# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Gregory Girolami'
_publ_contact_author_email       GIROLAMI@SCS.ILLINOIS.EDU

_publ_section_title              
;
Uranium-Hydrogen Interactions.
Synthesis and Crystal Structures
of Tris(N,N-Dimethylaminodiboranato)uranium(III)
;
loop_
_publ_author_name
'Gregory Girolami'
'Scott Daly'

# Attachment 'fa99sm_face.cif'

data_fa99sm_face
_database_code_depnum_ccdc_archive 'CCDC 748248'
#TrackingRef 'fa99sm_face.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'U(H3BNMe2BH3)3 crystals grown from pentane'
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H36 B6 N3 U'
_chemical_formula_sum            'C6 H36 B6 N3 U'
_chemical_formula_weight         453.27

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'
B B 0.0013 0.0007 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.9392(4)
_cell_length_b                   10.2456(3)
_cell_length_c                   11.4154(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1920(10)
_cell_angle_gamma                90.00
_cell_volume                     1849.54(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    7463
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.49

_exptl_crystal_description       platy
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    8.757
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.19022
_exptl_absorpt_correction_T_max  0.84296
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28641
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4251
_reflns_number_gt                3223
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker Apex'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4251
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
U1 U 0.265098(11) 0.161190(17) 0.840216(16) 0.02029(7) Uani 1 1 d . . .
N1 N 0.0888(3) 0.3614(4) 0.8009(4) 0.0272(10) Uani 1 1 d . . .
N2 N 0.2402(3) -0.1561(4) 0.9377(4) 0.0245(9) Uani 1 1 d . . .
N3 N 0.4342(3) 0.2176(4) 0.6738(4) 0.0216(9) Uani 1 1 d . . .
C1 C 0.0129(4) 0.3593(6) 0.8640(6) 0.0412(16) Uani 1 1 d . . .
H1A H 0.0070 0.4438 0.9023 0.062 Uiso 1 1 calc R . .
H1B H 0.0190 0.2902 0.9238 0.062 Uiso 1 1 calc R . .
H1C H -0.0374 0.3424 0.8075 0.062 Uiso 1 1 calc R . .
C2 C 0.0783(4) 0.4674(6) 0.7126(5) 0.0404(15) Uani 1 1 d . . .
H2A H 0.0273 0.4517 0.6571 0.061 Uiso 1 1 calc R . .
H2B H 0.1277 0.4699 0.6694 0.061 Uiso 1 1 calc R . .
H2C H 0.0731 0.5511 0.7527 0.061 Uiso 1 1 calc R . .
C3 C 0.1555(4) -0.2059(6) 0.9587(6) 0.0371(14) Uani 1 1 d . . .
H3A H 0.1408 -0.2821 0.9084 0.056 Uiso 1 1 calc R . .
H3B H 0.1131 -0.1374 0.9398 0.056 Uiso 1 1 calc R . .
H3C H 0.1570 -0.2309 1.0418 0.056 Uiso 1 1 calc R . .
C4 C 0.3037(4) -0.2605(5) 0.9700(5) 0.0360(14) Uani 1 1 d . . .
H4A H 0.3034 -0.2842 1.0531 0.054 Uiso 1 1 calc R . .
H4B H 0.3600 -0.2288 0.9579 0.054 Uiso 1 1 calc R . .
H4C H 0.2895 -0.3372 0.9202 0.054 Uiso 1 1 calc R . .
C5 C 0.4820(4) 0.1105(6) 0.6245(5) 0.0311(13) Uani 1 1 d . . .
H5A H 0.4810 0.1230 0.5392 0.047 Uiso 1 1 calc R . .
H5B H 0.4559 0.0265 0.6394 0.047 Uiso 1 1 calc R . .
H5C H 0.5407 0.1113 0.6623 0.047 Uiso 1 1 calc R . .
C6 C 0.4724(4) 0.3441(5) 0.6439(5) 0.0304(12) Uani 1 1 d . . .
H6A H 0.5313 0.3478 0.6806 0.046 Uiso 1 1 calc R . .
H6B H 0.4406 0.4163 0.6736 0.046 Uiso 1 1 calc R . .
H6C H 0.4704 0.3516 0.5580 0.046 Uiso 1 1 calc R . .
B1 B 0.1693(4) 0.3848(7) 0.8925(6) 0.0326(15) Uani 1 1 d . . .
H1D H 0.2266 0.4046 0.8430 0.039 Uiso 1 1 d R . .
H1E H 0.1821 0.2938 0.9509 0.039 Uiso 1 1 d R . .
H1F H 0.1583 0.4733 0.9506 0.039 Uiso 1 1 d R . .
B2 B 0.0972(4) 0.2257(7) 0.7371(6) 0.0307(15) Uani 1 1 d . . .
H2F H 0.0371 0.2066 0.6724 0.037 Uiso 1 1 d R . .
H2E H 0.1055 0.1438 0.8065 0.037 Uiso 1 1 d R . .
H2D H 0.1549 0.2281 0.6861 0.037 Uiso 1 1 d R . .
B3 B 0.2632(4) -0.0324(6) 1.0181(5) 0.0292(14) Uani 1 1 d . . .
H3D H 0.2097 0.0432 1.0017 0.035 Uiso 1 1 d R . .
