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_7720805
_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 Yb, C2 H3 N'
_chemical_formula_sum            'C20 H21 N8 O9 Yb'
_chemical_formula_weight         690.49
_chemical_name_systematic        VF-YbNO3tpa-1-2
_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             2025-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-12-04 deposited with the CCDC.	2025-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7909(3)
_cell_length_b                   8.27130(10)
_cell_length_c                   27.1978(3)
_cell_measurement_reflns_used    11666
_cell_measurement_temperature    129.99(10)
_cell_measurement_theta_max      79.5690
_cell_measurement_theta_min      3.3060
_cell_volume                     4832.05(10)
_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      129.99(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 0.994
_diffrn_measured_fraction_theta_max 0.965
_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     47.00  92.00   0.50    1.00    --  113.25 -94.00-180.00   90
  2  \w     44.00 110.00   0.50    1.00    --  113.25-125.00 -90.00  132
  3  \w     53.00 105.00   0.50    1.00    --  113.25-125.00   0.00  104
  4  \w     79.00 105.00   0.50    1.00    --  113.25 -94.00 120.00   52
  5  \w    -23.00  20.00   0.50    0.25    --   47.51 -19.00  90.00   86
  6  \w     61.00  99.00   0.50    1.00    --  113.25 -77.00  90.00   76
  7  \w     46.00  72.00   0.50    1.00    --  113.25 -77.00   0.00   52
  8  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00  30.00   50
  9  \w     42.00  71.00   0.50    1.00    --  113.25 -61.00  60.00   58
 10  \w     42.00  67.00   0.50    1.00    --  113.25 -61.00 -30.00   50
 11  \w     46.00 101.00   0.50    1.00    --  113.25 -77.00 -60.00  110
 12  \w      7.00  43.00   0.50    0.25    --   47.51 -76.00-108.00   72
 13  \w     45.00  70.00   0.50    1.00    --  113.25 -61.00-180.00   50
 14  \w     45.00  71.00   0.50    1.00    --  113.25 -61.00-150.00   52
 15  \w     49.00  88.00   0.50    1.00    --  113.25 -76.00-108.00   78
 16  \w     42.00  71.00   0.50    1.00    --  113.25 -61.00 150.00   58
 17  \w    103.00 178.00   0.50    1.00    --  113.25  15.00 -30.00  150
 18  \w     96.00 147.00   0.50    1.00    --  113.25  76.00  18.00  102
 19  \w    104.00 174.00   0.50    1.00    --  113.25  30.00   0.00  140
 20  \w   -116.00 -25.00   0.50    0.25    --  -47.51 -76.00-108.00  182
 21  \w   -140.00-115.00   0.50    1.00    --  -91.75 -76.00-108.00   50
 22  \w    -70.00  12.00   0.50    0.25    --  -47.51  76.00  18.00  164
 23  \w    -14.00  17.00   0.50    0.25    --  -47.51  19.00 150.00   62
 24  \w    -83.00 -58.00   0.50    1.00    --  -91.75  76.00  18.00   50
 25  \w    -68.00 -38.00   0.50    1.00    --  -91.75  61.00-120.00   60
 26  \w    -46.00 -20.00   0.50    1.00    --  -91.75  45.00-150.00   52
;
_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      0.0350564000
_diffrn_orient_matrix_UB_12      0.1093081000
_diffrn_orient_matrix_UB_13      -0.0318293000
_diffrn_orient_matrix_UB_21      0.0578695000
_diffrn_orient_matrix_UB_22      -0.1090980000
_diffrn_orient_matrix_UB_23      0.0123049000
_diffrn_orient_matrix_UB_31      -0.0237715000
_diffrn_orient_matrix_UB_32      -0.1040622000
_diffrn_orient_matrix_UB_33      -0.0462580000
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17308
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.013
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    7.770
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.275
_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    1.898
_exptl_crystal_description       needle
_exptl_crystal_F_000             2712
_exptl_crystal_preparation       'Magnetic properties,Luminescent'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile/Diisopropyl ether'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.000074(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   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0459P)^2^+6.5529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4722
_reflns_number_total             5091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02364e2.cif
_cod_data_source_block           vf-ybno3tpa-1-2_auto_red_abs
_cod_database_code               7720805
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H21 N8 O9 Yb'
_chemical_oxdiff_usercomment     'Colourless Needle in Oil at 130'
_cell_oxdiff_angle_alpha         89.9626(14)
_cell_oxdiff_angle_beta          99.7187(13)
_cell_oxdiff_angle_gamma         89.9735(17)
_cell_oxdiff_length_a            21.7948(4)
_cell_oxdiff_length_b            8.27262(19)
_cell_oxdiff_length_c            27.1904(3)
_cell_oxdiff_measurement_reflns_used 11666
_cell_oxdiff_volume              4832.08(16)
_shelx_estimated_absorpt_t_max   0.612
_shelx_estimated_absorpt_t_min   0.110
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C1(H1A,H1B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C18(H18), C3(H3), C11(H11), C4(H4), C10(H10), C15(H15),
 C5(H5), C6(H6), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_shelx_res_checksum              78832
_ins_header
;
TITL VF-YbNO3tpa-1-2_auto_RED_ABS in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  21.790935   8.271334  27.197816  90.0000  99.6982  90.0000
ZERR    8.00   0.000281   0.000117   0.000327   0.0000   0.0012   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H N O Yb
UNIT 160.00 168.00 64.00 72.00 8.00
REM  CrysAlisPro recorded range (K): Min=129.9; max=130.0; aver:130.0
TEMP -143
SIZE 0.07 0.08 0.51
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id 1-Yb
_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 2.691
_oxdiff_exptl_absorpt_empirical_full_min 0.625