Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Chris Russell School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287599' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email Chris.Russell@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the crystal structure in paper B009240L 'Syntheses and X-ray crystal structures of tris(imido) arsenate anions' by Lisa T. Burke, John C. Jeffery, Angela P. Leedham, Christopher A. Russell, submitted to Dalton Transactions for publication.There are three crystal structures included in this file. ; #================================================================= loop_ _publ_author_name 'Lisa T. Burke' 'John C. Jeffery' 'Angela P. Leedham' 'Christopher A. Russell' data_angas _database_code_CSD 153207 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H29 As Li3 N3 O4' _chemical_formula_weight 531.25 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.4043(6) _cell_length_b 12.4742(7) _cell_length_c 20.2378(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.8070(10) _cell_angle_gamma 90.00 _cell_volume 2539.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? 0.5 _exptl_crystal_size_mid ? 0.5 _exptl_crystal_size_min ? 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.374 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? 0.50 _exptl_absorpt_correction_T_max ? 0.76 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_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 16090 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5851 _reflns_number_gt 4524 _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^)+(0.0454P)^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 5851 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _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 As1 As 0.456396(17) 0.178823(14) 0.044442(9) 0.02489(6) Uani 1 1 d . . . N1 N 0.61936(14) 0.13781(12) 0.02987(7) 0.0259(3) Uani 1 1 d . . . C11 C 0.72877(18) 0.20375(14) 0.05485(9) 0.0274(4) Uani 1 1 d . . . C12 C 0.7421(2) 0.28542(16) 0.10354(10) 0.0366(4) Uani 1 1 d . . . H12 H 0.6700 0.2999 0.1231 0.044 Uiso 1 1 calc R . . C13 C 0.8577(2) 0.34597(17) 0.12411(12) 0.0475(5) Uani 1 1 d . . . H13 H 0.8628 0.4010 0.1572 0.057 Uiso 1 1 calc R . . C14 C 0.9641(2) 0.32781(18) 0.09767(12) 0.0491(6) Uani 1 1 d . . . H14 H 1.0423 0.3701 0.1119 0.059 Uiso 1 1 calc R . . C15 C 0.95645(19) 0.24638(18) 0.04954(11) 0.0418(5) Uani 1 1 d . . . H15 H 1.0295 0.2327 0.0306 0.050 Uiso 1 1 calc R . . C16 C 0.84252(18) 0.18600(15) 0.02965(10) 0.0310(4) Uani 1 1 d . . . O1 O 0.82742(13) 0.10217(11) -0.01730(7) 0.0359(3) Uani 1 1 d . . . C17 C 0.9203(2) 0.09692(19) -0.05908(12) 0.0488(6) Uani 1 1 d . . . H17A H 0.9208 0.1655 -0.0826 0.073 Uiso 1 1 calc R . . H17B H 0.8938 0.0396 -0.0929 0.073 Uiso 1 1 calc R . . H17C H 1.0095 0.0821 -0.0302 0.073 Uiso 1 1 calc R . . N2 N 0.36161(14) 0.13032(11) -0.04271(7) 0.0250(3) Uani 1 1 d . . . C21 C 0.25210(17) 0.18949(14) -0.07790(9) 0.0270(4) Uani 1 1 d . . . C22 C 0.20997(19) 0.29003(15) -0.06023(11) 0.0346(4) Uani 1 1 d . . . H22 H 0.2582 0.3232 -0.0191 0.041 Uiso 1 1 calc R . . C23 C 0.1004(2) 0.34268(17) -0.10072(12) 0.0451(5) Uani 1 1 d . . . H23 H 0.0755 0.4108 -0.0870 0.054 Uiso 1 1 calc R . . C24 C 0.0277(2) 0.29753(19) -0.16030(12) 0.0468(6) Uani 1 1 d . . . H24 H -0.0465 0.3344 -0.1881 0.056 Uiso 1 1 calc R . . C25 C 0.0634(2) 0.19769(19) -0.17974(10) 0.0418(5) Uani 1 1 d . . . H25 H 0.0137 0.1657 -0.2210 0.050 Uiso 1 1 calc R . . C26 C 0.17159(18) 0.14482(16) -0.13899(9) 0.0316(4) Uani 1 1 d . . . O2 O 0.21285(13) 0.04336(12) -0.15385(7) 0.0400(3) Uani 1 1 d . . . C27 C 0.1283(3) -0.0163(2) -0.20799(13) 0.0693(8) Uani 1 1 d . . . H27A H 0.0384 -0.0190 -0.2012 0.104 Uiso 1 1 calc R . . H27B H 0.1629 -0.0893 -0.2082 0.104 Uiso 1 1 calc R . . H27C H 0.1255 0.0186 -0.2517 0.104 Uiso 1 1 calc R . . N3 N 0.43715(15) 0.05354(12) 0.09106(7) 0.0271(3) Uani 1 1 d . . . C31 C 0.37538(17) 0.05883(14) 0.14400(8) 0.0253(4) Uani 1 1 d . . . C32 C 0.28178(18) 0.13525(16) 0.15251(10) 0.0323(4) Uani 1 1 d . . . H32 H 0.2570 0.1913 0.1200 0.039 Uiso 1 1 calc R . . C33 C 0.2245(2) 0.13074(18) 0.20752(11) 0.0423(5) Uani 1 1 d . . . H33 H 0.1612 0.1834 0.2118 0.051 Uiso 1 1 calc R . . C34 C 0.2585(2) 0.05153(19) 0.25530(11) 0.0506(6) Uani 1 1 d . . . H34 H 0.2209 0.0503 0.2934 0.061 Uiso 1 1 calc R . . C35 C 0.3482(2) -0.02732(19) 0.24795(11) 0.0473(5) Uani 1 1 d . . . H35 H 0.3705 -0.0836 0.2805 0.057 Uiso 1 1 calc R . . C36 C 0.40466(19) -0.02378(15) 0.19338(9) 0.0325(4) Uani 1 1 d . . . O3 O 0.49338(15) -0.10000(11) 0.18034(7) 0.0425(3) Uani 1 1 d . . . C37 C 0.5608(3) -0.1673(2) 0.23528(12) 0.0612(7) Uani 1 1 d . . . H37A H 0.6074 -0.1228 0.2739 0.092 Uiso 1 1 calc R . . H37B H 0.6253 -0.2122 0.2202 0.092 Uiso 1 1 calc R . . H37C H 0.4961 -0.2131 0.2494 0.092 Uiso 1 1 calc R . . Li1 Li 0.6859(3) 0.0057(2) -0.00827(15) 0.0295(6) Uani 1 1 d . . . Li2 Li 0.3809(3) -0.0043(2) -0.09787(15) 0.0306(7) Uani 1 1 d . . . Li3 Li 0.5375(3) 0.1513(3) -0.07828(17) 0.0353(7) Uani 1 1 d . . . O41 O 0.57774(15) 0.29984(11) -0.09972(8) 0.0452(4) Uani 1 1 d . . . C41 C 0.6726(4) 0.3358(2) -0.1340(2) 0.0927(12) Uani 1 1 d . . . H41A H 0.7419 0.2804 -0.1311 0.111 Uiso 1 1 calc R . . H41B H 0.6287 0.3485 -0.1828 0.111 Uiso 1 1 calc R . . C42 C 0.7305(4) 0.4299(3) -0.1042(3) 0.1314(18) Uani 1 1 d . . . H42A H 0.7431 0.4805 -0.1397 0.158 Uiso 1 1 calc R . . H42B H 0.8183 0.4149 -0.0726 0.158 Uiso 1 1 calc R . . C43 C 0.5343(2) 0.39257(18) -0.06961(13) 0.0519(6) Uani 1 1 d . . . H43A H 0.5250 0.3757 -0.0232 0.062 Uiso 1 1 calc R . . H43B H 0.4474 0.4177 -0.0979 0.062 Uiso 1 1 calc R . . C44 C 0.6385(3) 0.4765(2) -0.06618(18) 0.0845(10) Uani 1 1 d . . . H44A H 0.5983 0.5439 -0.0879 0.101 Uiso 1 1 calc R . . H44B H 0.6862 0.4917 -0.0182 0.101 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 