#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:26:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179412 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/09/4330906.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_4330906
loop_
_publ_author_name
'Manas Sutradhar'
'Marina V. Kirillova'
'M. Fátima C. Guedes da Silva'
'Luísa M. D. R. S. Martins'
'Armando J. L. Pombeiro'
_publ_section_title
;
 A Hexanuclear Mixed-Valence Oxovanadium(IV,V) Complex as a Highly
 Efficient Alkane Oxidation Catalyst
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11229
_journal_page_last               11231
_journal_paper_doi               10.1021/ic3017062
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C44 H48 N8 O22 V6'
_chemical_formula_sum            'C44 H48 N8 O22 V6'
_chemical_formula_weight         1346.54
_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                94.249(5)
_cell_angle_beta                 100.947(7)
_cell_angle_gamma                104.481(7)
_cell_formula_units_Z            1
_cell_length_a                   8.1285(14)
_cell_length_b                   10.733(2)
_cell_length_c                   16.031(3)
_cell_measurement_reflns_used    964
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      3.00
_cell_volume                     1318.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_sigmaI/netI    0.2529
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10646
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       prism
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4764
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.2398
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1180P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1767
_refine_ls_wR_factor_ref         0.2659
_reflns_number_gt                1733
_reflns_number_total             4764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3017062_si_001.cif
_cod_data_source_block           Compound1
_cod_original_cell_volume        1318.7(4)
_cod_database_code               4330906
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
C1 C 0.7336(19) -0.0292(13) 0.5058(9) 0.057(4) Uani 1 1 d .
C2 C 0.864(2) -0.0020(16) 0.5808(8) 0.069(4) Uani 1 1 d .
H2 H 0.8696 -0.0684 0.6164 0.083 Uiso 1 1 calc R
C3 C 0.980(2) 0.1142(16) 0.6043(9) 0.073(5) Uani 1 1 d .
H3 H 1.0660 0.1296 0.6561 0.088 Uiso 1 1 calc R
C4 C 0.976(2) 0.2074(15) 0.5548(9) 0.085(5) Uani 1 1 d .
H4 H 1.0614 0.2882 0.5712 0.102 Uiso 1 1 calc R
C5 C 0.8491(19) 0.1917(12) 0.4796(9) 0.070(4) Uani 1 1 d .
H5 H 0.8472 0.2621 0.4473 0.084 Uiso 1 1 calc R
C6 C 0.7267(17) 0.0735(12) 0.4522(7) 0.050(3) Uani 1 1 d .
C7 C 0.5951(17) 0.0535(11) 0.3741(8) 0.047(3) Uani 1 1 d .
C8 C 0.2452(17) -0.1729(12) 0.2457(8) 0.051(3) Uani 1 1 d .
C9 C 0.1007(16) -0.1962(11) 0.1724(8) 0.060(4) Uani 1 1 d .
H9A H 0.0781 -0.1135 0.1593 0.089 Uiso 1 1 calc R
H9B H -0.0033 -0.2530 0.1856 0.089 Uiso 1 1 calc R
H9C H 0.1298 -0.2379 0.1228 0.089 Uiso 1 1 calc R
C11 C 0.3494(15) 0.1477(10) -0.0994(7) 0.041(3) Uani 1 1 d .
C12 C 0.2893(14) 0.0957(11) -0.1851(7) 0.042(3) Uani 1 1 d .
H12 H 0.3193 0.1482 -0.2281 0.050 Uiso 1 1 calc R
C13 C 0.1889(14) -0.0279(11) -0.2089(7) 0.041(3) Uani 1 1 d .
H13 H 0.1477 -0.0619 -0.2678 0.049 Uiso 1 1 calc R
C14 C 0.1475(15) -0.1041(11) -0.1451(8) 0.047(3) Uani 1 1 d .
H14 H 0.0761 -0.1906 -0.1609 0.057 Uiso 1 1 calc R
C15 C 0.2079(15) -0.0564(10) -0.0599(8) 0.049(3) Uani 1 1 d .
