#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308493.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_4308493
loop_
_publ_author_name
'Mathieu Roger'
'Thérèse Arliguie'
'Pierre Thuéry'
'Marc Fourmigué'
'Michel Ephritikhine'
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      Bât. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       arliguie@drecam.cea.fr
_publ_contact_author_fax         '33 (0) 1 69 08 66 40'
_publ_contact_author_name        'T. Arliguie'
_publ_contact_author_phone       '33 (0) 1 69 08 60 42'
_publ_section_title
;
Tris(dithiolene) Complexes of Neodymium and Cerium: Mononuclear Species,
Chains, and Honeycomb Networks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              584
_journal_page_last               593
_journal_paper_doi               10.1021/ic049055i
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C42.5 H60.5 N2.5 Na3 Nd O9 S12'
_chemical_formula_weight         1348.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                114.415(3)
_cell_angle_beta                 91.860(3)
_cell_angle_gamma                116.398(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2753(9)
_cell_length_b                   14.8237(7)
_cell_length_c                   17.0518(10)
_cell_measurement_reflns_used    19776
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.76
_cell_volume                     2837.8(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ 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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.1003
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19776
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    1.431
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.218
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0431P)²+9.5422P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                7138
_reflns_number_total             9993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049055isi20041215_120324_3.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C42.50 H60.50 N2.50 Na3 Nd O9 S12'
_cod_database_code               4308493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Nd Nd 0.32083(3) 0.14793(3) 0.45607(3) 0.02909(12) Uani 1 1 d . . .
Na1 Na 0.0000 0.0000 0.5000 0.0684(16) Uani 1 2 d S . .
Na2 Na 0.5000 0.0000 0.5000 0.0347(9) Uani 1 2 d S . .
Na3 Na 0.5000 0.5000 0.5000 0.0395(10) Uani 1 2 d S . .
Na4 Na 0.1158(3) 0.7566(3) 0.9152(2) 0.0520(8) Uani 1 1 d . . .
Na5 Na 0.5000 0.5000 0.0000 0.0542(13) Uani 1 2 d S . .
S1A S 0.21287(14) 0.06094(15) 0.56640(12) 0.0316(4) Uani 1 1 d . . .
S2A S 0.10003(15) -0.02694(15) 0.35545(12) 0.0345(4) Uani 1 1 d . . .
S3A S 0.14114(16) -0.21532(16) 0.29164(13) 0.0413(5) Uani 1 1 d . . .
S4A S 0.26540(15) -0.12085(16) 0.51002(13) 0.0360(4) Uani 1 1 d . . .
C1A C 0.2033(5) -0.0592(6) 0.4742(5) 0.0302(16) Uani 1 1 d . . .
C2A C 0.1566(6) -0.0949(6) 0.3890(5) 0.0325(16) Uani 1 1 d . . .
C3A C 0.2283(6) -0.2564(6) 0.3284(5) 0.0394(19) Uani 1 1 d . . .
H3A1 H 0.2115 -0.3316 0.2826 0.047 Uiso 1 1 calc R . .
H3A2 H 0.3031 -0.2025 0.3361 0.047 Uiso 1 1 calc R . .
C4A C 0.2162(6) -0.2594(6) 0.4153(5) 0.0381(18) Uani 1 1 d . . .
H4A1 H 0.2550 -0.2943 0.4264 0.046 Uiso 1 1 calc R . .
H4A2 H 0.1401 -0.3075 0.4091 0.046 Uiso 1 1 calc R . .
S1B S 0.51773(15) 0.21941(15) 0.57025(12) 0.0328(4) Uani 1 1 d . . .
S2B S 0.42254(14) 0.02719(15) 0.35332(12) 0.0327(4) Uani 1 1 d . . .
S3B S 0.54063(16) 0.20127(17) 0.30392(13) 0.0381(4) Uani 1 1 d . . .
S4B S 0.64331(15) 0.40261(15) 0.52554(13) 0.0372(4) Uani 1 1 d . . .
C1B C 0.5538(6) 0.2531(6) 0.4838(5) 0.0325(16) Uani 1 1 d . . .
C2B C 0.5147(5) 0.1743(6) 0.3947(5) 0.0309(16) Uani 1 1 d . . .
C3B C 0.6323(7) 0.3512(8) 0.3491(6) 0.054(2) Uani 1 1 d . . .
H3B1 H 0.6733 0.3638 0.3068 0.064 Uiso 1 1 calc R . .
H3B2 H 0.5908 0.3898 0.3564 0.064 Uiso 1 1 calc R . .
C4B C 0.7115(6) 0.4050(7) 0.4388(6) 0.045(2) Uani 1 1 d . . .
H4B1 H 0.7645 0.4838 0.4556 0.054 Uiso 1 1 calc R . .
H4B2 H 0.7500 0.3637 0.4329 0.054 Uiso 1 1 calc R . .