As1 0.02765(10) 0.02201(9) 0.02725(10) -0.00462(7) 0.01111(7) -0.00055(7) N1 0.0242(7) 0.0241(7) 0.0312(8) -0.0062(6) 0.0106(6) -0.0039(6) C11 0.0289(9) 0.0248(9) 0.0275(9) 0.0007(7) 0.0054(7) -0.0027(7) C12 0.0372(11) 0.0334(10) 0.0386(11) -0.0094(8) 0.0088(9) -0.0051(8) C13 0.0476(13) 0.0394(12) 0.0500(13) -0.0156(10) 0.0023(10) -0.0099(10) C14 0.0352(11) 0.0448(13) 0.0615(14) -0.0096(11) 0.0018(10) -0.0164(10) C15 0.0300(10) 0.0429(12) 0.0521(13) -0.0008(10) 0.0099(9) -0.0078(9) C16 0.0296(9) 0.0291(9) 0.0346(10) 0.0001(8) 0.0085(8) -0.0053(8) O1 0.0314(7) 0.0363(8) 0.0469(8) -0.0098(6) 0.0224(6) -0.0085(6) C17 0.0460(13) 0.0503(14) 0.0623(14) -0.0100(11) 0.0365(12) -0.0100(10) N2 0.0258(7) 0.0236(7) 0.0258(7) -0.0031(6) 0.0072(6) 0.0013(6) C21 0.0254(8) 0.0268(9) 0.0325(9) 0.0056(7) 0.0141(7) -0.0011(7) C22 0.0312(10) 0.0262(9) 0.0494(12) 0.0039(8) 0.0159(9) 0.0017(7) C23 0.0380(11) 0.0322(11) 0.0699(15) 0.0158(10) 0.0227(11) 0.0089(9) C24 0.0336(11) 0.0556(15) 0.0545(14) 0.0298(11) 0.0171(10) 0.0151(10) C25 0.0301(10) 0.0632(15) 0.0333(10) 0.0128(10) 0.0100(8) 0.0033(9) C26 0.0255(9) 0.0407(11) 0.0308(9) 0.0042(8) 0.0114(8) 0.0015(8) O2 0.0313(7) 0.0483(9) 0.0355(7) -0.0149(6) -0.0002(6) 0.0040(6) C27 0.0557(16) 0.076(2) 0.0602(16) -0.0299(14) -0.0141(13) 0.0035(13) N3 0.0313(8) 0.0276(8) 0.0255(7) -0.0015(6) 0.0129(6) 0.0008(6) C31 0.0233(8) 0.0291(9) 0.0243(8) -0.0056(7) 0.0078(7) -0.0059(7) C32 0.0287(10) 0.0338(10) 0.0372(10) -0.0060(8) 0.0132(8) -0.0020(8) C33 0.0381(11) 0.0427(12) 0.0552(13) -0.0175(10) 0.0283(10) -0.0074(9) C34 0.0637(15) 0.0550(15) 0.0471(12) -0.0129(11) 0.0398(12) -0.0129(12) C35 0.0666(15) 0.0461(13) 0.0362(11) 0.0024(10) 0.0262(11) -0.0076(11) C36 0.0376(10) 0.0335(10) 0.0290(9) -0.0033(8) 0.0136(8) -0.0020(8) O3 0.0576(9) 0.0376(8) 0.0347(7) 0.0077(6) 0.0164(7) 0.0148(7) C37 0.0769(18) 0.0581(16) 0.0447(13) 0.0153(12) 0.0084(12) 0.0208(13) Li1 0.0312(16) 0.0265(15) 0.0338(16) -0.0032(12) 0.0135(13) -0.0026(12) Li2 0.0291(16) 0.0307(16) 0.0328(16) -0.0038(13) 0.0093(13) 0.0004(12) Li3 0.0380(18) 0.0358(18) 0.0360(17) -0.0018(14) 0.0164(14) -0.0026(14) O41 0.0557(9) 0.0364(8) 0.0502(9) -0.0011(6) 0.0257(8) -0.0108(7) C41 0.130(3) 0.0569(18) 0.129(3) -0.0111(18) 0.101(3) -0.0290(18) C42 0.104(3) 0.061(2) 0.264(6) -0.008(3) 0.111(4) -0.026(2) C43 0.0632(15) 0.0393(13) 0.0585(14) 0.0011(11) 0.0255(12) -0.0017(11) C44 0.104(3) 0.0447(16) 0.112(3) -0.0168(16) 0.040(2) -0.0275(16) _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 As1 N3 1.8626(15) . ? As1 N1 1.8652(14) . ? As1 N2 1.8869(14) . ? As1 Li1 2.733(3) 3_655 ? As1 Li2 2.800(3) 3_655 ? As1 Li3 2.841(3) . ? N1 C11 1.391(2) . ? N1 Li1 2.016(3) . ? N1 Li3 2.143(3) . ? N1 Li2 2.161(3) 3_655 ? C11 C12 1.399(2) . ? C11 C16 1.421(2) . ? C11 Li1 2.765(3) . ? C12 C13 1.391(3) . ? C13 C14 1.366(3) . ? C14 C15 1.395(3) . ? C15 C16 1.375(3) . ? C16 O1 1.394(2) . ? C16 Li1 2.769(3) . ? O1 C17 1.439(2) . ? O1 Li1 1.946(3) . ? N2 C21 1.391(2) . ? N2 Li2 2.054(3) . ? N2 Li1 2.109(3) 3_655 ? N2 Li3 2.147(3) . ? C21 C22 1.405(3) . ? C21 C26 1.418(3) . ? C22 C23 1.388(3) . ? C23 C24 1.370(3) . ? C24 C25 1.385(3) . ? C25 C26 1.381(3) . ? C26 O2 1.394(2) . ? O2 C27 1.426(2) . ? O2 Li2 1.918(3) . ? N3 C31 1.385(2) . ? N3 Li2 1.962(3) 3_655 ? N3 Li1 1.973(3) 3_655 ? N3 Li3 2.588(4) 3_655 ? C31 C32 1.404(3) . ? C31 C36 1.413(3) . ? C31 Li1 2.776(3) 3_655 ? C32 C33 1.391(3) . ? C33 C34 1.364(3) . ? C34 C35 1.390(3) . ? C35 C36 1.378(3) . ? C36 O3 1.397(2) . ? O3 C37 1.426(2) . ? O3 Li3 2.107(4) 3_655 ? Li1 N3 1.973(3) 3_655 ? Li1 N2 2.109(3) 3_655 ? Li1 Li2 2.421(4) 3_655 ? Li1 Li3 2.563(5) . ? Li1 As1 2.733(3) 3_655 ? Li1 C31 2.776(3) 3_655 ? Li1 Li2 3.230(4) . ? Li2 N3 1.962(3) 3_655 ? Li2 N1 2.161(3) 3_655 ? Li2 Li1 2.421(4) 3_655 ? Li2 Li3 2.499(4) . ? Li2 As1 2.800(3) 3_655 ? Li3 O41 1.973(4) . ? Li3 O3 2.107(4) 3_655 ? Li3 N3 2.588(4) 3_655 ? O41 C41 1.416(3) . ? O41 C43 1.433(3) . ? C41 C42 1.385(4) . ? C42 C44 1.492(5) . ? C43 C44 1.496(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 N3 As1 N1 94.00(6) . . ? N3 As1 N2 96.09(6) . . ? N1 As1 N2 92.48(6) . . ? N3 As1 Li1 46.22(8) . 3_655 ? N1 As1 Li1 100.29(8) . 3_655 ? N2 As1 Li1 50.34(8) . 3_655 ? N3 As1 Li2 44.33(8) . 3_655 ? N1 As1 Li2 50.46(8) . 3_655 ? N2 As1 Li2 103.39(8) . 3_655 ? Li1 As1 Li2 71.42(9) 3_655 3_655 ? N3 As1 Li3 115.83(8) . . ? N1 As1 Li3 48.97(8) . . ? N2 As1 Li3 49.08(8) . . ? Li1 As1 Li3 85.72(9) 3_655 . ? Li2 As1 Li3 87.60(9) 3_655 . ? C11 N1 As1 118.23(12) . . ? C11 N1 Li1 107.07(14) . . ? As1 N1 Li1 134.39(11) . . ? C11 N1 Li3 113.58(14) . . ? As1 N1 Li3 89.99(10) . . ? Li1 N1 Li3 76.03(13) . . ? C11 N1 Li2 111.00(14) . 3_655 ? As1 N1 Li2 87.81(10) . 3_655 ? Li1 N1 Li2 70.73(12) . 3_655 ? Li3 N1 Li2 130.24(14) . 3_655 ? N1 C11 C12 127.66(17) . . ? N1 C11 C16 117.19(15) . . ? C12 C11 C16 115.14(16) . . ? N1 C11 Li1 44.19(10) . . ? C12 C11 Li1 162.02(15) . . ? C16 C11 Li1 75.27(12) . . ? C13 C12 C11 121.9(2) . . ? C14 C13 C12 121.2(2) . . ? C13 C14 C15 119.12(19) . . ? C16 C15 C14 119.6(2) . . ? C15 C16 O1 123.29(17) . . ? C15 C16 C11 122.99(18) . . ? O1 C16 C11 113.73(15) . . ? C15 C16 Li1 158.22(16) . . ? O1 C16 Li1 41.07(9) . . ? C11 C16 Li1 74.97(12) . . ? C16 O1 C17 117.32(14) . . ? C16 O1 Li1 110.85(13) . . ? C17 O1 Li1 131.67(15) . . ? C21 N2 As1 118.19(11) . . ? C21 N2 Li2 109.65(14) . . ? As1 N2 Li2 132.05(11) . . ? C21 N2 Li1 114.44(14) . 3_655 ? As1 N2 Li1 86.13(10) . 3_655 ? Li2 N2 Li1 71.09(12) . 3_655 ? C21 N2 Li3 114.86(14) . . ? As1 N2 Li3 89.30(11) . . ? Li2 N2 Li3 72.98(13) . . ? Li1 N2 Li3 126.04(14) 3_655 . ? N2 C21 C22 127.70(17) . . ? N2 C21 C26 117.50(16) . . ? C22 C21 C26 114.80(17) . . ? C23 C22 C21 122.4(2) . . ? C24 C23 C22 120.7(2) . . ? C23 C24 C25 119.48(19) . . ? C26 C25 C24 119.8(2) . . ? C25 C26 O2 123.63(18) . . ? C25 C26 C21 122.86(19) . . ? O2 C26 C21 113.52(15) . . ? C26 O2 C27 118.40(16) . . ? C26 O2 Li2 116.00(14) . . ? C27 O2 Li2 125.60(17) . . ? C31 N3 As1 118.89(12) . . ? C31 N3 Li2 126.23(14) . 