#------------------------------------------------------------------------------
#$Date: 2016-10-07 10:37:42 +0300 (Fri, 07 Oct 2016) $
#$Revision: 187017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/73/4307304.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_4307304
loop_
_publ_author_name
'Bernd Morgenstern'
'Barbara Kutzky'
'Christian Neis'
'Stefan Stucky'
'Kaspar Hegetschweiler'
'Eugenio Garribba'
'Giovanni Micera'
_publ_section_title
;
Synthesis and Characterization of Vanadium(IV) Complexes with cis-Inositol
in Aqueous Solution and in the Solid-State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3903
_journal_page_last               3915
_journal_paper_doi               10.1021/ic0618504
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C24 H50 K2 O28 V'
_chemical_formula_weight         915.78
_chemical_name_systematic
; 
 ? 
;
_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                99.394(3)
_cell_angle_beta                 108.736(2)
_cell_angle_gamma                106.614(3)
_cell_formula_units_Z            1
_cell_length_a                   9.6731(5)
_cell_length_b                   9.8194(5)
_cell_length_c                   9.8842(4)
_cell_measurement_reflns_used    7404
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.87
_cell_measurement_theta_min      2.26
_cell_volume                     817.63(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27708
_diffrn_reflns_theta_full        37.94
_diffrn_reflns_theta_max         37.94
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             479
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0383
_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)+(0.0524P)²+0.0920P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                6423
_reflns_number_total             8136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0618504si20070214_125158_1.cif
_cod_data_source_block           '[V(inoH-3)2][K2(ino)2]x4H2O'
_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 
;
_cod_original_formula_sum        'C12 H25 K O14 V0.50'
_cod_database_code               4307304
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
V1 V 0.0000 0.0000 0.0000 0.00682(5) Uani 1 2 d S . .
C1 C -0.22313(13) 0.17274(13) 0.09342(11) 0.01030(18) Uani 1 1 d . . .
H1 H -0.3059(19) 0.2109(18) 0.0711(17) 0.008(4) Uiso 1 1 d . . .
O1 O -0.14951(11) 0.21116(11) 0.25160(9) 0.01346(16) Uani 1 1 d . . .
H1O H -0.061(3) 0.231(2) 0.274(2) 0.035(6) Uiso 1 1 d . . .
C2 C -0.10938(12) 0.24714(12) 0.02731(12) 0.00938(17) Uani 1 1 d . . .
H2 H -0.073(2) 0.3540(19) 0.0717(18) 0.012(4) Uiso 1 1 d . . .
O2 O 0.02082(9) 0.20088(9) 0.06471(9) 0.00971(14) Uani 1 1 d . . .
C3 C 0.19209(13) -0.20908(12) 0.14190(12) 0.00942(17) Uani 1 1 d . . .
H3 H 0.2710(18) -0.2507(18) 0.1684(17) 0.007(4) Uiso 1 1 d . . .
O3 O 0.08536(10) -0.27418(10) 0.20505(10) 0.01255(15) Uani 1 1 d . . .
H3O H 0.033(2) -0.231(2) 0.200(2) 0.025(5) Uiso 1 1 d . . .
C4 C 0.26372(12) -0.04079(12) 0.21239(11) 0.00876(17) Uani 1 1 d . . .
H4 H 0.322(2) -0.0207(19) 0.3169(19) 0.012(4) Uiso 1 1 d . . .
O4 O 0.14209(9) 0.01643(9) 0.19533(8) 0.00904(14) Uani 1 1 d . . .
C5 C -0.37565(12) -0.03087(12) -0.14295(12) 0.00941(17) Uani 1 1 d . . .
H5 H -0.4619(19) 0.0058(18) -0.1651(18) 0.010(4) Uiso 1 1 d . . .
O5 O -0.45154(10) -0.18660(10) -0.21095(10) 0.01255(15) Uani 1 1 d . . .
H5O H -0.396(2) -0.227(2) -0.186(2) 0.022(5) Uiso 1 1 d . . .
C6 C -0.29055(12) 0.00474(13) 0.02544(12) 0.00941(17) Uani 1 1 d . . .
