#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:51:26 +0100 (vie 25 de mar de 2016) $
#$Revision: 180099 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/45/7054524.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_7054524
loop_
_publ_author_name
'Ma, Xi Tong'
'Xing, Na'
'Yan, Zhi Dan'
'Zhang, Xiao Xi'
'Wu, Qiong'
'Xing, Yong Heng'
_publ_section_title
;
 Peroxo- and oxovanadium(iv) complexes with tridentate N-heterocycle
 ligands: synthesis, structure, and catalytic performance
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1067
_journal_paper_doi               10.1039/C4NJ01525H
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C23 H32 N8 O12 S V'
_chemical_formula_weight         695.57
_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                103.220(2)
_cell_angle_beta                 93.546(2)
_cell_angle_gamma                100.630(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9813(13)
_cell_length_b                   12.3482(15)
_cell_length_c                   13.2980(17)
_cell_measurement_reflns_used    2325
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.54
_cell_measurement_theta_min      2.48
_cell_volume                     1558.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8039
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.9643
_exptl_absorpt_correction_T_min  0.8982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0443
_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)+(0.0481P)²+0.8371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                3879
_reflns_number_total             5452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01525h2.cif
_cod_data_source_block           888
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 7054523--7054525.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054524
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
O4 O 0.6130(2) -0.30581(18) 0.16033(17) 0.0518(6) Uani 1 1 d .
C9 C 0.7784(6) 0.4319(4) 0.0069(4) 0.114(2) Uani 1 1 d .
H9A H 0.7124 0.4468 -0.0410 0.172 Uiso 1 1 calc R
H9B H 0.8114 0.3656 -0.0258 0.172 Uiso 1 1 calc R
H9C H 0.8538 0.4959 0.0272 0.172 Uiso 1 1 calc R
V1 V 0.90838(5) -0.08214(4) 0.13322(4) 0.03144(15) Uani 1 1 d .
S1 S 0.73704(8) -0.23131(6) 0.21725(6) 0.0352(2) Uani 1 1 d .
O2 O 0.8560(2) -0.24136(16) 0.15366(17) 0.0416(5) Uani 1 1 d .
O3 O 0.7289(2) -0.10941(15) 0.22422(15) 0.0355(5) Uani 1 1 d .
N3 N 0.7534(2) 0.2006(2) 0.0905(2) 0.0365(6) Uani 1 1 d .
N6 N 0.8748(2) 0.07637(18) 0.14927(17) 0.0296(5) Uani 1 1 d .
O1 O 1.0356(2) -0.09927(18) 0.07088(18) 0.0493(6) Uani 1 1 d .
N1 N 0.7611(3) -0.09315(19) 0.00923(18) 0.0352(6) Uani 1 1 d .
O12 O 0.5411(3) 0.45902(18) 0.77274(19) 0.0626(7) Uani 1 1 d .
H12A H 0.5675 0.5298 0.7997 0.094 Uiso 1 1 d R
N5 N 0.9135(3) 0.26634(19) 0.24639(19) 0.0379(6) Uani 1 1 d .
C12 C 0.9292(3) 0.1628(2) 0.2315(2) 0.0320(7) Uani 1 1 d .
N8 N 1.0144(3) 0.0134(2) 0.27848(19) 0.0374(6) Uani 1 1 d .
N2 N 0.7217(2) 0.0074(2) 0.00536(18) 0.0337(6) Uani 1 1 d .
N7 N 1.0080(2) 0.12734(19) 0.30303(18) 0.0351(6) Uani 1 1 d .
O11 O 0.6524(2) 0.50900(18) 0.64779(19) 0.0513(6) Uani 1 1 d .
O9 O 0.6431(3) 0.4129(2) 0.4127(2) 0.0669(7) Uani 1 1 d .
O7 O 0.6418(3) 0.14305(19) 0.31268(18) 0.0564(6) Uani 1 1 d .
O8 O 0.7513(2) 0.30472(19) 0.53759(18) 0.0528(6) Uani 1 1 d .
H8A H 0.7831 0.2876 0.4821 0.079 Uiso 1 1 calc R
C7 C 0.8248(3) 0.2841(2) 0.1721(2) 0.0371(7) Uani 1 1 d .
C6 C 0.7836(3) 0.1020(2) 0.0837(2) 0.0306(7) Uani 1 1 d .
O5 O 0.7658(2) -0.25106(19) 0.31761(17) 0.0510(6) Uani 1 1 d .
N4 N 0.8056(3) 0.3880(2) 0.1794(2) 0.0472(7) Uani 1 1 d .
O10 O 0.4302(2) 0.3265(2) 0.4237(2) 0.0693(8) Uani 1 1 d .
H10D H 0.4097 0.3649 0.3816 0.104 Uiso 1 1 d R
O6 O 0.6523(3) 0.0052(2) 0.39222(19) 0.0697(8) Uani 1 1 d .