3_655 ? As1 N3 Li2 94.11(11) . 3_655 ? C31 N3 Li1 110.25(14) . 3_655 ? As1 N3 Li1 90.83(11) . 3_655 ? Li2 N3 Li1 110.33(14) 3_655 3_655 ? C31 N3 Li3 101.75(13) . 3_655 ? As1 N3 Li3 138.66(10) . 3_655 ? Li2 N3 Li3 64.95(12) 3_655 3_655 ? Li1 N3 Li3 66.82(12) 3_655 3_655 ? N3 C31 C32 126.92(17) . . ? N3 C31 C36 116.97(15) . . ? C32 C31 C36 116.04(16) . . ? N3 C31 Li1 41.84(10) . 3_655 ? C32 C31 Li1 109.10(13) . 3_655 ? C36 C31 Li1 116.22(13) . 3_655 ? C33 C32 C31 121.51(19) . . ? C34 C33 C32 120.7(2) . . ? C33 C34 C35 119.72(18) . . ? C36 C35 C34 119.9(2) . . ? C35 C36 O3 124.58(18) . . ? C35 C36 C31 122.07(18) . . ? O3 C36 C31 113.34(15) . . ? C36 O3 C37 118.07(16) . . ? C36 O3 Li3 116.70(15) . 3_655 ? C37 O3 Li3 120.46(16) . 3_655 ? O1 Li1 N3 119.60(16) . 3_655 ? O1 Li1 N1 82.67(13) . . ? N3 Li1 N1 114.80(16) 3_655 . ? O1 Li1 N2 145.17(17) . 3_655 ? N3 Li1 N2 86.10(13) 3_655 3_655 ? N1 Li1 N2 108.91(14) . 3_655 ? O1 Li1 Li2 118.90(16) . 3_655 ? N3 Li1 Li2 118.67(16) 3_655 3_655 ? N1 Li1 Li2 57.43(11) . 3_655 ? N2 Li1 Li2 53.40(11) 3_655 3_655 ? O1 Li1 Li3 82.72(13) . . ? N3 Li1 Li3 68.14(13) 3_655 . ? N1 Li1 Li3 54.22(11) . . ? N2 Li1 Li3 131.08(16) 3_655 . ? Li2 Li1 Li3 103.11(15) 3_655 . ? O1 Li1 As1 150.06(14) . 3_655 ? N3 Li1 As1 42.95(7) 3_655 3_655 ? N1 Li1 As1 125.14(13) . 3_655 ? N2 Li1 As1 43.54(7) 3_655 3_655 ? Li2 Li1 As1 88.46(12) 3_655 3_655 ? Li3 Li1 As1 103.89(13) . 3_655 ? O1 Li1 C11 56.91(9) . . ? N3 Li1 C11 136.04(15) 3_655 . ? N1 Li1 C11 28.74(7) . . ? N2 Li1 C11 121.54(13) 3_655 . ? Li2 Li1 C11 69.23(11) 3_655 . ? Li3 Li1 C11 68.02(11) . . ? As1 Li1 C11 152.71(12) 3_655 . ? O1 Li1 C16 28.08(7) . . ? N3 Li1 C16 138.38(15) 3_655 . ? N1 Li1 C16 57.66(9) . . ? N2 Li1 C16 135.46(14) 3_655 . ? Li2 Li1 C16 92.40(12) 3_655 . ? Li3 Li1 C16 78.84(12) . . ? As1 Li1 C16 176.88(13) 3_655 . ? C11 Li1 C16 29.75(6) . . ? O1 Li1 C31 94.26(12) . 3_655 ? N3 Li1 C31 27.91(7) 3_655 3_655 ? N1 Li1 C31 126.98(15) . 3_655 ? N2 Li1 C31 103.16(12) 3_655 3_655 ? Li2 Li1 C31 146.18(15) 3_655 3_655 ? Li3 Li1 C31 72.84(11) . 3_655 ? As1 Li1 C31 61.26(7) 3_655 3_655 ? C11 Li1 C31 133.27(13) . 3_655 ? C16 Li1 C31 118.68(12) . 3_655 ? O1 Li1 Li2 129.01(15) . . ? N3 Li1 Li2 34.72(9) 3_655 . ? N1 Li1 Li2 82.09(12) . . ? N2 Li1 Li2 85.66(11) 3_655 . ? Li2 Li1 Li2 91.98(13) 3_655 . ? Li3 Li1 Li2 49.49(11) . . ? As1 Li1 Li2 55.26(8) 3_655 . ? C11 Li1 Li2 108.25(11) . . ? C16 Li1 Li2 127.68(12) . . ? C31 Li1 Li2 59.28(9) 3_655 . ? O2 Li2 N3 148.88(18) . 3_655 ? O2 Li2 N2 82.36(13) . . ? N3 Li2 N2 116.37(16) 3_655 . ? O2 Li2 N1 117.76(16) . 3_655 ? N3 Li2 N1 82.64(13) 3_655 3_655 ? N2 Li2 N1 105.53(14) . 3_655 ? O2 Li2 Li1 95.83(15) . 3_655 ? N3 Li2 Li1 115.21(16) 3_655 3_655 ? N2 Li2 Li1 55.50(11) . 3_655 ? N1 Li2 Li1 51.83(11) 3_655 3_655 ? O2 Li2 Li3 108.17(16) . . ? N3 Li2 Li3 69.73(13) 3_655 . ? N2 Li2 Li3 55.21(11) . . ? N1 Li2 Li3 127.17(16) 3_655 . ? Li1 Li2 Li3 100.84(15) 3_655 . ? O2 Li2 As1 147.01(16) . 3_655 ? N3 Li2 As1 41.56(7) 3_655 3_655 ? N2 Li2 As1 123.99(14) . 3_655 ? N1 Li2 As1 41.73(7) 3_655 3_655 ? Li1 Li2 As1 86.21(12) 3_655 3_655 ? Li3 Li2 As1 103.71(13) . 3_655 ? O2 Li2 Li1 159.37(16) . . ? N3 Li2 Li1 34.95(9) 3_655 . ? N2 Li2 Li1 83.21(11) . . ? N1 Li2 Li1 80.38(11) 3_655 . ? Li1 Li2 Li1 88.02(13) 3_655 . ? Li3 Li2 Li1 51.24(11) . . ? As1 Li2 Li1 53.33(8) 3_655 . ? O41 Li3 O3 93.28(14) . 3_655 ? O41 Li3 N1 104.29(16) . . ? O3 Li3 N1 154.00(19) 3_655 . ? O41 Li3 N2 115.80(17) . . ? O3 Li3 N2 111.25(16) 3_655 . ? N1 Li3 N2 78.37(12) . . ? O41 Li3 Li2 149.42(19) . . ? O3 Li3 Li2 71.28(13) 3_655 . ? N1 Li3 Li2 100.03(15) . . ? N2 Li3 Li2 51.81(11) . . ? O41 Li3 Li1 130.95(18) . . ? O3 Li3 Li1 104.25(15) 3_655 . ? N1 Li3 Li1 49.75(10) . . ? N2 Li3 Li1 99.96(14) . . ? Li2 Li3 Li1 79.27(14) . . ? O41 Li3 N3 150.76(16) . 3_655 ? O3 Li3 N3 66.20(10) 3_655 3_655 ? N1 Li3 N3 90.04(13) . 3_655 ? N2 Li3 N3 91.77(13) . 3_655 ? Li2 Li3 N3 45.32(10) . 3_655 ? Li1 Li3 N3 45.05(9) . 3_655 ? O41 Li3 As1 101.88(13) . . ? O3 Li3 As1 152.74(16) 3_655 . ? N1 Li3 As1 41.04(7) . . ? N2 Li3 As1 41.62(7) . . ? Li2 Li3 As1 84.57(11) . . ? Li1 Li3 As1 82.76(11) . . ? N3 Li3 As1 105.51(11) 3_655 . ? C41 O41 C43 106.69(17) . . ? C41 O41 Li3 128.26(18) . . ? C43 O41 Li3 123.84(15) . . ? C42 C41 O41 109.6(3) . . ? C41 C42 C44 106.8(3) . . ? O41 C43 C44 106.3(2) . . ? C42 C44 C43 104.9(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.462 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.050 #===END data_asbenm _database_code_CSD 153208 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 As Li3 N3 O2' _chemical_formula_weight 555.36 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.238(3) _cell_length_b 15.458(4) _cell_length_c 17.674(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.938(5) _cell_angle_gamma 90.00 _cell_volume 2796.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? 0.60 _exptl_crystal_size_mid ? 0.40 _exptl_crystal_size_min ? 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? 0.47 _exptl_absorpt_correction_T_max ? 