S1C S 0.36601(17) 0.36978(16) 0.58227(13) 0.0388(4) Uani 1 1 d . . .
S2C S 0.32811(15) 0.27184(16) 0.36191(12) 0.0350(4) Uani 1 1 d . . .
S3C S 0.10204(18) 0.2050(2) 0.33787(17) 0.0547(6) Uani 1 1 d . . .
S4C S 0.1339(2) 0.2878(2) 0.56138(17) 0.0550(6) Uani 1 1 d . . .
C1C C 0.2406(6) 0.3056(6) 0.5071(5) 0.0375(18) Uani 1 1 d . . .
C2C C 0.2253(6) 0.2691(6) 0.4177(5) 0.0362(17) Uani 1 1 d . . .
C3C C -0.0016(11) 0.1969(14) 0.3982(10) 0.115(5) Uani 1 1 d U . .
H3C1 H -0.0514 0.2102 0.3708 0.138 Uiso 1 1 calc R . .
H3C2 H -0.0422 0.1190 0.3887 0.138 Uiso 1 1 calc R . .
C4C C 0.0284(9) 0.2660(12) 0.4843(9) 0.100(4) Uani 1 1 d U . .
H4C1 H -0.0361 0.2413 0.5053 0.120 Uiso 1 1 calc R . .
H4C2 H 0.0480 0.3410 0.4913 0.120 Uiso 1 1 calc R . .
O1 O -0.0304(7) 0.7924(8) 1.0145(6) 0.096(3) Uani 1 1 d U . .
O2 O 0.2033(6) 0.9383(6) 1.0781(5) 0.085(2) Uani 1 1 d U . .
O3 O 0.2999(6) 0.8063(8) 1.0084(6) 0.087(2) Uani 1 1 d U . .
O4 O 0.2190(6) 0.6474(6) 0.8266(5) 0.073(2) Uani 1 1 d U . .
O5 O 0.0036(6) 0.5649(5) 0.7468(5) 0.0665(18) Uani 1 1 d . . .
O6 O -0.0779(5) 0.7000(5) 0.8406(5) 0.0664(19) Uani 1 1 d . . .
O7 O 0.7079(4) 0.5537(4) 0.0681(3) 0.0403(12) Uani 1 1 d . . .
O8 O 0.6201(5) 0.6818(5) 0.1700(4) 0.0472(14) Uani 1 1 d . . .
O9 O 0.4013(5) 0.5953(5) 0.1147(4) 0.0470(14) Uani 1 1 d . . .
C1 C 0.0282(11) 0.8727(12) 1.1082(9) 0.105(4) Uani 1 1 d U . .
H1A H 0.0506 0.8358 1.1340 0.126 Uiso 1 1 calc R . .
H1B H -0.0196 0.8942 1.1404 0.126 Uiso 1 1 calc R . .
C2 C 0.1240(9) 0.9760(8) 1.1180(7) 0.080(3) Uani 1 1 d U . .
H2A H 0.1569 1.0330 1.1805 0.096 Uiso 1 1 calc R . .
H2B H 0.1041 1.0089 1.0864 0.096 Uiso 1 1 calc R . .
C3 C 0.2688(10) 0.9409(10) 1.1311(10) 0.090(4) Uani 1 1 d U . .
H3A H 0.2284 0.8847 1.1501 0.108 Uiso 1 1 calc R . .
H3B H 0.3048 1.0159 1.1836 0.108 Uiso 1 1 calc R . .
C4 C 0.3502(8) 0.9183(8) 1.0939(7) 0.069(3) Uani 1 1 d U . .
H4A H 0.3941 0.9161 1.1370 0.083 Uiso 1 1 calc R . .
H4B H 0.3974 0.9800 1.0823 0.083 Uiso 1 1 calc R . .
C5 C 0.3635(12) 0.7821(12) 0.9647(9) 0.097(4) Uani 1 1 d U . .
H5A H 0.4209 0.7925 1.0054 0.116 Uiso 1 1 calc R . .
H5B H 0.3969 0.8367 0.9428 0.116 Uiso 1 1 calc R . .
C6 C 0.3145(9) 0.6689(10) 0.8906(8) 0.074(3) Uani 1 1 d U . .
H6A H 0.2885 0.6131 0.9120 0.089 Uiso 1 1 calc R . .
H6B H 0.3678 0.6604 0.8591 0.089 Uiso 1 1 calc R . .
C7 C 0.1602(11) 0.5429(11) 0.7627(9) 0.095(4) Uani 1 1 d U . .
H7A H 0.1225 0.4922 0.7871 0.114 Uiso 1 1 calc R . .
H7B H 0.2058 0.5175 0.7302 0.114 Uiso 1 1 calc R . .
