#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:51:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180099 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/45/7054523.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_7054523
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            'C21 H30 N8 O11 V2'
_chemical_formula_weight         672.41
_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                90.497(10)
_cell_angle_beta                 98.270(10)
_cell_angle_gamma                113.050(9)
_cell_formula_units_Z            2
_cell_length_a                   9.616(6)
_cell_length_b                   12.119(7)
_cell_length_c                   12.594(7)
_cell_measurement_reflns_used    2456
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.33
_cell_volume                     1333.0(14)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6781
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_correction_T_min  0.8602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.211
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0482
_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)+(0.0732P)²+1.0812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                3719
_reflns_number_total             4665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01525h2.cif
_cod_data_source_block           511
_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               7054523
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
V1 V 0.36323(7) 0.14114(5) 0.99673(5) 0.02610(18) Uani 1 1 d .
V2 V 0.65295(7) 0.48163(5) 0.41908(5) 0.03193(19) Uani 1 1 d .
N1 N 0.5657(3) 0.1822(3) 1.1105(2) 0.0293(7) Uani 1 1 d .
N2 N 0.7025(3) 0.2251(3) 1.0710(2) 0.0284(6) Uani 1 1 d .
N3 N 0.8118(3) 0.2729(3) 0.9154(2) 0.0305(7) Uani 1 1 d .
N4 N 0.8971(3) 0.3089(3) 0.7531(2) 0.0345(7) Uani 1 1 d .
N5 N 0.6378(3) 0.2330(3) 0.7481(2) 0.0310(7) Uani 1 1 d .
N6 N 0.5450(3) 0.1925(3) 0.9125(2) 0.0265(6) Uani 1 1 d .
N7 N 0.3776(3) 0.1556(3) 0.7594(2) 0.0289(7) Uani 1 1 d .
N8 N 0.2724(3) 0.1232(3) 0.8295(2) 0.0293(7) Uani 1 1 d .
C1 C 0.4836(6) 0.1093(4) 1.2816(3) 0.0488(11) Uani 1 1 d .
H1A H 0.3856 0.1000 1.2430 0.073 Uiso 1 1 calc R
H1B H 0.5084 0.1627 1.3447 0.073 Uiso 1 1 calc R
H1C H 0.4802 0.0324 1.3025 0.073 Uiso 1 1 calc R
C2 C 0.6018(5) 0.1600(3) 1.2118(3) 0.0336(8) Uani 1 1 d .
C3 C 0.7584(5) 0.1874(4) 1.2362(3) 0.0399(9) Uani 1 1 d .
H3B H 0.8105 0.1799 1.3021 0.048 Uiso 1 1 calc R
C4 C 0.8209(4) 0.2266(3) 1.1474(3) 0.0330(8) Uani 1 1 d .
C5 C 0.9791(5) 0.2613(4) 1.1264(3) 0.0485(11) Uani 1 1 d .
H5B H 1.0428 0.2558 1.1905 0.073 Uiso 1 1 calc R
H5C H 1.0174 0.3424 1.1053 0.073 Uiso 1 1 calc R
H5D H 0.9801 0.2082 1.0698 0.073 Uiso 1 1 calc R
C6 C 0.6911(4) 0.2321(3) 0.9611(3) 0.0262(7) Uani 1 1 d .
C7 C 0.7808(4) 0.2711(3) 0.8066(3) 0.0289(8) Uani 1 1 d .
C8 C 1.0561(4) 0.3453(4) 0.8083(3) 0.0394(9) Uani 1 1 d .
H8A H 1.1172 0.3323 0.7585 0.047 Uiso 1 1 calc R
H8B H 1.0574 0.2949 0.8676 0.047 Uiso 1 1 calc R
C9 C 1.1266(5) 0.4746(4) 0.8507(4) 0.0589(13) Uani 1 1 d .
H9A H 1.2295 0.4940 0.8860 0.088 Uiso 1 1 calc R
H9B H 1.0676 0.4876 0.9011 0.088 Uiso 1 1 calc R
H9C H 1.1279 0.5250 0.7921 0.088 Uiso 1 1 calc R
C10 C 0.8729(5) 0.3176(4) 0.6363(3) 0.0431(10) Uani 1 1 d .
H10A H 0.9635 0.3795 0.6161 0.052 Uiso 1 1 calc R
H10B H 0.7878 0.3413 0.6167 0.052 Uiso 1 1 calc R
C11 C 0.8400(6) 0.2012(5) 0.5751(4) 0.0614(13) Uani 1 1 d .
H11A H 0.8249 0.2109 0.4993 0.092 Uiso 1 1 calc R
H11B H 0.7492 0.1400 0.5937 0.092 Uiso 1 1 calc R
H11C H 0.9248 0.1781 0.5931 0.092 Uiso 1 1 calc R
C12 C 0.5291(4) 0.1973(3) 0.8061(3) 0.0266(7) Uani 1 1 d .
