Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bashall, Alan' 'Hopkins, Alexander D.' 'Kidd, Sara J.' 'McPartlin, M.' 'Steiner, Alexander' 'Wolf, Robert' 'Woods, Anthony D.' 'Wright, Dominic' _publ_contact_author_name 'Dr Dominic Wright' _publ_contact_author_address ; Chemistry Cambridge University Lensfield Rd Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'DSW1000@CAM.AC.UK' _publ_section_title ; Synthesis, Structures and Coordination behaviour of [As(NR)3]3- trianions ; ##################################### ## denoted 1.toluene in the text ## ##################################### data_dw0055 _database_code_CSD 169732 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C24 H54 As2 Li6 N6)0.5, (C24 H60 Li6 N6)0.5, (C7 H8) ; _chemical_formula_sum 'C31 H65 As Li6 N6' _chemical_formula_weight 638.45 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' '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' 'x, x-y, z' '-x+y, y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z' '-x, -x+y, -z' 'x-y, -y, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' 'y+2/3, x+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 'y+1/3, x+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' _cell_length_a 16.0568(12) _cell_length_b 16.0568(12) _cell_length_c 13.5862(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3033.5(4) _cell_formula_units_Z 3 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2822 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 2923 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 23.00 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 531 _reflns_number_gt 488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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. Complex disorder - each cluster is EITHER: (i) [{As(N(t-butyl))~3~}~2~Li~6~] (ii) [{NH(t-butyl))~3~}~2~Li~6~] (iii) [{As(N(t-butyl))~3~}{NH(t-butyl))~3~}Li~6~] i.e. three H can replace As at either end of the cluster. The ratio of As-capped ends to NH-capped ends is 1:1 but it is not possible to distinguish between molecules (i)-(iii) on the basis of the X-ray evidence alone. The total cell contents are thus The H atom of the N-H group was located in a difference Fourier map and refined with the N-H distance restrained to 0.88(1) \%A and an isotropic displacement parameter constrained to be 1.2 times U~eq~ for N. ; _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^)+(0.0722P)^2^+7.4975P] 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 531 _refine_ls_number_parameters 46 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.328 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.044 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 0.0000 0.0000 0.33666(11) 0.0538(7) Uani 0.50 6 d SP . 1 Li1 Li 0.1402(7) 0.0701(4) 0.5483(8) 0.086(3) Uani 1 2 d S . . N1 N 0.1274(4) 0.06371(19) 0.4000(3) 0.0842(15) Uani 1 2 d SD . . H1 H 0.087(7) 0.043(4) 0.341(5) 0.101 Uiso 0.50 2 d SPD A 2 C1 C 0.2239(7) 0.1120(3) 0.3517(5) 0.108(2) Uani 1 2 d S . . C2 C 0.2972(5) 0.1486(3) 0.4336(7) 0.139(3) Uani 1 2 d S . . H2A H 0.3037 0.2084 0.4601 0.209 Uiso 0.50 1 calc PR . . H2B H 0.3594 0.1609 0.4080 0.209 Uiso 0.50 1 calc PR . . H2C H 0.2760 0.1003 0.4861 0.209 Uiso 0.50 1 calc PR . . C3 C 0.2379(6) 0.1969(5) 0.2877(4) 0.176(3) Uani 1 1 d . . . H3A H 0.1886 0.1736 0.2362 0.264 Uiso 1 1 calc R . . H3B H 0.3018 0.2274 0.2574 0.264 Uiso 1 1 calc R . . H3C H 0.2321 0.2439 0.3289 0.264 Uiso 1 1 calc R . . C100 C 0.0869(8) 0.0869(8) 0.0000 0.262(8) Uani 1 2 d S . . H100 H 0.1482 0.1482 0.0000 0.314 Uiso 0.83 2 d SP B 1 C107 C 0.1860 0.1860 0.0000 0.314 Uiso 0.17 2 d SP C 2 H10A H 0.2291 0.1836 0.0496 0.393 Uiso 0.08 1 calc PR C 2 H10B H 0.1740 0.2387 0.0155 0.393 Uiso 0.08 1 calc PR C 2 H10C H 0.2159 0.1967 -0.0651 0.393 Uiso 0.08 1 calc PR C 2 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 0.0560(8) 0.0560(8) 0.0492(10) 0.000 0.000 0.0280(4) Li1 0.082(6) 0.076(4) 0.100(6) -0.013(3) -0.026(5) 0.041(3) N1 0.091(4) 0.082(2) 0.083(3) -0.0127(14) -0.025(3) 0.0453(18) C1 0.149(7) 0.109(4) 0.079(4) 0.014(2) 0.027(4) 0.074(4) C2 0.074(5) 0.175(7) 0.135(7) 0.014(2) 0.029(5) 0.037(2) C3 0.281(10) 0.139(5) 0.118(4) 0.054(4) 0.069(5) 0.113(6) C100 0.139(7) 0.139(7) 0.52(2) 0.003(5) -0.003(5) 0.080(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 N1 1.970(5) . ? As1 N1 1.970(5) 3 ? As1 N1 1.970(5) 2 ? As1 Li1 2.499(11) 21_556 ? As1 Li1 2.499(11) 20_556 ? As1 Li1 2.499(11) 19_556 ? As1 H1 1.21(10) . ? Li1 N1 1.995(8) 21_556 ? Li1 N1 1.995(8) 20_556 ? Li1 N1 2.022(11) . ? Li1 Li1 2.350(13) 20_556 ? Li1 Li1 2.350(13) 21_556 ? Li1 As1 2.499(11) 19_556 ? Li1 Li1 3.378(18) 3 ? Li1 Li1 3.378(18) 2 ? N1 C1 1.494(9) . ? N1 Li1 1.995(8) 20_556 ? N1 Li1 1.995(8) 21_556 ? N1 H1 0.981(10) . ? C1 C2 1.509(10) . ? C1 C3 1.537(6) 5 ? C1 C3 1.537(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C100 C100 1.395(12) 21 ? C100 C100 1.395(12) 20 ? C100 C107 1.591(12) . ? C100 H100 0.985(12) . ? C107 H100 0.6063 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? 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 N1 102.33(19) . 3 ? N1 As1 N1 102.33(19) . 2 ? N1 As1 N1 102.33(19) 3 2 ? N1 As1 Li1 51.37(8) . 21_556 ? N1 As1 Li1 115.4(3) 3 21_556 ? N1 As1 Li1 51.37(8) 2 21_556 ? N1 As1 Li1 51.37(8) . 20_556 ? N1 As1 Li1 51.37(8) 3 20_556 ? N1 As1 Li1 115.4(3) 2 20_556 ? Li1 As1 Li1 85.0(3) 21_556 20_556 ? N1 As1 Li1 115.4(3) . 19_556 ? N1 As1 Li1 51.37(8) 3 19_556 ? N1 As1 Li1 51.37(8) 2 19_556 ? Li1 As1 Li1 85.0(3) 21_556 19_556 ? Li1 As1 Li1 85.0(3) 20_556 19_556 ? N1 As1 H1 23(4) . . ? N1 As1 H1 115.4(18) 3 . ? N1 As1 H1 115.4(18) 2 . ? Li1 As1 H1 65(2) 21_556 . ? Li1 As1 H1 65(2) 20_556 . ? Li1 As1 H1 139(4) 19_556 . ? N1 Li1 N1 100.5(5) 21_556 20_556 ? N1 Li1 N1 107.7(4) 21_556 . ? N1 Li1 N1 107.7(4) 20_556 . ? N1 Li1 Li1 121.9(3) 21_556 20_556 ? N1 Li1 Li1 54.7(3) 20_556 20_556 ? N1 Li1 Li1 53.7(4) . 20_556 ? N1 Li1 Li1 54.7(3) 21_556 21_556 ? N1 Li1 Li1 121.9(3) 20_556 21_556 ? N1 Li1 Li1 53.7(4) . 21_556 ? Li1 Li1 Li1 91.9(6) 20_556 21_556 ? N1 Li1 As1 50.5(3) 21_556 19_556 ? N1 Li1 As1 50.5(3) 20_556 19_556 ? N1 Li1 As1 123.7(5) . 19_556 ? Li1 Li1 As1 91.5(3) 20_556 19_556 ? Li1 Li1 As1 91.5(3) 21_556 19_556 ? N1 Li1 Li1 85.6(3) 21_556 3 ? N1 Li1 Li1 32.2(3) 20_556 3 ? N1 Li1 Li1 85.6(3) . 3 ? Li1 Li1 Li1 44.1(3) 20_556 3 ? Li1 Li1 Li1 90.000(2) 21_556 3 ? As1 Li1 Li1 47.49(16) 19_556 3 ? N1 Li1 Li1 32.2(3) 21_556 2 ? N1 Li1 Li1 85.6(3) 20_556 2 ? N1 Li1 Li1 85.6(3) . 2 ? Li1 Li1 Li1 90.0 20_556 2 ? Li1 Li1 Li1 44.1(3) 21_556 2 ? As1 Li1 Li1 47.49(16) 19_556 2 ? Li1 Li1 Li1 60.000(1) 3 2 ? C1 N1 As1 128.0(4) . . ? C1 N1 Li1 120.9(3) . 20_556 ? As1 N1 Li1 78.2(3) . 20_556 ? C1 N1 Li1 120.9(3) . 21_556 ? As1 N1 Li1 78.2(3) . 21_556 ? Li1 N1 Li1 115.7(6) 20_556 21_556 ? C1 N1 Li1 111.0(5) . . ? As1 N1 Li1 121.0(4) . . ? Li1 N1 Li1 71.6(3) 20_556 . ? Li1 N1 Li1 71.6(3) 21_556 . ? C1 N1 H1 99(7) . . ? As1 N1 H1 29(7) . . ? Li1 N1 H1 93(4) 20_556 . ? Li1 N1 H1 93(4) 21_556 . ? Li1 N1 H1 150(7) . . ? N1 C1 C2 106.4(5) . . ? N1 C1 C3 111.2(5) . 5 ? C2 C1 C3 109.4(5) . 5 ? N1 C1 C3 111.2(5) . . ? C2 C1 C3 109.4(5) . . ? C3 C1 C3 109.2(6) 5 . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C100 C100 C100 120.000(1) 21 20 ? C100 C100 C107 120.0 21 . ? C100 C100 C107 120.0 20 . ? C100 C100 H100 120.0 21 . ? C100 C100 H100 120.0 20 . ? C107 C100 H100 0.0(5) . . ? C100 C107 H100 0.0(8) . . ? C100 C107 H10A 109.5 . . ? H100 C107 H10A 109.5 . . ? C100 C107 H10B 109.5 . . ? H100 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C100 C107 H10C 109.5 . . ? H100 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? #===END ############################# ## denoted 3 in the text ## ############################# data_dw0103 _database_code_CSD 169733 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H74 As2 Li6 N10 O6' _chemical_formula_sum 'C54 H74 As2 Li6 N10 O6' _chemical_formula_weight 1150.71 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.1001(5) _cell_length_b 12.9517(3) _cell_length_c 15.8827(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.239(2) _cell_angle_gamma 90.00 _cell_volume 2844.88(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10874 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 1.