Spectroscopic Characterization and Mechanistic Studies on Visible Light Photoredox Carbon‒Carbon Bond Formation by Bis(arylimino)acenaphthene Copper Photosensitizers
Ng, Yik Yie; Tan, Lisa Jiaying; Ng, Shue Mei; Chai, Yoke Tin; Ganguly, Rakesh; Du, Yonghua; Yeow, Edwin Kok Lee; Soo, Han Sen; ACS Catalysis 8 (2018) 11277–; doi:10.1021/acscatal.8b02502

data_4515793
_publ_section_title
;
 Spectroscopic Characterization and Mechanistic Studies on Visible Light
 Photoredox Carbon--Carbon Bond Formation by Bis(arylimino)acenaphthene
 Copper Photosensitizers
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11277
_journal_paper_doi               10.1021/acscatal.8b02502
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C76 H92 Br2 Cu F6 N12 O15 P'
_chemical_formula_weight         1781.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 114.7964(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.796(2)
_cell_length_b                   14.7426(14)
_cell_length_c                   22.903(3)
_cell_measurement_reflns_used    4169
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      20.2042
_cell_measurement_theta_min      2.2520
_cell_volume                     8213.5(15)
_computing_cell_refinement       'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.35A (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2015)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2015)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1565
_diffrn_reflns_av_unetI/netI     0.1821
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39682
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'
_exptl_absorpt_coefficient_mu    1.342
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.744
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     2354
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.1944
_refine_ls_R_factor_gt           0.0866
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2333
_refine_ls_wR_factor_ref         0.2711
_reflns_number_gt                3348
_reflns_number_total             8416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02502_si_002.cif
_cod_data_source_block           shs106s
_cod_original_cell_volume        8213.5(16)
_cod_database_code               4515793
_shelx_res_checksum              2030
_shelx_hkl_checksum              18022