 
data_squeezed1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C84 H76 K2 Li2 N12 Np4 O16' 
_chemical_formula_weight          2549.65 
 
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' 
 'Np'  'Np' -11.4937   4.1493 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.2009   0.2494 
 '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                    16.766(10) 
_cell_length_b                    14.812(9) 
_cell_length_c                    23.241(14) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.680(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      5732(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     205(2) 
_cell_measurement_reflns_used     5128
_cell_measurement_theta_min       4.82
_cell_measurement_theta_max       20.96
 
_exptl_crystal_description        prism 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.05 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.477 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2416 
_exptl_absorpt_coefficient_mu     3.722 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.4955 
_exptl_absorpt_correction_T_max   0.7446 
_exptl_absorpt_process_details    'SADABS 2008/1 Bruker AXS Madison WI' 
 
_exptl_special_details 
; 
Due to the radiation and contamination hazards imposed by 237Np, 
the crystal was contained inside a plastic microRT tube.  The 
crystal was small and weakly diffractining and frames collected 
at 240 seconds exposure.  Only one and a half data spheres were 
suitable for inclusion in the refinement. The structure is not of adequate quality for metric analysis but displays the neptunyl tetramic core similar to that seen in compund 1 in this paper.  Repeated attempts were made to grow larger crystals, but with the limited availability of neptunium and the difficulties involved in the the preparation of samples the strongest diffracting crystal 
was chosen after numerous attempts.  Np, O, N, K and Li atoms were refined anistopically with restraints, O2, O5, O7, O4 C13, C20, 
C22, C25, C33, C40, C41 and C42 were refined isostropically
Hydrogen atomes are in calculated positions.  SQUEEZE found 571 electrons in the voids of the unit cell, corresponding to approximately 286 electrons associated with each cluster and 
likely arise from solvent pyridine molecules not found in the structure.  
; 
 
_diffrn_ambient_temperature       205(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11300 
_diffrn_reflns_av_R_equivalents   0.0906 
_diffrn_reflns_av_sigmaI/netI     0.1713 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          4.83 
_diffrn_reflns_theta_max          21.38 
_reflns_number_total              5533 
_reflns_number_gt                 2936 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT'  
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
 
_refine_special_details 
; 
Refinement of F² against ALL reflections.  The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement.  R-factors based on F² are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. Restraints used DELU 0.01, SIMU 0.04 and ISOR 0.1 on all anistropic atoms
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1169P)²+724.3289P] where P=(Fo²+2Fc²)/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          5533 
_refine_ls_number_parameters      471 
_refine_ls_number_restraints      723 
_refine_ls_R_factor_all           0.2208 
_refine_ls_R_factor_gt            0.1446 
_refine_ls_wR_factor_ref          0.3537 
_refine_ls_wR_factor_gt           0.3153 
_refine_ls_goodness_of_fit_ref    1.061 
_refine_ls_restrained_S_all       1.001 
_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 
C1 C -0.054(3) 1.041(4) 0.1927(18) 0.065(6) Uani 1 1 d U . . 
C2 C 0.038(4) 0.612(5) -0.064(3) 0.111(12) Uani 1 1 d U . . 
H2A H 0.0347 0.5949 -0.1046 0.133 Uiso 1 1 calc R . . 
H2B H 0.0560 0.5594 -0.0414 0.133 Uiso 1 1 calc R . . 
C3 C -0.037(4) 0.635(4) -0.052(3) 0.102(11) Uani 1 1 d U . . 
H3A H -0.0710 0.5812 -0.0564 0.122 Uiso 1 1 calc R . . 
H3B H -0.0598 0.6790 -0.0797 0.122 Uiso 1 1 calc R . . 
C4 C 0.445(4) 0.672(6) 0.158(3) 0.124(15) Uani 1 1 d U . . 
H4 H 0.4811 0.6378 0.1826 0.149 Uiso 1 1 calc R . . 
C5 C -0.136(3) 0.790(4) 0.160(2) 0.084(9) Uani 1 1 d U . . 
H5 H -0.1098 0.8338 0.1835 0.101 Uiso 1 1 calc R . . 
C6 C -0.097(3) 0.773(4) 0.111(2) 0.072(7) Uani 1 1 d U . . 
