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_7720803
_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 Er N7 O9, C2 H3 N'
_chemical_formula_sum            'C20 H21 Er N8 O9'
_chemical_formula_weight         684.71
_chemical_name_systematic        MH3-017-ErNO3
_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             2023-12-19
_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                 99.7860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7876(2)
_cell_length_b                   8.28920(10)
_cell_length_c                   27.1254(2)
_cell_measurement_reflns_used    16049
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.7750
_cell_measurement_theta_min      3.3010
_cell_volume                     4827.61(8)
_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 0.989
_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    -61.00  16.00   0.50    0.05    --  -47.26  57.00  60.00  154
  2  \w    -44.00  24.00   0.50    0.05    --  -47.26  38.00   0.00  136
  3  \w    -10.00  27.00   0.50    0.05    --  -47.26  19.00 -30.00   74
  4  \w    -27.00  28.00   0.50    0.05    --  -47.26  19.00 -60.00  110
  5  \w   -122.00 -37.00   0.50    0.05    --  -47.26 -19.00-180.00  170
  6  \w     48.00  91.00   0.50    0.05    --   47.26-125.00 -90.00   86
  7  \w     57.00  84.00   0.50    0.05    --   47.26-125.00-150.00   54
  8  \w     43.00  78.00   0.50    0.17    --  113.25 -77.00   0.00   70
  9  \w     46.00  94.00   0.50    0.17    --  113.25 -77.00  60.00   96
 10  \w     61.00  96.00   0.50    0.17    --  113.25 -77.00 120.00   70
 11  \w     59.00  84.00   0.50    0.05    --   47.26-125.00 120.00   50
 12  \w     46.00  71.00   0.50    0.17    --  113.25 -61.00   0.00   50
 13  \w     42.00  67.00   0.50    0.17    --  113.25 -61.00 -60.00   50
 14  \w     42.00  67.00   0.50    0.17    --  113.25 -61.00 -90.00   50
 15  \w     44.00  83.00   0.50    0.17    --  113.25 -77.00-150.00   78
 16  \w     43.00  68.00   0.50    0.17    --  113.25 -61.00-120.00   50
 17  \w     42.00  67.00   0.50    0.17    --  113.25 -61.00-180.00   50
 18  \w     42.00  67.00   0.50    0.17    --  113.25 -61.00  30.00   50
 19  \w     45.00  70.00   0.50    0.17    --  113.25 -61.00  90.00   50
 20  \w     42.00  71.00   0.50    0.17    --  113.25 -61.00 150.00   58
 21  \w    122.00 149.00   0.50    0.17    --  113.25 125.00   0.00   54
 22  \w    -26.00  19.00   0.50    0.05    --   47.26 -38.00 120.00   90
 23  \w     52.00 105.00   0.50    0.17    --  113.25 -94.00 -30.00  106
 24  \w     55.00  81.00   0.50    0.17    --  113.25-125.00  30.00   52
 25  \w     43.00  68.00   0.50    0.17    --  113.25 -94.00 120.00   50
 26  \w     81.00 106.00   0.50    0.17    --  113.25 -94.00  90.00   50
 27  \w     74.00 105.00   0.50    0.17    --  113.25 -94.00  30.00   62
 28  \w     48.00 104.00   0.50    0.17    --  113.25 -94.00  60.00  112
 29  \w     67.00 105.00   0.50    0.17    --  113.25 -94.00   0.00   76
 30  \w     51.00 105.00   0.50    0.17    --  113.25 -94.00 -60.00  108
 31  \w     49.00 106.00   0.50    0.17    --  113.25 -94.00-180.00  114
 32  \w     73.00 106.00   0.50    0.17    --  113.25 -94.00-120.00   66
 33  \w     70.00  95.00   0.50    0.17    --  113.25 -94.00 -90.00   50
 34  \w     47.00 111.00   0.50    0.17    --  113.25-125.00 -90.00  128
 35  \w     75.00 101.00   0.50    0.17    --  113.25 -94.00 120.00   52
 36  \w     66.00 105.00   0.50    0.17    --  113.25 -94.00 150.00   78
 37  \w     94.00 140.00   0.50    0.17    --  113.25  77.00 -30.00   92
 38  \w     91.00 116.00   0.50    0.17    --  113.25  77.00-120.00   50
 39  \w    133.00 176.00   0.50    0.17    --  113.25  77.00-120.00   86
 40  \w    100.00 149.00   0.50    0.17    --  113.25  15.00-150.00   98
 41  \w    101.00 176.00   0.50    0.17    --  113.25  30.00 -60.00  150
 42  \w    153.00 178.00   0.50    0.17    --  113.25  15.00-150.00   50
 43  \w    100.00 131.00   0.50    0.17    --  113.25  15.00   0.00   62
 44  \w    101.00 177.00   0.50    0.17    --  113.25  45.00 150.00  152
 45  \w    103.00 169.00   0.50    0.17    --  113.25  30.00 120.00  132
 46  \w    100.00 129.00   0.50    0.17    --  113.25  15.00 120.00   58
 47  \w    101.00 164.00   0.50    0.17    --  113.25  15.00  60.00  126
 48  \w    101.00 126.00   0.50    0.17    --  113.25  15.00-120.00   50
 49  \w    149.00 177.00   0.50    0.17    --  113.25  15.00-120.00   56
;
_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      0.0435899000
_diffrn_orient_matrix_UB_12      0.0566470000
_diffrn_orient_matrix_UB_13      -0.0356714000
_diffrn_orient_matrix_UB_21      -0.0566747000
_diffrn_orient_matrix_UB_22      0.0251332000
_diffrn_orient_matrix_UB_23      -0.0417340000
_diffrn_orient_matrix_UB_31      -0.0060272000
_diffrn_orient_matrix_UB_32      0.1752427000
_diffrn_orient_matrix_UB_33      0.0175182000
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            30768
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.215
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.065
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.547
_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    1.884
_exptl_crystal_description       needle
_exptl_crystal_F_000             2696
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.000080(11)
_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   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0397P)^2^+15.5384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4837
_reflns_number_total             5228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           erno3_redabs
_cod_database_code               7720803
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H21O9N8Er
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.697
_shelx_estimated_absorpt_t_min   0.093
_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              13746
_olex2_submission_original_sample_id MH3-017-ErNO3
_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 1.364
_oxdiff_exptl_absorpt_empirical_full_min 0.790