Trinuclear copper(I) furanyl <i>ortho</i>-diphosphine halide clusters: structure, photophysical and photocatalytic hydrogen production properties.
Chen, Xiang; Liu, Li; Zhong, Xin-Xin; Li, Fa-Bao; Cong, Heng-Jiang; Li, Feng-Yan; Zhao, Yi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15223–15234; doi:10.1039/d5dt01864a

data_1575760
_publ_section_title
;
 Trinuclear copper(I) furanyl <i>ortho</i>-diphosphine halide clusters:
 structure, photophysical and photocatalytic hydrogen production
 properties.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15223
_journal_page_last               15234
_journal_paper_doi               10.1039/d5dt01864a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C56 H44 Cl3 Cu3 O2 P4, C H2 Cl2'
_chemical_formula_sum            'C57 H46 Cl5 Cu3 O2 P4'
_chemical_formula_weight         1254.69
_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             2019-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-31 deposited with the CCDC.	2025-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.8130(10)
_cell_angle_beta                 106.5680(10)
_cell_angle_gamma                97.1950(10)
_cell_formula_units_Z            2
_cell_length_a                   12.78510(10)
_cell_length_b                   13.4486(2)
_cell_length_c                   18.4148(2)
_cell_measurement_reflns_used    84949
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.9590
_cell_measurement_theta_min      3.5010
_cell_volume                     2809.91(6)
_computing_cell_refinement
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_collection
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_data_reduction
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'Hybrid Pixel Counting (HPC) detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HyPix-6000HE'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.949
_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    -84.00  39.00   0.50    0.50    --    5.00 -52.00 141.00  246
  2  \w    -82.00  42.00   0.50    0.50    --  -47.30  52.00 -74.00  248
  3  \w   -137.00 -13.00   0.50    0.50    --  -47.30 -52.00 141.00  248
  4  \w   -192.00 -68.00   0.50    0.50    -- -102.20 -52.00 141.00  248
  5  \w   -137.00 -13.00   0.50    0.50    -- -102.20  52.00 -74.00  248
  6  \w    -29.00  94.00   0.50    0.50    --    5.00  52.00 -74.00  246
  7  \w   -137.00  -8.00   0.50    0.50    --  -47.30 -75.00  90.00  258
  8  \w   -137.00  -8.00   0.50    0.50    --  -47.30 -75.00-120.00  258
  9  \w   -137.00  -8.00   0.50    0.50    --  -47.30 -75.00 -30.00  258
 10  \w   -151.00 -23.00   0.50    0.50    --  -62.00 -74.00 -95.05  256
 11  \w   -159.00 -31.00   0.50    0.50    --  -70.00 -75.00-142.18  256
 12  \w   -159.00 -31.00   0.50    0.50    --  -70.00 -75.00  21.58  256
 13  \w   -159.00 -32.00   0.50    0.50    --  -70.00 -73.00-171.52  254
 14  \w   -163.00 -35.00   0.50    0.50    --  -74.00 -75.00  73.54  256
 15  \w   -163.00 -35.00   0.50    0.50    --  -74.00 -75.00 128.30  256
 16  \w   -171.00 -43.00   0.50    0.50    --  -82.00 -74.00   3.16  256
 17  \w   -175.00 -47.00   0.50    0.50    --  -86.00 -75.00 -11.26  256
 18  \w   -175.00 -47.00   0.50    0.50    --  -86.00 -75.00 -84.20  256
 19  \w   -179.00 -53.00   0.50    0.50    --  -90.00 -72.00 148.69  252
 20  \w   -179.00 -51.00   0.50    0.50    --  -90.00 -74.00  74.03  256
 21  \w   -179.00 -51.00   0.50    0.50    --  -90.00 -74.00 109.98  256
 22  \w   -179.00 -51.00   0.50    0.50    --  -90.00 -74.00 -53.06  256
 23  \w   -179.00 -56.00   0.50    0.50    --  -90.00 -62.00  89.25  246
 24  \w   -179.00 -51.00   0.50    0.50    --  -90.00 -75.00 -90.16  256
 25  \w   -179.00 -55.00   0.50    0.50    --  -90.00 -65.00   4.16  248
 26  \w   -179.00 -52.00   0.50    0.50    --  -90.00 -73.00 -32.83  254
