Copper(ii) complexes of quinoline-based ligands for efficient photoredox catalysis of atom transfer radical addition (ATRA) reaction
Chaibuth, Pawittra; Chuaytanee, Nontakarn; Hojitsiriyanont, Jutawat; Chainok, Kittipong; Wacharasindhu, Sumrit; Reiser, Oliver; Sukwattanasinitt, Mongkol; New Journal of Chemistry 46 (2022) 12158–12168; doi:10.1039/D2NJ01218A

data_7061591
_publ_section_title
;
 Copper(ii) complexes of quinoline-based ligands for efficient photoredox
 catalysis of atom transfer radical addition (ATRA) reaction
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12158
_journal_page_last               12168
_journal_paper_doi               10.1039/D2NJ01218A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         '2(C27 H18 Cl Cu N4), Cl4 Cu'
_chemical_formula_sum            'C54 H36 Cl6 Cu3 N8'
_chemical_formula_weight         1200.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-02-21 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                111.357(4)
_cell_angle_beta                 98.835(4)
_cell_angle_gamma                115.205(4)
_cell_formula_units_Z            2
_cell_length_a                   13.9396(18)
_cell_length_b                   15.824(2)
_cell_length_c                   16.096(2)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.761
_cell_measurement_theta_min      2.96
_cell_volume                     2783.9(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_detector                 'Bruker PHOTON 200 area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 QUEST CMOS PHOTON II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            76310
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.821
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_type              Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0886 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.8792.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             1210
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         14494
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0615P)^2^+1.7606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10772
_reflns_number_total             14494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01218a2.cif
_cod_data_source_block           q3
_cod_depositor_comments
'Adding full bibliography for 7061589--7061591.cif.'
_cod_database_code               7061591
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.636
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cu3-Cl3 \\sim Cu3A-Cl3A
 with sigma of 0.02
 Cu3-Cl4 \\sim Cu3A-Cl4A
 with sigma of 0.02
 Cu3-Cl5 \\sim Cu3A-Cl5A
 with sigma of 0.02
 Cu3-Cl6 \\sim Cu3A-Cl6A
 with sigma of 0.02
 Cl4-Cl6 \\sim Cl4A-Cl6A
 with sigma of 0.04
 Cl5-Cl6 \\sim Cl5A-Cl6A
 with sigma of 0.04
 Cl4-Cl5 \\sim Cl4A-Cl5A
 with sigma of 0.04
 Cl3-Cl4 \\sim Cl3A-Cl4A
 with sigma of 0.04
 Cl3-Cl5 \\sim Cl3A-Cl5A
 with sigma of 0.04
 Cl3-Cl6 \\sim Cl3A-Cl6A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Cl6A) \\sim Ueq, Uanis(Cl4A) \\sim Ueq, Uanis(Cu3A) \\sim Ueq,
Uanis(Cl3A) \\sim Ueq, Uanis(Cl5A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cu3A, Cl3A, Cl4A, Cl5A, Cl6A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Cu3, Cl3, Cl4, Cl5, Cl6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(Cu3A)=Sof(Cl3A)=Sof(Cl4A)=Sof(Cl5A)=Sof(Cl6A)=1-FVAR(1)
 Sof(Cu3)=Sof(Cl3)=Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              82121
_shelx_fab_checksum              42575
_olex2_submission_special_instructions 'No special instructions were received'