Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001
data_global
_journal_coden_Cambridge  186
_audit_creation_date            01-04-10
_publ_contact_letter
;
These are the CIF format data for the paper 

Surprising Diversity of Non-classical Silicon-Hydrogen Interactions in 
Half-sandwich Complexes of Nb and Ta: M-H...Si-Cl Interligand 
Hypervalent Interaction (IHI) versus Stretched and Unstretched 
\b Si-H...M Agostic Bonding

G. I. Nikonov, P. Mountford, S. K. Ignatov, J. C. Green, 
P. A. Cooke, M. A. Leech,
L. G. Kuzmina, A. G. Razuvaev, N. H. Rees, A. J. Blake, J. A. K. Howard
and D. A. Lemenovskii
;
_publ_contact_author
;
Dr P. Mountford           
Inorganic Chemistry Laboratory
South Parks Road
Oxford
OX1 3QR
UK
;                                           
_publ_contact_author_phone      '+44 1865 272679'
_publ_contact_author_fax             '+44 1865 272690'
_publ_contact_author_email      Philip.Mountford@chem.ox.ac.uk

loop_
_publ_author_name
'G. I. Nikonov'
'P. Mountford'
'S. K. Ignatov'
'J. C. Green' 
'P. A. Cooke'
'M. A. Leech'
'L. G. Kuzmina'
'A. G. Razuvaev'
'N. H. Rees'
'A. J. Blake'
'J. A. K. Howard'
'D. A. Lemenovskii'

data_COMPOUND_6

_database_code_CSD	164933

#  Local code NBIMISI

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
[NbCp{eta-3-N(Ar)SiMe2-H}Cl(PMe3)] 
; 
_chemical_name_common             
' CpNb{eta-3-N(Ar)SiMe2-H}Cl(PMe3) '
_chemical_formula_moiety          
' C22 H38 Cl N Nb P Si' 
_chemical_formula_sum 
' C22 H38 Cl N Nb P Si' 
_chemical_formula_weight          503.95 

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' 
'Si'  'Si'   0.0817   0.0704 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'P'  'P'   0.1023   0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Nb'  'Nb'  -2.0727   0.6215 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting                  monoclinic 
_symmetry_space_group_name_H-M          'C 1 2/c 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' 
'-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                    31.391(6) 
_cell_length_b                    10.150(2) 
_cell_length_c                    16.945(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  111.30(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5030.2(17) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     49 
_cell_measurement_theta_min       12 
_cell_measurement_theta_max       15.5 

_exptl_crystal_description        tablet
_exptl_crystal_colour             'dark green/brown'
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.17
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.331 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2112 
_exptl_absorpt_coefficient_mu     0.704 
_exptl_absorpt_correction_type    'psi scans' 
_exptl_absorpt_correction_T_min   0.721 
_exptl_absorpt_correction_T_max   0.913 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(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        'Stoe STADI4 4-circle diffractometer' 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        'omega  scans'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   '60 minutes' 
_diffrn_standards_decay_%         'random variation +/- 7%' 
_diffrn_reflns_number             4813 
_diffrn_reflns_av_R_equivalents   0.0343 
_diffrn_reflns_av_sigmaI/netI     0.0541 
_diffrn_reflns_limit_h_min        -37 
_diffrn_reflns_limit_h_max        36 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.58 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              4437 
_reflns_number_observed           3557 
_reflns_threshold_expression      >2sigma(I) 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 

_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 w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+46.1766P] 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        'none required'
_refine_ls_number_reflns          4437 
_refine_ls_number_parameters      313 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0685 
_refine_ls_R_factor_obs           0.0500 
_refine_ls_wR_factor_all          0.1152 
_refine_ls_wR_factor_obs          0.1031 
_refine_ls_goodness_of_fit_all    1.024 
_refine_ls_restrained_S_all       1.024 
_refine_ls_shift/esd_max           0.003 
_refine_ls_shift/esd_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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Nb1 Nb 0.083516(14) 0.22888(4) 0.50036(2) 0.01822(13) Uani 1 d . . . 
Si1 Si 0.15169(5) 0.39940(14) 0.53619(8) 0.0220(3) Uani 1 d . . . 
P1 P 0.10043(5) 0.03076(14) 0.42371(8) 0.0271(3) Uani 1 d . . . 
Cl1 Cl 0.07492(5) 0.06848(14) 0.60528(8) 0.0328(3) Uani 1 d . . . 
N1 N 0.13740(13) 0.2971(4) 0.6024(2) 0.0202(9) Uani 1 d . . . 
C1 C 0.01316(17) 0.1949(6) 0.3740(3) 0.0325(13) Uani 1 d . . . 
H1A H 0.0074(4) 0.126(5) 0.339(2) 0.040(17) Uiso 1 calc R . . 
C2 C 0.03697(18) 0.3100(6) 0.3674(3) 0.0313(13) Uani 1 d . . . 
H2A H 0.0494(8) 0.3249(11) 0.329(2) 0.031(15) Uiso 1 calc R . . 
C3 C 0.03751(17) 0.3977(6) 0.4330(3) 0.0285(12) Uani 1 d . . . 
H3A H 0.0490(7) 0.477(5) 0.4418(6) 0.017(13) Uiso 1 calc R . . 
C4 C 0.01557(16) 0.3305(6) 0.4815(3) 0.0291(12) Uani 1 d . . . 
H4A H 0.0122(3) 0.360(2) 0.527(3) 0.042(18) Uiso 1 calc R . . 
C5 C 0.00043(17) 0.2078(6) 0.4434(3) 0.0291(12) Uani 1 d . . . 
H5A H -0.0126(10) 0.157(4) 0.4585(12) 0.033(18) Uiso 1 calc R . . 
C6 C 0.15640(15) 0.2908(5) 0.6932(3) 0.0170(9) Uani 1 d . . . 
C7 C 0.19339(15) 0.2076(5) 0.7356(3) 0.0205(10) Uani 1 d . . . 
C8 C 0.21332(17) 0.2127(5) 0.8234(3) 0.0237(11) Uani 1 d . . . 
H8A H 0.2373(13) 0.160(3) 0.8504(15) 0.016(12) Uiso 1 calc R . . 
C9 C 0.19716(17) 0.2960(5) 0.8698(3) 0.0265(12) Uani 1 d . . . 
H9A H 0.2118(8) 0.3012(6) 0.929(3) 0.025(13) Uiso 1 calc R . . 
C10 C 0.15893(17) 0.3726(5) 0.8284(3) 0.0252(11) Uani 1 d . . . 
H10A H 0.1466(7) 0.427(3) 0.8613(19) 0.031(15) Uiso 1 calc R . . 
C12 C 0.09569(17) 0.4566(5) 0.7003(3) 0.0246(11) Uani 1 d . . . 
H12A H 0.0862(4) 0.4493(6) 0.633(3) 0.015(12) Uiso 1 calc R . . 
C13 C 0.10437(19) 0.6025(5) 0.7243(3) 0.0319(13) Uani 1 d . . . 
H13A H 0.0760(8) 0.6541(16) 0.6947(16) 0.023(13) Uiso 1 calc R . . 
H13B H 0.1296(9) 0.6358(13) 0.7070(17) 0.040(16) Uiso 1 calc R . . 
H13C H 0.1132(10) 0.6125(7) 0.7867(17) 0.021(13) Uiso 1 calc R . . 
C14 C 0.05601(17) 0.4024(6) 0.7231(3) 0.0348(13) Uani 1 d . . . 
H14C H 0.0495(7) 0.312(3) 0.7029(18) 0.020(13) Uiso 1 calc R . . 
H14A H 0.0289(8) 0.457(2) 0.6966(17) 0.041(16) Uiso 1 calc R . . 
H14B H 0.0644(5) 0.404(3) 0.7844(17) 0.020(13) Uiso 1 calc R . . 
C15 C 0.21112(17) 0.1080(5) 0.6879(3) 0.0274(12) Uani 1 d . . . 
H15A H 0.1963(9) 0.1222(10) 0.632(4) 0.035(16) Uiso 1 calc R . . 
C16 C 0.26197(19) 0.1210(6) 0.7060(4) 0.0429(15) Uani 1 d . . . 
H16A H 0.2783(6) 0.106(4) 0.7637(19) 0.032(15) Uiso 1 calc R . . 
H16B H 0.2683(3) 0.206(3) 0.691(2) 0.06(2) Uiso 1 calc R . . 
H16C H 0.2707(4) 0.059(3) 0.674(2) 0.047(18) Uiso 1 calc R . . 
C17 C 0.1996(2) -0.0318(6) 0.7074(4) 0.0420(15) Uani 1 d . . . 
H17A H 0.1682(11) -0.0399(13) 0.692(2) 0.047(19) Uiso 1 calc R . . 
H17B H 0.2139(11) -0.0485(15) 0.765(2) 0.06(2) Uiso 1 calc R . . 
H17C H 0.2097(12) -0.092(2) 0.677(2) 0.05(2) Uiso 1 calc R . . 
C18 C 0.20976(18) 0.3798(6) 0.5321(3) 0.0337(13) Uani 1 d . . . 
H18A H 0.2155(5) 0.288(3) 0.526(2) 0.018(12) Uiso 1 calc R . . 
H18B H 0.2322(7) 0.413(3) 0.5834(18) 0.06(2) Uiso 1 calc R . . 
H18C H 0.2115(4) 0.428(3) 0.4846(19) 0.042(17) Uiso 1 calc R . . 
C19 C 0.1405(2) 0.5795(5) 0.5394(3) 0.0328(13) Uani 1 d . . . 
H19A H 0.1120(11) 0.5921(7) 0.543(2) 0.038(16) Uiso 1 calc R . . 
H19B H 0.1412(13) 0.6191(16) 0.491(2) 0.08(2) Uiso 1 calc R . . 
H19C H 0.1627(10) 0.6167(15) 0.586(2) 0.06(2) Uiso 1 calc R . . 
C11 C 0.13795(16) 0.3726(5) 0.7406(3) 0.0193(10) Uani 1 d . . . 
C20 C 0.0684(2) -0.1201(6) 0.4166(4) 0.0505(17) Uani 1 d . . . 
H20A H 0.0721(11) -0.149(2) 0.4712(18) 0.06(2) Uiso 1 calc R . . 
H20B H 0.0791(10) -0.185(3) 0.389(2) 0.053(19) Uiso 1 calc R . . 
H20C H 0.0373(11) -0.1043(12) 0.386(2) 0.05(2) Uiso 1 calc R . . 
C21 C 0.1585(2) -0.0278(7) 0.4767(4) 0.0487(18) Uani 1 d . . . 
H21A H 0.1645(6) -0.103(4) 0.4440(18) 0.056(19) Uiso 1 calc R . . 
H21B H 0.1626(5) -0.058(4) 0.535(2) 0.07(2) Uiso 1 calc R . . 
H21C H 0.1804(8) 0.045(3) 0.480(2) 0.07(3) Uiso 1 calc R . . 
C22 C 0.0990(2) 0.0518(7) 0.3164(3) 0.0460(17) Uani 1 d . . . 
H22A H 0.0686(10) 0.073(4) 0.2798(13) 0.014(12) Uiso 1 calc R . . 
H22B H 0.1083(12) -0.028(3) 0.2977(11) 0.06(2) Uiso 1 calc R . . 
H22C H 0.1193(11) 0.121(3) 0.3153(5) 0.08(3) Uiso 1 calc R . . 
H1   H 0.1225(16) 0.326(5) 0.457(3) 0.022(13) Uiso 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 
Nb1 0.0216(2) 0.0205(2) 0.0122(2) -0.00006(18) 0.00558(16) 0.00187(19) 
Si1 0.0279(7) 0.0234(8) 0.0155(6) 0.0005(6) 0.0089(5) -0.0006(6) 
P1 0.0359(7) 0.0254(7) 0.0188(6) -0.0040(6) 0.0083(6) 0.0035(6) 
Cl1 0.0418(8) 0.0321(7) 0.0221(6) 0.0056(6) 0.0088(5) -0.0083(6) 
N1 0.021(2) 0.022(2) 0.0160(19) -0.0001(17) 0.0054(16) 0.0021(17) 
C1 0.030(3) 0.037(3) 0.022(3) -0.006(3) -0.001(2) 0.004(2) 
C2 0.030(3) 0.041(4) 0.016(2) 0.005(2) -0.001(2) 0.002(2) 
C3 0.024(3) 0.026(3) 0.030(3) 0.003(2) 0.003(2) 0.003(2) 
C4 0.020(3) 0.039(3) 0.027(3) -0.001(2) 0.007(2) 0.006(2) 
C5 0.021(2) 0.038(3) 0.025(3) 0.005(2) 0.004(2) -0.004(2) 
C6 0.019(2) 0.018(2) 0.013(2) 0.0000(19) 0.0064(18) -0.0007(19) 
C7 0.022(2) 0.019(3) 0.020(2) -0.003(2) 0.0067(19) -0.001(2) 
C8 0.023(2) 0.024(3) 0.021(2) 0.006(2) 0.004(2) 0.004(2) 
C9 0.034(3) 0.031(3) 0.011(2) 0.002(2) 0.005(2) -0.003(2) 
C10 0.030(3) 0.030(3) 0.017(2) -0.005(2) 0.011(2) -0.005(2) 
C12 0.028(3) 0.028(3) 0.017(2) 0.001(2) 0.007(2) 0.003(2) 
C13 0.038(3) 0.034(3) 0.027(3) 0.005(2) 0.017(2) 0.013(3) 
C14 0.026(3) 0.043(4) 0.035(3) 0.004(3) 0.011(2) 0.006(3) 
C15 0.031(3) 0.023(3) 0.024(3) -0.003(2) 0.006(2) 0.009(2) 
C16 0.042(3) 0.042(4) 0.045(4) -0.009(3) 0.015(3) 0.013(3) 
C17 0.056(4) 0.030(3) 0.034(3) -0.005(3) 0.009(3) 0.006(3) 
C18 0.036(3) 0.036(3) 0.031(3) 0.003(3) 0.014(2) -0.001(3) 
C19 0.048(3) 0.031(3) 0.023(3) 0.001(2) 0.018(3) -0.001(3) 
C11 0.025(2) 0.018(2) 0.016(2) 0.000(2) 0.0096(19) 0.000(2) 
C20 0.059(5) 0.039(4) 0.057(4) -0.013(3) 0.026(4) -0.004(3) 
C21 0.056(4) 0.050(4) 0.033(3) -0.014(3) 0.007(3) 0.022(4) 
C22 0.068(4) 0.050(4) 0.021(3) 0.000(3) 0.017(3) 0.014(4) 

