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_7248202
_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         'C28 H59 O Si4 Yb'
_chemical_formula_sum            'C28 H59 O Si4 Yb'
_chemical_formula_weight         697.15
_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                89.3522(8)
_cell_angle_beta                 89.6376(8)
_cell_angle_gamma                89.7839(8)
_cell_formula_units_Z            4
_cell_length_a                   12.7256(7)
_cell_length_b                   13.6737(7)
_cell_length_c                   20.4896(11)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.77
_cell_measurement_theta_min      2.39
_cell_volume                     3565.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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
_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 0.914
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\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  0.0367
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.568
_diffrn_reflns_theta_min         0.994
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0635 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.8225.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         21831
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+3.8636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15452
_reflns_number_total             21831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp00281d3.cif
_cod_data_source_block           micha_p_1
_cod_depositor_comments
'Adding full bibliography for 7248201--7248203.cif.'
_cod_database_code               7248202
_shelx_shelxl_version_number     2019/1
_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. Restrained distances
 C8AA-H8AA \\sim C1B-H1BA \\sim C8B-H8B \\sim C1A-H1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si3C) = Uanis(Si3A)
Uanis(C8AB) = Uanis(C8AA)
Uanis(C143) = Uanis(C12B) = Uanis(C141) = Uanis(C14B) = Uanis(C13B) =
Uanis(C142)
4. Others
 Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C14B)=Sof(H14J)=Sof(H14K)=
 Sof(H14L)=Sof(C142)=Sof(H14M)=Sof(H14N)=Sof(H14O)=1-FVAR(1)
 Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C141)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C143)=Sof(H14G)=Sof(H14H)=Sof(H14I)=FVAR(1)
 Sof(Si3C)=Sof(C1)=Sof(H1B)=Sof(H1C)=Sof(H1D)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C8AB)=Sof(H8AB)=1-FVAR(2)
 Sof(H8AA)=Sof(Si3A)=Sof(C8AA)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C13A)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C8AB(H8AB), C8B(H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C17A(H17A), C18A(H18A), C19A(H19A), C17B(H17B), C18B(H18B), C19B(H19B)
5.c Idealised Me refined as rotating group:
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,
 H6AC), C7A(H7AA,H7AB,H7AC), C10A(H10A,H10B,H10C), C11A(H11A,H11B,H11C),
 C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C26A(H26A,
 H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,H28B,H28C), C12A(H12A,H12B,H12C),
 C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C1(H1B,H1C,H1D), C2(H2A,H2B,H2C),
 C3(H3A,H3B,H3C), C3B(H3BA,H3BB,H3BC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC),
  C6B(H6BA,H6BB,H6BC), C7B(H7BA,H7BB,H7BC), C10B(H10D,H10E,H10F), C11B(H11D,
 H11E,H11F), C22B(H22D,H22E,H22F), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F),
 C26B(H26D,H26E,H26F), C27B(H27D,H27E,H27F), C28B(H28D,H28E,H28F), C13B(H13D,
 H13E,H13F), C141(H14D,H14E,H14F), C143(H14G,H14H,H14I), C12B(H12D,H12E,H12F),
 C14B(H14J,H14K,H14L), C142(H14M,H14N,H14O)
;
_shelx_res_checksum              17398
_olex2_submission_special_instructions 'No special instructions were received'