Copper-Mediated Reduction of CO2 with pinB-SiMe2Ph via CO2 Insertion into a Copper-Silicon Bond
Christian Kleeberg; Man Sing Cheung; Zhenyang Lin; Todd B. Marder; Journal of the American Chemical Society 133 (2011) 19060–19063; doi:10.1021/ja208969d

data_4107168
_publ_contact_author_address
;
 Technische Universitaet Braunschweig
 Institut fuer Anorganische und Analytische Chemie
 Hagenring 30
 38106 Braunschweig
 Germany
;
_publ_contact_author_email       ch.kleeberg@tu-braunschweig.de
_publ_contact_author_fax         '+49 (0) 531 391-5387'
_publ_contact_author_name        'Christian Kleeberg'
_publ_contact_author_phone       '+49 (0) 531 391-5312'
_publ_section_title
;
 Copper-Mediated Reduction of CO2 with pinB-SiMe2Ph via CO2 Insertion into
 a Copper-Silicon Bond
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19060
_journal_page_last               19063
_journal_paper_doi               10.1021/ja208969d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C51 H70 B Cu N2 O6 Si2, 0.5 (C5 H12)'
_chemical_formula_sum            'C53.5 H76 B Cu N2 O6 Si2'
_chemical_formula_weight         973.69
_chemical_name_common            '[((iPrNHC)Cu-CO2-SiMe2Ph)(pinB-CO2-SiMe2Ph)]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.523(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.2913(6)
_cell_length_b                   23.7666(8)
_cell_length_c                   21.8524(9)
_cell_measurement_reflns_used    22202
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.2228
_cell_measurement_theta_min      3.2469
_cell_volume                     10871.8(7)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.)
;
_computing_publication_material
;
 WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
;
_computing_structure_refinement
;
 SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
;
_computing_structure_solution
;
 SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
 J. Appl. Crystallogr. 1993, 26, 343-350.)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1372
_diffrn_reflns_av_sigmaI/netI    0.1242
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            153861
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
 empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       'fragment of needle'
_exptl_crystal_F_000             4168
_exptl_crystal_recrystallization_method
;
 From a solution of [iPrNHC]CuOtBu and pinB-SiMe2Ph in PhMe under an 
 atmosphere of CO2 layered after 16 h with n-pentane at -20deg C.
;
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, rac. twin, 19022 Friedel pairs'
_refine_ls_abs_structure_Flack   0.36(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2428
_refine_ls_number_reflns         40159
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1930
_reflns_number_gt                27055
_reflns_number_total             40159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja208969d_si_001.cif
_cod_data_source_block           ck10ck
_cod_original_formula_sum        'C53.50 H76 B Cu N2 O6 Si2'
_cod_database_code               4107168