H3E H 0.3252 0.0126 0.9953 0.035 Uiso 1 1 d R . .
H3F H 0.2713 -0.0631 1.1158 0.035 Uiso 1 1 d R . .
B4 B 0.2391(5) -0.1184(6) 0.8049(6) 0.0334(15) Uani 1 1 d . . .
H4F H 0.2269 -0.2102 0.7473 0.040 Uiso 1 1 d R . .
H4E H 0.3032 -0.0737 0.7906 0.040 Uiso 1 1 d R . .
H4D H 0.1862 -0.0435 0.7791 0.040 Uiso 1 1 d R . .
B5 B 0.4411(4) 0.2049(7) 0.8122(5) 0.0294(14) Uani 1 1 d . . .
H5D H 0.4183 0.1032 0.8366 0.035 Uiso 1 1 d R . .
H5E H 0.3997 0.2834 0.8486 0.035 Uiso 1 1 d R . .
H5F H 0.5103 0.2190 0.8525 0.035 Uiso 1 1 d R . .
B6 B 0.3388(4) 0.2128(6) 0.6217(5) 0.0233(13) Uani 1 1 d . . .
H6F H 0.3327 0.2245 0.5208 0.028 Uiso 1 1 d R . .
H6E H 0.3030 0.2960 0.6613 0.028 Uiso 1 1 d R . .
H6D H 0.3104 0.1142 0.6446 0.028 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.02071(11) 0.01953(10) 0.02103(11) 0.00069(9) 0.00417(7) 0.00030(9)
N1 0.022(2) 0.026(3) 0.034(3) 0.0019(19) 0.0028(19) 0.0024(18)
N2 0.022(2) 0.020(2) 0.031(3) 0.0013(19) 0.0041(18) -0.0025(19)
N3 0.021(2) 0.024(2) 0.021(2) 0.0006(18) 0.0061(18) 0.0002(18)
C1 0.029(3) 0.053(4) 0.043(4) 0.002(3) 0.010(3) 0.007(3)
C2 0.039(4) 0.035(3) 0.046(4) 0.010(3) 0.003(3) 0.011(3)
C3 0.029(3) 0.028(3) 0.053(4) 0.006(3) 0.001(3) -0.011(3)
C4 0.032(3) 0.027(3) 0.048(4) 0.004(3) 0.003(3) 0.006(3)
C5 0.034(3) 0.034(3) 0.026(3) 0.004(2) 0.008(2) 0.012(3)
C6 0.027(3) 0.032(3) 0.032(3) -0.003(3) 0.005(2) -0.006(3)
B1 0.028(4) 0.029(3) 0.041(4) -0.003(3) 0.005(3) 0.008(3)
B2 0.023(3) 0.039(4) 0.031(4) -0.005(3) 0.005(3) 0.003(3)
B3 0.041(4) 0.027(3) 0.021(3) 0.001(3) 0.008(3) -0.004(3)
B4 0.042(4) 0.025(3) 0.034(4) 0.001(3) 0.003(3) 0.000(3)
B5 0.021(3) 0.042(4) 0.026(3) 0.003(3) 0.002(3) 0.000(3)
B6 0.024(3) 0.022(3) 0.023(3) 0.005(2) 0.000(2) -0.002(3)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
U1 B3 2.842(6) . ?
U1 B1 2.857(6) . ?
U1 B2 2.863(6) . ?
U1 B5 2.897(6) . ?
U1 B4 2.915(7) . ?
U1 B6 2.935(6) . ?
U1 H1D 2.5690 . ?
U1 H1E 2.3685 . ?
U1 H2E 2.5309 . ?
U1 H2D 2.4239 . ?
U1 H3D 2.4593 . ?
U1 H3E 2.4381 . ?
U1 H4E 2.5628 . ?
U1 H4D 2.4997 . ?
U1 H5D 2.5179 . ?
U1 H5E 2.4757 . ?
U1 H6E 2.5988 . ?
U1 H6D 2.4785 . ?
N1 C2 1.477(7) . ?
N1 C1 1.483(7) . ?
N1 B1 1.569(8) . ?
N1 B2 1.583(7) . ?
N2 C4 1.486(7) . ?
N2 C3 1.491(7) . ?
N2 B4 1.562(8) . ?
N2 B3 1.581(7) . ?
N3 C5 1.487(7) . ?
N3 C6 1.490(6) . ?
N3 B6 1.562(7) . ?
N3 B5 1.576(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
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 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
B1 H1D 1.1500 . ?
B1 H1E 1.1501 . ?
B1 H1F 1.1501 . ?
B2 H2F 1.1501 . ?
B2 H2E 1.1501 . ?
B2 H2D 1.1500 . ?
B3 H3D 1.1500 . ?
B3 H3E 1.1501 . ?
B3 H3F 1.1501 . ?
B4 H4F 1.1501 . ?
B4 H4E 1.1500 . ?
B4 H4D 1.1501 . ?
B5 H5D 1.1500 . ?
B5 H5E 1.1500 . ?
B5 H5F 1.1501 . ?
B6 H6F 1.1500 . ?
B6 H6E 1.1501 . ?
B6 H6D 1.1501 . ?

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
B3 U1 B1 110.90(19) . . ?
B3 U1 B2 111.2(2) . . ?
B1 U1 B2 53.45(19) . . ?
B3 U1 B5 106.51(19) . . ?
