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#$Date: 2025-08-21 01:01:10 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301838 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/51/4325123.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_4325123
loop_
_publ_author_name
'Richard A. Lewis'
'Guang Wu'
'Trevor W. Hayton'
_publ_section_title
;
 Stabilizing High-Valent Metal Ions with a Ketimide Ligand Set: Synthesis
 of Mn(N=CtBu2)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4660
_journal_page_last               4668
_journal_paper_doi               10.1021/ic200490v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C54 H108 Mn3 N6'
_chemical_formula_weight         1006.28
_chemical_name_systematic
; 
  di(Manganese (II) ketimide) Manganese (II) tetrakis(bistert-butyl ketimide) 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 133.615(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.201(4)
_cell_length_b                   11.2776(15)
_cell_length_c                   22.819(3)
_cell_measurement_temperature    150(2)
_cell_volume                     5999.5(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       omega
_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  0.1096
_diffrn_reflns_av_sigmaI/netI    0.1397
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            24543
_diffrn_reflns_theta_full        26.64
_diffrn_reflns_theta_max         26.64
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618333
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       brown
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0624
_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)+(0.0000P)²+22.1316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                3345
_reflns_number_total             6175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200490v_si_002_5.cif
_cod_data_source_block           Complex_6
_cod_original_cell_volume        5999.6(14)
_cod_database_code               4325123
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Mn1 Mn 0.0000 0.85307(8) 0.2500 0.0236(2) Uani 1 2 d S
Mn2 Mn 0.10232(3) 0.89214(6) 0.28672(4) 0.0274(2) Uani 1 1 d .
N2 N 0.07883(15) 0.9361(3) 0.34689(19) 0.0276(8) Uani 1 1 d .
N3 N 0.03692(15) 0.7707(3) 0.21141(19) 0.0272(8) Uani 1 1 d .
C19 C 0.03046(18) 0.6862(4) 0.1687(2) 0.0284(10) Uani 1 1 d .
N1 N 0.15367(15) 0.9846(3) 0.2922(2) 0.0327(9) Uani 1 1 d .
C2 C 0.24503(19) 1.0222(4) 0.3334(3) 0.0352(11) Uani 1 1 d .
C24 C 0.07916(19) 0.6638(4) 0.1701(3) 0.0334(11) Uani 1 1 d .
C10 C 0.10650(18) 0.9863(3) 0.4155(2) 0.0265(10) Uani 1 1 d .
C1 C 0.18420(19) 1.0579(4) 0.2942(2) 0.0300(10) Uani 1 1 d .
C7 C 0.1351(2) 1.2342(4) 0.2902(3) 0.0537(15) Uani 1 1 d .
H7A H 0.1142 1.3059 0.2621 0.081 Uiso 1 1 calc R
H7B H 0.1666 1.2511 0.3466 0.081 Uiso 1 1 calc R
H7C H 0.1101 1.1774 0.2839 0.081 Uiso 1 1 calc R
C17 C 0.2063(2) 1.0712(4) 0.5001(3) 0.0467(13) Uani 1 1 d .
H17A H 0.2465 1.0531 0.5404 0.070 Uiso 1 1 calc R
H17B H 0.1984 1.1367 0.5180 0.070 Uiso 1 1 calc R
H17C H 0.1955 1.0917 0.4503 0.070 Uiso 1 1 calc R
C16 C 0.1914(2) 0.8583(4) 0.4681(3) 0.0407(12) Uani 1 1 d .
H16A H 0.1903 0.8803 0.4264 0.061 Uiso 1 1 calc R
H16B H 0.1662 0.7922 0.4501 0.061 Uiso 1 1 calc R
H16C H 0.2298 0.8367 0.5161 0.061 Uiso 1 1 calc R
C6 C 0.1579(2) 1.1839(4) 0.2552(3) 0.0349(11) Uani 1 1 d .
C3 C 0.2567(2) 0.8932(4) 0.3596(4) 0.0551(15) Uani 1 1 d .
H3A H 0.2557 0.8828 0.4004 0.083 Uiso 1 1 calc R
H3B H 0.2939 0.8711 0.3812 0.083 Uiso 1 1 calc R
H3C H 0.2280 0.8440 0.3138 0.083 Uiso 1 1 calc R
C26 C 0.0825(2) 0.7736(5) 0.1333(3) 0.0521(14) Uani 1 1 d .
H26A H 0.0890 0.8430 0.1630 0.078 Uiso 1 1 calc R
H26B H 0.0470 0.7820 0.0777 0.078 Uiso 1 1 calc R
H26C H 0.1134 0.7641 0.1361 0.078 Uiso 1 1 calc R
C25 C 0.1357(2) 0.6467(5) 0.2574(3) 0.0448(13) Uani 1 1 d .
H25A H 0.1325 0.5803 0.2805 0.067 Uiso 1 1 calc R
H25B H 0.1445 0.7168 0.2880 0.067 Uiso 1 1 calc R
H25C H 0.1657 0.6320 0.2587 0.067 Uiso 1 1 calc R
C27 C 0.0745(2) 0.5559(5) 0.1242(4) 0.0620(17) Uani 1 1 d .
