#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:40:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179122 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308487.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_4308487
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
;
Homoleptic Tris(dithiolene) and Tetrakis(dithiolene) Complexes of
Uranium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              594
_journal_page_last               600
_journal_paper_doi               10.1021/ic049054q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C90 H126 N6 Na4 O18 S24 U2'
_chemical_formula_weight         2917.67
_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                101.530(4)
_cell_angle_beta                 104.101(5)
_cell_angle_gamma                102.537(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4359(5)
_cell_length_b                   16.2555(8)
_cell_length_c                   18.9962(10)
_cell_measurement_reflns_used    20231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.78
_cell_volume                     2940.2(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 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.1039
_diffrn_reflns_av_sigmaI/netI    0.1536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20231
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.537
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10294
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0675
_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)+(0.0578P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                6525
_reflns_number_total             10294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049054qsi20040716_091518_1.cif
_cod_data_source_block           3
_cod_database_code               4308487
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
U U 0.75361(4) 0.66387(3) 0.71196(2) 0.03014(14) Uani 1 1 d . . .
Na1 Na 0.5000 0.5000 0.5000 0.0391(15) Uani 1 2 d S . .
Na2 Na 0.6650(5) 0.7520(3) 0.1487(2) 0.0461(12) Uani 1 1 d . . .
Na3 Na 0.5000 1.0000 0.5000 0.0514(18) Uani 1 2 d S . .
S1A S 0.5496(3) 0.50582(18) 0.65696(14) 0.0327(6) Uani 1 1 d . . .
S2A S 0.5757(3) 0.67366(18) 0.58158(15) 0.0331(6) Uani 1 1 d . . .
S3A S 0.3781(3) 0.7332(2) 0.64784(16) 0.0399(7) Uani 1 1 d . . .
S4A S 0.3775(3) 0.5701(2) 0.74160(15) 0.0393(7) Uani 1 1 d . . .
C1A C 0.4634(10) 0.5851(7) 0.6732(5) 0.033(3) Uani 1 1 d . . .
C2A C 0.4699(11) 0.6534(7) 0.6399(6) 0.034(3) Uani 1 1 d . . .
C3A C 0.2543(12) 0.6903(8) 0.6916(7) 0.046(3) Uani 1 1 d . . .
H3A1 H 0.2065 0.7336 0.7041 0.055 Uiso 1 1 calc R . .
H3A2 H 0.1867 0.6389 0.6560 0.055 Uiso 1 1 calc R . .
C4A C 0.3178(13) 0.6659(9) 0.7627(6) 0.049(3) Uani 1 1 d . . .
H4A1 H 0.2500 0.6548 0.7892 0.059 Uiso 1 1 calc R . .
H4A2 H 0.3945 0.7146 0.7956 0.059 Uiso 1 1 calc R . .
S1B S 0.7798(3) 0.62984(19) 0.84938(16) 0.0400(7) Uani 1 1 d . . .
S2B S 0.7024(3) 0.8013(2) 0.79878(16) 0.0478(8) Uani 1 1 d . . .
S3B S 0.9807(4) 0.9078(2) 0.87002(18) 0.0588(10) Uani 1 1 d . . .
S4B S 1.0684(3) 0.7268(2) 0.91510(17) 0.0513(8) Uani 1 1 d . . .
C1B C 0.9005(11) 0.7289(8) 0.8673(6) 0.040(3) Uani 1 1 d . . .
C2B C 0.8696(12) 0.8007(7) 0.8500(6) 0.038(3) Uani 1 1 d . . .
C3B C 1.1385(13) 0.9056(9) 0.9325(7) 0.061(4) Uani 1 1 d . . .
H3B1 H 1.2108 0.9567 0.9363 0.073 Uiso 1 1 calc R . .
H3B2 H 1.1279 0.9090 0.9823 0.073 Uiso 1 1 calc R . .
C4B C 1.1808(13) 0.8255(10) 0.9075(8) 0.066(4) Uani 1 1 d . . .
H4B1 H 1.2742 0.8332 0.9377 0.079 Uiso 1 1 calc R . .
H4B2 H 1.1806 0.8183 0.8555 0.079 Uiso 1 1 calc R . .
S1C S 0.9304(3) 0.56985(19) 0.69061(15) 0.0353(7) Uani 1 1 d . . .
