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#$Date: 2025-08-22 01:24:23 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301857 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/81/7118194.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_7118194
loop_
_publ_author_name
'Yutronkie, Nathan J.'
'Kühne, Irina A'
'Korobkov, Ilia'
'Brusso, Jaclyn L.'
'Murugesu, Muralee'
_publ_section_title
;
 Connecting mononuclear dysprosium single-molecule magnets to form
 dinuclear complexes via in situ ligand oxidation
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   4
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              677
_journal_page_last               680
_journal_paper_doi               10.1039/c5cc07629c
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C14 H13 Dy N8 O8 S'
_chemical_formula_weight         615.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                69.422(2)
_cell_angle_beta                 77.825(2)
_cell_angle_gamma                77.336(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3478(3)
_cell_length_b                   10.5315(4)
_cell_length_c                   11.3151(4)
_cell_measurement_reflns_used    6292
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.75
_cell_volume                     1006.50(6)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-03 (Sheldrick, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13612
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.325
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    3.878
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.605
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0542P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4299
_reflns_number_total             4926
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc07629c2.cif
_cod_data_source_block           mm486
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7118194
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.675
_shelx_estimated_absorpt_t_max   0.830
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy1 Dy 0.68061(2) 0.35665(2) 0.25639(2) 0.02416(8) Uani 1 1 d . .
S1 S 0.27455(12) 0.75001(11) 0.39860(11) 0.0304(2) Uani 1 1 d . .
O1 O 0.2762(4) 0.7303(3) 0.5357(3) 0.0377(7) Uani 1 1 d . .
O2 O 0.6019(3) 0.5534(3) 0.0689(3) 0.0329(7) Uani 1 1 d . .
O3 O 0.8200(3) 0.4369(4) 0.0406(3) 0.0392(8) Uani 1 1 d . .
O4 O 0.7258(4) 0.5906(4) -0.1213(3) 0.0542(10) Uani 1 1 d . .
O5 O 0.7817(4) 0.1136(3) 0.2881(3) 0.0359(7) Uani 1 1 d . .
O6 O 0.9401(3) 0.2475(3) 0.2515(3) 0.0357(7) Uani 1 1 d . .
O7 O 1.0115(4) 0.0275(4) 0.3093(4) 0.0567(11) Uani 1 1 d . .
O8 O 0.5929(4) 0.2720(3) 0.1170(3) 0.0406(8) Uani 1 1 d . .
H8A H 0.6519 0.2033 0.0825 0.061 Uiso 1 1 d R U
H8B H 0.5046 0.3169 0.0712 0.061 Uiso 1 1 d R U
N1 N 0.5023(4) 0.5263(3) 0.3375(3) 0.0249(7) Uani 1 1 d . .
N2 N 0.2445(4) 0.6005(4) 0.3991(4) 0.0322(8) Uani 1 1 d . .
N3 N 0.4480(4) 0.7613(4) 0.3313(4) 0.0337(8) Uani 1 1 d . .
N4 N 0.4388(4) 0.2823(4) 0.3635(3) 0.0280(7) Uani 1 1 d . .
N5 N 0.7879(4) 0.5541(4) 0.2514(3) 0.0266(7) Uani 1 1 d . .
N6 N 0.7169(4) 0.5283(4) -0.0079(4) 0.0352(9) Uani 1 1 d . .
N7 N 0.9135(4) 0.1271(4) 0.2832(4) 0.0332(8) Uani 1 1 d . .
N8 N 0.7293(7) 0.0983(6) -0.0308(6) 0.0720(16) Uani 1 1 d . .
C1 C 0.3582(4) 0.5100(4) 0.3765(4) 0.0254(8) Uani 1 1 d . .
C2 C 0.5366(5) 0.6516(4) 0.3179(4) 0.0244(8) Uani 1 1 d . .
C3 C 0.3241(5) 0.3735(4) 0.3926(4) 0.0260(8) Uani 1 1 d . .
C4 C 0.1825(5) 0.3413(5) 0.4393(4) 0.0331(9) Uani 1 1 d . .
