#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:59:54 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179224 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/46/4314624.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_4314624
loop_
_publ_author_name
'Pijus K. Sasmal'
'Sounik Saha'
'Ritankar Majumdar'
'Rajan R. Dighe'
'Akhil R. Chakravarty'
_publ_contact_author_address
;Department of Inorganic and Physical Chemistry 
Indian Institute of Science
Bangalore 560 012. INDIA
;
_publ_contact_author_email       arc@ipc.iisc.ernet.in
_publ_contact_author_fax         91-080-23600683
_publ_contact_author_name        'Prof. A. R. Chakravarty'
_publ_contact_author_phone       91-080-22932533
_publ_section_title
;
 Photocytotoxic Oxovanadium(IV) Complexes Showing Light-Induced DNA and
 Protein Cleavage Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              849
_journal_page_last               859
_journal_paper_doi               10.1021/ic900701s
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C28 H31 Cl2 N7 O5 V'
_chemical_formula_sum            'C28 H31 Cl2 N7 O5 V'
_chemical_formula_weight         667.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.664(6)
_cell_angle_beta                 93.486(7)
_cell_angle_gamma                90.775(7)
_cell_formula_units_Z            2
_cell_length_a                   10.411(4)
_cell_length_b                   12.732(5)
_cell_length_c                   12.961(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.894
_cell_measurement_theta_min      0.841
_cell_volume                     1569.3(11)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart CCD Area Detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_sigmaI/netI    0.1725
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15007
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS(Sheldrick,1997)
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.2124
_refine_ls_R_factor_gt           0.1083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1816P)²+1.0894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2656
_refine_ls_wR_factor_ref         0.3309
_reflns_number_gt                2565
_reflns_number_total             5512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900701s_si_002.cif
_cod_data_source_block           arc1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1569.4(10)
_cod_database_code               4314624
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.56059(15) 0.36533(13) 0.30409(12) 0.0355(5) Uani 1 1 d . . .
Cl1 Cl 0.4447(3) -0.0239(2) 0.2248(2) 0.0677(9) Uani 1 1 d . . .
Cl2 Cl 0.9264(4) 0.0423(5) 0.2491(5) 0.152(2) Uani 1 1 d . . .
O1 O 0.5808(6) 0.4953(5) 0.3860(5) 0.0493(17) Uani 1 1 d . . .
N1 N 0.3850(7) 0.3182(6) 0.3504(6) 0.0394(18) Uani 1 1 d . . .
N2 N 0.6239(7) 0.2802(6) 0.4080(6) 0.0412(18) Uani 1 1 d . . .
N3 N 0.4656(6) 0.3819(5) 0.1673(6) 0.0346(17) Uani 1 1 d . . .
N4 N 0.3592(7) 0.3156(6) -0.0006(6) 0.046(2) Uani 1 1 d . . .
H4 H 0.3244 0.2676 -0.0644 0.055 Uiso 1 1 calc R . .
N5 N 0.5442(7) 0.1773(6) 0.1593(6) 0.0439(19) Uani 1 1 d . . .
H5 H 0.5173 0.1286 0.1901 0.053 Uiso 1 1 calc R . .
N6 N 0.7333(7) 0.3443(7) 0.2270(6) 0.0407(18) Uani 1 1 d . . .
N7 N 0.8715(8) 0.2490(7) 0.1026(7) 0.055(2) Uani 1 1 d . . .
H7 H 0.9058 0.1930 0.0507 0.066 Uiso 1 1 calc R . .
C1 C 0.2651(9) 0.3358(9) 0.3207(8) 0.057(3) Uani 1 1 d . . .
H1 H 0.2555 0.3759 0.2747 0.068 Uiso 1 1 calc R . .
C2 C 0.1553(11) 0.3005(11) 0.3515(10) 0.078(4) Uani 1 1 d . . .
H2 H 0.0741 0.3156 0.3279 0.094 Uiso 1 1 calc R . .
C3 C 0.1718(10) 0.2396(11) 0.4214(9) 0.070(3) Uani 1 1 d . . .