S2C S 0.9659(3) 0.78129(19) 0.69298(15) 0.0377(7) Uani 1 1 d . . .
S3C S 0.8971(3) 0.7293(2) 0.52724(16) 0.0443(8) Uani 1 1 d . . .
S4C S 0.8216(3) 0.51871(19) 0.52672(15) 0.0380(7) Uani 1 1 d . . .
C1C C 0.8956(10) 0.6081(7) 0.6099(6) 0.029(2) Uani 1 1 d . . .
C2C C 0.9201(11) 0.6944(7) 0.6114(6) 0.036(3) Uani 1 1 d . . .
C3C C 0.9530(12) 0.6484(8) 0.4718(6) 0.042(3) Uani 1 1 d . . .
H3C1 H 0.9655 0.6660 0.4275 0.051 Uiso 1 1 calc R . .
H3C2 H 1.0410 0.6452 0.5012 0.051 Uiso 1 1 calc R . .
C4C C 0.8506(12) 0.5598(8) 0.4479(6) 0.045(3) Uani 1 1 d . . .
H4C1 H 0.8832 0.5187 0.4171 0.054 Uiso 1 1 calc R . .
H4C2 H 0.7638 0.5629 0.4170 0.054 Uiso 1 1 calc R . .
O1 O 0.4250(10) 0.6283(6) 0.0666(4) 0.067(3) Uani 1 1 d DU . .
O2 O 0.5907(12) 0.7338(8) 0.0080(7) 0.106(4) Uani 1 1 d DU . .
O3 O 0.8257(10) 0.8601(6) 0.0885(5) 0.064(3) Uani 1 1 d . . .
O4 O 0.9357(10) 0.8420(7) 0.2306(6) 0.070(3) Uani 1 1 d . . .
O5 O 0.7434(10) 0.7854(7) 0.3021(5) 0.072(3) Uani 1 1 d U . .
O6 O 0.5021(11) 0.6689(7) 0.2159(6) 0.077(3) Uani 1 1 d U . .
O7 O 0.7322(18) 0.9887(12) 0.4545(10) 0.158(6) Uani 1 1 d U . .
O8 O 0.5372(12) 1.0574(7) 0.3825(6) 0.085(3) Uani 1 1 d DU . .
O9 O 0.2945(12) 1.0363(7) 0.4113(6) 0.084(3) Uani 1 1 d DU . .
N1 N 0.5587(11) 0.8740(7) 0.1538(6) 0.051(3) Uani 1 1 d . . .
N2 N 0.7822(10) 0.6361(6) 0.1247(5) 0.044(2) Uani 1 1 d . . .
N3 N 0.3727(10) 0.8464(6) 0.4213(5) 0.042(2) Uani 1 1 d . . .
C1 C 0.4192(16) 0.5994(8) -0.0088(6) 0.075(4) Uani 1 1 d DU . .
H1A H 0.3243 0.5703 -0.0384 0.090 Uiso 1 1 calc R . .
H1B H 0.4711 0.5568 -0.0132 0.090 Uiso 1 1 calc R . .
C2 C 0.4745(14) 0.6710(8) -0.0408(7) 0.065(4) Uani 1 1 d DU . .
H2A H 0.4961 0.6456 -0.0856 0.078 Uiso 1 1 calc R . .
H2B H 0.4034 0.6992 -0.0559 0.078 Uiso 1 1 calc R . .
C3 C 0.6295(18) 0.8083(11) -0.0189(8) 0.087(5) Uani 1 1 d U . .
H3A H 0.5918 0.8542 0.0010 0.105 Uiso 1 1 calc R . .
H3B H 0.5965 0.7930 -0.0735 0.105 Uiso 1 1 calc R . .
C4 C 0.7781(15) 0.8367(9) 0.0073(7) 0.063(4) Uani 1 1 d U . .
H4A H 0.8142 0.7901 -0.0127 0.075 Uiso 1 1 calc R . .
H4B H 0.8112 0.8868 -0.0105 0.075 Uiso 1 1 calc R . .
C5 C 0.9639(16) 0.8711(10) 0.1175(9) 0.074(4) Uani 1 1 d U . .
H5A H 1.0148 0.9113 0.0959 0.089 Uiso 1 1 calc R . .
H5B H 0.9840 0.8155 0.1047 0.089 Uiso 1 1 calc R . .
