Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DSW1000@CUS.CAM.AC.UK _publ_contact_author_name 'Dr Dominic S. Wright' _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name D.S.Wright A.Bashall F.Garcia A.A.Hopkins M.McPartlin ; J.A.Wood ; A.D.Woods data_sx468 _database_code_CSD 197231 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H68 As Li N2 O P4' _chemical_formula_weight 726.64 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.204(4) _cell_length_b 19.464(6) _cell_length_c 21.771(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8138(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_process_details psi-scans _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5296 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_sigmaI/netI 0.2982 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4317 _reflns_number_gt 1457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4317 _refine_ls_number_parameters 370 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.2643 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.91893(8) 0.57052(7) 0.60448(6) 0.0634(5) Uani 1 1 d . C . P1 P 0.98069(18) 0.64166(18) 0.66565(14) 0.0488(11) Uani 1 1 d . . . P2 P 0.91168(19) 0.72954(18) 0.68299(14) 0.0521(11) Uani 1 1 d . . . P3 P 0.80464(19) 0.6874(2) 0.68547(15) 0.0624(13) Uani 1 1 d . C . P4 P 0.80482(19) 0.59088(19) 0.63457(16) 0.0691(13) Uani 1 1 d D . . C11 C 0.9840(7) 0.6089(7) 0.7472(5) 0.058(4) Uani 1 1 d . B . H11 H 0.9362 0.6047 0.7627 0.070 Uiso 1 1 calc R . . C12 C 1.0185(7) 0.5399(7) 0.7513(6) 0.088(5) Uani 1 1 d . . . H12A H 0.9899 0.5075 0.7287 0.105 Uiso 0.65 1 calc PR A 1 H12B H 1.0626 0.5431 0.7298 0.105 Uiso 0.65 1 calc PR A 1 H12C H 1.0686 0.5429 0.7461 0.105 Uiso 0.35 1 calc PR A 2 H12D H 0.9994 0.5074 0.7221 0.105 Uiso 0.35 1 calc PR A 2 C13 C 1.0326(10) 0.5095(11) 0.8130(10) 0.058(6) Uiso 0.65 1 d P B 1 H13A H 1.0659 0.4724 0.8087 0.070 Uiso 0.65 1 calc PR B 1 H13B H 0.9898 0.4904 0.8293 0.070 Uiso 0.65 1 calc PR B 1 C13' C 0.9957(19) 0.521(2) 0.8243(17) 0.058(6) Uiso 0.35 1 d P B 2 H13C H 0.9507 0.5400 0.8353 0.070 Uiso 0.35 1 calc PR B 2 H13D H 0.9966 0.4722 0.8325 0.070 Uiso 0.35 1 calc PR B 2 C14 C 1.0611(7) 0.5625(7) 0.8579(5) 0.093(6) Uani 1 1 d . . . H14A H 1.0549 0.5449 0.8993 0.112 Uiso 0.65 1 calc PR B 1 H14B H 1.1107 0.5670 0.8509 0.112 Uiso 0.65 1 calc PR B 1 H14C H 1.0687 0.5474 0.8998 0.112 Uiso 0.35 1 calc PR B 2 H14D H 1.1040 0.5594 0.8347 0.112 Uiso 0.35 1 calc PR B 2 C15 C 1.0293(7) 0.6321(7) 0.8548(5) 0.071(5) Uani 1 1 d . B . H15A H 1.0569 0.6636 0.8792 0.086 Uiso 1 1 calc R . . H15B H 0.9830 0.6304 0.8725 0.086 Uiso 1 1 calc R . . C16 C 1.0245(6) 0.6593(6) 0.7890(5) 0.050(4) Uani 1 1 d . . . H16A H 1.0710 0.6658 0.7727 0.060 Uiso 1 1 calc R B . H16B H 1.0012 0.7035 0.7891 0.060 Uiso 1 1 calc R . . C21 C 0.9080(6) 0.7720(6) 0.6074(5) 0.045(3) Uani 1 1 d U . . H21 H 0.8896 0.7392 0.5774 0.054 Uiso 1 1 calc R . . C22 C 0.8599(7) 0.8338(6) 0.6093(6) 0.078(4) Uani 1 1 d U . . H22A H 0.8758 0.8651 0.6410 0.094 Uiso 1 1 calc R . . H22B H 0.8134 0.8186 0.6204 0.094 Uiso 1 1 calc R . . C23 C 0.8563(7) 0.8725(8) 0.5478(6) 0.100(6) Uani 1 1 d U . . H23A H 0.8351 0.8432 0.5169 0.120 Uiso 1 1 calc R . . H23B H 0.8275 0.9131 0.5524 0.120 Uiso 1 1 calc R . . C24 C 0.9269(7) 0.8931(6) 0.5273(6) 0.087(5) Uani 1 1 d U . . H24A H 0.9449 0.9277 0.5552 0.104 Uiso 1 1 calc R . . H24B H 0.9236 0.9136 0.4868 0.104 Uiso 1 1 calc R . . C25 C 0.9767(7) 0.8340(7) 0.5249(6) 0.089(5) Uani 1 1 d U . . H25A H 1.0228 0.8510 0.5147 0.107 Uiso 1 1 calc R . . H25B H 0.9625 0.8026 0.4926 0.107 Uiso 1 1 calc R . . C26 C 0.9802(6) 0.7948(6) 0.5863(5) 0.069(4) Uani 1 1 d U . . H26A H 1.0098 0.7547 0.5816 0.083 Uiso 1 1 calc R . . H26B H 1.0007 0.8241 0.6174 0.083 Uiso 1 1 calc R . . C31 C 0.7985(7) 0.6512(8) 0.7654(5) 0.065(5) Uani 1 1 d . . . H31 H 0.8297 0.6113 0.7676 0.078 Uiso 1 1 calc R C . C32 C 0.8210(7) 0.7014(7) 0.8143(5) 0.077(5) Uani 1 1 d . C . H32A H 0.7929 0.7427 0.8112 0.092 Uiso 1 1 calc R . . H32B H 0.8692 0.7143 0.8074 0.092 Uiso 1 1 calc R . . C33 C 0.8137(7) 0.6716(8) 0.8791(6) 0.105(6) Uani 1 1 d . . . H33A H 0.8239 0.7069 0.9092 0.126 Uiso 1 1 calc R C . H33B H 0.8470 0.6346 0.8845 0.126 Uiso 1 1 calc R . . C34 C 0.7399(9) 0.6443(10) 0.8890(7) 0.128(8) Uani 1 1 d . C . H34A H 0.7377 0.6220 0.9288 0.154 Uiso 1 1 calc R . . H34B H 0.7079 0.6829 0.8898 0.154 Uiso 1 1 calc R . . C35 C 0.7165(9) 0.5950(9) 0.8412(7) 0.116(7) Uani 1 1 d . . . H35A H 0.6682 0.5830 0.8484 0.140 Uiso 1 1 calc R C . H35B H 0.7440 0.5533 0.8441 0.140 Uiso 1 1 calc R . . C36 C 0.7240(6) 0.6255(8) 0.7761(6) 0.091(6) Uani 1 1 d . C . H36A H 0.7126 0.5908 0.7459 0.109 Uiso 1 1 calc R . . H36B H 0.6916 0.6634 0.7712 0.109 Uiso 1 1 calc R . . C41 C 0.7771(15) 0.6159(13) 0.5522(10) 0.077(7) Uiso 0.50 1 d PD C 1 H41 H 0.7280 0.6165 0.5643 0.092 Uiso 0.50 1 calc PR C 1 C42 C 0.7704(11) 0.6729(10) 0.5250(9) 0.041(5) Uiso 0.50 1 d PD C 1 H42A H 0.8158 0.6857 0.5091 0.049 Uiso 0.50 1 calc PR C 1 H42B H 0.7581 0.7069 0.5558 0.049 Uiso 0.50 1 calc PR C 1 C43 C 0.7165(12) 0.6796(11) 0.4707(11) 0.078(7) Uiso 0.50 1 d PD C 1 H43A H 0.6714 0.6921 0.4875 0.093 Uiso 0.50 1 calc PR C 1 H43B H 0.7313 0.7163 0.4436 0.093 Uiso 0.50 1 calc PR C 1 C44 C 0.7102(14) 0.6253(12) 0.4403(10) 0.090(8) Uiso 0.50 1 d PD C 1 H44A H 0.6616 0.6240 0.4284 0.108 Uiso 0.50 1 calc PR C 1 H44B H 0.7360 0.6337 0.4027 0.108 Uiso 0.50 1 calc PR C 1 C45 C 0.7245(12) 0.5659(12) 0.4545(10) 0.075(7) Uiso 0.50 1 d PD C 1 H45A H 0.7514 0.5458 0.4213 0.090 Uiso 0.50 1 calc PR C 1 H45B H 0.6814 0.5402 0.4576 0.090 Uiso 0.50 1 calc PR C 1 C46 C 0.7662(12) 0.5561(11) 0.5159(11) 0.072(7) Uiso 0.50 1 d PD C 1 H46A H 0.7417 0.5226 0.5408 0.087 Uiso 0.50 1 calc PR C 1 H46B H 0.8113 0.5367 0.5059 0.087 Uiso 0.50 1 calc PR C 1 C41' C 0.7475(14) 0.6082(14) 0.5678(10) 0.077(7) Uiso 0.50 1 d PD C 2 H41' H 0.7833 0.6237 0.5389 0.092 Uiso 0.50 1 calc PR C 2 C42' C 0.7058(11) 0.6541(10) 0.5600(8) 0.041(5) Uiso 0.50 1 d PD C 2 