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_7719118
_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         'C102 H84 Cu2 Fe3 P6, 2(B F4), 2[CH2Cl2]'
_chemical_formula_sum            'C104 H88 B2 Cl4 Cu2 F8 Fe3 P6'
_chemical_formula_weight         2133.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 128.902(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.6587(13)
_cell_length_b                   14.7541(2)
_cell_length_c                   25.9909(10)
_cell_measurement_reflns_used    8897
_cell_measurement_temperature    153
_cell_measurement_theta_max      54.5910
_cell_measurement_theta_min      3.4510
_cell_volume                     9746.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 0.940
_diffrn_measured_fraction_theta_max 0.940
_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      8.00  65.00   0.50   60.16    --   49.02 -73.00 135.00  114
  2  \w    -11.00  15.00   0.50   60.16    --  -49.02  19.00 150.00   52
  3  \w    -61.00 -35.00   0.50   60.16    -- -102.00  57.00  60.00   52
  4  \w    -56.00 -30.00   0.50   60.16    -- -102.00  57.00   0.00   52
  5  \w    -14.00  24.00   0.50   60.16    --  -49.02  19.00 -90.00   76
  6  \w    -63.00 -32.00   0.50   60.16    -- -102.00  57.00-120.00   62
  7  \w    -62.00 -32.00   0.50   60.16    -- -102.00  57.00 120.00   60
  8  \w   -155.00 -84.00   0.50   60.16    -- -102.00 -73.00 135.00  142
  9  \w   -173.00 -97.00   0.50   60.16    -- -102.00 -95.00  38.00  152
 10  \w   -169.00-115.00   0.50   60.16    -- -102.00 -58.00 -91.00  108
 11  \w   -114.00 -79.00   0.50   60.16    --  -49.02-125.00-150.00   70
;
_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      -0.0319004000
_diffrn_orient_matrix_UB_12      0.0671397000
_diffrn_orient_matrix_UB_13      -0.0581270000
_diffrn_orient_matrix_UB_21      0.0333501000
_diffrn_orient_matrix_UB_22      -0.0252119000
_diffrn_orient_matrix_UB_23      -0.0211004000
_diffrn_orient_matrix_UB_31      -0.0392588000
_diffrn_orient_matrix_UB_32      -0.0759272000
_diffrn_orient_matrix_UB_33      -0.0443958000
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13058
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        54.239
_diffrn_reflns_theta_max         54.239
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         5600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0403P)^2^+21.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0798
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5181
_reflns_number_total             5600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01099c2.cif
_cod_data_source_block           Cu2dppf3BF4
_cod_depositor_comments
'Adding full bibliography for 7719116--7719120.cif.'
_cod_original_cell_volume        9746.2(8)
_cod_database_code               7719118
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H Fe Cu P'
_cell_oxdiff_angle_alpha         90.016(3)
_cell_oxdiff_angle_beta          128.854(5)
_cell_oxdiff_angle_gamma         89.978(3)
_cell_oxdiff_length_a            32.6486(15)
_cell_oxdiff_length_b            14.7501(4)
_cell_oxdiff_length_c            25.9884(10)
_cell_oxdiff_measurement_reflns_used 8778
_cell_oxdiff_volume              9746.2(6)
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.739
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00G(H00G), C00I(H00I), C00J(H00J), C00L(H00L), C00N(H00N),
 C00O(H00O), C00Q(H00Q), C00R(H00R), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01S(H01S)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99030
_shelx_hkl_checksum              54790
_shelx_fab_checksum              50304
_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 1.575
_oxdiff_exptl_absorpt_empirical_full_min 0.600