Impact of anionic co-ligands on nuclearity and single-molecule magnetism in a {CoIII2DyIII} trimeric and two {CoIII2DyIII2} tetrameric complexes
Panja, Anangamohan; Jagličić, Zvonko; Jana, Narayan Ch.; Contesso, Scarlette; Nandy, Rakhi; Aravena, Daniel; New Journal of Chemistry 49 (2025) 7576–7588; doi:10.1039/D5NJ00766F

data_7063734
_publ_section_title
;
 Impact of anionic co-ligands on nuclearity and single-molecule magnetism
 in a {CoIII2DyIII} trimeric and two {CoIII2DyIII2} tetrameric complexes
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7576
_journal_page_last               7588
_journal_paper_doi               10.1039/D5NJ00766F
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety
'C48 H60 Co2 Dy N4 O16, 2(H2 O), 4(C H4 O), N O3, C2 H3 N'
_chemical_formula_sum            'C54 H83 Co2 Dy N6 O25'
_chemical_formula_weight         1496.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                102.619(2)
_cell_angle_beta                 101.993(2)
_cell_angle_gamma                97.689(2)
_cell_formula_units_Z            2
_cell_length_a                   12.9113(3)
_cell_length_b                   13.2394(3)
_cell_length_c                   19.7653(4)
_cell_measurement_reflns_used    29843
_cell_measurement_temperature    100.04(10)
_cell_measurement_theta_max      30.6490
_cell_measurement_theta_min      1.6710
_cell_volume                     3167.72(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.787
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -38.00   8.00   0.50    2.98    --    3.20 -23.00 157.00   92
  2  \w     31.00  69.00   0.50    2.98    --    3.20  23.00 -37.00   76
  3  \w      3.00  28.00   0.50    2.98    --   -4.45  23.00 -37.00   50
  4  \w    -71.00 -33.00   0.50    2.98    --   -4.45 -23.00 157.00   76
  5  \w    -64.00   2.00   0.50    2.98    --    3.20 -19.00 120.00  132
  6  \w    -42.00   7.00   0.50    2.98    --   -4.45 -77.00-150.00   98
  7  \w    -26.00  17.00   0.50    2.98    --   -4.45 -77.00 -90.00   86
  8  \w     -7.00  56.00   0.50    2.98    --   -4.45  37.00  60.00  126
  9  \w    -15.00  11.00   0.50    2.98    --   -4.45 -99.00 -30.00   52
 10  \w    -11.00  24.00   0.50    2.98    --   -4.45 -99.00  90.00   70
 11  \w    -28.00   5.00   0.50    2.98    --   -4.45  77.00   0.00   66
 12  \w    -70.00 -40.00   0.50    2.98    --   -4.45 -37.00-150.00   60
 13  \w    -39.00 -12.00   0.50    2.98    --   -4.45 -37.00-150.00   54
 14  \w     -2.00  28.00   0.50    2.98    --   -4.45 -99.00   0.00   60
 15  \w      5.00  62.00   0.50    2.98    --   -4.45  37.00 -60.00  114
 16  \w    -15.00  26.00   0.50    2.98    --   -4.45 -99.00  60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.682
_diffrn_reflns_theta_min         1.695
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light red'
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             1538
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.746
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         15455
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0474
_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/[\s^2^(Fo^2^)+(0.0540P)^2^+6.6910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11407
_reflns_number_total             15455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00766f2.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
'Adding full bibliography for 7063731--7063734.cif.'
_cod_database_code               7063734
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.719
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-H8
 0.87 with sigma of 0.01
 O21-H21A = O21-H21B
 0.87 with sigma of 0.02
 O22-H22A = O22-H22B
 0.87 with sigma of 0.02
 H16-H19
 2.4 with sigma of 0.02
 O19-H19
 0.9 with sigma of 0.02
 C25-H8
 1.923712 with sigma of 0.02
 Dy1-H8
 3.082931 with sigma of 0.02
 H21A-H21B
 1.38 with sigma of 0.04
 H22A-H22B
 1.38 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C56 \\sim C55 \\sim N6: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
Uanis(O26) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O13A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5A) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O26, N5, O23, O24
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O13A, C41, C40, O13
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5A, O5, C15, C16
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(O13)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(1)
 Sof(O13A)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Fixed Sof: O5(0.5) O24(0.7) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) O25(0.3)
 O5A(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5)
6.a Ternary CH refined with riding coordinates:
 C36(H36), C11(H11), C24(H24), C49(H49)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C23(H23A,H23B), C37(H37A,H37B), C48(H48A,H48B), C50(H50A,
 H50B), C25(H25A,H25B), C12(H12A,H12B), C35(H35A,H35B)
6.c Aromatic/amide H refined with riding coordinates:
 C47(H47), C9(H9), C22(H22), C7(H7), C29(H29), C4(H4A), C45(H45), C20(H20),
 C34(H34), C17(H17), C32(H32), C42(H42)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C6(H6A,H6B,H6C), C31(H31A,H31B,H31C), C52(H52A,H52B,
 H52C), C44(H44A,H44B,H44C), C53(H53A,H53B,H53C), C51(H51A,H51B,H51C), C54(H54A,
 H54B,H54C), C3(H3A,H3B,H3C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C),
 C56(H56A,H56B,H56C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C15(H15A,H15B,
 H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O12(H12), O4(H4), O16(H16), O18(H18), O19(H19), O20(H20A), O17(H17A)
;
_shelx_res_checksum              97910
_shelx_hkl_checksum              75496
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;