H15 H 0.1789 -0.1108 -0.0178 0.058 Uiso 1 1 calc R
C16 C 0.3115(13) 0.0710(9) -0.0339(7) 0.033(3) Uani 1 1 d .
C17 C 0.3759(14) 0.1193(10) 0.0552(7) 0.037(3) Uani 1 1 d .
C18 C 0.6345(15) 0.3813(12) 0.1909(7) 0.043(3) Uani 1 1 d .
C19 C 0.7108(16) 0.4412(11) 0.2823(7) 0.059(4) Uani 1 1 d .
H19A H 0.6715 0.3788 0.3208 0.089 Uiso 1 1 calc R
H19B H 0.6725 0.5193 0.2933 0.089 Uiso 1 1 calc R
H19C H 0.8381 0.4645 0.2923 0.089 Uiso 1 1 calc R
C21 C 0.319(3) -0.5203(19) 0.3895(16) 0.192(12) Uani 1 1 d DU
H21A H 0.2776 -0.5287 0.3266 0.231 Uiso 1 1 calc R
H21B H 0.4271 -0.5487 0.4016 0.231 Uiso 1 1 calc R
C22 C 0.190(3) -0.598(2) 0.4265(19) 0.212(12) Uani 1 1 d DU
H22A H 0.1685 -0.6894 0.4040 0.318 Uiso 1 1 calc R
H22B H 0.0821 -0.5717 0.4121 0.318 Uiso 1 1 calc R
H22C H 0.2307 -0.5867 0.4888 0.318 Uiso 1 1 calc R
C23 C 0.8013(14) 0.5991(10) -0.0435(8) 0.046(3) Uani 1 1 d .
H23A H 0.8960 0.5775 -0.0035 0.056 Uiso 1 1 calc R
H23B H 0.8197 0.6943 -0.0348 0.056 Uiso 1 1 calc R
C24 C 0.8073(17) 0.5569(12) -0.1347(8) 0.062(4) Uani 1 1 d .
H24A H 0.9208 0.6005 -0.1457 0.093 Uiso 1 1 calc R
H24B H 0.7152 0.5801 -0.1742 0.093 Uiso 1 1 calc R
H24C H 0.7898 0.4627 -0.1431 0.093 Uiso 1 1 calc R
N1 N 0.4843(14) -0.0605(9) 0.3455(7) 0.052(3) Uani 1 1 d .
N2 N 0.3563(12) -0.0585(8) 0.2710(5) 0.037(2) Uani 1 1 d .
N3 N 0.4809(10) 0.2365(8) 0.0810(5) 0.030(2) Uani 1 1 d .
N4 N 0.5296(11) 0.2644(8) 0.1708(6) 0.037(2) Uani 1 1 d .
O1 O 0.6121(11) -0.1439(9) 0.4853(5) 0.064(3) Uani 1 1 d .
O2 O 0.5862(9) 0.1523(6) 0.3316(4) 0.0422(19) Uani 1 1 d .
O3 O 0.2650(12) -0.2660(8) 0.2933(6) 0.067(3) Uani 1 1 d .
O4 O 0.3556(13) -0.3738(9) 0.4303(7) 0.090(3) Uani 1 1 d .
O5 O 0.4378(9) 0.2745(7) -0.0783(5) 0.045(2) Uani 1 1 d .
O6 O 0.3266(9) 0.0477(6) 0.1126(5) 0.0409(19) Uani 1 1 d .
O7 O 0.6809(9) 0.4513(6) 0.1336(5) 0.042(2) Uani 1 1 d .
O8 O 0.6371(9) 0.5359(6) -0.0254(4) 0.0366(19) Uani 1 1 d .
O10 O 0.5983(12) -0.2916(8) 0.3363(6) 0.075(3) Uani 1 1 d .
O20 O 0.7621(9) 0.3344(6) 0.0023(5) 0.048(2) Uani 1 1 d .
