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_7131299
_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         'C44 H38 Cu7 F6 N8 O4 S10, 4(C3 H6 O)'
_chemical_formula_sum            'C56 H62 Cu7 F6 N8 O8 S10'
_chemical_formula_weight         1854.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-22
_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                 91.1760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.63270(10)
_cell_length_b                   19.2788(3)
_cell_length_c                   18.8668(2)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.0850
_cell_measurement_theta_min      4.5900
_cell_volume                     3502.96(8)
_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      200.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     30.00  56.00   0.50    0.50    --    0.00  82.00-180.00   52
  2  \w     18.00  89.00   0.50    0.50    --    0.00  57.00 -30.00  142
  3  \w     19.00  87.00   0.50    0.50    --    0.00  38.00 -90.00  136
  4  \w    148.00 175.00   0.50    4.00    --   95.20  30.00 120.00   54
  5  \w     86.00 185.00   0.50    4.00    --   95.20  45.00 150.00  198
  6  \w      6.00  74.00   0.50    4.00    --   95.20 -61.00-120.00  136
  7  \w      7.00 124.00   0.50    4.00    --   95.20 -82.00-120.00  234
  8  \w     23.00  69.00   0.50    4.00    --   95.20 -30.00   0.00   92
  9  \w     90.00 115.00   0.50    4.00    --   95.20 -30.00   0.00   50
 10  \w     80.00 118.00   0.50    4.00    --   95.20 -61.00-120.00   76
 11  \w     10.00  36.00   0.50    4.00    --   95.20 -30.00 -90.00   52
 12  \w     74.00 100.00   0.50    4.00    --   95.20 -30.00 -90.00   52
 13  \w    140.00 177.00   0.50    4.00    --   95.20  30.00-180.00   74
 14  \w     76.00 131.00   0.50    4.00    --   95.20  45.00-180.00  110
 15  \w     87.00 145.00   0.50    4.00    --   95.20  30.00 120.00  116
;
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20888
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.039
_diffrn_reflns_theta_min         3.278
_exptl_absorpt_coefficient_mu    5.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88468
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1870
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.138
_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     452
_refine_ls_number_reflns         6930
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1138P)^2^+4.4999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5297
_reflns_number_total             6930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00275f2.cif
_cod_data_source_block           hy_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7131298--7131299.cif.'
_cod_database_code               7131299
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 F1-C22
 1.39 with sigma of 0.02
 O1-C21
 1.43 with sigma of 0.01
 O2-C21
 1.43 with sigma of 0.01
 Cu4-O1
 2.2 with sigma of 0.1
 C22-C21
 1.5 with sigma of 0.01
 F4-C22
 1.39 with sigma of 0.01
 F4-C22 = C22-F1
 1.39 with sigma of 0.02
 F7-C22 = C22-F5
 1.39 with sigma of 0.02
 F11-C22
 1.39 with sigma of 0.01
 F11-C21
 2 with sigma of 0.01
 F7-C22 = C22-F1
 1.39 with sigma of 0.02
 F4-F1
 1.39 with sigma of 0.04
 F7-F5
 1.39 with sigma of 0.04
 F7-F1
 1.39 with sigma of 0.04
3. Rigid bond restraints
 O1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F19, F11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F7 \\sim F1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
F1 \\sim F4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F11) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(F7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C21) = Uanis(C22)
Uanis(C15) = Uanis(C22) = Uanis(C21)
5. Others
 Fixed Sof: F1(0.5) F4(0.5) F5(0.5) F19(0.5) F7(0.5) F11(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C2(H2), C7(H7), C13(H13), C15(H15), C10(H10), C8(H8), C9(H9),
 C12(H12)
6.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C20(H20A,H20B,
 H20C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28702
_shelx_hkl_checksum              6295
_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
;