B1 U1 B5 116.7(2) . . ?
B2 U1 B5 141.91(19) . . ?
B3 U1 B4 53.05(18) . . ?
B1 U1 B4 138.3(2) . . ?
B2 U1 B4 93.5(2) . . ?
B5 U1 B4 105.1(2) . . ?
B3 U1 B6 140.74(18) . . ?
B1 U1 B6 108.31(19) . . ?
B2 U1 B6 93.56(17) . . ?
B5 U1 B6 51.86(17) . . ?
B4 U1 B6 97.15(18) . . ?
B3 U1 H1D 130.1 . . ?
B1 U1 H1D 23.7 . . ?
B2 U1 H1D 64.4 . . ?
B5 U1 H1D 95.0 . . ?
B4 U1 H1D 157.7 . . ?
B6 U1 H1D 87.6 . . ?
B3 U1 H1E 87.8 . . ?
B1 U1 H1E 23.1 . . ?
B2 U1 H1E 62.1 . . ?
B5 U1 H1E 125.7 . . ?
B4 U1 H1E 123.9 . . ?
B6 U1 H1E 131.3 . . ?
H1D U1 H1E 44.5 . . ?
B3 U1 H2E 87.6 . . ?
B1 U1 H2E 62.3 . . ?
B2 U1 H2E 23.6 . . ?
B5 U1 H2E 164.3 . . ?
B4 U1 H2E 77.7 . . ?
B6 U1 H2E 112.6 . . ?
H1D U1 H2E 80.4 . . ?
H1E U1 H2E 60.3 . . ?
B3 U1 H2D 130.1 . . ?
B1 U1 H2D 64.4 . . ?
B2 U1 H2D 23.3 . . ?
B5 U1 H2D 120.0 . . ?
B4 U1 H2D 95.7 . . ?
B6 U1 H2D 70.3 . . ?
H1D U1 H2D 65.3 . . ?
H1E U1 H2D 79.8 . . ?
H2E U1 H2D 44.5 . . ?
B3 U1 H3D 23.7 . . ?
B1 U1 H3D 89.2 . . ?
B2 U1 H3D 90.9 . . ?
B5 U1 H3D 127.0 . . ?
B4 U1 H3D 64.1 . . ?
B6 U1 H3D 160.9 . . ?
H1D U1 H3D 111.0 . . ?
H1E U1 H3D 66.7 . . ?
H2E U1 H3D 68.3 . . ?
H2D U1 H3D 112.8 . . ?
B3 U1 H3E 23.6 . . ?
B1 U1 H3E 121.4 . . ?
B2 U1 H3E 134.8 . . ?
B5 U1 H3E 83.1 . . ?
B4 U1 H3E 61.5 . . ?
B6 U1 H3E 124.5 . . ?
H1D U1 H3E 132.0 . . ?
H1E U1 H3E 99.5 . . ?
H2E U1 H3E 111.3 . . ?
H2D U1 H3E 152.5 . . ?
H3D U1 H3E 45.1 . . ?
B3 U1 H4E 61.7 . . ?
B1 U1 H4E 161.2 . . ?
B2 U1 H4E 111.2 . . ?
B5 U1 H4E 82.0 . . ?
B4 U1 H4E 23.1 . . ?
B6 U1 H4E 81.4 . . ?
H1D U1 H4E 167.9 . . ?
H1E U1 H4E 145.1 . . ?
H2E U1 H4E 99.3 . . ?
H2D U1 H4E 106.0 . . ?
H3D U1 H4E 79.7 . . ?
H3E U1 H4E 59.5 . . ?
B3 U1 H4D 64.1 . . ?
B1 U1 H4D 117.9 . . ?
B2 U1 H4D 70.6 . . ?
B5 U1 H4D 124.0 . . ?
B4 U1 H4D 22.9 . . ?
B6 U1 H4D 98.9 . . ?
H1D U1 H4D 134.9 . . ?
H1E U1 H4D 109.6 . . ?
H2E U1 H4D 55.8 . . ?
H2D U1 H4D 75.0 . . ?
H3D U1 H4D 65.3 . . ?
H3E U1 H4D 79.5 . . ?
H4E U1 H4D 43.5 . . ?
B3 U1 H5D 86.8 . . ?
B1 U1 H5D 137.5 . . ?
B2 U1 H5D 155.0 . . ?
B5 U1 H5D 23.2 . . ?
B4 U1 H5D 83.5 . . ?
B6 U1 H5D 62.4 . . ?
H1D U1 H5D 117.6 . . ?
H1E U1 H5D 138.7 . . ?
H2E U1 H5D 159.9 . . ?
H2D U1 H5D 132.1 . . ?
H3D U1 H5D 109.6 . . ?
H3E U1 H5D 64.6 . . ?
H4E U1 H5D 61.2 . . ?
H4D U1 H5D 104.6 . . ?
B3 U1 H5E 114.4 . . ?
B1 U1 H5E 94.0 . . ?
B2 U1 H5E 131.3 . . ?
B5 U1 H5E 23.0 . . ?
B4 U1 H5E 127.6 . . ?
B6 U1 H5E 60.3 . . ?
H1D U1 H5E 73.5 . . ?
H1E U1 H5E 103.2 . . ?
H2E U1 H5E 153.0 . . ?
H2D U1 H5E 115.5 . . ?
