#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/32/4313220.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_4313220
loop_
_publ_author_name
'Satyabrata Samanta'
'Dipesh Ghosh'
'Suman Mukhopadhyay'
'Akira Endo'
'Timothy J. R. Weakley'
'Muktimoy Chaudhury'
_publ_contact_author_address
;Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Oxovanadium(IV) and -(V) Complexes of Dithiocarbazate-Based Tridentate
 Schiff Base Ligands: Syntheses, Structure, and Photochemical Reactivity
 of Compounds Involving Imidazole Derivatives as Coligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1508
_journal_page_last               1517
_journal_paper_doi               10.1021/ic020438v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_structural     '(C3 H5 N2) (V O2 (C9 H7 Br N2 O S2) )'
_chemical_formula_sum            'C12 H12 Br N4 O3 S2 V'
_chemical_formula_weight         455.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.30(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.668(3)
_cell_length_b                   13.963(2)
_cell_length_c                   18.441(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      12.9
_cell_volume                     1714.1(9)
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Nonius CAD-4 serial diffractometer'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      -0.01079
_diffrn_orient_matrix_UB_12      -0.05828
_diffrn_orient_matrix_UB_13      -0.03150
_diffrn_orient_matrix_UB_21      0.02810
_diffrn_orient_matrix_UB_22      0.03989
_diffrn_orient_matrix_UB_23      -0.04329
_diffrn_orient_matrix_UB_31      0.14721
_diffrn_orient_matrix_UB_32      -0.01190
_diffrn_orient_matrix_UB_33      0.00913
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.029
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3428
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        3.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.177
_exptl_absorpt_correction_T_max  0.318
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews (1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             904.00
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.01
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.89
_refine_ls_goodness_of_fit_ref   2.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.091
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4Fₒ²/[σ²(I) + (0.020I)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.110
_refine_ls_wR_factor_ref         0.057
_reflns_number_gt                2090
_reflns_number_total             2996
_reflns_threshold_expression     I>1.00σ(I)
_cod_data_source_file            ic020438v_2.cif
_cod_data_source_block           mc12_2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 
;
_cod_original_cell_volume        1714.0(6)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C12 H12 Br N4 O3 S2 V '
_cod_database_code               4313220
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
'1/2-x,1/2+y,   -z'
'   -x,   -y,   -z'
'1/2+x,1/2-y,   +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_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Br -0.3166(1) 0.33867(6) 0.49113(4) 0.0961(3) 1.000 . Uani d ?
V 0.3224(1) 0.44109(6) 0.82839(5) 0.0373(3) 1.000 . Uani d ?
S(1) 0.5601(2) 0.5639(1) 0.85378(8) 0.0562(5) 1.000 . Uani d ?
S(2) 0.8360(3) 0.6646(1) 0.7639(1) 0.0710(6) 1.000 . Uani d ?
O(1) 0.2600(5) 0.4516(2) 0.9129(2) 0.046(1) 1.000 . Uani d ?
O(2) 0.4491(5) 0.3427(2) 0.8229(2) 0.044(1) 1.000 . Uani d ?
O(3) 0.0616(5) 0.4166(3) 0.7873(2) 0.047(1) 1.000 . Uani d ?
N(1) 0.5335(7) 0.5604(3) 0.7084(2) 0.046(1) 1.000 . Uani d ?
N(2) 0.3695(6) 0.5017(3) 0.7221(2) 0.038(1) 1.000 . Uani d ?
N(3) 0.3868(6) 0.2185(3) 0.9347(2) 0.047(1) 1.000 . Uani d ?
N(4) 0.3370(6) 0.1085(3) 1.0101(2) 0.048(2) 1.000 . Uani d ?
C(1) 0.871(1) 0.6731(5) 0.6690(4) 0.080(2) 1.000 . Uani d ?
C(2) 0.6262(8) 0.5894(4) 0.7675(3) 0.049(2) 1.000 . Uani d ?
C(3) 0.2697(8) 0.4791(4) 0.6630(3) 0.043(2) 1.000 . Uani d ?
C(4) 0.0848(8) 0.4248(3) 0.6582(3) 0.040(2) 1.000 . Uani d ?
