#------------------------------------------------------------------------------
#$Date: 2023-12-07 13:18:01 +0200 (Thu, 07 Dec 2023) $
#$Revision: 288121 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/93/7009302.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_7009302
loop_
_publ_author_name
'Ceccato, Augusto S.'
'Neves, Ademir'
'de Brito, Marcos A.'
'Drechsel, Sueli M.'
'Mangrich, Antonio S.'
'Werner, Rüdiger'
'Haase, Wolfgang'
'Bortoluzzi, Adailton J.'
_publ_section_title
;
 Magneto-structural correlation for binuclear octahedral
 vanadium(IV)--oxo complexes. Synthesis, structure and magnetic
 properties of a VIVO2+ complex with a new ligand derived from glycine
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1573
_journal_paper_doi               10.1039/a909846a
_journal_year                    2000
_chemical_formula_moiety
;
C32 H28 N2 O12 V2, 2(C6 H16 N), 4(C H2 Cl2)
;
_chemical_formula_sum            'C48 H68 Cl8 N4 O10 V2'
_chemical_formula_weight         1246.54
_chemical_name_systematic
;
Triethylammonium-bis{[N,N-bis(2-oxyphenyl)glycinate]
oxovanadium(IV)} dichloromethane solvate
;
_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           'SHELXL97 and manual editing'
_cell_angle_alpha                98.11(3)
_cell_angle_beta                 102.00(3)
_cell_angle_gamma                110.17(3)
_cell_formula_units_Z            1
_cell_length_a                   10.638(2)
_cell_length_b                   11.380(2)
_cell_length_c                   13.512(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      13.85
_cell_measurement_theta_min      7.57
_cell_volume                     1461.0(6)
_computing_cell_refinement
;
SET4 in CAD4 EXPRESS (Enraf-Nonius, 1994)  
;
_computing_data_collection       'CAD4-EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'HELENA (Spek, 1996)'
_computing_molecular_graphics
;
ZORTEP (Zsolnai et al., 1996)
;
_computing_publication_material
;
SHELXL97. All calculations were performed on a PC/Pentim II  computer
running LINUX.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       ω--2θ
_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  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5432
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        4.1
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'PLATON (Spek, 1990)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0031(14)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[σ²(Fo²)+(0.0681P)²+0.8873P] where P=3D(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                4570
_reflns_number_total             5133
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            a909846a.txt
_cod_data_source_block           9/02385B
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8873P] where P=3D(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=3D1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8873P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1461.0(4)
_cod_database_code               7009302
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.54336(4) 0.94422(3) 0.59474(3) 0.02129(14) Uani 1 d . . .
O1 O 0.69705(16) 1.05088(15) 0.65300(12) 0.0294(4) Uani 1 d . . .
O2 O 0.36293(16) 0.77177(14) 0.50926(12) 0.0273(3) Uani 1 d . . .
O3 O 0.26460(17) 0.55819(15) 0.48578(14) 0.0369(4) Uani 1 d . . .
O10 O 0.47505(17) 0.90904(15) 0.71489(12) 0.0296(4) Uani 1 d . . .
O20 O 0.56124(15) 0.94190(14) 0.44359(11) 0.0239(3) Uani 1 d . . .
N1 N 0.61691(18) 0.79208(17) 0.60899(14) 0.0226(4) Uani 1 d . . .
C1 C 0.4999(2) 0.6652(2) 0.58679(17) 0.0248(5) Uani 1 d . . .
H1A H 0.4864 0.6442 0.6519 0.030 Uiso 1 calc R . .
H1B H 0.5239 0.5995 0.5507 0.030 Uiso 1 calc R . .
C2 C 0.3655(2) 0.6641(2) 0.52113(17) 0.0256(5) Uani 1 d . . .
C10 C 0.7093(2) 0.8193(2) 0.71599(17) 0.0279(5) Uani 1 d . . .
H10A H 0.7865 0.9013 0.7290 0.033 Uiso 1 calc R . .
