#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/76/4327656.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_4327656
loop_
_publ_author_name
'Subodh Kanti Dutta'
'Satyabrata Samanta'
'Sujit Baran Kumar'
'Oc Hee Han'
'Pannee Burckel'
'A. Alan Pinkerton'
'Muktimoy Chaudhury'
_publ_contact_author
;
     A.A. Pinkerton
     Department of Chemistry
     University of Toledo
     Toledo
     OH 43606
     USA
;
_publ_contact_author_email       APinker@UofT02.UTOLEDO.EDU
_publ_contact_author_fax         '(419) 530 4033'
_publ_contact_author_phone       '(419) 530 4580'
_publ_section_title
;
 Mixed-Oxidation Divanadium(IV,V) Compound with Ligand Asymmetry:
 Electronic and Molecular Structure in Solution and in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1982
_journal_page_last               1988
_journal_paper_doi               10.1021/ic980743+
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        'crystallized from acetone-toluene'
_chemical_formula_structural     (ImH)[L1OV-(mue-O)-VOL2].(CH3)2CO.H2O
_chemical_formula_sum            'C24 H28 Br N6 O7 S4 V2'
_chemical_formula_weight         822.58
_chemical_name_systematic        ?
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_type_scat_source           International_Tables_for_Xray_Crystallography
_audit_creation_date             14-07-98
_audit_creation_method           from_MolEN_master_file_using_cif_in
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.740(2)
_cell_length_b                   18.912(4)
_cell_length_c                   17.163(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(1)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     3486.1(13)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294(1)
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       θ/θ
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  na
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3850
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.08
_diffrn_standards_decay_%        1.84
_diffrn_standards_interval_time  50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.931
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.8137
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.57
_exptl_crystal_description       'multifaceted, isotropic'
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.28
_refine_ls_abs_structure_details
;
?
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.810
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.118
_refine_ls_R_factor_obs          0.065
_refine_ls_shift/esd_max         0.081
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo²/ (σ²(Fo²) + 0.0016 Fo⁴)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.087
_reflns_number_observed          2119
_reflns_number_total             3850
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic9807432B.cif
_cod_data_source_block           Vpnma
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w = 4Fo^2^/
(\s^2^(Fo^2^) + 0.0016 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3486(2)
_cod_original_formula_sum        'C24 H28 Br1 N6 O7 S4 V2'
_cod_database_code               4327656
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x, -y+1/2, z'
'x+1/2, y, -z+1/2'
'-x, -y, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
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
BR 0.7730(1) -0.10209(8) 0.29260(8) 0.0741(4) Uani ?
V 1.1062(1) 0.15806(5) 0.04183(6) 0.0552(3) Uani ?
S1 1.2972(2) 0.1520(1) -0.0233(1) 0.0786(6) Uani ?
S2 1.4176(2) 0.0318(1) -0.0989(1) 0.0888(6) Uani ?
O1 1.1368(6) 0.2500 0.0615(3) 0.066(2) Uani ?
O2 0.9965(4) 0.1556(2) -0.0203(2) 0.072(1) Uani ?
O3 1.0409(4) 0.1453(2) 0.1436(2) 0.066(1) Uani ?
O4 0.835(1) 0.271(1) -0.1636(5) 0.173(7) Uani ?
O5 1.3770(9) -0.2500 -0.2539(4) 0.108(3) Uani ?
N1 1.1439(4) 0.0488(3) 0.0482(3) 0.055(1) Uani ?
N2 1.2304(5) 0.0157(3) -0.0019(3) 0.064(2) Uani ?
N3 1.2426(9) -0.258(1) 0.0106(5) 0.118(4) Uani ?
N4 1.3310(7) -0.245(1) -0.1004(4) 0.066(2) Uani ?
C1 0.9761(6) 0.0902(4) 0.1737(3) 0.065(2) Uani ?
C2 0.8902(6) 0.1033(4) 0.2350(4) 0.085(2) Uani ?
C3 0.8261(6) 0.0463(4) 0.2694(4) 0.092(2) Uani ?
C4 0.8448(7) -0.0223(4) 0.2423(4) 0.089(2) Uani ?
C5 0.9270(6) -0.0354(4) 0.1820(4) 0.078(2) Uani ?
C6 0.9919(6) 0.0214(3) 0.1465(3) 0.060(2) Uani ?
C7 1.0811(5) 0.0034(3) 0.0877(3) 0.059(2) Uani ?
C8 1.3025(6) 0.0620(3) -0.0354(3) 0.064(2) Uani ?
C9 1.3983(8) -0.0624(4) -0.0933(5) 0.103(3) Uani ?
C10 1.420(1) -0.241(1) -0.0442(6) 0.087(4) Uani ?
C11 1.362(1) -0.262(1) 0.0236(7) 0.092(4) Uani ?
C12 1.221(1) -0.261(1) -0.0639(6) 0.081(4) Uani ?