C(5) -0.0106(8) 0.3970(4) 0.7209(3) 0.038(2) 1.000 . Uani d ?
C(6) -0.1941(9) 0.3486(4) 0.7116(4) 0.048(2) 1.000 . Uani d ?
C(7) -0.280(1) 0.3315(4) 0.6444(3) 0.052(2) 1.000 . Uani d ?
C(8) -0.1902(9) 0.3610(4) 0.5834(3) 0.053(2) 1.000 . Uani d ?
C(9) -0.008(1) 0.4053(4) 0.5901(3) 0.055(2) 1.000 . Uani d ?
C(10) 0.3843(8) 0.2609(4) 1.0000(3) 0.051(2) 1.000 . Uani d ?
C(11) 0.3535(8) 0.1917(5) 1.0482(3) 0.055(2) 1.000 . Uani d ?
C(12) 0.3575(8) 0.1256(4) 0.9419(3) 0.048(2) 1.000 . Uani d ?
H(1) 0.9829 0.7131 0.6613 0.096 1.000 . Uiso c ?
H(2) 0.7538 0.6997 0.6450 0.096 1.000 . Uiso c ?
H(3) 0.8942 0.6111 0.6501 0.096 1.000 . Uiso c ?
H(4) 0.321(6) 0.498(3) 0.618(2) 0.02(1) 1.000 . Uiso d ?
H(5) -0.259(7) 0.333(4) 0.747(3) 0.05(2) 1.000 . Uiso d ?
H(6) -0.396(6) 0.304(3) 0.639(2) 0.02(1) 1.000 . Uiso d ?
H(7) 0.051(7) 0.425(3) 0.553(2) 0.03(1) 1.000 . Uiso d ?
H(8) 0.4065 0.2504 0.8901 0.056 1.000 . Uiso c ?
H(9) 0.3138 0.0472 1.0303 0.057 1.000 . Uiso c ?
H(10) 0.4011 0.3273 1.0099 0.061 1.000 . Uiso c ?
H(11) 0.3450 0.1993 1.0992 0.066 1.000 . Uiso c ?
H(12) 0.3525 0.0794 0.9039 0.058 1.000 . Uiso c ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 12
0 0 -12
-4 0 -4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S(1) V O(1) 87.2(1) . . . yes
S(1) V O(2) 106.4(1) . . . yes
S(1) V O(3) 143.4(1) . . . yes
S(1) V N(2) 76.5(1) . . . yes
O(1) V O(2) 107.2(2) . . . yes
O(1) V O(3) 96.9(2) . . . yes
O(1) V N(2) 151.4(2) . . . yes
O(2) V O(3) 107.0(2) . . . yes
O(2) V N(2) 99.9(2) . . . yes
O(3) V N(2) 83.4(2) . . . yes
V S(1) C(2) 99.9(2) . . . yes
C(1) S(2) C(2) 103.1(3) . . . yes
V O(3) C(5) 133.6(3) . . . yes
N(2) N(1) C(2) 111.8(4) . . . yes
V N(2) N(1) 123.1(3) . . . yes
V N(2) C(3) 125.1(4) . . . yes
N(1) N(2) C(3) 111.2(4) . . . yes
C(10) N(3) C(12) 109.5(4) . . . yes
C(10) N(3) H(8) 125.3 . . . no
C(12) N(3) H(8) 125.3 . . . no
C(11) N(4) C(12) 109.6(5) . . . yes
C(11) N(4) H(9) 125.2 . . . no
C(12) N(4) H(9) 125.2 . . . no
S(2) C(1) H(1) 109.4 . . . no
S(2) C(1) H(2) 109.5 . . . no
S(2) C(1) H(3) 109.4 . . . no
H(1) C(1) H(2) 109.5 . . . no
H(1) C(1) H(3) 109.4 . . . no
H(2) C(1) H(3) 109.5 . . . no
S(1) C(2) S(2) 114.1(3) . . . yes
S(1) C(2) N(1) 125.8(4) . . . yes
S(2) C(2) N(1) 120.1(4) . . . yes
N(2) C(3) C(4) 125.4(5) . . . yes
N(2) C(3) H(4) 119(2) . . . no
