Modulating the electronic properties of divalent lanthanoid complexes with subtle ligand tuning
Hay, Moya A.; Gable, Robert W.; Boskovic, Colette; Dalton Transactions  (2023) –; doi:10.1039/D2DT03782C

data_7712291
_publ_section_title
;
 Modulating the electronic properties of divalent lanthanoid complexes
 with subtle ligand tuning
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03782C
_journal_year                    2023
_chemical_formula_moiety         'C36 H36 N8 Yb, 2(C24 H20 B)'
_chemical_formula_sum            'C84 H76 B2 N8 Yb'
_chemical_formula_weight         1392.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-11 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2045(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.31789(11)
_cell_length_b                   14.28779(11)
_cell_length_c                   19.67463(15)
_cell_measurement_reflns_used    20372
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8930
_cell_measurement_theta_min      3.8190
_cell_volume                     3371.10(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_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   -120.00 -82.00   0.50    2.11    --  -48.20 -57.00  60.00   76
  2  \w   -117.00 -86.00   0.50    2.11    --  -48.20 -57.00  30.00   62
  3  \w   -120.00 -84.00   0.50    2.11    --  -48.20 -57.00   0.00   72
  4  \w   -115.00 -88.00   0.50    2.11    --  -48.20-125.00   0.00   54
  5  \w   -119.00 -87.00   0.50    2.11    --  -48.20-125.00  30.00   64
  6  \w   -152.00 -97.00   0.50    8.44    --  -86.25-125.00  60.00  110
  7  \w   -146.00-120.00   0.50    8.44    --  -86.25 -77.00   0.00   52
  8  \w   -158.00-101.00   0.50    8.44    --  -86.25 -77.00  60.00  114
  9  \w   -158.00-125.00   0.50    8.44    --  -86.25 -77.00 120.00   66
 10  \w    -42.00  25.00   0.50    2.11    --  -48.20  37.00 150.00  134
 11  \w    -10.00  23.00   0.50    2.11    --  -48.20  77.00 120.00   66
 12  \w    -16.00  27.00   0.50    2.11    --  -48.20  19.00  30.00   86
 13  \w    -20.00  27.00   0.50    2.11    --  -48.20  19.00 -90.00   94
 14  \w    -40.00 -14.00   0.50    8.44    --  -86.25  37.00  30.00   52
 15  \w    -71.00 -43.00   0.50    2.11    --  -48.20  77.00 120.00   56
 16  \w    -85.00 -23.00   0.50    2.11    --  -48.20 125.00 -60.00  124
 17  \w   -159.00 -77.00   0.50    8.44    --  -86.25 -37.00 -60.00  164
 18  \w     36.00  92.00   0.50    8.44    --  107.74 -99.00-120.00  112
 19  \w     81.00 106.00   0.50    8.44    --  107.74 -99.00-180.00   50
 20  \w     52.00 106.00   0.50    8.44    --  107.74 -99.00 -90.00  108
 21  \w     37.00  62.00   0.50    8.44    --  107.74 -57.00 -30.00   50
 22  \w     35.00  98.00   0.50    8.44    --  107.74 -99.00 -60.00  126
 23  \w     43.00 104.00   0.50    8.44    --  107.74 -99.00 -30.00  122
 24  \w     81.00 106.00   0.50    8.44    --  107.74 -99.00  30.00   50
 25  \w     50.00  76.00   0.50    8.44    --  107.74 -99.00  30.00   52
 26  \w     36.00 109.00   0.50    8.44    --  107.74-125.00  60.00  146
 27  \w     46.00 105.00   0.50    8.44    --  107.74 -99.00 150.00  118
 28  \w     36.00  62.00   0.50    8.44    --  107.74 -57.00 150.00   52
 29  \w     35.00 108.00   0.50    8.44    --  107.74-107.00 140.60  146
 30  \w     46.00  94.00   0.50    8.44    --  107.74-125.00 120.00   96
 31  \w     36.00  61.00   0.50    8.44    --  107.74 -57.00   0.00   50
 32  \w    105.00 177.00   0.50    8.44    --  107.74  37.00  60.00  144
 33  \w    111.00 148.00   0.50    8.44    --  107.74  77.00 -90.00   74
 34  \w    116.00 146.00   0.50    8.44    --  107.74  77.00-180.00   60
 35  \w    148.00 177.00   0.50    8.44    --  107.74  77.00-180.00   58
 36  \w    101.00 163.00   0.50    8.44    --  107.74 125.00-150.00  124
 37  \w     36.00  62.00   0.50    8.44    --  107.74 -57.00-150.00   52
 38  \w     35.00  60.00   0.50    8.44    --  107.74 -57.00-180.00   50
 39  \w     35.00  60.00   0.50    8.44    --  107.74 -99.00-180.00   50
 40  \w     95.00 177.00   0.50    8.44    --  107.74  44.00 133.36  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.105
_diffrn_reflns_theta_min         3.860
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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            'dark green'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       needle
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6035
_reflns_number_total             6994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03782c2.cif
_cod_data_source_block           1-yb
_cod_database_code               7712291
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31),
 C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41)
;
_shelx_res_checksum              60345
_shelx_hkl_checksum              77082
_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
;