#------------------------------------------------------------------------------
#$Date: 2025-08-21 01:27:06 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301840 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/67/4346721.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_4346721
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 Ta'
_chemical_formula_sum            'C36 H72 N4 Ta'
_chemical_formula_weight         741.95
_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                   16.5585(15)
_cell_length_b                   15.5818(15)
_cell_length_c                   15.3453(15)
_cell_measurement_temperature    103(2)
_cell_volume                     3959.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18382
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    2.800
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0245
_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)+(0.0222P)²+0.1325P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0554
_reflns_number_gt                2944
_reflns_number_total             4945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02017_si_001.cif
_cod_data_source_block           complex7
_cod_database_code               4346721
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-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
Ta1 Ta 0.419248(8) 0.2500 0.7500 0.01084(5) Uani 1 2 d S
N2 N 0.36855(14) 0.26040(17) 0.63717(15) 0.0139(5) Uani 1 1 d .
N1 N 0.47031(14) 0.36112(15) 0.76104(17) 0.0143(6) Uani 1 1 d .
C1 C 0.50007(18) 0.43548(19) 0.77142(17) 0.0142(7) Uani 1 1 d .
C11 C 0.40267(19) 0.2813(2) 0.4871(2) 0.0200(7) Uani 1 1 d .
C9 C 0.4661(2) 0.60160(19) 0.7704(2) 0.0253(9) Uani 1 1 d .
H9A H 0.4834 0.6089 0.7098 0.038 Uiso 1 1 calc R
H9B H 0.5116 0.6136 0.8095 0.038 Uiso 1 1 calc R
H9C H 0.4218 0.6414 0.7831 0.038 Uiso 1 1 calc R
C2 C 0.59229(18) 0.4483(2) 0.7771(2) 0.0210(7) Uani 1 1 d .
C15 C 0.24690(19) 0.27761(19) 0.54762(19) 0.0186(7) Uani 1 1 d .
C17 C 0.2247(2) 0.3664(2) 0.5113(2) 0.0341(9) Uani 1 1 d .
H17A H 0.1658 0.3714 0.5070 0.051 Uiso 1 1 calc R
H17B H 0.2487 0.3735 0.4534 0.051 Uiso 1 1 calc R
H17C H 0.2454 0.4110 0.5504 0.051 Uiso 1 1 calc R
C6 C 0.43732(19) 0.5093(2) 0.7844(2) 0.0195(7) Uani 1 1 d .
C18 C 0.20477(18) 0.2681(2) 0.6358(2) 0.0245(9) Uani 1 1 d .
H18A H 0.1463 0.2742 0.6280 0.037 Uiso 1 1 calc R
H18B H 0.2243 0.3127 0.6757 0.037 Uiso 1 1 calc R
H18C H 0.2167 0.2114 0.6602 0.037 Uiso 1 1 calc R
C3 C 0.63446(19) 0.3619(2) 0.7646(2) 0.0263(9) Uani 1 1 d .
H3A H 0.6165 0.3218 0.8098 0.040 Uiso 1 1 calc R
H3B H 0.6930 0.3698 0.7688 0.040 Uiso 1 1 calc R
H3C H 0.6209 0.3387 0.7070 0.040 Uiso 1 1 calc R
C4 C 0.6224(2) 0.5087(3) 0.7046(3) 0.0470(12) Uani 1 1 d .
H4A H 0.6810 0.5025 0.6981 0.070 Uiso 1 1 calc R
H4B H 0.6096 0.5682 0.7200 0.070 Uiso 1 1 calc R
H4C H 0.5959 0.4940 0.6496 0.070 Uiso 1 1 calc R
C10 C 0.33938(18) 0.27008(17) 0.56130(19) 0.0136(7) Uani 1 1 d .
C12 C 0.3730(2) 0.26750(19) 0.39294(18) 0.0213(8) Uani 1 1 d .
H12A H 0.3280 0.3066 0.3808 0.032 Uiso 1 1 calc R
H12B H 0.3549 0.2080 0.3859 0.032 Uiso 1 1 calc R
H12C H 0.4173 0.2791 0.3522 0.032 Uiso 1 1 calc R
C14 C 0.4374(2) 0.3723(2) 0.4963(2) 0.0349(10) Uani 1 1 d .
H14A H 0.4805 0.3807 0.4534 0.052 Uiso 1 1 calc R
H14B H 0.4593 0.3798 0.5551 0.052 Uiso 1 1 calc R
H14C H 0.3945 0.4145 0.4862 0.052 Uiso 1 1 calc R
C16 C 0.2154(2) 0.2058(2) 0.4880(2) 0.0319(9) Uani 1 1 d .
