Combined single crystal neutron diffraction and solution NMR relaxation studies of mono- and bis(silyl) substituted niobocene hydrides with nonclassical interligand interactions
Bakhmutov, Vladimir I.; Howard, Judith A. K.; Keen, David A.; Kuzmina, Lyudmila G.; Leech, Michael A.; Nikonov, Georgii I.; Vorontsov, Eugenii V.; Wilson, Chick C.; Journal of the Chemical Society, Dalton Transactions  (2000) 1631–; doi:10.1039/b000089m

data_7009332
_publ_section_title
;
 Combined single crystal neutron diffraction and solution NMR
 relaxation studies of mono- and bis(silyl) substituted niobocene
 hydrides with nonclassical interligand interactions
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1631
_journal_paper_doi               10.1039/b000089m
_journal_year                    2000
_chemical_formula_moiety         'C14 H23 Cl2 Nb1 Si2'
_chemical_formula_sum            'C14 H23 Cl2 Nb Si2'
_chemical_formula_weight         411.32
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             99-06-16
_audit_creation_method           CRYSTALS_ver_07-07-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   16.584(3)
_cell_length_b                   13.214(3)
_cell_length_c                   8.419(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    100
_cell_volume                     1844.9(7)
_computing_cell_refinement
;
?
;
_computing_data_collection
;
?
;
_computing_data_reduction
;
?
;
_computing_molecular_graphics
;
 CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      100
_diffrn_measurement_device       SXD
_diffrn_measurement_method       'Time of flight LAUE diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'ISIS spallation source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.5-5.0
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8886
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent and it is
calculated as: mu = 0.99 + 1.07 * lambda  [cm^-1]
;
_exptl_crystal_colour            'pale beige'
_exptl_crystal_density_diffrn    1.48
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_size_max          2.00
_exptl_crystal_size_mid          2.00
_exptl_crystal_size_min          1.00
_refine_diff_density_max         'not applicable'
_refine_diff_density_min         'not applicable'
_refine_ls_extinction_coef       103.3
_refine_ls_extinction_method     'Becker-Coppens Lorentzian model'
_refine_ls_goodness_of_fit_obs   1.185
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1537
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Chebychev polynomial with   3 parameters (Carruthers & Watkin, 1979)
 0.303 0.221 0.356E-01
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.098
_reflns_number_gt                1424
_reflns_number_total             1537
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            b000089m.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct_Methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1844.9(6)
_cod_original_formula_sum        'C14 H23 Cl2 Nb1 Si2'
_cod_database_code               7009332