_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 
Nb1 N1 2.051(4) . ? 
Nb1 C3 2.264(5) . ? 
Nb1 C4 2.285(5) . ? 
Nb1 C2 2.344(5) . ? 
Nb1 C5 2.439(5) . ? 
Nb1 C1 2.479(5) . ? 
Nb1 Cl1 2.4965(13) . ? 
Nb1 P1 2.5522(14) . ? 
Nb1 Si1 2.6458(15) . ? 
Nb1 H1 1.91(5) . ? 
Si1 N1 1.704(4) . ? 
Si1 C18 1.860(5) . ? 
Si1 C19 1.866(6) . ? 
Si1 H1 1.52(5) . ? 
P1 C20 1.812(7) . ? 
P1 C22 1.814(5) . ? 
P1 C21 1.816(6) . ? 
N1 C6 1.434(5) . ? 
C1 C5 1.378(7) . ? 
C1 C2 1.413(8) . ? 
C1 H1A 0.8857 . ? 
C2 C3 1.419(7) . ? 
C2 H2A 0.8878 . ? 
C3 C4 1.423(7) . ? 
C3 H3A 0.8729 . ? 
C4 C5 1.404(8) . ? 
C4 H4A 0.8659 . ? 
C5 H5A 0.7595 . ? 
C6 C7 1.405(6) . ? 
C6 C11 1.418(6) . ? 
C7 C8 1.390(6) . ? 
C7 C15 1.520(6) . ? 
C8 C9 1.371(7) . ? 
C8 H8A 0.9004 . ? 
C9 C10 1.388(7) . ? 
C9 H9A 0.9427 . ? 
C10 C11 1.390(6) . ? 
C10 H10A 0.9622 . ? 
C12 C11 1.515(7) . ? 
C12 C14 1.534(7) . ? 
C12 C13 1.534(7) . ? 
C12 H12A 1.0639 . ? 
C13 H13A 0.9967 . ? 
C13 H13B 0.9967 . ? 
C13 H13C 0.9967 . ? 
C14 H14C 0.9741 . ? 
C14 H14A 0.9741 . ? 
C14 H14B 0.9741 . ? 
C15 C16 1.518(7) . ? 
C15 C17 1.530(8) . ? 
C15 H15A 0.9008 . ? 
C16 H16A 0.9361 . ? 
C16 H16B 0.9361 . ? 
C16 H16C 0.9361 . ? 
C17 H17A 0.9284 . ? 
C17 H17B 0.9284 . ? 
C17 H17C 0.9284 . ? 
C18 H18A 0.9606 . ? 
C18 H18B 0.9606 . ? 
C18 H18C 0.9606 . ? 
C19 H19A 0.9252 . ? 
C19 H19B 0.9252 . ? 
C19 H19C 0.9252 . ? 
C20 H20A 0.9364 . ? 
C20 H20B 0.9364 . ? 
C20 H20C 0.9364 . ? 
C21 H21A 0.9957 . ? 
C21 H21B 0.9957 . ? 
C21 H21C 0.9957 . ? 
C22 H22A 0.9552 . ? 
C22 H22B 0.9552 . ? 
C22 H22C 0.9552 . ? 

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 
N1 Nb1 C3 110.45(18) . . ? 
N1 Nb1 C4 114.05(18) . . ? 
C3 Nb1 C4 36.46(19) . . ? 
N1 Nb1 C2 136.64(18) . . ? 
C3 Nb1 C2 35.82(19) . . ? 
C4 Nb1 C2 58.9(2) . . ? 
N1 Nb1 C5 143.04(16) . . ? 
C3 Nb1 C5 58.1(2) . . ? 
C4 Nb1 C5 34.39(19) . . ? 
C2 Nb1 C5 56.42(19) . . ? 
N1 Nb1 C1 168.08(17) . . ? 
C3 Nb1 C1 57.6(2) . . ? 
C4 Nb1 C1 56.54(19) . . ? 
C2 Nb1 C1 33.92(18) . . ? 
C5 Nb1 C1 32.54(17) . . ? 
N1 Nb1 Cl1 83.62(11) . . ? 
C3 Nb1 Cl1 129.66(14) . . ? 
C4 Nb1 Cl1 93.27(14) . . ? 
C2 Nb1 Cl1 136.25(14) . . ? 
C5 Nb1 Cl1 81.26(14) . . ? 
C1 Nb1 Cl1 103.38(14) . . ? 
N1 Nb1 P1 115.77(11) . . ? 
C3 Nb1 P1 123.52(14) . . ? 
C4 Nb1 P1 129.86(15) . . ? 
C2 Nb1 P1 87.71(14) . . ? 
C5 Nb1 P1 96.87(13) . . ? 
C1 Nb1 P1 74.67(14) . . ? 
Cl1 Nb1 P1 86.84(5) . . ? 
N1 Nb1 Si1 40.10(11) . . ? 
C3 Nb1 Si1 86.30(15) . . ? 
C4 Nb1 Si1 111.90(15) . . ? 
C2 Nb1 Si1 99.25(14) . . ? 
C5 Nb1 Si1 143.86(14) . . ? 
C1 Nb1 Si1 132.99(14) . . ? 
Cl1 Nb1 Si1 123.42(5) . . ? 
P1 Nb1 Si1 109.37(5) . . ? 
N1 Nb1 H1 72.8(14) . . ? 
C3 Nb1 H1 78.3(14) . . ? 
C4 Nb1 H1 114.1(14) . . ? 
C2 Nb1 H1 73.3(14) . . ? 
C5 Nb1 H1 129.3(14) . . ? 
C1 Nb1 H1 103.5(14) . . ? 
Cl1 Nb1 H1 149.2(14) . . ? 
P1 Nb1 H1 85.9(14) . . ? 
Si1 Nb1 H1 34.4(14) . . ? 
N1 Si1 C18 117.1(2) . . ? 
N1 Si1 C19 118.7(2) . . ? 
C18 Si1 C19 107.7(3) . . ? 
N1 Si1 Nb1 50.81(13) . . ? 
C18 Si1 Nb1 130.0(2) . . ? 
C19 Si1 Nb1 120.14(19) . . ? 
N1 Si1 H1 93.7(18) . . ? 
C18 Si1 H1 101.5(17) . . ? 
C19 Si1 H1 116.6(18) . . ? 
Nb1 Si1 H1 45.4(17) . . ? 
C20 P1 C22 102.8(3) . . ? 
C20 P1 C21 101.0(3) . . ? 
C22 P1 C21 100.9(3) . . ? 
C20 P1 Nb1 119.1(2) . . ? 
C22 P1 Nb1 118.9(2) . . ? 
C21 P1 Nb1 111.3(2) . . ? 
C6 N1 Si1 128.8(3) . . ? 
C6 N1 Nb1 141.6(3) . . ? 
Si1 N1 Nb1 89.09(16) . . ? 
C5 C1 C2 108.3(5) . . ? 
C5 C1 Nb1 72.2(3) . . ? 
C2 C1 Nb1 67.8(3) . . ? 
C5 C1 H1A 125.8 . . ? 
C2 C1 H1A 125.8 . . ? 
Nb1 C1 H1A 125.8 . . ? 
C1 C2 C3 108.2(5) . . ? 
C1 C2 Nb1 78.3(3) . . ? 
C3 C2 Nb1 69.0(3) . . ? 
C1 C2 H2A 125.9 . . ? 
C3 C2 H2A 125.9 . . ? 
Nb1 C2 H2A 118.6 . . ? 
C2 C3 C4 106.3(5) . . ? 
C2 C3 Nb1 75.2(3) . . ? 
C4 C3 Nb1 72.6(3) . . ? 
C2 C3 H3A 126.8 . . ? 
C4 C3 H3A 126.8 . . ? 
Nb1 C3 H3A 117.6 . . ? 
C5 C4 C3 108.2(5) . . ? 
C5 C4 Nb1 78.8(3) . . ? 
C3 C4 Nb1 71.0(3) . . ? 
C5 C4 H4A 125.9 . . ? 
C3 C4 H4A 125.9 . . ? 
Nb1 C4 H4A 116.3 . . ? 
C1 C5 C4 108.8(5) . . ? 
C1 C5 Nb1 75.3(3) . . ? 
C4 C5 Nb1 66.8(3) . . ? 
C1 C5 H5A 125.6 . . ? 
C4 C5 H5A 125.6 . . ? 
Nb1 C5 H5A 123.8 . . ? 
C7 C6 C11 119.6(4) . . ? 
C7 C6 N1 121.3(4) . . ? 
C11 C6 N1 119.1(4) . . ? 
C8 C7 C6 119.5(4) . . ? 
C8 C7 C15 119.0(4) . . ? 
C6 C7 C15 121.5(4) . . ? 
C9 C8 C7 121.3(5) . . ? 
C9 C8 H8A 119.3 . . ? 
C7 C8 H8A 119.3 . . ? 
C8 C9 C10 119.2(4) . . ? 
C8 C9 H9A 120.4 . . ? 
C10 C9 H9A 120.4 . . ? 
C9 C10 C11 121.9(5) . . ? 
C9 C10 H10A 119.1 . . ? 
C11 C10 H10A 119.1 . . ? 
C11 C12 C14 110.0(4) . . ? 
C11 C12 C13 112.4(4) . . ? 
C14 C12 C13 111.2(4) . . ? 
C11 C12 H12A 107.7 . . ? 
C14 C12 H12A 107.7 . . ? 
C13 C12 H12A 107.7 . . ? 
C12 C13 H13A 109.5 . . ? 
C12 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C12 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C12 C14 H14C 109.5 . . ? 
C12 C14 H14A 109.5 . . ? 
H14C C14 H14A 109.5 . . ? 
C12 C14 H14B 109.5 . . ? 
H14C C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
C16 C15 C7 113.4(4) . . ? 
C16 C15 C17 110.5(5) . . ? 
C7 C15 C17 110.0(4) . . ? 
C16 C15 H15A 107.6 . . ? 
C7 C15 H15A 107.6 . . ? 
C17 C15 H15A 107.6 . . ? 
C15 C16 H16A 109.5 . . ? 
C15 C16 H16B 109.5 . . ? 
H16A C16 H16B 109.5 . . ? 
C15 C16 H16C 109.5 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 109.5 . . ? 
C15 C17 H17A 109.5 . . ? 
C15 C17 H17B 109.5 . . ? 
H17A C17 H17B 109.5 . . ? 
C15 C17 H17C 109.5 . . ? 
H17A C17 H17C 109.5 . . ? 
H17B C17 H17C 109.5 . . ? 
Si1 C18 H18A 109.5 . . ? 
Si1 C18 H18B 109.5 . . ? 
H18A C18 H18B 109.5 . . ? 
Si1 C18 H18C 109.5 . . ? 
H18A C18 H18C 109.5 . . ? 
H18B C18 H18C 109.5 . . ? 
Si1 C19 H19A 109.5 . . ? 
Si1 C19 H19B 109.5 . . ? 
H19A C19 H19B 109.5 . . ? 
Si1 C19 H19C 109.5 . . ? 
H19A C19 H19C 109.5 . . ? 
H19B C19 H19C 109.5 . . ? 
C10 C11 C6 118.3(4) . . ? 
C10 C11 C12 118.7(4) . . ? 
C6 C11 C12 123.0(4) . . ? 
P1 C20 H20A 109.5 . . ? 
P1 C20 H20B 109.5 . . ? 
H20A C20 H20B 109.5 . . ? 
P1 C20 H20C 109.5 . . ? 
H20A C20 H20C 109.5 . . ? 
H20B C20 H20C 109.5 . . ? 
P1 C21 H21A 109.5 . . ? 
P1 C21 H21B 109.5 . . ? 
H21A C21 H21B 109.5 . . ? 
P1 C21 H21C 109.5 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 109.5 . . ? 
P1 C22 H22A 109.5 . . ? 
P1 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
P1 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 

_diffrn_measured_fraction_theta_max    0.468 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.468 
_refine_diff_density_max    1.427 
_refine_diff_density_min   -0.868 
_refine_diff_density_rms    0.110 

#===end

data_COMPOUND_8

_database_code_CSD	


#  Local code DURHAM

_audit_creation_method      CRYSTALS

_chemical_name_systematic
;
[Ta(N-2,6-C6H3i-Pr2)(Cp)(H)(SiMe2Cl)(PMe3)]
;
_cell_length_a                  15.893(1)
_cell_angle_alpha               90
_cell_length_b                  9.092(1)
_cell_angle_beta                112.568(3)
_cell_length_c                  19.136(2)
_cell_angle_gamma               90
_cell_volume                    2553.47
_symmetry_cell_setting          'Monoclinic '
_symmetry_space_group_name_H-M  'P 1 21/c 1 '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
'-x,y+1/2,-z+1/2'
'x,-y+1/2,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'Ta  '   -1.2580    6.5230   29.2024    1.7733
15.2293    9.3705   14.5135    0.2960    4.7649   63.3644    9.2435

'International_Tables_Vol_IV_Table_2.2B'
'Cl  '    0.1320    0.1590   11.4604    0.0104
7.1964    1.1662    6.2556   18.5194    1.6455   47.7784   -9.5574

'International_Tables_Vol_IV_Table_2.2B'
'Si  '    0.0720    0.0710    6.2915    2.4386
3.0353   32.3337    1.9891    0.6785    1.5410   81.6937    1.1407

'International_Tables_Vol_IV_Table_2.2B'
'P   '    0.0900    0.0950    6.4345    1.9067
4.1791   27.1570    1.7800    0.5260    1.4908   68.1645    1.1149

'International_Tables_Vol_IV_Table_2.2B'
'N   '    0.0040    0.0030   12.2126   0.0057
3.1322    9.8933    2.0125   28.997    1.1663    0.5826  -11.5290