H6A H 0.6892 -0.0211 0.3385 0.105 Uiso 1 1 d R
C13 C 1.0790(3) 0.1823(3) 0.3986(2) 0.0407(8) Uani 1 1 d .
C16 C 1.0901(3) -0.0010(3) 0.3582(3) 0.0453(8) Uani 1 1 d .
C20 C 0.6068(3) 0.2809(2) 0.5202(2) 0.0362(7) Uani 1 1 d .
C1 C 0.7026(4) -0.1673(3) -0.0777(3) 0.0478(8) Uani 1 1 d .
C18 C 0.6219(3) 0.1026(3) 0.3856(2) 0.0386(7) Uani 1 1 d .
C21 C 0.5644(3) 0.3478(3) 0.4451(3) 0.0420(8) Uani 1 1 d .
C19 C 0.5563(3) 0.1534(2) 0.4779(2) 0.0424(8) Uani 1 1 d .
H19A H 0.5730 0.1160 0.5327 0.051 Uiso 1 1 calc R
H19B H 0.4580 0.1382 0.4592 0.051 Uiso 1 1 calc R
C23 C 0.5853(3) 0.4352(3) 0.6816(3) 0.0409(8) Uani 1 1 d .
C15 C 1.1309(3) 0.1020(3) 0.4329(3) 0.0493(9) Uani 1 1 d .
H15A H 1.1847 0.1134 0.4956 0.059 Uiso 1 1 calc R
C14 C 1.0894(4) 0.3049(3) 0.4477(3) 0.0561(10) Uani 1 1 d .
H14A H 1.1438 0.3247 0.5139 0.084 Uiso 1 1 calc R
H14B H 0.9993 0.3195 0.4575 0.084 Uiso 1 1 calc R
H14C H 1.1318 0.3496 0.4036 0.084 Uiso 1 1 calc R
C4 C 0.6399(3) -0.0042(3) -0.0848(3) 0.0454(8) Uani 1 1 d .
C22 C 0.5473(4) 0.3131(3) 0.6237(3) 0.0464(8) Uani 1 1 d .
H22A H 0.4481 0.2920 0.6105 0.056 Uiso 1 1 calc R
H22B H 0.5762 0.2678 0.6685 0.056 Uiso 1 1 calc R
C11 C 0.8784(4) 0.4833(3) 0.2639(3) 0.0610(10) Uani 1 1 d .
H11A H 0.8921 0.4560 0.3259 0.073 Uiso 1 1 calc R
H11B H 0.8218 0.5398 0.2791 0.073 Uiso 1 1 calc R
C3 C 0.6260(4) -0.1147(3) -0.1365(3) 0.0584(10) Uani 1 1 d .
H3B H 0.5744 -0.1495 -0.2002 0.070 Uiso 1 1 calc R
C8 C 0.7126(4) 0.4121(3) 0.1006(4) 0.0733(13) Uani 1 1 d .
H8B H 0.6778 0.4788 0.1321 0.088 Uiso 1 1 calc R
H8C H 0.6351 0.3487 0.0790 0.088 Uiso 1 1 calc R
C17 C 1.1217(4) -0.1143(3) 0.3573(3) 0.0670(11) Uani 1 1 d .
H17A H 1.0782 -0.1681 0.2945 0.101 Uiso 1 1 calc R
H17B H 1.0880 -0.1389 0.4162 0.101 Uiso 1 1 calc R
H17C H 1.2191 -0.1090 0.3607 0.101 Uiso 1 1 calc R
C5 C 0.5868(4) 0.0907(3) -0.1133(3) 0.0639(11) Uani 1 1 d .
H5C H 0.5324 0.0634 -0.1796 0.096 Uiso 1 1 calc R
H5D H 0.6623 0.1497 -0.1172 0.096 Uiso 1 1 calc R
H5E H 0.5312 0.1204 -0.0616 0.096 Uiso 1 1 calc R
C2 C 0.7235(5) -0.2862(3) -0.1008(3) 0.0751(13) Uani 1 1 d .
H2A H 0.7822 -0.2958 -0.0449 0.113 Uiso 1 1 calc R
H2B H 0.7652 -0.3020 -0.1642 0.113 Uiso 1 1 calc R
H2C H 0.6366 -0.3374 -0.1081 0.113 Uiso 1 1 calc R
C10 C 1.0140(5) 0.5382(4) 0.2391(4) 0.0825(14) Uani 1 1 d .