H42C H 0.7281 0.6965 0.5729 0.049 Uiso 0.50 1 calc PR C 2 H42D H 0.6674 0.6461 0.5881 0.049 Uiso 0.50 1 calc PR C 2 C43' C 0.6723(13) 0.6680(11) 0.4926(10) 0.078(7) Uiso 0.50 1 d PD C 2 H43C H 0.6270 0.6893 0.4972 0.093 Uiso 0.50 1 calc PR C 2 H43D H 0.7020 0.6993 0.4699 0.093 Uiso 0.50 1 calc PR C 2 C44' C 0.6661(14) 0.6125(12) 0.4631(10) 0.090(8) Uiso 0.50 1 d PD C 2 H44C H 0.6210 0.6146 0.4431 0.108 Uiso 0.50 1 calc PR C 2 H44D H 0.7006 0.6141 0.4306 0.108 Uiso 0.50 1 calc PR C 2 C45' C 0.6703(13) 0.5548(11) 0.4858(10) 0.075(7) Uiso 0.50 1 d PD C 2 H45C H 0.6802 0.5221 0.4533 0.090 Uiso 0.50 1 calc PR C 2 H45D H 0.6255 0.5428 0.5032 0.090 Uiso 0.50 1 calc PR C 2 C46' C 0.7271(13) 0.5469(11) 0.5367(11) 0.072(7) Uiso 0.50 1 d PD C 2 H46C H 0.7100 0.5145 0.5671 0.087 Uiso 0.50 1 calc PR C 2 H46D H 0.7682 0.5267 0.5181 0.087 Uiso 0.50 1 calc PR C 2 Li1 Li 0.9390(10) 0.4400(12) 0.6390(9) 0.061(7) Uani 1 1 d . . . O1 O 0.8932(5) 0.4067(6) 0.7138(4) 0.087(4) Uani 1 1 d . C . C51 C 0.8386(15) 0.4432(12) 0.7439(13) 0.085(8) Uiso 0.64 1 d P C 1 H51A H 0.8159 0.4739 0.7151 0.101 Uiso 0.64 1 calc PR C 1 H51B H 0.8575 0.4704 0.7773 0.101 Uiso 0.64 1 calc PR C 1 C51' C 0.817(3) 0.424(3) 0.7180(19) 0.085(8) Uiso 0.36 1 d P C 2 H51C H 0.8105 0.4731 0.7204 0.101 Uiso 0.36 1 calc PR C 2 H51D H 0.7928 0.4073 0.6815 0.101 Uiso 0.36 1 calc PR C 2 C52 C 0.7895(11) 0.3944(14) 0.7673(13) 0.199(13) Uani 1 1 d . . . H52A H 0.7520 0.3860 0.7384 0.239 Uiso 0.64 1 calc PR C 1 H52B H 0.7702 0.4089 0.8064 0.239 Uiso 0.64 1 calc PR C 1 H52C H 0.7414 0.3812 0.7606 0.239 Uiso 0.36 1 calc PR C 2 H52D H 0.7924 0.4243 0.8028 0.239 Uiso 0.36 1 calc PR C 2 C53 C 0.8380(14) 0.3295(12) 0.7746(11) 0.210(15) Uani 1 1 d . C . H53A H 0.8407 0.3152 0.8172 0.252 Uiso 1 1 calc R . . H53B H 0.8210 0.2914 0.7501 0.252 Uiso 1 1 calc R . . C54 C 0.9026(10) 0.3518(10) 0.7535(8) 0.136(8) Uani 1 1 d . . . H54A H 0.9314 0.3657 0.7879 0.163 Uiso 1 1 calc R C . H54B H 0.9261 0.3146 0.7322 0.163 Uiso 1 1 calc R . . N1 N 0.9080(7) 0.3697(7) 0.5692(5) 0.083(4) Uani 1 1 d . C . N2 N 1.0399(6) 0.3986(7) 0.6281(6) 0.076(4) Uani 1 1 d . C . C1 C 0.8332(15) 0.3527(17) 0.5745(16) 0.122(14) Uiso 0.51 1 d P C 1 H1A H 0.8062 0.3941 0.5720 0.182 Uiso 0.51 1 calc PR C 1 H1B H 0.8247 0.3305 0.6132 0.182 Uiso 0.51 1 calc PR C 1 H1C H 0.8202 0.3224 0.5416 0.182 Uiso 0.51 1 calc PR C 1 C2 C 0.9084(15) 0.4065(13) 0.5042(11) 0.086(6) Uiso 0.51 1 d P C 1 H2A H 0.8738 0.4420 0.5037 0.130 Uiso 0.51 1 calc PR C 1 H2B H 0.8981 0.3734 0.4728 0.130 Uiso 0.51 1 calc PR C 1 H2C H 0.9534 0.4262 0.4969 0.130 Uiso 0.51 1 calc PR C 1 C3 C 0.954(2) 0.3232(18) 0.5710(17) 0.106(11) Uiso 0.51 1 d P C 1 H3A H 0.9517 0.2992 0.5320 0.127 Uiso 0.51 1 calc PR C 1 H3B H 0.9393 0.2906 0.6022 0.127 Uiso 0.51 1 calc PR C 1 C1' C 0.8760(15) 0.3062(14) 0.6011(13) 0.086(6) Uiso 0.49 1 d P C 2 H1'1 H 0.9070 0.2901 0.6325 0.130 Uiso 0.49 1 calc PR C 2 H1'2 H 0.8688 0.2705 0.5713 0.130 Uiso 0.49 1 calc PR C 2 H1'3 H 0.8322 0.3185 0.6192 0.130 Uiso 0.49 1 calc PR C 2 C2' C 0.8640(15) 0.3912(15) 0.5256(14) 0.086(6) Uiso 0.49 1 d P C 2 H2'1 H 0.8209 0.4050 0.5442 0.130 Uiso 0.49 1 calc PR C 2 H2'2 H 0.8555 0.3546 0.4971 0.130 Uiso 0.49 1 calc PR C 2 H2'3 H 0.8841 0.4296 0.5042 0.130 Uiso 0.49 1 calc PR C 2 C3' C 0.977(2) 0.347(2) 0.5463(15) 0.106(11) Uiso 0.49 1 d P C 2 H3'1 H 0.9695 0.3026 0.5267 0.127 Uiso 0.49 1 calc PR C 2 H3'2 H 0.9901 0.3787 0.5142 0.127 Uiso 0.49 1 calc PR C 2 C4 C 1.0300(9) 0.3404(8) 0.5832(9) 0.115(7) Uani 1 1 d . . . H4A H 1.0532 0.2998 0.5990 0.138 Uiso 0.51 1 calc PR C 1 H4B H 1.0521 0.3525 0.5446 0.138 Uiso 0.51 1 calc PR C 1 H4C H 1.0718 0.3363 0.5585 0.138 Uiso 0.49 1 calc PR C 2 H4D H 1.0248 0.2980 0.6062 0.138 Uiso 0.49 1 calc PR C 2 C5 C 1.0791(8) 0.3752(8) 0.6806(7) 0.147(7) Uani 1 1 d . . . H5A H 1.0531 0.3403 0.7018 0.221 Uiso 1 1 calc R C . H5B H 1.0874 0.4131 0.7078 0.221 Uiso 1 1 calc R . . H5C H 1.1227 0.3565 0.6671 0.221 Uiso 1 1 calc R . . C6 C 1.0821(7) 0.4508(7) 0.5981(6) 0.102(5) Uani 1 1 d . . . H6A H 1.0579 0.4678 0.5626 0.154 Uiso 1 1 calc R C . H6B H 1.1257 0.4311 0.5857 0.154 Uiso 1 1 calc R . . H6C H 1.0904 0.4880 0.6261 0.154 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 0.0839(11) 0.0683(10) 0.0381(8) -0.0020(10) -0.0142(10) -0.0189(12) P1 0.059(2) 0.054(2) 0.033(2) 0.001(2) -0.001(2) -0.015(2) P2 0.062(3) 0.057(3) 0.037(2) 0.000(2) -0.003(2) -0.021(3) P3 0.056(3) 0.085(3) 0.046(2) 0.011(3) -0.001(2) -0.032(3) P4 0.073(3) 0.076(3) 0.058(2) 0.021(2) -0.026(2) -0.032(3) C11 0.072(11) 0.055(10) 0.047(9) 0.009(9) -0.035(9) -0.012(10) C12 0.101(13) 0.112(14) 0.050(10) 0.000(11) -0.024(10) -0.045(13) C14 0.142(16) 0.081(12) 0.056(10) 0.024(10) -0.049(10) -0.008(13) C15 0.085(12) 0.084(13) 0.045(10) 0.010(10) -0.033(9) 0.001(11) C16 0.052(10) 0.048(11) 0.052(9) -0.012(8) -0.003(8) 0.006(9) C21 0.059(9) 0.043(8) 0.032(7) 0.000(7) -0.003(8) -0.010(7) C22 0.101(10) 0.078(11) 0.057(9) 0.015(9) 0.002(9) 0.016(9) C23 0.113(12) 0.119(15) 0.069(11) 0.045(10) -0.013(11) 0.035(12) C24 0.163(16) 0.043(10) 0.054(9) 0.006(8) 0.004(11) -0.013(10) C25 0.095(11) 0.121(14) 0.051(9) 0.042(10) 0.022(9) -0.001(10) C26 0.080(9) 0.072(11) 0.055(8) 0.027(8) 0.020(9) -0.020(8) C31 0.043(10) 0.113(14) 0.038(9) 0.021(9) 0.008(8) -0.007(10) C32 0.078(11) 0.129(15) 0.023(8) 0.027(10) 0.001(9) -0.021(11) C33 0.086(13) 0.175(17) 0.054(12) 0.029(11) 0.002(10) -0.031(13) C34 0.104(15) 0.20(2) 0.080(14) 0.051(16) 0.017(15) -0.039(16) C35 0.101(15) 0.15(2) 0.098(14) 0.057(15) 0.043(13) -0.034(14) C36 0.054(11) 0.139(16) 0.080(12) 0.015(12) 0.012(10) -0.036(11) Li1 0.056(16) 0.069(17) 0.058(14) 0.028(15) 0.003(13) -0.016(15) O1 0.096(9) 0.081(9) 0.084(8) 0.028(7) 0.004(7) -0.009(8) C52 0.16(2) 0.25(3) 0.19(3) 0.03(3) 0.112(19) -0.03(2) C53 0.32(4) 0.18(3) 0.128(19) 0.01(2) 0.11(3) -0.11(3) C54 0.21(3) 0.084(16) 0.118(16) 0.059(13) 0.034(18) 0.005(18) N1 0.086(12) 0.089(11) 0.074(9) -0.001(8) -0.025(9) 0.015(10) N2 0.069(10) 0.087(11) 0.072(9) 0.006(9) 