#------------------------------------------------------------------------------
#$Date: 2019-06-20 14:20:56 +0300 (Thu, 20 Jun 2019) $
#$Revision: 216234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/16/1551623.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_1551623
loop_
_publ_author_name
'MIKURIYA, Masahiro'
'FUKUTANI, Masami'
'YOSHIOKA, Daisuke'
_publ_section_title
;
 Synthesis and Crystal Structures of Dinuclear Dioxidovanadium(V) and
 Tetranuclear Oxidovanadium(IV) Complexes with
 2,6-Bis(hydroxymethyl)-4-methylphenol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              33
_journal_paper_doi               10.2116/xraystruct.31.33
_journal_volume                  31
_journal_year                    2015
_chemical_formula_sum            'C32 H58 N2 O20 S2 V4'
_chemical_formula_weight         1058.68
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                104.28(3)
_cell_angle_beta                 112.76(2)
_cell_angle_gamma                108.23(2)
_cell_formula_units_Z            1
_cell_length_a                   10.731(14)
_cell_length_b                   11.373(15)
_cell_length_c                   11.558(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1121(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.868
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6826
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  0.7922
_exptl_absorpt_correction_T_min  0.6408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      1.554
_exptl_crystal_density_method    floatation
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0514
_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)+(0.1004P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                3606
_reflns_number_total             4912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            31_33_2.txt
_cod_data_source_block           vmf2991
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/andrius/struct/COD-crude-data/automatic-downloads/current/J-STAGE/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 6524 2018-11-02 12:15:13Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1551623
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
V1 V 0.52764(5) 0.06079(5) 0.37302(5) 0.03003(16) Uani 1 1 d .
V2 V 0.25582(5) 0.04880(5) 0.41238(5) 0.02970(16) Uani 1 1 d .
S1 S 0.10405(8) -0.21390(8) 0.46733(8) 0.03165(19) Uani 1 1 d .
N1 N 0.1491(3) 0.7734(3) 0.8160(3) 0.0467(7) Uani 1 1 d .
H1A H 0.1232 0.7700 0.7315 0.056 Uiso 1 1 d R
O1 O 0.5971(2) -0.0792(2) 0.3759(2) 0.0313(5) Uani 1 1 d .
O2 O 0.3502(2) -0.0689(2) 0.3686(2) 0.0315(5) Uani 1 1 d .
O3 O 0.2106(2) 0.1891(2) 0.5202(2) 0.0374(5) Uani 1 1 d .
H3B H 0.1288 0.1819 0.4807 0.045 Uiso 1 1 d R
O4 O 0.4676(3) 0.0433(3) 0.2179(2) 0.0441(6) Uani 1 1 d .
O5 O 0.1456(3) 0.0360(3) 0.2653(2) 0.0459(6) Uani 1 1 d .
O6 O 0.7409(2) 0.2059(2) 0.4718(2) 0.0375(5) Uani 1 1 d .
O7 O 0.1063(2) -0.1036(2) 0.4213(3) 0.0409(6) Uani 1 1 d .
O8 O 0.0003(3) -0.3434(3) 0.3521(3) 0.0574(7) Uani 1 1 d .
O9 O 0.0620(3) -0.1932(3) 0.5739(3) 0.0549(7) Uani 1 1 d .
O10 O 0.4534(2) 0.1823(2) 0.4472(2) 0.0338(5) Uani 1 1 d .
C1 C 0.5026(3) -0.2112(3) 0.2830(3) 0.0310(6) Uani 1 1 d .
C2 C 0.3451(3) -0.2695(3) 0.2208(3) 0.0310(6) Uani 1 1 d .
C3 C 0.2603(4) -0.4058(3) 0.1253(3) 0.0390(7) Uani 1 1 d .
H3A H 0.1549 -0.4447 0.0822 0.047 Uiso 1 1 calc R
C4 C 0.3264(4) -0.4856(4) 0.0923(4) 0.0459(8) Uani 1 1 d .
C5 C 0.4829(4) -0.4262(4) 0.1596(4) 0.0454(8) Uani 1 1 d .
H5B H 0.5299 -0.4783 0.1404 0.054 Uiso 1 1 calc R
C6 C 0.5717(4) -0.2919(3) 0.2543(3) 0.0382(7) Uani 1 1 d .
C7 C 0.2301(5) -0.6337(4) -0.0113(5) 0.0667(12) Uani 1 1 d .
H7A H 0.2878 -0.6630 -0.0467 0.100 Uiso 1 1 calc R
H7B H 0.1412 -0.6430 -0.0861 0.100 Uiso 1 1 calc R
H7C H 0.2001 -0.6888 0.0332 0.100 Uiso 1 1 calc R
C8 C 0.2580(3) -0.1959(3) 0.2495(3) 0.0347(7) Uani 1 1 d .