C8 C 0.0817(9) 0.5398(8) 0.7026(7) 0.074(3) Uani 1 1 d U . .
H8A H 0.0432 0.4646 0.6504 0.089 Uiso 1 1 calc R . .
H8B H 0.1200 0.5956 0.6826 0.089 Uiso 1 1 calc R . .
C9 C -0.0589(10) 0.5873(11) 0.7051(8) 0.085(3) Uani 1 1 d U . .
H9A H -0.0956 0.5250 0.6445 0.102 Uiso 1 1 calc R . .
H9B H -0.0133 0.6569 0.7021 0.102 Uiso 1 1 calc R . .
C10 C -0.1384(9) 0.6007(9) 0.7516(7) 0.074(3) Uani 1 1 d U . .
H10A H -0.1835 0.5324 0.7566 0.089 Uiso 1 1 calc R . .
H10B H -0.1845 0.6136 0.7197 0.089 Uiso 1 1 calc R . .
C11 C -0.1468(9) 0.7291(11) 0.8859(9) 0.081(3) Uani 1 1 d . . .
H11A H -0.2030 0.6633 0.8887 0.098 Uiso 1 1 calc R . .
H11B H -0.1812 0.7533 0.8552 0.098 Uiso 1 1 calc R . .
C12 C -0.0844(10) 0.8208(11) 0.9745(9) 0.081(4) Uani 1 1 d . . .
H12A H -0.0339 0.8889 0.9714 0.097 Uiso 1 1 calc R . .
H12B H -0.1324 0.8384 1.0089 0.097 Uiso 1 1 calc R . .
N1 N 0.1858(5) 0.8775(5) 0.8441(4) 0.0397(15) Uani 1 1 d . . .
C13 C 0.1384(7) 0.9340(7) 0.8363(6) 0.048(2) Uani 1 1 d . . .
H13 H 0.0797 0.9285 0.8604 0.057 Uiso 1 1 calc R . .
C14 C 0.1722(8) 1.0002(8) 0.7942(7) 0.059(3) Uani 1 1 d . . .
H14 H 0.1370 1.0386 0.7905 0.070 Uiso 1 1 calc R . .
C15 C 0.2577(8) 1.0092(8) 0.7577(6) 0.057(2) Uani 1 1 d . . .
H15 H 0.2811 1.0540 0.7294 0.068 Uiso 1 1 calc R . .
C16 C 0.3082(7) 0.9520(7) 0.7632(6) 0.046(2) Uani 1 1 d . . .
H16 H 0.3664 0.9562 0.7388 0.055 Uiso 1 1 calc R . .
C17 C 0.2692(7) 0.8871(7) 0.8070(6) 0.046(2) Uani 1 1 d . . .
H17 H 0.3031 0.8476 0.8108 0.055 Uiso 1 1 calc R . .
N2 N 0.0445(10) 0.6012(11) 0.9636(9) 0.037(3) Uiso 0.50 1 d P . .
C18 C -0.0253(13) 0.4898(14) 0.9047(11) 0.037(4) Uiso 0.50 1 d P . .
C19 C -0.0758(16) 0.4060(17) 0.9296(13) 0.048(4) Uiso 0.50 1 d P . .
C20 C 0.0542(14) 0.5653(16) 0.9781(13) 0.048(4) Uiso 0.50 1 d P . .
C21 C -0.0233(14) 0.4529(16) 0.9203(11) 0.039(4) Uiso 0.50 1 d P . .
C22 C -0.0676(13) 0.3774(14) 0.9521(11) 0.037(4) Uiso 0.50 1 d P . .
C23 C 0.7745(7) 0.6666(7) 0.1425(5) 0.048(2) Uani 1 1 d . . .
H23A H 0.7949 0.7236 0.1225 0.057 Uiso 1 1 calc R . .
H23B H 0.8402 0.6735 0.1689 0.057 Uiso 1 1 calc R . .
C24 C 0.7129(7) 0.6858(7) 0.2090(5) 0.047(2) Uani 1 1 d . . .
H24A H 0.6901 0.6272 0.2274 0.057 Uiso 1 1 calc R . .
H24B H 0.7580 0.7599 0.2613 0.057 Uiso 1 1 calc R . .
C25 C 0.5612(7) 0.7102(7) 0.2349(5) 0.045(2) Uani 1 1 d . . .
H25A H 0.6081 0.7858 0.2853 0.054 Uiso 1 1 calc R . .
H25B H 0.5341 0.6548 0.2567 0.054 Uiso 1 1 calc R . .
C26 C 0.4684(7) 0.7077(7) 0.1874(5) 0.045(2) Uani 1 1 d . . .
H26A H 0.4268 0.7277 0.2283 0.054 Uiso 1 1 calc R . .
H26B H 0.4961 0.7629 0.1654 0.054 Uiso 1 1 calc R . .
