#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/30/4303066.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_4303066
loop_
_publ_author_name
'Jana Gáliková'
'Peter Schwendt'
'Jozef Tatiersky'
'Alan S. Tracey'
'Zdirad Žák'
_publ_section_title
;
Stereospecific Formation of Dinuclear Vanadium(V) Tartrato Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8423
_journal_page_last               8430
_journal_paper_doi               10.1021/ic901024p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C16 H28 N2 O14 V2'
_chemical_formula_weight         574.28
_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                68.550(10)
_cell_angle_beta                 86.610(10)
_cell_angle_gamma                66.380(10)
_cell_formula_units_Z            1
_cell_length_a                   7.5271(6)
_cell_length_b                   9.2238(8)
_cell_length_c                   9.9377(8)
_cell_measurement_reflns_used    3178
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.96
_cell_volume                     585.27(11)
_computing_cell_refinement
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 
;
_computing_data_reduction
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 
;
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_diffrn_measurement_method       omega-2theta
_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  0.0116
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'after every 100 frames'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  0.9177
_exptl_absorpt_correction_T_min  0.7495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 

Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0265
_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)+(0.0384P)²+0.4492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                1853
_reflns_number_total             2034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901024p_si_003.cif
_cod_data_source_block           mett
_cod_original_cell_volume        585.30(10)
_cod_database_code               4303066
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
V V 0.21043(4) 0.83468(4) 0.64673(3) 0.01697(12) Uani 1 1 d . . .
O11 O 0.1990(2) 1.00751(16) 0.47568(14) 0.0211(3) Uani 1 1 d . . .
O21 O 0.1602(2) 1.01429(17) 0.72438(14) 0.0238(3) Uani 1 1 d . . .
O31 O 0.1801(2) 1.26460(18) 0.67300(15) 0.0261(3) Uani 1 1 d . . .
O41 O 0.14207(18) 0.70222(17) 0.58175(14) 0.0203(3) Uani 1 1 d . . .
O51 O 0.05968(19) 0.76382(17) 0.80169(13) 0.0202(3) Uani 1 1 d . . .
O61 O -0.1703(2) 0.65985(18) 0.85446(14) 0.0267(3) Uani 1 1 d . . .
C11 C 0.2051(3) 1.1572(2) 0.48079(19) 0.0174(4) Uani 1 1 d . . .
H11 H 0.3317 1.1637 0.4507 0.021 Uiso 1 1 calc R . .
C21 C 0.1812(3) 1.1514(2) 0.6372(2) 0.0189(4) Uani 1 1 d . . .
C31 C -0.0350(3) 0.6891(2) 0.6227(2) 0.0181(4) Uani 1 1 d . . .
H31 H -0.0340 0.5796 0.6247 0.022 Uiso 1 1 calc R . .
C41 C -0.0561(3) 0.6988(2) 0.7752(2) 0.0188(4) Uani 1 1 d . . .
O O 0.4354(2) 0.72172(18) 0.70125(15) 0.0268(3) Uani 1 1 d . . .
N N 0.6303(2) 0.25386(19) 0.84246(16) 0.0179(3) Uani 1 1 d . . .
C12 C 0.7056(4) 0.0646(3) 0.8874(3) 0.0374(6) Uani 1 1 d . . .
H12A H 0.8232 0.0240 0.8400 0.056 Uiso 1 1 calc R . .
H12B H 0.6058 0.0356 0.8586 0.056 Uiso 1 1 calc R . .
H12C H 0.7371 0.0103 0.9931 0.056 Uiso 1 1 calc R . .
C22 C 0.4536(3) 0.3151(3) 0.9185(2) 0.0249(4) Uani 1 1 d . . .
H22A H 0.4881 0.2587 1.0239 0.037 Uiso 1 1 calc R . .
H22B H 0.3517 0.2877 0.8906 0.037 Uiso 1 1 calc R . .
H22C H 0.4056 0.4388 0.8906 0.037 Uiso 1 1 calc R . .
C32 C 0.7837(3) 0.3000(3) 0.8814(2) 0.0319(5) Uani 1 1 d . . .
H32A H 0.8216 0.2438 0.9864 0.048 Uiso 1 1 calc R . .
H32B H 0.7324 0.4239 0.8536 0.048 Uiso 1 1 calc R . .
H32C H 0.8978 0.2626 0.8296 0.048 Uiso 1 1 calc R . .
C42 C 0.5782(3) 0.3366(3) 0.6814(2) 0.0256(4) Uani 1 1 d . . .
H42A H 0.5332 0.4604 0.6512 0.038 Uiso 1 1 calc R . .
H42B H 0.4742 0.3105 0.6550 0.038 Uiso 1 1 calc R . .
H42C H 0.6931 0.2931 0.6325 0.038 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
_geom_angle_publ_flag
O V O41 102.81(7) . . ?
O V O11 106.31(7) . . ?
O41 V O11 101.34(6) . . ?
O V O51 108.48(7) . . ?
O41 V O51 81.13(6) . . ?
O11 V O51 143.60(6) . . ?
O V O21 100.43(7) . . ?
O41 V O21 154.55(6) . . ?
O11 V O21 81.77(5) . . ?
O51 V O21 81.80(6) . . ?
C11 O11 V 118.93(11) . . ?
C21 O21 V 116.16(11) . . ?
C31 O41 V 116.29(11) . . ?
C41 O51 V 116.47(11) . . ?
O11 C11 C31 107.81(15) . 2_576 ?
O11 C11 C21 108.25(14) . . ?
C31 C11 C21 109.90(15) 2_576 . ?
O11 C11 H11 110.3 . . ?
C31 C11 H11 110.3 2_576 . ?
C21 C11 H11 110.3 . . ?
O31 C21 O21 124.80(17) . . ?
O31 C21 C11 122.47(17) . . ?
O21 C21 C11 112.72(15) . . ?
O41 C31 C11 109.72(15) . 2_576 ?
O41 C31 C41 106.03(14) . . ?
C11 C31 C41 107.68(14) 2_576 . ?
O41 C31 H31 111.1 . . ?
C11 C31 H31 111.1 2_576 . ?
C41 C31 H31 111.1 . . ?
O61 C41 O51 125.47(17) . . ?
O61 C41 C31 123.71(17) . . ?
O51 C41 C31 110.72(15) . . ?
C32 N C12 109.92(17) . . ?
C32 N C42 108.78(16) . . ?
C12 N C42 109.30(16) . . ?
C32 N C22 109.57(15) . . ?
C12 N C22 109.35(16) . . ?
C42 N C22 109.89(15) . . ?
N C12 H12A 109.5 . . ?
N C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N C22 H22A 109.5 . . ?
N C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N C32 H32A 109.5 . . ?
N C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N C42 H42A 109.5 . . ?
N C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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
V O 1.5903(14) . ?
V O41 1.8151(13) . ?
V O11 1.8340(13) . ?
V O51 1.9334(13) . ?
V O21 1.9702(13) . ?
O11 C11 1.419(2) . ?
O21 C21 1.311(2) . ?
O31 C21 1.217(2) . ?
O41 C31 1.409(2) . ?
O51 C41 1.323(2) . ?
O61 C41 1.203(2) . ?
C11 C31 1.530(2) 2_576 ?
C11 C21 1.538(2) . ?
C11 H11 1.0000 . ?
C31 C11 1.530(2) 2_576 ?
C31 C41 1.545(2) . ?
C31 H31 1.0000 . ?
N C32 1.494(3) . ?
N C12 1.495(3) . ?
N C42 1.497(2) . ?
N C22 1.500(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139127025
