#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:22:52 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179018 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/16/4121633.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_4121633
loop_
_publ_author_name
'King, David M.'
'McMaster, Jonathan'
'Tuna, Floriana'
'McInnes, Eric J. L.'
'Lewis, William'
'Blake, Alexander J.'
'Liddle, Stephen T.'
_publ_section_title
;
 Synthesis and Characterization of an f-Block Terminal Parent Imido
 [U═NH] Complex: A Masked Uranium(IV) Nitride.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5619
_journal_paper_doi               10.1021/ja502405e
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C66 H152 N10 Na2 Si6 U2'
_chemical_formula_sum            'C66 H152 N10 Na2 Si6 U2'
_chemical_formula_weight         1776.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0952(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9841(2)
_cell_length_b                   13.84682(15)
_cell_length_c                   20.9585(2)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3110
_cell_measurement_theta_min      3.2630
_cell_volume                     4217.59(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0134869000
_diffrn_orient_matrix_UB_12      -0.1050750000
_diffrn_orient_matrix_UB_13      -0.0247460000
_diffrn_orient_matrix_UB_21      -0.0818853000
_diffrn_orient_matrix_UB_22      -0.0109404000
_diffrn_orient_matrix_UB_23      0.0318540000
_diffrn_orient_matrix_UB_31      -0.0658847000
_diffrn_orient_matrix_UB_32      0.0350609000
_diffrn_orient_matrix_UB_33      -0.0641446000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17321
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.446
_diffrn_reflns_theta_min         3.279
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    11.943
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.2224
_exptl_crystal_size_mid          0.1453
_exptl_crystal_size_min          0.0376
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8259
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0245P)²+0.6731P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0483
_refine_ls_wR_factor_ref         0.0500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7523
_reflns_number_total             8259
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja502405e_si_002.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 4121632--4121637.cif.'
_cod_original_cell_volume        4217.60(9)
_cod_database_code               4121633
#BEGIN Tags that were not found in dictionaries:
_nottingham_internal_coll_name   UDKIOW
_nottingham_internal_coll_number 12730
_nottingham_internal_coll_client DK/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time 1+4
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   DMK
_nottingham_internal_coll_date   16/08/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user DMK
_nottingham_internal_process_date 28/08/2013
_nottingham_internal_solution_user DMK
_nottingham_internal_solution_date 28/08/2013
_nottingham_internal_refinement_user DMK
_nottingham_internal_refinement_date 28/08/2013
_nottingham_internal_self_validation_user DMK
_nottingham_internal_self_validation_date 14/02/2014
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C66 H152 N10 Si6 Na2 U2'
_chemical_oxdiff_usercomment
'UDKIOW #12730 IN FOMBLIN FILM ON MICROMOUNT FOR DMK/STL'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Restrained distances
 N5-H5
 0.98 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),
 C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
U1 U 0.87978(2) 0.90945(2) 0.11912(2) 0.01621(3) Uani 1 1 d .
Si1 Si 0.86804(5) 0.64432(5) 0.09931(4) 0.01970(15) Uani 1 1 d .
Si2 Si 0.70876(5) 1.07273(6) 0.00833(4) 0.02430(16) Uani 1 1 d .
Si3 Si 1.03427(5) 1.01910(6) 0.26674(4) 0.02229(15) Uani 1 1 d .
Na1 Na 0.94335(9) 0.93192(10) -0.05089(6) 0.0325(3) Uani 1 1 d .
N1 N 0.86362(16) 0.74824(16) 0.14334(11) 0.0194(5) Uani 1 1 d .
N2 N 0.74100(16) 0.97547(17) 0.05993(11) 0.0205(5) Uani 1 1 d .
N3 N 0.92696(17) 0.99514(18) 0.21666(12) 0.0233(5) Uani 1 1 d .
N4 N 0.75291(16) 0.88974(18) 0.18901(11) 0.0196(5) Uani 1 1 d .
