#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316463.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_4316463
loop_
_publ_author_name
'Olivier Bénaud'
'Jean-Claude Berthet'
'Pierre Thuéry'
'Michel Ephritikhine'
_publ_section_title
;
 The Bis Metallacyclic Anion [U(N{SiMe3}2)(CH2SiMe2N{SiMe3})2]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8117
_journal_page_last               8130
_journal_paper_doi               10.1021/ic1012044
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C40.5 H80.5 N5.5 Na O6 Si6 U'
_chemical_formula_weight         1170.16
_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                 97.394(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0569(11)
_cell_length_b                   19.7051(19)
_cell_length_c                   18.6003(15)
_cell_measurement_reflns_used    185179
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.09
_cell_volume                     5836.2(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and seven ω scans with 2° steps (544 frames)'
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            185179
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         11000
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0760
_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)+(0.1425P)²+3.4315P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2364
_reflns_number_gt                6474
_reflns_number_total             11000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1012044_si_002_10.cif
_cod_data_source_block           8.0.5pyridine
_cod_original_cell_volume        5836.3(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C40.50 H80.50 N5.50 Na O6 Si6 U'
_cod_database_code               4316463
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.46779(2) 0.26150(2) 0.86016(2) 0.0716(2) Uani 1 1 d . . .
Na Na 0.7296(3) 0.3050(3) 0.6189(3) 0.1157(18) Uani 1 1 d . . .
Si1 Si 0.4438(3) 0.4090(2) 0.7588(2) 0.1179(13) Uani 1 1 d . . .
Si2 Si 0.2833(2) 0.3521(2) 0.8015(2) 0.1047(11) Uani 1 1 d . . .
Si3 Si 0.4056(3) 0.0972(2) 0.8880(2) 0.1115(12) Uani 1 1 d . . .
Si4 Si 0.4229(3) 0.1301(2) 0.7330(2) 0.1087(12) Uani 1 1 d . . .
Si5 Si 0.6738(4) 0.2388(4) 0.9382(3) 0.159(2) Uani 1 1 d . . .
Si6 Si 0.5754(3) 0.3415(3) 1.0101(2) 0.1377(18) Uani 1 1 d . . .
O1 O 0.5525(5) 0.2719(4) 0.7751(5) 0.085(2) Uani 1 1 d . . .
O2 O 0.6325(7) 0.3179(7) 0.6989(6) 0.165(5) Uani 1 1 d . . .
O3 O 0.3888(5) 0.2512(3) 0.9499(5) 0.082(2) Uani 1 1 d . . .
O4 O 0.3222(6) 0.1974(5) 1.0312(5) 0.112(3) Uani 1 1 d . . .
O5 O 0.6985(14) 0.4291(12) 0.5945(10) 0.240(8) Uani 1 1 d U . .
O6 O 0.6126(11) 0.2834(10) 0.5202(10) 0.200(6) Uani 1 1 d DU . .
N1 N 0.3911(6) 0.3493(5) 0.8054(5) 0.087(3) Uani 1 1 d . . .
N2 N 0.4296(6) 0.1535(5) 0.8248(5) 0.086(3) Uani 1 1 d . . .
N3 N 0.5824(6) 0.2828(6) 0.9435(5) 0.099(3) Uani 1 1 d . . .
N5 N 0.8471(8) 0.3484(6) 0.7079(6) 0.108(3) Uani 1 1 d . . .
C1 C 0.5622(9) 0.3910(10) 0.7804(9) 0.136(6) Uani 1 1 d . . .
H1A H 0.5933 0.4273 0.7607 0.163 Uiso 1 1 calc R . .
H1B H 0.5776 0.3905 0.8326 0.163 Uiso 1 1 calc R . .
C2 C 0.5872(9) 0.3218(10) 0.7483(8) 0.116(5) Uani 1 1 d . . .
C3 C 0.4212(9) 0.4069(9) 0.6571(8) 0.128(5) Uani 1 1 d . . .