H27A H 0.1039 0.5606 0.1234 0.093 Uiso 1 1 calc R
H27B H 0.0375 0.5558 0.0697 0.093 Uiso 1 1 calc R
H27C H 0.0792 0.4842 0.1509 0.093 Uiso 1 1 calc R
C15 C 0.17197(19) 0.9630(4) 0.4866(2) 0.0322(11) Uani 1 1 d .
C18 C 0.1872(2) 0.9287(5) 0.5649(3) 0.0477(13) Uani 1 1 d .
H18A H 0.2277 0.9148 0.6073 0.072 Uiso 1 1 calc R
H18B H 0.1668 0.8580 0.5557 0.072 Uiso 1 1 calc R
H18C H 0.1765 0.9920 0.5804 0.072 Uiso 1 1 calc R
C9 C 0.1960(3) 1.2808(5) 0.2663(4) 0.0700(19) Uani 1 1 d .
H9A H 0.1753 1.3545 0.2455 0.105 Uiso 1 1 calc R
H9B H 0.2067 1.2595 0.2375 0.105 Uiso 1 1 calc R
H9C H 0.2299 1.2895 0.3228 0.105 Uiso 1 1 calc R
C8 C 0.1075(3) 1.1637(5) 0.1649(3) 0.0658(17) Uani 1 1 d .
H8A H 0.0828 1.1037 0.1569 0.099 Uiso 1 1 calc R
H8B H 0.1215 1.1384 0.1410 0.099 Uiso 1 1 calc R
H8C H 0.0864 1.2362 0.1399 0.099 Uiso 1 1 calc R
C4 C 0.2516(3) 1.0319(6) 0.2733(5) 0.087(2) Uani 1 1 d .
H4A H 0.2869 0.9951 0.2959 0.131 Uiso 1 1 calc R
H4B H 0.2520 1.1139 0.2626 0.131 Uiso 1 1 calc R
H4C H 0.2200 0.9927 0.2238 0.131 Uiso 1 1 calc R
C5 C 0.2906(2) 1.0963(6) 0.4084(4) 0.090(3) Uani 1 1 d .
H5A H 0.2850 1.0925 0.4445 0.135 Uiso 1 1 calc R
H5B H 0.2877 1.1772 0.3928 0.135 Uiso 1 1 calc R
H5C H 0.3280 1.0660 0.4351 0.135 Uiso 1 1 calc R
C11 C 0.07351(18) 1.0679(4) 0.4276(2) 0.0288(10) Uani 1 1 d .
C20 C -0.02534(19) 0.6097(4) 0.1142(3) 0.0352(11) Uani 1 1 d .
C12 C 0.0223(2) 1.1245(4) 0.3466(3) 0.0446(13) Uani 1 1 d .
H12A H -0.0037 1.0636 0.3087 0.067 Uiso 1 1 calc R
H12B H 0.0355 1.1684 0.3261 0.067 Uiso 1 1 calc R
H12C H 0.0029 1.1771 0.3542 0.067 Uiso 1 1 calc R
C13 C 0.0506(2) 0.9915(4) 0.4559(3) 0.0435(13) Uani 1 1 d .
H13A H 0.0822 0.9622 0.5094 0.065 Uiso 1 1 calc R
H13B H 0.0293 0.9259 0.4195 0.065 Uiso 1 1 calc R
H13C H 0.0260 1.0386 0.4565 0.065 Uiso 1 1 calc R
C14 C 0.1071(2) 1.1728(4) 0.4850(3) 0.0429(13) Uani 1 1 d .
H14A H 0.0834 1.2157 0.4890 0.064 Uiso 1 1 calc R
H14B H 0.1183 1.2243 0.4645 0.064 Uiso 1 1 calc R
H14C H 0.1407 1.1443 0.5376 0.064 Uiso 1 1 calc R
C22 C -0.0586(2) 0.6361(5) 0.0245(3) 0.0528(15) Uani 1 1 d .
H22A H -0.0925 0.5877 -0.0100 0.079 Uiso 1 1 calc R
H22B H -0.0346 0.6186 0.0147 0.079 Uiso 1 1 calc R
H22C H -0.0694 0.7182 0.0132 0.079 Uiso 1 1 calc R
C23 C -0.0643(2) 0.6439(5) 0.1264(3) 0.0508(15) Uani 1 1 d .
H23A H -0.0995 0.6002 0.0894 0.076 Uiso 1 1 calc R
H23B H -0.0723 0.7273 0.1167 0.076 Uiso 1 1 calc R
H23C H -0.0458 0.6259 0.1810 0.076 Uiso 1 1 calc R
C21 C -0.0129(3) 0.4759(4) 0.1323(4) 0.0618(17) Uani 1 1 d .
