Unexpected reduction of vanadium(IV) to vanadium(III) in the presence of the chelate ligands 2,2'-bipyridine (bpy) and 1,8-hydroxyquinoline (Hquin)
Manos, Manolis J.; Tasiopoulos, Anastasios J.; Raptopoulou, Catherine; Terzis, Aris; Woollins, J. Derek; Slawin, Alexandra M. Z.; Keramidas, Anastasios D.; Kabanos, Themistoklis A.; Journal of the Chemical Society, Dalton Transactions  (2001) 1556–; doi:10.1039/b102095l

data_7010673
_publ_section_title
;
 Unexpected reduction of vanadium(IV) to vanadium(III) in the presence
 of the chelate ligands 2,2'-bipyridine (bpy) and 1,8-hydroxyquinoline
 (Hquin)
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1556
_journal_paper_doi               10.1039/b102095l
_journal_year                    2001
_chemical_compound_source        -
_chemical_formula_analytical     'C27.50 H20 N3 O3.50 V'
_chemical_formula_moiety         'C27 H18 N3 O3 V.[C H4 O]0.5'
_chemical_formula_structural     'C27.50 H20 N3 O3.50 V'
_chemical_formula_sum            'C27.5 H20 N3 O3.5 V'
_chemical_formula_weight         499.40
_chemical_melting_point          ?
_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                 97.921(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9438(10)
_cell_length_b                   13.4026(13)
_cell_length_c                   16.912(2)
_cell_measurement_reflns_used    106
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     2456.9(4)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_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      298(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10461
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.819375
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       prism
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .27
_exptl_crystal_size_min          .19
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0012(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.916
_refine_ls_goodness_of_fit_obs   0.969
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_restrained_S_obs      0.969
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_obs          0.0412
_refine_ls_shift/esd_max         0.072
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+0.2070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1708
_refine_ls_wR_factor_obs         0.1326
_reflns_number_observed          2756
_reflns_number_total             3515
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b102095l.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' 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^)+(0.1206P)^2^+0.2070P] 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^)+(0.1206P)^2^+0.2070P] 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      P2(1)/n
_cod_original_formula_sum        'C27.50 H20 N3 O3.50 V'
_cod_database_code               7010673