# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1696
 
data_tx420 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C24 H50 Li2 N3 O1.50 P3' 
_chemical_formula_weight          511.46 
 
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' 
 'P'  'P'   0.1023   0.0942 
 '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            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                    10.679(2) 
_cell_length_b                    21.224(8) 
_cell_length_c                    13.847(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.46(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      3124.0(15) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     223(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.48
_exptl_crystal_size_mid           0.32
_exptl_crystal_size_min           0.28
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.087 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1112 
_exptl_absorpt_coefficient_mu     0.211 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       223(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  93 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.2
_diffrn_reflns_number             4884 
_diffrn_reflns_av_R_equivalents   0.0749 
_diffrn_reflns_av_sigmaI/netI     0.1161 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        1 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.92 
_diffrn_reflns_theta_max          22.00 
_reflns_number_total              3836 
_reflns_number_gt                 1761 
_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^)+(0.1273P)^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          3836 
_refine_ls_number_parameters      308 
_refine_ls_number_restraints      66 
_refine_ls_R_factor_all           0.1543 
_refine_ls_R_factor_gt            0.0769 
_refine_ls_wR_factor_ref          0.2419 
_refine_ls_wR_factor_gt           0.1866 
_refine_ls_goodness_of_fit_ref    0.937 
_refine_ls_restrained_S_all       0.934 
_refine_ls_shift/su_max           1.995 
_refine_ls_shift/su_mean          0.101 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
P1 P 0.51907(17) 0.16920(9) 0.39093(12) 0.0491(6) Uani 1 1 d . A . 
P2 P 0.42145(17) 0.14557(9) 0.55736(13) 0.0496(6) Uani 1 1 d . . . 
P3 P 0.53082(18) 0.06861(9) 0.62548(13) 0.0520(6) Uani 1 1 d . . . 
N1 N 0.6374(5) 0.1191(3) 0.3919(4) 0.0480(15) Uani 1 1 d D A . 
C1 C 0.7249(6) 0.1221(3) 0.3149(4) 0.057(2) Uani 1 1 d D . . 
C11 C 0.8198(7) 0.0680(4) 0.3357(6) 0.078(3) Uani 1 1 d D . . 
H11A H 0.8680 0.0752 0.3977 0.117 Uiso 1 1 calc R . . 
H11B H 0.8762 0.0664 0.2849 0.117 Uiso 1 1 calc R . . 
H11C H 0.7749 0.0284 0.3377 0.117 Uiso 1 1 calc R . . 
C12 C 0.7992(8) 0.1837(4) 0.3188(7) 0.087(3) Uani 1 1 d D . . 
H12A H 0.7422 0.2186 0.3033 0.131 Uiso 1 1 calc R . . 
H12B H 0.8614 0.1822 0.2722 0.131 Uiso 1 1 calc R . . 
H12C H 0.8411 0.1895 0.3835 0.131 Uiso 1 1 calc R . . 
C13 C 0.6551(8) 0.1122(5) 0.2152(5) 0.093(3) Uani 1 1 d D . . 
H13A H 0.6092 0.0727 0.2144 0.140 Uiso 1 1 calc R . . 
H13B H 0.7149 0.1110 0.1668 0.140 Uiso 1 1 calc R . . 
H13C H 0.5965 0.1466 0.2009 0.140 Uiso 1 1 calc R . . 
N2 N 0.5358(5) 0.1960(2) 0.5138(4) 0.0459(14) Uani 1 1 d D . . 
C2 C 0.5372(6) 0.2650(3) 0.5375(5) 0.058(2) Uani 1 1 d D . . 
C21 C 0.5638(8) 0.2714(4) 0.6472(5) 0.078(3) Uani 1 1 d D . . 
H21A H 0.4986 0.2500 0.6788 0.117 Uiso 1 1 calc R . . 
H21B H 0.5650 0.3156 0.6648 0.117 Uiso 1 1 calc R . . 
H21C H 0.6448 0.2527 0.6678 0.117 Uiso 1 1 calc R . . 
