#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:28:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179921 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/16/7021632.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_7021632
loop_
_publ_author_name
'Drouza, Chryssoula'
'Vlasiou, Manos'
'Keramidas, Anastasios D.'
_publ_section_title
;
 Vanadium(iv/v)-p-dioxolene temperature induced electron transfer
 associated with ligation/deligation of solvent molecules.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11831
_journal_page_last               11840
_journal_paper_doi               10.1039/c3dt50619c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C20 H34 N2 O10 S2 V2'
_chemical_formula_weight         628.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 110.353(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.3994(8)
_cell_length_b                   6.7080(3)
_cell_length_c                   14.5850(8)
_cell_measurement_reflns_used    2339
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      76.9109
_cell_measurement_theta_min      3.2292
_cell_volume                     1229.10(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'WINGX 1.80.05'
_computing_publication_material  'WINGX 1.80.05'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 10.4223
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4865
_diffrn_reflns_theta_full        74.33
_diffrn_reflns_theta_max         76.9109
_diffrn_reflns_theta_min         3.2292
_exptl_absorpt_coefficient_mu    8.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.335
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0379
_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)+(0.0656P)²+0.5371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                2348
_reflns_number_total             2546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50619c.txt
_cod_data_source_block           shelxl
_cod_original_cell_volume        1229.10(11)
_cod_database_code               7021632
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, 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 0.75973(3) 0.14406(6) 0.72085(3) 0.01645(14) Uani 1 1 d .
S1 S 0.83741(4) 0.43591(9) 0.59609(4) 0.02186(16) Uani 1 1 d .
O4 O 0.74471(13) 0.0196(3) 0.62242(12) 0.0250(4) Uani 1 1 d .
O2 O 0.67397(13) 0.0007(3) 0.77212(13) 0.0239(4) Uani 1 1 d .
O5 O 0.86573(13) 0.3550(2) 0.70061(12) 0.0210(4) Uani 1 1 d .
O3 O 0.88613(12) 0.0239(2) 0.80260(11) 0.0192(3) Uani 1 1 d .
N1 N 0.77426(15) 0.3411(3) 0.85565(14) 0.0170(4) Uani 1 1 d .
O1 O 0.65715(13) 0.3369(2) 0.66777(12) 0.0212(4) Uani 1 1 d .
C5 C 0.88511(18) 0.3670(3) 0.92355(16) 0.0171(4) Uani 1 1 d .
H00A H 0.8846 0.4499 0.9779 0.021 Uiso 1 1 calc R
H00B H 0.9255 0.4366 0.8897 0.021 Uiso 1 1 calc R
C1 C 0.73159(18) 0.5374(3) 0.81373(17) 0.0203(5) Uani 1 1 d .
H01A H 0.7874 0.6152 0.8026 0.024 Uiso 1 1 calc R
H01B H 0.7068 0.6099 0.8593 0.024 Uiso 1 1 calc R
C4 C 0.6259(2) 0.1078(4) 0.82923(19) 0.0262(5) Uani 1 1 d .
H01C H 0.5956 0.0151 0.8634 0.031 Uiso 1 1 calc R
H01D H 0.5687 0.1897 0.7869 0.031 Uiso 1 1 calc R
C3 C 0.70684(17) 0.2390(4) 0.90268(16) 0.0204(4) Uani 1 1 d .
H01E H 0.6704 0.3372 0.9285 0.024 Uiso 1 1 calc R
H01F H 0.7511 0.1584 0.9567 0.024 Uiso 1 1 calc R
C6 C 0.94054(17) 0.1736(3) 0.96325(16) 0.0162(4) Uani 1 1 d .
C7 C 0.94015(17) 0.0172(3) 0.89900(16) 0.0159(4) Uani 1 1 d .
C2 C 0.63954(19) 0.5076(4) 0.71716(18) 0.0227(5) Uani 1 1 d .
H01G H 0.5736 0.4920 0.7299 0.027 Uiso 1 1 calc R
H01H H 0.6329 0.6242 0.6761 0.027 Uiso 1 1 calc R
C8 C 1.00111(17) -0.1532(3) 0.93737(17) 0.0172(4) Uani 1 1 d .
H1 H 1.0026 -0.2559 0.8951 0.021 Uiso 1 1 calc R
C9 C 0.9150(2) 0.6575(4) 0.6134(2) 0.0309(6) Uani 1 1 d .
H5A H 0.8842 0.7585 0.6420 0.046 Uiso 1 1 calc R
H5B H 0.9162 0.7032 0.5515 0.046 Uiso 1 1 calc R
H5C H 0.9863 0.6302 0.6562 0.046 Uiso 1 1 calc R
C10 C 0.9115(2) 0.2805(4) 0.54339(18) 0.0281(5) Uani 1 1 d .
