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_7720814
_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 N7 O9 Tb, C2 H3 N'
_chemical_formula_sum            'C20 H21 N8 O9 Tb'
_chemical_formula_weight         676.37
_chemical_name_systematic        MH3-017-TbNO3
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-15
_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                 99.773(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8449(3)
_cell_length_b                   8.31870(10)
_cell_length_c                   27.1436(4)
_cell_measurement_reflns_used    16880
_cell_measurement_temperature    100.00(15)
_cell_measurement_theta_max      79.3500
_cell_measurement_theta_min      3.3460
_cell_volume                     4860.99(12)
_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(15)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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    -53.00   7.00   0.50    0.77    --  -47.26  83.00  66.00  120
  2  \w    -19.00   7.00   0.50    0.77    --   47.26 -83.00 -54.00   52
  3  \w     11.00  73.00   0.50    0.77    --   47.26 -83.00 -54.00  124
  4  \w    -92.00 -67.00   0.50    3.09    --  -91.75  83.00  66.00   50
  5  \w   -146.00-120.00   0.50    3.09    --  -91.75 -83.00 -54.00   52
  6  \w    106.00 174.00   0.50    3.09    --  113.25  83.00  66.00  136
  7  \w    -53.00  20.00   0.50    0.77    --  -47.26  57.00-180.00  146
  8  \w    -86.00 -50.00   0.50    0.77    --  -47.26 125.00 -30.00   72
  9  \w   -114.00 -34.00   0.50    0.77    --  -47.26 -57.00 -90.00  160
 10  \w    -41.00 -13.00   0.50    0.77    --  -47.26 125.00 -30.00   56
 11  \w    -17.00  28.00   0.50    0.77    --   47.26 -19.00  30.00   90
 12  \w     10.00  40.00   0.50    0.77    --   47.26 -38.00-180.00   60
 13  \w    -21.00   7.00   0.50    0.77    --   47.26 -38.00-180.00   56
 14  \w    -26.00  29.00   0.50    0.77    --   47.26 -19.00 -60.00  110
 15  \w    -51.00 -26.00   0.50    3.09    --  -91.75  45.00  90.00   50
 16  \w    -54.00 -28.00   0.50    3.09    --  -91.75 125.00-180.00   52
 17  \w    -63.00 -28.00   0.50    3.09    --  -91.75  61.00 -30.00   70
 18  \w    -47.00 -21.00   0.50    3.09    --  -91.75  45.00 -90.00   52
 19  \w     45.00 108.00   0.50    3.09    --  113.25-108.00  63.54  126
 20  \w     42.00  67.00   0.50    3.09    --  113.25 -61.00 120.00   50
 21  \w    118.00 172.00   0.50    3.09    --  113.25  15.00  60.00  108
 22  \w     80.00 106.00   0.50    3.09    --  113.25-125.00-120.00   52
 23  \w     51.00  78.00   0.50    3.09    --  113.25-125.00-120.00   54
 24  \w     42.00 106.00   0.50    3.09    --  113.25 -94.00 -90.00  128
 25  \w     44.00  69.00   0.50    3.09    --  113.25 -61.00  90.00   50
 26  \w     42.00  67.00   0.50    3.09    --  113.25 -61.00 150.00   50
 27  \w     65.00  91.00   0.50    3.09    --  113.25 -77.00  60.00   52
 28  \w    101.00 171.00   0.50    3.09    --  113.25  15.00 120.00  140
 29  \w     56.00 111.00   0.50    3.09    --  113.25-125.00 -60.00  110
 30  \w     42.00  67.00   0.50    3.09    --  113.25 -61.00   0.00   50
 31  \w     53.00  78.00   0.50    3.09    --  113.25 -94.00 -60.00   50
 32  \w     81.00 106.00   0.50    3.09    --  113.25 -94.00 -60.00   50
 33  \w     68.00 107.00   0.50    3.09    --  113.25-109.00-103.16   78
 34  \w    102.00 145.00   0.50    3.09    --  113.25  45.00   0.00   86
 35  \w    147.00 175.00   0.50    3.09    --  113.25  45.00   0.00   56
 36  \w    101.00 163.00   0.50    3.09    --  113.25  45.00-120.00  124
 37  \w     42.00  71.00   0.50    3.09    --  113.25 -61.00-150.00   58
 38  \w     42.00  91.00   0.50    3.09    --  113.25 -77.00 150.00   98
