# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1780 data_dw9822 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10.50 H25.50 As0.50 Li0.50 N1.50 P1.50' _chemical_formula_weight 260.21 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' 'As' 'As' 0.0499 2.0058 '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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.218(5) _cell_length_b 11.182(6) _cell_length_c 15.967(8) _cell_angle_alpha 108.44(2) _cell_angle_beta 90.46(2) _cell_angle_gamma 108.01(2) _cell_volume 1474.6(13) _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 BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6466 _exptl_absorpt_correction_T_max 0.7412 _exptl_absorpt_process_details ? _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 4457 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3823 _reflns_number_gt 3107 _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^)+(0.0502P)^2^+0.8757P] 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 3823 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.849 _refine_ls_shift/su_mean 0.248 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 0.46497(5) 0.67598(5) 0.81539(3) 0.03191(18) Uani 1 1 d . . . P2 P 0.50285(14) 0.54478(12) 0.67733(8) 0.0300(3) Uani 1 1 d . . . P3 P 0.22688(13) 0.50986(12) 0.79250(8) 0.0291(3) Uani 1 1 d . . . P4 P 0.31896(14) 0.37397(11) 0.69257(8) 0.0288(3) Uani 1 1 d . . . N3 N 0.3260(5) 0.9643(4) 0.9201(3) 0.0384(10) Uani 1 1 d . . . C20 C 0.6812(5) 0.4999(5) 0.6944(3) 0.0382(12) Uani 1 1 d . . . C42 C 0.1365(6) 0.4132(5) 0.5639(3) 0.0444(13) Uani 1 1 d . . . H42A H 0.0597 0.3710 0.5114 0.067 Uiso 1 1 calc R . . H42B H 0.2292 0.4727 0.5505 0.067 Uiso 1 1 calc R . . H42C H 0.0948 0.4650 0.6135 0.067 Uiso 1 1 calc R . . C7 C 0.3115(7) 1.0964(5) 0.9383(4) 0.0528(15) Uani 1 1 d . . . H7A H 0.2605 1.1183 0.9920 0.079 Uiso 1 1 calc R . . H7B H 0.2505 1.0965 0.8878 0.079 Uiso 1 1 calc R . . H7C H 0.4138 1.1630 0.9473 0.079 Uiso 1 1 calc R . . C41 C 0.0311(6) 0.2107(5) 0.6081(3) 0.0472(14) Uani 1 1 d . . . H41A H -0.0110 0.2604 0.6584 0.071 Uiso 1 1 calc R . . H41B H 0.0562 0.1399 0.6225 0.071 Uiso 1 1 calc R . . H41C H -0.0450 0.1710 0.5553 0.071 Uiso 1 1 calc R . . C21 C 0.6959(6) 0.4667(5) 0.7786(4) 0.0488(14) Uani 1 1 d . . . H21A H 0.7935 0.4502 0.7840 0.073 Uiso 1 1 calc R . . H21B H 0.6106 0.3866 0.7757 0.073 Uiso 1 1 calc R . . H21C H 0.6933 0.5416 0.8303 0.073 Uiso 1 1 calc R . . C22 C 0.6772(6) 0.3836(5) 0.6127(4) 0.0575(16) Uani 1 1 d . . . H22A H 0.6618 0.4055 0.5592 0.086 Uiso 1 1 calc R . . H22B H 0.5925 0.3043 0.6119 0.086 Uiso 1 1 calc R . . H22C H 0.7746 0.3656 0.6140 0.086 Uiso 1 1 calc R . . C40 C 0.1767(5) 0.3056(4) 0.5895(3) 0.0326(11) Uani 1 1 d . . . C8 C 0.1711(6) 0.8651(5) 0.9066(4) 0.0500(14) Uani 1 1 d . . . H8A H 0.1227 0.8843 0.9615 0.075 Uiso 1 1 calc R . . H8B H 0.1792 0.7755 0.8907 0.075 Uiso 1 1 calc R . . H8C H 0.1085 0.8697 0.8585 0.075 Uiso 1 1 calc R . . N2 N 0.6132(4) 0.9994(4) 0.7536(3) 0.0385(10) Uani 1 1 d . . . N1 N 0.2893(5) 0.8998(4) 0.6860(3) 0.0380(10) Uani 1 1 d . . . C6 C 0.6551(6) 1.1434(5) 0.7985(4) 0.0559(15) Uani 1 1 d . . . H6A H 0.7341 1.1902 0.7685 0.084 Uiso 1 1 calc R . . H6B H 0.6952 1.1659 0.8606 0.084 Uiso 1 1 calc R . . H6C H 0.5642 1.1707 0.7965 0.084 Uiso 1 1 calc R . . C3 C 0.4058(7) 0.9776(6) 0.6459(4) 0.0607(17) Uani 1 1 d . . . H3A H 0.4141 1.0728 0.6717 0.073 Uiso 1 1 calc R . . H3B H 0.3735 0.9483 0.5813 0.073 Uiso 1 1 calc R . . C1 C 0.2413(6) 0.7581(5) 0.6328(4) 0.0522(15) Uani 1 1 d . . . H1A H 0.1968 0.7450 0.5733 0.078 Uiso 1 1 calc R . . H1B H 0.1643 0.7069 0.6614 0.078 Uiso 1 1 calc R . . H1C H 0.3305 0.7273 0.6279 0.078 Uiso 1 1 calc R . . C5 C 0.7500(6) 0.9614(6) 0.7602(4) 0.0559(16) Uani 1 1 d . . . H5A H 0.7242 0.8649 0.7309 0.084 Uiso 1 1 calc R . . H5B H 0.7870 0.9854 0.8229 0.084 Uiso 1 1 calc R . . H5C H 0.8303 1.0085 0.7311 0.084 Uiso 1 1 calc R . . C2 C 0.1545(7) 0.9437(6) 0.6907(4) 0.0566(16) Uani 1 1 d . . . H2A H 0.1843 1.0384 0.7267 0.085 Uiso 1 1 calc R . . H2B H 0.0761 0.8912 0.7179 0.085 Uiso 1 1 calc R . . H2C H 0.1130 0.9308 0.6306 0.085 Uiso 1 1 calc R . . C30 C 0.2202(5) 0.4446(5) 0.8894(3) 0.0337(11) Uani 1 1 d . . . C9 C 0.4156(5) 0.9607(5) 0.9961(3) 0.0391(12) Uani 1 1 d . . . H9A H 0.4042 0.8668 0.9887 0.047 Uiso 1 1 calc R . . H9B H 0.3738 0.9978 1.0517 0.047 Uiso 1 1 calc R . . C32 C 0.3568(6) 0.4028(5) 0.9052(3) 0.0423(13) Uani 1 1 d . . . H32A H 0.4516 0.4787 0.9156 0.063 Uiso 1 1 calc R . . H32B H 0.3607 0.3292 0.8529 0.063 Uiso 1 1 calc R . . H32C H 0.3464 0.3737 0.9573 0.063 Uiso 1 1 calc R . . C23 C 0.8170(5) 0.6219(5) 0.6993(4) 0.0507(15) Uani 1 1 d . . . H23A H 0.9128 0.6039 0.7071 0.076 Uiso 1 1 calc R . . H23B H 0.8138 0.6983 0.7497 0.076 Uiso 1 1 calc R . . H23C H 0.8119 0.6420 0.6441 0.076 Uiso 1 1 calc R . . C31 C 0.0736(6) 0.3252(5) 0.8687(3) 0.0453(13) Uani 1 1 d . . . H31A H 0.0608 0.2916 0.9188 0.068 Uiso 1 1 calc R . . H31B H 0.0801 0.2546 0.8152 0.068 Uiso 1 1 calc R . . H31C H -0.0146 0.3524 0.8587 0.068 Uiso 1 1 calc R . . C4 C 0.5608(6) 0.9642(6) 0.6597(4) 0.0606(17) Uani 1 1 d . . . H4A H 0.5556 0.8710 0.6279 0.073 Uiso 1 1 calc R . . H4B H 0.6364 1.0229 0.6338 0.073 Uiso 1 1 calc R . . C33 C 0.2113(7) 0.5556(5) 0.9713(3) 0.0496(14) Uani 1 1 d . . . H33A H 0.1220 0.5814 0.9614 0.074 Uiso 1 1 calc R . . H33B H 0.3050 0.6328 0.9829 0.074 Uiso 1 1 calc R . . H33C H 0.2012 0.5243 1.0225 0.074 Uiso 1 1 calc R . . C43 C 0.2482(6) 0.2289(5) 0.5142(3) 0.0514(15) Uani 1 1 d . . . H43A H 0.2728 0.1594 0.5305 0.077 Uiso 1 1 calc R . . H43B H 0.3424 0.2905 0.5038 0.077 Uiso 1 1 calc R . . H43C H 0.1754 0.1877 0.4600 0.077 Uiso 1 1 calc R . . Li1 Li 0.4139(9) 0.8909(8) 0.7982(5) 0.0355(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0349(3) 0.0234(3) 0.0334(3) 0.0074(2) 0.0053(2) 0.0062(2) P2 0.0321(7) 0.0286(7) 0.0315(7) 0.0121(5) 0.0088(5) 0.0108(5) P3 0.0296(7) 0.0265(7) 0.0295(7) 0.0076(5) 0.0053(5) 0.0086(5) P4 0.0323(7) 0.0246(7) 0.0276(7) 0.0068(5) 0.0034(5) 0.0085(5) N3 0.049(3) 0.026(2) 0.037(2) 0.0068(18) 0.000(2) 0.013(2) C20 0.034(3) 0.032(3) 0.054(3) 0.017(2) 0.014(2) 0.014(2) C42 0.049(3) 0.044(3) 0.038(3) 0.015(3) -0.009(2) 0.012(3) C7 0.069(4) 0.034(3) 0.055(4) 0.007(3) -0.006(3) 0.026(3) C41 0.047(3) 0.039(3) 0.043(3) 0.011(3) -0.012(3) 0.001(3) C21 0.037(3) 0.053(4) 0.073(4) 0.038(3) 0.010(3) 0.021(3) C22 0.049(3) 0.041(3) 0.081(4) 0.010(3) 0.024(3) 0.024(3) C40 0.038(3) 0.028(3) 0.026(3) 0.004(2) -0.001(2) 0.008(2) C8 0.049(3) 0.048(3) 0.053(3) 0.015(3) 0.009(3) 0.018(3) N2 0.036(2) 0.028(2) 0.051(3) 0.015(2) 0.005(2) 0.0080(19) N1 0.041(2) 0.032(2) 0.039(2) 0.0133(19) -0.0032(19) 0.0077(19) C6 0.047(3) 0.034(3) 0.082(4) 0.020(3) 0.010(3) 0.006(3) C3 0.060(4) 0.068(4) 0.056(4) 0.036(3) -0.001(3) 0.009(3) C1 0.053(3) 0.040(3) 0.055(4) 0.004(3) -0.009(3) 0.015(3) C5 0.043(3) 0.048(4) 0.082(4) 0.027(3) 0.019(3) 0.018(3) C2 0.066(4) 0.059(4) 0.053(4) 0.015(3) -0.001(3) 0.035(3) C30 0.040(3) 0.033(3) 0.024(3) 0.010(2) 0.008(2) 0.007(2) C9 0.057(3) 0.032(3) 0.033(3) 0.009(2) 0.006(3) 0.022(2) C32 0.050(3) 0.043(3) 0.036(3) 0.020(2) 0.001(2) 0.010(3) C23 0.029(3) 0.049(3) 0.080(4) 0.031(3) 0.016(3) 0.012(3) C31 0.047(3) 0.034(3) 0.048(3) 0.018(3) 0.013(3) 0.001(2) C4 0.052(4) 0.068(4) 0.054(4) 0.025(3) 0.016(3) 0.006(3) C33 0.070(4) 0.036(3) 0.037(3) 0.012(2) 0.019(3) 0.009(3) C43 0.065(4) 0.052(4) 0.030(3) 0.001(3) 0.000(3) 0.021(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 P2 2.3274(16) . ? As1 P3 2.3319(17) . ? As1 Li1 2.681(8) . ? P2 C20 1.902(5) . ? P2 P4 2.209(2) . ? P3 C30 1.902(5) . ? P3 P4 2.2047(18) . ? P4 C40 1.887(5) . ? N3 C7 1.462(6) . ? N3 C8 1.477(6) . ? N3 C9 1.480(6) . ? N3 Li1 2.132(9) . ? C20 C22 1.514(7) . ? C20 C23 1.519(7) . ? C20 C21 1.519(7) . ? C42 C40 1.529(7) . ? C41 C40 1.530(7) . ? C40 C43 1.524(6) . ? N2 C4 1.460(7) . ? N2 C5 1.462(6) . ? N2 C6 1.462(6) . ? N2 Li1 2.131(9) . ? N1 C3 1.452(7) . ? N1 C1 1.462(6) . ? N1 C2 1.465(6) . ? N1 Li1 2.165(9) . ? C3 C4 1.503(8) . ? C30 C32 1.516(7) . ? C30 C33 1.515(6) . ? C30 C31 1.522(6) . ? C9 C9 1.514(10) 2_677 ? 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 P2 As1 P3 85.06(6) . . ? P2 As1 Li1 108.85(17) . . ? P3 As1 Li1 107.31(18) . . ? C20 P2 P4 101.68(16) . . ? C20 P2 As1 107.26(16) . . ? P4 P2 As1 88.46(6) . . ? C30 P3 P4 102.18(16) . . ? C30 P3 As1 106.32(15) . . ? P4 P3 As1 88.45(7) . . ? C40 P4 P3 105.00(16) . . ? C40 P4 P2 106.05(16) . . ? P3 P4 P2 91.06(7) . . ? C7 N3 C8 108.8(4) . . ? C7 N3 C9 110.6(4) . . ? C8 N3 C9 108.5(4) . . ? C7 N3 Li1 114.8(4) . . ? C8 N3 Li1 102.3(4) . . ? C9 N3 Li1 111.3(4) . . ? C22 C20 C23 110.2(4) . . ? C22 C20 C21 111.0(4) . . ? C23 C20 C21 108.5(4) . . ? C22 C20 P2 106.4(4) . . ? C23 C20 P2 105.8(3) . . ? C21 C20 P2 114.8(3) . . ? C43 C40 C41 110.3(4) . . ? C43 C40 C42 109.6(4) . . ? C41 C40 C42 109.4(4) . . ? C43 C40 P4 106.9(3) . . ? C41 C40 P4 106.9(3) . . ? C42 C40 P4 113.6(3) . . ? C4 N2 C5 108.6(4) . . ? C4 N2 C6 110.5(4) . . ? C5 N2 C6 108.1(4) . . ? C4 N2 Li1 101.4(4) . . ? C5 N2 Li1 116.0(4) . . ? C6 N2 Li1 112.1(4) . . ? C3 N1 C1 110.6(4) . . ? C3 N1 C2 109.6(4) . . ? C1 N1 C2 108.3(4) . . ? C3 N1 Li1 104.7(4) . . ? C1 N1 Li1 98.0(4) . . ? C2 N1 Li1 124.9(4) . . ? N1 C3 C4 112.7(5) . . ? C32 C30 C33 109.5(4) . . ? C32 C30 C31 109.6(4) . . ? C33 C30 C31 110.2(4) . . ? C32 C30 P3 114.6(3) . . ? C33 C30 P3 106.6(3) . . ? C31 C30 P3 106.2(3) . . ? N3 C9 C9 112.1(5) . 