Adduct Formation between Alkali Metal Ions and Anionic LVVO2- (L2- = Tridentate ONS Ligands) Species: Syntheses, Structural Investigation, and Photochemical Studies
Satyabrata Samanta; Suman Mukhopadhyay; Debdas Mandal; Ray J. Butcher; Muktimoy Chaudhury; Inorganic Chemistry 42 (2003) 6284–6293; doi:10.1021/ic030080i

data_4314312
_publ_section_title
;
 Adduct Formation between Alkali Metal Ions and Anionic LVVO2- (L2- =
 Tridentate ONS Ligands) Species: Syntheses, Structural Investigation, and
 Photochemical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6284
_journal_page_last               6293
_journal_paper_doi               10.1021/ic030080i
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C9 H8 Cs N2 O3 S2 V'
_chemical_formula_weight         440.14
_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                 110.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.540(3)
_cell_length_b                   26.966(10)
_cell_length_c                   8.068(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.23
_cell_measurement_theta_min      4.44
_cell_volume                     1332.7(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2503
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.70
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.749
_exptl_absorpt_correction_T_max  0.5389
_exptl_absorpt_correction_T_min  0.1913
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.99
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.0015(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                1610
_reflns_number_total             2302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030080i_3.cif
_cod_data_source_block           mc4newa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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               4314312