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_1567801
_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         '2(C62 H88 Au10.5 P2 S6), C24 H20 B'
_chemical_formula_sum            'C148 H196 Au21 B P4 S12'
_chemical_formula_weight         6630.74
_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             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                69.4100(10)
_cell_angle_beta                 83.6220(10)
_cell_angle_gamma                74.5830(10)
_cell_formula_units_Z            2
_cell_length_a                   17.4996(2)
_cell_length_b                   21.3266(3)
_cell_length_c                   26.0965(4)
_cell_measurement_reflns_used    63025
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.31
_cell_measurement_theta_min      3.87
_cell_volume                     8787.5(2)
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49686
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        62.499
_diffrn_reflns_theta_max         62.499
_diffrn_reflns_theta_min         4.569
_exptl_absorpt_coefficient_mu    33.992
_exptl_crystal_density_diffrn    2.506
_exptl_crystal_description       block
_exptl_crystal_F_000             6000
_refine_diff_density_max         4.416
_refine_diff_density_min         -4.853
_refine_diff_density_rms         0.473
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1666
_refine_ls_number_reflns         26740
_refine_ls_number_restraints     1195
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+211.1135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23214
_reflns_number_total             26740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05291a2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               1567801
_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
 C108-C101
 1.55 with sigma of 0.01
 C108-C7AA
 1.55 with sigma of 0.01
 C7AA-C188
 1.55 with sigma of 0.01
 C188-C6AA
 1.55 with sigma of 0.01
 C6AA-C41
 1.55 with sigma of 0.01
 C101-C7AA
 2.5 with sigma of 0.01
 C101-C6AA
 2.5 with sigma of 0.01
 C41-C188
 2.5 with sigma of 0.01
 C108-C188
 2.5 with sigma of 0.01
 C6AA-C7AA
 2.5 with sigma of 0.01
 C101-C188
 2.93 with sigma of 0.01
 C7AA-C41
 2.93 with sigma of 0.01
 C108-C6AA
 2.93 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C04G \\sim C66 \\sim C72 \\sim C99 \\sim C90 \\sim C5AA: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C01Q \\sim C01Y \\sim C43 \\sim C27 \\sim C38 \\sim C01C: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C01X \\sim C03X \\sim C03J \\sim C02T \\sim C01T \\sim C03E: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C038 \\sim C01U \\sim C01A \\sim C03G \\sim C02F \\sim C04S: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C04N \\sim C32 \\sim C54 \\sim C04L \\sim C039 \\sim C04A: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C02W \\sim C02M: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
C04Z \\sim C02J \\sim C80 \\sim C103 \\sim C84 \\sim C75: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C043 \\sim C02S \\sim C35 \\sim C04P \\sim C04U \\sim C2AA: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C101 \\sim C41 \\sim C6AA \\sim C188 \\sim C7AA \\sim C108: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C01A) \\sim Ueq, Uanis(C01C) \\sim Ueq, Uanis(C01E) \\sim Ueq,
Uanis(C01H) \\sim Ueq, Uanis(C01K) \\sim Ueq, Uanis(C01L) \\sim Ueq,
Uanis(C01N) \\sim Ueq, Uanis(C01O) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C01R) \\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(C023) \\sim Ueq, Uanis(C024) \\sim Ueq, Uanis(C025) \\sim Ueq,
Uanis(C026) \\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(C02F) \\sim Ueq, Uanis(C02G) \\sim Ueq,
Uanis(C02H) \\sim Ueq, Uanis(C02I) \\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(C02S) \\sim Ueq, Uanis(C02T) \\sim Ueq, Uanis(C02U) \\sim Ueq,
Uanis(C02W) \\sim Ueq, Uanis(C02Y) \\sim Ueq, Uanis(C030) \\sim Ueq,
Uanis(C031) \\sim Ueq, Uanis(C032) \\sim Ueq, Uanis(C035) \\sim Ueq,
