# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Shu-Jian Chen'
_publ_contact_author_email       schen@ion.chem.utk.edu
loop_
_publ_author_name
'Shu-Jian Chen'
'Juan Li'
B.Dougan
C.Steren
'Xiaoping Wang'
'Xue-Tai Chen'
'Zhenyang Lin'
'Ziling Xue'

data_2
_database_code_depnum_ccdc_archive 'CCDC 811902'
#TrackingRef '4124_web_deposit_cif_file_0_Shu-JianChen_1297046362.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Tantalum hydride
;
_chemical_name_common            'Tantalum hydride'
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H64 N9 Ta3'
_chemical_formula_sum            'C24 H64 N9 Ta3'
_chemical_formula_weight         1021.69

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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhomic
_symmetry_space_group_name_H-M   Pna2(1)

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

_cell_length_a                   21.270(11)
_cell_length_b                   9.700(5)
_cell_length_c                   17.118(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3532(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       fragment
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1960
_exptl_absorpt_coefficient_mu    9.298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2578
_exptl_absorpt_correction_T_max  0.6535
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35048
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         28.36
_reflns_number_total             8156
_reflns_number_gt                7938
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^)+(0.0138P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_number_reflns         8156
_refine_ls_number_parameters     349
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0158
_refine_ls_wR_factor_ref         0.0351
_refine_ls_wR_factor_gt          0.0349
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.004
_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
Ta1 Ta 0.641863(5) 0.572437(11) 0.355687(10) 0.01368(3) Uani 1 1 d . . .
Ta2 Ta 0.621722(6) 0.497101(12) 0.529583(9) 0.01442(3) Uani 1 1 d . . .
Ta3 Ta 0.752755(6) 0.479917(12) 0.462759(9) 0.01754(3) Uani 1 1 d . . .
H1 H 0.6936(18) 0.375(4) 0.516(2) 0.026 Uiso 1 1 d . . .
N1 N 0.74106(12) 0.5662(3) 0.3622(2) 0.0201(6) Uani 1 1 d . . .
N2 N 0.57340(13) 0.5029(2) 0.43262(17) 0.0161(6) Uani 1 1 d . . .
N3 N 0.71220(14) 0.6044(3) 0.55688(17) 0.0218(6) Uani 1 1 d . . .
N4 N 0.62715(14) 0.4650(3) 0.25758(18) 0.0194(6) Uani 1 1 d . . .
N5 N 0.62062(13) 0.7463(2) 0.33291(16) 0.0189(6) Uani 1 1 d . . .
N6 N 0.57585(14) 0.6438(3) 0.59045(17) 0.0222(6) Uani 1 1 d . . .
N7 N 0.59476(13) 0.3226(3) 0.58225(17) 0.0209(6) Uani 1 1 d . . .
N8 N 0.77331(14) 0.2845(3) 0.43725(17) 0.0250(6) Uani 1 1 d . . .
N9 N 0.84011(16) 0.5337(4) 0.5004(2) 0.0318(7) Uani 1 1 d . . .
C1 C 0.78509(17) 0.6325(4) 0.3046(2) 0.0270(8) Uani 1 1 d . . .
C2 C 0.84933(19) 0.5615(5) 0.3046(3) 0.0435(12) Uani 1 1 d . . .
H2A H 0.8443 0.4649 0.2892 0.065 Uiso 1 1 calc R . .
H2B H 0.8675 0.5660 0.3572 0.065 Uiso 1 1 calc R . .
H2C H 0.8773 0.6082 0.2676 0.065 Uiso 1 1 calc R . .
C3 C 0.75834(18) 0.6299(5) 0.2228(2) 0.0377(10) Uani 1 1 d . . .
H3A H 0.7496 0.5344 0.2076 0.057 Uiso 1 1 calc R . .
H3B H 0.7888 0.6702 0.1864 0.057 Uiso 1 1 calc R . .
H3C H 0.7193 0.6834 0.2214 0.057 Uiso 1 1 calc R . .
C4 C 0.7937(2) 0.7832(4) 0.3297(3) 0.0434(12) Uani 1 1 d . . .
H4A H 0.7525 0.8277 0.3339 0.065 Uiso 1 1 calc R . .
H4B H 0.8192 0.8318 0.2908 0.065 Uiso 1 1 calc R . .
H4C H 0.8149 0.7862 0.3805 0.065 Uiso 1 1 calc R . .
C5 C 0.50701(16) 0.4629(3) 0.4141(2) 0.0213(7) Uani 1 1 d . . .
C6 C 0.50781(17) 0.3174(4) 0.3795(2) 0.0309(9) Uani 1 1 d . . .
H6A H 0.5319 0.3177 0.3307 0.046 Uiso 1 1 calc R . .
H6B H 0.4646 0.2875 0.3689 0.046 Uiso 1 1 calc R . .
H6C H 0.5275 0.2538 0.4167 0.046 Uiso 1 1 calc R . .
C7 C 0.47842(15) 0.5614(4) 0.3546(3) 0.0298(7) Uani 1 1 d . . .
H7A H 0.5029 0.5581 0.3061 0.045 Uiso 1 1 calc R . .
H7B H 0.4790 0.6554 0.3755 0.045 Uiso 1 1 calc R . .
H7C H 0.4349 0.5341 0.3438 0.045 Uiso 1 1 calc R . .
C8 C 0.46531(19) 0.4630(4) 0.4874(2) 0.0319(9) Uani 1 1 d . . .
H8A H 0.4678 0.5532 0.5129 0.048 Uiso 1 1 calc R . .
H8B H 0.4798 0.3914 0.5235 0.048 Uiso 1 1 calc R . .
H8C H 0.4217 0.4443 0.4724 0.048 Uiso 1 1 calc R . .
C9 C 0.73581(19) 0.5723(4) 0.6367(2) 0.0293(8) Uani 1 1 d . . .
H9A H 0.7801 0.5990 0.6407 0.044 Uiso 1 1 calc R . .
H9B H 0.7317 0.4732 0.6466 0.044 Uiso 1 1 calc R . .
H9C H 0.7112 0.6236 0.6754 0.044 Uiso 1 1 calc R . .
C10 C 0.70706(18) 0.7552(3) 0.5470(2) 0.0296(8) Uani 1 1 d . . .
H10A H 0.7488 0.7970 0.5516 0.044 Uiso 1 1 calc R . .
H10B H 0.6794 0.7930 0.5874 0.044 Uiso 1 1 calc R . .
