<i>Ab initio</i>-based determination of lanthanoid-radical exchange as visualised by inelastic neutron scattering.
Dunstan, Maja A.; Giansiracusa, Marcus J.; Calvello, Simone; Sorace, Lorenzo; Krause-Heuer, Anwen M; Soncini, Alessandro; Mole, Richard A.; Boskovic, Colette; Chemical science 15 (2024) 4466–4477; doi:10.1039/d3sc04229d

data_1570990
_publ_section_title
;
 <i>Ab initio</i>-based determination of lanthanoid-radical exchange as
 visualised by inelastic neutron scattering.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              4466
_journal_page_last               4477
_journal_paper_doi               10.1039/d3sc04229d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C25 H25 B2 Er0.04 N12 O2 Y0.96'
_chemical_formula_sum            'C25 H25 B2 Er0.04 N12 O2 Y0.96'
_chemical_formula_weight         639.23
_chemical_name_systematic
erbium(III)@yttrium(III)bis(tris-pyrazolylborato)(tropolonato)
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-10 deposited with the CCDC.	2024-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.33390(10)
_cell_length_b                   9.33390(10)
_cell_length_c                   31.9618(6)
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.7020
_cell_measurement_theta_min      4.9270
_cell_volume                     2784.57(7)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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     33.00 109.00   0.50    0.85    --  105.86-120.00-105.00  152
  2  \w     35.00  70.00   0.50    0.85    --  105.86 -61.00 150.00   70
  3  \w     36.00  71.00   0.50    0.85    --  105.86 -61.00 120.00   70
  4  \w     92.00 124.00   0.50    0.85    --  105.86  15.00   0.00   64
  5  \w    148.00 174.00   0.50    0.85    --  105.86  15.00   0.00   52
  6  \w    -33.00  10.00   0.50    0.21    --  -47.57  38.00  90.00   86
  7  \w    -92.00 -67.00   0.50    0.85    --  -86.25 155.00 135.00   50
  8  \w    -50.00 -23.00   0.50    0.85    --  -86.25  45.00 -90.00   54
  9  \w   -117.00 -75.00   0.50    0.21    --  -47.57-125.00  60.00   84
 10  \w   -115.00 -84.00   0.50    0.21    --  -47.57-125.00  30.00   62
 11  \w   -154.00 -96.00   0.50    0.85    --  -86.25-138.00  -4.00  116
 12  \w    -90.00 -65.00   0.50    0.85    --  -86.25-138.00  -4.00   50
;
_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      -0.0045855000
_diffrn_orient_matrix_UB_12      -0.0723774000
_diffrn_orient_matrix_UB_13      0.0432974000
_diffrn_orient_matrix_UB_21      0.0195811000
_diffrn_orient_matrix_UB_22      0.1470872000
_diffrn_orient_matrix_UB_23      0.0211475000
_diffrn_orient_matrix_UB_31      -0.1637733000
_diffrn_orient_matrix_UB_32      0.0195038000
_diffrn_orient_matrix_UB_33      0.0013083000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            9327
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.699
_diffrn_reflns_theta_min         4.936
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.788
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1301
_exptl_crystal_preparation
'Reaction of Y(III) nitrate hexahydrate or Er(III) nitrate hexahydrate with trispyrazolylborate and tropolonate. Crude compounds combined in 1:19 ratio before recrystallisation.'
_exptl_crystal_recrystallization_method
'Recrystallisation from hot methanol/ethyl acetate.'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 1000 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.037(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.5955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.603
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2673
_reflns_number_total             2772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04229d3.cif
_cod_data_source_block           er-y-trop
_cod_depositor_comments
'Adding full bibliography for 1570987--1570990.cif.'
_cod_original_cell_volume        2784.57(8)
_cod_database_code               1570990
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Y0.9 Er0.1 C25 H25 N12 O2 B2'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Shared sites
{Y1, Er1}
3. Uiso/Uaniso restraints and constraints
Uanis(Y1) = Uanis(Er1)
4. Others
 Sof(Er1)=0.5*(1-FVAR(2))
 Sof(Y1)=0.5*FVAR(2)
5.a Ternary CH refined with riding coordinates:
 B1(H1A)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C11(H11), C12(H12), C13(H13)
;
_shelx_res_checksum              72573
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.875