0.005(8) -0.007(9) C4 0.092(16) 0.108(16) 0.145(18) -0.046(14) 0.022(14) 0.042(14) C5 0.188(19) 0.146(17) 0.108(13) 0.014(14) -0.033(16) 0.052(17) C6 0.073(11) 0.121(15) 0.113(13) 0.000(13) 0.003(12) -0.013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 P1 2.258(4) . ? As1 P4 2.321(4) . ? As1 Li1 2.68(2) . ? P1 C11 1.887(12) . ? P1 P2 2.196(5) . ? P2 C21 1.843(11) . ? P2 P3 2.214(5) . ? P3 C31 1.881(11) . ? P3 P4 2.181(5) . ? P4 C41' 1.853(17) . ? P4 C41 1.933(18) . ? C11 C12 1.499(14) . ? C11 C16 1.548(14) . ? C12 C13 1.49(2) . ? C12 C13' 1.69(4) . ? C13 C14 1.52(2) . ? C13' C14 1.66(4) . ? C14 C15 1.487(15) . ? C15 C16 1.530(13) . ? C21 C22 1.517(13) . ? C21 C26 1.525(13) . ? C22 C23 1.538(15) . ? C23 C24 1.482(15) . ? C24 C25 1.498(15) . ? C25 C26 1.542(14) . ? C31 C32 1.510(15) . ? C31 C36 1.534(14) . ? C32 C33 1.530(14) . ? C33 C34 1.530(16) . ? C34 C35 1.486(18) . ? C35 C36 1.543(16) . ? C41 C42 1.26(2) . ? C41 C46 1.42(2) . ? C42 C43 1.577(19) . ? C43 C44 1.253(13) . ? C44 C45 1.228(13) . ? C45 C46 1.571(19) . ? C41' C42' 1.21(2) . ? C41' C46' 1.43(2) . ? C42' C43' 1.624(19) . ? C43' C44' 1.263(13) . ? C44' C45' 1.230(13) . ? C45' C46' 1.56(2) . ? Li1 O1 1.96(2) . ? Li1 N2 2.11(2) . ? Li1 N1 2.13(2) . ? Li1 C3 2.73(4) . ? O1 C54 1.386(15) . ? O1 C51 1.42(3) . ? O1 C51' 1.51(5) . ? C51 C52 1.43(3) . ? C51' C52 1.32(5) . ? C52 C53 1.58(2) . ? C53 C54 1.39(2) . ? N1 C3 1.26(4) . ? N1 C2' 1.34(3) . ? N1 C1 1.48(3) . ? N1 C3' 1.48(4) . ? N1 C1' 1.54(3) . ? N1 C2 1.59(2) . ? N2 C5 1.441(15) . ? N2 C6 1.454(13) . ? N2 C4 1.509(16) . ? C3 C4 1.53(4) . ? C3' C4 1.31(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 As1 P4 102.99(14) . . ? P1 As1 Li1 109.9(5) . . ? P4 As1 Li1 102.6(4) . . ? C11 P1 P2 97.0(5) . . ? C11 P1 As1 111.4(4) . . ? P2 P1 As1 105.19(17) . . ? C21 P2 P1 102.7(4) . . ? C21 P2 P3 98.8(4) . . ? P1 P2 P3 106.01(19) . . ? C31 P3 P4 98.5(5) . . ? C31 P3 P2 102.7(4) . . ? P4 P3 P2 107.8(2) . . ? C41' P4 C41 20.5(16) . . ? C41' P4 P3 103.9(9) . . ? C41 P4 P3 104.7(8) . . ? C41' P4 As1 111.7(10) . . ? C41 P4 As1 92.3(9) . . ? P3 P4 As1 106.97(18) . . ? C12 C11 C16 108.1(10) . . ? C12 C11 P1 111.9(10) . . ? C16 C11 P1 110.8(9) . . ? C13 C12 C11 119.2(14) . . ? C13 C12 C13' 27.6(15) . . ? C11 C12 C13' 97.8(17) . . ? C12 C13 C14 112.0(15) . . ? C14 C13' C12 96.6(19) . . ? C15 C14 C13 116.1(13) . . ? C15 C14 C13' 96.4(17) . . ? C13 C14 C13' 28.0(16) . . ? C14 C15 C16 112.5(11) . . ? C15 C16 C11 111.2(10) . . ? C22 C21 C26 109.4(10) . . ? C22 C21 P2 110.8(9) . . ? C26 C21 P2 111.3(8) . . ? C21 C22 C23 113.1(11) . . ? C24 C23 C22 110.7(12) . . ? C23 C24 C25 112.8(12) . . ? C24 C25 C26 112.2(12) . . ? C21 C26 C25 111.4(10) . . ? C32 C31 C36 111.7(11) . . ? C32 C31 P3 113.1(10) . . ? C36 C31 P3 108.7(9) . . ? C31 C32 C33 112.2(12) . . ? C32 C33 C34 110.3(11) . . ? C35 C34 C33 113.9(16) . . ? C34 C35 C36 111.5(14) . . ? C31 C36 C35 110.7(11) . . ? C42 C41 C46 116.4(17) . . ? C42 C41 P4 133.0(18) . . ? C46 C41 P4 110.5(17) . . ? C41 C42 C43 119.3(17) . . ? C44 C43 C42 113.0(16) . . ? C45 C44 C43 130(2) . . ? C44 C45 C46 116.3(16) . . ? C41 C46 C45 116.6(15) . . ? C42' C41' C46' 111.6(19) . . ? C42' C41' P4 130(2) . . ? C46' C41' P4 112.6(17) . . ? C41' C42' C43' 120.7(17) . . ? C44' C43' C42' 110.8(15) . . ? C45' C44' C43' 125(2) . . ? C44' C45' C46' 114.9(18) . . ? C41' C46' C45' 116.5(15) . . ? O1 Li1 N2 112.2(11) . . ? O1 Li1 N1 104.8(10) . . ? N2 Li1 N1 86.0(10) . . ? O1 Li1 As1 118.8(11) . . ? N2 Li1 As1 117.5(9) . . ? N1 Li1 As1 111.7(9) . . ? O1 Li1 C3 102.8(12) . . ? N2 Li1 C3 61.8(11) . . ? N1 Li1 C3 26.6(9) . . ? As1 Li1 C3 130.8(11) . . ? C54 O1 C51 101.3(14) . . ? C54 O1 C51' 105(2) . . ? C51 O1 C51' 32(2) . . ? C54 O1 Li1 135.5(14) . . ? C51 O1 Li1 123.1(16) . . ? C51' O1 Li1 114(2) . . ? O1 C51 C52 108.4(17) . . ? C52 C51' O1 110(3) . . ? C51' C52 C51 33(2) . . ? C51' C52 C53 101(3) . . ? C51 C52 C53 100.3(19) . . ? C54 C53 C52 104(2) . . ? O1 C54 C53 109(2) . . ? C3 N1 C2' 133(3) . . ? C3 N1 C1 121(2) . . ? C2' N1 C1 60.7(16) . . ? C3 N1 C3' 34(2) . . ? C2' N1 C3' 115(2) . . ? C1 N1 C3' 146(2) . . ? C3 N1 C1' 71.8(19) . . ? C2' N1 C1' 108.5(19) . . ? C1 N1 C1' 53.1(14) . . ? C3' N1 C1' 105(2) . . ? C3 N1 C2 110(2) . . ? C2' N1 C2 39.5(15) . . ? C1 N1 C2 100(2) . . ? C3' N1 C2 80.2(17) . . ? C1' N1 C2 139.7(16) . . ? C3 N1 Li1 104(2) . . ? C2' N1 Li1 118.7(16) . . ? C1 N1 Li1 111.1(16) . . ? C3' N1 Li1 100.7(17) . . ? C1' N1 Li1 107.8(13) . . ? C2 N1 Li1 110.2(13) . . ? C5 N2 C6 106.7(12) . . ? C5 N2 C4 110.0(13) . . ? C6 N2 C4 107.6(11) . . ? C5 N2 Li1 120.7(11) . . ? C6 N2 Li1 107.1(10) . . ? C4 N2 Li1 104.0(11) . . ? N1 C3 C4 121(3) . . ? N1 C3 Li1 49.1(15) . . ? C4 C3 Li1 79.7(16) . . ? C4 C3' N1 121(3) . . ? C3' C4 N2 115(2) . . ? C3' C4 C3 33(2) . . ? N2 C4 C3 113.5(18) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.332 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.075 data_dw0032 _database_code_CSD 197232 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H65 As Li N3 P4' _chemical_formula_weight 673.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.2635(3) _cell_length_b 15.4835(5) _cell_length_c 24.3220(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.165(2) _cell_angle_gamma 90.00 _cell_volume 3842.78(18) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25511 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7905 _exptl_absorpt_correction_T_max 0.8061 #_exptl_absorpt_correction_type 'multiscan' #_exptl_absorpt_process_details 'Sortav Blessing (1995) ' #_exptl_absorpt_correction_T_max 1.000 #_exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 28746 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8768 _reflns_number_gt 5935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0292P)^2^+0.5309P] 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 8768 _refine_ls_number_parameters 362 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 1.00667(2) 0.400092(15) 0.912137(9) 0.03318(8) Uani 1 1 d . . . P1 