Low-temperature oxobis(2,2,6,6-tetramethyl-3,5-heptanedionato)vanadium(IV)
Urs, Usha K.; Anitha, K. C.; Lakshmi Raghunathan, K.; Shivashankar, S. A.; Robinson, W. T.; Guru Row, T. N.; Acta Crystallographica Section E 57 (2001) m242–m243; doi:10.1107/S1600536801007760

data_2200349
_publ_section_title
;
 Low-temperature
 oxobis(2,2,6,6-tetramethyl-3,5-heptanedionato)vanadium(IV)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m242
_journal_page_last               m243
_journal_paper_doi               10.1107/S1600536801007760
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[V O (C11 H19 O2)2]'
_chemical_formula_moiety         'C22 H38 O5 V'
_chemical_formula_sum            'C22 H38 O5 V'
_chemical_formula_weight         433.46
_chemical_name_systematic
;
oxobis(2,2,6,6-tetramethyl-3,5-heptadionato)vanadium(IV)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.0250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4515(2)
_cell_length_b                   10.7953(3)
_cell_length_c                   12.7494(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8
_cell_volume                     1229.79(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    ' ORTEP-3 (Johnson, 1976; Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999) '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_measured_fraction_theta_full .982
_diffrn_measured_fraction_theta_max .982
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .093
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7897
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .429
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             466
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .40
_refine_diff_density_max         .95
_refine_diff_density_min         -1.01
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .92
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      .92
_refine_ls_R_factor_gt           .074
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0898P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .187
_reflns_number_gt                2751
_reflns_number_total             4217
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6017.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2200349
_cod_database_fobs_code          2200349