#------------------------------------------------------------------------------
#$Date: 2019-11-25 13:59:59 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/06/4130644.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_4130644
loop_
_publ_author_name
'Atzori, Matteo'
'Morra, Elena'
'Tesi, Lorenzo'
'Albino, Andrea'
'Chiesa, Mario'
'Sorace, Lorenzo'
'Sessoli, Roberta'
_publ_section_title
;
 Quantum Coherence Times Enhancement in Vanadium(IV)-based Potential
 Molecular Qubits: the Key Role of the Vanadyl Moiety.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11234
_journal_page_last               11244
_journal_paper_doi               10.1021/jacs.6b05574
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C54 H40 O P2 S10 V'
_chemical_formula_sum            'C54 H40 O P2 S10 V'
_chemical_formula_weight         1138.34
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.297(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.4747(5)
_cell_length_b                   12.7283(4)
_cell_length_c                   20.6032(5)
_cell_measurement_reflns_used    2105
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.0040
_cell_measurement_theta_min      4.3060
_cell_volume                     5346.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8942
_diffrn_reflns_theta_full        61.86
_diffrn_reflns_theta_max         61.86
_diffrn_reflns_theta_min         4.31
_diffrn_standards_number         9029
_exptl_absorpt_coefficient_mu    6.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0587
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                2169
_reflns_number_total             4061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b05574_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130644
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'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
V1 V 0.0000 0.07887(11) 0.2500 0.0550(4) Uani 1 2 d S
S1 S -0.01569(6) 0.01922(13) 0.35728(7) 0.0642(4) Uani 1 1 d .
S2 S 0.11259(6) 0.03168(14) 0.27270(7) 0.0735(5) Uani 1 1 d .
S3 S 0.08247(6) -0.01961(13) 0.47395(7) 0.0710(5) Uani 1 1 d .
S4 S 0.19348(6) -0.00914(13) 0.39940(7) 0.0708(5) Uani 1 1 d .
S5 S 0.21649(7) -0.05252(15) 0.54157(8) 0.0891(6) Uani 1 1 d .
O1 O 0.0000 0.2041(4) 0.2500 0.0773(16) Uani 1 2 d S
C1 C 0.0647(2) 0.0062(4) 0.3913(2) 0.0547(15) Uani 1 1 d .
C3 C 0.1670(2) -0.0294(4) 0.4753(3) 0.0645(16) Uani 1 1 d .
C2 C 0.1173(2) 0.0120(4) 0.3563(2) 0.0559(15) Uani 1 1 d .
P1 P 0.09283(7) 0.62497(12) 0.10129(7) 0.0568(4) Uani 1 1 d .
C2D C 0.0466(3) 0.6968(4) -0.0221(3) 0.0669(17) Uani 1 1 d .
H2D H 0.0048 0.6966 -0.0079 0.080 Uiso 1 1 calc R
C1C C 0.1082(2) 0.4879(4) 0.1107(3) 0.0554(15) Uani 1 1 d .
C1B C 0.1516(2) 0.6990(5) 0.1513(3) 0.0555(15) Uani 1 1 d .
C3C C 0.1025(3) 0.3301(7) 0.1744(4) 0.087(2) Uani 1 1 d .
H3C H 0.0913 0.2960 0.2117 0.105 Uiso 1 1 calc R
C1D C 0.1003(3) 0.6655(4) 0.0198(3) 0.0537(14) Uani 1 1 d .
C2B C 0.1962(3) 0.6509(5) 0.1976(3) 0.0694(17) Uani 1 1 d .
H2B H 0.1955 0.5785 0.2035 0.083 Uiso 1 1 calc R
C1A C 0.0116(3) 0.6474(5) 0.1222(3) 0.0578(16) Uani 1 1 d .
C2C C 0.0919(3) 0.4374(6) 0.1673(3) 0.0760(18) Uani 1 1 d .
H2C H 0.0742 0.4755 0.2000 0.091 Uiso 1 1 calc R
C5B C 0.1998(3) 0.8657(6) 0.1801(4) 0.085(2) Uani 1 1 d .
H5B H 0.2017 0.9381 0.1742 0.102 Uiso 1 1 calc R
C4B C 0.2424(4) 0.8186(7) 0.2261(4) 0.090(2) Uani 1 1 d .
H4B H 0.2722 0.8594 0.2518 0.108 Uiso 1 1 calc R
C6C C 0.1359(3) 0.4309(5) 0.0632(3) 0.0657(16) Uani 1 1 d .
H6C H 0.1478 0.4640 0.0258 0.079 Uiso 1 1 calc R
C3A C -0.1015(3) 0.5936(7) 0.1144(3) 0.099(2) Uani 1 1 d .