2_677 ? N2 C4 C3 112.4(5) . . ? N2 Li1 N3 125.5(4) . . ? N2 Li1 N1 85.2(3) . . ? N3 Li1 N1 112.3(4) . . ? N2 Li1 As1 107.4(3) . . ? N3 Li1 As1 101.5(3) . . ? N1 Li1 As1 127.1(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.439 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.070 data_dw9936 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H59 As Li N4 O P3' _chemical_formula_weight 642.56 _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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.651(2) _cell_length_b 12.638(3) _cell_length_c 13.991(3) _cell_angle_alpha 71.11(3) _cell_angle_beta 73.79(3) _cell_angle_gamma 64.61(3) _cell_volume 1737.0(6) _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 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method ? _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.142 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11462 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7903 _reflns_number_observed 6276 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _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 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^)+(0.0602P)^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 7903 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_obs 0.0362 _refine_ls_wR_factor_all 0.1173 _refine_ls_wR_factor_obs 0.0901 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 0.937 _refine_ls_restrained_S_all 1.082 _refine_ls_restrained_S_obs 0.937 _refine_ls_shift/esd_max -0.073 _refine_ls_shift/esd_mean 0.012 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 1.16621(2) -0.33020(2) 0.31436(2) 0.02284(9) Uani 1 d . . P1 P 1.34927(6) -0.43669(5) 0.21313(5) 0.02058(15) Uani 1 d . . P2 P 1.42009(6) -0.28977(5) 0.17953(5) 0.02067(14) Uani 1 d . . P3 P 1.22353(6) -0.16405(5) 0.22480(5) 0.02101(15) Uani 1 d . . N1 N 1.0039(2) -0.2675(2) -0.0969(2) 0.0394(6) Uani 1 d . . N2 N 0.9629(2) -0.2786(2) 0.0971(2) 0.0260(5) Uani 1 d . . N3 N 0.6522(2) 0.0054(2) 0.4057(2) 0.0316(5) Uani 1 d . . N4 N 0.8050(2) -0.1632(2) 0.31101(15) 0.0229(4) Uani 1 d . . O1 O 0.9279(2) -0.4560(2) 0.31619(15) 0.0360(4) Uani 1 d . . Li1 Li 0.9543(4) -0.3035(3) 0.2512(3) 0.0257(9) Uani 1 d . . C11 C 1.4623(2) -0.5618(2) 0.3016(2) 0.0261(5) Uani 1 d . . C12 C 1.4099(3) -0.6624(2) 0.3425(2) 0.0411(7) Uani 1 d . . H12A H 1.4015(3) -0.6854(2) 0.2850(2) 0.062 Uiso 1 calc R . H12B H 1.3253(3) -0.6343(2) 0.3850(2) 0.062 Uiso 1 calc R . H12C H 1.4692(3) -0.7323(2) 0.3838(2) 0.062 Uiso 1 calc R . C13 C 1.5944(2) -0.6043(2) 0.2349(2) 0.0329(6) Uani 1 d . . H13A H 1.6273(2) -0.5390(2) 0.2090(2) 0.049 Uiso 1 calc R . H13B H 1.5863(2) -0.6270(2) 0.1772(2) 0.049 Uiso 1 calc R . H13C H 1.6541(2) -0.6741(2) 0.2759(2) 0.049 Uiso 1 calc R . C14 C 1.4754(3) -0.5257(2) 0.3912(2) 0.0345(6) Uani 1 d . . H14A H 1.5092(3) -0.4610(2) 0.3647(2) 0.052 Uiso 1 calc R . H14B H 1.5346(3) -0.5956(2) 0.4326(2) 0.052 Uiso 1 calc R . H14C H 1.3908(3) -0.4975(2) 0.4336(2) 0.052 Uiso 1 calc R . C21 C 1.4528(2) -0.2430(2) 0.0350(2) 0.0267(5) Uani 1 d . . C22 C 1.4791(3) -0.1272(2) 0.0075(2) 0.0383(7) Uani 1 d . . H22A H 1.5498(3) -0.1413(2) 0.0407(2) 0.057 Uiso 1 calc R . H22B H 1.4014(3) -0.0632(2) 0.0310(2) 0.057 Uiso 1 calc R . H22C H 1.5030(3) -0.1030(2) -0.0670(2) 0.057 Uiso 1 calc R . C23 C 1.5734(3) -0.3435(2) -0.0018(2) 0.0382(7) Uani 1 d . . H23A H 1.6443(3) -0.3585(2) 0.0317(2) 0.057 Uiso 1 calc R . H23B H 1.5976(3) -0.3190(2) -0.0762(2) 0.057 Uiso 1 calc R . H23C H 1.5557(3) -0.4172(2) 0.0155(2) 0.057 Uiso 1 calc R . C24 C 1.3428(3) -0.2198(2) -0.0173(2) 0.0342(6) Uani 1 d . . H24A H 1.3253(3) -0.2937(2) 0.0000(2) 0.051 Uiso 1 calc R . H24B H 1.3670(3) -0.1954(2) -0.0916(2) 0.051 Uiso 1 calc R . H24C H 1.2654(3) -0.1556(2) 0.0063(2) 0.051 Uiso 1 calc R . C31 C 1.2472(2) -0.1031(2) 0.3231(2) 0.0249(5) Uani 1 d . . C32 C 1.1113(3) -0.0396(3) 0.3767(2) 0.0445(8) Uani 1 d . . H32A H 1.0591(3) 0.0212(3) 0.3255(2) 0.067 Uiso 1 calc R . H32B H 1.1164(3) -0.0005(3) 0.4247(2) 0.067 Uiso 1 calc R . H32C H 1.0716(3) -0.0990(3) 0.4142(2) 0.067 Uiso 1 calc R . C33 C 1.3106(3) -0.0122(2) 0.2637(2) 0.0400(7) Uani 1 d . . H33A H 1.2586(3) 0.0487(2) 0.2124(2) 0.060 Uiso 1 calc R . H33B H 1.3970(3) -0.0539(2) 0.2295(2) 0.060 Uiso 1 calc R . H33C H 1.3168(3) 0.0270(2) 0.3111(2) 0.060 Uiso 1 calc R . C34 C 1.3283(3) -0.1977(2) 0.4028(2) 0.0331(6) Uani 1 d . . H34A H 1.2877(3) -0.2563(2) 0.4410(2) 0.050 Uiso 1 calc R . H34B H 1.3345(3) -0.1585(2) 0.4502(2) 0.050 Uiso 1 calc R . H34C H 1.4148(3) -0.2392(2) 0.3685(2) 0.050 Uiso 1 calc R . C7 C 1.0050(4) -0.6665(3) 0.3506(3) 0.0687(12) Uani 1 d . . H7A H 1.0591(4) -0.6999(3) 0.2909(3) 0.082 Uiso 1 calc R . H7B H 1.0228(4) -0.7311(3) 0.4138(3) 0.082 Uiso 1 calc R . C8 C 0.8669(4) -0.6182(3) 0.3423(3) 0.0655(10) Uani 1 d . . H8A H 0.8200(4) -0.6607(3) 0.4013(3) 0.079 Uiso 1 calc R . H8B H 0.8563(4) -0.6284(3) 0.2785(3) 0.079 Uiso 1 calc R . C9 C 0.8170(3) -0.4881(3) 0.3416(3) 0.0515(8) Uani 1 d . . H9A H 0.7593(3) -0.4394(3) 0.2900(3) 0.062 Uiso 1 calc R . H9B H 0.7683(3) -0.4743(3) 0.4097(3) 0.062 Uiso 1 calc R . C10 C 1.0322(3) -0.5618(2) 0.3535(3) 0.0590(10) Uani 1 d . . H10A H 1.0365(3) -0.5658(2) 0.4244(3) 0.071 Uiso 1 calc R . H10B H 