H3D U1 H5E 127.6 . . ?
H3E U1 H5E 91.6 . . ?
H4E U1 H5E 104.8 . . ?
H4D U1 H5E 147.0 . . ?
H5D U1 H5E 44.2 . . ?
B3 U1 H6E 163.1 . . ?
B1 U1 H6E 85.4 . . ?
B2 U1 H6E 81.5 . . ?
B5 U1 H6E 60.5 . . ?
B4 U1 H6E 117.2 . . ?
B6 U1 H6E 23.0 . . ?
H1D U1 H6E 64.7 . . ?
H1E U1 H6E 108.3 . . ?
H2E U1 H6E 104.2 . . ?
H2D U1 H6E 59.9 . . ?
H3D U1 H6E 172.3 . . ?
H3E U1 H6E 142.5 . . ?
H4E U1 H6E 103.9 . . ?
H4D U1 H6E 112.6 . . ?
H5D U1 H6E 78.0 . . ?
H5E U1 H6E 58.4 . . ?
B3 U1 H6D 122.6 . . ?
B1 U1 H6D 124.6 . . ?
B2 U1 H6D 92.1 . . ?
B5 U1 H6D 62.3 . . ?
B4 U1 H6D 74.8 . . ?
B6 U1 H6D 22.6 . . ?
H1D U1 H6D 107.3 . . ?
H1E U1 H6D 146.8 . . ?
H2E U1 H6D 104.5 . . ?
H2D U1 H6D 70.6 . . ?
H3D U1 H6D 138.8 . . ?
H3E U1 H6D 113.6 . . ?
H4E U1 H6D 61.0 . . ?
H4D U1 H6D 77.2 . . ?
H5D U1 H6D 63.1 . . ?
H5E U1 H6D 77.5 . . ?
H6E U1 H6D 43.3 . . ?
C2 N1 C1 108.3(4) . . ?
C2 N1 B1 110.8(4) . . ?
C1 N1 B1 109.1(5) . . ?
C2 N1 B2 109.9(5) . . ?
C1 N1 B2 109.3(4) . . ?
B1 N1 B2 109.4(4) . . ?
C4 N2 C3 108.4(4) . . ?
C4 N2 B4 110.1(4) . . ?
C3 N2 B4 109.9(5) . . ?
C4 N2 B3 109.4(4) . . ?
C3 N2 B3 109.2(4) . . ?
B4 N2 B3 109.8(4) . . ?
C5 N3 C6 108.2(4) . . ?
C5 N3 B6 110.7(4) . . ?
C6 N3 B6 110.3(4) . . ?
C5 N3 B5 110.1(4) . . ?
C6 N3 B5 108.8(4) . . ?
B6 N3 B5 108.8(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 B1 U1 98.8(3) . . ?
N1 B1 H1D 109.5 . . ?
U1 B1 H1D 63.9 . . ?
N1 B1 H1E 109.5 . . ?
U1 B1 H1E 53.8 . . ?
H1D B1 H1E 109.5 . . ?
N1 B1 H1F 109.5 . . ?
U1 B1 H1F 151.3 . . ?
H1D B1 H1F 109.5 . . ?
H1E B1 H1F 109.5 . . ?
N1 B2 U1 98.2(3) . . ?
N1 B2 H2F 109.5 . . ?
U1 B2 H2F 152.2 . . ?
N1 B2 H2E 109.5 . . ?
U1 B2 H2E 61.8 . . ?
H2F B2 H2E 109.5 . . ?
N1 B2 H2D 109.5 . . ?
U1 B2 H2D 56.4 . . ?
H2F B2 H2D 109.5 . . ?
H2E B2 H2D 109.5 . . ?
N2 B3 U1 99.6(3) . . ?
N2 B3 H3D 109.5 . . ?
U1 B3 H3D 59.2 . . ?
N2 B3 H3E 109.5 . . ?
U1 B3 H3E 58.1 . . ?
H3D B3 H3E 109.5 . . ?
N2 B3 H3F 109.5 . . ?
U1 B3 H3F 150.9 . . ?
H3D B3 H3F 109.5 . . ?
H3E B3 H3F 109.5 . . ?
N2 B4 U1 97.2(3) . . ?
N2 B4 H4F 109.5 . . ?
U1 B4 H4F 153.3 . . ?
N2 B4 H4E 109.5 . . ?
U1 B4 H4E 61.0 . . ?
H4F B4 H4E 109.5 . . ?
N2 B4 H4D 109.5 . . ?
U1 B4 H4D 57.8 . . ?
H4F B4 H4D 109.5 . . ?
H4E B4 H4D 109.5 . . ?
N3 B5 U1 100.1(3) . . ?
N3 B5 H5D 109.5 . . ?
U1 B5 H5D 59.5 . . ?
N3 B5 H5E 109.5 . . ?
U1 B5 H5E 57.4 . . ?
H5D B5 H5E 109.5 . . ?
N3 B5 H5F 109.5 . . ?
U1 B5 H5F 150.4 . . ?
H5D B5 H5F 109.5 . . ?
H5E B5 H5F 109.5 . . ?
N3 B6 U1 99.0(3) . . ?
N3 B6 H6F 109.5 . . ?
U1 B6 H6F 151.4 . . ?
N3 B6 H6E 109.5 . . ?
U1 B6 H6E 61.9 . . ?
