Assembly of copper-clusters into a framework: enhancing the structural stability and photocatalytic HER performance.
Xu, Yue; Dong, Qing-Guo; Dong, Jian-Peng; Zhang, Huan; Li, Bo; Wang, Rui; Zang, Shuang-Quan; Chemical communications (Cambridge, England) 59 (2023) 3067–3070; doi:10.1039/d3cc00275f

data_7131298
_publ_section_title
;
 Assembly of copper-clusters into a framework: enhancing the structural
 stability and photocatalytic HER performance.
;
_journal_issue                   21
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3067
_journal_page_last               3070
_journal_paper_doi               10.1039/d3cc00275f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C48 H56 Cu8 N8 S12'
_chemical_formula_sum            'C48 H56 Cu8 N8 S12'
_chemical_formula_weight         1638.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-22 deposited with the CCDC.	2023-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1385(2)
_cell_length_b                   19.1450(5)
_cell_length_c                   15.7602(3)
_cell_measurement_reflns_used    4214
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      72.7040
_cell_measurement_theta_min      5.6280
_cell_volume                     3059.08(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      199.99(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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     40.00  83.00   0.50    0.50    --    0.00  82.00  30.00   86
  2  \w    -20.00  57.00   0.50    0.50    --    0.00  57.00   0.00  154
  3  \w     76.00 185.00   0.50    3.00    --   95.80  30.00 -30.00  218
  4  \w     12.00  44.00   0.50    3.00    --   95.80 -30.00-180.00   64
  5  \w     54.00  88.00   0.50    3.00    --   95.80 -30.00-180.00   68
  6  \w    112.00 167.00   0.50    3.00    --   95.80  30.00-180.00  110
  7  \w     27.00 109.00   0.50    3.00    --   95.80 -61.00 -60.00  164
  8  \w     80.00 111.00   0.50    3.00    --   95.80 -45.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10734
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.383
_diffrn_reflns_theta_min         3.633
_exptl_absorpt_coefficient_mu    7.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1595 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5537
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.4931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.616
_reflns_Friedel_fraction_full    0.836
_reflns_Friedel_fraction_max     0.770
_reflns_number_gt                4788
_reflns_number_total             5537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00275f2.cif
_cod_data_source_block           hy
_cod_depositor_comments
'Adding full bibliography for 7131298--7131299.cif.'
_cod_database_code               7131298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.223
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C5, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C11 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C21(H21), C27(H27), C4(H4), C25(H25), C26(H26), C7(H7), C3(H3),
 C1(H1), C2(H2)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C15(H15A,H15B,
 H15C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C14(H14A,
 H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              90920
_shelx_hkl_checksum              6978
_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
;