#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:22:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179107 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/69/4306963.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306963
loop_
_publ_author_name
'Konstantin Yu. Dorogov'
'Muhammed Yousufuddin'
'Nam-Nhat Ho'
'Andrei V. Churakov'
'Lyudmila G. Kuzmina'
'Arthur J. Schultz'
'Sax A. Mason'
'Judith A. K. Howard'
'Dmitry A. Lemenovskii'
'Robert Bau'
'Georgii I. Nikonov'
_publ_contact_author
; Dr Georgii I. Nikonov
  Chemistry Department, Brock University, 
  500 Glenridge Ave., St Catharines, L2S 3A1, 
  ON, Canada
;
_publ_contact_author_email       gnikonov@brocku.ca
_publ_section_title
;
Syntheses and Structures of Asymmetric Bis(silyl) Niobocene Hydrides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              147
_journal_page_last               160
_journal_paper_doi               10.1021/ic061314b
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C14 H23 Br Cl Nb Si2'
_chemical_formula_weight         455.77
_chemical_name_common
;  
(dimethylbromosilyl)(dimethylchlorosilyl)niobocene hydrid 
;
_chemical_name_systematic
;  
bis(cyclopentadienyl)(dimethylbromosilyl)
(dimethylchlorosilyl)(hydrido) niobium (V) 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6006(5)
_cell_length_b                   13.1582(4)
_cell_length_c                   8.4922(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1854.99(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            12244
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    3.063
_exptl_absorpt_correction_T_max  0.7917
_exptl_absorpt_correction_T_min  0.4224
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0201P)²+0.4830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                2283
_reflns_number_total             2568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061314bsi20060716_084620_09.cif
_cod_data_source_block           9
_cod_database_code               4306963
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.324229(9) 0.2500 0.099418(19) 0.01379(5) Uani 1 2 d S . .
Br1 Br 0.3543(3) -0.0630(3) 0.1464(4) 0.0224(3) Uani 0.4763(17) 1 d P A 1
Cl1 Cl 0.3478(6) -0.0544(8) 0.1400(9) 0.0298(14) Uani 0.5237(17) 1 d P A 2
Si1 Si 0.38835(2) 0.09478(3) 0.24115(4) 0.01746(8) Uani 1 1 d . . .
C1 C 0.23105(11) 0.2500 0.3143(3) 0.0222(4) Uani 1 2 d S . .
C2 C 0.21396(8) 0.16256(12) 0.22211(18) 0.0229(3) Uani 1 1 d . . .
C3 C 0.18809(8) 0.19601(12) 0.07319(19) 0.0239(3) Uani 1 1 d . . .
C4 C 0.44691(12) 0.2500 -0.0493(2) 0.0224(4) Uani 1 2 d S . .
C5 C 0.40275(9) 0.16280(12) -0.09510(18) 0.0243(3) Uani 1 1 d . . .
C6 C 0.33127(10) 0.19628(13) -0.16726(18) 0.0278(3) Uani 1 1 d . . .
C7 C 0.36505(10) 0.07787(13) 0.45561(19) 0.0262(3) Uani 1 1 d . A .
C8 C 0.50086(9) 0.08317(13) 0.2302(2) 0.0280(3) Uani 1 1 d . A .
H1 H 0.3894(15) 0.2500 0.252(3) 0.040(8) Uiso 1 2 d S . .
H5A H 0.4203(10) 0.0967(14) -0.085(2) 0.027(5) Uiso 1 1 d . . .
H7A H 0.3920(11) 0.0215(15) 0.495(2) 0.038(5) Uiso 1 1 d . . .
H7B H 0.3836(11) 0.1377(16) 0.514(2) 0.044(6) Uiso 1 1 d . . .
H7C H 0.3101(12) 0.0704(15) 0.481(2) 0.036(5) Uiso 1 1 d . . .
H3A H 0.1736(9) 0.1542(14) -0.014(2) 0.026(4) Uiso 1 1 d . . .
