#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/84/2208400.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2208400
loop_
_publ_author_name
'McLauchlan, Craig C.'
'McDonald, Kenneth J.'
_publ_section_title
;Cocrystallization of
 dichloro(N,N-dimethylformamide)[hydrotris(pyrazol-1-yl)borato]vanadium(III)
 with its partially oxidized analog
 chloro(N,N-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       'φ and ω'
_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/[σ²(Fo²)+(0.0723P)²+0.5753P] where P=(Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            om6287.cif
_cod_data_source_block           I
_cod_database_code               2208400
_cod_database_fobs_code          2208400
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.0733(4) 0.3920(3) -0.1179(3) 0.0440(9) Uani d . 1 . .
H H1 0.1358 0.4299 -0.1575 0.053 Uiso calc R 1 . .
C C1S 0.4331(4) 0.5640(3) -0.0296(2) 0.0335(7) Uani d . 1 . .
H H1S 0.4261 0.6296 -0.0095 0.040 Uiso calc R 1 . .
C C2 -0.0025(4) 0.3072(3) -0.1422(3) 0.0449(9) Uani d . 1 . .
H H2 -0.0022 0.2765 -0.1996 0.054 Uiso calc R 1 . .
C C2S 0.6679(4) 0.6115(3) -0.1073(3) 0.0482(10) Uani d . 1 . .
H H2S1 0.6447 0.6743 -0.0788 0.072 Uiso calc R 1 . .
H H2S2 0.6692 0.6194 -0.1730 0.072 Uiso calc R 1 . .
H H2S3 0.7699 0.5883 -0.0868 0.072 Uiso calc R 1 . .
C C3 -0.0789(4) 0.2764(3) -0.0652(3) 0.0414(8) Uani d . 1 . .
H H3 -0.1421 0.2198 -0.0599 0.050 Uiso calc R 1 . .
C C3S 0.5612(5) 0.4430(3) -0.1198(3) 0.0576(11) Uani d . 1 . .
H H3S1 0.4688 0.4049 -0.1039 0.086 Uiso calc R 1 . .
H H3S2 0.6541 0.4109 -0.0955 0.086 Uiso calc R 1 . .
H H3S3 0.5697 0.4474 -0.1856 0.086 Uiso calc R 1 . .
C C4 0.2606(4) 0.4071(3) 0.2140(2) 0.0379(8) Uani d . 1 . .
H H4 0.3478 0.4486 0.2228 0.045 Uiso calc R 1 . .
C C5 0.2237(4) 0.3273(3) 0.2688(3) 0.0425(8) Uani d . 1 . .
H H5 0.2785 0.3044 0.3203 0.051 Uiso calc R 1 . .
C C6 0.0903(4) 0.2892(3) 0.2313(3) 0.0403(8) Uani d . 1 . .
H H6 0.0355 0.2336 0.2527 0.048 Uiso calc R 1 . .
C C7 -0.2107(4) 0.5978(3) 0.1185(2) 0.0366(7) Uani d . 1 . .
H H7 -0.1907 0.6656 0.1118 0.044 Uiso calc R 1 . .
C C8 -0.3498(4) 0.5595(3) 0.1484(2) 0.0408(8) Uani d . 1 . .
H H8 -0.4407 0.5941 0.1660 0.049 Uiso calc R 1 . .
C C9 -0.3274(4) 0.4592(3) 0.1471(2) 0.0382(8) Uani d . 1 . .
H H9 -0.4016 0.4113 0.1641 0.046 Uiso calc R 1 . .
B B1 -0.0976(4) 0.3435(3) 0.1004(3) 0.0367(9) Uani d . 1 . .
H H1B -0.1664 0.2869 0.1155 0.044 Uiso calc R 1 . .
Cl Cl1 0.0599(2) 0.65803(16) -0.04142(14) 0.0351(4) Uani d P 0.53 A 1
O O1A 0.0664(8) 0.6100(6) -0.0391(5) 0.0467(17) Uani d P 0.47 A 2
Cl Cl2 0.21846(11) 0.63759(7) 0.15529(8) 0.0552(3) Uani d . 1 A .
N N1 0.0471(3) 0.4138(2) -0.0314(2) 0.0350(6) Uani d . 1 A .
N N1S 0.5482(3) 0.5400(2) -0.08221(19) 0.0366(6) Uani d . 1 . .
N N2 0.1565(3) 0.41708(19) 0.1475(2) 0.0332(6) Uani d . 1 A .
N N3 -0.1088(3) 0.5285(2) 0.10031(19) 0.0333(6) Uani d . 1 A .
N N4 -0.0477(3) 0.3410(2) 0.0011(2) 0.0351(6) Uani d . 1 . .
N N5 0.0504(3) 0.3438(2) 0.1596(2) 0.0346(6) Uani d . 1 . .
N N6 -0.1811(3) 0.4416(2) 0.1174(2) 0.0352(6) Uani d . 1 . .
O O1S 0.3310(3) 0.50463(18) -0.00430(17) 0.0401(6) Uani d . 1 A .