P 0.81883(6) 0.32786(4) 0.87715(2) 0.03103(15) Uani 1 1 d . . . P2 P 0.88217(6) 0.22373(4) 0.82569(2) 0.03064(15) Uani 1 1 d . . . P3 P 1.07536(6) 0.25929(4) 0.80053(2) 0.03044(14) Uani 1 1 d . . . P4 P 1.17094(6) 0.34084(4) 0.86634(2) 0.03127(15) Uani 1 1 d . . . Li1 Li 1.0830(4) 0.5701(3) 0.89638(15) 0.0407(10) Uani 1 1 d . . . N1 N 1.0779(2) 0.58907(15) 0.81057(8) 0.0492(6) Uani 1 1 d . . . C1 C 0.9489(3) 0.6000(2) 0.78124(12) 0.0692(9) Uani 1 1 d D . . H1A H 0.9552 0.5991 0.7413 0.093(3) Uiso 1 1 calc R . . H1B H 0.9121 0.6553 0.7916 0.093(3) Uiso 1 1 calc R . . H1C H 0.8919 0.5528 0.7909 0.093(3) Uiso 1 1 calc R . . C2 C 1.1671(4) 0.6494(3) 0.79112(14) 0.1258(18) Uani 1 1 d D . . H2A H 1.1631 0.6455 0.7508 0.093(3) Uiso 1 1 calc R . . H2B H 1.2562 0.6363 0.8076 0.093(3) Uiso 1 1 calc R . . H2C H 1.1432 0.7080 0.8016 0.093(3) Uiso 1 1 calc R . . N2 N 1.0071(2) 0.66970(14) 0.94030(8) 0.0474(6) Uani 1 1 d . . . C3 C 0.8804(3) 0.7008(2) 0.91428(12) 0.0651(8) Uani 1 1 d D . . H3A H 0.8473 0.7460 0.9373 0.093(3) Uiso 1 1 calc R . . H3B H 0.8179 0.6527 0.9104 0.093(3) Uiso 1 1 calc R . . H3C H 0.8912 0.7244 0.8777 0.093(3) Uiso 1 1 calc R . . C4 C 1.0986(3) 0.74180(19) 0.95253(13) 0.0719(9) Uani 1 1 d D . . H4A H 1.0575 0.7857 0.9740 0.093(3) Uiso 1 1 calc R . . H4B H 1.1208 0.7672 0.9178 0.093(3) Uiso 1 1 calc R . . H4C H 1.1785 0.7206 0.9739 0.093(3) Uiso 1 1 calc R . . N3 N 1.2740(2) 0.54474(14) 0.93323(8) 0.0464(5) Uani 1 1 d . . . C5 C 1.3836(3) 0.5987(2) 0.92117(13) 0.0749(10) Uani 1 1 d D . . H5A H 1.4654 0.5747 0.9395 0.093(3) Uiso 1 1 calc R . . H5B H 1.3713 0.6574 0.9348 0.093(3) Uiso 1 1 calc R . . H5C H 1.3879 0.6003 0.8811 0.093(3) Uiso 1 1 calc R . . C6 C 1.2750(3) 0.53364(19) 0.99307(10) 0.0612(8) Uani 1 1 d D . . H6A H 1.3577 0.5068 1.0081 0.093(3) Uiso 1 1 calc R . . H6B H 1.2017 0.4966 1.0007 0.093(3) Uiso 1 1 calc R . . H6C H 1.2663 0.5901 1.0105 0.093(3) Uiso 1 1 calc R . . C11 C 0.7273(2) 0.39726(14) 0.82244(9) 0.0320(5) Uani 1 1 d . . . H11 H 0.7874 0.4132 0.7943 0.038 Uiso 1 1 calc R . . C12 C 0.6812(2) 0.47945(15) 0.84917(9) 0.0394(6) Uani 1 1 d . . . H12A H 0.7585 0.5129 0.8650 0.047 Uiso 1 1 calc R . . H12B H 0.6297 0.4637 0.8798 0.047 Uiso 1 1 calc R . . C13 C 0.5971(3) 0.53588(17) 0.80751(10) 0.0487(7) Uani 1 1 d . . . H13A H 0.5653 0.5868 0.8268 0.058 Uiso 1 1 calc R . . H13B H 0.6512 0.5568 0.7789 0.058 Uiso 1 1 calc R . . C14 C 0.4808(2) 0.48575(18) 0.78000(10) 0.0513(7) Uani 1 1 d . . . H14A H 0.4218 0.4697 0.8080 0.062 Uiso 1 1 calc R . . H14B H 0.4308 0.5226 0.7519 0.062 Uiso 1 1 calc R . . C15 C 0.5263(3) 0.40494(18) 0.75274(11) 0.0529(7) Uani 1 1 d . . . H15A H 0.5781 0.4214 0.7223 0.063 Uiso 1 1 calc R . . H15B H 0.4490 0.3718 0.7366 0.063 Uiso 1 1 calc R . . C16 C 0.6099(2) 0.34791(17) 0.79396(10) 0.0460(6) Uani 1 1 d . . . H16A H 0.5554 0.3264 0.8222 0.055 Uiso 1 1 calc R . . H16B H 0.6416 0.2973 0.7743 0.055 Uiso 1 1 calc R . . C21 C 0.9235(2) 0.14198(14) 0.88165(8) 0.0289(5) Uani 1 1 d . . . H21 H 0.9662 0.1722 0.9152 0.035 Uiso 1 1 calc R . . C22 C 0.7947(2) 0.10210(15) 0.89551(9) 0.0381(6) Uani 1 1 d . . . H22A H 0.7491 0.0752 0.8619 0.046 Uiso 1 1 calc R . . H22B H 0.7375 0.1481 0.9078 0.046 Uiso 1 1 calc R . . C23 C 0.8180(2) 0.03402(16) 0.94091(10) 0.0443(6) Uani 1 1 d . . . H23A H 0.8542 0.0622 0.9758 0.053 Uiso 1 1 calc R . . H23B H 0.7334 0.0070 0.9472 0.053 Uiso 1 1 calc R . . C24 C 0.9123(3) -0.03537(16) 0.92558(10) 0.0478(7) Uani 1 1 d . . . H24A H 0.9312 -0.0755 0.9571 0.057 Uiso 1 1 calc R . . H24B H 0.8708 -0.0689 0.8937 0.057 Uiso 1 1 calc R . . C25 C 1.0398(2) 0.00376(16) 0.91075(10) 0.0444(6) Uani 1 1 d . . . H25A H 1.0963 -0.0426 0.8983 0.053 Uiso 1 1 calc R . . H25B H 1.0867 0.0309 0.9440 0.053 Uiso 1 1 calc R . . C26 C 1.0153(2) 0.07133(14) 0.86510(9) 0.0371(6) Uani 1 1 d . . . H26A H 0.9762 0.0431 0.8307 0.044 Uiso 1 1 calc R . . H26B H 1.0998 0.0974 0.8577 0.044 Uiso 1 1 calc R . . C31 C 1.0268(2) 0.34210(14) 0.74602(8) 0.0291(5) Uani 1 1 d . . . H31 H 0.9811 0.3907 0.7631 0.035 Uiso 1 1 calc R . . C32 C 1.1505(2) 0.37709(16) 0.72374(9) 0.0393(6) Uani 1 1 d . . . H32A H 1.2057 0.4063 0.7541 0.047 Uiso 1 1 calc R . . H32B H 1.2014 0.3282 0.7109 0.047 Uiso 1 1 calc R . . C33 C 1.1194(3) 0.44073(17) 0.67606(9) 0.0468(7) Uani 1 1 d . . . H33A H 1.0780 0.4931 0.6898 0.056 Uiso 1 1 calc R . . H33B H 1.2018 0.4584 0.6615 0.056 Uiso 1 1 calc R . . C34 C 1.0280(3) 0.40034(17) 0.62998(9) 0.0528(7) Uani 1 1 d . . . H34A H 1.0055 0.4435 0.6005 0.063 Uiso 1 1 calc R . . H34B H 1.0726 0.3513 0.6138 0.063 Uiso 1 1 calc R . . C35 C 0.9041(3) 0.36872(18) 0.65195(9) 0.0500(7) Uani 1 1 d . . . H35A H 0.8466 0.3413 0.6216 0.060 Uiso 1 1 calc R . . H35B H 0.8564 0.4185 0.6656 0.060 Uiso 1 1 calc R . . C36 C 0.9344(2) 0.30374(16) 0.69874(8) 0.0417(6) Uani 1 1 d . . . H36A H 0.9752 0.2517 0.6843 0.050 Uiso 1 1 calc R . . H36B H 0.8516 0.2859 0.7130 0.050 Uiso 1 1 calc R . . C41 C 1.2520(2) 0.25396(14) 0.91227(8) 0.0301(5) Uani 1 1 d . . . H41 H 1.1833 0.2131 0.9226 0.036 Uiso 1 1 calc R . . C42 C 1.3525(2) 0.20337(16) 0.88275(9) 0.0401(6) Uani 1 1 d . . . H42A H 1.3070 0.1742 0.8499 0.048 Uiso 1 1 calc R . . H42B H 1.4168 0.2442 0.8698 0.048 Uiso 1 1 calc R . . C43 C 1.4250(2) 0.13609(17) 0.92025(9) 0.0446(6) Uani 1 1 d . . . H43A H 1.4922 0.1075 0.9002 0.054 Uiso 1 1 calc R . . H43B H 1.3624 0.0914 0.9299 0.054 Uiso 1 1 calc R . . C44 C 1.4907(3) 0.17715(18) 0.97301(10) 0.0509(7) Uani 1 1 d . . . H44A H 1.5322 0.1317 0.9976 0.061 Uiso 1 1 calc R . . H44B H 1.5600 0.2175 0.9638 0.061 Uiso 1 1 calc R . . C45 C 1.3901(2) 0.22576(17) 1.00256(9) 0.0455(7) Uani 1 1 d . . . H45A H 1.4342 0.2538 1.0361 0.055 Uiso 1 1 calc R . . H45B H 1.3247 0.1845 1.0143 0.055 Uiso 1 1 calc R . . C46 C 1.3206(2) 0.29428(15) 0.96489(8) 0.0386(6) Uani 1 1 d . . . H46A H 1.3854 0.3373 0.9549 0.046 Uiso 1 1 calc R . . H46B H 1.2552 0.3247 0.9850 0.046 Uiso 1 1 calc R . . H1N H 1.0923 0.5261 0.8000 0.174(19) Uiso 1 1 d RD . . H2N H 1.0020 0.6385 0.9753 0.109(12) Uiso 1 1 d RD . . H3N H 1.2807 0.4782 0.9198 0.092(10) Uiso 1 1 d RD . . 