C7 C -0.198(4) 0.631(5) 0.102(3) 0.109(12) Uani 1 1 d U . . 
H7 H -0.2171 0.5772 0.0850 0.130 Uiso 1 1 calc R . . 
C8 C 0.151(4) 0.682(5) -0.088(2) 0.103(11) Uani 1 1 d U . . 
H8 H 0.1507 0.6360 -0.1147 0.124 Uiso 1 1 calc R . . 
C9 C 0.284(4) 0.733(5) -0.126(3) 0.110(12) Uani 1 1 d U . . 
H9 H 0.2926 0.6774 -0.1420 0.132 Uiso 1 1 calc R . . 
C10 C 0.473(4) 0.735(6) 0.110(3) 0.132(17) Uani 1 1 d U . . 
H10 H 0.5241 0.7434 0.0998 0.158 Uiso 1 1 calc R . . 
C11 C 0.268(3) 1.104(3) 0.029(2) 0.063(9) Uani 1 1 d U . . 
C12 C 0.410(4) 1.061(4) 0.050(3) 0.095(13) Uani 1 1 d U . . 
H12 H 0.4500 1.0303 0.0738 0.114 Uiso 1 1 calc R . . 
C13 C 0.430(5) 1.105(5) 0.003(3) 0.113(16) Uiso 1 1 d U . . 
H13 H 0.4833 1.1103 -0.0036 0.135 Uiso 1 1 calc R . . 
C14 C -0.130(4) 0.677(4) 0.084(2) 0.088(8) Uani 1 1 d U . . 
C15 C -0.200(4) 0.760(5) 0.182(3) 0.104(12) Uani 1 1 d U . . 
H15 H -0.2206 0.7877 0.2132 0.125 Uiso 1 1 calc R . . 
C16 C -0.236(4) 0.675(5) 0.151(3) 0.114(13) Uani 1 1 d U . . 
H16 H -0.2823 0.6503 0.1622 0.137 Uiso 1 1 calc R . . 
C17 C -0.112(4) 0.645(4) 0.030(2) 0.091(10) Uani 1 1 d U . . 
H17 H -0.1489 0.6063 0.0099 0.110 Uiso 1 1 calc R . . 
C18 C 0.211(4) 0.757(5) -0.084(2) 0.101(10) Uani 1 1 d U . . 
C19 C 0.350(4) 0.876(5) -0.098(2) 0.099(12) Uani 1 1 d U . . 
H19 H 0.3969 0.9104 -0.0950 0.119 Uiso 1 1 calc R . . 
C20 C 0.333(5) 0.816(5) -0.132(3) 0.117(15) Uiso 1 1 d U . . 
H20 H 0.3526 0.8222 -0.1677 0.141 Uiso 1 1 calc R . . 
C21 C 0.281(3) 0.886(5) -0.060(2) 0.090(11) Uani 1 1 d U . . 
H21 H 0.2812 0.9409 -0.0405 0.108 Uiso 1 1 calc R . . 
C22 C 0.373(5) 1.142(5) -0.034(3) 0.119(19) Uiso 1 1 d U . . 
H22 H 0.3844 1.1676 -0.0681 0.142 Uiso 1 1 calc R . . 
C23 C 0.071(4) 0.963(4) 0.2462(18) 0.080(10) Uani 1 1 d U . . 
H23 H 0.0893 0.9316 0.2796 0.096 Uiso 1 1 calc R . . 
C24 C -0.014(4) 0.989(4) 0.2428(18) 0.078(9) Uani 1 1 d U . . 
C25 C 0.285(4) 1.140(4) -0.017(2) 0.081(13) Uiso 1 1 d U . . 
H25 H 0.2438 1.1658 -0.0425 0.097 Uiso 1 1 calc R . . 
C26 C 0.215(4) 0.825(5) -0.049(2) 0.083(9) Uani 1 1 d U . . 
C27 C 0.308(4) 0.753(5) 0.090(3) 0.105(12) Uani 1 1 d U . . 
H27 H 0.2628 0.7676 0.0651 0.126 Uiso 1 1 calc R . . 
C28 C 0.209(4) 0.943(4) 0.231(2) 0.089(11) Uani 1 1 d U . . 
