Neutron and X-ray Diffraction Studies and DFT Calculations of Asymmetric Bis(silyl) Niobocene Hydrides
Dorogov, Konstantin Yu.; Dumont, Elise; Ho, Nam-Nhat; Churakov, Andrei V.; Kuzmina, Lyudmila G.; Poblet, Josep-Maria; Schultz, Arthur J.; Howard, Judith A. K.; Bau, Robert; Lledos, Agusti; Nikonov, Georgii I.; Organometallics 23 (2004) 2845–2847; doi:10.1021/om034239a

data_4062570
_publ_contact_author
; Dr Georgii I. Nikonov
  Department of Chemistry, Moscow State University
  Vorob'evy Gory, Moscow 119899, Russia
;
_publ_section_title
'Neutron and X-ray Diffraction Studies and DFT Calculations of Asymmetric Bis(silyl) Niobocene Hydrides'
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2845
_journal_page_last               2847
_journal_paper_doi               10.1021/om034239a
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C14 H24 Cl Nb Si2'
_chemical_formula_weight         376.87
_chemical_name_common
;  
(dimethylsilyl)(dimethylchlorosilyl)niobocene hydrid 
;
_chemical_name_systematic
;  
bis(cyclopentadienyl)(dimethylsilyl)
(dimethylchlorosilyl)(hydrido) niobium (V) 
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2004-04-16T09:30
_audit_creation_method           SHELXL-97
_audit_update_record
' 2004-04-16T09:30  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.627(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6876(4)
_cell_length_b                   8.5767(3)
_cell_length_c                   14.5354(4)
_cell_measurement_reflns_used    4966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.29
_cell_measurement_theta_min      2.37
_cell_volume                     1702.96(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10937
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.987
_exptl_absorpt_correction_T_max  0.56074
_exptl_absorpt_correction_T_min  0.43381
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.43
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3709
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+1.1278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                3478
_reflns_number_total             3709
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om034239asi20040421_035914-EDITED.cif
_cod_data_source_block           p
_cod_database_code               4062570