H3A H 0.4317 0.3621 0.6401 0.192 Uiso 1 1 calc R . .
H3B H 0.4568 0.4389 0.6369 0.192 Uiso 1 1 calc R . .
H3C H 0.3634 0.4186 0.6426 0.192 Uiso 1 1 calc R . .
C4 C 0.4182(14) 0.4989(12) 0.7973(12) 0.198(9) Uani 1 1 d U . .
H4A H 0.3776 0.4940 0.8306 0.297 Uiso 1 1 calc R . .
H4B H 0.3960 0.5279 0.7581 0.297 Uiso 1 1 calc R . .
H4C H 0.4687 0.5185 0.8221 0.297 Uiso 1 1 calc R . .
C5 C 0.2251(8) 0.3904(9) 0.7172(8) 0.125(5) Uani 1 1 d . . .
H5A H 0.2408 0.4372 0.7139 0.187 Uiso 1 1 calc R . .
H5B H 0.1658 0.3873 0.7191 0.187 Uiso 1 1 calc R . .
H5C H 0.2390 0.3663 0.6755 0.187 Uiso 1 1 calc R . .
C6 C 0.2525(9) 0.4001(9) 0.8801(9) 0.130(5) Uani 1 1 d . . .
H6A H 0.2607 0.3720 0.9226 0.195 Uiso 1 1 calc R . .
H6B H 0.1944 0.4128 0.8703 0.195 Uiso 1 1 calc R . .
H6C H 0.2865 0.4401 0.8879 0.195 Uiso 1 1 calc R . .
C7 C 0.2382(10) 0.2654(8) 0.8083(10) 0.121(5) Uani 1 1 d U . .
H7A H 0.2330 0.2438 0.7616 0.182 Uiso 1 1 calc R . .
H7B H 0.1837 0.2688 0.8241 0.182 Uiso 1 1 calc R . .
H7C H 0.2745 0.2390 0.8425 0.182 Uiso 1 1 calc R . .
C8 C 0.4322(9) 0.1369(7) 0.9817(6) 0.104(4) Uani 1 1 d . . .
H8A H 0.4246 0.1036 1.0187 0.125 Uiso 1 1 calc R . .
H8B H 0.4905 0.1512 0.9885 0.125 Uiso 1 1 calc R . .
C9 C 0.3756(7) 0.1980(7) 0.9897(7) 0.094(4) Uani 1 1 d . . .
C10 C 0.2905(10) 0.0741(9) 0.8818(9) 0.142(6) Uani 1 1 d . . .
H10A H 0.2588 0.1134 0.8925 0.214 Uiso 1 1 calc R . .
H10B H 0.2833 0.0388 0.9160 0.214 Uiso 1 1 calc R . .
H10C H 0.2709 0.0585 0.8337 0.214 Uiso 1 1 calc R . .
C11 C 0.4682(11) 0.0155(9) 0.8873(9) 0.149(6) Uani 1 1 d . . .
H11A H 0.4703 0.0016 0.8382 0.224 Uiso 1 1 calc R . .
H11B H 0.4418 -0.0192 0.9126 0.224 Uiso 1 1 calc R . .
H11C H 0.5243 0.0230 0.9109 0.224 Uiso 1 1 calc R . .
C12 C 0.3412(12) 0.0633(10) 0.7039(10) 0.165(7) Uani 1 1 d U . .
H12A H 0.3472 0.0264 0.7378 0.248 Uiso 1 1 calc R . .
H12B H 0.3487 0.0469 0.6566 0.248 Uiso 1 1 calc R . .
H12C H 0.2862 0.0828 0.7025 0.248 Uiso 1 1 calc R . .
C13 C 0.5262(12) 0.1017(11) 0.7073(10) 0.163(7) Uani 1 1 d U . .
H13A H 0.5695 0.1324 0.7273 0.244 Uiso 1 1 calc R . .