H6A H 0.2928(10) 0.1568(15) -0.209(2) 0.035(5) Uiso 1 1 d . . .
H1A H 0.2486(14) 0.2500 0.417(3) 0.022(6) Uiso 1 2 d S . .
H2A H 0.2156(10) 0.0963(13) 0.257(2) 0.026(5) Uiso 1 1 d . . .
H4A H 0.4983(14) 0.2500 -0.004(3) 0.026(6) Uiso 1 2 d S . .
H8A H 0.5180(10) 0.0220(14) 0.282(2) 0.031(5) Uiso 1 1 d . . .
H8B H 0.5226(12) 0.0822(15) 0.127(2) 0.042(6) Uiso 1 1 d . . .
H8C H 0.5219(11) 0.1370(16) 0.280(2) 0.041(6) Uiso 1 1 d . . .
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'
Si Si 0.0817 0.0704 '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'
Br Br -0.2901 2.4595 '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'
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
C6 Nb1 C6 34.63(8) . 7_565 ?
C6 Nb1 C3 92.66(6) . 7_565 ?
C6 Nb1 C3 82.45(5) 7_565 7_565 ?
C6 Nb1 C3 82.45(5) . . ?
C6 Nb1 C3 92.66(6) 7_565 . ?
C3 Nb1 C3 34.74(7) 7_565 . ?
C6 Nb1 C1 139.39(6) . . ?
C6 Nb1 C1 139.39(6) 7_565 . ?
C3 Nb1 C1 57.13(6) 7_565 . ?
C3 Nb1 C1 57.13(6) . . ?
C6 Nb1 C5 34.27(5) . . ?
C6 Nb1 C5 57.22(5) 7_565 . ?
C3 Nb1 C5 126.51(6) 7_565 . ?
C3 Nb1 C5 108.01(5) . . ?
C1 Nb1 C5 151.33(4) . . ?
C6 Nb1 C5 57.22(5) . 7_565 ?
C6 Nb1 C5 34.27(5) 7_565 7_565 ?
C3 Nb1 C5 108.01(5) 7_565 7_565 ?
C3 Nb1 C5 126.51(6) . 7_565 ?
C1 Nb1 C5 151.33(4) . 7_565 ?
C5 Nb1 C5 57.21(8) . 7_565 ?
C6 Nb1 C4 57.01(6) . . ?
C6 Nb1 C4 57.01(6) 7_565 . ?
C3 Nb1 C4 139.27(6) 7_565 . ?
C3 Nb1 C4 139.27(6) . . ?
C1 Nb1 C4 162.10(7) . . ?
C5 Nb1 C4 34.36(5) . . ?
C5 Nb1 C4 34.36(5) 7_565 . ?
C6 Nb1 C2 107.99(5) . . ?
C6 Nb1 C2 126.45(6) 7_565 . ?
C3 Nb1 C2 57.27(5) 7_565 . ?
C3 Nb1 C2 34.22(5) . . ?
C1 Nb1 C2 34.48(5) . . ?
C5 Nb1 C2 118.98(5) . . ?
C5 Nb1 C2 160.65(5) 7_565 . ?
C4 Nb1 C2 151.28(4) . . ?
C6 Nb1 C2 126.45(6) . 7_565 ?
C6 Nb1 C2 107.99(5) 7_565 7_565 ?
C3 Nb1 C2 34.22(5) 7_565 7_565 ?
C3 Nb1 C2 57.27(5) . 7_565 ?
C1 Nb1 C2 34.48(4) . 7_565 ?
C5 Nb1 C2 160.65(5) . 7_565 ?
C5 Nb1 C2 118.98(5) 7_565 7_565 ?
C4 Nb1 C2 151.28(4) . 7_565 ?
C2 Nb1 C2 57.29(7) . 7_565 ?
C6 Nb1 Si1 130.94(4) . 7_565 ?
C6 Nb1 Si1 100.81(4) 7_565 7_565 ?
C3 Nb1 Si1 101.40(4) 7_565 7_565 ?
