#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:15:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179404 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/01/4330174.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_4330174
loop_
_publ_author_name
'Pabitra B. Chatterjee'
'Debbie C. Crans'
_publ_section_title
;
 Solid-to-Solid Oxidation of a Vanadium(IV) to a Vanadium(V) Compound:
 Chemisty of a Sulfur-Containing Siderophore
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9144
_journal_page_last               9146
_journal_paper_doi               10.1021/ic301026b
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C17 H11 N3 O3 S2 V'
_chemical_formula_weight         420.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.912(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9856(12)
_cell_length_b                   8.5662(8)
_cell_length_c                   16.0313(15)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.62
_cell_measurement_theta_min      2.74
_cell_volume                     1654.5(3)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2009)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17269
_diffrn_reflns_theta_full        24.81
_diffrn_reflns_theta_max         24.81
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.7263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE (Bruker, 2009)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       rod
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.268
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0503
_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)+(0.0568P)²+3.4681P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                1781
_reflns_number_total             2795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301026b_si_002.cif
_cod_data_source_block           dc01
_cod_original_cell_volume        1654.4(3)
_cod_database_code               4330174
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
V1 V 0.26997(6) 0.27905(9) 0.05111(5) 0.0233(3) Uani 1 1 d .
C1 C 0.3793(4) -0.0329(5) 0.0423(3) 0.0255(12) Uani 1 1 d .
H1 H 0.3105 -0.0520 -0.0029 0.031 Uiso 1 1 calc R
C2 C 0.4582(4) -0.1491(6) 0.0639(3) 0.0292(12) Uani 1 1 d .
H2 H 0.4437 -0.2436 0.0331 0.035 Uiso 1 1 calc R
C3 C 0.5594(4) -0.1222(6) 0.1324(3) 0.0295(12) Uani 1 1 d .
H3 H 0.6136 -0.1995 0.1494 0.035 Uiso 1 1 calc R
C4 C 0.5790(4) 0.0191(6) 0.1749(3) 0.0276(12) Uani 1 1 d .
H4 H 0.6469 0.0387 0.2210 0.033 Uiso 1 1 calc R
C5 C 0.4975(4) 0.1335(5) 0.1494(3) 0.0205(11) Uani 1 1 d .
C6 C 0.5131(4) 0.2898(5) 0.1903(3) 0.0214(11) Uani 1 1 d .
C7 C 0.6113(4) 0.3381(6) 0.2558(3) 0.0281(12) Uani 1 1 d .
H7 H 0.6713 0.2702 0.2771 0.034 Uiso 1 1 calc R
C8 C 0.6200(4) 0.4880(6) 0.2896(3) 0.0290(13) Uani 1 1 d .
H8 H 0.6863 0.5229 0.3328 0.035 Uiso 1 1 calc R
C9 C 0.5295(4) 0.5840(6) 0.2584(3) 0.0270(12) Uani 1 1 d .
H9 H 0.5330 0.6852 0.2803 0.032 Uiso 1 1 calc R
C10 C 0.4325(4) 0.5282(6) 0.1935(3) 0.0259(12) Uani 1 1 d .
H10 H 0.3710 0.5937 0.1729 0.031 Uiso 1 1 calc R
C11 C 0.2421(4) 0.5917(6) -0.0667(3) 0.0294(13) Uani 1 1 d .
C12 C 0.1778(4) 0.6066(6) -0.0057(3) 0.0246(12) Uani 1 1 d .
C13 C 0.1188(4) 0.7416(6) -0.0080(3) 0.0293(13) Uani 1 1 d .
H13 H 0.1158 0.8205 -0.0487 0.035 Uiso 1 1 calc R
C14 C 0.0646(4) 0.7583(6) 0.0504(3) 0.0320(13) Uani 1 1 d .
H14 H 0.0239 0.8481 0.0495 0.038 Uiso 1 1 calc R
C15 C 0.0715(4) 0.6398(6) 0.1104(3) 0.0289(12) Uani 1 1 d .
H15 H 0.0362 0.6497 0.1510 0.035 Uiso 1 1 calc R
C16 C 0.1309(4) 0.5065(6) 0.1102(3) 0.0249(12) Uani 1 1 d .
C17 C 0.1410(4) 0.3791(6) 0.1786(3) 0.0332(13) Uani 1 1 d .
