#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:55:18 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179399 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/96/4329642.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_4329642
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            'C41 H52 N O5 V'
_chemical_formula_weight         689.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.287(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.606(2)
_cell_length_b                   19.171(3)
_cell_length_c                   14.294(2)
_cell_measurement_temperature    120(1)
_cell_volume                     3712.6(10)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (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 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.0868
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36407
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9578
_exptl_absorpt_correction_T_min  0.9519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7019
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0404P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                4368
_reflns_number_total             7019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3007525_si_002_4.cif
_cod_data_source_block           apx1403
_cod_original_cell_volume        3712.7(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329642
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.98809(4) 0.97514(2) 0.21022(3) 0.01797(13) Uani 1 1 d .
N1 N 0.99678(16) 1.09018(11) 0.23541(14) 0.0176(5) Uani 1 1 d .
O1 O 1.04040(13) 0.95644(9) 0.31058(12) 0.0219(5) Uani 1 1 d .
O2 O 0.96545(13) 0.89077(9) 0.16009(12) 0.0196(4) Uani 1 1 d .
O3 O 0.85474(13) 0.99138(9) 0.21052(12) 0.0179(4) Uani 1 1 d .
O4 O 1.07703(14) 0.99509(9) 0.12514(12) 0.0197(4) Uani 1 1 d .
O5 O 0.83013(14) 0.59546(9) 0.03273(13) 0.0247(5) Uani 1 1 d .
C1 C 0.8092(2) 1.02141(14) 0.28080(18) 0.0178(6) Uani 1 1 d .
C2 C 0.7294(2) 0.98830(13) 0.31858(19) 0.0189(6) Uani 1 1 d .
C3 C 0.6922(2) 1.02105(14) 0.39468(18) 0.0198(6) Uani 1 1 d .
H3 H 0.6397 0.9999 0.4209 0.024 Uiso 1 1 calc R
C4 C 0.7286(2) 1.08375(14) 0.43451(18) 0.0187(6) Uani 1 1 d .
C5 C 0.80208(19) 1.11636(14) 0.39057(18) 0.0185(6) Uani 1 1 d .
H5 H 0.8253 1.1595 0.4127 0.022 Uiso 1 1 calc R
C6 C 0.84282(19) 1.08643(13) 0.31344(18) 0.0164(6) Uani 1 1 d .
C7 C 0.9186(2) 1.12497(14) 0.26700(18) 0.0181(6) Uani 1 1 d .
C8 C 0.9098(2) 1.19719(13) 0.25934(18) 0.0196(6) Uani 1 1 d .
H8 H 0.8544 1.2195 0.2786 0.023 Uiso 1 1 calc R
C9 C 0.9827(2) 1.23548(14) 0.22353(19) 0.0215(7) Uani 1 1 d .
H9 H 0.9769 1.2836 0.2172 0.026 Uiso 1 1 calc R
C10 C 1.0642(2) 1.20138(13) 0.19719(19) 0.0197(6) Uani 1 1 d .
H10 H 1.1150 1.2267 0.1740 0.024 Uiso 1 1 calc R
C11 C 1.0718(2) 1.12896(13) 0.20493(18) 0.0176(6) Uani 1 1 d .
C12 C 1.1639(2) 1.09509(13) 0.18228(18) 0.0180(6) Uani 1 1 d .
C13 C 1.2530(2) 1.13145(14) 0.19832(19) 0.0211(7) Uani 1 1 d .
H13 H 1.2525 1.1755 0.2255 0.025 Uiso 1 1 calc R
C14 C 1.3412(2) 1.10447(14) 0.17542(19) 0.0210(7) Uani 1 1 d .
C15 C 1.3387(2) 1.03741(14) 0.13661(19) 0.0229(7) Uani 1 1 d .
H15 H 1.3978 1.0182 0.1211 0.027 Uiso 1 1 calc R
C16 C 1.2535(2) 0.99782(13) 0.11985(19) 0.0198(7) Uani 1 1 d .
C17 C 1.1651(2) 1.02801(14) 0.14283(18) 0.0176(6) Uani 1 1 d .