H4A H 0.1032 0.4076 0.4596 0.040 Uiso 1 1 calc R U
C5 C 0.1593(5) 0.2104(6) 0.4558(5) 0.0401(11) Uani 1 1 d . .
H5A H 0.0631 0.1859 0.4857 0.048 Uiso 1 1 calc R U
C6 C 0.2767(6) 0.1167(5) 0.4284(5) 0.0396(11) Uani 1 1 d . .
H6A H 0.2634 0.0256 0.4416 0.047 Uiso 1 1 calc R U
C7 C 0.4136(5) 0.1556(5) 0.3818(5) 0.0344(10) Uani 1 1 d . .
H7A H 0.4940 0.0902 0.3617 0.041 Uiso 1 1 calc R U
C8 C 0.6957(5) 0.6644(4) 0.2730(4) 0.0269(8) Uani 1 1 d . .
C9 C 0.7488(6) 0.7845(5) 0.2565(5) 0.0358(10) Uani 1 1 d . .
H9A H 0.6829 0.8612 0.2727 0.043 Uiso 1 1 calc R U
C10 C 0.8963(6) 0.7909(5) 0.2169(5) 0.0413(11) Uani 1 1 d . .
H10A H 0.9337 0.8721 0.2050 0.050 Uiso 1 1 calc R U
C11 C 0.9913(6) 0.6779(5) 0.1942(5) 0.0390(11) Uani 1 1 d . .
H11A H 1.0942 0.6801 0.1665 0.047 Uiso 1 1 calc R U
C12 C 0.9314(5) 0.5615(5) 0.2131(5) 0.0336(10) Uani 1 1 d . .
H12A H 0.9958 0.4836 0.1979 0.040 Uiso 1 1 calc R U
C13 C 0.7198(7) 0.0080(7) -0.0580(6) 0.0549(15) Uani 1 1 d . .
C14 C 0.7074(9) -0.1088(8) -0.0892(7) 0.078(2) Uani 1 1 d . .
H14A H 0.6621 -0.1753 -0.0134 0.093 Uiso 1 1 calc R U
H14B H 0.8062 -0.1515 -0.1188 0.093 Uiso 1 1 calc R U
H14C H 0.6454 -0.0799 -0.1569 0.093 Uiso 1 1 calc R U
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'
Dy Dy -0.1892 4.4098 '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
O1 Dy1 O8 135.01(12) 2_666 .
O1 Dy1 O6 73.65(12) 2_666 .
O8 Dy1 O6 102.62(11) . .
O1 Dy1 O5 75.37(11) 2_666 .
O8 Dy1 O5 68.69(10) . .
O6 Dy1 O5 51.96(11) . .
O1 Dy1 N1 82.08(11) 2_666 .
O8 Dy1 N1 115.55(11) . .
O6 Dy1 N1 141.57(11) . .
O5 Dy1 N1 147.26(12) . .
O1 Dy1 O3 138.90(11) 2_666 .
O8 Dy1 O3 71.24(12) . .
O6 Dy1 O3 69.05(11) . .
O5 Dy1 O3 94.25(12) . .
N1 Dy1 O3 118.19(11) . .
O1 Dy1 N5 84.14(12) 2_666 .
O8 Dy1 N5 140.61(12) . .
O6 Dy1 N5 82.02(11) . .
O5 Dy1 N5 133.08(11) . .
N1 Dy1 N5 66.00(11) . .
O3 Dy1 N5 74.34(12) . .
O1 Dy1 N4 80.03(12) 2_666 .
O8 Dy1 N4 72.26(12) . .
O6 Dy1 N4 135.55(11) . .
O5 Dy1 N4 87.25(12) . .
N1 Dy1 N4 65.43(12) . .
O3 Dy1 N4 140.04(11) . .
N5 Dy1 N4 130.42(12) . .
O1 Dy1 O2 150.89(11) 2_666 .
O8 Dy1 O2 70.58(11) . .
O6 Dy1 O2 119.68(11) . .
O5 Dy1 O2 133.66(11) . .
N1 Dy1 O2 72.15(11) . .
