Tetradentate N2S2 Vanadyl(IV) Coordination Complexes: Synthesis, Characterization, and Reactivity Studies
Roxanne M. Jenkins; Tiffany A. Pinder; Michelle L. Hatley; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 50 (2011) 1849–1855; doi:10.1021/ic1022533

data_4324530
_publ_section_title
;
 Tetradentate N2S2 Vanadyl(IV) Coordination Complexes: Synthesis,
 Characterization, and Reactivity Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1849
_journal_page_last               1855
_journal_paper_doi               10.1021/ic1022533
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C22 H50 N4 O4 S2 V'
_chemical_formula_weight         549.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                72.63(5)
_cell_angle_beta                 79.92(4)
_cell_angle_gamma                80.36(5)
_cell_formula_units_Z            2
_cell_length_a                   8.894(5)
_cell_length_b                   12.219(7)
_cell_length_c                   13.832(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1401.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19908
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            bluepurple
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             594
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0550P)^2^+0.5571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                3793
_reflns_number_total             4891
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022533_si_004.cif
_cod_data_source_block           rx12
_cod_original_cell_volume        1401.9(13)
_cod_database_code               4324530