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_7720811
_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 Sm, C2 H3 N'
_chemical_formula_sum            'C20 H21 N8 O9 Sm'
_chemical_formula_weight         667.80
_chemical_name_systematic        MH3-017-SmNO3
_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                 99.8490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8885(3)
_cell_length_b                   8.37110(10)
_cell_length_c                   27.1008(3)
_cell_measurement_reflns_used    17319
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      79.9740
_cell_measurement_theta_min      3.3210
_cell_volume                     4892.52(11)
_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(14)
_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 0.986
_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     45.00  71.00   0.50    0.53    --  113.25-125.00-180.00   52
  2  \w     52.00 103.00   0.50    0.53    --  113.25-125.00-120.00  102
  3  \w     44.00  78.00   0.50    0.53    --  113.25-125.00 -60.00   68
  4  \w     57.00 106.00   0.50    0.53    --  113.25 -94.00 -60.00   98
  5  \w     62.00 108.00   0.50    0.53    --  113.25-125.00  30.00   92
  6  \w     75.00 108.00   0.50    0.53    --  113.25-106.00  59.64   66
  7  \w     50.00  76.00   0.50    0.53    --  113.25 -94.00  90.00   52
  8  \w     81.00 106.00   0.50    0.53    --  113.25 -94.00  90.00   50
  9  \w     49.00 101.00   0.50    0.53    --  113.25 -94.00  60.00  104
 10  \w     80.00 105.00   0.50    0.53    --  113.25 -94.00   0.00   50
 11  \w     42.00  72.00   0.50    0.53    --  113.25 -94.00-120.00   60
 12  \w     58.00 106.00   0.50    0.53    --  113.25 -94.00-180.00   96
 13  \w     64.00 104.00   0.50    0.53    --  113.25 -94.00-150.00   80
 14  \w     75.00 105.00   0.50    0.53    --  113.25 -94.00-120.00   60
 15  \w     73.00 103.00   0.50    0.53    --  113.25 -94.00 -90.00   60
 16  \w     53.00 102.00   0.50    0.53    --  113.25 -94.00 120.00   98
 17  \w     51.00 105.00   0.50    0.53    --  113.25 -94.00 150.00  108
 18  \w     43.00  71.00   0.50    0.53    --  113.25 -61.00   0.00   56
 19  \w     42.00  67.00   0.50    0.53    --  113.25 -61.00 -60.00   50
 20  \w     44.00  71.00   0.50    0.53    --  113.25 -61.00 -90.00   54
 21  \w     42.00  91.00   0.50    0.53    --  113.25 -77.00 -30.00   98
 22  \w     43.00  95.00   0.50    0.53    --  113.25 -77.00  60.00  104
 23  \w     46.00  71.00   0.50    0.53    --  113.25 -61.00  90.00   50
 24  \w    132.00 178.00   0.50    0.53    --  113.25  15.00 -30.00   92
 25  \w    100.00 172.00   0.50    0.53    --  113.25  61.00  90.00  144
 26  \w    104.00 137.00   0.50    0.53    --  113.25  61.00 150.00   66
 27  \w    144.00 178.00   0.50    0.53    --  113.25  61.00 150.00   68
 28  \w    117.00 170.00   0.50    0.53    --  113.25  30.00 120.00  106
 29  \w    116.00 173.00   0.50    0.53    --  113.25  30.00  60.00  114
 30  \w     37.00 120.00   0.50    0.13    --   47.51  38.00  60.00  166
 31  \w    100.00 125.00   0.50    0.53    --  113.25  15.00 -30.00   50
 32  \w    101.00 172.00   0.50    0.53    --  113.25  15.00  30.00  142
 33  \w    102.00 164.00   0.50    0.53    --  113.25  45.00-180.00  124
 34  \w    118.00 177.00   0.50    0.53    --  113.25  15.00-120.00  118
 35  \w    118.00 151.00   0.50    0.53    --  113.25 125.00  30.00   66
 36  \w    132.00 165.00   0.50    0.53    --  113.25 125.00 150.00   66
 37  \w    -23.00  30.00   0.50    0.13    --   47.51 -19.00  90.00  106
 38  \w     36.00  70.00   0.50    0.13    --   47.51 -77.00  90.00   68
 39  \w    -16.00  23.00   0.50    0.13    --   47.51 -19.00-120.00   78
 40  \w    -61.00  20.00   0.50    0.13    --  -47.51  57.00 -30.00  162
 41  \w    -30.00  25.00   0.50    0.13    --  -47.51  38.00 -90.00  110
 42  \w    -29.00  23.00   0.50    0.13    --  -47.51  19.00-120.00  104
 43  \w    -68.00 -28.00   0.50    0.53    --  -91.75  61.00-120.00   80
 44  \w    -50.00 -21.00   0.50    0.53    --  -91.75  45.00  60.00   58
 45  \w    -49.00 -21.00   0.50    0.53    --  -91.75  45.00 120.00   56
 46  \w    -48.00 -22.00   0.50    0.53    --  -91.75  45.00 150.00   52
;
_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      0.0502341000
_diffrn_orient_matrix_UB_12      0.0841691000
_diffrn_orient_matrix_UB_13      -0.0238909000
_diffrn_orient_matrix_UB_21      -0.0058491000
_diffrn_orient_matrix_UB_22      0.1495221000
_diffrn_orient_matrix_UB_23      0.0320884000
_diffrn_orient_matrix_UB_31      0.0504679000
_diffrn_orient_matrix_UB_32      -0.0664972000
_diffrn_orient_matrix_UB_33      0.0415861000
_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  0.0667
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            30830
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.483
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.630
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.657
_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    1.813
_exptl_crystal_description       needle
_exptl_crystal_F_000             2648
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropylether'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.000056(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   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+6.7752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0730
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4970
_reflns_number_total             5289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           mh3-017-smno3_2_redabs
_cod_database_code               7720811
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H21N8O9Sm
_chemical_oxdiff_usercomment     100K
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.155
_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              2333
_ins_header
;
TITL MH3-017-SmNO3_2_REDABS in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  21.888493   8.371081  27.100840  90.0000  99.8494  90.0000
ZERR    8.00   0.000267   0.000116   0.000318   0.0000   0.0011   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N O Sm
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 0.03 0.16
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id MH3-017-SmNO3
_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 3.344
_oxdiff_exptl_absorpt_empirical_full_min 0.520