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 0.03645(15) 0.02871(15) 0.03355(13) -0.00239(10) -0.00002(10) 0.00422(11) P1 0.0337(4) 0.0265(3) 0.0330(3) 0.0040(2) 0.0043(2) 0.0024(3) P2 0.0361(4) 0.0257(3) 0.0299(3) 0.0026(2) 0.0027(2) -0.0008(3) P3 0.0360(4) 0.0293(3) 0.0261(3) 0.0019(2) 0.0034(2) 0.0019(3) P4 0.0345(4) 0.0302(4) 0.0288(3) 0.0018(2) 0.0016(2) 0.0008(3) Li1 0.046(3) 0.034(2) 0.042(2) 0.0021(18) 0.0039(18) 0.004(2) N1 0.0547(16) 0.0482(15) 0.0457(12) 0.0065(10) 0.0100(11) -0.0081(12) C1 0.059(2) 0.086(3) 0.0615(18) 0.0028(16) 0.0045(16) -0.0049(18) C2 0.094(3) 0.207(5) 0.075(2) 0.046(3) 0.003(2) -0.070(3) N2 0.0591(16) 0.0347(13) 0.0495(13) 0.0010(10) 0.0107(11) 0.0135(11) C3 0.067(2) 0.063(2) 0.0661(18) -0.0034(15) 0.0139(16) 0.0219(17) C4 0.081(2) 0.0403(19) 0.094(2) -0.0056(16) 0.0046(18) 0.0091(18) N3 0.0424(14) 0.0404(14) 0.0553(13) -0.0125(10) 0.0008(10) 0.0048(11) C5 0.0421(19) 0.096(3) 0.086(2) -0.0117(19) 0.0066(16) -0.0009(18) C6 0.066(2) 0.059(2) 0.0557(17) -0.0075(14) -0.0082(14) 0.0148(16) C11 0.0291(13) 0.0309(13) 0.0364(12) 0.0072(10) 0.0047(10) 0.0030(11) C12 0.0380(15) 0.0335(15) 0.0467(14) 0.0023(11) 0.0046(11) 0.0066(12) C13 0.0503(18) 0.0402(16) 0.0571(15) 0.0140(12) 0.0121(13) 0.0151(14) C14 0.0353(16) 0.063(2) 0.0561(16) 0.0197(14) 0.0070(12) 0.0118(14) C15 0.0388(16) 0.061(2) 0.0562(16) 0.0071(14) -0.0072(12) 0.0052(14) C16 0.0356(15) 0.0453(17) 0.0553(15) 0.0055(12) -0.0041(12) 0.0000(13) C21 0.0351(13) 0.0242(12) 0.0270(11) 0.0017(9) 0.0020(9) -0.0010(11) C22 0.0350(14) 0.0305(14) 0.0486(14) 0.0088(11) 0.0044(11) 0.0002(11) C23 0.0436(16) 0.0353(15) 0.0552(15) 0.0150(12) 0.0113(12) -0.0007(13) C24 0.0583(18) 0.0301(15) 0.0546(15) 0.0138(12) 0.0041(13) -0.0020(13) C25 0.0491(17) 0.0313(15) 0.0534(15) 0.0071(11) 0.0076(12) 0.0095(13) C26 0.0456(16) 0.0289(14) 0.0372(12) 0.0019(10) 0.0065(11) 0.0045(12) C31 0.0327(13) 0.0273(13) 0.0272(11) 0.0033(9) 0.0037(9) 0.0020(10) C32 0.0384(15) 0.0441(16) 0.0360(12) 0.0051(11) 0.0066(10) -0.0021(12) C33 0.0555(18) 0.0475(17) 0.0381(13) 0.0080(12) 0.0090(12) -0.0095(14) C34 0.078(2) 0.0478(17) 0.0323(13) 0.0106(12) 0.0042(13) -0.0057(15) C35 0.0591(19) 0.0545(18) 0.0331(13) 0.0054(12) -0.0106(12) -0.0061(15) C36 0.0476(16) 0.0444(16) 0.0318(12) 0.0044(11) -0.0021(11) -0.0107(13) C41 0.0304(13) 0.0306(13) 0.0294(11) 0.0013(9) 0.0033(9) 0.0023(10) C42 0.0399(15) 0.0462(16) 0.0347(12) -0.0047(11) 0.0052(10) 0.0081(12) C43 0.0381(15) 0.0482(17) 0.0474(14) -0.0014(12) 0.0045(11) 0.0160(13) C44 0.0448(17) 0.0572(19) 0.0486(15) 0.0020(13) -0.0053(12) 0.0176(14) C45 0.0478(16) 0.0525(18) 0.0339(13) -0.0011(12) -0.0061(11) 0.0127(14) C46 0.0410(15) 0.0389(15) 0.0346(12) -0.0041(10) -0.0022(10) 0.0056(12) _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 P4 2.3083(6) . ? As1 P1 2.3107(7) . ? As1 Li1 2.784(4) . ? P1 C11 1.881(2) . ? P1 P2 2.1825(8) . ? P2 C21 1.874(2) . ? P2 P3 2.2069(8) . ? P3 C31 1.873(2) . ? P3 P4 2.1867(8) . ? P4 C41 1.884(2) . ? Li1 N2 2.076(4) . ? Li1 N1 2.103(4) . ? Li1 N3 2.103(5) . ? N1 C2 1.424(4) . ? N1 C1 1.445(3) . ? N1 H1N 1.0224 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N2 C3 1.465(3) . ? N2 C4 1.469(4) . ? N2 H2N 0.9856 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N3 C6 1.464(3) . ? N3 C5 1.456(3) . ? N3 H3N 1.0845 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C12 1.527(3) . ? C11 C16 1.529(3) . ? C11 H11 1.0000 . ? C12 C13 1.532(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.518(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.513(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.528(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C22 1.529(3) . ? C21 C26 1.526(3) . ? C21 H21 1.0000 . ? C22 C23 1.527(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.519(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.521(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.527(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C36 1.530(3) . ? C31 C32 1.532(3) . ? C31 H31 1.0000 . ? C32 C33 1.529(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.517(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.513(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.526(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C41 C46 1.526(3) . ? C41 C42 1.534(3) . ? C41 H41 1.0000 . ? C42 C43 1.525(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.523(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.519(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.528(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 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 P4 As1 P1 104.70(2) . . ? P4 As1 Li1 94.49(8) . . ? P1 As1 Li1 130.01(9) . . ? C11 P1 P2 99.97(7) . . ? C11 P1 As1 108.50(7) . . ? P2 P1 As1 106.30(3) . . ? C21 P2 P1 98.09(7) . . ? C21 P2 P3 103.29(7) . . ? P1 P2 P3 107.86(3) . . ? C31 P3 P4 100.79(7) . . ? C31 P3 P2 100.85(7) . . ? P4 P3 P2 106.66(3) . . ? C41 P4 P3 99.01(7) . . ? C41 P4 As1 107.25(6) . . ? P3 P4 As1 106.82(3) . . ? N2 Li1 N1 115.8(2) . . ? N2 Li1 N3 107.69(19) . . ? N1 Li1 N3 111.84(19) . . ? N2 Li1 As1 120.33(17) . . ? N1 Li1 As1 106.95(17) . . ? N3 Li1 As1 91.63(15) . . ? C2 N1 C1 110.3(3) . . ? C2 N1 Li1 118.2(2) . . ? C1 N1 Li1 115.5(2) . . ? C2 N1 H1N 115.3 . . ? C1 N1 H1N 97.9 . . ? Li1 N1 H1N 97.3 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 N2 C4 110.9(2) . . ? C3 N2 Li1 112.8(2) . . ? C4 N2 Li1 113.7(2) . . ? C3 N2 H2N 114.1 . . ? C4 N2 H2N 106.8 . . ? Li1 N2 H2N 98.0 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 N3 C5 110.1(2) . . ? C6 N3 Li1 110.63(19) . . ? C5 N3 Li1 120.8(2) . . ? C6 N3 H3N 101.1 . . ? C5 N3 H3N 114.1 . . ? Li1 N3 H3N 97.8 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C16 110.14(19) . . ? C12 C11 P1 109.20(15) . . ? C16 C11 P1 110.14(16) . . ? C12 C11 H11 109.1 . . ? C16 C11 H11 109.1 . . ? P1 C11 H11 109.1 . . ? C11 C12 C13 111.84(19) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 111.1(2) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 110.5(2) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C14 C15 C16 111.6(2) . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C11 C16 C15 111.6(2) . . ? C11 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C11 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C22 C21 C26 109.98(19) . . ? C22 C21 P2 107.41(15) . . ? C26 C21 P2 113.00(14) . . ? C22 C21 H21 108.8 . . ? C26 C21 H21 108.8 . . ? P2 C21 H21 108.8 . . ? C21 C22 C23 111.50(19) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 111.42(19) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 111.3(2) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.5(2) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 110.95(17) . . ? C25 C26 H26A 109.4 . . ? C21 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C21 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C36 C31 C32 110.00(17) . . ? C36 C31 P3 111.26(15) . . ? C32 C31 P3 108.95(15) . . ? C36 C31 H31 108.9 . . ? C32 C31 H31 108.9 . . ? P3 C31 H31 108.9 . . ? C33 C32 C31 112.5(2) . . ? C33 C32 H32A 109.1 . . ? C31 C32 H32A 109.1 . . ? C33 C32 H32B 109.1 . . ? C31 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 110.9(2) . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.44(19) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.4(2) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 111.4(2) . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C31 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C46 C41 C42 109.18(18) . . ? C46 C41 P4 109.86(15) . . ? C42 C41 P4 111.32(14) . . ? C46 C41 H41 108.8 . . ? C42 C41 H41 108.8 . . ? P4 C41 H41 108.8 . . ? C43 C42 C41 112.24(17) . . ? C43 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? C43 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? C42 C43 C44 111.2(2) . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 110.1(2) . . ? C45 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? C45 C44 H44B 109.6 . . ? C43 C44 H44B 109.6 . . ? H44A C44 H44B 108.2 . . ? C44 C45 C46 110.94(19) . . ? C44 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C41 111.25(19) . . ? C45 C46 H46A 109.4 . . ? C41 C46 H46A 109.4 . . ? C45 C46 H46B 109.4 . . ? C41 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P4 As1 P1 C11 -98.79(7) . . . . ? Li1 As1 P1 C11 10.23(13) . . . . ? P4 As1 P1 P2 7.95(3) . . . . ? Li1 As1 P1 P2 116.96(10) . . . . ? C11 P1 P2 C21 -162.96(10) . . . . ? As1 P1 P2 C21 84.27(7) . . . . ? C11 P1 P2 P3 90.20(8) . . . . ? As1 P1 P2 P3 -22.57(4) . . . . ? C21 P2 P3 C31 -178.89(10) . . . . ? P1 P2 P3 C31 -75.72(7) . . . . ? C21 P2 P3 P4 -74.04(7) . . . . ? P1 P2 P3 P4 29.13(4) . . . . ? C31 P3 P4 C41 -167.20(9) . . . . ? P2 P3 P4 C41 87.90(7) . . . . ? C31 P3 P4 As1 81.60(7) . . . . ? P2 P3 P4 As1 -23.30(4) . . . . ? P1 As1 P4 C41 -95.92(8) . . . . ? Li1 As1 P4 C41 130.66(11) . . . . ? P1 As1 P4 P3 9.45(3) . . . . ? Li1 As1 P4 P3 -123.97(8) . . . . ? P4 As1 Li1 N2 -167.00(19) . . . . ? P1 As1 Li1 N2 79.5(2) . . . . ? P4 As1 Li1 N1 58.07(16) . . . . ? P1 As1 Li1 N1 -55.4(2) . . . . ? P4 As1 Li1 N3 -55.37(12) . . . . ? P1 As1 Li1 N3 -168.83(7) . . . . ? N2 Li1 N1 C2 72.9(4) . . . . ? N3 Li1 N1 C2 -51.0(4) . . . . ? As1 Li1 N1 C2 -149.9(3) . . . . ? N2 Li1 N1 C1 -60.9(3) . . . . ? N3 Li1 N1 C1 175.2(2) . . . . ? As1 Li1 N1 C1 76.3(2) . . . . ? N1 Li1 N2 C3 46.6(3) . . . . ? N3 Li1 N2 C3 172.7(2) . . . . ? As1 Li1 N2 C3 -84.6(2) . . . . ? N1 Li1 N2 C4 -80.7(3) . . . . ? N3 Li1 N2 C4 45.3(3) . . . . ? As1 Li1 N2 C4 148.1(2) . . . . ? N2 Li1 N3 C6 50.4(3) . . . . ? N1 Li1 N3 C6 178.8(2) . . . . ? As1 Li1 N3 C6 -72.2(2) . . . . ? N2 Li1 N3 C5 -80.3(3) . . . . ? N1 Li1 N3 C5 48.0(3) . . . . ? As1 Li1 N3 C5 157.02(19) . . . . ? P2 P1 C11 C12 -175.94(14) . . . . ? As1 P1 C11 C12 -64.89(16) . . . . ? P2 P1 C11 C16 62.99(16) . . . . ? As1 P1 C11 C16 174.04(14) . . . . ? C16 C11 C12 C13 -54.7(3) . . . . ? P1 C11 C12 C13 -175.76(17) . . . . ? C11 C12 C13 C14 56.1(3) . . . . ? C12 C13 C14 C15 -56.1(3) . . . . ? C13 C14 C15 C16 56.4(3) . . . . ? C12 C11 C16 C15 54.5(3) . . . . ? P1 C11 C16 C15 175.01(17) . . . . ? C14 C15 C16 C11 -56.1(3) . . . . ? P1 P2 C21 C22 78.52(15) . . . . ? P3 P2 C21 C22 -170.88(13) . . . . ? P1 P2 C21 C26 -160.00(15) . . . . ? P3 P2 C21 C26 -49.40(17) . . . . ? C26 C21 C22 C23 56.5(2) . . . . ? P2 C21 C22 C23 179.87(16) . . . . ? C21 C22 C23 C24 -55.5(3) . . . . ? C22 C23 C24 C25 54.2(3) . . . . ? C23 C24 C25 C26 -54.8(3) . . . . ? C24 C25 C26 C21 56.5(3) . . . . ? C22 C21 C26 C25 -56.8(2) . . . . ? P2 C21 C26 C25 -176.82(17) . . . . ? P4 P3 C31 C36 -169.35(14) . . . . ? P2 P3 C31 C36 -59.85(16) . . . . ? P4 P3 C31 C32 69.22(15) . . . . ? P2 P3 C31 C32 178.71(14) . . . . ? C36 C31 C32 C33 53.8(3) . . . . ? P3 C31 C32 C33 176.00(16) . . . . ? C31 C32 C33 C34 -55.3(3) . . . . ? C32 C33 C34 C35 56.3(3) . . . . ? C33 C34 C35 C36 -57.6(3) . . . . ? C34 C35 C36 C31 57.1(3) . . . . ? C32 C31 C36 C35 -54.2(3) . . . . ? P3 C31 C36 C35 -175.03(17) . . . . ? P3 P4 C41 C46 -176.31(14) . . . . ? As1 P4 C41 C46 -65.46(15) . . . . ? P3 P4 C41 C42 62.63(16) . . . . ? As1 P4 C41 C42 173.48(14) . . . . ? C46 C41 C42 C43 55.3(3) . . . . ? P4 C41 C42 C43 176.73(17) . . . . ? C41 C42 C43 C44 -55.7(3) . . . . ? C42 C43 C44 C45 55.8(3) . . . . ? C43 C44 C45 C46 -57.3(3) . . . . ? C44 C45 C46 C41 58.6(3) . . . . ? C42 C41 C46 C45 -56.4(2) . . . . ? P4 C41 C46 C45 -178.73(16) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.300 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.059 data_dw0014 _database_code_CSD 197233 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H60 As N2 Na P4' _chemical_formula_weight 670.59 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 10.8971(3) _cell_length_b 17.5762(6) _cell_length_c 19.5359(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.037(2) _cell_angle_gamma 90.00 _cell_volume 3739.