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_1567800
_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         'C118 H182 Au22 Fe P2 S14, 2(C H2 Cl2)'
_chemical_formula_sum            'C120 H186 Au22 Cl4 Fe P2 S14'
_chemical_formula_weight         6670.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2022-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                80.682(2)
_cell_angle_beta                 82.909(2)
_cell_angle_gamma                63.942(2)
_cell_formula_units_Z            2
_cell_length_a                   15.8416(5)
_cell_length_b                   17.5548(5)
_cell_length_c                   29.6424(8)
_cell_measurement_reflns_used    38738
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      3.88
_cell_volume                     7295.0(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.1039
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            49548
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        64.998
_diffrn_reflns_theta_max         64.998
_diffrn_reflns_theta_min         3.883
_exptl_absorpt_coefficient_mu    44.222
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_description       block
_exptl_crystal_F_000             5984
_refine_diff_density_max         3.015
_refine_diff_density_min         -2.666
_refine_diff_density_rms         0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1486
_refine_ls_number_reflns         23672
_refine_ls_number_restraints     849
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1018
_refine_ls_R_factor_gt           0.0679
_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^)+(0.1149P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15230
_reflns_number_total             23672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05291a2.cif
_cod_data_source_block           Au22-DPPF
_cod_database_code               1567800
_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, All C(H,H,H,H) groups
2. Restrained distances
 C1CA-C0CA
 1.55 with sigma of 0.01
 C5-C0CA = C1CA-C0CA = C83-C1CA = C9BA-C83 = C9BA-C8BA = C8BA-C5
 1.55 with sigma of 0.01
 C7BA-C0CA = C8BA-C7BA
 1.55 with sigma of 0.01
 C2CA-C01O = C82-C2CA
 1.55 with sigma of 0.01
 C2CA-C74
 2.9 with sigma of 0.01
 C11-C19
 2.9 with sigma of 0.01
 C6CA-C11 = C6CA-C1 = C19-C1
 1.55 with sigma of 0.01
 C27-C11
 1.55 with sigma of 0.01
 C267-C19 = C27-C267
 1.55 with sigma of 0.01
 C267-C6CA
 2.9 with sigma of 0.01
 C6CA-C27
 2.5 with sigma of 0.01
 C6CA-C19
 2.5 with sigma of 0.01
 C9BA-C7BA
 2.5 with sigma of 0.01
 C1CA-C7BA
 2.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C0CA \\sim C1CA \\sim C8BA \\sim C9BA \\sim C83 \\sim C5 \\sim C7BA: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C018) \\sim Ueq, Uanis(C01A) \\sim Ueq, Uanis(C01B) \\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(C01W) \\sim Ueq,
Uanis(C01X) \\sim Ueq, Uanis(C01Y) \\sim Ueq, Uanis(C01Z) \\sim Ueq,
Uanis(C020) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C022) \\sim Ueq,
Uanis(C025) \\sim Ueq, Uanis(C026) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C028) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C02A) \\sim Ueq,
Uanis(C02C) \\sim Ueq, Uanis(C02D) \\sim Ueq, Uanis(C02E) \\sim Ueq,
Uanis(C02G) \\sim Ueq, Uanis(C02J) \\sim Ueq, Uanis(C02K) \\sim Ueq,
Uanis(C02L) \\sim Ueq, Uanis(C02M) \\sim Ueq, Uanis(C02N) \\sim Ueq,
Uanis(C02Q) \\sim Ueq, Uanis(C02R) \\sim Ueq, Uanis(C02U) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C68)
