#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329640.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_4329640
loop_
_publ_author_name
'Guoqi Zhang'
'Brian L. Scott'
'Ruilian Wu'
'L. A. Pete Silks'
'Susan K. Hanson'
_publ_section_title
;
 Aerobic Oxidation Reactions Catalyzed by Vanadium Complexes of
 Bis(Phenolate) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7354
_journal_page_last               7361
_journal_paper_doi               10.1021/ic3007525
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C52 H76 N4 O8 V2'
_chemical_formula_weight         987.05
_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                98.926(3)
_cell_angle_beta                 110.301(2)
_cell_angle_gamma                96.924(3)
_cell_formula_units_Z            1
_cell_length_a                   10.437(2)
_cell_length_b                   10.557(2)
_cell_length_c                   12.651(3)
_cell_measurement_temperature    120(1)
_cell_volume                     1268.4(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12067
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9588
_exptl_absorpt_correction_T_min  0.9588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0649P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                3337
_reflns_number_total             4561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3007525_si_002_2.cif
_cod_data_source_block           apx857
_cod_original_cell_volume        1268.6(5)
_cod_database_code               4329640
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 0.50747(5) 0.65694(5) 0.52360(4) 0.02072(18) Uani 1 1 d .
N1 N 0.6288(2) 0.7868(2) 0.4621(2) 0.0196(6) Uani 1 1 d .
N2 N 0.0680(3) 0.8473(3) 0.4879(3) 0.0456(8) Uani 1 1 d .
O1 O 0.4301(2) 0.76665(19) 0.56272(17) 0.0256(5) Uani 1 1 d .
O2 O 0.6745(2) 0.67044(19) 0.65648(16) 0.0223(5) Uani 1 1 d .
O3 O 0.5644(2) 0.50196(19) 0.43042(16) 0.0205(5) Uani 1 1 d .
O4 O 0.3338(2) 0.5912(2) 0.36202(17) 0.0240(5) Uani 1 1 d .
C1 C 0.7826(3) 0.7703(3) 0.7114(2) 0.0224(7) Uani 1 1 d .
C2 C 0.8809(3) 0.7611(3) 0.8162(2) 0.0235(7) Uani 1 1 d .
H2 H 0.8663 0.6886 0.8469 0.028 Uiso 1 1 calc R
C3 C 1.0001(3) 0.8557(3) 0.8767(2) 0.0246(7) Uani 1 1 d .
C4 C 1.0222(3) 0.9645(3) 0.8294(3) 0.0259(7) Uani 1 1 d .
C5 C 0.9230(3) 0.9736(3) 0.7264(3) 0.0249(7) Uani 1 1 d .
H5 H 0.9375 1.0461 0.6957 0.030 Uiso 1 1 calc R
C6 C 0.8024(3) 0.8802(3) 0.6660(3) 0.0218(7) Uani 1 1 d .
C8 C 1.1040(3) 0.8381(3) 0.9872(3) 0.0322(8) Uani 1 1 d .
H8A H 1.0692 0.7609 1.0076 0.048 Uiso 1 1 calc R
H8B H 1.1194 0.9126 1.0473 0.048 Uiso 1 1 calc R
H8C H 1.1901 0.8295 0.9776 0.048 Uiso 1 1 calc R
C9 C 1.1516(3) 1.0679(3) 0.8901(3) 0.0351(8) Uani 1 1 d .
H9A H 1.1496 1.1350 0.8466 0.053 Uiso 1 1 calc R
H9B H 1.2321 1.0293 0.8966 0.053 Uiso 1 1 calc R
H9C H 1.1557 1.1051 0.9656 0.053 Uiso 1 1 calc R
C7 C 0.6993(3) 0.9046(3) 0.5573(2) 0.0242(7) Uani 1 1 d .
H7A H 0.6286 0.9437 0.5764 0.029 Uiso 1 1 calc R
H7B H 0.7471 0.9678 0.5289 0.029 Uiso 1 1 calc R
C10 C 0.5315(3) 0.8270(3) 0.3597(2) 0.0231(7) Uani 1 1 d .
H10A H 0.4604 0.8613 0.3820 0.028 Uiso 1 1 calc R
H10B H 0.4854 0.7490 0.2999 0.028 Uiso 1 1 calc R
C11 C 0.5913(3) 0.9263(3) 0.3070(3) 0.0297(8) Uani 1 1 d .
