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#$Date: 2025-08-21 01:27:06 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301840 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/67/4346715.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_4346715
loop_
_publ_author_name
'Damon, Peter L.'
'Liss, Cameron J.'
'Lewis, Richard A.'
'Morochnik, Simona'
'Szpunar, David E.'
'Telser, Joshua'
'Hayton, Trevor W.'
_publ_section_title
;
 Quantifying the Electron Donor and Acceptor Abilities of the Ketimide
 Ligands in M(N═C(t)Bu2)4 (M = V, Nb, Ta).
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10081
_journal_page_last               10095
_journal_paper_doi               10.1021/acs.inorgchem.5b02017
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C36 H72 N4 V'
_chemical_formula_sum            'C36 H72 N4 V'
_chemical_formula_weight         611.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4644(7)
_cell_length_b                   15.4726(8)
_cell_length_c                   15.2508(9)
_cell_measurement_reflns_used    219
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      11.819
_cell_measurement_theta_min      0
_cell_volume                     3885.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega scan'
_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  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37185
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0402
_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)+(0.0480P)²+1.9906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                3191
_reflns_number_total             4378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02017_si_001.cif
_cod_data_source_block           complex1
_cod_database_code               4346715
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x+1/2, -y, z'
'-x, -y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'
'x-1/2, 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 0.42497(2) 0.2500 0.2500 0.01251(11) Uani 1 2 d S
N1 N 0.38058(8) 0.23892(9) 0.14006(9) 0.0161(3) Uani 1 1 d .
N2 N 0.46944(8) 0.14193(9) 0.26173(9) 0.0157(3) Uani 1 1 d .
C1 C 0.35271(10) 0.22861(10) 0.06384(11) 0.0159(3) Uani 1 1 d .
C2 C 0.25991(11) 0.22336(12) 0.04802(11) 0.0199(4) Uani 1 1 d .
C3 C 0.23039(12) 0.29779(13) -0.01080(13) 0.0299(5) Uani 1 1 d .
H3A H 0.1709 0.3006 -0.0091 0.045 Uiso 1 1 calc R
H3B H 0.2483 0.2877 -0.0712 0.045 Uiso 1 1 calc R
H3C H 0.2531 0.3525 0.0104 0.045 Uiso 1 1 calc R
C4 C 0.21630(11) 0.23260(13) 0.13619(12) 0.0264(4) Uani 1 1 d .
H4A H 0.1575 0.2284 0.1271 0.040 Uiso 1 1 calc R
H4B H 0.2294 0.2889 0.1621 0.040 Uiso 1 1 calc R
H4C H 0.2341 0.1865 0.1758 0.040 Uiso 1 1 calc R
C5 C 0.23546(13) 0.13550(13) 0.00896(13) 0.0311(5) Uani 1 1 d .
H5A H 0.2525 0.0891 0.0487 0.047 Uiso 1 1 calc R
H5B H 0.2619 0.1279 -0.0481 0.047 Uiso 1 1 calc R
H5C H 0.1764 0.1335 0.0014 0.047 Uiso 1 1 calc R
C6 C 0.41783(11) 0.21609(12) -0.01009(11) 0.0211(4) Uani 1 1 d .
C7 C 0.38956(12) 0.23271(12) -0.10455(11) 0.0242(4) Uani 1 1 d .
H7A H 0.4346 0.2216 -0.1451 0.036 Uiso 1 1 calc R
H7B H 0.3720 0.2929 -0.1103 0.036 Uiso 1 1 calc R
H7C H 0.3441 0.1942 -0.1185 0.036 Uiso 1 1 calc R
C8 C 0.44864(14) 0.12287(14) -0.00144(13) 0.0363(5) Uani 1 1 d .
H8A H 0.4919 0.1127 -0.0444 0.054 Uiso 1 1 calc R
H8B H 0.4038 0.0826 -0.0122 0.054 Uiso 1 1 calc R
H8C H 0.4700 0.1137 0.0578 0.054 Uiso 1 1 calc R
C9 C 0.48849(12) 0.27828(16) 0.00711(14) 0.0378(5) Uani 1 1 d .
H9A H 0.5127 0.2654 0.0643 0.057 Uiso 1 1 calc R
H9B H 0.4684 0.3379 0.0068 0.057 Uiso 1 1 calc R
H9C H 0.5296 0.2713 -0.0388 0.057 Uiso 1 1 calc R
C10 C 0.49719(10) 0.06677(11) 0.27327(10) 0.0161(4) Uani 1 1 d .
C11 C 0.43194(11) -0.00574(11) 0.28639(13) 0.0223(4) Uani 1 1 d .
C12 C 0.3979(2) 0.00533(17) 0.37848(18) 0.0662(10) Uani 1 1 d .
