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_1569760
_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 H41 Cu N6 O2'
_chemical_formula_sum            'C56 H41 Cu N6 O2'
_chemical_formula_weight         893.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-10
_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                90
_cell_angle_beta                 102.2042(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4587(2)
_cell_length_b                   13.34870(17)
_cell_length_c                   20.0214(2)
_cell_measurement_reflns_used    12353
_cell_measurement_temperature    100.03(13)
_cell_measurement_theta_max      76.0120
_cell_measurement_theta_min      3.1450
_cell_volume                     4299.34(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Shelxtl-Plus/XP, Bruker AXS, Inc. 2009'
_computing_publication_material  'Shelxtl-Plus, Bruker AXS, Inc. 2009'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -72.00  19.00   0.50   14.00    --  -48.57  80.00-146.00  182
  2  \w    -10.00  70.00   0.50   14.00    --   48.57 -80.00  90.00  160
  3  \w     47.00 132.00   0.50   47.00    --  107.75 -80.00  90.00  170
  4  \w    120.00 172.00   0.50   47.00    --  107.75  80.00-146.00  104
  5  \w    -61.00  24.00   0.50   14.00    --  -48.57  38.00 -30.00  170
  6  \w     35.00  66.00   0.50   47.00    --  107.75 -99.00-120.00   62
  7  \w     75.00 105.00   0.50   47.00    --  107.75 -99.00-120.00   60
  8  \w     37.00 123.00   0.50   47.00    --  107.75 -57.00 -60.00  172
  9  \w     95.00 177.00   0.50   47.00    --  107.75 125.00 150.00  164
 10  \w     95.00 178.00   0.50   47.00    --  107.75  19.00-150.00  166
 11  \w     95.00 176.00   0.50   47.00    --  107.75  38.00 150.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0073425000
_diffrn_orient_matrix_UB_12      -0.0873114000
_diffrn_orient_matrix_UB_13      -0.0512880000
_diffrn_orient_matrix_UB_21      0.0690088000
_diffrn_orient_matrix_UB_22      0.0470986000
_diffrn_orient_matrix_UB_23      -0.0311261000
_diffrn_orient_matrix_UB_31      0.0660066000
_diffrn_orient_matrix_UB_32      -0.0589621000
_diffrn_orient_matrix_UB_33      0.0509614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23523
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.042
_diffrn_reflns_theta_min         3.166
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.25a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       needle
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8651
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0633P)^2^+3.6102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7583
_reflns_number_total             8651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03428c2.cif
_cod_data_source_block           76p_auto
_cod_depositor_comments
'Adding full bibliography for 1569760--1569761.cif.'
_cod_original_cell_volume        4299.35(10)
_cod_database_code               1569760
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P F Cu'
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 N5-H5
 0.84 with sigma of 0.02
 O1-H14
 0.84 with sigma of 0.02
 C36-H5 \\sim C35-H5
 with sigma of 0.01
3. Others
 Sof(H14)=1-FVAR(1)
 Sof(H5)=FVAR(1)
 Uiso(H14)=Uiso(H5)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5A), C6(H6), C8(H8), C9(H9), C15(H15), C17(H17), C24(H24),
  C26(H26), C31(H31), C32(H32), C33(H33), C40(H40), C41(H41), C42(H42),
 C43(H43), C47(H47), C48(H48), C52(H52), C53(H53), C54(H54)
4.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,
 H28C), C29(H29B,H29C,H29A), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              79072
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.471
_oxdiff_exptl_absorpt_empirical_full_min 0.617