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_7719120
_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         'C78 H64 Cu O2 P4, B F4, 0.25[C4H10O]'
_chemical_formula_sum            'C78 H64 B Cu F4 O2 P4'
_chemical_formula_weight         1307.635
_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'
_symmetry_Int_Tables_number      60
_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            4
_cell_length_a                   18.3976(1)
_cell_length_b                   18.2710(1)
_cell_length_c                   18.6164(1)
_cell_measurement_reflns_used    41470
_cell_measurement_temperature    153
_cell_measurement_theta_max      76.2190
_cell_measurement_theta_min      2.3990
_cell_volume                     6257.76(6)
_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  'olex2.refine 1.5 (Bourhis et al., 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 0.9970
_diffrn_measured_fraction_theta_max 0.9831
_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     63.00 121.00   0.50    5.58    --   49.02 148.00  84.00  116
  2  \w     77.00 174.00   0.50    5.58    --  102.75 127.00   9.00  194
  3  \w     95.00 174.00   0.50    5.58    --  102.75  37.00-120.00  158
  4  \w     94.00 174.00   0.50    5.58    --  102.75   8.00-177.00  160
  5  \w     95.00 174.00   0.50    5.58    --  102.75  37.00  90.00  158
  6  \w     31.00 111.00   0.50    5.58    --  102.75-125.00 -30.00  160
  7  \w     31.00  69.00   0.50    5.58    --  102.75 -57.00-120.00   76
  8  \w     31.00  69.00   0.50    5.58    --  102.75 -57.00 -90.00   76
  9  \w     31.00 106.00   0.50    5.58    --  102.75 -99.00-180.00  150
 10  \w     31.00  69.00   0.50    5.58    --  102.75 -57.00-180.00   76
 11  \w     28.00 104.00   0.50    5.58    --   49.02  77.00 -30.00  152
 12  \w     31.00  69.00   0.50    5.58    --  102.75 -57.00 150.00   76
 13  \w    -14.00  24.00   0.50    5.58    --  -49.02  19.00 -60.00   76
 14  \w    -14.00  24.00   0.50    5.58    --  -49.02  19.00   0.00   76
 15  \w    -37.00  23.00   0.50    5.58    --  -49.02  37.00-120.00  120
 16  \w    -62.00  23.00   0.50    5.58    --  -49.02  57.00-180.00  170
 17  \w    -65.00 -30.00   0.50    5.58    -- -102.00  57.00   0.00   70
 18  \w   -109.00 -30.00   0.50    5.58    -- -102.00 123.00 -79.00  158
 19  \w    -65.00 -30.00   0.50    5.58    -- -102.00  57.00-150.00   70
 20  \w   -111.00 -30.00   0.50    5.58    -- -102.00 125.00-180.00  162
 21  \w   -121.00 -74.00   0.50    5.58    --  -49.02-125.00 -30.00   94
;
_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      0.0736947000
_diffrn_orient_matrix_UB_12      0.0407583000
_diffrn_orient_matrix_UB_13      0.0009706000
_diffrn_orient_matrix_UB_21      -0.0407289000
_diffrn_orient_matrix_UB_22      0.0727892000
_diffrn_orient_matrix_UB_23      -0.0086124000
_diffrn_orient_matrix_UB_31      -0.0051075000
_diffrn_orient_matrix_UB_32      0.0071129000
_diffrn_orient_matrix_UB_33      0.0822712000
_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  0.0229
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.9831
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56712
_diffrn_reflns_point_group_measured_fraction_full 0.9970
_diffrn_reflns_point_group_measured_fraction_max 0.9831
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.54
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62545
_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    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             2716.766
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.9664
_refine_diff_density_min         -0.4815
_refine_diff_density_rms         0.0994
_refine_ls_d_res_high            0.7927
_refine_ls_d_res_low             12.9641
_refine_ls_goodness_of_fit_ref   1.0057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    60
_refine_ls_number_parameters     430
_refine_ls_number_reflns         6470
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.0000
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0090P)^2^+33.1842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6253
_reflns_number_total             6470
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt01099c2.cif
_cod_data_source_block           CuXantPhos2BF4
_cod_depositor_comments
'Adding full bibliography for 7719116--7719120.cif.'
_cod_database_code               7719120
_chemical_oxdiff_formula         'C O H P Cu B F'
_diffrn_oxdiff_digest_hkl
;
010e759ca02f63ba48a2917c386c5902cd3b0a
;
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H01b,H01c,H01e} of C01I
 At 1.5 times of:
  {H00a,H00g,H00h} of C00X
2. Restrained distances
 B2-F3 = B2-F4 = B2-F5 = B2-F6
 1.42 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
 F3-F4 \\sim F3-F5 \\sim F3-F6 \\sim F4-F5 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.02
 B2-F3 \\sim B2-F4 \\sim B2-F5 \\sim B2-F6
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
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
4. Rigid body (RIGU) restrains
 B2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: B2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5)
6.a Riding coordinates:
 C00C(H00C), C00D(H00D), C00J(H00J), C00K(H00K), C00O(H00O), C00R(H00R),
 C00T(H00T), C011(H011), C014(H014), C016(H016), C017(H017), C018(H018),
 C01A(H01A), C01D(H01D), C01G(H01G), C01H(H01H), C01I(H01b,H01c,H01e),
 C01S(H01S)
6.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C02D(H02D), C02A(H02A), C02B(H02B), C00E(H00E), C00F(H00F),
 C00U(H00U), C012(H012), C013(H013)
6.c Idealised Me refined as rotating group:
 C00X(H00a,H00g,H00h)
;
_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 3.443
_oxdiff_exptl_absorpt_empirical_full_min 0.670