O3 Dy1 O2 51.66(10) . .
N5 Dy1 O2 73.29(11) . .
N4 Dy1 O2 100.62(11) . .
O1 Dy1 N7 70.67(11) 2_666 .
O8 Dy1 N7 86.93(11) . .
O6 Dy1 N7 26.02(11) . .
O5 Dy1 N7 26.09(11) . .
N1 Dy1 N7 152.60(11) . .
O3 Dy1 N7 82.68(11) . .
N5 Dy1 N7 107.21(11) . .
N4 Dy1 N7 111.04(11) . .
O2 Dy1 N7 133.19(11) . .
O1 Dy1 N6 156.67(12) 2_666 .
O8 Dy1 N6 66.54(12) . .
O6 Dy1 N6 94.65(11) . .
O5 Dy1 N6 113.66(12) . .
N1 Dy1 N6 96.36(11) . .
O3 Dy1 N6 25.77(10) . .
N5 Dy1 N6 74.12(11) . .
N4 Dy1 N6 120.64(11) . .
O2 Dy1 N6 26.06(10) . .
N7 Dy1 N6 107.44(11) . .
O1 S1 N3 104.2(2) . .
O1 S1 N2 104.3(2) . .
N3 S1 N2 105.82(19) . .
S1 O1 Dy1 164.0(2) . 2_666
N6 O2 Dy1 94.6(2) . .
N6 O3 Dy1 96.4(3) . .
N7 O5 Dy1 95.0(2) . .
N7 O6 Dy1 95.4(2) . .
C1 N1 C2 117.4(3) . .
C1 N1 Dy1 120.5(3) . .
C2 N1 Dy1 120.5(3) . .
C1 N2 S1 118.9(3) . .
C2 N3 S1 119.2(3) . .
C7 N4 C3 117.9(4) . .
C7 N4 Dy1 121.7(3) . .
C3 N4 Dy1 120.0(3) . .
C12 N5 C8 118.8(4) . .
C12 N5 Dy1 121.8(3) . .
C8 N5 Dy1 118.9(3) . .
O4 N6 O3 122.5(4) . .
O4 N6 O2 120.9(4) . .
O3 N6 O2 116.6(4) . .
O4 N6 Dy1 173.3(3) . .
O3 N6 Dy1 57.8(2) . .
O2 N6 Dy1 59.4(2) . .
O7 N7 O6 121.3(4) . .
O7 N7 O5 121.6(4) . .
O6 N7 O5 117.0(3) . .
O7 N7 Dy1 172.6(3) . .
O6 N7 Dy1 58.57(19) . .
O5 N7 Dy1 58.94(19) . .
N2 C1 N1 128.3(4) . .
N2 C1 C3 115.8(4) . .
N1 C1 C3 115.9(3) . .
N3 C2 N1 128.4(4) . .
N3 C2 C8 116.5(4) . .
N1 C2 C8 115.2(3) . .
N4 C3 C4 122.4(4) . .
N4 C3 C1 116.2(4) . .
C4 C3 C1 121.4(4) . .
C5 C4 C3 118.4(4) . .
C6 C5 C4 119.2(5) . .
C5 C6 C7 119.3(5) . .
N4 C7 C6 122.7(4) . .
N5 C8 C9 121.1(4) . .
N5 C8 C2 117.3(4) . .
C9 C8 C2 121.5(4) . .
C10 C9 C8 119.4(5) . .
C9 C10 C11 119.6(4) . .
C10 C11 C12 118.0(5) . .
N5 C12 C11 123.0(4) . .
N8 C13 C14 178.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy1 O1 2.293(3) 2_666
Dy1 O8 2.411(3) .
Dy1 O6 2.444(3) .
Dy1 O5 2.452(3) .
Dy1 N1 2.452(3) .
Dy1 O3 2.463(3) .
Dy1 N5 2.478(3) .
Dy1 N4 2.479(4) .
Dy1 O2 2.497(3) .
Dy1 N7 2.851(3) .
Dy1 N6 2.893(4) .
S1 O1 1.494(3) .
