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_4133646
_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         'C24 H41 I N4 Yb, C7 H8'
_chemical_formula_sum            'C31 H49 I N4 Yb'
_chemical_formula_weight         777.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.4110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8400(2)
_cell_length_b                   20.3740(4)
_cell_length_c                   14.4408(3)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.968
_cell_measurement_theta_min      4.745
_cell_volume                     3186.49(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      170.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34297
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.944
_diffrn_reflns_theta_min         4.743
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.001
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1419 before and 0.0795 after correction. The Ratio of minimum to maximum transmission is 0.5627. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6058
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0346P)^2^+2.3753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5486
_reflns_number_total             6058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b12138_si_002.cif
_cod_data_source_block           mjl18637_0m
_cod_database_code               4133646
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.753
_shelx_estimated_absorpt_t_min   0.521
_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
 C5AA-C2AA = C6AA-C5AA = C6AA-C3AA = C3AA-C0AA = C1AA-C0AA = C2AA-C1AA
 1.39 with sigma of 0.01
 C4AA-C0AA
 1.55 with sigma of 0.01
 C1C-C1B = C1G-C1B = C1G-C1F = C1F-C1E = C1E-C1D = C1D-C1C
 1.39 with sigma of 0.01
 C1B-C1A
 1.55 with sigma of 0.01
 C1C-C1A \\sim C1A-C1G
 with sigma of 0.01
 C1B-C1E \\sim C1F-C1C \\sim C1D-C1G \\sim C0AA-C5AA \\sim C6AA-C1AA \\sim
C2AA-C3AA
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1G \\sim C1D \\sim C1F \\sim C1E \\sim C4AA
\\sim C1AA \\sim C0AA \\sim C2AA \\sim C3AA \\sim C5AA \\sim C6AA: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C1F, C1A, C1B, C1C, C1G, C1D, C1E, C6AA, C1AA, C0AA, C2AA, C3AA, C4AA, C5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C1AA)=Sof(H1AA)=Sof(C3AA)=Sof(H3AA)=Sof(C0AA)=Sof(C5AA)=Sof(H5AA)=
 Sof(C2AA)=Sof(H2AA)=Sof(C6AA)=Sof(H6AA)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=Sof(C1B)=Sof(C1C)=Sof(H1CA)=Sof(C1D)=
 Sof(H1D)=Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=Sof(C1G)=Sof(H1G)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C16(H16), C17(H17), C1AA(H1AA), C3AA(H3AA), C5AA(H5AA),
 C2AA(H2AA), C6AA(H6AA), C1C(H1CA), C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G)
6.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), C4AA(H4AA,H4AB,H4AC), C1A(H1AB,H1AC,H1AD)
;
_shelx_res_checksum              37183
_shelx_hkl_checksum              57892
_olex2_submission_special_instructions 'No special instructions were received'