C27 C 0.3055(7) 0.5839(9) 0.0751(6) 0.061(3) Uani 1 1 d . . .
H27A H 0.3238 0.6393 0.0537 0.074 Uiso 1 1 calc R . .
H27B H 0.2656 0.5989 0.1192 0.074 Uiso 1 1 calc R . .
C28 C 0.2365(7) 0.4651(9) -0.0011(6) 0.063(3) Uani 1 1 d . . .
H28A H 0.2205 0.4095 0.0199 0.076 Uiso 1 1 calc R . .
H28B H 0.1685 0.4556 -0.0256 0.076 Uiso 1 1 calc R . .
N3 N 0.4322(5) 0.3560(6) 0.0509(5) 0.0444(16) Uani 1 1 d . . .
C29 C 0.3829(7) 0.2440(7) 0.0034(6) 0.046(2) Uani 1 1 d . . .
H29 H 0.3670 0.2115 -0.0585 0.056 Uiso 1 1 calc R . .
C30 C 0.3537(7) 0.1725(7) 0.0409(6) 0.051(2) Uani 1 1 d . . .
H30 H 0.3185 0.0934 0.0048 0.061 Uiso 1 1 calc R . .
C31 C 0.3775(8) 0.2197(7) 0.1332(6) 0.055(2) Uani 1 1 d . . .
H31 H 0.3586 0.1734 0.1603 0.066 Uiso 1 1 calc R . .
C32 C 0.4297(7) 0.3366(7) 0.1832(6) 0.046(2) Uani 1 1 d . . .
H32 H 0.4464 0.3716 0.2452 0.056 Uiso 1 1 calc R . .
C33 C 0.4565(7) 0.4002(7) 0.1402(6) 0.048(2) Uani 1 1 d . . .
H33 H 0.4941 0.4796 0.1748 0.057 Uiso 1 1 calc R . .
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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'
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
S1A Nd S1C 89.32(5) . . ?
S1A Nd S1B 86.86(5) . . ?
S1C Nd S1B 81.11(6) . . ?
S1A Nd S2C 144.37(5) . . ?
S1C Nd S2C 71.75(5) . . ?
S1B Nd S2C 118.24(5) . . ?
S1A Nd S2B 114.23(5) . . ?
S1C Nd S2B 141.99(6) . . ?
S1B Nd S2B 71.46(5) . . ?
S2C Nd S2B 98.38(5) . . ?
S1A Nd C1C 89.35(15) . . ?
S1C Nd C1C 35.78(16) . . ?
S1B Nd C1C 116.83(17) . . ?
S2C Nd C1C 57.58(16) . . ?
S2B Nd C1C 155.93(16) . . ?
S1A Nd S2A 71.43(5) . . ?
S1C Nd S2A 119.35(6) . . ?
S1B Nd S2A 148.95(6) . . ?
S2C Nd S2A 91.50(6) . . ?
S2B Nd S2A 97.01(5) . . ?
C1C Nd S2A 85.64(16) . . ?
S1A Nd C1B 122.56(16) . . ?
S1C Nd C1B 85.06(15) . . ?
S1B Nd C1B 35.79(15) . . ?
S2C Nd C1B 86.49(15) . . ?
S2B Nd C1B 57.32(14) . . ?
C1C Nd C1B 114.9(2) . . ?
S2A Nd C1B 153.49(15) . . ?
S1A Nd C2B 136.45(15) . . ?
S1C Nd C2B 107.18(14) . . ?
S1B Nd C2B 57.72(15) . . ?
S2C Nd C2B 78.88(15) . . ?
S2B Nd C2B 35.44(14) . . ?
C1C Nd C2B 127.4(2) . . ?
S2A Nd C2B 126.59(14) . . ?
C1B Nd C2B 27.3(2) . . ?
S1A Nd C1A 35.66(14) . . ?
S1C Nd C1A 124.97(14) . . ?
S1B Nd C1A 92.24(14) . . ?
S2C Nd C1A 148.39(15) . . ?
S2B Nd C1A 82.77(13) . . ?
C1C Nd C1A 117.9(2) . . ?
S2A Nd C1A 57.19(14) . . ?
C1B Nd C1A 119.09(19) . . ?
C2B Nd C1A 114.70(19) . . ?
S1A Nd C2C 108.93(15) . . ?
S1C Nd C2C 57.24(15) . . ?
S1B Nd C2C 134.16(15) . . ?
S2C Nd C2C 35.47(15) . . ?
S2B Nd C2C 130.91(15) . . ?
C1C Nd C2C 27.1(2) . . ?
S2A Nd C2C 75.34(15) . . ?
C1B Nd C2C 115.0(2) . . ?
C2B Nd C2C 113.9(2) . . ?
C1A Nd C2C 125.9(2) . . ?
S1A Nd C2A 56.77(14) . . ?