'International_Tables_Vol_IV_Table_2.2B'
'C   '    0.0020    0.0020    2.3100   20.8439
1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
'H   '    0.0000    0.0000    0.4930   10.5109
0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C22 H38 Cl1 N1 P1 Si1 Ta1 '
_chemical_formula_moiety
' C22 H38 Cl1 N1 P1 Si1 Ta1 '
_chemical_compound_source
;
[Ta(N-2,6-C6H3i-Pr2)(Cp)(PMe3)2] + HSiMe2Cl
;
_chemical_formula_weight                592.01
_chemical_melting_point                 'not measured'
_cell_measurement_reflns_used           499
_cell_measurement_theta_min             14.01
_cell_measurement_theta_max             26.53
_cell_measurement_temperature           150
_cell_formula_units_Z                   4
_exptl_crystal_description              Block
_exptl_crystal_colour                   Orange
_exptl_crystal_size_min                 0.15
_exptl_crystal_size_mid                 0.20
_exptl_crystal_size_max                 0.27
_exptl_crystal_density_diffrn           1.54
_exptl_crystal_density_method           none
_exptl_crystal_density_meas             'not measured'
_exptl_crystal_F_000                    1184
_exptl_absorpt_coefficient_mu           4.53
_exptl_absorpt_correction_type          'multi-scan'
_exptl_absorpt_correction_T_min         0.368
_exptl_absorpt_correction_T_max         0.615
_exptl_absorpt_process_details       'SADABS (Sheldrick, 1996)'
_diffrn_measurement_device-type   'Bruker SMART CCD'
_diffrn_radiation_monochromator         'graphite'
_diffrn_radiation_source                'fine-focus sealed tube'
_diffrn_standards_interval_time         ?
_diffrn_standards_interval_count        ?
_diffrn_radiation_type                  'Mo K\a'
_diffrn_radiation_wavelength            0.71073
_diffrn_measurement_method              '\w-scan'
_diffrn_standards_number                0
_diffrn_standards_decay_%               0.00
_diffrn_ambient_temperature             150
_diffrn_reflns_number                   23837
_reflns_number_total                    5838
_diffrn_reflns_av_R_equivalents         0.05
_reflns_number_observed                 4115
_diffrn_reflns_theta_min                0.96
_diffrn_reflns_theta_max                27.53
_diffrn_reflns_limit_h_min              -20
_diffrn_reflns_limit_h_max              19
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              11
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              24
_reflns_limit_h_min                     -20
_reflns_limit_h_max                     19
_reflns_limit_k_min                     0
_reflns_limit_k_max                     11
_reflns_limit_l_min                     0
_reflns_limit_l_max                     24
_reflns_observed_criterion              >3.00\s(I)
_refine_diff_density_min                -0.63
_refine_diff_density_max                1.03
_refine_ls_number_reflns                4115
_refine_ls_structure_factor_coef        F
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_extinction_coef              30.8(41)
_refine_ls_number_restraints            0
_refine_ls_number_parameters            249
_refine_ls_R_factor_obs                 0.0300
_refine_ls_wR_factor_obs                0.0349
_refine_ls_goodness_of_fit_obs          1.0268
_refine_ls_shift/esd_max                0.0019
_refine_ls_abs_structure_flack          'not refined'
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             'Chebychev polynomial'
_refine_ls_hydrogen_treatment           'mixed'
_atom_sites_solution_primary            'direct methods'
_atom_sites_solution_hydrogens          'geometric and Fourier maps'
_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction
;
Bruker SAINT
CRYSTALS (Watkin et al, 1996)
;
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)'
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
Ta1 0.28759(1) 0.23348(2) 0.81398(1) 0.0191 1.0000 Uani
Cl1 0.4140(1) 0.4683(2) 0.71043(9) 0.0410 1.0000 Uani
N1 0.2152(3) 0.3917(4) 0.8089(2) 0.0193 1.0000 Uani
P1 0.2853(1) 0.1058(2) 0.93185(9) 0.0309 1.0000 Uani
Si1 0.4219(1) 0.4001(2) 0.82183(8) 0.0239 1.0000 Uani
C1 0.3474(5) 0.1108(6) 0.7286(4) 0.0359 1.0000 Uani
C2 0.3443(4) -0.0001(6) 0.7788(4) 0.0371 1.0000 Uani
C3 0.2518(4) -0.0205(6) 0.7683(4) 0.0363 1.0000 Uani
C4 0.1971(4) 0.0755(7) 0.7109(4) 0.0366 1.0000 Uani
C5 0.2569(4) 0.1580(6) 0.6870(3) 0.0342 1.0000 Uani
C6 0.1575(3) 0.5132(5) 0.7940(3) 0.0190 1.0000 Uani
C7 0.1308(4) 0.5884(6) 0.7239(3) 0.0262 1.0000 Uani
C8 0.0698(4) 0.7069(7) 0.7102(4) 0.0397 1.0000 Uani
C9 0.0368(4) 0.7535(7) 0.7642(4) 0.0446 1.0000 Uani
C10 0.0639(4) 0.6822(7) 0.8323(4) 0.0373 1.0000 Uani
C11 0.1247(4) 0.5630(5) 0.8496(3) 0.0252 1.0000 Uani
C12 0.1654(4) 0.5400(6) 0.6635(3) 0.0291 1.0000 Uani
C13 0.1918(5) 0.6706(7) 0.6249(4) 0.0476 1.0000 Uani
C14 0.0942(5) 0.4427(8) 0.6051(4) 0.0461 1.0000 Uani
C15 0.1575(4) 0.4912(6) 0.9270(3) 0.0257 1.0000 Uani
C16 0.2397(4) 0.5753(7) 0.9816(3) 0.0349 1.0000 Uani
C17 0.0843(5) 0.4823(8) 0.9610(4) 0.0440 1.0000 Uani
C18 0.5425(4) 0.3322(7) 0.8641(4) 0.0393 1.0000 Uani
C19 0.4198(4) 0.5843(7) 0.8663(4) 0.0390 1.0000 Uani
C20 0.3278(6) 0.2082(8) 1.0195(4) 0.0504 1.0000 Uani
C21 0.3557(5) -0.0606(8) 0.9598(4) 0.0507 1.0000 Uani
C22 0.1727(5) 0.0426(7) 0.9251(4) 0.0434 1.0000 Uani
H1 0.376(8) 0.25(1) 0.893(6) 0.09(4) 1.0000 Uiso
H11 0.4012(5) 0.1479(6) 0.7234(4) 0.0501 1.0000 Uiso
H21 0.3955(4) -0.0525(6) 0.8138(4) 0.0473 1.0000 Uiso
H31 0.2300(4) -0.0885(6) 0.7959(4) 0.0461 1.0000 Uiso
H41 0.1319(4) 0.0833(7) 0.6916(4) 0.0456 1.0000 Uiso
H51 0.2391(4) 0.2334(6) 0.6490(3) 0.0438 1.0000 Uiso
H81 0.0505(4) 0.7569(7) 0.6624(4) 0.0471 1.0000 Uiso
H91 -0.0046(4) 0.8350(7) 0.7537(4) 0.0537 1.0000 Uiso
H101 0.0407(4) 0.7146(7) 0.8693(4) 0.0474 1.0000 Uiso
H121 0.2200(4) 0.4841(6) 0.6886(3) 0.0344 1.0000 Uiso
H131 0.2131(5) 0.6345(7) 0.5875(4) 0.0601 1.0000 Uiso
H132 0.2392(5) 0.7265(7) 0.6621(4) 0.0601 1.0000 Uiso
H133 0.1395(5) 0.7321(7) 0.6010(4) 0.0601 1.0000 Uiso
H141 0.1164(5) 0.4125(8) 0.5672(4) 0.0562 1.0000 Uiso
H142 0.0828(5) 0.3575(8) 0.6297(4) 0.0562 1.0000 Uiso
H143 0.0387(5) 0.4972(8) 0.5817(4) 0.0562 1.0000 Uiso
H151 0.1735(4) 0.3923(6) 0.9195(3) 0.0348 1.0000 Uiso
H161 0.2604(4) 0.5297(7) 1.0305(3) 0.0453 1.0000 Uiso
H162 0.2225(4) 0.6752(7) 0.9856(3) 0.0453 1.0000 Uiso
H163 0.2878(4) 0.5739(7) 0.9629(3) 0.0453 1.0000 Uiso
H171 0.1095(5) 0.4359(8) 1.0098(4) 0.0588 1.0000 Uiso
H172 0.0643(5) 0.5798(8) 0.9664(4) 0.0588 1.0000 Uiso
H173 0.0335(5) 0.4258(8) 0.9281(4) 0.0588 1.0000 Uiso
H181 0.5465(4) 0.2381(7) 0.8428(4) 0.0479 1.0000 Uiso
H182 0.5611(4) 0.3228(7) 0.9179(4) 0.0479 1.0000 Uiso
H183 0.5817(4) 0.4009(7) 0.8532(4) 0.0479 1.0000 Uiso
H191 0.3589(4) 0.6229(7) 0.8461(4) 0.0483 1.0000 Uiso
H192 0.4393(4) 0.5728(7) 0.9201(4) 0.0483 1.0000 Uiso
H193 0.4599(4) 0.6509(7) 0.8553(4) 0.0483 1.0000 Uiso
H201 0.3234(6) 0.1488(8) 1.0594(4) 0.0587 1.0000 Uiso
H202 0.3903(6) 0.2343(8) 1.0315(4) 0.0587 1.0000 Uiso
H203 0.2922(6) 0.2959(8) 1.0141(4) 0.0587 1.0000 Uiso
H211 0.3510(5) -0.1016(8) 1.0044(4) 0.0648 1.0000 Uiso
H212 0.4180(5) -0.0359(8) 0.9701(4) 0.0648 1.0000 Uiso
H213 0.3348(5) -0.1313(8) 0.9195(4) 0.0648 1.0000 Uiso
H221 0.1782(5) -0.0038(7) 0.9717(4) 0.0607 1.0000 Uiso
H222 0.1322(5) 0.1253(7) 0.9157(4) 0.0607 1.0000 Uiso
H223 0.1488(5) -0.0266(7) 0.8843(4) 0.0607 1.0000 Uiso
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 0.0210(1) 0.0158(1) 0.0237(1) -0.00066(8) 0.01202(7) -0.00043(8)
Cl1 0.0356(8) 0.0551(9) 0.0330(8) 0.0075(6) 0.0139(6) -0.0147(7)
N1 0.023(2) 0.018(2) 0.017(2) -0.002(1) 0.008(2) -0.001(2)
P1 0.0363(8) 0.0252(7) 0.0328(8) 0.0099(6) 0.0151(7) 0.0045(6)
Si1 0.0209(7) 0.0247(7) 0.0255(7) 0.0003(5) 0.0082(6) -0.0030(5)
C1 0.046(4) 0.029(3) 0.043(4) -0.012(2) 0.028(3) -0.003(2)
C2 0.036(3) 0.024(3) 0.056(4) -0.010(3) 0.023(3) 0.001(2)
C3 0.043(4) 0.021(3) 0.050(4) -0.011(2) 0.022(3) -0.005(2)
C4 0.032(3) 0.031(3) 0.044(4) -0.018(3) 0.011(3) -0.004(2)
C5 0.043(4) 0.031(3) 0.029(3) -0.011(2) 0.014(3) -0.003(2)
C6 0.017(2) 0.013(2) 0.025(2) -0.001(2) 0.006(2) -0.002(2)
C7 0.024(3) 0.024(2) 0.025(3) 0.001(2) 0.003(2) -0.004(2)
C8 0.034(3) 0.032(3) 0.044(3) 0.014(3) 0.004(3) 0.004(2)
C9 0.029(3) 0.035(3) 0.071(4) 0.007(3) 0.020(3) 0.015(2)
C10 0.032(3) 0.028(3) 0.056(4) -0.005(3) 0.020(3) 0.004(2)
C11 0.021(3) 0.022(2) 0.034(3) -0.002(2) 0.012(2) -0.001(2)
C12 0.034(3) 0.030(3) 0.018(2) 0.006(2) 0.005(2) -0.006(2)
C13 0.068(5) 0.031(3) 0.048(4) 0.008(3) 0.026(4) -0.011(3)
C14 0.045(4) 0.052(4) 0.035(4) -0.006(3) 0.008(3) -0.015(3)
C15 0.027(3) 0.027(3) 0.026(3) -0.003(2) 0.014(2) -0.001(2)
C16 0.034(3) 0.038(3) 0.034(3) -0.010(2) 0.014(3) -0.007(2)
C17 0.042(4) 0.056(4) 0.040(4) -0.015(3) 0.022(3) -0.014(3)
C18 0.026(3) 0.035(3) 0.056(4) 0.005(3) 0.015(3) -0.000(2)
C19 0.034(3) 0.030(3) 0.051(4) -0.007(3) 0.015(3) -0.009(2)
C20 0.066(5) 0.051(4) 0.028(3) 0.010(3) 0.011(3) 0.007(3)
C21 0.053(4) 0.041(4) 0.058(5) 0.025(3) 0.021(4) 0.014(3)
C22 0.051(4) 0.039(3) 0.052(4) 0.009(3) 0.033(4) -0.003(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ta1 . N1 . 1.821(4)    yes
Ta1 . P1 . 2.550(1)    yes
Ta1 . Si1 . 2.574(1)    yes
Ta1 . C1 . 2.451(5)    yes
Ta1 . C3 . 2.457(5)    yes
Ta1 . C4 . 2.418(6)    yes
Ta1 . C5 . 2.388(6)    yes
Ta1 . H1 . 1.6(1)    no
N1 . C6 . 1.394(6)    yes
P1 . C20 . 1.808(7)    yes
P1 . C21 . 1.835(7)    yes
P1 . C22 . 1.836(7)    yes
P1 . H1 . 2.3(1)    no
Si1 . C18 . 1.877(6)    yes
Si1 . C19 . 1.884(6)    yes
Si1 . Cl1 . 2.177(2)    yes
Si1 . H1 . 2.3(1)    no
C1 . C2 . 1.406(9)    yes
C1 . C5 . 1.416(9)    yes
C2 . C3 . 1.417(9)    yes
C3 . C4 . 1.412(9)    yes
C4 . C5 . 1.417(9)    yes
C6 . C7 . 1.417(7)    yes
C6 . C11 . 1.426(7)    yes
C7 . C8 . 1.405(8)    yes
C7 . C12 . 1.524(8)    yes
C8 . C9 . 1.39(1)    yes
C9 . C10 . 1.37(1)    yes
C10 . C11 . 1.405(8)    yes
C11 . C15 . 1.517(8)    yes
C12 . C13 . 1.538(8)    yes
C12 . C14 . 1.530(8)    yes
C15 . C16 . 1.528(8)    yes
C15 . C17 . 1.538(8)    yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ta1 . P1 . 100.6(1)    yes
N1 . Ta1 . Si1 . 91.8(1)    yes
P1 . Ta1 . Si1 . 120.63(5)    yes
N1 . Ta1 . C1 . 136.3(2)    yes
P1 . Ta1 . C1 . 121.6(2)    yes
Si1 . Ta1 . C1 . 77.4(1)    yes
N1 . Ta1 . C3 . 132.0(2)    yes
P1 . Ta1 . C3 . 78.8(2)    yes
Si1 . Ta1 . C3 . 130.3(1)    yes
C1 . Ta1 . C3 . 55.3(2)    yes
N1 . Ta1 . C4 . 105.1(2)    yes
P1 . Ta1 . C4 . 104.2(2)    yes
Si1 . Ta1 . C4 . 128.1(2)    yes
C1 . Ta1 . C4 . 56.4(2)    yes
C3 . Ta1 . C4 . 33.7(2)    yes
N1 . Ta1 . C5 . 107.2(2)    yes
P1 . Ta1 . C5 . 134.6(2)    yes
Si1 . Ta1 . C5 . 94.0(2)    yes
C1 . Ta1 . C5 . 34.0(2)    yes
C3 . Ta1 . C5 . 55.9(2)    yes
C4 . Ta1 . C5 . 34.3(2)    yes
N1 . Ta1 . H1 . 107.7(36)    no
P1 . Ta1 . H1 . 60.8(37)    no
Si1 . Ta1 . H1 . 60.1(37)    no
C1 . Ta1 . H1 . 103.1(38)    no
C2 . Ta1 . H1 . 91.8(36)    no
C3 . Ta1 . H1 . 113.0(36)    no
C4 . Ta1 . H1 . 145.9(36)    no
C5 . Ta1 . H1 . 136.7(38)    no
Ta1 . N1 . C6 . 171.7(4)    yes
Ta1 . P1 . C20 . 117.4(2)    yes
Ta1 . P1 . C21 . 114.8(2)    yes
C20 . P1 . C21 . 100.7(4)    yes
Ta1 . P1 . C22 . 115.1(2)    yes
C20 . P1 . C22 . 103.5(4)    yes
C21 . P1 . C22 . 103.4(3)    yes
Ta1 . P1 . H1 . 38.9(28)    no
C20 . P1 . H1 . 87.7(27)    no
C21 . P1 . H1 . 99.3(27)    no
C22 . P1 . H1 . 152.1(28)    no
Ta1 . Si1 . Cl1 . 112.05(7)    yes
Ta1 . Si1 . C18 . 121.2(2)    yes
Cl1 . Si1 . C18 . 100.4(2)    yes
Ta1 . Si1 . C19 . 113.0(2)    yes
Cl1 . Si1 . C19 . 100.6(2)    yes
C18 . Si1 . C19 . 106.9(3)    yes
Ta1 . Si1 . H1 . 38.6(28)    no
Cl1 . Si1 . H1 . 148.7(27)    no
C18 . Si1 . H1 . 92.6(28)    no
C19 . Si1 . H1 . 102.6(26)    no
Ta1 . C1 . C2 . 75.3(3)    yes
Ta1 . C1 . C5 . 70.6(3)    yes
C2 . C1 . C5 . 107.8(6)    yes
C1 . C2 . C3 . 107.7(6)    yes
Ta1 . C3 . C2 . 75.0(3)    yes
Ta1 . C3 . C4 . 71.6(3)    yes
C2 . C3 . C4 . 108.9(6)    yes
Ta1 . C4 . C3 . 74.7(3)    yes
Ta1 . C4 . C5 . 71.7(3)    yes
C3 . C4 . C5 . 106.8(5)    yes
Ta1 . C5 . C1 . 75.4(3)    yes
Ta1 . C5 . C4 . 74.0(3)    yes
C1 . C5 . C4 . 108.7(6)    yes
N1 . C6 . C7 . 120.7(4)    yes
N1 . C6 . C11 . 119.9(4)    yes
C7 . C6 . C11 . 119.4(4)    yes
C6 . C7 . C8 . 118.7(5)    yes
C6 . C7 . C12 . 121.0(5)    yes
C8 . C7 . C12 . 120.2(5)    yes
C7 . C8 . C9 . 121.6(6)    yes
C8 . C9 . C10 . 119.5(5)    yes
C9 . C10 . C11 . 121.7(6)    yes
C6 . C11 . C10 . 119.0(5)    yes
C6 . C11 . C15 . 120.3(4)    yes
C10 . C11 . C15 . 120.7(5)    yes
C7 . C12 . C13 . 112.7(5)    yes
C7 . C12 . C14 . 109.9(5)    yes
C13 . C12 . C14 . 110.9(5)    yes
C11 . C15 . C16 . 109.6(5)    yes
C11 . C15 . C17 . 113.8(5)    yes
C16 . C15 . C17 . 108.9(5)    yes
#===end


