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#$Date: 2025-08-20 17:59:05 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/20/4112084.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_4112084
loop_
_publ_author_name
'Lollita Lecren'
'Olivier Roubeau'
'Claude Coulon'
'Yang-Guang Li'
'Xavier F. Le Goff'
'Wolfgang Wernsdorfer'
'Hitoshi Miyasaka'
'Rodolphe Clérac'
_publ_section_title
;
 Slow Relaxation in a One-Dimensional Rational Assembly of
 Antiferromagnetically Coupled [Mn4] Single-Molecule Magnets
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17353
_journal_page_last               17363
_journal_paper_doi               10.1021/ja0551685
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C36 H48 Cl2 Mn4 N8 O26'
_chemical_formula_weight         1299.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                78.20(3)
_cell_angle_beta                 84.40(3)
_cell_angle_gamma                67.70(3)
_cell_formula_units_Z            1
_cell_length_a                   10.084(2)
_cell_length_b                   11.692(2)
_cell_length_c                   12.112(2)
_cell_measurement_temperature    150(1)
_cell_volume                     1293.0(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       CCD
_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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8569
_diffrn_reflns_theta_full        26.66
_diffrn_reflns_theta_max         26.66
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  0.6956
_exptl_absorpt_correction_T_min  0.5650
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(blessing, 1995, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       'parallelepipedic plate'
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5385
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1987
_reflns_number_gt                2948
_reflns_number_total             5385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0551685si20050729_012425.cif
_cod_data_source_block           l1
_cod_database_code               4112084
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 0.28067(8) 0.80960(8) -0.02307(7) 0.0412(3) Uani 1 1 d . . .
Mn2 Mn -0.01070(8) 1.02775(8) -0.13666(7) 0.0385(3) Uani 1 1 d . . .
O1 O 0.0371(3) 0.8777(3) -0.0151(3) 0.0367(8) Uani 1 1 d . . .
O2 O 0.1876(4) 0.9791(4) -0.1493(3) 0.0450(10) Uani 1 1 d . . .
O3 O -0.2115(3) 1.0875(4) -0.1184(3) 0.0417(9) Uani 1 1 d . . .
O13 O 0.6754(5) 0.7594(6) 0.0446(6) 0.102(2) Uani 1 1 d . . .
O11 O 0.4946(4) 0.7010(5) 0.0698(4) 0.0650(13) Uani 1 1 d . . .
O12 O 0.4850(5) 0.8613(5) -0.0543(5) 0.0694(13) Uani 1 1 d . . .
O1W O 0.3478(5) 0.7109(4) -0.1660(4) 0.0652(12) Uani 1 1 d . . .
H4AA H 0.3132 0.6408 -0.1636 0.098 Uiso 1 1 d R . .
H4AB H 0.3925 0.7237 -0.2146 0.098 Uiso 1 1 d R . .
O2W O 0.6931(9) 0.4749(10) 0.4207(7) 0.160(3) Uani 1 1 d . . .
H2WB H 0.6539 0.4794 0.3620 0.240 Uiso 1 1 d R . .
H2WA H 0.7336 0.5197 0.4347 0.240 Uiso 1 1 d R . .
O3W O 0.7287(7) 0.4773(6) 0.1953(6) 0.111(2) Uani 1 1 d . . .
H3WB H 0.6809 0.5439 0.1553 0.167 Uiso 1 1 d R . .
H3WA H 0.8133 0.4499 0.2135 0.167 Uiso 1 1 d R . .
Cl1 Cl 0.5341(3) 0.2307(3) 0.4723(2) 0.1007(8) Uani 1 1 d D . .