H28A H 0.2373 0.9875 0.2561 0.106 Uiso 1 1 calc R . . 
H28B H 0.2052 0.8878 0.2529 0.106 Uiso 1 1 calc R . . 
C29 C -0.056(4) 0.960(4) 0.289(2) 0.089(11) Uani 1 1 d U . . 
H29 H -0.0277 0.9334 0.3217 0.107 Uiso 1 1 calc R . . 
C30 C -0.182(4) 1.028(4) 0.240(2) 0.089(11) Uani 1 1 d U . . 
H30 H -0.2364 1.0390 0.2407 0.107 Uiso 1 1 calc R . . 
C31 C -0.136(4) 0.971(5) 0.286(2) 0.102(12) Uani 1 1 d U . . 
H31 H -0.1638 0.9423 0.3136 0.123 Uiso 1 1 calc R . . 
C32 C -0.136(3) 1.067(4) 0.193(2) 0.079(9) Uani 1 1 d U . . 
H32 H -0.1607 1.1071 0.1656 0.095 Uiso 1 1 calc R . . 
C33 C 0.191(4) 0.696(4) 0.266(2) 0.090(14) Uiso 1 1 d U . . 
H33 H 0.2457 0.6872 0.2656 0.107 Uiso 1 1 calc R . . 
C34 C 0.077(5) 0.716(5) 0.323(3) 0.121(14) Uani 1 1 d U . . 
H34 H 0.0577 0.7203 0.3583 0.145 Uiso 1 1 calc R . . 
C35 C 0.053(4) 0.709(5) 0.217(3) 0.107(13) Uani 1 1 d U . . 
H35 H 0.0203 0.7138 0.1817 0.129 Uiso 1 1 calc R . . 
C36 C 0.021(5) 0.714(5) 0.263(3) 0.119(14) Uani 1 1 d U . . 
H36 H -0.0347 0.7161 0.2619 0.142 Uiso 1 1 calc R . . 
C37 C 0.159(5) 0.711(5) 0.317(3) 0.115(14) Uani 1 1 d U . . 
H37 H 0.1942 0.7180 0.3504 0.139 Uiso 1 1 calc R . . 
C38 C 0.356(4) 0.669(5) 0.162(3) 0.101(13) Uani 1 1 d U . . 
H38 H 0.3427 0.6357 0.1935 0.121 Uiso 1 1 calc R . . 
C39 C 0.379(4) 0.787(6) 0.079(3) 0.132(16) Uani 1 1 d U . . 
H39 H 0.3796 0.8377 0.0555 0.158 Uiso 1 1 calc R . . 
C40 C 0.250(3) 0.927(4) 0.186(2) 0.076(13) Uiso 1 1 d U . . 
H40A H 0.2320 0.8687 0.1703 0.091 Uiso 1 1 calc R . . 
H40B H 0.3056 0.9205 0.2014 0.091 Uiso 1 1 calc R . . 
C41 C 0.325(3) 1.059(4) 0.066(2) 0.072(11) Uiso 1 1 d U . . 
C42 C 0.306(4) 1.003(4) 0.115(2) 0.080(15) Uiso 1 1 d U . . 
H42 H 0.3500 0.9702 0.1323 0.096 Uiso 1 1 calc R . . 
K1 K -0.1028(6) 0.9807(8) 0.0518(4) 0.055(3) Uani 1 1 d U . . 
Li1 Li 0.186(6) 0.675(8) 0.130(4) 0.098(13) Uani 1 1 d U . . 
N1 N -0.041(3) 0.669(3) 0.0044(19) 0.086(9) Uani 1 1 d U . . 
N2 N 0.104(3) 0.685(4) -0.0531(18) 0.097(9) Uani 1 1 d U . . 
N3 N 0.247(2) 0.990(2) 0.1373(13) 0.041(9) Uiso 1 1 d U . . 
N4 N 0.126(3) 0.977(3) 0.2103(16) 0.085(9) Uani 1 1 d U . . 
N5 N 0.138(3) 0.695(3) 0.217(2) 0.092(12) Uiso 1 1 d U . . 
N6 N 0.300(3) 0.699(4) 0.1338(19) 0.094(11) Uani 1 1 d U . . 
