Exploring catalytic activity modulations: photoredox catalysis with substituted copper(i)-dipyridylamine derivatives
Villegas-Menares, Alondra; Hansmann, Yannik Sebastian; Bayas, Max; Verdugo, Camilo; Erazo, Ignacio; Zuñiga, Cesar; Gonzalez, Iván; Galdámez, Antonio; Villa, Lucrezia; Natali, Mirco; Cabrera, Alan R.; Dalton Transactions 54 (2025) 7306–7314; doi:10.1039/D4DT03337J

data_7718512
_publ_section_title
;
 Exploring catalytic activity modulations: photoredox catalysis with
 substituted copper(i)-dipyridylamine derivatives
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              7306
_journal_page_last               7314
_journal_paper_doi               10.1039/D4DT03337J
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C56 H39 Cu F6 N3 P2, C H2 Cl2, B F4'
_chemical_formula_sum            'C57 H41 B Cl2 Cu F10 N3 P2'
_chemical_formula_weight         1165.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-30 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.38420(10)
_cell_length_b                   19.9197(2)
_cell_length_c                   21.0692(2)
_cell_measurement_reflns_used    42759
_cell_measurement_temperature    99.97(10)
_cell_measurement_theta_max      76.1030
_cell_measurement_theta_min      3.0210
_cell_volume                     5197.55(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60749
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.854
_diffrn_reflns_theta_min         3.053
_exptl_absorpt_coefficient_mu    2.801
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 4488 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         10811
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0482P)^2^+2.1345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                10407
_reflns_number_total             10811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03337j2.cif
_cod_data_source_block           mib-059_v1
_cod_depositor_comments
'Adding full bibliography for 7718511--7718513.cif.'
_cod_database_code               7718512
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.393
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Cu(H) groups
2. Restrained distances
 C57-Cl1
 1.74 with sigma of 0.02
 C57-Cl2
 1.74 with sigma of 0.02
 C57'-Cl2'
 1.74 with sigma of 0.02
 C57'-Cl1'
 1.74 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C57) = Uanis(C57')
Uanis(Cl1) = Uanis(Cl1')
Uanis(Cl2) = Uanis(Cl2')
4. Rigid body (RIGU) restrains
 C57, Cl1, Cl2, C57', Cl1', Cl2'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C57')=Sof(H57C)=Sof(H57D)=Sof(Cl1')=Sof(Cl2')=1-FVAR(1)
 Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(Cl1)=Sof(Cl2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C57'(H57C,H57D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C37(H37),
 C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
;
_shelx_res_checksum              77465
_shelx_hkl_checksum              9453
_olex2_submission_special_instructions 'No special instructions were received'