V V1 0.11994(6) 0.53328(5) 0.04922(6) 0.0467(2) Uani d . 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1 C1 C2 111.1(4) ?
N1 C1 H1 124.5 ?
C2 C1 H1 124.5 ?
O1S C1S N1S 123.3(3) ?
O1S C1S H1S 118.4 ?
N1S C1S H1S 118.4 ?
C1 C2 C3 105.4(3) ?
C1 C2 H2 127.3 ?
C3 C2 H2 127.3 ?
N1S C2S H2S1 109.5 ?
N1S C2S H2S2 109.5 ?
H2S1 C2S H2S2 109.5 ?
N1S C2S H2S3 109.5 ?
H2S1 C2S H2S3 109.5 ?
H2S2 C2S H2S3 109.5 ?
N4 C3 C2 107.8(3) ?
N4 C3 H3 126.1 ?
C2 C3 H3 126.1 ?
N1S C3S H3S1 109.5 ?
N1S C3S H3S2 109.5 ?
H3S1 C3S H3S2 109.5 ?
N1S C3S H3S3 109.5 ?
H3S1 C3S H3S3 109.5 ?
H3S2 C3S H3S3 109.5 ?
N2 C4 C5 110.8(3) ?
N2 C4 H4 124.6 ?
C5 C4 H4 124.6 ?
C6 C5 C4 104.6(3) ?
C6 C5 H5 127.7 ?
C4 C5 H5 127.7 ?
N5 C6 C5 108.7(3) ?
N5 C6 H6 125.7 ?
C5 C6 H6 125.7 ?
N3 C7 C8 111.6(3) ?
N3 C7 H7 124.2 ?
C8 C7 H7 124.2 ?
C7 C8 C9 104.6(3) ?
C7 C8 H8 127.7 ?
C9 C8 H8 127.7 ?
N6 C9 C8 108.0(3) ?
N6 C9 H9 126.0 ?
C8 C9 H9 126.0 ?
N4 B1 N6 107.8(3) ?
N4 B1 N5 108.3(3) ?
N6 B1 N5 106.7(3) ?
N4 B1 H1B 111.3 ?
N6 B1 H1B 111.3 ?
N5 B1 H1B 111.3 ?
C1 N1 N4 105.9(3) ?
C1 N1 V1 131.6(3) ?
N4 N1 V1 122.5(2) ?
C1S N1S C3S 121.4(3) ?
C1S N1S C2S 121.1(3) ?
C3S N1S C2S 117.4(3) ?
C4 N2 N5 105.9(3) ?
C4 N2 V1 131.6(2) ?
N5 N2 V1 121.8(2) ?
C7 N3 N6 106.7(3) ?
C7 N3 V1 132.1(2) ?
N6 N3 V1 121.19(19) ?
C3 N4 N1 109.8(3) ?
C3 N4 B1 131.1(3) ?
N1 N4 B1 119.1(3) ?
C6 N5 N2 110.0(3) ?
C6 N5 B1 131.1(3) ?
N2 N5 B1 118.5(3) ?
C9 N6 N3 109.1(3) ?
C9 N6 B1 129.7(3) ?
N3 N6 B1 121.1(2) ?
C1S O1S V1 128.4(2) ?
O1A V1 O1S 93.4(3) ?
O1A V1 N3 92.4(3) ?
O1S V1 N3 166.77(11) y
O1A V1 N1 88.0(3) ?
O1S V1 N1 83.92(10) y
N3 V1 N1 84.43(11) y
O1A V1 N2 168.9(3) ?
O1S V1 N2 89.47(10) y
N3 V1 N2 82.65(10) y
N1 V1 N2 81.71(11) y
O1A V1 Cl1 12.8(3) ?
O1S V1 Cl1 96.90(9) y
N3 V1 Cl1 91.38(9) y
N1 V1 Cl1 100.56(10) y
N2 V1 Cl1 173.41(9) y
O1A V1 Cl2 103.7(3) ?
O1S V1 Cl2 93.35(8) y
N3 V1 Cl2 96.79(8) y
N1 V1 Cl2 168.16(9) y
N2 V1 Cl2 86.76(8) y
Cl1 V1 Cl2 91.20(7) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 1.334(5) ?
C1 C2 1.380(6) ?
C1 H1 0.9500 ?
C1S O1S 1.254(4) ?
C1S N1S 1.302(4) ?
C1S H1S 0.9500 ?
C2 C3 1.383(6) ?
C2 H2 0.9500 ?
C2S N1S 1.469(4) ?
C2S H2S1 0.9800 ?
C2S H2S2 0.9800 ?
C2S H2S3 0.9800 ?
C3 N4 1.349(5) ?
C3 H3 0.9500 ?
C3S N1S 1.446(5) ?
C3S H3S1 0.9800 ?
C3S H3S2 0.9800 ?
C3S H3S3 0.9800 ?
C4 N2 1.339(5) ?
C4 C5 1.398(5) ?
C4 H4 0.9500 ?
C5 C6 1.377(5) ?
C5 H5 0.9500 ?
C6 N5 1.344(5) ?
C6 H6 0.9500 ?
C7 N3 1.319(4) ?