Np1 Np 0.10628(10) 1.06446(13) 0.11083(6) 0.0433(7) Uani 1 1 d U . . 
Np2 Np 0.05587(11) 0.80361(14) 0.02566(7) 0.0481(7) Uani 1 1 d U . . 
O1 O 0.0826(16) 0.958(2) 0.0725(11) 0.054(5) Uani 1 1 d U . . 
O2 O 0.1371(19) 1.165(2) 0.1498(12) 0.057(8) Uiso 1 1 d U . . 
O3 O 0.1200(18) 0.735(2) 0.0807(11) 0.063(6) Uani 1 1 d U . . 
O4 O -0.0134(16) 0.8639(17) -0.0336(10) 0.036(7) Uiso 1 1 d U . . 
O5 O -0.0394(19) 0.816(2) 0.0891(12) 0.055(8) Uiso 1 1 d U . . 
O6 O 0.162(2) 0.853(3) -0.0155(11) 0.071(6) Uani 1 1 d U . . 
O7 O 0.1900(17) 1.0993(19) 0.0389(11) 0.045(7) Uiso 1 1 d U . . 
O8 O -0.0228(19) 1.059(2) 0.1490(11) 0.064(5) Uani 1 1 d U . . 
 
 
_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 
C1 O8 1.23(5) . ? 
C1 C32 1.43(7) . ? 
C1 C24 1.49(7) . ? 
C1 K1 3.40(4) . ? 
C2 C3 1.38(8) . ? 
C2 N2 1.54(8) . ? 
C3 N1 1.41(6) . ? 
C4 C38 1.50(8) . ? 
C4 C10 1.57(10) . ? 
C5 C15 1.30(7) . ? 
C5 C6 1.40(7) . ? 
C6 O5 1.32(5) . ? 
C6 C14 1.62(8) . ? 
C6 K1 3.37(6) . ? 
C7 C14 1.42(8) . ? 
C7 C16 1.51(9) . ? 
C8 N2 1.19(7) . ? 
C8 C18 1.49(9) . ? 
C9 C20 1.49(9) . ? 
C9 C18 1.67(8) . ? 
C10 C39 1.83(9) . ? 
C11 C25 1.27(6) . ? 
C11 O7 1.35(5) . ? 
C11 C41 1.38(7) . ? 
C11 K1 3.39(5) 3_575 ? 
C12 C13 1.36(8) . ? 
C12 C41 1.51(8) . ? 
C13 C22 1.32(9) . ? 
C14 C17 1.40(7) . ? 
C15 C16 1.55(9) . ? 
C17 N1 1.45(7) . ? 
C18 C26 1.30(8) . ? 
C19 C20 1.21(8) . ? 
C19 C21 1.54(7) . ? 
C21 C26 1.48(8) . ? 
C22 C25 1.57(8) . ? 
C23 N4 1.33(6) . ? 
C23 C24 1.46(7) . ? 
C24 C29 1.42(7) . ? 
C25 K1 3.54(6) 3_575 ? 
C26 O6 1.32(6) . ? 
C26 K1 3.44(7) 3_575 ? 
C27 N6 1.31(7) . ? 
C27 C39 1.33(9) . ? 
C27 Li1 2.62(14) . ? 
C28 C40 1.33(6) . ? 
C28 N4 1.50(7) . ? 
C29 C31 1.35(8) . ? 
C30 C31 1.50(8) . ? 
C30 C32 1.53(7) . ? 
C33 C37 1.37(8) . ? 
C33 N5 1.37(7) . ? 
C34 C37 1.38(9) . ? 
C34 C36 1.59(9) . ? 
C35 C36 1.25(7) . ? 
C35 N5 1.44(7) . ? 
C38 N6 1.17(6) . ? 
C40 N3 1.46(6) . ? 
C41 C42 1.48(7) . ? 
C42 N3 1.19(6) . ? 
K1 O7 2.70(3) 3_575 ? 
K1 O8 2.75(3) . ? 
K1 O6 2.75(4) 3_575 ? 
K1 O5 2.76(3) . ? 
K1 O4 3.08(3) 3_575 ? 
K1 O1 3.09(3) 3_575 ? 
K1 O1 3.11(3) . ? 
K1 O4 3.14(3) . ? 
K1 C11 3.39(5) 3_575 ? 