C18 C 0.6866(2) 0.91880(14) 0.2790(2) 0.0229(7) Uani 1 1 d .
C19 C 0.7654(2) 0.86123(13) 0.29191(19) 0.0229(7) Uani 1 1 d .
H19A H 0.8203 0.8733 0.2575 0.034 Uiso 1 1 calc R
H19B H 0.7376 0.8178 0.2689 0.034 Uiso 1 1 calc R
H19C H 0.7874 0.8567 0.3574 0.034 Uiso 1 1 calc R
C20 C 0.6508(2) 0.92655(14) 0.1746(2) 0.0279(7) Uani 1 1 d .
H20A H 0.6004 0.9616 0.1673 0.042 Uiso 1 1 calc R
H20B H 0.6245 0.8829 0.1509 0.042 Uiso 1 1 calc R
H20C H 0.7052 0.9400 0.1403 0.042 Uiso 1 1 calc R
C21 C 0.5982(2) 0.89552(15) 0.3300(2) 0.0318(8) Uani 1 1 d .
H21A H 0.6193 0.8869 0.3949 0.048 Uiso 1 1 calc R
H21B H 0.5710 0.8536 0.3016 0.048 Uiso 1 1 calc R
H21C H 0.5489 0.9315 0.3254 0.048 Uiso 1 1 calc R
C22 C 0.6864(2) 1.11279(14) 0.52270(19) 0.0234(7) Uani 1 1 d .
C23 C 0.6831(2) 1.05594(15) 0.5975(2) 0.0330(8) Uani 1 1 d .
H23A H 0.6422 1.0182 0.5729 0.049 Uiso 1 1 calc R
H23B H 0.6563 1.0750 0.6519 0.049 Uiso 1 1 calc R
H23C H 0.7486 1.0390 0.6148 0.049 Uiso 1 1 calc R
C24 C 0.5818(2) 1.13914(17) 0.4954(2) 0.0384(9) Uani 1 1 d .
H24A H 0.5837 1.1760 0.4503 0.058 Uiso 1 1 calc R
H24B H 0.5540 1.1563 0.5503 0.058 Uiso 1 1 calc R
H24C H 0.5419 1.1016 0.4686 0.058 Uiso 1 1 calc R
C25 C 0.7485(2) 1.17351(16) 0.5654(2) 0.0407(9) Uani 1 1 d .
H25A H 0.8150 1.1580 0.5815 0.061 Uiso 1 1 calc R
H25B H 0.7209 1.1898 0.6209 0.061 Uiso 1 1 calc R
H25C H 0.7485 1.2108 0.5206 0.061 Uiso 1 1 calc R
C26 C 1.4367(2) 1.14730(14) 0.1873(2) 0.0249(7) Uani 1 1 d .
C27 C 1.4378(2) 1.19632(15) 0.2726(2) 0.0336(8) Uani 1 1 d .
H27A H 1.3853 1.2297 0.2623 0.050 Uiso 1 1 calc R
H27B H 1.4999 1.2203 0.2808 0.050 Uiso 1 1 calc R
H27C H 1.4288 1.1695 0.3279 0.050 Uiso 1 1 calc R
C28 C 1.4428(2) 1.19119(16) 0.0984(2) 0.0404(9) Uani 1 1 d .
H28A H 1.4418 1.1610 0.0448 0.061 Uiso 1 1 calc R
H28B H 1.5030 1.2177 0.1039 0.061 Uiso 1 1 calc R
H28C H 1.3875 1.2224 0.0909 0.061 Uiso 1 1 calc R
C29 C 1.5283(2) 1.10120(15) 0.2022(2) 0.0380(9) Uani 1 1 d .
H29A H 1.5218 1.0702 0.2540 0.057 Uiso 1 1 calc R
H29B H 1.5857 1.1300 0.2157 0.057 Uiso 1 1 calc R
H29C H 1.5352 1.0745 0.1464 0.057 Uiso 1 1 calc R
C30 C 1.2570(2) 0.92315(14) 0.0785(2) 0.0223(7) Uani 1 1 d .
C31 C 1.3624(2) 0.90107(15) 0.0631(2) 0.0354(8) Uani 1 1 d .
