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_7712294
_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
'1.755(C22.794 H23.934 N4.559 Yb0.57), 2(C24 H20 B)'
_chemical_formula_sum            'C88 H82 B2 N8 Yb'
_chemical_formula_weight         1446.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                103.4083(14)
_cell_angle_beta                 111.5188(13)
_cell_angle_gamma                109.1372(13)
_cell_formula_units_Z            1
_cell_length_a                   11.04793(17)
_cell_length_b                   13.51325(19)
_cell_length_c                   14.7018(2)
_cell_measurement_reflns_used    11857
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.7590
_cell_measurement_theta_min      3.5490
_cell_volume                     1767.44(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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_temperature      100.15
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_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    -70.00 -33.00   0.50    7.00    --  -47.45  89.00 -52.00   74
  2  \w    -27.00  12.00   0.50    7.00    --  -47.45  89.00 -52.00   78
  3  \w    -14.00  60.00   0.50    7.00    --   47.45 -89.00-168.00  148
  4  \w    -78.00 -53.00   0.50   20.00    --  -86.25  89.00 -52.00   50
  5  \w   -155.00-118.00   0.50   20.00    --  -86.25 -89.00-168.00   74
  6  \w     60.00  86.00   0.50   20.00    --  107.75 -89.00-168.00   52
  7  \w    -42.00  -6.00   0.50    7.00    --  -47.45  38.00  30.00   72
  8  \w   -109.00 -82.00   0.50    7.00    --  -47.45-125.00-180.00   54
  9  \w    -29.00  19.00   0.50    7.00    --  -47.45  19.00-120.00   96
 10  \w   -117.00 -79.00   0.50    7.00    --  -47.45-125.00 -30.00   76
 11  \w    -59.00 -20.00   0.50    7.00    --  -47.45  57.00  90.00   78
 12  \w      1.00  26.00   0.50    7.00    --  -47.45  38.00  30.00   50
 13  \w    -12.00  24.00   0.50    7.00    --  -47.45  57.00  90.00   72
 14  \w    -27.00  29.00   0.50    7.00    --   47.45 -19.00-120.00  112
 15  \w    -47.00 -22.00   0.50   20.00    --  -86.25  45.00 -30.00   50
 16  \w    -50.00 -20.00   0.50   20.00    --  -86.25  45.00-120.00   60
 17  \w    -37.00 -11.00   0.50   20.00    --  -86.25  30.00 150.00   52
 18  \w    -37.00 -12.00   0.50   20.00    --  -86.25  30.00 120.00   50
 19  \w    -50.00 -15.00   0.50   20.00    --  -86.25  45.00  30.00   70
 20  \w    -37.00 -12.00   0.50   20.00    --  -86.25  30.00  60.00   50
 21  \w    -68.00 -42.00   0.50   20.00    --  -86.25  61.00  30.00   52
 22  \w     36.00 107.00   0.50   20.00    --  107.75-104.00-130.05  142
 23  \w     37.00 156.00   0.50   20.00    --  107.75   0.00 -60.00  238
 24  \w     50.00  77.00   0.50   20.00    --  107.75 -77.00 -90.00   54
 25  \w     81.00 106.00   0.50   20.00    --  107.75 -94.00   0.00   50
 26  \w     36.00  85.00   0.50   20.00    --  107.75 -94.00 150.00   98
 27  \w     35.00  71.00   0.50   20.00    --  107.75 -61.00 -30.00   72
 28  \w     35.00  67.00   0.50   20.00    --  107.75 -94.00   0.00   64
 29  \w     85.00 177.00   0.50   20.00    --  107.75  77.00 -60.00  184
 30  \w     45.00  96.00   0.50   20.00    --  107.75   0.00 120.00  102
 31  \w     99.00 178.00   0.50   20.00    --  107.75   0.00 120.00  158
 32  \w     38.00  77.00   0.50   20.00    --  107.75 -77.00-120.00   78
 33  \w     39.00  70.00   0.50   20.00    --  107.75 -61.00  30.00   62
 34  \w     77.00 103.00   0.50   20.00    --  107.75 -94.00 -30.00   52
 35  \w     68.00 100.00   0.50   20.00    --  107.75 -77.00 120.00   64
 36  \w     77.00 105.00   0.50   20.00    --  107.75 -95.00  41.63   56
 37  \w     89.00 125.00   0.50   20.00    --  107.75-143.00   9.08   72
 38  \w     55.00  85.00   0.50   20.00    --  107.75-143.00   9.08   60
 39  \w     39.00 105.00   0.50   20.00    --  107.75 -94.00  90.00  132
 40  \w     80.00 107.00   0.50   20.00    --  107.75-102.00 128.25   54
 41  \w     42.00  76.00   0.50   20.00    --  107.75-102.00 128.25   68
 42  \w     44.00  69.00   0.50   20.00    --  107.75 -61.00-120.00   50
 43  \w     35.00 104.00   0.50   20.00    --  107.75 -94.00-120.00  138
 44  \w     36.00  66.00   0.50   20.00    --  107.75 -95.00  41.63   60
 45  \w    104.00 166.00   0.50   20.00    --  107.75  89.00 -52.00  124
;
_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  0.0541
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.686
_diffrn_reflns_theta_min         3.527
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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            Red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.410