H3A H -0.1338 0.5453 0.1005 0.119 Uiso 1 1 calc R
C3D C 0.0556(3) 0.7282(5) -0.0852(3) 0.0778(19) Uani 1 1 d .
H3D H 0.0197 0.7494 -0.1131 0.093 Uiso 1 1 calc R
C5C C 0.1457(3) 0.3223(6) 0.0717(4) 0.0791(19) Uani 1 1 d .
H5C H 0.1636 0.2832 0.0396 0.095 Uiso 1 1 calc R
C5D C 0.1702(3) 0.6984(5) -0.0654(3) 0.0730(18) Uani 1 1 d .
H5D H 0.2118 0.6991 -0.0801 0.088 Uiso 1 1 calc R
C6D C 0.1627(3) 0.6678(4) -0.0031(3) 0.0656(17) Uani 1 1 d .
H6D H 0.1992 0.6483 0.0244 0.079 Uiso 1 1 calc R
C4C C 0.1291(3) 0.2744(6) 0.1266(5) 0.090(2) Uani 1 1 d .
H4C H 0.1359 0.2026 0.1318 0.108 Uiso 1 1 calc R
C4A C -0.1171(3) 0.6808(8) 0.1477(4) 0.097(2) Uani 1 1 d .
H4A H -0.1605 0.6928 0.1555 0.117 Uiso 1 1 calc R
C2A C -0.0369(3) 0.5771(6) 0.1014(3) 0.087(2) Uani 1 1 d .
H2A H -0.0263 0.5176 0.0783 0.105 Uiso 1 1 calc R
C3B C 0.2415(3) 0.7125(7) 0.2348(3) 0.088(2) Uani 1 1 d .
H3B H 0.2714 0.6813 0.2657 0.105 Uiso 1 1 calc R
C6B C 0.1544(3) 0.8081(6) 0.1425(3) 0.0732(18) Uani 1 1 d .
H6B H 0.1256 0.8409 0.1114 0.088 Uiso 1 1 calc R
C5A C -0.0700(4) 0.7509(6) 0.1697(3) 0.087(2) Uani 1 1 d .
H5A H -0.0810 0.8096 0.1932 0.104 Uiso 1 1 calc R
C4D C 0.1169(4) 0.7282(5) -0.1064(3) 0.0772(19) Uani 1 1 d .
H4D H 0.1225 0.7485 -0.1489 0.093 Uiso 1 1 calc R
C6A C -0.0052(3) 0.7342(5) 0.1568(3) 0.0754(18) Uani 1 1 d .
H6A H 0.0270 0.7822 0.1717 0.091 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O1 V1 S2 104.58(5) . .
O1 V1 S2 104.58(5) . 2
S2 V1 S2 150.84(11) . 2
O1 V1 S1 108.55(5) . 2
S2 V1 S1 83.76(5) . 2
S2 V1 S1 87.05(5) 2 2
O1 V1 S1 108.55(5) . .
S2 V1 S1 87.05(5) . .
S2 V1 S1 83.76(5) 2 .
S1 V1 S1 142.90(10) 2 .
C1 S1 V1 101.54(17) . .
C2 S2 V1 101.24(16) . .
C3 S3 C1 98.5(2) . .
C3 S4 C2 98.2(2) . .
C2 C1 S1 123.6(4) . .
C2 C1 S3 115.2(4) . .
S1 C1 S3 121.2(3) . .
S5 C3 S4 123.9(3) . .
S5 C3 S3 124.2(3) . .
S4 C3 S3 111.9(3) . .
C1 C2 S2 124.3(4) . .
C1 C2 S4 116.1(4) . .
S2 C2 S4 119.5(3) . .
C1D P1 C1A 110.3(3) . .
C1D P1 C1C 111.0(3) . .
C1A P1 C1C 106.9(3) . .
C1D P1 C1B 106.3(3) . .
C1A P1 C1B 111.9(3) . .
C1C P1 C1B 110.6(3) . .
C3D C2D C1D 120.0(5) . .
C3D C2D H2D 120.0 . .
C1D C2D H2D 120.0 . .
C6C C1C C2C 119.6(6) . .
C6C C1C P1 121.2(5) . .
C2C C1C P1 119.2(5) . .
C2B C1B C6B 119.3(5) . .
C2B C1B P1 121.8(5) . .
C6B C1B P1 118.9(5) . .
C4C C3C C2C 120.2(7) . .
C4C C3C H3C 119.9 . .
C2C C3C H3C 119.9 . .
C2D C1D C6D 118.4(5) . .
C2D C1D P1 122.5(4) . .
C6D C1D P1 119.1(4) . .
C3B C2B C1B 119.3(6) . .
