#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/30/4303067.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_4303067
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            'C24 H44 N2 O14 V2'
_chemical_formula_weight         686.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.03(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7340(2)
_cell_length_b                   17.8983(3)
_cell_length_c                   13.5159(3)
_cell_measurement_reflns_used    22427
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      3.0
_cell_volume                     3050.30(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38490
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'after every 100 frames'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.7722
_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    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0278
_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)+(0.0528P)²+0.2640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                5003
_reflns_number_total             5996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901024p_si_004.cif
_cod_data_source_block           nett
_cod_database_code               4303067
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.93798(2) 0.098648(15) 0.53636(2) 0.01404(9) Uani 1 1 d . . .
O11 O 1.07958(9) 0.09830(6) 0.57801(8) 0.0162(2) Uani 1 1 d . . .
O21 O 0.93546(9) 0.07133(7) 0.67524(8) 0.0185(3) Uani 1 1 d . . .
O31 O 1.03886(9) 0.03514(7) 0.81462(9) 0.0236(3) Uani 1 1 d . . .
O41 O 0.94226(9) 0.05837(6) 0.41277(8) 0.0172(3) Uani 1 1 d . . .
O51 O 0.79795(9) 0.05229(6) 0.51773(8) 0.0177(3) Uani 1 1 d . . .
O61 O 0.67858(9) -0.00500(7) 0.40459(9) 0.0268(3) Uani 1 1 d . . .
C11 C 1.11836(12) 0.05727(9) 0.66471(12) 0.0149(3) Uani 1 1 d . . .
H11 H 1.1811 0.0831 0.7026 0.018 Uiso 1 1 calc R . .
C21 C 1.02695(13) 0.05381(9) 0.72773(12) 0.0165(3) Uani 1 1 d . . .
C31 C 0.85239(12) 0.02258(9) 0.36165(12) 0.0150(3) Uani 1 1 d . . .
H31 H 0.8264 0.0507 0.2991 0.018 Uiso 1 1 calc R . .
C41 C 0.76573(13) 0.02161(9) 0.43051(12) 0.0169(3) Uani 1 1 d . . .
OW1 O 0.90789(9) 0.18493(6) 0.52239(9) 0.0232(3) Uani 1 1 d . . .
V2 V 0.45869(2) 0.087773(15) 0.06301(2) 0.01359(9) Uani 1 1 d . . .
O12 O 0.53465(8) 0.00307(6) 0.10441(8) 0.0143(2) Uani 1 1 d . . .
O22 O 0.60075(9) 0.12498(6) 0.05031(9) 0.0179(3) Uani 1 1 d . . .
O32 O 0.77017(9) 0.10990(7) 0.11978(9) 0.0225(3) Uani 1 1 d . . .
O42 O 0.32940(8) 0.04774(6) 0.01980(8) 0.0154(2) Uani 1 1 d . . .
O52 O 0.41790(9) 0.15279(6) -0.05179(8) 0.0168(3) Uani 1 1 d . . .
O62 O 0.30682(10) 0.15754(7) -0.19607(9) 0.0231(3) Uani 1 1 d . . .
C12 C 0.64464(12) 0.01068(9) 0.13528(12) 0.0144(3) Uani 1 1 d . . .
H12 H 0.6608 0.0065 0.2096 0.017 Uiso 1 1 calc R . .
C22 C 0.67954(13) 0.08767(9) 0.10025(12) 0.0157(3) Uani 1 1 d . . .
C32 C 0.29866(13) 0.05146(9) -0.08509(12) 0.0154(3) Uani 1 1 d . . .
H32 H 0.2199 0.0478 -0.1029 0.019 Uiso 1 1 calc R . .
C42 C 0.34059(13) 0.12723(9) -0.11754(12) 0.0162(3) Uani 1 1 d . . .
OW2 O 0.43922(9) 0.12986(7) 0.16270(9) 0.0211(3) Uani 1 1 d . . .
