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
Stephen Sproules; Thomas Weyhermüller; Serena DeBeer; Karl Wieghardt; Inorganic Chemistry 49 (2010) 5241–5261; doi:10.1021/ic100344f

data_4315651
_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_moiety         '2(C24 H20 P), C12 N6 S6 V'
_chemical_formula_sum            'C60 H40 N6 P2 S6 V'
_chemical_formula_weight         1150.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8571(14)
_cell_length_b                   15.3014(11)
_cell_length_c                   18.1429(15)
_cell_measurement_temperature    100(2)
_cell_volume                     5512.6(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'724 images at 0.5 deg. stepwise rotation in phi, 30 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  0.1467
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47812
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.9798
_exptl_absorpt_correction_T_min  0.8535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             2364
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0574
_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/[\s^2^(Fo^2^)+(0.0175P)^2^+7.9682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3766
_reflns_number_total             5390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100344f_si_002_3.cif
_cod_data_source_block           2c
_cod_database_code               4315651