Divalent Ytterbium Complex-Catalyzed Homo- and Cross-Coupling of Primary Arylsilanes.
Liu, Xiaojuan; Xiang, Li; Louyriac, Elisa; Maron, Laurent; Leng, Xuebing; Chen, Yaofeng; Journal of the American Chemical Society 141 (2019) 138–142; doi:10.1021/jacs.8b12138

data_4133647
_publ_section_title
;
 Divalent Ytterbium Complex-Catalyzed Homo- and Cross-Coupling of Primary
 Arylsilanes.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              138
_journal_page_last               142
_journal_paper_doi               10.1021/jacs.8b12138
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C28 H52 N4 Si Yb'
_chemical_formula_sum            'C28 H52 N4 Si Yb'
_chemical_formula_weight         645.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.361(3)
_cell_length_b                   20.959(4)
_cell_length_c                   21.535(4)
_cell_measurement_reflns_used    4351
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.204
_cell_measurement_theta_min      2.162
_cell_volume                     6482(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0920
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47025
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         1.891
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0720 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.8743. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7440
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+4.8735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4041
_reflns_number_total             7440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12138_si_002.cif
_cod_data_source_block           mo_dm18077_0m
_cod_database_code               4133647
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.719
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C9
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C8, C9
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N4 \\sim C9 \\sim C8 \\sim N3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C16(H16), C17(H17)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_shelx_res_checksum              93744
_shelx_hkl_checksum              15779
_olex2_submission_special_instructions 'No special instructions were received'