H13B H 0.5235 0.1011 0.6554 0.244 Uiso 1 1 calc R . .
H13C H 0.5386 0.0569 0.7259 0.244 Uiso 1 1 calc R . .
C14 C 0.3909(10) 0.2007(8) 0.6698(7) 0.121(5) Uani 1 1 d . . .
H14A H 0.3320 0.2095 0.6693 0.182 Uiso 1 1 calc R . .
H14B H 0.4018 0.1885 0.6219 0.182 Uiso 1 1 calc R . .
H14C H 0.4223 0.2407 0.6853 0.182 Uiso 1 1 calc R . .
C15 C 0.7272(13) 0.2066(13) 1.0327(11) 0.180(8) Uani 1 1 d U . .
H15A H 0.7375 0.2444 1.0652 0.271 Uiso 1 1 calc R . .
H15B H 0.7795 0.1849 1.0270 0.271 Uiso 1 1 calc R . .
H15C H 0.6908 0.1748 1.0522 0.271 Uiso 1 1 calc R . .
C16 C 0.7524(15) 0.2846(15) 0.9004(13) 0.199(9) Uani 1 1 d U . .
H16A H 0.7532 0.2708 0.8510 0.298 Uiso 1 1 calc R . .
H16B H 0.8061 0.2757 0.9277 0.298 Uiso 1 1 calc R . .
H16C H 0.7405 0.3323 0.9018 0.298 Uiso 1 1 calc R . .
C17 C 0.6429(16) 0.1521(14) 0.8751(13) 0.222(10) Uani 1 1 d U . .
H17A H 0.6262 0.1165 0.9054 0.333 Uiso 1 1 calc R . .
H17B H 0.6909 0.1378 0.8532 0.333 Uiso 1 1 calc R . .
H17C H 0.5975 0.1625 0.8380 0.333 Uiso 1 1 calc R . .
C18 C 0.6691(13) 0.3980(13) 1.0191(12) 0.195(9) Uani 1 1 d U . .
H18A H 0.7188 0.3715 1.0326 0.293 Uiso 1 1 calc R . .
H18B H 0.6639 0.4315 1.0556 0.293 Uiso 1 1 calc R . .
H18C H 0.6728 0.4200 0.9736 0.293 Uiso 1 1 calc R . .
C19 C 0.5636(12) 0.3007(11) 1.1023(7) 0.149(7) Uani 1 1 d . . .
H19A H 0.5057 0.2897 1.1042 0.224 Uiso 1 1 calc R . .
H19B H 0.5826 0.3319 1.1405 0.224 Uiso 1 1 calc R . .
H19C H 0.5967 0.2600 1.1082 0.224 Uiso 1 1 calc R . .
C20 C 0.4806(11) 0.4017(9) 0.9834(8) 0.142(6) Uani 1 1 d . . .
H20A H 0.4829 0.4191 0.9355 0.214 Uiso 1 1 calc R . .
H20B H 0.4829 0.4387 1.0172 0.214 Uiso 1 1 calc R . .
H20C H 0.4292 0.3770 0.9843 0.214 Uiso 1 1 calc R . .
N4 N 0.7649(9) 0.1865(6) 0.6420(9) 0.182(4) Uani 1 1 d GU . .
C21 C 0.7975(9) 0.1488(8) 0.5889(7) 0.189(4) Uani 1 1 d GU . .
H21 H 0.8124 0.1703 0.5479 0.227 Uiso 1 1 calc R . .
C22 C 0.8078(9) 0.0791(8) 0.5971(8) 0.190(4) Uani 1 1 d GU . .
H22 H 0.8296 0.0539 0.5616 0.228 Uiso 1 1 calc R . .
C23 C 0.7855(9) 0.0470(6) 0.6584(9) 0.191(4) Uani 1 1 d GU . .
H23 H 0.7924 0.0004 0.6639 0.229 Uiso 1 1 calc R . .
C24 C 0.7529(9) 0.0847(8) 0.7115(7) 0.196(4) Uani 1 1 d GU . .
