Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2002

data_ort
_database_code_CSD                  157841

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Georgii I. Nikonov'
'Sergei F. Vyboishchikov'
'Lyudmila G. Kuzmina'
'Judith A. K. Howard'

_publ_requested_journal       'Chemical Communications'


_publ_contact_author_name     	'Dr Georgii I. Nikonov'  
_publ_contact_author_address 
;
Chemistry Department
Moscow State University
Chemistry Department, Moscow State
Moscow
119899
RUSSIAN FEDERATION
;

_publ_contact_author_email       'NIKONOV@ORG.CHEM.MSU.SU'
_publ_contact_author_fax '+7 095 932 8846' 
_publ_contact_author_phone '+7 095 939 1234' 

_publ_section_title		
;
Serendipitous syntheses and structures of [Cp2NbH{SiMe2)2(mu-NR)}].
;


_audit_creation_method SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common ? 
_chemical_formula_moiety 'Cp2NbH(SiMe2)2NBu-t'
_chemical_formula_structural ? 
_chemical_formula_analytical ? 
_chemical_formula_sum 'C18 H32 N Nb Si2' 
_chemical_formula_weight 411.54 
_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' 
'Si' 'Si' 0.0817 0.0704 
'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 'orthorhombic' 
_symmetry_space_group_name_H-M 'Pnma' 

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

_cell_length_a 17.4105(4) 
_cell_length_b 13.2514(3) 
_cell_length_c 8.6175(2) 
_cell_angle_alpha 90.00 
_cell_angle_beta 90.00 
_cell_angle_gamma 90.00 
_cell_volume 1988.17(8) 
_cell_formula_units_Z 4 
_cell_measurement_temperature 150.0(2) 
_cell_measurement_reflns_used ? 
_cell_measurement_theta_min ? 
_cell_measurement_theta_max ? 

