In vitro cytotoxicity and catalytic evaluation of dioxidovanadium(V) complexes in azohydrazone ligand environment
Mohanty, Monalisa; MAURYA, Shailendra K; Banerjee, Atanu; Patra, Sushree Aradhana; Maurya, Mannar Ram; Crochet, Aurelien; Brzezinski, Krzysztof; Dinda, Rupam; New Journal of Chemistry 43 (2019) 17680–17695; doi:10.1039/C9NJ01815H

data_7058542
_publ_section_title
;
 In vitro cytotoxicity and catalytic evaluation of dioxidovanadium(V)
 complexes in azohydrazone ligand environment
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17680
_journal_page_last               17695
_journal_paper_doi               10.1039/C9NJ01815H
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C20 H14 N4 O4 V, C6 H16 N'
_chemical_formula_sum            'C26 H30 N5 O4 V'
_chemical_formula_weight         527.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-13 deposited with the CCDC.    2019-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.002(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9776(6)
_cell_length_b                   8.6271(7)
_cell_length_c                   22.0397(18)
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.42
_cell_measurement_theta_min      1.85
_cell_volume                     1323.48(19)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2009)'
_computing_data_collection       'X-Area (Stoe & Cie, 2009)'
_computing_data_reduction        'X-RED32(Stoe & Cie, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1554
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17318
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.214
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Stoe IPDS2'
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.9303
_exptl_absorpt_correction_T_min  0.7082
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 711 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.0077(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2275
_reflns_number_total             4684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01815h2.cif
_cod_data_source_block           platon_pl
_cod_database_code               7058542
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-H5A
 0.85 with sigma of 0.02
 N5-C21
 1.44 with sigma of 0.02
3. Rigid bond restraints
 C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C26, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C25 \\sim C26 \\sim N5: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C21) = Uanis(C25) = Uanis(C23)
Uanis(C22) = Uanis(C26) = Uanis(C24)
5.a Ternary CH refined with riding coordinates and stretchable bonds:
 N5(H5A)
5.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
5.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              32420
_olex2_submission_special_instructions 'No special instructions were received'