H6 H -0.365(2) -0.039(2) 0.0650(19) 0.016(4) Uiso 1 1 d . . .
O6 O -0.17428(9) -0.05961(9) 0.05819(9) 0.00961(14) Uani 1 1 d . . .
K1 K -0.12575(3) 0.10753(3) 0.49297(3) 0.01131(5) Uani 1 1 d . . .
C7 C 0.30500(13) 0.44968(12) 0.79386(11) 0.00960(17) Uani 1 1 d . . .
H7 H 0.4124(18) 0.5207(18) 0.8367(16) 0.005(3) Uiso 1 1 d . . .
O7 O 0.24215(11) 0.47695(10) 0.90376(9) 0.01276(15) Uani 1 1 d . . .
H7O H 0.150(3) 0.444(2) 0.870(2) 0.027(5) Uiso 1 1 d . . .
C8 C 0.31141(12) 0.29338(12) 0.76614(11) 0.00967(17) Uani 1 1 d . . .
O8 O 0.16234(10) 0.18035(10) 0.72560(9) 0.01118(14) Uani 1 1 d . . .
H8O H 0.170(2) 0.139(2) 0.800(2) 0.025(5) Uiso 1 1 d . . .
H8 H 0.3809(19) 0.2934(19) 0.8586(18) 0.010(4) Uiso 1 1 d . . .
C9 C 0.38109(12) 0.27396(12) 0.64893(12) 0.00921(17) Uani 1 1 d . . .
H9 H 0.4852(19) 0.3531(18) 0.6904(17) 0.008(4) Uiso 1 1 d . . .
O9 O -0.39672(10) -0.13290(9) 0.37295(10) 0.01198(15) Uani 1 1 d . . .
H9O H -0.460(3) -0.138(2) 0.409(2) 0.032(6) Uiso 1 1 d . . .
C10 C 0.28962(12) 0.29727(12) 0.50131(11) 0.00881(17) Uani 1 1 d . . .
H10 H 0.350(2) 0.292(2) 0.4377(19) 0.016(4) Uiso 1 1 d . . .
O10 O 0.13784(9) 0.18563(9) 0.42405(9) 0.01019(14) Uani 1 1 d . . .
H10O H 0.145(2) 0.139(2) 0.360(2) 0.027(5) Uiso 1 1 d . . .
C11 C -0.28482(13) 0.54675(12) 0.46449(11) 0.00927(17) Uani 1 1 d . . .
H11 H -0.3946(19) 0.4790(19) 0.4207(18) 0.011(4) Uiso 1 1 d . . .
O11 O -0.20112(10) 0.51247(10) 0.59454(9) 0.01188(15) Uani 1 1 d . . .
H11O H -0.231(3) 0.540(3) 0.658(2) 0.038(6) Uiso 1 1 d . . .
C12 C 0.21842(13) 0.48622(12) 0.65270(11) 0.00955(17) Uani 1 1 d . . .
H12 H 0.2366(19) 0.5883(19) 0.6766(18) 0.011(4) Uiso 1 1 d . . .
O12 O 0.05436(10) 0.40561(10) 0.59875(9) 0.01194(15) Uani 1 1 d . . .
H12O H 0.018(2) 0.456(2) 0.611(2) 0.020(5) Uiso 1 1 d . . .
O1W O -0.62393(10) -0.20175(10) -0.50146(10) 0.01279(15) Uani 1 1 d . . .
H1W H -0.575(2) -0.204(2) -0.409(2) 0.025(5) Uiso 1 1 d . . .
H2W H -0.683(3) -0.285(3) -0.541(2) 0.032(6) Uiso 1 1 d . . .
O2W O 0.29602(11) 0.39600(11) 0.17716(10) 0.01379(16) Uani 1 1 d . . .
H3W H 0.305(2) 0.437(2) 0.109(2) 0.025(5) Uiso 1 1 d . . .
H4W H 0.196(3) 0.323(3) 0.130(3) 0.056(8) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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
O2 V1 O2 180.00(6) . 2 ?
O2 V1 O6 89.32(4) . . ?
O2 V1 O6 90.68(4) 2 . ?
O2 V1 O6 90.68(4) . 2 ?