N1 N 0.62423(12) 0.15849(9) 0.72207(13) 0.0271(4) Uani 1 1 d . . .
C13 C 0.58573(16) 0.21876(11) 0.78770(16) 0.0348(5) Uani 1 1 d . . .
H13A H 0.5140 0.2347 0.7572 0.042 Uiso 1 1 calc R . .
H13B H 0.5789 0.1965 0.8536 0.042 Uiso 1 1 calc R . .
C23 C 0.65557(19) 0.28762(12) 0.80450(17) 0.0412(5) Uani 1 1 d . . .
H23A H 0.6178 0.3268 0.8359 0.062 Uiso 1 1 calc R . .
H23B H 0.6728 0.3056 0.7402 0.062 Uiso 1 1 calc R . .
H23C H 0.7211 0.2749 0.8482 0.062 Uiso 1 1 calc R . .
C33 C 0.55554(16) 0.09021(11) 0.73214(18) 0.0342(5) Uani 1 1 d . . .
H33A H 0.5610 0.0770 0.8038 0.041 Uiso 1 1 calc R . .
H33B H 0.4807 0.1036 0.7089 0.041 Uiso 1 1 calc R . .
C43 C 0.58355(17) 0.02205(12) 0.67496(18) 0.0401(5) Uani 1 1 d . . .
H43A H 0.5293 -0.0165 0.6774 0.060 Uiso 1 1 calc R . .
H43B H 0.6527 0.0027 0.7052 0.060 Uiso 1 1 calc R . .
H43C H 0.5868 0.0358 0.6053 0.060 Uiso 1 1 calc R . .
C53 C 0.74057(15) 0.14067(12) 0.75395(16) 0.0321(5) Uani 1 1 d . . .
H53A H 0.7827 0.1859 0.7444 0.039 Uiso 1 1 calc R . .
H53B H 0.7620 0.1014 0.7092 0.039 Uiso 1 1 calc R . .
C63 C 0.76871(18) 0.11450(14) 0.86125(17) 0.0426(6) Uani 1 1 d . . .
H63A H 0.8442 0.1016 0.8738 0.064 Uiso 1 1 calc R . .
H63B H 0.7261 0.0705 0.8724 0.064 Uiso 1 1 calc R . .
H63C H 0.7540 0.1546 0.9068 0.064 Uiso 1 1 calc R . .
C73 C 0.61565(15) 0.18376(11) 0.61349(15) 0.0315(5) Uani 1 1 d . . .
H73A H 0.6498 0.2334 0.6117 0.038 Uiso 1 1 calc R . .
H73B H 0.6561 0.1484 0.5770 0.038 Uiso 1 1 calc R . .
C83 C 0.50329(18) 0.18916(13) 0.55863(18) 0.0438(6) Uani 1 1 d . . .
H83A H 0.5048 0.2116 0.4927 0.066 Uiso 1 1 calc R . .
H83B H 0.4604 0.2203 0.5972 0.066 Uiso 1 1 calc R . .
H83C H 0.4722 0.1391 0.5506 0.066 Uiso 1 1 calc R . .
N2 N 0.12039(11) 0.17079(7) 0.20130(10) 0.0153(3) Uani 1 1 d . . .
C14 C 0.01623(14) 0.17487(11) 0.24341(14) 0.0271(4) Uani 1 1 d . . .
H14A H -0.0422 0.1782 0.1870 0.033 Uiso 1 1 calc R . .
H14B H 0.0068 0.1277 0.2794 0.033 Uiso 1 1 calc R . .
C24 C 0.00593(17) 0.23910(12) 0.31341(16) 0.0363(5) Uani 1 1 d . . .
H24A H -0.0592 0.2332 0.3437 0.054 Uiso 1 1 calc R . .
H24B H 0.0030 0.2862 0.2761 0.054 Uiso 1 1 calc R . .
H24C H 0.0673 0.2397 0.3660 0.054 Uiso 1 1 calc R . .
