Bis(tetrabutylammonium) bis(malonato)oxovanadate(IV)
Therrien, Bruno; Stanislas, Sandrine; Stoeckli-Evans, Helen; Shul'pin, Georgiy B.; Süss-Fink, Georg; Acta Crystallographica Section E 58 (2002) m215–m216; doi:10.1107/S1600536802005913

data_2201088
_publ_section_title
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 Bis(tetrabutylammonium) bis(malonato)oxovanadate(IV)
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_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m215
_journal_page_last               m216
_journal_paper_doi               10.1107/S1600536802005913
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C16 H36 N)2 [V O (C3 H2 O4)2]'
_chemical_formula_moiety         '2C16 H36 N 1+, C6 H4 O9 V 2-'
_chemical_formula_sum            'C38 H76 N2 O9 V'
_chemical_formula_weight         755.95
_chemical_name_systematic
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Bis(tetrabutylammonium) bis(malonato)oxovanadate(IV)
;
_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           SHELXL97
_cell_angle_alpha                92.613(11)
_cell_angle_beta                 90.303(11)
_cell_angle_gamma                95.348(11)
_cell_formula_units_Z            2
_cell_length_a                   9.6847(9)
_cell_length_b                   13.3123(13)
_cell_length_c                   17.1221(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      1.99
_cell_volume                     2195.5(4)
_computing_cell_refinement       'CELL (Stoe & Cie, 1997)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1997)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1997)'
_computing_molecular_graphics    'PLATON/PLUTON (Spek, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Stoe Image Plate Diffraction System'
_diffrn_measurement_method       '\f oscillation'
_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  0.1266
_diffrn_reflns_av_sigmaI/netI    0.1890
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17277
_diffrn_reflns_theta_full        25.87
_diffrn_reflns_theta_max         25.87
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.56
_refine_ls_extinction_coef       0.0137(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.76
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7920
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.76
_refine_ls_R_factor_all          0.145
_refine_ls_R_factor_gt           0.068
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0859P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.159
_refine_ls_wR_factor_ref         0.183
_reflns_number_gt                3112
_reflns_number_total             7920
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6115.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               2201088
_cod_database_fobs_code          2201088