C13 C 0.3886(5) 0.1544(4) 0.5609(3) 0.0453(10) Uani 1 1 d .
H13A H 0.3160 0.1283 0.4956 0.068 Uiso 1 1 calc R
H13B H 0.4550 0.1121 0.5646 0.068 Uiso 1 1 calc R
H13C H 0.4482 0.2392 0.5619 0.068 Uiso 1 1 calc R
C14 C 0.3058(4) 0.1289(3) 0.6546(3) 0.0331(8) Uani 1 1 d .
C15 C 0.1549(4) 0.0776(4) 0.6591(3) 0.0386(9) Uani 1 1 d .
H15A H 0.0764 0.0490 0.6006 0.046 Uiso 1 1 calc R
C16 C 0.1371(4) 0.0750(3) 0.7671(3) 0.0335(8) Uani 1 1 d .
C17 C -0.0083(5) 0.0257(4) 0.8112(4) 0.0494(11) Uani 1 1 d .
H17A H 0.0134 0.0352 0.8883 0.074 Uiso 1 1 calc R
H17B H -0.0615 -0.0581 0.7885 0.074 Uiso 1 1 calc R
H17C H -0.0710 0.0681 0.7853 0.074 Uiso 1 1 calc R
C18 C 0.8141(4) 0.6817(3) 0.5644(3) 0.0360(9) Uani 1 1 d .
C19 C 0.7334(4) 0.5773(3) 0.6318(3) 0.0324(8) Uani 1 1 d .
H19 H 0.8094 0.5575 0.6790 0.039 Uiso 1 1 calc R
C20 C 0.3642(4) 0.3874(3) 0.3016(3) 0.0332(8) Uani 1 1 d .
H20 H 0.2998 0.3185 0.2509 0.040 Uiso 1 1 calc R
C21 C 0.4548(5) 0.4939(3) 0.2414(3) 0.0370(9) Uani 1 1 d .
O1W O 0.4507(4) 0.3488(3) 0.9885(3) 0.0687(10) Uani 1 1 d .
H1WA H 0.4961 0.3827 1.0504 0.103 Uiso 1 1 d R
H1WB H 0.3750 0.3676 0.9690 0.103 Uiso 1 1 d R
O1 O 0.3146(4) 0.0014(2) 1.0053(2) 0.0526(8) Uani 1 1 d .
O2 O 0.7771(3) 0.4311(3) 0.4020(2) 0.0519(8) Uani 1 1 d .
O3 O 0.1878(4) 0.1617(3) 1.0135(3) 0.0662(10) Uani 1 1 d .
O4 O 0.2870(4) 0.1832(3) 1.1081(3) 0.0626(9) Uani 1 1 d .
O5 O 0.7795(3) 0.6494(2) 0.4619(2) 0.0416(7) Uani 1 1 d .
O6 O 0.8979(3) 0.7802(3) 0.6036(2) 0.0507(8) Uani 1 1 d .
O7 O 0.6393(3) 0.4786(2) 0.56184(19) 0.0358(6) Uani 1 1 d .
H7A H 0.6551 0.4179 0.5843 0.043 Uiso 1 1 d R
O8 O 0.4744(3) 0.3602(2) 0.3688(2) 0.0351(6) Uani 1 1 d .
H8C H 0.4341 0.3284 0.4227 0.042 Uiso 1 1 d R
O9 O 0.3959(4) 0.5217(3) 0.1595(2) 0.0540(8) Uani 1 1 d .
O10 O 0.5951(3) 0.5486(2) 0.2872(2) 0.0400(7) 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'
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 O4 102.70(17) . .
O1 V1 O3 102.69(18) . .
O4 V1 O3 43.79(15) . .
O1 V1 N6 104.73(15) . .
O4 V1 N6 144.97(14) . .
O3 V1 N6 144.39(14) . .
O1 V1 N1 92.23(14) . .
O4 V1 N1 85.04(14) . .
O3 V1 N1 128.52(14) . .
N6 V1 N1 72.59(12) . .
O1 V1 N8 93.88(14) . .
O4 V1 N8 126.97(15) . .
O3 V1 N8 83.63(14) . .
N6 V1 N8 72.31(11) . .
N1 V1 N8 144.79(11) . .
O2 V2 O8 104.05(15) . .
O2 V2 O7 106.94(14) . .
O8 V2 O7 98.91(12) . .
O2 V2 O5 101.58(15) . .
O8 V2 O5 152.99(13) . .
O7 V2 O5 81.50(11) . .
O2 V2 O10 110.00(14) . .
