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_4107169
_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         'C36 H47 Cu N2 O2 Si, C3 H7'
_chemical_formula_sum            'C39 H54 Cu N2 O2 Si'
_chemical_formula_weight         674.47
_chemical_name_common            '[(iPrNHC)Cu-CO2-SiMe2Ph]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.8940(10)
_cell_angle_beta                 81.3130(10)
_cell_angle_gamma                73.5300(10)
_cell_formula_units_Z            4
_cell_length_a                   13.5028(4)
_cell_length_b                   17.0624(5)
_cell_length_c                   18.3259(6)
_cell_measurement_reflns_used    8205
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.34
_cell_volume                     3839.2(2)
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_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
;
 SHELXS-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122)' 
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 6K CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58610
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2006/1 (Bruker AXS), R(int)=0.1228 before correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_recrystallization_method
;
 From a solution in 
 PhMe/n-hexane at -20deg C
;
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         18541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0981P)^2^+0.9116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1727
_reflns_number_gt                13437
_reflns_number_total             18541
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja208969d_si_002.cif
_cod_data_source_block           09s309m
_cod_database_code               4107169