K1 C26 3.44(7) 3_575 ? 
Li1 O3 1.74(9) . ? 
Li1 N6 1.93(11) . ? 
Li1 N5 2.27(11) . ? 
Li1 Np2 3.61(8) . ? 
N1 Np2 2.58(4) . ? 
N2 Np2 2.72(4) . ? 
N3 Np1 2.61(4) . ? 
N4 Np1 2.64(4) . ? 
Np1 O2 1.79(3) . ? 
Np1 O1 1.84(3) . ? 
Np1 O7 2.36(3) . ? 
Np1 O8 2.43(3) . ? 
Np1 O4 2.47(2) 3_575 ? 
Np1 K1 3.832(9) 3_575 ? 
Np2 O3 1.87(3) . ? 
Np2 O4 1.92(2) . ? 
Np2 O6 2.24(3) . ? 
Np2 O5 2.30(3) . ? 
Np2 O1 2.55(3) . ? 
Np2 K1 3.795(11) 3_575 ? 
O1 K1 3.09(3) 3_575 ? 
O4 Np1 2.47(2) 3_575 ? 
O4 K1 3.08(3) 3_575 ? 
O6 K1 2.75(4) 3_575 ? 
O7 K1 2.70(3) 3_575 ? 
 
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 
O8 C1 C32 117(4) . . ? 
O8 C1 C24 124(5) . . ? 
C32 C1 C24 119(5) . . ? 
O8 C1 K1 49(2) . . ? 
C32 C1 K1 87(3) . . ? 
C24 C1 K1 131(4) . . ? 
C3 C2 N2 117(5) . . ? 
C2 C3 N1 115(6) . . ? 
C38 C4 C10 116(6) . . ? 
C15 C5 C6 138(6) . . ? 
O5 C6 C5 132(5) . . ? 
O5 C6 C14 120(5) . . ? 
C5 C6 C14 108(5) . . ? 
O5 C6 K1 52(2) . . ? 
C5 C6 K1 100(4) . . ? 
C14 C6 K1 130(3) . . ? 
C14 C7 C16 115(6) . . ? 
N2 C8 C18 116(6) . . ? 
C20 C9 C18 110(6) . . ? 
C4 C10 C39 103(5) . . ? 
C25 C11 O7 119(5) . . ? 
C25 C11 C41 121(6) . . ? 
O7 C11 C41 119(4) . . ? 
C25 C11 K1 86(4) . 3_575 ? 
O7 C11 K1 48(2) . 3_575 ? 
C41 C11 K1 129(4) . 3_575 ? 
C13 C12 C41 122(6) . . ? 
C22 C13 C12 120(8) . . ? 
C17 C14 C7 111(6) . . ? 
C17 C14 C6 123(5) . . ? 
C7 C14 C6 124(6) . . ? 
C5 C15 C16 112(6) . . ? 
C7 C16 C15 122(6) . . ? 
C14 C17 N1 124(5) . . ? 
C26 C18 C8 126(6) . . ? 
C26 C18 C9 122(6) . . ? 
C8 C18 C9 111(5) . . ? 
C20 C19 C21 108(7) . . ? 
C19 C20 C9 129(7) . . ? 
C26 C21 C19 132(6) . . ? 
C13 C22 C25 118(7) . . ? 
N4 C23 C24 132(4) . . ? 
C29 C24 C23 116(5) . . ? 
C29 C24 C1 122(5) . . ? 
C23 C24 C1 122(5) . . ? 
C11 C25 C22 122(6) . . ? 
C11 C25 K1 73(4) . 3_575 ? 
C22 C25 K1 140(4) . 3_575 ? 
C18 C26 O6 129(6) . . ? 
C18 C26 C21 111(6) . . ? 
O6 C26 C21 119(6) . . ? 
C18 C26 K1 130(4) . 3_575 ? 
O6 C26 K1 48(3) . 3_575 ? 
C21 C26 K1 84(4) . 3_575 ? 
N6 C27 C39 124(6) . . ? 
N6 C27 Li1 45(3) . . ? 
C39 C27 Li1 169(5) . . ? 
C40 C28 N4 111(4) . . ? 
C31 C29 C24 120(6) . . ? 
C31 C30 C32 118(5) . . ? 