1.1151(3) -0.5618(2) 0.3095(3) 0.071 Uiso 1 calc R . C1 C 1.0206(3) -0.1669(3) -0.0797(2) 0.0431(7) Uani 1 d . . H1A H 0.9634(3) -0.0898(3) -0.1176(2) 0.052 Uiso 1 calc R . H1B H 1.1106(3) -0.1725(3) -0.1061(2) 0.052 Uiso 1 calc R . C2 C 0.9881(3) -0.1693(2) 0.0361(2) 0.0373(7) Uani 1 d . . H2A H 1.0610(3) -0.1671(2) 0.0575(2) 0.045 Uiso 1 calc R . H2B H 0.9113(3) -0.0971(2) 0.0486(2) 0.045 Uiso 1 calc R . C3 C 1.0953(3) -0.3789(3) -0.0451(2) 0.0391(7) Uani 1 d . . H3A H 1.1842(3) -0.3836(3) -0.0767(2) 0.047 Uiso 1 calc R . H3B H 1.0845(3) -0.4486(3) -0.0537(2) 0.047 Uiso 1 calc R . C4 C 1.0752(3) -0.3853(2) 0.0701(2) 0.0328(6) Uani 1 d . . H4A H 1.0604(3) -0.4599(2) 0.1107(2) 0.039 Uiso 1 calc R . H4B H 1.1536(3) -0.3878(2) 0.0869(2) 0.039 Uiso 1 calc R . C5 C 0.8745(3) -0.2647(3) -0.0503(2) 0.0498(8) Uani 1 d . . H5A H 0.8626(3) -0.3317(3) -0.0630(2) 0.060 Uiso 1 calc R . H5B H 0.8108(3) -0.1881(3) -0.0827(2) 0.060 Uiso 1 calc R . C6 C 0.8500(3) -0.2758(3) 0.0657(2) 0.0391(7) Uani 1 d . . H6A H 0.7728(3) -0.2064(3) 0.0837(2) 0.047 Uiso 1 calc R . H6B H 0.8335(3) -0.3504(3) 0.1029(2) 0.047 Uiso 1 calc R . C15 C 0.6707(3) -0.1253(3) 0.2985(3) 0.0487(9) Uani 1 d . . H15A H 0.6441(3) -0.1955(3) 0.3257(3) 0.058 Uiso 1 calc R . H15B H 0.6641(3) -0.0952(3) 0.2248(3) 0.058 Uiso 1 calc R . C16 C 0.8095(3) -0.2044(2) 0.4217(2) 0.0430(8) Uani 1 d . . H16A H 0.8987(3) -0.2289(2) 0.4327(2) 0.052 Uiso 1 calc R . H16B H 0.7846(3) -0.2756(2) 0.4506(2) 0.052 Uiso 1 calc R . C17 C 0.5794(3) -0.0251(3) 0.3556(2) 0.0420(7) Uani 1 d . . H17A H 0.5334(3) 0.0475(3) 0.3063(2) 0.050 Uiso 1 calc R . H17B H 0.5145(3) -0.0530(3) 0.4075(2) 0.050 Uiso 1 calc R . C18 C 0.7491(3) 0.0438(2) 0.3288(2) 0.0383(7) Uani 1 d . . H18A H 0.7998(3) 0.0631(2) 0.3623(2) 0.046 Uiso 1 calc R . H18B H 0.7061(3) 0.1177(2) 0.2790(2) 0.046 Uiso 1 calc R . C19 C 0.8401(3) -0.0559(2) 0.2718(2) 0.0367(7) Uani 1 d . . H19A H 0.8357(3) -0.0247(2) 0.1977(2) 0.044 Uiso 1 calc R . H19B H 0.9298(3) -0.0788(2) 0.2805(2) 0.044 Uiso 1 calc R . C20 C 0.7177(3) -0.1037(2) 0.4777(2) 0.0388(7) Uani 1 d . . H20A H 0.6531(3) -0.1316(2) 0.5301(2) 0.047 Uiso 1 calc R . H20B H 0.7675(3) -0.0856(2) 0.5131(2) 0.047 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 0.01673(15) 0.02406(14) 0.0280(2) -0.00807(11) -0.00121(10) -0.00791(10) P1 0.0180(3) 0.0200(3) 0.0240(3) -0.0064(2) -0.0031(3) -0.0066(2) P2 0.0187(3) 0.0221(3) 0.0224(3) -0.0058(2) -0.0031(3) -0.0085(2) P3 0.0193(3) 0.0200(3) 0.0250(3) -0.0065(2) -0.0059(3) -0.0062(2) N1 0.0398(15) 0.0507(14) 0.0283(13) -0.0077(11) -0.0047(11) -0.0190(12) N2 0.0212(11) 0.0311(11) 0.0257(11) -0.0077(9) -0.0037(9) -0.0091(9) N3 0.0281(12) 0.0291(11) 0.0360(13) -0.0134(10) -0.0018(10) -0.0073(9) N4 0.0179(10) 0.0250(10) 0.0238(11) -0.0075(8) -0.0012(8) -0.0064(8) O1 0.0310(11) 0.0305(9) 0.0473(12) 0.0000(8) -0.0103(9) -0.0162(8) Li1 0.024(2) 0.022(2) 0.030(2) -0.007(2) -0.003(2) -0.009(2) C11 0.0193(13) 0.0216(11) 0.0331(14) -0.0055(10) -0.0047(11) -0.0041(10) C12 0.036(2) 0.0240(13) 0.055(2) 0.0055(13) -0.0135(14) -0.0106(12) C13 0.0217(14) 0.0294(13) 0.042(2) -0.0126(12) -0.0044(12) -0.0021(11) C14 0.032(2) 0.0336(14) 0.0277(15) -0.0029(12) -0.0105(12) -0.0026(12) C21 0.0288(14) 0.0304(13) 0.0232(13) -0.0051(10) -0.0003(11) -0.0164(11) C22 0.044(2) 0.041(2) 0.033(2) -0.0010(13) -0.0002(13) -0.0282(14) C23 0.034(2) 0.049(2) 0.031(2) -0.0151(13) 0.0077(12) -0.0186(13) C24 0.041(2) 0.044(2) 0.0213(14) -0.0034(12) -0.0054(12) -0.0216(13) C31 0.0243(13) 0.0250(12) 0.0293(14) -0.0127(10) -0.0041(11) -0.0085(10) C32 0.031(2) 0.053(2) 0.060(2) -0.040(2) -0.0025(14) -0.0092(14) C33 0.056(2) 0.0361(15) 0.041(2) -0.0042(13) -0.0182(15) -0.0263(14) C34 0.041(2) 0.0352(14) 0.0288(15) -0.0080(12) -0.0118(12) -0.0148(12) C7 0.091(3) 0.034(2) 0.096(3) -0.006(2) -0.053(3) -0.021(2) C8 0.072(3) 0.061(2) 0.080(3) -0.017(2) -0.003(2) -0.045(2) C9 0.043(2) 0.059(2) 0.058(2) -0.010(2) 0.004(2) -0.033(2) C10 0.062(2) 0.031(2) 0.090(3) 0.008(2) -0.048(2) -0.017(2) C1 0.047(2) 0.040(2) 0.036(2) -0.0006(13) -0.0049(14) -0.0170(14) C2 0.044(2) 0.0335(14) 0.034(2) -0.0064(12) -0.0051(13) -0.0160(13) C3 0.040(2) 0.045(2) 0.033(2) -0.0152(13) 0.0035(13) -0.0170(14) C4 0.0304(15) 0.0328(13) 0.0312(15) -0.0081(12) -0.0073(12) -0.0064(11) C5 0.041(2) 0.076(2) 0.040(2) -0.012(2) -0.0106(15) -0.027(2) C6 0.026(2) 0.055(2) 0.039(2) -0.0150(14) -0.0061(13) -0.0135(13) C15 0.0215(15) 0.062(2) 0.075(2) -0.047(2) -0.0068(15) -0.0055(14) C16 0.049(2) 0.0340(14) 0.028(2) -0.0096(12) 0.0011(13) -0.0021(13) C17 0.0194(14) 0.050(2) 0.060(2) -0.031(2) -0.0029(14) -0.0046(13) C18 0.040(2) 0.0271(13) 0.044(2) -0.0117(12) 0.0009(14) -0.0107(12) C19 0.031(2) 0.0307(13) 0.043(2) -0.0122(13) 0.0059(13) -0.0118(12) C20 0.044(2) 0.0337(14) 0.033(2) -0.0145(12) 0.0019(13) -0.0096(13) _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 P1 2.3349(12) . ? As1 P3 2.3360(10) . ? As1 