#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:16:01 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179238 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/58/4315801.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_4315801
loop_
_publ_author_name
'Susan K. Hanson'
'R. Tom Baker'
'John C. Gordon'
'Brian L. Scott'
'David L. Thorn'
_publ_section_title
;
 Aerobic Oxidation of Lignin Models Using a Base Metal Vanadium Catalyst
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5611
_journal_page_last               5618
_journal_paper_doi               10.1021/ic100528n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C11 H15 N O7 S2 V'
_chemical_formula_weight         388.30
_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                82.2480(10)
_cell_angle_beta                 69.0760(10)
_cell_angle_gamma                70.1570(10)
_cell_formula_units_Z            2
_cell_length_a                   8.2720(12)
_cell_length_b                   9.1873(13)
_cell_length_c                   11.4084(16)
_cell_measurement_temperature    120(1)
_cell_volume                     761.66(19)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8680
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.958
_exptl_absorpt_correction_T_max  0.9103
_exptl_absorpt_correction_T_min  0.8316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             398
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.486
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.486
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0375P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                3121
_reflns_number_total             3516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100528n_si_001_4.cif
_cod_data_source_block           apx911
_cod_database_code               4315801
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 0.39057(5) 0.66338(4) 0.22257(3) 0.01320(12) Uani 1 1 d . . .
S1 S 0.13653(7) 0.77135(6) 0.05728(5) 0.01466(14) Uani 1 1 d . . .
S2 S 0.58280(8) 0.73279(7) 0.39682(5) 0.01678(15) Uani 1 1 d . . .
O1 O 0.4448(2) 0.47834(19) 0.22049(16) 0.0230(4) Uani 1 1 d . . .
O2 O 0.3329(2) 0.71588(18) 0.06119(14) 0.0162(3) Uani 1 1 d . . .
O3 O 0.4390(2) 0.6677(2) 0.38709(15) 0.0211(4) Uani 1 1 d . . .
O4 O 0.6150(2) 0.72609(18) 0.12713(14) 0.0151(3) Uani 1 1 d . . .
O5 O 0.7396(2) 0.9154(2) 0.04927(16) 0.0211(4) Uani 1 1 d . . .
O6 O 0.1211(2) 0.72776(18) 0.32531(15) 0.0163(3) Uani 1 1 d . . .
O7 O -0.1371(2) 0.9157(2) 0.41713(16) 0.0243(4) Uani 1 1 d . . .
N1 N 0.3051(2) 0.9101(2) 0.23789(17) 0.0130(4) Uani 1 1 d . . .
C1 C 0.6110(3) 0.8700(3) 0.1117(2) 0.0153(5) Uani 1 1 d . . .
C2 C 0.4261(3) 0.9843(3) 0.1803(2) 0.0136(4) Uani 1 1 d . . .
C3 C 0.3787(3) 1.1421(3) 0.1883(2) 0.0183(5) Uani 1 1 d . . .
H3 H 0.4618 1.1947 0.1459 0.022 Uiso 1 1 calc R . .
C4 C 0.2014(3) 1.2204(3) 0.2624(2) 0.0203(5) Uani 1 1 d . . .
H4 H 0.1663 1.3267 0.2724 0.024 Uiso 1 1 calc R . .
C5 C 0.0760(3) 1.1407(3) 0.3216(2) 0.0189(5) Uani 1 1 d . . .
H5 H -0.0426 1.1923 0.3708 0.023 Uiso 1 1 calc R . .
C6 C 0.1335(3) 0.9833(3) 0.3051(2) 0.0152(5) Uani 1 1 d . . .
C7 C 0.0266(3) 0.8702(3) 0.3549(2) 0.0159(5) Uani 1 1 d . . .
C8 C 0.0769(3) 0.5987(3) 0.0831(2) 0.0217(5) Uani 1 1 d . . .
H8A H 0.1690 0.5219 0.0247 0.033 Uiso 1 1 calc R . .
H8B H -0.0382 0.6195 0.0714 0.033 Uiso 1 1 calc R . .
H8C H 0.0677 0.5614 0.1673 0.033 Uiso 1 1 calc R . .
C9 C 0.1658(3) 0.7976(3) -0.1052(2) 0.0199(5) Uani 1 1 d . . .
