#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:13:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179236 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/56/4315649.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_4315649
loop_
_publ_author_name
'Stephen Sproules'
'Thomas Weyhermüller'
'Serena DeBeer'
'Karl Wieghardt'
_publ_section_title
;
 Six-Membered Electron Transfer Series [V(dithiolene)3]z (z= 1+, 0, 1-,
 2-, 3-, 4-). An X-ray Absorption Spectroscopic and Density Functional
 Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5241
_journal_page_last               5261
_journal_paper_doi               10.1021/ic100344f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C42 H30 S6 V'
_chemical_formula_weight         777.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_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                 107.282(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1064(6)
_cell_length_b                   11.2530(4)
_cell_length_c                   17.9293(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3680.8(2)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'2488 images at 0.5 deg. stepwise rotation in omega and phi, 15 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67120
_diffrn_reflns_theta_full        37.50
_diffrn_reflns_theta_max         37.50
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.8194
_exptl_absorpt_correction_T_min  0.5218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         9662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0423
_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)+(0.0442P)²+3.6628P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                7362
_reflns_number_total             9662
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100344f_si_002_1.cif
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315649
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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.0000 0.78316(2) 0.2500 0.01181(5) Uani 1 2 d S . .
S1 S 0.031631(14) 0.86913(3) 0.145193(16) 0.01453(5) Uani 1 1 d . . .
C2 C 0.11954(6) 0.92052(10) 0.17801(6) 0.01414(17) Uani 1 1 d . . .
C3 C 0.15853(6) 0.91008(10) 0.25688(6) 0.01373(17) Uani 1 1 d . . .
S4 S 0.117066(15) 0.84916(3) 0.319592(16) 0.01473(5) Uani 1 1 d . . .
C11 C 0.15200(6) 0.97451(11) 0.12032(6) 0.01582(18) Uani 1 1 d . . .
C12 C 0.21911(7) 0.93291(13) 0.11402(8) 0.0223(2) Uani 1 1 d . . .
H12 H 0.2423 0.8666 0.1441 0.027 Uiso 1 1 calc R . .
C13 C 0.25193(7) 0.98871(15) 0.06368(8) 0.0267(3) Uani 1 1 d . . .
H13 H 0.2975 0.9605 0.0595 0.032 Uiso 1 1 calc R . .
C14 C 0.21817(7) 1.08549(14) 0.01958(8) 0.0249(3) Uani 1 1 d . . .
H14 H 0.2413 1.1249 -0.0136 0.030 Uiso 1 1 calc R . .
C15 C 0.15061(8) 1.12491(12) 0.02396(7) 0.0217(2) Uani 1 1 d . . .
H15 H 0.1270 1.1899 -0.0073 0.026 Uiso 1 1 calc R . .
C16 C 0.11733(7) 1.06954(11) 0.07394(7) 0.01779(19) Uani 1 1 d . . .
H16 H 0.0710 1.0964 0.0765 0.021 Uiso 1 1 calc R . .
C21 C 0.23489(6) 0.95179(10) 0.29302(6) 0.01473(17) Uani 1 1 d . . .
C22 C 0.25693(7) 1.06555(11) 0.27861(8) 0.0201(2) Uani 1 1 d . . .
H22 H 0.2237 1.1159 0.2423 0.024 Uiso 1 1 calc R . .
C23 C 0.32737(7) 1.10553(12) 0.31721(8) 0.0221(2) Uani 1 1 d . . .
H23 H 0.3421 1.1830 0.3071 0.026 Uiso 1 1 calc R . .
C24 C 0.37619(7) 1.03228(12) 0.37048(8) 0.0216(2) Uani 1 1 d . . .
H24 H 0.4239 1.0604 0.3976 0.026 Uiso 1 1 calc R . .
C25 C 0.35533(6) 0.91813(12) 0.38410(8) 0.0210(2) Uani 1 1 d . . .
H25 H 0.3890 0.8675 0.4197 0.025 Uiso 1 1 calc R . .
C26 C 0.28482(6) 0.87797(11) 0.34544(7) 0.01731(19) Uani 1 1 d . . .
H26 H 0.2706 0.7998 0.3548 0.021 Uiso 1 1 calc R . .
S31 S 0.046911(15) 0.62534(2) 0.336183(16) 0.01458(5) Uani 1 1 d . . .
C32 C 0.02216(6) 0.49398(10) 0.28902(7) 0.01467(18) Uani 1 1 d . . .
C41 C 0.05116(6) 0.38454(10) 0.33367(7) 0.01676(19) Uani 1 1 d . . .
C42 C 0.08236(8) 0.29439(12) 0.29989(9) 0.0256(3) Uani 1 1 d . . .
H42 H 0.0865 0.3042 0.2488 0.031 Uiso 1 1 calc R . .
C43 C 0.10711(10) 0.19085(14) 0.34122(10) 0.0342(3) Uani 1 1 d . . .
