#------------------------------------------------------------------------------
#$Date: 2015-09-30 09:24:48 +0300 (Wed, 30 Sep 2015) $
#$Revision: 159057 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/23/7222357.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_7222357
loop_
_publ_author_name
'Adach, Anna'
'Daszkiewicz, Marek'
'Tyszka-Czochara, Małgorzata'
'Barszcz, Boleslaw'
_publ_section_title
;
 New oxovanadium(IV) complexes with pincer ligand obtained in situ:
 experimental and theoretical studies on the structure, spectroscopic
 properties and antitumour activity.
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA12561H
_journal_year                    2015
_chemical_formula_moiety         'C14 H19 N7 O S2 V, C7 H8'
_chemical_formula_sum            'C21 H27 N7 O S2 V'
_chemical_formula_weight         508.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-06-19 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.466(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.7159(7)
_cell_length_b                   16.2503(12)
_cell_length_c                   10.3876(8)
_cell_measurement_reflns_used    1578
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.98
_cell_volume                     1266.65(18)
_computing_cell_refinement       'CrysAlis 1.171.32.6'
_computing_data_collection       'CrysAlis 1.171.32.6'
_computing_data_reduction        'CrysAlis 1.171.33.42'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11488
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis 1.171.33.42'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0596P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1578
_reflns_number_total             2403
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra12561h1.cif
_cod_data_source_block           g-1
_cod_database_code               7222357
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
V1 V 0.25519(8) 0.2500 0.94126(6) 0.0486(2) Uani 1 2 d S T P
S2 S 0.28025(13) 0.04300(5) 0.61874(9) 0.0871(3) Uani 1 1 d . . .
O1 O 0.4483(3) 0.2500 1.0358(3) 0.0652(7) Uani 1 2 d S T P
N1 N -0.0466(4) 0.2500 0.8290(3) 0.0472(7) Uani 1 2 d S T P
H1 H -0.0495 0.2500 0.7342 0.057 Uiso 1 2 calc R U P
N2 N 0.2762(3) 0.16245(14) 0.8072(2) 0.0625(6) Uani 1 1 d . . .
N11 N -0.0456(3) 0.14544(12) 0.98938(19) 0.0487(5) Uani 1 1 d . . .
N12 N 0.1312(2) 0.16210(13) 1.04033(18) 0.0482(5) Uani 1 1 d . . .
C2 C 0.2777(3) 0.11291(16) 0.7280(3) 0.0521(7) Uani 1 1 d . . .
C13 C 0.1744(3) 0.11987(15) 1.1543(2) 0.0485(6) Uani 1 1 d . . .
C14 C 0.0264(4) 0.07618(17) 1.1717(3) 0.0592(7) Uani 1 1 d . . .
H14 H 0.0215 0.0421 1.2427 0.071 Uiso 1 1 calc R U .
C15 C -0.1103(3) 0.09258(16) 1.0652(3) 0.0532(7) Uani 1 1 d . . .
C16 C 0.3541(4) 0.1243(2) 1.2442(3) 0.0716(8) Uani 1 1 d . . .
H16A H 0.4086 0.1760 1.2319 0.107 Uiso 0.5 1 calc R U P
H16B H 0.4263 0.0801 1.2246 0.107 Uiso 0.5 1 calc R U P
H16C H 0.3439 0.1199 1.3343 0.107 Uiso 0.5 1 calc R U P
H16D H 0.3772 0.0747 1.2953 0.107 Uiso 0.5 1 calc R U P
H16E H 0.3596 0.1706 1.3026 0.107 Uiso 0.5 1 calc R U P
H16F H 0.4420 0.1307 1.1929 0.107 Uiso 0.5 1 calc R U P
C17 C -0.2993(3) 0.0625(2) 1.0285(3) 0.0756(9) Uani 1 1 d . . .
H17A H -0.3473 0.0709 0.9356 0.113 Uiso 0.5 1 calc R U P
H17B H -0.3692 0.0923 1.0781 0.113 Uiso 0.5 1 calc R U P
H17C H -0.3022 0.0049 1.0484 0.113 Uiso 0.5 1 calc R U P
H17D H -0.3318 0.0412 1.1058 0.113 Uiso 0.5 1 calc R U P
H17E H -0.3099 0.0197 0.9633 0.113 Uiso 0.5 1 calc R U P
H17F H -0.3770 0.1072 0.9930 0.113 Uiso 0.5 1 calc R U P
C18 C -0.1282(4) 0.17348(18) 0.8562(3) 0.0654(8) Uani 1 1 d . . .