C13 0.916(1) 0.262(1) -0.2112(7) 0.135(6) Uani ?
C14 1.050(2) 0.2500 -0.1871(9) 0.159(7) Uani ?
C15 0.902(2) 0.285(1) -0.2946(8) 0.18(1) Uani ?
H1 0.8762 0.1502 0.2528 0.1110 Uiso calc
H2 0.7699 0.0547 0.3111 0.1190 Uiso calc
H3 0.9400 -0.0825 0.1644 0.1013 Uiso calc
H4 1.0947 -0.0453 0.0773 0.0764 Uiso calc
H5 1.4574 -0.0848 -0.1263 0.1343 Uiso calc
H6 1.4107 -0.0775 -0.0411 0.1343 Uiso calc
H7 1.3166 -0.0746 -0.1096 0.1343 Uiso calc
H8 1.5063 -0.2318 -0.0516 0.1160 Uiso calc
H9 1.4011 -0.2668 0.0730 0.1167 Uiso calc
H10 1.1801 -0.2575 0.0498 0.0870 Uiso calc
H11 1.1443 -0.2725 -0.0883 0.1085 Uiso calc
H12 1.3428 -0.2370 -0.1546 0.1298 Uiso calc
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
S1 V O1 88.7(2)
S1 V O2 109.1(2)
S1 V O3 139.3(1)
S1 V N1 79.0(1)
O1 V O2 106.8(2)
O1 V O3 91.0(2)
O1 V N1 154.3(2)
O2 V O3 109.9(2)
O2 V N1 98.5(2)
O3 V N1 84.2(2)
V S1 C8 97.8(2)
C8 S2 C9 102.1(4)
V O3 C1 129.7(4)
V N1 N2 121.9(3)
V N1 C7 125.6(4)
N2 N1 C7 111.8(5)
N1 N2 C8 111.2(5)
C11 N3 C12 1091(1)
C11 N3 H10 124.99
C12 N3 H10 124.77
C10 N4 C12 107.1(8)
C10 N4 H12 126.32
C12 N4 H12 126.56
O3 C1 C2 118.8(6)
O3 C1 C6 121.9(5)
C2 C1 C6 119.4(6)
C1 C2 C3 119.6(7)
C1 C2 H1 120.22
C3 C2 H1 120.23
C2 C3 C4 120.2(7)
C2 C3 H2 119.87
C4 C3 H2 119.90
BR C4 C3 122.0(5)
BR C4 C5 117.1(6)
C3 C4 C5 120.6(7)
C4 C5 C6 119.9(7)
C4 C5 H3 120.04
C6 C5 H3 120.05
C1 C6 C5 120.3(6)
C1 C6 C7 122.7(6)
C5 C6 C7 116.8(6)
N1 C7 C6 124.3(6)
N1 C7 H4 117.87
C6 C7 H4 117.87
C7 C7 H4 999.99
S1 C8 S2 115.1(4)
S1 C8 N2 126.4(5)
S2 C8 N2 118.5(5)
S2 C9 H5 109.47
S2 C9 H6 109.51
S2 C9 H7 109.43
H5 C9 H6 109.47
H5 C9 H7 109.47
H6 C9 H7 109.47
N4 C10 C11 105(1)
N4 C10 H8 126.95
C11 C10 H8 127.12
N3 C11 C10 106(1)
N3 C11 H9 126.43
C10 C11 H9 125.49
N3 C12 N4 1061(1)
N3 C12 H11 126.79
N4 C12 H11 126.63
O4 C13 C14 122(1)
O4 C13 C15 122(2)
C14 C13 C15 114(1)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
BR C4 1.902(8)
V S1 2.339(2)
V O1 1.801(2)
V O2 1.590(4)
V O3 1.898(4)
V N1 2.109(5)
S1 C8 1.716(7)
S2 C8 1.745(6)
S2 C9 1.795(8)
O3 C1 1.355(8)
O4 C13 1.21(2)
N1 N2 1.413(7)
N1 C7 1.286(8)
N2 C8 1.302(8)
N3 C11 1.30(2)
N3 C12 1.30(1)
N3 H10 0.9500
N4 C10 1.36(1)
N4 C12 1.37(1)
N4 H12 0.9500
C1 C2 1.421(9)
C1 C6 1.392(9)
C2 C3 1.41(1)
C2 H1 0.9500
C3 C4 1.39(1)
C3 H2 0.9500
C4 C5 1.38(1)
C5 C6 1.419(9)
C5 H3 0.9500
C6 C7 1.433(8)
C7 H4 0.9500
C9 H5 0.9500
C9 H6 0.9500
C9 H7 0.9500
C10 C11 1.38(2)
C10 H8 0.9500
C11 H9 0.9500
C12 H11 0.9500
C13 C14 1.52(2)
C13 C15 1.50(2)