N5 N 0.98083(17) 0.92309(19) 0.06518(12) 0.0237(5) Uani 1 1 d D
H5 H 1.0328(18) 0.879(2) 0.0709(19) 0.036 Uiso 1 1 d DR
C1 C 0.8766(2) 0.6806(2) 0.01330(14) 0.0253(6) Uani 1 1 d .
H1 H 0.9349 0.7184 0.0192 0.030 Uiso 1 1 calc R
C2 C 0.8865(3) 0.5926(3) -0.02949(17) 0.0394(8) Uani 1 1 d .
H2A H 0.9362 0.5509 -0.0053 0.059 Uiso 1 1 calc GR
H2B H 0.9010 0.6147 -0.0702 0.059 Uiso 1 1 calc GR
H2C H 0.8287 0.5563 -0.0402 0.059 Uiso 1 1 calc GR
C3 C 0.7997(2) 0.7455(2) -0.02605(14) 0.0315(7) Uani 1 1 d .
H3A H 0.7421 0.7087 -0.0381 0.047 Uiso 1 1 calc GR
H3B H 0.8162 0.7679 -0.0660 0.047 Uiso 1 1 calc GR
H3C H 0.7917 0.8012 0.0008 0.047 Uiso 1 1 calc GR
C4 C 0.7625(2) 0.5660(2) 0.09898(15) 0.0286(7) Uani 1 1 d .
H4 H 0.7552 0.5683 0.1451 0.034 Uiso 1 1 calc R
C5 C 0.7726(3) 0.4585(2) 0.08430(19) 0.0400(8) Uani 1 1 d .
H5A H 0.7858 0.4516 0.0410 0.060 Uiso 1 1 calc GR
H5B H 0.7152 0.4247 0.0846 0.060 Uiso 1 1 calc GR
H5C H 0.8232 0.4307 0.1180 0.060 Uiso 1 1 calc GR
C6 C 0.6727(2) 0.6054(3) 0.05662(17) 0.0344(7) Uani 1 1 d .
H6A H 0.6670 0.6739 0.0666 0.052 Uiso 1 1 calc GR
H6B H 0.6209 0.5695 0.0659 0.052 Uiso 1 1 calc GR
H6C H 0.6724 0.5981 0.0101 0.052 Uiso 1 1 calc GR
C7 C 0.9736(2) 0.5669(2) 0.13427(16) 0.0298(7) Uani 1 1 d .
H7 H 0.9651 0.5042 0.1099 0.036 Uiso 1 1 calc R
C8 C 1.0614(2) 0.6134(3) 0.12423(18) 0.0376(8) Uani 1 1 d .
H8A H 1.0591 0.6156 0.0771 0.056 Uiso 1 1 calc GR
H8B H 1.1147 0.5753 0.1471 0.056 Uiso 1 1 calc GR
H8C H 1.0667 0.6792 0.1420 0.056 Uiso 1 1 calc GR
C9 C 0.9852(3) 0.5441(3) 0.20782(18) 0.0428(9) Uani 1 1 d .
H9A H 0.9948 0.6043 0.2331 0.064 Uiso 1 1 calc GR
H9B H 1.0385 0.5017 0.2231 0.064 Uiso 1 1 calc GR
H9C H 0.9297 0.5119 0.2140 0.064 Uiso 1 1 calc GR
C10 C 0.8395(2) 0.7381(2) 0.20736(13) 0.0217(6) Uani 1 1 d .
H10A H 0.8877 0.7684 0.2424 0.026 Uiso 1 1 calc R
H10B H 0.8361 0.6687 0.2181 0.026 Uiso 1 1 calc R
C11 C 0.7474(2) 0.7860(2) 0.20455(13) 0.0221(6) Uani 1 1 d .
H11A H 0.6987 0.7546 0.1704 0.027 Uiso 1 1 calc R
H11B H 0.7314 0.7786 0.2474 0.027 Uiso 1 1 calc R
C12 C 0.6668(2) 1.0367(3) -0.08181(16) 0.0321(7) Uani 1 1 d .