 39  \w     44.00  69.00   0.50    3.09    --  113.25 -61.00 -60.00   50
 40  \w     97.00 129.00   0.50    3.09    --  113.25 125.00 120.00   64
 41  \w    145.00 170.00   0.50    3.09    --  113.25  61.00  60.00   50
 42  \w     81.00 106.00   0.50    3.09    --  113.25 -94.00 120.00   50
 43  \w    133.00 158.00   0.50    3.09    --  113.25 125.00 120.00   50
 44  \w     85.00 111.00   0.50    3.09    --  113.25-125.00 -90.00   52
 45  \w     52.00  77.00   0.50    3.09    --  113.25-125.00  90.00   50
 46  \w     86.00 111.00   0.50    3.09    --  113.25-125.00  90.00   50
 47  \w     44.00  69.00   0.50    3.09    --  113.25 -94.00 150.00   50
 48  \w     81.00 106.00   0.50    3.09    --  113.25 -94.00 150.00   50
 49  \w    103.00 158.00   0.50    3.09    --  113.25  30.00 150.00  110
 50  \w    106.00 168.00   0.50    3.09    --  113.25  45.00-180.00  124
 51  \w     44.00  71.00   0.50    3.09    --  113.25 -61.00-180.00   54
 52  \w     46.00  71.00   0.50    3.09    --  113.25 -61.00 -90.00   50
 53  \w     99.00 124.00   0.50    3.09    --  113.25  61.00  60.00   50
 54  \w     42.00  68.00   0.50    3.09    --  113.25 -94.00 120.00   52
 55  \w     43.00 106.00   0.50    3.09    --  113.25 -94.00  90.00  126
 56  \w     61.00 102.00   0.50    3.09    --  113.25 -94.00 -30.00   82
 57  \w     53.00  96.00   0.50    3.09    --  113.25 -77.00   0.00   86
 58  \w    100.00 164.00   0.50    3.09    --  113.25  15.00   0.00  128
 59  \w     79.00 104.00   0.50    3.09    --  113.25-125.00-180.00   50
 60  \w     86.00 111.00   0.50    3.09    --  113.25-125.00 150.00   50
 61  \w     83.00 108.00   0.50    3.09    --  113.25 -83.00 -54.00   50
;
_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      0.0067578000
_diffrn_orient_matrix_UB_12      -0.0795217000
_diffrn_orient_matrix_UB_13      -0.0500772000
_diffrn_orient_matrix_UB_21      0.0528944000
_diffrn_orient_matrix_UB_22      0.1176268000
_diffrn_orient_matrix_UB_23      -0.0055634000
_diffrn_orient_matrix_UB_31      0.0477143000
_diffrn_orient_matrix_UB_32      -0.1188014000
_diffrn_orient_matrix_UB_33      0.0279511000
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32459
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.159
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.916
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.431
_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    1.848
_exptl_crystal_description       needle
_exptl_crystal_F_000             2672
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.00026(2)
_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   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+9.9344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4723
_reflns_number_total             5232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3-017-tbno3_redabs
_cod_database_code               7720814
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H21O9N8Tb
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.680
_shelx_estimated_absorpt_t_min   0.064
_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)
1.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              35792
_ins_header
;
TITL MH3-017-TbNO3_REDABS in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  21.844865   8.318741  27.143594  90.0000  99.7729  90.0000
ZERR    8.00   0.000327   0.000121   0.000439   0.0000   0.0015   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N O Tb
UNIT 160.00 168.00 64.00 72.00 8.00
REM  CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0
TEMP -173
SIZE 0.03 0.08 0.41
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id MH3-017-TbNO3
_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 2.692
_oxdiff_exptl_absorpt_empirical_full_min 0.536