S1C Nd C2A 140.09(13) . . ?
S1B Nd C2A 113.76(16) . . ?
S2C Nd C2A 122.76(16) . . ?
S2B Nd C2A 76.57(13) . . ?
C1C Nd C2A 115.8(2) . . ?
S2A Nd C2A 35.51(16) . . ?
C1B Nd C2A 129.27(19) . . ?
C2B Nd C2A 112.00(19) . . ?
C1A Nd C2A 26.6(2) . . ?
C2C Nd C2A 110.7(2) . . ?
S1A Na1 S1A 180.0 2_556 . ?
S1A Na1 S2A 72.17(5) . . ?
S1A Na1 S2A 107.83(5) . 2_556 ?
S1A Na1 S2A 107.83(5) 2_556 . ?
S1A Na1 S2A 72.17(5) . . ?
S2A Na1 S2A 180.000(1) 2_556 . ?
S1B Na2 S1B 180.0 2_656 . ?
S1B Na2 S2B 109.60(5) 2_656 . ?
S1B Na2 S2B 70.40(5) . . ?
S1B Na2 S2B 70.40(5) . . ?
S1B Na2 S2B 109.60(5) . 2_656 ?
S2B Na2 S2B 180.00(7) . 2_656 ?
S1B Na2 S4A 85.80(5) 2_656 . ?
S1B Na2 S4A 94.20(5) . . ?
S2B Na2 S4A 89.20(5) . . ?
S2B Na2 S4A 90.80(5) 2_656 . ?
S1B Na2 S4A 94.19(5) . . ?
S1B Na2 S4A 85.81(5) . 2_656 ?
S2B Na2 S4A 90.81(5) . 2_656 ?
S2B Na2 S4A 89.19(5) . . ?
S4A Na2 S4A 180.0 . 2_656 ?
S1C Na3 S1C 180.0 2_666 . ?
S1C Na3 S2C 69.63(5) . . ?
S1C Na3 S2C 110.37(5) . 2_666 ?
S1C Na3 S2C 110.37(5) 2_666 . ?
S1C Na3 S2C 69.63(5) . . ?
S2C Na3 S2C 180.0 2_666 . ?
S1C Na3 S4B 97.22(5) 2_666 . ?
S1C Na3 S4B 82.78(5) . . ?
S2C Na3 S4B 88.32(5) 2_666 . ?
S2C Na3 S4B 91.68(5) . . ?
S1C Na3 S4B 82.78(5) . . ?
S1C Na3 S4B 97.22(5) . 2_666 ?
S2C Na3 S4B 91.68(5) . . ?
S2C Na3 S4B 88.32(5) . 2_666 ?
S4B Na3 S4B 180.0 . 2_666 ?
N1 Na4 N2 169.2(4) . . ?
N1 Na4 O6 87.2(2) . . ?
N2 Na4 O6 93.5(4) . . ?
N1 Na4 O3 100.3(3) . . ?
N2 Na4 O3 79.8(4) . . ?
O6 Na4 O3 171.7(3) . . ?
N1 Na4 O2 92.0(2) . . ?
N2 Na4 O2 97.6(4) . . ?
O6 Na4 O2 113.6(3) . . ?
O3 Na4 O2 63.0(3) . . ?
N1 Na4 O4 86.8(2) . . ?
N2 Na4 O4 83.6(3) . . ?
O6 Na4 O4 121.5(3) . . ?
O3 Na4 O4 62.9(3) . . ?
O2 Na4 O4 124.7(3) . . ?
N1 Na4 O5 89.5(2) . . ?
N2 Na4 O5 81.5(3) . . ?
O6 Na4 O5 60.7(2) . . ?
O3 Na4 O5 122.3(3) . . ?
O2 Na4 O5 174.0(3) . . ?
O4 Na4 O5 61.1(3) . . ?
N1 Na4 O1 114.7(3) . . ?
N2 Na4 O1 74.4(4) . . ?
O6 Na4 O1 57.3(3) . . ?
O3 Na4 O1 115.7(3) . . ?
O2 Na4 O1 63.6(3) . . ?
O4 Na4 O1 157.6(3) . . ?
O5 Na4 O1 110.6(3) . . ?
N3 Na5 N3 180.0 2_665 . ?
N3 Na5 O9 95.5(2) 2_665 . ?
N3 Na5 O9 84.5(2) . . ?
N3 Na5 O9 84.5(2) 2_665 2_665 ?
N3 Na5 O9 95.5(2) . 2_665 ?
O9 Na5 O9 180.0 . 2_665 ?
N3 Na5 O7 92.40(19) 2_665 . ?
N3 Na5 O7 87.60(19) . . ?
O9 Na5 O7 118.41(16) . . ?
O9 Na5 O7 61.59(16) 2_665 . ?
N3 Na5 O7 87.60(19) 2_665 2_665 ?
