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_7720813
_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 Ho N4'
_chemical_formula_sum            'C18 H18 Cl3 Ho N4'
_chemical_formula_weight         561.64
_chemical_name_systematic        MH3-017-HoCl
_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     dual
_audit_creation_date             2023-12-19
_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                 104.4010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.59630(10)
_cell_length_b                   16.17730(10)
_cell_length_c                   14.63440(10)
_cell_measurement_reflns_used    18712
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.5270
_cell_measurement_theta_min      3.1670
_cell_volume                     1971.19(3)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     36.00  82.00   0.50    0.05    --   47.26-125.00-180.00   92
  2  \w     49.00 101.00   0.50    0.06    --  113.25 -94.00 -90.00  104
  3  \w     86.00 111.00   0.50    0.06    --  113.25-125.00  30.00   50
  4  \w     71.00 106.00   0.50    0.06    --  113.25 -94.00   0.00   70
  5  \w     80.00 106.00   0.50    0.06    --  113.25 -94.00 -60.00   52
  6  \w     71.00 106.00   0.50    0.06    --  113.25 -94.00 -30.00   70
  7  \w     44.00  70.00   0.50    0.06    --  113.25 -94.00  60.00   52
  8  \w     75.00 101.00   0.50    0.06    --  113.25 -94.00  60.00   52
  9  \w     49.00  74.00   0.50    0.06    --  113.25 -97.00 106.06   50
 10  \w     50.00 101.00   0.50    0.06    --  113.25 -94.00 150.00  102
 11  \w     80.00 106.00   0.50    0.06    --  113.25 -97.00 106.06   52
 12  \w     45.00 100.00   0.50    0.06    --  113.25 -94.00 120.00  110
 13  \w     43.00 106.00   0.50    0.06    --  113.25 -94.00  30.00  126
 14  \w     44.00  70.00   0.50    0.06    --  113.25 -94.00 -30.00   52
 15  \w     49.00 106.00   0.50    0.06    --  113.25 -94.00-120.00  114
 16  \w     45.00 102.00   0.50    0.06    --  113.25 -94.00-180.00  114
 17  \w     42.00 106.00   0.50    0.06    --  113.25 -94.00-150.00  128
 18  \w     64.00  94.00   0.50    0.06    --  113.25 -77.00 -90.00   60
 19  \w     62.00  88.00   0.50    0.06    --  113.25 -77.00-150.00   52
 20  \w     46.00  71.00   0.50    0.06    --  113.25 -61.00-180.00   50
 21  \w     42.00  71.00   0.50    0.06    --  113.25 -61.00-120.00   58
 22  \w     42.00  71.00   0.50    0.06    --  113.25 -61.00 -90.00   58
 23  \w     46.00  71.00   0.50    0.06    --  113.25 -61.00 -60.00   50
 24  \w     45.00  77.00   0.50    0.06    --  113.25 -77.00  60.00   64
 25  \w    117.00 172.00   0.50    0.06    --  113.25  15.00 -30.00  110
 26  \w    138.00 163.00   0.50    0.06    --  113.25  77.00 120.00   50
 27  \w     97.00 136.00   0.50    0.06    --  113.25  77.00 120.00   78
 28  \w    103.00 139.00   0.50    0.06    --  113.25  61.00 120.00   72
 29  \w    107.00 135.00   0.50    0.06    --  113.25  61.00  30.00   56
 30  \w    123.00 161.00   0.50    0.06    --  113.25  45.00  60.00   76
 31  \w    102.00 172.00   0.50    0.06    --  113.25  45.00  90.00  140
 32  \w    143.00 178.00   0.50    0.06    --  113.25  61.00  30.00   70
 33  \w    102.00 178.00   0.50    0.06    --  113.25  45.00   0.00  152
 34  \w    101.00 171.00   0.50    0.06    --  113.25  30.00 -90.00  140
 35  \w    104.00 139.00   0.50    0.06    --  113.25  30.00-120.00   70
 36  \w    103.00 151.00   0.50    0.06    --  113.25  30.00-180.00   96
 37  \w    122.00 178.00   0.50    0.06    --  113.25  45.00-180.00  112
 38  \w     27.00 120.00   0.50    0.05    --   47.26  77.00-120.00  186
 39  \w    -70.00 -15.00   0.50    0.05    --  -47.26  77.00  60.00  110
 40  \w    -61.00  22.00   0.50    0.05    --  -47.26  57.00-150.00  166
 41  \w    -20.00  24.00   0.50    0.05    --  -47.26  38.00 -30.00   88
 42  \w      0.00  25.00   0.50    0.05    --  -47.26  77.00  60.00   50
 43  \w    -51.00 -21.00   0.50    0.06    --  -91.75  45.00  30.00   60
 44  \w    -51.00 -24.00   0.50    0.06    --  -91.75  45.00  90.00   54
 45  \w    -51.00 -20.00   0.50    0.06    --  -91.75  45.00  60.00   62
 46  \w    -50.00 -24.00   0.50    0.06    --  -91.75  45.00-120.00   52
 47  \w   -162.00-127.00   0.50    0.06    --  -91.75 -45.00 -90.00   70
 48  \w   -104.00 -79.00   0.50    0.06    --  -91.75 -45.00 -90.00   50
 49  \w    -44.00 -16.00   0.50    0.05    --  -47.26 125.00 120.00   56
 50  \w    -83.00 -47.00   0.50    0.05    --  -47.26 125.00 120.00   72
;
_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      -0.1475567000
_diffrn_orient_matrix_UB_12      0.0554264000
_diffrn_orient_matrix_UB_13      -0.0049936000
_diffrn_orient_matrix_UB_21      -0.0371255000
_diffrn_orient_matrix_UB_22      -0.0010240000
_diffrn_orient_matrix_UB_23      -0.1085407000
_diffrn_orient_matrix_UB_31      -0.1053329000
_diffrn_orient_matrix_UB_32      -0.0774093000
_diffrn_orient_matrix_UB_33      -0.0021669000
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.019
_diffrn_reflns_theta_min         4.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.311
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.893
_exptl_crystal_description       needle
_exptl_crystal_F_000             1088
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.00092(7)
_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   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+2.0591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4193
_reflns_number_total             4278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3-017-hocl_auto_redabs
_cod_database_code               7720813
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18N4Cl3HoH18
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.193
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C13(H13A,H13B)
1.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              2679
_ins_header
;
TITL MH3-017-HoCl_auto_REDABS in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   8.596259  16.177291  14.634369  90.0000 104.4008  90.0000
ZERR    4.00   0.000055   0.000089   0.000096   0.0000   0.0007   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N Cl Ho
UNIT 72.00 72.00 16.00 12.00 4.00
REM  CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0
TEMP -173
SIZE 0.03 0.06 0.22
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id MH3-017-HoCl
_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 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.682