 27  \w   -183.00 -55.00   0.50    0.50    --  -94.00 -74.00-172.37  256
 28  \w   -183.00 -56.00   0.50    0.50    --  -94.00 -73.00-138.21  254
 29  \w   -183.00 -55.00   0.50    0.50    --  -94.00 -75.00-148.01  256
 30  \w   -183.00 -56.00   0.50    0.50    --  -94.00 -73.00 140.98  254
 31  \w   -183.00 -56.00   0.50    0.50    --  -94.00 -73.00-120.00  254
 32  \w   -183.00 -56.00   0.50    0.50    --  -94.00 -73.00-120.00  254
 33  \w   -187.00 -59.00   0.50    0.50    --  -98.00 -75.00  60.88  256
 34  \w   -142.00 -13.00   0.50    0.50    -- -102.20  75.00  30.00  258
 35  \w   -142.00 -13.00   0.50    0.50    -- -102.20  75.00-120.00  258
 36  \w   -142.00 -13.00   0.50    0.50    -- -102.20  75.00-180.00  258
 37  \w   -142.00 -13.00   0.50    0.50    -- -102.20  75.00 -30.00  258
 38  \w   -192.00 -63.00   0.50    0.50    -- -102.20 -75.00   0.00  258
 39  \w   -142.00 -13.00   0.50    0.50    -- -102.20  75.00  90.00  258
 40  \w    -34.00  94.00   0.50    0.50    --    5.00  75.00  60.00  256
 41  \w   -137.00 -15.00   0.50    0.50    --  -47.30 -75.00   0.00  244
 42  \w   -155.00 -27.00   0.50    0.50    --  -66.00 -75.00  63.20  256
 43  \w   -159.00 -31.00   0.50    0.50    --  -70.00 -75.00 148.30  256
 44  \w   -163.00 -35.00   0.50    0.50    --  -74.00 -75.00 -33.59  256
 45  \w   -163.00 -35.00   0.50    0.50    --  -74.00 -75.00  -6.46  256
 46  \w   -163.00 -36.00   0.50    0.50    --  -74.00 -73.00 -70.51  254
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       'profile data from \w-scans and \phi-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0681828000
_diffrn_orient_matrix_UB_12      0.0319049000
_diffrn_orient_matrix_UB_13      -0.0494928000
_diffrn_orient_matrix_UB_21      0.0114407000
_diffrn_orient_matrix_UB_22      -0.1165874000
_diffrn_orient_matrix_UB_23      -0.0328489000
_diffrn_orient_matrix_UB_31      -0.1092271000
_diffrn_orient_matrix_UB_32      -0.0263883000
_diffrn_orient_matrix_UB_33      -0.0722397000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'VariMax VHF'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            121055
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.529
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    4.904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.132
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10888
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0552
_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^)+(0.1026P)^2^+3.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10520
_reflns_number_total             10888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01864a2.cif
_cod_data_source_block           cx-fn-cl-200k-190924
_cod_depositor_comments
'Adding full bibliography for 1575758--1575760.cif.'
_cod_database_code               1575760
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'H C P O Cu Cl'
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-C57 \\sim Cl5-C57
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl5 \\sim C57 \\sim Cl4: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B)
4.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C44(H44), C30(H30), C36(H36), C46(H46), C15(H15), C40(H40),
 C50(H50), C54(H54), C52(H52), C12(H12), C34(H34), C56(H56), C24(H24), C37(H37),
  C31(H31), C14(H14), C28(H28), C25(H25), C39(H39), C55(H55), C53(H53),
 C26(H26), C38(H38), C6(H6), C47(H47), C2(H2), C48(H48), C8(H8), C11(H11),
 C49(H49), C27(H27), C32(H32), C33(H33), C18(H18), C5(H5), C3(H3), C4(H4),
 C10(H10), C20(H20), C22(H22), C19(H19), C9(H9), C21(H21)
;
_shelx_res_checksum              95721
_shelx_hkl_checksum              67615
_shelx_fab_checksum              88530
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.821