Ligand-controlled exposure of active sites on the Pd<sub>1</sub>Ag<sub>14</sub> nanocluster surface to boost electrocatalytic CO<sub>2</sub> reduction.
Ma, Along; Ren, Yonggang; Zuo, Yang; Wang, Jiawei; Huang, Shutong; Ma, Xiaoshuang; Wang, Shuxin; Chemical communications (Cambridge, England) 60 (2024) 3162–3165; doi:10.1039/d4cc00152d

data_7132732
_publ_section_title
;
 Ligand-controlled exposure of active sites on the
 Pd<sub>1</sub>Ag<sub>14</sub> nanocluster surface to boost
 electrocatalytic CO<sub>2</sub> reduction.
;
_journal_issue                   23
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3162
_journal_page_last               3165
_journal_paper_doi               10.1039/d4cc00152d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C192 H138 Ag14 F36 P8 Pd S6, 2(C H2 Cl2)'
_chemical_formula_sum            'C194 H142 Ag14 Cl4 F36 P8 Pd S6'
_chemical_formula_weight         5355.57
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-10 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.07(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.460(9)
_cell_length_b                   36.131(11)
_cell_length_c                   18.471(6)
_cell_measurement_reflns_used    9430
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.242
_cell_measurement_theta_min      2.276
_cell_volume                     10945(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62648
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.058
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.541
_exptl_absorpt_correction_T_max  0.1378
_exptl_absorpt_correction_T_min  0.0816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0647 after correction.
The Ratio of minimum to maximum transmission is 0.5922.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             5236
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         19235
_refine_ls_number_restraints     1082
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0931
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+194.1753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1956
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13403
_reflns_number_total             19235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00152d2.cif
_cod_data_source_block           wsx0428a_0m
_cod_depositor_comments
'Adding full bibliography for 7132732--7132733.cif.'
_cod_database_code               7132732
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.887
_olex2_refinement_description
;
1. Others
 Fixed Sof: Pd7(0.5)
 Fixed Uiso: H86(0.082) H28(0.079) H34(0.09) H14(0.07) H9(0.068) H39(0.074)
 H88(0.072) H91(0.068) H21(0.057) H35(0.065) H105(0.086) H54(0.083) H4(0.055)
 H3(0.077) H10(0.078) H23(0.08) H2(0.064) H19(0.074) H8(0.08) H61(0.081)
 H78(0.106) H27(0.101) H7(0.07) H6(0.061) H68(0.093) H69(0.098) H70(0.103)
 H11(0.089) H41(0.077) H49(0.102) H31(0.056) H42(0.072) H29(0.078) H60(0.069)
 H25(0.061) H26(0.061) H22(0.076) H17(0.069) H30(0.059) H15(0.048) H45(0.071)
 H64(0.076) H71(0.088) H33(0.081) H18(0.061) H38(0.13) H37(0.113) H57(0.135)
 H50(0.14) H40(0.133) H46(0.135) H52(0.149) H44(0.118) H43(0.141) H58(0.146)
 H55(0.121) H51(0.147) H56(0.146) H59(0.138) H63(0.147) H65(0.095) H72(0.128)
 H66(0.1) H76(0.067) H74(0.057) H79(0.062) H89(0.084) H92(0.064) H85(0.097)