H31A H 1.3615 0.8551 0.0364 0.053 Uiso 1 1 calc R
H31B H 1.4021 0.9009 0.1222 0.053 Uiso 1 1 calc R
H31C H 1.3897 0.9333 0.0211 0.053 Uiso 1 1 calc R
C32 C 1.1959(2) 0.92079(15) -0.01726(19) 0.0305(8) Uani 1 1 d .
H32A H 1.1954 0.8740 -0.0414 0.046 Uiso 1 1 calc R
H32B H 1.2247 0.9515 -0.0602 0.046 Uiso 1 1 calc R
H32C H 1.1295 0.9353 -0.0101 0.046 Uiso 1 1 calc R
C33 C 1.2167(2) 0.86981(13) 0.14529(19) 0.0246(7) Uani 1 1 d .
H33A H 1.1482 0.8792 0.1510 0.037 Uiso 1 1 calc R
H33B H 1.2530 0.8732 0.2060 0.037 Uiso 1 1 calc R
H33C H 1.2237 0.8237 0.1207 0.037 Uiso 1 1 calc R
C34 C 0.9186(2) 0.88263(14) 0.06648(19) 0.0238(7) Uani 1 1 d U
H34A H 0.9623 0.8985 0.0210 0.029 Uiso 1 1 calc R
H34B H 0.8586 0.9101 0.0588 0.029 Uiso 1 1 calc R
C35 C 0.8950(2) 0.80684(14) 0.05123(18) 0.0208(7) Uani 1 1 d .
C36 C 0.9673(2) 0.76004(14) 0.03031(19) 0.0217(7) Uani 1 1 d .
H36 H 1.0299 0.7767 0.0211 0.026 Uiso 1 1 calc R
C37 C 0.9491(2) 0.68922(14) 0.02279(18) 0.0196(6) Uani 1 1 d .
H37 H 0.9986 0.6587 0.0081 0.024 Uiso 1 1 calc R
C38 C 0.8563(2) 0.66431(14) 0.03737(18) 0.0193(7) Uani 1 1 d .
C39 C 0.7823(2) 0.71025(14) 0.05645(19) 0.0257(7) Uani 1 1 d .
H39 H 0.7195 0.6936 0.0649 0.031 Uiso 1 1 calc R
C40 C 0.8018(2) 0.78072(15) 0.06294(19) 0.0255(7) Uani 1 1 d .
H40 H 0.7516 0.8113 0.0754 0.031 Uiso 1 1 calc R
C41 C 0.9055(2) 0.54800(13) 0.0091(2) 0.0246(7) Uani 1 1 d U
H41A H 0.9249 0.5593 -0.0520 0.037 Uiso 1 1 calc R
H41B H 0.8805 0.5012 0.0088 0.037 Uiso 1 1 calc R
H41C H 0.9616 0.5518 0.0547 0.037 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'
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 O2 101.84(9)
O1 V1 O4 112.29(9)
O2 V1 O4 91.30(8)
O1 V1 O3 113.40(9)
O2 V1 O3 91.17(8)
O4 V1 O3 132.62(8)
O1 V1 N1 93.72(8)
O2 V1 N1 164.44(8)
O4 V1 N1 82.69(8)
O3 V1 N1 82.55(8)
C7 N1 C11 117.8(2)
C7 N1 V1 120.20(17)
C11 N1 V1 121.03(17)
C34 O2 V1 121.19(15)
C1 O3 V1 126.23(16)
C17 O4 V1 126.79(16)
C38 O5 C41 115.8(2)
O3 C1 C6 118.0(2)
O3 C1 C2 120.9(2)
C6 C1 C2 121.1(2)
C3 C2 C1 116.5(2)
C3 C2 C18 121.7(2)
C1 C2 C18 121.9(2)
C2 C3 C4 124.4(3)
C5 C4 C3 116.6(2)
C5 C4 C22 123.4(2)
C3 C4 C22 120.0(2)
C4 C5 C6 121.9(2)