data_COMPOUND_13

_database_code_CSD	


#  Local code TAOTF

_audit_creation_method            SHELXL 

_chemical_name_systematic 
; 
{[TaCp(2,6-C6H3Pri2)(PMe3)2(Cl)](OTf)}
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'C23 H40 Cl N P2 Ta, C F3 O3 S' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C24 H40 Cl F3 N O3 P2 S Ta' 
_chemical_formula_weight          757.97 
_chemical_melting_point           ? 
_chemical_compound_source         ? 

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' 
'F'  'F'   0.0171   0.0103 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'P'  'P'   0.1023   0.0942 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'S'  'S'   0.1246   0.1234 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Ta'  'Ta'  -0.7052   6.5227 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            'triclinic' 
_symmetry_space_group_name_H-M    'P-1'

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, -y, -z' 

_cell_length_a                    11.224(2) 
_cell_length_b                    11.281(2) 
_cell_length_c                    13.562(3) 
_cell_angle_alpha                 100.71(3) 
_cell_angle_beta                  104.08(3) 
_cell_angle_gamma                 106.70(3) 
_cell_volume                      1533.5(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     520 
_cell_measurement_theta_min       14.2 
_cell_measurement_theta_max       25.5 
_exptl_crystal_description        'needle' 
_exptl_crystal_colour             'yellow' 
_exptl_crystal_size_max           0.70 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.642 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              756 
_exptl_absorpt_coefficient_mu     3.887 
_exptl_absorpt_correction_type    'sadabs' 
_exptl_absorpt_correction_T_min   0.789203 
_exptl_absorpt_correction_T_max   1.000000 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       153(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        ? 
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11041 
_diffrn_reflns_av_R_equivalents   0.0617 
_diffrn_reflns_av_sigmaI/netI     0.1441 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.61 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              6658 
_reflns_number_observed           4416 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 584 with very negative
F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors

wR and all goodnesses 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 observed
criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0267P)^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     calcd 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.000(15) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          6074 
_refine_ls_number_parameters      326 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1085 
_refine_ls_R_factor_obs           0.0537 
_refine_ls_wR_factor_all          0.0870 
_refine_ls_wR_factor_obs          0.0746 
_refine_ls_goodness_of_fit_all    0.949 
_refine_ls_goodness_of_fit_obs    1.025 
_refine_ls_restrained_S_all       0.962 
_refine_ls_restrained_S_obs       1.025 
_refine_ls_shift/esd_max          -1.770 
_refine_ls_shift/esd_mean         0.005 

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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Ta1 Ta -0.27898(3) 0.75675(3) 0.74319(3) 0.01903(11) Uani 1 d . . 
Cl1 Cl -0.3520(2) 0.5464(2) 0.61300(14) 0.0278(4) Uani 1 d . . 
P1 P -0.4541(2) 0.6038(2) 0.80192(14) 0.0232(5) Uani 1 d . . 
P2 P -0.2008(2) 0.8072(2) 0.58363(14) 0.0232(4) Uani 1 d . . 
S1 S -0.1488(2) 0.6969(2) 0.18488(15) 0.0287(5) Uani 1 d . . 
O1 O -0.1601(5) 0.7291(5) 0.2889(4) 0.0451(15) Uani 1 d . . 
O2 O -0.0692(5) 0.8022(5) 0.1573(4) 0.046(2) Uani 1 d . . 
O3 O -0.2690(5) 0.6159(5) 0.1032(4) 0.046(2) Uani 1 d . . 
N1 N -0.3888(5) 0.8468(5) 0.7265(4) 0.0217(14) Uani 1 d . . 
C1 C -0.0775(8) 0.7161(8) 0.8350(6) 0.041(2) Uani 1 d . . 
H1A H -0.0540(8) 0.6409(8) 0.8113(6) 0.049 Uiso 1 calc R . 
C2 C -0.1483(7) 0.7276(7) 0.9044(6) 0.032(2) Uani 1 d . . 
H2A H -0.1803(7) 0.6627(7) 0.9399(6) 0.039 Uiso 1 calc R . 
C3 C -0.1540(6) 0.8528(7) 0.9252(5) 0.026(2) Uani 1 d . . 
H3A H -0.1845(6) 0.8915(7) 0.9806(5) 0.031 Uiso 1 calc R . 
C4 C -0.0834(7) 0.9194(7) 0.8660(5) 0.027(2) Uani 1 d . . 
H4A H -0.0587(7) 1.0120(7) 0.8730(5) 0.032 Uiso 1 calc R . 
C5 C -0.0363(7) 0.8349(7) 0.8100(6) 0.032(2) Uani 1 d . . 
H5A H 0.0229(7) 0.8573(7) 0.7685(6) 0.038 Uiso 1 calc R . 
C6 C -0.4731(7) 0.9195(7) 0.7274(5) 0.023(2) Uani 1 d . . 
C7 C -0.5951(7) 0.8791(6) 0.6461(5) 0.025(2) Uani 1 d . . 
C8 C -0.6787(7) 0.9468(7) 0.6541(6) 0.031(2) Uani 1 d . . 
H8A H -0.7583(7) 0.9208(7) 0.6006(6) 0.037 Uiso 1 calc R . 
C9 C -0.6478(8) 1.0539(7) 0.7403(6) 0.035(2) Uani 1 d . . 
H9A H -0.7070(8) 1.0961(7) 0.7454(6) 0.042 Uiso 1 calc R . 
C10 C -0.5280(7) 1.0942(7) 0.8166(6) 0.030(2) Uani 1 d . . 
H10A H -0.5056(7) 1.1660(7) 0.8730(6) 0.036 Uiso 1 calc R . 
C11 C -0.4393(7) 1.0313(6) 0.8122(5) 0.025(2) Uani 1 d . . 
C12 C -0.6381(7) 0.7676(6) 0.5448(5) 0.026(2) Uani 1 d . . 
H12A H -0.5783(7) 0.7194(6) 0.5548(5) 0.031 Uiso 1 calc R . 
C13 C -0.6290(8) 0.8209(8) 0.4487(6) 0.040(2) Uani 1 d . . 
H13A H -0.6561(8) 0.7506(8) 0.3865(6) 0.060 Uiso 1 calc R . 
H13B H -0.5402(8) 0.8745(8) 0.4612(6) 0.060 Uiso 1 calc R . 
H13C H -0.6852(8) 0.8707(8) 0.4389(6) 0.060 Uiso 1 calc R . 
C14 C -0.7794(7) 0.6732(7) 0.5194(6) 0.034(2) Uani 1 d . . 
H14A H -0.8009(7) 0.6062(7) 0.4560(6) 0.051 Uiso 1 calc R . 
H14B H -0.8396(7) 0.7188(7) 0.5095(6) 0.051 Uiso 1 calc R . 
H14C H -0.7853(7) 0.6360(7) 0.5770(6) 0.051 Uiso 1 calc R . 
C15 C -0.3075(7) 1.0860(6) 0.8968(5) 0.026(2) Uani 1 d . . 
H15A H -0.2590(7) 1.0293(6) 0.8805(5) 0.031 Uiso 1 calc R . 
C16 C -0.2283(8) 1.2182(8) 0.8949(8) 0.070(3) Uani 1 d . . 
H16A H -0.1454(8) 1.2493(8) 0.9498(8) 0.105 Uiso 1 calc R . 
H16B H -0.2752(8) 1.2759(8) 0.9062(8) 0.105 Uiso 1 calc R . 
H16C H -0.2141(8) 1.2135(8) 0.8275(8) 0.105 Uiso 1 calc R . 
C17 C -0.3163(8) 1.0861(9) 1.0061(6) 0.059(3) Uani 1 d . . 
H17A H -0.2298(8) 1.1217(9) 1.0564(6) 0.088 Uiso 1 calc R . 
H17B H -0.3575(8) 0.9994(9) 1.0076(6) 0.088 Uiso 1 calc R . 
H17C H -0.3673(8) 1.1371(9) 1.0238(6) 0.088 Uiso 1 calc R . 
C18 C -0.1082(7) 0.9761(6) 0.6040(6) 0.037(2) Uani 1 d . . 
H18A H -0.1567(7) 1.0280(6) 0.6256(6) 0.055 Uiso 1 calc R . 
H18B H -0.0937(7) 0.9888(6) 0.5392(6) 0.055 Uiso 1 calc R . 
H18C H -0.0254(7) 1.0006(6) 0.6579(6) 0.055 Uiso 1 calc R . 
C19 C -0.3368(6) 0.7695(7) 0.4642(5) 0.030(2) Uani 1 d . . 
H19A H -0.3962(6) 0.8114(7) 0.4795(5) 0.044 Uiso 1 calc R . 
H19B H -0.3819(6) 0.6781(7) 0.4394(5) 0.044 Uiso 1 calc R . 
H19C H -0.3040(6) 0.7993(7) 0.4108(5) 0.044 Uiso 1 calc R . 
C20 C -0.0982(7) 0.7232(7) 0.5438(6) 0.034(2) Uani 1 d . . 
H20A H -0.0234(7) 0.7387(7) 0.6035(6) 0.051 Uiso 1 calc R . 
H20B H -0.0693(7) 0.7537(7) 0.4891(6) 0.051 Uiso 1 calc R . 
H20C H -0.1472(7) 0.6325(7) 0.5177(6) 0.051 Uiso 1 calc R . 
C21 C -0.4804(7) 0.6809(7) 0.9204(6) 0.035(2) Uani 1 d . . 
H21A H -0.4006(7) 0.7109(7) 0.9785(6) 0.052 Uiso 1 calc R . 
H21B H -0.5479(7) 0.6202(7) 0.9360(6) 0.052 Uiso 1 calc R . 
H21C H -0.5065(7) 0.7526(7) 0.9094(6) 0.052 Uiso 1 calc R . 
C22 C -0.6138(6) 0.5560(7) 0.7047(5) 0.030(2) Uani 1 d . . 
H22A H -0.6119(6) 0.5131(7) 0.6373(5) 0.046 Uiso 1 calc R . 
H22B H -0.6365(6) 0.6309(7) 0.6993(5) 0.046 Uiso 1 calc R . 
H22C H -0.6779(6) 0.4985(7) 0.7259(5) 0.046 Uiso 1 calc R . 
C23 C -0.4367(8) 0.4548(7) 0.8242(6) 0.037(2) Uani 1 d . . 
H23A H -0.3532(8) 0.4736(7) 0.8755(6) 0.055 Uiso 1 calc R . 
H23B H -0.4424(8) 0.3993(7) 0.7590(6) 0.055 Uiso 1 calc R . 
H23C H -0.5054(8) 0.4128(7) 0.8498(6) 0.055 Uiso 1 calc R . 
C24 C -0.0556(9) 0.5903(9) 0.1942(8) 0.048(2) Uani 1 d . . 
F1 F -0.0381(5) 0.5474(5) 0.1000(4) 0.068(2) Uani 1 d . . 
F2 F -0.1169(5) 0.4857(5) 0.2204(5) 0.075(2) Uani 1 d . . 
F3 F 0.0628(5) 0.6480(6) 0.2643(5) 0.085(2) Uani 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 0.0201(2) 0.0193(2) 0.0165(2) 0.00462(11) 0.00589(12) 0.00529(12) 
Cl1 0.0330(11) 0.0230(10) 0.0247(10) 0.0036(8) 0.0116(9) 0.0057(8) 
P1 0.0251(11) 0.0237(11) 0.0200(11) 0.0069(8) 0.0095(9) 0.0047(9) 
P2 0.0230(11) 0.0248(11) 0.0207(11) 0.0060(8) 0.0084(9) 0.0055(9) 
S1 0.0334(12) 0.0259(11) 0.0263(11) 0.0107(8) 0.0118(10) 0.0054(9) 
O1 0.062(4) 0.040(3) 0.035(3) 0.011(3) 0.028(3) 0.011(3) 
O2 0.072(4) 0.032(3) 0.033(3) 0.016(3) 0.025(3) 0.006(3) 
O3 0.028(3) 0.050(4) 0.043(4) 0.013(3) -0.001(3) -0.001(3) 
N1 0.020(3) 0.029(3) 0.009(3) 0.006(2) 0.000(3) 0.003(3) 
C1 0.040(5) 0.044(5) 0.035(5) 0.004(4) -0.007(4) 0.031(4) 
C2 0.030(5) 0.031(5) 0.021(4) 0.009(3) -0.004(4) -0.002(4) 
C3 0.018(4) 0.032(4) 0.021(4) 0.001(3) 0.007(3) 0.002(3) 
C4 0.020(4) 0.030(4) 0.021(4) 0.007(3) -0.003(3) 0.002(3) 
C5 0.011(4) 0.050(5) 0.023(4) 0.007(4) 0.001(3) 0.000(4) 
C6 0.019(4) 0.029(4) 0.018(4) 0.007(3) 0.001(3) 0.009(3) 
C7 0.033(5) 0.022(4) 0.027(4) 0.010(3) 0.018(4) 0.012(4) 
C8 0.031(5) 0.035(5) 0.027(4) 0.012(4) 0.002(4) 0.018(4) 
C9 0.041(5) 0.038(5) 0.045(5) 0.022(4) 0.028(5) 0.023(4) 
C10 0.032(5) 0.031(4) 0.032(5) 0.005(4) 0.017(4) 0.015(4) 
C11 0.028(5) 0.028(4) 0.019(4) 0.006(3) 0.013(4) 0.008(4) 
C12 0.027(4) 0.028(4) 0.022(4) 0.006(3) 0.005(3) 0.014(4) 
C13 0.044(5) 0.052(5) 0.029(5) 0.013(4) 0.015(4) 0.020(4) 
C14 0.025(5) 0.031(5) 0.038(5) -0.003(4) 0.007(4) 0.008(4) 
C15 0.029(5) 0.019(4) 0.023(4) -0.003(3) 0.007(4) 0.007(3) 
C16 0.044(6) 0.066(7) 0.071(7) 0.031(5) -0.003(5) -0.014(5) 
C17 0.040(6) 0.086(7) 0.031(5) 0.010(5) 0.004(4) 0.003(5) 
C18 0.037(5) 0.030(5) 0.040(5) 0.015(4) 0.017(4) 0.000(4) 
C19 0.024(4) 0.044(5) 0.024(4) 0.014(4) 0.007(4) 0.014(4) 
C20 0.033(5) 0.040(5) 0.043(5) 0.017(4) 0.025(4) 0.018(4) 
C21 0.037(5) 0.039(5) 0.032(5) 0.018(4) 0.019(4) 0.009(4) 
C22 0.028(5) 0.037(5) 0.028(4) 0.011(3) 0.015(4) 0.007(4) 
C23 0.047(5) 0.033(5) 0.038(5) 0.013(4) 0.017(4) 0.019(4) 
C24 0.046(6) 0.062(6) 0.053(6) 0.033(5) 0.032(5) 0.018(5) 
F1 0.076(4) 0.060(3) 0.091(4) 0.018(3) 0.059(4) 0.029(3) 
F2 0.088(4) 0.068(4) 0.126(5) 0.067(4) 0.073(4) 0.051(3) 
F3 0.036(3) 0.155(6) 0.075(4) 0.065(4) 0.010(3) 0.037(4) 

