#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:55:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179906 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/02/7020246.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7020246
loop_
_publ_author_name
'Copping, Roy'
'Mougel, Victor'
'Den Auwer, Christophe'
'Berthon, Claude'
'Moisy, Philippe'
'Mazzanti, Marinella'
_publ_section_title
;
 A tetrameric neptunyl(v) cluster supported by a Schiff base ligand.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10900
_journal_page_last               10902
_journal_paper_doi               10.1039/c2dt31072d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C84 H76 K2 Li2 N12 Np4 O16'
_chemical_formula_weight         2549.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.680(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.766(10)
_cell_length_b                   14.812(9)
_cell_length_c                   23.241(14)
_cell_measurement_reflns_used    5128
_cell_measurement_temperature    205(2)
_cell_measurement_theta_max      20.96
_cell_measurement_theta_min      4.82
_cell_volume                     5732(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      205(2)
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1713
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11300
_diffrn_reflns_theta_full        21.38
_diffrn_reflns_theta_max         21.38
_diffrn_reflns_theta_min         4.83
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.450
_refine_diff_density_min         -3.997
_refine_diff_density_rms         0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5533
_refine_ls_number_restraints     723
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.2208
_refine_ls_R_factor_gt           0.1446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1169P)²+724.3289P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3153
_refine_ls_wR_factor_ref         0.3537
_reflns_number_gt                2936
_reflns_number_total             5533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31072d.cif
_cod_data_source_block           squeezed1
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7020246
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'
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
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
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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