H8B H 0.2067 -0.1797 0.1698 0.042 Uiso 1 1 calc R
H8C H 0.1806 -0.2544 0.2616 0.042 Uiso 1 1 calc R
C9 C 0.2591(4) 0.2292(4) 0.6665(3) 0.0400(8) Uani 1 1 d .
H9B H 0.2157 0.1500 0.6819 0.048 Uiso 1 1 calc R
H9C H 0.2252 0.2943 0.6965 0.048 Uiso 1 1 calc R
C10 C 0.4875(5) 0.3138(4) 0.4526(5) 0.0596(11) Uani 1 1 d .
H10A H 0.5896 0.3576 0.4707 0.089 Uiso 1 1 calc R
H10B H 0.4781 0.3660 0.5250 0.089 Uiso 1 1 calc R
H10C H 0.4182 0.3077 0.3657 0.089 Uiso 1 1 calc R
C21 C 0.3003(6) 0.7781(6) 0.8817(6) 0.0844(16) Uani 1 1 d .
H21A H 0.3204 0.7680 0.9671 0.101 Uiso 1 1 calc R
H21B H 0.3774 0.8661 0.9043 0.101 Uiso 1 1 calc R
C22 C 0.3102(7) 0.6659(6) 0.7875(7) 0.0944(19) Uani 1 1 d .
H22A H 0.4094 0.6716 0.8333 0.142 Uiso 1 1 calc R
H22B H 0.2927 0.6769 0.7037 0.142 Uiso 1 1 calc R
H22C H 0.2349 0.5786 0.7659 0.142 Uiso 1 1 calc R
C23 C 0.0284(5) 0.6507(5) 0.8001(5) 0.0763(14) Uani 1 1 d .
H23A H 0.0459 0.5728 0.7707 0.092 Uiso 1 1 calc R
H23B H 0.0366 0.6647 0.8896 0.092 Uiso 1 1 calc R
C24 C -0.1271(5) 0.6189(7) 0.7003(7) 0.101(2) Uani 1 1 d .
H24A H -0.1987 0.5393 0.6957 0.152 Uiso 1 1 calc R
H24B H -0.1375 0.6019 0.6107 0.152 Uiso 1 1 calc R
H24C H -0.1464 0.6946 0.7295 0.152 Uiso 1 1 calc R
C25 C 0.1535(7) 0.9020(5) 0.9027(6) 0.0863(16) Uani 1 1 d .
H25A H 0.0507 0.8912 0.8679 0.104 Uiso 1 1 calc R
H25B H 0.1928 0.9120 0.9974 0.104 Uiso 1 1 calc R
C26 C 0.2476(7) 1.0269(5) 0.9012(6) 0.102(2) Uani 1 1 d .
H26A H 0.2463 1.1039 0.9573 0.152 Uiso 1 1 calc R
H26B H 0.2079 1.0189 0.8080 0.152 Uiso 1 1 calc R
H26C H 0.3501 1.0395 0.9374 0.152 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'
S S 0.1246 0.1234 '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
O4 V1 O1 102.52(12) . .
O4 V1 O10 103.94(13) . .
O1 V1 O10 151.16(10) . .
O4 V1 O2 104.56(12) . .
O1 V1 O2 84.77(14) . .
O10 V1 O2 77.70(14) . .
O4 V1 O6 103.16(12) . .
O1 V1 O6 90.77(14) . .
O10 V1 O6 94.18(14) . .
O2 V1 O6 152.24(11) . .
O5 V2 O10 99.55(14) . .
O5 V2 O2 103.45(13) . .
O10 V2 O2 76.97(14) . .
O5 V2 O7 98.44(14) . .
O10 V2 O7 159.92(9) . .
O2 V2 O7 90.24(14) . .
O5 V2 O3 94.21(14) . .
O10 V2 O3 97.00(13) . .
O2 V2 O3 162.02(9) . .
O7 V2 O3 90.48(14) . .
O5 V2 O1 175.05(11) . 2_656
O10 V2 O1 81.18(11) . 2_656
O2 V2 O1 81.49(11) . 2_656
O7 V2 O1 81.66(12) . 2_656
O3 V2 O1 80.84(12) . 2_656
O8 S1 O9 112.2(2) . .
O8 S1 O7 109.83(19) . .
O9 S1 O7 107.58(16) . .
O8 S1 O6 108.52(16) . 2_656
O9 S1 O6 109.01(16) . 2_656
O7 S1 O6 109.68(13) . 2_656
C21 N1 C23 112.0(4) . .
C21 N1 C25 109.6(4) . .
C23 N1 C25 109.3(4) . .