C6 C 1.0060(14) 0.9053(9) 0.1984(8) 0.062(4) Uani 1 1 d . . .
H6A H 0.9831 0.9600 0.2115 0.074 Uiso 1 1 calc R . .
H6B H 1.1047 0.9165 0.2186 0.074 Uiso 1 1 calc R . .
C7 C 0.9562(16) 0.8757(11) 0.3064(9) 0.077(5) Uani 1 1 d U . .
H7A H 0.9190 0.9254 0.3137 0.092 Uiso 1 1 calc R . .
H7B H 1.0541 0.8957 0.3328 0.092 Uiso 1 1 calc R . .
C8 C 0.8871(15) 0.8072(11) 0.3381(9) 0.078(5) Uani 1 1 d U . .
H8A H 0.9200 0.7559 0.3286 0.094 Uiso 1 1 calc R . .
H8B H 0.9070 0.8295 0.3921 0.094 Uiso 1 1 calc R . .
C9 C 0.6643(15) 0.7282(11) 0.3328(8) 0.075(4) Uani 1 1 d U . .
H9A H 0.6795 0.7553 0.3856 0.090 Uiso 1 1 calc R . .
H9B H 0.6913 0.6744 0.3289 0.090 Uiso 1 1 calc R . .
C10 C 0.5207(13) 0.7095(10) 0.2915(6) 0.058(4) Uani 1 1 d . . .
H10A H 0.4642 0.6712 0.3122 0.070 Uiso 1 1 calc R . .
H10B H 0.4936 0.7633 0.2954 0.070 Uiso 1 1 calc R . .
C11 C 0.3896(14) 0.6050(10) 0.1777(8) 0.069(4) Uani 1 1 d U . .
H11A H 0.3112 0.6261 0.1823 0.082 Uiso 1 1 calc R . .
H11B H 0.3886 0.5578 0.2019 0.082 Uiso 1 1 calc R . .
C12 C 0.3689(17) 0.5687(9) 0.0986(8) 0.073(5) Uani 1 1 d . . .
H12A H 0.4095 0.5204 0.0927 0.087 Uiso 1 1 calc R . .
H12B H 0.2710 0.5458 0.0728 0.087 Uiso 1 1 calc R . .
C13 C 0.4231(15) 0.8484(10) 0.1334(8) 0.063(4) Uani 1 1 d . . .
H13 H 0.3812 0.7900 0.1285 0.075 Uiso 1 1 calc R . .
C14 C 0.3379(16) 0.9019(11) 0.1186(8) 0.070(4) Uani 1 1 d . . .
H14 H 0.2427 0.8794 0.1040 0.084 Uiso 1 1 calc R . .
C15 C 0.3961(16) 0.9865(11) 0.1258(8) 0.063(4) Uani 1 1 d . . .
H15 H 0.3419 1.0242 0.1174 0.075 Uiso 1 1 calc R . .
C16 C 0.5366(17) 1.0164(9) 0.1458(7) 0.059(4) Uani 1 1 d . . .
H16 H 0.5794 1.0745 0.1501 0.071 Uiso 1 1 calc R . .
C17 C 0.6144(14) 0.9588(10) 0.1597(8) 0.060(4) Uani 1 1 d . . .
H17 H 0.7097 0.9800 0.1737 0.072 Uiso 1 1 calc R . .
C18 C 0.8027(12) 0.5917(8) 0.1772(6) 0.045(3) Uani 1 1 d . . .
H18 H 0.7516 0.5952 0.2109 0.054 Uiso 1 1 calc R . .
C19 C 0.8926(12) 0.5420(8) 0.1848(7) 0.052(3) Uani 1 1 d . . .
H19 H 0.9033 0.5129 0.2224 0.063 Uiso 1 1 calc R . .
C20 C 0.9684(13) 0.5370(8) 0.1326(8) 0.059(4) Uani 1 1 d . . .
H20 H 1.0305 0.5036 0.1349 0.071 Uiso 1 1 calc R . .
C21 C 0.9503(13) 0.5802(8) 0.0803(7) 0.053(3) Uani 1 1 d . . .
H21 H 1.0005 0.5770 0.0460 0.064 Uiso 1 1 calc R . .