O8 V2 O10 80.84(12) . .
O7 V2 O10 141.96(12) . .
O5 V2 O10 82.55(12) . .
C2 N1 N2 105.0(3) . .
C2 N1 V1 137.2(3) . .
N2 N1 V1 116.7(2) . .
C4 N2 C6 131.4(3) . .
C4 N2 N1 111.0(3) . .
C6 N2 N1 115.8(3) . .
C6 N3 C7 113.8(3) . .
C7 N4 C10 121.0(3) . .
C7 N4 C8 121.3(3) . .
C10 N4 C8 117.7(3) . .
C12 N5 C7 113.7(3) . .
C12 N6 C6 113.8(3) . .
C12 N6 V1 123.3(2) . .
C6 N6 V1 122.7(2) . .
C14 N7 C12 132.7(3) . .
C14 N7 N8 111.0(3) . .
C12 N7 N8 115.9(3) . .
C16 N8 N7 105.0(3) . .
C16 N8 V1 138.0(2) . .
N7 N8 V1 116.4(2) . .
N1 C2 C3 110.3(3) . .
N1 C2 C1 121.5(4) . .
C3 C2 C1 128.1(4) . .
C4 C3 C2 107.9(4) . .
C3 C4 N2 105.8(3) . .
C3 C4 C5 130.8(4) . .
N2 C4 C5 123.3(3) . .
N3 C6 N6 126.9(3) . .
N3 C6 N2 121.2(3) . .
N6 C6 N2 112.0(3) . .
N4 C7 N3 118.0(3) . .
N4 C7 N5 117.1(3) . .
N3 C7 N5 124.8(3) . .
N4 C8 C9 112.5(4) . .
N4 C10 C11 112.3(4) . .
N5 C12 N6 126.9(3) . .
N5 C12 N7 121.2(3) . .
N6 C12 N7 111.9(3) . .
C15 C14 N7 105.7(3) . .
C15 C14 C13 130.7(4) . .
N7 C14 C13 123.6(3) . .
C14 C15 C16 108.0(3) . .
N8 C16 C15 110.3(3) . .
N8 C16 C17 122.4(4) . .
C15 C16 C17 127.3(4) . .
O6 C18 O5 125.4(4) . .
O6 C18 C19 122.8(3) . .
O5 C18 C19 111.7(3) . .
O7 C19 C20 109.1(3) . 2_666
O7 C19 C18 108.1(3) . .
C20 C19 C18 109.5(3) 2_666 .
O8 C20 C19 110.3(3) . 2_666
O8 C20 C21 105.4(3) . .
C19 C20 C21 109.8(3) 2_666 .
O9 C21 O10 125.7(4) . .
O9 C21 C20 121.7(4) . .
O10 C21 C20 112.7(3) . .
O4 O3 V1 67.7(2) . .
O3 O4 V1 68.5(2) . .
C18 O5 V2 117.6(2) . .
C19 O7 V2 119.9(2) . .
C20 O8 V2 117.7(2) . .
C21 O10 V2 115.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.579(3) .
V1 O4 1.828(3) .
V1 O3 1.839(4) .
V1 N6 2.064(3) .
V1 N1 2.126(3) .
V1 N8 2.136(3) .
V2 O2 1.578(3) .
V2 O8 1.791(3) .
V2 O7 1.821(3) .
V2 O5 1.939(3) .
V2 O10 1.959(3) .
N1 C2 1.330(5) .
N1 N2 1.381(4) .
N2 C4 1.375(5) .
N2 C6 1.378(4) .
N3 C6 1.292(4) .
N3 C7 1.358(5) .
N4 C7 1.318(4) .
N4 C10 1.467(5) .
N4 C8 1.475(5) .
N5 C12 1.297(4) .
N5 C7 1.362(5) .
N6 C12 1.332(4) .
N6 C6 1.341(4) .
N7 C14 1.371(5) .
N7 C12 1.376(4) .
N7 N8 1.381(4) .
N8 C16 1.324(5) .
C1 C2 1.481(5) .
C2 C3 1.395(6) .
C3 C4 1.348(5) .
C4 C5 1.476(6) .
C8 C9 1.500(6) .
C10 C11 1.498(6) .
C13 C14 1.485(5) .
C14 C15 1.346(5) .
C15 C16 1.394(5) .
C16 C17 1.482(5) .
C18 O6 1.201(5) .
C18 O5 1.302(5) .
C18 C19 1.538(5) .
C19 O7 1.389(4) .
C19 C20 1.517(5) 2_666
C20 O8 1.403(5) .
C20 C19 1.517(5) 2_666
C20 C21 1.526(5) .
C21 O9 1.219(5) .
C21 O10 1.289(5) .
O3 O4 1.368(5) .
