Bis(acetylamido)oxovanadium(IV) complexes: solid state and solution studies
Debbie C. Crans; A. Raza Khan; Mohammed Mahroof-Tahir; Sujit Mondal; Susie M. Miller; Agnete la Cour; Oren P. Anderson; Tamás Jakusch; Tamás Kiss; J. Chem. Soc., Dalton Trans.  (2001) 3337–3345; doi:10.1039/b101718g

data_7010650
_publ_section_title
;
 Bis(acetylamido)oxovanadium(IV) complexes: solid state and solution
 studies
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3337
_journal_page_last               3345
_journal_paper_doi               10.1039/b101718g
_journal_year                    2001
_chemical_formula_sum            'C18 H26 N2 O5 V'
_chemical_formula_weight         401.35
_chemical_name_common            VO(acac-NMe2)2
_chemical_name_systematic
Bis(N,N'-dimethylacetylacetamido)oxovanadium(IV)
_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                 90.19(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.005(2)
_cell_length_b                   19.610(6)
_cell_length_c                   14.601(4)
_cell_measurement_temperature    166(2)
_cell_volume                     2005.7(10)
_computing_cell_refinement       'SMART, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      166(2)
_diffrn_measurement_device       'Bruker AXS SMART CCD area detector'
_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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10311
_diffrn_reflns_theta_max         28.65
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'prismatic shape'
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_hydrogen_treatment    'riding model used in refinement'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_obs          0.0613
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+1.7875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1823
_refine_ls_wR_factor_obs         0.1604
_reflns_number_observed          3445
_reflns_number_total             4767
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b101718g.txt
_cod_data_source_block           dc36sad
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+1.7875P] 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^)+(0.0924P)^2^+1.7875P] 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        2005.5(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010650
_abstract
;
VO(acac-NME2)2 exists as a discrete mononulear complex with the vanadium'
atom in a distorted square pyramidal coordination environment. Two oxygen 
atoms of each of the NMe2-acac- ligands (V-O = 1.976(2), 1.958(2), 1.958(2) 
1.966(2) A) coordinate to the vanadium atom in the equatorial plane.  The oxo 
group (V-O = 1.597(2) A) occupies the apical position and the vanadium atom 
lies 0.59 A above the least-aquares equatorial plane.'
;