C22 C 0.8573(13) 0.6302(9) 0.0759(7) 0.054(3) Uani 1 1 d . . .
H22 H 0.8465 0.6600 0.0388 0.065 Uiso 1 1 calc R . .
C23 C 0.773(2) 1.0572(16) 0.4205(12) 0.136(8) Uani 1 1 d U . .
H23A H 0.8519 1.0524 0.4036 0.163 Uiso 1 1 calc R . .
H23B H 0.7942 1.1143 0.4553 0.163 Uiso 1 1 calc R . .
C24 C 0.651(2) 1.0425(14) 0.3570(11) 0.116(7) Uani 1 1 d U . .
H24A H 0.6721 1.0816 0.3263 0.139 Uiso 1 1 calc R . .
H24B H 0.6262 0.9829 0.3261 0.139 Uiso 1 1 calc R . .
C25 C 0.4197(15) 1.0444(13) 0.3220(8) 0.107(6) Uani 1 1 d DU . .
H25A H 0.3803 0.9827 0.2965 0.128 Uiso 1 1 calc R . .
H25B H 0.4429 1.0753 0.2861 0.128 Uiso 1 1 calc R . .
C26 C 0.3207(16) 1.0795(10) 0.3552(8) 0.082(5) Uani 1 1 d DU . .
H26A H 0.3588 1.1420 0.3779 0.099 Uiso 1 1 calc R . .
H26B H 0.2354 1.0698 0.3160 0.099 Uiso 1 1 calc R . .
C27 C 0.221(2) 1.0764(16) 0.4516(13) 0.134(8) Uani 1 1 d U . .
H27A H 0.1482 1.0907 0.4180 0.161 Uiso 1 1 calc R . .
H27B H 0.2811 1.1299 0.4880 0.161 Uiso 1 1 calc R . .
C28 C 0.162(3) 1.0141(17) 0.4906(14) 0.153(9) Uani 1 1 d U . .
H28A H 0.0947 1.0342 0.5116 0.183 Uiso 1 1 calc R . .
H28B H 0.1174 0.9566 0.4559 0.183 Uiso 1 1 calc R . .
C29 C 0.3768(13) 0.7817(8) 0.4560(7) 0.052(3) Uani 1 1 d . . .
H29 H 0.4370 0.7945 0.5043 0.062 Uiso 1 1 calc R . .
C30 C 0.2941(12) 0.6964(8) 0.4218(6) 0.044(3) Uani 1 1 d . . .
H30 H 0.3003 0.6534 0.4472 0.053 Uiso 1 1 calc R . .
C31 C 0.2067(12) 0.6760(8) 0.3534(7) 0.048(3) Uani 1 1 d . . .
H31 H 0.1520 0.6189 0.3304 0.058 Uiso 1 1 calc R . .
C32 C 0.1978(14) 0.7407(9) 0.3164(7) 0.061(4) Uani 1 1 d . . .
H32 H 0.1372 0.7281 0.2683 0.073 Uiso 1 1 calc R . .
C33 C 0.2819(14) 0.8256(8) 0.3533(7) 0.054(3) Uani 1 1 d . . .
H33 H 0.2742 0.8695 0.3292 0.065 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'
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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'
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
S1C U S2B 148.17(9) . . ?
S1C U S1B 88.38(9) . . ?
S2B U S1B 74.71(9) . . ?
S1C U S2C 76.56(9) . . ?
S2B U S2C 88.26(10) . . ?
S1B U S2C 119.21(9) . . ?
S1C U S2A 115.09(8) . . ?
S2B U S2A 92.58(9) . . ?
S1B U S2A 146.37(9) . . ?
S2C U S2A 90.71(8) . . ?
S1C U S1A 86.34(9) . . ?
S2B U S1A 117.99(10) . . ?
S1B U S1A 85.03(8) . . ?
S2C U S1A 149.29(8) . . ?
S2A U S1A 73.54(8) . . ?
S1C U C1B 90.6(3) . . ?
S2B U C1B 59.8(3) . . ?
S1B U C1B 36.1(2) . . ?
S2C U C1B 84.8(2) . . ?
S2A U C1B 152.1(3) . . ?
S1A U C1B 121.1(2) . . ?
S1C U C1C 36.8(2) . . ?
S2B U C1C 147.2(2) . . ?
S1B U C1C 125.2(2) . . ?