_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 N1 1.809(6) . ? 
Ta1 C3 2.384(7) . ? 
Ta1 C4 2.393(7) . ? 
Ta1 C2 2.454(7) . ? 
Ta1 Cl1 2.458(2) . ? 
Ta1 C5 2.478(7) . ? 
Ta1 C1 2.512(7) . ? 
Ta1 P1 2.607(2) . ? 
Ta1 P2 2.621(2) . ? 
P1 C22 1.809(7) . ? 
P1 C21 1.812(7) . ? 
P1 C23 1.817(7) . ? 
P2 C20 1.804(7) . ? 
P2 C19 1.817(7) . ? 
P2 C18 1.820(7) . ? 
S1 O1 1.436(5) . ? 
S1 O2 1.437(5) . ? 
S1 O3 1.438(5) . ? 
S1 C24 1.809(9) . ? 
N1 C6 1.421(8) . ? 
C1 C2 1.383(11) . ? 
C1 C5 1.419(10) . ? 
C2 C3 1.411(10) . ? 
C3 C4 1.425(9) . ? 
C4 C5 1.407(10) . ? 
C6 C7 1.420(9) . ? 
C6 C11 1.425(9) . ? 
C7 C8 1.381(9) . ? 
C7 C12 1.545(9) . ? 
C8 C9 1.408(10) . ? 
C9 C10 1.372(10) . ? 
C10 C11 1.384(9) . ? 
C11 C15 1.507(9) . ? 
C12 C13 1.545(9) . ? 
C12 C14 1.547(9) . ? 
C15 C17 1.509(10) . ? 
C15 C16 1.510(10) . ? 
C24 F3 1.324(9) . ? 
C24 F2 1.342(9) . ? 
C24 F1 1.360(9) . ? 

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 
N1 Ta1 C3 100.9(2) . . ? 
N1 Ta1 C4 101.0(2) . . ? 
C3 Ta1 C4 34.7(2) . . ? 
N1 Ta1 C2 130.3(3) . . ? 
C3 Ta1 C2 33.9(2) . . ? 
C4 Ta1 C2 56.0(2) . . ? 
N1 Ta1 Cl1 115.9(2) . . ? 
C3 Ta1 Cl1 137.6(2) . . ? 
C4 Ta1 Cl1 140.7(2) . . ? 
C2 Ta1 Cl1 103.8(2) . . ? 
N1 Ta1 C5 129.7(3) . . ? 
C3 Ta1 C5 56.3(2) . . ? 
C4 Ta1 C5 33.5(2) . . ? 
C2 Ta1 C5 54.9(2) . . ? 
Cl1 Ta1 C5 107.4(2) . . ? 
N1 Ta1 C1 154.9(2) . . ? 
C3 Ta1 C1 55.3(3) . . ? 
C4 Ta1 C1 55.2(3) . . ? 
C2 Ta1 C1 32.3(2) . . ? 
Cl1 Ta1 C1 89.2(2) . . ? 
C5 Ta1 C1 33.0(2) . . ? 
N1 Ta1 P1 85.7(2) . . ? 
C3 Ta1 P1 88.3(2) . . ? 
C4 Ta1 P1 123.0(2) . . ? 
C2 Ta1 P1 76.6(2) . . ? 
Cl1 Ta1 P1 75.05(6) . . ? 
C5 Ta1 P1 131.0(2) . . ? 
C1 Ta1 P1 100.3(2) . . ? 
N1 Ta1 P2 92.8(2) . . ? 
C3 Ta1 P2 125.3(2) . . ? 
C4 Ta1 P2 90.9(2) . . ? 
C2 Ta1 P2 126.7(2) . . ? 
Cl1 Ta1 P2 75.06(6) . . ? 
C5 Ta1 P2 74.2(2) . . ? 
C1 Ta1 P2 95.4(2) . . ? 
P1 Ta1 P2 145.86(6) . . ? 
C22 P1 C21 101.9(3) . . ? 
C22 P1 C23 105.3(3) . . ? 
C21 P1 C23 104.6(3) . . ? 
C22 P1 Ta1 109.6(2) . . ? 
C21 P1 Ta1 113.9(2) . . ? 
C23 P1 Ta1 119.8(3) . . ? 
C20 P2 C19 104.7(3) . . ? 
C20 P2 C18 104.2(4) . . ? 
C19 P2 C18 103.5(3) . . ? 
C20 P2 Ta1 116.2(2) . . ? 
C19 P2 Ta1 112.5(2) . . ? 
C18 P2 Ta1 114.4(3) . . ? 
O1 S1 O2 114.8(3) . . ? 
O1 S1 O3 115.0(3) . . ? 
O2 S1 O3 115.3(3) . . ? 
O1 S1 C24 103.2(4) . . ? 
O2 S1 C24 104.1(4) . . ? 
O3 S1 C24 102.1(4) . . ? 
C6 N1 Ta1 172.6(5) . . ? 
C2 C1 C5 108.5(7) . . ? 
C2 C1 Ta1 71.5(4) . . ? 
C5 C1 Ta1 72.1(4) . . ? 
C1 C2 C3 109.2(7) . . ? 
C1 C2 Ta1 76.2(4) . . ? 
C3 C2 Ta1 70.3(4) . . ? 
C2 C3 C4 106.8(6) . . ? 
C2 C3 Ta1 75.8(4) . . ? 
C4 C3 Ta1 73.0(4) . . ? 
C5 C4 C3 108.3(7) . . ? 
C5 C4 Ta1 76.5(4) . . ? 
C3 C4 Ta1 72.3(4) . . ? 
C4 C5 C1 107.3(7) . . ? 
C4 C5 Ta1 69.9(4) . . ? 
C1 C5 Ta1 74.8(4) . . ? 
C7 C6 N1 120.5(6) . . ? 
C7 C6 C11 118.9(7) . . ? 
N1 C6 C11 120.6(6) . . ? 
C8 C7 C6 118.7(6) . . ? 
C8 C7 C12 117.0(7) . . ? 
C6 C7 C12 124.1(6) . . ? 
C7 C8 C9 122.4(7) . . ? 
C10 C9 C8 118.1(7) . . ? 
C9 C10 C11 122.1(7) . . ? 
C10 C11 C6 119.6(7) . . ? 
C10 C11 C15 118.5(6) . . ? 
C6 C11 C15 121.9(6) . . ? 
C7 C12 C13 110.5(6) . . ? 
C7 C12 C14 113.0(6) . . ? 
C13 C12 C14 108.6(6) . . ? 
C11 C15 C17 113.2(6) . . ? 
C11 C15 C16 112.2(6) . . ? 
C17 C15 C16 110.9(6) . . ? 
F3 C24 F2 108.2(7) . . ? 
F3 C24 F1 106.6(7) . . ? 
F2 C24 F1 106.8(7) . . ? 
F3 C24 S1 112.2(7) . . ? 
F2 C24 S1 111.7(6) . . ? 
F1 C24 S1 111.1(6) . . ? 