 H95A(0.199) H95B(0.199)
 Fixed X: Pd7(0.5) H86(0.029401) H28(-0.051203) H34(-0.026914) H14(0.077978)
 H9(0.134296) H39(0.048838) H88(0.132331) H91(0.244411) H21(0.273)
 H35(0.077427) H105(0.059244) H54(0.069047) H4(0.31019) H3(0.300388)
 H10(0.174916) H23(0.806716) H2(0.753739) H19(0.85453) H8(0.931414)
 H61(0.907508) H78(0.927758) H27(0.889076) H7(0.768221) H6(0.686048)
 H68(0.845582) H69(0.588753) H70(0.630253) H11(0.677899) H41(0.642546)
 H49(0.5949) H31(0.266963) H42(0.166378) H29(0.203663) H60(0.341532)
 H25(0.442118) H26(0.490674) H22(0.61232) H17(0.727926) H30(0.721887)
 H15(0.600242) H45(0.466325) H64(0.437814) H71(0.366488) H33(0.323672)
 H18(0.352182) H38(0.927513) H37(0.800128) H57(0.721497) H50(0.848881)
 H40(0.95189) H46(0.454807) H52(0.474461) H44(0.556037) H43(0.598307)
 H58(0.516731) H55(0.553668) H51(0.785112) H56(0.80334) H59(0.696733)
 H63(0.571897) H65(0.443646) H72(0.287643) H66(0.349831) H76(0.830787)
 H74(0.585487) H79(0.723749) H89(0.65594) H92(0.759727) H85(0.901324)
 H95A(0.192638) H95B(0.141459)
 Fixed Y: Pd7(0.5) H86(0.425271) H28(0.474245) H34(0.534493) H14(0.545769)
 H9(0.436547) H39(0.585077) H88(0.636268) H91(0.630486) H21(0.573512)
 H35(0.528102) H105(0.41667) H54(0.457547) H4(0.470878) H3(0.430001)
 H10(0.402897) H23(0.617149) H2(0.525081) H19(0.492396) H8(0.522087)
 H61(0.584464) H78(0.663124) H27(0.653767) H7(0.622139) H6(0.599868)
 H68(0.640852) H69(0.716342) H70(0.726098) H11(0.676457) H41(0.607303)
 H49(0.656944) H31(0.554733) H42(0.527311) H29(0.48827) H60(0.476652)
 H25(0.504075) H26(0.585875) H22(0.588662) H17(0.557114) H30(0.522779)
 H15(0.519991) H45(0.606228) H64(0.669373) H71(0.700588) H33(0.668658)
 H18(0.605513) H38(0.375393) H37(0.36215) H57(0.323483) H50(0.336725)
 H40(0.36268) H46(0.289975) H52(0.352565) H44(0.369494) H43(0.261243)
 H58(0.244313) H55(0.292621) H51(0.281356) H56(0.229896) H59(0.209799)
 H63(0.241161) H65(0.346188) H72(0.272232) H66(0.365106) H76(0.448673)
 H74(0.438261) H79(0.44974) H89(0.303888) H92(0.389766) H85(0.307963)
 H95A(0.61423) H95B(0.594444)
 Fixed Z: Pd7(0.5) H86(0.286224) H28(0.218241) H34(0.267287) H14(0.384316)
 H9(0.403256) H39(0.596113) H88(0.600249) H91(0.559029) H21(0.513673)
 H35(0.550756) H105(0.604879) H54(0.510184) H4(0.628754) H3(0.72345)
 H10(0.711513) H23(0.826646) H2(0.693271) H19(0.788842) H8(0.903315)
 H61(0.922218) H78(0.644951) H27(0.511843) H7(0.446037) H6(0.513337)
 H68(0.712253) H69(0.80015) H70(0.693916) H11(0.639872) H41(0.798295)
 H49(0.85234) H31(0.687308) H42(0.726762) H29(0.834361) H60(0.902508)
 H25(0.863056) H26(0.887115) H22(0.992564) H17(0.988773) H30(0.879533)
 H15(0.774083) H45(0.637468) H64(0.615925) H71(0.683947) H33(0.773512)
 H18(0.795055) H38(0.866751) H37(0.774571) H57(0.942846) H50(1.035027)
 H40(0.996981) H46(0.939275) H52(0.918181) H44(0.846123) H43(0.816251)
 H58(0.888309) H55(0.644516) H51(0.793321) H56(0.724039) H59(0.614995)
 H63(0.575232) H65(0.572397) H72(0.611419) H66(0.741564) H76(0.874988)
 H74(0.812697) H79(1.038031) H89(0.498574) H92(0.639182) H85(0.603039)
 H95A(0.749665) H95B(0.795767)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12517
_shelx_hkl_checksum              14256
_shelx_fab_checksum              63882
_olex2_submission_special_instructions 'No special instructions were received'