#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301814.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_4301814
loop_
_publ_author_name
'Hiroki Hiraga'
'Hitoshi Miyasaka'
'Rodolphe Clérac'
'Marc Fourmigué'
'Masahiro Yamashita'
_publ_section_title
;
[MIII(dmit)2]--Coordinated MnIIISalen-Type Dimers (MIII= NiIII, AuIII;
dmit2-= 1,3-Dithiol-2-thione-4,5-dithiolate): Design of Single-Component
Conducting Single-Molecule Magnet-Based Materials
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2887
_journal_page_last               2898
_journal_paper_doi               10.1021/ic802110b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C56 H52 Mn2 N4 Ni2 O4 S20'
_chemical_formula_weight         1713.52
_space_group_IT_number           2
_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                74.047(2)
_cell_angle_beta                 78.740(2)
_cell_angle_gamma                78.576(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6580(8)
_cell_length_b                   13.1671(11)
_cell_length_c                   15.1286(13)
_cell_measurement_temperature    120(2)
_cell_volume                     1607.1(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16953
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  0.6355
_exptl_absorpt_correction_T_min  0.4618
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0373
_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)+(0.0350P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                5322
_reflns_number_total             7380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802110b_si_002_3.cif
_cod_data_source_block           2a
_cod_original_cell_volume        1607.2(2)
_cod_database_code               4301814
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.93518(6) 0.49962(4) 0.11470(3) 0.01597(12) Uani 1 1 d . . .
O1 O 0.8363(3) 0.47903(17) 0.02131(15) 0.0178(5) Uani 1 1 d . . .
C1 C 0.7600(4) 0.3958(2) 0.0297(2) 0.0158(7) Uani 1 1 d . . .
C2 C 0.6483(4) 0.4055(3) -0.0277(2) 0.0177(7) Uani 1 1 d . . .
H1 H 0.6179 0.4729 -0.0681 0.021 Uiso 1 1 calc R . .
C3 C 0.5805(4) 0.3189(3) -0.0271(2) 0.0196(7) Uani 1 1 d . . .
H2 H 0.5036 0.3286 -0.0669 0.024 Uiso 1 1 calc R . .
C4 C 0.6210(4) 0.2175(3) 0.0300(2) 0.0182(7) Uani 1 1 d . . .
C5 C 0.5541(4) 0.1223(3) 0.0242(3) 0.0280(9) Uani 1 1 d . . .
H3 H 0.6227 0.0894 -0.0233 0.042 Uiso 1 1 calc R . .
H4 H 0.4465 0.1458 0.0076 0.042 Uiso 1 1 calc R . .
H5 H 0.5495 0.0700 0.0846 0.042 Uiso 1 1 calc R . .
C6 C 0.7239(4) 0.2095(3) 0.0901(2) 0.0183(7) Uani 1 1 d . . .
H6 H 0.7493 0.1424 0.1321 0.022 Uiso 1 1 calc R . .
C7 C 0.7943(4) 0.2959(3) 0.0926(2) 0.0169(7) Uani 1 1 d . . .
C8 C 0.9099(4) 0.2750(3) 0.1539(2) 0.0193(7) Uani 1 1 d . . .
H7 H 0.9346 0.2031 0.1879 0.023 Uiso 1 1 calc R . .
N1 N 0.9841(3) 0.3441(2) 0.16749(18) 0.0153(6) Uani 1 1 d . . .
C9 C 1.1238(4) 0.3083(2) 0.2197(2) 0.0177(7) Uani 1 1 d . . .
C10 C 1.2709(4) 0.3015(3) 0.1448(2) 0.0234(8) Uani 1 1 d . . .
H8 H 1.2616 0.2516 0.1092 0.035 Uiso 1 1 calc R . .
H9 H 1.3671 0.2763 0.1745 0.035 Uiso 1 1 calc R . .
H10 H 1.2779 0.3724 0.1028 0.035 Uiso 1 1 calc R . .
C11 C 1.1201(4) 0.1980(2) 0.2865(2) 0.0240(8) Uani 1 1 d . . .