\\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C98) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C1AA) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C74) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C6AA)
\\sim Ueq, Uanis(C5AA) \\sim Ueq, Uanis(C7AA) \\sim Ueq, Uanis(C0BA) \\sim Ueq,
Uanis(C9AA) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C4AA)
\\sim Ueq, Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C61) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C8AA) \\sim Ueq, Uanis(C1BA) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C5BA) \\sim Ueq, Uanis(C6BA) \\sim Ueq, Uanis(C2BA) \\sim Ueq,
Uanis(C0CA) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C4BA) \\sim Ueq,
Uanis(C1CA) \\sim Ueq, Uanis(C8BA) \\sim Ueq, Uanis(C9BA) \\sim Ueq,
Uanis(C4CA) \\sim Ueq, Uanis(C3CA) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C2CA)
\\sim Ueq, Uanis(C5CA) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C7BA) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C6CA) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C267) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S010
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 S010, C11, C19, C1, C6CA, C27, C267
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: S013(0.6) H0CA(0.6) H0CB(0.6) H0CC(0.4) H0CD(0.4) H8BA(0.6)
 H8BB(0.6) H8BC(0.4) H8BD(0.4) S1(0.4) C5(0.6) H5(0.6) C7BA(0.4) H7BA(0.4)
6.a Ternary CH refined with riding coordinates:
 C01B(H01B), C01C(H01C), C01I(H01K), C01M(H01P), C01O(H01Q), C01P(H01R),
 C01W(H01Y), C022(H022), C029(H029), C45(H45), C66(H66), C7AA(H7AA), C5(H5),
 C7BA(H7BA), C11(H11)
6.b Secondary CH2 refined with riding coordinates:
 C01D(H01D,H01E), C01E(H01F,H01G), C01J(H01L,H01M), C01U(H01W,H01X), C01X(H01Z,
 H), C020(H02A,H02B), C021(H02C,H02D), C025(H02E,H02F), C027(H02G,H02H),
 C02A(H02I,H02J), C02C(H02K,H02L), C02D(H02M,H02N), C02E(H02O,H02P), C02J(H02Q,
 H02R), C02M(H02U,H02V), C02Q(H02W,H02X), C49(H49A,H49B), C50(H50A,H50B),
 C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B), C67(H67A,H67B), C68(H68A,H68B),
  C71(H71A,H71B), C84(H84A,H84B), C90(H90A,H90B), C94(H94A,H94B), C98(H98A,
 H98B), C47(H47A,H47B), C48(H48A,H48B), C1AA(H1AA,H1AB), C57(H57A,H57B),
 C63(H63A,H63B), C0AA(H0AB,H0AC), C74(H74A,H74B), C78(H78A,H78B), C79(H79A,
 H79B), C82(H82A,H82B), C6AA(H6AA,H6AB), C5AA(H5AA,H5AB), C0BA(H0BA,H0BB),
 C9AA(H9AA,H9AB), C54(H54A,H54B), C55(H55A,H55B), C4AA(H4AA,H4AB), C2AA(H2AA,
 H2AB), C3AA(H3AA,H3AB), C61(H61A,H61B), C62(H62A,H62B), C8AA(H8AA,H8AB),
 C1BA(H1BA,H1BB), C46(H46A,H46B), C5BA(H5BA,H5BB), C6BA(H6BA,H6BB), C2BA(H2BA,
 H2BB), C0CA(H0CA,H0CB), C0CA(H0CC,H0CD), C3BA(H3BA,H3BB), C4BA(H4BA,H4BB),
 C1CA(H1CA,H1CB), C8BA(H8BA,H8BB), C8BA(H8BC,H8BD), C9BA(H9BA,H9BB), C4CA(H4CA,
 H4CB), C3CA(H3CA,H3CB), C77(H77A,H77B), C2CA(H2CA,H2CB), C5CA(H5CA,H5CB),
 C83(H83A,H83B), C19(H19A,H19B), C1(H1A,H1B), C6CA(H6CA,H6CB), C27(H27A,H27B),
 C267(H26A,H26B)
6.c Aromatic/amide H refined with riding coordinates:
 C01A(H01A), C01F(H01H), C01G(H01I), C01H(H01J), C01K(H01N), C01L(H01O),
 C01Q(H01S), C01R(H01T), C01S(H01U), C01T(H01V), C01Y(H01), C01Z(H0AA),
 C026(H026), C028(H028), C02K(H02S), C02L(H02T), C02R(H02Y), C02U(H02Z),
 C42(H42), C51(H51), C58(H58), C59(H59), C64(H64), C69(H69), C70(H70), C72(H72),
  C75(H75), C96(H96)
;
_shelx_res_checksum              66315
_shelx_fab_checksum              8577
_olex2_submission_special_instructions 'No special instructions were received'