Li1 2.702(4) . ? P1 C11 1.904(3) . ? P1 P2 2.2093(10) . ? P2 C21 1.890(3) . ? P2 P3 2.2117(12) . ? P3 C31 1.908(2) . ? N1 C5 1.456(4) . ? N1 C3 1.458(4) . ? N1 C1 1.465(4) . ? N2 C2 1.472(3) . ? N2 C6 1.483(3) . ? N2 C4 1.488(3) . ? N2 Li1 2.056(5) . ? N3 C18 1.457(4) . ? N3 C20 1.458(4) . ? N3 C17 1.466(3) . ? N4 C15 1.471(3) . ? N4 C16 1.474(3) . ? N4 C19 1.475(3) . ? N4 Li1 2.091(4) . ? O1 C10 1.430(3) . ? O1 C9 1.435(3) . ? O1 Li1 1.963(4) . ? C11 C12 1.522(4) . ? C11 C14 1.529(3) . ? C11 C13 1.530(3) . ? C21 C24 1.525(4) . ? C21 C22 1.528(3) . ? C21 C23 1.530(3) . ? C31 C34 1.524(4) . ? C31 C33 1.523(4) . ? C31 C32 1.533(4) . ? C7 C8 1.480(5) . ? C7 C10 1.502(4) . ? C8 C9 1.488(4) . ? C1 C2 1.551(4) . ? C3 C4 1.542(4) . ? C5 C6 1.538(4) . ? C15 C17 1.548(3) . ? C16 C20 1.546(3) . ? C18 C19 1.543(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 P1 As1 P3 84.94(4) . . ? P1 As1 Li1 109.01(9) . . ? P3 As1 Li1 108.46(9) . . ? C11 P1 P2 101.60(8) . . ? C11 P1 As1 108.08(8) . . ? P2 P1 As1 88.85(4) . . ? C21 P2 P1 104.62(8) . . ? C21 P2 P3 105.17(9) . . ? P1 P2 P3 91.02(4) . . ? C31 P3 P2 102.72(8) . . ? C31 P3 As1 107.38(8) . . ? P2 P3 As1 88.76(4) . . ? C5 N1 C3 108.1(2) . . ? C5 N1 C1 109.3(2) . . ? C3 N1 C1 107.6(2) . . ? C2 N2 C6 107.8(2) . . ? C2 N2 C4 108.3(2) . . ? C6 N2 C4 107.4(2) . . ? C2 N2 Li1 112.4(2) . . ? C6 N2 Li1 116.5(2) . . ? C4 N2 Li1 104.1(2) . . ? C18 N3 C20 108.5(2) . . ? C18 N3 C17 109.0(2) . . ? C20 N3 C17 107.7(2) . . ? C15 N4 C16 107.5(2) . . ? C15 N4 C19 107.8(2) . . ? C16 N4 C19 107.5(2) . . ? C15 N4 Li1 121.9(2) . . ? C16 N4 Li1 103.4(2) . . ? C19 N4 Li1 107.9(2) . . ? C10 O1 C9 107.1(2) . . ? C10 O1 Li1 119.8(2) . . ? C9 O1 Li1 133.1(2) . . ? O1 Li1 N2 105.4(2) . . ? O1 Li1 N4 110.4(2) . . ? N2 Li1 N4 112.7(2) . . ? O1 Li1 As1 105.3(2) . . ? N2 Li1 As1 117.7(2) . . ? N4 Li1 As1 105.0(2) . . ? C12 C11 C14 109.6(2) . . ? C12 C11 C13 110.1(2) . . ? C14 C11 C13 109.2(2) . . ? C12 C11 P1 106.2(2) . . ? C14 C11 P1 115.2(2) . . ? C13 C11 P1 106.5(2) . . ? C24 C21 C22 108.9(2) . . ? C24 C21 C23 109.3(2) . . ? C22 C21 C23 109.9(2) . . ? C24 C21 P2 114.6(2) . . ? C22 C21 P2 106.7(2) . . ? C23 C21 P2 107.3(2) . . ? C34 C31 C33 109.4(2) . . ? C34 C31 C32 109.4(2) . . ? C33 C31 C32 110.4(2) . . ? C34 C31 P3 115.2(2) . . ? C33 C31 P3 107.0(2) . . ? C32 C31 P3 105.4(2) . . ? C8 C7 C10 105.8(3) . . ? C7 C8 C9 106.2(3) . . ? O1 C9 C8 106.1(3) . . ? O1 C10 C7 105.9(3) . . ? N1 C1 C2 110.5(2) . . ? N2 C2 C1 110.7(2) . . ? N1 C3 C4 111.3(2) . . ? N2 C4 C3 110.3(2) . . ? N1 C5 C6 111.6(2) . . ? N2 C6 C5 110.3(2) . . ? N4 C15 C17 111.1(2) . . ? N4 C16 C20 111.0(2) . . ? N3 C17 C15 110.6(2) . . ? N3 C18 C19 110.8(2) . . ? N4 C19 C18 111.1(2) . . ? N3 C20 C16 110.8(2) . . ? _refine_diff_density_max 0.398 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.115 data_dw9912 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.50 H73 As Li N2 O P3' _chemical_formula_weight 814.81 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' 'P' 'P' 0.1023 0.0942 '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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.518(6) _cell_length_b 17.347(4) _cell_length_c 11.166(4) _cell_angle_alpha 100.07(2) _cell_angle_beta 112.31(3) _cell_angle_gamma 79.90(3) _cell_volume 2192.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.918 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7702 _exptl_absorpt_correction_T_max 0.8376 _exptl_absorpt_process_details ? _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_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 10544 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10082 _reflns_number_gt 7622 _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^)+(0.0540P)^2^+2.2734P] 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 10082 _refine_ls_number_parameters 468 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 1.151 _refine_ls_shift/su_mean 0.006 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 0.17787(3) 0.337546(19) 0.69772(3) 0.03015(10) Uani 1 1 d . . . P1 P 0.23964(6) 0.20801(4) 0.75364(7) 0.02047(15) Uani 1 1 d . . . C1 C 0.0842(5) 0.3118(3) 0.2269(4) 0.0795(16) Uani 1 1 d . . . H1A H 0.0445 0.2754 0.1516 0.119 Uiso 1 1 calc R . . H1B H 0.1312 0.3416 0.2030 0.119 Uiso 1 1 calc R . . H1C H 0.0263 0.3484 0.2544 0.119 Uiso 1 1 calc R . . C2 C 0.0885(6) 0.2190(4) 0.3584(5) 0.099(2) Uani 1 1 d . . . H2A H 0.0471 0.1871 0.2776 0.148 Uiso 1 1 calc R . . H2B H 0.0321 0.2527 0.3919 0.148 Uiso 1 1 calc R . . H2C H 0.1390 0.1841 0.4233 0.148 Uiso 1 1 calc R . . C3 C 0.2512(5) 0.2202(5) 0.2944(7) 0.134(3) Uani 1 1 d . . . H3A H 0.2307 0.1656 0.2687 0.160 Uiso 1 1 calc R . . H3B H 0.2484 0.2394 0.2147 0.160 Uiso 1 1 calc R . . C4 C 0.3615(5) 0.2158(4) 0.3752(7) 0.117(3) Uani 1 1 d . . . H4A H 0.4099 0.2077 0.3205 0.140 Uiso 1 1 calc R . . H4B H 0.3774 0.1670 0.4170 0.140 