S1 N3 1.650(4) .
S1 N2 1.656(4) .
O1 Dy1 2.293(3) 2_666
O2 N6 1.275(5) .
O3 N6 1.266(5) .
O4 N6 1.213(5) .
O5 N7 1.259(5) .
O6 N7 1.256(5) .
O7 N7 1.225(5) .
N1 C1 1.355(5) .
N1 C2 1.358(5) .
N2 C1 1.310(5) .
N3 C2 1.302(5) .
N4 C7 1.342(6) .
N4 C3 1.342(5) .
N5 C12 1.330(6) .
N5 C8 1.351(5) .
N8 C13 1.123(8) .
C1 C3 1.481(6) .
C2 C8 1.487(6) .
C3 C4 1.387(6) .
C4 C5 1.385(7) .
C5 C6 1.367(7) .
C6 C7 1.370(7) .
C8 C9 1.397(6) .
C9 C10 1.365(7) .
C10 C11 1.388(7) .
C11 C12 1.389(6) .
C13 C14 1.427(9) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
N3 S1 O1 Dy1 -65.8(9) 2_666
N2 S1 O1 Dy1 45.0(9) 2_666
O1 S1 N2 C1 -95.4(4) .
N3 S1 N2 C1 14.3(4) .
O1 S1 N3 C2 94.8(4) .
N2 S1 N3 C2 -14.9(4) .
Dy1 O3 N6 O4 -172.1(4) .
Dy1 O3 N6 O2 8.6(4) .
Dy1 O2 N6 O4 172.2(4) .
Dy1 O2 N6 O3 -8.4(4) .
Dy1 O6 N7 O7 -171.3(4) .
Dy1 O6 N7 O5 8.1(4) .
Dy1 O5 N7 O7 171.3(4) .
Dy1 O5 N7 O6 -8.0(4) .
S1 N2 C1 N1 -8.1(6) .
S1 N2 C1 C3 173.5(3) .
C2 N1 C1 N2 -0.4(6) .
Dy1 N1 C1 N2 -165.9(3) .
C2 N1 C1 C3 178.0(3) .
Dy1 N1 C1 C3 12.5(4) .
S1 N3 C2 N1 9.4(6) .
S1 N3 C2 C8 -171.9(3) .
C1 N1 C2 N3 -0.3(6) .
Dy1 N1 C2 N3 165.3(3) .
C1 N1 C2 C8 -179.0(3) .
Dy1 N1 C2 C8 -13.4(4) .
C7 N4 C3 C4 -0.6(6) .
Dy1 N4 C3 C4 172.6(3) .
C7 N4 C3 C1 177.3(4) .
Dy1 N4 C3 C1 -9.5(5) .
N2 C1 C3 N4 176.8(4) .
N1 C1 C3 N4 -1.8(5) .
N2 C1 C3 C4 -5.3(6) .
N1 C1 C3 C4 176.1(4) .
N4 C3 C4 C5 -0.2(6) .
C1 C3 C4 C5 -178.0(4) .
C3 C4 C5 C6 1.5(7) .
C4 C5 C6 C7 -1.9(7) .
C3 N4 C7 C6 0.1(7) .
Dy1 N4 C7 C6 -173.0(4) .
C5 C6 C7 N4 1.1(7) .
C12 N5 C8 C9 -0.4(6) .
Dy1 N5 C8 C9 -172.4(3) .
C12 N5 C8 C2 -179.0(4) .
Dy1 N5 C8 C2 9.1(5) .
N3 C2 C8 N5 -176.2(4) .
N1 C2 C8 N5 2.6(5) .
N3 C2 C8 C9 5.2(6) .
N1 C2 C8 C9 -175.9(4) .
N5 C8 C9 C10 0.5(7) .
C2 C8 C9 C10 179.0(4) .
C8 C9 C10 C11 -0.3(7) .
C9 C10 C11 C12 -0.1(8) .
C8 N5 C12 C11 0.0(7) .
Dy1 N5 C12 C11 171.8(4) .
C10 C11 C12 N5 0.2(7) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168350619
