Molecular Rearrangements of a Low-Valent Niobium Amide: Ligand C−H Bond Oxidative Addition and Reductive Elimination
Tayebani, Maryam; Feghali, Khalil; Gambarotta, Sandro; Yap, Glenn; Organometallics 17 (1998) 4282–; doi:10.1021/om980302y

data_4078402
_publ_section_title
;
 Molecular Rearrangements of a Low-Valent Niobium Amide:&#x00A0; Ligand
 C&#x2212;H Bond Oxidative Addition and Reductive Elimination
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4282
_journal_paper_doi               10.1021/om980302y
_journal_volume                  17
_journal_year                    1998
_chemical_formula_sum            'C79 H89 Li N9 Nb2'
_chemical_formula_weight         1357.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.936(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4635(8)
_cell_length_b                   39.259(2)
_cell_length_c                   14.4266(9)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     7597.1(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere scans'
_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  0.1974
_diffrn_reflns_av_sigmaI/netI    0.1920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27521
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             2844
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.771
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.220
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         8696
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.220
_refine_ls_R_factor_all          0.1559
_refine_ls_R_factor_obs          0.0913
_refine_ls_shift/esd_max         0.094
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2911
_refine_ls_wR_factor_obs         0.2505
_reflns_number_observed          4834
_reflns_number_total             8705
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980302y.cif
_cod_data_source_block           sg010
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1486P)^2^+0.0000P] 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^)+(0.1486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7597.0(8)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078402