Geometry and electronic structure of Yb(III)[CH(SiMe<sub>3</sub>)<sub>2</sub>]<sub>3</sub> from EPR and solid-state NMR augmented by computations.
Ashuiev, Anton; Allouche, Florian; Islam, Md Ashraful; Carvalho, José P; Sanders, Kevin J.; Conley, Matthew P.; Klose, Daniel; Lapadula, Giuseppe; Wörle, Michael; Baabe, Dirk; Walter, Marc D.; Pell, Andrew J.; Copéret, Christophe; Jeschke, Gunnar; Pintacuda, Guido; Andersen, Richard A.; Physical chemistry chemical physics : PCCP 26 (2024) 8734–8747; doi:10.1039/d4cp00281d

data_7248203
_publ_section_title
;
 Geometry and electronic structure of
 Yb(III)[CH(SiMe<sub>3</sub>)<sub>2</sub>]<sub>3</sub> from EPR and
 solid-state NMR augmented by computations.
;
_journal_issue                   11
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              8734
_journal_page_last               8747
_journal_paper_doi               10.1039/d4cp00281d
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C35 H61 O2 Si2 Yb'
_chemical_formula_sum            'C35 H61 O2 Si2 Yb'
_chemical_formula_weight         743.05
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-25 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                106.806(2)
_cell_angle_beta                 102.024(2)
_cell_angle_gamma                90.3602(19)
_cell_formula_units_Z            4
_cell_length_a                   12.6785(3)
_cell_length_b                   14.3864(3)
_cell_length_c                   22.0939(5)
_cell_measurement_reflns_used    23329
_cell_measurement_temperature    100.6(8)
_cell_measurement_theta_max      30.1610
_cell_measurement_theta_min      1.5290
_cell_volume                     3763.59(16)
_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
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.6(8)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -102.00 -34.00   1.00   30.00    --  -26.23-179.00-180.00   68
  2  \w      9.00  99.00   1.00   30.00    --   26.70  38.00  60.00   90
  3  \w    -46.00  50.00   1.00   30.00    --   26.70 -38.00  60.00   96
  4  \w     -3.00  91.00   1.00   30.00    --   26.70  77.00  90.00   94
  5  \w     -3.00  97.00   1.00   30.00    --   26.70  77.00 -60.00  100
  6  \w    -25.00  69.00   1.00   30.00    --   26.70 -99.00  30.00   94
  7  \w     21.00  99.00   1.00   30.00    --   26.70  38.00-180.00   78
  8  \w     -1.00  94.00   1.00   30.00    --   26.70  77.00-150.00   95
  9  \w    -35.00  57.00   1.00   30.00    --   26.70 -77.00-180.00   92
 10  \w   -102.00 -34.00   1.00   30.00    --  -26.23-179.00  90.00   68
 11  \w      5.00  44.00   1.00   30.00    --   26.70  57.00 -30.00   39
 12  \w      5.00  95.00   1.00   30.00    --   26.70  57.00-150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0265847000
_diffrn_orient_matrix_UB_12      0.0256299000
_diffrn_orient_matrix_UB_13      0.0322233000
_diffrn_orient_matrix_UB_21      0.0314298000
_diffrn_orient_matrix_UB_22      0.0287235000
_diffrn_orient_matrix_UB_23      -0.0119021000
_diffrn_orient_matrix_UB_31      -0.0399235000
_diffrn_orient_matrix_UB_32      0.0344110000
_diffrn_orient_matrix_UB_33      0.0012493000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79428
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.517
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.850
_refine_diff_density_min         -2.257
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         18679
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0368P)^2^+45.8338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15168
_reflns_number_total             18679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp00281d3.cif
_cod_data_source_block           mpc516-2
_cod_depositor_comments
'Adding full bibliography for 7248201--7248203.cif.'
_cod_original_cell_volume        3763.58(16)
_cod_database_code               7248203
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         'Yb1 Si2 O2 C50 H80'
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9661(5)
 0.0339(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 C8A, C9A, C10A, C11A, C12A, C13A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C27B, C32B, C33B, C34B, C35B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C8A, C9A, C10A, C11A, C12A, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27B, C32B, C33B, C34B, C35B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C10A(H10A), C11A(H11A), C12A(H12A), C24A(H24A), C25A(H25A), C26A(H26A),
 C10B(H10B), C11B(H11B), C12B(H12B), C24B(H24B), C25B(H25B), C26B(H26B)
5.b Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,
 H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,H7AC), C15A(H15A,H15B,H15C),
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C19A(H19A,H19B,H19C), C20A(H20A,
 H20B,H20C), C21A(H21A,H21B,H21C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C),
 C31A(H31A,H31B,H31C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C35A(H35A,
 H35B,H35C), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC),
 C5B(H5BA,H5BB,H5BC), C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C15B(H15D,H15E,
 H15F), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C18B(H18A,H18B,H18C),
 C19B(H19D,H19E,H19F), C21B(H21D,H21E,H21F), C29B(H29D,H29E,H29F), C30B(H30D,
 H30E,H30F), C31B(H31D,H31E,H31F), C33B(H33D,H33E,H33F), C34B(H34D,H34E,H34F),
 C35B(H35D,H35E,H35F)
;
_shelx_res_checksum              56416
_olex2_exptl_crystal_mounting_method tip-mounted
_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 1.251
_oxdiff_exptl_absorpt_empirical_full_min 0.838