C3 Nb1 Si1 131.84(4) . 7_565 ?
C1 Nb1 Si1 84.92(3) . 7_565 ?
C5 Nb1 Si1 118.21(4) . 7_565 ?
C5 Nb1 Si1 73.75(4) 7_565 7_565 ?
C4 Nb1 Si1 84.04(3) . 7_565 ?
C2 Nb1 Si1 119.22(4) . 7_565 ?
C2 Nb1 Si1 74.61(4) 7_565 7_565 ?
C6 Nb1 Si1 100.81(4) . . ?
C6 Nb1 Si1 130.94(4) 7_565 . ?
C3 Nb1 Si1 131.84(4) 7_565 . ?
C3 Nb1 Si1 101.40(4) . . ?
C1 Nb1 Si1 84.92(3) . . ?
C5 Nb1 Si1 73.75(4) . . ?
C5 Nb1 Si1 118.21(4) 7_565 . ?
C4 Nb1 Si1 84.04(3) . . ?
C2 Nb1 Si1 74.61(4) . . ?
C2 Nb1 Si1 119.22(4) 7_565 . ?
Si1 Nb1 Si1 103.616(18) 7_565 . ?
C7 Si1 C8 104.12(8) . . ?
C7 Si1 Cl1 101.88(19) . . ?
C8 Si1 Cl1 102.0(3) . . ?
C7 Si1 Br1 100.49(9) . . ?
C8 Si1 Br1 98.87(13) . . ?
Cl1 Si1 Br1 4.0(4) . . ?
C7 Si1 Nb1 117.30(5) . . ?
C8 Si1 Nb1 116.66(6) . . ?
Cl1 Si1 Nb1 112.8(3) . . ?
Br1 Si1 Nb1 116.56(13) . . ?
C2 C1 C2 108.20(19) . 7_565 ?
C2 C1 Nb1 73.06(10) . . ?
C2 C1 Nb1 73.06(10) 7_565 . ?
C3 C2 C1 107.65(14) . . ?
C3 C2 Nb1 72.09(8) . . ?
C1 C2 Nb1 72.46(9) . . ?
C2 C3 C3 108.24(9) . 7_565 ?
C2 C3 Nb1 73.69(8) . . ?
C3 C3 Nb1 72.63(4) 7_565 . ?
C5 C4 C5 108.26(19) 7_565 . ?
C5 C4 Nb1 72.82(9) 7_565 . ?
C5 C4 Nb1 72.82(9) . . ?
C6 C5 C4 107.61(15) . . ?
C6 C5 Nb1 72.03(8) . . ?
C4 C5 Nb1 72.82(9) . . ?
C5 C6 C6 108.25(10) . 7_565 ?
C5 C6 Nb1 73.70(9) . . ?
C6 C6 Nb1 72.69(4) 7_565 . ?
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 C6 2.3753(15) . ?
Nb1 C6 2.3753(15) 7_565 ?
Nb1 C3 2.3794(13) 7_565 ?
Nb1 C3 2.3794(13) . ?
Nb1 C1 2.3923(19) . ?
Nb1 C5 2.3967(14) . ?
Nb1 C5 2.3967(14) 7_565 ?
Nb1 C4 2.3966(19) . ?
Nb1 C2 2.4000(14) . ?
Nb1 C2 2.4000(14) 7_565 ?
Nb1 Si1 2.5986(4) 7_565 ?
Nb1 Si1 2.5986(4) . ?
Br1 Si1 2.298(4) . ?
Cl1 Si1 2.246(8) . ?
Si1 C7 1.8751(16) . ?
Si1 C8 1.8764(16) . ?
C1 C2 1.420(2) . ?
C1 C2 1.420(2) 7_565 ?
C2 C3 1.406(2) . ?
C3 C3 1.421(3) 7_565 ?
C4 C5 1.4159(19) 7_565 ?
C4 C5 1.4159(19) . ?
C5 C6 1.406(2) . ?
C6 C6 1.414(3) 7_565 ?