H9A H 0.2023 0.8881 -0.1360 0.030 Uiso 1 1 calc R . .
H9B H 0.0528 0.8103 -0.1175 0.030 Uiso 1 1 calc R . .
H9C H 0.2580 0.7087 -0.1500 0.030 Uiso 1 1 calc R . .
C10 C 0.5007(3) 0.7887(3) 0.5554(2) 0.0227(5) Uani 1 1 d . . .
H10A H 0.3870 0.8709 0.5716 0.034 Uiso 1 1 calc R . .
H10B H 0.5879 0.8236 0.5712 0.034 Uiso 1 1 calc R . .
H10C H 0.4828 0.7017 0.6094 0.034 Uiso 1 1 calc R . .
C11 C 0.7679(3) 0.5660(3) 0.4024(2) 0.0243(5) Uani 1 1 d . . .
H11A H 0.7265 0.5008 0.4718 0.036 Uiso 1 1 calc R . .
H11B H 0.8619 0.5968 0.4127 0.036 Uiso 1 1 calc R . .
H11C H 0.8154 0.5103 0.3257 0.036 Uiso 1 1 calc R . .
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
_geom_angle_publ_flag
O1 V1 O4 108.84(8) . . ?
O1 V1 O2 99.08(8) . . ?
O4 V1 O2 84.97(6) . . ?
O1 V1 O6 102.78(8) . . ?
O4 V1 O6 148.37(7) . . ?
O2 V1 O6 91.04(6) . . ?
O1 V1 O3 95.04(8) . . ?
O4 V1 O3 89.23(6) . . ?
O2 V1 O3 165.82(7) . . ?
O6 V1 O3 87.13(7) . . ?
O1 V1 N1 176.10(8) . . ?
O4 V1 N1 74.40(7) . . ?
O2 V1 N1 83.24(7) . . ?
O6 V1 N1 73.97(7) . . ?
O3 V1 N1 82.73(7) . . ?
O2 S1 C8 103.41(10) . . ?
O2 S1 C9 104.03(10) . . ?
C8 S1 C9 98.42(12) . . ?
O3 S2 C10 104.10(11) . . ?
O3 S2 C11 104.26(11) . . ?
C10 S2 C11 98.91(12) . . ?
S1 O2 V1 123.04(9) . . ?
S2 O3 V1 123.84(10) . . ?
C1 O4 V1 122.38(14) . . ?
C7 O6 V1 122.30(14) . . ?
C6 N1 C2 122.4(2) . . ?
C6 N1 V1 118.84(15) . . ?
C2 N1 V1 118.76(15) . . ?
O5 C1 O4 125.3(2) . . ?
O5 C1 C2 120.8(2) . . ?
O4 C1 C2 113.89(19) . . ?
N1 C2 C3 121.0(2) . . ?
N1 C2 C1 110.43(19) . . ?
C3 C2 C1 128.5(2) . . ?
C2 C3 C4 117.5(2) . . ?
C3 C4 C5 120.6(2) . . ?
C6 C5 C4 117.9(2) . . ?
N1 C6 C5 120.4(2) . . ?
N1 C6 C7 110.52(19) . . ?
C5 C6 C7 129.1(2) . . ?
O7 C7 O6 125.0(2) . . ?
O7 C7 C6 120.7(2) . . ?
O6 C7 C6 114.30(19) . . ?
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 1.6055(17) . ?
V1 O4 2.0195(16) . ?
V1 O2 2.0202(15) . ?
V1 O6 2.0295(16) . ?
V1 O3 2.0623(16) . ?
V1 N1 2.1445(19) . ?
S1 O2 1.5440(16) . ?
S1 C8 1.774(2) . ?
S1 C9 1.775(2) . ?
S2 O3 1.5424(16) . ?
S2 C10 1.770(2) . ?
S2 C11 1.774(3) . ?
O4 C1 1.301(3) . ?
O5 C1 1.221(3) . ?
O6 C7 1.294(3) . ?
O7 C7 1.234(3) . ?
N1 C6 1.330(3) . ?
N1 C2 1.331(3) . ?
C1 C2 1.527(3) . ?
C2 C3 1.374(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.396(3) . ?
C5 C6 1.377(3) . ?
C6 C7 1.513(3) . ?
