#------------------------------------------------------------------------------
#$Date: 2021-07-05 11:35:41 +0300 (Mon, 05 Jul 2021) $
#$Revision: 266985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/39/1563918.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_1563918
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 O7 V'
_chemical_formula_weight         546.45
_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                99.478(2)
_cell_angle_beta                 94.723(2)
_cell_angle_gamma                95.263(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8843(4)
_cell_length_b                   12.5167(7)
_cell_length_c                   13.5651(7)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.44
_cell_volume                     1308.35(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0208
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46719
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_correction_T_min  0.8819
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1997)'
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0380
_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)+(0.0447P)²+0.6721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                4526
_reflns_number_total             5330
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ICA-2018-483-329.cif
_cod_data_source_block           3
_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               1563918
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 0.78749(4) 0.43944(3) 1.26582(2) 0.03373(11) Uani 1 1 d . . .
O1 O 0.75184(17) 0.58225(12) 1.34858(11) 0.0433(3) Uani 1 1 d . . .
O2 O 0.70362(18) 0.32967(12) 1.14146(11) 0.0433(3) Uani 1 1 d . . .
O3 O 0.56117(16) 0.48022(12) 1.21383(10) 0.0405(3) Uani 1 1 d . . .
O4 O 0.90200(17) 0.53243(12) 1.16853(11) 0.0424(3) Uani 1 1 d . . .
O5 O 0.71853(18) 0.36621(12) 1.34243(11) 0.0442(3) Uani 1 1 d . . .
O6 O 0.7444(3) 1.04584(16) 1.60815(19) 0.0949(7) Uani 1 1 d . . .
O7 O 0.5394(3) -0.06870(15) 0.78150(14) 0.0742(6) Uani 1 1 d . . .
N1 N 1.0256(2) 0.60091(14) 1.42181(13) 0.0407(4) Uani 1 1 d . . .
N2 N 1.0196(2) 0.50352(13) 1.35786(12) 0.0351(3) Uani 1 1 d . . .
N3 N 0.9845(2) 0.33700(13) 1.23081(12) 0.0351(4) Uani 1 1 d . . .
N4 N 0.9479(2) 0.24665(13) 1.15726(13) 0.0392(4) Uani 1 1 d . . .
C1 C 0.8753(3) 0.63588(16) 1.41036(15) 0.0390(4) Uani 1 1 d . . .
C2 C 0.8440(3) 0.74178(17) 1.46807(16) 0.0436(5) Uani 1 1 d . . .
C3 C 0.6901(3) 0.7835(2) 1.4489(2) 0.0598(6) Uani 1 1 d . . .
H3 H 0.6055 0.7427 1.4024 0.072 Uiso 1 1 calc R . .
C4 C 0.6610(4) 0.8840(2) 1.4976(2) 0.0738(8) Uani 1 1 d . . .
H4 H 0.5569 0.9108 1.4842 0.089 Uiso 1 1 calc R . .
C5 C 0.7853(4) 0.9453(2) 1.5663(2) 0.0651(7) Uani 1 1 d . . .
C6 C 0.9379(4) 0.9042(2) 1.5885(2) 0.0615(7) Uani 1 1 d . . .
H6 H 1.0208 0.9445 1.6364 0.074 Uiso 1 1 calc R . .
C7 C 0.9665(3) 0.80290(19) 1.53907(18) 0.0528(6) Uani 1 1 d . . .
H7 H 1.0695 0.7754 1.5537 0.063 Uiso 1 1 calc R . .
C8 C 1.1576(2) 0.45468(16) 1.35368(14) 0.0352(4) Uani 1 1 d . . .
C9 C 1.3215(3) 0.49596(19) 1.41582(17) 0.0466(5) Uani 1 1 d . . .
H9A H 1.3019 0.5525 1.4694 0.070 Uiso 1 1 calc R . .
H9B H 1.4018 0.5246 1.3748 0.070 Uiso 1 1 calc R . .
H9C H 1.3669 0.4374 1.4435 0.070 Uiso 1 1 calc R . .
C10 C 1.1359(2) 0.35520(16) 1.27960(15) 0.0357(4) Uani 1 1 d . . .
C11 C 1.2747(3) 0.28367(18) 1.26066(18) 0.0488(5) Uani 1 1 d . . .
