#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:08:17 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179715 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/17/7001775.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_7001775
loop_
_publ_author_name
'Pattanayak, Poulami'
'Pratihar, Jahar Lal'
'Patra, Debprasad'
'Mitra, Soham'
'Bhattacharyya, Arindam'
'Man Lee, Hon'
'Chattopadhyay, Surajit'
_publ_section_title
;
 Synthesis, structure and reactivity of azosalophen complexes of
 vanadium(IV): studies on cytotoxic properties
;
_journal_issue                   31
_journal_name_full               'Dalton Transactions'
_journal_page_first              6220
_journal_paper_doi               10.1039/b903352a
_journal_year                    2009
_chemical_formula_moiety         'C19 H15 N3 O4 V'
_chemical_formula_sum            'C19 H15 N3 O4 V'
_chemical_formula_weight         400.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.807(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.149(2)
_cell_length_b                   11.6449(14)
_cell_length_c                   12.0062(14)
_cell_measurement_temperature    150(2)
_cell_volume                     1656.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_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  0.0824
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19714
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.9453
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0430P)²+0.2526P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                2840
_reflns_number_total             4269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903352a.txt
_cod_data_source_block           s1v
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001775
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
H1B H 0.418(3) 0.423(3) 0.022(3) 0.047(10) Uiso 1 1 d . . .
H1A H 0.475(3) 0.364(3) 0.118(3) 0.048(10) Uiso 1 1 d . . .
C12 C 0.40488(19) 0.43015(18) 0.35787(18) 0.0169(5) Uani 1 1 d . . .
C7 C 0.29654(19) 0.46197(19) 0.29854(18) 0.0174(5) Uani 1 1 d . . .
C8 C 0.2011(2) 0.4248(2) 0.3339(2) 0.0233(5) Uani 1 1 d . . .
H8 H 0.1280 0.4451 0.2917 0.028 Uiso 1 1 calc R . .
C9 C 0.2134(2) 0.3584(2) 0.4307(2) 0.0255(6) Uani 1 1 d . . .
H9 H 0.1486 0.3333 0.4558 0.031 Uiso 1 1 calc R . .
C10 C 0.3207(2) 0.32807(19) 0.49174(19) 0.0221(5) Uani 1 1 d . . .
H10 H 0.3284 0.2832 0.5591 0.027 Uiso 1 1 calc R . .
C11 C 0.4153(2) 0.36195(19) 0.45606(18) 0.0192(5) Uani 1 1 d . . .
H11 H 0.4879 0.3393 0.4978 0.023 Uiso 1 1 calc R . .
C13 C 0.59907(19) 0.43650(18) 0.35201(18) 0.0174(5) Uani 1 1 d . . .
H13 H 0.6112 0.3822 0.4126 0.021 Uiso 1 1 calc R . .
C14 C 0.69535(19) 0.47276(19) 0.31157(18) 0.0184(5) Uani 1 1 d . . .
C15 C 0.8012(2) 0.43646(19) 0.37549(19) 0.0217(5) Uani 1 1 d . . .
H15 H 0.8042 0.3903 0.4413 0.026 Uiso 1 1 calc R . .
C16 C 0.9001(2) 0.4658(2) 0.3455(2) 0.0247(5) Uani 1 1 d . . .
H16 H 0.9708 0.4419 0.3907 0.030 Uiso 1 1 calc R . .
C17 C 0.8947(2) 0.5317(2) 0.2470(2) 0.0251(5) Uani 1 1 d . . .
H17 H 0.9625 0.5516 0.2247 0.030 Uiso 1 1 calc R . .
C18 C 0.7934(2) 0.56814(19) 0.1823(2) 0.0217(5) Uani 1 1 d . . .
H18 H 0.7924 0.6119 0.1153 0.026 Uiso 1 1 calc R . .
C19 C 0.69102(19) 0.54221(19) 0.21269(19) 0.0183(5) Uani 1 1 d . . .
C1 C 0.18058(19) 0.62673(19) 0.04692(18) 0.0187(5) Uani 1 1 d . . .
C6 C 0.0671(2) 0.6530(2) -0.0035(2) 0.0227(5) Uani 1 1 d . . .
H6 H 0.0092 0.6258 0.0315 0.027 Uiso 1 1 calc R . .
C5 C 0.0381(2) 0.7166(2) -0.1012(2) 0.0267(6) Uani 1 1 d . . .
H5 H -0.0386 0.7350 -0.1331 0.032 Uiso 1 1 calc R . .
C4 C 0.1242(2) 0.7544(2) -0.1537(2) 0.0240(5) Uani 1 1 d . . .
H4 H 0.1049 0.7978 -0.2223 0.029 Uiso 1 1 calc R . .
C3 C 0.2349(2) 0.73001(19) -0.10844(19) 0.0197(5) Uani 1 1 d . . .
H3 H 0.2907 0.7565 -0.1465 0.024 Uiso 1 1 calc R . .
C2 C 0.26870(19) 0.66634(19) -0.00634(18) 0.0172(5) Uani 1 1 d . . .