O2 V1 O6 89.32(4) 2 2 ?
O6 V1 O6 180.00(7) . 2 ?
O2 V1 O4 90.00(3) . 2 ?
O2 V1 O4 90.00(3) 2 2 ?
O6 V1 O4 89.50(3) . 2 ?
O6 V1 O4 90.50(3) 2 2 ?
O2 V1 O4 90.00(3) . . ?
O2 V1 O4 90.00(3) 2 . ?
O6 V1 O4 90.50(3) . . ?
O6 V1 O4 89.50(3) 2 . ?
O4 V1 O4 180.00(6) 2 . ?
O1 C1 C2 110.98(9) . . ?
O1 C1 C6 111.17(9) . . ?
C2 C1 C6 110.66(8) . . ?
C1 O1 K1 144.41(8) . . ?
O2 C2 C1 109.80(9) . . ?
O2 C2 C3 110.36(8) . 2 ?
C1 C2 C3 110.21(9) . 2 ?
C2 O2 V1 122.36(7) . . ?
O3 C3 C2 110.57(9) . 2 ?
O3 C3 C4 109.39(9) . . ?
C2 C3 C4 110.96(9) 2 . ?
C3 O3 K1 118.21(6) . 2_556 ?
O4 C4 C5 112.19(9) . 2 ?
O4 C4 C3 109.40(8) . . ?
C5 C4 C3 109.92(9) 2 . ?
C4 O4 V1 120.53(6) . . ?
O5 C5 C6 111.54(9) . . ?
O5 C5 C4 111.82(9) . 2 ?
C6 C5 C4 110.76(9) . 2 ?
O6 C6 C5 110.15(8) . . ?
O6 C6 C1 112.58(9) . . ?
C5 C6 C1 109.12(9) . . ?
C6 O6 V1 120.94(7) . . ?
O1 K1 O9 99.21(3) . . ?
O1 K1 O12 73.32(3) . . ?
O9 K1 O12 155.58(3) . . ?
O1 K1 O10 62.81(3) . . ?
O9 K1 O10 132.48(3) . . ?
O12 K1 O10 65.51(3) . . ?
O1 K1 O8 121.59(3) . . ?
O9 K1 O8 134.13(3) . . ?
O12 K1 O8 65.24(3) . . ?
O10 K1 O8 63.36(3) . . ?
O1 K1 O1W 85.84(3) . 2_455 ?
O9 K1 O1W 71.32(3) . 2_455 ?
O12 K1 O1W 84.81(3) . 2_455 ?
O10 K1 O1W 141.24(3) . 2_455 ?
O8 K1 O1W 127.01(3) . 2_455 ?
O1 K1 O3 126.88(3) . 2_556 ?
O9 K1 O3 110.10(3) . 2_556 ?
O12 K1 O3 61.60(3) . 2_556 ?
O10 K1 O3 115.63(3) . 2_556 ?
O8 K1 O3 62.91(3) . 2_556 ?
O1W K1 O3 64.49(2) 2_455 2_556 ?
O1 K1 O10 138.53(3) . 2_556 ?
O9 K1 O10 59.36(2) . 2_556 ?
O12 K1 O10 140.09(2) . 2_556 ?
O10 K1 O10 103.84(2) . 2_556 ?
O8 K1 O10 75.55(2) . 2_556 ?
O1W K1 O10 114.89(3) 2_455 2_556 ?
O3 K1 O10 94.55(2) 2_556 2_556 ?
O1 K1 O8 82.50(3) . 2_556 ?
O9 K1 O8 58.18(2) . 2_556 ?
O12 K1 O8 140.13(3) . 2_556 ?
O10 K1 O8 75.38(2) . 2_556 ?
O8 K1 O8 104.26(2) . 2_556 ?
O1W K1 O8 125.11(3) 2_455 2_556 ?
O3 K1 O8 150.62(3) 2_556 2_556 ?
O10 K1 O8 56.07(2) 2_556 2_556 ?
O1 K1 K1 106.85(2) . 2_556 ?
O9 K1 K1 94.68(2) . 2_556 ?
O12 K1 K1 109.71(2) . 2_556 ?