H18A H -0.1135 0.1320 0.7924 0.079 Uiso 1 1 calc R U .
H18B H -0.2548 0.1818 0.8480 0.079 Uiso 1 1 calc R U .
C21 C -0.1029(5) 0.2500 0.4747(4) 0.0590(10) Uani 1 2 d S T P
C22 C -0.1815(4) 0.1775(2) 0.4969(3) 0.0726(8) Uani 1 1 d . . .
H22 H -0.1299 0.1278 0.4818 0.087 Uiso 1 1 calc R U .
C23 C -0.3361(5) 0.1774(3) 0.5414(3) 0.0949(12) Uani 1 1 d . . .
H23 H -0.3877 0.1277 0.5565 0.114 Uiso 1 1 calc R U .
C24 C -0.4146(6) 0.2500 0.5635(5) 0.108(2) Uani 1 2 d S T P
H24 H -0.5195 0.2500 0.5930 0.129 Uiso 1 2 calc R U P
C25 C 0.0648(7) 0.2500 0.4245(5) 0.0926(15) Uani 1 2 d S T P
H25A H 0.0181 0.2500 0.3293 0.139 Uiso 1 2 d S U P
H25B H 0.1295 0.2015 0.4515 0.139 Uiso 1 1 d . U .
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'
S S 0.1246 0.1234 '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
O1 V1 N2 102.27(9) . .
O1 V1 N2 102.27(9) . 4_565
N2 V1 N2 89.35(12) . 4_565
O1 V1 N12 99.52(9) . .
N2 V1 N12 88.73(8) . .
N2 V1 N12 158.03(9) 4_565 .
O1 V1 N12 99.52(9) . 4_565
N2 V1 N12 158.03(9) . 4_565
N2 V1 N12 88.72(8) 4_565 4_565
N12 V1 N12 84.96(11) . 4_565
O1 V1 N1 171.74(12) . .
N2 V1 N1 83.52(8) . .
N2 V1 N1 83.52(8) 4_565 .
N12 V1 N1 74.52(7) . .
N12 V1 N1 74.52(7) 4_565 .
C18 N1 C18 118.0(3) . 4_565
C18 N1 V1 109.15(15) . .
C18 N1 V1 109.15(15) 4_565 .
C18 N1 H1 106.7 . .
C18 N1 H1 106.7 4_565 .
V1 N1 H1 106.7 . .
C2 N2 V1 176.1(2) . .
C15 N11 N12 111.96(19) . .
C15 N11 C18 128.3(2) . .
N12 N11 C18 118.8(2) . .
C13 N12 N11 105.1(2) . .
C13 N12 V1 136.64(18) . .
N11 N12 V1 117.90(14) . .
N2 C2 S2 179.4(3) . .
N12 C13 C14 109.4(2) . .
N12 C13 C16 122.3(2) . .
C14 C13 C16 128.2(2) . .
C15 C14 C13 107.3(2) . .
C15 C14 H14 126.3 . .
C13 C14 H14 126.3 . .
N11 C15 C14 106.2(2) . .
N11 C15 C17 122.3(2) . .
C14 C15 C17 131.6(3) . .
C13 C16 H16A 109.5 . .
C13 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C13 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C13 C16 H16D 109.5 . .
H16A C16 H16D 141.1 . .
H16B C16 H16D 56.3 . .
H16C C16 H16D 56.3 . .
C13 C16 H16E 109.5 . .
H16A C16 H16E 56.3 . .
H16B C16 H16E 141.1 . .
H16C C16 H16E 56.3 . .
H16D C16 H16E 109.5 . .
C13 C16 H16F 109.5 . .
H16A C16 H16F 56.3 . .
H16B C16 H16F 56.3 . .
H16C C16 H16F 141.1 . .
H16D C16 H16F 109.5 . .
H16E C16 H16F 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C17 H17D 109.5 . .
