#------------------------------------------------------------------------------
#$Date: 2021-07-05 11:35:41 +0300 (Mon, 05 Jul 2021) $
#$Revision: 266985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/39/1563917.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_1563917
loop_
_publ_author_name
'Srivastava, Ankit Kumar'
'Ghosh, Sabari'
'Jana, Subhendu'
'Pal, Samudranil'
_publ_section_title
;
 Ternary pentagonal-bipyramidal oxovanadium(V) complexes containing five-
 and six-membered chelate rings: Syntheses, structures and properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              329
_journal_page_last               336
_journal_paper_doi               10.1016/j.ica.2018.08.036
_journal_volume                  483
_journal_year                    2018
_chemical_formula_sum            'C25 H27 N4 O5 V'
_chemical_formula_weight         514.45
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.7130(10)
_cell_angle_beta                 96.2190(10)
_cell_angle_gamma                96.8230(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9483(3)
_cell_length_b                   12.3434(4)
_cell_length_c                   13.6255(4)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.59
_cell_volume                     1276.51(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'MERCURY (Macrae et al, 2008)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47625
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9266
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1997)'
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0391
_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/[σ²(Fo²)+(0.0506P)²+0.5037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                4343
_reflns_number_total             5235
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ICA-2018-483-329.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563917
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.27453(4) -0.04749(3) 0.76470(2) 0.03662(11) Uani 1 1 d . . .
O1 O 0.25343(17) 0.10355(12) 0.85430(11) 0.0488(4) Uani 1 1 d . . .
O2 O 0.17608(18) -0.16668(12) 0.63579(11) 0.0461(3) Uani 1 1 d . . .
O3 O 0.05091(16) -0.00629(12) 0.71427(10) 0.0426(3) Uani 1 1 d . . .
O4 O 0.38995(16) 0.04165(12) 0.67036(11) 0.0440(3) Uani 1 1 d . . .
O5 O 0.20475(18) -0.12000(12) 0.83806(11) 0.0480(3) Uani 1 1 d . . .
N1 N 0.5260(2) 0.12028(16) 0.93331(13) 0.0486(4) Uani 1 1 d . . .
N2 N 0.5119(2) 0.01957(14) 0.86231(12) 0.0412(4) Uani 1 1 d . . .
N3 N 0.4623(2) -0.15374(14) 0.72346(12) 0.0403(4) Uani 1 1 d . . .
N4 N 0.4190(2) -0.24753(14) 0.64364(13) 0.0459(4) Uani 1 1 d . . .
C1 C 0.3810(3) 0.15854(18) 0.92182(15) 0.0454(5) Uani 1 1 d . . .
C2 C 0.3619(3) 0.27071(19) 0.98400(17) 0.0524(5) Uani 1 1 d . . .
C3 C 0.2292(4) 0.3239(2) 0.9554(2) 0.0772(8) Uani 1 1 d . . .
H3 H 0.1476 0.2869 0.8996 0.093 Uiso 1 1 calc R . .
C4 C 0.2164(4) 0.4320(3) 1.0090(3) 0.0913(10) Uani 1 1 d . . .
H4 H 0.1267 0.4670 0.9878 0.110 Uiso 1 1 calc R . .
C5 C 0.3328(4) 0.4893(2) 1.0928(2) 0.0788(9) Uani 1 1 d . . .
C6 C 0.4619(4) 0.4343(3) 1.1221(2) 0.0807(9) Uani 1 1 d . . .
H6 H 0.5402 0.4703 1.1798 0.097 Uiso 1 1 calc R . .
C7 C 0.4796(3) 0.3269(2) 1.06883(19) 0.0656(7) Uani 1 1 d . . .
H7 H 0.5701 0.2925 1.0898 0.079 Uiso 1 1 calc R . .
C8 C 0.6458(2) -0.03052(19) 0.85411(15) 0.0439(5) Uani 1 1 d . . .
C9 C 0.8150(3) 0.0135(2) 0.91866(18) 0.0616(6) Uani 1 1 d . . .
H9A H 0.8073 0.0826 0.9672 0.092 Uiso 1 1 calc R . .
H9B H 0.8996 0.0273 0.8762 0.092 Uiso 1 1 calc R . .
H9C H 0.8470 -0.0410 0.9543 0.092 Uiso 1 1 calc R . .