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method ? _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 1.078 _exptl_absorpt_correction_T_min 0.927 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 18697 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6530 _reflns_number_observed 4939 _reflns_observed_criterion >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+1.6959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6514 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_obs 0.0387 _refine_ls_wR_factor_all 0.1682 _refine_ls_wR_factor_obs 0.0706 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 2.192 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group As1 As 0.04715(3) 0.073795(15) 0.926468(14) 0.03615(10) Uani 1 d . . P1 P -0.13051(6) 0.14347(4) 0.90381(4) 0.0360(2) Uani 1 d . . P2 P -0.08574(6) 0.22751(4) 0.82578(4) 0.0350(2) Uani 1 d . . P3 P 0.09035(6) 0.19341(4) 0.78284(3) 0.0329(2) Uani 1 d . . P4 P 0.19282(6) 0.12940(4) 0.86200(4) 0.0318(2) Uani 1 d . . Na1 Na -0.01890(10) 0.09521(6) 1.07075(6) 0.0439(3) Uani 1 d . . N1 N -0.2020(2) 0.13745(13) 1.12569(12) 0.0460(6) Uani 1 d . . N2 N 0.0376(2) 0.21781(13) 1.12914(13) 0.0498(6) Uani 1 d . . C1 C -0.3140(3) 0.1206(2) 1.0849(2) 0.0811(12) Uani 1 d . . H1A H -0.3210(12) 0.0655(3) 1.0780(11) 0.122 Uiso 1 calc R . H1B H -0.3105(11) 0.1459(12) 1.0403(5) 0.122 Uiso 1 calc R . H1C H -0.3855(3) 0.1390(13) 1.1090(6) 0.122 Uiso 1 calc R . C2 C -0.2074(3) 0.0960(2) 1.1905(2) 0.0606(9) Uani 1 d . . H2A H -0.2230(19) 0.0420(3) 1.1812(2) 0.091 Uiso 1 calc R . H2B H -0.2737(12) 0.1167(8) 1.2175(5) 0.091 Uiso 1 calc R . H2C H -0.1290(7) 0.1015(10) 1.2162(5) 0.091 Uiso 1 calc R . C3 C 0.0478(3) 0.2675(2) 1.0698(2) 0.0718(11) Uani 1 d . . H3A H 0.1165(12) 0.2508(7) 1.0425(6) 0.086 Uiso 1 calc R . H3B H 0.0622(18) 0.3199(3) 1.0852(2) 0.086 Uiso 1 calc R . H3C H -0.0285(8) 0.2653(9) 1.0417(6) 0.086 Uiso 1 calc R . C4 C 0.1522(4) 0.2215(3) 1.1708(2) 0.1018(14) Uani 1 d . . H4A H 0.1453(11) 0.1890(14) 1.2112(8) 0.153 Uiso 1 calc R . H4B H 0.1673(15) 0.2741(4) 1.1853(13) 0.153 Uiso 1 calc R . H4C H 0.2204(6) 0.2038(16) 1.1436(5) 0.153 Uiso 1 calc R . C5 C -0.1885(3) 0.2187(2) 1.1375(2) 0.0728(11) Uani 1 d . . H5A H -0.2543(3) 0.2358(2) 1.1676(2) 0.087 Uiso 1 calc R . H5B H -0.1996(3) 0.2456(2) 1.0933(2) 0.087 Uiso 1 calc R . C6 C -0.0665(4) 0.2403(2) 1.1697(2) 0.0771(12) Uani 1 d . . H6A H -0.0643(4) 0.2962(2) 1.1763(2) 0.093 Uiso 1 calc R . H6B H -0.0579(4) 0.2163(2) 1.2154(2) 0.093 Uiso 1 calc R . C11 C -0.2338(2) 0.07975(15) 0.85023(15) 0.0396(7) Uani 1 d . . H11 H -0.1892(2) 0.06250(15) 0.80916(15) 0.048 Uiso 1 calc R . C12 C -0.3498(3) 0.1225(2) 0.8267(2) 0.0542(8) Uani 1 d . . H12A H -0.3920(3) 0.1415(2) 0.8674(2) 0.065 Uiso 1 calc R . H12B H -0.3267(3) 0.1669(2) 0.7989(2) 0.065 Uiso 1 calc R . C13 C -0.4379(3) 0.0722(2) 0.7845(2) 0.0629(9) Uani 1 d . . H13A H -0.5130(3) 0.1014(2) 0.7718(2) 0.075 Uiso 1 calc R . H13B H -0.3986(3) 0.0566(2) 0.7418(2) 0.075 Uiso 1 calc R . C14 C -0.4722(3) 0.0024(2) 0.8246(2) 0.0582(9) Uani 1 d . . H14A H -0.5197(3) 0.0178(2) 0.8646(2) 0.070 Uiso 1 calc R . H14B H -0.5249(3) -0.0311(2) 0.7953(2) 0.070 Uiso 1 calc R . C15 C -0.3593(3) -0.0409(2) 0.8490(2) 0.0773(12) Uani 1 d . . H15A H -0.3165(3) -0.0611(2) 0.8090(2) 0.093 Uiso 1 calc R . H15B H -0.3840(3) -0.0845(2) 0.8774(2) 0.093 Uiso 1 calc R . C16 C -0.2715(3) 0.0107(2) 0.8912(2) 0.0641(10) Uani 1 d . . H16A H -0.3122(3) 0.0277(2) 0.9330(2) 0.077 Uiso 1 calc R . H16B H -0.1973(3) -0.0185(2) 0.9055(2) 0.077 Uiso 1 calc R . C21 C -0.0467(2) 0.31193(14) 0.88074(14) 0.0360(6) Uani 1 d . . H21 H 0.0056(2) 0.29488(14) 0.92095(14) 0.043 Uiso 1 calc R . C22 C -0.1674(3) 0.3442(2) 0.9065(2) 0.0501(8) Uani 1 d . . H22A H -0.2230(3) 0.3561(2) 0.8667(2) 0.060 Uiso 1 calc R . H22B H -0.2078(3) 0.3052(2) 0.9345(2) 0.060 Uiso 1 calc R . C23 C -0.1470(3) 0.4162(2) 0.9494(2) 0.0581(9) Uani 1 d . . H23A H -0.2274(3) 0.4370(2) 0.9623(2) 0.070 Uiso 1 calc R . H23B H -0.0997(3) 0.4033(2) 0.9920(2) 0.070 Uiso 1 calc R . C24 C -0.0784(3) 0.4757(2) 0.9102(2) 0.0635(9) Uani 1 d . . H24A H -0.0615(3) 0.5201(2) 0.9403(2) 0.076 Uiso 1 calc R . H24B H -0.1302(3) 0.4931(2) 0.8706(2) 0.076 Uiso 1 calc R . C25 C 0.0416(3) 0.4447(2) 0.8850(2) 0.0598(9) Uani 1 d . . H25A H 0.0972(3) 0.4331(2) 0.9248(2) 0.072 Uiso 1 calc R . H25B H 0.0815(3) 0.4840(2) 0.8571(2) 0.072 Uiso 1 calc R . C26 C 0.0217(3) 0.37268(15) 0.8422(2) 0.0483(8) Uani 1 d . . H26A H -0.0256(3) 0.38564(15) 0.7995(2) 0.058 Uiso 1 calc R . H26B H 0.1023(3) 0.35236(15) 0.8292(2) 0.058 Uiso 1 calc R . C31 C 0.0380(2) 0.11134(14) 0.72805(13) 0.0335(6) Uani 1 d . . H31 H 0.0043(2) 0.07125(14) 0.75845(13) 0.040 Uiso 1 calc R . C32 C -0.0621(3) 0.1339(2) 0.6753(2) 0.0566(9) Uani 1 d . . H32A H -0.0313(3) 0.1750(2) 0.6459(2) 0.068 Uiso 1 calc R . H32B H -0.1341(3) 0.1536(2) 0.6993(2) 0.068 Uiso 1 calc R . C33 C -0.1013(3) 0.0661(2) 0.6308(2) 0.0680(10) Uani 1 d . . H33A H -0.1401(3) 0.0273(2) 0.6597(2) 0.082 Uiso 1 calc R . H33B H -0.1633(3) 0.0831(2) 0.5958(2) 0.082 Uiso 1 calc R . C34 C 0.0058(3) 0.0307(2) 0.5955(2) 0.0630(10) Uani 1 d . . H34A H 0.0380(3) 0.0671(2) 0.5619(2) 0.076 Uiso 1 calc R . H34B H -0.0223(3) -0.0154(2) 0.5703(2) 0.076 Uiso 1 calc R . C35 C 0.1073(3) 0.0093(2) 0.6472(2) 0.0613(9) Uani 1 d . . H35A H 0.1789(3) -0.0100(2) 0.6227(2) 0.074 Uiso 1 calc R . H35B H 0.0781(3) -0.0319(2) 0.6770(2) 0.074 Uiso 1 calc R . C36 C 0.1468(3) 0.0777(2) 0.6914(2) 0.0515(8) Uani 1 d . . H36A H 0.2106(3) 0.0615(2) 0.7256(2) 0.062 Uiso 1 calc R . H36B H 0.1829(3) 0.1172(2) 0.6620(2) 0.062 Uiso 1 calc R . C41 C 0.2668(2) 0.20910(14) 0.91252(13) 0.0319(6) Uani 1 d . . H41 H 0.2021(2) 0.24543(14) 0.92698(13) 0.038 Uiso 1 calc R . C42 C 0.3585(2) 0.2513(2) 0.86844(14) 0.0411(7) Uani 1 d . . H42A H 0.4155(2) 0.2140(2) 0.84872(14) 0.049 Uiso 1 calc R . H42B H 0.3133(2) 0.2769(2) 0.83005(14) 0.049 Uiso 1 calc R . C43 C 0.4325(3) 0.3105(2) 0.9096(2) 0.0534(8) Uani 1 d . . H43A H 0.4946(3) 0.3334(2) 0.8801(2) 0.064 Uiso 1 calc R . H43B