#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/26/7022632.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_7022632
loop_
_publ_author_name
'Ren, Dong Xue'
'Xing, Na'
'Shan, Hui'
'Chen, Chen'
'Cao, Yun Zhu'
'Xing, Yong Heng'
_publ_section_title
;
 Novel vanadium(III) complexes with rigid phenylpolycarboxylate ligands:
 synthesis, structures and application in C-H bond activation.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5379
_journal_page_last               5389
_journal_paper_doi               10.1039/c3dt32472a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C24 H22 N2 O22 V2'
_chemical_formula_weight         792.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_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                103.42(3)
_cell_angle_beta                 109.89(3)
_cell_angle_gamma                90.08(3)
_cell_formula_units_Z            1
_cell_length_a                   8.1031(16)
_cell_length_b                   9.7398(19)
_cell_length_c                   10.142(2)
_cell_measurement_temperature    293(2)
_cell_volume                     729.3(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7242
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0286
_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)+(0.0470P)²+0.2016P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                2935
_reflns_number_total             3320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32472a.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        729.3(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7022632
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
H1WA H 0.879(6) 0.931(5) 0.664(5) 0.106(15) Uiso 1 1 d .
H1WB H 0.964(6) 1.013(4) 0.767(5) 0.100(15) Uiso 1 1 d .
V1 V 0.87882(3) 0.30396(3) 0.09094(3) 0.01693(9) Uani 1 1 d .
O1 O 1.03361(16) 0.27493(12) -0.03633(13) 0.0248(3) Uani 1 1 d .
H1A H 1.1327 0.2184 0.0099 0.070(9) Uiso 1 1 d R
H1B H 1.0756 0.3505 -0.0507 0.045(7) Uiso 1 1 d R
O2 O 0.74173(17) 0.33164(16) 0.23003(14) 0.0356(3) Uani 1 1 d .
H2A H 0.6475 0.3671 0.2095 0.047(7) Uiso 1 1 d R
H2B H 0.7817 0.3163 0.3140 0.036(6) Uiso 1 1 d R
O3 O 0.77898(15) 0.47302(12) 0.01287(12) 0.0225(2) Uani 1 1 d .
O4 O 0.56486(17) 0.56537(13) -0.13613(14) 0.0303(3) Uani 1 1 d .
O5 O 0.85622(16) 0.08833(12) 0.06007(14) 0.0276(3) Uani 1 1 d .
O6 O 0.70115(19) -0.12071(13) -0.06176(17) 0.0385(3) Uani 1 1 d .
O7 O 1.09364(15) 0.27286(12) 0.26828(13) 0.0266(3) Uani 1 1 d .
O8 O 1.05784(16) 0.48139(12) 0.22824(13) 0.0288(3) Uani 1 1 d .
O9 O 1.14215(19) 0.73070(16) 0.50268(15) 0.0380(3) Uani 1 1 d .
O10 O 1.2786(2) 0.78873(16) 0.36364(17) 0.0413(4) Uani 1 1 d .
H10 H 1.2147 0.8501 0.3564 0.059(8) Uiso 1 1 d R
N1 N 0.63973(18) 0.22768(14) -0.08154(14) 0.0197(3) Uani 1 1 d .
C1 C 0.6283(2) 0.46497(17) -0.08861(17) 0.0200(3) Uani 1 1 d .
C2 C 0.5377(2) 0.31809(17) -0.14536(17) 0.0208(3) Uani 1 1 d .
C3 C 0.3733(2) 0.2747(2) -0.25050(19) 0.0292(4) Uani 1 1 d .
H3 H 0.2838 0.3459 -0.2959 0.048(7) Uiso 1 1 d R
C4 C 0.3172(3) 0.1307(2) -0.2914(2) 0.0363(4) Uani 1 1 d .
H4 H 0.1989 0.0982 -0.3703 0.047(7) Uiso 1 1 d R
C5 C 0.4261(3) 0.0369(2) -0.2274(2) 0.0331(4) Uani 1 1 d .
H5 H 0.3854 -0.0831 -0.2457 0.069(9) Uiso 1 1 d R
C6 C 0.5871(2) 0.08960(17) -0.12119(18) 0.0240(3) Uani 1 1 d .
C7 C 0.7238(2) 0.00870(17) -0.0363(2) 0.0252(3) Uani 1 1 d .
