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_4133625
_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            'C51 H68 N4 O4 Si2'
_chemical_formula_weight         857.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6523(2)
_cell_length_b                   17.3543(3)
_cell_length_c                   18.3413(2)
_cell_measurement_reflns_used    10437
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.9250
_cell_measurement_theta_min      3.4760
_cell_volume                     4982.13(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (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  0.0604
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34017
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.490
_diffrn_reflns_theta_max         67.490
_diffrn_reflns_theta_min         3.506
_exptl_absorpt_coefficient_mu    1.002
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       rod
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2851 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.978(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         8971
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0586P)^2^+1.1478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7526
_reflns_number_total             8971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11899_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4133625
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              79870
_shelx_hkl_checksum              7985