H12 H 0.6462 1.0969 -0.1076 0.039 Uiso 1 1 calc R
C13 C 0.5848(2) 0.9676(3) -0.09404(16) 0.0393(8) Uani 1 1 d .
H13A H 0.6036 0.9068 -0.0708 0.059 Uiso 1 1 calc GR
H13B H 0.5634 0.9551 -0.1413 0.059 Uiso 1 1 calc GR
H13C H 0.5350 0.9968 -0.0778 0.059 Uiso 1 1 calc GR
C14 C 0.7429(2) 0.9912(3) -0.10925(18) 0.0408(9) Uani 1 1 d .
H14A H 0.7911 1.0392 -0.1090 0.061 Uiso 1 1 calc GR
H14B H 0.7170 0.9693 -0.1544 0.061 Uiso 1 1 calc GR
H14C H 0.7695 0.9360 -0.0819 0.061 Uiso 1 1 calc GR
C15 C 0.8146(2) 1.1494(3) 0.0135(2) 0.0391(8) Uani 1 1 d .
H15 H 0.8619 1.1055 0.0027 0.047 Uiso 1 1 calc R
C16 C 0.8008(3) 1.2313(3) -0.0375(2) 0.0564(11) Uani 1 1 d .
H16A H 0.7725 1.2053 -0.0812 0.085 Uiso 1 1 calc GR
H16B H 0.8605 1.2600 -0.0376 0.085 Uiso 1 1 calc GR
H16C H 0.7606 1.2808 -0.0260 0.085 Uiso 1 1 calc GR
C17 C 0.8581(3) 1.1911(3) 0.0816(2) 0.0544(12) Uani 1 1 d .
H17A H 0.8131 1.2318 0.0959 0.082 Uiso 1 1 calc GR
H17B H 0.9120 1.2300 0.0795 0.082 Uiso 1 1 calc GR
H17C H 0.8771 1.1382 0.1131 0.082 Uiso 1 1 calc GR
C18 C 0.6094(2) 1.1410(2) 0.02973(17) 0.0299(7) Uani 1 1 d .
H18 H 0.5628 1.0904 0.0322 0.036 Uiso 1 1 calc R
C19 C 0.6308(3) 1.1909(3) 0.0970(2) 0.0465(9) Uani 1 1 d .
H19A H 0.6727 1.1504 0.1293 0.070 Uiso 1 1 calc GR
H19B H 0.5735 1.2005 0.1109 0.070 Uiso 1 1 calc GR
H19C H 0.6597 1.2536 0.0939 0.070 Uiso 1 1 calc GR
C20 C 0.5588(3) 1.2126(3) -0.0226(2) 0.0437(9) Uani 1 1 d .
H20A H 0.6001 1.2659 -0.0265 0.066 Uiso 1 1 calc GR
H20B H 0.5047 1.2381 -0.0098 0.066 Uiso 1 1 calc GR
H20C H 0.5392 1.1795 -0.0651 0.066 Uiso 1 1 calc GR
C21 C 0.66611(19) 0.9160(2) 0.07527(14) 0.0205(5) Uani 1 1 d .
H21A H 0.6753 0.8474 0.0653 0.025 Uiso 1 1 calc R
H21B H 0.6061 0.9370 0.0473 0.025 Uiso 1 1 calc R
C22 C 0.6650(2) 0.9260(2) 0.14722(14) 0.0230(6) Uani 1 1 d .
H22A H 0.6566 0.9947 0.1576 0.028 Uiso 1 1 calc R
H22B H 0.6130 0.8887 0.1561 0.028 Uiso 1 1 calc R
C23 C 1.1197(2) 0.9335(3) 0.24252(17) 0.0317(7) Uani 1 1 d .