H10C H 0.6896 0.7758 0.4953 0.044 Uiso 1 1 calc R . .
C11 C 0.64659(18) 0.3212(3) 0.2591(2) 0.0306(9) Uani 1 1 d . . .
H11A H 0.6108 0.2624 0.2451 0.046 Uiso 1 1 calc R . .
H11B H 0.6613 0.2973 0.3116 0.046 Uiso 1 1 calc R . .
H11C H 0.6807 0.3070 0.2215 0.046 Uiso 1 1 calc R . .
C12 C 0.6062(2) 0.5052(4) 0.1801(2) 0.0279(9) Uani 1 1 d . . .
H12A H 0.6399 0.4881 0.1423 0.042 Uiso 1 1 calc R . .
H12B H 0.5955 0.6035 0.1800 0.042 Uiso 1 1 calc R . .
H12C H 0.5691 0.4511 0.1657 0.042 Uiso 1 1 calc R . .
C13 C 0.60310(17) 0.8885(3) 0.3173(2) 0.0240(7) Uani 1 1 d . . .
C14 C 0.53120(19) 0.9064(4) 0.3189(3) 0.0407(11) Uani 1 1 d . . .
H14A H 0.5122 0.8498 0.2778 0.061 Uiso 1 1 calc R . .
H14B H 0.5206 1.0035 0.3100 0.061 Uiso 1 1 calc R . .
H14C H 0.5150 0.8773 0.3699 0.061 Uiso 1 1 calc R . .
C15 C 0.6277(3) 0.9293(4) 0.2366(3) 0.0457(12) Uani 1 1 d . . .
H15A H 0.6071 0.8727 0.1966 0.069 Uiso 1 1 calc R . .
H15B H 0.6732 0.9144 0.2345 0.069 Uiso 1 1 calc R . .
H15C H 0.6185 1.0268 0.2269 0.069 Uiso 1 1 calc R . .
C16 C 0.6310(2) 0.9817(4) 0.3815(3) 0.0372(11) Uani 1 1 d . . .
H16A H 0.6770 0.9771 0.3795 0.056 Uiso 1 1 calc R . .
H16B H 0.6164 0.9501 0.4328 0.056 Uiso 1 1 calc R . .
H16C H 0.6174 1.0770 0.3730 0.056 Uiso 1 1 calc R . .
C17 C 0.5824(2) 0.6609(4) 0.6749(2) 0.0359(9) Uani 1 1 d . . .
H17A H 0.5406 0.6687 0.6987 0.054 Uiso 1 1 calc R . .
H17B H 0.6066 0.7446 0.6859 0.054 Uiso 1 1 calc R . .
H17C H 0.6043 0.5808 0.6968 0.054 Uiso 1 1 calc R . .
C18 C 0.54207(19) 0.7614(4) 0.5585(2) 0.0332(9) Uani 1 1 d . . .
H18A H 0.4994 0.7636 0.5800 0.050 Uiso 1 1 calc R . .
H18B H 0.5400 0.7531 0.5015 0.050 Uiso 1 1 calc R . .
H18C H 0.5641 0.8466 0.5724 0.050 Uiso 1 1 calc R . .
C19 C 0.54958(19) 0.3176(4) 0.6472(2) 0.0328(9) Uani 1 1 d . . .
H19A H 0.5130 0.2625 0.6318 0.049 Uiso 1 1 calc R . .
H19B H 0.5360 0.4114 0.6602 0.049 Uiso 1 1 calc R . .
H19C H 0.5696 0.2757 0.6929 0.049 Uiso 1 1 calc R . .
C20 C 0.60896(18) 0.1828(4) 0.5566(2) 0.0280(8) Uani 1 1 d . . .
H20A H 0.6270 0.1305 0.6002 0.042 Uiso 1 1 calc R . .
H20B H 0.6392 0.1860 0.5135 0.042 Uiso 1 1 calc R . .
H20C H 0.5702 0.1378 0.5390 0.042 Uiso 1 1 calc R . .
C21 C 0.77754(19) 0.1796(4) 0.4981(2) 0.0378(10) Uani 1 1 d . . .
H21A H 0.8198 0.1392 0.4979 0.057 Uiso 1 1 calc R . .
H21B H 0.7464 0.1073 0.4881 0.057 Uiso 1 1 calc R . .
H21C H 0.7693 0.2218 0.5491 0.057 Uiso 1 1 calc R . .
C22 C 0.79020(19) 0.2256(4) 0.3618(3) 0.0357(9) Uani 1 1 d . . .
H22A H 0.7653 0.1422 0.3525 0.054 Uiso 1 1 calc R . .
H22B H 0.8350 0.2020 0.3616 0.054 Uiso 1 1 calc R . .
H22D H 0.7817 0.2929 0.3204 0.054 Uiso 1 1 calc R . .
C23 C 0.86376(18) 0.6677(5) 0.5273(3) 0.0485(12) Uani 1 1 d . . .
H23A H 0.8783 0.6596 0.5814 0.073 Uiso 1 1 calc R . .
H23D H 0.8300 0.7362 0.5244 0.073 Uiso 1 1 calc R . .
H23B H 0.8988 0.6969 0.4939 0.073 Uiso 1 1 calc R . .
C24 C 0.8939(2) 0.4371(5) 0.4983(3) 0.0417(11) Uani 1 1 d . . .
H24D H 0.9112 0.4269 0.5511 0.063 Uiso 1 1 calc R . .
H24A H 0.9264 0.4733 0.4633 0.063 Uiso 1 1 calc R . .
