Silicon-Mediated Selective Homo- and Heterocoupling of Carbon Monoxide.
Wang, Yuwen; Kostenko, Arseni; Hadlington, Terrance J.; Luecke, Marcel-Philip; Yao, Shenglai; Driess, Matthias; Journal of the American Chemical Society 141 (2019) 626–634; doi:10.1021/jacs.8b11899

data_4133630
_publ_section_title
;
 Silicon-Mediated Selective Homo- and Heterocoupling of Carbon Monoxide.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              626
_journal_page_last               634
_journal_paper_doi               10.1021/jacs.8b11899
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C55 H67 N5 O2 Si2'
_chemical_formula_weight         886.31
_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
_audit_creation_method           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.9921(3)
_cell_length_b                   21.7092(4)
_cell_length_c                   27.5293(4)
_cell_measurement_reflns_used    13104
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9320
_cell_measurement_theta_min      3.1840
_cell_volume                     10155.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            71457
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.000
_diffrn_reflns_theta_min         3.673
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9630
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+3.4562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7022
_reflns_number_total             9630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11899_si_002.cif
_cod_data_source_block           6
_cod_database_code               4133630
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.958
_shelx_res_checksum              17427
_shelx_hkl_checksum              61455