C21 N1 H1A 110.3 . .
C23 N1 H1A 107.1 . .
C25 N1 H1A 108.5 . .
C1 O1 V1 120.6(2) . .
C1 O1 V2 115.37(19) . 2_656
V1 O1 V2 112.40(11) . 2_656
C8 O2 V1 115.49(19) . .
C8 O2 V2 119.03(19) . .
V1 O2 V2 101.82(15) . .
C9 O3 V2 123.04(19) . .
C9 O3 H3B 109.3 . .
V2 O3 H3B 115.3 . .
S1 O6 V1 136.75(16) 2_656 .
S1 O7 V2 138.12(15) . .
C10 O10 V1 125.3(2) . .
C10 O10 V2 125.5(2) . .
V1 O10 V2 102.03(14) . .
O1 C1 C2 123.8(3) . .
O1 C1 C6 116.5(3) . .
C2 C1 C6 119.6(3) . .
C1 C2 C3 118.3(3) . .
C1 C2 C8 124.7(3) . .
C3 C2 C8 117.0(3) . .
C4 C3 C2 122.7(3) . .
C4 C3 H3A 118.6 . .
C2 C3 H3A 118.6 . .
C5 C4 C3 117.4(3) . .
C5 C4 C7 121.5(3) . .
C3 C4 C7 121.0(4) . .
C6 C5 C4 122.0(3) . .
C6 C5 H5B 119.0 . .
C4 C5 H5B 119.0 . .
C5 C6 C1 119.7(3) . .
C5 C6 C9 122.3(3) . 2_656
C1 C6 C9 117.9(3) . 2_656
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O2 C8 C2 113.9(3) . .
O2 C8 H8B 108.8 . .
C2 C8 H8B 108.8 . .
O2 C8 H8C 108.8 . .
C2 C8 H8C 108.8 . .
H8B C8 H8C 107.7 . .
O3 C9 C6 108.0(3) . 2_656
O3 C9 H9B 110.1 . .
C6 C9 H9B 110.1 2_656 .
O3 C9 H9C 110.1 . .
C6 C9 H9C 110.1 2_656 .
H9B C9 H9C 108.4 . .
O10 C10 H10A 109.5 . .
O10 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
O10 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N1 C21 C22 111.6(5) . .
N1 C21 H21A 109.3 . .
C22 C21 H21A 109.3 . .
N1 C21 H21B 109.3 . .
C22 C21 H21B 109.3 . .
H21A C21 H21B 108.0 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C24 C23 N1 114.0(4) . .
C24 C23 H23A 108.8 . .
N1 C23 H23A 108.8 . .
C24 C23 H23B 108.8 . .
N1 C23 H23B 108.8 . .
H23A C23 H23B 107.6 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 N1 113.2(5) . .
C26 C25 H25A 108.9 . .
N1 C25 H25A 108.9 . .
C26 C25 H25B 108.9 . .
N1 C25 H25B 108.9 . .
H25A C25 H25B 107.7 . .
C25 C26 H26A 109.5 . .
C25 C26 H26B 109.5 . .
H26A C26 H26B 109.5 . .
C25 C26 H26C 109.5 . .
H26A C26 H26C 109.5 . .
H26B C26 H26C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O4 1.588(3) .
V1 O1 1.960(3) .
V1 O10 1.978(3) .
V1 O2 1.983(3) .
V1 O6 1.988(3) .
V2 O5 1.589(3) .
V2 O10 1.996(3) .
V2 O2 1.997(3) .
V2 O7 2.016(3) .
V2 O3 2.075(3) .
V2 O1 2.203(3) 2_656
S1 O8 1.429(3) .
S1 O9 1.459(3) .
S1 O7 1.476(3) .
S1 O6 1.497(3) 2_656
N1 C21 1.478(6) .
N1 C23 1.489(5) .
N1 C25 1.531(6) .
N1 H1A 0.8922 .
O1 C1 1.359(4) .
O1 V2 2.203(3) 2_656
O2 C8 1.425(4) .
O3 C9 1.459(4) .
O3 H3B 0.7821 .
O6 S1 1.497(3) 2_656
O10 C10 1.403(5) .
C1 C2 1.391(5) .
C1 C6 1.402(4) .
C2 C3 1.395(5) .
C2 C8 1.510(4) .
C3 C4 1.384(5) .
C3 H3A 0.9300 .
C4 C5 1.379(5) .
C4 C7 1.515(5) .
C5 C6 1.377(5) .
C5 H5B 0.9300 .
C6 C9 1.492(5) 2_656
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 C6 1.492(5) 2_656
C9 H9B 0.9700 .
C9 H9C 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C21 C22 1.521(8) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
C23 C24 1.474(7) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 C26 1.472(8) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