C22 C 0.4119(7) 0.2974(4) 0.5060(7) 0.083(3) Uani 1 1 d D . . 
H22A H 0.3949 0.2948 0.4361 0.124 Uiso 1 1 calc R . . 
H22B H 0.4164 0.3413 0.5256 0.124 Uiso 1 1 calc R . . 
H22C H 0.3448 0.2767 0.5365 0.124 Uiso 1 1 calc R . . 
C23 C 0.6424(8) 0.2965(4) 0.4881(6) 0.079(2) Uani 1 1 d D . . 
H23A H 0.7222 0.2771 0.5103 0.118 Uiso 1 1 calc R . . 
H23B H 0.6452 0.3410 0.5040 0.118 Uiso 1 1 calc R . . 
H23C H 0.6266 0.2914 0.4183 0.118 Uiso 1 1 calc R . . 
N3 N 0.4065(5) 0.1171(2) 0.4365(3) 0.0448(14) Uani 1 1 d D A . 
C3 C 0.2751(6) 0.1111(3) 0.3868(5) 0.056(2) Uani 1 1 d D . . 
C31 C 0.2048(6) 0.0619(4) 0.4426(6) 0.070(2) Uani 1 1 d D . . 
H31A H 0.2476 0.0217 0.4411 0.105 Uiso 1 1 calc R . . 
H31B H 0.1194 0.0576 0.4126 0.105 Uiso 1 1 calc R . . 
H31C H 0.2030 0.0755 0.5094 0.105 Uiso 1 1 calc R . . 
C32 C 0.2870(7) 0.0882(4) 0.2828(5) 0.074(2) Uani 1 1 d D . . 
H32A H 0.3367 0.1180 0.2497 0.111 Uiso 1 1 calc R . . 
H32B H 0.2039 0.0847 0.2482 0.111 Uiso 1 1 calc R . . 
H32C H 0.3278 0.0473 0.2848 0.111 Uiso 1 1 calc R . . 
C33 C 0.2038(7) 0.1732(4) 0.3834(6) 0.074(2) Uani 1 1 d D . . 
H33A H 0.2040 0.1900 0.4486 0.110 Uiso 1 1 calc R . . 
H33B H 0.1177 0.1663 0.3564 0.110 Uiso 1 1 calc R . . 
H33C H 0.2442 0.2030 0.3431 0.110 Uiso 1 1 calc R . . 
C41 C 0.5153(6) 0.0789(5) 0.7581(5) 0.076(3) Uani 1 1 d D . . 
H41A H 0.5327 0.0368 0.7872 0.091 Uiso 0.765(10) 1 calc PR A 1 
H41B H 0.5014 0.1249 0.7606 0.091 Uiso 0.235(10) 1 calc PR A 2 
C42 C 0.3884(9) 0.0960(6) 0.7842(6) 0.062(3) Uiso 0.765(10) 1 d PD A 1 
H42A H 0.3256 0.0682 0.7501 0.074 Uiso 0.765(10) 1 calc PR A 1 
H42B H 0.3689 0.1394 0.7637 0.074 Uiso 0.765(10) 1 calc PR A 1 
C42' C 0.401(2) 0.0561(15) 0.7995(17) 0.062(3) Uiso 0.235(10) 1 d PD A 2 
H42C H 0.4075 0.0105 0.8107 0.074 Uiso 0.235(10) 1 calc PR A 2 
H42D H 0.3272 0.0636 0.7529 0.074 Uiso 0.235(10) 1 calc PR A 2 
C43 C 0.3814(10) 0.0900(6) 0.8972(6) 0.129(4) Uani 1 1 d D . . 
H43A H 0.2980 0.1031 0.9137 0.155 Uiso 0.765(10) 1 calc PR A 1 
H43B H 0.3947 0.0461 0.9173 0.155 Uiso 0.765(10) 1 calc PR A 1 
H43C H 0.3058 0.1161 0.8852 0.155 Uiso 0.235(10) 1 calc PR A 2 
H43D H 0.3615 0.0572 0.9430 0.155 Uiso 0.235(10) 1 calc PR A 2 
C44 C 0.4759(10) 0.1291(7) 0.9469(8) 0.150(5) Uani 1 1 d D A . 
