#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/31/4313129.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313129
loop_
_publ_author_name
'Kenichi Oyaizu'
'Eniya Listiani Dewi'
'Eishun Tsuchida'
_publ_contact_author
;
Eishun Tsuchida
Advanced Research Institute for Science and Engineering, Waseda 
University, Tokyo 169-8555, JAPAN
;
_publ_contact_author_email       eishun@mn.waseda.ac.jp
_publ_contact_author_fax         +81-3-3205-4740
_publ_contact_author_phone       +81-3-5286-3120
_publ_section_title
;
 Coordination of BF4-to Oxovanadium(V) Complexes, Evidenced by the Redox
 Potential of Oxovanadium(IV/V) Couples in CH2Cl2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1070
_journal_page_last               1075
_journal_paper_doi               10.1021/ic0205987
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Prepared from H2(salpn) and VOSO4'
_chemical_formula_analytical     'C21 H23 B F4 N3 O3 V '
_chemical_formula_moiety         'C21 H23 B F4 N3 O3 V '
_chemical_formula_structural     VO(salpn)
_chemical_formula_sum            'C21 H23 B F4 N3 O3 V'
_chemical_formula_weight         503.18
_chemical_name_common
;
[N,N'-2,2-dimethylpropylenebis(salicylideneaminnato)]oxovanadium(V) 
tetrafluoroborate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             'Fri Sep 27 115647 2002'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             'Fri Sep 27 115647 2002'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.19(2)
_cell_length_b                   17.43(2)
_cell_length_c                   12.97(2)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      10.0
_cell_volume                     4564(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    ORTEP
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.04338
_diffrn_orient_matrix_UB_12      0.00720
_diffrn_orient_matrix_UB_13      -0.03592
_diffrn_orient_matrix_UB_21      0.02300
_diffrn_orient_matrix_UB_22      -0.00243
_diffrn_orient_matrix_UB_23      -0.06821
_diffrn_orient_matrix_UB_31      -0.00648
_diffrn_orient_matrix_UB_32      -0.05686
_diffrn_orient_matrix_UB_33      -0.00164
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.00
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.67
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2064.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.47
_refine_ls_abs_structure_details None
_refine_ls_abs_structure_Flack   None
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_all   Undetermined
_refine_ls_goodness_of_fit_obs   1.700
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     279
_refine_ls_number_reflns         2080
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          Undetermined
_refine_ls_R_factor_obs          0.0730
_refine_ls_shift/esd_max         0.0060
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00090|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         Undetermined
_refine_ls_wR_factor_obs         0.0880
_reflns_number_observed          2080
_reflns_number_total             6163
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ic0205987_2.cif
_cod_data_source_block           '[VO(salpn)NCCH3][BF4]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00090|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4564(14)
_cod_original_sg_symbol_Hall     undetermined
_cod_original_sg_symbol_H-M      'P b c a '
_cod_original_formula_sum        'C21 H23 B F4 N3 O3 V '
_cod_database_code               4313129
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2+x,1/2-y,   -z'
'   -x,1/2+y,1/2-z'
'1/2-x,   -y,1/2+z'
'   -x,   -y,   -z'
'1/2-x,1/2+y,   +z'
'   +x,1/2-y,1/2+z'
'1/2+x,   +y,1/2-z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_refinement_flags
V1 0.96973(7) 0.19795(7) 0.20965(9) 0.0390(4) Uani d . 1.00 .
F1 1.2802(7) -0.0230(7) 0.555(1) 0.1103 Uiso d . 0.39 .
F2 1.2463(8) 0.0655(9) 0.6668(8) 0.1103 Uiso d . 0.39 .
F3 1.1873(5) 0.0418(9) 0.526(1) 0.1103 Uiso d . 0.39 .
F4 1.2846(7) 0.1005(8) 0.513(1) 0.1103 Uiso d . 0.39 .
F5 1.242(1) 0.019(1) 0.449(1) 0.1164 Uiso d . 0.29 .
F6 1.1893(9) 0.056(1) 0.591(2) 0.1164 Uiso d . 0.29 .
F7 1.258(1) 0.1363(8) 0.512(2) 0.1164 Uiso d . 0.29 .
F8 1.2977(9) 0.035(1) 0.595(1) 0.1164 Uiso d . 0.29 .
F9 1.3236(6) 0.071(1) 0.539(1) 0.1117 Uiso d . 0.32 .
F10 1.2278(9) 0.084(1) 0.621(1) 0.1117 Uiso d . 0.32 .
F11 1.2456(9) -0.0184(8) 0.523(2) 0.1117 Uiso d . 0.32 .
F12 1.2318(9) 0.096(1) 0.451(1) 0.1117 Uiso d . 0.32 .
O1 1.0298(3) 0.2767(3) 0.2093(4) 0.046(2) Uani d . 1.00 .
O2 1.0256(3) 0.1165(3) 0.1910(4) 0.047(2) Uani d . 1.00 .
O3 0.9368(3) 0.2073(3) 0.0997(4) 0.057(2) Uani d . 1.00 .
N1 0.9083(3) 0.2746(3) 0.2863(5) 0.038(2) Uani d . 1.00 .
