Relative Reactivity of the Metal−Amido versus Metal−Imido Bond in Linked Cp-Amido and Half-Sandwich Complexes of Vanadium
Bouwkamp, Marco W.; Batinas, Aurora A.; Witte, Peter T.; Hubregtse, Ton; Dam, Jeroen; Meetsma, Auke; Teuben, Jan H.; Hessen, Bart; Organometallics 27 (2008) 4071–; doi:10.1021/om8003306

data_4071720
_publ_section_title
;
 Relative Reactivity of the Metal&#x2212;Amido versus Metal&#x2212;Imido
 Bond in Linked Cp-Amido and Half-Sandwich Complexes of Vanadium
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4071
_journal_paper_doi               10.1021/om8003306
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C22 H34 N2 O V, C24 H20 B'
_chemical_formula_sum            'C46 H54 B N2 O V'
_chemical_formula_weight         712.70
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2004-03-03  09:11:52'
_audit_creation_method
;
 PLATON <TABLE ACC> option
 SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?

2008-04-02 # Formatted by publCIF
;
_cell_angle_alpha                93.630(2)
_cell_angle_beta                 94.974(2)
_cell_angle_gamma                104.100(1)
_cell_formula_units_Z            2
_cell_length_a                   9.2873(9)
_cell_length_b                   12.827(1)
_cell_length_c                   16.830(2)
_cell_measurement_reflns_used    3813
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.44
_cell_volume                     1929.8(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2003)
 PLATON (Spek, 1994)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
  Bruker Smart Apex
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13857
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_max  0.9544
_exptl_absorpt_correction_T_min  0.8591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, 2001))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.54
_refine_diff_density_rms         0.09
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+5.22P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2313
_reflns_number_gt                4562
_reflns_number_total             6687
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8003306-file002.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan'
changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4071720
_vrn_publ_code_void_volume       18.9
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.0