Homoleptic copper(I)-bisphosphine complexes as photoredox catalysts.
Saha, Priya; Tomita, Ryunosuke; Tsuneda, Takao; Jiang, Pingyu; Taketsugu, Tetsuya; Jin, Mingoo; Huang, Dennis Chung-Yang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11725–11731; doi:10.1039/d5dt01099c

data_7719119
_publ_section_title
;
 Homoleptic copper(I)-bisphosphine complexes as photoredox catalysts.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11725
_journal_page_last               11731
_journal_paper_doi               10.1039/d5dt01099c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C72 H56 Cu O2 P4, B F4'
_chemical_formula_sum            'C72 H56 B Cu F4 O2 P4'
_chemical_formula_weight         1227.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-04 deposited with the CCDC.	2025-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.13810(10)
_cell_length_b                   24.51420(10)
_cell_length_c                   24.82890(10)
_cell_measurement_reflns_used    80434
_cell_measurement_temperature    153
_cell_measurement_theta_max      76.2400
_cell_measurement_theta_min      2.5190
_cell_volume                     12257.27(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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   -119.00 -67.00   0.50    0.21    --  -48.41-137.00  48.00  104
  2  \w   -120.00 -40.00   0.50    0.21    --  -48.41  -8.00 -86.00  160
  3  \w    -14.00  25.00   0.50    0.21    --  -48.41  19.00 120.00   78
  4  \w    -22.00  61.00   0.50    0.21    --   48.41 -57.00 120.00  166
  5  \w     31.00 120.00   0.50    0.21    --  102.75-137.00  48.00  178
  6  \w     31.00 111.00   0.50    0.21    --  102.75-125.00 -30.00  160
  7  \w     31.00 106.00   0.50    0.21    --  102.75 -99.00-150.00  150
  8  \w     31.00  69.00   0.50    0.21    --  102.75 -57.00 -90.00   76
  9  \w     31.00  69.00   0.50    0.21    --  102.75 -57.00-120.00   76
 10  \w     31.00 106.00   0.50    0.21    --  102.75 -99.00-180.00  150
 11  \w     31.00  69.00   0.50    0.21    --  102.75 -57.00 -60.00   76
 12  \w     95.00 174.00   0.50    0.21    --  102.75  37.00 -60.00  158
 13  \w     90.00 174.00   0.50    0.21    --  102.75  57.00 -60.00  168
 14  \w     41.00  79.00   0.50    0.21    --   48.41  37.00-150.00   76
 15  \w     31.00 106.00   0.50    0.21    --  102.75 -99.00  90.00  150
 16  \w     36.00 119.00   0.50    0.21    --   48.41  57.00 120.00  166
 17  \w    -23.00  41.00   0.50    0.21    --   48.41 -37.00 150.00  128
 18  \w   -164.00 -56.00   0.50    0.21    -- -102.00-152.00 -31.00  216
 19  \w   -171.00 -93.00   0.50    0.21    -- -102.00  -8.00 -86.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0748027000
_diffrn_orient_matrix_UB_12      0.0111568000
_diffrn_orient_matrix_UB_13      -0.0069355000
_diffrn_orient_matrix_UB_21      -0.0136900000
_diffrn_orient_matrix_UB_22      0.0618339000
_diffrn_orient_matrix_UB_23      -0.0000569000
_diffrn_orient_matrix_UB_31      0.0083714000
_diffrn_orient_matrix_UB_32      0.0012829000
_diffrn_orient_matrix_UB_33      0.0616526000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            113586
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.333
_diffrn_reflns_theta_min         2.840
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         12704
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0432P)^2^+6.5316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11694
_reflns_number_total             12704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01099c2.cif
_cod_data_source_block           CuDPEphos2BF4
_cod_depositor_comments
'Adding full bibliography for 7719116--7719120.cif.'
_cod_database_code               7719119
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu C H P O B F'
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.798
_diffrn_oxdiff_digest_hkl
;
017a0318ef492614b24b9d66af8bb8ee328db1
;
_olex2_refinement_description
;
1. Restrained distances
 B1-F1 = B1-F2 = B1-F7 = B1-F8
 1.42 with sigma of 0.02
 B2-F3 = B2-F4 = B2-F5 = B2-F6
 1.42 with sigma of 0.02
 F1-F2 \\sim F2-F7 \\sim F7-F8 \\sim F8-F1 \\sim F2-F8 \\sim F1-F7
 with sigma of 0.04
 B2-F3 \\sim B2-F4 \\sim B2-F5 \\sim B2-F6
 with sigma of 0.02
 F3-F4 \\sim F4-F5 \\sim F5-F6 \\sim F6-F3 \\sim F4-F6 \\sim F3-F5
 with sigma of 0.04
 F1-F2 \\sim F1-F7 \\sim F1-F8 \\sim F2-F7 \\sim F2-F8 \\sim F7-F8
 with sigma of 0.02
 B1-F1 \\sim B1-F2 \\sim B1-F7 \\sim B1-F8
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
B1 \\sim F1 \\sim F2 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
B2 \\sim F3 \\sim F4 \\sim F5 \\sim F6: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 B1, F1, F2, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: B2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5) B1(0.5) F1(0.5) F2(0.5)
 F7(0.5) F8(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C59(H59), C34(H34), C7(H7), C53(H53), C49(H49), C58(H58), C46(H46), C33(H33),
 C55(H55), C6(H6), C52(H52), C30(H30), C14(H14), C27(H27), C57(H57), C32(H32),
 C50(H50), C45(H45), C56(H56), C64(H64), C43(H43), C65(H65), C44(H44), C20(H20),
  C5(H5), C51(H51), C62(H62), C26(H26), C31(H31), C40(H40), C10(H10), C79(H79),
 C12(H12), C63(H63), C25(H25), C16(H16), C24(H24), C36(H36), C13(H13), C4(H4),
 C19(H19), C11(H11), C39(H39), C38(H38), C37(H37), C73(H73), C18(H18), C78(H78),
  C17(H17), C77(H77), C75(H75), C72(H72), C69(H69), C76(H76), C71(H71), C70(H70)
;
_shelx_res_checksum              29601
_shelx_hkl_checksum              63073
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.828