H3 H 0.0999 0.2143 0.4455 0.084 Uiso 1 1 calc R . .
C4 C 0.2926(10) 0.2175(8) 0.4541(8) 0.053(3) Uani 1 1 d . . .
C5 C 0.3194(12) 0.1581(8) 0.5282(8) 0.062(3) Uani 1 1 d . . .
H5A H 0.2513 0.1315 0.5556 0.075 Uiso 1 1 calc R . .
C6 C 0.4405(13) 0.1410(9) 0.5574(9) 0.066(3) Uani 1 1 d . . .
H6 H 0.4539 0.1034 0.6053 0.079 Uiso 1 1 calc R . .
C7 C 0.5493(10) 0.1783(8) 0.5176(8) 0.049(3) Uani 1 1 d . . .
C8 C 0.6764(12) 0.1623(9) 0.5439(9) 0.063(3) Uani 1 1 d . . .
H8 H 0.6956 0.1223 0.5888 0.076 Uiso 1 1 calc R . .
C9 C 0.7715(12) 0.2041(11) 0.5049(10) 0.078(4) Uani 1 1 d . . .
H9 H 0.8567 0.1938 0.5235 0.094 Uiso 1 1 calc R . .
C10 C 0.7439(10) 0.2634(9) 0.4364(8) 0.059(3) Uani 1 1 d . . .
H10 H 0.8116 0.2918 0.4099 0.071 Uiso 1 1 calc R . .
C11 C 0.5269(9) 0.2396(7) 0.4487(7) 0.040(2) Uani 1 1 d . . .
C12 C 0.3989(8) 0.2584(7) 0.4177(7) 0.036(2) Uani 1 1 d . . .
C13 C 0.4248(8) 0.4753(7) 0.1459(7) 0.033(2) Uani 1 1 d . . .
C14 C 0.4403(9) 0.5893(8) 0.2078(8) 0.050(3) Uani 1 1 d . . .
H14 H 0.4842 0.6173 0.2789 0.060 Uiso 1 1 calc R . .
C15 C 0.3896(10) 0.6643(8) 0.1634(9) 0.055(3) Uani 1 1 d . . .
H15 H 0.4008 0.7431 0.2047 0.066 Uiso 1 1 calc R . .
C16 C 0.3225(10) 0.6222(10) 0.0577(10) 0.060(3) Uani 1 1 d . . .
H16 H 0.2893 0.6740 0.0300 0.072 Uiso 1 1 calc R . .
C17 C 0.3036(9) 0.5065(9) -0.0071(8) 0.049(3) Uani 1 1 d . . .
H17 H 0.2576 0.4786 -0.0772 0.059 Uiso 1 1 calc R . .
C18 C 0.3578(8) 0.4331(8) 0.0390(7) 0.039(2) Uani 1 1 d . . .
C19 C 0.4251(9) 0.2888(8) 0.0785(8) 0.042(2) Uani 1 1 d . . .
C20 C 0.4452(9) 0.1721(7) 0.0699(7) 0.045(2) Uani 1 1 d . . .
H20A H 0.4737 0.1250 -0.0039 0.054 Uiso 1 1 calc R . .
H20B H 0.3652 0.1381 0.0793 0.054 Uiso 1 1 calc R . .
C21 C 0.8512(10) 0.5345(11) 0.2941(9) 0.066(3) Uani 1 1 d . . .
H21 H 0.7942 0.5746 0.3474 0.079 Uiso 1 1 calc R . .
C22 C 0.9612(12) 0.5906(12) 0.2754(11) 0.087(4) Uani 1 1 d . . .
H22 H 0.9751 0.6693 0.3156 0.104 Uiso 1 1 calc R . .
C23 C 1.0481(12) 0.5295(13) 0.1978(12) 0.086(4) Uani 1 1 d . . .
H23 H 1.1203 0.5678 0.1886 0.103 Uiso 1 1 calc R . .
C24 C 1.0295(10) 0.4156(12) 0.1356(11) 0.075(4) Uani 1 1 d . . .