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 17280 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _reflns_number_total 6470 _reflns_number_gt 5280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0350P)^2^+1.1053P] 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 6470 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.527 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.060 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 0.093969(14) 0.597668(14) 0.134413(12) 0.02352(7) Uani 1 1 d . . . O1 O 0.21829(10) 0.46844(11) -0.08125(9) 0.0311(3) Uani 1 1 d . . . O2 O -0.15759(10) 0.73278(11) -0.05359(9) 0.0301(3) Uani 1 1 d . . . O3 O 0.01642(12) 0.27697(11) 0.17561(10) 0.0400(4) Uani 1 1 d . . . N1 N 0.15386(11) 0.55768(12) 0.04476(10) 0.0239(3) Uani 1 1 d . . . N2 N -0.00315(11) 0.66319(12) 0.05335(10) 0.0250(3) Uani 1 1 d . . . N3 N 0.03044(12) 0.47446(12) 0.14657(10) 0.0259(3) Uani 1 1 d . . . N4 N 0.24773(13) 0.75880(13) -0.07618(12) 0.0351(4) Uani 1 1 d . . . N5 N 0.18330(13) 0.85533(14) 0.06780(12) 0.0356(4) Uani 1 1 d . . . Li1 Li 0.0857(2) 0.4829(3) -0.0600(2) 0.0283(7) Uani 1 1 d . . . Li2 Li 0.1457(3) 0.7085(3) 0.0010(2) 0.0342(8) Uani 1 1 d . . . Li3 Li 0.0553(3) 0.3583(3) 0.0744(2) 0.0326(8) Uani 1 1 d . . . C1 C 0.24474(13) 0.51357(14) 0.06538(12) 0.0241(4) Uani 1 1 d . . . C2 C 0.28246(14) 0.46629(15) -0.00234(13) 0.0279(4) Uani 1 1 d . . . C3 C 0.37400(16) 0.42471(17) 0.00922(16) 0.0375(5) Uani 1 1 d . . . H3 H 0.3969 0.3959 -0.0381 0.045 Uiso 1 1 calc R . . C4 C 0.43289(17) 0.42513(18) 0.09072(17) 0.0437(6) Uani 1 1 d . . . H4 H 0.4964 0.3975 0.0992 0.052 Uiso 1 1 calc R . . C5 C 0.39806(16) 0.46602(17) 0.15882(15) 0.0393(5) Uani 1 1 d . . . H5 H 0.4372 0.4647 0.2147 0.047 Uiso 1 1 calc R . . C6 C 0.30571(14) 0.50932(15) 0.14642(14) 0.0311(4) Uani 1 1 d . . . H6 H 0.2834 0.5368 0.1945 0.037 Uiso 1 1 calc R . . C7 C 0.24862(18) 0.42291(18) -0.15379(14) 0.0389(5) Uani 1 1 d . . . H7A H 0.3075 0.4573 -0.1634 0.058 Uiso 1 1 calc R . . H7B H 0.1974 0.4309 -0.2048 0.058 Uiso 1 1 calc R . . H7C H 0.2618 0.3493 -0.1428 0.058 Uiso 1 1 calc R . . C8 C -0.06253(14) 0.73221(13) 0.08595(12) 0.0240(4) Uani 1 1 d . . . C9 C -0.14710(14) 0.76930(14) 0.02985(13) 0.0258(4) Uani 1 1 d . . . C10 C -0.21302(15) 0.83434(15) 0.05619(14) 0.0317(5) Uani 1 1 d . . . H10 H -0.2696 0.8547 0.0168 0.038 Uiso 1 1 calc R . . C11 C -0.19692(16) 0.87049(16) 0.14085(15) 0.0344(5) Uani 1 1 d . . . H11 H -0.2420 0.9154 0.1594 0.041 Uiso 1 1 calc R . . C12 C -0.11437(15) 0.83962(15) 0.19675(14) 0.0326(5) Uani 1 1 d . . . H12 H -0.1017 0.8652 0.2539 0.039 Uiso 1 1 calc R . . C13 C -0.04918(15) 0.77137(15) 0.17059(13) 0.0278(4) Uani 1 1 d . . . H13 H 0.0062 0.7504 0.2111 0.033 Uiso 1 1 calc R . . C14 C -0.24188(16) 0.76264(18) -0.11450(14) 0.0383(5) Uani 1 1 d . . . H14A H -0.2405 0.7304 -0.1701 0.057 Uiso 1 1 calc R . . H14B H -0.2430 0.8379 -0.1209 0.057 Uiso 1 1 calc R . . H14C H -0.2999 0.7401 -0.0942 0.057 Uiso 1 1 calc R . . C15 C 0.01509(14) 0.44693(16) 0.22693(12) 0.0271(4) Uani 1 1 d . . . C16 C 0.00654(15) 0.34058(17) 0.24434(14) 0.0332(5) Uani 1 1 d . . . C17 C -0.01255(17) 0.3036(2) 0.32103(15) 0.0435(6) Uani 1 1 d . . . H17 H -0.0181 0.2314 0.3296 0.052 Uiso 1 1 calc R . . C18 C -0.02371(17) 0.3729(2) 0.38594(15) 0.0470(6) Uani 1 1 d . . . H18 H -0.0378 0.3485 0.4385 0.056 Uiso 1 1 calc R . . C19 C -0.01391(17) 0.4765(2) 0.37243(14) 0.0445(6) Uani 1 1 d . . . H19 H -0.0198 0.5239 0.4167 0.053 Uiso 1 1 calc R . . C20 C 0.00454(16) 0.51343(18) 0.29509(14) 0.0370(5) Uani 1 1 d . . . H20 H 0.0103 0.5858 0.2878 0.044 Uiso 1 1 calc R . . C21 C 0.0354(2) 0.16976(18) 0.19411(19) 0.0534(7) Uani 1 1 d . . . H21A H -0.0228 0.1369 0.2069 0.080 Uiso 1 1 calc R . . H21B H 0.0884 0.1631 0.2438 0.080 Uiso 1 1 calc R . . H21C H 0.0534 0.1360 0.1443 0.080 Uiso 1 1 calc R . . C31 C 0.25524(17) 0.87105(17) -0.06089(16) 0.0412(6) Uani 1 1 d . . . H31A H 0.1967 0.9054 -0.0935 0.049 Uiso 1 1 calc R . . H31B H 0.3119 0.8982 -0.0820 0.049 Uiso 1 1 calc R . . C32 C 0.26557(17) 0.89590(17) 0.03292(17) 0.0410(6) Uani 1 1 d . . . H32A H 0.3264 0.8655 0.0650 0.049 Uiso 1 1 calc R . . H32B H 0.2693 0.9717 0.0409 0.049 Uiso 1 1 calc R . . C33 C 0.34064(18) 0.70989(18) -0.03968(18) 0.0485(6) Uani 1 1 d . . . H33A H 0.3929 0.7464 -0.0597 0.073 Uiso 1 1 calc R . . H33B H 0.3395 0.6376 -0.0581 0.073 Uiso 1 1 calc R . . H33C H 0.3514 0.7130 0.0231 0.073 Uiso 1 1 calc R . . C34 C 0.2267(2) 0.7397(2) -0.16826(17) 0.0552(7) Uani 1 1 d . . . H34A H 0.2799 0.7660 -0.1937 0.083 Uiso 1 1 calc R . . H34B H 0.1666 0.7749 -0.1942 0.083 Uiso 1 1 calc R . . H34C H 0.2195 0.6653 -0.1788 0.083 Uiso 1 1 calc R . . C35 C 0.2110(2) 0.8526(2) 0.16167(17) 0.0617(8) Uani 1 1 d . . . H35A H 0.2309 0.9217 0.1832 0.093 Uiso 1 1 calc R . . H35B H 0.2648 0.8043 0.1786 0.093 Uiso 1 1 calc R . . H35C H 0.1557 0.8299 0.1860 0.093 Uiso 1 1 calc R . . C36 C 0.09923(18) 0.92333(18) 0.0435(2) 0.0517(7) Uani 1 1 d . . . H36A H 0.1154 0.9925 0.0669 0.078 Uiso 1 1 calc R . . H36B H 0.0448 0.8957 0.0666 0.078 Uiso 1 1 calc R . . H36C H 0.0813 0.9272 -0.0192 0.078 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 0.02557(11) 0.02477(11) 0.02000(11) -0.00224(7) 0.00390(8) 0.00212(8) O1 0.0323(7) 0.0367(8) 0.0264(7) -0.0044(6) 0.0111(6) 0.0029(6) O2 0.0313(8) 0.0323(7) 0.0254(7) -0.0008(6) 0.0019(6) 0.0084(6) O3 0.0551(10) 0.0271(7) 0.0418(9) 0.0062(6) 0.0192(8) 0.0023(7) N1 0.0230(8) 0.0268(8) 0.0225(8) 0.0006(6) 0.0058(6) 0.0037(7) N2 0.0283(8) 0.0236(8) 0.0226(8) -0.0012(6) 0.0041(7) 0.0046(7) N3 0.0323(9) 0.0255(8) 0.0201(8) 0.0019(6) 0.0060(7) 0.0011(7) N4 0.0381(10) 0.0334(9) 0.0369(10) 0.0010(8) 0.0147(8) 0.0008(8) N5 0.0348(10) 0.0320(9) 0.0416(11) -0.0028(8) 0.0113(8) -0.0002(8) Li1 0.0273(17) 0.0288(16) 0.0279(18) -0.0004(14) 0.0034(14) 0.0017(14) Li2 0.040(2) 0.0306(17) 0.0331(19) 0.0041(15) 0.0089(16) 0.0019(15) Li3 0.039(2) 0.0325(18) 0.0256(18) -0.0011(14) 0.0051(15) 0.0078(16) C1 0.0248(9) 0.0207(9) 0.0278(10) -0.0003(7) 0.0075(8) -0.0007(7) C2 0.0288(10) 0.0270(10) 0.0291(10) -0.0011(8) 0.0086(8) -0.0004(8) C3 0.0327(12) 0.0392(12) 0.0443(13) -0.0047(10) 0.0163(10) 0.0032(9) C4 0.0268(11) 0.0477(13) 0.0562(16) -0.0041(11) 0.0073(11) 0.0089(10) C5 0.0325(11) 0.0410(12) 0.0406(13) -0.0045(10) -0.0020(10) 0.0049(10) C6 0.0281(10) 0.0332(11) 0.0310(11) -0.0041(9) 0.0034(9) 0.0031(9) C7 0.0469(14) 0.0439(12) 0.0304(12) -0.0062(10) 0.0184(10) 0.0007(10) C8 0.0262(10) 0.0192(9) 0.0279(10) 0.0004(7) 0.0088(8) -0.0009(7) C9 0.0308(10) 0.0221(9) 0.0253(10) 0.0009(7) 0.0073(8) -0.0009(8) C10 0.0310(11) 0.0297(10) 0.0353(12) 0.0036(9) 0.0083(9) 0.0059(9) C11 0.0381(12) 0.0290(10) 0.0399(12) -0.0008(9) 0.0169(10) 0.0068(9) C12 0.0390(12) 0.0296(10) 0.0319(11) -0.0064(9) 0.0137(9) -0.0016(9) C13 0.0278(10) 0.0293(10) 0.0267(10) -0.0028(8) 0.0064(8) -0.0005(8) C14 0.0358(12) 0.0401(12) 0.0347(12) 0.0002(10) -0.0035(10) 0.0057(10) C15 0.0223(9) 0.0362(11) 0.0223(10) 0.0038(8) 0.0030(8) 0.0056(8) C16 0.0314(11) 0.0395(11) 0.0300(11) 0.0057(9) 0.0091(9) 0.0023(9) C17 0.0390(13) 0.0527(14) 0.0398(13) 0.0172(11) 0.0102(10) -0.0019(11) C18 0.0355(12) 0.0810(18) 0.0268(12) 0.0161(12) 0.0120(10) 0.0032(13) C19 0.0381(12) 0.0709(17) 0.0260(11) 0.0019(11) 0.0099(10) 0.0144(12) C20 0.0390(12) 0.0455(13) 0.0268(11) 0.0004(9) 0.0070(9) 0.0099(10) C21 0.0597(17) 0.0300(12) 0.0745(19) 0.0134(12) 0.0236(15) 0.0058(11) C31 0.0385(12) 0.0321(11) 0.0578(16) 0.0093(11) 0.0216(11) 0.0033(10) C32 0.0344(12) 0.0302(11) 0.0608(16) -0.0063(10) 0.0151(11) -0.0036(9) C33 0.0455(14) 0.0344(12) 0.0689(18) 0.0031(12) 0.0193(13) 0.0052(11) C34 0.0593(17) 0.0679(17) 0.0431(15) -0.0052(13) 0.0213(13) -0.0002(14) C35 0.0678(19) 0.0746(19) 0.0428(16) -0.0180(14) 0.0106(14) -0.0184(16) C36 0.0425(14) 0.0372(13) 0.082(2) 0.0030(13) 0.0291(14) 0.0047(11) _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 1.8584(16) . ? As1 N1 1.8648(15) . ? As1 N2 1.8883(16) . ? As1 Li2 2.772(4) . ? As1 Li1 2.782(3) 3_565 ? O1 C2 1.396(2) . ? O1 C7 1.432(2) . ? O1 Li1 1.972(4) . ? O2 C9 1.387(2) . ? O2 C14 1.432(2) . ? O2 Li3 1.940(4) 3_565 ? O3 C16 1.396(3) . ? O3 C21 1.434(3) . ? O3 Li3 2.083(4) . ? N1 C1 1.383(2) . ? N1 Li1 2.002(4) . ? N1 Li2 2.069(4) . ? N2 C8 1.392(2) . ? N2 Li3 2.037(4) 3_565 ? N2 Li1 2.235(4) 3_565 ? N2 Li2 2.474(4) . ? N3 C15 1.382(2) . ? N3 Li3 1.965(4) . ? N3 Li1 2.000(4) 3_565 ? N4 C34 1.456(3) . ? N4 C33 1.469(3) . ? N4 C31 1.474(3) . ? N4 Li2 2.165(4) . ? N5 C35 1.466(3) . ? N5 C36 1.467(3) . ? N5 C32 1.476(3) . ? N5 Li2 2.192(4) . ? Li1 N3 2.000(4) 3_565 ? Li1 N2 2.235(4) 3_565 ? Li1 C1 2.723(4) . ? Li1 C2 2.755(4) . ? Li1 Li3 2.775(5) . ? Li1 As1 2.782(3) 3_565 ? Li1 Li3 2.839(5) 3_565 ? Li1 Li2 3.142(5) . ? Li1 Li1 3.386(7) 3_565 ? Li2 Li3 2.982(5) 3_565 ? Li3 O2 1.940(4) 3_565 ? Li3 N2 2.037(4) 3_565 ? Li3 Li1 2.839(5) 3_565 ? Li3 Li2 2.982(5) 3_565 ? C1 C6 1.403(3) . ? C1 C2 1.428(3) . ? C2 C3 1.377(3) . ? C3 C4 1.395(3) . ? C3 H3 0.9500 . ? C4 C5 1.378(3) . ? C4 H4 0.9500 . ? C5 C6 1.396(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.415(3) . ? C8 C9 1.426(3) . ? C9 C10 1.378(3) . ? C10 C11 1.400(3) . ? C10 H10 0.9500 . ? C11 C12 1.379(3) . ? C11 H11 0.9500 . ? C12 C13 1.396(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.414(3) . ? C15 C16 1.415(3) . ? C16 C17 1.383(3) . ? C17 C18 1.399(4) . ? C17 H17 0.9500 . ? C18 C19 1.370(4) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 C32 1.503(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 98.05(7) . . ? N3 As1 N2 99.00(7) . . ? N1 As1 N2 88.88(7) . . ? N3 As1 Li2 136.72(9) . . ? N1 As1 Li2 48.28(9) . . ? N2 As1 Li2 60.65(9) . . ? N3 As1 Li1 45.92(8) . 3_565 ? N1 As1 Li1 94.70(8) . 3_565 ? N2 As1 Li1 53.10(8) . 3_565 ? Li2 As1 Li1 102.89(11) . 3_565 ? C2 O1 C7 118.12(16) . . ? C2 O1 Li1 108.58(15) . . ? C7 O1 Li1 128.21(17) . . ? C9 O2 C14 118.24(16) . . ? C9 O2 Li3 115.17(15) . 3_565 ? C14 O2 Li3 126.57(16) . 3_565 ? C16 O3 C21 117.02(18) . . ? C16 O3 Li3 112.74(15) . . ? C21 O3 Li3 125.54(17) . . ? C1 N1 As1 118.07(13) . . ? C1 N1 Li1 105.65(15) . . ? As1 N1 Li1 123.61(12) . . ? C1 N1 Li2 117.27(16) . . ? As1 N1 Li2 89.44(12) . . ? Li1 N1 Li2 101.01(15) . . ? C8 N2 As1 116.35(13) . . ? C8 N2 Li3 109.35(16) . 3_565 ? As1 N2 Li3 133.68(13) . 3_565 ? C8 N2 Li1 99.77(14) . 3_565 ? As1 N2 Li1 84.40(10) . 3_565 ? Li3 N2 Li1 80.87(14) 3_565 3_565 ? C8 N2 Li2 125.71(14) . . ? As1 N2 Li2 77.64(10) . . ? Li3 N2 Li2 82.13(14) 3_565 . ? Li1 N2 Li2 134.48(13) 3_565 . ? C15 N3 As1 118.87(13) . . ? C15 N3 Li3 114.79(16) . . ? As1 N3 Li3 116.90(13) . . ? C15 N3 Li1 116.84(16) . 