Uiso 1 1 calc R . . C5 C 0.4765(5) 0.2429(4) 0.5974(5) 0.0855(17) Uani 1 1 d . . . H5A H 0.5482 0.2141 0.5882 0.128 Uiso 1 1 calc R . . H5B H 0.4330 0.2065 0.6133 0.128 Uiso 1 1 calc R . . H5C H 0.4959 0.2847 0.6709 0.128 Uiso 1 1 calc R . . C6 C 0.4776(5) 0.3220(3) 0.4469(5) 0.0696(14) Uani 1 1 d . . . H6A H 0.5451 0.2868 0.4375 0.104 Uiso 1 1 calc R . . H6B H 0.5041 0.3647 0.5170 0.104 Uiso 1 1 calc R . . H6C H 0.4323 0.3442 0.3649 0.104 Uiso 1 1 calc R . . O1 O 0.2400(2) 0.45216(14) 0.4816(2) 0.0403(6) Uani 1 1 d . . . N1 N 0.1585(3) 0.2676(2) 0.3327(3) 0.0480(8) Uani 1 1 d . . . N2 N 0.4055(3) 0.27781(19) 0.4781(3) 0.0442(7) Uani 1 1 d . . . Li1 Li 0.2512(5) 0.3389(4) 0.5031(6) 0.0413(13) Uani 1 1 d . . . P2 P 0.33317(7) 0.26139(4) 0.95739(7) 0.02404(16) Uani 1 1 d . . . C20 C 0.4850(3) 0.20658(16) 1.0092(3) 0.0267(6) Uani 1 1 d . . . C21 C 0.5645(3) 0.25632(18) 1.1253(3) 0.0334(7) Uani 1 1 d . . . H21A H 0.5314 0.2693 1.1950 0.040 Uiso 1 1 calc R . . H21B H 0.5697 0.3063 1.0977 0.040 Uiso 1 1 calc R . . C22 C 0.5385(3) 0.18700(18) 0.9023(3) 0.0283(6) Uani 1 1 d . . . H22A H 0.4879 0.1550 0.8263 0.034 Uiso 1 1 calc R . . H22B H 0.5439 0.2364 0.8732 0.034 Uiso 1 1 calc R . . C23 C 0.4779(3) 0.12910(17) 1.0535(3) 0.0310(7) Uani 1 1 d . . . H23A H 0.4271 0.0963 0.9790 0.037 Uiso 1 1 calc R . . H23B H 0.4436 0.1408 1.1223 0.037 Uiso 1 1 calc R . . C24 C 0.6776(3) 0.1340(2) 1.2219(3) 0.0429(8) Uani 1 1 d . . . H24A H 0.7559 0.1046 1.2577 0.051 Uiso 1 1 calc R . . H24B H 0.6443 0.1464 1.2915 0.051 Uiso 1 1 calc R . . C25 C 0.6003(3) 0.08363(19) 1.1067(3) 0.0356(7) Uani 1 1 d . . . H25A H 0.5949 0.0336 1.1357 0.043 Uiso 1 1 calc R . . C26 C 0.6513(3) 0.06423(18) 0.9991(3) 0.0360(7) Uani 1 1 d . . . H26A H 0.6008 0.0314 0.9243 0.043 Uiso 1 1 calc R . . H26B H 0.7294 0.0340 1.0319 0.043 Uiso 1 1 calc R . . C27 C 0.6602(3) 0.14109(19) 0.9549(3) 0.0342(7) Uani 1 1 d . . . H27A H 0.6939 0.1285 0.8846 0.041 Uiso 1 1 calc R . . C28 C 0.7390(3) 0.1907(2) 1.0710(4) 0.0417(8) Uani 1 1 d . . . H28A H 0.7468 0.2399 1.0432 0.050 Uiso 1 1 calc R . . H28B H 0.8174 0.1610 1.1050 0.050 Uiso 1 1 calc R . . C29 C 0.6868(3) 0.21055(19) 1.1779(3) 0.0403(8) Uani 1 1 d . . . H29A H 0.7380 0.2434 1.2537 0.048 Uiso 1 1 calc R . . P3 P 0.34582(6) 0.36713(4) 0.87727(7) 0.01938(15) Uani 1 1 d . . . C41 C 0.3271(3) 0.4981(2) 0.5762(4) 0.0472(9) Uani 1 1 d . . . H41A H 0.3947 0.4944 0.5491 0.057 Uiso 1 1 calc R . . H41B H 0.3543 0.4787 0.6625 0.057 Uiso 1 1 calc R . . C30 C 0.2943(2) 0.45198(16) 0.9831(3) 0.0227(6) Uani 1 1 d . . . C31 C 0.1959(3) 0.43861(17) 1.0245(3) 0.0295(6) Uani 1 1 d . . . H31A H 0.2219 0.3940 1.0774 0.035 Uiso 1 1 calc R . . H31B H 0.1276 0.4252 0.9462 0.035 Uiso 1 1 calc R . . C32 C 0.2516(3) 0.52181(17) 0.9020(3) 0.0297(6) Uani 1 1 d . . . H32A H 0.3141 0.5312 0.8743 0.036 Uiso 1 1 calc R . . H32B H 0.1839 0.5090 0.8227 0.036 Uiso 1 1 calc R . . C33 C 0.3987(3) 0.47338(18) 1.1052(3) 0.0307(7) Uani 1 1 d . . . H33A H 0.4266 0.4293 1.1594 0.037 Uiso 1 1 calc R . . H33B H 0.4628 0.4819 1.0795 0.037 Uiso 1 1 calc R . . C34 C 0.2666(3) 0.5343(2) 1.2253(3) 0.0441(9) Uani 1 1 d . . . H34A H 0.2937 0.4907 1.2804 0.053 Uiso 1 1 calc R . . H34B H 0.2445 0.5824 1.2771 0.053 Uiso 1 1 calc R . . C35 C 0.1615(3) 0.51358(19) 1.1047(3) 0.0361(7) Uani 1 1 d . . . H35A H 0.0979 0.5043 1.1320 0.043 Uiso 1 1 calc R . . C36 C 0.1191(3) 0.58186(18) 1.0215(4) 0.0372(8) Uani 1 1 d . . . H36A H 0.0954 0.6301 1.0720 0.045 Uiso 1 1 calc R . . H36B H 0.0507 0.5689 0.9430 0.045 Uiso 1 1 calc R . . C37 C 0.2170(3) 0.59635(18) 0.9811(3) 0.0343(7) Uani 1 1 d . . . H37A H 0.1894 0.6409 0.9265 0.041 Uiso 1 1 calc R . . C38 C 0.3217(3) 0.61671(19) 1.1007(3) 0.0363(7) Uani 1 1 d . . . H38A H 0.3002 0.6653 1.1521 0.044 Uiso 1 1 calc R . . H38B H 0.3845 0.6265 1.0740 0.044 Uiso 1 1 calc R . . C39 C 0.3645(3) 0.5482(2) 1.1843(3) 0.0356(7) Uani 1 1 d . . . H39A H 0.4333 0.5616 1.2637 0.043 Uiso 1 1 calc R . . C10 C 0.1096(3) 0.17221(17) 0.7669(3) 0.0281(6) Uani 1 1 d . . . C11 C 0.0438(3) 0.22883(19) 0.8447(4) 0.0382(8) Uani 1 1 d . . . H11A H 0.0155 0.2792 0.8061 0.046 Uiso 1 1 calc R . . H11B H 0.0969 0.2403 0.9358 0.046 Uiso 1 1 calc R . . C12 C 0.0260(3) 0.1542(2) 0.6272(3) 0.0447(9) Uani 1 1 d . . . H12A H 0.0677 0.1178 0.5762 0.054 Uiso 1 1 calc R . . H12B H -0.0033 0.2036 0.5859 0.054 Uiso 1 1 calc R . . C13 C 0.1527(3) 0.09554(19) 0.8300(4) 0.0393(8) Uani 1 1 d . . . H13A H 0.2062 0.1067 0.9211 0.047 Uiso 1 1 calc R . . H13B H 0.1962 0.0582 0.7819 0.047 Uiso 1 1 calc R . . C14 C 0.0497(3) 0.0582(2) 0.8281(4) 0.0455(9) Uani 1 1 d . . . H14A H 0.0792 0.0081 0.8692 0.055 Uiso 1 1 calc R . . C15 C -0.0314(4) 0.0403(2) 0.6887(5) 0.0568(11) Uani 1 1 d . . . H15A H -0.0973 0.0153 0.6872 0.068 Uiso 1 1 calc R . . H15B H 0.0108 0.0031 0.6391 0.068 Uiso 1 1 calc R . . C16 C -0.0771(3) 0.1165(3) 0.6259(4) 0.0534(10) Uani 1 1 d . . . H16A H -0.1311 0.1048 0.5340 0.064 Uiso 1 1 calc R . . C17 C -0.1416(3) 0.1744(3) 0.7033(5) 0.0565(11) Uani 1 1 d . . . H17A H -0.1710 0.2240 0.6626 0.068 Uiso 1 1 calc R . . H17B H -0.2091 0.1513 0.7021 0.068 Uiso 1 1 calc R . . C18 C -0.0600(3) 0.1916(2) 0.8426(4) 0.0444(9) Uani 1 1 d . . . H18A H -0.1026 0.2292 0.8927 0.053 Uiso 1 1 calc R . . C19 C -0.0160(3) 0.1154(2) 0.9051(4) 0.0466(9) Uani 1 1 d . . . H19A H -0.0824 0.0915 0.9047 0.056 Uiso 1 1 calc R . . H19B H 0.0364 0.1265 0.9967 0.056 Uiso 1 1 calc R . . C42 C 0.2707(4) 0.5814(2) 0.5829(4) 0.0567(11) Uani 1 1 d . . . H42A H 0.2824 0.6108 0.5213 0.068 Uiso 1 1 calc R . . H42B H 0.3017 0.6092 0.6722 0.068 Uiso 1 1 calc R . . C43 C 0.1448(4) 0.5721(3) 0.5449(4) 0.0608(12) Uani 1 1 d . . . H43A H 0.1271 0.5656 0.6215 0.073 Uiso 1 1 calc R . . H43B H 0.0941 0.6182 0.5040 0.073 Uiso 1 1 calc R . . C44 C 0.1292(3) 0.4993(3) 0.4497(4) 0.0535(10) Uani 1 1 d . . . H44A H 0.0707 0.4702 0.4563 0.064 Uiso 1 1 calc R . . H44B H 0.1026 0.5130 0.3596 0.064 Uiso 1 1 calc R . . C1T C -0.6660(12) 0.0039(9) 0.5411(12) 0.090(5) Uiso 0.50 1 d PD A -1 H1TA H -0.6493 0.0118 0.6352 0.135 Uiso 0.50 1 calc PR A -1 H1TB H -0.6986 -0.0460 0.5035 0.135 Uiso 0.50 1 calc PR A -1 H1TC H -0.7221 0.0475 0.5005 0.135 Uiso 0.50 1 calc PR A -1 C2T C -0.5597(7) 0.0018(6) 0.5174(9) 0.0612(10) Uiso 0.50 1 d PG A -1 C3T C -0.4573(8) 0.0070(9) 0.6252(9) 0.0612(10) Uiso 0.50 1 d PGD A -1 H3TA H -0.4611 0.0139 0.7098 0.073 Uiso 0.50 1 calc PR A -1 C4T C -0.3530(8) 0.0028(5) 0.6144(9) 0.0612(10) Uiso 0.50 1 d PG A -1 H4TA H -0.2864 0.0089 0.6916 0.073 Uiso 0.50 1 calc PR A -1 C5T C -0.3390(10) -0.0100(7) 0.4958(12) 0.0612(10) Uiso 0.50 1 d PG A -1 H5TA H -0.2652 -0.0162 0.4872 0.073 Uiso 0.50 1 calc PR A -1 C6T C -0.4443(8) -0.0129(5) 0.3885(10) 0.0612(10) Uiso 0.50 1 d PG A -1 H6TA H -0.4413 -0.0176 0.3038 0.073 Uiso 0.50 1 calc PR A -1 C7T C -0.5497(10) -0.0096(9) 0.3983(11) 0.0612(10) Uiso 0.50 1 d PGD A -1 H7TA H -0.6168 -0.0152 0.3216 0.073 Uiso 0.50 1 calc PR A -1 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 0.03430(18) 0.03121(17) 0.02384(16) 0.00481(12) 0.00824(13) -0.00469(13) P1 0.0203(3) 0.0191(3) 0.0235(3) -0.0006(3) 0.0102(3) -0.0035(3) C1 0.108(4) 0.083(4) 0.036(2) 0.013(2) 0.009(3) -0.018(3) C2 0.151(6) 0.109(5) 0.054(3) -0.011(3) 0.035(3) -0.086(5) C3 0.058(3) 0.157(7) 0.111(5) -0.089(5) 0.004(3) 0.010(4) C4 0.057(3) 0.118(5) 0.126(5) -0.080(4) 0.020(3) -0.008(3) C5 0.097(4) 0.095(4) 0.072(3) 0.043(3) 0.037(3) 0.017(3) C6 0.088(4) 0.064(3) 0.082(3) 0.013(3) 0.060(3) -0.002(3) O1 0.0395(13) 0.0420(13) 0.0405(13) 0.0071(11) 0.0137(11) -0.0067(11) N1 0.0466(18) 0.062(2) 0.0315(15) -0.0011(14) 0.0108(14) -0.0097(16) N2 0.0441(18) 0.0509(18) 0.0361(16) 0.0004(13) 0.0127(14) -0.0106(14) Li1 0.047(3) 0.051(4) 0.029(3) 0.002(2) 0.015(3) -0.015(3) P2 0.0259(4) 0.0213(3) 0.0260(4) 0.0028(3) 0.0111(3) -0.0017(3) C20 0.0289(15) 0.0201(13) 0.0299(15) 0.0048(11) 0.0104(12) 0.0016(11) C21 0.0340(17) 0.0258(15) 0.0327(16) 0.0006(12) 0.0050(14) -0.0032(13) C22 0.0289(15) 0.0271(15) 0.0312(15) 0.0079(12) 0.0131(13) 0.0006(12) C23 0.0337(17) 0.0262(15) 0.0358(17) 0.0076(12) 0.0141(14) -0.0028(12) C24 0.045(2) 0.0399(19) 0.0335(18) 0.0121(15) 0.0032(16) 0.0045(16) C25 0.0392(18) 0.0257(15) 0.0422(18) 0.0143(13) 0.0125(15) 0.0006(13) C26 0.0325(17) 0.0247(15) 0.047(2) 0.0059(14) 0.0107(15) 0.0008(13) C27 0.0304(16) 0.0306(16) 0.0453(19) 0.0073(14) 0.0185(15) 0.0013(13) C28 0.0265(16) 0.0324(17) 0.063(2) 0.0120(16) 0.0099(16) -0.0018(13) C29 0.0345(18) 0.0291(16) 0.0418(19) 0.0021(14) -0.0029(15) -0.0046(14) P3 0.0202(3) 0.0185(3) 0.0211(3) 0.0024(3) 0.0100(3) -0.0007(3) C41 0.040(2) 0.058(2) 0.041(2) 0.0014(17) 0.0121(17) -0.0072(17) C30 0.0226(13) 0.0221(13) 0.0241(14) 0.0032(11) 0.0086(11) -0.0031(11) C31 0.0335(16) 0.0226(14) 0.0397(17) 0.0014(12) 0.0215(14) -0.0056(12) C32 0.0320(16) 0.0261(15) 0.0317(16) 0.0075(12) 0.0104(13) -0.0038(12) C33 0.0246(15) 0.0327(16) 0.0295(15) 0.0013(12) 0.0062(12) -0.0001(12) C34 0.061(2) 0.0380(19) 0.0365(18) -0.0020(15) 0.0265(18) -0.0009(17) C35 0.0378(18) 0.0323(17) 0.048(2) -0.0023(14) 0.0279(16) -0.0070(14) C36 0.0280(16) 0.0257(15) 0.055(2) -0.0031(14) 0.0164(15) -0.0016(12) C37 0.0358(17) 0.0207(14) 0.0455(19) 0.0062(13) 0.0135(15) -0.0015(12) C38 0.0331(17) 0.0284(16) 0.048(2) -0.0040(14) 0.0166(15) -0.0086(13) C39 0.0303(16) 0.0385(18) 0.0300(16) -0.0030(13) 0.0055(13) -0.0033(13) C10 0.0270(15) 0.0251(14) 0.0308(15) 0.0006(12) 0.0103(13) -0.0023(11) C11 0.0397(19) 0.0287(16) 0.053(2) -0.0025(15) 0.0267(17) -0.0059(14) C12 0.039(2) 0.058(2) 0.0365(19) 0.0027(17) 0.0102(16) -0.0155(17) C13 0.0320(17) 0.0319(17) 0.055(2) 0.0104(15) 0.0159(16) -0.0022(14) C14 0.0360(19) 0.0320(18) 0.072(3) 0.0171(17) 0.0187(18) -0.0047(14) C15 0.048(2) 0.044(2) 0.083(3) -0.012(2) 0.030(2) -0.0224(18) C16 0.039(2) 0.071(3) 0.044(2) 0.0024(19) 0.0015(17) -0.0228(19) C17 