H44A H 0.4758 0.1210 1.0166 0.180 Uiso 0.765(10) 1 calc PR A 1 
H44B H 0.4506 0.1731 0.9359 0.180 Uiso 0.765(10) 1 calc PR A 1 
H44C H 0.4640 0.1352 1.0156 0.180 Uiso 0.235(10) 1 calc PR A 2 
H44D H 0.4855 0.1698 0.9150 0.180 Uiso 0.235(10) 1 calc PR A 2 
C45 C 0.6039(11) 0.1228(7) 0.9224(8) 0.094(4) Uiso 0.765(10) 1 d PD A 1 
H45A H 0.6405 0.0838 0.9504 0.113 Uiso 0.765(10) 1 calc PR A 1 
H45B H 0.6543 0.1583 0.9498 0.113 Uiso 0.765(10) 1 calc PR A 1 
C45' C 0.578(3) 0.0842(19) 0.931(2) 0.094(4) Uiso 0.235(10) 1 d PD A 2 
H45C H 0.5515 0.0431 0.9546 0.113 Uiso 0.235(10) 1 calc PR A 2 
H45D H 0.6512 0.0971 0.9748 0.113 Uiso 0.235(10) 1 calc PR A 2 
C46 C 0.6068(10) 0.1217(6) 0.8111(7) 0.073(3) Uiso 0.765(10) 1 d PD A 1 
H46A H 0.5913 0.1645 0.7863 0.088 Uiso 0.765(10) 1 calc PR A 1 
H46B H 0.6915 0.1095 0.7965 0.088 Uiso 0.765(10) 1 calc PR A 1 
C46' C 0.626(2) 0.0728(19) 0.8291(17) 0.073(3) Uiso 0.235(10) 1 d PD A 2 
H46C H 0.6898 0.1041 0.8164 0.088 Uiso 0.235(10) 1 calc PR A 2 
H46D H 0.6628 0.0307 0.8259 0.088 Uiso 0.235(10) 1 calc PR A 2 
O5 O 0.8609(5) 0.1487(3) 0.6016(4) 0.0769(16) Uani 1 1 d D . . 
C52 C 0.969(2) 0.1839(17) 0.5801(17) 0.091(4) Uiso 0.297(13) 1 d PD B 3 
H52A H 0.9466 0.2276 0.5631 0.109 Uiso 0.297(13) 1 calc PR B 3 
H52B H 1.0087 0.1648 0.5261 0.109 Uiso 0.297(13) 1 calc PR B 3 
C52' C 0.9365(11) 0.2038(6) 0.6187(12) 0.091(4) Uiso 0.703(13) 1 d PD B 4 
H52C H 0.8947 0.2343 0.6580 0.109 Uiso 0.703(13) 1 calc PR B 4 
H52D H 0.9525 0.2238 0.5573 0.109 Uiso 0.703(13) 1 calc PR B 4 
C53 C 1.0563(9) 0.1815(6) 0.6716(8) 0.115(4) Uani 1 1 d D . . 
H53A H 1.1445 0.1836 0.6576 0.137 Uiso 0.297(13) 1 calc PR B 3 
H53B H 1.0391 0.2160 0.7154 0.137 Uiso 0.297(13) 1 calc PR B 3 
H53C H 1.1218 0.1771 0.6270 0.137 Uiso 0.703(13) 1 calc PR B 4 
H53D H 1.0856 0.2113 0.7229 0.137 Uiso 0.703(13) 1 calc PR B 4 
C54 C 1.0280(10) 0.1213(6) 0.7124(9) 0.129(4) Uani 1 1 d D B . 