C1 C6 C5 119.2(2)
C1 C6 C7 121.3(2)
C5 C6 C7 119.5(2)
N1 C7 C8 121.5(2)
N1 C7 C6 120.1(2)
C8 C7 C6 118.4(2)
C9 C8 C7 120.2(3)
C10 C9 C8 118.6(2)
C9 C10 C11 120.6(3)
N1 C11 C10 121.0(2)
N1 C11 C12 120.4(2)
C10 C11 C12 118.6(2)
C13 C12 C17 118.7(2)
C13 C12 C11 119.1(2)
C17 C12 C11 122.2(2)
C14 C13 C12 122.4(3)
C13 C14 C15 116.7(3)
C13 C14 C26 121.5(2)
C15 C14 C26 121.7(3)
C16 C15 C14 124.1(3)
C15 C16 C17 117.1(2)
C15 C16 C30 121.0(2)
C17 C16 C30 121.9(2)
O4 C17 C16 121.8(2)
O4 C17 C12 117.3(2)
C16 C17 C12 120.9(2)
C21 C18 C20 107.4(2)
C21 C18 C19 107.7(2)
C20 C18 C19 110.0(2)
C21 C18 C2 111.4(2)
C20 C18 C2 110.4(2)
C19 C18 C2 109.9(2)
C24 C22 C23 109.1(2)
C24 C22 C25 108.5(2)
C23 C22 C25 108.3(2)
C24 C22 C4 108.7(2)
C23 C22 C4 110.7(2)
C25 C22 C4 111.6(2)
C29 C26 C14 112.2(2)
C29 C26 C28 109.1(3)
C14 C26 C28 108.2(2)
C29 C26 C27 107.2(2)
C14 C26 C27 111.2(2)
C28 C26 C27 108.9(2)
C31 C30 C33 107.3(2)
C31 C30 C32 107.5(2)
C33 C30 C32 109.9(2)
C31 C30 C16 111.9(2)
C33 C30 C16 110.7(2)
C32 C30 C16 109.5(2)
O2 C34 C35 108.1(2)
C36 C35 C40 117.9(2)
C36 C35 C34 120.8(3)
C40 C35 C34 121.2(3)
C37 C36 C35 121.8(3)
C36 C37 C38 119.1(3)
O5 C38 C37 124.2(2)
O5 C38 C39 115.7(2)
C37 C38 C39 120.0(3)
C40 C39 C38 119.9(3)
C39 C40 C35 121.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 O1 1.5827(18)
V1 O2 1.7845(17)
V1 O4 1.8333(18)
V1 O3 1.8413(19)
V1 N1 2.236(2)
N1 C7 1.367(3)
N1 C11 1.366(3)
O2 C34 1.437(3)
O3 C1 1.356(3)
O4 C17 1.357(3)
O5 C38 1.367(3)
O5 C41 1.434(3)
C1 C6 1.393(4)
C1 C2 1.407(4)
C2 C3 1.391(4)
C2 C18 1.541(4)
C3 C4 1.401(4)
C4 C5 1.378(4)
C4 C22 1.537(4)
C5 C6 1.402(3)
C6 C7 1.475(4)
C7 C8 1.393(3)
C8 C9 1.370(4)
C9 C10 1.370(4)
C10 C11 1.396(3)
C11 C12 1.474(4)
C12 C13 1.399(4)
C12 C17 1.405(3)
C13 C14 1.374(4)
C14 C15 1.399(4)
C14 C26 1.533(4)
C15 C16 1.388(4)
C16 C17 1.400(4)
C16 C30 1.551(4)
C18 C21 1.529(4)
C18 C20 1.533(4)
C18 C19 1.538(4)
C22 C24 1.527(4)
C22 C23 1.531(4)
C22 C25 1.532(4)
C26 C29 1.527(4)
C26 C28 1.532(4)
C26 C27 1.538(4)
C30 C31 1.531(4)
C30 C33 1.534(4)
C30 C32 1.535(4)
C34 C35 1.500(4)
C35 C36 1.385(4)
C35 C40 1.387(4)
C36 C37 1.382(4)
C37 C38 1.384(4)
C38 C39 1.383(4)
C39 C40 1.378(4)