H23 H 1.1148 0.9459 0.1948 0.038 Uiso 1 1 calc R
C24 C 1.1007(3) 0.8262(3) 0.2477(3) 0.0565(12) Uani 1 1 d .
H24A H 1.1084 0.8087 0.2941 0.085 Uiso 1 1 calc GR
H24B H 1.1439 0.7888 0.2292 0.085 Uiso 1 1 calc GR
H24C H 1.0375 0.8119 0.2234 0.085 Uiso 1 1 calc GR
C25 C 1.2202(2) 0.9542(3) 0.27746(18) 0.0384(8) Uani 1 1 d .
H25A H 1.2335 1.0228 0.2728 0.058 Uiso 1 1 calc GR
H25B H 1.2608 0.9150 0.2577 0.058 Uiso 1 1 calc GR
H25C H 1.2306 0.9381 0.3242 0.058 Uiso 1 1 calc GR
C26 C 1.0761(2) 1.1470(2) 0.25557(15) 0.0283(6) Uani 1 1 d .
H26 H 1.1356 1.1561 0.2892 0.034 Uiso 1 1 calc R
C27 C 1.0958(3) 1.1637(3) 0.18815(17) 0.0387(8) Uani 1 1 d .
H27A H 1.1466 1.1219 0.1834 0.058 Uiso 1 1 calc GR
H27B H 1.1128 1.2314 0.1843 0.058 Uiso 1 1 calc GR
H27C H 1.0407 1.1485 0.1536 0.058 Uiso 1 1 calc GR
C28 C 1.0094(3) 1.2244(2) 0.26846(17) 0.0370(8) Uani 1 1 d .
H28A H 0.9505 1.2185 0.2358 0.055 Uiso 1 1 calc GR
H28B H 1.0355 1.2886 0.2651 0.055 Uiso 1 1 calc GR
H28C H 0.9997 1.2157 0.3127 0.055 Uiso 1 1 calc GR
C29 C 1.0328(2) 1.0114(3) 0.35714(15) 0.0307(7) Uani 1 1 d .
H29 H 0.9800 1.0525 0.3620 0.037 Uiso 1 1 calc R
C30 C 1.0141(3) 0.9110(3) 0.3807(2) 0.0529(12) Uani 1 1 d .
H30A H 0.9629 0.8814 0.3484 0.079 Uiso 1 1 calc GR
H30B H 0.9980 0.9162 0.4232 0.079 Uiso 1 1 calc GR
H30C H 1.0692 0.8709 0.3856 0.079 Uiso 1 1 calc GR
C31 C 1.1175(3) 1.0534(3) 0.40439(16) 0.0442(9) Uani 1 1 d .
H31A H 1.1714 1.0139 0.4034 0.066 Uiso 1 1 calc GR
H31B H 1.1081 1.0538 0.4491 0.066 Uiso 1 1 calc GR
H31C H 1.1275 1.1196 0.3911 0.066 Uiso 1 1 calc GR
C32 C 0.8449(2) 1.0315(2) 0.23694(16) 0.0288(7) Uani 1 1 d .
H32A H 0.8085 1.0735 0.2019 0.035 Uiso 1 1 calc R
H32B H 0.8649 1.0707 0.2774 0.035 Uiso 1 1 calc R
C33 C 0.7854(2) 0.9488(2) 0.24965(14) 0.0272(6) Uani 1 1 d .
H33A H 0.8212 0.9077 0.2855 0.033 Uiso 1 1 calc R
H33B H 0.7318 0.9748 0.2638 0.033 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 '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
N1 U1 N2 111.54(8) . .
N1 U1 N3 109.00(8) . .
N1 U1 N4 69.88(8) . .
N2 U1 N4 70.83(8) . .
N3 U1 N2 108.00(9) . .
N3 U1 N4 71.04(8) . .
N5 U1 N1 109.35(9) . .
N5 U1 N2 110.10(9) . .
N5 U1 N3 108.80(9) . .