_exptl_crystal_description 'block'
_exptl_crystal_colour 'yellow' 
_exptl_crystal_size_max 0.36 
_exptl_crystal_size_mid 0.34 
_exptl_crystal_size_min 0.24 
_exptl_crystal_density_meas ? 
_exptl_crystal_density_diffrn 1.375 
_exptl_crystal_density_method ? 
_exptl_crystal_F_000 864 
_exptl_absorpt_coefficient_mu 0.724 
_exptl_absorpt_correction_type 'none'
_exptl_absorpt_correction_T_min ? 
_exptl_absorpt_correction_T_max ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature 150.0(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 12810 
_diffrn_reflns_av_R_equivalents 0.0970 
_diffrn_reflns_av_sigmaI/netI 0.0467 
_diffrn_reflns_limit_h_min -22 
_diffrn_reflns_limit_h_max 22 
_diffrn_reflns_limit_k_min -17 
_diffrn_reflns_limit_k_max 16 
_diffrn_reflns_limit_l_min -11 
_diffrn_reflns_limit_l_max 11 
_diffrn_reflns_theta_min 2.34 
_diffrn_reflns_theta_max 26.50 
_reflns_number_total 2151 
_reflns_number_observed 1993 
_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 52 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^)+(0.0266P)^2^+5.1267P] 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 ? 
_refine_ls_extinction_method none 
_refine_ls_extinction_coef ? 
_refine_ls_number_reflns 2099 
_refine_ls_number_parameters 200 
_refine_ls_number_restraints 0 
_refine_ls_R_factor_all 0.0545 
_refine_ls_R_factor_obs 0.0500 
_refine_ls_wR_factor_all 0.1170 
_refine_ls_wR_factor_obs 0.1122 
_refine_ls_goodness_of_fit_all 1.228 
_refine_ls_goodness_of_fit_obs 1.246 
_refine_ls_restrained_S_all 1.246 
_refine_ls_restrained_S_obs 1.246 
_refine_ls_shift/esd_max 0.000 
_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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
Nb1 Nb 0.81312(3) 0.7500 0.59972(5) 0.0253(2) Uani 1 d S . 
Si1 Si 0.87285(8) 0.7500 0.3124(2) 0.0287(4) Uani 1 d S . 
Si2 Si 0.96556(8) 0.7500 0.5568(2) 0.0297(4) Uani 1 d S . 
N1 N 0.9717(2) 0.7500 0.3533(5) 0.0291(10) Uani 1 d S . 
C1 C 0.8324(3) 0.9278(4) 0.5673(5) 0.0360(9) Uani 1 d . . 
C2 C 0.7568(3) 0.9062(4) 0.5152(5) 0.0399(10) Uani 1 d . . 
C3 C 0.7141(2) 0.8714(4) 0.6437(5) 0.0383(10) Uani 1 d . . 
C4 C 0.7627(3) 0.8734(4) 0.7756(5) 0.0397(11) Uani 1 d . . 
C5 C 0.8355(3) 0.9081(4) 0.7289(5) 0.0408(11) Uani 1 d . . 
C6 C 0.8463(3) 0.8621(5) 0.1857(6) 0.053(2) Uani 1 d . . 
C7 C 1.0198(3) 0.8615(5) 0.6425(5) 0.0480(13) Uani 1 d . . 
C8 C 1.0389(3) 0.7500 0.2484(7) 0.0378(14) Uani 1 d S . 
C9 C 1.0502(7) 0.8699(10) 0.2133(14) 0.052(3) Uani 0.50 d P . 
C10 C 1.1120(5) 0.7128(9) 0.3199(12) 0.050(3) Uani 0.50 d P . 
C11 C 1.0247(6) 0.7000(9) 0.0949(10) 0.047(2) Uani 0.50 d P . 
H9A H 1.0131(65) 0.8990(77) 0.1596(134) 0.025(28) Uiso 0.50 d P . 
H9B H 1.0560(75) 0.9047(88) 0.3224(145) 0.065(34) Uiso 0.50 d P . 
H9C H 1.0964(62) 0.8722(77) 0.1637(119) 0.045(27) Uiso 0.50 d P . 
H10A H 1.1041(54) 0.6371(75) 0.3264(101) 0.026(22) Uiso 0.50 d P . 
H10B H 1.1485(44) 0.7147(51) 0.2445(86) 0.021(21) Uiso 0.50 d P . 
H10C H 1.1272(40) 0.7500 0.4113(80) 0.037(18) Uiso 1 d S . 
H11A H 1.0169(77) 0.6250(103) 0.1086(134) 0.044(36) Uiso 0.50 d P . 
H11B H 0.9756(50) 0.7368(179) 0.0289(99) 0.065(37) Uiso 0.50 d P . 
H11C H 1.0705(51) 0.7041(61) 0.0145(105) 0.040(26) Uiso 0.50 d P . 
H1A H 0.8711(26) 0.9503(33) 0.5103(52) 0.032(11) Uiso 1 d . . 
H2A H 0.7373(33) 0.9169(40) 0.4168(59) 0.058(16) Uiso 1 d . . 
H3A H 0.6624(33) 0.8525(38) 0.6469(59) 0.052(15) Uiso 1 d . . 
H4A H 0.7508(34) 0.8497(40) 0.8751(62) 0.061(16) Uiso 1 d . . 
H5A H 0.8762(28) 0.9156(38) 0.7889(57) 0.046(14) Uiso 1 d . . 
H6A H 0.8685(34) 0.8561(41) 0.0956(63) 0.055(16) Uiso 1 d . . 
H6B H 0.8636(36) 0.9275(49) 0.2216(73) 0.074(22) Uiso 1 d . . 
H6C H 0.7836(35) 0.8644(41) 0.1664(62) 0.063(16) Uiso 1 d . . 
H7A H 1.0774(37) 0.8560(41) 0.6232(60) 0.061(16) Uiso 1 d . . 
H7B H 1.0172(33) 0.8615(40) 0.7441(70) 0.060(16) Uiso 1 d . . 
H7C H 0.9999(33) 0.9278(41) 0.6141(59) 0.053(16) Uiso 1 d . . 
H2 H 0.9015 0.7500 0.7117 0.035 Uiso 0.50 d SP . 
H1 H 0.7736 0.7500 0.4186 0.035 Uiso 0.50 d SP . 