Uanis(C037) \\sim Ueq, Uanis(C038) \\sim Ueq, Uanis(C039) \\sim Ueq,
Uanis(C03A) \\sim Ueq, Uanis(C03B) \\sim Ueq, Uanis(C03D) \\sim Ueq,
Uanis(C03E) \\sim Ueq, Uanis(C03F) \\sim Ueq, Uanis(C03G) \\sim Ueq,
Uanis(C03H) \\sim Ueq, Uanis(C03I) \\sim Ueq, Uanis(C03J) \\sim Ueq,
Uanis(C03K) \\sim Ueq, Uanis(C03L) \\sim Ueq, Uanis(C03M) \\sim Ueq,
Uanis(C03P) \\sim Ueq, Uanis(C03R) \\sim Ueq, Uanis(C03T) \\sim Ueq,
Uanis(C03U) \\sim Ueq, Uanis(C03V) \\sim Ueq, Uanis(C03W) \\sim Ueq,
Uanis(C03X) \\sim Ueq, Uanis(C042) \\sim Ueq, Uanis(C043) \\sim Ueq,
Uanis(C046) \\sim Ueq, Uanis(C047) \\sim Ueq, Uanis(C04A) \\sim Ueq,
Uanis(C04C) \\sim Ueq, Uanis(C04D) \\sim Ueq, Uanis(C04G) \\sim Ueq,
Uanis(C04H) \\sim Ueq, Uanis(C04I) \\sim Ueq, Uanis(C04J) \\sim Ueq,
Uanis(C04L) \\sim Ueq, Uanis(C04M) \\sim Ueq, Uanis(C04N) \\sim Ueq,
Uanis(C04O) \\sim Ueq, Uanis(C04P) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C04Q)
\\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C053) \\sim Ueq, Uanis(C04S) \\sim Ueq, Uanis(C04U) \\sim Ueq,
Uanis(C04V) \\sim Ueq, Uanis(C04Z) \\sim Ueq, Uanis(C052) \\sim Ueq, Uanis(C36)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C65) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq,
Uanis(C99) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C54) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C0AA)
\\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C1AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq, Uanis(C5AA) \\sim Ueq, Uanis(C75)
\\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(C84) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C108) \\sim Ueq, Uanis(C111) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C6AA) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C7AA)
\\sim Ueq, Uanis(C188) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C01A(H01A), C01E(H01E), C01N(H01O), C01Q(H01Q), C025(H025), C029(H029),
 C02E(H02U), C02Q(H3AA), C02S(H4AA), C02Y(H02Y), C031(H031), C101(H101)
4.b Secondary CH2 refined with riding coordinates:
 C01C(H01B,H01C), C01K(H01K,H01L), C01L(H01M,H01N), C01R(H01P,H01R), C01U(H01D,
 H01F), C01V(H01G,H01H), C01Y(H01I,H01J), C020(H02A,H02B), C023(H02C,H02D),
 C024(H02N,H02O), C026(H02P,H02Q), C02C(H02R,H02S), C02F(H02E,H02F), C02G(H02V,
 H02X), C02I(H02G,H02H), C02K(H02I,H02J), C02L(H2AA,H), C02R(H02K,H02L),
 C030(H03O,H03P), C032(H03A,H03B), C037(H03Q,H03R), C038(H03C,H03D), C03A(H03E,
 H03F), C03B(H03S,H03T), C03F(H03H,H03I), C03G(H03J,H03K), C03I(H03L,H03M),
 C03L(H03W,H03Y), C03R(H5AA,HA), C042(H04G,H04H), C043(H04I,H04J), C046(H04K,
 H04M), C047(H04A,H04B), C04C(H04C,H04D), C04D(H04P,H04R), C04P(H04V,H04W),
 C04S(H04E,H04F), C04U(H04X,H04Y), C04V(H04Z,HB), C27(H27A,H27B), C29(H29A,
 H29B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C2AA(H2AB,H2AC),
 C38(H38A,H38B), C42(H42A,H42B), C43(H43A,H43B), C51(H51A,H51B), C53(H53A,H53B),
  C3AA(H3AB,H3AC), C67(H67A,H67B), C79(H79A,H79B), C92(H92A,H92B), C108(H10A,
 H10B), C1(H1A,H1B), C6AA(H6AA,H6AB), C41(H41A,H41B), C7AA(H7AA,H7AB),
 C188(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C01T(H01T), C01W(H01W), C01Z(H01Z), C028(H028), C02H(H02Z), C02J(H02),
 C02M(H02M), C02T(H02T), C02U(H0BA), C02W(H02W), C039(H039), C03D(H1BA),
 C03E(H03G), C03H(H03U), C03J(H03N), C03K(H03V), C03M(H03Z), C03P(H03),
 C03T(H8AA), C03U(H2BA), C03V(H3BA), C03W(H9AA), C03X(H03X), C04H(H04S),
 C04I(H04T), C04J(H04U), C04L(H04L), C04M(H04), C04N(H04N), C04O(H04O),
 C04Q(H04Q), C88(H88), C86(H86), C104(H104), C053(H053), C052(H052), C36(H36),
 C61(H61), C62(H62), C65(H65), C66(H66), C71(H71), C72(H72), C74(H74), C83(H83),
  C90(H90), C91(H91), C99(H99), C32(H32), C46(H46), C54(H54), C0AA(H0AA),
 C69(H69), C70(H70), C1AA(H1AA), C4AA(H4AB), C5AA(H5AB), C75(H75), C77(H77),
 C80(H80), C84(H84), C94(H94), C103(H103), C111(H111)
4.d Fitted hexagon refined as free rotating group:
 C37(C04Q,C88,C86,C104,C053)
;
_shelx_res_checksum              2784
_shelx_fab_checksum              10988
_olex2_submission_special_instructions 'No special instructions were received'