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_1575759
_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 Br3 Cu3 O2 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C58 H48 Br3 Cl4 Cu3 O2 P4'
_chemical_formula_weight         1472.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 111.4798(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.87931(5)
_cell_length_b                   25.12831(8)
_cell_length_c                   18.02014(7)
_cell_measurement_reflns_used    96324
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.9850
_cell_measurement_theta_min      3.1180
_cell_volume                     5848.27(4)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(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 0.995
_diffrn_measured_fraction_theta_max 0.987
_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  38.00   0.50    0.50    --    5.00 -57.00   0.00  244
  2  \w    -28.00  94.00   0.50    0.50    --    5.00  57.00-150.00  244
  3  \w   -136.00  -9.00   0.50    0.50    --  -46.90 -76.00 -90.00  254
  4  \w    -85.00  42.00   0.50    0.50    --  -46.90  76.00  90.00  254
  5  \w    -84.00  42.00   0.50    0.50    --  -46.90  38.00  30.00  252
  6  \w   -192.00 -65.00   0.50    0.50    -- -102.20 -72.00-100.07  254
  7  \w   -192.00 -64.00   0.50    0.50    -- -102.20 -76.00  60.00  256
  8  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00 -30.00  256
  9  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00  90.00  256
 10  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00-180.00  256
 11  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00-150.00  256
 12  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00 -90.00  256
 13  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00   0.00  256
 14  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00 150.00  256
 15  \w   -192.00 -69.00   0.50    0.50    -- -102.20 -50.00 -76.51  246
 16  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00-120.00  256
 17  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00  60.00  256
 18  \w   -192.00 -64.00   0.50    0.50    -- -102.20 -76.00 -13.61  256
 19  \w   -192.00 -64.00   0.50    0.50    -- -102.20 -76.00  10.52  256
 20  \w   -141.00 -13.00   0.50    0.50    -- -102.20  76.00  30.00  256
 21  \w   -192.00 -66.00   0.50    0.50    -- -102.20 -70.00 -76.20  252
 22  \w   -136.00  -9.00   0.50    0.50    --  -46.90 -76.00  30.00  254
 23  \w   -136.00 -14.00   0.50    0.50    --  -46.90 -57.00 150.00  244
 24  \w   -136.00  -9.00   0.50    0.50    --  -46.90 -76.00   0.00  254
 25  \w   -136.00 -95.00   0.50    0.50    --  -46.90 -76.00 150.00   82
 26  \w   -136.00  -9.00   0.50    0.50    --  -46.90 -76.00 120.00  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      -0.0287718000
_diffrn_orient_matrix_UB_12      -0.0160553000
_diffrn_orient_matrix_UB_13      0.0717506000
_diffrn_orient_matrix_UB_21      -0.0877457000
_diffrn_orient_matrix_UB_22      0.0415078000
_diffrn_orient_matrix_UB_23      -0.0247522000
_diffrn_orient_matrix_UB_31      -0.0755599000
_diffrn_orient_matrix_UB_32      -0.0421543000
_diffrn_orient_matrix_UB_33      -0.0517724000
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            128394
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.107
_diffrn_reflns_theta_min         3.168
_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    6.713
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68336
_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    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.077
_refine_diff_density_min         -1.550
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11744
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0970P)^2^+14.5276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11333
_reflns_number_total             11744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01864a2.cif
_cod_data_source_block           cx-fn-br-200k-190924
_cod_depositor_comments
'Adding full bibliography for 1575758--1575760.cif.'
_cod_database_code               1575759
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'H C O P Cu Br'
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.689
_reflns_odcompleteness_completeness 98.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-C57 \\sim Cl2-C57 \\sim Cl3-C58 \\sim Cl4-C58
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl3 \\sim C58: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Cl1 \\sim Cl2 \\sim C57: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
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
4.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C58(H58A,H58B)
4.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C13(H13), C16(H16),
 C41(H41), C6(H6), C2(H2), C36(H36), C40(H40), C22(H22), C44(H44), C50(H50),
 C34(H34), C46(H46), C3(H3), C5(H5), C8(H8), C30(H30), C39(H39), C38(H38),
 C37(H37), C21(H21), C12(H12), C28(H28), C18(H18), C49(H49), C4(H4), C48(H48),
 C47(H47), C20(H20), C33(H33), C31(H31), C32(H32), C24(H24), C19(H19), C11(H11),
  C10(H10), C27(H27), C26(H26), C9(H9), C25(H25)
4.c Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56)
;
_shelx_res_checksum              94421
_shelx_hkl_checksum              21941
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.778