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_4078401
_publ_section_title
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 Molecular Rearrangements of a Low-Valent Niobium Amide:&#x00A0; Ligand
 C&#x2212;H Bond Oxidative Addition and Reductive Elimination
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_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            'C12 H32 Cl5 N4 Nb2'
_chemical_formula_weight         595.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.843(9)
_cell_length_b                   8.509(9)
_cell_length_c                   13.218(7)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    117(2)
_cell_measurement_theta_max      14.20
_cell_measurement_theta_min      10.31
_cell_volume                     2232(3)
_computing_cell_refinement       MSC/AFC
_computing_data_collection       MSC/AFC
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      117(2)
_diffrn_measurement_device       'AFC6S diffractometer'
_diffrn_measurement_method       2theta-omega
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1904
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  0.99618
_exptl_absorpt_correction_T_min  0.65304
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    idealized
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_refine_ls_number_reflns         1899
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_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_obs          0.0222
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0590
_refine_ls_wR_factor_obs         0.0457
_reflns_number_observed          1697
_reflns_number_total             1904
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om980302y.cif
_cod_data_source_block           sg001
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.2698P] 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^)+(0.0235P)^2^+0.2698P] 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      Pna2(1)
_cod_database_code               4078401