C8 C 1.1508(2) 0.40176(17) 0.29925(17) 0.0220(3) Uani 1 1 d .
C9 C 1.3280(2) 0.45468(17) 0.40890(16) 0.0206(3) Uani 1 1 d .
C10 C 1.3776(2) 0.59956(17) 0.46679(16) 0.0206(3) Uani 1 1 d .
C11 C 1.2494(2) 0.71097(18) 0.44335(17) 0.0231(3) Uani 1 1 d .
C12 C 1.4500(2) 0.35633(17) 0.44247(17) 0.0227(3) Uani 1 1 d .
H12 H 1.4058 0.2434 0.3885 0.044(6) Uiso 1 1 d R
O1W O 0.9160(3) 1.0062(2) 0.6931(2) 0.0523(5) Uani 1 1 d .
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
O3 V1 O2 92.36(6) .
O3 V1 O5 145.98(5) .
O2 V1 O5 91.79(6) .
O3 V1 O1 90.51(5) .
O2 V1 O1 175.69(5) .
O5 V1 O1 87.62(6) .
O3 V1 N1 72.97(6) .
O2 V1 N1 88.60(6) .
O5 V1 N1 73.40(6) .
O1 V1 N1 95.32(5) .
O3 V1 O7 136.13(5) .
O2 V1 O7 85.34(5) .
O5 V1 O7 77.87(6) .
O1 V1 O7 90.36(5) .
N1 V1 O7 150.42(5) .
O3 V1 O8 74.96(5) .
O2 V1 O8 90.03(6) .
O5 V1 O8 138.79(5) .
O1 V1 O8 87.61(6) .
N1 V1 O8 147.81(5) .
O7 V1 O8 61.26(5) .
C1 O3 V1 123.24(11) .
C7 O5 V1 122.77(11) .
C8 O7 V1 90.36(10) .
C8 O8 V1 90.10(10) .
C2 N1 C6 120.32(14) .
C2 N1 V1 120.01(11) .
C6 N1 V1 119.58(11) .
O4 C1 O3 124.38(16) .
O4 C1 C2 122.77(15) .
O3 C1 C2 112.84(14) .
N1 C2 C3 122.12(15) .
N1 C2 C1 110.57(14) .
C3 C2 C1 127.31(15) .
C2 C3 C4 117.74(17) .
C5 C4 C3 119.75(17) .
C6 C5 C4 118.76(17) .
N1 C6 C5 121.28(16) .
N1 C6 C7 110.85(15) .
C5 C6 C7 127.87(16) .
O6 C7 O5 126.61(17) .
O6 C7 C6 120.12(16) .
O5 C7 C6 113.27(14) .
O8 C8 O7 117.96(15) .
O8 C8 C9 120.96(15) .
O7 C8 C9 120.94(14) .
C12 C9 C10 120.34(15) .
C12 C9 C8 118.02(15) .
C10 C9 C8 121.36(14) .
C12 C10 C9 119.02(15) 2_866
C12 C10 C11 117.83(15) 2_866
C9 C10 C11 123.03(15) .
O9 C11 O10 125.05(16) .
O9 C11 C10 122.29(15) .
O10 C11 C10 112.41(15) .
C10 C12 C9 120.64(15) 2_866
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O3 2.0410(12) .
V1 O2 2.0463(14) .
V1 O5 2.0487(12) .
V1 O1 2.0621(13) .
V1 N1 2.1100(17) .
V1 O7 2.1167(14) .
V1 O8 2.1287(16) .
O3 C1 1.290(2) .
O4 C1 1.227(2) .
O5 C7 1.281(2) .
O6 C7 1.227(2) .
O7 C8 1.267(2) .
O8 C8 1.257(2) .
O9 C11 1.207(2) .
O10 C11 1.303(2) .
N1 C2 1.334(2) .
N1 C6 1.335(2) .
C1 C2 1.498(2) .
C2 C3 1.383(2) .
C3 C4 1.394(3) .
C4 C5 1.387(3) .
C5 C6 1.382(3) .
C6 C7 1.503(2) .
C8 C9 1.487(2) .
C9 C12 1.391(2) .
C9 C10 1.397(2) .
C10 C12 1.387(2) 2_866
C10 C11 1.506(2) .
C12 C10 1.387(2) 2_866
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168347928