0.78 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17608 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6405 _reflns_number_gt 5352 _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 XP _computing_publication_material XCIF _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^)+(0.0675P)^2^+1.7484P] 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 6405 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 As1 As 0.80790(2) 0.469772(16) 0.059432(15) 0.02786(10) Uani 1 1 d . . . N1 N 0.8334(2) 0.42180(14) -0.03673(12) 0.0289(4) Uani 1 1 d . . . C11 C 0.7118(2) 0.38104(17) -0.06523(16) 0.0328(5) Uani 1 1 d . . . H11A H 0.6992 0.3980 -0.1189 0.039 Uiso 1 1 calc R . . H11B H 0.6380 0.4056 -0.0368 0.039 Uiso 1 1 calc R . . C12 C 0.7030(2) 0.28291(17) -0.06061(14) 0.0296(5) Uani 1 1 d . . . C13 C 0.5855(3) 0.24392(18) -0.04154(17) 0.0362(6) Uani 1 1 d . . . H13 H 0.5124 0.2793 -0.0304 0.043 Uiso 1 1 calc R . . C14 C 0.5722(3) 0.1543(2) -0.03832(19) 0.0479(7) Uani 1 1 d . . . H14 H 0.4909 0.1292 -0.0252 0.058 Uiso 1 1 calc R . . C15 C 0.6763(4) 0.1026(2) -0.0540(2) 0.0531(9) Uani 1 1 d . . . H15 H 0.6678 0.0415 -0.0516 0.064 Uiso 1 1 calc R . . C16 C 0.7946(4) 0.1395(2) -0.0736(2) 0.0513(8) Uani 1 1 d . . . H16 H 0.8669 0.1034 -0.0846 0.062 Uiso 1 1 calc R . . C17 C 0.8080(3) 0.2288(2) -0.07721(17) 0.0398(6) Uani 1 1 d . . . H17 H 0.8893 0.2533 -0.0911 0.048 Uiso 1 1 calc R . . N2 N 0.9648(2) 0.43376(14) 0.10668(12) 0.0296(4) Uani 1 1 d . . . C21 C 0.9403(3) 0.39684(17) 0.18174(15) 0.0320(5) Uani 1 1 d . . . H21A H 0.8557 0.4194 0.1996 0.038 Uiso 1 1 calc R . . H21B H 1.0091 0.4179 0.2172 0.038 Uiso 1 1 calc R . . C22 C 0.9367(2) 0.29843(17) 0.18600(14) 0.0304(5) Uani 1 1 d . . . C23 C 0.8734(3) 0.24882(19) 0.13036(16) 0.0384(6) Uani 1 1 d . . . H23 H 0.8337 0.2769 0.0881 0.046 Uiso 1 1 calc R . . C24 C 0.8676(3) 0.1597(2) 0.13580(19) 0.0482(7) Uani 1 1 d . . . H24 H 0.8240 0.1272 0.0974 0.058 Uiso 1 1 calc R . . C25 C 0.9249(3) 0.1176(2) 0.1970(2) 0.0507(8) Uani 1 1 d . . . H25 H 0.9212 0.0564 0.2007 0.061 Uiso 1 1 calc R . . C26 C 0.9874(3) 0.1654(2) 0.25246(19) 0.0475(7) Uani 1 1 d . . . H26 H 1.0268 0.1369 0.2946 0.057 Uiso 1 1 calc R . . C27 C 0.9934(3) 0.2546(2) 0.24721(16) 0.0382(6) Uani 1 1 d . . . H27 H 1.0368 0.2866 0.2860 0.046 Uiso 1 1 calc R . . N3 N 0.8507(2) 0.58597(13) 0.03909(12) 0.0281(4) Uani 1 1 d . . . C31 C 0.7473(3) 0.64271(18) 0.0665(2) 0.0430(7) Uani 1 1 d . . . H31A H 0.7303 0.6289 0.1202 0.052 Uiso 1 1 calc R . . H31B H 0.6660 0.6315 0.0370 0.052 Uiso 1 1 calc R . . C32 C 0.7822(2) 0.73736(18) 0.05995(16) 0.0342(6) Uani 1 1 d . . . C33 C 0.8233(3) 0.7731(2) -0.00801(18) 0.0433(7) Uani 1 1 d . . . H33 H 0.8299 0.7374 -0.0515 0.052 Uiso 1 1 calc R . . C34 C 0.8549(3) 0.8606(2) -0.0131(2) 0.0535(8) Uani 1 1 d . . . H34 H 0.8844 0.8839 -0.0596 0.064 Uiso 1 1 calc R . . C35 C 0.8434(4) 0.9136(2) 0.0496(3) 0.0582(9) Uani 1 1 d . . . H35 H 0.8640 0.9734 0.0463 0.070 Uiso 1 1 calc R . . C36 C 0.8019(3) 0.8791(2) 0.1165(2) 0.0533(8) Uani 1 1 d . . . H36 H 0.7931 0.9154 0.1595 0.064 Uiso 1 1 calc R . . C37 C 0.7727(3) 0.7923(2) 0.12192(19) 0.0434(7) Uani 1 1 d . . . H37 H 0.7455 0.7695 0.1690 0.052 Uiso 1 1 calc R . . Li1 Li 0.8404(4) 0.5500(3) -0.0732(2) 0.0276(8) Uani 1 1 d . . . Li2 Li 0.9912(4) 0.3636(3) 0.0113(3) 0.0343(9) Uani 1 1 d . . . Li3 Li 1.0101(4) 0.5655(3) 0.1092(3) 0.0331(9) Uani 1 1 d . . . O41 O 0.69741(18) 0.58462(15) -0.14227(12) 0.0419(5) Uani 1 1 d . . . C42 C 0.5613(3) 0.5743(3) -0.1221(2) 0.0533(8) Uani 1 1 d . . . H42A H 0.5506 0.5817 -0.0669 0.064 Uiso 1 1 calc R . . H42B H 0.5291 0.5162 -0.1367 0.064 Uiso 1 1 calc R . . C43 C 0.4886(3) 0.6427(3) -0.1644(2) 0.0653(11) Uani 1 1 d . . . H43A H 0.4883 0.6978 -0.1359 0.078 Uiso 1 1 calc R . . H43B H 0.3973 0.6248 -0.1752 0.078 Uiso 1 1 calc R . . C44 C 0.5645(3) 0.6510(3) -0.2362(2) 0.0551(9) Uani 1 1 d . . . H44A H 0.5533 0.7091 -0.2589 0.066 Uiso 1 1 calc R . . H44B H 0.5374 0.6066 -0.2736 0.066 Uiso 1 1 calc R . . C45 C 0.7034(3) 0.6369(2) -0.20958(18) 0.0457(7) Uani 1 1 d . . . H45A H 0.7538 0.6068 -0.2490 0.055 Uiso 1 1 calc R . . H45B H 0.7462 0.6929 -0.1982 0.055 Uiso 1 1 calc R . . O51 O 1.0286(2) 0.61475(15) 0.21083(12) 0.0452(5) Uani 1 1 d . . . C52 C 0.9191(3) 0.6109(3) 0.26165(19) 0.0526(8) Uani 1 1 d . . . H52A H 0.8493 0.5733 0.2405 0.063 Uiso 1 1 calc R . . H52B H 0.8827 0.6693 0.2700 0.063 Uiso 1 1 calc R . . C53 C 0.9724(4) 0.5739(3) 0.3346(2) 0.0669(11) Uani 1 1 d . . . H53A H 0.9728 0.5099 0.3337 0.080 Uiso 1 1 calc R . . H53B H 0.9219 0.5941 0.3786 0.080 Uiso 1 1 calc R . . C54 C 1.1114(5) 0.6106(3) 0.3362(2) 0.0706(12) Uani 1 1 d . . . H54A H 1.1130 0.6706 0.3559 0.085 Uiso 1 1 calc R . . H54B H 1.1709 0.5743 0.3675 0.085 Uiso 1 1 calc R . . C55 C 1.1479(3) 0.6078(2) 0.2534(2) 0.0546(8) Uani 1 1 d . . . H55A H 1.2070 0.6563 0.2412 0.066 Uiso 1 1 calc R . . H55B H 1.1926 0.5527 0.2417 0.066 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 As1 0.02764(14) 0.02515(14) 0.03087(15) 0.00227(10) 0.00342(9) 0.00017(9) N1 0.0295(10) 0.0251(10) 0.0321(11) -0.0018(9) -0.0002(8) -0.0036(8) C11 0.0302(12) 0.0263(13) 0.0418(15) 0.0011(11) -0.0049(10) 0.0009(9) C12 0.0353(12) 0.0260(12) 0.0271(12) -0.0036(10) -0.0059(10) 0.0011(10) C13 0.0348(13) 0.0304(14) 0.0431(15) 0.0031(11) -0.0042(11) -0.0019(10) C14 0.0507(17) 0.0377(16) 0.0550(19) 0.0090(14) -0.0106(14) -0.0122(13) C15 0.077(2) 0.0239(15) 0.057(2) 0.0007(13) -0.0218(17) -0.0020(14) C16 0.066(2) 0.0355(17) 0.0525(19) -0.0105(14) -0.0122(16) 0.0180(15) C17 0.0403(14) 0.0375(15) 0.0415(15) -0.0076(12) -0.0010(12) 0.0058(12) N2 0.0313(10) 0.0283(11) 0.0293(11) 0.0055(9) 0.0024(8) 0.0013(8) C21 0.0379(13) 0.0286(13) 0.0296(13) 0.0019(10) 0.0010(10) 0.0002(10) C22 0.0317(12) 0.0326(13) 0.0269(12) 0.0041(10) 0.0021(9) -0.0008(10) C23 0.0469(15) 0.0366(15) 0.0317(14) 0.0053(11) -0.0032(12) -0.0043(12) C24 0.064(2) 0.0362(16) 0.0439(17) -0.0011(13) -0.0018(14) -0.0106(14) C25 0.0552(18) 0.0319(16) 0.065(2) 0.0113(15) 0.0021(16) -0.0022(13) C26 0.0462(16) 0.0435(17) 0.0526(19) 0.0219(15) -0.0053(14) -0.0006(13) C27 0.0393(14) 0.0413(16) 0.0337(14) 0.0090(12) -0.0022(11) -0.0045(11) N3 0.0287(10) 0.0217(10) 0.0341(11) -0.0001(8) 0.0032(8) 0.0042(8) C31 0.0399(15) 0.0273(14) 0.062(2) -0.0064(13) 0.0142(13) 0.0018(11) C32 0.0282(12) 0.0301(13) 0.0442(15) -0.0055(11) -0.0008(11) 0.0078(10) C33 0.0481(16) 0.0376(16) 0.0442(16) 0.0007(13) -0.0026(13) 0.0109(13) C34 