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 0.0192(2) 0.0326(3) 0.0241(2) 0.000 0.0072(2) 0.000 
Si1 0.0206(7) 0.0514(11) 0.0140(6) 0.000 -0.0018(5) 0.000 
Si2 0.0167(6) 0.0552(11) 0.0174(6) 0.000 -0.0030(5) 0.000 
N1 0.018(2) 0.054(3) 0.016(2) 0.000 0.003(2) 0.000 
C1 0.032(2) 0.035(2) 0.041(2) -0.003(2) 0.004(2) -0.004(2) 
C2 0.033(2) 0.050(3) 0.037(2) 0.003(2) -0.004(2) 0.005(2) 
C3 0.025(2) 0.045(3) 0.045(2) -0.007(2) 0.002(2) 0.003(2) 
C4 0.039(2) 0.049(3) 0.031(2) -0.016(2) 0.010(2) -0.003(2) 
C5 0.037(2) 0.051(3) 0.035(2) -0.011(2) -0.005(2) -0.010(2) 
C6 0.041(3) 0.090(5) 0.028(2) 0.028(3) 0.005(2) 0.013(3) 
C7 0.026(2) 0.086(4) 0.031(2) -0.009(2) -0.004(2) -0.013(3) 
C8 0.025(3) 0.059(4) 0.029(3) 0.000 0.011(2) 0.000 
C9 0.044(6) 0.057(7) 0.054(6) -0.005(5) 0.024(5) -0.021(6) 
C10 0.024(4) 0.078(10) 0.049(5) -0.013(5) 0.013(4) 0.002(4) 
C11 0.047(5) 0.063(7) 0.030(4) -0.020(4) 0.019(4) -0.011(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 
Nb1 C3 2.389(4) 7_575 ? 
Nb1 C3 2.389(4) . ? 
Nb1 C1 2.396(5) . ? 
Nb1 C1 2.396(5) 7_575 ? 
Nb1 C4 2.397(4) . ? 
Nb1 C4 2.397(4) 7_575 ? 
Nb1 C2 2.403(5) 7_575 ? 
Nb1 C2 2.403(5) . ? 
Nb1 C5 2.405(5) . ? 
Nb1 C5 2.405(5) 7_575 ? 
Nb1 Si2 2.6796(15) . ? 
Nb1 Si1 2.6856(14) . ? 
Si1 N1 1.756(5) . ? 
Si1 C6 1.901(5) 7_575 ? 
Si1 C6 1.901(5) . ? 
Si1 Si2 2.654(2) . ? 
Si2 N1 1.757(4) . ? 
Si2 C7 1.903(5) . ? 
Si2 C7 1.903(5) 7_575 ? 
N1 C8 1.479(7) . ? 
C1 C5 1.418(6) . ? 
C1 C2 1.420(6) . ? 
C2 C3 1.411(6) . ? 
C3 C4 1.418(6) . ? 
C4 C5 1.407(6) . ? 
C8 C10 1.497(11) 7_575 ? 
C8 C10 1.497(11) . ? 
C8 C11 1.500(10) . ? 
C8 C11 1.500(10) 7_575 ? 
C8 C9 1.630(13) . ? 
C8 C9 1.630(13) 7_575 ? 
C9 C11 1.45(2) 7_575 ? 
C9 C10 1.79(2) 7_575 ? 
C10 C10 0.99(2) 7_575 ? 
C10 C9 1.79(2) 7_575 ? 
C11 C11 1.33(2) 7_575 ? 
C11 C9 1.45(2) 7_575 ? 