H12A H 0.3754 0.0636 0.3848 0.099 Uiso 1 1 calc R
H12B H 0.4414 -0.0031 0.4215 0.099 Uiso 1 1 calc R
H12C H 0.3550 -0.0374 0.3885 0.099 Uiso 1 1 calc R
C13 C 0.36432(15) 0.00769(16) 0.2194(2) 0.0612(9) Uani 1 1 d .
H13A H 0.3215 -0.0353 0.2289 0.092 Uiso 1 1 calc R
H13B H 0.3864 0.0011 0.1601 0.092 Uiso 1 1 calc R
H13C H 0.3416 0.0659 0.2261 0.092 Uiso 1 1 calc R
C14 C 0.45962(13) -0.09943(12) 0.27415(15) 0.0347(5) Uani 1 1 d .
H14A H 0.5035 -0.1123 0.3156 0.052 Uiso 1 1 calc R
H14B H 0.4793 -0.1075 0.2141 0.052 Uiso 1 1 calc R
H14C H 0.4138 -0.1384 0.2849 0.052 Uiso 1 1 calc R
C15 C 0.59021(11) 0.05166(11) 0.27960(12) 0.0216(4) Uani 1 1 d .
C16 C 0.61979(13) -0.00996(15) 0.20756(17) 0.0431(6) Uani 1 1 d .
H16A H 0.5972 0.0081 0.1510 0.065 Uiso 1 1 calc R
H16B H 0.6018 -0.0689 0.2209 0.065 Uiso 1 1 calc R
H16C H 0.6792 -0.0084 0.2048 0.065 Uiso 1 1 calc R
C17 C 0.63417(11) 0.13763(12) 0.26577(13) 0.0271(4) Uani 1 1 d .
H17A H 0.6164 0.1791 0.3104 0.041 Uiso 1 1 calc R
H17B H 0.6214 0.1602 0.2073 0.041 Uiso 1 1 calc R
H17C H 0.6929 0.1287 0.2708 0.041 Uiso 1 1 calc R
C18 C 0.61327(14) 0.01801(14) 0.37058(15) 0.0384(5) Uani 1 1 d .
H18A H 0.6722 0.0098 0.3736 0.058 Uiso 1 1 calc R
H18B H 0.5860 -0.0373 0.3812 0.058 Uiso 1 1 calc R
H18C H 0.5964 0.0600 0.4152 0.058 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'
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
N2 V1 N2 132.94(9) . 2
N2 V1 N1 98.91(6) . 2
N2 V1 N1 99.37(6) 2 2
N2 V1 N1 99.37(6) . .
N2 V1 N1 98.91(6) 2 .
N1 V1 N1 133.12(9) 2 .
C1 N1 V1 177.23(13) . .
C10 N2 V1 176.74(13) . .
N1 C1 C2 120.64(15) . .
N1 C1 C6 115.47(15) . .
C2 C1 C6 123.78(14) . .
C4 C2 C5 107.45(15) . .
C4 C2 C3 107.09(15) . .
C5 C2 C3 110.68(15) . .
C4 C2 C1 108.72(14) . .
C5 C2 C1 111.41(15) . .
C3 C2 C1 111.30(14) . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C2 C5 H5A 109.5 . .
C2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C9 C6 C8 108.93(17) . .
C9 C6 C7 106.59(16) . .
C8 C6 C7 109.76(15) . .
C9 C6 C1 108.58(14) . .
C8 C6 C1 106.28(15) . .
C7 C6 C1 116.53(15) . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N2 C10 C15 120.31(15) . .
N2 C10 C11 115.45(15) . .
C15 C10 C11 124.12(15) . .
C12 C11 C13 109.5(2) . .
C12 C11 C14 109.19(18) . .
C13 C11 C14 105.34(17) . .
C12 C11 C10 106.85(16) . .
C13 C11 C10 108.50(15) . .
C14 C11 C10 117.29(16) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C17 C15 C18 107.68(16) . .
C17 C15 C16 106.95(16) . .
C18 C15 C16 111.04(18) . .
C17 C15 C10 109.12(14) . .
C18 C15 C10 110.65(16) . .
C16 C15 C10 111.24(15) . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 N2 1.8341(14) .
V1 N2 1.8341(14) 2
V1 N1 1.8370(14) 2
V1 N1 1.8371(14) .
N1 C1 1.260(2) .
N2 C10 1.262(2) .
C1 C2 1.549(2) .
C1 C6 1.568(2) .
C2 C4 1.531(2) .
C2 C5 1.538(3) .
C2 C3 1.539(3) .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C9 1.532(3) .
C6 C8 1.535(3) .
C6 C7 1.536(2) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C15 1.552(2) .
C10 C11 1.566(2) .
C11 C12 1.522(3) .
C11 C13 1.526(3) .
C11 C14 1.531(3) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 C17 1.529(2) .
C15 C18 1.530(3) .
C15 C16 1.534(3) .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168338529