H21A H 0.0150 0.4636 0.1898 0.093 Uiso 1 1 calc R
H21B H 0.0017 0.4460 0.1101 0.093 Uiso 1 1 calc R
H21C H -0.0477 0.4350 0.1083 0.093 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'
Mn Mn 0.3368 0.7283 '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 Mn1 N2 127.38(19) . 2
N2 Mn1 N3 111.88(13) . 2
N2 Mn1 N3 90.91(13) 2 2
N2 Mn1 N3 90.91(13) . .
N2 Mn1 N3 111.88(13) 2 .
N3 Mn1 N3 128.03(18) 2 .
N2 Mn1 Mn2 123.77(10) . 2
N2 Mn1 Mn2 46.01(10) 2 2
N3 Mn1 Mn2 46.89(9) 2 2
N3 Mn1 Mn2 145.12(9) . 2
N2 Mn1 Mn2 46.01(10) . .
N2 Mn1 Mn2 123.77(10) 2 .
N3 Mn1 Mn2 145.12(9) 2 .
N3 Mn1 Mn2 46.89(9) . .
Mn2 Mn1 Mn2 162.01(4) 2 .
N1 Mn2 N2 122.57(15) . .
N1 Mn2 N3 139.97(15) . .
N2 Mn2 N3 94.75(14) . .
N1 Mn2 Mn1 153.96(12) . .
N2 Mn2 Mn1 48.39(10) . .
N3 Mn2 Mn1 48.50(10) . .
C10 N2 Mn2 131.6(3) . .
C10 N2 Mn1 142.7(3) . .
Mn2 N2 Mn1 85.60(13) . .
C19 N3 Mn2 131.9(3) . .
C19 N3 Mn1 143.4(3) . .
Mn2 N3 Mn1 84.60(12) . .
N3 C19 C20 121.0(4) . .
N3 C19 C24 118.1(4) . .
C20 C19 C24 120.9(4) . .
C1 N1 Mn2 172.5(4) . .
C3 C2 C5 107.4(4) . .
C3 C2 C4 105.8(4) . .
C5 C2 C4 110.2(5) . .
C3 C2 C1 110.4(4) . .
C5 C2 C1 111.2(4) . .
C4 C2 C1 111.6(4) . .
C25 C24 C26 110.2(4) . .
C25 C24 C27 104.8(4) . .
C26 C24 C27 105.9(4) . .
C25 C24 C19 108.9(4) . .
C26 C24 C19 107.8(4) . .
C27 C24 C19 119.0(4) . .
N2 C10 C15 119.9(4) . .
N2 C10 C11 119.4(4) . .
C15 C10 C11 120.7(3) . .
N1 C1 C2 119.7(4) . .
N1 C1 C6 118.0(4) . .
C2 C1 C6 122.3(4) . .
C7 C6 C8 108.5(4) . .
C7 C6 C9 105.6(4) . .
C8 C6 C9 108.4(4) . .
C7 C6 C1 107.7(4) . .
C8 C6 C1 106.6(4) . .
C9 C6 C1 119.6(4) . .
C16 C15 C17 107.2(4) . .
C16 C15 C18 105.3(4) . .
C17 C15 C18 111.1(4) . .
C16 C15 C10 111.2(3) . .
C17 C15 C10 110.2(4) . .
C18 C15 C10 111.6(4) . .
C14 C11 C12 104.4(4) . .
C14 C11 C13 109.6(4) . .
C12 C11 C13 108.2(4) . .
C14 C11 C10 116.2(4) . .
C12 C11 C10 109.2(3) . .
C13 C11 C10 109.0(4) . .
C23 C20 C21 107.2(4) . .
C23 C20 C22 106.8(4) . .
C21 C20 C22 110.9(4) . .
C23 C20 C19 110.9(3) . .
C21 C20 C19 112.6(4) . .
C22 C20 C19 108.3(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N2 2.113(3) .
Mn1 N2 2.113(3) 2
Mn1 N3 2.120(3) 2
Mn1 N3 2.120(3) .
Mn1 Mn2 2.8183(8) 2
Mn1 Mn2 2.8183(8) .
Mn2 N1 1.885(4) .
Mn2 N2 2.034(4) .
Mn2 N3 2.067(3) .
N2 C10 1.281(5) .
N3 C19 1.273(5) .
C19 C20 1.561(6) .
C19 C24 1.567(6) .
N1 C1 1.260(5) .
C2 C3 1.518(6) .
C2 C5 1.522(7) .
C2 C4 1.527(7) .
C2 C1 1.544(6) .
C24 C25 1.522(6) .
C24 C26 1.540(7) .
C24 C27 1.545(6) .
C10 C15 1.558(6) .
C10 C11 1.568(6) .
C1 C6 1.577(6) .
C7 C6 1.520(7) .
C17 C15 1.529(6) .
C16 C15 1.525(6) .
C6 C8 1.522(7) .
C6 C9 1.528(7) .
C15 C18 1.541(6) .
C11 C14 1.526(6) .
C11 C12 1.530(6) .
C11 C13 1.536(6) .
C20 C23 1.510(7) .
C20 C21 1.542(7) .
C20 C22 1.549(7) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139135720