H24 H 1.0866 0.3757 0.0823 0.090 Uiso 1 1 calc R . .
C25 C 0.9202(10) 0.3582(10) 0.1535(9) 0.055(3) Uani 1 1 d . . .
C26 C 0.8329(9) 0.4183(9) 0.2299(8) 0.044(2) Uani 1 1 d . . .
C27 C 0.7602(9) 0.2435(8) 0.1475(8) 0.046(2) Uani 1 1 d . . .
C28 C 0.6748(9) 0.1428(8) 0.1179(9) 0.057(3) Uani 1 1 d . . .
H28A H 0.7109 0.0929 0.1514 0.069 Uiso 1 1 calc R . .
H28B H 0.6672 0.1005 0.0366 0.069 Uiso 1 1 calc R . .
OW1 O 0.2885(8) 0.1392(7) -0.2049(6) 0.093(3) Uani 1 1 d . . .
OW2 O 1.1060(9) 0.1249(9) 0.0174(9) 0.127(4) Uani 1 1 d . . .
OW4 O 1.1666(12) -0.0294(14) 0.1259(10) 0.197(7) Uani 1 1 d . . .
OW3 O 0.9907(10) -0.0848(11) 0.3709(17) 0.210(8) Uani 1 1 d . . .
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'
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 N3 99.7(3) . . ?
O1 V1 N6 98.7(3) . . ?
N3 V1 N6 90.6(3) . . ?
O1 V1 N1 102.7(3) . . ?
N3 V1 N1 90.3(3) . . ?
N6 V1 N1 158.1(3) . . ?
O1 V1 N2 102.6(3) . . ?
N3 V1 N2 156.5(3) . . ?
N6 V1 N2 93.1(3) . . ?
N1 V1 N2 77.8(3) . . ?
O1 V1 N5 171.1(3) . . ?
N3 V1 N5 74.8(3) . . ?
N6 V1 N5 74.7(3) . . ?
N1 V1 N5 84.4(3) . . ?
N2 V1 N5 83.8(3) . . ?
C1 N1 C12 116.9(8) . . ?
C1 N1 V1 129.0(6) . . ?
C12 N1 V1 114.1(6) . . ?
C10 N2 C11 118.2(8) . . ?
C10 N2 V1 127.9(7) . . ?
C11 N2 V1 113.9(6) . . ?
C19 N3 C13 106.8(7) . . ?
C19 N3 V1 119.3(5) . . ?
C13 N3 V1 133.8(6) . . ?
C19 N4 C18 107.9(7) . . ?
C19 N4 H4 126.0 . . ?
C18 N4 H4 126.0 . . ?
C20 N5 C28 114.2(7) . . ?
C20 N5 V1 109.6(5) . . ?
C28 N5 V1 109.2(5) . . ?
C20 N5 H5 107.9 . . ?
C28 N5 H5 107.9 . . ?
V1 N5 H5 107.9 . . ?
C27 N6 C26 104.8(8) . . ?
C27 N6 V1 120.7(6) . . ?
C26 N6 V1 134.1(7) . . ?
C27 N7 C25 107.8(8) . . ?
C27 N7 H7 126.1 . . ?
C25 N7 H7 126.1 . . ?
N1 C1 C2 126.0(10) . . ?
N1 C1 H1 117.0 . . ?
C2 C1 H1 117.0 . . ?
C1 C2 C3 116.2(10) . . ?
C1 C2 H2 121.9 . . ?
C3 C2 H2 121.9 . . ?
C4 C3 C2 120.8(10) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C12 118.1(9) . . ?
C3 C4 C5 124.8(10) . . ?
C12 C4 C5 117.1(10) . . ?
C6 C5 C4 121.2(10) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C5 C6 C7 122.4(10) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C8 C7 C11 117.0(9) . . ?
C8 C7 C6 125.1(10) . . ?
C11 C7 C6 117.9(10) . . ?
C9 C8 C7 120.2(10) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 120.5(11) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
N2 C10 C9 121.7(11) . . ?
N2 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N2 C11 C7 122.5(9) . . ?