H54A H 1.0547 0.1200 0.7821 0.155 Uiso 0.297(13) 1 calc PR B 3 
H54B H 1.0692 0.0870 0.6802 0.155 Uiso 0.297(13) 1 calc PR B 3 
H54C H 0.9999 0.1268 0.7772 0.155 Uiso 0.703(13) 1 calc PR B 4 
H54D H 1.1027 0.0942 0.7177 0.155 Uiso 0.703(13) 1 calc PR B 4 
C55 C 0.8896(17) 0.1167(15) 0.6942(17) 0.080(4) Uiso 0.297(13) 1 d PD B 3 
H55A H 0.8625 0.0726 0.6901 0.095 Uiso 0.297(13) 1 calc PR B 3 
H55B H 0.8484 0.1377 0.7457 0.095 Uiso 0.297(13) 1 calc PR B 3 
C55' C 0.9259(12) 0.0927(5) 0.6454(10) 0.080(4) Uiso 0.703(13) 1 d PD B 4 
H55C H 0.9605 0.0665 0.5960 0.095 Uiso 0.703(13) 1 calc PR B 4 
H55D H 0.8691 0.0671 0.6809 0.095 Uiso 0.703(13) 1 calc PR B 4 
Li1 Li 0.6929(11) 0.1359(6) 0.5386(9) 0.057(3) Uani 1 1 d . A . 
Li2 Li 0.5380(11) 0.0442(6) 0.4214(8) 0.056(3) Uani 1 1 d . . . 
C4S C 0.8920(15) 0.0000(7) 0.9529(13) 0.157(5) Uani 1 1 d . . . 
C1S C 1.0854(16) -0.0015(7) 0.9397(12) 0.154(5) Uani 1 1 d . . . 
O1S O 0.977(2) -0.0219(11) 0.8966(12) 0.149(7) Uani 0.50 1 d P . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
P1 0.0496(11) 0.0578(12) 0.0392(10) 0.0041(9) 0.0009(8) 0.0002(10) 
P2 0.0471(11) 0.0604(12) 0.0410(10) 0.0003(9) 0.0020(8) 0.0021(10) 
P3 0.0545(12) 0.0620(13) 0.0390(10) 0.0051(9) 0.0014(9) 0.0010(10) 
N1 0.041(3) 0.064(4) 0.040(3) 0.010(3) 0.005(3) 0.003(3) 
C1 0.054(5) 0.083(5) 0.037(4) 0.001(4) 0.011(3) 0.008(5) 
C11 0.062(5) 0.102(7) 0.072(6) -0.003(5) 0.018(4) 0.021(5) 
C12 0.069(6) 0.102(7) 0.097(7) 0.002(6) 0.038(5) -0.015(6) 
C13 0.082(6) 0.156(9) 0.042(4) -0.004(5) 0.012(4) 0.007(6) 
N2 0.049(3) 0.049(3) 0.039(3) 0.000(3) 0.005(3) 0.001(3) 
C2 0.059(5) 0.069(5) 0.046(4) -0.005(4) 0.007(4) 0.002(4) 
C21 0.097(6) 0.075(6) 0.064(5) -0.027(4) 0.016(5) -0.013(5) 
C22 0.082(6) 0.061(5) 0.104(7) -0.003(5) 0.002(5) 0.014(5) 
C23 0.097(7) 0.067(5) 0.073(6) -0.009(4) 0.017(5) -0.018(5) 
N3 0.040(3) 0.059(4) 0.034(3) -0.006(3) -0.004(2) -0.002(3) 
C3 0.037(4) 0.073(5) 0.056(5) 0.000(4) -0.007(4) 0.005(4) 
C31 0.036(4) 0.090(6) 0.082(6) 0.000(5) -0.004(4) -0.003(4) 
C32 0.064(5) 0.102(6) 0.053(5) -0.014(5) -0.015(4) 0.010(5) 
C33 0.066(5) 0.086(6) 0.066(5) 0.002(5) -0.013(4) 0.016(5) 
