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_7720815
_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 N4 Tm'
_chemical_formula_sum            'C18 H18 Cl3 N4 Tm'
_chemical_formula_weight         565.64
_chemical_name_systematic        MH3-017-TmCl
_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             2023-12-20
_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                 104.3090(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.56790(10)
_cell_length_b                   16.12840(10)
_cell_length_c                   14.62620(10)
_cell_measurement_reflns_used    17917
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.3440
_cell_measurement_theta_min      4.1360
_cell_volume                     1958.44(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      99.99(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 0.991
_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     43.00  84.00   0.50    0.05    --   47.51-125.00 120.00   82
  2  \w     61.00  94.00   0.50    0.05    --  113.25-125.00 120.00   66
  3  \w     44.00 108.00   0.50    0.05    --  113.25-108.00 112.42  128
  4  \w     72.00 107.00   0.50    0.05    --  113.25-104.00 163.24   70
  5  \w     48.00  74.00   0.50    0.05    --  113.25-125.00  60.00   52
  6  \w     48.00 106.00   0.50    0.05    --  113.25-105.00  48.19  116
  7  \w     51.00 103.00   0.50    0.05    --  113.25 -94.00 -60.00  104
  8  \w     59.00 103.00   0.50    0.05    --  113.25 -94.00 -30.00   88
  9  \w     65.00 103.00   0.50    0.05    --  113.25 -94.00 -90.00   76
 10  \w     42.00 106.00   0.50    0.05    --  113.25 -94.00-120.00  128
 11  \w     55.00 106.00   0.50    0.05    --  113.25 -94.00-150.00  102
 12  \w     42.00 105.00   0.50    0.05    --  113.25 -94.00-180.00  126
 13  \w     70.00 100.00   0.50    0.05    --  113.25 -94.00   0.00   60
 14  \w     72.00 100.00   0.50    0.05    --  113.25 -94.00  30.00   56
 15  \w     80.00 105.00   0.50    0.05    --  113.25 -94.00  90.00   50
 16  \w     53.00 106.00   0.50    0.05    --  113.25 -94.00 120.00  106
 17  \w    -22.00  30.00   0.50    0.05    --   47.51 -19.00 120.00  104
 18  \w     48.00  99.00   0.50    0.05    --  113.25 -77.00 120.00  102
 19  \w     42.00  75.00   0.50    0.05    --  113.25 -77.00 -30.00   66
 20  \w     42.00  71.00   0.50    0.05    --  113.25 -61.00 -90.00   58
 21  \w     46.00  71.00   0.50    0.05    --  113.25 -61.00-120.00   50
 22  \w    -20.00  59.00   0.50    0.05    --   47.51 -57.00-120.00  158
 23  \w    147.00 176.00   0.50    0.05    --  113.25  30.00 -30.00   58
 24  \w    122.00 148.00   0.50    0.05    --  113.25  77.00  30.00   52
 25  \w     91.00 118.00   0.50    0.05    --  113.25  77.00  30.00   54
 26  \w    107.00 178.00   0.50    0.05    --  113.25  45.00 150.00  142
 27  \w    103.00 164.00   0.50    0.05    --  113.25  61.00  90.00  122
 28  \w    103.00 163.00   0.50    0.05    --  113.25  45.00 120.00  120
 29  \w     99.00 160.00   0.50    0.05    --  113.25  61.00  60.00  122
 30  \w    131.00 160.00   0.50    0.05    --  113.25  45.00 -90.00   58
 31  \w    101.00 128.00   0.50    0.05    --  113.25  45.00 -90.00   54
 32  \w    110.00 144.00   0.50    0.05    --  113.25  30.00 -30.00   68
 33  \w    101.00 168.00   0.50    0.05    --  113.25  45.00-120.00  134
 34  \w    101.00 157.00   0.50    0.05    --  113.25  45.00-150.00  112
 35  \w     98.00 176.00   0.50    0.05    --  113.25  61.00-180.00  156
 36  \w    -68.00 -26.00   0.50    0.05    --  -47.51  77.00-180.00   84
 37  \w     -7.00  19.00   0.50    0.05    --  -47.51  77.00-180.00   52
 38  \w   -117.00 -39.00   0.50    0.05    --  -47.51   0.00  30.00  156
 39  \w    -27.00  26.00   0.50    0.05    --  -47.51  19.00  90.00  106
 40  \w    -16.00  21.00   0.50    0.05    --  -47.51   0.00  30.00   74
 41  \w    -51.00 -26.00   0.50    0.05    --  -91.75  45.00  30.00   50
 42  \w    -50.00 -20.00   0.50    0.05    --  -91.75  45.00  90.00   60
 43  \w    -85.00 -47.00   0.50    0.05    --  -91.75 125.00 -60.00   76
 44  \w    -51.00 -25.00   0.50    0.05    --  -91.75  45.00 -90.00   52
 45  \w    -62.00 -34.00   0.50    0.05    --  -47.51 -57.00 -60.00   56
 46  \w   -111.00 -81.00   0.50    0.05    --  -47.51 -57.00 -60.00   60
;
_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      -0.1354414000
_diffrn_orient_matrix_UB_12      -0.0502338000
_diffrn_orient_matrix_UB_13      0.0263340000
_diffrn_orient_matrix_UB_21      0.0808676000
_diffrn_orient_matrix_UB_22      0.0126187000
_diffrn_orient_matrix_UB_23      0.1054945000
_diffrn_orient_matrix_UB_31      -0.0977643000
_diffrn_orient_matrix_UB_32      0.0801892000
_diffrn_orient_matrix_UB_33      -0.0000832000
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26501
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.095
_diffrn_reflns_theta_min         4.153
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.324
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.333
_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    1.918
_exptl_crystal_description       needle
_exptl_crystal_F_000             1096
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0426P)^2^+4.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4167
_reflns_number_total             4245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3-017-tmcl_auto_redabs
_cod_database_code               7720815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18N4Cl3TmH18
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.638
_shelx_estimated_absorpt_t_min   0.122
_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              2977
_ins_header
;
TITL MH3-017-TmCl_auto_REDABS in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   8.567893  16.128417  14.626211  90.0000 104.3087  90.0000
ZERR    4.00   0.000060   0.000092   0.000102   0.0000   0.0007   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N Cl Tm
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 0.04 0.13 0.29
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id MH3-017-TmCl
_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 3.192
_oxdiff_exptl_absorpt_empirical_full_min 0.520