C7 C8 1.380(5) ?
C7 H7 0.9500 ?
C8 C9 1.387(6) ?
C8 H8 0.9500 ?
C9 N6 1.355(4) ?
C9 H9 0.9500 ?
B1 N4 1.534(5) ?
B1 N6 1.545(5) ?
B1 N5 1.546(5) ?
B1 H1B 1.0000 ?
Cl1 V1 2.234(2) y
O1A V1 1.741(8) y
Cl2 V1 2.2872(13) y
N1 N4 1.375(4) ?
N1 V1 2.121(3) y
N2 N5 1.369(4) ?
N2 V1 2.181(3) y
N3 N6 1.366(4) ?
N3 V1 2.109(3) y
O1S V1 2.019(2) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C1 C2 C3 0.0(4)
C1 C2 C3 N4 -0.2(4)
N2 C4 C5 C6 0.0(4)
C4 C5 C6 N5 -0.6(4)
N3 C7 C8 C9 -0.3(4)
C7 C8 C9 N6 -0.1(4)
C2 C1 N1 N4 0.2(4)
C2 C1 N1 V1 -178.1(2)
O1S C1S N1S C3S 3.7(5)
O1S C1S N1S C2S -177.8(3)
C5 C4 N2 N5 0.5(4)
C5 C4 N2 V1 170.5(2)
C8 C7 N3 N6 0.6(4)
C8 C7 N3 V1 177.9(2)
C2 C3 N4 N1 0.3(4)
C2 C3 N4 B1 -178.7(3)
C1 N1 N4 C3 -0.3(4)
V1 N1 N4 C3 178.2(2)
C1 N1 N4 B1 178.9(3)
V1 N1 N4 B1 -2.6(4)
N6 B1 N4 C3 -123.5(4)
N5 B1 N4 C3 121.4(4)
N6 B1 N4 N1 57.5(4)
N5 B1 N4 N1 -57.6(4)
C5 C6 N5 N2 0.9(4)
C5 C6 N5 B1 -171.0(3)
C4 N2 N5 C6 -0.9(4)
V1 N2 N5 C6 -172.1(2)
C4 N2 N5 B1 172.2(3)
V1 N2 N5 B1 1.0(4)
N4 B1 N5 C6 -131.0(4)
N6 B1 N5 C6 113.2(4)
N4 B1 N5 N2 57.7(4)
N6 B1 N5 N2 -58.1(4)
C8 C9 N6 N3 0.5(4)
C8 C9 N6 B1 -178.0(3)
C7 N3 N6 C9 -0.7(4)
V1 N3 N6 C9 -178.3(2)
C7 N3 N6 B1 177.9(3)
V1 N3 N6 B1 0.3(4)
N4 B1 N6 C9 121.3(4)
N5 B1 N6 C9 -122.5(4)
N4 B1 N6 N3 -57.0(4)
N5 B1 N6 N3 59.2(4)
N1S C1S O1S V1 -163.1(2)
C1S O1S V1 O1A 53.2(4)
C1S O1S V1 N3 169.2(4)
C1S O1S V1 N1 140.8(3)
C1S O1S V1 N2 -137.5(3)
C1S O1S V1 Cl1 40.8(3)
C1S O1S V1 Cl2 -50.8(3)
C7 N3 V1 O1A -49.2(4)
N6 N3 V1 O1A 127.8(4)
C7 N3 V1 O1S -165.3(4)
N6 N3 V1 O1S 11.7(7)
C7 N3 V1 N1 -136.9(3)
N6 N3 V1 N1 40.1(3)
C7 N3 V1 N2 140.8(3)
N6 N3 V1 N2 -42.3(2)
C7 N3 V1 Cl1 -36.4(3)
N6 N3 V1 Cl1 140.5(2)
C7 N3 V1 Cl2 55.0(3)
N6 N3 V1 Cl2 -128.1(2)
C1 N1 V1 O1A 46.1(4)
N4 N1 V1 O1A -132.0(3)
C1 N1 V1 O1S -47.6(3)
N4 N1 V1 O1S 134.4(2)
C1 N1 V1 N3 138.7(3)
N4 N1 V1 N3 -39.3(2)
C1 N1 V1 N2 -137.9(3)
N4 N1 V1 N2 44.0(2)
C1 N1 V1 Cl1 48.3(3)
N4 N1 V1 Cl1 -129.7(2)
C1 N1 V1 Cl2 -124.8(4)
N4 N1 V1 Cl2 57.2(5)
C4 N2 V1 O1A 169.6(13)
N5 N2 V1 O1A -21.7(14)
C4 N2 V1 O1S 64.2(3)
N5 N2 V1 O1S -127.1(2)
C4 N2 V1 N3 -126.5(3)
N5 N2 V1 N3 42.2(2)
C4 N2 V1 N1 148.1(3)
N5 N2 V1 N1 -43.2(2)
C4 N2 V1 Cl1 -101.3(8)
N5 N2 V1 Cl1 67.4(9)
C4 N2 V1 Cl2 -29.2(3)
N5 N2 V1 Cl2 139.5(2)
