Experimental and theoretical insights into magnetic exchange and anisotropy in multinuclear cobalt complexes displaying slow relaxation.
Jana, Narayan Ch; Čižmár, Erik; Brandão, Paula; Pramanik, Kuheli; Panja, Anangamohan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10403–10415; doi:10.1039/d5dt01197c

data_7718853
_publ_section_title
;
 Experimental and theoretical insights into magnetic exchange and
 anisotropy in multinuclear cobalt complexes displaying slow relaxation.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10403
_journal_page_last               10415
_journal_paper_doi               10.1039/d5dt01197c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C16 H17 N O3)'
_chemical_formula_sum            'C32 H34 N2 O6'
_chemical_formula_weight         542.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-18 deposited with the CCDC.	2025-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.339(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3196(12)
_cell_length_b                   7.1596(6)
_cell_length_c                   28.319(2)
_cell_measurement_reflns_used    5233
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      29.7510
_cell_measurement_theta_min      1.6230
_cell_volume                     2688.9(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_environment      N~2~
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.783
_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     16.00  66.00   0.50    7.42    --    1.32-146.00-177.00  100
  2  \w     16.00  62.00   0.50    7.42    --   -2.64-146.00-177.00   92
  3  \w    -15.00  32.00   0.50    7.42    --   -2.64 -99.00 120.00   94
  4  \w    -26.00  18.00   0.50    7.42    --   -2.64  77.00 -60.00   88
  5  \w    -64.00  -1.00   0.50    7.42    --   -2.64 -37.00-180.00  126
  6  \w    -22.00  20.00   0.50    7.42    --   -2.64  77.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0187519000
_diffrn_orient_matrix_UB_12      0.0381315000
_diffrn_orient_matrix_UB_13      -0.0221996000
_diffrn_orient_matrix_UB_21      0.0167552000
_diffrn_orient_matrix_UB_22      -0.0802472000
_diffrn_orient_matrix_UB_23      -0.0116718000
_diffrn_orient_matrix_UB_31      -0.0472175000
_diffrn_orient_matrix_UB_32      -0.0437253000
_diffrn_orient_matrix_UB_33      0.0020188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.783
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            23623
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.961
_diffrn_reflns_theta_min         1.757
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39197
_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 orange'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0662P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3932
_reflns_number_total             6113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01197c2.cif
_cod_data_source_block           H2L
_cod_depositor_comments
'Adding full bibliography for 7718853--7718856.cif.'
_cod_database_code               7718853
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C16A(H16C,H16D), C16B(H16A,H16B)
1.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C11B(H11B), C7B(H7B), C7A(H7A), C9B(H9B), C12A(H12A), C11A(H11A),
 C4B(H4B), C4A(H4A), C12B(H12B), C14A(H14A), C13A(H13A), C14B(H14B), C13B(H13B)
1.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC), C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,
 H6BC)
1.d Idealised tetrahedral OH refined as rotating group:
 O1B(H1B), O1A(H1A), O3B(H3B), O3A(H3A)
;
_shelx_res_checksum              951
_shelx_hkl_checksum              44886
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.669
_oxdiff_exptl_absorpt_empirical_full_min 0.531