N5 U1 N4 179.02(9) . .
N1 Si1 C1 107.91(12) . .
N1 Si1 C4 109.62(13) . .
N1 Si1 C7 113.68(13) . .
C1 Si1 C4 113.05(14) . .
C7 Si1 C1 105.76(14) . .
C7 Si1 C4 106.88(15) . .
N2 Si2 C12 113.11(14) . .
N2 Si2 C15 107.49(14) . .
N2 Si2 C18 110.85(13) . .
C12 Si2 C18 105.96(15) . .
C15 Si2 C12 105.84(16) . .
C15 Si2 C18 113.60(16) . .
N3 Si3 C23 107.81(13) . .
N3 Si3 C26 112.88(14) . .
N3 Si3 C29 111.12(14) . .
C23 Si3 C26 106.41(15) . .
C23 Si3 C29 113.73(15) . .
C29 Si3 C26 104.90(14) . .
U1 Na1 H5 105.7(8) 3_775 .
N5 Na1 U1 112.80(7) . 3_775
N5 Na1 U1 25.76(6) 3_775 3_775
N5 Na1 N5 99.99(9) 3_775 .
N5 Na1 H5 21.0(4) . .
N5 Na1 H5 101.9(9) 3_775 .
Si1 N1 U1 132.02(12) . .
C10 N1 U1 110.65(17) . .
C10 N1 Si1 117.20(18) . .
Si2 N2 U1 135.90(13) . .
C21 N2 U1 106.84(17) . .
C21 N2 Si2 117.22(19) . .
Si3 N3 U1 132.33(13) . .
C32 N3 U1 109.28(18) . .
C32 N3 Si3 118.4(2) . .
C11 N4 U1 107.69(16) . .
C11 N4 C22 111.8(2) . .
C11 N4 C33 111.7(2) . .
C22 N4 U1 106.80(16) . .
C22 N4 C33 112.1(2) . .
C33 N4 U1 106.39(16) . .
U1 N5 Na1 122.36(12) . .
U1 N5 Na1 125.10(12) . 3_775
U1 N5 H5 123(2) . .
Na1 N5 Na1 80.01(9) 3_775 .
Na1 N5 H5 98(2) . .
Na1 N5 H5 99(2) 3_775 .
Si1 C1 H1 106.2 . .
C2 C1 Si1 112.4(2) . .
C2 C1 H1 106.2 . .
C3 C1 Si1 116.6(2) . .
C3 C1 H1 106.2 . .
C3 C1 C2 108.4(3) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3B 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si1 C4 H4 105.3 . .
C5 C4 Si1 115.4(2) . .
C5 C4 H4 105.3 . .
C6 C4 Si1 114.3(2) . .
C6 C4 H4 105.3 . .
C6 C4 C5 110.3(3) . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5B 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.5 . .
C4 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
Si1 C7 H7 107.6 . .
C8 C7 Si1 111.9(2) . .
C8 C7 H7 107.6 . .
C8 C7 C9 109.5(3) . .
C9 C7 Si1 112.4(2) . .
C9 C7 H7 107.6 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N1 C10 H10A 109.6 . .
N1 C10 H10B 109.6 . .
N1 C10 C11 110.1(2) . .
H10A C10 H10B 108.2 . .
C11 C10 H10A 109.6 . .
C11 C10 H10B 109.6 . .
N4 C11 C10 109.5(2) . .
N4 C11 H11A 109.8 . .
N4 C11 H11B 109.8 . .
C10 C11 H11A 109.8 . .
C10 C11 H11B 109.8 . .
H11A C11 H11B 108.2 . .
Si2 C12 H12 107.5 . .
C13 C12 Si2 112.8(2) . .
C13 C12 H12 107.5 . .
C13 C12 C14 108.7(3) . .
C14 C12 Si2 112.5(2) . .
C14 C12 H12 107.5 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13B 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Si2 C15 H15 106.0 . .