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 
C3 Nb1 C3 84.7(2) 7_575 . ? 
C3 Nb1 C1 141.4(2) 7_575 . ? 
C3 Nb1 C1 57.1(2) . . ? 
C3 Nb1 C1 57.1(2) 7_575 7_575 ? 
C3 Nb1 C1 141.4(2) . 7_575 ? 
C1 Nb1 C1 159.0(2) . 7_575 ? 
C3 Nb1 C4 95.5(2) 7_575 . ? 
C3 Nb1 C4 34.5(2) . . ? 
C1 Nb1 C4 56.9(2) . . ? 
C1 Nb1 C4 142.8(2) 7_575 . ? 
C3 Nb1 C4 34.5(2) 7_575 7_575 ? 
C3 Nb1 C4 95.5(2) . 7_575 ? 
C1 Nb1 C4 142.8(2) . 7_575 ? 
C1 Nb1 C4 56.9(2) 7_575 7_575 ? 
C4 Nb1 C4 86.1(2) . 7_575 ? 
C3 Nb1 C2 34.2(2) 7_575 7_575 ? 
C3 Nb1 C2 109.5(2) . 7_575 ? 
C1 Nb1 C2 150.3(2) . 7_575 ? 
C1 Nb1 C2 34.43(15) 7_575 7_575 ? 
C4 Nb1 C2 129.0(2) . 7_575 ? 
C4 Nb1 C2 56.9(2) 7_575 7_575 ? 
C3 Nb1 C2 109.5(2) 7_575 . ? 
C3 Nb1 C2 34.2(2) . . ? 
C1 Nb1 C2 34.43(15) . . ? 
C1 Nb1 C2 150.3(2) 7_575 . ? 
C4 Nb1 C2 56.9(2) . . ? 
C4 Nb1 C2 129.0(2) 7_575 . ? 
C2 Nb1 C2 118.9(2) 7_575 . ? 
C3 Nb1 C5 129.1(2) 7_575 . ? 
C3 Nb1 C5 57.1(2) . . ? 
C1 Nb1 C5 34.35(15) . . ? 
C1 Nb1 C5 152.6(2) 7_575 . ? 
C4 Nb1 C5 34.1(2) . . ? 
C4 Nb1 C5 111.2(2) 7_575 . ? 
C2 Nb1 C5 163.1(2) 7_575 . ? 
C2 Nb1 C5 57.1(2) . . ? 
C3 Nb1 C5 57.1(2) 7_575 7_575 ? 
C3 Nb1 C5 129.1(2) . 7_575 ? 
C1 Nb1 C5 152.6(2) . 7_575 ? 
C1 Nb1 C5 34.35(15) 7_575 7_575 ? 
C4 Nb1 C5 111.2(2) . 7_575 ? 
C4 Nb1 C5 34.1(2) 7_575 7_575 ? 
C2 Nb1 C5 57.1(2) 7_575 7_575 ? 
C2 Nb1 C5 163.1(2) . 7_575 ? 
C5 Nb1 C5 121.3(2) . 7_575 ? 
C3 Nb1 Si2 137.46(11) 7_575 . ? 
C3 Nb1 Si2 137.46(11) . . ? 
C1 Nb1 Si2 81.10(11) . . ? 
C1 Nb1 Si2 81.10(11) 7_575 . ? 
C4 Nb1 Si2 116.75(11) . . ? 
C4 Nb1 Si2 116.75(11) 7_575 . ? 
C2 Nb1 Si2 111.25(11) 7_575 . ? 
C2 Nb1 Si2 111.25(11) . . ? 
C5 Nb1 Si2 84.46(12) . . ? 
C5 Nb1 Si2 84.46(12) 7_575 . ? 
C3 Nb1 Si1 115.20(11) 7_575 . ? 
C3 Nb1 Si1 115.20(11) . . ? 
C1 Nb1 Si1 80.70(11) . . ? 
C1 Nb1 Si1 80.70(11) 7_575 . ? 
C4 Nb1 Si1 136.47(12) . . ? 
C4 Nb1 Si1 136.47(12) 7_575 . ? 
C2 Nb1 Si1 83.03(11) 7_575 . ? 
C2 Nb1 Si1 83.03(11) . . ? 
C5 Nb1 Si1 111.35(11) . . ? 
C5 Nb1 Si1 111.35(11) 7_575 . ? 
Si2 Nb1 Si1 59.29(4) . . ? 