C41 0.059(5) 0.129(7) 0.040(4) -0.007(5) 0.001(4) -0.006(5) 
C43 0.104(8) 0.219(13) 0.071(6) -0.041(8) 0.045(6) -0.013(9) 
C44 0.141(11) 0.238(15) 0.072(7) -0.084(9) 0.016(7) 0.017(11) 
O5 0.059(3) 0.088(4) 0.080(4) 0.010(3) -0.013(3) -0.020(3) 
C53 0.071(7) 0.140(10) 0.126(9) 0.000(8) -0.026(6) -0.020(7) 
C54 0.110(9) 0.137(10) 0.130(10) 0.009(8) -0.043(7) -0.017(8) 
Li1 0.049(7) 0.066(8) 0.058(7) 0.003(6) 0.006(6) -0.002(6) 
Li2 0.054(7) 0.061(8) 0.054(7) 0.010(6) 0.001(6) -0.007(6) 
C4S 0.179(14) 0.149(12) 0.140(13) -0.045(10) 0.004(12) 0.029(11) 
C1S 0.160(14) 0.185(13) 0.118(12) -0.038(10) 0.014(10) -0.032(11) 
O1S 0.137(15) 0.21(2) 0.097(12) -0.021(13) 0.012(12) -0.012(16) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
P1 N1 1.651(5) . ? 
P1 N2 1.787(5) . ? 
P1 N3 1.792(5) . ? 
P1 P2 2.666(3) . ? 
P1 Li2 2.690(12) . ? 
P1 Li1 2.721(12) . ? 
P2 N3 1.772(5) . ? 
P2 N2 1.773(6) . ? 
P2 P3 2.171(3) . ? 
P2 Li1 2.943(12) . ? 
P3 C41 1.872(7) . ? 
P3 Li2 2.570(12) 3_656 ? 
P3 Li1 2.624(12) . ? 
P3 Li2 2.881(12) . ? 
N1 C1 1.485(7) . ? 
N1 Li2 1.975(13) . ? 
N1 Li1 2.091(13) . ? 
C1 C13 1.519(8) . ? 
C1 C12 1.528(8) . ? 
C1 C11 1.540(8) . ? 
N2 C2 1.499(8) . ? 
N2 Li1 2.110(13) . ? 
C2 C23 1.525(8) . ? 
C2 C21 1.524(8) . ? 
C2 C22 1.531(8) . ? 
N3 C3 1.509(7) . ? 
N3 Li2 2.112(13) . ? 
C3 C33 1.521(8) . ? 
C3 C32 1.537(8) . ? 
C3 C31 1.536(8) . ? 
C41 C46' 1.469(16) . ? 
C41 C46 1.477(10) . ? 
C41 C42 1.481(10) . ? 
C41 C42' 1.482(16) . ? 
C42 C43 1.579(11) . ? 
C42' C43 1.564(16) . ? 
C43 C44 1.431(11) . ? 
C44 C45 1.445(12) . ? 
C44 C45' 1.478(17) . ? 
C45 C46 1.546(12) . ? 
C45' C46' 1.570(17) . ? 
O5 C52' 1.427(11) . ? 
O5 C52 1.433(16) . ? 
O5 C55 1.457(15) . ? 
O5 C55' 1.477(10) . ? 
O5 Li1 1.938(13) . ? 
C52 C53 1.498(16) . ? 
C52' C53 1.489(12) . ? 
C53 C54 1.440(13) . ? 
C54 C55 1.478(16) . ? 
C54 C55' 1.492(12) . ? 
Li2 P3 2.570(12) 3_656 ? 
Li2 Li2 3.04(2) 3_656 ? 
C4S O1S 1.33(2) . ? 
C4S C1S 1.484(18) 3_757 ? 
C1S O1S 1.325(19) . ? 
C1S C4S 1.484(18) 3_757 ? 
 
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 P1 N2 101.0(3) . . ? 
N1 P1 N3 97.9(3) . . ? 
N2 P1 N3 82.6(2) . . ? 
N1 P1 P2 103.51(19) . . ? 
N2 P1 P2 41.31(18) . . ? 