_refine_diff_density_max    1.013 
_refine_diff_density_min   -0.731 
_refine_diff_density_rms    0.192 

#===end




----------
X-Sun-Data-Type: default
X-Sun-Data-Name: 133301-2
X-Sun-Charset: us-ascii
X-Sun-Content-Lines: 963


data_compound1
_database_code_CSD 133301

#  CpTa(NAr)(H)(SiMe2Cl)(PMe3)  (Compound 1)
#  Local code DURHAM

_audit_creation_method      CRYSTALS


_chemical_name_systematic
;
CpTa(N-2,6-C6H3i-Pr2)(H)(SiMe2Cl)(PMe3)
;
_cell_length_a                  15.893(1)
_cell_angle_alpha               90
_cell_length_b                  9.092(1)
_cell_angle_beta                112.568(3)
_cell_length_c                  19.136(2)
_cell_angle_gamma               90
_cell_volume                    2553.47
_symmetry_cell_setting          'Monoclinic '
_symmetry_space_group_name_H-M  'P 1 21/c 1 '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
'-x,y+1/2,-z+1/2'
'x,-y+1/2,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'Ta  '   -1.2580    6.5230   29.2024    1.7733
15.2293    9.3705   14.5135    0.2960    4.7649   63.3644    9.2435

'International_Tables_Vol_IV_Table_2.2B'
'Cl  '    0.1320    0.1590   11.4604    0.0104
7.1964    1.1662    6.2556   18.5194    1.6455   47.7784   -9.5574

'International_Tables_Vol_IV_Table_2.2B'
'Si  '    0.0720    0.0710    6.2915    2.4386
3.0353   32.3337    1.9891    0.6785    1.5410   81.6937    1.1407

'International_Tables_Vol_IV_Table_2.2B'
'P   '    0.0900    0.0950    6.4345    1.9067
4.1791   27.1570    1.7800    0.5260    1.4908   68.1645    1.1149

'International_Tables_Vol_IV_Table_2.2B'
'N   '    0.0040    0.0030   12.2126   0.0057
3.1322    9.8933    2.0125   28.997    1.1663    0.5826  -11.5290

'International_Tables_Vol_IV_Table_2.2B'
'C   '    0.0020    0.0020    2.3100   20.8439
1.0200   10.2075    1.5886    0.5687    0.8650   51.6512    0.2156
'International_Tables_Vol_IV_Table_2.2B'
'H   '    0.0000    0.0000    0.4930   10.5109
0.3229   26.1257    0.1402    3.1424    0.0408   57.7997    0.0030
'International_Tables_Vol_IV_Table_2.2B'
_chemical_formula_sum
' C22 H38 Cl1 N1 P1 Si1 Ta1 '
_chemical_formula_moiety
' C22 H38 Cl1 N1 P1 Si1 Ta1 '
_chemical_compound_source
;
[Ta(N-2,6-C6H3i-Pr2)(Cp)(PMe3)2] + HSiMe2Cl
;
_chemical_formula_weight                592.01
_chemical_melting_point                 'not measured'
_cell_measurement_reflns_used           499
_cell_measurement_theta_min             14.01
_cell_measurement_theta_max             26.53
_cell_measurement_temperature           150
_cell_formula_units_Z                   4
_exptl_crystal_description              Block
_exptl_crystal_colour                   Orange
_exptl_crystal_size_min                 0.15
_exptl_crystal_size_mid                 0.20
_exptl_crystal_size_max                 0.27
_exptl_crystal_density_diffrn           1.54
_exptl_crystal_density_method           none
_exptl_crystal_density_meas             'not measured'
_exptl_crystal_F_000                    1184
_exptl_absorpt_coefficient_mu           4.53
_exptl_absorpt_correction_type          'multi-scan'
_exptl_absorpt_correction_T_min         0.368
_exptl_absorpt_correction_T_max         0.615
_exptl_absorpt_process_details       'SADABS (Sheldrick, 1996)'
_diffrn_measurement_device-type   'Bruker SMART CCD'
_diffrn_radiation_monochromator         'graphite'
_diffrn_radiation_source                'fine-focus sealed tube'
_diffrn_standards_interval_time         ?
_diffrn_standards_interval_count        ?
_diffrn_radiation_type                  'Mo K\a'
_diffrn_radiation_wavelength            0.71073
_diffrn_measurement_method              '\w-scan'
_diffrn_standards_number                0
_diffrn_standards_decay_%               0.00
_diffrn_ambient_temperature             150
_diffrn_reflns_number                   23837
_reflns_number_total                    5838
_diffrn_reflns_av_R_equivalents         0.05
_reflns_number_observed                 4115
_diffrn_reflns_theta_min                0.96
_diffrn_reflns_theta_max                27.53
_diffrn_reflns_limit_h_min              -20
_diffrn_reflns_limit_h_max              19
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              11
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              24
_reflns_limit_h_min                     -20
_reflns_limit_h_max                     19
_reflns_limit_k_min                     0
_reflns_limit_k_max                     11
_reflns_limit_l_min                     0
_reflns_limit_l_max                     24
_reflns_observed_criterion              >3.00\s(I)
_refine_diff_density_min                -0.63
_refine_diff_density_max                1.03
_refine_ls_number_reflns                4115
_refine_ls_structure_factor_coef        F
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_extinction_coef              30.8(41)
_refine_ls_number_restraints            0
_refine_ls_number_parameters            249
_refine_ls_R_factor_obs                 0.0300
_refine_ls_wR_factor_obs                0.0349
_refine_ls_goodness_of_fit_obs          1.0268
_refine_ls_shift/esd_max                0.0019
_refine_ls_abs_structure_flack          'not refined'
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             'Chebychev polynomial'
_refine_ls_hydrogen_treatment           'mixed'
_atom_sites_solution_primary            'direct methods'
_atom_sites_solution_hydrogens          'geometric and Fourier maps'
_computing_data_collection        'Bruker SMART'
_computing_cell_refinement        'Bruker SMART'
_computing_data_reduction
;
Bruker SAINT
CRYSTALS (Watkin et al, 1996)
;
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)'
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin et al, 1996)
;
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_thermal_displace_type
Ta1 0.28759(1) 0.23348(2) 0.81398(1) 0.0191 1.0000 Uani
Cl1 0.4140(1) 0.4683(2) 0.71043(9) 0.0410 1.0000 Uani
N1 0.2152(3) 0.3917(4) 0.8089(2) 0.0193 1.0000 Uani
P1 0.2853(1) 0.1058(2) 0.93185(9) 0.0309 1.0000 Uani
Si1 0.4219(1) 0.4001(2) 0.82183(8) 0.0239 1.0000 Uani
C1 0.3474(5) 0.1108(6) 0.7286(4) 0.0359 1.0000 Uani
C2 0.3443(4) -0.0001(6) 0.7788(4) 0.0371 1.0000 Uani
C3 0.2518(4) -0.0205(6) 0.7683(4) 0.0363 1.0000 Uani
C4 0.1971(4) 0.0755(7) 0.7109(4) 0.0366 1.0000 Uani
C5 0.2569(4) 0.1580(6) 0.6870(3) 0.0342 1.0000 Uani
C6 0.1575(3) 0.5132(5) 0.7940(3) 0.0190 1.0000 Uani
C7 0.1308(4) 0.5884(6) 0.7239(3) 0.0262 1.0000 Uani
C8 0.0698(4) 0.7069(7) 0.7102(4) 0.0397 1.0000 Uani
C9 0.0368(4) 0.7535(7) 0.7642(4) 0.0446 1.0000 Uani
C10 0.0639(4) 0.6822(7) 0.8323(4) 0.0373 1.0000 Uani
C11 0.1247(4) 0.5630(5) 0.8496(3) 0.0252 1.0000 Uani
C12 0.1654(4) 0.5400(6) 0.6635(3) 0.0291 1.0000 Uani
C13 0.1918(5) 0.6706(7) 0.6249(4) 0.0476 1.0000 Uani
C14 0.0942(5) 0.4427(8) 0.6051(4) 0.0461 1.0000 Uani
C15 0.1575(4) 0.4912(6) 0.9270(3) 0.0257 1.0000 Uani
C16 0.2397(4) 0.5753(7) 0.9816(3) 0.0349 1.0000 Uani
C17 0.0843(5) 0.4823(8) 0.9610(4) 0.0440 1.0000 Uani
C18 0.5425(4) 0.3322(7) 0.8641(4) 0.0393 1.0000 Uani
C19 0.4198(4) 0.5843(7) 0.8663(4) 0.0390 1.0000 Uani
C20 0.3278(6) 0.2082(8) 1.0195(4) 0.0504 1.0000 Uani
C21 0.3557(5) -0.0606(8) 0.9598(4) 0.0507 1.0000 Uani
C22 0.1727(5) 0.0426(7) 0.9251(4) 0.0434 1.0000 Uani
H1 0.376(8) 0.25(1) 0.893(6) 0.09(4) 1.0000 Uiso
H11 0.4012(5) 0.1479(6) 0.7234(4) 0.0501 1.0000 Uiso
H21 0.3955(4) -0.0525(6) 0.8138(4) 0.0473 1.0000 Uiso
H31 0.2300(4) -0.0885(6) 0.7959(4) 0.0461 1.0000 Uiso
H41 0.1319(4) 0.0833(7) 0.6916(4) 0.0456 1.0000 Uiso
H51 0.2391(4) 0.2334(6) 0.6490(3) 0.0438 1.0000 Uiso
H81 0.0505(4) 0.7569(7) 0.6624(4) 0.0471 1.0000 Uiso
H91 -0.0046(4) 0.8350(7) 0.7537(4) 0.0537 1.0000 Uiso
H101 0.0407(4) 0.7146(7) 0.8693(4) 0.0474 1.0000 Uiso
H121 0.2200(4) 0.4841(6) 0.6886(3) 0.0344 1.0000 Uiso
H131 0.2131(5) 0.6345(7) 0.5875(4) 0.0601 1.0000 Uiso
H132 0.2392(5) 0.7265(7) 0.6621(4) 0.0601 1.0000 Uiso
H133 0.1395(5) 0.7321(7) 0.6010(4) 0.0601 1.0000 Uiso
H141 0.1164(5) 0.4125(8) 0.5672(4) 0.0562 1.0000 Uiso
H142 0.0828(5) 0.3575(8) 0.6297(4) 0.0562 1.0000 Uiso
H143 0.0387(5) 0.4972(8) 0.5817(4) 0.0562 1.0000 Uiso
H151 0.1735(4) 0.3923(6) 0.9195(3) 0.0348 1.0000 Uiso
H161 0.2604(4) 0.5297(7) 1.0305(3) 0.0453 1.0000 Uiso
H162 0.2225(4) 0.6752(7) 0.9856(3) 0.0453 1.0000 Uiso
H163 0.2878(4) 0.5739(7) 0.9629(3) 0.0453 1.0000 Uiso
H171 0.1095(5) 0.4359(8) 1.0098(4) 0.0588 1.0000 Uiso
H172 0.0643(5) 0.5798(8) 0.9664(4) 0.0588 1.0000 Uiso
H173 0.0335(5) 0.4258(8) 0.9281(4) 0.0588 1.0000 Uiso
H181 0.5465(4) 0.2381(7) 0.8428(4) 0.0479 1.0000 Uiso
H182 0.5611(4) 0.3228(7) 0.9179(4) 0.0479 1.0000 Uiso
H183 0.5817(4) 0.4009(7) 0.8532(4) 0.0479 1.0000 Uiso
H191 0.3589(4) 0.6229(7) 0.8461(4) 0.0483 1.0000 Uiso
H192 0.4393(4) 0.5728(7) 0.9201(4) 0.0483 1.0000 Uiso
H193 0.4599(4) 0.6509(7) 0.8553(4) 0.0483 1.0000 Uiso
H201 0.3234(6) 0.1488(8) 1.0594(4) 0.0587 1.0000 Uiso
H202 0.3903(6) 0.2343(8) 1.0315(4) 0.0587 1.0000 Uiso
H203 0.2922(6) 0.2959(8) 1.0141(4) 0.0587 1.0000 Uiso
H211 0.3510(5) -0.1016(8) 1.0044(4) 0.0648 1.0000 Uiso
H212 0.4180(5) -0.0359(8) 0.9701(4) 0.0648 1.0000 Uiso
H213 0.3348(5) -0.1313(8) 0.9195(4) 0.0648 1.0000 Uiso
H221 0.1782(5) -0.0038(7) 0.9717(4) 0.0607 1.0000 Uiso
H222 0.1322(5) 0.1253(7) 0.9157(4) 0.0607 1.0000 Uiso
H223 0.1488(5) -0.0266(7) 0.8843(4) 0.0607 1.0000 Uiso
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 0.0210(1) 0.0158(1) 0.0237(1) -0.00066(8) 0.01202(7) -0.00043(8)
Cl1 0.0356(8) 0.0551(9) 0.0330(8) 0.0075(6) 0.0139(6) -0.0147(7)
N1 0.023(2) 0.018(2) 0.017(2) -0.002(1) 0.008(2) -0.001(2)
P1 0.0363(8) 0.0252(7) 0.0328(8) 0.0099(6) 0.0151(7) 0.0045(6)
Si1 0.0209(7) 0.0247(7) 0.0255(7) 0.0003(5) 0.0082(6) -0.0030(5)
C1 0.046(4) 0.029(3) 0.043(4) -0.012(2) 0.028(3) -0.003(2)
C2 0.036(3) 0.024(3) 0.056(4) -0.010(3) 0.023(3) 0.001(2)
C3 0.043(4) 0.021(3) 0.050(4) -0.011(2) 0.022(3) -0.005(2)
C4 0.032(3) 0.031(3) 0.044(4) -0.018(3) 0.011(3) -0.004(2)
C5 0.043(4) 0.031(3) 0.029(3) -0.011(2) 0.014(3) -0.003(2)
C6 0.017(2) 0.013(2) 0.025(2) -0.001(2) 0.006(2) -0.002(2)
C7 0.024(3) 0.024(2) 0.025(3) 0.001(2) 0.003(2) -0.004(2)
C8 0.034(3) 0.032(3) 0.044(3) 0.014(3) 0.004(3) 0.004(2)
C9 0.029(3) 0.035(3) 0.071(4) 0.007(3) 0.020(3) 0.015(2)
C10 0.032(3) 0.028(3) 0.056(4) -0.005(3) 0.020(3) 0.004(2)
C11 0.021(3) 0.022(2) 0.034(3) -0.002(2) 0.012(2) -0.001(2)
C12 0.034(3) 0.030(3) 0.018(2) 0.006(2) 0.005(2) -0.006(2)
C13 0.068(5) 0.031(3) 0.048(4) 0.008(3) 0.026(4) -0.011(3)
C14 0.045(4) 0.052(4) 0.035(4) -0.006(3) 0.008(3) -0.015(3)
C15 0.027(3) 0.027(3) 0.026(3) -0.003(2) 0.014(2) -0.001(2)
C16 0.034(3) 0.038(3) 0.034(3) -0.010(2) 0.014(3) -0.007(2)
C17 0.042(4) 0.056(4) 0.040(4) -0.015(3) 0.022(3) -0.014(3)
C18 0.026(3) 0.035(3) 0.056(4) 0.005(3) 0.015(3) -0.000(2)
C19 0.034(3) 0.030(3) 0.051(4) -0.007(3) 0.015(3) -0.009(2)
C20 0.066(5) 0.051(4) 0.028(3) 0.010(3) 0.011(3) 0.007(3)
C21 0.053(4) 0.041(4) 0.058(5) 0.025(3) 0.021(4) 0.014(3)
C22 0.051(4) 0.039(3) 0.052(4) 0.009(3) 0.033(4) -0.003(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ta1 . N1 . 1.821(4)    yes
Ta1 . P1 . 2.550(1)    yes
Ta1 . Si1 . 2.574(1)    yes
Ta1 . C1 . 2.451(5)    yes
Ta1 . C3 . 2.457(5)    yes
Ta1 . C4 . 2.418(6)    yes
Ta1 . C5 . 2.388(6)    yes
Ta1 . H1 . 1.6(1)    no
N1 . C6 . 1.394(6)    yes
P1 . C20 . 1.808(7)    yes
P1 . C21 . 1.835(7)    yes
P1 . C22 . 1.836(7)    yes
P1 . H1 . 2.3(1)    no
Si1 . C18 . 1.877(6)    yes
Si1 . C19 . 1.884(6)    yes
Si1 . Cl1 . 2.177(2)    yes
Si1 . H1 . 2.3(1)    no
C1 . C2 . 1.406(9)    yes
C1 . C5 . 1.416(9)    yes
C2 . C3 . 1.417(9)    yes
C3 . C4 . 1.412(9)    yes
C4 . C5 . 1.417(9)    yes
C6 . C7 . 1.417(7)    yes
C6 . C11 . 1.426(7)    yes
C7 . C8 . 1.405(8)    yes
C7 . C12 . 1.524(8)    yes
C8 . C9 . 1.39(1)    yes
C9 . C10 . 1.37(1)    yes
C10 . C11 . 1.405(8)    yes
C11 . C15 . 1.517(8)    yes
C12 . C13 . 1.538(8)    yes
C12 . C14 . 1.530(8)    yes
C15 . C16 . 1.528(8)    yes
C15 . C17 . 1.538(8)    yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Ta1 . P1 . 100.6(1)    yes
N1 . Ta1 . Si1 . 91.8(1)    yes
P1 . Ta1 . Si1 . 120.63(5)    yes
N1 . Ta1 . C1 . 136.3(2)    yes
P1 . Ta1 . C1 . 121.6(2)    yes
Si1 . Ta1 . C1 . 77.4(1)    yes
N1 . Ta1 . C3 . 132.0(2)    yes
P1 . Ta1 . C3 . 78.8(2)    yes
Si1 . Ta1 . C3 . 130.3(1)    yes
C1 . Ta1 . C3 . 55.3(2)    yes
N1 . Ta1 . C4 . 105.1(2)    yes
P1 . Ta1 . C4 . 104.2(2)    yes
Si1 . Ta1 . C4 . 128.1(2)    yes
C1 . Ta1 . C4 . 56.4(2)    yes
C3 . Ta1 . C4 . 33.7(2)    yes
N1 . Ta1 . C5 . 107.2(2)    yes
P1 . Ta1 . C5 . 134.6(2)    yes
Si1 . Ta1 . C5 . 94.0(2)    yes
C1 . Ta1 . C5 . 34.0(2)    yes
C3 . Ta1 . C5 . 55.9(2)    yes
C4 . Ta1 . C5 . 34.3(2)    yes
N1 . Ta1 . H1 . 107.7(36)    no
P1 . Ta1 . H1 . 60.8(37)    no
Si1 . Ta1 . H1 . 60.1(37)    no
C1 . Ta1 . H1 . 103.1(38)    no
C2 . Ta1 . H1 . 91.8(36)    no
C3 . Ta1 . H1 . 113.0(36)    no
C4 . Ta1 . H1 . 145.9(36)    no
C5 . Ta1 . H1 . 136.7(38)    no
Ta1 . N1 . C6 . 171.7(4)    yes
Ta1 . P1 . C20 . 117.4(2)    yes
Ta1 . P1 . C21 . 114.8(2)    yes
C20 . P1 . C21 . 100.7(4)    yes
Ta1 . P1 . C22 . 115.1(2)    yes
C20 . P1 . C22 . 103.5(4)    yes
C21 . P1 . C22 . 103.4(3)    yes
Ta1 . P1 . H1 . 38.9(28)    no
C20 . P1 . H1 . 87.7(27)    no
C21 . P1 . H1 . 99.3(27)    no
C22 . P1 . H1 . 152.1(28)    no
Ta1 . Si1 . Cl1 . 112.05(7)    yes
Ta1 . Si1 . C18 . 121.2(2)    yes
Cl1 . Si1 . C18 . 100.4(2)    yes
Ta1 . Si1 . C19 . 113.0(2)    yes
Cl1 . Si1 . C19 . 100.6(2)    yes
C18 . Si1 . C19 . 106.9(3)    yes
Ta1 . Si1 . H1 . 38.6(28)    no
Cl1 . Si1 . H1 . 148.7(27)    no
C18 . Si1 . H1 . 92.6(28)    no
C19 . Si1 . H1 . 102.6(26)    no
Ta1 . C1 . C2 . 75.3(3)    yes
Ta1 . C1 . C5 . 70.6(3)    yes
C2 . C1 . C5 . 107.8(6)    yes
C1 . C2 . C3 . 107.7(6)    yes
Ta1 . C3 . C2 . 75.0(3)    yes
Ta1 . C3 . C4 . 71.6(3)    yes
C2 . C3 . C4 . 108.9(6)    yes
Ta1 . C4 . C3 . 74.7(3)    yes
Ta1 . C4 . C5 . 71.7(3)    yes
C3 . C4 . C5 . 106.8(5)    yes
Ta1 . C5 . C1 . 75.4(3)    yes
Ta1 . C5 . C4 . 74.0(3)    yes
C1 . C5 . C4 . 108.7(6)    yes
N1 . C6 . C7 . 120.7(4)    yes
N1 . C6 . C11 . 119.9(4)    yes
C7 . C6 . C11 . 119.4(4)    yes
C6 . C7 . C8 . 118.7(5)    yes
C6 . C7 . C12 . 121.0(5)    yes
C8 . C7 . C12 . 120.2(5)    yes
C7 . C8 . C9 . 121.6(6)    yes
C8 . C9 . C10 . 119.5(5)    yes
C9 . C10 . C11 . 121.7(6)    yes
C6 . C11 . C10 . 119.0(5)    yes
C6 . C11 . C15 . 120.3(4)    yes
C10 . C11 . C15 . 120.7(5)    yes
C7 . C12 . C13 . 112.7(5)    yes
C7 . C12 . C14 . 109.9(5)    yes
C13 . C12 . C14 . 110.9(5)    yes
C11 . C15 . C16 . 109.6(5)    yes
C11 . C15 . C17 . 113.8(5)    yes
C16 . C15 . C17 . 108.9(5)    yes