C16 C15 Si2 113.9(3) . .
C16 C15 H15 106.0 . .
C17 C15 Si2 115.2(3) . .
C17 C15 H15 106.0 . .
C17 C15 C16 109.0(3) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16B 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17B 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
Si2 C18 H18 105.1 . .
C19 C18 Si2 116.1(2) . .
C19 C18 H18 105.1 . .
C19 C18 C20 108.8(3) . .
C20 C18 Si2 115.5(2) . .
C20 C18 H18 105.1 . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19B 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C18 C20 H20A 109.5 . .
C18 C20 H20B 109.5 . .
C18 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
N2 C21 H21A 109.5 . .
N2 C21 H21B 109.5 . .
N2 C21 C22 110.8(2) . .
H21A C21 H21B 108.1 . .
C22 C21 H21A 109.5 . .
C22 C21 H21B 109.5 . .
N4 C22 C21 109.5(2) . .
N4 C22 H22A 109.8 . .
N4 C22 H22B 109.8 . .
C21 C22 H22A 109.8 . .
C21 C22 H22B 109.8 . .
H22A C22 H22B 108.2 . .
Si3 C23 H23 105.7 . .
C24 C23 Si3 116.1(3) . .
C24 C23 H23 105.7 . .
C24 C23 C25 109.1(3) . .
C25 C23 Si3 113.7(2) . .
C25 C23 H23 105.7 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24B 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C23 C25 H25A 109.5 . .
C23 C25 H25B 109.5 . .
C23 C25 H25C 109.5 . .
H25A C25 H25B 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
Si3 C26 H26 107.1 . .
C27 C26 Si3 113.3(2) . .
C27 C26 H26 107.1 . .
C27 C26 C28 109.7(3) . .
C28 C26 Si3 112.2(2) . .
C28 C26 H26 107.1 . .
Na1 C27 H27A 68.2 3_775 .
Na1 C27 H27B 109.1 3_775 .
C26 C27 Na1 139.4(2) . 3_775
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27B 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
H28A C28 H28B 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
Si3 C29 H29 105.8 . .
C30 C29 Si3 114.9(3) . .
C30 C29 H29 105.8 . .
C31 C29 Si3 114.6(2) . .
C31 C29 H29 105.8 . .
C31 C29 C30 109.2(3) . .
C29 C30 H30A 109.5 . .
C29 C30 H30B 109.5 . .
C29 C30 H30C 109.5 . .
H30A C30 H30B 109.5 . .
H30A C30 H30C 109.5 . .
H30B C30 H30C 109.5 . .
C29 C31 H31A 109.5 . .
C29 C31 H31B 109.5 . .
C29 C31 H31C 109.5 . .
H31A C31 H31B 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N3 C32 H32A 109.4 . .
N3 C32 H32B 109.4 . .
N3 C32 C33 111.0(3) . .
H32A C32 H32B 108.0 . .
C33 C32 H32A 109.4 . .
C33 C32 H32B 109.4 . .
N4 C33 C32 110.4(2) . .
N4 C33 H33A 109.6 . .
N4 C33 H33B 109.6 . .
C32 C33 H33A 109.6 . .
C32 C33 H33B 109.6 . .
H33A C33 H33B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N1 2.315(2) .
U1 N2 2.333(2) .
U1 N3 2.320(2) .
U1 N4 2.681(2) .
U1 N5 2.107(2) .
Si1 N1 1.719(2) .
Si1 C1 1.905(3) .
Si1 C4 1.916(3) .
Si1 C7 1.903(3) .
Si2 N2 1.721(2) .
Si2 C12 1.906(4) .
Si2 C15 1.890(3) .
Si2 C18 1.907(3) .
Si3 N3 1.725(3) .
Si3 C23 1.902(3) .
Si3 C26 1.912(3) .
Si3 C29 1.903(3) .
Na1 N5 2.363(3) .