H24 H 0.7380 0.0632 0.7525 0.236 Uiso 1 1 calc R . .
C25 C 0.7426(8) 0.1544(8) 0.7033(7) 0.195(4) Uani 1 1 d GU . .
H25 H 0.7208 0.1796 0.7388 0.234 Uiso 1 1 calc R . .
C26 C 0.8395(11) 0.3928(9) 0.7579(9) 0.139(6) Uani 1 1 d . . .
H26 H 0.7853 0.4076 0.7618 0.167 Uiso 1 1 calc R . .
C27 C 0.9020(14) 0.4205(10) 0.8053(8) 0.145(6) Uani 1 1 d . . .
H27 H 0.8931 0.4537 0.8390 0.174 Uiso 1 1 calc R . .
C28 C 0.9764(16) 0.3951(13) 0.7983(13) 0.170(8) Uani 1 1 d U . .
H28 H 1.0222 0.4114 0.8292 0.204 Uiso 1 1 calc R . .
C29 C 0.9911(14) 0.3478(14) 0.7500(14) 0.185(9) Uani 1 1 d . . .
H29 H 1.0441 0.3302 0.7463 0.222 Uiso 1 1 calc R . .
C30 C 0.9186(11) 0.3275(10) 0.7057(9) 0.127(5) Uani 1 1 d . . .
H30 H 0.9252 0.2948 0.6709 0.152 Uiso 1 1 calc R . .
C31 C 0.618(2) 0.462(2) 0.593(2) 0.289(16) Uani 1 1 d U . .
H31A H 0.6050 0.4649 0.6421 0.347 Uiso 1 1 calc R . .
H31B H 0.5762 0.4329 0.5661 0.347 Uiso 1 1 calc R . .
C32 C 0.6087(17) 0.5300(15) 0.5608(16) 0.220(10) Uani 1 1 d DU . .
H32A H 0.5999 0.5637 0.5971 0.264 Uiso 1 1 calc R . .
H32B H 0.5621 0.5316 0.5221 0.264 Uiso 1 1 calc R . .
C33 C 0.6911(19) 0.5412(18) 0.5320(19) 0.298(16) Uani 1 1 d DU . .
H33A H 0.7155 0.5843 0.5489 0.358 Uiso 1 1 calc R . .
H33B H 0.6831 0.5412 0.4795 0.358 Uiso 1 1 calc R . .
C34 C 0.7481(19) 0.4826(18) 0.5608(18) 0.255(13) Uani 1 1 d DU . .
H34A H 0.7740 0.4628 0.5214 0.306 Uiso 1 1 calc R . .
H34B H 0.7924 0.4995 0.5967 0.306 Uiso 1 1 calc R . .
C35 C 0.608(2) 0.3174(17) 0.4505(14) 0.258(13) Uani 1 1 d DU . .
H35A H 0.6527 0.3029 0.4241 0.309 Uiso 1 1 calc R . .
H35B H 0.6104 0.3663 0.4566 0.309 Uiso 1 1 calc R . .
C36 C 0.522(2) 0.296(2) 0.411(2) 0.36(2) Uani 1 1 d DU . .
H36A H 0.5287 0.2703 0.3675 0.437 Uiso 1 1 calc R . .
H36B H 0.4870 0.3350 0.3977 0.437 Uiso 1 1 calc R . .
C37 C 0.483(2) 0.2510(14) 0.4661(15) 0.227(14) Uani 1 1 d DU . .
H37A H 0.4261 0.2649 0.4705 0.272 Uiso 1 1 calc R . .
H37B H 0.4831 0.2035 0.4522 0.272 Uiso 1 1 calc R . .
C38 C 0.5413(13) 0.2635(11) 0.5363(14) 0.176(10) Uani 1 1 d D . .
H38A H 0.5174 0.2978 0.5650 0.211 Uiso 1 1 calc R . .