C29 C31 C30 122(6) . . ? 
C1 C32 C30 118(5) . . ? 
C37 C33 N5 116(6) . . ? 
C37 C34 C36 114(6) . . ? 
C36 C35 N5 122(7) . . ? 
C35 C36 C34 119(7) . . ? 
C33 C37 C34 126(7) . . ? 
N6 C38 C4 134(7) . . ? 
C27 C39 C10 120(7) . . ? 
C28 C40 N3 121(5) . . ? 
C11 C41 C42 123(5) . . ? 
C11 C41 C12 117(5) . . ? 
C42 C41 C12 119(5) . . ? 
N3 C42 C41 134(6) . . ? 
O7 K1 O8 175.8(10) 3_575 . ? 
O7 K1 O6 90.5(9) 3_575 3_575 ? 
O8 K1 O6 89.9(10) . 3_575 ? 
O7 K1 O5 90.7(9) 3_575 . ? 
O8 K1 O5 89.0(10) . . ? 
O6 K1 O5 178.5(11) 3_575 . ? 
O7 K1 O4 121.0(8) 3_575 3_575 ? 
O8 K1 O4 62.6(8) . 3_575 ? 
O6 K1 O4 60.0(9) 3_575 3_575 ? 
O5 K1 O4 118.5(9) . 3_575 ? 
O7 K1 O1 60.4(8) 3_575 3_575 ? 
O8 K1 O1 123.2(9) . 3_575 ? 
O6 K1 O1 61.5(8) 3_575 3_575 ? 
O5 K1 O1 118.4(9) . 3_575 ? 
O4 K1 O1 60.6(7) 3_575 3_575 ? 
O7 K1 O1 121.0(9) 3_575 . ? 
O8 K1 O1 62.3(9) . . ? 
O6 K1 O1 117.7(10) 3_575 . ? 
O5 K1 O1 60.8(9) . . ? 
O4 K1 O1 57.7(8) 3_575 . ? 
O1 K1 O1 87.8(7) 3_575 . ? 
O7 K1 O4 61.3(8) 3_575 . ? 
O8 K1 O4 121.9(9) . . ? 
O6 K1 O4 118.8(8) 3_575 . ? 
O5 K1 O4 61.1(7) . . ? 
O4 K1 O4 88.2(7) 3_575 . ? 
O1 K1 O4 57.3(7) 3_575 . ? 
O1 K1 O4 59.7(7) . . ? 
O7 K1 C6 84.6(10) 3_575 . ? 
O8 K1 C6 93.6(11) . . ? 
O6 K1 C6 159.1(12) 3_575 . ? 
O5 K1 C6 22.1(10) . . ? 
O4 K1 C6 138.8(11) 3_575 . ? 
O1 K1 C6 130.8(11) 3_575 . ? 
O1 K1 C6 81.8(11) . . ? 
O4 K1 C6 76.4(10) . . ? 
O7 K1 C11 21.9(9) 3_575 3_575 ? 
O8 K1 C11 154.1(11) . 3_575 ? 
O6 K1 C11 85.3(11) 3_575 3_575 ? 
O5 K1 C11 96.2(11) . 3_575 ? 
O4 K1 C11 133.3(10) 3_575 3_575 ? 
O1 K1 C11 76.1(10) 3_575 3_575 ? 
O1 K1 C11 141.3(10) . 3_575 ? 
O4 K1 C11 82.2(10) . 3_575 ? 
C6 K1 C11 82.7(12) . 3_575 ? 
O7 K1 C1 156.4(11) 3_575 . ? 
O8 K1 C1 19.6(10) . . ? 
O6 K1 C1 95.7(11) 3_575 . ? 
O5 K1 C1 83.6(11) . . ? 
O4 K1 C1 81.4(10) 3_575 . ? 
O1 K1 C1 141.6(11) 3_575 . ? 
O1 K1 C1 75.8(10) . . ? 
O4 K1 C1 132.3(11) . . ? 
C6 K1 C1 81.5(13) . . ? 
C11 K1 C1 136.0(12) 3_575 . ? 
O7 K1 C26 96.1(11) 3_575 3_575 ? 
O8 K1 C26 82.9(11) . 3_575 ? 
