Vanadium(V) Complexes with Substituted 1,5-bis(2-hydroxybenzaldehyde)carbohydrazones and Their Use As Catalyst Precursors in Oxidation of Cyclohexane.
Dragancea, Diana; Talmaci, Natalia; Shova, Sergiu; Novitchi, Ghenadie; Darvasiová, Denisa; Rapta, Peter; Breza, Martin; Galanski, Markus; Kož\?íšek, Jozef; Martins, Nuno M. R.; Martins, Luísa M D R S; Pombeiro, Armando J. L.; Arion, Vladimir B.; Inorganic chemistry 55 (2016) 9187–9203; doi:10.1021/acs.inorgchem.6b01011

data_4348138
_publ_section_title
;
 Vanadium(V) Complexes with Substituted
 1,5-bis(2-hydroxybenzaldehyde)carbohydrazones and Their Use As Catalyst
 Precursors in Oxidation of Cyclohexane.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9187
_journal_page_last               9203
_journal_paper_doi               10.1021/acs.inorgchem.6b01011
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C15 H11 N4 O7 V2, C H4 O, H4 N'
_chemical_formula_sum            'C16 H19 N5 O8 V2'
_chemical_formula_weight         511.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                65.847(7)
_cell_angle_beta                 84.709(6)
_cell_angle_gamma                74.717(7)
_cell_formula_units_Z            2
_cell_length_a                   9.1328(7)
_cell_length_b                   10.9497(8)
_cell_length_c                   11.1790(7)
_cell_measurement_reflns_used    1982
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      26.8430
_cell_measurement_theta_min      1.9910
_cell_volume                     983.82(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -76.00  -38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352 -178.0000   90.0000 38

  2 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000 -180.0000 47

  3 omega  -14.00   23.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.9352  -99.0000 -120.0000 37

  4 omega    9.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570   57.0000  120.0000 72

  5 omega   35.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570  178.0000    0.0000 42

  6 omega    0.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570   38.0000   60.0000 79

  7 omega   -3.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.3570  -19.0000 -120.0000 42
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0599336000
_diffrn_orient_matrix_UB_12      0.0242131000
_diffrn_orient_matrix_UB_13      0.0113921000
_diffrn_orient_matrix_UB_21      0.0440783000
_diffrn_orient_matrix_UB_22      -0.0690581000
_diffrn_orient_matrix_UB_23      0.0299230000
_diffrn_orient_matrix_UB_31      0.0308116000
_diffrn_orient_matrix_UB_32      0.0040787000
_diffrn_orient_matrix_UB_33      -0.0617391000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7173
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3467
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                2507
_reflns_number_total             3467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01011_si_002.cif
_cod_data_source_block           shi_2249_dili
_cod_original_cell_volume        983.82(13)
_cod_database_code               4348138
_chemical_oxdiff_formula         'C20H42 N6 O6 V1'
_chemical_oxdiff_usercomment     TN3_38
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups, All O(H) groups
2. Restrained distances
 N5-H5B \\sim N5-H5C \\sim N5-H5D \\sim N5-H5A
 with sigma of 0.01
3.a Riding coordinates:
 N5(H5A,H5B,H5C,H5D)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2A), C3(H3), C4(H4), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13),
  C14(H14)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
3.d Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'