Photocatalytic carboxylation of aryl halides/alkenes with a copper(I) complex bypassing the demand for dual catalysts.
David, A. John; Seethapathy, Logeshwari; Kumar, S. Vijay; Das, Rajorshi; Das, Anjan; Chemical communications (Cambridge, England) 61 (2025) 17677–17680; doi:10.1039/d5cc04943a

data_7135090
_publ_section_title
;
 Photocatalytic carboxylation of aryl halides/alkenes with a copper(I)
 complex bypassing the demand for dual catalysts.
;
_journal_issue                   90
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17677
_journal_page_last               17680
_journal_paper_doi               10.1039/d5cc04943a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C24 H16 Cl Cu N4, 2.3[CH3CN]'
_chemical_formula_sum            'C28.6 H22.9 Cl Cu N6.3'
_chemical_formula_weight         553.82
_chemical_name_systematic        Copper(I)Phen
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-27 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.687(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.240(2)
_cell_length_b                   30.200(3)
_cell_length_c                   7.4950(6)
_cell_measurement_reflns_used    8824
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      2.21
_cell_measurement_theta_min      25.67
_cell_volume                     5213.1(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX III CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35604
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_min         2.208
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       needle
_exptl_crystal_F_000             2277
_exptl_crystal_preparation       'Slow evaporation'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH3CN and DMF'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5331
_refine_ls_number_restraints     484
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0503P)^2^+10.7902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3904
_reflns_number_total             5331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04943a2.cif
_cod_data_source_block           cuphen_a
_cod_depositor_comments          'Adding full bibliography for 7135090.cif.'
_cod_original_formula_sum        'C28.60 H22.90 Cl Cu N6.30'
_cod_database_code               7135090
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.669
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C3(H3), C2(H2), C1(H1),
 C24(H24), C23(H23), C20(H20), C21(H21), C22(H22), C15(H15), C14(H14), C13(H13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              47145
_shelx_hkl_checksum              20741
_shelx_fab_checksum              93794
_olex2_submission_original_sample_id CuPhen
_olex2_submission_special_instructions 'No special instructions were received'