Donor Properties of the Vanadyl Ion: Reactions of Vanadyl Salicylaldimine β-Ketimine and Acetylacetonato Complexes with Groups 14 and 15 Lewis Acids
B. Cashin; D. Cunningham; P. Daly; P. McArdle; M. Munroe; N. Ní Chonchubhair; Inorganic Chemistry 41 (2002) 773–782; doi:10.1021/ic010366s

data_4317537
_publ_section_title
;
 Donor Properties of the Vanadyl Ion: Reactions of Vanadyl Salicylaldimine
 \b-Ketimine and Acetylacetonato Complexes with Groups 14 and 15 Lewis
 Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              773
_journal_page_last               782
_journal_paper_doi               10.1021/ic010366s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C50 H49 Cl2 N5 O11 Pb V2'
_chemical_formula_weight         1275.91
_chemical_name_common            PbPh2Cl2.VO(3-MeOsalen).VO(3-MeOsalen).H2O
_chemical_name_systematic
;
  {Diphenyllead 
dichloride.[N,N'-bis(3-methoxysalicylidene)ethane-1,2-diaminato]oxovan 
adium(IV)}(1/1).[N,N'-bis(3-methoxysalicylidene)ethane-1,2-diaminato]m 
onoaqua oxovanadium(IV)(1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.559(11)
_cell_angle_beta                 82.276(8)
_cell_angle_gamma                66.166(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0059(11)
_cell_length_b                   12.872(2)
_cell_length_c                   19.360(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2596.1(6)
_computing_cell_refinement
'XDS (Wolfgan Kabsch, University of Heidelberg, 2000)'
_computing_data_collection       XDS
_computing_data_reduction        'XCAD (McArdle & Higgins, 1995)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Marr Research 180mm Image Plate'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10071
_diffrn_reflns_theta_full        21.07
_diffrn_reflns_theta_max         21.07
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    3.753
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0214
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.3899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0509
_reflns_number_gt                4925
_reflns_number_total             5154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010366s_9.cif
_cod_data_source_block           PbPh2Cl2.VO(3-MeOsalen).VO(3-MeOsalen).H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2596.2(5)
_cod_database_code               4317537