N1 Si1 C6 110.7(2) . 7_575 ? 
N1 Si1 C6 110.7(2) . . ? 
C6 Si1 C6 102.8(4) 7_575 . ? 
N1 Si1 Si2 40.96(14) . . ? 
C6 Si1 Si2 127.1(2) 7_575 . ? 
C6 Si1 Si2 127.1(2) . . ? 
N1 Si1 Nb1 101.20(14) . . ? 
C6 Si1 Nb1 115.8(2) 7_575 . ? 
C6 Si1 Nb1 115.8(2) . . ? 
Si2 Si1 Nb1 60.24(4) . . ? 
N1 Si2 C7 110.9(2) . . ? 
N1 Si2 C7 110.9(2) . 7_575 ? 
C7 Si2 C7 101.9(4) . 7_575 ? 
N1 Si2 Si1 40.94(15) . . ? 
C7 Si2 Si1 127.6(2) . . ? 
C7 Si2 Si1 127.6(2) 7_575 . ? 
N1 Si2 Nb1 101.4(2) . . ? 
C7 Si2 Nb1 116.0(2) . . ? 
C7 Si2 Nb1 116.0(2) 7_575 . ? 
Si1 Si2 Nb1 60.47(4) . . ? 
C8 N1 Si1 130.8(4) . . ? 
C8 N1 Si2 131.1(4) . . ? 
Si1 N1 Si2 98.1(2) . . ? 
C5 C1 C2 108.0(4) . . ? 
C5 C1 Nb1 73.2(3) . . ? 
C2 C1 Nb1 73.1(3) . . ? 
C3 C2 C1 107.8(4) . . ? 
C3 C2 Nb1 72.3(3) . . ? 
C1 C2 Nb1 72.5(3) . . ? 
C2 C3 C4 108.0(4) . . ? 
C2 C3 Nb1 73.5(3) . . ? 
C4 C3 Nb1 73.1(3) . . ? 
C5 C4 C3 108.3(4) . . ? 
C5 C4 Nb1 73.3(3) . . ? 
C3 C4 Nb1 72.5(2) . . ? 
C4 C5 C1 107.8(4) . . ? 
C4 C5 Nb1 72.6(3) . . ? 
C1 C5 Nb1 72.5(3) . . ? 
N1 C8 C10 114.9(5) . 7_575 ? 
N1 C8 C10 114.9(5) . . ? 
C10 C8 C10 38.4(10) 7_575 . ? 
N1 C8 C11 114.1(5) . . ? 
C10 C8 C11 130.5(7) 7_575 . ? 
C10 C8 C11 111.0(7) . . ? 
N1 C8 C11 114.1(5) . 7_575 ? 
C10 C8 C11 111.0(7) 7_575 7_575 ? 
C10 C8 C11 130.5(7) . 7_575 ? 
C11 C8 C11 52.4(10) . 7_575 ? 
N1 C8 C9 102.1(4) . . ? 
C10 C8 C9 69.7(7) 7_575 . ? 
C10 C8 C9 107.2(8) . . ? 
C11 C8 C9 106.7(7) . . ? 
C11 C8 C9 54.9(6) 7_575 . ? 
N1 C8 C9 102.1(4) . 7_575 ? 
C10 C8 C9 107.2(8) 7_575 7_575 ? 
C10 C8 C9 69.7(7) . 7_575 ? 
C11 C8 C9 54.9(6) . 7_575 ? 
C11 C8 C9 106.7(7) 7_575 7_575 ? 
C9 C8 C9 154.4(8) . 7_575 ? 
C11 C9 C8 58.0(6) 7_575 . ? 
C11 C9 C10 98.8(10) 7_575 7_575 ? 
C8 C9 C10 51.7(6) . 7_575 ? 
C10 C10 C8 70.8(5) 7_575 . ? 
C10 C10 C9 127.8(5) 7_575 7_575 ? 
C8 C10 C9 58.7(5) . 7_575 ? 
C11 C11 C9 129.8(7) 7_575 7_575 ? 
C11 C11 C8 63.8(5) 7_575 . ? 
C9 C11 C8 67.1(7) 7_575 . ? 

_refine_diff_density_max 1.720 
_refine_diff_density_min -0.905 
_refine_diff_density_rms 0.097