Insights into mechanisms of diphosphine-mediated controlled surface construction on Au nanoclusters
Li, Qinzhen; Yang, Sha; Chai, Jinsong; Zhang, Hui; Zhu, Manzhou; Nanoscale  (2022) –; doi:10.1039/D2NR05291A

data_1567799
_publ_section_title
;
 Insights into mechanisms of diphosphine-mediated controlled surface
 construction on Au nanoclusters
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D2NR05291A
_journal_year                    2022
_chemical_formula_moiety         'C148 H220 Au25 P4 S16, 2(C12 H10 B0.5)'
_chemical_formula_sum            'C172 H240 Au25 B P4 S16'
_chemical_formula_weight         7879.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.254(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.7888(10)
_cell_length_b                   17.4433(4)
_cell_length_c                   31.9121(9)
_cell_measurement_reflns_used    20412
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.10
_cell_measurement_theta_min      6.19
_cell_volume                     21461.1(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.1037
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            44862
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.654
_diffrn_reflns_theta_min         6.197
_exptl_absorpt_coefficient_mu    33.236
_exptl_crystal_density_diffrn    2.439
_exptl_crystal_description       block
_exptl_crystal_F_000             14272
_refine_diff_density_max         2.304
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         19420
_refine_ls_number_restraints     707
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11782
_reflns_number_total             19420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05291a2.cif
_cod_data_source_block           1_sq_s
_cod_original_cell_volume        21461.1(10)
_cod_database_code               1567799
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C46-B40 = C6AA-B40
 1.7 with sigma of 0.01
3. Restrained planarity
 B40, C46, C3AA, C34
 with sigma of 0.1
 B40, C6AA, C9AA, C7AA
 with sigma of 0.1
4. Rigid bond restraints
 B40, C103, C4AA, C2AA, C34, C3AA, C46, C6AA, C274, C5, C9AA, C7AA, C8AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
P00N \\sim C013 \\sim C014 \\sim C016 \\sim C01A \\sim C01B \\sim C01H \\sim
C11 \\sim C18 \\sim C26 \\sim C27 \\sim C35 \\sim C38 \\sim C0AA \\sim C44
\\sim C63 \\sim C012 \\sim C00S \\sim P00M \\sim C011 \\sim C01I \\sim C01S
\\sim C01Y \\sim C23 \\sim C9 \\sim C1AA \\sim C41 \\sim C60: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C00O) \\sim Ueq, Uanis(C00R) \\sim Ueq, Uanis(C00S) \\sim Ueq,
Uanis(C00T) \\sim Ueq, Uanis(C00U) \\sim Ueq, Uanis(C00V) \\sim Ueq,
Uanis(C00W) \\sim Ueq, Uanis(C00Y) \\sim Ueq, Uanis(C00Z) \\sim Ueq,
Uanis(C011) \\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(C013) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C014) \\sim Ueq, Uanis(C015) \\sim Ueq,
Uanis(C016) \\sim Ueq, Uanis(C017) \\sim Ueq, Uanis(C018) \\sim Ueq,
Uanis(C019) \\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C01C) \\sim Ueq,
Uanis(C01D) \\sim Ueq, Uanis(C01E) \\sim Ueq, Uanis(C01F) \\sim Ueq,
Uanis(C01G) \\sim Ueq, Uanis(C01H) \\sim Ueq, Uanis(C01I) \\sim Ueq,
Uanis(C01J) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C01L) \\sim Ueq,
Uanis(C01M) \\sim Ueq, Uanis(C01N) \\sim Ueq, Uanis(C01O) \\sim Ueq,
Uanis(C01P) \\sim Ueq, Uanis(C01Q) \\sim Ueq, Uanis(C01R) \\sim Ueq,
Uanis(C01S) \\sim Ueq, Uanis(C01T) \\sim Ueq, Uanis(C01U) \\sim Ueq,
Uanis(C01V) \\sim Ueq, Uanis(C01X) \\sim Ueq, Uanis(C01Y) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C0AA) \\sim Ueq,
Uanis(C1AA) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C3AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq,
Uanis(C274) \\sim Ueq, Uanis(C9AA) \\sim Ueq, Uanis(C8AA) \\sim Ueq,
Uanis(C7AA) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(B40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: B40(0.5)
7.a Ternary CH refined with riding coordinates:
 C00O(H00O), C00R(H00R), C00T(H00T), C00U(H00U), C00W(H00W), C017(H017),
 C01G(H01Q), C1(H1)
7.b Secondary CH2 refined with riding coordinates:
 C00V(H00B,H00A), C00Y(H00D,H00C), C00Z(H00E,H00F), C015(H01A,H01C), C018(H01D,
 H01E), C019(H01F,H01G), C01C(H01I,H01J), C01D(H01K,H01L), C01E(H01N,H01M),
 C01F(H01O,H01P), C01J(H01S,H01T), C01K(H01V,H01U), C01L(H01X,H01W), C01M(H,
 H01Y), C01N(H01Z,HA), C01O(HB,H01), C01P(H0AA,HC), C01Q(HD,H1AA), C01R(HE,
 H2AA), C01T(H4AA,HF), C01U(HG,H5AA), C01V(HH,H6AA), C01X(H7AA,HI), C2(H2A,H2B),
  C4(H4B,H4A), C7(H7A,H7B), C8(H8B,H8A), C10(H10B,H10A), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C19(H19B,H19A), C20(H20B,H20A),
  C21(H21A,H21B), C25(H25A,H25B), C28(H28B,H28A), C30(H30A,H30B), C33(H33B,
 H33A), C37(H37A,H37B)
7.c Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C012(H012), C013(H013), C01B(H01B), C38(H38), C63(H63), C44(H44),
 C016(H016), C01A(H01H), C01H(H01R), C01S(H3AA), C01Y(H8AA), C11(H11), C23(H23),
  C26(H26), C27(H27), C35(H35), C9(H9), C0AA(H0AB), C1AA(H1AB), C41(H41),
 C60(H60), C103(H103), C4AA(H4AB), C34(H34), C3AA(H3AB), C2AA(H2AB), C274(H274),
  C9AA(H9AA), C8AA(H8AB), C7AA(H7AB), C5(H5)
7.d Fitted hexagon refined as free rotating group:
 C013(C01B,C38,C63,C44,C18), C103(C4AA,C34,C46,C3AA,C2AA), C6AA(C274,C9AA,C8AA,
 C7AA,C5)
;
_shelx_res_checksum              49048
_shelx_fab_checksum              34004
_olex2_submission_special_instructions 'No special instructions were received'