O10 K1 K1 55.914(19) . 2_556 ?
O8 K1 K1 56.253(19) . 2_556 ?
O1W K1 K1 162.75(2) 2_455 2_556 ?
O3 K1 K1 113.47(2) 2_556 2_556 ?
O10 K1 K1 47.923(17) 2_556 2_556 ?
O8 K1 K1 48.010(16) 2_556 2_556 ?
O7 C7 C12 110.43(9) . . ?
O7 C7 C8 111.60(9) . . ?
C12 C7 C8 114.34(8) . . ?
O8 C8 C9 112.43(9) . . ?
O8 C8 C7 112.54(9) . . ?
C9 C8 C7 108.22(9) . . ?
C8 O8 K1 132.06(7) . . ?
C8 O8 K1 111.23(6) . 2_556 ?
K1 O8 K1 75.74(2) . 2_556 ?
O9 C9 C8 109.47(9) 2_556 . ?
O9 C9 C10 111.66(8) 2_556 . ?
C8 C9 C10 113.67(9) . . ?
C9 O9 K1 116.31(6) 2_556 . ?
O10 C10 C11 112.70(8) . 2_566 ?
O10 C10 C9 112.69(9) . . ?
C11 C10 C9 107.71(8) 2_566 . ?
C10 O10 K1 132.35(6) . . ?
C10 O10 K1 111.28(6) . 2_556 ?
K1 O10 K1 76.16(2) . 2_556 ?
O11 C11 C12 108.19(8) . 2_566 ?
O11 C11 C10 112.79(8) . 2_566 ?
C12 C11 C10 114.84(9) 2_566 2_566 ?
O12 C12 C11 111.72(8) . 2_566 ?
O12 C12 C7 110.28(9) . . ?
C11 C12 C7 109.64(8) 2_566 . ?
C12 O12 K1 133.30(6) . . ?
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 O2 1.9023(8) . ?
V1 O2 1.9023(8) 2 ?
V1 O6 1.9194(8) . ?
V1 O6 1.9194(8) 2 ?
V1 O4 1.9260(7) 2 ?
V1 O4 1.9260(7) . ?
C1 O1 1.4256(13) . ?
C1 C2 1.5262(17) . ?
C1 C6 1.5296(16) . ?
O1 K1 2.7118(9) . ?
C2 O2 1.4184(13) . ?
C2 C3 1.5305(15) 2 ?
C3 O3 1.4251(15) . ?
C3 C2 1.5305(15) 2 ?
C3 C4 1.5348(15) . ?
O3 K1 3.0050(9) 2_556 ?
C4 O4 1.4177(13) . ?
C4 C5 1.5289(16) 2 ?
C5 O5 1.4264(14) . ?
C5 C6 1.5282(15) . ?
C5 C4 1.5289(16) 2 ?
C6 O6 1.4172(13) . ?
K1 O9 2.7205(9) . ?
K1 O12 2.7587(10) . ?
K1 O10 2.7788(9) . ?
K1 O8 2.7878(8) . ?
K1 O1W 2.8482(9) 2_455 ?
K1 O3 3.0050(9) 2_556 ?
K1 O10 3.1006(9) 2_556 ?
K1 O8 3.1187(9) 2_556 ?
K1 K1 3.6351(5) 2_556 ?
C7 O7 1.4296(14) . ?
C7 C12 1.5366(15) . ?
C7 C8 1.5371(16) . ?
C8 O8 1.4283(14) . ?
C8 C9 1.5284(16) . ?
O8 K1 3.1187(9) 2_556 ?
C9 O9 1.4251(13) 2_556 ?
C9 C10 1.5361(15) . ?
O9 C9 1.4251(13) 2_556 ?
C10 O10 1.4236(13) . ?
C10 C11 1.5310(15) 2_566 ?
O10 K1 3.1006(9) 2_556 ?
C11 O11 1.4317(13) . ?
C11 C12 1.5276(15) 2_566 ?
C11 C10 1.5310(15) 2_566 ?
C12 O12 1.4247(14) . ?
C12 C11 1.5276(15) 2_566 ?
O1W K1 2.8482(9) 2_455 ?
