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_7720807
_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 Yb'
_chemical_formula_sum            'C18 H18 Cl3 N4 Yb'
_chemical_formula_weight         569.75
_chemical_name_systematic        MH3-017-YbCl
_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             2023-12-21
_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                 104.2910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.55520(10)
_cell_length_b                   16.11430(10)
_cell_length_c                   14.61710(10)
_cell_measurement_reflns_used    19029
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      80.1100
_cell_measurement_theta_min      3.1430
_cell_volume                     1952.77(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      100.01(10)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -68.00  21.00   0.50    0.05    --  -47.26  77.00 -60.00  178
  2  \w      3.00  28.00   0.50    0.05    --  -47.26  19.00-120.00   50
  3  \w    -16.00  22.00   0.50    0.05    --  -47.26  19.00  90.00   76
  4  \w    -50.00 -23.00   0.50    0.05    --  -91.75  45.00 150.00   54
  5  \w    -51.00 -26.00   0.50    0.05    --  -91.75  45.00   0.00   50
  6  \w    -56.00 -22.00   0.50    0.05    --  -91.75 125.00 -60.00   68
  7  \w   -131.00-101.00   0.50    0.05    --  -91.75 -30.00 -90.00   60
  8  \w   -118.00 -28.00   0.50    0.05    --  -47.26 -77.00-180.00  180
  9  \w     42.00  94.00   0.50    0.05    --  113.25 -77.00-180.00  104
 10  \w     42.00  94.00   0.50    0.05    --  113.25 -77.00-120.00  104
 11  \w     42.00  67.00   0.50    0.05    --  113.25 -61.00 -90.00   50
 12  \w     49.00  75.00   0.50    0.05    --  113.25 -77.00 -60.00   52
 13  \w     42.00  79.00   0.50    0.05    --  113.25 -77.00   0.00   74
 14  \w     46.00  71.00   0.50    0.05    --  113.25 -61.00  30.00   50
 15  \w     46.00  72.00   0.50    0.05    --  113.25 -77.00  90.00   52
 16  \w     42.00  69.00   0.50    0.05    --  113.25 -61.00 120.00   54
 17  \w    -26.00  27.00   0.50    0.05    --   47.26 -38.00 120.00  106
 18  \w    -25.00  30.00   0.50    0.05    --   47.26 -19.00-180.00  110
 19  \w     80.00 105.00   0.50    0.05    --  113.25 -94.00 -60.00   50
 20  \w     50.00 111.00   0.50    0.05    --  113.25-125.00-150.00  122
 21  \w     59.00 102.00   0.50    0.05    --  113.25-125.00-180.00   86
 22  \w     57.00 106.00   0.50    0.05    --  113.25 -99.00-177.46   98
 23  \w     34.00  86.00   0.50    0.05    --   47.26-125.00 -60.00  104
 24  \w     54.00  88.00   0.50    0.05    --   47.26-125.00  60.00   68
 25  \w     48.00 109.00   0.50    0.05    --  113.25-113.00 120.22  122
 26  \w     52.00  85.00   0.50    0.05    --  113.25-125.00  90.00   66
 27  \w     79.00 104.00   0.50    0.05    --  113.25 -94.00  90.00   50
 28  \w     49.00 106.00   0.50    0.05    --  113.25 -94.00   0.00  114
 29  \w     46.00  74.00   0.50    0.05    --  113.25 -94.00 -30.00   56
 30  \w     75.00 106.00   0.50    0.05    --  113.25 -94.00  30.00   62
 31  \w     78.00 106.00   0.50    0.05    --  113.25 -94.00 -30.00   56
 32  \w     81.00 106.00   0.50    0.05    --  113.25 -94.00 -90.00   50
 33  \w     80.00 105.00   0.50    0.05    --  113.25 -94.00-150.00   50
 34  \w     47.00 104.00   0.50    0.05    --  113.25 -94.00-120.00  114
 35  \w    101.00 174.00   0.50    0.05    --  113.25  30.00  60.00  146
 36  \w    118.00 176.00   0.50    0.05    --  113.25  61.00   0.00  116
 37  \w    106.00 148.00   0.50    0.05    --  113.25  61.00 -30.00   84
 38  \w     99.00 178.00   0.50    0.05    --  113.25  61.00 -90.00  158
 39  \w     94.00 142.00   0.50    0.05    --  113.25  77.00-150.00   96
 40  \w    145.00 176.00   0.50    0.05    --  113.25  77.00-150.00   62
 41  \w    107.00 158.00   0.50    0.05    --  113.25  77.00-120.00  102
 42  \w    120.00 165.00   0.50    0.05    --  113.25  30.00-150.00   90
 43  \w    116.00 175.00   0.50    0.05    --  113.25  30.00-180.00  118
 44  \w    122.00 178.00   0.50    0.05    --  113.25  45.00 -60.00  112
 45  \w    150.00 176.00   0.50    0.05    --  113.25  45.00 120.00   52
 46  \w    101.00 132.00   0.50    0.05    --  113.25  45.00 120.00   62
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206386000
_diffrn_orient_matrix_UB_12      -0.0163424000
_diffrn_orient_matrix_UB_13      -0.1002007000
_diffrn_orient_matrix_UB_21      -0.1122097000
_diffrn_orient_matrix_UB_22      -0.0759005000
_diffrn_orient_matrix_UB_23      -0.0087767000
_diffrn_orient_matrix_UB_31      -0.1467404000
_diffrn_orient_matrix_UB_32      0.0557326000
_diffrn_orient_matrix_UB_33      -0.0413695000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25695
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.194
_diffrn_reflns_theta_min         4.155
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    12.709
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.442
_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    1.938
_exptl_crystal_description       needle
_exptl_crystal_F_000             1100
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.00118(6)
_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   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         4222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0388P)^2^+3.5774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4197
_reflns_number_total             4222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3-017-ybcl_auto_redabs
_cod_database_code               7720807
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18N4H18YbCl3
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.411
_shelx_estimated_absorpt_t_min   0.136
_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              29999
_ins_header
;
TITL MH3-017-YbCl_auto_REDABS in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   8.555219  16.114266  14.617113  90.0000 104.2911  90.0000
ZERR    4.00   0.000054   0.000095   0.000098   0.0000   0.0007   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N Cl Yb
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 0.08 0.13 0.26
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id MH3-017-YbCl
_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 4.163
_oxdiff_exptl_absorpt_empirical_full_min 0.654