 94.8(3) . . ? N7 Li3 Li1 55.8(2) . . ? N4 Li3 P4 40.71(12) . . ? C5 Li3 P4 140.0(3) . . ? N1 Li3 P4 87.2(2) . . ? N7 Li3 P4 37.70(11) . . ? Li1 Li3 P4 91.7(2) . . ? N4 Li3 Li4 142.4(3) . . ? C5 Li3 Li4 50.3(2) . . ? N1 Li3 Li4 70.7(2) . . ? N7 Li3 Li4 126.2(3) . . ? Li1 Li3 Li4 71.8(2) . . ? P4 Li3 Li4 150.7(3) . . ? N4 Li3 P3 39.77(13) . . ? C5 Li3 P3 157.3(3) . . ? N1 Li3 P3 37.76(12) . . ? N7 Li3 P3 87.2(2) . . ? Li1 Li3 P3 115.9(3) . . ? P4 Li3 P3 57.75(12) . . ? Li4 Li3 P3 107.1(2) . . ? N4 Li3 Li2 85.1(2) . . ? C5 Li3 Li2 111.4(3) . . ? N1 Li3 Li2 53.4(2) . . ? N7 Li3 Li2 49.9(2) . . ? Li1 Li3 Li2 54.6(2) . . ? P4 Li3 Li2 59.5(2) . . ? Li4 Li3 Li2 91.5(2) . . ? P3 Li3 Li2 61.5(2) . . ? N6 Li4 N2 80.2(2) . . ? N6 Li4 C5 132.2(3) . . ? N2 Li4 C5 146.4(3) . . ? N6 Li4 P1 38.17(12) . . ? N2 Li4 P1 42.00(12) . . ? C5 Li4 P1 168.6(3) . . ? N6 Li4 Li5 47.4(2) . . ? N2 Li4 Li5 83.8(2) . . ? C5 Li4 Li5 110.6(3) . . ? P1 Li4 Li5 59.0(2) . . ? N6 Li4 Li3 135.6(3) . . ? N2 Li4 Li3 101.3(3) . . ? C5 Li4 Li3 51.3(2) . . ? P1 Li4 Li3 128.2(3) . . ? Li5 Li4 Li3 88.3(3) . . ? N6 Li4 Li1 97.5(3) . . ? N2 Li4 Li1 131.6(3) . . ? C5 Li4 Li1 48.7(2) . . ? P1 Li4 Li1 121.0(2) . . ? Li5 Li4 Li1 62.1(2) . . ? Li3 Li4 Li1 48.6(2) . . ? N6 Li5 N3 81.2(2) . . ? N6 Li5 C1 129.9(3) . . ? N3 Li5 C1 148.8(3) . . ? N6 Li5 P1 38.81(13) . . ? N3 Li5 P1 42.43(13) . . ? C1 Li5 P1 168.7(3) . . ? N6 Li5 Li4 47.4(2) . . ? N3 Li5 Li4 86.4(2) . . ? C1 Li5 Li4 113.1(3) . . ? P1 Li5 Li4 60.2(2) . . ? N6 Li5 Li2 141.2(3) . . ? N3 Li5 Li2 104.0(3) . . ? C1 Li5 Li2 52.7(2) . . ? P1 Li5 Li2 133.6(3) . . ? Li4 Li5 Li2 94.1(3) . . ? N6 Li5 Li1 99.2(3) . . ? N3 Li5 Li1 135.3(3) . . ? C1 Li5 Li1 49.7(2) . . ? P1 Li5 Li1 124.4(3) . . ? Li4 Li5 Li1 64.2(2) . . ? Li2 Li5 Li1 50.0(2) . . ? N6 Li5 P2 86.4(2) . . ? N3 Li5 P2 33.70(12) . . ? C1 Li5 P2 132.1(3) . . ? P1 Li5 P2 55.43(11) . . ? Li4 Li5 P2 65.6(2) . . ? Li2 Li5 P2 79.3(2) . . ? Li1 Li5 P2 101.7(2) . . ? P2 N1 P3 113.10(14) . . ? P2 N1 Li3 137.5(2) . . ? P3 N1 Li3 89.6(2) . . ? P2 N1 Li2 135.3(2) . . ? P3 N1 Li2 89.1(2) . . ? Li3 N1 Li2 77.0(2) . . ? C2 C1 Li5 134.1(3) . . ? C2 C1 Li2 79.8(2) . . ? Li5 C1 Li2 77.7(3) . . ? C2 C1 Li1 120.4(3) . . ? Li5 C1 Li1 84.5(3) . . ? Li2 C1 Li1 65.1(2) . . ? C1 C2 C3 115.3(3) . . ? C4 C3 C2 113.0(5) . . ? C6 C5 Li4 77.5(3) . . ? C6 