#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/09/4310992.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_4310992
loop_
_publ_author_name
'Bernd Morgenstern'
'Stefan Steinhauser'
'Kaspar Hegetschweiler'
'Eugenio Garribba'
'Giovanni Micera'
'Daniele Sanna'
'László Nagy'
_publ_section_title
;
 Complex Formation of Vanadium(IV) with
 1,3,5-Triamino-1,3,5-trideoxy-cis-inositol and Related Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3116
_journal_page_last               3126
_journal_paper_doi               10.1021/ic0352046
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24 H83 N6 O32.5 V5'
_chemical_formula_weight         1230.66
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 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                 108.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.720(3)
_cell_length_b                   14.309(3)
_cell_length_c                   14.430(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2688.1(11)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED (STOE, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADI4'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2470
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.9979
_exptl_absorpt_correction_T_min  0.9256
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1052P)²+5.6829P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1688
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                2131
_reflns_number_total             2470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0352046si20040212_051426_2.cif
_cod_data_source_block           '[V(tdci)2][V4O12]x14.5H2O'
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2688.1(10)
_cod_original_formula_sum        'C24 H83 N6 O32.50 V5'
_cod_database_code               4310992
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -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 0.0000 0.0000 0.5000 0.0208(3) Uani 1 4 d S . .
V2 V -0.18729(7) 0.0000 0.90913(7) 0.0375(3) Uani 1 2 d S . .
V3 V 0.0000 0.15159(8) 1.0000 0.0456(4) Uani 1 2 d S . .
O1 O 0.1315(3) 0.0000 0.4780(2) 0.0292(8) Uani 1 2 d S . .
O2 O -0.04615(18) -0.09423(17) 0.39979(16) 0.0252(5) Uani 1 1 d . . .
C1 C 0.1396(4) 0.0000 0.3822(4) 0.0335(12) Uani 1 2 d S . .
H1 H 0.203(6) 0.0000 0.393(5) 0.043(18) Uiso 1 2 d S . .
C2 C 0.0896(3) -0.0855(3) 0.3235(3) 0.0341(9) Uani 1 1 d . . .
H2 H 0.091(3) -0.086(3) 0.255(3) 0.041(12) Uiso 1 1 d . . .
C3 C -0.0257(3) -0.0882(3) 0.3101(2) 0.0262(8) Uani 1 1 d . . .
H3 H -0.057(3) -0.136(3) 0.273(3) 0.020(9) Uiso 1 1 d . . .
C4 C -0.0731(4) 0.0000 0.2534(3) 0.0269(11) Uani 1 2 d S . .
H4 H -0.062(4) 0.0000 0.198(4) 0.024(13) Uiso 1 2 d S . .
N2 N 0.1412(3) -0.1747(3) 0.3718(2) 0.0465(10) Uani 1 1 d . . .
HN2 H 0.126(4) -0.181(4) 0.433(4) 0.065(16) Uiso 1 1 d . . .
C21 C 0.0934(5) -0.2600(4) 0.3167(4) 0.078(2) Uani 1 1 d . . .
H21A H 0.0209 -0.2596 0.3073 0.117 Uiso 1 1 calc R . .
H21B H 0.1237 -0.3146 0.3530 0.117 Uiso 1 1 calc R . .
H21C H 0.1047 -0.2606 0.2544 0.117 Uiso 1 1 calc R . .
C22 C 0.2544(5) 0.1742(7) 0.3866(5) 0.082(2) Uani 1 1 d . . .
H22A H 0.265(4) 0.156(4) 0.320(4) 0.063(16) Uiso 1 1 d . . .
H22B H 0.283(5) 0.233(5) 0.406(4) 0.08(2) Uiso 1 1 d . . .
H22C H 0.289(7) 0.128(7) 0.445(7) 0.14(4) Uiso 1 1 d . . .
N4 N -0.1884(3) 0.0000 0.2346(3) 0.0271(9) Uani 1 2 d S . .
C41 C -0.2401(3) -0.0854(3) 0.1808(3) 0.0431(10) Uani 1 1 d . . .
H41A H -0.3126 -0.0820 0.1708 0.065 Uiso 1 1 calc R . .
H41B H -0.2123 -0.1401 0.2183 0.065 Uiso 1 1 calc R . .
H41C H -0.2284 -0.0887 0.1187 0.065 Uiso 1 1 calc R . .
OV1 O -0.0262(5) 0.1603(5) 1.0914(4) 0.0551(17) Uani 0.50 1 d P . .
OV2 O -0.2761(5) -0.0414(5) 0.9487(5) 0.0589(18) Uani 0.50 1 d P . .
OV3 O -0.2403(5) -0.0459(6) 0.7994(5) 0.0619(19) Uani 0.50 1 d P . .
OV4 O -0.0038(5) 0.2576(5) 1.0566(5) 0.0585(18) Uani 0.50 1 d P . .
OV5 O 0.1228(5) 0.0952(5) 1.0071(5) 0.0558(17) Uani 0.50 1 d P . .
OV6 O 0.0969(5) 0.0838(5) 1.0995(4) 0.0531(17) Uani 0.50 1 d P . .
