#------------------------------------------------------------------------------
#$Date: 2021-07-05 11:35:41 +0300 (Mon, 05 Jul 2021) $
#$Revision: 266985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/39/1563921.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_1563921
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            'C33 H27 N4 O5 V'
_chemical_formula_weight         610.53
_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                113.5270(10)
_cell_angle_beta                 108.4360(10)
_cell_angle_gamma                98.184(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1240(4)
_cell_length_b                   12.3131(4)
_cell_length_c                   13.4539(5)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.90
_cell_volume                     1524.56(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            49430
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.9160
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick 1997)'
_exptl_crystal_colour            'Dark Brown'
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.191
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0475
_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/[σ²(Fo²)+(0.0616P)²+1.1034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                4741
_reflns_number_total             5347
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ICA-2018-483-329.cif
_cod_data_source_block           6
_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_cell_volume        1524.56(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1563921
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 0.38893(4) 0.32779(4) 0.68173(4) 0.04304(15) Uani 1 1 d . . .
O1 O 0.26697(18) 0.28064(18) 0.75129(16) 0.0525(5) Uani 1 1 d . . .
O2 O 0.57903(18) 0.37931(18) 0.70404(16) 0.0528(5) Uani 1 1 d . . .
O3 O 0.50263(18) 0.37206(18) 0.84837(15) 0.0527(5) Uani 1 1 d . . .
O4 O 0.40495(18) 0.14736(16) 0.62818(16) 0.0504(4) Uani 1 1 d . . .
O5 O 0.36522(19) 0.45837(17) 0.70528(16) 0.0542(5) Uani 1 1 d . . .
N1 N 0.0897(2) 0.2044(2) 0.5744(2) 0.0477(5) Uani 1 1 d . . .
N2 N 0.1917(2) 0.23013(19) 0.54326(18) 0.0428(5) Uani 1 1 d . . .
N3 N 0.3915(2) 0.29236(19) 0.51277(18) 0.0424(5) Uani 1 1 d . . .
N4 N 0.5114(2) 0.3205(2) 0.50690(19) 0.0470(5) Uani 1 1 d . . .
C1 C 0.1407(3) 0.2367(2) 0.6876(2) 0.0454(6) Uani 1 1 d . . .
C2 C 0.0497(3) 0.2250(3) 0.7451(3) 0.0511(6) Uani 1 1 d . . .
C3 C 0.1005(3) 0.2718(3) 0.8671(3) 0.0635(8) Uani 1 1 d . . .
H3 H 0.1919 0.3070 0.9125 0.076 Uiso 1 1 calc R . .
C4 C 0.0146(4) 0.2659(4) 0.9214(4) 0.0830(11) Uani 1 1 d . . .
H4 H 0.0487 0.2967 1.0034 0.100 Uiso 1 1 calc R . .
C5 C -0.1192(4) 0.2156(4) 0.8559(4) 0.0854(11) Uani 1 1 d . . .
H5 H -0.1764 0.2130 0.8931 0.103 Uiso 1 1 calc R . .
C6 C -0.1698(4) 0.1689(4) 0.7352(4) 0.0838(11) Uani 1 1 d . . .
H6 H -0.2614 0.1343 0.6908 0.101 Uiso 1 1 calc R . .
C7 C -0.0866(3) 0.1724(3) 0.6787(3) 0.0654(8) Uani 1 1 d . . .
H7 H -0.1218 0.1396 0.5965 0.078 Uiso 1 1 calc R . .
C8 C 0.1633(2) 0.2118(2) 0.4348(2) 0.0420(5) Uani 1 1 d . . .
C9 C 0.0260(3) 0.1718(2) 0.3448(2) 0.0450(6) Uani 1 1 d . . .
C10 C -0.0728(3) 0.0718(3) 0.3238(3) 0.0574(7) Uani 1 1 d . . .
H10 H -0.0522 0.0268 0.3649 0.069 Uiso 1 1 calc R . .
C11 C -0.2006(3) 0.0397(3) 0.2423(3) 0.0738(10) Uani 1 1 d . . .
H11 H -0.2658 -0.0286 0.2265 0.089 Uiso 1 1 calc R . .
C12 C -0.2325(3) 0.1083(4) 0.1841(3) 0.0834(11) Uani 1 1 d . . .
H12 H -0.3198 0.0879 0.1309 0.100 Uiso 1 1 calc R . .
C13 C -0.1353(4) 0.2074(3) 0.2044(3) 0.0762(10) Uani 1 1 d . . .
H13 H -0.1571 0.2535 0.1647 0.091 Uiso 1 1 calc R . .
C14 C -0.0068(3) 0.2381(3) 0.2828(3) 0.0571(7) Uani 1 1 d . . .
H14 H 0.0589 0.3035 0.2946 0.068 Uiso 1 1 calc R . .