H24B H 0.8796 0.3471 0.4793 0.063 Uiso 1 1 calc 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
Ta1 0.01301(5) 0.01561(5) 0.01241(6) 0.00056(5) 0.00083(6) -0.00058(4)
Ta2 0.01208(6) 0.01933(5) 0.01184(6) 0.00027(5) 0.00044(6) -0.00015(5)
Ta3 0.01122(6) 0.02492(6) 0.01647(7) 0.00175(6) 0.00023(5) -0.00022(5)
N1 0.0158(12) 0.0255(14) 0.0190(15) 0.0045(12) 0.0037(14) -0.0017(10)
N2 0.0100(13) 0.0225(13) 0.0158(15) 0.0007(10) 0.0000(12) -0.0011(10)
N3 0.0197(15) 0.0262(14) 0.0196(15) -0.0005(11) -0.0055(12) -0.0034(12)
N4 0.0234(15) 0.0192(12) 0.0157(16) -0.0004(11) -0.0002(12) 0.0034(11)
N5 0.0224(14) 0.0149(12) 0.0195(16) 0.0010(10) 0.0015(10) -0.0004(10)
N6 0.0191(14) 0.0282(14) 0.0194(15) -0.0043(12) 0.0015(12) 0.0016(12)
N7 0.0172(14) 0.0263(14) 0.0192(15) 0.0012(11) 0.0018(12) -0.0020(11)
N8 0.0204(15) 0.0283(14) 0.0265(17) 0.0026(12) 0.0055(12) 0.0054(12)
N9 0.0139(16) 0.0498(19) 0.0316(19) -0.0026(15) -0.0033(14) -0.0029(14)
C1 0.0167(17) 0.0366(19) 0.028(2) 0.0111(16) 0.0048(15) -0.0009(15)
C2 0.019(2) 0.072(3) 0.039(3) 0.022(2) 0.0123(18) 0.004(2)
C3 0.028(2) 0.061(3) 0.024(2) 0.014(2) 0.0124(17) -0.0009(19)
C4 0.034(2) 0.042(2) 0.054(3) 0.0090(19) 0.007(2) -0.0163(18)
C5 0.0114(16) 0.0262(15) 0.026(2) 0.0023(14) -0.0036(14) -0.0027(13)
C6 0.0264(19) 0.0308(17) 0.036(2) -0.0041(15) -0.0044(15) -0.0064(15)
C7 0.0183(16) 0.0381(18) 0.033(2) 0.0113(19) -0.007(2) -0.0034(14)
C8 0.0186(19) 0.050(2) 0.027(2) -0.0012(17) 0.0005(16) -0.0069(17)
C9 0.027(2) 0.042(2) 0.019(2) 0.0013(16) -0.0090(16) -0.0061(16)
C10 0.0250(18) 0.0276(16) 0.036(2) -0.0033(15) -0.0012(16) -0.0052(15)
C11 0.040(2) 0.0202(16) 0.032(2) -0.0070(15) -0.0041(17) 0.0045(15)
C12 0.035(2) 0.0313(19) 0.017(2) -0.0006(15) -0.0050(18) 0.0023(16)
C13 0.0279(19) 0.0192(15) 0.0249(19) 0.0035(14) 0.0028(15) 0.0033(14)
C14 0.032(2) 0.0238(17) 0.066(3) 0.0049(18) -0.008(2) 0.0083(16)
C15 0.081(4) 0.0253(19) 0.031(3) 0.0117(17) 0.019(2) 0.007(2)
C16 0.045(3) 0.0210(17) 0.046(3) -0.0012(16) -0.008(2) -0.0039(16)
C17 0.034(2) 0.051(2) 0.023(2) -0.0086(18) 0.0023(17) 0.0024(19)
C18 0.028(2) 0.0303(18) 0.041(2) -0.0047(17) 0.0004(17) 0.0075(16)
C19 0.030(2) 0.040(2) 0.028(2) 0.0106(16) 0.0096(17) 0.0037(17)
C20 0.0264(19) 0.0260(16) 0.032(2) 0.0013(15) -0.0010(16) -0.0039(15)
C21 0.029(2) 0.043(2) 0.041(2) 0.0155(18) 0.0070(18) 0.0163(18)
C22 0.036(2) 0.0365(18) 0.035(2) -0.0001(19) 0.010(2) 0.0091(16)
C23 0.021(2) 0.065(3) 0.060(3) -0.013(3) -0.002(2) -0.0191(19)
C24 0.016(2) 0.068(3) 0.041(3) 0.009(2) -0.0011(18) 0.005(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
Ta1 N5 1.789(3) . ?
Ta1 N4 2.001(3) . ?
Ta1 N2 2.076(3) . ?
Ta1 N1 2.114(3) . ?
Ta1 Ta2 3.0950(15) . ?
Ta1 Ta3 3.1190(11) . ?
Ta2 N2 1.953(3) . ?
Ta2 N7 2.002(3) . ?
Ta2 N6 2.016(3) . ?
Ta2 N3 2.237(3) . ?
Ta2 Ta3 3.0173(13) . ?
Ta2 H1 1.95(4) . ?
Ta3 N1 1.930(3) . ?
Ta3 N8 1.994(3) . ?
Ta3 N9 2.034(3) . ?
Ta3 N3 2.191(3) . ?
Ta3 H1 1.86(4) . ?
N1 C1 1.505(4) . ?
N2 C5 1.498(4) . ?
N3 C10 1.476(4) . ?
N3 C9 1.489(5) . ?
N4 C12 1.453(5) . ?
N4 C11 1.455(4) . ?
N5 C13 1.454(4) . ?
N6 C18 1.455(5) . ?
N6 C17 1.462(5) . ?
N7 C20 1.457(5) . ?
N7 C19 1.470(5) . ?
N8 C22 1.458(5) . ?
N8 C21 1.459(4) . ?
N9 C23 1.468(6) . ?
N9 C24 1.479(5) . ?
C1 C3 1.511(5) . ?
C1 C2 1.530(5) . ?
C1 C4 1.534(5) . ?
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 C7 1.524(5) . ?
C5 C6 1.531(5) . ?
C5 C8 1.535(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
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 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.530(5) . ?
C13 C14 1.539(5) . ?
C13 C16 1.541(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
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 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
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 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22D 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23D 0.9800 . ?
C23 H23B 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?

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
N5 Ta1 N4 105.58(12) . . ?
N5 Ta1 N2 105.52(11) . . ?
N4 Ta1 N2 104.67(12) . . ?
N5 Ta1 N1 106.89(11) . . ?
N4 Ta1 N1 100.70(12) . . ?
N2 Ta1 N1 131.10(12) . . ?
N5 Ta1 Ta2 113.41(9) . . ?
N4 Ta1 Ta2 131.50(9) . . ?
N2 Ta1 Ta2 38.38(8) . . ?
N1 Ta1 Ta2 94.62(9) . . ?
N5 Ta1 Ta3 126.18(9) . . ?
N4 Ta1 Ta3 117.49(8) . . ?
N2 Ta1 Ta3 93.68(9) . . ?
N1 Ta1 Ta3 37.42(9) . . ?
Ta2 Ta1 Ta3 58.10(2) . . ?
N2 Ta2 N7 104.85(11) . . ?
N2 Ta2 N6 99.46(12) . . ?
N7 Ta2 N6 103.04(12) . . ?
N2 Ta2 N3 128.08(11) . . ?