3_565 ? As1 N3 Li1 92.20(11) . 3_565 ? Li3 N3 Li1 91.46(15) . 3_565 ? C34 N4 C33 108.3(2) . . ? C34 N4 C31 109.10(19) . . ? C33 N4 C31 109.29(18) . . ? C34 N4 Li2 119.35(18) . . ? C33 N4 Li2 106.68(17) . . ? C31 N4 Li2 103.75(16) . . ? C35 N5 C36 108.9(2) . . ? C35 N5 C32 108.5(2) . . ? C36 N5 C32 109.96(18) . . ? C35 N5 Li2 117.56(18) . . ? C36 N5 Li2 106.65(18) . . ? C32 N5 Li2 105.13(16) . . ? O1 Li1 N3 125.82(18) . 3_565 ? O1 Li1 N1 82.57(14) . . ? N3 Li1 N1 129.37(18) 3_565 . ? O1 Li1 N2 116.57(16) . 3_565 ? N3 Li1 N2 84.37(13) 3_565 3_565 ? N1 Li1 N2 122.70(17) . 3_565 ? O1 Li1 C1 57.72(10) . . ? N3 Li1 C1 155.53(17) 3_565 . ? N1 Li1 C1 29.28(7) . . ? N2 Li1 C1 116.81(14) 3_565 . ? O1 Li1 C2 28.70(7) . . ? N3 Li1 C2 152.47(17) 3_565 . ? N1 Li1 C2 58.15(10) . . ? N2 Li1 C2 114.70(14) 3_565 . ? C1 Li1 C2 30.20(7) . . ? O1 Li1 Li3 111.70(16) . . ? N3 Li1 Li3 117.44(16) 3_565 . ? N1 Li1 Li3 76.29(13) . . ? N2 Li1 Li3 46.46(10) 3_565 . ? C1 Li1 Li3 75.57(12) . . ? C2 Li1 Li3 89.72(13) . . ? O1 Li1 As1 134.98(16) . 3_565 ? N3 Li1 As1 41.88(8) 3_565 3_565 ? N1 Li1 As1 141.69(16) . 3_565 ? N2 Li1 As1 42.50(7) 3_565 3_565 ? C1 Li1 As1 156.58(14) . 3_565 ? C2 Li1 As1 152.44(14) . 3_565 ? Li3 Li1 As1 81.03(12) . 3_565 ? O1 Li1 Li3 136.70(17) . 3_565 ? N3 Li1 Li3 43.78(10) 3_565 3_565 ? N1 Li1 Li3 86.08(14) . 3_565 ? N2 Li1 Li3 104.72(15) 3_565 3_565 ? C1 Li1 Li3 114.67(14) . 3_565 ? C2 Li1 Li3 136.68(15) . 3_565 ? Li3 Li1 Li3 105.81(14) . 3_565 ? As1 Li1 Li3 70.86(11) 3_565 3_565 ? O1 Li1 Li2 86.23(13) . . ? N3 Li1 Li2 95.19(14) 3_565 . ? N1 Li1 Li2 40.28(10) . . ? N2 Li1 Li2 152.14(16) 3_565 . ? C1 Li1 Li2 60.34(10) . . ? C2 Li1 Li2 77.13(11) . . ? Li3 Li1 Li2 112.11(15) . . ? As1 Li1 Li2 130.40(13) 3_565 . ? Li3 Li1 Li2 59.55(12) 3_565 . ? O1 Li1 Li1 155.9(2) . 3_565 ? N3 Li1 Li1 76.84(13) 3_565 3_565 ? N1 Li1 Li1 75.44(14) . 3_565 ? N2 Li1 Li1 69.42(12) 3_565 3_565 ? C1 Li1 Li1 98.37(15) . 3_565 ? C2 Li1 Li1 127.29(17) . 3_565 ? Li3 Li1 Li1 53.76(12) . 3_565 ? As1 Li1 Li1 66.25(10) 3_565 3_565 ? Li3 Li1 Li1 52.05(11) 3_565 3_565 ? Li2 Li1 Li1 83.32(14) . 3_565 ? N1 Li2 N4 118.32(18) . . ? N1 Li2 N5 131.61(19) . . ? N4 Li2 N5 83.58(14) . . ? N1 Li2 N2 70.03(12) . . ? N4 Li2 N2 164.35(19) . . ? N5 Li2 N2 100.63(15) . . ? N1 Li2 As1 42.27(8) . . ? N4 Li2 As1 153.06(17) . . ? N5 Li2 As1 98.87(14) . . ? N2 Li2 As1 41.71(7) . . ? N1 Li2 Li3 81.22(14) . 3_565 ? N4 Li2 Li3 123.01(17) . 3_565 ? N5 Li2 Li3 124.59(17) . 3_565 ? N2 Li2 Li3 42.60(10) . 3_565 ? As1 Li2 Li3 77.62(11) . 3_565 ? N1 Li2 Li1 38.71(10) . . ? N4 Li2 Li1 105.89(15) . . ? N5 Li2 Li1 168.91(18) . . ? N2 Li2 Li1 71.82(11) . . ? As1 Li2 Li1 70.07(10) . . ? Li3 Li2 Li1 55.16(11) 3_565 . ? O2 Li3 N3 142.0(2) 3_565 . ? O2 Li3 N2 83.33(14) 3_565 3_565 ? N3 Li3 N2 127.94(19) . 3_565 ? O2 Li3 O3 98.06(16) 3_565 . ? N3 Li3 O3 80.37(14) . . ? N2 Li3 O3 126.96(19) 3_565 . ? O2 Li3 Li1 89.52(15) 3_565 . ? N3 Li3 Li1 94.32(15) . . ? N2 Li3 Li1 52.67(11) 3_565 . ? O3 Li3 Li1 172.35(18) . . ? O2 Li3 Li1 163.51(19) 3_565 3_565 ? N3 Li3 Li1 44.76(11) . 3_565 ? N2 Li3 Li1 84.70(14) 3_565 3_565 ? O3 Li3 Li1 98.19(15) . 3_565 ? Li1 Li3 Li1 74.19(14) . 3_565 ? O2 Li3 Li2 115.79(16) 3_565 3_565 ? N3 Li3 Li2 101.11(16) . 3_565 ? N2 Li3 Li2 55.27(12) 3_565 3_565 ? O3 Li3 Li2 77.91(14) . 3_565 ? Li1 Li3 Li2 97.89(14) . 3_565 ? Li1 Li3 Li2 65.29(12) 3_565 3_565 ? N1 C1 C6 127.41(17) . . ? N1 C1 C2 117.57(17) . . ? C6 C1 C2 115.02(17) . . ? N1 C1 Li1 45.07(11) . . ? C6 C1 Li1 159.35(16) . . ? C2 C1 Li1 76.17(13) . . ? C3 C2 O1 123.65(18) . . ? C3 C2 C1 122.97(19) . . ? O1 C2 C1 113.36(16) . . ? C3 C2 Li1 158.68(17) . . ? O1 C2 Li1 42.73(11) . . ? C1 C2 Li1 73.63(13) . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.4(2) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 122.2(2) . . ? C5 C6 H6 118.9 . . ? C1 C6 H6 118.9 . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C13 127.26(18) . . ? N2 C8 C9 118.32(17) . . ? C13 C8 C9 114.42(17) . . ? C10 C9 O2 123.06(18) . . ? C10 C9 C8 123.20(18) . . ? O2 C9 C8 113.74(16) . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.69(19) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 121.0(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 122.45(19) . . ? C12 C13 H13 118.8 . . ? C8 C13 H13 118.8 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C20 127.49(19) . . ? N3 C15 C16 117.80(18) . . ? C20 C15 C16 114.70(18) . . ? C17 C16 O3 123.4(2) . . ? C17 C16 C15 123.2(2) . . ? O3 C16 C15 113.36(17) . . ? C16 C17 C18 119.7(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 118.9(2) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.2(2) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C15 122.2(2) . . ? C19 C20 H20 118.9 . . ? C15 C20 H20 118.9 . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C31 C32 111.36(18) . . ? N4 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? N4 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? N5 C32 C31 111.37(19) . . ? N5 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? N5 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? N4 C33 H33A 109.5 . . ? N4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 H34A 109.5 . . ? N4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? #===END ############################# ## denoted 6 in the text ## ############################# data_dw0125 _database_code_CSD 169734 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H63 As7 Li3 N3 O3' _chemical_formula_sum 'C30 H63 As7 Li3 N3 O3' _chemical_formula_weight 1059.09 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' _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 11.3301(3) _cell_length_b 14.5022(5) _cell_length_c 15.8403(6) _cell_angle_alpha 116.203(2) _cell_angle_beta 98.386(2) _cell_angle_gamma 103.745(2) _cell_volume 2172.48(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 21759 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 5.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_T_max 0.473 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 25432 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.47 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 9891 _reflns_number_gt 7412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0267P)^2^+2.8873P] 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 9891 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.756 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.103 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 0.01946(4) 0.03676(3) 0.70966(3) 0.03463(10) Uani 1 1 d . . . As2 As 0.08835(4) 0.22134(3) 0.84451(3) 0.03318(10) Uani 1 1 d . . . As3 As 0.17047(4) 0.19640(3) 0.97926(3) 0.03515(11) Uani 1 1 d . . . As4 As 0.28340(4) 0.30311(3) 0.82056(3) 0.03815(11) Uani 1 1 d . . . As5 As 0.30854(4) 0.10158(4) 0.91363(3) 0.03671(11) Uani 1 1 d . . . As6 As 0.20842(4) -0.00465(3) 0.73395(3) 0.03672(11) Uani 1 1 d . . . As7 As 0.38320(4) 0.17201(4) 0.80701(3) 0.03893(11) Uani 1 1 d . . . Li1 Li 0.1436(7) 0.1556(6) 0.6374(5) 0.0415(16) Uani 1 1 d . . . Li2 Li -0.0281(7) 0.0079(6) 0.8579(6) 0.0458(18) Uani 1 1 d . . . Li3 Li 0.3444(8) 0.3829(6) 1.0196(6) 0.054(2) Uani 1 1 d . B . N1 N 0.2126(3) 0.0662(3) 0.5272(3) 0.0391(8) Uani 1 1 d . . . H1A H 0.2091 0.0038 0.5304 0.047 Uiso 1 1 calc R . . H1B H 0.1545 0.0442 0.4691 0.047 Uiso 1 1 calc R . . N2 N 0.0015(3) -0.1221(3) 0.8645(3) 0.0424(8) Uani 1 1 d . . . H2A H 0.0875 -0.1030 0.8895 0.051 Uiso 1 1 calc R . . H2B H -0.0351 -0.1296 0.9104 0.051 Uiso 1 1 calc R . . N3 N 0.5265(3) 0.4025(3) 1.0811(3) 0.0490(9) Uani 1 1 d . B . H3A H 0.5565 0.3622 1.0313 0.059 Uiso 1 1 calc R . . H3B H 0.5746 0.4748 1.1072 0.059 Uiso 1 1 calc R . . O1 O 0.0267(3) 0.2094(3) 0.5841(2) 0.0475(8) Uani 1 1 d . . . O2 O -0.1872(3) 0.0218(3) 0.8851(3) 0.0592(9) Uani 1 1 d . . . O3 O 0.2968(4) 0.5116(3) 1.0855(3) 0.0788(13) Uani 1 1 d . . . C11 C 0.3386(4) 0.1067(4) 0.5162(3) 0.0397(10) Uani 1 1 d . . . H11 H 0.4036 0.1145 0.5712 0.048 Uiso 1 1 calc R . . C12 C 0.3617(4) 0.2181(4) 0.5264(4) 0.0509(12) Uani 1 1 d . . . H12A H 0.3561 0.2688 0.5915 0.061 Uiso 1 1 calc R . . H12B H 0.2950 0.2137 0.4755 0.061 Uiso 1 1 calc R . . C13 C 0.4919(5) 0.2632(5) 0.5159(4) 0.0623(14) Uani 1 1 d . . . H13A H 0.5005 0.3337 0.5178 0.075 Uiso 1 1 calc R . . H13B H 0.5588 0.2773 0.5722 0.075 Uiso 1 1 calc R . . C14 C 0.5109(5) 0.1859(5) 0.4220(4) 0.0633(15) Uani 1 1 d . . . H14A H 0.5988 0.2152 0.4212 0.076 Uiso 1 1 calc R . . H14B H 0.4524 0.1804 0.3657 0.076 Uiso 1 1 calc R . . C15 C 0.4873(5) 0.0733(5) 0.4105(4) 0.0642(15) Uani 1 1 d . . . H15A H 0.5535 0.0769 0.4613 0.077 Uiso 1 1 calc R . . H15B H 0.4932 0.0231 0.3453 0.077 Uiso 1 1 calc R . . C16 C 0.3568(4) 0.0287(4) 0.4203(4) 0.0492(11) Uani 1 1 d . . . H16A H 0.2905 0.0162 0.3644 0.059 Uiso 1 1 calc R . . H16B H 0.3467 -0.0425 0.4172 0.059 Uiso 1 1 calc R . . C21 C -0.0413(5) -0.2307(4) 0.7776(4) 0.0621(14) Uani 1 1 d . A . H21 H 0.0169 -0.2232 0.7374 0.075 Uiso 1 1 calc R . . C22 C -0.0208(5) -0.3196(4) 0.7968(4) 0.0537(12) Uani 1 1 d . . . H22A H -0.0715 -0.3287 0.8402 0.064 Uiso 0.741(16) 1 calc PR A 3 H22B H 0.0697 -0.2973 0.8315 0.064 Uiso 0.741(16) 1 calc PR A 3 H22C H -0.0305 -0.3037 0.8624 0.064 Uiso 0.259(16) 1 calc PR A 4 H22D H 0.0674 -0.3177 0.7985 0.064 Uiso 0.259(16) 1 calc PR A 4 C23 C -0.0584(10) -0.4292(6) 0.7019(6) 0.062(2) Uiso 0.741(16) 1 d P A 3 H23A H 