0.0537(19) 0.0437(19) 0.063(2) 0.0187(16) 0.0000(16) 0.0090(14) C35 0.0558(19) 0.0258(15) 0.093(3) -0.0008(17) -0.0077(18) 0.0046(13) C36 0.0539(19) 0.0374(17) 0.068(2) -0.0190(16) -0.0076(16) 0.0045(14) C37 0.0429(15) 0.0414(16) 0.0459(17) -0.0074(13) 0.0004(13) 0.0064(12) Li1 0.0282(19) 0.0197(19) 0.035(2) 0.0045(16) -0.0065(16) -0.0003(14) Li2 0.034(2) 0.026(2) 0.042(3) -0.0009(19) 0.0026(18) 0.0014(17) Li3 0.035(2) 0.029(2) 0.035(2) -0.0041(18) 0.0025(18) -0.0008(17) O41 0.0348(10) 0.0513(13) 0.0395(11) 0.0126(9) -0.0016(8) 0.0039(9) C42 0.0402(16) 0.062(2) 0.058(2) 0.0210(17) 0.0077(14) 0.0069(15) C43 0.0461(18) 0.071(3) 0.079(3) 0.038(2) 0.0114(17) 0.0092(17) C44 0.0489(18) 0.061(2) 0.056(2) 0.0207(17) -0.0051(15) -0.0002(15) C45 0.0431(15) 0.0511(19) 0.0428(17) 0.0137(14) 0.0032(13) 0.0037(13) O51 0.0451(11) 0.0543(14) 0.0362(11) -0.0104(10) 0.0010(9) -0.0005(10) C52 0.0537(18) 0.061(2) 0.0432(18) -0.0134(16) 0.0074(14) -0.0011(15) C53 0.092(3) 0.069(3) 0.0398(18) -0.0022(18) 0.0023(18) -0.014(2) C54 0.097(3) 0.061(3) 0.054(2) 0.0020(18) -0.024(2) -0.008(2) C55 0.0524(18) 0.0458(19) 0.065(2) -0.0096(16) -0.0108(16) 0.0010(14) _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 As1 N1 1.876(2) . ? As1 N2 1.882(2) . ? As1 N3 1.885(2) . ? As1 Li2 2.644(4) . ? As1 Li1 2.677(4) . ? As1 Li3 2.681(4) . ? N1 C11 1.477(3) . ? N1 Li2 2.024(5) . ? N1 Li3 2.078(5) 3_765 ? N1 Li1 2.086(5) . ? C11 C12 1.522(4) . ? C12 C13 1.392(4) . ? C12 C17 1.398(4) . ? C13 C14 1.393(4) . ? C14 C15 1.364(5) . ? C15 C16 1.388(5) . ? C16 C17 1.388(5) . ? N2 C21 1.469(3) . ? N2 Li2 2.026(5) . ? N2 Li3 2.088(5) . ? N2 Li1 2.105(5) 3_765 ? C21 C22 1.524(4) . ? C22 C27 1.394(4) . ? C22 C23 1.398(4) . ? C23 C24 1.382(4) . ? C24 C25 1.384(5) . ? C25 C26 1.376(5) . ? C26 C27 1.384(4) . ? N3 C31 1.463(3) . ? N3 Li2 2.018(5) 3_765 ? N3 Li3 2.058(5) . ? N3 Li1 2.061(5) . ? C31 C32 1.511(4) . ? C32 C37 1.391(4) . ? C32 C33 1.394(4) . ? C33 C34 1.394(5) . ? C34 C35 1.384(5) . ? C35 C36 1.371(6) . ? C36 C37 1.379(5) . ? Li1 O41 1.965(4) . ? Li1 N2 2.105(5) 3_765 ? Li1 Li2 2.427(6) 3_765 ? Li1 Li3 2.443(6) 3_765 ? Li2 N3 2.018(5) 3_765 ? Li2 Li3 2.397(7) 3_765 ? Li2 Li1 2.427(6) 3_765 ? Li3 O51 1.957(5) . ? Li3 N1 2.078(5) 3_765 ? Li3 Li2 2.397(7) 3_765 ? Li3 Li1 2.443(6) 3_765 ? O41 C45 1.440(3) . ? O41 C42 1.453(4) . ? C42 C43 1.487(5) . ? C43 C44 1.504(5) . ? C44 C45 1.506(4) . ? O51 C55 1.428(4) . ? O51 C52 1.449(4) . ? C52 C53 1.505(5) . ? C53 C54 1.532(6) . ? C54 C55 1.517(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 As1 N2 98.90(9) . . ? N1 As1 N3 99.65(9) . . ? N2 As1 N3 99.61(9) . . ? N1 As1 Li2 49.72(12) . . ? N2 As1 Li2 49.77(13) . . ? N3 As1 Li2 111.21(12) . . ? N1 As1 Li1 50.89(11) . . ? N2 As1 Li1 114.08(11) . . ? N3 As1 Li1 50.12(11) . . ? Li2 As1 Li1 84.68(14) . . ? N1 As1 Li3 113.41(11) . . ? N2 As1 Li3 50.87(12) . . ? N3 As1 Li3 49.92(12) . . ? Li2 As1 Li3 84.25(14) . . ? Li1 As1 Li3 85.71(13) . . ? C11 N1 As1 110.41(16) . . ? C11 N1 Li2 128.0(2) . . ? As1 N1 Li2 85.26(16) . . ? C11 N1 Li3 119.0(2) . 3_765 ? As1 N1 Li3 129.89(16) . 3_765 ? Li2 N1 Li3 71.49(19) . 3_765 ? C11 N1 Li1 109.48(19) . . ? As1 N1 Li1 84.84(15) . . ? Li2 N1 Li1 121.39(19) . . ? Li3 N1 Li1 71.86(19) 3_765 . ? N1 C11 C12 117.2(2) . . ? C13 C12 C17 117.6(3) . . ? C13 C12 C11 119.8(2) . . ? C17 C12 C11 122.6(2) . . ? C12 C13 C14 121.7(3) . . ? C15 C14 C13 119.8(3) . . ? C14 C15 C16 119.9(3) . . ? C17 C16 C15 120.5(3) . . ? C16 C17 C12 120.5(3) . . ? C21 N2 As1 111.01(16) . . ? C21 N2 Li2 124.7(2) . . ? As1 N2 Li2 85.06(16) . . ? C21 N2 Li3 113.6(2) . . ? As1 N2 Li3 84.78(15) . . ? Li2 N2 Li3 120.5(2) . . ? C21 N2 Li1 118.5(2) . 3_765 ? As1 N2 Li1 130.21(16) . 3_765 ? Li2 N2 Li1 71.93(19) . 3_765 ? Li3 N2 Li1 71.26(18) . 3_765 ? N2 C21 C22 115.9(2) . . ? C27 C22 C23 117.5(3) . . ? C27 C22 C21 120.9(2) . . ? C23 C22 C21 121.6(2) . . ? C24 C23 C22 121.2(3) . . ? C23 C24 C25 120.3(3) . . ? C26 C25 C24 119.4(3) . . ? C25 C26 C27 120.5(3) . . ? C26 C27 C22 121.2(3) . . ? C31 N3 As1 109.65(17) . . ? C31 N3 Li2 120.3(2) . 3_765 ? As1 N3 Li2 130.05(16) . 3_765 ? C31 N3 Li3 117.6(2) . . ? As1 N3 Li3 85.58(15) . . ? Li2 N3 Li3 72.0(2) 3_765 . ? C31 N3 Li1 117.0(2) . . ? As1 N3 Li1 85.32(14) . . ? Li2 N3 Li1 73.01(19) 3_765 . ? Li3 N3 Li1 124.47(19) . . ? N3 C31 C32 112.4(2) . . ? C37 C32 C33 117.6(3) . . ? C37 C32 C31 120.7(3) . . ? C33 C32 C31 121.7(3) . . ? C32 C33 C34 121.0(3) . . ? C35 C34 C33 119.9(3) . . ? C36 C35 C34 119.5(3) . . ? C35 C36 C37 120.6(3) . . ? C36 C37 C32 121.4(3) . . ? O41 Li1 N3 123.4(2) . . ? O41 Li1 N1 114.9(2) . . ? N3 Li1 N1 87.73(18) . . ? O41 Li1 N2 119.5(2) . 3_765 ? N3 Li1 N2 101.83(19) . 3_765 ? N1 Li1 N2 103.75(19) . 3_765 ? O41 Li1 Li2 130.3(2) . 3_765 ? N3 Li1 Li2 52.67(16) . 3_765 ? N1 Li1 Li2 114.3(2) . 3_765 ? N2 Li1 Li2 52.53(16) 3_765 3_765 ? O41 Li1 Li3 120.0(2) . 3_765 ? N3 Li1 Li3 115.2(2) . 3_765 ? N1 Li1 Li3 53.91(16) . 3_765 ? N2 Li1 Li3 54.06(16) 3_765 3_765 ? Li2 Li1 Li3 94.4(2) 3_765 3_765 ? O41 Li1 As1 124.6(2) . . ? N3 Li1 As1 44.56(10) . . ? N1 Li1 As1 44.27(10) . . ? N2 Li1 As1 115.69(17) 3_765 . ? Li2 Li1 As1 87.62(17) 3_765 . ? Li3 Li1 As1 88.69(17) 3_765 . ? N3 Li2 N1 106.5(2) 3_765 . ? N3 Li2 N2 106.2(2) 3_765 . ? N1 Li2 N2 89.69(19) . . ? N3 Li2 Li3 54.76(17) 3_765 3_765 ? N1 Li2 Li3 55.29(17) . 3_765 ? N2 Li2 Li3 119.7(2) . 3_765 ? N3 Li2 Li1 54.33(16) 3_765 3_765 ? N1 Li2 Li1 120.0(2) . 3_765 ? N2 Li2 Li1 55.55(17) . 3_765 ? Li3 Li2 Li1 98.2(2) 3_765 3_765 ? N3 Li2 As1 118.7(2) 3_765 . ? N1 Li2 As1 45.01(11) . . ? N2 Li2 As1 45.18(11) . . ? Li3 Li2 As1 90.47(18) 3_765 . ? Li1 Li2 As1 90.94(18) 3_765 . ? O51 Li3 N3 123.8(2) . . ? O51 Li3 N1 117.7(2) . 3_765 ? N3 Li3 N1 103.1(2) . 3_765 ? O51 Li3 N2 114.7(2) . . ? N3 Li3 N2 87.90(19) . . ? N1 Li3 N2 104.6(2) 3_765 . ? O51 Li3 Li2 129.6(3) . 