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_7063733
_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         'C66 H56 Co2 Dy2 N8 O34, 2(O)'
_chemical_formula_sum            'C66 H56 Co2 Dy2 N8 O36'
_chemical_formula_weight         1980.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 90.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.9723(9)
_cell_length_b                   10.8697(3)
_cell_length_c                   24.8686(6)
_cell_measurement_reflns_used    17311
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      30.8480
_cell_measurement_theta_min      1.6450
_cell_volume                     7561.3(4)
_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      200.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.772
_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    -42.00  27.00   0.50    4.51    --    3.20 -77.00-110.00  138
  2  \w    -28.00  21.00   0.50    4.51    --   -4.60  77.00  16.00   98
  3  \w    -15.00  30.00   0.50    4.51    --   -4.60 -99.00-120.00   90
  4  \w    -28.00  16.00   0.50    4.51    --   -4.60  77.00 -90.00   88
  5  \w     -7.00  28.00   0.50    4.51    --   -4.60  37.00  90.00   70
  6  \w    -25.00  21.00   0.50    4.51    --   -4.60  77.00 150.00   92
;
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.772
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33460
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.772
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.590
_diffrn_reflns_theta_min         2.010
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40202
_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            'dark red'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8981
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0499P)^2^+17.8764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7824
_reflns_number_total             8981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00766f2.cif
_cod_data_source_block           complex-3
_cod_depositor_comments
'Adding full bibliography for 7063731--7063734.cif.'
_cod_database_code               7063733
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.637
_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
2. Restrained distances
 H4-O4
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O16 \\sim O18 \\sim O17: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008 within 1.7A
Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O19, O20
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O19(0.65) O20(0.35) O17(0.3) O18(0.7)
6.a Ternary CH refined with riding coordinates:
 C11(H11A)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4A), C19(H19), C29(H29), C15(H15), C33(H33), C31(H31), C30(H30),
 C7(H7), C22(H22), C26(H26), C16(H16), C25(H25), C17(H17), C24(H24)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              70040
_shelx_hkl_checksum              39932
_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
;