Cocrystallization of dichloro(<i>N</i>,<i>N</i>-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]vanadium(III) with its partially oxidized analog chloro(<i>N</i>,<i>N</i>-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]oxovanadium(IV)
McLauchlan, Craig C.; McDonald, Kenneth J.; Acta Crystallographica Section E 62 (2006) m588–m590; doi:10.1107/S1600536806005423

data_2208400
_publ_section_title
;Cocrystallization of
 dichloro(<i>N</i>,<i>N</i>-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]vanadium(III)
 with its partially oxidized analog
 chloro(<i>N</i>,<i>N</i>-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]oxovanadium(IV)
;
_journal_coeditor_code           OM6287
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m588
_journal_page_last               m590
_journal_paper_doi               10.1107/S1600536806005423
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'[V (C9 H10 B N6) Cl2 (C3 H6 N O)] [V (C9 H10 B N6) Cl O (C3 H6 N O)]'
_chemical_formula_moiety
'C12 H17 B Cl1.53 N7 O1.47 V, C12 H17 B Cl1.53 N7 O1.47 V'
_chemical_formula_sum            'C24 H34 B2 Cl3.06 N14 O2.94 V2'
_chemical_formula_weight         797.66
_chemical_melting_point          456.0(10)
_chemical_name_common
;Dichloro-O-(dimethylformamide)[hydrotris(pyrazol-1-yl)borato]vanadium(III)
Chloro-O-(N,N-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]oxovanadium(IV)
;
_chemical_name_systematic
;
dichloro(N,N-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]vanadium(III)
chloro(N,N-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]oxovanadium(IV)
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            2
_cell_length_a                   8.6005(5)
_cell_length_b                   13.7002(10)
_cell_length_c                   14.8204(13)
_cell_measurement_reflns_used    5892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.1
_cell_volume                     1746.3(2)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2005)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2005)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur3 diffractometer equipped with a CCD detector
;
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15979
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.39
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Clark & Reid, 1995)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             815
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.583
_refine_ls_abs_structure_details
;
1714 Friedel pairs (Flack, 1983)
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.5753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                3370
_reflns_number_total             3987
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6287.cif
_cod_data_source_block           I
_cod_database_code               2208400
_cod_database_fobs_code          2208400