N1 N 0.3971(3) 0.1070(4) 0.0834(2) 0.0203(9) Uani 1 1 d .
N2 N 0.4233(3) 0.3840(4) 0.1591(2) 0.0221(9) Uani 1 1 d .
N3 N 0.1834(3) 0.4879(4) 0.0522(2) 0.0217(9) Uani 1 1 d .
O1 O 0.2352(3) 0.6947(4) -0.1219(2) 0.0435(10) Uani 1 1 d .
O2 O 0.0980(4) 0.3976(4) 0.2342(3) 0.0502(11) Uani 1 1 d .
O3 O 0.1826(3) 0.1692(4) -0.0228(2) 0.0314(9) Uani 1 1 d .
S2 S 0.21592(11) 0.21470(16) 0.17585(9) 0.0374(4) Uani 1 1 d .
S1 S 0.32806(11) 0.43305(15) -0.05213(9) 0.0314(4) 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'
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
O3 V1 N3 105.71(15)
O3 V1 N1 92.51(16)
N3 V1 N1 161.76(14)
O3 V1 N2 165.63(16)
N3 V1 N2 88.66(13)
N1 V1 N2 73.13(14)
O3 V1 S2 97.68(13)
N3 V1 S2 82.36(12)
N1 V1 S2 94.54(11)
N2 V1 S2 84.41(10)
O3 V1 S1 97.37(13)
N3 V1 S1 81.27(12)
N1 V1 S1 97.53(11)
N2 V1 S1 84.20(10)
S2 V1 S1 160.23(6)
N1 C1 C2 123.0(4)
C1 C2 C3 118.5(5)
C4 C3 C2 119.3(5)
C3 C4 C5 119.9(4)
N1 C5 C4 121.2(4)
N1 C5 C6 115.6(4)
C4 C5 C6 123.2(4)
N2 C6 C7 121.8(4)
N2 C6 C5 114.9(4)
C7 C6 C5 123.2(4)
C6 C7 C8 119.7(5)
C9 C8 C7 118.8(4)
C8 C9 C10 118.9(5)
N2 C10 C9 122.9(4)
O1 C11 C12 119.8(5)
O1 C11 S1 122.4(4)
C12 C11 S1 117.8(4)
N3 C12 C13 122.1(5)
N3 C12 C11 118.5(4)
C13 C12 C11 119.3(5)
C14 C13 C12 119.4(5)
C13 C14 C15 118.9(5)
C16 C15 C14 119.9(5)
N3 C16 C15 121.7(5)
N3 C16 C17 118.8(4)
C15 C16 C17 119.4(5)
O2 C17 C16 119.5(5)
O2 C17 S2 122.7(4)
C16 C17 S2 117.8(4)
C1 N1 C5 118.0(4)
C1 N1 V1 121.5(3)
C5 N1 V1 120.4(3)
C10 N2 C6 117.8(4)
C10 N2 V1 126.4(3)
C6 N2 V1 115.7(3)
C16 N3 C12 118.0(4)
C16 N3 V1 120.7(3)
C12 N3 V1 121.3(3)
C17 S2 V1 100.13(19)
C11 S1 V1 99.79(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 O3 1.605(3)
V1 N3 2.116(4)
V1 N1 2.127(4)
V1 N2 2.280(4)
V1 S2 2.4172(17)
V1 S1 2.4454(16)
C1 N1 1.346(6)
C1 C2 1.377(7)
C2 C3 1.382(7)
C3 C4 1.366(7)
C4 C5 1.387(6)
C5 N1 1.357(5)
C5 C6 1.471(7)
C6 N2 1.351(6)
C6 C7 1.378(6)
C7 C8 1.382(7)
C8 C9 1.367(7)
C9 C10 1.385(6)
C10 N2 1.340(6)
C11 O1 1.229(6)
C11 C12 1.509(7)
C11 S1 1.719(5)
C12 N3 1.360(6)
C12 C13 1.380(7)
C13 C14 1.373(7)
C14 C15 1.379(7)
C15 C16 1.378(7)