S2C U C1C 59.7(2) . . ?
S2A U C1C 81.8(2) . . ?
S1A U C1C 91.5(2) . . ?
C1B U C1C 118.5(3) . . ?
S1C U C1A 122.3(2) . . ?
S2B U C1A 84.6(2) . . ?
S1B U C1A 88.3(2) . . ?
S2C U C1A 148.6(2) . . ?
S2A U C1A 59.2(2) . . ?
S1A U C1A 36.0(2) . . ?
C1B U C1A 117.0(3) . . ?
C1C U C1A 118.5(3) . . ?
S1C U C2B 111.2(2) . . ?
S2B U C2B 37.0(2) . . ?
S1B U C2B 58.2(2) . . ?
S2C U C2B 73.3(2) . . ?
S2A U C2B 125.4(2) . . ?
S1A U C2B 137.3(2) . . ?
C1B U C2B 27.5(3) . . ?
C1C U C2B 126.3(3) . . ?
C1A U C2B 115.2(3) . . ?
S1C U C2A 136.7(2) . . ?
S2B U C2A 75.1(2) . . ?
S1B U C2A 110.1(2) . . ?
S2C U C2A 121.1(2) . . ?
S2A U C2A 36.4(2) . . ?
S1A U C2A 58.1(2) . . ?
C1B U C2A 127.5(3) . . ?
C1C U C2A 113.9(3) . . ?
C1A U C2A 27.7(3) . . ?
C2B U C2A 111.8(3) . . ?
S1C U C2C 58.7(2) . . ?
S2B U C2C 120.2(2) . . ?
S1B U C2C 139.2(2) . . ?
S2C U C2C 36.0(2) . . ?
S2A U C2C 74.1(2) . . ?
S1A U C2C 113.3(2) . . ?
C1B U C2C 114.5(3) . . ?
C1C U C2C 27.3(3) . . ?
C1A U C2C 128.4(3) . . ?
C2B U C2C 109.0(3) . . ?
C2A U C2C 110.5(3) . . ?
S2A Na1 S2A 180.00(13) 2_666 . ?
S2A Na1 S1A 71.87(8) 2_666 2_666 ?
S2A Na1 S1A 108.13(8) . 2_666 ?
S2A Na1 S1A 108.13(8) 2_666 . ?
S2A Na1 S1A 71.87(8) . . ?
S1A Na1 S1A 179.999(1) 2_666 . ?
S2A Na1 S4C 92.85(8) 2_666 . ?
S2A Na1 S4C 87.15(8) . . ?
S1A Na1 S4C 93.01(7) 2_666 . ?
S1A Na1 S4C 86.99(7) . . ?
S2A Na1 S4C 87.15(8) 2_666 2_666 ?
S2A Na1 S4C 92.85(8) . 2_666 ?
S1A Na1 S4C 86.99(7) 2_666 2_666 ?
S1A Na1 S4C 93.01(7) . 2_666 ?
S4C Na1 S4C 179.999(1) . 2_666 ?
N1 Na2 N2 170.1(4) . . ?
N1 Na2 O2 84.1(4) . . ?
N2 Na2 O2 87.6(4) . . ?
N1 Na2 O6 93.1(4) . . ?
N2 Na2 O6 95.8(4) . . ?
O2 Na2 O6 121.7(4) . . ?
N1 Na2 O1 94.0(4) . . ?
N2 Na2 O1 86.9(3) . . ?
O2 Na2 O1 63.1(3) . . ?
O6 Na2 O1 59.0(3) . . ?
N1 Na2 O5 91.4(4) . . ?
N2 Na2 O5 96.7(3) . . ?
O2 Na2 O5 175.3(4) . . ?
O6 Na2 O5 60.0(3) . . ?
O1 Na2 O5 119.0(3) . . ?
N1 Na2 O3 79.1(3) . . ?
N2 Na2 O3 92.2(3) . . ?
O2 Na2 O3 61.1(3) . . ?
O6 Na2 O3 171.6(4) . . ?
O1 Na2 O3 124.2(3) . . ?
O5 Na2 O3 116.5(3) . . ?
N1 Na2 O4 100.4(4) . . ?
N2 Na2 O4 78.9(3) . . ?
O2 Na2 O4 118.5(4) . . ?
O6 Na2 O4 119.3(3) . . ?