H 0.3768(3) 0.3516(2) 0.9240(2) 0.064 Uiso 1 calc R . C44 C 0.4963(3) 0.2761(2) 0.9724(2) 0.0528(8) Uani 1 d . . H44A H 0.5586(3) 0.2388(2) 0.9581(2) 0.063 Uiso 1 calc R . H44B H 0.5390(3) 0.3166(2) 0.9992(2) 0.063 Uiso 1 calc R . C45 C 0.4040(3) 0.2368(2) 1.0166(2) 0.0488(8) Uani 1 d . . H45A H 0.3459(3) 0.2749(2) 1.0340(2) 0.059 Uiso 1 calc R . H45B H 0.4474(3) 0.2130(2) 1.0565(2) 0.059 Uiso 1 calc R . C46 C 0.3329(2) 0.17608(15) 0.97601(14) 0.0394(7) Uani 1 d . . H46A H 0.2719(2) 0.15235(15) 1.00572(14) 0.047 Uiso 1 calc R . H46B H 0.3904(2) 0.13589(15) 0.96188(14) 0.047 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0416(2) 0.0333(2) 0.0336(2) 0.00600(13) 0.00159(13) -0.00667(13) P1 0.0395(4) 0.0340(4) 0.0350(4) -0.0002(3) 0.0082(3) -0.0055(3) P2 0.0372(4) 0.0327(4) 0.0353(4) 0.0017(3) 0.0035(3) -0.0008(3) P3 0.0386(4) 0.0336(4) 0.0269(4) 0.0021(3) 0.0041(3) -0.0023(3) P4 0.0354(4) 0.0305(4) 0.0296(4) -0.0003(3) 0.0022(3) -0.0023(3) Na1 0.0499(7) 0.0381(6) 0.0444(7) -0.0064(5) 0.0129(6) -0.0032(5) N1 0.0431(14) 0.0485(15) 0.047(2) 0.0023(12) 0.0112(12) 0.0020(12) N2 0.059(2) 0.0483(15) 0.043(2) -0.0101(13) 0.0123(13) -0.0110(13) C1 0.052(2) 0.114(3) 0.078(3) 0.025(2) 0.005(2) -0.003(2) C2 0.068(2) 0.060(2) 0.055(2) 0.002(2) 0.014(2) -0.008(2) C3 0.081(3) 0.059(2) 0.077(3) 0.005(2) 0.034(2) -0.006(2) C4 0.098(3) 0.121(4) 0.084(3) -0.015(3) -0.019(3) -0.036(3) C5 0.071(2) 0.046(2) 0.105(3) 0.007(2) 0.054(2) 0.014(2) C6 0.113(3) 0.049(2) 0.072(3) -0.027(2) 0.047(2) -0.023(2) C11 0.0367(15) 0.037(2) 0.045(2) -0.0048(14) 0.0089(13) -0.0048(13) C12 0.045(2) 0.045(2) 0.071(2) 0.009(2) -0.006(2) -0.005(2) C13 0.051(2) 0.067(2) 0.070(2) 0.003(2) -0.012(2) -0.010(2) C14 0.043(2) 0.063(2) 0.069(2) -0.004(2) -0.001(2) -0.017(2) C15 0.060(2) 0.045(2) 0.125(4) 0.007(2) -0.015(2) -0.018(2) C16 0.050(2) 0.052(2) 0.089(3) 0.024(2) -0.017(2) -0.014(2) C21 0.0368(15) 0.0316(14) 0.039(2) -0.0008(13) 0.0012(13) 0.0031(13) C22 0.042(2) 0.041(2) 0.068(2) -0.007(2) 0.010(2) 0.0031(14) C23 0.056(2) 0.045(2) 0.074(2) -0.014(2) 0.010(2) 0.009(2) C24 0.071(2) 0.034(2) 0.086(3) -0.011(2) -0.001(2) 0.003(2) C25 0.060(2) 0.038(2) 0.082(3) -0.001(2) 0.004(2) -0.010(2) C26 0.051(2) 0.038(2) 0.057(2) 0.0029(15) 0.006(2) -0.0023(14) C31 0.042(2) 0.0323(14) 0.027(2) 0.0000(12) 0.0007(12) -0.0039(13) C32 0.075(2) 0.053(2) 0.041(2) -0.0080(15) -0.021(2) 0.008(2) C33 0.082(2) 0.065(2) 0.055(2) -0.011(2) -0.033(2) 0.006(2) C34 0.104(3) 0.049(2) 0.036(2) -0.011(2) -0.003(2) -0.012(2) C35 0.069(2) 0.059(2) 0.055(2) -0.026(2) -0.001(2) 0.002(2) C36 0.054(2) 0.053(2) 0.047(2) -0.014(2) 0.009(2) -0.003(2) C41 0.0317(14) 0.0299(14) 0.034(2) -0.0033(12) 0.0038(12) -0.0006(12) C42 0.037(2) 0.043(2) 0.043(2) 0.0070(14) 0.0021(14) -0.0045(14) C43 0.052(2) 0.044(2) 0.065(2) 0.003(2) 0.004(2) -0.015(2) C44 0.043(2) 0.053(2) 0.062(2) -0.013(2) -0.004(2) -0.015(2) C45 0.045(2) 0.055(2) 0.046(2) -0.007(2) -0.0082(15) -0.005(2) C46 0.040(2) 0.041(2) 0.038(2) 0.0014(13) -0.0014(13) -0.0036(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 P4 2.2810(7) . ? As1 P1 2.3201(8) . ? As1 Na1 2.9578(11) . ? As1 Na1 2.9870(10) 3_557 ? P1 C11 1.880(3) . ? P1 P2 2.1901(10) . ? P2 C21 1.872(3) . ? P2 P3 2.2045(10) . ? P3 C31 1.873(2) . ? P3 P4 2.1866(10) . ? P4 C41 1.879(2) . ? Na1 N1 2.416(2) . ? Na1 N2 2.505(3) . ? Na1 As1 2.9870(10) 3_557 ? N1 C5 1.453(4) . ? N1 C1 1.464(4) . ? N1 C2 1.464(4) . ? N2 C3 1.460(4) . ? N2 C6 1.461(4) . ? N2 C4 1.467(4) . ? C5 C6 1.500(5) . ? C11 C16 1.517(4) . ? C11 C12 1.527(4) . ? C12 C13 1.525(4) . ? C13 C14 1.509(4) . ? C14 C15 1.509(4) . ? C15 C16 1.537(4) . ? C21 C26 1.518(4) . ? C21 C22 1.534(3) . ? C22 C23 1.529(4) . ? C23 C24 1.510(4) . ? C24 C25 1.514(4) . ? C25 C26 1.530(4) . ? C31 C32 1.526(4) . ? C31 C36 1.526(4) . ? C32 C33 1.528(4) . ? C33 C34 1.511(4) . ? C34 C35 1.518(4) . ? C35 C36 1.533(4) . ? C41 C46 1.527(3) . ? C41 C42 1.533(3) . ? C42 C43 1.528(4) . ? C43 C44 1.514(4) . ? C44 C45 1.515(4) . ? C45 C46 1.525(4) . ? 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 P4 As1 P1 105.12(3) . . ? P4 As1 Na1 132.01(3) . . ? P1 As1 Na1 83.40(3) . . ? P4 As1 Na1 120.68(3) . 3_557 ? P1 As1 Na1 116.26(3) . 3_557 ? Na1 As1 Na1 94.61(3) . 3_557 ? C11 P1 P2 99.10(9) . . ? C11 P1 As1 105.72(9) . . ? P2 P1 As1 106.49(3) . . ? C21 P2 P1 100.79(9) . . ? C21 P2 P3 104.51(8) . . ? P1 P2 P3 107.45(4) . . ? C31 P3 P4 98.36(8) . . ? C31 P3 P2 100.10(8) . . ? P4 P3 P2 107.48(4) . . ? C41 P4 P3 100.76(8) . . ? C41 P4 As1 108.88(8) . . ? P3 P4 As1 105.25(3) . . ? N1 Na1 N2 74.14(8) . . ? N1 Na1 As1 134.05(7) . . ? N2 Na1 As1 118.64(7) . . ? N1 Na1 As1 102.13(7) . 3_557 ? N2 Na1 As1 150.58(7) . 3_557 ? As1 Na1 As1 85.39(3) . 3_557 ? C5 N1 C1 111.3(3) . . ? C5 N1 C2 111.0(3) . . ? C1 N1 C2 108.2(2) . . ? C5 N1 Na1 107.0(2) . . ? C1 N1 Na1 112.4(2) . . ? C2 N1 Na1 106.9(2) . . ? C3 N2 C6 110.6(3) . . ? C3 N2 C4 109.1(3) . . ? C6 N2 C4 110.4(3) . . ? C3 N2 Na1 100.2(2) . . ? C6 N2 Na1 107.3(2) . . ? C4 N2 Na1 118.7(2) . . ? N1 C5 C6 113.5(3) . . ? N2 C6 C5 113.4(3) . . ? C16 C11 C12 108.4(2) . . ? C16 C11 P1 110.5(2) . . ? C12 C11 P1 110.3(2) . . ? C13 C12 C11 112.1(2) . . ? C14 C13 C12 110.7(3) . . ? C15 C14 C13 111.1(3) . . ? C14 C15 C16 110.9(3) . . ? C11 C16 C15 111.4(3) . . ? C26 C21 C22 110.2(2) . . ? C26 C21 P2 112.2(2) . . ? C22 C21 P2 107.5(2) . . ? C23 C22 C21 112.1(2) . . ? C24 C23 C22 111.1(3) . . ? C23 C24 C25 111.4(2) . . ? C24 C25 C26 111.6(2) . . ? C21 C26 C25 111.9(2) . . ? C32 C31 C36 109.4(2) . . ? C32 C31 P3 112.4(2) . . ? C36 C31 P3 109.9(2) . . ? C31 C32 C33 111.1(2) . . ? C34 C33 C32 112.2(3) . . ? C33 C34 C35 110.8(3) . . ? C34 C35 C36 111.3(3) . . ? C31 C36 C35 111.2(2) . . ? C46 C41 C42 110.0(2) . . ? C46 C41 P4 108.9(2) . . ? C42 C41 P4 110.0(2) . . ? C43 C42 C41 112.1(2) . . ? C44 C43 C42 111.9(2) . . ? C45 C44 C43 110.4(2) . . ? C44 C45 C46 111.0(2) . . ? C45 C46 C41 111.9(2) . . ? _refine_diff_density_max 0.341 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.054