H38B H 0.5481 0.2220 0.5645 0.211 Uiso 1 1 calc R . .
C39 C 0.547(3) 0.0548(19) 0.5072(11) 0.170(9) Uani 1 1 d . . .
C40 C 0.467(3) 0.066(3) 0.5113(15) 0.219(16) Uani 1 1 d . . .
C41 C 0.420(2) 0.007(3) 0.5036(13) 0.204(16) Uani 1 1 d . . .
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'
Si Si 0.0817 0.0704 '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'
Na Na 0.0362 0.0249 '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
O1 U O3 177.0(3) . . ?
O1 U N1 87.5(3) . . ?
O3 U N1 94.4(3) . . ?
O1 U N3 87.3(3) . . ?
O3 U N3 89.7(3) . . ?
N1 U N3 120.2(4) . . ?
O1 U N2 92.7(3) . . ?
O3 U N2 88.5(3) . . ?
N1 U N2 117.9(3) . . ?
N3 U N2 121.9(4) . . ?
O2 Na O4 173.7(5) . 4_665 ?
O2 Na N4 98.9(5) . . ?
O4 Na N4 87.1(5) 4_665 . ?
O2 Na O6 89.2(6) . . ?
O4 Na O6 88.2(5) 4_665 . ?
N4 Na O6 95.9(6) . . ?
O2 Na N5 92.9(4) . . ?
O4 Na N5 88.6(4) 4_665 . ?
N4 Na N5 94.2(5) . . ?
O6 Na N5 169.3(6) . . ?
O2 Na O5 82.8(6) . . ?
O4 Na O5 91.3(5) 4_665 . ?
N4 Na O5 177.9(7) . . ?
O6 Na O5 85.4(7) . . ?
N5 Na O5 84.4(6) . . ?
N1 Si1 C3 116.2(6) . . ?
N1 Si1 C1 107.6(6) . . ?
C3 Si1 C1 105.3(7) . . ?
N1 Si1 C4 106.7(7) . . ?
C3 Si1 C4 111.2(9) . . ?
C1 Si1 C4 109.6(9) . . ?
N1 Si2 C6 110.5(7) . . ?
N1 Si2 C7 111.4(6) . . ?
C6 Si2 C7 105.4(8) . . ?
N1 Si2 C5 116.0(6) . . ?
C6 Si2 C5 107.3(7) . . ?
C7 Si2 C5 105.6(8) . . ?
N2 Si3 C10 114.9(7) . . ?
N2 Si3 C11 112.4(6) . . ?
C10 Si3 C11 108.1(8) . . ?
N2 Si3 C8 108.7(6) . . ?
C10 Si3 C8 104.8(7) . . ?
C11 Si3 C8 107.3(7) . . ?
N2 Si4 C14 113.4(6) . . ?
N2 Si4 C13 112.4(7) . . ?
C14 Si4 C13 104.2(8) . . ?
N2 Si4 C12 114.5(7) . . ?
C14 Si4 C12 102.4(8) . . ?
C13 Si4 C12 108.9(9) . . ?
N3 Si5 C16 115.0(10) . . ?
N3 Si5 C15 113.0(8) . . ?
C16 Si5 C15 105.6(11) . . ?
N3 Si5 C17 107.6(8) . . ?
C16 Si5 C17 108.8(12) . . ?
C15 Si5 C17 106.4(11) . . ?
N3 Si6 C18 110.0(8) . . ?
N3 Si6 C19 112.8(7) . . ?
C18 Si6 C19 109.9(9) . . ?
N3 Si6 C20 110.5(6) . . ?
C18 Si6 C20 104.8(10) . . ?
C19 Si6 C20 108.6(8) . . ?
C2 O1 U 133.9(9) . . ?
C2 O2 Na 172.4(12) . . ?
C9 O3 U 129.9(7) . . ?
C9 O4 Na 174.9(9) . 4_566 ?
C31 O5 C34 101(3) . . ?
