Correlating luminescence and single-molecule magnetism for two series of heteroleptic lanthanoid complexes.
González, Jonay; Fagundes, Vinicius K.; Hay, Moya A.; Dallerba, Elena; Massi, Massimiliano; Hall, Christopher R.; Giansiracusa, Marcus J.; Boskovic, Colette; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1792–1805; doi:10.1039/d5dt02364e

data_7720804
_publ_section_title
;
 Correlating luminescence and single-molecule magnetism for two series of
 heteroleptic lanthanoid complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1792
_journal_page_last               1805
_journal_paper_doi               10.1039/d5dt02364e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C18 H18 Cl3 Dy N4'
_chemical_formula_sum            'C18 H18 Cl3 Dy N4'
_chemical_formula_weight         559.21
_chemical_name_systematic        MH3-017-DyCl
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-12-04 deposited with the CCDC.	2025-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.4710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.60610(10)
_cell_length_b                   16.21160(10)
_cell_length_c                   14.63640(10)
_cell_measurement_reflns_used    22971
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4510
_cell_measurement_theta_min      2.7460
_cell_volume                     1977.27(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_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    -86.00 -16.00   0.50    0.06    --  -47.56 125.00-150.00  140
  2  \w    -85.00 -19.00   0.50    0.25    --  -91.75 125.00-120.00  132
  3  \w   -119.00 -35.00   0.50    0.06    --  -47.56 -45.00   1.70  168
  4  \w   -119.00 -34.00   0.50    0.06    --  -47.56 -44.00  51.01  170
  5  \w   -119.00 -35.00   0.50    0.06    --  -47.56 -45.00 151.59  168
  6  \w   -121.00 -51.00   0.50    0.06    --  -47.56 -37.00  90.00  140
  7  \w   -119.00 -34.00   0.50    0.06    --  -47.56 -44.00 -81.26  170
  8  \w   -119.00 -34.00   0.50    0.06    --  -47.56 -44.00-158.94  170
  9  \w   -165.00 -79.00   0.50    0.25    --  -91.75 -35.00-132.10  172
 10  \w   -163.00 -91.00   0.50    0.25    --  -91.75 -49.00-146.28  144
 11  \w   -163.00-103.00   0.50    0.25    --  -91.75 -57.00 -90.00  120
 12  \w   -163.00 -95.00   0.50    0.25    --  -91.75 -51.00  15.70  136
 13  \w   -163.00-110.00   0.50    0.25    --  -91.75 -77.00 120.00  106
 14  \w   -163.00-106.00   0.50    0.25    --  -91.75 -99.00   0.00  114
 15  \w   -163.00 -94.00   0.50    0.25    --  -91.75-125.00 -60.00  138
 16  \w   -163.00-106.00   0.50    0.25    --  -91.75 -99.00  30.00  114
 17  \w    -72.00 -19.00   0.50    0.25    --  -91.75  57.00-120.00  106
 18  \w    -72.00 -19.00   0.50    0.25    --  -91.75  57.00   0.00  106
 19  \w    -72.00 -19.00   0.50    0.25    --  -91.75  57.00  60.00  106
 20  \w    -72.00 -19.00   0.50    0.25    --  -91.75  57.00 120.00  106
 21  \w    -44.00 -18.00   0.50    0.25    --  -91.75  37.00 150.00   52
 22  \w   -114.00 -19.00   0.50    0.25    --  -91.75  77.00  60.00  190
 23  \w    -44.00 -18.00   0.50    0.25    --  -91.75  37.00   0.00   52
 24  \w    -44.00 -18.00   0.50    0.25    --  -91.75  37.00 -30.00   52
 25  \w    -44.00 -18.00   0.50    0.25    --  -91.75  37.00-150.00   52
 26  \w    -44.00 -18.00   0.50    0.25    --  -91.75  37.00-180.00   52
 27  \w    -62.00  25.00   0.50    0.06    --  -47.56  57.00-150.00  174
 28  \w    -21.00  28.00   0.50    0.06    --  -47.56  19.00-180.00   98
 29  \w    -21.00  28.00   0.50    0.06    --  -47.56  19.00 -60.00   98
 30  \w    -21.00  28.00   0.50    0.06    --  -47.56  19.00 -30.00   98
 31  \w    -21.00  28.00   0.50    0.06    --  -47.56  19.00  90.00   98
 32  \w    -26.00  34.00   0.50    0.06    --   47.56 -37.00  60.00  120
 33  \w     35.00 112.00   0.50    0.25    --  108.00-125.00 150.00  154
 34  \w     35.00 108.00   0.50    0.25    --  108.00-108.00 153.16  146
 35  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00  90.00  142
 36  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00   0.00  142
 37  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00 -30.00  142
 38  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00 -90.00  142
 39  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00-120.00  142
 40  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00-180.00  142
 41  \w     35.00 106.00   0.50    0.25    --  108.00 -99.00-150.00  142
 42  \w     36.00  62.00   0.50    0.25    --  108.00 -57.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0373319000
_diffrn_orient_matrix_UB_12      0.0904525000
_diffrn_orient_matrix_UB_13      -0.0297586000
_diffrn_orient_matrix_UB_21      0.0437729000
_diffrn_orient_matrix_UB_22      0.0262446000
_diffrn_orient_matrix_UB_23      0.1044740000
_diffrn_orient_matrix_UB_31      0.1757307000
_diffrn_orient_matrix_UB_32      0.0126900000
_diffrn_orient_matrix_UB_33      -0.0037029000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36893
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.976
_diffrn_reflns_theta_min         4.143
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_description       needle
_exptl_crystal_F_000             1084
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0471P)^2^+4.3872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3839
_reflns_number_total             4023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3_017dyclredabs
_cod_original_cell_volume        1977.26(3)
_cod_database_code               7720804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         DyC20H20N6Cl6
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C1(H1A,H1B), C7(H7A,H7B)
1.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C10(H10), C3(H3), C4(H4), C12(H12), C16(H16), C6(H6), C18(H18),
 C9(H9), C11(H11), C5(H5), C17(H17)
;
_shelx_res_checksum              86081
_olex2_submission_original_sample_id MH3-017-DyCl
_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 3.936
_oxdiff_exptl_absorpt_empirical_full_min 0.430