(<i>OC</i>-6-13)-Difluoridooxidobis(propan-2-ol)(propan-2-olato)vanadium(V)
Kohl, Julia; Wiedemann, Dennis; Acta Crystallographica Section C 69 (2013) 1482–1484; doi:10.1107/S0108270113029776

data_2019278
_publ_section_title
;
 (<i>OC</i>-6-13)-Difluoridooxidobis(propan-2-ol)(propan-2-olato)vanadium(V)
;
_journal_coeditor_code           EG3138
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1482
_journal_page_last               1484
_journal_paper_doi               10.1107/S0108270113029776
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[V (C3 H7 O) F2 O (C3 H8 O)2]'
_chemical_formula_moiety         'C9 H23 F2 O4 V'
_chemical_formula_structural
'F2 O (O (C H (C H3)2)) (O H (C H (C H3)2))2 V'
_chemical_formula_sum            'C9 H23 F2 O4 V'
_chemical_formula_weight         284.21
_chemical_name_systematic
;
(<i>OC</i>-6--13)-Difluoridooxidobis(propan-2-ol)(propan-2-olato)vanadium(V)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                97.315(7)
_cell_angle_beta                 97.690(7)
_cell_angle_gamma                92.324(7)
_cell_formula_units_Z            4
_cell_length_a                   9.0943(9)
_cell_length_b                   9.9151(8)
_cell_length_c                   16.4279(13)
_cell_measurement_reflns_used    2615
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.5898
_cell_measurement_theta_min      3.4772
_cell_volume                     1453.5(2)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
;
WinGX (Farrugia, 2012), Mercury (Macrae et al., 2008), PLATON/MOLFIT (Spek,
2009), PLATON/PLUTON (Spek, 2009) and CSM website (Zayit et al., 2011)
;
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10818
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.477
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       coloumn
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.887
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    heteroxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5702
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                4505
_reflns_number_total             5702
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3138.cif
_cod_data_source_block           I
_cod_database_code               2019278
_shelx_estimated_absorpt_t_min   0.575
_shelx_estimated_absorpt_t_max   0.910
_shelx_hkl_checksum              27466
_shelx_res_checksum              35136
_shelxl_version_number           .2013