C3B C2B H2B 120.3 . .
C1B C2B H2B 120.3 . .
C6A C1A C2A 118.5(5) . .
C6A C1A P1 122.6(5) . .
C2A C1A P1 118.9(5) . .
C3C C2C C1C 119.5(6) . .
C3C C2C H2C 120.2 . .
C1C C2C H2C 120.2 . .
C4B C5B C6B 120.9(7) . .
C4B C5B H5B 119.5 . .
C6B C5B H5B 119.5 . .
C3B C4B C5B 120.8(7) . .
C3B C4B H4B 119.6 . .
C5B C4B H4B 119.6 . .
C1C C6C C5C 119.4(6) . .
C1C C6C H6C 120.3 . .
C5C C6C H6C 120.3 . .
C4A C3A C2A 119.6(7) . .
C4A C3A H3A 120.2 . .
C2A C3A H3A 120.2 . .
C4D C3D C2D 120.3(6) . .
C4D C3D H3D 119.9 . .
C2D C3D H3D 119.9 . .
C4C C5C C6C 120.2(7) . .
C4C C5C H5C 119.9 . .
C6C C5C H5C 119.9 . .
C6D C5D C4D 120.4(6) . .
C6D C5D H5D 119.8 . .
C4D C5D H5D 119.8 . .
C5D C6D C1D 120.7(5) . .
C5D C6D H6D 119.7 . .
C1D C6D H6D 119.7 . .
C5C C4C C3C 121.0(7) . .
C5C C4C H4C 119.5 . .
C3C C4C H4C 119.5 . .
C3A C4A C5A 120.8(7) . .
C3A C4A H4A 119.6 . .
C5A C4A H4A 119.6 . .
C1A C2A C3A 120.9(6) . .
C1A C2A H2A 119.6 . .
C3A C2A H2A 119.6 . .
C4B C3B C2B 120.1(7) . .
C4B C3B H3B 119.9 . .
C2B C3B H3B 119.9 . .
C5B C6B C1B 119.5(6) . .
C5B C6B H6B 120.3 . .
C1B C6B H6B 120.3 . .
C4A C5A C6A 119.7(7) . .
C4A C5A H5A 120.2 . .
C6A C5A H5A 120.2 . .
C3D C4D C5D 120.3(6) . .
C3D C4D H4D 119.8 . .
C5D C4D H4D 119.8 . .
C1A C6A C5A 120.6(6) . .
C1A C6A H6A 119.7 . .
C5A C6A H6A 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.594(5) .
V1 S2 2.3864(14) .
V1 S2 2.3864(14) 2
V1 S1 2.3867(14) 2
V1 S1 2.3867(14) .
S1 C1 1.736(5) .
S2 C2 1.735(5) .
S3 C3 1.733(5) .
S3 C1 1.740(5) .
S4 C3 1.721(5) .
S4 C2 1.743(5) .
S5 C3 1.650(5) .
C1 C2 1.351(5) .
P1 C1D 1.776(5) .
P1 C1A 1.779(5) .
P1 C1C 1.780(6) .
P1 C1B 1.780(6) .
C2D C3D 1.387(7) .
C2D C1D 1.392(7) .
C2D H2D 0.9300 .
C1C C6C 1.382(7) .
C1C C2C 1.399(7) .
C1B C2B 1.399(7) .
C1B C6B 1.402(7) .
C3C C4C 1.366(9) .
C3C C2C 1.389(8) .
C3C H3C 0.9300 .
C1D C6D 1.402(6) .
C2B C3B 1.391(7) .
C2B H2B 0.9300 .
C1A C6A 1.375(7) .
C1A C2A 1.375(7) .
C2C H2C 0.9300 .
C5B C4B 1.366(8) .
C5B C6B 1.367(7) .
C5B H5B 0.9300 .
C4B C3B 1.363(8) .
C4B H4B 0.9300 .
C6C C5C 1.405(8) .
C6C H6C 0.9300 .
C3A C4A 1.357(9) .
C3A C2A 1.391(8) .
C3A H3A 0.9300 .
C3D C4D 1.369(7) .
C3D H3D 0.9300 .
C5C C4C 1.355(8) .
C5C H5C 0.9300 .
C5D C6D 1.363(7) .
C5D C4D 1.371(7) .
C5D H5D 0.9300 .
C6D H6D 0.9300 .
C4C H4C 0.9300 .
C4A C5A 1.360(9) .
C4A H4A 0.9300 .
C2A H2A 0.9300 .
C3B H3B 0.9300 .
C6B H6B 0.9300 .
C5A C6A 1.393(7) .
C5A H5A 0.9300 .
C4D H4D 0.9300 .
C6A H6A 0.9300 .