O1 Na2 O4 165.6(4) . . ?
O5 Na2 O4 60.7(3) . . ?
O3 Na2 O4 59.8(3) . . ?
N3 Na3 N3 180.000(2) 2_676 . ?
N3 Na3 O9 97.9(3) 2_676 . ?
N3 Na3 O9 82.1(3) . . ?
N3 Na3 O9 82.1(3) 2_676 2_676 ?
N3 Na3 O9 97.9(3) . 2_676 ?
O9 Na3 O9 180.0(4) . 2_676 ?
N3 Na3 O8 86.2(3) 2_676 . ?
N3 Na3 O8 93.8(3) . . ?
O9 Na3 O8 60.8(4) . . ?
O9 Na3 O8 119.2(4) 2_676 . ?
N3 Na3 O8 93.8(3) 2_676 2_676 ?
N3 Na3 O8 86.2(3) . 2_676 ?
O9 Na3 O8 119.2(4) . 2_676 ?
O9 Na3 O8 60.8(4) 2_676 2_676 ?
O8 Na3 O8 179.999(3) . 2_676 ?
N3 Na3 O7 89.2(4) 2_676 . ?
N3 Na3 O7 90.8(4) . . ?
O9 Na3 O7 119.7(5) . . ?
O9 Na3 O7 60.3(5) 2_676 . ?
O8 Na3 O7 60.2(5) . . ?
O8 Na3 O7 119.8(5) 2_676 . ?
N3 Na3 O7 90.8(4) 2_676 2_676 ?
N3 Na3 O7 89.2(4) . 2_676 ?
O9 Na3 O7 60.3(5) . 2_676 ?
O9 Na3 O7 119.7(5) 2_676 2_676 ?
O8 Na3 O7 119.8(5) . 2_676 ?
O8 Na3 O7 60.2(5) 2_676 2_676 ?
O7 Na3 O7 179.998(3) . 2_676 ?
C1A S1A U 74.9(3) . . ?
C1A S1A Na1 93.3(3) . . ?
U S1A Na1 96.47(8) . . ?
C2A S2A U 75.7(3) . . ?
C2A S2A Na1 93.8(4) . . ?
U S2A Na1 99.15(9) . . ?
C2A S3A C3A 103.1(5) . . ?
C1A S4A C4A 105.8(5) . . ?
C2A C1A S1A 123.3(8) . . ?
C2A C1A S4A 125.2(9) . . ?
S1A C1A S4A 111.4(6) . . ?
C2A C1A U 77.3(6) . . ?
S1A C1A U 69.1(3) . . ?
S4A C1A U 122.8(5) . . ?
C1A C2A S2A 123.4(9) . . ?
C1A C2A S3A 126.9(8) . . ?
S2A C2A S3A 109.7(6) . . ?
C1A C2A U 75.0(6) . . ?
S2A C2A U 67.9(3) . . ?
S3A C2A U 130.7(5) . . ?
C4A C3A S3A 113.3(8) . . ?
C3A C4A S4A 111.7(8) . . ?
C1B S1B U 74.9(4) . . ?
C2B S2B U 75.7(4) . . ?
C2B S3B C3B 104.3(6) . . ?
C1B S4B C4B 103.9(6) . . ?
C2B C1B S1B 124.0(9) . . ?
C2B C1B S4B 124.1(9) . . ?
S1B C1B S4B 111.9(7) . . ?
C2B C1B U 77.9(7) . . ?
S1B C1B U 69.0(3) . . ?
S4B C1B U 129.0(5) . . ?
C1B C2B S3B 128.8(9) . . ?
C1B C2B S2B 123.9(9) . . ?
S3B C2B S2B 107.3(6) . . ?
C1B C2B U 74.6(7) . . ?
S3B C2B U 130.6(5) . . ?
S2B C2B U 67.3(3) . . ?
C4B C3B S3B 113.1(9) . . ?
C3B C4B S4B 112.9(9) . . ?
C1C S1C U 76.1(3) . . ?
C2C S2C U 77.6(4) . . ?
C2C S3C C3C 99.3(5) . . ?
C1C S4C C4C 107.5(5) . . ?
C1C S4C Na1 101.0(3) . . ?
C4C S4C Na1 101.5(4) . . ?
C2C C1C S1C 124.0(8) . . ?