C15 C 0.2830(3) 0.2440(2) 0.4156(2) 0.0417(5) Uani 1 1 d . . .
C16 C 0.2807(3) 0.2198(2) 0.2981(2) 0.0467(6) Uani 1 1 d . . .
C17 C 0.2048(3) 0.1056(3) 0.1996(3) 0.0611(8) Uani 1 1 d . . .
H17 H 0.1537 0.0451 0.2073 0.073 Uiso 1 1 calc R . .
C18 C 0.2046(4) 0.0810(3) 0.0901(3) 0.0819(11) Uani 1 1 d . . .
H18 H 0.1552 0.0033 0.0247 0.098 Uiso 1 1 calc R . .
C19 C 0.2773(4) 0.1712(4) 0.0773(3) 0.0879(12) Uani 1 1 d . . .
H19 H 0.2761 0.1546 0.0032 0.105 Uiso 1 1 calc R . .
C20 C 0.3522(4) 0.2865(3) 0.1752(3) 0.0761(10) Uani 1 1 d . . .
H20 H 0.4009 0.3478 0.1668 0.091 Uiso 1 1 calc R . .
C21 C 0.3543(3) 0.3100(3) 0.2842(3) 0.0571(7) Uani 1 1 d . . .
H21 H 0.4056 0.3871 0.3499 0.069 Uiso 1 1 calc R . .
C22 C 0.6049(3) 0.3660(2) 0.6140(2) 0.0460(6) Uani 1 1 d . . .
C23 C 0.7459(3) 0.4024(2) 0.6321(3) 0.0498(6) Uani 1 1 d . . .
C24 C 0.7800(3) 0.3796(3) 0.5367(3) 0.0625(8) Uani 1 1 d . . .
H24 H 0.7140 0.3435 0.4600 0.075 Uiso 1 1 calc R . .
C25 C 0.9127(4) 0.4109(3) 0.5563(4) 0.0760(10) Uani 1 1 d . . .
H25 H 0.9359 0.3952 0.4924 0.091 Uiso 1 1 calc R . .
C26 C 1.0104(3) 0.4651(3) 0.6695(4) 0.0774(11) Uani 1 1 d . . .
H26 H 1.0995 0.4856 0.6819 0.093 Uiso 1 1 calc R . .
C27 C 0.9776(3) 0.4892(3) 0.7643(4) 0.0697(9) Uani 1 1 d . . .
H27 H 1.0442 0.5270 0.8410 0.084 Uiso 1 1 calc R . .
C28 C 0.8454(3) 0.4572(3) 0.7459(3) 0.0583(7) Uani 1 1 d . . .
H28 H 0.8231 0.4727 0.8102 0.070 Uiso 1 1 calc R . .
C33 C 0.4570(4) -0.0281(3) 0.6359(3) 0.0735(9) Uani 1 1 d . . .
H33A H 0.4096 -0.0626 0.5514 0.110 Uiso 1 1 calc R . .
H33B H 0.4120 -0.0740 0.6640 0.110 Uiso 1 1 calc R . .
H33C H 0.5460 -0.0334 0.6539 0.110 Uiso 1 1 calc R . .
C32 C 0.4623(3) 0.1063(3) 0.6960(3) 0.0501(6) Uani 1 1 d . . .
C31 C 0.5277(3) 0.1761(3) 0.8201(3) 0.0600(7) Uani 1 1 d . . .
H31 H 0.5628 0.1345 0.8610 0.072 Uiso 1 1 calc R . .
C30 C 0.5451(3) 0.3012(3) 0.8879(2) 0.0536(7) Uani 1 1 d . . .
C29 C 0.6198(4) 0.3651(4) 1.0210(3) 0.0840(11) Uani 1 1 d . . .
H29A H 0.6223 0.4508 1.0532 0.126 Uiso 1 1 calc R . .
H29B H 0.7091 0.3604 1.0411 0.126 Uiso 1 1 calc R . .
H29C H 0.5756 0.3248 1.0537 0.126 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 98.43(9) . .
O5 V1 O2 96.53(9) . .
O3 V1 O2 73.08(8) . .
O5 V1 O1 95.44(9) . .
O3 V1 O1 72.90(8) . .
O2 V1 O1 145.20(8) . .
O5 V1 O4 172.83(9) . .
O3 V1 O4 88.73(8) . .
O2 V1 O4 85.68(8) . .
O1 V1 O4 86.46(8) . .
O5 V1 N2 91.28(9) . .
O3 V1 N2 143.63(8) . .
O2 V1 N2 140.67(8) . .
O1 V1 N2 71.33(8) . .
O4 V1 N2 82.77(7) . .
O5 V1 N3 92.19(9) . .
O3 V1 N3 143.82(8) . .
O2 V1 N3 71.40(8) . .
O1 V1 N3 140.51(8) . .