C16 N3 1.352(6)
C16 C17 1.518(7)
C17 O2 1.226(6)
C17 S2 1.721(6)
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
N1 C1 C2 C3 1.6(7)
C1 C2 C3 C4 -1.5(7)
C2 C3 C4 C5 0.3(7)
C3 C4 C5 N1 1.1(7)
C3 C4 C5 C6 -178.5(4)
N1 C5 C6 N2 2.7(6)
C4 C5 C6 N2 -177.8(4)
N1 C5 C6 C7 -177.5(4)
C4 C5 C6 C7 2.0(7)
N2 C6 C7 C8 -1.5(7)
C5 C6 C7 C8 178.7(4)
C6 C7 C8 C9 1.5(7)
C7 C8 C9 C10 -0.5(7)
C8 C9 C10 N2 -0.6(8)
O1 C11 C12 N3 177.4(4)
S1 C11 C12 N3 -5.6(5)
O1 C11 C12 C13 -4.9(7)
S1 C11 C12 C13 172.0(3)
N3 C12 C13 C14 0.6(7)
C11 C12 C13 C14 -177.0(4)
C12 C13 C14 C15 0.6(7)
C13 C14 C15 C16 -0.9(7)
C14 C15 C16 N3 0.0(7)
C14 C15 C16 C17 178.0(4)
N3 C16 C17 O2 176.8(4)
C15 C16 C17 O2 -1.3(7)
N3 C16 C17 S2 -2.0(6)
C15 C16 C17 S2 180.0(3)
C2 C1 N1 C5 -0.3(7)
C2 C1 N1 V1 -177.4(4)
C4 C5 N1 C1 -1.1(6)
C6 C5 N1 C1 178.5(4)
C4 C5 N1 V1 176.1(3)
C6 C5 N1 V1 -4.3(5)
O3 V1 N1 C1 -0.4(4)
N3 V1 N1 C1 176.9(4)
N2 V1 N1 C1 -179.8(4)
S2 V1 N1 C1 97.5(3)
S1 V1 N1 C1 -98.2(3)
O3 V1 N1 C5 -177.5(3)
N3 V1 N1 C5 -0.2(7)
N2 V1 N1 C5 3.2(3)
S2 V1 N1 C5 -79.6(3)
S1 V1 N1 C5 84.7(3)
C9 C10 N2 C6 0.6(7)
C9 C10 N2 V1 -179.0(4)
C7 C6 N2 C10 0.5(7)
C5 C6 N2 C10 -179.7(4)
C7 C6 N2 V1 -179.9(4)
C5 C6 N2 V1 0.0(5)
O3 V1 N2 C10 175.4(6)
N3 V1 N2 C10 -3.0(4)
N1 V1 N2 C10 178.1(4)
S2 V1 N2 C10 -85.4(4)
S1 V1 N2 C10 78.4(4)
O3 V1 N2 C6 -4.2(8)
N3 V1 N2 C6 177.4(3)
N1 V1 N2 C6 -1.6(3)
S2 V1 N2 C6 94.9(3)
S1 V1 N2 C6 -101.2(3)
C15 C16 N3 C12 1.1(6)
C17 C16 N3 C12 -176.9(4)
C15 C16 N3 V1 -178.2(3)
C17 C16 N3 V1 3.8(5)
C13 C12 N3 C16 -1.4(6)
C11 C12 N3 C16 176.2(4)
C13 C12 N3 V1 177.9(3)
C11 C12 N3 V1 -4.5(5)
O3 V1 N3 C16 92.7(3)
N1 V1 N3 C16 -84.4(6)
N2 V1 N3 C16 -87.7(3)
S2 V1 N3 C16 -3.1(3)
S1 V1 N3 C16 -172.0(3)
O3 V1 N3 C12 -86.6(3)
N1 V1 N3 C12 96.3(5)
N2 V1 N3 C12 93.0(3)
S2 V1 N3 C12 177.6(3)
S1 V1 N3 C12 8.7(3)
O2 C17 S2 V1 -179.1(4)
C16 C17 S2 V1 -0.4(4)
O3 V1 S2 C17 -103.3(2)
N3 V1 S2 C17 1.59(19)
N1 V1 S2 C17 163.5(2)
N2 V1 S2 C17 91.0(2)
S1 V1 S2 C17 35.9(3)
O1 C11 S1 V1 -172.6(4)
C12 C11 S1 V1 10.5(4)
O3 V1 S1 C11 95.7(2)
N3 V1 S1 C11 -9.15(18)
N1 V1 S1 C11 -170.77(19)
N2 V1 S1 C11 -98.68(19)
S2 V1 S1 C11 -43.6(2)
