Hydrogen-bonded sheets in racemic <i>cis</i>-(2,2'-bipyridyl-κ^2^<i>N</i>,<i>N</i>')oxo(pentane-2,4-dionato-κ^2^<i>O</i>,<i>O</i>')(thiocyanato-κ<i>N</i>)vanadium(IV)
Kavitha, Savaridasson Jose; Panchanatheswaran, Krishnaswamy; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 62 (2006) m177–m179; doi:10.1107/S0108270106008158

data_2015294
_publ_section_title
;Hydrogen-bonded sheets in racemic
 <i>cis</i>-(2,2'-bipyridyl-\k^2^<i>N</i>,<i>N</i>')oxo(pentane-2,4-dionato-\k^2^<i>O</i>,<i>O</i>')(thiocyanato-\k<i>N</i>)vanadium(IV)
;
_journal_coeditor_code           FA3005
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m177
_journal_page_last               m179
_journal_paper_doi               10.1107/S0108270106008158
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[V (C5 H7 O2) (N C S) O (C10 H8 N2)]'
_chemical_formula_moiety         'C16 H15 N3 O3 S V'
_chemical_formula_sum            'C16 H15 N3 O3 S V'
_chemical_formula_weight         380.32
_chemical_name_systematic
;
racemic
cis-(2,2'-bipyridyl-\k^2^N,N')oxo(pentane-2,4-dionato-
\k^2^O,O')(thiocyanato-\kN)vanadium(IV)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   15.0522(10)
_cell_length_b                   29.721(2)
_cell_length_c                   15.3753(10)
_cell_measurement_reflns_used    7898
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.98
_cell_volume                     6878.4(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'OSCAIL and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'OSCAIL (McArdle, 2003) and SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40301
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.693
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0615P)^2^+3.5919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                5904
_reflns_number_total             7898
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3005.cif
_cod_data_source_block           I
_cod_database_code               2015294