O4 V1 N3 82.03(7) . .
N2 V1 N3 69.82(8) . .
C1 O1 V1 118.82(16) . .
C22 O2 V1 119.55(17) . .
C30 O3 V1 128.13(18) . .
C32 O4 V1 125.97(17) . .
C1 N1 N2 108.2(2) . .
C8 N2 N1 118.8(2) . .
C8 N2 V1 122.14(17) . .
N1 N2 V1 118.16(16) . .
C15 N3 N4 118.8(2) . .
C15 N3 V1 122.47(17) . .
N4 N3 V1 118.71(15) . .
C22 N4 N3 107.8(2) . .
O1 C1 N1 122.3(2) . .
O1 C1 C2 118.9(2) . .
N1 C1 C2 118.8(2) . .
C3 C2 C7 119.5(3) . .
C3 C2 C1 119.7(3) . .
C7 C2 C1 120.7(3) . .
C2 C3 C4 119.7(3) . .
C5 C4 C3 120.5(4) . .
C4 C5 C6 120.0(3) . .
C5 C6 C7 120.7(4) . .
C6 C7 C2 119.6(3) . .
N2 C8 C15 112.2(2) . .
N2 C8 C9 123.6(2) . .
C15 C8 C9 124.1(2) . .
C14 C9 C10 119.2(3) . .
C14 C9 C8 119.3(2) . .
C10 C9 C8 121.5(2) . .
C11 C10 C9 119.9(3) . .
C10 C11 C12 120.3(3) . .
C11 C12 C13 120.1(3) . .
C14 C13 C12 120.1(3) . .
C13 C14 C9 120.3(3) . .
C13 C14 C23 113.9(2) . 2_666
C9 C14 C23 124.64(18) . 2_666
N3 C15 C8 112.4(2) . .
N3 C15 C16 124.0(2) . .
C8 C15 C16 123.5(2) . .
C17 C16 C21 119.0(3) . .
C17 C16 C15 119.8(2) . .
C21 C16 C15 121.3(2) . .
C18 C17 C16 120.2(3) . .
C19 C18 C17 120.3(3) . .
C18 C19 C20 119.8(3) . .
C21 C20 C19 119.8(3) . .
C20 C21 C16 120.9(3) . .
O2 C22 N4 122.6(2) . .
O2 C22 C23 118.6(2) . .
N4 C22 C23 118.8(2) . .
C28 C23 C24 119.4(3) . .
C28 C23 C22 119.4(3) . .
C24 C23 C22 121.1(3) . .
C25 C24 C23 119.6(3) . .
C26 C25 C24 120.3(3) . .
C27 C26 C25 120.4(3) . .
C26 C27 C28 119.8(3) . .
C27 C28 C23 120.3(3) . .
O4 C32 C31 124.6(3) . .
O4 C32 C33 115.8(3) . .
C31 C32 C33 119.6(3) . .
C30 C31 C32 126.4(3) . .
O3 C30 C31 125.8(3) . .
O3 C30 C29 113.5(3) . .
C31 C30 C29 120.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O5 1.5880(19) .
V1 O3 1.9895(18) .
V1 O2 2.0072(18) .
V1 O1 2.0165(18) .
V1 O4 2.0983(18) .
V1 N2 2.146(2) .
V1 N3 2.147(2) .
O1 C1 1.286(3) .
O2 C22 1.285(3) .
O3 C30 1.264(3) .
O4 C32 1.260(3) .
N1 C1 1.306(3) .
N1 N2 1.366(3) .
N2 C8 1.306(3) .
N3 C15 1.302(3) .
N3 N4 1.365(3) .
N4 C22 1.309(3) .
C1 C2 1.478(4) .
C2 C3 1.383(4) .
C2 C7 1.385(4) .
C3 C4 1.384(5) .
C4 C5 1.360(6) .
C5 C6 1.366(6) .
C6 C7 1.377(5) .
C8 C15 1.465(4) .
C8 C9 1.476(3) .
C9 C14 1.391(4) .
C9 C10 1.394(4) .
C10 C11 1.374(4) .
C11 C12 1.375(6) .
C12 C13 1.380(5) .
C13 C14 1.369(4) .
C14 C23 4.419(4) 2_666
C15 C16 1.479(3) .
C16 C17 1.383(4) .
C16 C21 1.393(4) .
C17 C18 1.380(4) .
C18 C19 1.379(5) .
C19 C20 1.386(5) .
C20 C21 1.369(4) .
C22 C23 1.481(4) .
C23 C28 1.384(4) .
C23 C24 1.386(4) .
C24 C25 1.381(5) .
C25 C26 1.371(5) .
C26 C27 1.368(5) .
C27 C28 1.380(4) .
C33 C32 1.506(4) .
C32 C31 1.401(4) .
C31 C30 1.386(4) .
C30 C29 1.505(4) .