H43 H 0.1280 0.1299 0.3180 0.041 Uiso 1 1 calc R . .
C44 C 0.10178(9) 0.17491(13) 0.41623(10) 0.0311(3) Uani 1 1 d . . .
H44 H 0.1178 0.1028 0.4435 0.037 Uiso 1 1 calc R . .
C45 C 0.07297(8) 0.26500(12) 0.45106(8) 0.0253(2) Uani 1 1 d . . .
H45 H 0.0701 0.2554 0.5027 0.030 Uiso 1 1 calc R . .
C46 C 0.04834(7) 0.36963(11) 0.41011(7) 0.0196(2) Uani 1 1 d . . .
H46 H 0.0294 0.4316 0.4345 0.024 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'
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
_geom_angle_publ_flag
S4 V1 S4 142.910(19) 2 . ?
S4 V1 S1 82.800(11) 2 . ?
S4 V1 S1 82.131(10) . . ?
S4 V1 S1 82.131(11) 2 2 ?
S4 V1 S1 82.800(10) . 2 ?
S1 V1 S1 131.307(18) . 2 ?
S4 V1 S31 76.782(10) 2 2 ?
S4 V1 S31 135.186(12) . 2 ?
S1 V1 S31 85.625(10) . 2 ?
S1 V1 S31 134.380(11) 2 2 ?
S4 V1 S31 135.185(12) 2 . ?
S4 V1 S31 76.782(10) . . ?
S1 V1 S31 134.382(11) . . ?
S1 V1 S31 85.623(10) 2 . ?
S31 V1 S31 81.816(16) 2 . ?
C2 S1 V1 108.95(4) . . ?
C3 C2 C11 122.23(9) . . ?
C3 C2 S1 119.72(8) . . ?
C11 C2 S1 118.05(8) . . ?
C2 C3 C21 125.14(10) . . ?
C2 C3 S4 119.43(8) . . ?
C21 C3 S4 115.41(8) . . ?
C3 S4 V1 109.60(4) . . ?
C16 C11 C12 119.47(11) . . ?
C16 C11 C2 120.41(10) . . ?
C12 C11 C2 120.08(10) . . ?
C13 C12 C11 120.06(12) . . ?
C14 C13 C12 120.06(12) . . ?
C13 C14 C15 120.07(11) . . ?
C14 C15 C16 120.25(12) . . ?
C15 C16 C11 120.03(11) . . ?
C22 C21 C26 119.13(10) . . ?
C22 C21 C3 121.36(10) . . ?
C26 C21 C3 119.44(10) . . ?
C23 C22 C21 120.31(11) . . ?
C24 C23 C22 120.14(12) . . ?
C25 C24 C23 120.03(11) . . ?
C24 C25 C26 119.87(12) . . ?
C25 C26 C21 120.51(11) . . ?
C32 S31 V1 109.56(4) . . ?
C32 C32 C41 123.77(6) 2 . ?
C32 C32 S31 119.50(4) 2 . ?
C41 C32 S31 116.71(8) . . ?
C46 C41 C42 118.81(11) . . ?
C46 C41 C32 120.78(10) . . ?
C42 C41 C32 120.41(11) . . ?
C43 C42 C41 119.89(13) . . ?
C42 C43 C44 120.94(14) . . ?
C45 C44 C43 119.61(13) . . ?
C44 C45 C46 119.82(13) . . ?
C45 C46 C41 120.85(12) . . ?
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 S4 2.3352(3) 2 ?
V1 S4 2.3352(3) . ?
V1 S1 2.3467(3) . ?
V1 S1 2.3467(3) 2 ?
V1 S31 2.3499(3) 2 ?
V1 S31 2.3500(3) . ?
S1 C2 1.7073(11) . ?
C2 C3 1.3937(15) . ?
C2 C11 1.4849(15) . ?
C3 C21 1.4855(15) . ?
C3 S4 1.7003(11) . ?
C11 C16 1.3953(17) . ?
C11 C12 1.4007(16) . ?
C12 C13 1.3923(18) . ?
C13 C14 1.387(2) . ?
C14 C15 1.389(2) . ?
C15 C16 1.3907(17) . ?
C21 C22 1.3956(17) . ?
C21 C26 1.3968(16) . ?
C22 C23 1.3924(17) . ?
C23 C24 1.3901(19) . ?
C24 C25 1.3880(18) . ?
C25 C26 1.3944(17) . ?
S31 C32 1.6988(12) . ?
C32 C32 1.404(2) 2 ?
C32 C41 1.4836(16) . ?
C41 C46 1.3976(17) . ?
C41 C42 1.4021(17) . ?
C42 C43 1.386(2) . ?
C43 C44 1.390(2) . ?
C44 C45 1.387(2) . ?
C45 C46 1.3934(18) . ?