N7 Ta2 N3 123.08(11) . . ?
N6 Ta2 N3 88.84(12) . . ?
N2 Ta2 Ta3 99.52(9) . . ?
N7 Ta2 Ta3 112.87(8) . . ?
N6 Ta2 Ta3 133.00(8) . . ?
N3 Ta2 Ta3 46.40(8) . . ?
N2 Ta2 Ta1 41.30(8) . . ?
N7 Ta2 Ta1 132.26(8) . . ?
N6 Ta2 Ta1 113.42(9) . . ?
N3 Ta2 Ta1 88.39(8) . . ?
Ta3 Ta2 Ta1 61.349(10) . . ?
N2 Ta2 H1 109.2(11) . . ?
N7 Ta2 H1 76.4(11) . . ?
N6 Ta2 H1 150.6(11) . . ?
N3 Ta2 H1 68.4(11) . . ?
Ta3 Ta2 H1 36.4(11) . . ?
Ta1 Ta2 H1 85.4(11) . . ?
N1 Ta3 N8 104.20(13) . . ?
N1 Ta3 N9 106.78(13) . . ?
N8 Ta3 N9 96.48(13) . . ?
N1 Ta3 N3 111.47(12) . . ?
N8 Ta3 N3 140.50(11) . . ?
N9 Ta3 N3 89.17(13) . . ?
N1 Ta3 Ta2 101.25(8) . . ?
N8 Ta3 Ta2 109.76(8) . . ?
N9 Ta3 Ta2 135.19(10) . . ?
N3 Ta3 Ta2 47.70(7) . . ?
N1 Ta3 Ta1 41.73(8) . . ?
N8 Ta3 Ta1 108.10(9) . . ?
N9 Ta3 Ta1 143.41(10) . . ?
N3 Ta3 Ta1 88.61(8) . . ?
Ta2 Ta3 Ta1 60.55(3) . . ?
N1 Ta3 H1 126.0(11) . . ?
N8 Ta3 H1 74.6(11) . . ?
N9 Ta3 H1 127.2(11) . . ?
N3 Ta3 H1 71.0(11) . . ?
Ta2 Ta3 H1 38.6(11) . . ?
Ta1 Ta3 H1 86.2(11) . . ?
C1 N1 Ta3 133.6(2) . . ?
C1 N1 Ta1 125.0(2) . . ?
Ta3 N1 Ta1 100.85(13) . . ?
C5 N2 Ta2 131.9(2) . . ?
C5 N2 Ta1 127.7(2) . . ?
Ta2 N2 Ta1 100.32(12) . . ?
C10 N3 C9 109.7(3) . . ?
C10 N3 Ta3 119.4(2) . . ?
C9 N3 Ta3 115.3(2) . . ?
C10 N3 Ta2 111.9(2) . . ?
C9 N3 Ta2 112.6(2) . . ?
Ta3 N3 Ta2 85.90(10) . . ?
C12 N4 C11 111.1(3) . . ?
C12 N4 Ta1 132.4(2) . . ?
C11 N4 Ta1 116.1(2) . . ?
C13 N5 Ta1 178.0(3) . . ?
C18 N6 C17 109.3(3) . . ?
C18 N6 Ta2 126.7(2) . . ?
C17 N6 Ta2 123.0(2) . . ?
C20 N7 C19 109.4(3) . . ?
C20 N7 Ta2 126.3(2) . . ?
C19 N7 Ta2 123.7(2) . . ?
C22 N8 C21 110.1(3) . . ?
C22 N8 Ta3 128.4(2) . . ?
C21 N8 Ta3 121.4(2) . . ?
C23 N9 C24 107.7(3) . . ?
C23 N9 Ta3 129.7(3) . . ?
C24 N9 Ta3 122.4(3) . . ?
N1 C1 C3 111.5(3) . . ?
N1 C1 C2 111.3(3) . . ?
C3 C1 C2 109.2(3) . . ?
N1 C1 C4 107.3(3) . . ?
C3 C1 C4 108.7(3) . . ?
C2 C1 C4 108.8(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C7 110.8(3) . . ?
N2 C5 C6 108.1(3) . . ?
C7 C5 C6 108.9(3) . . ?
N2 C5 C8 111.8(3) . . ?
C7 C5 C8 108.4(3) . . ?
C6 C5 C8 108.9(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 C15 108.9(3) . . ?
N5 C13 C14 111.0(3) . . ?
C15 C13 C14 109.0(4) . . ?
N5 C13 C16 109.1(3) . . ?
C15 C13 C16 111.2(3) . . ?
C14 C13 C16 107.7(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N6 C17 H17A 109.5 . . ?
N6 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N6 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N6 C18 H18A 109.5 . . ?
N6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C19 H19A 109.5 . . ?
N7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N7 C20 H20A 109.5 . . ?
N7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N8 C21 H21A 109.5 . . ?
N8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C22 H22A 109.5 . . ?
N8 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N8 C22 H22D 109.5 . . ?
H22A C22 H22D 109.5 . . ?
H22B C22 H22D 109.5 . . ?
N9 C23 H23A 109.5 . . ?
N9 C23 H23D 109.5 . . ?
H23A C23 H23D 109.5 . . ?
N9 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23D C23 H23B 109.5 . . ?
N9 C24 H24D 109.5 . . ?
N9 C24 H24A 109.5 . . ?
H24D C24 H24A 109.5 . . ?
N9 C24 H24B 109.5 . . ?
H24D C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         0.897
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.096

#===END

# Attachment '4125_web_deposit_cif_file_1_Shu-JianChen_1297046362.cif'

data_4
_database_code_depnum_ccdc_archive 'CCDC 811903'
#TrackingRef '4125_web_deposit_cif_file_1_Shu-JianChen_1297046362.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Tantalum oxo hydride
;
_chemical_name_common            'Tantalum oxo hydride'
_chemical_melting_point          ?
_chemical_formula_moiety         C24H64N9OTa3
_chemical_formula_sum            C24H64N9OTa3
_chemical_formula_weight         1037.69

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'
Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhomic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   9.289(4)
_cell_length_b                   17.389(7)
_cell_length_c                   23.143(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3738(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       fragment
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    8.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1269
_exptl_absorpt_correction_T_max  0.2724
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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       multi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38925
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8559
_reflns_number_gt                8314
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^)+(0.0561P)^2^+18.8072P] 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     SHELXL
_refine_ls_extinction_coef       0.00023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(2)
_refine_ls_number_reflns         8559
_refine_ls_number_parameters     345
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.1082
_refine_ls_wR_factor_gt          0.1076
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.416
_refine_ls_shift/su_mean         0.025

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
Ta1 Ta 0.59090(4) 0.952344(19) 0.030927(14) 0.02773(9) Uani 1 1 d . . .
