#------------------------------------------------------------------------------
#$Date: 2020-10-06 13:25:26 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257823 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/92/7059261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7059261
loop_
_publ_author_name
'Biswas, Nirmalendu'
'Bera, Sachinath'
'Sepay, Nayim'
'Pal, Amrita'
'Halder, Tanmoy'
'Ray, Sudipta'
'Acharyya, Swarnali'
'Biswas, Anup Kumar'
'Drew, Michael G. B.'
'Ghosh, Tapas'
_publ_section_title
;
 Simultaneous formation of non-oxidovanadium(iv) and oxidovanadium(v)
 complexes incorporating phenol-based hydrazone ligands in aerobic
 conditions
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3700
_journal_page_last               3716
_journal_paper_doi               10.1039/C9NJ06114B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C32 H30 N6 O6 V'
_chemical_formula_weight         645.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-25 deposited with the CCDC.	2020-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.035(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0164(9)
_cell_length_b                   9.5390(9)
_cell_length_c                   27.584(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2896.8(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1178
_diffrn_reflns_av_unetI/netI     0.1887
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            4539
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.158
_exptl_absorpt_coefficient_mu    0.400
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             1340
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2413
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.1015
_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/[σ²(Fo²)+(0.0059P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1473
_reflns_number_total             2413
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9nj06114b2.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 7059256--7059262.cif.

 Adding full bibliography for 7059256--7059262.cif.
;
_cod_original_cell_volume        2896.9(4)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7059261
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
V1 V 0.750000 0.12387(17) 0.500000 0.0160(4) Uani 1 2 d S T P
O1 O 0.8349(4) -0.0209(4) 0.53238(15) 0.0178(11) Uani 1 1 d . . .
O2 O 0.7826(4) 0.1942(4) 0.43714(15) 0.0192(11) Uani 1 1 d . . .
O4 O 1.0925(4) 0.0213(5) 0.70582(16) 0.0299(13) Uani 1 1 d . . .
N1 N 0.9171(5) 0.2256(5) 0.50746(19) 0.0178(13) Uani 1 1 d . . .
N2 N 0.9488(5) 0.3104(5) 0.46841(19) 0.0216(14) Uani 1 1 d . . .
N3 N 1.0699(6) 0.4730(7) 0.4052(2) 0.0348(18) Uani 1 1 d D . .
H3A H 1.068(6) 0.449(7) 0.4356(10) 0.042 Uiso 1 1 d D U .
H3B H 1.130(4) 0.520(7) 0.394(2) 0.042 Uiso 1 1 d D U .
C1 C 0.9782(6) 0.1134(7) 0.5814(2) 0.0194(16) Uani 1 1 d . . .
C2 C 0.9009(6) -0.0038(7) 0.5732(2) 0.0206(17) Uani 1 1 d . . .
C3 C 0.8947(6) -0.1050(7) 0.6089(2) 0.0221(17) Uani 1 1 d . . .
H3 H 0.845298 -0.182893 0.603423 0.026 Uiso 1 1 calc R U .
C4 C 0.9591(6) -0.0938(7) 0.6520(2) 0.0226(18) Uani 1 1 d . . .
H4 H 0.953058 -0.163460 0.675384 0.027 Uiso 1 1 calc R U .
C5 C 1.0343(6) 0.0230(7) 0.6610(2) 0.0219(18) Uani 1 1 d . . .
C6 C 1.0424(5) 0.1226(7) 0.6262(2) 0.0206(16) Uani 1 1 d . . .
H6 H 1.092372 0.199695 0.632154 0.025 Uiso 1 1 calc R U .
C7 C 0.9975(6) 0.2154(6) 0.5433(2) 0.0167(16) Uani 1 1 d . U .
C8 C 0.8717(6) 0.2842(7) 0.4325(3) 0.0226(17) Uani 1 1 d . . .
C9 C 0.8807(6) 0.3521(7) 0.3848(2) 0.0185(17) Uani 1 1 d . . .
C10 C 0.9783(6) 0.4393(7) 0.3726(3) 0.0252(18) Uani 1 1 d . . .
C11 C 0.9804(7) 0.4910(7) 0.3251(3) 0.033(2) Uani 1 1 d . . .
H11 H 1.043006 0.550748 0.316758 0.040 Uiso 1 1 calc R U .
C12 C 0.8939(7) 0.4567(8) 0.2910(3) 0.036(2) Uani 1 1 d . . .
H12 H 0.899018 0.490742 0.259530 0.043 Uiso 1 1 calc R U .
C13 C 0.7975(6) 0.3704(8) 0.3030(2) 0.0302(19) Uani 1 1 d . . .
H13 H 0.737561 0.347429 0.279723 0.036 Uiso 1 1 calc R U .
C14 C 0.7917(6) 0.3199(7) 0.3491(2) 0.0237(18) Uani 1 1 d . . .
H14 H 0.727064 0.262608 0.356988 0.028 Uiso 1 1 calc R U .
C15 C 1.1133(5) 0.2977(7) 0.5428(2) 0.0253(18) Uani 1 1 d . . .