OW1 O 0.2989(4) 0.0000 0.6339(4) 0.0561(14) Uani 1 2 d S . .
HW1 H 0.260(7) 0.0000 0.594(6) 0.06(3) Uiso 1 2 d S . .
OW2 O -0.1512(3) -0.2325(3) 0.4433(2) 0.0543(9) Uani 1 1 d . . .
HW21 H -0.120(5) -0.195(5) 0.433(4) 0.064(19) Uiso 1 1 d . . .
OW3 O -0.1418(3) 0.3027(3) 1.1549(3) 0.0750(12) Uani 1 1 d . . .
OW4 O 0.0000 -0.3678(6) 0.5000 0.048(2) Uani 0.50 2 d SP . .
OW5 O -0.4861(7) 0.0000 0.8637(9) 0.066(3) Uani 0.50 2 d SP . .
OW7 O -0.4402(12) 0.0000 0.6982(13) 0.132(8) Uani 0.50 2 d SP . .
HW7 H -0.442(4) -0.051(3) 0.660(3) 0.029(11) Uiso 1 1 d . . .
OW8 O -0.0318(18) 0.4302(19) 1.012(3) 0.143(12) Uani 0.26 1 d P . .
OW9 O 0.448(2) -0.056(2) 0.667(2) 0.062(8) Uani 0.12 1 d P . .
HN4 H -0.190(8) 0.0000 0.302(7) 0.10(3) Uiso 1 2 d S . .
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
O1 V1 O1 180.0 5_556 . ?
O1 V1 O2 91.17(10) 5_556 . ?
O1 V1 O2 88.83(10) . . ?
O1 V1 O2 88.83(10) 5_556 5_556 ?
O1 V1 O2 91.17(10) . 5_556 ?
O2 V1 O2 180.0 . 5_556 ?
O1 V1 O2 88.83(10) 5_556 2_556 ?
O1 V1 O2 91.17(10) . 2_556 ?
O2 V1 O2 91.48(14) . 2_556 ?
O2 V1 O2 88.52(14) 5_556 2_556 ?
O1 V1 O2 91.17(10) 5_556 6 ?
O1 V1 O2 88.83(10) . 6 ?
O2 V1 O2 88.52(14) . 6 ?
O2 V1 O2 91.48(14) 5_556 6 ?
O2 V1 O2 180.0 2_556 6 ?
OV2 V2 OV2 43.1(6) 6 . ?
OV2 V2 OV3 109.4(3) 6 . ?
OV2 V2 OV3 92.3(3) . . ?
OV2 V2 OV3 92.3(3) 6 6 ?
OV2 V2 OV3 109.4(3) . 6 ?
OV3 V2 OV3 46.7(6) . 6 ?
OV2 V2 OV6 154.8(4) 6 5_557 ?
OV2 V2 OV6 113.8(4) . 5_557 ?
OV3 V2 OV6 76.6(3) . 5_557 ?
OV3 V2 OV6 108.0(3) 6 5_557 ?
OV2 V2 OV6 113.8(4) 6 2_557 ?
OV2 V2 OV6 154.8(4) . 2_557 ?
OV3 V2 OV6 108.0(3) . 2_557 ?
OV3 V2 OV6 76.6(3) 6 2_557 ?
OV6 V2 OV6 86.1(5) 5_557 2_557 ?
OV2 V2 OV5 76.0(3) 6 2_557 ?
OV2 V2 OV5 107.4(3) . 2_557 ?
OV3 V2 OV5 153.1(4) . 2_557 ?
OV3 V2 OV5 107.9(4) 6 2_557 ?
OV6 V2 OV5 110.3(3) 5_557 2_557 ?
OV6 V2 OV5 48.8(3) 2_557 2_557 ?
OV2 V2 OV5 107.4(3) 6 5_557 ?
OV2 V2 OV5 76.0(3) . 5_557 ?
OV3 V2 OV5 107.9(4) . 5_557 ?
OV3 V2 OV5 153.1(4) 6 5_557 ?
OV6 V2 OV5 48.8(3) 5_557 5_557 ?
OV6 V2 OV5 110.3(3) 2_557 5_557 ?
OV5 V2 OV5 94.8(5) 2_557 5_557 ?
OV1 V3 OV1 170.3(6) 2_557 . ?
OV1 V3 OV4 113.5(4) 2_557 . ?
OV1 V3 OV4 56.8(4) . . ?
OV1 V3 OV4 56.8(4) 2_557 2_557 ?
OV1 V3 OV4 113.5(4) . 2_557 ?
OV4 V3 OV4 57.7(5) . 2_557 ?
OV1 V3 OV5 117.6(3) 2_557 2_557 ?
OV1 V3 OV5 67.1(3) . 2_557 ?
OV4 V3 OV5 104.3(3) . 2_557 ?
OV4 V3 OV5 121.4(3) 2_557 2_557 ?
OV1 V3 OV5 67.1(3) 2_557 . ?
OV1 V3 OV5 117.6(3) . . ?
OV4 V3 OV5 121.4(3) . . ?
OV4 V3 OV5 104.3(3) 2_557 . ?
