Syntheses and Structures of Asymmetric Bis(silyl) Niobocene Hydrides
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; Inorganic Chemistry 46 (2007) 147–160; doi:10.1021/ic061314b

data_4306960
_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_moiety         'C14 H23 Cl F Nb Si2'
_chemical_formula_sum            'C14 H23 Cl F Nb Si2'
_chemical_formula_weight         394.86
_chemical_name_common
;  
(dimethylchlorosilyl)(dimethylfluorosilyl)niobocene hydrid 
;
_chemical_name_systematic
;  
bis(cyclopentadienyl)(dimethylchlorosilyl)
(dimethylfluorosilyl)(hydrido) niobium (V) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.760(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.6577(5)
_cell_length_b                   9.0181(3)
_cell_length_c                   25.8731(9)
_cell_measurement_reflns_used    5285
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      30.076
_cell_measurement_theta_min      2.663
_cell_volume                     3370.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            11019
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.8884
_exptl_absorpt_correction_T_min  0.7936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0281P)^2^+2.8666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                3595
_reflns_number_total             4288
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061314bsi20060716_084620_06.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4306960