#==end

data_compound2
_database_code_CSD 133302

#  CpNb{eta-3-N(Ar)SiMe2-H}Cl(PMe3)  (Compound 2)
#  local code NBIMSI

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
CpNb{eta-3-N(Ar)SiMe2-H}Cl(PMe3)
;
_chemical_name_common
' CpNb{eta-3-N(2,6-C6H3Pri2)SiMe2-H}Cl(PMe3) '
_chemical_formula_moiety
' C22 H38 Cl N Nb P Si'
_chemical_formula_sum
' C22 H38 Cl N Nb P Si'
_chemical_formula_weight          503.95

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'
'Si'  'Si'   0.0817   0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'P'  'P'   0.1023   0.0942
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl'  'Cl'   0.1484   0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Nb'  'Nb'  -2.0727   0.6215
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'C 1 2/c 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'
'-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                    31.391(6)
_cell_length_b                    10.150(2)
_cell_length_c                    16.945(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  111.30(3)
_cell_angle_gamma                 90.00
_cell_volume                      5030.2(17)
_cell_formula_units_Z             8
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     49
_cell_measurement_theta_min       12
_cell_measurement_theta_max       15.5

_exptl_crystal_description        tablet
_exptl_crystal_colour             'dark green/brown'
_exptl_crystal_size_max           0.19
_exptl_crystal_size_mid           0.17
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_diffrn     1.331
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2112
_exptl_absorpt_coefficient_mu     0.704
_exptl_absorpt_correction_type    'psi scans'
_exptl_absorpt_correction_T_min   0.721
_exptl_absorpt_correction_T_max   0.913

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       293(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        'Stoe STADI4 4-circle diffractometer'
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        'omega  scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   '60 minutes'
_diffrn_standards_decay_%         'random variation +/- 7%'
_diffrn_reflns_number             4813
_diffrn_reflns_av_R_equivalents   0.0343
_diffrn_reflns_av_sigmaI/netI     0.0541
_diffrn_reflns_limit_h_min        -37
_diffrn_reflns_limit_h_max        36
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          2.58
_diffrn_reflns_theta_max          25.05
_reflns_number_total              4437
_reflns_number_observed           3557
_reflns_threshold_expression      >2sigma(I)
_reflns_observed_criterion        >2sigma(I)

_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'

_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 w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+46.1766P] 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        'none required'
_refine_ls_number_reflns          4437
_refine_ls_number_parameters      313
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0685
_refine_ls_R_factor_obs           0.0500
_refine_ls_wR_factor_all          0.1152
_refine_ls_wR_factor_obs          0.1031
_refine_ls_goodness_of_fit_all    1.024
_refine_ls_restrained_S_all       1.024
_refine_ls_shift/esd_max           0.003
_refine_ls_shift/esd_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.083516(14) 0.22888(4) 0.50036(2) 0.01822(13) Uani 1 d . . .
Si1 Si 0.15169(5) 0.39940(14) 0.53619(8) 0.0220(3) Uani 1 d . . .
P1 P 0.10043(5) 0.03076(14) 0.42371(8) 0.0271(3) Uani 1 d . . .
Cl1 Cl 0.07492(5) 0.06848(14) 0.60528(8) 0.0328(3) Uani 1 d . . .
N1 N 0.13740(13) 0.2971(4) 0.6024(2) 0.0202(9) Uani 1 d . . .
C1 C 0.01316(17) 0.1949(6) 0.3740(3) 0.0325(13) Uani 1 d . . .
H1A H 0.0074(4) 0.126(5) 0.339(2) 0.040(17) Uiso 1 calc R . .
C2 C 0.03697(18) 0.3100(6) 0.3674(3) 0.0313(13) Uani 1 d . . .
H2A H 0.0494(8) 0.3249(11) 0.329(2) 0.031(15) Uiso 1 calc R . .
C3 C 0.03751(17) 0.3977(6) 0.4330(3) 0.0285(12) Uani 1 d . . .
H3A H 0.0490(7) 0.477(5) 0.4418(6) 0.017(13) Uiso 1 calc R . .
C4 C 0.01557(16) 0.3305(6) 0.4815(3) 0.0291(12) Uani 1 d . . .
H4A H 0.0122(3) 0.360(2) 0.527(3) 0.042(18) Uiso 1 calc R . .
C5 C 0.00043(17) 0.2078(6) 0.4434(3) 0.0291(12) Uani 1 d . . .
H5A H -0.0126(10) 0.157(4) 0.4585(12) 0.033(18) Uiso 1 calc R . .
C6 C 0.15640(15) 0.2908(5) 0.6932(3) 0.0170(9) Uani 1 d . . .
C7 C 0.19339(15) 0.2076(5) 0.7356(3) 0.0205(10) Uani 1 d . . .
C8 C 0.21332(17) 0.2127(5) 0.8234(3) 0.0237(11) Uani 1 d . . .
H8A H 0.2373(13) 0.160(3) 0.8504(15) 0.016(12) Uiso 1 calc R . .
C9 C 0.19716(17) 0.2960(5) 0.8698(3) 0.0265(12) Uani 1 d . . .
H9A H 0.2118(8) 0.3012(6) 0.929(3) 0.025(13) Uiso 1 calc R . .
C10 C 0.15893(17) 0.3726(5) 0.8284(3) 0.0252(11) Uani 1 d . . .
H10A H 0.1466(7) 0.427(3) 0.8613(19) 0.031(15) Uiso 1 calc R . .
C12 C 0.09569(17) 0.4566(5) 0.7003(3) 0.0246(11) Uani 1 d . . .
H12A H 0.0862(4) 0.4493(6) 0.633(3) 0.015(12) Uiso 1 calc R . .
C13 C 0.10437(19) 0.6025(5) 0.7243(3) 0.0319(13) Uani 1 d . . .
H13A H 0.0760(8) 0.6541(16) 0.6947(16) 0.023(13) Uiso 1 calc R . .
H13B H 0.1296(9) 0.6358(13) 0.7070(17) 0.040(16) Uiso 1 calc R . .
H13C H 0.1132(10) 0.6125(7) 0.7867(17) 0.021(13) Uiso 1 calc R . .
C14 C 0.05601(17) 0.4024(6) 0.7231(3) 0.0348(13) Uani 1 d . . .
H14C H 0.0495(7) 0.312(3) 0.7029(18) 0.020(13) Uiso 1 calc R . .
H14A H 0.0289(8) 0.457(2) 0.6966(17) 0.041(16) Uiso 1 calc R . .
H14B H 0.0644(5) 0.404(3) 0.7844(17) 0.020(13) Uiso 1 calc R . .
C15 C 0.21112(17) 0.1080(5) 0.6879(3) 0.0274(12) Uani 1 d . . .
H15A H 0.1963(9) 0.1222(10) 0.632(4) 0.035(16) Uiso 1 calc R . .
C16 C 0.26197(19) 0.1210(6) 0.7060(4) 0.0429(15) Uani 1 d . . .
H16A H 0.2783(6) 0.106(4) 0.7637(19) 0.032(15) Uiso 1 calc R . .
H16B H 0.2683(3) 0.206(3) 0.691(2) 0.06(2) Uiso 1 calc R . .
H16C H 0.2707(4) 0.059(3) 0.674(2) 0.047(18) Uiso 1 calc R . .
C17 C 0.1996(2) -0.0318(6) 0.7074(4) 0.0420(15) Uani 1 d . . .
H17A H 0.1682(11) -0.0399(13) 0.692(2) 0.047(19) Uiso 1 calc R . .
H17B H 0.2139(11) -0.0485(15) 0.765(2) 0.06(2) Uiso 1 calc R . .
H17C H 0.2097(12) -0.092(2) 0.677(2) 0.05(2) Uiso 1 calc R . .
C18 C 0.20976(18) 0.3798(6) 0.5321(3) 0.0337(13) Uani 1 d . . .
H18A H 0.2155(5) 0.288(3) 0.526(2) 0.018(12) Uiso 1 calc R . .
H18B H 0.2322(7) 0.413(3) 0.5834(18) 0.06(2) Uiso 1 calc R . .
H18C H 0.2115(4) 0.428(3) 0.4846(19) 0.042(17) Uiso 1 calc R . .
C19 C 0.1405(2) 0.5795(5) 0.5394(3) 0.0328(13) Uani 1 d . . .
H19A H 0.1120(11) 0.5921(7) 0.543(2) 0.038(16) Uiso 1 calc R . .
H19B H 0.1412(13) 0.6191(16) 0.491(2) 0.08(2) Uiso 1 calc R . .
H19C H 0.1627(10) 0.6167(15) 0.586(2) 0.06(2) Uiso 1 calc R . .
C11 C 0.13795(16) 0.3726(5) 0.7406(3) 0.0193(10) Uani 1 d . . .
C20 C 0.0684(2) -0.1201(6) 0.4166(4) 0.0505(17) Uani 1 d . . .
H20A H 0.0721(11) -0.149(2) 0.4712(18) 0.06(2) Uiso 1 calc R . .
H20B H 0.0791(10) -0.185(3) 0.389(2) 0.053(19) Uiso 1 calc R . .
H20C H 0.0373(11) -0.1043(12) 0.386(2) 0.05(2) Uiso 1 calc R . .
C21 C 0.1585(2) -0.0278(7) 0.4767(4) 0.0487(18) Uani 1 d . . .
H21A H 0.1645(6) -0.103(4) 0.4440(18) 0.056(19) Uiso 1 calc R . .
H21B H 0.1626(5) -0.058(4) 0.535(2) 0.07(2) Uiso 1 calc R . .
H21C H 0.1804(8) 0.045(3) 0.480(2) 0.07(3) Uiso 1 calc R . .
C22 C 0.0990(2) 0.0518(7) 0.3164(3) 0.0460(17) Uani 1 d . . .
H22A H 0.0686(10) 0.073(4) 0.2798(13) 0.014(12) Uiso 1 calc R . .
H22B H 0.1083(12) -0.028(3) 0.2977(11) 0.06(2) Uiso 1 calc R . .
H22C H 0.1193(11) 0.121(3) 0.3153(5) 0.08(3) Uiso 1 calc R . .
H1   H 0.1225(16) 0.326(5) 0.457(3) 0.022(13) Uiso 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
Nb1 0.0216(2) 0.0205(2) 0.0122(2) -0.00006(18) 0.00558(16) 0.00187(19)
Si1 0.0279(7) 0.0234(8) 0.0155(6) 0.0005(6) 0.0089(5) -0.0006(6)
P1 0.0359(7) 0.0254(7) 0.0188(6) -0.0040(6) 0.0083(6) 0.0035(6)
Cl1 0.0418(8) 0.0321(7) 0.0221(6) 0.0056(6) 0.0088(5) -0.0083(6)
N1 0.021(2) 0.022(2) 0.0160(19) -0.0001(17) 0.0054(16) 0.0021(17)
C1 0.030(3) 0.037(3) 0.022(3) -0.006(3) -0.001(2) 0.004(2)
C2 0.030(3) 0.041(4) 0.016(2) 0.005(2) -0.001(2) 0.002(2)
C3 0.024(3) 0.026(3) 0.030(3) 0.003(2) 0.003(2) 0.003(2)
C4 0.020(3) 0.039(3) 0.027(3) -0.001(2) 0.007(2) 0.006(2)
C5 0.021(2) 0.038(3) 0.025(3) 0.005(2) 0.004(2) -0.004(2)
C6 0.019(2) 0.018(2) 0.013(2) 0.0000(19) 0.0064(18) -0.0007(19)
C7 0.022(2) 0.019(3) 0.020(2) -0.003(2) 0.0067(19) -0.001(2)
C8 0.023(2) 0.024(3) 0.021(2) 0.006(2) 0.004(2) 0.004(2)
C9 0.034(3) 0.031(3) 0.011(2) 0.002(2) 0.005(2) -0.003(2)
C10 0.030(3) 0.030(3) 0.017(2) -0.005(2) 0.011(2) -0.005(2)
C12 0.028(3) 0.028(3) 0.017(2) 0.001(2) 0.007(2) 0.003(2)
C13 0.038(3) 0.034(3) 0.027(3) 0.005(2) 0.017(2) 0.013(3)
C14 0.026(3) 0.043(4) 0.035(3) 0.004(3) 0.011(2) 0.006(3)
C15 0.031(3) 0.023(3) 0.024(3) -0.003(2) 0.006(2) 0.009(2)
C16 0.042(3) 0.042(4) 0.045(4) -0.009(3) 0.015(3) 0.013(3)
C17 0.056(4) 0.030(3) 0.034(3) -0.005(3) 0.009(3) 0.006(3)
C18 0.036(3) 0.036(3) 0.031(3) 0.003(3) 0.014(2) -0.001(3)
C19 0.048(3) 0.031(3) 0.023(3) 0.001(2) 0.018(3) -0.001(3)
C11 0.025(2) 0.018(2) 0.016(2) 0.000(2) 0.0096(19) 0.000(2)
C20 0.059(5) 0.039(4) 0.057(4) -0.013(3) 0.026(4) -0.004(3)
C21 0.056(4) 0.050(4) 0.033(3) -0.014(3) 0.007(3) 0.022(4)
C22 0.068(4) 0.050(4) 0.021(3) 0.000(3) 0.017(3) 0.014(4)

