Cuprous Cluster-Based Coordination Sheets as Photocatalytic Regulators to Activate Oxygen, Benzoquinone, and Thianthrenium Salts.
Huang, Huilin; Jing, Xu; Zhong, Bingwen; Meng, Changgong; Duan, Chunying; ACS applied materials & interfaces 13 (2021) 58498–58507; doi:10.1021/acsami.1c16280

data_4519206
_publ_section_title
;
 Cuprous Cluster-Based Coordination Sheets as Photocatalytic Regulators to
 Activate Oxygen, Benzoquinone, and Thianthrenium Salts.
;
_journal_issue                   49
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              58498
_journal_page_last               58507
_journal_paper_doi               10.1021/acsami.1c16280
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety
'C48 H60 Cu4 I4 N20 S6, 1.5(C8 H6), 4.5(O), 3(C1.5 H3 N0.5)'
_chemical_formula_sum            'C61.5 H58.5 Cu4 I4 N18.5 O7.5 S6'
_chemical_formula_weight         2130.88
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   20.5000(3)
_cell_length_b                   20.5000(3)
_cell_length_c                   87.071(3)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.43
_cell_volume                     31689.2(13)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       115
_diffrn_reflns_limit_l_min       -115
_diffrn_reflns_number            138960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.087
_diffrn_reflns_theta_min         2.342
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6123
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.8211.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_F_000             12492
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.492
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         8593
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1082P)^2^+416.6472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6765
_reflns_number_total             8593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am1c16280_si_003.cif
_cod_data_source_block           1_b
_cod_original_cell_volume        31689.2(14)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C61.50 H58.50 Cu4 I4 N18.50 O7.50 S6'
_cod_database_code               4519206
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C19
 1.2 with sigma of 0.02
 C19-C10
 1.3 with sigma of 0.02
 C19-C22
 2.3 with sigma of 0.02
3. Restrained planarity
 C7, C10, C19, C23, C22, C28, C11, C9
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7 \\sim C19 \\sim C10 \\sim C23 \\sim C22 \\sim C28 \\sim C11 \\sim C9: within
2.8A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2.8A
Uanis(N1) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N9) \\sim
Ueq, Uanis(N10) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(N12) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1#) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4#) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Fixed Sof: C7(0.5) H7A(0.5) C10(0.5) C23(0.5) H23(0.5) C28(0.5) H28(0.5)
 C9(0.5) H9(0.5) C11(0.5) H11A(0.5) C22(0.5) H22(0.5) C19(0.5) C21(0.5) N3(0.5)
6.a Riding coordinates:
 N7(H7), N8(H8), N9(H9A,H9B,H9C), N10(H10), N11(H11), N12(H12A,H12B,H12C)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4#(H4#), C5(H5), C12(H12), C13(H13), C14(H14), C16(H16),
 C18(H18), C20(H20), C23(H23), C28(H28), C9(H9), C11(H11A), C22(H22)
6.c Fitted hexagon refined as free rotating group:
 C10(C23,C28,C9,C11,C22)
6.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
6.e :
 C7(H7A)
;
_shelx_res_checksum              7848
_shelx_hkl_checksum              55434
_olex2_submission_special_instructions 'No special instructions were received'