Ta2 Ta 0.69769(4) 1.087811(19) 0.102672(16) 0.03042(10) Uani 1 1 d . . .
Ta3 Ta 0.60839(4) 0.943639(18) 0.179619(14) 0.02815(9) Uani 1 1 d . . .
O1 O 0.7240(6) 0.9744(3) 0.1062(3) 0.0295(12) Uani 1 1 d . . .
N1 N 0.7243(9) 1.0545(5) 0.0087(3) 0.0398(18) Uani 1 1 d . . .
N2 N 0.4829(8) 0.8942(5) 0.1049(3) 0.0339(16) Uani 1 1 d . . .
N3 N 0.6924(9) 1.0586(4) 0.1959(3) 0.0355(16) Uani 1 1 d . . .
N4 N 0.4521(8) 0.9541(5) -0.0223(3) 0.0361(17) Uani 1 1 d . A .
N5 N 0.7128(9) 0.8677(5) 0.0014(3) 0.0381(18) Uani 1 1 d . . .
N6 N 0.5930(11) 1.1874(5) 0.0912(4) 0.045(2) Uani 1 1 d . . .
N7 N 0.9026(10) 1.1245(5) 0.1039(4) 0.050(2) Uani 1 1 d . . .
N8 N 0.4443(11) 0.9417(5) 0.2361(4) 0.050(2) Uani 1 1 d . . .
N9 N 0.7228(10) 0.8692(4) 0.2072(3) 0.0354(17) Uani 1 1 d . B .
C1 C 0.8697(13) 1.0301(8) -0.0093(5) 0.056(3) Uani 1 1 d . . .
H1A H 0.9262 1.0754 -0.0204 0.084 Uiso 1 1 calc R . .
H1B H 0.8622 0.9950 -0.0422 0.084 Uiso 1 1 calc R . .
H1C H 0.9172 1.0038 0.0230 0.084 Uiso 1 1 calc R . .
C2 C 0.6617(16) 1.1100(8) -0.0324(5) 0.060(3) Uani 1 1 d . . .
H2A H 0.6655 1.0885 -0.0715 0.089 Uiso 1 1 calc R . .
H2B H 0.7166 1.1580 -0.0311 0.089 Uiso 1 1 calc R . .
H2C H 0.5613 1.1201 -0.0218 0.089 Uiso 1 1 calc R . .
C3 C 0.3260(10) 0.9102(10) 0.1076(5) 0.066(4) Uani 1 1 d . . .
H3A H 0.2889 0.8955 0.1456 0.099 Uiso 1 1 calc R . .
H3B H 0.2764 0.8805 0.0776 0.099 Uiso 1 1 calc R . .
H3C H 0.3092 0.9652 0.1012 0.099 Uiso 1 1 calc R . .
C4 C 0.4970(14) 0.8112(6) 0.1026(5) 0.053(3) Uani 1 1 d . . .
H4C H 0.4527 0.7920 0.0670 0.080 Uiso 1 1 calc R . .
H4D H 0.4486 0.7883 0.1360 0.080 Uiso 1 1 calc R . .
H4E H 0.5992 0.7973 0.1031 0.080 Uiso 1 1 calc R . .
C5 C 0.7044(14) 1.1081(6) 0.2497(5) 0.047(2) Uani 1 1 d . . .
C6 C 0.8394(17) 1.0819(8) 0.2808(6) 0.072(4) Uani 1 1 d . . .
H6A H 0.9234 1.0913 0.2562 0.108 Uiso 1 1 calc R . .
H6B H 0.8323 1.0269 0.2893 0.108 Uiso 1 1 calc R . .
H6C H 0.8497 1.1107 0.3170 0.108 Uiso 1 1 calc R . .
C7 C 0.5731(19) 1.0994(8) 0.2881(5) 0.067(4) Uani 1 1 d . . .
H7A H 0.5600 1.0450 0.2980 0.100 Uiso 1 1 calc R . .
H7B H 0.4878 1.1181 0.2675 0.100 Uiso 1 1 calc R . .
H7C H 0.5868 1.1294 0.3235 0.100 Uiso 1 1 calc R . .
C8 C 0.7249(16) 1.1910(7) 0.2325(6) 0.060(3) Uani 1 1 d . . .
H8A H 0.6396 1.2089 0.2115 0.090 Uiso 1 1 calc R . .
H8B H 0.8098 1.1955 0.2076 0.090 Uiso 1 1 calc R . .
H8C H 0.7385 1.2224 0.2672 0.090 Uiso 1 1 calc R . .
C9 C 0.3305(10) 0.9680(6) -0.0605(4) 0.051(3) Uani 1 1 d D . .
C10 C 0.232(2) 1.0264(10) -0.0313(9) 0.054(4) Uiso 0.57(2) 1 d PD A 1
H10A H 0.1909 1.0038 0.0038 0.082 Uiso 0.57(2) 1 calc PR A 1
H10B H 0.1540 1.0406 -0.0578 0.082 Uiso 0.57(2) 1 calc PR A 1
H10C H 0.2874 1.0724 -0.0212 0.082 Uiso 0.57(2) 1 calc PR A 1
C11 C 0.243(3) 0.8986(10) -0.0769(11) 0.078(6) Uiso 0.57(2) 1 d PD A 1
H11A H 0.2056 0.8740 -0.0419 0.117 Uiso 0.57(2) 1 calc PR A 1
H11B H 0.3034 0.8622 -0.0981 0.117 Uiso 0.57(2) 1 calc PR A 1
H11C H 0.1621 0.9146 -0.1014 0.117 Uiso 0.57(2) 1 calc PR A 1
C12 C 0.386(2) 1.0061(13) -0.1160(7) 0.069(5) Uiso 0.57(2) 1 d PD A 1
H12A H 0.4522 1.0477 -0.1060 0.104 Uiso 0.57(2) 1 calc PR A 1
H12B H 0.3040 1.0271 -0.1377 0.104 Uiso 0.57(2) 1 calc PR A 1
H12C H 0.4355 0.9678 -0.1397 0.104 Uiso 0.57(2) 1 calc PR A 1
C10B C 0.255(3) 1.0440(10) -0.0536(12) 0.054(4) Uiso 0.43(2) 1 d PD A 2
H10D H 0.1966 1.0431 -0.0185 0.082 Uiso 0.43(2) 1 calc PR A 2
H10E H 0.1934 1.0533 -0.0872 0.082 Uiso 0.43(2) 1 calc PR A 2
H10F H 0.3271 1.0851 -0.0508 0.082 Uiso 0.43(2) 1 calc PR A 2
C11B C 0.220(3) 0.9039(13) -0.0496(14) 0.078(6) Uiso 0.43(2) 1 d PD A 2
H11D H 0.2093 0.8957 -0.0079 0.117 Uiso 0.43(2) 1 calc PR A 2
H11E H 0.2522 0.8563 -0.0679 0.117 Uiso 0.43(2) 1 calc PR A 2
H11F H 0.1264 0.9191 -0.0659 0.117 Uiso 0.43(2) 1 calc PR A 2
C12B C 0.379(3) 0.9596(17) -0.1229(7) 0.069(5) Uiso 0.43(2) 1 d PD A 2
H12D H 0.3709 0.9057 -0.1348 0.104 Uiso 0.43(2) 1 calc PR A 2
H12E H 0.4800 0.9760 -0.1263 0.104 Uiso 0.43(2) 1 calc PR A 2
H12F H 0.3189 0.9917 -0.1479 0.104 Uiso 0.43(2) 1 calc PR A 2
C13 C 0.8461(12) 0.8404(7) 0.0261(6) 0.056(3) Uani 1 1 d . . .