C10 C 0.6159(3) -0.13298(18) 0.77303(16) 0.0438(5) Uani 1 1 d . . .
C11 C 0.7504(3) -0.2058(2) 0.7490(2) 0.0616(6) Uani 1 1 d . . .
H11A H 0.7060 -0.2675 0.6908 0.092 Uiso 1 1 calc R . .
H11B H 0.7837 -0.2347 0.8065 0.092 Uiso 1 1 calc R . .
H11C H 0.8482 -0.1621 0.7341 0.092 Uiso 1 1 calc R . .
C12 C 0.2633(3) -0.24567(17) 0.60114(15) 0.0431(5) Uani 1 1 d . . .
C13 C 0.1849(3) -0.33505(17) 0.51020(16) 0.0455(5) Uani 1 1 d . . .
C14 C 0.2813(3) -0.40810(19) 0.45503(19) 0.0569(6) Uani 1 1 d . . .
H14 H 0.3976 -0.4028 0.4768 0.068 Uiso 1 1 calc R . .
C15 C 0.2050(3) -0.4882(2) 0.3683(2) 0.0645(7) Uani 1 1 d . . .
H15 H 0.2716 -0.5358 0.3318 0.077 Uiso 1 1 calc R . .
C16 C 0.0326(3) -0.50004(19) 0.33380(18) 0.0586(6) Uani 1 1 d . . .
C17 C -0.0636(3) -0.4280(2) 0.39081(19) 0.0605(6) Uani 1 1 d . . .
H17 H -0.1806 -0.4347 0.3699 0.073 Uiso 1 1 calc R . .
C18 C 0.0111(3) -0.34703(19) 0.47751(17) 0.0530(5) Uani 1 1 d . . .
H18 H -0.0557 -0.3000 0.5144 0.064 Uiso 1 1 calc R . .
C19 C 0.3163(6) 0.6083(3) 1.1488(3) 0.1132(14) Uani 1 1 d . . .
H19A H 0.2854 0.6501 1.1002 0.170 Uiso 1 1 calc R . .
H19B H 0.4237 0.6443 1.1893 0.170 Uiso 1 1 calc R . .
H19C H 0.2295 0.6060 1.1923 0.170 Uiso 1 1 calc R . .
C20 C -0.0508(4) -0.5882(2) 0.2393(2) 0.0822(9) Uani 1 1 d . . .
H20A H -0.1583 -0.5687 0.2152 0.123 Uiso 1 1 calc R . .
H20B H -0.0698 -0.6602 0.2549 0.123 Uiso 1 1 calc R . .
H20C H 0.0225 -0.5921 0.1874 0.123 Uiso 1 1 calc R . .
C21 C -0.1543(3) 0.0862(3) 0.6470(3) 0.0933(11) Uani 1 1 d . . .
H21A H -0.2327 0.0171 0.6321 0.140 Uiso 1 1 calc R . .
H21B H -0.1700 0.1216 0.5917 0.140 Uiso 1 1 calc R . .
H21C H -0.1756 0.1358 0.7087 0.140 Uiso 1 1 calc R . .
C22 C 0.0265(3) 0.0614(2) 0.66027(19) 0.0572(6) Uani 1 1 d . . .
C23 C 0.1482(3) 0.1131(3) 0.6149(3) 0.0890(11) Uani 1 1 d . . .
H23 H 0.1115 0.1611 0.5766 0.107 Uiso 1 1 calc R . .
C24 C 0.3206(3) 0.1010(2) 0.62046(19) 0.0549(6) Uani 1 1 d . . .
C25 C 0.4334(4) 0.1622(3) 0.5629(3) 0.0831(9) Uani 1 1 d . . .
H25A H 0.4876 0.1090 0.5183 0.125 Uiso 1 1 calc R . .
H25B H 0.5192 0.2164 0.6103 0.125 Uiso 1 1 calc R . .
H25C H 0.3653 0.2003 0.5233 0.125 Uiso 1 1 calc R . .
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
O5 V1 O3 97.70(7) . .
O5 V1 O1 96.13(7) . .
O3 V1 O1 72.78(6) . .
O5 V1 O2 94.11(7) . .
O3 V1 O2 73.27(6) . .
O1 V1 O2 145.53(6) . .
O5 V1 O4 174.17(7) . .
O3 V1 O4 88.04(5) . .