H6F B6 H6E 109.5 . . ?
N3 B6 H6D 109.5 . . ?
U1 B6 H6D 55.8 . . ?
H6F B6 H6D 109.5 . . ?
H6E B6 H6D 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.905
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.167


# Attachment 'fa24u_face.cif'

data_fa24u_face
_database_code_depnum_ccdc_archive 'CCDC 748249'
#TrackingRef 'fa24u_face.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'U(H3BNMe2BH3)3 crystals grown from toluene'
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H36 B6 N3 U'
_chemical_formula_sum            'C6 H36 B6 N3 U'
_chemical_formula_weight         453.27

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'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.3571(6)
_cell_length_b                   10.8128(6)
_cell_length_c                   14.6145(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.116(3)
_cell_angle_gamma                90.00
_cell_volume                     1941.60(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    14808
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      28.74

_exptl_crystal_description       platy
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    8.342
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.45595
_exptl_absorpt_correction_T_max  0.75389
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23364
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         28.74
_reflns_number_total             5035
_reflns_number_gt                3716
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker Apex'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5035
_refine_ls_number_parameters     223
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
U1 U -0.199469(15) 0.950209(16) 0.205436(12) 0.02264(7) Uani 1 1 d . . .
N1 N -0.2504(4) 1.1137(4) -0.0009(3) 0.0335(11) Uani 1 1 d . . .
C1 C -0.1650(6) 1.1859(6) -0.0428(5) 0.0538(18) Uani 1 1 d . . .
H1A H -0.1579 1.1543 -0.1048 0.081 Uiso 1 1 calc R . .
H1B H -0.0953 1.1773 -0.0047 0.081 Uiso 1 1 calc R . .
H1C H -0.1859 1.2733 -0.0466 0.081 Uiso 1 1 calc R . .
C2 C -0.3549(6) 1.1223(7) -0.0602(4) 0.0537(18) Uani 1 1 d . . .
H2A H -0.3770 1.2091 -0.0666 0.081 Uiso 1 1 calc R . .
H2B H -0.4108 1.0754 -0.0323 0.081 Uiso 1 1 calc R . .
H2C H -0.3462 1.0879 -0.1211 0.081 Uiso 1 1 calc R . .
B1 B -0.2641(6) 1.1684(6) 0.0975(5) 0.0356(15) Uani 1 1 d D . .
H11 H -0.333(3) 1.114(4) 0.130(3) 0.027(14) Uiso 1 1 d D . .
H12 H -0.184(3) 1.162(6) 0.148(3) 0.06(2) Uiso 1 1 d D . .
H13 H -0.290(4) 1.266(3) 0.100(3) 0.025(13) Uiso 1 1 d D . .
B2 B -0.2128(6) 0.9739(6) 0.0095(5) 0.0364(15) Uani 1 1 d D . .
H21 H -0.125(2) 0.983(6) 0.050(4) 0.044(17) Uiso 1 1 d D . .
H22 H -0.281(4) 0.921(5) 0.044(4) 0.052(18) Uiso 1 1 d D . .
H23 H -0.204(5) 0.930(5) -0.057(3) 0.041(16) Uiso 1 1 d D . .
N2 N -0.4159(3) 0.9037(4) 0.3376(3) 0.0265(9) Uani 1 1 d . . .
C3 C -0.4184(6) 0.8074(6) 0.4097(5) 0.0520(18) Uani 1 1 d . . .
H3A H -0.4201 0.8471 0.4699 0.078 Uiso 1 1 calc R . .
H3B H -0.3532 0.7556 0.4108 0.078 Uiso 1 1 calc R . .
H3C H -0.4834 0.7559 0.3962 0.078 Uiso 1 1 calc R . .
C4 C -0.5176(5) 0.9757(6) 0.3321(5) 0.0513(17) Uani 1 1 d . . .
H4A H -0.5800 0.9195 0.3214 0.077 Uiso 1 1 calc R . .
H4B H -0.5191 1.0349 0.2813 0.077 Uiso 1 1 calc R . .
H4C H -0.5215 1.0204 0.3900 0.077 Uiso 1 1 calc R . .
B3 B -0.3139(6) 0.9921(7) 0.3628(5) 0.0352(15) Uani 1 1 d D . .
H31 H -0.239(3) 0.924(4) 0.366(4) 0.037(16) Uiso 1 1 d D . .
H32 H -0.313(4) 1.067(3) 0.305(2) 0.021(14) Uiso 1 1 d D . .
H33 H -0.326(4) 1.028(5) 0.432(2) 0.027(14) Uiso 1 1 d D . .
B4 B -0.4033(5) 0.8402(6) 0.2426(4) 0.0327(14) Uani 1 1 d D . .
H41 H -0.399(5) 0.919(4) 0.188(3) 0.039(16) Uiso 1 1 d D . .
H42 H -0.318(3) 0.790(4) 0.248(4) 0.035(15) Uiso 1 1 d D . .
H43 H -0.478(3) 0.789(5) 0.221(4) 0.06(2) Uiso 1 1 d D . .
N3 N -0.0953(3) 0.5883(4) 0.1618(3) 0.0252(9) Uani 1 1 d . . .
C5 C -0.1828(5) 0.5113(6) 0.1957(5) 0.0479(17) Uani 1 1 d . . .