C(4) C(3) H(4) 116(2) . . . no
C(3) C(4) C(5) 121.3(5) . . . yes
C(3) C(4) C(9) 119.3(5) . . . yes
C(5) C(4) C(9) 119.3(5) . . . yes
O(3) C(5) C(4) 123.2(5) . . . yes
O(3) C(5) C(6) 119.0(5) . . . yes
C(4) C(5) C(6) 117.8(5) . . . yes
C(5) C(6) C(7) 121.1(6) . . . yes
C(5) C(6) H(5) 121(4) . . . no
C(7) C(6) H(5) 117(4) . . . no
C(6) C(7) C(8) 121.2(6) . . . yes
C(6) C(7) H(6) 121(3) . . . no
C(8) C(7) H(6) 118(3) . . . no
Br C(8) C(7) 120.0(5) . . . yes
Br C(8) C(9) 120.5(5) . . . yes
C(7) C(8) C(9) 119.5(6) . . . yes
C(4) C(9) C(8) 121.1(6) . . . yes
C(4) C(9) H(7) 117(3) . . . no
C(8) C(9) H(7) 122(3) . . . no
N(3) C(10) C(11) 106.8(5) . . . yes
N(3) C(10) H(10) 126.6 . . . no
C(11) C(10) H(10) 126.6 . . . no
N(4) C(11) C(10) 106.5(5) . . . yes
N(4) C(11) H(11) 126.8 . . . no
C(10) C(11) H(11) 126.8 . . . no
N(3) C(12) N(4) 107.7(5) . . . yes
N(3) C(12) H(12) 126.2 . . . no
N(4) C(12) H(12) 126.1 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br C(8) 1.881(6) . . yes
V S(1) 2.364(2) . . yes
V O(1) 1.643(3) . . yes
V O(2) 1.619(3) . . yes
V O(3) 1.888(4) . . yes
V N(2) 2.174(4) . . yes
S(1) C(2) 1.712(6) . . yes
S(2) C(1) 1.784(7) . . yes
S(2) C(2) 1.753(6) . . yes
O(3) C(5) 1.318(5) . . yes
N(1) N(2) 1.401(5) . . yes
N(1) C(2) 1.288(6) . . yes
N(2) C(3) 1.283(6) . . yes
N(3) C(10) 1.342(6) . . yes
N(3) C(12) 1.320(7) . . yes
N(3) H(8) 0.95 . . no
N(4) C(11) 1.360(7) . . yes
N(4) C(12) 1.294(6) . . yes
N(4) H(9) 0.95 . . no
C(1) H(1) 0.95 . . no
C(1) H(2) 0.95 . . no
C(1) H(3) 0.95 . . no
C(3) C(4) 1.446(7) . . yes
C(3) H(4) 0.96(4) . . no
C(4) C(5) 1.405(6) . . yes
C(4) C(9) 1.395(7) . . yes
C(5) C(6) 1.400(7) . . yes
C(6) C(7) 1.355(8) . . yes
C(6) H(5) 0.83(5) . . no
C(7) C(8) 1.367(8) . . yes
C(7) H(6) 0.87(4) . . no
C(8) C(9) 1.364(8) . . yes
C(9) H(7) 0.85(4) . . no
C(10) C(11) 1.337(7) . . yes
C(10) H(10) 0.95 . . no
C(11) H(11) 0.95 . . no
C(12) H(12) 0.95 . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
S(1) C(12) 3.633(6) . 4 no
O(1) N(4) 2.709(5) . 2_557 no
O(1) C(12) 2.969(6) . 4_455 no
O(1) C(10) 3.194(7) . . no
O(1) N(3) 3.381(6) . . no
O(1) N(3) 3.480(6) . 4_455 no
O(1) C(11) 3.520(7) . 2_557 no
O(1) N(4) 3.529(6) . 4_455 no
O(2) N(3) 2.743(5) . . no
O(2) C(6) 3.232(7) . 1_655 no
O(2) C(12) 3.426(7) . 4 no
O(2) C(6) 3.469(7) . 4 no