N3 Na5 O7 92.40(19) . 2_665 ?
O9 Na5 O7 61.59(16) . 2_665 ?
O9 Na5 O7 118.41(16) 2_665 2_665 ?
O7 Na5 O7 180.0 . 2_665 ?
N3 Na5 O8 86.0(2) 2_665 . ?
N3 Na5 O8 94.0(2) . . ?
O9 Na5 O8 59.77(16) . . ?
O9 Na5 O8 120.23(16) 2_665 . ?
O7 Na5 O8 60.06(15) . . ?
O7 Na5 O8 119.94(15) 2_665 . ?
N3 Na5 O8 94.0(2) 2_665 2_665 ?
N3 Na5 O8 86.0(2) . 2_665 ?
O9 Na5 O8 120.23(16) . 2_665 ?
O9 Na5 O8 59.77(16) 2_665 2_665 ?
O7 Na5 O8 119.94(15) . 2_665 ?
O7 Na5 O8 60.06(15) 2_665 2_665 ?
O8 Na5 O8 180.0 . 2_665 ?
C1A S1A Na1 92.8(2) . . ?
C1A S1A Nd 75.2(2) . . ?
Na1 S1A Nd 101.55(6) . . ?
C2A S2A Na1 90.4(2) . . ?
C2A S2A Nd 74.2(2) . . ?
Na1 S2A Nd 98.70(6) . . ?
C2A S3A C3A 104.7(4) . . ?
C1A S4A C4A 103.8(3) . . ?
C1A S4A Na2 103.9(2) . . ?
C4A S4A Na2 99.6(2) . . ?
C2A C1A S1A 123.1(5) . . ?
C2A C1A S4A 126.3(5) . . ?
S1A C1A S4A 110.5(4) . . ?
C2A C1A Nd 77.4(4) . . ?
S1A C1A Nd 69.1(2) . . ?
S4A C1A Nd 124.7(3) . . ?
C1A C2A S2A 124.9(5) . . ?
C1A C2A S3A 126.8(6) . . ?
S2A C2A S3A 108.2(4) . . ?
C1A C2A Nd 76.0(4) . . ?
S2A C2A Nd 70.3(2) . . ?
S3A C2A Nd 127.3(3) . . ?
C4A C3A S3A 112.5(5) . . ?
C3A C4A S4A 113.9(5) . . ?
C1B S1B Na2 100.5(2) . . ?
C1B S1B Nd 73.6(2) . . ?
Na2 S1B Nd 96.81(5) . . ?
C2B S2B Nd 73.4(2) . . ?
C2B S2B Na2 98.5(3) . . ?
Nd S2B Na2 93.98(5) . . ?
C2B S3B C3B 107.3(4) . . ?
C1B S4B C4B 102.1(4) . . ?
C1B S4B Na3 105.9(2) . . ?
C4B S4B Na3 101.2(3) . . ?
C2B C1B S1B 124.2(5) . . ?
C2B C1B S4B 123.8(6) . . ?
S1B C1B S4B 112.0(4) . . ?
C2B C1B Nd 76.9(4) . . ?
S1B C1B Nd 70.6(2) . . ?
S4B C1B Nd 124.1(3) . . ?
C1B C2B S2B 123.7(6) . . ?
C1B C2B S3B 127.2(5) . . ?
S2B C2B S3B 109.0(4) . . ?
C1B C2B Nd 75.8(4) . . ?
S2B C2B Nd 71.2(2) . . ?
S3B C2B Nd 123.4(3) . . ?
C4B C3B S3B 113.8(6) . . ?
C3B C4B S4B 111.9(6) . . ?
C1C S1C Nd 73.5(2) . . ?
C1C S1C Na3 97.3(3) . . ?
Nd S1C Na3 99.05(6) . . ?
C2C S2C Nd 74.2(3) . . ?
C2C S2C Na3 95.5(3) . . ?
Nd S2C Na3 97.50(6) . . ?
C2C S3C C3C 106.8(5) . . ?
C1C S4C C4C 103.2(5) . . ?
C2C C1C S1C 124.4(6) . . ?
C2C C1C S4C 124.0(6) . . ?
S1C C1C S4C 111.6(4) . . ?
C2C C1C Nd 78.6(4) . . ?
S1C C1C Nd 70.7(2) . . ?
S4C C1C Nd 121.2(3) . . ?
C1C C2C S2C 123.9(6) . . ?
C1C C2C S3C 127.1(6) . . ?
S2C C2C S3C 108.9(4) . . ?
C1C C2C Nd 74.3(4) . . ?
S2C C2C Nd 70.4(2) . . ?
S3C C2C Nd 126.2(3) . . ?
C4C C3C S3C 118.7(11) . . ?
C3C C4C S4C 124.3(11) . . ?
C12 O1 C1 116.9(12) . . ?
