Photochemical charge accumulation in a heteroleptic copper(i)-anthraquinone molecular dyad <i>via</i> proton-coupled electron transfer.
Xie, Zhu-Lin; Gupta, Nikita; Niklas, Jens; Poluektov, Oleg G.; Lynch, Vincent M.; Glusac, Ksenija D.; Mulfort, Karen L.; Chemical science 14 (2023) 10219–10235; doi:10.1039/d3sc03428c

data_1569761
_publ_section_title
;
 Photochemical charge accumulation in a heteroleptic
 copper(i)-anthraquinone molecular dyad <i>via</i> proton-coupled electron
 transfer.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              10219
_journal_page_last               10235
_journal_paper_doi               10.1039/d3sc03428c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C56 H40 Cu N6 O2, F6 P'
_chemical_formula_sum            'C56 H40 Cu F6 N6 O2 P'
_chemical_formula_weight         1037.45
_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             2020-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2023-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                82.066(2)
_cell_angle_beta                 88.421(2)
_cell_angle_gamma                72.642(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8051(3)
_cell_length_b                   13.6401(3)
_cell_length_c                   20.0438(5)
_cell_measurement_reflns_used    16448
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      73.1
_cell_measurement_theta_min      3.40
_cell_volume                     2792.30(13)
_computing_cell_refinement
'CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)'
_computing_data_collection
'CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)'
_computing_data_reduction
'CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)'
_computing_molecular_graphics    'Shelxtl-Plus\XP, Bruker AXS, Inc. 2009'
_computing_publication_material  'Shelxtl-Plus\XP, Bruker AXS, Inc. 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 0.995
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31613
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.331
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.70a (Rigaku Oxford Diffraction, 2020)
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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       plank
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         10925
_refine_ls_number_restraints     600
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+1.2395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9572
_reflns_number_total             10925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03428c2.cif
_cod_data_source_block           zsx-1-135-3rd
_cod_depositor_comments
'Adding full bibliography for 1569760--1569761.cif.'
_cod_original_cell_volume        2792.31(13)
_cod_database_code               1569761
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F3-P1
 1.57 with sigma of 0.03
 F2-F4
 2.43 with sigma of 0.04
 F5-F1
 2.43 with sigma of 0.04
 P1-F5
 1.57 with sigma of 0.03
 F5-F2
 2.43 with sigma of 0.04
 F1-P1
 1.57 with sigma of 0.03
 F1-F6
 2.43 with sigma of 0.04
 F6-P1
 1.57 with sigma of 0.03
 F3-F4
 2.43 with sigma of 0.04
 F2-P1
 1.57 with sigma of 0.03
 F5-F6
 2.43 with sigma of 0.04
 P1-F4
 1.57 with sigma of 0.03
 F5-F4
 2.43 with sigma of 0.04
 F1-F3
 2.43 with sigma of 0.04
 F6-F2
 2.43 with sigma of 0.04
 F3-F6
 2.43 with sigma of 0.04
 F4-F1
 2.43 with sigma of 0.04
 F3-F2
 2.43 with sigma of 0.04
 P2-F1A = P2-F2A = P2-F3A = P2-F4A = P2-F5A = P2-F6A
 1.57 with sigma of 0.03
 F1A-F3A = F1A-F4A = F1A-F5A = F1A-F6A = F2A-F3A = F2A-F4A = F2A-F5A = F2A-F6A
 2.43 with sigma of 0.04
 F3A-F4A = F3A-F6A = F4A-F5A = F5A-F6A
 2.43 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1 \\sim P2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F1A \\sim F2A \\sim F3A
\\sim F4A \\sim F5A \\sim F6A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(P2)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15), C17(H17),
 C24(H24), C26(H26), C31(H31), C32(H32), C33(H33), C38(H38), C39(H39), C40(H40),
  C48(H48), C49(H49), C50(H50), C51(H51), C55(H55), C56(H56)
5.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91943
_shelx_fab_checksum              77751
_olex2_submission_special_instructions 'No special instructions were received'