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_4071719
_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         'C19 H29 N2 V'
_chemical_formula_sum            'C19 H29 N2 V'
_chemical_formula_weight         336.39
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2005-02-22  09:19:32'
_audit_creation_method
;
 PLATON <TABLE ACC> option 
 SHELXL97-2 & Manual Editing 
;
_audit_update_record
;
?

2008-04-02 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 116.596(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.380(1)
_cell_length_b                   11.0573(9)
_cell_length_c                   13.949(1)
_cell_measurement_reflns_used    4615
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.46
_cell_volume                     1845.3(2)
_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, 2004) 
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_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  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14733
_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         26.73
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.9335
_exptl_absorpt_correction_T_min  0.8176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2000))'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         3905
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0576P)^2^+1.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1292
_reflns_number_gt                2797
_reflns_number_total             3905
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8003306-file001.cif
_cod_data_source_block           CP970
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071719
_vrn_publ_code_frame_time_sec    10.0
_vrn_publ_code_meas_time_hour    8.0