C12 O1 Na4 107.2(7) . . ?
C1 O1 Na4 109.5(7) . . ?
C3 O2 C2 115.9(10) . . ?
C3 O2 Na4 116.0(8) . . ?
C2 O2 Na4 114.6(6) . . ?
C5 O3 C4 117.4(10) . . ?
C5 O3 Na4 117.1(8) . . ?
C4 O3 Na4 112.9(6) . . ?
C7 O4 C6 115.1(9) . . ?
C7 O4 Na4 117.9(7) . . ?
C6 O4 Na4 111.9(6) . . ?
C9 O5 C8 116.9(9) . . ?
C9 O5 Na4 106.5(7) . . ?
C8 O5 Na4 108.8(5) . . ?
C11 O6 C10 110.9(9) . . ?
C11 O6 Na4 125.0(7) . . ?
C10 O6 Na4 120.6(6) . . ?
C28 O7 C23 109.9(6) 2_665 . ?
C28 O7 Na5 112.2(5) 2_665 . ?
C23 O7 Na5 115.3(5) . . ?
C24 O8 C25 111.3(6) . . ?
C24 O8 Na5 116.3(4) . . ?
C25 O8 Na5 117.6(4) . . ?
C27 O9 C26 110.9(6) . . ?
C27 O9 Na5 116.2(5) . . ?
C26 O9 Na5 117.4(4) . . ?
O1 C1 C2 111.1(11) . . ?
C1 C2 O2 106.5(9) . . ?
O2 C3 C4 114.2(13) . . ?
C3 C4 O3 111.6(9) . . ?
O3 C5 C6 115.7(13) . . ?
C5 C6 O4 109.8(8) . . ?
O4 C7 C8 108.2(11) . . ?
C7 C8 O5 111.4(9) . . ?
O5 C9 C10 111.2(10) . . ?
C9 C10 O6 106.7(9) . . ?
O6 C11 C12 108.3(9) . . ?
O1 C12 C11 110.8(11) . . ?
C13 N1 C17 116.0(7) . . ?
C13 N1 Na4 120.5(5) . . ?
C17 N1 Na4 123.4(5) . . ?
N1 C13 C14 122.9(8) . . ?
C15 C14 C13 119.9(9) . . ?
C16 C15 C14 119.4(8) . . ?
C15 C16 C17 117.2(8) . . ?
N1 C17 C16 124.6(8) . . ?
C22 N2 C18 114.4(15) 2_567 . ?
C18 N2 C19 102.2(12) . 2_567 ?
C21 C18 N2 111(3) . . ?
N2 C18 C19 123.4(16) . . ?
N2 C18 C22 116.8(13) . . ?
C22 C19 C21 121(4) . . ?
C21 C19 C20 110(2) . 2_567 ?
C18 C19 C20 120.1(17) . 2_567 ?
C21 C19 N2 116(2) . 2_567 ?
C22 C19 C20 110(3) . . ?
N2 C20 C21 107(3) . . ?
N2 C20 C19 121(3) . 2_567 ?
C21 C20 C19 115.2(17) . 2_567 ?
N2 C20 C21 126(2) . 2_567 ?
C18 C20 C21 114.0(15) . 2_567 ?
N2 C20 C19 113(2) . . ?
C22 C20 C19 114.6(16) 2_567 . ?
C18 C21 C19 125(3) . . ?
C22 C21 C20 119.7(17) . . ?
N2 C21 C20 102.7(12) . 2_567 ?
C19 C22 C20 103(3) . 2_567 ?
N2 C22 C21 126.9(16) 2_567 . ?
N2 C22 C18 128.5(13) 2_567 . ?
O7 C23 C24 108.8(7) . . ?
O8 C24 C23 108.7(7) . . ?
O8 C25 C26 106.5(6) . . ?
O9 C26 C25 108.6(7) . . ?
O9 C27 C28 109.8(8) . . ?
O7 C28 C27 109.5(7) 2_665 . ?
C29 N3 C33 116.8(7) . . ?
C29 N3 Na5 128.9(6) . . ?
C33 N3 Na5 114.1(5) . . ?
N3 C29 C30 123.1(8) . . ?
C29 C30 C31 119.2(8) . . ?
C32 C31 C30 118.0(8) . . ?
C33 C32 C31 118.6(8) . . ?
N3 C33 C32 124.3(8) . . ?
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
Nd S1A 2.8292(18) . ?
Nd S1C 2.8347(19) . ?
Nd S1B 2.8469(19) . ?
Nd S2C 2.8710(19) . ?
Nd S2B 2.8748(18) . ?
Nd S2A 2.8819(19) . ?
Nd C1C 2.881(7) . ?
Nd C1B 2.897(7) . ?
Nd C2B 2.910(7) . ?
Nd C1A 2.928(7) . ?
Nd C2C 2.933(7) . ?