N2 C11 C12 117.5(8) . . ?
C7 C11 C12 120.0(8) . . ?
N1 C12 C4 122.0(8) . . ?
N1 C12 C11 116.6(7) . . ?
C4 C12 C11 121.4(8) . . ?
C14 C13 N3 131.5(8) . . ?
C14 C13 C18 120.5(8) . . ?
N3 C13 C18 108.0(7) . . ?
C13 C14 C15 118.9(9) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 120.5(10) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 122.2(9) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C18 116.0(9) . . ?
C16 C17 H17 122.0 . . ?
C18 C17 H17 122.0 . . ?
N4 C18 C13 106.0(7) . . ?
N4 C18 C17 132.1(9) . . ?
C13 C18 C17 121.9(9) . . ?
N3 C19 N4 111.3(8) . . ?
N3 C19 C20 123.6(8) . . ?
N4 C19 C20 125.0(8) . . ?
C19 C20 N5 108.7(7) . . ?
C19 C20 H20A 110.0 . . ?
N5 C20 H20A 110.0 . . ?
C19 C20 H20B 110.0 . . ?
N5 C20 H20B 110.0 . . ?
H20A C20 H20B 108.3 . . ?
C26 C21 C22 117.2(11) . . ?
C26 C21 H21 121.4 . . ?
C22 C21 H21 121.4 . . ?
C23 C22 C21 121.1(13) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C22 121.2(12) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 118.4(12) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
N7 C25 C26 106.1(9) . . ?
N7 C25 C24 132.9(10) . . ?
C26 C25 C24 120.8(11) . . ?
C21 C26 N6 129.4(9) . . ?
C21 C26 C25 121.3(10) . . ?
N6 C26 C25 109.2(9) . . ?
N6 C27 N7 111.9(8) . . ?
N6 C27 C28 121.3(8) . . ?
N7 C27 C28 126.8(9) . . ?
C27 C28 N5 110.5(8) . . ?
C27 C28 H28A 109.6 . . ?
N5 C28 H28A 109.6 . . ?
C27 C28 H28B 109.6 . . ?
N5 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.570(6) . ?
V1 N3 2.064(7) . ?
V1 N6 2.079(7) . ?
V1 N1 2.111(7) . ?
V1 N2 2.123(7) . ?
V1 N5 2.372(7) . ?
N1 C1 1.332(11) . ?
N1 C12 1.372(10) . ?
N2 C10 1.326(11) . ?
N2 C11 1.354(11) . ?
N3 C19 1.320(10) . ?
N3 C13 1.391(10) . ?
N4 C19 1.357(11) . ?
N4 C18 1.373(11) . ?
N4 H4 0.8600 . ?
N5 C20 1.483(10) . ?
N5 C28 1.499(11) . ?
N5 H5 0.9100 . ?
N6 C27 1.330(11) . ?
N6 C26 1.380(11) . ?
N7 C27 1.341(11) . ?
N7 C25 1.352(12) . ?
N7 H7 0.8600 . ?
C1 C2 1.362(14) . ?
C1 H1 0.9300 . ?
C2 C3 1.414(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.372(15) . ?
C3 H3 0.9300 . ?
C4 C12 1.401(12) . ?
C4 C5 1.459(14) . ?
C5 C6 1.340(15) . ?
C5 H5A 0.9300 . ?
C6 C7 1.423(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.384(14) . ?
C7 C11 1.415(12) . ?
C8 C9 1.335(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.398(15) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.421(12) . ?
C13 C14 1.348(12) . ?
C13 C18 1.404(11) . ?
C14 C15 1.393(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.391(14) . ?
C15 H15 0.9300 . ?
C16 C17 1.376(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.404(12) . ?
C17 H17 0.9300 . ?
C19 C20 1.464(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C26 1.380(14) . ?
C21 C22 1.425(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.391(17) . ?
C22 H22 0.9300 . ?
C23 C24 1.351(16) . ?
C23 H23 0.9300 . ?
C24 C25 1.425(14) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(12) . ?
C27 C28 1.455(13) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
