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_4306957
_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 H24 Br Nb Si2'
_chemical_formula_sum            'C14 H24 Br Nb Si2'
_chemical_formula_weight         421.33
_chemical_name_common
;  
(dimethylsilyl)(dimethylbromosilyl)niobocene hydrid 
;
_chemical_name_systematic
;  
bis(cyclopentadienyl)(dimethylsilyl)
(dimethylbromosilyl)(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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.408(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.9449(5)
_cell_length_b                   8.9330(3)
_cell_length_c                   26.0528(9)
_cell_measurement_temperature    120.0(2)
_cell_volume                     3431.3(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       '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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            12752
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_T_max  0.6665
_exptl_absorpt_correction_T_min  0.5438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            light-beige
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.709
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.173
_refine_ls_extinction_coef       0.0010(2)
_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   1.183
_refine_ls_goodness_of_fit_obs   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3423
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.178
_refine_ls_restrained_S_obs      1.281
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         -6.012
_refine_ls_shift/esd_mean        0.117
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+3.8077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1690
_refine_ls_wR_factor_obs         0.1535
_reflns_number_observed          2654
_reflns_number_total             3749
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ic061314bsi20060716_084620_03.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+3.8077P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+3.8077P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4306957