H13A H 0.9251 0.8500 -0.0011 0.084 Uiso 1 1 calc R . .
H13B H 0.8387 0.7851 0.0336 0.084 Uiso 1 1 calc R . .
H13C H 0.8650 0.8676 0.0624 0.084 Uiso 1 1 calc R . .
C14 C 0.6838(15) 0.8201(7) -0.0505(5) 0.056(3) Uani 1 1 d . . .
H14A H 0.6715 0.7662 -0.0390 0.084 Uiso 1 1 calc R . .
H14B H 0.7649 0.8242 -0.0774 0.084 Uiso 1 1 calc R . .
H14C H 0.5958 0.8383 -0.0695 0.084 Uiso 1 1 calc R . .
C15 C 0.4300(17) 1.1936(9) 0.0850(7) 0.075(4) Uani 1 1 d . . .
H15A H 0.4039 1.1907 0.0440 0.113 Uiso 1 1 calc R . .
H15B H 0.3974 1.2428 0.1010 0.113 Uiso 1 1 calc R . .
H15C H 0.3840 1.1513 0.1060 0.113 Uiso 1 1 calc R . .
C16 C 0.6619(18) 1.2645(6) 0.0846(6) 0.062(4) Uani 1 1 d . . .
H16A H 0.6158 1.3012 0.1110 0.094 Uiso 1 1 calc R . .
H16B H 0.6505 1.2824 0.0447 0.094 Uiso 1 1 calc R . .
H16C H 0.7646 1.2607 0.0939 0.094 Uiso 1 1 calc R . .
C17 C 0.9868(19) 1.1732(10) 0.0659(7) 0.084(5) Uani 1 1 d . . .
H17A H 1.0786 1.1481 0.0571 0.125 Uiso 1 1 calc R . .
H17B H 1.0050 1.2226 0.0849 0.125 Uiso 1 1 calc R . .
H17C H 0.9335 1.1819 0.0299 0.125 Uiso 1 1 calc R . .
C18 C 1.0101(15) 1.0861(9) 0.1458(6) 0.074(4) Uani 1 1 d . . .
H18A H 1.0762 1.1250 0.1611 0.111 Uiso 1 1 calc R . .
H18B H 1.0651 1.0466 0.1252 0.111 Uiso 1 1 calc R . .
H18C H 0.9573 1.0623 0.1778 0.111 Uiso 1 1 calc R . .
C19 C 0.3154(15) 0.9871(8) 0.2339(6) 0.060(3) Uani 1 1 d . . .
H19A H 0.3016 1.0133 0.2709 0.089 Uiso 1 1 calc R . .
H19B H 0.2327 0.9536 0.2262 0.089 Uiso 1 1 calc R . .
H19C H 0.3238 1.0254 0.2030 0.089 Uiso 1 1 calc R . .
C20 C 0.4322(17) 0.8881(8) 0.2868(5) 0.064(4) Uani 1 1 d . . .
H20A H 0.3352 0.8660 0.2880 0.096 Uiso 1 1 calc R . .
H20B H 0.4503 0.9166 0.3226 0.096 Uiso 1 1 calc R . .
H20C H 0.5032 0.8467 0.2829 0.096 Uiso 1 1 calc R . .
C21 C 0.8322(12) 0.8178(5) 0.2287(4) 0.052(3) Uani 1 1 d D . .