O30 O 0.2484(10) 0.1798(7) 0.2589(5) 0.048(2) Uani 1 1 d .
V1 V 0.4720(3) -0.2402(2) 0.38754(16) 0.0663(8) Uani 1 1 d .
V2 V 0.5940(2) 0.37603(16) 0.01148(12) 0.0378(6) Uani 1 1 d .
V3 V 0.3963(3) 0.12395(17) 0.23262(12) 0.0390(6) 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_3
O1 C1 C2 121.9(12) .
O1 C1 C6 120.1(12) .
C2 C1 C6 117.9(13) .
C3 C2 C1 122.5(13) .
C3 C2 H2 118.7 .
C1 C2 H2 118.7 .
C4 C3 C2 119.5(14) .
C4 C3 H3 120.2 .
C2 C3 H3 120.2 .
C3 C4 C5 122.7(16) .
C3 C4 H4 118.7 .
C5 C4 H4 118.7 .
C6 C5 C4 120.0(13) .
C6 C5 H5 120.0 .
C4 C5 H5 120.0 .
C5 C6 C7 121.4(11) .
C5 C6 C1 117.3(12) .
C7 C6 C1 121.3(12) .
O2 C7 N1 119.6(11) .
O2 C7 C6 118.8(11) .
N1 C7 C6 121.6(11) .
N2 C8 O3 116.7(12) .
N2 C8 C9 122.4(11) .
O3 C8 C9 120.8(11) .
C8 C9 H9A 109.5 .
C8 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C8 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
O5 C11 C12 119.9(10) .
O5 C11 C16 119.5(10) .
C12 C11 C16 120.6(10) .
C13 C12 C11 121.6(10) .
C13 C12 H12 119.2 .
C11 C12 H12 119.2 .
C12 C13 C14 118.5(11) .
C12 C13 H13 120.7 .
C14 C13 H13 120.7 .
C15 C14 C13 121.2(11) .
C15 C14 H14 119.4 .
C13 C14 H14 119.4 .
C14 C15 C16 121.2(11) .
C14 C15 H15 119.4 .
C16 C15 H15 119.4 .
C15 C16 C11 116.8(10) .
C15 C16 C17 120.8(10) .
C11 C16 C17 122.4(9) .
O6 C17 N3 118.6(10) .
O6 C17 C16 119.7(9) .
N3 C17 C16 121.8(9) .
O7 C18 N4 121.8(11) .
O7 C18 C19 115.9(10) .
N4 C18 C19 122.3(11) .
C18 C19 H19A 109.5 .
C18 C19 H19B 109.5 .
H19A C19 H19B 109.5 .
C18 C19 H19C 109.5 .
H19A C19 H19C 109.5 .
H19B C19 H19C 109.5 .
C22 C21 O4 108(2) .
C22 C21 H21A 110.1 .
O4 C21 H21A 110.1 .
C22 C21 H21B 110.1 .
O4 C21 H21B 110.1 .
H21A C21 H21B 108.4 .
C21 C22 H22A 109.5 .
C21 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
C21 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
O8 C23 C24 110.6(9) .
O8 C23 H23A 109.5 .
C24 C23 H23A 109.5 .
O8 C23 H23B 109.5 .
C24 C23 H23B 109.5 .
H23A C23 H23B 108.1 .
C23 C24 H24A 109.5 .
C23 C24 H24B 109.5 .
H24A C24 H24B 109.5 .
C23 C24 H24C 109.5 .
H24A C24 H24C 109.5 .
H24B C24 H24C 109.5 .
C7 N1 N2 113.2(9) .
C7 N1 V1 130.7(9) .
N2 N1 V1 116.0(7) .
C8 N2 N1 111.5(9) .
C8 N2 V3 137.2(8) .
N1 N2 V3 111.3(6) .
C17 N3 N4 112.7(8) .
C17 N3 V2 130.4(7) .
N4 N3 V2 116.8(6) .
C18 N4 N3 108.8(9) .
C18 N4 V3 137.6(8) .