C31 O5 Na 127(2) . . ?
C34 O5 Na 130.6(17) . . ?
C38 O6 C35 114(2) . . ?
C38 O6 Na 119.5(16) . . ?
C35 O6 Na 122.0(18) . . ?
Si2 N1 Si1 120.5(6) . . ?
Si2 N1 U 121.5(5) . . ?
Si1 N1 U 117.6(5) . . ?
Si3 N2 Si4 120.6(6) . . ?
Si3 N2 U 119.1(5) . . ?
Si4 N2 U 120.3(5) . . ?
Si6 N3 Si5 121.3(6) . . ?
Si6 N3 U 119.6(6) . . ?
Si5 N3 U 119.1(6) . . ?
C30 N5 C26 115.2(16) . . ?
C30 N5 Na 119.7(11) . . ?
C26 N5 Na 125.1(12) . . ?
C2 C1 Si1 112.1(11) . . ?
C2 C1 H1A 109.2 . . ?
Si1 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
Si1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O2 C2 O1 125.0(17) . . ?
O2 C2 C1 122.6(16) . . ?
O1 C2 C1 112.3(11) . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 Si3 110.3(9) . . ?
C9 C8 H8A 109.6 . . ?
Si3 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
Si3 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
O4 C9 O3 122.6(12) . . ?
O4 C9 C8 121.8(12) . . ?
O3 C9 C8 115.6(10) . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si4 C14 H14A 109.5 . . ?
Si4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si5 C15 H15A 109.5 . . ?
Si5 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si5 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si5 C16 H16A 109.5 . . ?
Si5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si5 C17 H17A 109.5 . . ?
Si5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si6 C18 H18A 109.5 . . ?
Si6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si6 C19 H19A 109.5 . . ?
Si6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si6 C20 H20A 109.5 . . ?
Si6 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si6 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C21 N4 C25 120.0 . . ?
C21 N4 Na 119.3(8) . . ?
C25 N4 Na 120.2(8) . . ?
C22 C21 N4 120.0 . . ?
C22 C21 H21 120.0 . . ?
N4 C21 H21 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 N4 120.0 . . ?
C24 C25 H25 120.0 . . ?
N4 C25 H25 120.0 . . ?
N5 C26 C27 127.4(17) . . ?
N5 C26 H26 116.3 . . ?
C27 C26 H26 116.3 . . ?
C28 C27 C26 112.6(19) . . ?
C28 C27 H27 123.7 . . ?
C26 C27 H27 123.7 . . ?
C27 C28 C29 125(2) . . ?
C27 C28 H28 117.5 . . ?
C29 C28 H28 117.5 . . ?
C28 C29 C30 113(2) . . ?
C28 C29 H29 123.5 . . ?
C30 C29 H29 123.5 . . ?
N5 C30 C29 126.8(19) . . ?
N5 C30 H30 116.6 . . ?
C29 C30 H30 116.6 . . ?
O5 C31 C32 118(3) . . ?
O5 C31 H31A 107.8 . . ?
C32 C31 H31A 107.8 . . ?
O5 C31 H31B 107.8 . . ?
C32 C31 H31B 107.8 . . ?
H31A C31 H31B 107.2 . . ?
C31 C32 C33 103(3) . . ?
C31 C32 H32A 111.1 . . ?
C33 C32 H32A 111.1 . . ?
C31 C32 H32B 111.1 . . ?
C33 C32 H32B 111.1 . . ?
H32A C32 H32B 109.1 . . ?
C32 C33 C34 106(2) . . ?
C32 C33 H33A 110.5 . . ?
C34 C33 H33A 110.5 . . ?
C32 C33 H33B 110.5 . . ?
C34 C33 H33B 110.5 . . ?
H33A C33 H33B 108.7 . . ?
O5 C34 C33 111(2) . . ?
O5 C34 H34A 109.5 . . ?
C33 C34 H34A 109.5 . . ?
O5 C34 H34B 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
O6 C35 C36 104(2) . . ?