H5A H -0.2540 0.5411 0.1686 0.072 Uiso 1 1 calc R . .
H5B H -0.1786 0.5172 0.2629 0.072 Uiso 1 1 calc R . .
H5C H -0.1734 0.4249 0.1779 0.072 Uiso 1 1 calc R . .
C6 C -0.0986(6) 0.5723(6) 0.0607(4) 0.0476(17) Uani 1 1 d . . .
H6A H -0.0923 0.4842 0.0462 0.071 Uiso 1 1 calc R . .
H6B H -0.0380 0.6176 0.0383 0.071 Uiso 1 1 calc R . .
H6C H -0.1676 0.6044 0.0307 0.071 Uiso 1 1 calc R . .
B5 B -0.1182(5) 0.7251(5) 0.1815(4) 0.0266(13) Uani 1 1 d D . .
H51 H -0.192(2) 0.750(5) 0.150(3) 0.022(13) Uiso 1 1 d D . .
H52 H -0.069(3) 0.790(4) 0.158(3) 0.025(14) Uiso 1 1 d D . .
H53 H -0.126(4) 0.744(5) 0.2483(18) 0.029(14) Uiso 1 1 d D . .
B6 B 0.0168(5) 0.5441(6) 0.2086(5) 0.0291(13) Uani 1 1 d D . .
H61 H 0.077(4) 0.599(5) 0.190(4) 0.046(17) Uiso 1 1 d D . .
H62 H 0.025(6) 0.457(3) 0.184(4) 0.06(2) Uiso 1 1 d D . .
H63 H 0.016(5) 0.542(5) 0.2780(16) 0.032(15) Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
U1 0.02169(11) 0.02058(9) 0.02456(11) -0.00092(8) -0.00263(7) -0.00026(8)
N1 0.044(3) 0.029(2) 0.026(2) 0.0066(18) -0.003(2) 0.002(2)
C1 0.064(5) 0.044(4) 0.055(4) 0.017(3) 0.016(4) -0.002(3)
C2 0.062(5) 0.053(4) 0.040(4) 0.007(3) -0.022(3) -0.003(3)
B1 0.042(4) 0.025(3) 0.038(4) 0.001(3) -0.005(3) 0.005(3)
B2 0.047(4) 0.034(3) 0.029(3) 0.000(3) 0.007(3) 0.003(3)
N2 0.019(2) 0.030(2) 0.031(2) 0.0018(18) 0.0035(18) 0.0013(17)
C3 0.047(4) 0.055(4) 0.055(4) 0.018(3) 0.008(3) 0.001(3)
C4 0.038(4) 0.046(4) 0.070(5) -0.003(3) 0.005(3) 0.015(3)
B3 0.039(4) 0.037(3) 0.029(4) -0.008(3) 0.000(3) -0.002(3)
B4 0.025(3) 0.033(3) 0.040(4) -0.007(3) 0.000(3) -0.007(3)
N3 0.023(2) 0.0222(19) 0.029(2) -0.0050(16) -0.0043(18) 0.0008(17)
C5 0.028(3) 0.033(3) 0.082(5) -0.002(3) 0.005(3) -0.008(2)
C6 0.050(4) 0.057(4) 0.032(3) -0.016(3) -0.009(3) 0.018(3)
B5 0.027(3) 0.025(3) 0.027(3) 0.000(2) -0.002(3) 0.004(2)
B6 0.025(3) 0.024(3) 0.037(3) -0.003(3) 0.000(3) 0.006(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
U1 B6 2.665(6) 2 ?
U1 B5 2.670(6) . ?
U1 B3 2.861(7) . ?
U1 B2 2.862(7) . ?
U1 B4 2.889(6) . ?
U1 B1 2.902(6) . ?
U1 H11 2.59(5) . ?
U1 H12 2.46(7) . ?
U1 H21 2.57(6) . ?
U1 H22 2.48(6) . ?
U1 H31 2.46(5) . ?
U1 H32 2.47(5) . ?
U1 H41 2.47(6) . ?
U1 H42 2.40(5) . ?
U1 H51 2.31(5) . ?
U1 H52 2.51(5) . ?
U1 H53 2.46(5) . ?
N1 C2 1.480(7) . ?
N1 C1 1.495(7) . ?
N1 B1 1.581(8) . ?
N1 B2 1.583(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
B1 H11 1.17(2) . ?
B1 H12 1.17(2) . ?
B1 H13 1.10(3) . ?
B2 H21 1.18(2) . ?
B2 H22 1.18(2) . ?
B2 H23 1.10(3) . ?
N2 C4 1.473(7) . ?
N2 C3 1.484(7) . ?
N2 B4 1.572(7) . ?
N2 B3 1.593(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
B3 H31 1.18(2) . ?
B3 H32 1.18(2) . ?
B3 H33 1.10(3) . ?
B4 H41 1.17(2) . ?
B4 H42 1.18(2) . ?
B4 H43 1.10(3) . ?
N3 C6 1.484(7) . ?
N3 C5 1.491(7) . ?
N3 B5 1.540(7) . ?
N3 B6 1.553(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
B5 H51 1.01(2) . ?
B5 H52 1.01(2) . ?
B5 H53 1.01(2) . ?
B6 U1 2.665(6) 2_545 ?
B6 H61 1.02(2) . ?
B6 H62 1.02(2) . ?
