New Hindered Amide Base for Aryne Insertion into Si-P, Si-S, Si-N, and C-C Bonds.
Mesgar, Milad; Nguyen-Le, Justin; Daugulis, Olafs; Journal of the American Chemical Society 140 (2018) 13703–13710; doi:10.1021/jacs.8b07064

data_4132864
_publ_section_title
;
 New Hindered Amide Base for Aryne Insertion into Si-P, Si-S, Si-N, and
 C-C Bonds.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13703
_journal_page_last               13710
_journal_paper_doi               10.1021/jacs.8b07064
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C165 H252 Li8 N8'
_chemical_formula_weight         2403.25
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                95.3440(10)
_cell_angle_beta                 90.5550(10)
_cell_angle_gamma                108.0450(10)
_cell_formula_units_Z            1
_cell_length_a                   11.8908(3)
_cell_length_b                   15.5218(3)
_cell_length_c                   19.7689(5)
_cell_measurement_reflns_used    9153
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      66.64
_cell_measurement_theta_min      3.57
_cell_volume                     3451.27(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38423
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.732
_diffrn_reflns_theta_max         66.732
_diffrn_reflns_theta_min         2.246
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6147
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1322
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         11892
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^+1.7182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10221
_reflns_number_total             11892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b07064_si_001.cif
_cod_data_source_block           Adm2NLi_XW114
_cod_database_code               4132864
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              51009
_shelx_hkl_checksum              31881