N3 P1 P2 41.30(16) . . ? 
N1 P1 Li2 47.0(3) . . ? 
N2 P1 Li2 99.5(3) . . ? 
N3 P1 Li2 51.6(3) . . ? 
P2 P1 Li2 73.1(3) . . ? 
N1 P1 Li1 50.2(3) . . ? 
N2 P1 Li1 50.8(3) . . ? 
N3 P1 Li1 90.4(3) . . ? 
P2 P1 Li1 66.2(2) . . ? 
Li2 P1 Li1 65.8(4) . . ? 
N3 P2 N2 83.6(2) . . ? 
N3 P2 P3 98.60(19) . . ? 
N2 P2 P3 104.07(19) . . ? 
N3 P2 P1 41.89(17) . . ? 
N2 P2 P1 41.70(17) . . ? 
P3 P2 P1 106.18(9) . . ? 
N3 P2 Li1 83.9(3) . . ? 
N2 P2 Li1 45.2(3) . . ? 
P3 P2 Li1 59.5(2) . . ? 
P1 P2 Li1 57.8(2) . . ? 
C41 P3 P2 104.2(3) . . ? 
C41 P3 Li2 107.8(4) . 3_656 ? 
P2 P3 Li2 117.5(3) . 3_656 ? 
C41 P3 Li1 120.7(4) . . ? 
P2 P3 Li1 75.1(3) . . ? 
Li2 P3 Li1 125.2(4) 3_656 . ? 
C41 P3 Li2 174.9(4) . . ? 
P2 P3 Li2 76.8(2) . . ? 
Li2 P3 Li2 67.6(4) 3_656 . ? 
Li1 P3 Li2 64.4(4) . . ? 
C1 N1 P1 120.0(4) . . ? 
C1 N1 Li2 124.8(6) . . ? 
P1 N1 Li2 95.4(4) . . ? 
C1 N1 Li1 123.4(5) . . ? 
P1 N1 Li1 92.5(4) . . ? 
Li2 N1 Li1 92.6(5) . . ? 
N1 C1 C13 111.0(6) . . ? 
N1 C1 C12 111.8(6) . . ? 
C13 C1 C12 111.0(7) . . ? 
N1 C1 C11 106.3(5) . . ? 
C13 C1 C11 109.0(6) . . ? 
C12 C1 C11 107.5(6) . . ? 
C2 N2 P2 120.5(4) . . ? 
C2 N2 P1 121.2(4) . . ? 
P2 N2 P1 97.0(3) . . ? 
C2 N2 Li1 124.3(5) . . ? 
P2 N2 Li1 98.2(4) . . ? 
P1 N2 Li1 88.2(4) . . ? 
N2 C2 C23 108.8(6) . . ? 
N2 C2 C21 107.6(6) . . ? 
C23 C2 C21 109.4(6) . . ? 
N2 C2 C22 112.7(6) . . ? 
C23 C2 C22 109.6(6) . . ? 
C21 C2 C22 108.6(6) . . ? 
C3 N3 P2 117.1(4) . . ? 
C3 N3 P1 121.1(4) . . ? 
P2 N3 P1 96.8(2) . . ? 
C3 N3 Li2 119.5(5) . . ? 
P2 N3 Li2 110.0(4) . . ? 
P1 N3 Li2 86.7(4) . . ? 
N3 C3 C33 112.5(6) . . ? 
N3 C3 C32 107.4(5) . . ? 
C33 C3 C32 109.3(6) . . ? 
N3 C3 C31 107.8(5) . . ? 
C33 C3 C31 109.7(6) . . ? 
C32 C3 C31 110.1(6) . . ? 
C46' C41 C46 43.1(14) . . ? 
C46' C41 C42 123.7(12) . . ? 
C46 C41 C42 107.7(8) . . ? 
C46' C41 C42' 110.7(19) . . ? 
C46 C41 C42' 122.7(10) . . ? 
C42 C41 C42' 34.6(13) . . ? 