B6 H63 1.02(2) . ?

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
B6 U1 B5 95.59(19) 2 . ?
B6 U1 B3 91.6(2) 2 . ?
B5 U1 B3 118.3(2) . . ?
B6 U1 B2 113.2(2) 2 . ?
B5 U1 B2 86.16(19) . . ?
B3 U1 B2 144.0(2) . . ?
B6 U1 B4 141.25(19) 2 . ?
B5 U1 B4 89.83(19) . . ?
B3 U1 B4 53.02(18) . . ?
B2 U1 B4 105.5(2) . . ?
B6 U1 B1 96.70(19) 2 . ?
B5 U1 B1 139.07(19) . . ?
B3 U1 B1 100.2(2) . . ?
B2 U1 B1 53.16(18) . . ?
B4 U1 B1 104.0(2) . . ?
B6 U1 H11 114.3(8) 2 . ?
B5 U1 H11 143.1(11) . . ?
B3 U1 H11 83.6(9) . . ?
B2 U1 H11 62.9(10) . . ?
B4 U1 H11 80.4(5) . . ?
B1 U1 H11 23.8(4) . . ?
B6 U1 H12 73.3(6) 2 . ?
B5 U1 H12 139.6(14) . . ?
B3 U1 H12 101.0(15) . . ?
B2 U1 H12 64.7(12) . . ?
B4 U1 H12 123.4(10) . . ?
B1 U1 H12 23.4(5) . . ?
H11 U1 H12 44.3(11) . . ?
B6 U1 H21 90.0(6) 2 . ?
B5 U1 H21 80.5(14) . . ?
B3 U1 H21 160.8(13) . . ?
B2 U1 H21 24.3(5) . . ?
B4 U1 H21 128.7(7) . . ?
B1 U1 H21 60.6(13) . . ?
H11 U1 H21 78.3(14) . . ?
H12 U1 H21 61(2) . . ?
B6 U1 H22 137.2(6) 2 . ?
B5 U1 H22 83.0(14) . . ?
B3 U1 H22 126.8(10) . . ?
B2 U1 H22 24.1(5) . . ?
B4 U1 H22 81.5(6) . . ?
B1 U1 H22 61.9(13) . . ?
H11 U1 H22 60.5(18) . . ?
H12 U1 H22 80.5(16) . . ?
H21 U1 H22 47.4(10) . . ?
B6 U1 H31 80.7(12) 2 . ?
B5 U1 H31 97.9(8) . . ?
B3 U1 H31 24.1(5) . . ?
B2 U1 H31 165.2(10) . . ?
B4 U1 H31 60.5(12) . . ?
B1 U1 H31 122.6(7) . . ?
H11 U1 H31 107.6(9) . . ?
H12 U1 H31 117.6(17) . . ?
H21 U1 H31 170.4(13) . . ?
H22 U1 H31 142.0(12) . . ?
B6 U1 H32 92.0(11) 2 . ?
B5 U1 H32 142.1(6) . . ?
B3 U1 H32 24.1(5) . . ?
B2 U1 H32 124.3(7) . . ?
B4 U1 H32 62.5(10) . . ?
B1 U1 H32 76.2(5) . . ?
H11 U1 H32 61.5(12) . . ?
H12 U1 H32 78.0(15) . . ?
H21 U1 H32 136.6(14) . . ?
H22 U1 H32 115.1(16) . . ?
H31 U1 H32 46.9(10) . . ?
B6 U1 H41 152.2(13) 2 . ?
B5 U1 H41 104.3(11) . . ?
B3 U1 H41 62.1(12) . . ?
B2 U1 H41 87.6(9) . . ?
B4 U1 H41 23.7(5) . . ?
B1 U1 H41 80.8(6) . . ?
H11 U1 H41 57.7(10) . . ?
H12 U1 H41 101.8(9) . . ?
H21 U1 H41 111.9(9) . . ?
H22 U1 H41 65.6(14) . . ?
H31 U1 H41 77.6(14) . . ?
H32 U1 H41 60.4(17) . . ?
B6 U1 H42 131.8(11) 2 . ?
B5 U1 H42 67.9(7) . . ?
B3 U1 H42 62.5(11) . . ?
B2 U1 H42 110.6(13) . . ?
B4 U1 H42 23.5(6) . . ?
B1 U1 H42 126.0(7) . . ?
H11 U1 H42 103.0(6) . . ?
H12 U1 H42 146.8(12) . . ?
H21 U1 H42 128.0(17) . . ?
H22 U1 H42 87.4(13) . . ?
H31 U1 H42 58.8(18) . . ?
H32 U1 H42 79.4(13) . . ?
H41 U1 H42 45.3(11) . . ?
B6 U1 H51 117.2(6) 2 . ?
B5 U1 H51 22.0(6) . . ?
B3 U1 H51 118.0(12) . . ?
B2 U1 H51 74.7(11) . . ?
B4 U1 H51 75.4(10) . . ?
B1 U1 H51 126.2(9) . . ?
H11 U1 H51 122.6(12) . . ?
H12 U1 H51 138.3(19) . . ?
H21 U1 H51 77.9(18) . . ?
H22 U1 H51 64.9(16) . . ?
H31 U1 H51 104.1(15) . . ?
H32 U1 H51 136.8(14) . . ?