Nd C2A 2.946(7) . ?
Na1 S1A 2.7968(19) . ?
Na1 S1A 2.7968(19) 2_556 ?
Na1 S2A 2.8629(18) 2_556 ?
Na1 S2A 2.8629(18) . ?
Na2 S1B 2.8469(18) . ?
Na2 S1B 2.8469(18) 2_656 ?
Na2 S2B 2.9480(19) . ?
Na2 S2B 2.9480(19) 2_656 ?
Na2 S4A 3.0675(19) . ?
Na2 S4A 3.0675(19) 2_656 ?
Na3 S1C 2.9126(19) . ?
Na3 S1C 2.9126(19) 2_666 ?
Na3 S2C 2.9439(19) 2_666 ?
Na3 S2C 2.9439(19) . ?
Na3 S4B 3.090(2) 2_666 ?
Na3 S4B 3.090(2) . ?
Na4 N1 2.442(7) . ?
Na4 N2 2.562(14) . ?
Na4 O6 2.608(7) . ?
Na4 O3 2.648(8) . ?
Na4 O2 2.669(8) . ?
Na4 O4 2.705(8) . ?
Na4 O5 2.793(7) . ?
Na4 O1 2.825(9) . ?
Na5 N3 2.448(6) 2_665 ?
Na5 N3 2.448(6) . ?
Na5 O9 2.734(5) . ?
Na5 O9 2.734(6) 2_665 ?
Na5 O7 2.774(5) . ?
Na5 O7 2.774(5) 2_665 ?
Na5 O8 2.778(5) . ?
Na5 O8 2.778(5) 2_665 ?
S1A C1A 1.765(7) . ?
S2A C2A 1.778(8) . ?
S3A C2A 1.780(7) . ?
S3A C3A 1.802(8) . ?
S4A C1A 1.772(7) . ?
S4A C4A 1.794(7) . ?
C1A C2A 1.351(10) . ?
C3A C4A 1.514(11) . ?
S1B C1B 1.766(8) . ?
S2B C2B 1.761(7) . ?
S3B C2B 1.763(7) . ?
S3B C3B 1.783(9) . ?
S4B C1B 1.781(7) . ?
S4B C4B 1.800(8) . ?
C1B C2B 1.372(10) . ?
C3B C4B 1.527(12) . ?
S1C C1C 1.756(8) . ?
S2C C2C 1.769(8) . ?
S3C C2C 1.773(8) . ?
S3C C3C 1.817(12) . ?
S4C C1C 1.784(7) . ?
S4C C4C 1.785(14) . ?
C1C C2C 1.362(11) . ?
C3C C4C 1.309(17) . ?
O1 C12 1.314(13) . ?
O1 C1 1.457(15) . ?
O2 C3 1.256(13) . ?
O2 C2 1.534(13) . ?
O3 C5 1.272(14) . ?
O3 C4 1.506(13) . ?
O4 C7 1.297(14) . ?
O4 C6 1.543(12) . ?
O5 C9 1.353(13) . ?
O5 C8 1.462(12) . ?
O6 C11 1.379(12) . ?
O6 C10 1.467(12) . ?
O7 C28 1.416(10) 2_665 ?
O7 C23 1.438(9) . ?
O8 C24 1.428(10) . ?
O8 C25 1.450(9) . ?
O9 C27 1.411(10) . ?
O9 C26 1.423(9) . ?
C1 C2 1.469(16) . ?
C3 C4 1.443(16) . ?
C5 C6 1.431(17) . ?
C7 C8 1.466(17) . ?
C9 C10 1.443(15) . ?
C11 C12 1.436(17) . ?
N1 C13 1.329(10) . ?
N1 C17 1.346(10) . ?
C13 C14 1.378(12) . ?
C14 C15 1.365(13) . ?
C15 C16 1.361(12) . ?
C16 C17 1.392(11) . ?
N2 C20 0.732(19) . ?
N2 C22 1.33(2) 2_567 ?
N2 C18 1.35(2) . ?
N2 C21 1.74(2) . ?
N2 C19 1.92(3) 2_567 ?
C18 C20 1.31(2) . ?
C18 C19 1.38(3) . ?
C19 C20 1.43(3) 2_567 ?
C20 C21 1.38(3) . ?
C20 C19 1.43(3) 2_567 ?
C21 C22 1.36(3) . ?
C22 N2 1.33(2) 2_567 ?
C23 C24 1.471(11) . ?
C25 C26 1.507(11) . ?
C27 C28 1.497(12) . ?
C28 O7 1.416(10) 2_665 ?
N3 C29 1.312(10) . ?
N3 C33 1.345(10) . ?
C29 C30 1.375(12) . ?
C30 C31 1.388(12) . ?
C31 C32 1.368(11) . ?
C32 C33 1.357(11) . ?