C2C C1C S4C 125.3(8) . . ?
S1C C1C S4C 110.8(6) . . ?
C2C C1C U 79.7(6) . . ?
S1C C1C U 67.0(3) . . ?
S4C C1C U 124.9(5) . . ?
C1C C2C S2C 125.2(8) . . ?
C1C C2C S3C 121.7(8) . . ?
S2C C2C S3C 113.0(6) . . ?
C1C C2C U 72.9(6) . . ?
S2C C2C U 66.4(3) . . ?
S3C C2C U 134.9(5) . . ?
C4C C3C S3C 111.6(8) . . ?
C3C C4C S4C 113.3(8) . . ?
C12 O1 C1 117.5(10) . . ?
C12 O1 Na2 118.9(8) . . ?
C1 O1 Na2 112.1(8) . . ?
C2 O2 C3 113.5(12) . . ?
C2 O2 Na2 123.0(9) . . ?
C3 O2 Na2 118.3(9) . . ?
C5 O3 C4 113.6(11) . . ?
C5 O3 Na2 113.5(8) . . ?
C4 O3 Na2 112.6(8) . . ?
C7 O4 C6 111.9(12) . . ?
C7 O4 Na2 114.4(8) . . ?
C6 O4 Na2 115.9(8) . . ?
C9 O5 C8 113.2(11) . . ?
C9 O5 Na2 116.6(9) . . ?
C8 O5 Na2 115.8(8) . . ?
C11 O6 C10 119.3(11) . . ?
C11 O6 Na2 122.3(8) . . ?
C10 O6 Na2 116.5(8) . . ?
C28 O7 C23 111(2) 2_676 . ?
C28 O7 Na3 113.7(16) 2_676 . ?
C23 O7 Na3 111.2(14) . . ?
C25 O8 C24 111.8(13) . . ?
C25 O8 Na3 117.4(10) . . ?
C24 O8 Na3 117.5(10) . . ?
C27 O9 C26 110.9(13) . . ?
C27 O9 Na3 111.8(12) . . ?
C26 O9 Na3 118.9(9) . . ?
C13 N1 C17 115.2(12) . . ?
C13 N1 Na2 113.6(9) . . ?
C17 N1 Na2 129.8(9) . . ?
C18 N2 C22 116.6(11) . . ?
C18 N2 Na2 116.3(8) . . ?
C22 N2 Na2 124.6(8) . . ?
C33 N3 C29 116.8(10) . . ?
C33 N3 Na3 124.8(8) . . ?
C29 N3 Na3 117.1(8) . . ?
O1 C1 C2 113.5(10) . . ?
O2 C2 C1 114.4(11) . . ?
O2 C3 C4 105.6(13) . . ?
O3 C4 C3 110.0(11) . . ?
O3 C5 C6 109.9(12) . . ?
C5 C6 O4 109.2(12) . . ?
O4 C7 C8 110.2(14) . . ?
O5 C8 C7 107.4(12) . . ?
O5 C9 C10 108.5(12) . . ?
O6 C10 C9 108.4(11) . . ?
O6 C11 C12 118.0(12) . . ?
O1 C12 C11 112.3(12) . . ?
N1 C13 C14 125.1(15) . . ?
C15 C14 C13 118.6(15) . . ?
C14 C15 C16 118.8(14) . . ?
C15 C16 C17 119.1(13) . . ?
N1 C17 C16 123.3(13) . . ?
N2 C18 C19 125.2(11) . . ?
C18 C19 C20 116.5(11) . . ?
C21 C20 C19 119.6(13) . . ?
C20 C21 C22 121.0(13) . . ?
N2 C22 C21 121.1(12) . . ?
O7 C23 C24 102.9(19) . . ?
O8 C24 C23 111.1(18) . . ?
O8 C25 C26 106.2(13) . . ?
O9 C26 C25 109.3(13) . . ?
O9 C27 C28 107(2) . . ?
O7 C28 C27 106(2) 2_676 . ?
N3 C29 C30 122.2(11) . . ?
C31 C30 C29 120.5(11) . . ?
C30 C31 C32 119.2(12) . . ?
C31 C32 C33 118.4(11) . . ?
N3 C33 C32 123.0(12) . . ?
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
U S1C 2.692(3) . ?
U S2B 2.734(3) . ?