H11 H 1.0134 0.1944 0.3225 0.036 Uiso 1 1 calc R . .
H12 H 1.1982 0.1855 0.3288 0.036 Uiso 1 1 calc R . .
H13 H 1.1465 0.1432 0.2509 0.036 Uiso 1 1 calc R . .
C12 C 1.1211(4) 0.3948(2) 0.2713(2) 0.0174(7) Uani 1 1 d . . .
C13 C 1.2835(4) 0.3911(3) 0.2970(2) 0.0222(8) Uani 1 1 d . . .
H14 H 1.3563 0.4183 0.2409 0.033 Uiso 1 1 calc R . .
H15 H 1.3260 0.3172 0.3259 0.033 Uiso 1 1 calc R . .
H16 H 1.2731 0.4355 0.3409 0.033 Uiso 1 1 calc R . .
C14 C 0.9981(4) 0.3828(3) 0.3594(2) 0.0247(8) Uani 1 1 d . . .
H17 H 0.9887 0.4442 0.3859 0.037 Uiso 1 1 calc R . .
H18 H 1.0320 0.3169 0.4048 0.037 Uiso 1 1 calc R . .
H19 H 0.8946 0.3796 0.3441 0.037 Uiso 1 1 calc R . .
N2 N 1.0681(3) 0.5006(2) 0.20662(18) 0.0148(6) Uani 1 1 d . . .
C15 C 1.0979(4) 0.5872(3) 0.2198(2) 0.0180(7) Uani 1 1 d . . .
H20 H 1.1633 0.5786 0.2657 0.022 Uiso 1 1 calc R . .
C16 C 1.0428(4) 0.6951(2) 0.1726(2) 0.0165(7) Uani 1 1 d . . .
C17 C 1.0870(4) 0.7774(3) 0.2007(2) 0.0209(8) Uani 1 1 d . . .
H21 H 1.1550 0.7591 0.2468 0.025 Uiso 1 1 calc R . .
C18 C 1.0347(4) 0.8833(3) 0.1636(2) 0.0207(8) Uani 1 1 d . . .
C19 C 1.0795(5) 0.9713(3) 0.1957(3) 0.0295(9) Uani 1 1 d . . .
H22 H 0.9977 0.9896 0.2459 0.044 Uiso 1 1 calc R . .
H23 H 1.0874 1.0345 0.1435 0.044 Uiso 1 1 calc R . .
H24 H 1.1824 0.9468 0.2183 0.044 Uiso 1 1 calc R . .
C20 C 0.9349(4) 0.9073(3) 0.0961(2) 0.0221(8) Uani 1 1 d . . .
H25 H 0.8952 0.9800 0.0705 0.026 Uiso 1 1 calc R . .
C21 C 0.8921(4) 0.8293(3) 0.0654(2) 0.0196(7) Uani 1 1 d . . .
H26 H 0.8259 0.8490 0.0183 0.024 Uiso 1 1 calc R . .
C22 C 0.9454(4) 0.7208(2) 0.1030(2) 0.0160(7) Uani 1 1 d . . .
O2 O 0.9010(3) 0.64793(16) 0.07190(15) 0.0178(5) Uani 1 1 d . . .
Ni1 Ni 0.67634(5) 0.96932(3) 0.38708(3) 0.02018(12) Uani 1 1 d . . .
S1 S 0.80016(11) 0.98681(7) 0.49090(6) 0.0268(2) Uani 1 1 d . . .
C23 C 0.7401(4) 1.1184(3) 0.4919(2) 0.0207(8) Uani 1 1 d . . .
S2 S 0.80266(11) 1.17682(7) 0.56636(6) 0.0250(2) Uani 1 1 d . . .
C24 C 0.6960(4) 1.3032(3) 0.5321(2) 0.0206(8) Uani 1 1 d . . .
S3 S 0.70214(11) 1.40382(7) 0.57542(6) 0.0269(2) Uani 1 1 d . . .
S4 S 0.58629(10) 1.31464(7) 0.44454(6) 0.0226(2) Uani 1 1 d . . .