C22 C 0.765(2) 0.7381(8) 0.2355(8) 0.062(5) Uiso 0.678(19) 1 d PD B 1
H22A H 0.7460 0.7162 0.1973 0.094 Uiso 0.678(19) 1 calc PR B 1
H22B H 0.6751 0.7423 0.2572 0.094 Uiso 0.678(19) 1 calc PR B 1
H22C H 0.8322 0.7046 0.2565 0.094 Uiso 0.678(19) 1 calc PR B 1
C23 C 0.891(2) 0.8429(12) 0.2869(6) 0.077(6) Uiso 0.678(19) 1 d PD B 1
H23A H 0.9675 0.8810 0.2811 0.116 Uiso 0.678(19) 1 calc PR B 1
H23B H 0.9305 0.7982 0.3073 0.116 Uiso 0.678(19) 1 calc PR B 1
H23C H 0.8136 0.8657 0.3099 0.116 Uiso 0.678(19) 1 calc PR B 1
C24 C 0.958(2) 0.8104(13) 0.1865(8) 0.083(6) Uiso 0.678(19) 1 d PD B 1
H24A H 0.9215 0.8136 0.1468 0.124 Uiso 0.678(19) 1 calc PR B 1
H24B H 1.0056 0.7608 0.1922 0.124 Uiso 0.678(19) 1 calc PR B 1
H24C H 1.0266 0.8522 0.1933 0.124 Uiso 0.678(19) 1 calc PR B 1
C22B C 0.819(5) 0.7362(11) 0.2071(15) 0.062(5) Uiso 0.322(19) 1 d PD B 2
H22D H 0.8189 0.7360 0.1648 0.094 Uiso 0.322(19) 1 calc PR B 2
H22E H 0.7293 0.7136 0.2214 0.094 Uiso 0.322(19) 1 calc PR B 2
H22F H 0.9009 0.7059 0.2212 0.094 Uiso 0.322(19) 1 calc PR B 2
C23B C 0.827(5) 0.817(2) 0.2947(6) 0.077(6) Uiso 0.322(19) 1 d PD B 2
H23D H 0.8678 0.8653 0.3095 0.116 Uiso 0.322(19) 1 calc PR B 2
H23E H 0.8834 0.7737 0.3092 0.116 Uiso 0.322(19) 1 calc PR B 2
H23F H 0.7271 0.8123 0.3075 0.116 Uiso 0.322(19) 1 calc PR B 2
C24B C 0.976(3) 0.851(2) 0.2100(18) 0.083(6) Uiso 0.322(19) 1 d PD B 2
H24D H 0.9797 0.8535 0.1678 0.124 Uiso 0.322(19) 1 calc PR B 2
H24E H 1.0539 0.8179 0.2242 0.124 Uiso 0.322(19) 1 calc PR B 2
H24F H 0.9871 0.9027 0.2261 0.124 Uiso 0.322(19) 1 calc PR B 2
H1 H 0.517(9) 1.053(5) 0.076(3) 0.007(19) Uiso 1 1 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
Ta1 0.02670(16) 0.03279(17) 0.02370(15) -0.00396(12) -0.00123(12) 0.00676(13)
Ta2 0.03649(18) 0.02395(16) 0.03081(17) 0.00385(14) -0.00156(15) -0.00219(14)
Ta3 0.03719(18) 0.02357(15) 0.02368(15) 0.00105(11) -0.00247(13) -0.00315(13)
O1 0.027(3) 0.025(3) 0.036(3) 0.000(2) 0.004(2) 0.002(2)
N1 0.040(4) 0.044(4) 0.036(4) 0.004(3) 0.009(3) -0.003(4)
N2 0.031(4) 0.040(4) 0.030(3) -0.006(3) -0.008(3) -0.004(3)
N3 0.042(4) 0.021(3) 0.043(4) -0.009(3) -0.006(3) -0.004(3)
N4 0.035(4) 0.050(5) 0.023(3) -0.004(3) -0.004(3) 0.018(3)
N5 0.036(4) 0.043(4) 0.035(4) 0.001(3) 0.006(3) 0.016(4)
N6 0.064(6) 0.028(4) 0.043(5) 0.004(3) 0.002(4) 0.011(4)
N7 0.051(5) 0.040(4) 0.059(5) 0.006(4) 0.002(5) -0.020(4)
N8 0.065(6) 0.037(4) 0.047(5) 0.013(4) 0.010(4) 0.008(4)
N9 0.054(5) 0.022(3) 0.031(4) 0.009(3) -0.012(3) 0.000(3)
C1 0.044(6) 0.075(8) 0.049(6) 0.004(6) 0.017(5) 0.002(6)
C2 0.080(9) 0.064(7) 0.035(5) 0.012(5) -0.005(6) -0.003(6)
C3 0.025(5) 0.124(12) 0.048(6) -0.016(8) 0.009(4) -0.016(6)
C4 0.065(7) 0.043(5) 0.052(6) -0.010(5) -0.001(6) -0.024(5)
C5 0.062(7) 0.033(5) 0.046(6) -0.013(4) -0.006(5) -0.003(5)
C6 0.097(11) 0.063(8) 0.058(7) -0.021(6) -0.051(7) 0.007(8)
C7 0.112(12) 0.060(7) 0.029(5) -0.017(5) 0.015(6) -0.021(8)
C8 0.077(9) 0.038(6) 0.066(7) -0.015(5) -0.014(7) -0.001(6)
C9 0.040(5) 0.084(8) 0.028(4) -0.008(5) -0.010(4) 0.019(5)
C13 0.041(6) 0.052(6) 0.074(8) -0.013(6) -0.008(6) 0.020(5)
C14 0.069(8) 0.047(6) 0.052(6) -0.014(5) -0.004(6) 0.034(6)
C15 0.077(10) 0.056(8) 0.094(11) -0.006(7) -0.012(8) 0.024(7)
C16 0.100(11) 0.020(4) 0.068(8) 0.004(4) -0.009(7) -0.004(5)
C17 0.087(11) 0.088(11) 0.076(9) 0.006(8) 0.019(9) -0.049(10)
C18 0.054(7) 0.084(10) 0.084(9) -0.034(8) -0.017(7) -0.020(7)
C19 0.062(7) 0.054(7) 0.063(7) -0.001(6) 0.022(6) -0.004(6)
C20 0.088(10) 0.060(7) 0.044(6) 0.024(5) 0.018(6) -0.013(7)
C21 0.056(7) 0.037(5) 0.062(7) 0.007(5) -0.018(5) 0.012(5)

_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
Ta1 N4 1.784(7) . ?
Ta1 N5 1.978(8) . ?
Ta1 O1 2.170(6) . ?
Ta1 N1 2.227(9) . ?
Ta1 N2 2.227(8) . ?
Ta2 H1 1.89(8) . ?
Ta2 O1 1.989(6) . ?
Ta2 N6 2.003(8) . ?
Ta2 N7 2.008(9) . ?
Ta2 N3 2.217(8) . ?
Ta2 N1 2.265(8) . ?
Ta3 N9 1.793(8) . ?
Ta3 N8 2.008(10) . ?
Ta3 O1 2.080(6) . ?
Ta3 N3 2.180(7) . ?
Ta3 N2 2.256(7) . ?
N1 C1 1.475(14) . ?
N1 C2 1.473(14) . ?
N2 C4 1.449(14) . ?
N2 C3 1.485(13) . ?
N3 C5 1.517(12) . ?
N4 C9 1.455(11) . ?
N5 C13 1.444(13) . ?
N5 C14 1.485(13) . ?
N6 C16 1.494(14) . ?
N6 C15 1.525(18) . ?
N7 C17 1.450(15) . ?
N7 C18 1.545(18) . ?
N8 C19 1.435(16) . ?
N8 C20 1.503(13) . ?
N9 C21 1.441(12) . ?
C5 C8 1.508(16) . ?
C5 C6 1.516(18) . ?
C5 C7 1.516(19) . ?
C9 C10B 1.504(9) . ?
C9 C11 1.504(9) . ?
C9 C12B 1.520(9) . ?
C9 C10 1.526(9) . ?