3_765 ? N3 Li3 Li2 53.21(16) . 3_765 ? N1 Li3 Li2 53.22(16) 3_765 3_765 ? N2 Li3 Li2 115.4(2) . 3_765 ? O51 Li3 Li1 118.2(2) . 3_765 ? N3 Li3 Li1 116.7(2) . 3_765 ? N1 Li3 Li1 54.23(16) 3_765 3_765 ? N2 Li3 Li1 54.68(15) . 3_765 ? Li2 Li3 Li1 95.6(2) 3_765 3_765 ? O51 Li3 As1 125.3(2) . . ? N3 Li3 As1 44.50(11) . . ? N1 Li3 As1 116.7(2) 3_765 . ? N2 Li3 As1 44.36(11) . . ? Li2 Li3 As1 88.15(18) 3_765 . ? Li1 Li3 As1 89.70(17) 3_765 . ? C45 O41 C42 108.6(2) . . ? C45 O41 Li1 128.7(2) . . ? C42 O41 Li1 121.7(2) . . ? O41 C42 C43 105.8(3) . . ? C42 C43 C44 102.9(3) . . ? C43 C44 C45 102.9(3) . . ? O41 C45 C44 106.7(2) . . ? C55 O51 C52 109.5(3) . . ? C55 O51 Li3 121.5(2) . . ? C52 O51 Li3 119.2(2) . . ? O51 C52 C53 105.9(3) . . ? C52 C53 C54 101.5(3) . . ? C55 C54 C53 102.4(3) . . ? O51 C55 C54 106.5(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.357 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.071 #===END data_/tintin3/people/jeffery/chris/asli/asli _database_code_CSD 153209 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H38 As Li3 N3 O5' _chemical_formula_weight 604.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'As' 'As' 0.0499 2.0058 '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 10.500(2) _cell_length_b 17.511(3) _cell_length_c 16.330(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.62(2) _cell_angle_gamma 90.00 _cell_volume 2929.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method ? _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min ? 0.62 _exptl_absorpt_correction_T_max ? 0.84 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18250 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6617 _reflns_number_observed 4139 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART area detector _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material XCIF _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6617 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_obs 0.0458 _refine_ls_wR_factor_all 0.1018 _refine_ls_wR_factor_obs 0.0920 _refine_ls_goodness_of_fit_all 1.112 _refine_ls_goodness_of_fit_obs 1.292 _refine_ls_restrained_S_all 1.112 _refine_ls_restrained_S_obs 1.292 _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 As1 As 0.90804(3) 0.87179(2) 0.44504(2) 0.02515(10) Uani 1 d . . Li1 Li 0.8192(5) 1.0000(3) 0.5133(3) 0.0305(13) Uani 1 d . . N1 N 0.9194(2) 1.09794(14) 0.5494(2) 0.0254(6) Uani 1 d . . Li2 Li 1.0974(5) 0.9240(3) 0.5870(3) 0.0323(13) Uani 1 d . . N2 N 0.9102(2) 0.90320(15) 0.55367(15) 0.0272(6) Uani 1 d . . Li3 Li 1.0129(6) 0.9719(3) 0.3437(3) 0.0345(14) Uani 1 d . . N3 N 1.1581(2) 1.03591(14) 0.60678(15) 0.0246(6) Uani 1 d . . C11 C 0.8280(3) 1.1534(2) 0.5564(2) 0.0274(8) Uani 1 d . . C12 C 0.8403(3) 1.2332(2) 0.5496(2) 0.0346(8) Uani 1 d . . H12A H 0.9188(3) 1.2540(2) 0.5391(2) 0.042 Uiso 1 calc R . C13 C 0.7395(4) 1.2820(2) 0.5581(2) 0.0456(10) Uani 1 d . . H13A H 0.7503(4) 1.3355(2) 0.5528(2) 0.055 Uiso 1 calc R . C14 C 0.6252(4) 1.2548(2) 0.5741(2) 0.0516(11) Uani 1 d . . H14A H 0.5586(4) 1.2892(2) 0.5812(2) 0.062 Uiso 1 calc R . C15 C 0.6067(3) 1.1761(2) 0.5799(2) 0.0427(10) Uani 1 d . . H15A H 0.5274(3) 1.1565(2) 0.5902(2) 0.051 Uiso 1 calc R . C16 C 0.7056(3) 1.1277(2) 0.5703(2) 0.0308(8) Uani 1 d . . C17 C 0.5878(4) 1.0172(2) 0.6043(2) 0.0532(11) Uani 1 d . . H17A H 0.5937(13) 0.9614(2) 0.6058(14) 0.080 Uiso 1 calc R . H17B H 0.5051(4) 1.0326(11) 0.5674(9) 0.080 Uiso 1 calc R . H17C H 0.5918(14) 1.0367(11) 0.6610(6) 0.080 Uiso 1 calc R . O17 O 0.6950(2) 1.04805(13) 0.57260(14) 0.0358(6) Uani 1 d . . C21 C 0.8352(3) 0.8667(2) 0.6016(2) 0.0235(7) Uani 1 d . . C22 C 0.7244(3) 0.8213(2) 0.5734(2) 0.0277(8) Uani 1 d . . H22A H 0.6952(3) 0.8124(2) 0.5149(2) 0.033 Uiso 1 calc R . C23 C 0.6559(3) 0.7889(2) 0.6286(2) 0.0359(9) Uani 1 d . . H23A H 0.5817(3) 0.7579(2) 0.6077(2) 0.043 Uiso 1 calc R . C24 C 0.6956(3) 0.8017(2) 0.7140(2) 0.0372(9) Uani 1 d . . H24A H 0.7109(3) 0.7512(2) 0.7416(2) 0.045 Uiso 1 calc R . H24B H 0.6215(3) 0.8254(2) 0.7329(2) 0.045 Uiso 1 calc R . C25 C 0.8052(3) 0.8462(2) 0.7445(2) 0.0331(8) Uani 1 d . . H25A H 0.8328(3) 0.8553(2) 0.8030(2) 0.040 Uiso 1 calc R . C26 C 0.8734(3) 0.8770(2) 0.6899(2) 0.0245(7) Uani 1 d . . C27 C 1.0611(4) 0.9093(2) 0.7973(2) 0.0424(10) Uani 1 d . . H27A H 1.0130(9) 0.9258(11) 0.8392(2) 0.064 Uiso 1 calc R . H27B H 1.1429(10) 0.9382(10) 0.8047(5) 0.064 Uiso 1 calc R . H27C H 1.0807(18) 0.8547(3) 0.8042(5) 0.064 Uiso 1 calc R . O27 O 0.9836(2) 0.92301(13) 0.71490(12) 0.0327(6) Uani 1 d . . C31 C 1.2699(3) 1.0381(2) 0.6705(2) 0.0238(7) Uani 1 d . . C32 C 1.3316(3) 1.1026(2) 0.7119(2) 0.0308(8) Uani 1 d . . H32A H 1.2958(3) 1.1516(2) 0.6956(2) 0.037 Uiso 1 calc R . C33 C 1.4430(3) 1.0979(2) 0.7757(2) 0.0354(9) Uani 1 d . . H33A H 1.4820(3) 1.1434(2) 0.8014(2) 0.042 Uiso 1 calc R . C34 C 1.4976(3) 1.0285(2) 0.8022(2) 0.0370(9) Uani 1 d . . H34A H 1.5730(3) 1.0258(2) 0.8466(2) 0.044 Uiso 1 calc R . C35 C 1.4407(3) 0.9619(2) 0.7631(2) 0.0343(9) Uani 1 d . . H35A H 1.4776(3) 0.9134(2) 0.7803(2) 0.041 Uiso 1 calc R . C36 C 1.3311(3) 0.9671(2) 0.6998(2) 0.0264(8) Uani 1 d . . C37 C 1.3351(4) 0.8323(2) 0.6698(2) 0.0466(10) Uani 1 d . . H37A H 1.2891(12) 0.7947(4) 0.6296(9) 0.070 Uiso 1 calc R . H37B H 1.3374(19) 0.8146(6) 0.7271(5) 0.070 Uiso 1 calc R . H37C H 1.4245(7) 0.8384(3) 0.6620(13) 0.070 Uiso 1 calc R . O37 O 1.2688(2) 0.90360(12) 0.65636(13) 0.0317(5) Uani 1 d . . O51 O 1.0256(2) 0.91178(14) 0.24491(14) 0.0398(6) Uani 1 d . . C52 C 0.9762(4) 0.8344(2) 0.2287(2) 0.0411(9) Uani 1 d . . H52A H 0.8862(4) 0.8351(2) 0.1941(2) 0.049 Uiso 1 calc R . H52B H 0.9757(4) 0.8077(2) 0.2821(2) 0.049 Uiso 1 calc R . C53 C 1.0660(5) 0.7952(3) 0.1830(4) 0.094(2) Uani 1 d . . H53A H 1.1129(5) 0.7532(3) 0.2175(4) 0.113 Uiso 1 calc R . H53B H 1.0162(5) 0.7736(3) 0.1295(4) 0.113 Uiso 1 calc R . C54 C 1.1567(5) 