Racemic <i>cis</i>-methoxobis(2-methyl-3-oxo-4<i>H</i>-pyran-4-olato)oxovanadium(V) redetermined at 120K: hydrogen-bonded ribbons containing <i>R</i>~2~^2^(7), <i>R</i>~2~^2^(14) and <i>R</i>~4~^4^(18) rings
Kavitha, Savaridasson Jose; Panchanatheswaran, Krishnaswamy; Low, John N.; Glidewell, Christopher; Acta Crystallographica Section C 62 (2006) m116–m118; doi:10.1107/S0108270106003404

data_2014403
_publ_section_title
;
 Racemic
 <i>cis</i>-methoxobis(2-methyl-3-oxo-4<i>H</i>-pyran-4-olato)oxovanadium(V)
 redetermined at 120K: hydrogen-bonded ribbons containing
 <i>R</i>~2~^2^(7), <i>R</i>~2~^2^(14) and <i>R</i>~4~^4^(18) rings
;
_journal_coeditor_code           SK1897
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m116
_journal_page_last               m118
_journal_paper_doi               10.1107/S0108270106003404
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[V (C H3 O) (C6 H5 O3)2 O]'
_chemical_formula_moiety         'C13 H13 O8 V'
_chemical_formula_sum            'C13 H13 O8 V'
_chemical_formula_weight         348.17
_chemical_name_systematic
;
Racemic cis-methoxobis(2-methyl-3-oxo-4H-pyran-4-olato)oxovanadium(V)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.937(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.007(2)
_cell_length_b                   7.6637(6)
_cell_length_c                   13.3083(10)
_cell_measurement_reflns_used    3249
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.13
_cell_volume                     2849.7(4)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) and COLLECT'
_computing_data_collection       'COLLECT (Hooft, 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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0915
_diffrn_reflns_av_sigmaI/netI    0.1154
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10000
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.13
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.489
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3249
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+6.4183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                1976
_reflns_number_total             3249
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1897.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014403
_cod_database_fobs_code          2014403