C25 C 0.6402(4) 1.1839(3) 0.4329(2) 0.0204(8) Uani 1 1 d . . .
S5 S 0.57380(11) 1.13621(7) 0.35511(6) 0.0254(2) Uani 1 1 d . . .
S6 S 0.55612(11) 0.94936(7) 0.28117(6) 0.0248(2) Uani 1 1 d . . .
C26 C 0.6070(4) 0.8146(3) 0.2899(2) 0.0194(7) Uani 1 1 d . . .
S7 S 0.54937(11) 0.74867(7) 0.21964(6) 0.0227(2) Uani 1 1 d . . .
C27 C 0.6442(4) 0.6225(3) 0.2641(2) 0.0201(7) Uani 1 1 d . . .
S8 S 0.64599(10) 0.51615(7) 0.22312(6) 0.0223(2) Uani 1 1 d . . .
S9 S 0.73707(10) 0.61606(7) 0.35623(6) 0.0224(2) Uani 1 1 d . . .
C28 C 0.6996(4) 0.7505(3) 0.3536(2) 0.0197(7) Uani 1 1 d . . .
S10 S 0.77367(11) 0.80185(7) 0.42676(6) 0.0251(2) Uani 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'
S S 0.1246 0.1234 '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'
Ni Ni 0.3393 1.1124 '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
_geom_angle_publ_flag
O2 Mn1 O1 93.20(9) . . ?
O2 Mn1 N1 174.79(10) . . ?
O1 Mn1 N1 91.93(10) . . ?
O2 Mn1 N2 93.93(10) . . ?
O1 Mn1 N2 169.83(10) . . ?
N1 Mn1 N2 80.86(10) . . ?
O2 Mn1 S8 87.89(7) . . ?
O1 Mn1 S8 89.16(7) . . ?
N1 Mn1 S8 93.12(8) . . ?
N2 Mn1 S8 98.33(8) . . ?
C1 O1 Mn1 125.38(19) . . ?
O1 C1 C2 119.9(3) . . ?
O1 C1 C7 122.5(3) . . ?
C2 C1 C7 117.5(3) . . ?
C3 C2 C1 121.1(3) . . ?
C2 C3 C4 122.2(3) . . ?
C6 C4 C3 116.5(3) . . ?
C6 C4 C5 122.4(3) . . ?
C3 C4 C5 121.1(3) . . ?
C4 C6 C7 123.1(3) . . ?
C6 C7 C1 119.3(3) . . ?
C6 C7 C8 117.5(3) . . ?
C1 C7 C8 122.9(3) . . ?
N1 C8 C7 126.5(3) . . ?
C8 N1 C9 120.6(3) . . ?
C8 N1 Mn1 123.6(2) . . ?
C9 N1 Mn1 115.69(19) . . ?
N1 C9 C11 112.8(3) . . ?
N1 C9 C10 105.2(3) . . ?
C11 C9 C10 108.3(3) . . ?
N1 C9 C12 106.4(2) . . ?
C11 C9 C12 111.7(3) . . ?
C10 C9 C12 112.4(3) . . ?
N2 C12 C13 111.5(3) . . ?
N2 C12 C14 107.1(2) . . ?
C13 C12 C14 109.0(3) . . ?
N2 C12 C9 106.2(2) . . ?
C13 C12 C9 111.5(3) . . ?
C14 C12 C9 111.4(3) . . ?
C15 N2 C12 119.0(3) . . ?
C15 N2 Mn1 123.3(2) . . ?
C12 N2 Mn1 117.30(19) . . ?
N2 C15 C16 127.1(3) . . ?
C22 C16 C17 119.8(3) . . ?
C22 C16 C15 123.1(3) . . ?
C17 C16 C15 117.0(3) . . ?
C18 C17 C16 121.9(3) . . ?
C17 C18 C20 117.5(3) . . ?
C17 C18 C19 121.7(3) . . ?
C20 C18 C19 120.8(3) . . ?
C21 C20 C18 122.2(3) . . ?
C20 C21 C22 120.6(3) . . ?