H11A H 0.6585 0.8920 0.2791 0.036 Uiso 1 1 calc R
H11B H 0.6390 1.0053 0.3652 0.036 Uiso 1 1 calc R
C12 C 0.4762(3) 0.9580(3) 0.2077(3) 0.0314(8) Uani 1 1 d .
H12A H 0.4219 0.8785 0.1548 0.047 Uiso 1 1 calc R
H12B H 0.5166 1.0119 0.1685 0.047 Uiso 1 1 calc R
H12C H 0.4175 1.0037 0.2372 0.047 Uiso 1 1 calc R
C13 C 0.7385(3) 0.7266(3) 0.4333(2) 0.0203(7) Uani 1 1 d .
H13A H 0.7977 0.7930 0.4172 0.024 Uiso 1 1 calc R
H13B H 0.7959 0.6977 0.5002 0.024 Uiso 1 1 calc R
C14 C 0.6828(3) 0.6138(3) 0.3328(2) 0.0205(7) Uani 1 1 d .
C15 C 0.7220(3) 0.6121(3) 0.2377(3) 0.0229(7) Uani 1 1 d .
H15 H 0.7814 0.6847 0.2367 0.027 Uiso 1 1 calc R
C16 C 0.6764(3) 0.5069(3) 0.1448(2) 0.0231(7) Uani 1 1 d .
C17 C 0.5855(3) 0.3988(3) 0.1463(2) 0.0225(7) Uani 1 1 d .
C18 C 0.5463(3) 0.3990(3) 0.2404(2) 0.0216(7) Uani 1 1 d .
H18 H 0.4854 0.3271 0.2407 0.026 Uiso 1 1 calc R
C19 C 0.5955(3) 0.5038(3) 0.3342(2) 0.0194(7) Uani 1 1 d .
C20 C 0.7263(3) 0.5093(3) 0.0454(3) 0.0313(8) Uani 1 1 d .
H20A H 0.7825 0.4441 0.0434 0.047 Uiso 1 1 calc R
H20B H 0.7804 0.5938 0.0560 0.047 Uiso 1 1 calc R
H20C H 0.6475 0.4917 -0.0259 0.047 Uiso 1 1 calc R
C21 C 0.5310(3) 0.2822(3) 0.0478(3) 0.0314(8) Uani 1 1 d .
H21A H 0.4634 0.2218 0.0597 0.047 Uiso 1 1 calc R
H21B H 0.6064 0.2404 0.0438 0.047 Uiso 1 1 calc R
H21C H 0.4883 0.3098 -0.0230 0.047 Uiso 1 1 calc R
C22 C 0.1995(3) 0.6314(3) 0.3386(3) 0.0285(8) Uani 1 1 d .
H22 H 0.2156 0.7196 0.3845 0.034 Uiso 1 1 calc R
C24 C 0.1378(4) 0.6373(4) 0.2133(3) 0.0407(9) Uani 1 1 d .
H24A H 0.2042 0.6904 0.1940 0.061 Uiso 1 1 calc R
H24B H 0.0555 0.6745 0.1994 0.061 Uiso 1 1 calc R
H24C H 0.1143 0.5507 0.1667 0.061 Uiso 1 1 calc R
C23 C 0.1069(3) 0.5422(3) 0.3755(3) 0.0352(8) Uani 1 1 d .
H23A H 0.0847 0.4562 0.3281 0.053 Uiso 1 1 calc R
H23B H 0.0227 0.5749 0.3671 0.053 Uiso 1 1 calc R
H23C H 0.1541 0.5388 0.4547 0.053 Uiso 1 1 calc R
C25 C 0.1126(3) 0.8093(4) 0.5712(3) 0.0355(8) Uani 1 1 d .
C26 C 0.1691(4) 0.7595(4) 0.6730(3) 0.0428(9) Uani 1 1 d .
H26A H 0.1673 0.6677 0.6519 0.064 Uiso 1 1 calc R
H26B H 0.1147 0.7732 0.7198 0.064 Uiso 1 1 calc R
H26C H 0.2634 0.8041 0.7157 0.064 Uiso 1 1 calc R
H4 H 0.318(4) 0.496(4) 0.344(3) 0.080 Uiso 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 O2 104.67(10) . .