H15A H 1.178584 0.237199 0.534041 0.038 Uiso 1 1 calc R U .
H15B H 1.130499 0.336276 0.574440 0.038 Uiso 1 1 calc R U .
H15C H 1.104874 0.372356 0.519583 0.038 Uiso 1 1 calc R U .
C16 C 1.1534(6) 0.1459(7) 0.7197(3) 0.038(2) Uani 1 1 d . . .
H16A H 1.181213 0.138913 0.752969 0.057 Uiso 1 1 calc R U .
H16B H 1.098831 0.223872 0.715946 0.057 Uiso 1 1 calc R U .
H16C H 1.221731 0.159591 0.699532 0.057 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 V1 O1 85.2(3) 2_656 .
O1 V1 O2 86.17(18) 2_656 .
O1 V1 O2 125.84(18) . .
O1 V1 O2 125.83(18) 2_656 2_656
O1 V1 O2 86.17(18) . 2_656
O2 V1 O2 138.7(3) . 2_656
O1 V1 N1 144.4(2) 2_656 .
O1 V1 N1 82.66(19) . .
O2 V1 N1 74.42(19) . .
O2 V1 N1 86.6(2) 2_656 .
O1 V1 N1 82.65(19) 2_656 2_656
O1 V1 N1 144.4(2) . 2_656
O2 V1 N1 86.60(19) . 2_656
O2 V1 N1 74.42(19) 2_656 2_656
N1 V1 N1 124.5(3) . 2_656
C2 O1 V1 124.1(4) . .
C8 O2 V1 119.0(4) . .
C5 O4 C16 115.9(5) . .
C7 N1 N2 116.3(5) . .
C7 N1 V1 127.8(4) . .
N2 N1 V1 115.9(4) . .
C8 N2 N1 107.4(5) . .
C10 N3 H3A 122(5) . .
C10 N3 H3B 116(5) . .
H3A N3 H3B 121(7) . .
C6 C1 C2 118.0(6) . .
C6 C1 C7 120.8(6) . .
C2 C1 C7 121.0(6) . .
O1 C2 C3 118.5(6) . .
O1 C2 C1 122.6(6) . .
C3 C2 C1 118.8(6) . .
C4 C3 C2 121.8(6) . .
C4 C3 H3 119.1 . .
C2 C3 H3 119.1 . .
C3 C4 C5 120.0(6) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
C6 C5 O4 127.3(6) . .
C6 C5 C4 118.9(6) . .
O4 C5 C4 113.8(6) . .
C5 C6 C1 122.4(6) . .
C5 C6 H6 118.8 . .
C1 C6 H6 118.8 . .
N1 C7 C1 118.9(6) . .
N1 C7 C15 120.5(6) . .
C1 C7 C15 120.3(6) . .
N2 C8 O2 121.3(6) . .
N2 C8 C9 122.0(6) . .
O2 C8 C9 116.7(6) . .
C14 C9 C10 118.9(6) . .
C14 C9 C8 117.7(6) . .
C10 C9 C8 123.3(6) . .
N3 C10 C11 119.7(7) . .
N3 C10 C9 122.3(6) . .
C11 C10 C9 118.0(6) . .
C12 C11 C10 122.0(7) . .
C12 C11 H11 119.0 . .
C10 C11 H11 119.0 . .
C11 C12 C13 120.1(7) . .
C11 C12 H12 120.0 . .
C13 C12 H12 120.0 . .
C14 C13 C12 119.4(7) . .
C14 C13 H13 120.3 . .
C12 C13 H13 120.3 . .
C13 C14 C9 121.6(7) . .
C13 C14 H14 119.2 . .
C9 C14 H14 119.2 . .
C7 C15 H15A 109.5 . .
C7 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C7 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
O4 C16 H16A 109.5 . .
O4 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O4 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.876(4) 2_656
V1 O1 1.877(4) .
V1 O2 1.905(4) .
V1 O2 1.905(4) 2_656
V1 N1 2.085(5) .
V1 N1 2.085(5) 2_656
O1 C2 1.329(7) .
O2 C8 1.313(7) .
O4 C5 1.372(7) .
O4 C16 1.411(7) .
N1 C7 1.308(7) .
N1 N2 1.401(7) .
N2 C8 1.306(7) .
N3 C10 1.367(9) .
N3 H3A 0.87(2) .
N3 H3B 0.87(2) .
C1 C6 1.405(8) .
C1 C2 1.418(9) .
C1 C7 1.452(9) .
C2 C3 1.382(9) .
C3 C4 1.367(8) .
C3 H3 0.9300 .
C4 C5 1.405(9) .
C4 H4 0.9300 .
C5 C6 1.357(9) .
C6 H6 0.9300 .
C7 C15 1.498(8) .
C8 C9 1.473(9) .
C9 C14 1.399(8) .
C9 C10 1.409(9) .
C10 C11 1.401(9) .
C11 C12 1.356(9) .
C11 H11 0.9300 .
C12 C13 1.393(9) .
C12 H12 0.9300 .
C13 C14 1.364(9) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N3 H3A N2 0.87(2) 2.09(6) 2.719(9) 128(6)
