Visible-Light Photoredox Catalysis: Selective Reduction of Carbon Dioxide to Carbon Monoxide by a Nickel N-Heterocyclic Carbene-Isoquinoline Complex
V. Sara Thoi; Nikolay Kornienko; Charles G. Margarit; Peidong Yang; Christopher J. Chang; Journal of the American Chemical Society 135 (2013) 14413–14424; doi:10.1021/ja4074003

data_4120850
_publ_section_title
;
 Visible-Light Photoredox Catalysis: Selective Reduction of Carbon Dioxide
 to Carbon Monoxide by a Nickel N-Heterocyclic Carbene-Isoquinoline
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14413
_journal_page_last               14424
_journal_paper_doi               10.1021/ja4074003
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '2(C27 H22 N6 Ni), 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C30 H30 F12 N6 Ni P2'
_chemical_formula_weight         799.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.9270(14)
_cell_length_b                   26.7769(13)
_cell_length_c                   8.3326(4)
_cell_measurement_reflns_used    38688
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.307
_cell_measurement_theta_min      2.56
_cell_volume                     6008.0(5)
_computing_cell_refinement       'Bruker APEX2 v. 2009.3'
_computing_data_collection       'Bruker APEX2 v. 2009.3'
_computing_data_reduction        'Bruker APEX2 v. 2009.3'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            37547
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.862
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.6947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         10712
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0258P)^2^+5.4963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                8160
_reflns_number_total             10712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4074003_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4120850