O6 K1 C26 21.0(10) 3_575 3_575 ? 
O5 K1 C26 159.6(11) . 3_575 ? 
O4 K1 C26 74.0(12) 3_575 3_575 ? 
O1 K1 C26 81.5(10) 3_575 3_575 ? 
O1 K1 C26 129.1(12) . 3_575 ? 
O4 K1 C26 138.5(10) . 3_575 ? 
C6 K1 C26 139.6(14) . 3_575 ? 
C11 K1 C26 83.6(13) 3_575 3_575 ? 
C1 K1 C26 82.5(12) . 3_575 ? 
O3 Li1 N6 119(6) . . ? 
O3 Li1 N5 105(5) . . ? 
N6 Li1 N5 113(5) . . ? 
O3 Li1 C27 90(5) . . ? 
N6 Li1 C27 29(2) . . ? 
N5 Li1 C27 129(6) . . ? 
O3 Li1 Np2 2(2) . . ? 
N6 Li1 Np2 117(5) . . ? 
N5 Li1 Np2 106(3) . . ? 
C27 Li1 Np2 88(3) . . ? 
C3 N1 C17 115(5) . . ? 
C3 N1 Np2 112(4) . . ? 
C17 N1 Np2 130(3) . . ? 
C8 N2 C2 112(5) . . ? 
C8 N2 Np2 138(5) . . ? 
C2 N2 Np2 108(3) . . ? 
C42 N3 C40 119(5) . . ? 
C42 N3 Np1 127(4) . . ? 
C40 N3 Np1 113(3) . . ? 
C23 N4 C28 116(4) . . ? 
C23 N4 Np1 127(3) . . ? 
C28 N4 Np1 117(3) . . ? 
C33 N5 C35 123(5) . . ? 
C33 N5 Li1 119(5) . . ? 
C35 N5 Li1 118(4) . . ? 
C38 N6 C27 121(6) . . ? 
C38 N6 Li1 133(6) . . ? 
C27 N6 Li1 106(5) . . ? 
O2 Np1 O1 175.5(13) . . ? 
O2 Np1 O7 90.8(11) . . ? 
O1 Np1 O7 87.6(11) . . ? 
O2 Np1 O8 93.4(12) . . ? 
O1 Np1 O8 89.9(12) . . ? 
O7 Np1 O8 153.2(10) . . ? 
O2 Np1 O4 97.4(11) . 3_575 ? 
O1 Np1 O4 86.3(10) . 3_575 ? 
O7 Np1 O4 76.7(9) . 3_575 ? 
O8 Np1 O4 76.5(9) . 3_575 ? 
O2 Np1 N3 92.1(12) . . ? 
O1 Np1 N3 83.5(11) . . ? 
O7 Np1 N3 70.4(10) . . ? 
O8 Np1 N3 135.8(10) . . ? 
O4 Np1 N3 145.8(9) 3_575 . ? 
O2 Np1 N4 88.2(14) . . ? 
O1 Np1 N4 89.9(14) . . ? 
O7 Np1 N4 134.7(13) . . ? 
O8 Np1 N4 72.0(13) . . ? 
O4 Np1 N4 148.2(12) 3_575 . ? 
N3 Np1 N4 64.4(13) . . ? 
O2 Np1 K1 130.6(10) . . ? 
O1 Np1 K1 53.7(9) . . ? 
O7 Np1 K1 114.4(7) . . ? 
O8 Np1 K1 45.8(6) . . ? 
O4 Np1 K1 53.5(6) 3_575 . ? 
N3 Np1 K1 135.4(8) . . ? 
N4 Np1 K1 99.8(10) . . ? 
O2 Np1 K1 127.9(9) . 3_575 ? 
O1 Np1 K1 52.7(9) . 3_575 ? 
O7 Np1 K1 44.1(7) . 3_575 ? 
O8 Np1 K1 116.2(6) . 3_575 ? 
O4 Np1 K1 54.8(6) 3_575 3_575 ? 
N3 Np1 K1 93.9(7) . 3_575 ? 
N4 Np1 K1 139.9(11) . 3_575 ? 
K1 Np1 K1 71.4(2) . 3_575 ? 
O3 Np2 O4 175.1(13) . . ? 
O3 Np2 O6 92.6(13) . . ? 