C5 Li3 131.7(3) . . ? Li4 C5 Li3 78.4(3) . . ? C6 C5 Li1 152.0(3) . . ? Li4 C5 Li1 85.9(3) . . ? Li3 C5 Li1 64.6(2) . . ? C7 C6 C5 121.7(4) . . ? C8 C7 C6 120.4(6) . . ? C21 N2 P2 119.1(2) . . ? C21 N2 P1 119.3(2) . . ? P2 N2 P1 97.11(11) . . ? C21 N2 Li4 121.2(2) . . ? P2 N2 Li4 107.2(2) . . ? P1 N2 Li4 86.3(2) . . ? N2 C21 C22 111.9(3) . . ? N2 C21 C24 108.0(2) . . ? C22 C21 C24 109.9(3) . . ? N2 C21 C23 108.0(3) . . ? C22 C21 C23 109.4(3) . . ? C24 C21 C23 109.6(3) . . ? C31 N3 P2 120.3(2) . . ? C31 N3 P1 121.4(2) . . ? P2 N3 P1 97.83(12) . . ? C31 N3 Li5 118.4(3) . . ? P2 N3 Li5 105.9(2) . . ? P1 N3 Li5 86.5(2) . . ? N3 C31 C32 108.0(3) . . ? N3 C31 C34 107.5(3) . . ? C32 C31 C34 109.4(3) . . ? N3 C31 C33 111.4(3) . . ? C32 C31 C33 109.8(3) . . ? C34 C31 C33 110.7(3) . . ? C41 N4 P3 122.2(2) . . ? C41 N4 P4 122.1(2) . . ? P3 N4 P4 96.64(12) . . ? C41 N4 Li3 123.0(3) . . ? P3 N4 Li3 93.4(2) . . ? P4 N4 Li3 91.7(2) . . ? N4 C41 C44 112.5(3) . . ? N4 C41 C42 107.9(3) . . ? C44 C41 C42 109.3(3) . . ? N4 C41 C43 108.3(3) . . ? C44 C41 C43 109.3(3) . . ? C42 C41 C43 109.4(3) . . ? C51 N5 P3 120.7(2) . . ? C51 N5 P4 120.2(2) . . ? P3 N5 P4 96.40(12) . . ? C51 N5 Li2 124.5(2) . . ? P3 N5 Li2 96.3(2) . . ? P4 N5 Li2 91.4(2) . . ? N5 C51 C53 108.1(2) . . ? N5 C51 C54 112.1(3) . . ? C53 C51 C54 109.8(3) . . ? N5 C51 C52 108.6(3) . . ? C53 C51 C52 108.9(3) . . ? C54 C51 C52 109.3(3) . . ? C61 N6 P1 120.2(2) . . ? C61 N6 Li4 126.9(2) . . ? P1 N6 Li4 93.9(2) . . ? C61 N6 Li5 127.9(3) . . ? P1 N6 Li5 92.3(2) . . ? Li4 N6 Li5 85.1(3) . . ? N6 C61 C64 112.0(3) . . ? N6 C61 C62 112.0(3) . . ? C64 C61 C62 108.8(3) . . ? N6 C61 C63 106.6(3) . . ? C64 C61 C63 109.1(3) . . ? C62 C61 C63 108.2(3) . . ? C71 N7 P4 114.3(2) . . ? C71 N7 Li1 97.8(2) . . ? P4 N7 Li1 147.8(2) . . ? C71 N7 Li2 135.5(2) . . ? P4 N7 Li2 89.8(2) . . ? Li1 N7 Li2 67.5(2) . . ? C71 N7 Li3 134.6(2) . . ? P4 N7 Li3 88.3(2) . . ? Li1 N7 Li3 66.0(2) . . ? Li2 N7 Li3 79.4(2) . . ? N7 C71 C74 109.4(3) . . ? N7 C71 C73 111.7(3) . . ? C74 C71 C73 108.2(3) . . ? N7 C71 C72 112.0(3) . . ? C74 C71 C72 107.0(3) . . ? C73 C71 C72 108.3(3) . . ? N7 C71 Li1 49.8(2) . . ? C74 C71 Li1 59.6(2) . . ? C73 C71 Li1 123.4(3) . . ? C72 C71 Li1 128.3(3) . . ? _refine_diff_density_max 0.287 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.046