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_1575758
_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 Cu3 I3 O2 P4'
_chemical_formula_sum            'C56 H44 Cu3 I3 O2 P4'
_chemical_formula_weight         1444.11
_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             2019-08-14
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0784(2)
_cell_length_b                   17.9614(2)
_cell_length_c                   18.4220(2)
_cell_measurement_reflns_used    24016
_cell_measurement_temperature    297.06(10)
_cell_measurement_theta_max      74.2390
_cell_measurement_theta_min      3.3910
_cell_volume                     5981.87(11)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.06(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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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      9.00  45.00   0.50    5.00    --    5.00  43.00 169.00   72
  2  \w    -74.00 -49.00   0.50    5.00    --  -47.20 -43.00  18.00   50
  3  \w    -46.00 -21.00   0.50    5.00    --  -47.20  43.00 169.00   50
  4  \w   -138.00-113.00   0.50    5.00    -- -102.20 -43.00  18.00   50
  5  \w    -76.00 -51.00   0.50    5.00    -- -102.20  43.00 169.00   50
  6  \w     24.00  50.00   0.50    5.00    --    5.00  57.00-150.00   52
  7  \w    -81.00  33.00   0.50    5.00    --  -47.20  57.00  30.00  228
  8  \w   -150.00-100.00   0.50    5.00    -- -102.20 -57.00-150.00  100
  9  \w   -142.00 -13.00   0.50    5.00    -- -102.20  75.00-150.00  258
 10  \w   -183.00 -79.00   0.50    5.00    -- -102.20 -57.00 150.00  208
 11  \w    -99.00 -74.00   0.50    5.00    --  -47.20 -56.00  64.00   50
 12  \w   -132.00-101.00   0.50    5.00    --  -47.20 -38.00 -30.00   62
 13  \w    -90.00 -26.00   0.50    5.00    --  -47.20 -38.00 -30.00  128
 14  \w   -131.00-104.00   0.50    5.00    -- -108.20 -57.00 120.00   54
 15  \w   -197.00-139.00   0.50    5.00    -- -108.20 -57.00 120.00  116
 16  \w   -107.00 -53.00   0.50    5.00    -- -108.20  57.00  60.00  108
 17  \w   -104.00 -78.00   0.50    5.00    -- -108.20  57.00 -90.00   52
 18  \w   -138.00-113.00   0.50    5.00    -- -108.20  57.00  60.00   50
 19  \w    -47.00 -22.00   0.50    5.00    --    5.00 -56.00  64.00   50
;
_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      0.0255970000
_diffrn_orient_matrix_UB_12      0.0707956000
_diffrn_orient_matrix_UB_13      0.0400295000
_diffrn_orient_matrix_UB_21      -0.0600436000
_diffrn_orient_matrix_UB_22      0.0454379000
_diffrn_orient_matrix_UB_23      -0.0395325000
_diffrn_orient_matrix_UB_31      -0.0548489000
_diffrn_orient_matrix_UB_32      -0.0166972000
_diffrn_orient_matrix_UB_33      0.0618262000
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29664
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.477
_diffrn_reflns_theta_max         67.476
_diffrn_reflns_theta_min         5.984
_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    14.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22040
_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    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.033
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5278
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0579
_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^)+(0.1303P)^2^+15.7228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1793
_refine_ls_wR_factor_ref         0.1800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5138
_reflns_number_total             5278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01864a2.cif
_cod_data_source_block           cx-fn-i-rm-20190630
_cod_depositor_comments
'Adding full bibliography for 1575758--1575760.cif.'
_cod_database_code               1575758
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C56H44Cu2I2O2P4
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.386
_reflns_odcompleteness_completeness 98.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C28(H28), C8(H8), C3(H3), C12(H12), C2(H2), C18(H18), C9(H9),
 C4(H4), C10(H10), C11(H11), C20(H20), C6(H6), C16(H16), C24(H24), C25(H25),
 C26(H26), C22(H22), C19(H19), C21(H21), C5(H5), C27(H27)
;
_shelx_res_checksum              96736
_shelx_hkl_checksum              86463
_shelx_fab_checksum              28309
_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 2.832
_oxdiff_exptl_absorpt_empirical_full_min 0.644