O7 O 0.6559(12) 0.2443(13) 0.5053(11) 0.209(5) Uani 1 1 d D A 1
O8 O 0.4094(18) 0.3397(15) 0.4382(17) 0.152(7) Uani 0.60 1 d PD A 1
O9 O 0.615(2) 0.158(3) 0.3979(19) 0.199(13) Uani 0.60 1 d PD A 1
O10 O 0.4758(9) 0.1515(11) 0.5556(8) 0.095(3) Uani 0.60 1 d P A 1
O8A O 0.473(3) 0.3638(18) 0.430(3) 0.172(15) Uani 0.40 1 d PDU A 2
O9A O 0.552(3) 0.175(2) 0.375(2) 0.100(7) Uani 0.40 1 d PDU A 2
O10A O 0.501(4) 0.243(4) 0.576(2) 0.239(16) Uani 0.40 1 d PDU A 2
N1 N 0.2204(4) 0.6412(5) 0.0561(4) 0.0430(11) Uani 1 1 d . . .
N2 N 0.0007(5) 1.1811(5) -0.2496(4) 0.0457(12) Uani 1 1 d . . .
N3 N -0.0661(5) 0.9469(5) -0.2656(4) 0.0501(12) Uani 1 1 d . . .
N4 N 0.5544(5) 0.7746(6) 0.0197(6) 0.0618(16) Uani 1 1 d . . .
C1 C 0.0811(5) 0.6570(5) 0.0523(5) 0.0401(13) Uani 1 1 d . . .
C2 C 0.0322(6) 0.5614(6) 0.0994(5) 0.0466(14) Uani 1 1 d . . .
H2A H -0.0644 0.5744 0.0966 0.056 Uiso 1 1 calc R . .
C3 C 0.1252(7) 0.4496(6) 0.1493(6) 0.0553(16) Uani 1 1 d . . .
H3B H 0.0933 0.3848 0.1810 0.066 Uiso 1 1 calc R . .
C4 C 0.2687(7) 0.4315(6) 0.1530(6) 0.0628(18) Uani 1 1 d . . .
H4A H 0.3347 0.3549 0.1872 0.075 Uiso 1 1 calc R . .
C5 C 0.3111(6) 0.5293(6) 0.1053(6) 0.0506(15) Uani 1 1 d . . .
H5A H 0.4076 0.5171 0.1072 0.061 Uiso 1 1 calc R . .
C6 C -0.0173(5) 0.7805(5) -0.0100(5) 0.0434(14) Uani 1 1 d . . .
H6A H -0.0291 0.7719 -0.0860 0.052 Uiso 1 1 calc R . .
H6B H -0.1107 0.8036 0.0275 0.052 Uiso 1 1 calc R . .
C7 C 0.1356(6) 1.1808(6) -0.2675(5) 0.0478(14) Uani 1 1 d . . .
C8 C 0.1605(7) 1.2832(7) -0.3280(5) 0.0578(17) Uani 1 1 d . . .
H8B H 0.2536 1.2819 -0.3387 0.069 Uiso 1 1 calc R . .
C9 C 0.0474(8) 1.3882(7) -0.3731(6) 0.070(2) Uani 1 1 d . . .
H9B H 0.0633 1.4589 -0.4130 0.084 Uiso 1 1 calc R . .
C10 C -0.0890(8) 1.3878(7) -0.3586(6) 0.070(2) Uani 1 1 d . . .
H10B H -0.1663 1.4576 -0.3898 0.083 Uiso 1 1 calc R . .
C11 C -0.1101(6) 1.2832(6) -0.2978(5) 0.0514(15) Uani 1 1 d . . .
H11B H -0.2024 1.2822 -0.2893 0.062 Uiso 1 1 calc R . .
C12 C 0.2495(6) 1.0610(6) -0.2165(6) 0.0565(17) Uani 1 1 d . . .
H12A H 0.3089 1.0205 -0.2760 0.068 Uiso 1 1 calc R . .
H12B H 0.3101 1.0790 -0.1705 0.068 Uiso 1 1 calc R . .
C13 C -0.2073(6) 0.9648(6) -0.2589(5) 0.0474(14) Uani 1 1 d . . .
C14 C -0.2635(8) 0.9143(8) -0.3273(7) 0.074(2) Uani 1 1 d . . .
H14A H -0.3609 0.9287 -0.3230 0.088 Uiso 1 1 calc R . .
C15 C -0.1766(9) 0.8435(9) -0.4012(8) 0.091(3) Uani 1 1 d . . .