N3 N4 V3 113.1(6) .
C1 O1 V1 136.5(8) .
C7 O2 V3 117.2(7) .
C8 O3 V1 121.3(8) .
C21 O4 V1 123.2(10) .
C11 O5 V2 137.7(7) .
C17 O6 V3 118.4(7) .
C18 O7 V2 118.3(7) .
C23 O8 V2 122.5(6) .
C23 O8 V2 128.3(5) 2_665
V2 O8 V2 108.3(3) 2_665
O10 V1 O4 107.3(5) .
O10 V1 O1 105.8(5) .
O4 V1 O1 100.5(5) .
O10 V1 O3 99.8(4) .
O4 V1 O3 88.6(4) .
O1 V1 O3 148.6(4) .
O10 V1 N1 101.3(4) .
O4 V1 N1 148.6(4) .
O1 V1 N1 83.6(4) .
O3 V1 N1 73.8(4) .
O20 V2 O5 100.8(4) .
O20 V2 O8 101.8(3) .
O5 V2 O8 102.9(3) .
O20 V2 O7 95.4(4) .
O5 V2 O7 154.7(3) .
O8 V2 O7 92.6(3) .
O20 V2 N3 101.3(3) .
O5 V2 N3 83.6(3) .
O8 V2 N3 154.4(3) .
O7 V2 N3 74.2(3) .
O20 V2 O8 173.0(3) 2_665
O5 V2 O8 83.5(3) 2_665
O8 V2 O8 71.7(3) 2_665
O7 V2 O8 82.6(3) 2_665
N3 V2 O8 84.6(3) 2_665
O30 V3 O2 108.8(4) .
O30 V3 O6 110.2(4) .
O2 V3 O6 141.0(3) .
O30 V3 N2 105.4(4) .
O2 V3 N2 78.6(3) .
O6 V3 N2 90.5(3) .
O30 V3 N4 105.0(4) .
O2 V3 N4 94.3(3) .
O6 V3 N4 76.5(3) .
N2 V3 N4 149.5(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.345(14) .
C1 C2 1.399(18) .
C1 C6 1.452(16) .
C2 C3 1.342(19) .
C2 H2 0.9500 .
C3 C4 1.326(19) .
C3 H3 0.9500 .
C4 C5 1.396(17) .
C4 H4 0.9500 .
C5 C6 1.383(16) .
C5 H5 0.9500 .
C6 C7 1.448(16) .
C7 O2 1.311(12) .
C7 N1 1.314(14) .
C8 N2 1.311(13) .
C8 O3 1.325(14) .
C8 C9 1.452(16) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C11 O5 1.354(12) .
C11 C12 1.391(14) .
C11 C16 1.414(14) .
C12 C13 1.356(14) .
C12 H12 0.9500 .
C13 C14 1.395(15) .
C13 H13 0.9500 .
C14 C15 1.372(15) .
C14 H14 0.9500 .
C15 C16 1.399(14) .
C15 H15 0.9500 .
C16 C17 1.434(14) .
C17 O6 1.300(12) .
C17 N3 1.316(12) .
C18 O7 1.282(13) .
C18 N4 1.306(13) .
C18 C19 1.504(15) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C21 C22 1.420(17) .
C21 O4 1.59(2) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 O8 1.431(12) .
C23 C24 1.511(16) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
N1 N2 1.433(12) .
N1 V1 2.075(9) .
N2 V3 2.063(9) .
N3 N4 1.406(11) .
N3 V2 2.069(8) .
N4 V3 2.060(9) .
O1 V1 1.820(10) .
O2 V3 1.938(7) .
O3 V1 1.982(9) .
O4 V1 1.770(9) .
O5 V2 1.803(7) .
O6 V3 1.952(7) .
O7 V2 1.984(7) .
O8 V2 1.829(6) .
O8 V2 2.343(7) 2_665
O10 V1 1.603(9) .
O20 V2 1.569(7) .
O30 V3 1.580(7) .
V2 O8 2.343(7) 2_665