N3 N 0.49645(16) 0.47138(15) 0.31313(15) 0.0161(4) Uani 1 1 d . . .
N2 N 0.29198(16) 0.53547(16) 0.20195(15) 0.0174(4) Uani 1 1 d . . .
N1 N 0.19366(16) 0.55841(16) 0.14378(16) 0.0204(4) Uani 1 1 d . . .
O1 O 0.59641(13) 0.58132(13) 0.14756(12) 0.0197(3) Uani 1 1 d . . .
O2 O 0.37633(13) 0.64689(13) 0.03307(12) 0.0191(3) Uani 1 1 d . . .
O3 O 0.42624(15) 0.41476(16) 0.08797(16) 0.0217(4) Uani 1 1 d . . .
O4 O 0.45735(14) 0.70451(13) 0.26423(13) 0.0224(4) Uani 1 1 d . . .
V V 0.44893(3) 0.59179(3) 0.18496(3) 0.01607(11) 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'
V V 0.3005 0.5294 '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'
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
C7 C12 C11 118.4(2) . . ?
C7 C12 N3 116.38(19) . . ?
C11 C12 N3 125.2(2) . . ?
C8 C7 C12 121.1(2) . . ?
C8 C7 N2 123.3(2) . . ?
C12 C7 N2 115.66(19) . . ?
C9 C8 C7 119.5(2) . . ?
C8 C9 C10 120.1(2) . . ?
C11 C10 C9 121.0(2) . . ?
C10 C11 C12 120.0(2) . . ?
N3 C13 C14 125.5(2) . . ?
C15 C14 C13 116.4(2) . . ?
C15 C14 C19 118.9(2) . . ?
C13 C14 C19 124.7(2) . . ?
C16 C15 C14 122.0(2) . . ?
C15 C16 C17 118.6(2) . . ?
C18 C17 C16 121.2(2) . . ?
C17 C18 C19 121.5(2) . . ?
O1 C19 C18 118.5(2) . . ?
O1 C19 C14 123.7(2) . . ?
C18 C19 C14 117.8(2) . . ?
N1 C1 C6 113.78(19) . . ?
N1 C1 C2 126.7(2) . . ?
C6 C1 C2 119.5(2) . . ?
C5 C6 C1 121.8(2) . . ?
C6 C5 C4 118.6(2) . . ?
C3 C4 C5 121.4(2) . . ?
C4 C3 C2 121.8(2) . . ?
O2 C2 C3 118.7(2) . . ?
O2 C2 C1 124.5(2) . . ?
C3 C2 C1 116.8(2) . . ?
C13 N3 C12 121.93(19) . . ?
C13 N3 V 124.63(15) . . ?
C12 N3 V 113.42(14) . . ?
N1 N2 C7 115.68(18) . . ?
N1 N2 V 130.81(15) . . ?
C7 N2 V 113.46(14) . . ?
N2 N1 C1 119.97(19) . . ?
C19 O1 V 127.64(14) . . ?
C2 O2 V 127.16(13) . . ?
O4 V O1 104.26(8) . . ?
O4 V O2 103.93(7) . . ?
O1 V O2 93.07(6) . . ?
O4 V N3 98.17(8) . . ?
O1 V N3 90.56(7) . . ?
O2 V N3 155.95(7) . . ?
O4 V N2 98.00(8) . . ?
O1 V N2 156.81(7) . . ?
O2 V N2 87.75(7) . . ?
N3 V N2 79.80(7) . . ?
O4 V O3 172.28(7) . . ?
O1 V O3 81.01(6) . . ?
O2 V O3 81.17(7) . . ?
N3 V O3 75.93(7) . . ?
N2 V O3 76.21(7) . . ?
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
C12 C7 1.400(3) . ?
C12 C11 1.404(3) . ?
C12 N3 1.422(3) . ?
C7 C8 1.389(3) . ?
C7 N2 1.433(3) . ?
C8 C9 1.375(3) . ?
C9 C10 1.392(3) . ?
C10 C11 1.371(3) . ?
C13 N3 1.296(3) . ?
C13 C14 1.426(3) . ?
C14 C15 1.408(3) . ?
C14 C19 1.428(3) . ?
C15 C16 1.371(3) . ?
C16 C17 1.399(3) . ?
C17 C18 1.369(3) . ?
C18 C19 1.404(3) . ?
C19 O1 1.320(3) . ?
C1 N1 1.389(3) . ?
C1 C6 1.411(3) . ?
C1 C2 1.439(3) . ?
C6 C5 1.366(3) . ?
C5 C4 1.406(3) . ?
C4 C3 1.364(3) . ?
C3 C2 1.413(3) . ?
C2 O2 1.308(3) . ?
N3 V 2.0673(18) . ?
N2 N1 1.271(3) . ?
N2 V 2.0689(19) . ?
O1 V 1.9452(15) . ?
O2 V 1.9499(15) . ?
O3 V 2.3537(17) . ?
O4 V 1.6112(16) . ?