H15A H -0.2130 0.8063 -0.4453 0.109 Uiso 1 1 calc R . .
C16 C -0.0342(9) 0.8280(9) -0.4095(7) 0.086(3) Uani 1 1 d . . .
H16A H 0.0266 0.7828 -0.4614 0.103 Uiso 1 1 calc R . .
C17 C 0.0163(8) 0.8798(7) -0.3409(6) 0.0668(19) Uani 1 1 d . . .
H17A H 0.1130 0.8681 -0.3465 0.080 Uiso 1 1 calc R . .
C18 C -0.2951(6) 1.0427(7) -0.1756(6) 0.0538(16) Uani 1 1 d . . .
H18A H -0.3724 1.1140 -0.2144 0.065 Uiso 1 1 calc R . .
H18B H -0.3375 0.9930 -0.1205 0.065 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'
Cl Cl 0.1484 0.1585 '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
O2 Mn1 O1W 85.67(17) . .
O2 Mn1 O3 93.21(15) . 2_575
O1W Mn1 O3 178.87(17) . 2_575
O2 Mn1 O1 69.37(13) . .
O1W Mn1 O1 105.76(15) . .
O3 Mn1 O1 73.88(13) 2_575 .
O2 Mn1 N1 135.46(15) . .
O1W Mn1 N1 83.09(17) . .
O3 Mn1 N1 97.78(16) 2_575 .
O1 Mn1 N1 72.59(14) . .
O2 Mn1 O11 138.07(16) . .
O1W Mn1 O11 94.52(18) . .
O3 Mn1 O11 86.27(16) 2_575 .
O1 Mn1 O11 147.95(16) . .
N1 Mn1 O11 85.84(17) . .
O2 Mn1 O12 83.67(16) . .
O1W Mn1 O12 88.81(18) . .
O3 Mn1 O12 91.00(16) 2_575 .
O1 Mn1 O12 147.81(16) . .
N1 Mn1 O12 138.73(17) . .
O11 Mn1 O12 54.45(17) . .
O2 Mn2 O3 175.39(17) . .
O2 Mn2 O1 82.75(15) . .
O3 Mn2 O1 98.52(16) . .
O2 Mn2 N2 81.11(18) . .
O3 Mn2 N2 96.99(18) . .
O1 Mn2 N2 162.08(16) . .
O2 Mn2 N3 104.50(18) . .
O3 Mn2 N3 79.77(16) . .
O1 Mn2 N3 97.79(17) . .
N2 Mn2 N3 93.75(19) . .
O2 Mn2 O1 95.85(15) . 2_575
O3 Mn2 O1 80.03(14) . 2_575
O1 Mn2 O1 80.56(15) . 2_575
N2 Mn2 O1 93.38(16) . 2_575
N3 Mn2 O1 159.24(15) . 2_575
C6 O1 Mn2 123.0(3) . .
C6 O1 Mn1 113.8(3) . .
Mn2 O1 Mn1 100.25(14) . .
C6 O1 Mn2 120.0(3) . 2_575
Mn2 O1 Mn2 99.44(15) . 2_575
Mn1 O1 Mn2 95.31(13) . 2_575
C12 O2 Mn2 120.0(3) . .
C12 O2 Mn1 131.2(3) . .
Mn2 O2 Mn1 107.63(17) . .
C18 O3 Mn2 120.3(3) . .
C18 O3 Mn1 127.5(3) . 2_575
Mn2 O3 Mn1 110.77(16) . 2_575
N4 O11 Mn1 94.6(4) . .
N4 O12 Mn1 94.0(4) . .
O10A Cl1 O9 148.2(19) . .
O10A Cl1 O7 78.9(18) . .
O9 Cl1 O7 90.4(11) . .
O10A Cl1 O9A 156(2) . .
O7 Cl1 O9A 115.7(12) . .
O10A Cl1 O8 89.2(18) . .
O9 Cl1 O8 121.7(14) . .
O7 Cl1 O8 119.8(11) . .
O9A Cl1 O8 98.3(14) . .
