Exploring the effect of hydroxylic and non-hydroxylic solvents on the reaction of [VIVO(β-diketonate)2] with 2-Aminobenzoylhydrazide in aerobic and anaerobic conditions. Valence delocalisation in mixed-valence VIV-O-VV species
Biswas, Nirmalendu; Patra, Debashis; Mondal, Bipul; Bera, Sachinath; Acharyya, Swarnali; Biswas, Anup Kumar; Mukhopadhyay, Titas Kumar; Pal, Amrita; Drew, Michael G. B.; Ghosh, Tapas; Dalton Trans.  (2017) –; doi:10.1039/C7DT01776F

data_7043638
_publ_section_title
;
 Exploring the effect of hydroxylic and non-hydroxylic solvents on the
 reaction of [VIVO(\b-diketonate)2] with 2-Aminobenzoylhydrazide in
 aerobic and anaerobic conditions. Valence delocalisation in mixed-valence
 VIV-O-VV species
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01776F
_journal_year                    2017
_chemical_formula_moiety         'C34 H30 N6 O7 V2'
_chemical_formula_sum            'C34 H30 N6 O7 V2'
_chemical_formula_weight         736.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-03
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2017-01-25 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.955(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.5136(2)
_cell_length_b                   12.2629(12)
_cell_length_c                   18.5071(17)
_cell_measurement_reflns_used    13083
_cell_measurement_temperature    99.7(4)
_cell_measurement_theta_max      25.0070
_cell_measurement_theta_min      1.9900
_cell_volume                     6470.3(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.7(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9160
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -23.00   29.00   1.0000   71.1500
omega____ theta____ kappa____ phi______ frames
    -       27.3512   38.0000    0.0000 52

  2 omega   38.00  108.00   1.0000   71.1500
omega____ theta____ kappa____ phi______ frames
    -       27.3512   38.0000    0.0000 70

  3 omega    8.00   82.00   1.0000   71.1500
omega____ theta____ kappa____ phi______ frames
    -       27.3512   77.0000  120.0000 74

  4 omega  -19.00   79.00   1.0000   71.1500
omega____ theta____ kappa____ phi______ frames
    -       27.3512  -99.0000 -150.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0089324000
_diffrn_orient_matrix_UB_12      -0.0540138000
_diffrn_orient_matrix_UB_13      -0.0010550000
_diffrn_orient_matrix_UB_21      -0.0230042000
_diffrn_orient_matrix_UB_22      -0.0208353000
_diffrn_orient_matrix_UB_23      0.0046344000
_diffrn_orient_matrix_UB_31      -0.0034846000
_diffrn_orient_matrix_UB_32      -0.0010230000
_diffrn_orient_matrix_UB_33      -0.0380226000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24641
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         11399
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+5.9117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                9693
_reflns_number_total             11399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01776f2.cif
_cod_data_source_block           8
_cod_original_cell_volume        6470.28(10)
_cod_database_code               7043638
_chemical_oxdiff_formula         C34H30N6O7V2
_reflns_odcompleteness_completeness 86.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32