4f-intermediate valence in an ytterbium-bipyridine coordination solid.
Luneva, Evgeniia; Dunstan, Maja A.; Aribot, Frédéric; Yutronkie, Nathan J.; McPeak, Joseph E.; Rogalev, Andrei; Nocton, Grégory; Pedersen, Kasper S.; Chemical communications (Cambridge, England) 61 (2025) 14999–15002; doi:10.1039/d5cc04048e

data_1575485
_publ_section_title
;
 4f-intermediate valence in an ytterbium-bipyridine coordination solid.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14999
_journal_page_last               15002
_journal_paper_doi               10.1039/d5cc04048e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C32 H42 N2 Yb'
_chemical_formula_sum            'C32 H42 N2 Yb'
_chemical_formula_weight         627.71
_chemical_name_systematic
catena-[bis(pentamethylcyclopentadienyl)ytterbium(2,2'-methyl-4,4'-bipyridine)]
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2025-06-27
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-07-16 deposited with the CCDC.	2025-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.643(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5522(17)
_cell_length_b                   16.718(3)
_cell_length_c                   18.078(3)
_cell_measurement_reflns_used    839
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      65.4720
_cell_measurement_theta_min      3.5950
_cell_volume                     2846.2(9)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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    -53.00  32.00   1.00   30.00    --  -40.81  24.00 -22.00   85
  2  \w   -119.00 -33.00   1.00   30.00    --  -40.81 -24.00 172.00   86
  3  \w     -6.00  19.00   1.00   30.00    --   40.81 -24.00 172.00   25
  4  \w     78.00 118.00   1.00   30.00    --   40.81  24.00 -22.00   40
  5  \w    104.00 129.00   1.00  125.00    --  112.00  24.00 -22.00   25
  6  \w     35.00 124.00   1.00  125.00    --  112.00 -24.00 172.00   89
  7  \w     39.00  85.00   1.00   30.00    --   40.81-125.00   0.00   46
  8  \w     43.00  90.00   1.00   30.00    --   40.81-125.00-150.00   47
  9  \w      8.00  36.00   1.00   30.00    --   40.81 -99.00-180.00   28
 10  \w     52.00  84.00   1.00  125.00    --  112.00-111.00   0.00   32
 11  \w    128.00 178.00   1.00  125.00    --  112.00  77.00-120.00   50
 12  \w     32.00  91.00   1.00  125.00    --  112.00 -94.00  30.00   59
 13  \w    107.00 142.00   1.00  125.00    --  112.00 111.00 -30.00   35
 14  \w     56.00 113.00   1.00  125.00    --  112.00 -61.00  30.00   57
 15  \w     86.00 177.00   1.00  125.00    --  112.00  30.00   0.00   91
 16  \w     40.00 139.00   1.00  125.00    --  112.00 -61.00-180.00   99
 17  \w     37.00  98.00   1.00  125.00    --  112.00 -94.00  60.00   61
 18  \w     37.00  64.00   1.00  125.00    --  112.00 -94.00-120.00   27
 19  \w     77.00 106.00   1.00  125.00    --  112.00-111.00  30.00   29
 20  \w    113.00 160.00   1.00  125.00    --  112.00 111.00-150.00   47
 21  \w     41.00  73.00   1.00  125.00    --  112.00-111.00-180.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0665792000
_diffrn_orient_matrix_UB_12      -0.0078855000
_diffrn_orient_matrix_UB_13      -0.0717101000
_diffrn_orient_matrix_UB_21      0.1404791000
_diffrn_orient_matrix_UB_22      -0.0278542000
_diffrn_orient_matrix_UB_23      0.0475954000
_diffrn_orient_matrix_UB_31      -0.0508238000
_diffrn_orient_matrix_UB_32      -0.0874169000
_diffrn_orient_matrix_UB_33      -0.0085820000
_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  0.2168
_diffrn_reflns_av_unetI/netI     0.2754
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18026
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.971
_diffrn_reflns_theta_min         3.625
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.219
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.780
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_preparation
'Reaction of YbCp*2 and 2,2'-dimethyl-4,4'-bipyridine'
_exptl_crystal_recrystallization_method 'Crystals obtained from melt reaction'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.558
_refine_diff_density_min         -2.480
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1768
_refine_ls_R_factor_gt           0.0772
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2753
_reflns_number_total             5908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04048e2.cif
_cod_data_source_block           YbCp2_Me2bipy
_cod_depositor_comments
'Adding full bibliography for 1575484--1575485.cif.'
_cod_original_cell_volume        2846.1(8)
_cod_database_code               1575485
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C32H42N2Yb
_cell_oxdiff_angle_alpha         89.924(9)
_cell_oxdiff_angle_beta          99.554(11)
_cell_oxdiff_angle_gamma         90.031(11)
_cell_oxdiff_length_a            9.5517(15)
_cell_oxdiff_length_b            16.7297(18)
_cell_oxdiff_length_c            18.062(2)
_cell_oxdiff_measurement_reflns_used 839
_cell_oxdiff_volume              2846.2(6)
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C15)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C4(H4), C10(H10), C9(H9), C1(H1)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C11(H11A,H11B,
 H11C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C32(H32A,
 H32B,H32C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              95896
_shelx_hkl_checksum              63443
_olex2_exptl_crystal_mounting_method 'Mounted in polybutenes on a nylon loop'
_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 2.395
_oxdiff_exptl_absorpt_empirical_full_min 0.655