O1 V1 O4 86.57(6) . .
O2 V1 O4 86.48(6) . .
O5 V1 N3 92.47(7) . .
O3 V1 N3 143.68(6) . .
O1 V1 N3 140.67(6) . .
O2 V1 N3 71.28(6) . .
O4 V1 N3 82.21(6) . .
O5 V1 N2 94.05(7) . .
O3 V1 N2 142.89(6) . .
O1 V1 N2 71.04(6) . .
O2 V1 N2 140.81(6) . .
O4 V1 N2 81.91(6) . .
N3 V1 N2 70.12(6) . .
C1 O1 V1 119.69(13) . .
C12 O2 V1 119.27(13) . .
C22 O3 V1 127.57(13) . .
C24 O4 V1 126.60(13) . .
C1 N1 N2 107.35(16) . .
C8 N2 N1 118.42(17) . .
C8 N2 V1 122.00(14) . .
N1 N2 V1 119.54(12) . .
C10 N3 N4 118.76(17) . .
C10 N3 V1 121.88(14) . .
N4 N3 V1 119.35(12) . .
C12 N4 N3 107.47(16) . .
O1 C1 N1 122.3(2) . .
O1 C1 C2 117.93(19) . .
N1 C1 C2 119.70(19) . .
C3 C2 C7 118.6(2) . .
C3 C2 C1 119.8(2) . .
C7 C2 C1 121.5(2) . .
C2 C3 C4 120.4(3) . .
C5 C4 C3 121.7(3) . .
C6 C5 C4 117.3(3) . .
C6 C5 C19 122.4(3) . .
C4 C5 C19 120.3(4) . .
C5 C6 C7 122.2(3) . .
C6 C7 C2 119.8(3) . .
N2 C8 C10 112.78(18) . .
N2 C8 C9 124.2(2) . .
C10 C8 C9 122.99(19) . .
N3 C10 C8 113.18(18) . .
N3 C10 C11 124.0(2) . .
C8 C10 C11 122.79(19) . .
O2 C12 N4 122.18(19) . .
O2 C12 C13 118.24(19) . .
N4 C12 C13 119.58(19) . .
C18 C13 C14 118.6(2) . .
C18 C13 C12 119.72(19) . .
C14 C13 C12 121.6(2) . .
C15 C14 C13 120.1(2) . .
C14 C15 C16 121.9(2) . .
C15 C16 C17 117.5(2) . .
C15 C16 C20 121.8(2) . .
C17 C16 C20 120.7(3) . .
C18 C17 C16 121.2(2) . .
C17 C18 C13 120.5(2) . .
O3 C22 C23 126.0(2) . .
O3 C22 C21 114.7(2) . .
C23 C22 C21 119.3(2) . .
C22 C23 C24 126.8(2) . .
O4 C24 C23 124.3(2) . .
O4 C24 C25 116.6(2) . .
C23 C24 C25 119.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.5921(14) .
V1 O3 2.0013(13) .
V1 O1 2.0085(15) .
V1 O2 2.0162(14) .
V1 O4 2.0953(13) .
V1 N3 2.1354(16) .
V1 N2 2.1396(16) .
O1 C1 1.294(2) .
O2 C12 1.291(2) .
O3 C22 1.255(3) .
O4 C24 1.247(2) .
N1 C1 1.304(3) .
N1 N2 1.366(2) .
N2 C8 1.295(3) .
N3 C10 1.296(3) .
N3 N4 1.367(2) .
N4 C12 1.313(3) .
C1 C2 1.476(3) .
C2 C3 1.376(4) .
C2 C7 1.387(3) .
C3 C4 1.382(4) .
C4 C5 1.376(5) .
C5 C6 1.371(5) .
C5 C19 1.515(4) .
C6 C7 1.384(4) .
C8 C10 1.444(3) .
C8 C9 1.490(3) .
C10 C11 1.491(3) .
C12 C13 1.471(3) .
C13 C18 1.384(3) .
C13 C14 1.390(3) .
C14 C15 1.375(3) .
C15 C16 1.378(4) .
C16 C17 1.394(4) .
C16 C20 1.504(3) .
C17 C18 1.376(3) .
C21 C22 1.506(3) .
C22 C23 1.377(3) .
C23 C24 1.391(3) .
C24 C25 1.504(3) .