H11A H 1.2251 0.2103 1.2353 0.073 Uiso 1 1 calc R . .
H11B H 1.3450 0.2854 1.3223 0.073 Uiso 1 1 calc R . .
H11C H 1.3433 0.3091 1.2122 0.073 Uiso 1 1 calc R . .
C12 C 0.7949(3) 0.25179(16) 1.11338(15) 0.0380(4) Uani 1 1 d . . .
C13 C 0.7249(3) 0.16710(16) 1.02732(15) 0.0397(4) Uani 1 1 d . . .
C14 C 0.8223(3) 0.08700(19) 0.98673(18) 0.0541(6) Uani 1 1 d . . .
H14 H 0.9334 0.0855 1.0150 0.065 Uiso 1 1 calc R . .
C15 C 0.7563(3) 0.0098(2) 0.9052(2) 0.0623(7) Uani 1 1 d . . .
H15 H 0.8227 -0.0437 0.8790 0.075 Uiso 1 1 calc R . .
C16 C 0.5917(3) 0.01141(19) 0.86189(17) 0.0516(6) Uani 1 1 d . . .
C17 C 0.4934(3) 0.09030(19) 0.90102(18) 0.0534(6) Uani 1 1 d . . .
H17 H 0.3828 0.0922 0.8721 0.064 Uiso 1 1 calc R . .
C18 C 0.5608(3) 0.16697(18) 0.98411(17) 0.0491(5) Uani 1 1 d . . .
H18 H 0.4935 0.2195 1.0112 0.059 Uiso 1 1 calc R . .
C19 C 0.8656(6) 1.1141(3) 1.6785(3) 0.1035(13) Uani 1 1 d . . .
H19A H 0.8259 1.1845 1.6948 0.155 Uiso 1 1 calc R . .
H19B H 0.9729 1.1214 1.6503 0.155 Uiso 1 1 calc R . .
H19C H 0.8804 1.0828 1.7382 0.155 Uiso 1 1 calc R . .
C20 C 0.3780(4) -0.0690(3) 0.7290(2) 0.0755(8) Uani 1 1 d . . .
H20A H 0.3587 -0.1303 0.6752 0.113 Uiso 1 1 calc R . .
H20B H 0.3741 -0.0029 0.7020 0.113 Uiso 1 1 calc R . .
H20C H 0.2908 -0.0738 0.7739 0.113 Uiso 1 1 calc R . .
C21 C 0.3493(3) 0.5696(3) 1.1431(3) 0.0988(13) Uani 1 1 d . . .
H21A H 0.2781 0.5015 1.1254 0.148 Uiso 1 1 calc R . .
H21B H 0.3351 0.6114 1.0902 0.148 Uiso 1 1 calc R . .
H21C H 0.3173 0.6095 1.2042 0.148 Uiso 1 1 calc R . .
C22 C 0.5331(3) 0.5484(2) 1.1579(2) 0.0587(6) Uani 1 1 d . . .
C23 C 0.6552(3) 0.6035(3) 1.1124(3) 0.0943(13) Uani 1 1 d . . .
H23 H 0.6168 0.6529 1.0737 0.113 Uiso 1 1 calc R . .
C24 C 0.8295(3) 0.5930(2) 1.1181(2) 0.0569(6) Uani 1 1 d . . .
C25 C 0.9416(4) 0.6583(3) 1.0598(3) 0.0887(11) Uani 1 1 d . . .
H25A H 1.0312 0.7021 1.1049 0.133 Uiso 1 1 calc R . .
H25B H 0.8740 0.7046 1.0269 0.133 Uiso 1 1 calc R . .
H25C H 0.9909 0.6097 1.0104 0.133 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 O1 95.68(7) . .
O5 V1 O3 97.71(7) . .
O1 V1 O3 72.78(6) . .
O5 V1 O2 95.31(7) . .
O1 V1 O2 145.27(6) . .
O3 V1 O2 73.16(6) . .
O5 V1 O4 174.56(7) . .
O1 V1 O4 86.10(6) . .
O3 V1 O4 87.73(6) . .
O2 V1 O4 86.04(6) . .
O5 V1 N3 91.73(7) . .
O1 V1 N3 140.95(6) . .
O3 V1 N3 143.89(6) . .