H41 U1 H51 85.1(14) . . ?
H42 U1 H51 57.4(14) . . ?
B6 U1 H52 81.7(10) 2 . ?
B5 U1 H52 22.3(5) . . ?
B3 U1 H52 135.9(9) . . ?
B2 U1 H52 75.8(10) . . ?
B4 U1 H52 111.5(6) . . ?
B1 U1 H52 123.8(8) . . ?
H11 U1 H52 138.7(14) . . ?
H12 U1 H52 118.1(15) . . ?
H21 U1 H52 63.3(15) . . ?
H22 U1 H52 81.7(18) . . ?
H31 U1 H52 112.6(11) . . ?
H32 U1 H52 159.5(11) . . ?
H41 U1 H52 122.7(15) . . ?
H42 U1 H52 90.1(9) . . ?
H51 U1 H52 37.8(12) . . ?
B6 U1 H53 87.4(11) 2 . ?
B5 U1 H53 22.3(5) . . ?
B3 U1 H53 98.0(7) . . ?
B2 U1 H53 108.4(5) . . ?
B4 U1 H53 83.3(12) . . ?
B1 U1 H53 161.2(6) . . ?
H11 U1 H53 158.3(15) . . ?
H12 U1 H53 153.1(16) . . ?
H21 U1 H53 101.2(15) . . ?
H22 U1 H53 103.0(16) . . ?
H31 U1 H53 76.1(9) . . ?
H32 U1 H53 122.1(8) . . ?
H41 U1 H53 103.8(14) . . ?
H42 U1 H53 59.9(13) . . ?
H51 U1 H53 38.2(13) . . ?
H52 U1 H53 38.5(12) . . ?
C2 N1 C1 109.7(5) . . ?
C2 N1 B1 109.7(5) . . ?
C1 N1 B1 109.0(5) . . ?
C2 N1 B2 110.2(5) . . ?
C1 N1 B2 109.0(5) . . ?
B1 N1 B2 109.2(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 B1 U1 98.0(3) . . ?
N1 B1 H11 109(2) . . ?
U1 B1 H11 63(3) . . ?
N1 B1 H12 113(3) . . ?
U1 B1 H12 56(3) . . ?
H11 B1 H12 109(4) . . ?
N1 B1 H13 117(3) . . ?
U1 B1 H13 145(3) . . ?
H11 B1 H13 104(4) . . ?
H12 B1 H13 105(4) . . ?
N1 B2 U1 99.6(3) . . ?
N1 B2 H21 102(3) . . ?
U1 B2 H21 64(3) . . ?
N1 B2 H22 107(3) . . ?
U1 B2 H22 59(3) . . ?
H21 B2 H22 119(4) . . ?
N1 B2 H23 112(3) . . ?
U1 B2 H23 148(3) . . ?
H21 B2 H23 108(4) . . ?
H22 B2 H23 108(4) . . ?
C4 N2 C3 109.2(5) . . ?
C4 N2 B4 110.3(5) . . ?
C3 N2 B4 109.4(5) . . ?
C4 N2 B3 110.2(5) . . ?
C3 N2 B3 109.4(5) . . ?
B4 N2 B3 108.4(4) . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 B3 U1 99.6(3) . . ?
N2 B3 H31 104(3) . . ?
U1 B3 H31 59(3) . . ?
N2 B3 H32 108(2) . . ?
U1 B3 H32 59(2) . . ?
H31 B3 H32 113(4) . . ?
N2 B3 H33 104(3) . . ?
U1 B3 H33 156(3) . . ?
H31 B3 H33 111(4) . . ?
H32 B3 H33 115(4) . . ?
N2 B4 U1 99.0(3) . . ?
N2 B4 H41 107(3) . . ?
U1 B4 H41 58(3) . . ?
N2 B4 H42 109(3) . . ?
U1 B4 H42 54(3) . . ?
H41 B4 H42 106(4) . . ?
N2 B4 H43 108(3) . . ?
U1 B4 H43 152(3) . . ?
H41 B4 H43 106(4) . . ?
H42 B4 H43 120(4) . . ?
C6 N3 C5 108.8(5) . . ?
C6 N3 B5 108.2(4) . . ?
C5 N3 B5 108.7(4) . . ?
C6 N3 B6 109.3(4) . . ?
C5 N3 B6 109.1(4) . . ?
B5 N3 B6 112.7(4) . . ?
N3 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 B5 U1 168.5(4) . . ?
N3 B5 H51 110(3) . . ?
U1 B5 H51 59(3) . . ?
N3 B5 H52 118(3) . . ?
U1 B5 H52 70(3) . . ?
H51 B5 H52 102(4) . . ?
N3 B5 H53 115(3) . . ?
U1 B5 H53 67(3) . . ?
H51 B5 H53 102(4) . . ?
H52 B5 H53 108(4) . . ?
N3 B6 U1 174.7(4) . 2_545 ?
N3 B6 H61 111(4) . . ?
U1 B6 H61 75(3) 2_545 . ?
N3 B6 H62 104(4) . . ?
U1 B6 H62 73(4) 2_545 . ?
H61 B6 H62 110(5) . . ?
N3 B6 H63 110(3) . . ?
U1 B6 H63 67(3) 2_545 . ?
H61 B6 H63 112(4) . . ?
H62 B6 H63 110(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.74
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         4.175
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.191