O4 Np2 O6 89.2(11) . . ? 
O3 Np2 O5 89.5(12) . . ? 
O4 Np2 O5 90.9(10) . . ? 
O6 Np2 O5 153.2(11) . . ? 
O3 Np2 O1 97.6(12) . . ? 
O4 Np2 O1 87.2(10) . . ? 
O6 Np2 O1 77.3(11) . . ? 
O5 Np2 O1 75.9(10) . . ? 
O3 Np2 N1 90.7(15) . . ? 
O4 Np2 N1 84.7(13) . . ? 
O6 Np2 N1 133.1(13) . . ? 
O5 Np2 N1 73.6(13) . . ? 
O1 Np2 N1 148.2(12) . . ? 
O3 Np2 N2 85.4(14) . . ? 
O4 Np2 N2 91.1(13) . . ? 
O6 Np2 N2 67.1(14) . . ? 
O5 Np2 N2 139.7(14) . . ? 
O1 Np2 N2 144.4(13) . . ? 
N1 Np2 N2 66.6(15) . . ? 
O3 Np2 Li1 2(2) . . ? 
O4 Np2 Li1 176(2) . . ? 
O6 Np2 Li1 90.6(19) . . ? 
O5 Np2 Li1 91.2(17) . . ? 
O1 Np2 Li1 97(2) . . ? 
N1 Np2 Li1 92(2) . . ? 
N2 Np2 Li1 85(2) . . ? 
O3 Np2 K1 130.2(11) . 3_575 ? 
O4 Np2 K1 53.7(8) . 3_575 ? 
O6 Np2 K1 45.9(10) . 3_575 ? 
O5 Np2 K1 115.8(8) . 3_575 ? 
O1 Np2 K1 54.0(7) . 3_575 ? 
N1 Np2 K1 136.0(11) . 3_575 ? 
N2 Np2 K1 97.4(11) . 3_575 ? 
Li1 Np2 K1 128(2) . 3_575 ? 
O3 Np2 K1 128.0(9) . . ? 
O4 Np2 K1 54.7(7) . . ? 
O6 Np2 K1 116.4(10) . . ? 
O5 Np2 K1 45.5(8) . . ? 
O1 Np2 K1 53.9(6) . . ? 
N1 Np2 K1 97.3(11) . . ? 
N2 Np2 K1 144.3(11) . . ? 
Li1 Np2 K1 129.1(16) . . ? 
K1 Np2 K1 71.7(3) 3_575 . ? 
Np1 O1 Np2 175.8(15) . . ? 
Np1 O1 K1 99.0(12) . 3_575 ? 
Np2 O1 K1 84.1(8) . 3_575 ? 
Np1 O1 K1 97.8(11) . . ? 
Np2 O1 K1 84.8(7) . . ? 
K1 O1 K1 92.2(7) 3_575 . ? 
Li1 O3 Np2 176(4) . . ? 
Np2 O4 Np1 177.5(14) . 3_575 ? 
Np2 O4 K1 96.1(10) . 3_575 ? 
Np1 O4 K1 86.3(7) 3_575 3_575 ? 
Np2 O4 K1 95.5(8) . . ? 
Np1 O4 K1 85.2(7) 3_575 . ? 
K1 O4 K1 91.8(7) 3_575 . ? 
C6 O5 Np2 144(3) . . ? 
C6 O5 K1 106(3) . . ? 
Np2 O5 K1 98.0(10) . . ? 
C26 O6 Np2 141(4) . . ? 
C26 O6 K1 111(3) . 3_575 ? 
Np2 O6 K1 98.4(13) . 3_575 ? 
C11 O7 Np1 143(3) . . ? 
C11 O7 K1 110(2) . 3_575 ? 
Np1 O7 K1 98.3(10) . 3_575 ? 
C1 O8 Np1 142(3) . . ? 
C1 O8 K1 112(3) . . ? 
Np1 O8 K1 94.8(9) . . ? 
 
_diffrn_measured_fraction_theta_max    0.854 
_diffrn_reflns_theta_full              21.38 
_diffrn_measured_fraction_theta_full   0.854 
_refine_diff_density_max    4.450 
_refine_diff_density_min   -3.997 
_refine_diff_density_rms    0.348 