H16A H 0.2382 0.1507 0.5065 0.048 Uiso 1 1 calc R
H16B H 0.2314 0.2176 0.4277 0.048 Uiso 1 1 calc R
H16C H 0.1563 0.2033 0.4918 0.048 Uiso 1 1 calc R
C13 C 0.4718(2) 0.2163(2) 0.5014(2) 0.0362(10) Uani 1 1 d .
H13A H 0.4500 0.1578 0.5002 0.054 Uiso 1 1 calc R
H13B H 0.4973 0.2270 0.5580 0.054 Uiso 1 1 calc R
H13C H 0.5121 0.2227 0.4550 0.054 Uiso 1 1 calc R
C7 C 0.3671(2) 0.4959(3) 0.7208(3) 0.0492(13) Uani 1 1 d .
H7A H 0.3271 0.5415 0.7290 0.074 Uiso 1 1 calc R
H7B H 0.3419 0.4401 0.7320 0.074 Uiso 1 1 calc R
H7C H 0.3875 0.4975 0.6609 0.074 Uiso 1 1 calc R
C8 C 0.4052(3) 0.5011(3) 0.8778(3) 0.0549(14) Uani 1 1 d .
H8A H 0.3622 0.5433 0.8872 0.082 Uiso 1 1 calc R
H8B H 0.4492 0.5115 0.9192 0.082 Uiso 1 1 calc R
H8C H 0.3836 0.4431 0.8866 0.082 Uiso 1 1 calc R
C5 C 0.6160(2) 0.4819(2) 0.8675(3) 0.0427(11) Uani 1 1 d .
H5A H 0.5981 0.4410 0.9121 0.064 Uiso 1 1 calc R
H5B H 0.5901 0.5376 0.8776 0.064 Uiso 1 1 calc R
H5C H 0.6747 0.4885 0.8706 0.064 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'
Ta Ta -0.7052 6.5227 '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 Ta1 N2 128.46(14) . 4_556
N2 Ta1 N1 100.75(11) . 4_556
N2 Ta1 N1 101.16(11) 4_556 4_556
N2 Ta1 N1 101.16(11) . .
N2 Ta1 N1 100.75(11) 4_556 .
N1 Ta1 N1 128.16(14) 4_556 .
C10 N2 Ta1 176.1(2) . .
C1 N1 Ta1 176.3(2) . .
N1 C1 C2 120.6(3) . .
N1 C1 C6 115.5(3) . .
C2 C1 C6 123.7(3) . .
C14 C11 C12 109.5(3) . .
C14 C11 C13 108.4(3) . .
C12 C11 C13 106.1(3) . .
C14 C11 C10 106.7(3) . .
C12 C11 C10 117.1(3) . .
C13 C11 C10 108.7(3) . .
C3 C2 C5 107.3(3) . .
C3 C2 C4 107.4(3) . .
C5 C2 C4 111.2(3) . .
C3 C2 C1 109.3(3) . .
C5 C2 C1 110.4(3) . .
C4 C2 C1 111.1(3) . .
C18 C15 C16 107.5(3) . .
C18 C15 C17 107.4(3) . .
C16 C15 C17 111.0(3) . .
C18 C15 C10 108.9(2) . .
C16 C15 C10 111.2(2) . .
C17 C15 C10 110.7(3) . .
C7 C6 C9 106.0(3) . .
C7 C6 C8 108.7(3) . .
C9 C6 C8 108.5(3) . .
C7 C6 C1 108.8(3) . .
C9 C6 C1 117.8(3) . .
C8 C6 C1 106.7(3) . .
N2 C10 C15 120.6(3) . .
N2 C10 C11 115.3(3) . .
C15 C10 C11 123.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta1 N2 1.931(2) .
Ta1 N2 1.931(2) 4_556
Ta1 N1 1.934(2) 4_556
Ta1 N1 1.934(2) .
N2 C10 1.269(3) .
N1 C1 1.269(4) .
C1 C2 1.542(4) .
C1 C6 1.563(4) .
C11 C14 1.536(4) .
C11 C12 1.541(4) .
C11 C13 1.545(5) .
C11 C10 1.558(4) .
C9 C6 1.530(4) .
C2 C3 1.529(4) .
C2 C5 1.534(5) .
C2 C4 1.540(5) .
C15 C18 1.530(4) .
C15 C16 1.536(4) .
C15 C17 1.536(4) .
C15 C10 1.550(4) .
C6 C7 1.531(5) .
C6 C8 1.534(5) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168338531