C46' C41 P3 120.4(12) . . ? 
C46 C41 P3 116.3(6) . . ? 
C42 C41 P3 115.8(5) . . ? 
C42' C41 P3 119.7(9) . . ? 
C41 C42 C43 110.6(7) . . ? 
C41 C42' C43 111.4(12) . . ? 
C44 C43 C42' 122.6(10) . . ? 
C44 C43 C42 109.4(9) . . ? 
C42' C43 C42 32.6(12) . . ? 
C43 C44 C45 118.2(10) . . ? 
C43 C44 C45' 93(2) . . ? 
C45 C44 C45' 34.9(17) . . ? 
C44 C45 C46 110.2(10) . . ? 
C44 C45' C46' 123(2) . . ? 
C41 C46 C45 115.5(9) . . ? 
C41 C46' C45' 106(2) . . ? 
C52' O5 C52 32.0(14) . . ? 
C52' O5 C55 99.6(13) . . ? 
C52 O5 C55 108.6(12) . . ? 
C52' O5 C55' 110.8(7) . . ? 
C52 O5 C55' 98.5(14) . . ? 
C55 O5 C55' 38.1(12) . . ? 
C52' O5 Li1 132.4(7) . . ? 
C52 O5 Li1 135.3(9) . . ? 
C55 O5 Li1 116.1(9) . . ? 
C55' O5 Li1 116.8(6) . . ? 
O5 C52 C53 104.7(12) . . ? 
O5 C52' C53 105.5(9) . . ? 
C54 C53 C52' 105.8(9) . . ? 
C54 C53 C52 103.1(13) . . ? 
C52' C53 C52 30.6(14) . . ? 
C53 C54 C55 103.6(13) . . ? 
C53 C54 C55' 106.6(9) . . ? 
C55 C54 C55' 37.6(12) . . ? 
O5 C55 C54 104.0(12) . . ? 
O5 C55' C54 102.4(8) . . ? 
O5 Li1 N1 128.8(6) . . ? 
O5 Li1 N2 132.5(7) . . ? 
N1 Li1 N2 78.3(4) . . ? 
O5 Li1 P3 119.5(6) . . ? 
N1 Li1 P3 102.4(5) . . ? 
N2 Li1 P3 81.6(4) . . ? 
O5 Li1 P1 147.0(6) . . ? 
N1 Li1 P1 37.3(2) . . ? 
N2 Li1 P1 41.0(2) . . ? 
P3 Li1 P1 93.0(4) . . ? 
O5 Li1 P2 145.9(6) . . ? 
N1 Li1 P2 84.7(4) . . ? 
N2 Li1 P2 36.6(2) . . ? 
P3 Li1 P2 45.46(19) . . ? 
P1 Li1 P2 56.0(2) . . ? 
N1 Li2 N3 78.9(5) . . ? 
N1 Li2 P3 147.5(6) . 3_656 ? 
N3 Li2 P3 122.0(5) . 3_656 ? 
N1 Li2 P1 37.7(3) . . ? 
N3 Li2 P1 41.7(3) . . ? 
P3 Li2 P1 149.7(5) 3_656 . ? 
N1 Li2 P3 97.1(5) . . ? 
N3 Li2 P3 72.0(4) . . ? 
P3 Li2 P3 112.4(4) 3_656 . ? 
P1 Li2 P3 88.2(4) . . ? 
N1 Li2 Li2 146.1(8) . 3_656 ? 
N3 Li2 Li2 99.0(6) . 3_656 ? 
P3 Li2 Li2 61.1(4) 3_656 3_656 ? 
P1 Li2 Li2 134.4(7) . 3_656 ? 
P3 Li2 Li2 51.4(4) . 3_656 ? 
O1S C4S C1S 122.6(15) . 3_757 ? 
O1S C1S C4S 120.6(15) . 3_757 ? 
C1S O1S C4S 103.7(17) . . ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              22.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.338 
_refine_diff_density_min   -0.345 
_refine_diff_density_rms    0.075