O2 V1 N3 71.31(6) . .
O4 V1 N3 83.69(6) . .
O5 V1 N2 94.86(7) . .
O1 V1 N2 71.14(6) . .
O3 V1 N2 142.72(6) . .
O2 V1 N2 140.23(6) . .
O4 V1 N2 80.83(6) . .
N3 V1 N2 70.05(6) . .
C1 O1 V1 119.78(13) . .
C12 O2 V1 119.00(12) . .
C22 O3 V1 128.19(14) . .
C24 O4 V1 126.30(14) . .
C5 O6 C19 118.7(3) . .
C16 O7 C20 119.1(2) . .
C1 N1 N2 107.12(16) . .
C8 N2 N1 118.25(16) . .
C8 N2 V1 122.30(13) . .
N1 N2 V1 119.43(12) . .
C10 N3 N4 118.84(16) . .
C10 N3 V1 122.13(13) . .
N4 N3 V1 118.97(12) . .
C12 N4 N3 107.22(16) . .
O1 C1 N1 122.52(19) . .
O1 C1 C2 117.79(18) . .
N1 C1 C2 119.68(18) . .
C7 C2 C3 118.6(2) . .
C7 C2 C1 121.9(2) . .
C3 C2 C1 119.5(2) . .
C4 C3 C2 120.8(2) . .
C3 C4 C5 120.2(3) . .
O6 C5 C4 115.2(3) . .
O6 C5 C6 124.8(3) . .
C4 C5 C6 120.0(2) . .
C7 C6 C5 119.5(2) . .
C6 C7 C2 120.9(2) . .
N2 C8 C10 112.61(17) . .
N2 C8 C9 124.27(19) . .
C10 C8 C9 123.11(17) . .
N3 C10 C8 112.80(17) . .
N3 C10 C11 123.98(19) . .
C8 C10 C11 123.21(17) . .
O2 C12 N4 122.52(18) . .
O2 C12 C13 118.24(18) . .
N4 C12 C13 119.23(18) . .
C18 C13 C14 118.3(2) . .
C18 C13 C12 120.25(19) . .
C14 C13 C12 121.40(19) . .
C15 C14 C13 120.7(2) . .
C14 C15 C16 120.3(2) . .
O7 C16 C17 124.8(2) . .
O7 C16 C15 115.4(2) . .
C17 C16 C15 119.8(2) . .
C16 C17 C18 119.3(2) . .
C13 C18 C17 121.5(2) . .
O3 C22 C23 125.5(2) . .
O3 C22 C21 114.7(2) . .
C23 C22 C21 119.8(2) . .
C22 C23 C24 126.9(2) . .
O4 C24 C23 124.6(2) . .
O4 C24 C25 116.5(2) . .
C23 C24 C25 118.9(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.5909(14) .
V1 O1 2.0045(14) .
V1 O3 2.0051(13) .
V1 O2 2.0142(14) .
V1 O4 2.1026(14) .
V1 N3 2.1376(16) .
V1 N2 2.1389(16) .
O1 C1 1.289(2) .
O2 C12 1.290(2) .
O3 C22 1.253(3) .
O4 C24 1.248(3) .
O6 C5 1.371(3) .
O6 C19 1.408(4) .
O7 C16 1.362(3) .
O7 C20 1.406(3) .
N1 C1 1.306(3) .
N1 N2 1.369(2) .
N2 C8 1.297(2) .
N3 C10 1.298(2) .
N3 N4 1.371(2) .
N4 C12 1.312(3) .
C1 C2 1.477(3) .
C2 C7 1.384(3) .
C2 C3 1.387(3) .
C3 C4 1.369(4) .
C4 C5 1.376(4) .
C5 C6 1.381(4) .
C6 C7 1.381(3) .
C8 C10 1.453(3) .
C8 C9 1.484(3) .
C10 C11 1.488(3) .
C12 C13 1.473(3) .
C13 C18 1.376(3) .
C13 C14 1.388(3) .
C14 C15 1.374(3) .
C15 C16 1.383(3) .
C16 C17 1.376(3) .
C17 C18 1.388(3) .
C21 C22 1.500(3) .
C22 C23 1.379(4) .
C23 C24 1.389(3) .
C24 C25 1.506(3) .