Na1 N5 2.362(3) 3_775
Na1 H5 2.68(3) .
N1 C10 1.479(3) .
N2 C21 1.489(3) .
N3 C32 1.483(4) .
N4 C11 1.480(4) .
N4 C22 1.481(4) .
N4 C33 1.490(4) .
N5 Na1 2.362(3) 3_775
N5 H5 0.970(10) .
C1 H1 1.0000 .
C1 C2 1.541(4) .
C1 C3 1.534(4) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4 1.0000 .
C4 C5 1.535(4) .
C4 C6 1.521(5) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7 1.0000 .
C7 C8 1.524(5) .
C7 C9 1.541(5) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C10 C11 1.518(4) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12 1.0000 .
C12 C13 1.528(5) .
C12 C14 1.533(4) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15 1.0000 .
C15 C16 1.536(5) .
C15 C17 1.532(6) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18 1.0000 .
C18 C19 1.532(5) .
C18 C20 1.536(5) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C21 C22 1.518(4) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 H23 1.0000 .
C23 C24 1.522(5) .
C23 C25 1.533(4) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 H25A 0.9800 .
C25 H25B 0.9800 .
C25 H25C 0.9800 .
C26 H26 1.0000 .
C26 C27 1.530(4) .
C26 C28 1.534(5) .
C27 Na1 3.090(4) 3_775
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29 1.0000 .
C29 C30 1.524(5) .
C29 C31 1.522(5) .
C30 H30A 0.9800 .
C30 H30B 0.9800 .
C30 H30C 0.9800 .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C32 C33 1.514(5) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
U1 N1 C10 C11 62.3(2) .
U1 N2 C21 C22 65.5(2) .
U1 N3 C32 C33 61.8(3) .
U1 N4 C11 C10 27.9(2) .
U1 N4 C22 C21 26.2(3) .
U1 N4 C33 C32 27.4(3) .
Si1 N1 C10 C11 -114.1(2) .
Si2 N2 C21 C22 -112.7(2) .
Si3 N3 C32 C33 -116.7(2) .
Si3 C26 C27 Na1 15.0(5) 3_775
N1 C10 C11 N4 -59.7(3) .
N2 Si2 C15 C16 171.4(3) .
N2 Si2 C15 C17 -61.7(3) .
N2 C21 C22 N4 -62.2(3) .
N3 C32 C33 N4 -60.2(3) .
C1 Si1 N1 U1 -6.6(2) .
C1 Si1 N1 C10 168.9(2) .
C4 Si1 N1 U1 -130.07(17) .
C4 Si1 N1 C10 45.4(2) .
C7 Si1 N1 U1 110.40(18) .
C7 Si1 N1 C10 -74.1(2) .
C11 N4 C22 C21 -91.4(3) .
C11 N4 C33 C32 144.7(3) .
C12 Si2 N2 U1 106.22(19) .
C12 Si2 N2 C21 -76.3(2) .
C12 Si2 C15 C16 50.2(3) .
C12 Si2 C15 C17 177.2(3) .
C15 Si2 N2 U1 -10.3(2) .
C15 Si2 N2 C21 167.3(2) .
C18 Si2 N2 U1 -134.95(18) .
C18 Si2 N2 C21 42.6(2) .
C18 Si2 C15 C16 -65.6(4) .
C18 Si2 C15 C17 61.4(3) .
C22 N4 C11 C10 144.9(2) .
C22 N4 C33 C32 -89.0(3) .
C23 Si3 N3 U1 -15.1(2) .
C23 Si3 N3 C32 163.0(2) .
C26 Si3 N3 U1 102.09(19) .
C26 Si3 N3 C32 -79.7(3) .
C28 C26 C27 Na1 -111.4(4) 3_775
C29 Si3 N3 U1 -140.39(18) .
C29 Si3 N3 C32 37.8(3) .
C33 N4 C11 C10 -88.6(3) .
C33 N4 C22 C21 142.3(2) .