C34 C 0.21457(14) 0.16391(11) 0.28540(14) 0.0254(4) Uani 1 1 d . . .
H34A H 0.2790 0.1519 0.2551 0.031 Uiso 1 1 calc R . .
H34B H 0.2262 0.2131 0.3188 0.031 Uiso 1 1 calc R . .
C44 C 0.20187(16) 0.10597(12) 0.36345(15) 0.0298(4) Uani 1 1 d . . .
H44A H 0.2686 0.1009 0.4088 0.045 Uiso 1 1 calc R . .
H44B H 0.1833 0.0579 0.3309 0.045 Uiso 1 1 calc R . .
H44C H 0.1454 0.1213 0.4015 0.045 Uiso 1 1 calc R . .
C54 C 0.11965(17) 0.10209(10) 0.13526(15) 0.0293(4) Uani 1 1 d . . .
H54A H 0.1904 0.0970 0.1136 0.035 Uiso 1 1 calc R . .
H54B H 0.1080 0.0575 0.1757 0.035 Uiso 1 1 calc R . .
C64 C 0.0372(2) 0.10269(13) 0.04380(15) 0.0432(6) Uani 1 1 d . . .
H64A H 0.0448 0.0578 0.0040 0.065 Uiso 1 1 calc R . .
H64B H 0.0467 0.1472 0.0037 0.065 Uiso 1 1 calc R . .
H64C H -0.0337 0.1035 0.0642 0.065 Uiso 1 1 calc R . .
C74 C 0.13420(14) 0.24196(10) 0.14365(14) 0.0239(4) Uani 1 1 d . . .
H74A H 0.0681 0.2510 0.0973 0.029 Uiso 1 1 calc R . .
H74B H 0.1431 0.2841 0.1916 0.029 Uiso 1 1 calc R . .
C84 C 0.22587(16) 0.24279(11) 0.08431(16) 0.0326(5) Uani 1 1 d . . .
H84A H 0.2306 0.2920 0.0535 0.049 Uiso 1 1 calc R . .
H84B H 0.2148 0.2045 0.0320 0.049 Uiso 1 1 calc R . .
H84C H 0.2918 0.2324 0.1288 0.049 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
OW1 V1 O11 104.60(6) . . ?
OW1 V1 O41 108.12(6) . . ?
O11 V1 O41 97.31(5) . . ?
OW1 V1 O21 108.75(6) . . ?
O11 V1 O21 81.32(5) . . ?
O41 V1 O21 142.19(5) . . ?
OW1 V1 O51 101.32(6) . . ?
O11 V1 O51 152.92(5) . . ?
O41 V1 O51 81.82(5) . . ?
O21 V1 O51 83.08(5) . . ?
C11 O11 V1 118.49(10) . . ?
C21 O21 V1 116.62(10) . . ?
C31 O41 V1 120.19(10) . . ?
C41 O51 V1 117.32(10) . . ?
O11 C11 C31 111.12(13) . 3_756 ?
O11 C11 C21 106.07(12) . . ?
C31 C11 C21 108.60(13) 3_756 . ?
O31 C21 O21 124.83(16) . . ?
O31 C21 C11 123.18(15) . . ?
O21 C21 C11 111.97(13) . . ?
O41 C31 C11 109.38(13) . 3_756 ?
O41 C31 C41 108.12(12) . . ?
C11 C31 C41 110.37(13) 3_756 . ?
O61 C41 O51 125.57(16) . . ?
O61 C41 C31 122.26(15) . . ?
O51 C41 C31 112.18(13) . . ?
OW2 V2 O42 102.56(6) . . ?
OW2 V2 O12 105.62(6) . . ?
O42 V2 O12 100.78(5) . . ?
OW2 V2 O52 109.57(5) . . ?
O42 V2 O52 81.42(5) . . ?
O12 V2 O52 143.36(5) . . ?
OW2 V2 O22 99.68(6) . . ?
