#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/67/7026731.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_7026731
loop_
_publ_author_name
'Nishina, Masafumi'
'Moriuchi, Toshiyuki'
'Hirao, Toshikazu'
_publ_section_title
;
 Synthesis of (arylimido)vanadium complexes and their application for
 oxidative coupling reactions of silyl enol ether derivatives.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9936
_journal_page_last               9940
_journal_paper_doi               10.1039/c0dt00633e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C8 H10 Cl2 N O V '
_chemical_formula_sum            'C8 H10 Cl2 N O V'
_chemical_formula_weight         258.02
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   11.6418(14)
_cell_length_b                   7.8118(8)
_cell_length_c                   24.194(3)
_cell_measurement_reflns_used    12585
_cell_measurement_temperature    173.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     2200.3(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 5.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19050
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.28
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2503
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0362P)²+0.8069P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                2218
_reflns_number_total             2503
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c0dt00633e.txt
_cod_data_source_block           vanadium_complex_1b
_cod_original_cell_volume        2200.2(4)
_cod_original_formula_sum        'C8 H10 Cl2 N O V '
_cod_database_code               7026731
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,+Z
3 +X,1/2-Y,1/2+Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 1/2+X,1/2-Y,-Z
7 -X,1/2+Y,1/2-Z
8 1/2+X,+Y,1/2-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
V(1) V 0.43288(3) 0.54226(4) 0.556627(11) 0.02164(11) Uani 1.00 1 d .
Cl(1) Cl 0.52184(4) 0.77715(6) 0.586389(19) 0.03478(13) Uani 1.00 1 d .
Cl(2) Cl 0.25152(4) 0.57914(7) 0.53162(2) 0.03543(14) Uani 1.00 1 d .
O(1) O 0.51984(10) 0.37195(15) 0.52703(5) 0.0229(2) Uani 1.00 1 d .
N(1) N 0.40745(14) 0.46012(19) 0.61850(6) 0.0271(3) Uani 1.00 1 d .
C(1) C 0.38428(16) 0.4105(2) 0.67214(7) 0.0258(3) Uani 1.00 1 d .
C(2) C 0.28075(17) 0.3279(2) 0.68445(8) 0.0337(4) Uani 1.00 1 d .
C(3) C 0.25738(17) 0.2854(2) 0.73909(9) 0.0389(4) Uani 1.00 1 d .
C(4) C 0.33503(18) 0.3229(2) 0.78028(8) 0.0373(4) Uani 1.00 1 d .
C(5) C 0.43825(18) 0.4038(2) 0.76786(8) 0.0362(4) Uani 1.00 1 d .
C(6) C 0.46389(17) 0.4470(2) 0.71384(8) 0.0310(4) Uani 1.00 1 d .
C(7) C 0.55040(16) 0.2074(2) 0.55178(8) 0.0271(3) Uani 1.00 1 d .
C(8) C 0.64420(17) 0.2273(2) 0.59432(8) 0.0355(4) Uani 1.00 1 d .
H(1) H 0.2274 0.3014 0.6560 0.040 Uiso 1.00 1 c R
H(2) H 0.1872 0.2300 0.7481 0.047 Uiso 1.00 1 c R
H(3) H 0.3179 0.2933 0.8175 0.045 Uiso 1.00 1 c R
H(4) H 0.4913 0.4294 0.7965 0.043 Uiso 1.00 1 c R
H(5) H 0.5348 0.5009 0.7051 0.037 Uiso 1.00 1 c R
H(6) H 0.5765 0.1281 0.5224 0.032 Uiso 1.00 1 c R
H(7) H 0.4816 0.1569 0.5695 0.032 Uiso 1.00 1 c R
H(8) H 0.6627 0.1152 0.6101 0.043 Uiso 1.00 1 c R
H(9) H 0.6180 0.3042 0.6237 0.043 Uiso 1.00 1 c R
H(10) H 0.7128 0.2755 0.5767 0.043 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
V V 0.300 0.529
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl(1) V(1) Cl(2) 115.12(2) yes . .
Cl(1) V(1) O(1) 118.12(4) yes . .
Cl(1) V(1) O(1) 86.00(3) yes . 5_666
Cl(1) V(1) N(1) 96.33(5) yes . .
Cl(2) V(1) O(1) 121.21(4) yes . .
Cl(2) V(1) O(1) 87.00(3) yes . 5_666
Cl(2) V(1) N(1) 97.29(5) yes . .
O(1) V(1) O(1) 73.84(4) yes . 5_666
O(1) V(1) N(1) 99.91(6) yes . .
O(1) V(1) N(1) 173.66(6) yes 5_666 .
V(1) O(1) V(1) 106.16(5) yes . 5_666
V(1) O(1) C(7) 128.12(10) yes . .
V(1) O(1) C(7) 125.68(10) yes 5_666 .
V(1) N(1) C(1) 173.46(13) yes . .
N(1) C(1) C(2) 119.85(16) yes . .