H10B H 0.7478 0.7536 0.7194 0.033 Uiso 1 calc R . .
C11 C 0.6374(2) 0.8234(2) 0.80036(17) 0.0278(5) Uani 1 d . . .
C12 C 0.5293(2) 0.8705(2) 0.79618(17) 0.0261(5) Uani 1 d . . .
C13 C 0.4757(3) 0.8738(2) 0.88261(19) 0.0337(5) Uani 1 d . . .
H13A H 0.4051 0.9045 0.8818 0.040 Uiso 1 calc R . .
C14 C 0.5245(3) 0.8329(3) 0.9690(2) 0.0423(6) Uani 1 d . . .
H14A H 0.4875 0.8376 1.0254 0.051 Uiso 1 calc R . .
C15 C 0.6273(3) 0.7855(3) 0.9720(2) 0.0489(7) Uani 1 d . . .
H15A H 0.6598 0.7572 1.0296 0.059 Uiso 1 calc R . .
C16 C 0.6818(3) 0.7804(3) 0.8880(2) 0.0402(6) Uani 1 d . . .
H16A H 0.7506 0.7472 0.8898 0.048 Uiso 1 calc R . .
C20 C 0.7040(2) 0.7936(2) 0.53476(18) 0.0265(5) Uani 1 d . . .
H20A H 0.7492 0.7339 0.5461 0.032 Uiso 1 calc R . .
H20B H 0.7764 0.8790 0.5499 0.032 Uiso 1 calc R . .
C21 C 0.6229(2) 0.7585(2) 0.42234(17) 0.0252(5) Uani 1 d . . .
C22 C 0.5570(2) 0.8355(2) 0.38017(17) 0.0242(4) Uani 1 d . . .
C23 C 0.4905(2) 0.8025(2) 0.27429(18) 0.0287(5) Uani 1 d . . .
H23A H 0.4478 0.8535 0.2458 0.034 Uiso 1 calc R . .
C24 C 0.4875(3) 0.6938(2) 0.21088(19) 0.0333(5) Uani 1 d . . .
H24A H 0.4430 0.6728 0.1401 0.040 Uiso 1 calc R . .
C25 C 0.5501(3) 0.6162(2) 0.2521(2) 0.0354(6) Uani 1 d . . .
H25A H 0.5472 0.5430 0.2096 0.042 Uiso 1 calc R . .
C26 C 0.6168(2) 0.6491(2) 0.35701(19) 0.0307(5) Uani 1 d . . .
H26A H 0.6587 0.5971 0.3848 0.037 Uiso 1 calc R . .
N1N N 0.0612(2) 0.5897(2) 0.34320(17) 0.0317(4) Uani 1 d . . .
H1NA H 0.121(3) 0.590(3) 0.394(2) 0.043(8) Uiso 1 d . . .
C11N C -0.0648(3) 0.4706(3) 0.3314(2) 0.0452(7) Uani 1 d . . .
H11A H -0.0930 0.4758 0.3951 0.054 Uiso 1 calc R . .
H11B H -0.0393 0.3966 0.3222 0.054 Uiso 1 calc R . .
C12N C -0.1874(3) 0.4491(4) 0.2417(3) 0.0741(12) Uani 1 d . . .
H12B H -0.2635 0.3717 0.2392 0.111 Uiso 1 calc R . .
H12C H -0.1615 0.4413 0.1778 0.111 Uiso 1 calc R . .
H12D H -0.2153 0.5208 0.2508 0.111 Uiso 1 calc R . .
C21N C 0.1170(3) 0.5926(3) 0.2501(2) 0.0446(6) Uani 1 d . . .
H21A H 0.2000 0.6705 0.2650 0.054 Uiso 1 calc R . .
H21B H 0.0483 0.5958 0.1920 0.054 Uiso 1 calc R . .
C22N C 0.1526(3) 0.4783(3) 0.2193(3) 0.0547(8) Uani 1 d . . .