_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
Nb1 N1 2.051(4) . ?
Nb1 C3 2.264(5) . ?
Nb1 C4 2.285(5) . ?
Nb1 C2 2.344(5) . ?
Nb1 C5 2.439(5) . ?
Nb1 C1 2.479(5) . ?
Nb1 Cl1 2.4965(13) . ?
Nb1 P1 2.5522(14) . ?
Nb1 Si1 2.6458(15) . ?
Nb1 H1 1.91(5) . ?
Si1 N1 1.704(4) . ?
Si1 C18 1.860(5) . ?
Si1 C19 1.866(6) . ?
Si1 H1 1.52(5) . ?
P1 C20 1.812(7) . ?
P1 C22 1.814(5) . ?
P1 C21 1.816(6) . ?
N1 C6 1.434(5) . ?
C1 C5 1.378(7) . ?
C1 C2 1.413(8) . ?
C1 H1A 0.8857 . ?
C2 C3 1.419(7) . ?
C2 H2A 0.8878 . ?
C3 C4 1.423(7) . ?
C3 H3A 0.8729 . ?
C4 C5 1.404(8) . ?
C4 H4A 0.8659 . ?
C5 H5A 0.7595 . ?
C6 C7 1.405(6) . ?
C6 C11 1.418(6) . ?
C7 C8 1.390(6) . ?
C7 C15 1.520(6) . ?
C8 C9 1.371(7) . ?
C8 H8A 0.9004 . ?
C9 C10 1.388(7) . ?
C9 H9A 0.9427 . ?
C10 C11 1.390(6) . ?
C10 H10A 0.9622 . ?
C12 C11 1.515(7) . ?
C12 C14 1.534(7) . ?
C12 C13 1.534(7) . ?
C12 H12A 1.0639 . ?
C13 H13A 0.9967 . ?
C13 H13B 0.9967 . ?
C13 H13C 0.9967 . ?
C14 H14C 0.9741 . ?
C14 H14A 0.9741 . ?
C14 H14B 0.9741 . ?
C15 C16 1.518(7) . ?
C15 C17 1.530(8) . ?
C15 H15A 0.9008 . ?
C16 H16A 0.9361 . ?
C16 H16B 0.9361 . ?
C16 H16C 0.9361 . ?
C17 H17A 0.9284 . ?
C17 H17B 0.9284 . ?
C17 H17C 0.9284 . ?
C18 H18A 0.9606 . ?
C18 H18B 0.9606 . ?
C18 H18C 0.9606 . ?
C19 H19A 0.9252 . ?
C19 H19B 0.9252 . ?
C19 H19C 0.9252 . ?
C20 H20A 0.9364 . ?
C20 H20B 0.9364 . ?
C20 H20C 0.9364 . ?
C21 H21A 0.9957 . ?
C21 H21B 0.9957 . ?
C21 H21C 0.9957 . ?
C22 H22A 0.9552 . ?
C22 H22B 0.9552 . ?
C22 H22C 0.9552 . ?

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
N1 Nb1 C3 110.45(18) . . ?
N1 Nb1 C4 114.05(18) . . ?
C3 Nb1 C4 36.46(19) . . ?
N1 Nb1 C2 136.64(18) . . ?
C3 Nb1 C2 35.82(19) . . ?
C4 Nb1 C2 58.9(2) . . ?
N1 Nb1 C5 143.04(16) . . ?
C3 Nb1 C5 58.1(2) . . ?
C4 Nb1 C5 34.39(19) . . ?
C2 Nb1 C5 56.42(19) . . ?
N1 Nb1 C1 168.08(17) . . ?
C3 Nb1 C1 57.6(2) . . ?
C4 Nb1 C1 56.54(19) . . ?
C2 Nb1 C1 33.92(18) . . ?
C5 Nb1 C1 32.54(17) . . ?
N1 Nb1 Cl1 83.62(11) . . ?
C3 Nb1 Cl1 129.66(14) . . ?
C4 Nb1 Cl1 93.27(14) . . ?
C2 Nb1 Cl1 136.25(14) . . ?
C5 Nb1 Cl1 81.26(14) . . ?
C1 Nb1 Cl1 103.38(14) . . ?
N1 Nb1 P1 115.77(11) . . ?
C3 Nb1 P1 123.52(14) . . ?
C4 Nb1 P1 129.86(15) . . ?
C2 Nb1 P1 87.71(14) . . ?
C5 Nb1 P1 96.87(13) . . ?
C1 Nb1 P1 74.67(14) . . ?
Cl1 Nb1 P1 86.84(5) . . ?
N1 Nb1 Si1 40.10(11) . . ?
C3 Nb1 Si1 86.30(15) . . ?
C4 Nb1 Si1 111.90(15) . . ?
C2 Nb1 Si1 99.25(14) . . ?
C5 Nb1 Si1 143.86(14) . . ?
C1 Nb1 Si1 132.99(14) . . ?
Cl1 Nb1 Si1 123.42(5) . . ?
P1 Nb1 Si1 109.37(5) . . ?
N1 Nb1 H1 72.8(14) . . ?
C3 Nb1 H1 78.3(14) . . ?
C4 Nb1 H1 114.1(14) . . ?
C2 Nb1 H1 73.3(14) . . ?
C5 Nb1 H1 129.3(14) . . ?
C1 Nb1 H1 103.5(14) . . ?
Cl1 Nb1 H1 149.2(14) . . ?
P1 Nb1 H1 85.9(14) . . ?
Si1 Nb1 H1 34.4(14) . . ?
N1 Si1 C18 117.1(2) . . ?
N1 Si1 C19 118.7(2) . . ?
C18 Si1 C19 107.7(3) . . ?
N1 Si1 Nb1 50.81(13) . . ?
C18 Si1 Nb1 130.0(2) . . ?
C19 Si1 Nb1 120.14(19) . . ?
N1 Si1 H1 93.7(18) . . ?
C18 Si1 H1 101.5(17) . . ?
C19 Si1 H1 116.6(18) . . ?
Nb1 Si1 H1 45.4(17) . . ?
C20 P1 C22 102.8(3) . . ?
C20 P1 C21 101.0(3) . . ?
C22 P1 C21 100.9(3) . . ?
C20 P1 Nb1 119.1(2) . . ?
C22 P1 Nb1 118.9(2) . . ?
C21 P1 Nb1 111.3(2) . . ?
C6 N1 Si1 128.8(3) . . ?
C6 N1 Nb1 141.6(3) . . ?
Si1 N1 Nb1 89.09(16) . . ?
C5 C1 C2 108.3(5) . . ?
C5 C1 Nb1 72.2(3) . . ?
C2 C1 Nb1 67.8(3) . . ?
C5 C1 H1A 125.8 . . ?
C2 C1 H1A 125.8 . . ?
Nb1 C1 H1A 125.8 . . ?
C1 C2 C3 108.2(5) . . ?
C1 C2 Nb1 78.3(3) . . ?
C3 C2 Nb1 69.0(3) . . ?
C1 C2 H2A 125.9 . . ?
C3 C2 H2A 125.9 . . ?
Nb1 C2 H2A 118.6 . . ?
C2 C3 C4 106.3(5) . . ?
C2 C3 Nb1 75.2(3) . . ?
C4 C3 Nb1 72.6(3) . . ?
C2 C3 H3A 126.8 . . ?
C4 C3 H3A 126.8 . . ?
Nb1 C3 H3A 117.6 . . ?
C5 C4 C3 108.2(5) . . ?
C5 C4 Nb1 78.8(3) . . ?
C3 C4 Nb1 71.0(3) . . ?
C5 C4 H4A 125.9 . . ?
C3 C4 H4A 125.9 . . ?
Nb1 C4 H4A 116.3 . . ?
C1 C5 C4 108.8(5) . . ?
C1 C5 Nb1 75.3(3) . . ?
C4 C5 Nb1 66.8(3) . . ?
C1 C5 H5A 125.6 . . ?
C4 C5 H5A 125.6 . . ?
Nb1 C5 H5A 123.8 . . ?
C7 C6 C11 119.6(4) . . ?
C7 C6 N1 121.3(4) . . ?
C11 C6 N1 119.1(4) . . ?
C8 C7 C6 119.5(4) . . ?
C8 C7 C15 119.0(4) . . ?
C6 C7 C15 121.5(4) . . ?
C9 C8 C7 121.3(5) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C9 C10 C11 121.9(5) . . ?
C9 C10 H10A 119.1 . . ?
C11 C10 H10A 119.1 . . ?
C11 C12 C14 110.0(4) . . ?
C11 C12 C13 112.4(4) . . ?
C14 C12 C13 111.2(4) . . ?
C11 C12 H12A 107.7 . . ?
C14 C12 H12A 107.7 . . ?
C13 C12 H12A 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C16 C15 C7 113.4(4) . . ?
C16 C15 C17 110.5(5) . . ?
C7 C15 C17 110.0(4) . . ?
C16 C15 H15A 107.6 . . ?
C7 C15 H15A 107.6 . . ?
C17 C15 H15A 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C11 C6 118.3(4) . . ?
C10 C11 C12 118.7(4) . . ?
C6 C11 C12 123.0(4) . . ?
P1 C20 H20A 109.5 . . ?
P1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
P1 C21 H21A 109.5 . . ?
P1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
P1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P1 C22 H22A 109.5 . . ?
P1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
P1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_diffrn_measured_fraction_theta_max    0.468
_diffrn_reflns_theta_full              25.05
_diffrn_measured_fraction_theta_full   0.468
_refine_diff_density_max    1.427
_refine_diff_density_min   -0.868
_refine_diff_density_rms    0.110

#==end