U S1B 2.737(3) . ?
U S2C 2.741(3) . ?
U S2A 2.766(3) . ?
U S1A 2.774(3) . ?
U C1B 2.831(10) . ?
U C1C 2.838(10) . ?
U C1A 2.865(10) . ?
U C2B 2.871(11) . ?
U C2A 2.895(11) . ?
U C2C 2.921(10) . ?
Na1 S2A 2.772(3) 2_666 ?
Na1 S2A 2.772(3) . ?
Na1 S1A 2.878(3) 2_666 ?
Na1 S1A 2.878(3) . ?
Na1 S4C 3.206(3) . ?
Na1 S4C 3.206(3) 2_666 ?
Na2 N1 2.471(11) . ?
Na2 N2 2.487(11) . ?
Na2 O2 2.531(13) . ?
Na2 O6 2.663(11) . ?
Na2 O1 2.721(10) . ?
Na2 O5 2.733(10) . ?
Na2 O3 2.769(10) . ?
Na2 O4 2.774(11) . ?
Na3 N3 2.517(9) 2_676 ?
Na3 N3 2.517(9) . ?
Na3 O9 2.640(10) . ?
Na3 O9 2.640(10) 2_676 ?
Na3 O8 2.665(10) . ?
Na3 O8 2.665(10) 2_676 ?
Na3 O7 2.793(18) . ?
Na3 O7 2.793(18) 2_676 ?
S1A C1A 1.745(11) . ?
S2A C2A 1.772(10) . ?
S3A C2A 1.777(11) . ?
S3A C3A 1.793(11) . ?
S4A C1A 1.774(10) . ?
S4A C4A 1.808(12) . ?
C1A C2A 1.381(14) . ?
C3A C4A 1.521(16) . ?
S1B C1B 1.728(12) . ?
S2B C2B 1.783(12) . ?
S3B C2B 1.779(12) . ?
S3B C3B 1.792(15) . ?
S4B C1B 1.777(12) . ?
S4B C4B 1.826(14) . ?
C1B C2B 1.356(16) . ?
C3B C4B 1.490(19) . ?
S1C C1C 1.753(10) . ?
S2C C2C 1.759(10) . ?
S3C C2C 1.781(11) . ?
S3C C3C 1.804(12) . ?
S4C C1C 1.790(10) . ?
S4C C4C 1.821(11) . ?
C1C C2C 1.364(14) . ?
C3C C4C 1.503(15) . ?
O1 C12 1.349(14) . ?
O1 C1 1.397(9) . ?
O2 C2 1.382(19) . ?
O2 C3 1.424(17) . ?
O3 C5 1.370(16) . ?
O3 C4 1.442(14) . ?
O4 C7 1.380(17) . ?
O4 C6 1.454(14) . ?
O5 C9 1.416(15) . ?
O5 C8 1.420(16) . ?
O6 C11 1.319(15) . ?
O6 C10 1.402(14) . ?
O7 C28 1.34(2) 2_676 ?
O7 C23 1.43(2) . ?
O8 C25 1.405(19) . ?
O8 C24 1.44(2) . ?
O9 C27 1.38(2) . ?
O9 C26 1.436(19) . ?
N1 C13 1.318(16) . ?
N1 C17 1.345(16) . ?
N2 C18 1.345(14) . ?
N2 C22 1.354(15) . ?
N3 C33 1.331(14) . ?
N3 C29 1.351(15) . ?
C1 C2 1.490(19) . ?
C3 C4 1.44(2) . ?
C5 C6 1.444(18) . ?
C7 C8 1.501(19) . ?
C9 C10 1.445(18) . ?
C11 C12 1.442(18) . ?
C13 C14 1.392(18) . ?
C14 C15 1.34(2) . ?
C15 C16 1.370(19) . ?
C16 C17 1.389(18) . ?
C18 C19 1.366(16) . ?
C19 C20 1.411(18) . ?
C20 C21 1.328(17) . ?
C21 C22 1.393(17) . ?
C23 C24 1.46(2) . ?
C25 C26 1.49(2) . ?
C27 C28 1.49(3) . ?
C28 O7 1.34(2) 2_676 ?
C29 C30 1.391(16) . ?
C30 C31 1.323(15) . ?
C31 C32 1.383(17) . ?
C32 C33 1.398(17) . ?