H17A C17 H17D 141.1 . .
H17B C17 H17D 56.3 . .
H17C C17 H17D 56.3 . .
C15 C17 H17E 109.5 . .
H17A C17 H17E 56.3 . .
H17B C17 H17E 141.1 . .
H17C C17 H17E 56.3 . .
H17D C17 H17E 109.5 . .
C15 C17 H17F 109.5 . .
H17A C17 H17F 56.3 . .
H17B C17 H17F 56.3 . .
H17C C17 H17F 141.1 . .
H17D C17 H17F 109.5 . .
H17E C17 H17F 109.5 . .
N1 C18 N11 109.9(2) . .
N1 C18 H18A 109.7 . .
N11 C18 H18A 109.7 . .
N1 C18 H18B 109.7 . .
N11 C18 H18B 109.7 . .
H18A C18 H18B 108.2 . .
C22 C21 C22 118.8(4) . 4_565
C22 C21 C25 120.6(2) . .
C22 C21 C25 120.6(2) 4_565 .
C21 C22 C23 120.7(3) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C24 C23 C22 120.5(4) . .
C24 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C23 C24 C23 118.9(5) . 4_565
C23 C24 H24 120.5 . .
C23 C24 H24 120.5 4_565 .
C21 C25 H25A 102.0 . .
C21 C25 H25B 109.7 . .
H25A C25 H25B 110.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.582(3) .
V1 N2 2.024(2) .
V1 N2 2.024(2) 4_565
V1 N12 2.115(2) .
V1 N12 2.115(2) 4_565
V1 N1 2.349(3) .
S2 C2 1.609(3) .
N1 C18 1.451(3) .
N1 C18 1.451(3) 4_565
N1 H1 0.9800 .
N2 C2 1.153(3) .
N11 C15 1.338(3) .
N11 N12 1.370(3) .
N11 C18 1.455(3) .
N12 C13 1.341(3) .
C13 C14 1.392(3) .
C13 C16 1.482(3) .
C14 C15 1.365(4) .
C14 H14 0.9300 .
C15 C17 1.501(4) .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C16 H16D 0.9600 .
C16 H16E 0.9600 .
C16 H16F 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C17 H17D 0.9600 .
C17 H17E 0.9600 .
C17 H17F 0.9600 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C21 C22 1.369(3) .
C21 C22 1.369(3) 4_565
C21 C25 1.504(6) .
C22 C23 1.376(4) .
C22 H22 0.9300 .
C23 C24 1.370(4) .
C23 H23 0.9300 .
C24 C23 1.370(4) 4_565
C24 H24 0.9300 .
C25 H25A 0.9709 .
C25 H25B 0.9399 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C16 H16A O1 0.96 2.45 3.181(4) 133.2 .
C22 H22 S2 0.93 3.09 3.799(3) 134.0 3_556
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_4
C15 N11 N12 C13 -2.2(2) . .
C18 N11 N12 C13 -171.9(2) . .
C15 N11 N12 V1 -176.38(16) . .
C18 N11 N12 V1 13.9(3) . .
N11 N12 C13 C14 1.3(3) . .
V1 N12 C13 C14 173.85(18) . .
N11 N12 C13 C16 -177.1(2) . .
V1 N12 C13 C16 -4.5(4) . .
N12 C13 C14 C15 -0.1(3) . .
C16 C13 C14 C15 178.2(2) . .
N12 N11 C15 C14 2.1(3) . .
C18 N11 C15 C14 170.7(2) . .
N12 N11 C15 C17 -178.0(2) . .
C18 N11 C15 C17 -9.5(4) . .
C13 C14 C15 N11 -1.2(3) . .
C13 C14 C15 C17 179.0(3) . .
C18 N1 C18 N11 -92.6(3) 4_565 .
V1 N1 C18 N11 32.7(3) . .
C15 N11 C18 N1 159.8(2) . .
N12 N11 C18 N1 -32.4(3) . .
C22 C21 C22 C23 -0.4(6) 4_565 .
C25 C21 C22 C23 -179.2(4) . .
C21 C22 C23 C24 0.4(5) . .
C22 C23 C24 C23 -0.4(7) . 4_565