O(2) C(10) 3.509(7) . . no
O(2) N(3) 3.578(6) . 4 no
O(3) C(12) 3.283(7) . 4_455 no
O(3) N(3) 3.560(6) . 4_455 no
N(1) C(6) 3.470(7) . 1_655 no
N(2) C(6) 3.625(7) . 1_655 no
N(3) N(3) 3.448(3) . 4 no
N(3) N(3) 3.448(3) . 4_455 no
N(3) C(10) 3.476(7) . 4 no
N(3) C(10) 3.636(7) . 4_455 no
N(4) C(10) 3.523(7) . 4_455 no
C(10) C(11) 3.271(8) . 4 no
C(10) C(10) 3.348(2) . 4 no
C(10) C(10) 3.348(2) . 4_455 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Br C(8) C(7) C(6) . . . . -178.5(4) no
Br C(8) C(9) C(4) . . . . 178.1(4) no
V S(1) C(2) S(2) . . . . -169.4(2) no
V S(1) C(2) N(1) . . . . 12.4(5) no
V O(3) C(5) C(4) . . . . -25.4(7) no
V O(3) C(5) C(6) . . . . 156.5(4) no
V N(2) N(1) C(2) . . . . -13.3(6) no
V N(2) C(3) C(4) . . . . 13.1(8) no
S(1) V O(3) C(5) . . . . 88.2(5) no
S(1) V N(2) N(1) . . . . 16.2(3) no
S(1) V N(2) C(3) . . . . -173.5(4) no
S(1) C(2) S(2) C(1) . . . . 177.8(3) no
S(1) C(2) N(1) N(2) . . . . -1.5(7) no
S(2) C(2) N(1) N(2) . . . . -179.6(3) no
O(1) V S(1) C(2) . . . . -168.5(2) no
O(1) V O(3) C(5) . . . . -177.3(4) no
O(1) V N(2) N(1) . . . . 73.1(5) no
O(1) V N(2) C(3) . . . . -116.7(5) no
O(2) V S(1) C(2) . . . . 84.4(2) no
O(2) V O(3) C(5) . . . . -66.9(5) no
O(2) V N(2) N(1) . . . . -88.4(4) no
O(2) V N(2) C(3) . . . . 81.9(4) no
O(3) V S(1) C(2) . . . . -70.8(3) no
O(3) V N(2) N(1) . . . . 165.4(4) no
O(3) V N(2) C(3) . . . . -24.3(4) no
O(3) C(5) C(4) C(3) . . . . -1.2(8) no
O(3) C(5) C(4) C(9) . . . . -176.7(5) no
O(3) C(5) C(6) C(7) . . . . 176.3(5) no
N(1) N(2) C(3) C(4) . . . . -175.6(5) no
N(1) C(2) S(2) C(1) . . . . -3.9(5) no
N(2) V S(1) C(2) . . . . -12.1(2) no
N(2) V O(3) C(5) . . . . 31.5(4) no
N(2) C(3) C(4) C(5) . . . . 4.5(8) no
N(2) C(3) C(4) C(9) . . . . -180.0(5) no
N(3) C(10) C(11) N(4) . . . . -0.3(6) no
N(3) C(12) N(4) C(11) . . . . -0.1(6) no
N(4) C(12) N(3) C(10) . . . . -0.1(6) no
C(2) N(1) N(2) C(3) . . . . 175.2(5) no
C(3) C(4) C(5) C(6) . . . . 177.0(5) no
C(3) C(4) C(9) C(8) . . . . -174.8(5) no
C(4) C(5) C(6) C(7) . . . . -1.9(8) no
C(4) C(9) C(8) C(7) . . . . -2.8(9) no
C(5) C(4) C(9) C(8) . . . . 0.8(8) no
C(5) C(6) C(7) C(8) . . . . 0.0(9) no
C(6) C(5) C(4) C(9) . . . . 1.5(7) no
C(6) C(7) C(8) C(9) . . . . 2.4(9) no
C(10) C(11) N(4) C(12) . . . . 0.3(6) no
C(11) C(10) N(3) C(12) . . . . 0.3(6) no
