Chloro[hydrotris(pyrazol-1-yl)borato]oxo(1<i>H</i>-pyrazole)vanadium(IV)
McLauchlan, Craig C.; McDonald, Kenneth J.; Acta Crystallographica Section E 61 (2005) m2379–m2381; doi:10.1107/S1600536805033568

data_2207121
_publ_section_title
;
 Chloro[hydrotris(pyrazol-1-yl)borato]oxo(1<i>H</i>-pyrazole)vanadium(IV)
;
_journal_coeditor_code           AC6210
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2379
_journal_page_last               m2381
_journal_paper_doi               10.1107/S1600536805033568
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[V (C9 H10 B N6) Cl O (C3 H4 N2)]'
_chemical_formula_moiety         'C12 H14 B Cl N8 O V'
_chemical_formula_sum            'C12 H14 B Cl N8 O V'
_chemical_formula_weight         383.51
_chemical_name_systematic
;
Chloro[hydrotris(pyrazol-1-yl)borato]oxo(1H-pyrazole)vanadium(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.642(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3295(5)
_cell_length_b                   12.6110(8)
_cell_length_c                   15.3711(12)
_cell_measurement_reflns_used    7083
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4982
_cell_measurement_theta_min      3.9821
_cell_volume                     1609.34(19)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2004)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2004)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    SHELXL97
_computing_publication_material  'WinGX (Farrugia, 1999)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23290
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        <1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.96211
_exptl_absorpt_correction_T_min  0.90131
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Analytical numeric absorption correction using a multifaceted crystal model
based on expressions derived by R.C. Clark & J.S. Reid.  (Clark & Reid,
1995)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.06957
_exptl_crystal_size_mid          0.04788
_exptl_crystal_size_min          0.02159
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.624
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.235
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+3.4547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                3483
_reflns_number_total             3685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ac6210.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2207121
_cod_database_fobs_code          2207121