H10A H 1.0568 0.5995 0.2970 0.124 Uiso 1 1 calc R
H10B H 1.0011 0.5674 0.1789 0.124 Uiso 1 1 calc R
H10C H 1.0713 0.4832 0.2252 0.124 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
O1 V1 N6 111.05(10)
O1 V1 O2 97.93(10)
N6 V1 O2 150.98(9)
O1 V1 N1 99.50(11)
N6 V1 N1 74.54(9)
O2 V1 N1 99.75(9)
O1 V1 N8 98.98(11)
N6 V1 N8 74.20(9)
O2 V1 N8 103.63(9)
N1 V1 N8 147.72(9)
O1 V1 O3 163.39(10)
N6 V1 O3 85.55(8)
O2 V1 O3 65.51(7)
N1 V1 O3 85.31(9)
N8 V1 O3 84.47(9)
O5 S1 O4 112.52(14)
O5 S1 O3 111.79(13)
O4 S1 O3 109.89(13)
O5 S1 O2 111.45(13)
O4 S1 O2 110.13(13)
O3 S1 O2 100.43(11)
S1 O2 V1 101.49(10)
S1 O3 V1 92.55(9)
C6 N3 C7 114.3(2)
C12 N6 C6 114.0(2)
C12 N6 V1 123.25(19)
C6 N6 V1 122.41(18)
C1 N1 N2 105.7(2)
C1 N1 V1 138.4(2)
N2 N1 V1 115.34(17)
C12 N5 C7 114.1(2)
N5 C12 N6 126.6(3)
N5 C12 N7 122.0(3)
N6 C12 N7 111.3(2)
C16 N8 N7 105.4(2)
C16 N8 V1 139.6(2)
N7 N8 V1 114.99(16)
C4 N2 N1 111.3(2)
C4 N2 C6 132.0(3)
N1 N2 C6 116.1(2)
C13 N7 N8 110.9(2)
C13 N7 C12 132.9(2)
N8 N7 C12 116.2(2)
N4 C7 N3 117.3(3)
N4 C7 N5 118.2(3)
N3 C7 N5 124.4(3)
N3 C6 N6 126.1(3)
N3 C6 N2 122.2(3)
N6 C6 N2 111.6(2)
C7 N4 C11 121.3(3)
C7 N4 C8 120.5(3)
C11 N4 C8 118.2(3)
C15 C13 N7 105.4(3)
C15 C13 C14 130.6(3)
N7 C13 C14 123.9(3)
N8 C16 C15 109.9(3)
N8 C16 C17 120.4(3)
C15 C16 C17 129.7(3)
O8 C20 C21 108.4(2)
O8 C20 C19 108.9(2)
C21 C20 C19 112.1(3)
O8 C20 C22 109.5(3)
C21 C20 C22 111.3(3)
C19 C20 C22 106.6(2)
N1 C1 C3 109.6(3)
N1 C1 C2 120.7(3)
C3 C1 C2 129.7(3)
O7 C18 O6 123.5(3)
O7 C18 C19 124.9(3)
O6 C18 C19 111.6(3)
O9 C21 O10 125.0(3)
O9 C21 C20 123.8(3)
O10 C21 C20 111.1(3)
C18 C19 C20 114.5(3)
O11 C23 O12 121.1(3)
O11 C23 C22 123.6(3)
O12 C23 C22 115.4(3)
C13 C15 C16 108.3(3)
C3 C4 N2 105.0(3)
C3 C4 C5 131.2(3)
N2 C4 C5 123.7(3)
C23 C22 C20 116.5(3)
N4 C11 C10 113.2(3)
C4 C3 C1 108.4(3)
N4 C8 C9 113.8(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O4 S1 1.448(2)
C9 C8 1.492(6)
V1 O1 1.579(2)
V1 N6 2.012(2)
V1 O2 2.0237(19)
V1 N1 2.103(2)
V1 N8 2.118(2)
V1 O3 2.240(2)
S1 O5 1.432(2)
S1 O3 1.5043(19)
S1 O2 1.507(2)
N3 C6 1.292(3)
N3 C7 1.367(4)
N6 C12 1.345(3)
N6 C6 1.350(3)
N1 C1 1.324(4)
N1 N2 1.381(3)
O12 C23 1.305(4)
N5 C12 1.289(3)
N5 C7 1.367(4)
C12 N7 1.393(4)
N8 C16 1.327(4)
N8 N7 1.384(3)
N2 C4 1.372(4)
N2 C6 1.389(3)
N7 C13 1.377(4)
O11 C23 1.217(4)
O9 C21 1.190(4)
O7 C18 1.200(4)
O8 C20 1.412(3)
C7 N4 1.316(4)
N4 C11 1.468(4)
N4 C8 1.473(5)
O10 C21 1.317(4)
O6 C18 1.313(4)
C13 C15 1.352(4)
C13 C14 1.487(4)
C16 C15 1.397(4)
C16 C17 1.488(5)
C20 C21 1.520(4)
C20 C19 1.522(4)
C20 C22 1.531(4)
C1 C3 1.400(5)
C1 C2 1.485(5)
C18 C19 1.493(4)
C23 C22 1.493(4)
C4 C3 1.357(5)
C4 C5 1.485(5)
C11 C10 1.490(5)