H22B H 0.1881 0.4856 0.1597 0.082 Uiso 1 calc R . .
H22C H 0.0705 0.4009 0.2026 0.082 Uiso 1 calc R . .
H22D H 0.2221 0.4755 0.2760 0.082 Uiso 1 calc R . .
C31N C 0.0397(3) 0.7115(2) 0.3744(2) 0.0409(6) Uani 1 d . . .
H31A H 0.1196 0.7840 0.3719 0.049 Uiso 1 calc R . .
H31B H -0.0417 0.7096 0.3248 0.049 Uiso 1 calc R . .
C32N C 0.0204(3) 0.7304(3) 0.4812(2) 0.0493(7) Uani 1 d . . .
H32A H 0.0071 0.8094 0.4976 0.074 Uiso 1 calc R . .
H32B H 0.1014 0.7341 0.5308 0.074 Uiso 1 calc R . .
H32C H -0.0599 0.6598 0.4838 0.074 Uiso 1 calc R . .
C41 C 0.1983(3) 0.9884(3) 0.7413(3) 0.0532(8) Uani 1 d . . .
H41A H 0.2666 1.0586 0.7974 0.064 Uiso 1 calc R . .
H41B H 0.2480 0.9533 0.7009 0.064 Uiso 1 calc R . .
Cl42 Cl 0.09799(9) 0.86788(9) 0.79403(8) 0.0684(3) Uani 1 d . . .
Cl43 Cl 0.09310(9) 1.04762(8) 0.66132(8) 0.0633(3) Uani 1 d . . .
C51 C 0.1641(4) 0.8592(4) 1.0855(3) 0.0740(11) Uani 1 d D . .
Cl52 Cl 0.1595(7) 0.7110(4) 1.0216(4) 0.0666(14) Uani 0.50 d PDU . .
Cl53 Cl 0.0070(4) 0.8635(4) 1.0736(4) 0.0978(13) Uani 0.50 d PDU . .
Cl52' Cl 0.1798(7) 0.7272(6) 1.0282(6) 0.095(2) Uani 0.50 d PDU . .
Cl53' Cl -0.0210(6) 0.8068(7) 1.0927(4) 0.154(3) Uani 0.50 d PDU . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 V1 O10 99.77(8) . . ?
O1 V1 O20 100.85(7) . 2_676 ?
O10 V1 O20 95.92(7) . 2_676 ?
O1 V1 O20 96.45(8) . . ?
O10 V1 O20 163.77(7) . . ?
O20 V1 O20 81.38(7) 2_676 . ?
O1 V1 N1 90.94(8) . . ?
O10 V1 N1 86.11(7) . . ?
O20 V1 N1 167.48(7) 2_676 . ?
O20 V1 N1 93.22(7) . . ?
O1 V1 O2 166.44(7) . . ?
O10 V1 O2 84.49(7) . . ?
O20 V1 O2 91.43(6) 2_676 . ?
O20 V1 O2 79.60(7) . . ?
N1 V1 O2 76.44(7) . . ?
C2 O2 V1 117.98(14) . . ?
C12 O10 V1 129.19(14) . . ?
C22 O20 V1 126.69(14) . 2_676 ?
C22 O20 V1 122.20(13) . . ?
V1 O20 V1 98.62(7) 2_676 . ?
C1 N1 C10 109.47(17) . . ?
C1 N1 C20 111.43(17) . . ?
C10 N1 C20 107.48(17) . . ?
C1 N1 V1 111.72(13) . . ?
C10 N1 V1 109.80(13) . . ?
C20 N1 V1 106.82(13) . . ?
N1 C1 C2 112.10(17) . . ?
O3 C2 O2 125.1(2) . . ?
O3 C2 C1 117.81(19) . . ?
O2 C2 C1 117.01(19) . . ?
N1 C10 C11 114.03(18) . . ?
C16 C11 C12 118.8(2) . . ?
C16 C11 C10 117.7(2) . . ?
C12 C11 C10 123.5(2) . . ?