O10A Cl1 O8A 94.1(18) . .
O9 Cl1 O8A 116.0(19) . .
O7 Cl1 O8A 90.2(14) . .
O9A Cl1 O8A 104.2(17) . .
O10A Cl1 O10 54.0(17) . .
O9 Cl1 O10 106.9(13) . .
O7 Cl1 O10 115.4(7) . .
O9A Cl1 O10 102.1(12) . .
O8 Cl1 O10 102.7(9) . .
O8A Cl1 O10 129.6(15) . .
C5 N1 C1 117.9(5) . .
C5 N1 Mn1 125.5(4) . .
C1 N1 Mn1 116.7(4) . .
C7 N2 C11 118.8(5) . .
C7 N2 Mn2 113.5(4) . .
C11 N2 Mn2 127.4(4) . .
C17 N3 C13 118.0(6) . .
C17 N3 Mn2 130.9(4) . .
C13 N3 Mn2 111.0(4) . .
O13 N4 O12 122.8(6) . .
O13 N4 O11 120.4(7) . .
O12 N4 O11 116.9(5) . .
N1 C1 C2 121.5(5) . .
N1 C1 C6 117.0(5) . .
C2 C1 C6 121.4(5) . .
C3 C2 C1 119.7(5) . .
C2 C3 C4 119.5(6) . .
C5 C4 C3 118.3(6) . .
N1 C5 C4 123.1(6) . .
O1 C6 C1 111.6(4) . .
N2 C7 C8 121.1(6) . .
N2 C7 C12 114.2(5) . .
C8 C7 C12 124.7(5) . .
C7 C8 C9 119.8(6) . .
C10 C9 C8 119.5(7) . .
C9 C10 C11 119.2(7) . .
N2 C11 C10 121.5(6) . .
O2 C12 C7 110.5(4) . .
N3 C13 C14 120.7(6) . .
N3 C13 C18 115.9(5) . .
C14 C13 C18 123.4(6) . .
C15 C14 C13 120.1(7) . .
C14 C15 C16 118.9(7) . .
C17 C16 C15 118.9(7) . .
N3 C17 C16 123.3(7) . .
O3 C18 C13 112.1(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O2 2.185(4) .
Mn1 O1W 2.187(5) .
Mn1 O3 2.201(4) 2_575
Mn1 O1 2.275(3) .
Mn1 N1 2.277(5) .
Mn1 O11 2.312(5) .
Mn1 O12 2.336(4) .
Mn2 O2 1.860(3) .
Mn2 O3 1.881(3) .
Mn2 O1 1.980(4) .
Mn2 N2 2.055(5) .
Mn2 N3 2.195(5) .
Mn2 O1 2.277(4) 2_575
O1 C6 1.426(6) .
O1 Mn2 2.277(4) 2_575
O2 C12 1.415(7) .
O3 C18 1.436(7) .
O3 Mn1 2.201(4) 2_575
O13 N4 1.224(6) .
O11 N4 1.257(7) .
O12 N4 1.238(7) .
Cl1 O10A 1.30(2) .
Cl1 O9 1.356(17) .
Cl1 O7 1.401(9) .
Cl1 O9A 1.421(18) .
Cl1 O8 1.431(12) .
Cl1 O8A 1.441(19) .
Cl1 O10 1.462(9) .
N1 C5 1.335(7) .
N1 C1 1.350(6) .
N2 C7 1.355(7) .
N2 C11 1.358(8) .
N3 C17 1.337(8) .
N3 C13 1.355(7) .
C1 C2 1.386(8) .
C1 C6 1.501(8) .
C2 C3 1.346(9) .
C3 C4 1.385(8) .
C4 C5 1.369(9) .
C7 C8 1.367(9) .
C7 C12 1.492(9) .
C8 C9 1.374(10) .
C9 C10 1.371(10) .
C10 C11 1.372(10) .
C13 C14 1.379(9) .
C13 C18 1.490(8) .
C14 C15 1.362(11) .
C15 C16 1.374(11) .
C16 C17 1.356(10) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139118905