H7A H 0.8786 0.1515 0.5295 0.042 Uiso 1 1 calc R
H7B H 0.9830 0.2667 0.5885 0.042 Uiso 1 1 calc R
H7C H 0.9126 0.3398 0.4839 0.042 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'
N N 0.0311 0.0180 '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'
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
O4 V1 O2 100.87(9) .
O4 V1 O1 98.35(8) .
O2 V1 O1 93.28(8) .
O4 V1 O3 98.55(8) .
O2 V1 O3 94.03(8) .
O1 V1 O3 159.96(8) .
O4 V1 O5 96.03(8) .
O2 V1 O5 163.09(7) .
O1 V1 O5 84.85(7) .
O3 V1 O5 82.74(7) .
O4 V1 N1 175.95(8) .
O2 V1 N1 80.45(7) .
O1 V1 N1 77.72(7) .
O3 V1 N1 85.14(7) .
O5 V1 N1 82.73(7) .
O5 S1 C9 102.90(12) .
O5 S1 C10 103.79(11) .
C9 S1 C10 99.45(13) .
C4 O2 V1 116.71(15) .
S1 O5 V1 115.62(9) .
C7 O3 V1 135.95(14) .
C3 N1 C1 113.15(18) .
C3 N1 C5 112.11(17) .
C1 N1 C5 109.00(17) .
C3 N1 V1 104.14(13) .
C1 N1 V1 104.49(13) .
C5 N1 V1 113.72(13) .
C2 O1 V1 125.72(14) .
N1 C5 C6 113.70(18) .
N1 C5 H00A 108.8 .
C6 C5 H00A 108.8 .
N1 C5 H00B 108.8 .
C6 C5 H00B 108.8 .
H00A C5 H00B 107.7 .
N1 C1 C2 109.64(19) .
N1 C1 H01A 109.7 .
C2 C1 H01A 109.7 .
N1 C1 H01B 109.7 .
C2 C1 H01B 109.7 .
H01A C1 H01B 108.2 .
O2 C4 C3 110.6(2) .
O2 C4 H01C 109.5 .
C3 C4 H01C 109.5 .
O2 C4 H01D 109.5 .
C3 C4 H01D 109.5 .
H01C C4 H01D 108.1 .
N1 C3 C4 110.13(18) .
N1 C3 H01E 109.6 .
C4 C3 H01E 109.6 .
N1 C3 H01F 109.6 .
C4 C3 H01F 109.6 .
H01E C3 H01F 108.1 .
C8 C6 C7 119.4(2) 3_757
C8 C6 C5 120.5(2) 3_757
C7 C6 C5 120.0(2) .
O3 C7 C8 118.3(2) .
O3 C7 C6 123.3(2) .
C8 C7 C6 118.4(2) .
O1 C2 C1 110.54(18) .
O1 C2 H01G 109.5 .
C1 C2 H01G 109.5 .
O1 C2 H01H 109.5 .
C1 C2 H01H 109.5 .
H01G C2 H01H 108.1 .
C6 C8 C7 122.2(2) 3_757
C6 C8 H1 118.9 3_757
C7 C8 H1 118.9 .
S1 C9 H5A 109.5 .
S1 C9 H5B 109.5 .
H5A C9 H5B 109.5 .
S1 C9 H5C 109.5 .
H5A C9 H5C 109.5 .
H5B C9 H5C 109.5 .
S1 C10 H7A 109.5 .
S1 C10 H7B 109.5 .
H7A C10 H7B 109.5 .
S1 C10 H7C 109.5 .
H7A C10 H7C 109.5 .
H7B C10 H7C 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 1.6117(17) .
V1 O2 1.8446(17) .
V1 O1 1.8498(17) .
V1 O3 1.8801(16) .
V1 O5 2.0974(17) .
V1 N1 2.3206(19) .
S1 O5 1.5361(17) .
S1 C9 1.781(3) .
S1 C10 1.787(3) .
O2 C4 1.414(3) .
O3 C7 1.340(3) .
N1 C3 1.479(3) .
N1 C1 1.480(3) .
N1 C5 1.481(3) .
O1 C2 1.416(3) .
C5 C6 1.507(3) .
C5 H00A 0.9700 .
C5 H00B 0.9700 .
C1 C2 1.529(3) .
C1 H01A 0.9700 .
C1 H01B 0.9700 .
C4 C3 1.513(3) .
C4 H01C 0.9700 .
C4 H01D 0.9700 .
C3 H01E 0.9700 .
C3 H01F 0.9700 .
C6 C8 1.394(3) 3_757
C6 C7 1.406(3) .
C7 C8 1.403(3) .
C2 H01G 0.9700 .
C2 H01H 0.9700 .
C8 C6 1.394(3) 3_757
C8 H1 0.9300 .
C9 H5A 0.9600 .
C9 H5B 0.9600 .
C9 H5C 0.9600 .
C10 H7A 0.9600 .
C10 H7B 0.9600 .
C10 H7C 0.9600 .