O42 V2 O22 156.01(5) . . ?
O12 V2 O22 81.62(5) . . ?
O52 V2 O22 82.76(5) . . ?
C12 O12 V2 117.88(9) . . ?
C22 O22 V2 115.57(10) . . ?
C32 O42 V2 114.46(10) . . ?
C42 O52 V2 114.94(10) . . ?
O12 C12 C32 107.95(12) . 3_655 ?
O12 C12 C22 108.18(12) . . ?
C32 C12 C22 109.77(13) 3_655 . ?
O32 C22 O22 125.49(15) . . ?
O32 C22 C12 122.13(14) . . ?
O22 C22 C12 112.36(13) . . ?
O42 C32 C12 109.07(12) . 3_655 ?
O42 C32 C42 105.49(12) . . ?
C12 C32 C42 107.96(13) 3_655 . ?
O62 C42 O52 125.15(15) . . ?
O62 C42 C32 123.09(15) . . ?
O52 C42 C32 111.73(13) . . ?
C53 N1 C33 110.90(14) . . ?
C53 N1 C13 111.40(16) . . ?
C33 N1 C13 106.36(14) . . ?
C53 N1 C73 105.75(14) . . ?
C33 N1 C73 111.09(16) . . ?
C13 N1 C73 111.43(14) . . ?
C23 C13 N1 115.68(16) . . ?
C43 C33 N1 115.01(17) . . ?
N1 C53 C63 115.26(16) . . ?
C83 C73 N1 115.11(17) . . ?
C74 N2 C14 108.83(13) . . ?
C74 N2 C54 111.70(14) . . ?
C14 N2 C54 109.00(14) . . ?
C74 N2 C34 108.22(13) . . ?
C14 N2 C34 111.05(13) . . ?
C54 N2 C34 108.04(13) . . ?
C24 C14 N2 115.47(16) . . ?
C44 C34 N2 115.12(15) . . ?
C64 C54 N2 115.03(17) . . ?
C84 C74 N2 115.86(14) . . ?
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 OW1 1.5959(12) . ?
V1 O11 1.8124(11) . ?
V1 O41 1.8271(11) . ?
V1 O21 1.9444(12) . ?
V1 O51 1.9509(11) . ?
O11 C11 1.4122(19) . ?
O21 C21 1.3146(19) . ?
O31 C21 1.210(2) . ?
O41 C31 1.4058(18) . ?
O51 C41 1.313(2) . ?
O61 C41 1.214(2) . ?
C11 C31 1.531(2) 3_756 ?
C11 C21 1.537(2) . ?
C31 C11 1.531(2) 3_756 ?
C31 C41 1.540(2) . ?
V2 OW2 1.5931(12) . ?
V2 O42 1.8156(11) . ?
V2 O12 1.8428(11) . ?
V2 O52 1.9509(11) . ?
V2 O22 1.9577(11) . ?
O12 C12 1.4110(18) . ?
O22 C22 1.3111(19) . ?
O32 C22 1.214(2) . ?
O42 C32 1.4187(19) . ?
O52 C42 1.313(2) . ?
O62 C42 1.216(2) . ?
C12 C32 1.535(2) 3_655 ?
C12 C22 1.543(2) . ?
C32 C12 1.535(2) 3_655 ?
C32 C42 1.543(2) . ?
N1 C53 1.518(2) . ?
N1 C33 1.520(2) . ?
N1 C13 1.521(3) . ?
N1 C73 1.525(2) . ?
C13 C23 1.518(3) . ?
C33 C43 1.513(3) . ?
C53 C63 1.519(3) . ?
C73 C83 1.520(3) . ?
N2 C74 1.516(2) . ?
N2 C14 1.516(2) . ?
N2 C54 1.519(2) . ?
N2 C34 1.538(2) . ?
C14 C24 1.506(3) . ?
C34 C44 1.504(3) . ?
C54 C64 1.506(3) . ?
C74 C84 1.506(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139127026