C9 C12 1.532(9) . ?
C9 C11B 1.538(10) . ?
C21 C22B 1.510(10) . ?
C21 C23 1.518(9) . ?
C21 C24B 1.516(10) . ?
C21 C24 1.527(9) . ?
C21 C22 1.528(9) . ?
C21 C23B 1.527(10) . ?

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
N4 Ta1 N5 100.8(3) . . ?
N4 Ta1 O1 164.4(3) . . ?
N5 Ta1 O1 94.7(3) . . ?
N4 Ta1 N1 103.2(4) . . ?
N5 Ta1 N1 101.2(3) . . ?
O1 Ta1 N1 74.2(3) . . ?
N4 Ta1 N2 102.3(3) . . ?
N5 Ta1 N2 100.7(3) . . ?
O1 Ta1 N2 73.7(2) . . ?
N1 Ta1 N2 142.3(3) . . ?
H1 Ta2 O1 79(3) . . ?
H1 Ta2 N6 79(3) . . ?
O1 Ta2 N6 157.2(3) . . ?
H1 Ta2 N7 162(2) . . ?
O1 Ta2 N7 101.4(3) . . ?
N6 Ta2 N7 100.8(4) . . ?
H1 Ta2 N3 103(2) . . ?
O1 Ta2 N3 74.7(3) . . ?
N6 Ta2 N3 108.4(3) . . ?
N7 Ta2 N3 94.6(4) . . ?
H1 Ta2 N1 73(2) . . ?
O1 Ta2 N1 76.9(3) . . ?
N6 Ta2 N1 98.4(3) . . ?
N7 Ta2 N1 89.5(4) . . ?
N3 Ta2 N1 151.5(3) . . ?
N9 Ta3 N8 101.9(4) . . ?
N9 Ta3 O1 99.8(3) . . ?
N8 Ta3 O1 158.1(3) . . ?
N9 Ta3 N3 112.9(3) . . ?
N8 Ta3 N3 100.1(4) . . ?
O1 Ta3 N3 73.8(3) . . ?
N9 Ta3 N2 107.7(3) . . ?
N8 Ta3 N2 95.7(4) . . ?
O1 Ta3 N2 74.8(3) . . ?
N3 Ta3 N2 131.9(3) . . ?
Ta2 O1 Ta3 103.0(3) . . ?
Ta2 O1 Ta1 94.1(2) . . ?
Ta3 O1 Ta1 108.4(2) . . ?
C1 N1 C2 111.6(9) . . ?
C1 N1 Ta1 110.2(7) . . ?
C2 N1 Ta1 116.8(7) . . ?
C1 N1 Ta2 116.3(7) . . ?
C2 N1 Ta2 114.1(7) . . ?
Ta1 N1 Ta2 85.5(3) . . ?
C4 N2 C3 106.1(9) . . ?
C4 N2 Ta1 112.5(7) . . ?
C3 N2 Ta1 112.9(8) . . ?
C4 N2 Ta3 111.2(7) . . ?
C3 N2 Ta3 113.8(7) . . ?
Ta1 N2 Ta3 100.5(3) . . ?
C5 N3 Ta3 133.5(7) . . ?
C5 N3 Ta2 131.9(6) . . ?
Ta3 N3 Ta2 92.8(3) . . ?
C9 N4 Ta1 169.7(7) . . ?
C13 N5 C14 107.0(8) . . ?
C13 N5 Ta1 126.8(7) . . ?
C14 N5 Ta1 126.2(7) . . ?
C16 N6 C15 110.6(10) . . ?
C16 N6 Ta2 125.6(9) . . ?
C15 N6 Ta2 123.8(8) . . ?
C17 N7 C18 106.6(11) . . ?
C17 N7 Ta2 133.5(10) . . ?
C18 N7 Ta2 119.0(7) . . ?
C19 N8 C20 107.9(10) . . ?
C19 N8 Ta3 126.9(7) . . ?
C20 N8 Ta3 125.1(8) . . ?
C21 N9 Ta3 171.2(7) . . ?
N3 C5 C8 109.5(9) . . ?
N3 C5 C6 106.3(9) . . ?
C8 C5 C6 107.9(11) . . ?
N3 C5 C7 111.4(9) . . ?
C8 C5 C7 110.6(11) . . ?
C6 C5 C7 110.9(11) . . ?
N4 C9 C10B 116.2(13) . . ?
N4 C9 C11 116.2(14) . . ?
C10B C9 C11 118.7(17) . . ?
N4 C9 C12B 109.2(14) . . ?
C10B C9 C12B 108.9(9) . . ?
C11 C9 C12B 81.1(12) . . ?
N4 C9 C10 107.9(10) . . ?
C10B C9 C10 24.3(10) . . ?
C11 C9 C10 108.7(8) . . ?
C12B C9 C10 131.6(14) . . ?
N4 C9 C12 108.8(12) . . ?
C10B C9 C12 82.2(11) . . ?
C11 C9 C12 108.5(8) . . ?
C12B C9 C12 31.4(10) . . ?
C10 C9 C12 106.5(8) . . ?
N4 C9 C11B 107.4(15) . . ?
C10B C9 C11B 107.9(9) . . ?
C11 C9 C11B 25.6(12) . . ?
C12B C9 C11B 106.7(9) . . ?
C10 C9 C11B 90.4(12) . . ?
C12 C9 C11B 132.5(15) . . ?
N9 C21 C22B 114.3(17) . . ?
N9 C21 C23 112.5(12) . . ?
C22B C21 C23 126.3(18) . . ?
N9 C21 C24B 107(2) . . ?
C22B C21 C24B 109.4(10) . . ?
C23 C21 C24B 80.0(16) . . ?
N9 C21 C24 111.7(12) . . ?
C22B C21 C24 76.7(15) . . ?
C23 C21 C24 108.5(8) . . ?
C24B C21 C24 34.6(14) . . ?
N9 C21 C22 108.1(11) . . ?
C22B C21 C22 31.6(14) . . ?
C23 C21 C22 108.4(8) . . ?
C24B C21 C22 137.0(19) . . ?
C24 C21 C22 107.5(8) . . ?
N9 C21 C23B 109.1(19) . . ?
C22B C21 C23B 108.7(10) . . ?
C23 C21 C23B 29.1(15) . . ?
C24B C21 C23B 108.3(10) . . ?
C24 C21 C23B 132(2) . . ?
C22 C21 C23B 82.9(14) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         6.897
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.215

#===END