OV5 V3 OV5 128.0(5) 2_557 . ?
OV1 V3 OV6 71.1(3) 2_557 2_557 ?
OV1 V3 OV6 114.3(3) . 2_557 ?
OV4 V3 OV6 133.6(3) . 2_557 ?
OV4 V3 OV6 102.1(3) 2_557 2_557 ?
OV5 V3 OV6 47.2(3) 2_557 2_557 ?
OV5 V3 OV6 103.3(3) . 2_557 ?
OV1 V3 OV6 114.3(3) 2_557 . ?
OV1 V3 OV6 71.1(3) . . ?
OV4 V3 OV6 102.1(3) . . ?
OV4 V3 OV6 133.6(3) 2_557 . ?
OV5 V3 OV6 103.3(3) 2_557 . ?
OV5 V3 OV6 47.2(3) . . ?
OV6 V3 OV6 118.2(5) 2_557 . ?
C1 O1 V1 121.6(3) . . ?
C3 O2 V1 122.1(2) . . ?
O1 C1 C2 112.4(3) . . ?
O1 C1 C2 112.4(3) . 6 ?
C2 C1 C2 106.9(4) . 6 ?
N2 C2 C1 110.9(3) . . ?
N2 C2 C3 110.5(3) . . ?
C1 C2 C3 110.9(3) . . ?
O2 C3 C2 112.5(3) . . ?
O2 C3 C4 111.5(3) . . ?
C2 C3 C4 107.1(3) . . ?
N4 C4 C3 109.7(3) . . ?
N4 C4 C3 109.7(3) . 6 ?
C3 C4 C3 110.8(4) . 6 ?
C21 N2 C22 110.0(5) . 6 ?
C21 N2 C2 112.3(3) . . ?
C22 N2 C2 111.9(5) 6 . ?
C41 N4 C41 109.0(4) . 6 ?
C41 N4 C4 112.8(3) . . ?
C41 N4 C4 112.8(3) 6 . ?
V3 OV1 OV4 69.9(4) . . ?
OV2 OV2 V2 68.4(3) 6 . ?
OV3 OV3 V2 66.6(3) 6 . ?
OV1 OV4 OV4 113.5(3) . 2_557 ?
OV1 OV4 V3 53.2(3) . . ?
OV4 OV4 V3 61.2(3) 2_557 . ?
OV6 OV5 V3 68.1(3) . . ?
OV6 OV5 V2 62.4(3) . 5_557 ?
V3 OV5 V2 126.8(4) . 5_557 ?
OV5 OV6 V2 68.9(4) . 5_557 ?
OV5 OV6 V3 64.8(3) . . ?
V2 OV6 V3 129.8(3) 5_557 . ?
OW9 OW7 OW9 57.7(19) 1_455 6_455 ?
OW9 OW9 OW7 61.2(10) 6 1_655 ?
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 1.927(3) 5_556 ?
V1 O1 1.927(3) . ?
V1 O2 1.932(2) . ?
V1 O2 1.932(2) 5_556 ?
V1 O2 1.932(2) 2_556 ?
V1 O2 1.932(2) 6 ?
V2 OV2 1.612(6) 6 ?
V2 OV2 1.612(6) . ?
V2 OV3 1.655(6) . ?
V2 OV3 1.655(6) 6 ?
V2 OV6 1.757(6) 5_557 ?
V2 OV6 1.757(6) 2_557 ?
V2 OV5 1.850(7) 2_557 ?
V2 OV5 1.850(7) 5_557 ?
V3 OV1 1.477(6) 2_557 ?
V3 OV1 1.477(6) . ?
V3 OV4 1.732(7) . ?
V3 OV4 1.732(7) 2_557 ?
V3 OV5 1.842(6) 2_557 ?
V3 OV5 1.842(6) . ?
V3 OV6 1.888(6) 2_557 ?
V3 OV6 1.888(6) . ?
O1 C1 1.422(6) . ?
O2 C3 1.411(4) . ?
C1 C2 1.522(5) . ?
C1 C2 1.522(5) 6 ?
C2 N2 1.518(5) . ?
C2 C3 1.532(5) . ?
C3 C4 1.533(4) . ?
C4 N4 1.519(6) . ?
C4 C3 1.533(4) 6 ?
N2 C21 1.491(7) . ?
N2 C22 1.500(7) 6 ?
C22 N2 1.500(7) 6 ?
N4 C41 1.501(5) . ?
N4 C41 1.501(5) 6 ?
OV1 OV4 1.543(11) . ?
OV2 OV2 1.184(16) 6 ?
OV3 OV3 1.312(17) 6 ?
OV4 OV4 1.670(14) 2_557 ?
OV5 OV6 1.492(9) . ?
OV5 V2 1.850(7) 5_557 ?
OV6 V2 1.757(6) 5_557 ?
OW7 OW9 1.66(3) 1_455 ?
OW7 OW9 1.66(3) 6_455 ?
OW8 OW8 1.03(5) 2_557 ?
OW9 OW9 1.61(6) 6 ?
OW9 OW7 1.66(3) 1_655 ?