0.8518(2) 0.1672(4) 0.101(2) Uani 1 d . . H54A H 1.2472(5) 0.8346(2) 0.1904(4) 0.121 Uiso 1 calc R . H54B H 1.1462(5) 0.8591(2) 0.1059(4) 0.121 Uiso 1 calc R . C55 C 1.1331(4) 0.9217(2) 0.2053(2) 0.0531(11) Uani 1 d . . H55A H 1.1129(4) 0.9624(2) 0.1623(2) 0.064 Uiso 1 calc R . H55B H 1.2118(4) 0.9371(2) 0.2474(2) 0.064 Uiso 1 calc R . O41 O 0.1608(4) 0.0744(2) 0.0447(2) 0.0995(13) Uani 1 d . . C42 C 0.2559(6) 0.1311(3) 0.0370(3) 0.098(2) Uani 1 d . . H42A H 0.3024(6) 0.1483(3) 0.0933(3) 0.118 Uiso 1 calc R . H42B H 0.2124(6) 0.1758(3) 0.0058(3) 0.118 Uiso 1 calc R . C43 C 0.3494(5) 0.0976(3) -0.0083(3) 0.0740(15) Uani 1 d . . H43A H 0.4328(5) 0.0850(3) 0.0309(3) 0.089 Uiso 1 calc R . H43B H 0.3671(5) 0.1332(3) -0.0515(3) 0.089 Uiso 1 calc R . C44 C 0.2836(5) 0.0271(3) -0.0476(3) 0.083(2) Uani 1 d . . H44A H 0.2526(5) 0.0342(3) -0.1089(3) 0.100 Uiso 1 calc R . H44C H 0.3443(5) -0.0168(3) -0.0376(3) 0.100 Uiso 1 calc R . C45 C 0.1764(5) 0.0147(3) -0.0088(3) 0.0703(14) Uani 1 d . . H45B H 0.0955(5) 0.0092(3) -0.0528(3) 0.084 Uiso 1 calc R . H45A H 0.1903(5) -0.0335(3) 0.0235(3) 0.084 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 As1 0.0289(2) 0.0209(2) 0.0257(2) -0.0017(2) 0.00604(12) -0.0025(2) Li1 0.033(3) 0.023(3) 0.036(3) -0.005(3) 0.009(3) -0.002(3) N1 0.027(2) 0.0204(14) 0.0303(14) -0.0023(12) 0.0086(12) -0.0001(12) Li2 0.033(3) 0.028(3) 0.033(3) 0.000(3) 0.002(3) 0.000(3) N2 0.032(2) 0.0267(15) 0.0242(14) -0.0006(12) 0.0085(12) -0.0049(13) Li3 0.043(4) 0.026(3) 0.038(3) 0.003(3) 0.016(3) 0.001(3) N3 0.0235(15) 0.0246(15) 0.0236(14) -0.0016(12) 0.0004(11) -0.0012(12) C11 0.028(2) 0.029(2) 0.022(2) -0.0058(14) 0.0004(14) 0.0037(15) C12 0.039(2) 0.024(2) 0.037(2) -0.002(2) 0.000(2) 0.005(2) C13 0.054(3) 0.027(2) 0.045(2) -0.005(2) -0.012(2) 0.011(2) C14 0.042(3) 0.050(3) 0.056(3) -0.011(2) -0.003(2) 0.025(2) C15 0.034(2) 0.045(3) 0.048(2) -0.009(2) 0.006(2) 0.012(2) C16 0.028(2) 0.032(2) 0.030(2) -0.006(2) 0.0029(14) 0.006(2) C17 0.043(2) 0.054(3) 0.072(3) -0.006(2) 0.034(2) -0.009(2) O17 0.0322(14) 0.0319(14) 0.0489(15) -0.0056(12) 0.0206(12) -0.0019(11) C21 0.024(2) 0.019(2) 0.029(2) -0.0023(15) 0.0077(13) 0.0018(15) C22 0.026(2) 0.025(2) 0.031(2) -0.0024(15) 0.0060(15) -0.0011(15) C23 0.033(2) 0.028(2) 0.048(2) -0.003(2) 0.013(2) -0.004(2) C24 0.041(2) 0.022(2) 0.054(2) 0.010(2) 0.022(2) 0.010(2) C25 0.043(2) 0.032(2) 0.026(2) 0.0026(15) 0.011(2) 0.003(2) C26 0.026(2) 0.018(2) 0.029(2) 0.0030(15) 0.0061(14) 0.002(2) C27 0.047(2) 0.045(2) 0.030(2) 0.000(2) -0.004(2) -0.008(2) O27 0.0362(14) 0.0326(14) 0.0256(12) 0.0025(10) -0.0014(10) -0.0075(11) C31 0.020(2) 0.030(2) 0.023(2) -0.0036(14) 0.0099(14) -0.0009(14) C32 0.031(2) 0.032(2) 0.030(2) -0.0052(15) 0.007(2) -0.001(2) C33 0.031(2) 0.040(2) 0.034(2) -0.011(2) 0.004(2) -0.005(2) C34 0.026(2) 0.052(3) 0.029(2) 0.000(2) -0.002(2) -0.002(2) C35 0.027(2) 0.037(2) 0.037(2) 0.006(2) 0.003(2) 0.001(2) C36 0.024(2) 0.029(2) 0.028(2) -0.0010(15) 0.0075(15) -0.002(2) C37 0.041(2) 0.028(2) 0.065(3) 0.002(2) -0.001(2) 0.008(2) O37 0.0266(13) 0.0265(13) 0.0389(13) -0.0026(11) 0.0002(10) -0.0004(11) O51 0.051(2) 0.0318(14) 0.0431(14) -0.0055(12) 0.0247(13) -0.0062(12) C52 0.045(2) 0.038(2) 0.043(2) -0.005(2) 0.015(2) -0.011(2) C53 0.104(4) 0.051(3) 0.157(5) -0.037(3) 0.095(4) -0.025(3) C54 0.120(5) 0.040(3) 0.181(6) -0.035(3) 0.119(5) -0.022(3) C55 0.066(3) 0.048(3) 0.056(2) -0.010(2) 0.037(2) -0.012(2) O41 0.126(3) 0.095(3) 0.098(3) -0.034(2) 0.069(2) -0.050(3) C42 0.153(5) 0.074(4) 0.091(4) -0.035(3) 0.075(4) -0.059(4) C43 0.091(4) 0.071(3) 0.063(3) -0.001(3) 0.023(3) -0.041(3) C44 0.087(4) 0.081(4) 0.091(4) -0.031(3) 0.039(3) -0.040(3) C45 0.070(3) 0.074(3) 0.072(3) -0.025(3) 0.027(3) -0.039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 N2 1.853(2) . ? As1 N1 1.871(3) 3_776 ? As1 N3 1.885(3) 3_776 ? As1 Li1 2.759(5) . ? As1 Li3 2.796(5) . ? As1 Li2 2.854(5) . ? Li1 O17 1.974(6) . ? Li1 N2 1.987(6) . ? Li1 N1 2.030(6) . ? Li1 N3 2.122(6) 3_776 ? Li1 Li2 2.418(8) 3_776 ? Li1 Li3 2.647(8) 3_776 ? Li1 C21 2.731(6) . ? Li1 C11 2.773(6) . ? Li1 C16 2.788(6) . ? Li1 Li2 3.197(8) . ? N1 C11 1.388(4) . ? N1 As1 1.871(3) 3_776 ? N1 Li3 2.123(6) 3_776 ? N1 Li2 2.229(6) 3_776 ? Li2 O37 1.939(6) . ? Li2 N2 1.955(6) . ? Li2 N3 2.065(6) . ? Li2 N1 2.229(6) 3_776 ? Li2 Li1 2.418(8) 3_776 ? Li2 Li3 2.553(8) 3_776 ? Li2 O27 2.623(6) . ? N2 C21 1.382(4) . ? Li3 O51 1.955(6) . ? Li3 O27 2.079(6) 3_776 ? Li3 N1 2.123(6) 3_776 ? Li3 N3 2.128(6) 3_776 ? Li3 Li2 2.553(8) 3_776 ? Li3 Li1 2.647(8) 3_776 ? N3 C31 1.389(4) . ? N3 As1 1.885(3) 3_776 ? N3 Li1 2.122(6) 3_776 ? N3 Li3 2.128(6) 3_776 ? C11 C12 1.410(4) . ? C11 C16 1.425(4) . ? C12 C13 1.391(5) . ? C13 C14 1.369(5) . ? C14 C15 1.396(5) . ? C15 C16 1.376(4) . ? C16 O17 1.401(4) . ? C17 O17 1.442(4) . ? C21 C22 1.401(4) . ? C21 C26 1.421(4) . ? C22 C23 1.392(4) . ? C23 C24 1.382(4) . ? C24 C25 1.389(5) . ? C25 C26 1.370(4) . ? C26 O27 1.396(4) . ? C27 O27 1.432(4) . ? O27 Li3 2.079(6) 3_776 ? C31 C32 1.400(4) . ? C31 C36 1.433(4) . ? C32 C33 1.390(4) . ? C33 C34 1.372(5) . ? C34 C35 1.400(5) . ? C35 C36 1.371(4) . ? C36 O37 1.402(4) . ? C37 O37 1.423(4) . ? O51 C55 1.429(4) . ? O51 C52 1.454(4) . ? C52 C53 1.491(5) . ? C53 C54 1.437(5) . ? C54 C55 1.420(5) . ? O41 C45 1.394(5) . ? O41 C42 1.433(5) . ? C42 C43 1.473(6) . ? C43 C44 1.489(6) . ? C44 C45 1.423(6) . ? 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 As1 N1 93.44(11) . 3_776 ? N2 As1 N3 95.83(11) . 3_776 ? N1 As1 N3 92.10(11) 3_776 3_776 ? N2 As1 Li1 46.06(14) . . ? N1 As1 Li1 99.15(14) 3_776 . ? N3 As1 Li1 50.16(13) 3_776 . ? N2 As1 Li3 117.17(14) . . ? N1 As1 Li3 49.38(14) 3_776 . ? N3 As1 Li3 49.53(14) 3_776 . ? Li1 As1 Li3 86.6(2) . . ? N2 As1 Li2 42.82(14) . . ? N1 As1 Li2 51.28(13) 3_776 . ? N3 As1 Li2 102.30(13) 3_776 . ? Li1 As1 Li2 69.4(2) . . ? Li3 As1 Li2 89.2(2) . . ? O17 Li1 N2 121.5(3) . . ? O17 Li1 N1 81.6(2) . . ? N2 Li1 N1 116.3(3) . . ? O17 Li1 N3 143.1(3) . 