N2 0.9043(3) 0.1156(3) 0.2672(5) 0.039(2) Uani d . 1.00 .
N3 1.0152(4) 0.1844(4) 0.3887(6) 0.050(2) Uani d . 1.00 .
C1 1.0459(4) 0.3293(4) 0.2816(6) 0.043(2) Uani d . 1.00 .
C2 1.1100(4) 0.3609(5) 0.2853(7) 0.051(3) Uani d . 1.00 .
C3 1.1259(4) 0.4113(5) 0.3626(8) 0.061(3) Uani d . 1.00 .
C4 1.0802(5) 0.4344(5) 0.4341(7) 0.060(3) Uani d . 1.00 .
C5 1.0163(4) 0.4069(4) 0.4294(6) 0.045(3) Uani d . 1.00 .
C6 0.9981(4) 0.3544(4) 0.3541(6) 0.039(2) Uani d . 1.00 .
C7 0.9299(4) 0.3302(4) 0.3425(6) 0.042(2) Uani d . 1.00 .
C8 0.8356(4) 0.2695(4) 0.2717(6) 0.045(3) Uani d . 1.00 .
C9 0.8061(4) 0.1969(5) 0.3157(7) 0.048(2) Uani d . 1.00 .
C10 0.8319(4) 0.1262(5) 0.2577(7) 0.053(3) Uani d . 1.00 .
C11 0.9234(4) 0.0530(4) 0.3087(6) 0.043(2) Uani d . 1.00 .
C12 0.9905(4) 0.0259(4) 0.3155(6) 0.038(2) Uani d . 1.00 .
C13 1.0060(5) -0.0370(4) 0.3781(6) 0.051(3) Uani d . 1.00 .
C14 1.0690(6) -0.0656(5) 0.3831(9) 0.073(4) Uani d . 1.00 .
C15 1.1171(5) -0.0334(6) 0.3213(9) 0.071(4) Uani d . 1.00 .
C16 1.1031(5) 0.0272(5) 0.2530(8) 0.061(3) Uani d . 1.00 .
C17 1.0401(4) 0.0579(4) 0.2527(6) 0.041(2) Uani d . 1.00 .
C18 0.8191(4) 0.1907(5) 0.4311(7) 0.058(3) Uani d . 1.00 .
C19 0.7313(4) 0.2012(6) 0.2968(9) 0.090(4) Uani d . 1.00 .
C20 1.0595(5) 0.1964(5) 0.4388(6) 0.047(3) Uani d . 1.00 .
C21 1.1176(5) 0.2153(7) 0.5007(7) 0.086(4) Uani d . 1.00 .
B1 1.2492(8) 0.0539(8) 0.550(1) 0.093(4) Uiso d . 1.00 .
H2 1.1417 0.3476 0.2342 0.0507 Uiso calc . 1.00 .
H3 1.1699 0.4309 0.3663 0.0621 Uiso calc . 1.00 .
H4 1.0925 0.4696 0.4869 0.0595 Uiso calc . 1.00 .
H5 0.9843 0.4248 0.4784 0.0456 Uiso calc . 1.00 .
H7 0.8977 0.3583 0.3803 0.0418 Uiso calc . 1.00 .
H8b 0.8264 0.2710 0.2001 0.0456 Uiso calc . 1.00 .
H8a 0.8156 0.3119 0.3049 0.0456 Uiso calc . 1.00 .
H10b 0.8211 0.1316 0.1867 0.0532 Uiso calc . 1.00 .
H10a 0.8102 0.0821 0.2846 0.0532 Uiso calc . 1.00 .
H11 0.8900 0.0207 0.3369 0.0431 Uiso calc . 1.00 .
H13 0.9718 -0.0603 0.4183 0.0507 Uiso calc . 1.00 .
H14 1.0793 -0.1064 0.4288 0.0735 Uiso calc . 1.00 .
H15 1.1611 -0.0527 0.3248 0.0709 Uiso calc . 1.00 .
H16 1.1363 0.0472 0.2083 0.0608 Uiso calc . 1.00 .
H18a 0.8005 0.1433 0.4559 0.0583 Uiso calc . 1.00 .
H18b 0.8655 0.1900 0.4435 0.0583 Uiso calc . 1.00 .
H18c 0.7993 0.2320 0.4662 0.0583 Uiso calc . 1.00 .
H19a 0.7139 0.2458 0.3293 0.0899 Uiso calc . 1.00 .
H19b 0.7233 0.2047 0.2241 0.0899 Uiso calc . 1.00 .
H19c 0.7106 0.1570 0.3231 0.0899 Uiso calc . 1.00 .
H21a 1.1224 0.1777 0.5543 0.0861 Uiso calc . 1.00 .
H21b 1.1557 0.2155 0.4593 0.0861 Uiso calc . 1.00 .
H21c 1.1115 0.2642 0.5320 0.0861 Uiso calc . 1.00 .
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 168 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0 184 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 24 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N 0 24 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
V 0 8 0.300 0.529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
B 0 8 0.001 0.001
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F 0 32 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_reflns_number
6163