N(1) C(1) C(6) 119.41(16) yes . .
C(2) C(1) C(6) 120.73(16) yes . .
C(1) C(2) C(3) 118.77(17) yes . .
C(2) C(3) C(4) 120.60(18) yes . .
C(3) C(4) C(5) 120.51(18) yes . .
C(4) C(5) C(6) 120.12(18) yes . .
C(1) C(6) C(5) 119.26(18) yes . .
O(1) C(7) C(8) 111.42(14) yes . .
C(1) C(2) H(1) 120.6 no . .
C(3) C(2) H(1) 120.6 no . .
C(2) C(3) H(2) 119.7 no . .
C(4) C(3) H(2) 119.7 no . .
C(3) C(4) H(3) 119.7 no . .
C(5) C(4) H(3) 119.8 no . .
C(4) C(5) H(4) 119.9 no . .
C(6) C(5) H(4) 119.9 no . .
C(1) C(6) H(5) 120.4 no . .
C(5) C(6) H(5) 120.4 no . .
O(1) C(7) H(6) 109.3 no . .
O(1) C(7) H(7) 109.3 no . .
C(8) C(7) H(6) 109.3 no . .
C(8) C(7) H(7) 109.4 no . .
H(6) C(7) H(7) 108.0 no . .
C(7) C(8) H(8) 109.5 no . .
C(7) C(8) H(9) 109.5 no . .
C(7) C(8) H(10) 109.5 no . .
H(8) C(8) H(9) 109.5 no . .
H(8) C(8) H(10) 109.5 no . .
H(9) C(8) H(10) 109.5 no . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
V(1) Cl(1) 2.2266(5) yes .
V(1) Cl(2) 2.2151(5) yes .
V(1) O(1) 1.8187(12) yes .
V(1) O(1) 2.2019(12) yes 5_666
V(1) N(1) 1.6554(14) yes .
O(1) C(7) 1.462(2) yes .
N(1) C(1) 1.381(2) yes .
C(1) C(2) 1.399(2) yes .
C(1) C(6) 1.399(2) yes .
C(2) C(3) 1.390(2) yes .
C(3) C(4) 1.377(2) yes .
C(4) C(5) 1.390(2) yes .
C(5) C(6) 1.382(2) yes .
C(7) C(8) 1.509(2) yes .
C(2) H(1) 0.950 no .
C(3) H(2) 0.950 no .
C(4) H(3) 0.950 no .
C(5) H(4) 0.950 no .
C(6) H(5) 0.950 no .
C(7) H(6) 0.990 no .
C(7) H(7) 0.990 no .
C(8) H(8) 0.980 no .
C(8) H(9) 0.980 no .
C(8) H(10) 0.980 no .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Cl(1) V(1) O(1) V(1) -76.27(5) . . 5_666
Cl(1) V(1) O(1) C(7) 105.71(12) . . .
Cl(1) V(1) O(1) V(1) 120.81(5) . 5_666 5_666
Cl(1) V(1) O(1) C(7) -57.27(11) . 5_666 5_666
Cl(1) V(1) N(1) C(1) 36.2(12) . . .
Cl(2) V(1) O(1) V(1) 76.15(5) . . 5_666
Cl(2) V(1) O(1) C(7) -101.86(12) . . .
Cl(2) V(1) O(1) V(1) -123.74(5) . 5_666 5_666
Cl(2) V(1) O(1) C(7) 58.18(12) . 5_666 5_666
Cl(2) V(1) N(1) C(1) -80.2(12) . . .
O(1) V(1) O(1) C(7) -178.08(13) . 5_666 5_666
O(1) V(1) O(1) C(7) -178.01(13) 5_666 . .
O(1) V(1) N(1) C(1) 156.2(12) . . .
N(1) V(1) O(1) V(1) -178.99(6) . . 5_666
N(1) V(1) O(1) C(7) 3.00(14) . . .
O(1) V(1) N(1) C(1) 147.4(10) 5_666 . .
N(1) V(1) O(1) V(1) 9.1(6) . 5_666 5_666
N(1) V(1) O(1) C(7) -169.0(5) . 5_666 5_666
V(1) O(1) C(7) C(8) -76.87(17) . . .
V(1) O(1) C(7) C(8) 105.48(15) 5_666 . .
V(1) N(1) C(1) C(2) 108.2(12) . . .
V(1) N(1) C(1) C(6) -70.4(13) . . .
N(1) C(1) C(2) C(3) -177.45(17) . . .
N(1) C(1) C(6) C(5) 177.24(17) . . .
C(2) C(1) C(6) C(5) -1.4(2) . . .
C(6) C(1) C(2) C(3) 1.1(2) . . .
C(1) C(2) C(3) C(4) -0.4(3) . . .
C(2) C(3) C(4) C(5) -0.1(2) . . .
C(3) C(4) C(5) C(6) -0.1(2) . . .
C(4) C(5) C(6) C(1) 0.8(3) . . .