3_776 ? N2 Li1 N3 84.9(2) . 3_776 ? N1 Li1 N3 111.3(3) . 3_776 ? O17 Li1 Li2 118.3(3) . 3_776 ? N2 Li1 Li2 118.4(3) . 3_776 ? N1 Li1 Li2 59.4(2) . 3_776 ? N3 Li1 Li2 53.6(2) 3_776 3_776 ? O17 Li1 Li3 82.7(2) . 3_776 ? N2 Li1 Li3 71.7(2) . 3_776 ? N1 Li1 Li3 52.0(2) . 3_776 ? N3 Li1 Li3 133.1(3) 3_776 3_776 ? Li2 Li1 Li3 103.0(3) 3_776 3_776 ? O17 Li1 C21 94.4(2) . . ? N2 Li1 C21 28.98(12) . . ? N1 Li1 C21 126.9(3) . . ? N3 Li1 C21 103.2(2) 3_776 . ? Li2 Li1 C21 147.0(3) 3_776 . ? Li3 Li1 C21 75.0(2) 3_776 . ? O17 Li1 As1 149.6(3) . . ? N2 Li1 As1 42.16(12) . . ? N1 Li1 As1 127.2(3) . . ? N3 Li1 As1 43.02(12) 3_776 . ? Li2 Li1 As1 88.3(2) 3_776 . ? Li3 Li1 As1 106.8(2) 3_776 . ? C21 Li1 As1 61.95(13) . . ? O17 Li1 C11 56.8(2) . . ? N2 Li1 C11 139.1(3) . . ? N1 Li1 C11 28.62(12) . . ? N3 Li1 C11 121.2(2) 3_776 . ? Li2 Li1 C11 69.0(2) 3_776 . ? Li3 Li1 C11 67.5(2) 3_776 . ? C21 Li1 C11 134.4(2) . . ? As1 Li1 C11 153.6(2) . . ? O17 Li1 C16 28.13(12) . . ? N2 Li1 C16 141.6(3) . . ? N1 Li1 C16 57.2(2) . . ? N3 Li1 C16 133.6(3) 3_776 . ? Li2 Li1 C16 91.7(2) 3_776 . ? Li3 Li1 C16 78.9(2) 3_776 . ? C21 Li1 C16 119.4(2) . . ? As1 Li1 C16 174.2(2) . . ? C11 Li1 C16 29.69(11) . . ? O17 Li1 Li2 129.8(3) . . ? N2 Li1 Li2 35.5(2) . . ? N1 Li1 Li2 82.5(2) . . ? N3 Li1 Li2 86.9(2) 3_776 . ? Li2 Li1 Li2 92.7(2) 3_776 . ? Li3 Li1 Li2 50.8(2) 3_776 . ? C21 Li1 Li2 59.9(2) . . ? As1 Li1 Li2 56.70(14) . . ? C11 Li1 Li2 109.3(2) . . ? C16 Li1 Li2 129.1(2) . . ? C11 N1 As1 118.5(2) . 3_776 ? C11 N1 Li1 106.9(3) . . ? As1 N1 Li1 133.5(2) 3_776 . ? C11 N1 Li3 116.6(2) . 3_776 ? As1 N1 Li3 88.6(2) 3_776 3_776 ? Li1 N1 Li3 79.2(2) . 3_776 ? C11 N1 Li2 107.3(2) . 3_776 ? As1 N1 Li2 87.8(2) 3_776 3_776 ? Li1 N1 Li2 69.0(2) . 3_776 ? Li3 N1 Li2 131.5(2) 3_776 3_776 ? O37 Li2 N2 151.3(3) . . ? O37 Li2 N3 82.4(2) . . ? N2 Li2 N3 118.5(3) . . ? O37 Li2 N1 114.4(3) . 3_776 ? N2 Li2 N1 80.5(2) . 3_776 ? N3 Li2 N1 105.9(3) . 3_776 ? O37 Li2 Li1 94.0(3) . 3_776 ? N2 Li2 Li1 113.9(3) . 3_776 ? N3 Li2 Li1 55.8(2) . 3_776 ? N1 Li2 Li1 51.6(2) 3_776 3_776 ? O37 Li2 Li3 109.0(3) . 3_776 ? N2 Li2 Li3 74.4(2) . 3_776 ? N3 Li2 Li3 53.6(2) . 3_776 ? N1 Li2 Li3 128.4(3) 3_776 3_776 ? Li1 Li2 Li3 100.0(3) 3_776 3_776 ? O37 Li2 O27 93.4(2) . . ? N2 Li2 O27 67.4(2) . . ? N3 Li2 O27 93.5(2) . . ? N1 Li2 O27 147.6(3) 3_776 . ? Li1 Li2 O27 147.0(3) 3_776 . ? Li3 Li2 O27 47.3(2) 3_776 . ? O37 Li2 As1 143.9(3) . . ? N2 Li2 As1 40.10(12) . . ? N3 Li2 As1 124.6(2) . . ? N1 Li2 As1 40.91(11) 3_776 . ? Li1 Li2 As1 85.3(2) 3_776 . ? Li3 Li2 As1 106.6(2) 3_776 . ? O27 Li2 As1 106.7(2) . . ? O37 Li2 Li1 162.2(3) . . ? N2 Li2 Li1 36.2(2) . . ? N3 Li2 Li1 83.6(2) . . ? N1 Li2 Li1 80.2(2) 3_776 . ? Li1 Li2 Li1 87.3(2) 3_776 . ? Li3 Li2 Li1 53.4(2) 3_776 . ? O27 Li2 Li1 76.4(2) . . ? As1 Li2 Li1 53.89(13) . . ? C21 N2 As1 121.0(2) . . ? C21 N2 Li2 126.2(3) . . ? As1 N2 Li2 97.1(2) . . ? C21 N2 Li1 106.9(3) . . ? As1 N2 Li1 91.8(2) . . ? Li2 N2 Li1 108.4(3) . . ? O51 Li3 O27 94.9(2) . 3_776 ? O51 Li3 N1 107.3(3) . 3_776 ? O27 Li3 N1 148.4(3) 3_776 3_776 ? O51 Li3 N3 119.7(3) . 3_776 ? O27 Li3 N3 109.5(3) 3_776 3_776 ? N1 Li3 N3 79.0(2) 3_776 3_776 ? O51 Li3 Li2 150.4(3) . 3_776 ? O27 Li3 Li2 68.1(2) 3_776 3_776 ? N1 Li3 Li2 98.6(2) 3_776 3_776 ? N3 Li3 Li2 51.4(2) 3_776 3_776 ? O51 Li3 Li1 132.5(3) . 3_776 ? O27 Li3 Li1 99.6(3) 3_776 3_776 ? N1 Li3 Li1 48.9(2) 3_776 3_776 ? N3 Li3 Li1 97.5(2) 3_776 3_776 ? Li2 Li3 Li1 75.8(2) 3_776 3_776 ? O51 Li3 As1 104.9(2) . . ? O27 Li3 As1 151.2(3) 3_776 . ? N1 Li3 As1 41.98(12) 3_776 . ? N3 Li3 As1 42.37(12) 3_776 . ? Li2 Li3 As1 84.9(2) 3_776 . ? Li1 Li3 As1 82.3(2) 3_776 . ? C31 N3 As1 118.7(2) . 3_776 ? C31 N3 Li2 109.0(2) . . ? As1 N3 Li2 132.3(2) 3_776 . ? C31 N3 Li1 116.9(2) . 3_776 ? As1 N3 Li1 86.8(2) 3_776 3_776 ? Li2 N3 Li1 70.5(2) . 3_776 ? C31 N3 Li3 111.3(2) . 3_776 ? As1 N3 Li3 88.1(2) 3_776 3_776 ? Li2 N3 Li3 75.0(2) . 3_776 ? Li1 N3 Li3 127.4(2) 3_776 3_776 ? N1 C11 C12 127.6(3) . . ? N1 C11 C16 117.2(3) . . ? C12 C11 C16 115.3(3) . . ? N1 C11 Li1 44.5(2) . . ? C12 C11 Li1 159.8(3) . . ? C16 C11 Li1 75.8(2) . . ? C13 C12 C11 121.1(3) . . ? C14 C13 C12 121.5(4) . . ? C13 C14 C15 119.9(3) . . ? C16 C15 C14 118.7(4) . . ? C15 C16 O17 122.9(3) . . ? C15 C16 C11 123.6(3) . . ? O17 C16 C11 113.5(3) . . ? C15 C16 Li1 157.0(3) . . ? O17 C16 Li1 41.6(2) . . ? C11 C16 Li1 74.5(2) . . ? C16 O17 C17 117.1(3) . . ? C16 O17 Li1 110.2(2) . . ? C17 O17 Li1 131.9(3) . . ? N2 C21 C22 127.7(3) . . ? N2 C21 C26 116.5(3) . . ? C22 C21 C26 115.8(3) . . ? N2 C21 Li1 44.1(2) . . ? C22 C21 Li1 111.2(2) . . ? C26 C21 Li1 113.5(2) . . ? C23 C22 C21 121.9(3) . . ? C22 C23 C24 120.1(3) . . ? C23 C24 C25 119.8(3) . . ? C26 C25 C24 119.8(3) . . ? C25 C26 O27 123.7(3) . . ? C25 C26 C21 122.6(3) . . ? O27 C26 C21 113.7(3) . . ? C26 O27 C27 116.3(2) . . ? C26 O27 Li3 118.3(2) . 3_776 ? C27 O27 Li3 121.1(3) . 3_776 ? C26 O27 Li2 105.3(2) . . ? C27 O27 Li2 119.0(2) . . ? Li3 O27 Li2 64.6(2) 3_776 . ? N3 C31 C32 127.6(3) . . ? N3 C31 C36 118.0(3) . . ? C32 C31 C36 114.3(3) . . ? C33 C32 C31 122.6(3) . . ? C34 C33 C32 121.0(3) . . ? C33 C34 C35 119.1(3) . . ? C36 C35 C34 119.5(3) . . ? C35 C36 O37 123.3(3) . . ? C35 C36 C31 123.5(3) . . ? O37 C36 C31 113.2(3) . . ? C36 O37 C37 117.4(2) . . ? C36 O37 Li2 114.9(2) . . ? C37 O37 Li2 127.7(3) . . ? C55 O51 C52 108.4(3) . . ? C55 O51 Li3 120.8(3) . . ? C52 O51 Li3 124.5(3) . . ? O51 C52 C53 106.3(3) . . ? C54 C53 C52 106.8(4) . . ? C55 C54 C53 109.3(4) . . ? C54 C55 O51 108.9(3) . . ? C45 O41 C42 106.6(3) . . ? O41 C42 C43 108.8(4) . . ? C42 C43 C44 104.4(4) . . ? C45 C44 C43 105.8(4) . . ? O41 C45 C44 112.1(4) . . ? _refine_diff_density_max 0.541 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.078