0.0250(18) 0.064(3) 0.082(3) 0.030(2) 0.0122(19) -0.0029(17) C18 0.040(2) 0.0359(18) 0.068(3) 0.0053(17) 0.0328(19) -0.0025(15) C19 0.040(2) 0.052(2) 0.057(2) 0.0136(18) 0.0211(18) -0.0128(17) C42 0.069(3) 0.047(2) 0.049(2) -0.0007(18) 0.016(2) -0.012(2) C43 0.055(3) 0.065(3) 0.054(3) 0.008(2) 0.018(2) 0.012(2) C44 0.039(2) 0.065(3) 0.059(3) 0.011(2) 0.0186(19) -0.0055(19) _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 P3 2.3498(14) . ? As1 P1 2.3562(10) . ? As1 Li1 2.666(6) . ? P1 C10 1.905(3) . ? P1 P2 2.2417(14) . ? C1 N1 1.442(5) . ? C2 N1 1.449(6) . ? C3 C4 1.330(7) . ? C3 N1 1.459(6) . ? C4 N2 1.441(6) . ? C5 N2 1.457(6) . ? C6 N2 1.448(5) . ? O1 C44 1.431(5) . ? O1 C41 1.440(4) . ? O1 Li1 1.994(7) . ? N1 Li1 2.121(7) . ? N2 Li1 2.127(7) . ? P2 C20 1.891(3) . ? P2 P3 2.2302(11) . ? C20 C21 1.531(4) . ? C20 C23 1.539(4) . ? C20 C22 1.541(4) . ? C21 C29 1.541(5) . ? C22 C27 1.536(4) . ? C23 C25 1.540(4) . ? C24 C25 1.521(5) . ? C24 C29 1.531(5) . ? C25 C26 1.526(5) . ? C26 C27 1.535(4) . ? C27 C28 1.527(5) . ? C28 C29 1.530(5) . ? P3 C30 1.902(3) . ? C41 C42 1.496(6) . ? C30 C33 1.531(4) . ? C30 C31 1.535(4) . ? C30 C32 1.537(4) . ? C31 C35 1.538(4) . ? C32 C37 1.528(4) . ? C33 C39 1.529(4) . ? C34 C35 1.524(5) . ? C34 C39 1.529(5) . ? C35 C36 1.529(5) . ? C36 C37 1.529(5) . ? C37 C38 1.514(5) . ? C38 C39 1.535(5) . ? C10 C12 1.527(5) . ? C10 C13 1.531(4) . ? C10 C11 1.535(4) . ? C11 C18 1.539(5) . ? C12 C16 1.540(5) . ? C13 C14 1.534(5) . ? C14 C15 1.514(6) . ? C14 C19 1.534(5) . ? C15 C16 1.523(6) . ? C16 C17 1.533(6) . ? C17 C18 1.513(6) . ? C18 C19 1.521(5) . ? C42 C43 1.499(6) . ? C43 C44 1.490(6) . ? C1T C2T 1.444(16) . ? C2T C3T 1.3900 . ? C2T C7T 1.360(13) . ? C3T C4T 1.345(15) . ? C4T C5T 1.376(15) . ? C5T C6T 1.406(15) . ? C6T C7T 1.355(14) . ? 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 P3 As1 P1 83.67(4) . . ? P3 As1 Li1 100.13(14) . . ? P1 As1 Li1 103.78(14) . . ? C10 P1 P2 103.17(10) . . ? C10 P1 As1 106.23(10) . . ? P2 P1 As1 87.36(4) . . ? C4 C3 N1 121.6(5) . . ? C3 C4 N2 122.3(5) . . ? C44 O1 C41 109.0(3) . . ? C44 O1 Li1 119.4(3) . . ? C41 O1 Li1 117.8(3) . . ? C1 N1 C2 108.3(4) . . ? C1 N1 C3 108.2(5) . . ? C2 N1 C3 111.7(5) . . ? C1 N1 Li1 113.8(3) . . ? C2 N1 Li1 112.0(3) . . ? C3 N1 Li1 102.8(3) . . ? C4 N2 C6 111.3(4) . . ? C4 N2 C5 109.0(5) . . ? C6 N2 C5 108.1(4) . . ? C4 N2 Li1 102.3(3) . . ? C6 N2 Li1 117.9(3) . . ? C5 N2 Li1 107.8(3) . . ? O1 Li1 N1 115.0(3) . . ? O1 Li1 N2 109.0(3) . . ? N1 Li1 N2 86.7(3) . . ? O1 Li1 As1 106.1(3) . . ? N1 Li1 As1 111.6(3) . . ? N2 Li1 As1 127.9(3) . . ? C20 P2 P3 105.10(10) . . ? C20 P2 P1 105.89(10) . . ? P3 P2 P1 89.16(5) . . ? C21 C20 C23 109.0(3) . . ? C21 C20 C22 108.6(3) . . ? C23 C20 C22 108.8(2) . . ? C21 C20 P2 108.4(2) . . ? C23 C20 P2 106.8(2) . . ? C22 C20 P2 115.0(2) . . ? C20 C21 C29 110.0(3) . . ? C27 C22 C20 110.1(3) . . ? C20 C23 C25 110.0(3) . . ? C25 C24 C29 109.6(3) . . ? C24 C25 C26 110.0(3) . . ? C24 C25 C23 109.4(3) . . ? C26 C25 C23 109.2(3) . . ? C25 C26 C27 109.4(3) . . ? C28 C27 C26 109.1(3) . . ? C28 C27 C22 109.8(3) . . ? C26 C27 C22 109.5(3) . . ? C27 C28 C29 109.4(3) . . ? C28 C29 C24 109.2(3) . . ? C28 C29 C21 110.0(3) . . ? C24 C29 C21 109.1(3) . . ? C30 P3 P2 102.74(9) . . ? C30 P3 As1 105.30(10) . . ? P2 P3 As1 87.79(5) . . ? O1 C41 C42 106.5(3) . . ? C33 C30 C31 109.0(2) . . ? C33 C30 C32 108.4(2) . . ? C31 C30 C32 108.4(2) . . ? C33 C30 P3 108.64(19) . . ? C31 C30 P3 116.50(19) . . ? C32 C30 P3 105.56(19) . . ? C30 C31 C35 109.9(2) . . ? C37 C32 C30 110.8(3) . . ? C39 C33 C30 110.3(2) . . ? C35 C34 C39 109.8(3) . . ? C34 C35 C36 109.3(3) . . ? C34 C35 C31 109.7(3) . . ? C36 C35 C31 109.4(3) . . ? C35 C36 C37 109.3(3) . . ? C38 C37 C32 109.3(3) . . ? C38 C37 C36 110.1(3) . . ? C32 C37 C36 109.2(3) . . ? C37 C38 C39 109.4(3) . . ? C34 C39 C33 109.3(3) . . ? C34 C39 C38 109.0(3) . . ? C33 C39 C38 109.7(3) . . ? C12 C10 C13 109.0(3) . . ? C12 C10 C11 109.0(3) . . ? C13 C10 C11 108.1(3) . . ? C12 C10 P1 106.0(2) . . ? C13 C10 P1 107.7(2) . . ? C11 C10 P1 116.8(2) . . ? C10 C11 C18 110.0(3) . . ? C10 C12 C16 110.4(3) . . ? C10 C13 C14 110.3(3) . . ? C15 C14 C19 109.7(3) . . ? C15 C14 C13 109.6(3) . . ? C19 C14 C13 109.5(3) . . ? C14 C15 C16 109.6(3) . . ? C15 C16 C17 109.8(4) . . ? C15 C16 C12 109.3(3) . . ? C17 C16 C12 108.7(3) . . ? C18 C17 C16 109.6(3) . . ? C17 C18 C19 109.6(3) . . ? C17 C18 C11 109.8(3) . . ? C19 C18 C11 109.6(3) . . ? C18 C19 C14 109.1(3) . . ? C41 C42 C43 103.1(3) . . ? C44 C43 C42 103.6(3) . . ? O1 C44 C43 106.8(3) . . ? C3T C2T C7T 116.6(10) . . ? C3T C2T C1T 117.6(9) . . ? C7T C2T C1T 125.7(7) . . ? C2T C3T C4T 122.6(10) . . ? C5T C4T C3T 122.5(10) . . ? C4T C5T C6T 113.6(10) . . ? C5T C6T C7T 124.2(11) . . ? C6T C7T C2T 120.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.825 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.074