Stepwise assembly of thiacalix[4]arene-protected Ag/Ti bimetallic nanoclusters: accurate identification of catalytic Ag sites in CO<sub>2</sub> electroreduction.
Tian, Yi-Qi; Mu, Wen-Lei; Wu, Lin-Lin; Yi, Xiao-Yi; Yan, Jun; Liu, Chao; Chemical science 14 (2023) 10212–10218; doi:10.1039/d3sc02793g

data_1569794
_publ_section_title
;
 Stepwise assembly of thiacalix[4]arene-protected Ag/Ti bimetallic
 nanoclusters: accurate identification of catalytic Ag sites in
 CO<sub>2</sub> electroreduction.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              10212
_journal_page_last               10218
_journal_paper_doi               10.1039/d3sc02793g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_sum            'C441 H508 Ag16 N26 Na2 O109 S32 Ti16'
_chemical_formula_weight         11480.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-05-13 deposited with the CCDC.	2023-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.2730(15)
_cell_length_b                   44.470(3)
_cell_length_c                   38.489(3)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      48.18
_cell_measurement_theta_min      3.27
_cell_volume                     38123(5)
_computing_cell_refinement       'SAINT V8.40C (?, 2016)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'SAINT V8.40C (?, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER D8 VENTURE PHOTON II'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            392236
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        48.408
_diffrn_reflns_theta_max         48.408
_diffrn_reflns_theta_min         1.996
_exptl_absorpt_coefficient_mu    3.827
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       block
_exptl_crystal_F_000             11692
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.856
_exptl_transmission_factor_min   0.756
_refine_diff_density_max         1.772
_refine_diff_density_min         -2.088
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.500(14)
_refine_ls_extinction_coef       0.00101(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4126
_refine_ls_number_reflns         55921
_refine_ls_number_restraints     11107
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0891
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+220.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2265
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                49717
_reflns_number_total             55921
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc02793g2.cif
_cod_data_source_block           Ti8Ag8
_cod_depositor_comments
'Adding full bibliography for 1569790--1569794.cif.'
_cod_database_code               1569794
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.701
_shelx_estimated_absorpt_t_max   0.701
_shelx_res_checksum              78836
_shelx_fab_checksum              62987