O2 C22 C16 123.3(3) . . ?
O2 C22 C21 118.8(3) . . ?
C16 C22 C21 117.9(3) . . ?
C22 O2 Mn1 129.0(2) . . ?
S1 Ni1 S5 92.90(4) . . ?
S1 Ni1 S10 85.32(4) . . ?
S5 Ni1 S10 176.94(4) . . ?
S1 Ni1 S6 178.70(4) . . ?
S5 Ni1 S6 88.07(4) . . ?
S10 Ni1 S6 93.75(4) . . ?
C23 S1 Ni1 102.59(12) . . ?
C25 C23 S1 121.2(3) . . ?
C25 C23 S2 116.3(3) . . ?
S1 C23 S2 122.50(19) . . ?
C24 S2 C23 97.27(16) . . ?
S3 C24 S2 123.7(2) . . ?
S3 C24 S4 123.1(2) . . ?
S2 C24 S4 113.2(2) . . ?
C24 S4 C25 97.61(16) . . ?
C23 C25 S5 120.5(3) . . ?
C23 C25 S4 115.6(3) . . ?
S5 C25 S4 123.85(19) . . ?
C25 S5 Ni1 102.67(12) . . ?
C26 S6 Ni1 101.55(12) . . ?
C28 C26 S6 121.5(3) . . ?
C28 C26 S7 114.6(3) . . ?
S6 C26 S7 123.90(19) . . ?
C27 S7 C26 98.28(16) . . ?
S8 C27 S9 123.1(2) . . ?
S8 C27 S7 124.1(2) . . ?
S9 C27 S7 112.7(2) . . ?
C27 S8 Mn1 103.02(12) . . ?
C27 S9 C28 97.87(16) . . ?
C26 C28 S10 121.5(3) . . ?
C26 C28 S9 116.3(3) . . ?
S10 C28 S9 122.23(19) . . ?
C28 S10 Ni1 101.72(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O2 1.863(2) . ?
Mn1 O1 1.892(2) . ?
Mn1 N1 1.975(3) . ?
Mn1 N2 1.975(3) . ?
Mn1 S8 2.7172(10) . ?
O1 C1 1.353(4) . ?
C1 C2 1.387(4) . ?
C1 C7 1.411(4) . ?
C2 C3 1.379(4) . ?
C3 C4 1.397(4) . ?
C4 C6 1.362(4) . ?
C4 C5 1.511(4) . ?
C6 C7 1.405(4) . ?
C7 C8 1.431(4) . ?
C8 N1 1.291(4) . ?
N1 C9 1.501(4) . ?
C9 C11 1.526(4) . ?
C9 C10 1.537(5) . ?
C9 C12 1.543(4) . ?
C12 N2 1.511(4) . ?
C12 C13 1.519(4) . ?
C12 C14 1.527(5) . ?
N2 C15 1.291(4) . ?
C15 C16 1.436(4) . ?
C16 C22 1.404(4) . ?
C16 C17 1.408(4) . ?
C17 C18 1.373(4) . ?
C18 C20 1.395(5) . ?
C18 C19 1.513(5) . ?
C20 C21 1.374(5) . ?
C21 C22 1.404(4) . ?
C22 O2 1.325(4) . ?
Ni1 S1 2.1502(10) . ?
Ni1 S5 2.1590(10) . ?
Ni1 S10 2.1602(10) . ?
Ni1 S6 2.1704(10) . ?
S1 C23 1.711(3) . ?
C23 C25 1.368(4) . ?
C23 S2 1.742(3) . ?
S2 C24 1.731(3) . ?
C24 S3 1.645(4) . ?
C24 S4 1.734(3) . ?
S4 C25 1.740(3) . ?
C25 S5 1.710(3) . ?
S6 C26 1.715(3) . ?
C26 C28 1.368(4) . ?
C26 S7 1.738(3) . ?
S7 C27 1.717(3) . ?
C27 S8 1.677(4) . ?
C27 S9 1.715(3) . ?
S9 C28 1.727(3) . ?
C28 S10 1.718(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139126575