0.0008 -0.4239 0.6628 0.074 Uiso 0.741(16) 1 calc PR A 3 H23B H -0.0525 -0.4867 0.7183 0.074 Uiso 0.741(16) 1 calc PR A 3 C23' C -0.114(3) -0.4385(18) 0.7186(18) 0.062(2) Uiso 0.259(16) 1 d P A 4 H23C H -0.0602 -0.4842 0.6970 0.074 Uiso 0.259(16) 1 calc PR A 4 H23D H -0.1634 -0.4657 0.7546 0.074 Uiso 0.259(16) 1 calc PR A 4 C24 C -0.1924(7) -0.4600(4) 0.6421(5) 0.084(2) Uani 1 1 d . . . H24A H -0.2116 -0.5271 0.5784 0.100 Uiso 0.741(16) 1 calc PR A 3 H24B H -0.2522 -0.4766 0.6773 0.100 Uiso 0.741(16) 1 calc PR A 3 H24C H -0.2758 -0.5035 0.6399 0.100 Uiso 0.259(16) 1 calc PR A 4 H24D H -0.1681 -0.5088 0.5857 0.100 Uiso 0.259(16) 1 calc PR A 4 C25 C -0.2131(5) -0.3718(4) 0.6230(4) 0.0595(13) Uani 1 1 d . A . H25A H -0.3049 -0.3914 0.5937 0.071 Uiso 1 1 calc R . . H25B H -0.1689 -0.3674 0.5747 0.071 Uiso 1 1 calc R . . C26 C -0.1659(6) -0.2614(4) 0.7148(4) 0.0766(19) Uani 1 1 d . . . H26A H -0.1655 -0.2053 0.6951 0.092 Uiso 1 1 calc R A . H26B H -0.2271 -0.2599 0.7536 0.092 Uiso 1 1 calc R . . C31 C 0.5510(5) 0.3721(5) 1.1596(4) 0.0735(17) Uani 1 1 d . . . H31 H 0.5100 0.2923 1.1349 0.088 Uiso 0.369(13) 1 calc PR B 1 H31' H 0.4854 0.2985 1.1322 0.088 Uiso 0.631(13) 1 calc PR B 2 C32 C 0.7106(15) 0.4122(17) 1.1921(12) 0.060(2) Uiso 0.369(13) 1 d P B 1 H32A H 0.7531 0.4918 1.2370 0.072 Uiso 0.369(13) 1 calc PR B 1 H32B H 0.7462 0.3856 1.1359 0.072 Uiso 0.369(13) 1 calc PR B 1 C32' C 0.6755(9) 0.3535(10) 1.1770(7) 0.060(2) Uiso 0.631(13) 1 d P B 2 H32C H 0.6771 0.2929 1.1154 0.072 Uiso 0.631(13) 1 calc PR B 2 H32D H 0.7452 0.4201 1.1933 0.072 Uiso 0.631(13) 1 calc PR B 2 C33 C 0.6997(8) 0.3265(9) 1.2580(7) 0.128(3) Uani 1 1 d . . . H33A H 0.6273 0.2569 1.2203 0.153 Uiso 0.369(13) 1 calc PR B 1 H33B H 0.7791 0.3114 1.2709 0.153 Uiso 0.369(13) 1 calc PR B 1 H33C H 0.6427 0.2516 1.2352 0.153 Uiso 0.631(13) 1 calc PR B 2 H33D H 0.7882 0.3276 1.2722 0.153 Uiso 0.631(13) 1 calc PR B 2 C34 C 0.6801(6) 0.4007(6) 1.3468(5) 0.0841(19) Uani 1 1 d . B . H34A H 0.7428 0.4748 1.3744 0.101 Uiso 1 1 calc R . . H34B H 0.6915 0.3765 1.3959 0.101 Uiso 1 1 calc R . . C35 C 0.5471(7) 0.4035(8) 1.3239(6) 0.105(3) Uani 1 1 d . . . H35A H 0.5331 0.4547 1.3850 0.126 Uiso 1 1 calc R B . H35B H 0.4852 0.3299 1.2992 0.126 Uiso 1 1 calc R . . C36 C 0.5244(8) 0.4393(7) 1.2472(6) 0.100(2) Uani 1 1 d . B . H36A H 0.4349 0.4354 1.2311 0.121 Uiso 1 1 calc R . . H36B H 0.5791 0.5162 1.2749 0.121 Uiso 1 1 calc R . . C101 C -0.0600(4) 0.2516(4) 0.6332(4) 0.0512(12) Uani 1 1 d . . . H10A H -0.0152 0.3246 0.6918 0.061 Uiso 1 1 calc R . . H10B H -0.1065 0.2019 0.6538 0.061 Uiso 1 1 calc R . . C102 C -0.1482(4) 0.2581(4) 0.5576(4) 0.0525(12) Uani 1 1 d . . . H10C H -0.1898 0.3121 0.5888 0.063 Uiso 1 1 calc R . . H10D H -0.2143 0.1861 0.5115 0.063 Uiso 1 1 calc R . . C103 C -0.0620(5) 0.2942(4) 0.5055(4) 0.0490(11) Uani 1 1 d . . . H10E H -0.0317 0.3747 0.5351 0.059 Uiso 1 1 calc R . . H10F H -0.1060 0.2605 0.4348 0.059 Uiso 1 1 calc R . . C104 C 0.0472(4) 0.2539(4) 0.5204(3) 0.0472(11) Uani 1 1 d . . . H10G H 0.0491 0.1971 0.4566 0.057 Uiso 1 1 calc R . . H10H H 0.1290 0.3150 0.5506 0.057 Uiso 1 1 calc R . . C201 C -0.3002(4) -0.0643(4) 0.8603(4) 0.0527(12) Uani 1 1 d . . . H20A H -0.2858 -0.1034 0.8964 0.063 Uiso 1 1 calc R . . H20B H -0.3272 -0.1171 0.7890 0.063 Uiso 1 1 calc R . . C202 C -0.4012(5) -0.0146(5) 0.8880(5) 0.0665(15) Uani 1 1 d . . . H20C H -0.4650 -0.0311 0.8288 0.080 Uiso 1 1 calc R . . H20D H -0.4446 -0.0419 0.9265 0.080 Uiso 1 1 calc R . . C203 C -0.3284(5) 0.1048(5) 0.9484(5) 0.084(2) Uani 1 1 d . . . H20E H -0.2997 0.1270 1.0188 0.101 Uiso 1 1 calc R . . H20F H -0.3805 0.1481 0.9407 0.101 Uiso 1 1 calc R . . C204 C -0.2168(5) 0.1197(5) 0.9081(5) 0.0725(17) Uani 1 1 d . . . H20G H -0.2401 0.1259 0.8486 0.087 Uiso 1 1 calc R . . H20H H -0.1444 0.1855 0.9578 0.087 Uiso 1 1 calc R . . C301 C 0.1628(13) 0.5077(11) 1.0603(11) 0.0643(15) Uiso 0.442(8) 1 d P C 5 H30A H 0.1363 0.4943 0.9923 0.077 Uiso 0.442(8) 1 calc PR C 5 H30B H 0.1057 0.4476 1.0646 0.077 Uiso 0.442(8) 1 calc PR C 5 C311 C 0.1952(10) 0.5293(9) 1.0336(8) 0.0643(15) Uiso 0.558(8) 1 d P C 6 H31A H 0.2063 0.5176 0.9692 0.077 Uiso 0.558(8) 1 calc PR C 6 H31B H 0.1122 0.4771 1.0220 0.077 Uiso 0.558(8) 1 calc PR C 6 C302 C 0.1555(12) 0.6019(11) 1.1225(10) 0.0643(15) Uiso 0.442(8) 1 d P C 5 H30C H 0.0907 0.5890 1.1555 0.077 Uiso 0.442(8) 1 calc PR C 5 H30D H 0.1285 0.6376 1.0861 0.077 Uiso 0.442(8) 1 calc PR C 5 C312 C 0.1990(10) 0.6345(9) 1.0900(8) 0.0643(15) Uiso 0.558(8) 1 d P C 6 H31C H 0.1121 0.6367 1.0888 0.077 Uiso 0.558(8) 1 calc PR C 6 H31D H 0.2397 0.6817 1.0650 0.077 Uiso 0.558(8) 1 calc PR C 6 C303 C 0.2779(6) 0.6745(5) 1.1966(5) 0.0821(19) Uani 1 1 d . . . H30E H 0.2679 0.7090 1.2635 0.099 Uiso 0.442(8) 1 calc PR C 5 H30F H 0.3207 0.7322 1.1830 0.099 Uiso 0.442(8) 1 calc PR C 5 H30G H 0.3372 0.7503 1.2268 0.099 Uiso 0.558(8) 1 calc PR C 6 H30H H 0.2215 0.6717 1.2383 0.099 Uiso 0.558(8) 1 calc PR C 6 C304 C 0.3491(5) 0.5966(4) 1.1846(4) 0.0580(13) Uani 1 1 d . C . H30I H 0.4408 0.6337 1.1985 0.070 Uiso 1 1 calc R . . H30J H 0.3379 0.5673 1.2298 0.070 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 0.0329(2) 0.0332(2) 0.0278(2) 0.01246(19) 0.00355(17) 0.00327(17) As2 0.0332(2) 0.0315(2) 0.0327(2) 0.01406(19) 0.00947(17) 0.01133(17) As3 0.0391(2) 0.0352(2) 0.0264(2) 0.01275(19) 0.01102(17) 0.00869(18) As4 0.0401(2) 0.0312(2) 0.0368(2) 0.0171(2) 0.00839(19) 0.00263(18) As5 0.0355(2) 0.0398(2) 0.0347(2) 0.0192(2) 0.00716(18) 0.01292(19) As6 0.0420(2) 0.0306(2) 0.0327(2) 0.01097(19) 0.01299(19) 0.01233(19) As7 0.0311(2) 0.0433(3) 0.0398(3) 0.0191(2) 0.01381(18) 0.00891(19) Li1 0.043(4) 0.050(4) 0.035(4) 0.019(4) 0.016(3) 0.021(3) Li2 0.053(4) 0.036(4) 0.055(5) 0.025(4) 0.026(4) 0.015(3) Li3 0.052(4) 0.038(4) 0.051(5) 0.011(4) -0.003(4) 0.014(4) N1 0.0396(19) 0.042(2) 0.034(2) 0.0187(17) 0.0107(15) 0.0120(16) N2 0.053(2) 0.0331(19) 0.039(2) 0.0156(17) 0.0198(17) 0.0124(17) N3 0.044(2) 0.039(2) 0.050(2) 0.0167(19) 0.0040(18) 0.0093(17) O1 0.0528(18) 0.065(2) 0.0458(19) 0.0345(17) 0.0231(15) 0.0351(17) O2 0.0482(18) 0.049(2) 0.093(3) 0.037(2) 0.0408(19) 0.0224(16) O3 0.068(2) 0.048(2) 0.077(3) 0.001(2) -0.014(2) 0.0299(19) C11 0.035(2) 0.050(3) 0.034(2) 0.020(2) 0.0118(18) 0.014(2) C12 0.047(3) 0.049(3) 0.054(3) 0.024(3) 0.016(2) 0.014(2) C13 0.049(3) 0.061(3) 0.075(4) 0.038(3) 0.017(3) 0.007(3) C14 0.047(3) 0.098(5) 0.062(4) 0.054(4) 0.021(3) 0.020(3) C15 0.054(3) 0.089(4) 0.063(4) 0.040(3) 0.031(3) 0.034(3) C16 0.049(3) 0.054(3) 0.046(3) 0.022(2) 0.018(2) 0.022(2) C21 0.075(4) 0.036(3) 0.054(3) 0.016(3) 0.001(3) 0.007(3) C22 0.068(3) 0.040(3) 0.048(3) 0.015(2) 0.015(2) 0.024(2) C24 0.118(5) 0.039(3) 0.065(4) 0.012(3) 0.004(4) 0.018(3) C25 0.073(3) 0.042(3) 0.046(3) 0.014(2) 0.009(3) 0.008(3) C26 0.103(5) 0.038(3) 0.063(4) 0.016(3) -0.009(3) 0.018(3) C31 0.061(3) 0.088(4) 0.056(4) 0.023(3) -0.003(3) 0.037(3) C33 0.121(7) 0.196(10) 0.105(7) 0.087(7) 0.025(5) 0.100(7) C34 0.078(4) 0.093(5) 0.066(4) 0.043(4) 0.001(3) 0.009(4) C35 0.114(6) 0.166(8) 0.101(6) 0.100(6) 0.052(5) 0.073(6) C36 0.111(5) 0.144(7) 0.098(6) 0.076(6) 0.056(5) 0.079(5) C101 0.055(3) 0.062(3) 0.057(3) 0.036(3) 0.030(2) 0.033(3) C102 0.044(3) 0.048(3) 0.065(3) 0.026(3) 0.012(2) 0.021(2) C103 0.064(3) 0.045(3) 0.046(3) 0.025(2) 0.017(2) 0.026(2) C104 0.057(3) 0.046(3) 0.043(3) 0.023(2) 0.019(2) 0.020(2) C201 0.043(3) 0.062(3) 0.053(3) 0.033(3) 0.010(2) 0.010(2) C202 0.050(3) 0.088(4) 0.074(4) 0.048(4) 0.018(3) 0.026(3) C203 0.054(3) 0.091(5) 0.086(5) 0.020(4) 0.017(3) 0.041(3) C204 0.063(3) 0.053(3) 0.104(5) 0.036(3) 0.032(3) 0.027(3) C303 0.069(4) 0.060(4) 0.091(5) 0.008(3) 0.035(3) 0.029(3) C304 0.062(3) 0.045(3) 0.051(3) 0.015(3) 0.018(3) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 As6 2.3806(6) . ? As1 As2 2.4100(6) . ? As1 Li2 2.667(8) . ? As1 Li1 2.705(7) . ? As2 As3 2.4114(6) . ? As2 As4 2.4147(6) . ? As2 Li2 3.176(7) . ? As2 Li1 3.191(7) . ? As2 Li3 3.207(8) . ? As3 As5 2.3776(6) . ? As3 Li3 2.680(8) . ? As3 Li2 2.721(8) . ? As4 As7 2.3814(6) . ? As4 Li1 2.659(7) . ? As4 Li3 2.743(9) . ? As5 As6 2.4732(6) . ? As5 As7 2.4781(6) . ? As6 As7 2.4753(6) . ? Li1 O1 1.955(7) . ? Li1 N1 2.055(8) . ? Li2 O2 1.948(8) . ? Li2 N2 2.036(8) . ? Li3 O3 1.946(9) . ? Li3 N3 2.043(8) . ? N1 C11 1.475(5) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C21 1.462(6) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C31 1.503(7) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? O1 C101 1.426(5) . ? O1 C104 1.436(5) . ? O2 C201 1.419(5) . ? O2 C204 1.438(6) . ? O3 C304 1.417(6) . ? O3 C311 1.455(10) . ? O3 C301 1.494(13) . ? C11 C12 1.503(6) . ? C11 C16 1.522(6) . ? C11 H11 1.0000 . ? C12 C13 1.529(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.501(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.513(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.526(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C26 1.443(7) . ? C21 C22 1.509(6) . ? C21 H21 1.0000 . ? C22 C23 1.532(9) . ? C22 C23' 1.58(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 H22C 0.9900 . ? C22 H22D 0.9900 . ? C23 C24 1.512(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23' C24 1.26(2) . ? C23' H23C 0.9900 . ? C23' H23D 0.9900 . ? C24 C25 1.498(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 0.9900 . ? C24 H24D 0.9900 . ? C25 C26 1.509(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C36 1.425(9) . ? C31 C32' 1.507(10) . ? C31 C32 1.685(16) . ? C31 H31 1.0000 . ? C31 H31' 1.0000 . ? C32 C33 1.938(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32' C33 1.505(12) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33 C34 1.433(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 H33C 0.9900 . ? C33 H33D 0.9900 . ? C34 C35 1.512(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.531(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C101 C102 1.497(6) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.511(7) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.519(6) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C201 C202 1.509(7) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 C203 1.491(8) . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.510(8) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C301 C302 1.317(18) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C311 C312 1.372(14) . ? C311 H31A 0.9900 . ? C311 H31B 0.9900 . ? C302 C303 1.466(14) . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C312 C303 1.561(12) . ? C312 H31C 0.9900 . ? C312 H31D 0.9900 . ? C303 C304 1.500(7) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C303 H30G 0.9900 . ? C303 H30H 0.9900 . ? C304 H30I 0.9900 . ? C304 H30J 0.9900 . ? 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 As6 As1 As2 99.67(2) . . ? As6 As1 Li2 88.85(16) . . ? As2 As1 Li2 77.28(16) . . ? As6 As1 Li1 85.17(14) . . ? As2 As1 Li1 76.95(16) . . ? Li2 As1 Li1 152.1(2) . . ? As1 As2 As3 100.69(2) . . ? As1 As2 As4 101.38(2) . . ? As3 As2 As4 100.58(2) . . ? As1 As2 Li2 54.98(15) . . ? As3 As2 Li2 56.31(15) . . ? As4 As2 Li2 135.20(13) . . ? As1 As2 Li1 55.68(14) . . ? As3 As2 Li1 132.37(12) . . ? As4 As2 Li1 54.52(13) . . ? Li2 As2 Li1 109.9(2) . . ? As1 As2 Li3 135.09(14) . . ? As3 As2 Li3 54.78(16) . . ? As4 As2 Li3 56.30(17) . . ? Li2 As2 Li3 110.7(2) . . ? Li1 As2 Li3 110.1(2) . . ? As5 As3 As2 99.60(2) . . ? As5 As3 Li3 88.92(18) . . ? As2 As3 Li3 77.90(17) . . ? As5 As3 Li2 88.29(16) . . ? As2 As3 Li2 76.19(16) . . ? Li3 As3 Li2 153.1(2) . . ? As7 As4 As2 99.32(2) . . ? As7 As4 Li1 85.03(15) . . ? As2 As4 Li1 77.79(16) . . ? As7 As4 Li3 88.55(16) . . ? As2 As4 Li3 76.61(18) . . ? Li1 As4 Li3 152.2(2) . . ? As3 As5 As6 105.25(2) . . ? As3 As5 As7 105.03(2) . . ? As6 As5 As7 59.990(17) . . ? As1 As6 As5 104.94(2) . . ? As1 As6 As7 105.00(2) . . ? As5 As6 As7 60.102(17) . . ? As4 As7 As6 105.63(2) . . ? As4 As7 As5 105.04(2) . . ? As6 As7 As5 59.908(17) . . ? O1 Li1 N1 108.1(4) . . ? O1 Li1 As4 112.0(3) . . ? N1 Li1 As4 124.9(3) . . ? O1 Li1 As1 108.9(3) . . ? N1 Li1 As1 112.6(3) . . ? As4 Li1 As1 88.2(2) . . ? O1 Li1 As2 99.2(3) . . ? N1 Li1 As2 151.2(3) . . ? As4 Li1 As2 47.70(12) . . ? As1 Li1 As2 47.37(11) . . ? O2 Li2 N2 110.8(4) . . ? O2 Li2 As1 115.9(3) . . ? N2 Li2 As1 117.6(3) . . ? O2 Li2 As3 111.5(3) . . ? N2 Li2 As3 111.9(3) . . ? As1 Li2 As3 87.1(2) . . ? O2 Li2 As2 102.0(3) . . ? N2 Li2 As2 146.7(3) . . ? As1 Li2 As2 47.74(12) . . ? As3 Li2 As2 47.50(11) . . ? O3 Li3 N3 114.0(4) . . ? O3 Li3 As3 113.8(4) . . ? N3 Li3 As3 114.6(3) . . ? O3 Li3 As4 111.2(3) . . ? N3 Li3 As4 113.9(4) . . ? As3 Li3 As4 86.4(2) . . ? O3 Li3 As2 100.4(3) . . ? N3 Li3 As2 145.6(4) . . ? As3 Li3 As2 47.32(12) . . ? As4 Li3 As2 47.09(12) . . ? C11 N1 Li1 124.6(3) . . ? C11 N1 H1A 106.2 . . ? Li1 N1 H1A 106.2 . . ? C11 N1 H1B 106.2 . . ? Li1 N1 H1B 106.2 . . ? H1A N1 H1B 106.4 . . ? C21 N2 Li2 121.9(4) . . ? C21 N2 H2A 106.9 . . ? Li2 N2 H2A 106.9 . . ? C21 N2 H2B 106.9 . . ? Li2 N2 H2B 106.9 . . ? H2A N2 H2B 106.7 . . ? C31 N3 Li3 118.7(4) . . ? C31 N3 H3A 107.6 . . ? Li3 N3 H3A 107.6 . . ? C31 N3 H3B 107.6 . . ? Li3 N3 H3B 107.6 . . ? H3A N3 H3B 107.1 . . ? C101 O1 C104 107.7(3) . . ? C101 O1 Li1 122.2(3) . . ? C104 O1 Li1 125.5(3) . . ? C201 O2 C204 108.8(4) . . ? C201 O2 Li2 127.0(4) . . ? C204 O2 Li2 122.1(4) . . ? C304 O3 C311 111.3(5) . . ? C304 O3 C301 103.8(7) . . ? C311 O3 C301 28.2(6) . . ? C304 O3 Li3 127.7(4) . . ? C311 O3 Li3 121.0(6) . . ? C301 O3 Li3 121.5(6) . . ? N1 C11 C12 110.2(3) . . ? N1 C11 C16 113.0(4) . . ? C12 C11 C16 110.7(4) . . ? N1 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C16 C11 H11 107.6 . . ? C11 C12 C13 111.8(4) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 112.1(4) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C13 C14 C15 111.7(4) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 111.2(4) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C11 C16 C15 111.8(4) . . ? C11 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C11 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C26 C21 N2 114.0(4) . . ? C26 C21 C22 113.7(4) . . ? N2 C21 C22 115.0(4) . . ? C26 C21 H21 104.1 . . ? N2 C21 H21 104.1 . . ? C22 C21 H21 104.1 . . ? C21 C22 C23 112.4(5) . . ? C21 C22 C23' 114.6(9) . . ? C23 C22 C23' 26.9(10) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C23' C22 H22A 83.8 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? C23' C22 H22B 127.7 . . ? H22A C22 H22B 107.9 . . ? C21 C22 H22C 108.6 . . ? C23 C22 H22C 130.1 . . ? C23' C22 H22C 108.6 . . ? H22A C22 H22C 28.1 . . ? H22B C22 H22C 82.1 . . ? C21 C22 H22D 108.6 . . ? C23 C22 H22D 85.1 . . ? C23' C22 H22D 108.6 . . ? H22A C22 H22D 129.9 . . ? H22B C22 H22D 27.2 . . ? H22C C22 H22D 107.6 . . ? C24 C23 C22 110.4(7) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C24 C23' C22 123.5(16) . . ? C24 C23' H23C 106.5 . . ? C22 C23' H23C 106.5 . . ? C24 C23' H23D 106.5 . . ? C22 C23' H23D 106.5 . . ? H23C C23' H23D 106.5 . . ? C23' C24 C25 121.8(11) . . ? C23' C24 C23 28.4(13) . . ? C25 C24 C23 113.0(6) . . ? C23' C24 H24A 122.5 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? C23' C24 H24B 80.7 . . ? C25 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C23' C24 H24C 106.9 . . ? C25 C24 H24C 106.9 . . ? C23 C24 H24C 132.5 . . ? H24A C24 H24C 80.1 . . ? H24B C24 H24C 30.8 . . ? C23' C24 H24D 106.9 . . ? C25 C24 H24D 106.9 . . ? C23 C24 H24D 85.7 . . ? H24A C24 H24D 27.5 . . ? H24B C24 H24D 131.1 . . ? H24C C24 H24D 106.7 . . ? C24 C25 C26 112.8(4) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C21 C26 C25 116.0(5) . . ? C21 C26 H26A 108.3 . . ? C25 C26 H26A 108.3 . . ? C21 C26 H26B 108.3 . . ? C25 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C36 C31 N3 113.4(5) . . ? C36 C31 C32' 114.1(6) . . ? N3 C31 C32' 114.9(6) . . ? C36 C31 C32 103.5(8) . . ? N3 C31 C32 100.7(7) . . ? C32' C31 C32 26.7(6) . . ? C36 C31 H31 112.8 . . ? N3 C31 H31 112.8 . . ? C32' C31 H31 86.2 . . ? C32 C31 H31 112.8 . . ? C36 C31 H31' 104.3 . . ? N3 C31 H31' 104.3 . . ? C32' C31 H31' 104.3 . . ? C32 C31 H31' 130.9 . . ? H31 C31 H31' 18.1 . . ? C31 C32 C33 88.1(9) . . ? C31 C32 H32A 114.0 . . ? C33 C32 H32A 114.0 . . ? C31 C32 H32B 114.0 . . ? C33 C32 H32B 114.0 . . ? H32A C32 H32B 111.2 . . ? C33 C32' C31 114.0(7) . . ? C33 C32' H32C 108.8 . . ? C31 C32' H32C 108.8 . . ? C33 C32' H32D 108.8 . . ? C31 C32' H32D 108.8 . . ? H32C C32' H32D 107.7 . . ? C34 C33 C32' 113.2(7) . . ? C34 C33 C32 99.5(8) . . ? C32' C33 C32 20.9(6) . . ? C34 C33 H33A 111.9 . . ? C32' C33 H33A 91.6 . . ? C32 C33 H33A 111.9 . . ? C34 C33 H33B 111.9 . . ? C32' C33 H33B 117.0 . . ? C32 C33 H33B 111.9 . . ? H33A C33 H33B 109.6 . . ? C34 C33 H33C 108.9 . . ? C32' C33 H33C 108.9 . . ? C32 C33 H33C 129.7 . . ? H33A C33 H33C 18.5 . . ? H33B C33 H33C 95.1 . . ? C34 C33 H33D 108.9 . . ? C32' C33 H33D 108.9 . . ? C32 C33 H33D 100.7 . . ? H33A C33 H33D 121.3 . . ? H33B C33 H33D 12.9 . . ? H33C C33 H33D 107.7 . . ? C33 C34 C35 108.8(6) . . ? C33 C34 H34A 109.9 . . ? C35 C34 H34A 109.9 . . ? C33 C34 H34B 109.9 . . ? C35 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? C34 C35 C36 111.9(6) . . ? C34 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C31 C36 C35 111.6(6) . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36B 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? O1 C101 C102 103.8(4) . . ? O1 C101 H10A 111.0 . . ? C102 C101 H10A 111.0 . . ? O1 C101 H10B 111.0 . . ? C102 C101 H10B 111.0 . . ? H10A C101 H10B 109.0 . . ? C101 C102 C103 103.5(4) . . ? C101 C102 H10C 111.1 . . ? C103 C102 H10C 111.1 . . ? C101 C102 H10D 111.1 . . ? C103 C102 H10D 111.1 . . ? H10C C102 H10D 109.0 . . ? C102 C103 C104 103.5(3) . . ? C102 C103 H10E 111.1 . . ? C104 C103 H10E 111.1 . . ? C102 C103 H10F 111.1 . . ? C104 C103 H10F 111.1 . . ? H10E C103 H10F 109.0 . . ? O1 C104 C103 107.0(4) . . ? O1 C104 H10G 110.3 . . ? C103 C104 H10G 110.3 . . ? O1 C104 H10H 110.3 . . ? C103 C104 H10H 110.3 . . ? H10G C104 H10H 108.6 . . ? O2 C201 C202 107.9(4) . . ? O2 C201 H20A 110.1 . . ? C202 C201 H20A 110.1 . . ? O2 C201 H20B 110.1 . . ? C202 C201 H20B 110.1 . . ? H20A C201 H20B 108.4 . . ? C203 C202 C201 103.4(4) . . ? C203 C202 H20C 111.1 . . ? C201 C202 H20C 111.1 . . ? C203 C202 H20D 111.1 . . ? C201 C202 H20D 111.1 . . ? H20C C202 H20D 109.0 . . ? C202 C203 C204 103.9(5) . . ? C202 C203 H20E 111.0 . . ? C204 C203 H20E 111.0 . . ? C202 C203 H20F 111.0 . . ? C204 C203 H20F 111.0 . . ? H20E C203 H20F 109.0 . . ? O2 C204 C203 103.1(5) . . ? O2 C204 H20G 111.1 . . ? C203 C204 H20G 111.1 . . ? O2 C204 H20H 111.1 . . ? C203 C204 H20H 111.1 . . ? H20G C204 H20H 109.1 . . ? C302 C301 O3 108.6(11) . . ? C302 C301 H30A 110.0 . . ? O3 C301 H30A 110.0 . . ? C302 C301 H30B 110.0 . . ? O3 C301 H30B 110.0 . . ? H30A C301 H30B 108.4 . . ? C312 C311 O3 108.4(8) . . ? C312 C311 H31A 110.0 . . ? O3 C311 H31A 110.0 . . ? C312 C311 H31B 110.0 . . ? O3 C311 H31B 110.0 . . ? H31A C311 H31B 108.4 . . ? C301 C302 C303 111.2(11) . . ? C301 C302 H30C 109.4 . . ? C303 C302 H30C 109.4 . . ? C301 C302 H30D 109.4 . . ? C303 C302 H30D 109.4 . . ? H30C C302 H30D 108.0 . . ? C311 C312 C303 106.5(8) . . ? C311 C312 H31C 110.4 . . ? C303 C312 H31C 110.4 . . ? C311 C312 H31D 110.4 . . ? C303 C312 H31D 110.4 . . ? H31C C312 H31D 108.6 . . ? C302 C303 C304 101.9(6) . . ? C302 C303 C312 36.6(6) . . ? C304 C303 C312 104.7(5) . . ? C302 C303 H30E 111.4 . . ? C304 C303 H30E 111.4 . . ? C312 C303 H30E 137.1 . . ? C302 C303 H30F 111.4 . . ? C304 C303 H30F 111.4 . . ? C312 C303 H30F 76.9 . . ? H30E C303 H30F 109.3 . . ? C302 C303 H30G 140.2 . . ? C304 C303 H30G 110.8 . . ? C312 C303 H30G 110.8 . . ? H30E C303 H30G 77.4 . . ? H30F C303 H30G 35.5 . . ? C302 C303 H30H 78.5 . . ? C304 C303 H30H 110.8 . . ? C312 C303 H30H 110.8 . . ? H30E C303 H30H 34.3 . . ? H30F C303 H30H 133.1 . . ? H30G C303 H30H 108.9 . . ? O3 C304 C303 105.6(4) . . ? O3 C304 H30I 110.6 . . ? C303 C304 H30I 110.6 . . ? O3 C304 H30J 110.6 . . ? C303 C304 H30J 110.6 . . ? H30I C304 H30J 108.7 . . ? #===END ############################# ## denoted 4 in the text ## ############################# data_dw0132 _database_code_CSD 169735 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H82 As2 Li8 N16 O6, 2(C4 H8 O)' _chemical_formula_sum 'C72 H98 As2 Li8 N16 O8' _chemical_formula_weight 1521.02 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8168(6) _cell_length_b 13.2090(6) _cell_length_c 14.3578(5) _cell_angle_alpha 82.657(3) _cell_angle_beta 71.871(3) _cell_angle_gamma 69.363(2) _cell_volume 1992.75(15) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 29512 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 19493 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _reflns_number_total 6933 _reflns_number_gt 5736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0557P)^2^+1.2934P] 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 6933 _refine_ls_number_parameters 591 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.836 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.059 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 -0.06539(3) 0.11850(2) -0.10435(2) 0.04220(12) Uani 1 1 d . . . N1 N 0.0594(2) 0.1527(2) -0.20482(17) 0.0468(6) Uani 1 1 d . A . N2 N -0.1378(2) 0.0775(2) -0.18425(17) 0.0459(6) Uani 1 1 d . A . N3 N -0.1750(2) 0.26008(19) -0.10248(18) 0.0461(6) Uani 1 1 d . . . N4 N 0.2150(2) -0.0100(2) -0.17428(18) 0.0480(6) Uani 1 1 d . . . N5 N -0.0438(2) -0.1070(2) -0.14222(18) 0.0486(6) Uani 1 1 d . . . N6 N -0.2158(2) 0.2568(2) 0.07047(18) 0.0496(6) Uani 1 1 d . . . N7 N -0.0802(3) 0.2814(2) -0.3606(2) 0.0603(7) Uani 1 1 d D A . H1N H -0.020(2) 0.290(3) -0.4120(17) 0.064(11) Uiso 1 1 d D . . N8 N -0.2928(3) 0.3043(2) -0.3171(2) 0.0575(7) Uani 1 1 d . A . Li1 Li -0.1007(5) 0.0989(4) 0.0922(4) 0.0505(12) Uani 1 1 d . . . Li2 Li -0.0202(5) 0.1268(5) -0.3105(4) 0.0534(13) Uani 1 1 d . . . Li3 Li -0.0580(5) 0.3047(4) -0.2297(4) 0.0538(13) Uani 1 1 d . A . Li4 Li -0.2766(5) 0.2260(5) -0.1858(4) 0.0540(13) Uani 1 1 d . A . C1 C 0.1793(3) 0.0893(2) -0.2209(2) 0.0454(7) Uani 1 1 d . . . C2 C 0.3407(3) -0.0653(3) -0.1945(3) 0.0613(9) Uani 1 1 d . . . H2 H 0.3657 -0.1331 -0.1618 0.074 Uiso 1 1 calc R A . C3 C 0.4337(4) -0.0315(4) -0.2579(3) 0.0751(11) Uani 1 1 d . A . H3 H 0.5201 -0.0734 -0.2675 0.090 Uiso 1 1 calc R . . C4 C 0.3981(4) 0.0660(3) -0.3081(3) 0.0725(11) Uani 1 1 d . . . H4 H 0.4600 0.0913 -0.3545 0.087 Uiso 1 1 calc R A . C5 C 0.2747(3) 0.1244(3) -0.2900(2) 0.0594(9) Uani 1 1 d . A . H5 H 0.2505 0.1911 -0.3245 0.071 Uiso 1 1 calc R . . C10 C -0.1231(3) -0.0279(2) -0.1863(2) 0.0448(7) Uani 1 1 d . . . C11 C -0.0386(4) -0.2101(3) -0.1469(3) 0.0649(9) Uani 1 1 d . . . H11 H 0.0120 -0.2641 -0.1126 0.078 Uiso 1 1 calc R A . C12 C -0.1006(4) -0.2433(3) -0.1971(3) 0.0775(11) Uani 1 1 d . A . H12 H -0.0912 -0.3175 -0.1991 0.093 Uiso 1 1 calc R . . C13 C -0.1780(4) -0.1637(3) -0.2451(3) 0.0711(10) Uani 1 1 d . . . H13 H -0.2215 -0.1829 -0.2819 0.085 Uiso 1 1 calc R A . C14 C -0.1904(3) -0.0585(3) -0.2386(2) 0.0574(8) Uani 1 1 d . A . H14 H -0.2451 -0.0040 -0.2695 0.069 Uiso 1 1 calc R . . C20 C -0.2328(3) 0.3088(2) -0.0155(2) 0.0447(7) Uani 1 1 d . . . C21 C -0.2813(3) 0.3111(3) 0.1544(2) 0.0602(9) Uani 1 1 d . . . H21 H -0.2690 0.2739 0.2135 0.072 Uiso 1 1 calc R . . C22 C -0.3627(4) 0.4133(3) 0.1623(3) 0.0674(10) Uani 1 1 d . . . H22 H -0.4075 0.4461 0.2242 0.081 Uiso 1 1 calc R . . C23 C -0.3781(4) 0.4687(3) 0.0751(3) 0.0703(10) Uani 1 1 d . . . H23 H -0.4327 0.5416 0.0764 0.084 Uiso 1 1 calc R . . C24 C -0.3146(3) 0.4177(3) -0.0116(3) 0.0600(9) Uani 1 1 d . . . H24 H -0.3251 0.4556 -0.0708 0.072 Uiso 1 1 calc R . . C30 C -0.1874(4) 0.3127(3) -0.3867(2) 0.0544(8) Uani 1 1 d . . . C31 C -0.4021(4) 0.3378(3) -0.3403(3) 0.0721(10) Uani 1 1 d . . . H31 H -0.4754 0.3333 -0.2906 0.087 Uiso 1 1 calc R A . C32 C -0.4152(5) 0.3782(4) -0.4307(4) 0.0869(13) Uani 1 1 d . A . H32 H -0.4949 0.4009 -0.4434 0.104 Uiso 1 1 calc R . . C33 C -0.3089(5) 0.3845(4) -0.5023(3) 0.0868(13) Uani 1 1 d . . . H33 H -0.3143 0.4109 -0.5660 0.104 Uiso 1 1 calc R A . C34 C -0.1963(4) 0.3532(3) -0.4825(3) 0.0702(11) Uani 1 1 d . A . H34 H -0.1232 0.3582 -0.5322 0.084 Uiso 1 1 calc R . . O1 O 0.0831(3) 0.0187(2) -0.40744(18) 0.0765(7) Uani 0.40 1 d PD A 1 C40 C 0.1641(16) -0.0870(11) -0.3828(9) 0.061(5) Uani 0.40 1 d PD A 1 H40A H 0.1626 -0.0900 -0.3132 0.073 Uiso 0.40 1 calc PR A 1 H40B H 0.1346 -0.1449 -0.3935 0.073 Uiso 0.40 1 calc PR A 1 C41 C 0.2847(13) -0.1004(15) -0.4434(11) 0.073(5) Uani 0.40 1 d PD A 1 H41A H 0.3182 -0.1680 -0.4806 0.087 Uiso 0.40 1 calc PR A 1 H41B H 0.3421 -0.1036 -0.4046 0.087 Uiso 0.40 1 calc PR A 1 C42 C 0.272(2) 0.001(2) -0.5146(14) 0.135(12) Uani 0.40 1 d PD A 1 H42A H 0.2997 0.0545 -0.4940 0.162 Uiso 0.40 1 calc PR A 1 H42B H 0.3226 -0.0206 -0.5826 0.162 Uiso 0.40 1 calc PR A 1 C43 C 0.1362(19) 0.045(2) -0.5072(14) 0.078(6) Uani 0.40 1 d PD A 1 H43A H 0.1087 0.1244 -0.5197 0.093 Uiso 0.40 1 calc PR A 1 H43B H 0.1146 0.0098 -0.5528 0.093 Uiso 0.40 1 calc PR A 1 O1' O 0.0831(3) 0.0187(2) -0.40744(18) 0.0765(7) Uani 0.60 1 d PD A 2 C40' C 0.1416(16) -0.0935(9) -0.3869(12) 0.116(7) Uani 0.60 1 d PD A 2 H40C H 0.1261 -0.1075 -0.3154 0.139 Uiso 0.60 1 calc PR A 2 H40D H 0.1087 -0.1394 -0.4135 0.139 Uiso 0.60 1 calc PR A 2 C41' C 0.2694(17) -0.1139(18) -0.4332(17) 0.175(10) Uani 0.60 1 d PD A 2 H41C H 0.3145 -0.1920 -0.4458 0.209 Uiso 0.60 1 calc PR A 2 H41D H 0.3094 -0.0883 -0.3940 0.209 Uiso 0.60 1 calc PR A 2 C42' C 0.2672(10) -0.0466(15) -0.5312(9) 0.123(5) Uani 0.60 1 d PD A 2 H42C H 0.3479 -0.0326 -0.5626 0.147 Uiso 0.60 1 calc PR A 2 H42D H 0.2485 -0.0827 -0.5781 0.147 Uiso 0.60 1 calc PR A 2 C43' C 0.1623(15) 0.0542(16) -0.4937(10) 0.114(8) Uani 0.60 1 d PD A 2 H43C H 0.1943 0.1075 -0.4771 0.137 Uiso 0.60 1 calc PR A 2 H43D H 0.1157 0.0873 -0.5426 0.137 Uiso 0.60 1 calc PR A 2 O2 O -0.0044(3) 0.4254(2) -0.21432(18) 0.0708(7) Uani 0.45 1 d PD A 1 C50 C 0.032(2) 0.4020(15) -0.1238(10) 0.079(6) Uani 0.45 1 d PD A 1 H50A H 0.0719 0.3234 -0.1146 0.095 Uiso 0.45 1 calc PR A 1 H50B H -0.0425 0.4295 -0.0664 0.095 Uiso 0.45 1 calc PR A 1 C51 C 0.1244(15) 0.4622(12) -0.1394(11) 0.073(4) Uani 0.45 1 d PD A 1 H51A H 0.0801 0.5367 -0.1147 0.087 Uiso 0.45 1 calc PR A 1 H51B H 0.1889 0.4243 -0.1048 0.087 Uiso 0.45 1 calc PR A 1 C52 C 0.1821(17) 0.464(2) -0.2436(15) 0.121(10) Uani 0.45 1 d PD A 1 H52A H 0.2624 0.4029 -0.2623 0.145 Uiso 0.45 1 calc PR A 1 H52B H 0.1997 0.5325 -0.2647 0.145 Uiso 0.45 1 calc PR A 1 C53 C 0.0894(19) 0.454(2) -0.2897(9) 0.090(11) Uani 0.45 1 d PD A 1 H53A H 0.0515 0.5235 -0.3212 0.108 Uiso 0.45 1 calc PR A 1 H53B H 0.1318 0.3976 -0.3402 0.108 Uiso 0.45 1 calc PR A 1 O2' O -0.0044(3) 0.4254(2) -0.21432(18) 0.0708(7) Uani 0.55 1 d PD A 2 C50' C 0.0063(16) 0.4431(12) -0.1203(8) 0.076(5) Uani 0.55 1 d PD A 2 H50C H -0.0307 0.3977 -0.0681 0.092 Uiso 0.55 1 calc PR A 2 H50D H -0.0357 0.5201 -0.1020 0.092 Uiso 0.55 1 calc PR A 2 C51' C 0.1473(18) 0.4099(16) -0.1383(16) 0.155(9) Uani 0.55 1 d PD A 2 H51C H 0.1672 0.4578 -0.1027 0.186 Uiso 0.55 1 calc PR A 2 H51D H 0.1803 0.3345 -0.1146 0.186 Uiso 0.55 1 calc PR A 2 C52' C 0.2040(13) 0.4182(16) -0.2419(14) 0.088(5) Uani 0.55 1 d PD A 2 H52C H 0.2695 0.3487 -0.2668 0.106 Uiso 0.55 1 calc PR A 2 H52D H 0.2435 0.4754 -0.2565 0.106 Uiso 0.55 1 calc PR A 2 C53' C 0.0996(12) 0.4460(14) -0.2883(9) 0.076(7) Uani 0.55 1 d PD A 2 H53C H 0.0759 0.5230 -0.3096 0.091 Uiso 0.55 1 calc PR A 2 H53D H 0.1256 0.4006 -0.3460 0.091 Uiso 0.55 1 calc PR A 2 O3 O -0.4480(2) 0.2258(2) -0.10844(19) 0.0737(7) Uani 0.40 1 d PD A 1 C60 C -0.537(3) 0.199(3) -0.1330(13) 0.140(14) Uani 0.40 1 d PD A 1 H60A H -0.4967 0.1523 -0.1909 0.168 Uiso 0.40 1 calc PR A 1 H60B H -0.6006 0.2655 -0.1494 0.168 Uiso 0.40 1 calc PR A 1 C61 C -0.599(3) 0.141(3) -0.0478(16) 0.139(15) Uani 0.40 1 d PD A 1 H61A H -0.6914 0.1679 -0.0362 0.167 Uiso 0.40 1 calc PR A 1 H61B H -0.5662 0.0625 -0.0587 0.167 Uiso 0.40 1 calc PR A 1 C62 C -0.567(3) 0.166(3) 0.0329(15) 0.188(19) Uani 0.40 1 d PD A 1 H62A H -0.5379 0.0989 0.0716 0.226 Uiso 0.40 1 calc PR A 1 H62B H -0.6408 0.2180 0.0764 0.226 Uiso 0.40 1 calc PR A 1 C63 C -0.466(3) 0.211(2) -0.0075(8) 0.106(12) Uani 0.40 1 d PD A 1 H63A H -0.4893 0.2814 0.0231 0.127 Uiso 0.40 1 