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         7230
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0678P)^2^+2.0747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6367
_reflns_number_total             7230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03782c2.cif
_cod_data_source_block           2_yb
_cod_original_cell_volume        1767.44(5)
_cod_database_code               7712294
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.694
_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. Shared sites
{Yb1, Yb1A}
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, N2
 with sigma of 0.1
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, N2A
 with sigma of 0.1
 C8, C9, C10, C11, C12, C13, C14, N3
 with sigma of 0.1
 C8A, C9A, C10A, C11A, C12A, C13A, C14A, N3A
 with sigma of 0.1
 C15, C16, C17, C18, C19, C20, C21, N4
 with sigma of 0.1
 C15A, C16A, C17A, C18A, C19A, C20A, C21A, N4A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C1A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C8 \\sim C8A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C15 \\sim C15A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
N4 \\sim N4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C12A)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C5A) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.03
Uanis(Yb1) = Uanis(Yb1A)
Uanis(N1) = Uanis(N1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(N2) = Uanis(N2A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
Uanis(N3) = Uanis(N3A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C19) = Uanis(C19A)
Uanis(C20) = Uanis(C20A)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
Uanis(C36) = Uanis(C36A)
Uanis(C37) = Uanis(C37A)
Uanis(C38) = Uanis(C38A)
Uanis(C39) = Uanis(C39A)
Uanis(C40) = Uanis(C40A)
Uanis(C41) = Uanis(C41A)
Uanis(C42) = Uanis(C42A)
Uanis(C43) = Uanis(C43A)
Uanis(C44) = Uanis(C44A)
Uanis(C45) = Uanis(C45A)
5. Same fragment restrains
{Yb1, N1, N2, N3, N4, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13,
C14, C15, C16, C17, C18, C19, C20, C21} sigma for 1-2: 0.012, 1-3: 0.024
as in
{Yb1A, N1A, N2A, N3A, N4A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A,
C11A, C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A}
{C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36,
C37, C38, C39, C40, C41, C42, C43, C44, C45, B1} sigma for 1-2: 0.012, 1-3:
0.024
as in
{C22A, C23A, C24A, C25A, C26A, C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A,
C35A, C36A, C37A, C38A, C39A, C40A, C41A, C42A, C43A, C44A, C45A, B1A}
6. Others
 Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(N4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(C17A)=
 Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=1-FVAR(1)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C14A)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=0.66667*(1-FVAR(2))
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=0.66666*(1-FVAR(2))
 Sof(Yb1A)=0.5*(1-FVAR(2))
 Sof(Yb1)=0.5*FVAR(2)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=0.66666*FVAR(2)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 0.66667*FVAR(2)
 Sof(N1)=Sof(N2)=Sof(N3)=Sof(N4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=
 Sof(C19)=Sof(H19)=Sof(C20)=FVAR(1)
 Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C37A)=
 Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(C41A)=
 Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=
 Sof(C45A)=Sof(H45A)=Sof(B1A)=1-FVAR(2)
 Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=
 Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=
 Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(C35)=
 Sof(H35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(H39)=Sof(C40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(B1)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C1A(H1AA,H1AB), C8A(H8AA,H8AB),
 C15A(H15C,H15D)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C3A(H3A), C4A(H4A), C5A(H5A), C10A(H10A), C11A(H11A), C12A(H12A),
 C17A(H17A), C18A(H18A), C19A(H19A), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A),
 C29A(H29A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C35A(H35A),
 C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A), C41A(H41A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A)
7.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C7A(H7AA,H7AB,
 H7AC), C14A(H14D,H14E,H14F), C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              62682
_shelx_hkl_checksum              66142
_olex2_submission_special_instructions 'No special instructions were received'