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_7248201
_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         'C21 H57 Si6 Yb1, 0.5(C7 H20 Si2)'
_chemical_formula_sum            'C24.5 H67 Si7 Yb'
_chemical_formula_weight         731.45
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.1800(8)
_cell_length_b                   16.1800(8)
_cell_length_c                   8.5692(4)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.354
_cell_measurement_theta_min      2.518
_cell_volume                     1942.80(16)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29458
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.522
_diffrn_reflns_theta_min         1.453
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1058 before and 0.0656 after correction.
The Ratio of minimum to maximum transmission is 0.7667.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       plate
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1790 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0359
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                3755
_reflns_number_total             3935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp00281d3.cif
_cod_data_source_block           mpc035yb
_cod_depositor_comments
'Adding full bibliography for 7248201--7248203.cif.'
_cod_original_cell_volume        1942.8(2)
_cod_original_formula_sum        'C24.50 H67 Si7 Yb'
_cod_database_code               7248201
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.779
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-Si3
 1.76 with sigma of 0.02
 C8-Si4
 1.77 with sigma of 0.02
 Si3-C13 = Si3-C12 = Si4-C11 = Si4-C9
 1.86 with sigma of 0.02
 Si3-C14 = Si4-C10
 1.87 with sigma of 0.02
 C8-C12 = C8-C11
 2.95 with sigma of 0.04
 C8-C10
 3.05 with sigma of 0.04
 C8-C13
 3 with sigma of 0.04
 C8-C14 = C8-C9
 2.98 with sigma of 0.04
 Si3-C13 \\sim Si3-C12 \\sim Si3-C14 \\sim Si4-C11 \\sim Si4-C10 \\sim Si4-C9
 with sigma of 0.02
 C13-C12 \\sim C12-C14 \\sim C14-C13 \\sim C11-C10 \\sim C10-C9 \\sim C9-C11
 with sigma of 0.04
 C8-C13 \\sim C8-C12 \\sim C8-C14 \\sim C8-C11 \\sim C8-C10 \\sim C8-C9
 with sigma of 0.04
 C8-Si3 \\sim C8-Si4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si3 \\sim Si4 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim
C14: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uiso(C13) = Uiso(Si3) = Uiso(C12) = Uiso(C14) = Uiso(C8) = Uiso(Si4) =
Uiso(C11) = Uiso(C9) = Uiso(C10)
4. Rigid body (RIGU) restrains
 Si3, Si4, C8, C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Si3(0.16667) Si4(0.16667) C8(0.16667) H8A(0.16667) H8B(0.16667)
 C9(0.16667) H9A(0.16667) H9B(0.16667) H9C(0.16667) C10(0.16667) H10A(0.16667)
 H10B(0.16667) H10C(0.16667) C11(0.16667) H11A(0.16667) H11B(0.16667)
 H11C(0.16667) C12(0.16667) H12A(0.16667) H12B(0.16667) H12C(0.16667)
 C13(0.16667) H13A(0.16667) H13B(0.16667) H13C(0.16667) C14(0.16667)
 H14A(0.16667) H14B(0.16667) H14C(0.16667)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              49915
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'