calc PR A 1 H63B H -0.3876 0.1618 0.0060 0.127 Uiso 0.40 1 calc PR A 1 O3' O -0.4480(2) 0.2258(2) -0.10844(19) 0.0737(7) Uani 0.60 1 d PD A 2 C60' C -0.5127(19) 0.1662(19) -0.1324(13) 0.133(8) Uani 0.60 1 d PD A 2 H60C H -0.4571 0.0903 -0.1460 0.160 Uiso 0.60 1 calc PR A 2 H60D H -0.5397 0.1981 -0.1915 0.160 Uiso 0.60 1 calc PR A 2 C61' C -0.625(2) 0.170(3) -0.0469(17) 0.145(11) Uani 0.60 1 d PD A 2 H61C H -0.7037 0.2207 -0.0597 0.174 Uiso 0.60 1 calc PR A 2 H61D H -0.6336 0.0974 -0.0305 0.174 Uiso 0.60 1 calc PR A 2 C62' C -0.596(2) 0.208(2) 0.0297(11) 0.188(11) Uani 0.60 1 d PD A 2 H62C H -0.6101 0.1629 0.0899 0.226 Uiso 0.60 1 calc PR A 2 H62D H -0.6502 0.2841 0.0452 0.226 Uiso 0.60 1 calc PR A 2 C63' C -0.4624(19) 0.199(2) -0.0092(9) 0.161(13) Uani 0.60 1 d PD A 2 H63C H -0.4433 0.2509 0.0231 0.194 Uiso 0.60 1 calc PR A 2 H63D H -0.4067 0.1251 0.0000 0.194 Uiso 0.60 1 calc PR A 2 O4 O -0.2984(9) 0.6113(5) -0.3189(5) 0.210(3) Uani 1 1 d . B 1 C70 C -0.1796(6) 0.6158(6) -0.4040(6) 0.134(2) Uani 1 1 d . B 1 H70A H -0.1189 0.6298 -0.3773 0.160 Uiso 1 1 calc R B 1 H70B H -0.1376 0.5455 -0.4376 0.160 Uiso 1 1 calc R B 1 C71 C -0.2137(5) 0.6914(5) -0.4651(4) 0.0988(17) Uani 1 1 d . B 1 H71A H -0.1638 0.6675 -0.5327 0.119 Uiso 1 1 calc R B 1 H71B H -0.1968 0.7562 -0.4532 0.119 Uiso 1 1 calc R B 1 C72 C -0.3338(8) 0.7162(6) -0.4562(5) 0.142(2) Uani 1 1 d . B 1 H72A H -0.3428 0.6940 -0.5161 0.170 Uiso 1 1 calc R B 1 H72B H -0.3737 0.7958 -0.4519 0.170 Uiso 1 1 calc R B 1 C73 C -0.4005(6) 0.6671(6) -0.3725(5) 0.128(2) Uani 1 1 d . B 1 H73A H -0.4297 0.6137 -0.3923 0.154 Uiso 1 1 calc R B 1 H73B H -0.4739 0.7221 -0.3310 0.154 Uiso 1 1 calc R B 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 0.0443(2) 0.04293(19) 0.03852(17) 0.00760(12) -0.01696(13) -0.01186(14) N1 0.0414(15) 0.0529(15) 0.0456(13) 0.0108(11) -0.0155(11) -0.0166(12) N2 0.0517(15) 0.0488(15) 0.0435(13) 0.0098(11) -0.0219(11) -0.0206(12) N3 0.0463(15) 0.0407(14) 0.0514(14) 0.0083(11) -0.0220(12) -0.0106(12) N4 0.0426(15) 0.0544(15) 0.0475(14) 0.0028(11) -0.0181(11) -0.0134(12) N5 0.0493(15) 0.0461(15) 0.0540(15) 0.0060(11) -0.0204(12) -0.0175(12) N6 0.0496(15) 0.0470(15) 0.0488(14) -0.0009(11) -0.0160(12) -0.0103(12) N7 0.065(2) 0.0683(19) 0.0521(16) 0.0190(14) -0.0263(15) -0.0263(16) N8 0.0629(18) 0.0542(17) 0.0600(16) 0.0139(13) -0.0316(15) -0.0179(14) Li1 0.055(3) 0.053(3) 0.044(3) 0.009(2) -0.020(2) -0.017(3) Li2 0.058(3) 0.062(3) 0.047(3) 0.010(2) -0.023(2) -0.023(3) Li3 0.059(3) 0.056(3) 0.057(3) 0.017(2) -0.027(3) -0.030(3) Li4 0.049(3) 0.062(3) 0.056(3) 0.012(2) -0.027(2) -0.019(3) C1 0.0507(19) 0.0511(18) 0.0391(15) 0.0025(13) -0.0182(13) -0.0191(15) C2 0.053(2) 0.062(2) 0.068(2) 0.0055(17) -0.0257(17) -0.0127(18) C3 0.040(2) 0.086(3) 0.096(3) 0.004(2) -0.0200(19) -0.018(2) C4 0.051(2) 0.082(3) 0.085(3) 0.007(2) -0.0148(19) -0.031(2) C5 0.052(2) 0.066(2) 0.060(2) 0.0104(16) -0.0139(16) -0.0247(18) C10 0.0450(17) 0.0500(18) 0.0393(15) 0.0051(13) -0.0108(13) -0.0186(14) C11 0.061(2) 0.049(2) 0.087(3) 0.0063(18) -0.029(2) -0.0164(18) C12 0.079(3) 0.056(2) 0.110(3) -0.002(2) -0.037(2) -0.029(2) C13 0.074(3) 0.074(3) 0.083(3) -0.005(2) -0.033(2) -0.034(2) C14 0.058(2) 0.065(2) 0.0574(19) 0.0032(16) -0.0243(16) -0.0260(18) C20 0.0395(16) 0.0426(16) 0.0556(18) 0.0038(14) -0.0195(14) -0.0143(14) C21 0.062(2) 0.061(2) 0.0521(19) -0.0050(16) -0.0145(16) -0.0140(18) C22 0.058(2) 0.066(2) 0.073(2) -0.0166(19) -0.0096(18) -0.019(2) C23 0.055(2) 0.048(2) 0.100(3) -0.014(2) -0.020(2) -0.0053(17) C24 0.056(2) 0.0471(19) 0.075(2) 0.0070(17) -0.0268(18) -0.0095(16) C30 0.073(2) 0.0456(18) 0.0521(18) 0.0105(14) -0.0326(17) -0.0200(17) C31 0.069(3) 0.064(2) 0.088(3) 0.012(2) -0.041(2) -0.017(2) C32 0.096(3) 0.080(3) 0.104(3) 0.022(2) -0.070(3) -0.024(3) C33 0.120(4) 0.085(3) 0.072(3) 0.027(2) -0.064(3) -0.032(3) C34 0.100(3) 0.066(2) 0.056(2) 0.0226(17) -0.041(2) -0.033(2) O1 0.0788(18) 0.090(2) 0.0587(15) 0.0045(14) -0.0164(13) -0.0306(16) C40 0.092(14) 0.068(10) 0.034(5) 0.007(6) -0.020(7) -0.041(10) C41 0.048(8) 0.087(11) 0.070(8) -0.032(8) -0.021(6) 0.006(7) C42 0.15(2) 0.21(3) 0.061(9) -0.044(13) 0.008(11) -0.10(2) C43 0.058(8) 0.115(13) 0.038(7) 0.011(8) -0.010(6) -0.011(8) O1' 0.0788(18) 0.090(2) 0.0587(15) 0.0045(14) -0.0164(13) -0.0306(16) C40' 0.079(8) 0.088(10) 0.151(13) -0.057(8) 0.001(7) -0.004(7) C41' 0.15(2) 0.136(16) 0.22(2) 0.008(14) -0.052(18) -0.041(15) C42' 0.068(6) 0.179(14) 0.080(8) -0.024(8) 0.003(5) -0.004(7) C43' 0.096(13) 0.165(13) 0.051(7) -0.012(6) -0.003(8) -0.020(10) O2 0.0849(19) 0.0839(18) 0.0644(15) 0.0140(13) -0.0293(13) -0.0512(16) C50 0.115(13) 0.077(13) 0.066(7) -0.007(7) -0.025(7) -0.056(10) C51 0.079(9) 0.087(9) 0.073(7) 0.011(6) -0.045(6) -0.036(7) C52 0.099(14) 0.16(3) 0.131(16) -0.020(14) -0.020(12) -0.088(17) C53 0.13(2) 0.115(19) 0.070(14) 0.000(10) -0.039(13) -0.084(15) O2' 0.0849(19) 0.0839(18) 0.0644(15) 0.0140(13) -0.0293(13) -0.0512(16) C50' 0.121(10) 0.070(10) 0.059(5) 0.004(5) -0.026(5) -0.059(8) C51' 0.113(12) 0.20(2) 0.176(16) 0.084(16) -0.098(12) -0.059(15) C52' 0.069(7) 0.093(10) 0.111(10) -0.021(6) -0.024(6) -0.032(6) C53' 0.071(10) 0.055(8) 0.072(11) 0.021(6) 0.003(7) -0.016(7) O3 0.0646(17) 0.096(2) 0.0720(16) 0.0177(14) -0.0259(13) -0.0411(15) C60 0.093(13) 0.29(4) 0.089(14) 0.070(17) -0.054(12) -0.13(2) C61 0.18(3) 0.18(3) 0.13(2) 0.073(17) -0.06(2) -0.15(3) C62 0.20(3) 0.33(4) 0.14(2) 0.17(3) -0.12(2) -0.22(3) C63 0.17(3) 0.148(19) 0.037(9) 0.023(10) -0.010(11) -0.119(19) O3' 0.0646(17) 0.096(2) 0.0720(16) 0.0177(14) -0.0259(13) -0.0411(15) C60' 0.131(14) 0.158(12) 0.148(16) -0.040(11) -0.027(10) -0.092(11) C61' 0.075(8) 0.19(2) 0.18(2) 0.030(15) -0.045(10) -0.062(10) C62' 0.177(17) 0.28(2) 0.117(14) -0.048(14) 0.055(13) -0.161(17) C63' 0.138(19) 0.30(3) 0.115(16) 0.083(16) -0.071(13) -0.15(2) O4 0.309(9) 0.183(6) 0.161(5) 0.029(4) -0.083(6) -0.106(6) C70 0.097(4) 0.145(6) 0.165(7) -0.049(5) -0.014(5) -0.051(4) C71 0.074(3) 0.100(4) 0.111(4) 0.029(3) -0.005(3) -0.046(3) C72 0.162(7) 0.159(6) 0.101(4) 0.035(4) -0.027(4) -0.073(6) C73 0.120(5) 0.137(5) 0.118(5) 0.010(4) -0.022(4) -0.047(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 N1 1.854(2) . ? As1 N2 1.855(2) . ? As1 N3 1.860(2) . ? As1 Li1 2.714(5) . ? As1 Li2 2.835(5) . ? As1 Li3 2.867(5) . ? As1 Li1 2.871(5) 2 ? As1 Li4 2.917(5) . ? N1 C1 1.331(4) . ? N1 Li3 2.060(6) . ? N1 Li2 2.135(6) . ? N2 C10 1.344(4) . ? N2 Li4 2.069(6) . ? N2 Li2 2.100(6) . ? N3 C20 1.344(4) . ? N3 Li3 2.079(6) . ? N3 Li4 2.120(6) . ? N4 C2 1.358(4) . ? N4 C1 1.381(4) . ? N4 Li1 2.089(6) 2 ? N5 C11 1.351(4) . ? N5 C10 1.371(4) . ? N5 Li1 2.087(6) 2 ? N6 C21 1.347(4) . ? N6 C20 1.370(4) . ? N6 Li1 2.097(6) . ? N7 C30 1.342(4) . ? N7 Li2 2.028(6) . ? N7 Li3 2.051(6) . ? N7 H1N 0.877(10) . ? N8 C31 1.342(5) . ? N8 C30 1.362(4) . ? N8 Li4 2.061(6) . ? Li1 N5 2.087(6) 2 ? Li1 N4 2.089(6) 2 ? Li1 As1 2.871(5) 2 ? Li2 O1 1.920(6) . ? Li2 Li3 2.589(8) . ? Li2 Li4 2.920(8) . ? Li3 O2 1.971(6) . ? Li3 C50 2.747(14) . ? Li3 Li4 2.978(8) . ? Li4 O3 1.985(6) . ? C1 C5 1.423(4) . ? C2 C3 1.362(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(6) . ? C3 H3 0.9500 . ? C4 C5 1.346(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C10 C14 1.426(4) . ? C11 C12 1.372(5) . ? C11 H11 0.9500 . ? C12 C13 1.395(6) . ? C12 H12 0.9500 . ? C13 C14 1.357(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C20 C24 1.418(4) . ? C21 C22 1.348(5) . ? C21 H21 0.9500 . ? C22 C23 1.396(6) . ? C22 H22 0.9500 . ? C23 C24 1.357(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C30 C34 1.432(4) . ? C31 C32 1.373(6) . ? C31 H31 0.9500 . ? C32 C33 1.375(6) . ? C32 H32 0.9500 . ? C33 C34 1.356(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O1 C43 1.427(13) . ? O1 C40 1.460(12) . ? C40 C41 1.381(14) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.568(17) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.47(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C40' C41' 1.390(14) . ? C40' H40C 0.9900 . ? C40' H40D 0.9900 . ? C41' C42' 1.568(15) . ? C41' H41C 0.9900 . ? C41' H41D 0.9900 . ? C42' C43' 1.485(17) . ? C42' H42C 0.9900 . ? C42' H42D 0.9900 . ? C43' H43C 0.9900 . ? C43' H43D 0.9900 . ? O2 C53 1.409(12) . ? O2 C50 1.453(12) . ? C50 C51 1.518(14) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.439(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.492(13) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C50' C51' 1.510(14) . ? C50' H50C 0.9900 . ? C50' H50D 0.9900 . ? C51' C52' 1.437(13) . ? C51' H51C 0.9900 . ? C51' H51D 0.9900 . ? C52' C53' 1.493(12) . ? C52' H52C 0.9900 . ? C52' H52D 0.9900 . ? C53' H53C 0.9900 . ? C53' H53D 0.9900 . ? O3 C60 1.370(12) . ? O3 C63 1.396(10) . ? C60 C61 1.486(17) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.429(15) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.444(16) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C60' C61' 1.492(16) . ? C60' H60C 0.9900 . ? C60' H60D 0.9900 . ? C61' C62' 1.440(14) . ? C61' H61C 0.9900 . ? C61' H61D 0.9900 . ? C62' C63' 1.473(15) . ? C62' H62C 0.9900 . ? C62' H62D 0.9900 . ? C63' H63C 0.9900 . ? C63' H63D 0.9900 . ? O4 C73 1.548(9) . ? O4 C70 1.562(9) . ? C70 C71 1.281(9) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.307(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.436(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? 