O6 C35 H35A 110.9 . . ?
C36 C35 H35A 110.9 . . ?
O6 C35 H35B 110.9 . . ?
C36 C35 H35B 110.9 . . ?
H35A C35 H35B 109.0 . . ?
C35 C36 C37 105(3) . . ?
C35 C36 H36A 110.8 . . ?
C37 C36 H36A 110.8 . . ?
C35 C36 H36B 110.8 . . ?
C37 C36 H36B 110.8 . . ?
H36A C36 H36B 108.9 . . ?
C38 C37 C36 103(2) . . ?
C38 C37 H37A 111.2 . . ?
C36 C37 H37A 111.2 . . ?
C38 C37 H37B 111.2 . . ?
C36 C37 H37B 111.2 . . ?
H37A C37 H37B 109.1 . . ?
O6 C38 C37 108(2) . . ?
O6 C38 H38A 110.0 . . ?
C37 C38 H38A 110.0 . . ?
O6 C38 H38B 110.0 . . ?
C37 C38 H38B 110.0 . . ?
H38A C38 H38B 108.4 . . ?
C40 C39 C41 125(3) . 3_656 ?
C39 C40 C41 111(4) . . ?
C39 C41 C40 124(4) 3_656 . ?
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 O1 2.224(8) . ?
U O3 2.232(7) . ?
U N1 2.287(9) . ?
U N3 2.287(9) . ?
U N2 2.287(9) . ?
Na O2 2.302(10) . ?
Na O4 2.346(9) 4_665 ?
Na N4 2.429(13) . ?
Na O6 2.488(19) . ?
Na N5 2.495(13) . ?
Na O5 2.52(2) . ?
Si1 N1 1.742(10) . ?
Si1 C3 1.880(16) . ?
Si1 C1 1.925(17) . ?
Si1 C4 1.97(2) . ?
Si2 N1 1.723(10) . ?
Si2 C6 1.860(15) . ?
Si2 C7 1.868(15) . ?
Si2 C5 1.876(15) . ?
Si3 N2 1.697(10) . ?
Si3 C10 1.893(15) . ?
Si3 C11 1.898(17) . ?
Si3 C8 1.908(13) . ?
Si4 N2 1.759(10) . ?
Si4 C14 1.851(15) . ?
Si4 C13 1.870(17) . ?
Si4 C12 1.887(19) . ?
Si5 N3 1.718(13) . ?
Si5 C16 1.77(2) . ?
Si5 C15 1.96(2) . ?
Si5 C17 2.10(3) . ?
Si6 N3 1.708(12) . ?
Si6 C18 1.86(2) . ?
Si6 C19 1.925(15) . ?
Si6 C20 1.944(19) . ?
O1 C2 1.264(17) . ?
O2 C2 1.245(15) . ?
O3 C9 1.316(15) . ?
O4 C9 1.225(12) . ?
O4 Na 2.346(9) 4_566 ?
O5 C31 1.44(3) . ?
O5 C34 1.50(3) . ?
O6 C38 1.28(2) . ?
O6 C35 1.45(3) . ?
N5 C30 1.224(17) . ?
N5 C26 1.294(17) . ?
C1 C2 1.56(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.527(17) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
N4 C21 1.3900 . ?
N4 C25 1.3900 . ?
C21 C22 1.3900 . ?
C21 H21 0.9300 . ?
C22 C23 1.3900 . ?
C22 H22 0.9300 . ?
C23 C24 1.3900 . ?
C23 H23 0.9300 . ?
C24 C25 1.3900 . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 C27 1.36(2) . ?
C26 H26 0.9300 . ?
C27 C28 1.32(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.34(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.40(3) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C32 1.46(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.51(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.53(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.54(5) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.55(5) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.53(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.31(4) . ?
C39 C41 1.35(4) 3_656 ?
C40 C41 1.39(5) . ?
C41 C39 1.35(4) 3_656 ?