O1 V1 O3 104.28(9) . 2_666
O2 V1 O3 85.44(8) . 2_666
O1 V1 O3 164.96(9) . .
O2 V1 O3 90.37(8) . .
O3 V1 O3 76.46(8) 2_666 .
O1 V1 O4 90.12(9) . .
O2 V1 O4 164.49(8) . .
O3 V1 O4 86.40(8) 2_666 .
O3 V1 O4 74.89(8) . .
O1 V1 N1 94.36(10) . .
O2 V1 N1 87.57(9) . .
O3 V1 N1 161.20(9) 2_666 .
O3 V1 N1 86.16(8) . .
O4 V1 N1 96.06(8) . .
C7 N1 C13 108.2(2) . .
C7 N1 C10 109.2(2) . .
C13 N1 C10 111.2(2) . .
C7 N1 V1 107.12(17) . .
C13 N1 V1 112.50(17) . .
C10 N1 V1 108.47(17) . .
C1 O2 V1 130.24(18) . .
C19 O3 V1 126.22(17) . 2_666
C19 O3 V1 126.60(17) . .
V1 O3 V1 103.54(8) 2_666 .
C22 O4 V1 123.88(18) . .
O2 C1 C2 118.2(3) . .
O2 C1 C6 122.8(3) . .
C2 C1 C6 118.9(3) . .
C1 C2 C3 122.7(3) . .
C2 C3 C4 118.4(3) . .
C2 C3 C8 120.1(3) . .
C4 C3 C8 121.4(3) . .
C5 C4 C3 118.4(3) . .
C5 C4 C9 121.2(3) . .
C3 C4 C9 120.4(3) . .
C4 C5 C6 123.6(3) . .
C1 C6 C5 117.9(3) . .
C1 C6 C7 123.7(3) . .
C5 C6 C7 118.4(3) . .
N1 C7 C6 115.5(2) . .
N1 C10 C11 118.2(2) . .
C10 C11 C12 110.3(3) . .
C14 C13 N1 114.2(2) . .
C19 C14 C15 118.1(3) . .
C19 C14 C13 120.5(3) . .
C15 C14 C13 121.4(3) . .
C16 C15 C14 122.9(3) . .
C15 C16 C17 118.1(3) . .
C15 C16 C20 120.3(3) . .
C17 C16 C20 121.5(3) . .
C18 C17 C16 119.6(3) . .
C18 C17 C21 119.5(3) . .
C16 C17 C21 120.8(3) . .
C17 C18 C19 121.6(3) . .
O3 C19 C18 122.2(3) . .
O3 C19 C14 118.2(2) . .
C18 C19 C14 119.6(3) . .
O4 C22 C23 110.3(3) . .
O4 C22 C24 109.0(3) . .
C23 C22 C24 113.5(3) . .
N2 C25 C26 178.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O1 1.601(2) .
V1 O2 1.928(2) .
V1 O3 2.004(2) 2_666
V1 O3 2.131(2) .
V1 O4 2.152(2) .
V1 N1 2.164(2) .
N1 C7 1.496(4) .
N1 C13 1.497(3) .
N1 C10 1.501(4) .
N2 C25 1.150(4) .
O2 C1 1.345(3) .
O3 C19 1.367(3) .
O3 V1 2.004(2) 2_666
O4 C22 1.459(4) .
C1 C2 1.393(4) .
C1 C6 1.396(4) .
C2 C3 1.391(4) .
C3 C4 1.406(4) .
C3 C8 1.497(4) .
C4 C5 1.380(4) .
C4 C9 1.507(4) .
C5 C6 1.393(4) .
C6 C7 1.505(4) .
C10 C11 1.510(4) .
C11 C12 1.521(4) .
C13 C14 1.491(4) .
C14 C19 1.393(4) .
C14 C15 1.397(4) .
C15 C16 1.387(4) .
C16 C17 1.400(4) .
C16 C20 1.521(4) .
C17 C18 1.387(4) .
C17 C21 1.502(4) .
C18 C19 1.389(4) .
C22 C23 1.506(4) .
C22 C24 1.504(4) .
C25 C26 1.429(5) .