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 96.33(11) . . ? N1 As1 N3 91.46(11) . . ? N2 As1 N3 91.23(11) . . ? N1 As1 Li1 131.15(14) . . ? N2 As1 Li1 131.62(14) . . ? N3 As1 Li1 95.59(14) . . ? N1 As1 Li2 48.85(14) . . ? N2 As1 Li2 47.79(13) . . ? N3 As1 Li2 87.55(14) . . ? Li1 As1 Li2 176.84(16) . . ? N1 As1 Li3 45.80(14) . . ? N2 As1 Li3 88.81(13) . . ? N3 As1 Li3 46.40(14) . . ? Li1 As1 Li3 128.73(16) . . ? Li2 As1 Li3 54.01(16) . . ? N1 As1 Li1 91.02(13) . 2 ? N2 As1 Li1 91.82(13) . 2 ? N3 As1 Li1 175.84(13) . 2 ? Li1 As1 Li1 80.26(17) . 2 ? Li2 As1 Li1 96.60(15) . 2 ? Li3 As1 Li1 136.51(16) . 2 ? N1 As1 Li4 98.06(13) . . ? N2 As1 Li4 44.88(14) . . ? N3 As1 Li4 46.45(14) . . ? Li1 As1 Li4 121.18(16) . . ? Li2 As1 Li4 61.00(16) . . ? Li3 As1 Li4 61.97(15) . . ? Li1 As1 Li4 136.35(16) 2 . ? C1 N1 As1 120.0(2) . . ? C1 N1 Li3 144.4(3) . . ? As1 N1 Li3 94.00(18) . . ? C1 N1 Li2 111.0(2) . . ? As1 N1 Li2 90.30(18) . . ? Li3 N1 Li2 76.2(2) . . ? C10 N2 As1 118.2(2) . . ? C10 N2 Li4 138.4(3) . . ? As1 N2 Li4 95.88(19) . . ? C10 N2 Li2 111.7(2) . . ? As1 N2 Li2 91.36(18) . . ? Li4 N2 Li2 88.9(2) . . ? C20 N3 As1 117.92(19) . . ? C20 N3 Li3 130.3(3) . . ? As1 N3 Li3 93.22(19) . . ? C20 N3 Li4 122.0(2) . . ? As1 N3 Li4 94.06(18) . . ? Li3 N3 Li4 90.3(2) . . ? C2 N4 C1 117.0(3) . . ? C2 N4 Li1 114.0(3) . 2 ? C1 N4 Li1 128.2(2) . 2 ? C11 N5 C10 117.6(3) . . ? C11 N5 Li1 112.0(3) . 2 ? C10 N5 Li1 129.1(2) . 2 ? C21 N6 C20 117.9(3) . . ? C21 N6 Li1 113.3(3) . . ? C20 N6 Li1 128.8(2) . . ? C30 N7 Li2 116.8(3) . . ? C30 N7 Li3 128.0(3) . . ? Li2 N7 Li3 78.8(2) . . ? C30 N7 H1N 108(2) . . ? Li2 N7 H1N 108(2) . . ? Li3 N7 H1N 114(2) . . ? C31 N8 C30 118.5(3) . . ? C31 N8 Li4 121.8(3) . . ? C30 N8 Li4 119.4(3) . . ? N5 Li1 N4 119.0(2) 2 2 ? N5 Li1 N6 108.7(3) 2 . ? N4 Li1 N6 108.9(3) 2 . ? N5 Li1 As1 116.6(2) 2 . ? N4 Li1 As1 118.3(2) 2 . ? N6 Li1 As1 75.46(16) . . ? N5 Li1 As1 72.68(16) 2 2 ? N4 Li1 As1 73.84(17) 2 2 ? N6 Li1 As1 175.2(2) . 2 ? As1 Li1 As1 99.74(17) . 2 ? O1 Li2 N7 116.6(3) . . ? O1 Li2 N2 116.5(3) . . ? N7 Li2 N2 118.6(3) . . ? O1 Li2 N1 118.3(3) . . ? N7 Li2 N1 98.6(3) . . ? N2 Li2 N1 81.5(2) . . ? O1 Li2 Li3 149.3(3) . . ? N7 Li2 Li3 50.99(19) . . ? N2 Li2 Li3 91.7(2) . . ? N1 Li2 Li3 50.60(18) . . ? O1 Li2 As1 130.8(3) . . ? N7 Li2 As1 111.2(2) . . ? N2 Li2 As1 40.85(11) . . ? N1 Li2 As1 40.86(11) . . ? Li3 Li2 As1 63.62(16) . . ? O1 Li2 Li4 144.1(3) . . ? N7 Li2 Li4 73.7(2) . . ? N2 Li2 Li4 45.11(16) . . ? N1 Li2 Li4 91.7(2) . . ? Li3 Li2 Li4 65.1(2) . . ? As1 Li2 Li4 60.89(15) . . ? O2 Li3 N7 120.8(3) . . ? O2 Li3 N1 115.2(3) . . ? N7 Li3 N1 100.3(3) . . ? O2 Li3 N3 114.5(3) . . ? N7 Li3 N3 117.3(3) . . ? N1 Li3 N3 80.0(2) . . ? O2 Li3 Li2 151.8(3) . . ? N7 Li3 Li2 50.22(18) . . ? N1 Li3 Li2 53.19(19) . . ? N3 Li3 Li2 90.1(2) . . ? O2 Li3 C50 30.6(3) . . ? N7 Li3 C50 149.9(4) . . ? N1 Li3 C50 92.5(4) . . ? N3 Li3 C50 91.6(4) . . ? Li2 Li3 C50 144.7(5) . . ? O2 Li3 As1 128.7(2) . . ? N7 Li3 As1 109.3(2) . . ? N1 Li3 As1 40.19(11) . . ? N3 Li3 As1 40.38(11) . . ? Li2 Li3 As1 62.37(16) . . ? C50 Li3 As1 98.1(3) . . ? O2 Li3 Li4 144.8(3) . . ? N7 Li3 Li4 72.1(2) . . ? N1 Li3 Li4 91.7(2) . . ? N3 Li3 Li4 45.38(16) . . ? Li2 Li3 Li4 62.8(2) . . ? C50 Li3 Li4 135.0(4) . . ? As1 Li3 Li4 59.85(14) . . ? O3 Li4 N8 106.8(3) . . ? O3 Li4 N2 113.2(3) . . ? N8 Li4 N2 120.2(3) . . ? O3 Li4 N3 113.9(3) . . ? N8 Li4 N3 122.3(3) . . ? N2 Li4 N3 78.6(2) . . ? O3 Li4 As1 119.1(2) . . ? N8 Li4 As1 134.1(3) . . ? N2 Li4 As1 39.23(11) . . ? N3 Li4 As1 39.49(11) . . ? O3 Li4 Li2 153.8(3) . . ? N8 Li4 Li2 80.0(2) . . ? N2 Li4 Li2 45.98(16) . . ? N3 Li4 Li2 80.8(2) . . ? As1 Li4 Li2 58.11(14) . . ? O3 Li4 Li3 152.5(3) . . ? N8 Li4 Li3 82.2(2) . . ? N2 Li4 Li3 82.0(2) . . ? N3 Li4 Li3 44.29(16) . . ? As1 Li4 Li3 58.18(14) . . ? Li2 Li4 Li3 52.07(18) . . ? N1 C1 N4 122.7(3) . . ? N1 C1 C5 118.7(3) . . ? N4 C1 C5 118.5(3) . . ? N4 C2 C3 125.3(3) . . ? N4 C2 H2 117.3 . . ? C3 C2 H2 117.3 . . ? C2 C3 C4 117.9(4) . . ? C2 C3 H3 121.1 . . ? C4 C3 H3 121.1 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C1 122.0(3) . . ? C4 C5 H5 119.0 . . ? C1 C5 H5 119.0 . . ? N2 C10 N5 122.6(3) . . ? N2 C10 C14 118.4(3) . . ? N5 C10 C14 118.9(3) . . ? N5 C11 C12 125.3(3) . . ? N5 C11 H11 117.3 . . ? C12 C11 H11 117.3 . . ? C11 C12 C13 117.4(4) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C14 C13 C12 119.2(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C10 121.5(3) . . ? C13 C14 H14 119.3 . . ? C10 C14 H14 119.3 . . ? N3 C20 N6 122.2(3) . . ? N3 C20 C24 119.5(3) . . ? N6 C20 C24 118.4(3) . . ? N6 C21 C22 126.1(3) . . ? N6 C21 H21 117.0 . . ? C22 C21 H21 117.0 . . ? C21 C22 C23 116.8(3) . . ? C21 C22 H22 121.6 . . ? C23 C22 H22 121.6 . . ? C24 C23 C22 119.5(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C20 121.3(3) . . ? C23 C24 H24 119.3 . . ? C20 C24 H24 119.3 . . ? N7 C30 N8 117.1(3) . . ? N7 C30 C34 123.9(3) . . ? N8 C30 C34 119.0(3) . . ? N8 C31 C32 124.5(4) . . ? N8 C31 H31 117.8 . . ? C32 C31 H31 117.8 . . ? C31 C32 C33 117.6(4) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C30 120.0(4) . . ? C33 C34 H34 120.0 . . ? C30 C34 H34 120.0 . . ? C43 O1 C40 108.8(9) . . ? C43 O1 Li2 122.6(11) . . ? C40 O1 Li2 122.1(6) . . ? C41 C40 O1 106.9(9) . . ? C41 C40 H40A 110.3 . . ? O1 C40 H40A 110.3 . . ? C41 C40 H40B 110.3 . . ? O1 C40 H40B 110.3 . . ? H40A C40 H40B 108.6 . . ? C40 C41 C42 105.5(10) . . ? C40 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? C40 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.8 . . ? C43 C42 C41 104.6(12) . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42A 110.8 . . ? C43 C42 H42B 110.8 . . ? C41 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? O1 C43 C42 100.6(13) . . ? O1 C43 H43A 111.7 . . ? C42 C43 H43A 111.7 . . ? O1 C43 H43B 111.7 . . ? C42 C43 H43B 111.7 . . ? H43A C43 H43B 109.4 . . ? C41' C40' H40C 110.8 . . ? C41' C40' H40D 110.8 . . ? H40C C40' H40D 108.9 . . ? C40' C41' C42' 101.9(12) . . ? C40' C41' H41C 111.4 . . ? C42' C41' H41C 111.4 . . ? C40' C41' H41D 111.4 . . ? C42' C41' H41D 111.4 . . ? H41C C41' H41D 109.3 . . ? C43' C42' C41' 100.3(10) . . ? C43' C42' H42C 111.7 . . ? C41' C42' H42C 111.7 . . ? C43' C42' H42D 111.7 . . ? C41' C42' H42D 111.7 . . ? H42C C42' H42D 109.5 . . ? C42' C43' H43C 111.0 . . ? C42' C43' H43D 111.0 . . ? H43C C43' H43D 109.0 . . ? C53 O2 C50 110.2(9) . . ? C53 O2 Li3 120.9(8) . . ? C50 O2 Li3 105.7(7) . . ? O2 C50 C51 102.6(9) . . ? O2 C50 Li3 43.7(4) . . ? C51 C50 Li3 140.1(8) . . ? O2 C50 H50A 111.2 . . ? C51 C50 H50A 111.2 . . ? Li3 C50 H50A 74.8 . . ? O2 C50 H50B 111.2 . . ? C51 C50 H50B 111.2 . . ? Li3 C50 H50B 102.7 . . ? H50A C50 H50B 109.2 . . ? C52 C51 C50 105.7(10) . . ? C52 C51 H51A 110.6 . . ? C50 C51 H51A 110.6 . . ? C52 C51 H51B 110.6 . . ? C50 C51 H51B 110.6 . . ? H51A C51 H51B 108.7 . . ? C51 C52 C53 106.0(10) . . ? C51 C52 H52A 110.5 . . ? C53 C52 H52A 110.5 . . ? C51 C52 H52B 110.5 . . ? C53 C52 H52B 110.5 . . ? H52A C52 H52B 108.7 . . ? O2 C53 C52 107.1(10) . . ? O2 C53 H53A 110.3 . . ? C52 C53 H53A 110.3 . . ? O2 C53 H53B 110.3 . . ? C52 C53 H53B 110.3 . . ? H53A C53 H53B 108.6 . . ? C51' C50' H50C 111.2 . . ? C51' C50' H50D 111.2 . . ? H50C C50' H50D 109.1 . . ? C52' C51' C50' 107.9(10) . . ? C52' C51' H51C 110.1 . . ? C50' C51' H51C 110.1 . . ? C52' C51' H51D 110.1 . . ? C50' C51' H51D 110.1 . . ? H51C C51' H51D 108.4 . . ? C51' C52' C53' 106.1(10) . . ? C51' C52' H52C 110.5 . . ? C53' C52' H52C 110.5 . . ? C51' C52' H52D 110.5 . . ? C53' C52' H52D 110.5 . . ? H52C C52' H52D 108.7 . . ? C52' C53' H53C 110.5 . . ? C52' C53' H53D 110.5 . . ? H53C C53' H53D 108.7 . . ? C60 O3 C63 109.1(9) . . ? C60 O3 Li4 131.5(10) . . ? C63 O3 Li4 115.0(10) . . ? O3 C60 C61 108.2(12) . . ? O3 C60 H60A 110.1 . . ? C61 C60 H60A 110.1 . . ? O3 C60 H60B 110.1 . . ? C61 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? C62 C61 C60 104.5(12) . . ? C62 C61 H61A 110.9 . . ? C60 C61 H61A 110.9 . . ? C62 C61 H61B 110.9 . . ? C60 C61 H61B 110.9 . . ? H61A C61 H61B 108.9 . . ? C61 C62 C63 107.1(12) . . ? C61 C62 H62A 110.3 . . ? C63 C62 H62A 110.3 . . ? C61 C62 H62B 110.3 . . ? C63 C62 H62B 110.3 . . ? H62A C62 H62B 108.5 . . ? O3 C63 C62 108.5(11) . . ? O3 C63 H63A 110.0 . . ? C62 C63 H63A 110.0 . . ? O3 C63 H63B 110.0 . . ? C62 C63 H63B 110.0 . . ? H63A C63 H63B 108.4 . . ? C61' C60' H60C 110.2 . . ? C61' C60' H60D 110.2 . . ? H60C C60' H60D 108.5 . . ? C62' C61' C60' 102.2(10) . . ? C62' C61' H61C 111.3 . . ? C60' C61' H61C 111.3 . . ? C62' C61' H61D 111.3 . . ? C60' C61' H61D 111.3 . . ? H61C C61' H61D 109.2 . . ? C61' C62' C63' 105.4(12) . . ? C61' C62' H62C 110.7 . . ? C63' C62' H62C 110.7 . . ? C61' C62' H62D 110.7 . . ? C63' C62' H62D 110.7 . . ? H62C C62' H62D 108.8 . . ? C62' C63' H63C 111.1 . . ? C62' C63' H63D 111.1 . . ? H63C C63' H63D 109.1 . . ? C73 O4 C70 98.8(5) . . ? C71 C70 O4 109.3(6) . . ? C71 C70 H70A 109.8 . . ? O4 C70 H70A 109.8 . . ? C71 C70 H70B 109.8 . . ? O4 C70 H70B 109.8 . . ? H70A C70 H70B 108.3 . . ? C70 C71 C72 110.7(5) . . ? C70 C71 H71A 109.5 . . ? C72 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 108.1 . . ? C71 C72 C73 114.2(6) . . ? C71 C72 H72A 108.7 . . ? C73 C72 H72A 108.7 . . ? C71 C72 H72B 108.7 . . ? C73 C72 H72B 108.7 . . ? H72A C72 H72B 107.6 . . ? C72 C73 O4 102.1(6) . . ? C72 C73 H73A 111.3 . . ? O4 C73 H73A 111.3 . . ? C72 C73 H73B 111.3 . . ? O4 C73 H73B 111.3 . . ? H73A C73 H73B 109.2 . . ? #===END