O10 C12 C13 118.7(2) . . ?
O10 C12 C11 124.0(2) . . ?
C13 C12 C11 117.3(2) . . ?
C14 C13 C12 122.2(2) . . ?
C15 C14 C13 120.3(2) . . ?
C14 C15 C16 119.0(2) . . ?
C15 C16 C11 122.4(2) . . ?
N1 C20 C21 113.85(18) . . ?
C26 C21 C22 119.0(2) . . ?
C26 C21 C20 119.2(2) . . ?
C22 C21 C20 121.8(2) . . ?
O20 C22 C23 121.2(2) . . ?
O20 C22 C21 119.4(2) . . ?
C23 C22 C21 119.3(2) . . ?
C24 C23 C22 120.4(2) . . ?
C25 C24 C23 120.6(2) . . ?
C26 C25 C24 119.1(2) . . ?
C25 C26 C21 121.5(2) . . ?
H1NA N1N C21N 109(2) . . ?
H1NA N1N C31N 105(2) . . ?
C21N N1N C31N 110.0(2) . . ?
H1NA N1N C11N 105(2) . . ?
C21N N1N C11N 114.1(2) . . ?
C31N N1N C11N 113.1(2) . . ?
N1N C11N C12N 114.3(3) . . ?
N1N C21N C22N 113.2(2) . . ?
C32N C31N N1N 112.6(2) . . ?
Cl43 C41 Cl42 111.41(17) . . ?
Cl53 C51 Cl52 113.4(3) . . ?
Cl53 C51 Cl52' 120.0(4) . . ?
Cl52' C51 Cl52 6.6(4) . . ?
Cl53 C51 Cl53' 22.4(2) . . ?
Cl52' C51 Cl53' 105.9(4) . . ?
Cl52 C51 Cl53' 99.4(4) . . ?
Cl53' Cl53 C51 95.9(7) . . ?
Cl53 Cl53' C51 61.8(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.6102(18) . ?
V1 O10 1.9487(16) . ?
V1 O20 2.0323(15) 2_676 ?
V1 O20 2.0876(15) . ?
V1 N1 2.1476(18) . ?
V1 O2 2.1703(19) . ?
O2 C2 1.267(3) . ?
O3 C2 1.251(3) . ?
O10 C12 1.334(3) . ?
O20 C22 1.362(3) . ?
O20 V1 2.0323(15) 2_676 ?
N1 C1 1.486(3) . ?
N1 C10 1.492(3) . ?
N1 C20 1.498(3) . ?
C1 C2 1.513(3) . ?
C10 C11 1.504(3) . ?
C11 C16 1.399(3) . ?
C11 C12 1.421(3) . ?
C12 C13 1.404(3) . ?
C13 C14 1.385(4) . ?
C14 C15 1.373(4) . ?
C15 C16 1.379(4) . ?
C20 C21 1.502(3) . ?
C21 C26 1.394(3) . ?
C21 C22 1.409(3) . ?
C22 C23 1.390(3) . ?
C23 C24 1.388(3) . ?
C24 C25 1.387(4) . ?
C25 C26 1.379(4) . ?
N1N H1NA 0.84(3) . ?
N1N C21N 1.498(3) . ?
N1N C31N 1.498(3) . ?
N1N C11N 1.502(3) . ?
C11N C12N 1.506(5) . ?
C21N C22N 1.504(4) . ?
C31N C32N 1.497(4) . ?
C41 Cl43 1.759(3) . ?
C41 Cl42 1.764(3) . ?
C51 Cl53 1.664(6) . ?
C51 Cl52' 1.669(7) . ?
C51 Cl52 1.763(5) . ?
C51 Cl53' 1.879(7) . ?
Cl53 Cl53' 0.719(8) . ?
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
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1N H1NA O2 0.84(3) 2.66(3) 3.277(3) 131(3) . .
N1N H1NA O3 0.84(3) 1.92(3) 2.742(3) 165(3) . .
