An atomically precise Au<sub>10</sub>(DPPF)<sub>4</sub>PPh<sub>3</sub> cluster catalyst for N-hydroformylation of amines.
Li, Guangjun; Li, Guoao; Liang, Xinyi; Tian, Yiqi; Lu, Jinzhi; Xu, Xinyi; Liu, Xu; Ma, Jing; Li, Shuhua; Zhu, Yan; Chemical science 16 (2025) 18642–18651; doi:10.1039/d5sc06255a

data_1575732
_publ_section_title
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 An atomically precise Au<sub>10</sub>(DPPF)<sub>4</sub>PPh<sub>3</sub>
 cluster catalyst for N-hydroformylation of amines.
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_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              18642
_journal_page_last               18651
_journal_paper_doi               10.1039/d5sc06255a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C154 H127 Au10 Fe4 P9, C H2 Cl2, Cl, 7[CH2Cl2]'
_chemical_formula_sum            'C162 H143 Au10 Cl17 Fe4 P9'
_chemical_formula_weight         5164.20
_chemical_name_systematic        Au10(DPPF)4PPh3
_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     iterative
_audit_creation_date             2025-04-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.172(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8219(15)
_cell_length_b                   31.443(3)
_cell_length_c                   33.812(3)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.29
_cell_volume                     17703(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            121626
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.825
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.951
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3463
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1690 before and 0.0857 after correction.
The Ratio of minimum to maximum transmission is 0.4645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       plate
_exptl_crystal_F_000             9732
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.989
_refine_diff_density_min         -1.539
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1606
_refine_ls_number_reflns         36085
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0470P)^2^+233.9905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24800
_reflns_number_total             36085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06255a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1575732.cif.'
_cod_database_code               1575732
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C051 \\sim C02E \\sim C42 \\sim C37: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
Uanis(C42) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(C051) \\sim Ueq, Uanis(C02E) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C0AA(H0Aa,H0Ab)
3.b Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00X(H00X), C00Y(H00Y), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01I(H01I), C01M(H01M), C01P(H01P), C01Q(H01Q), C01S(H01S), C01T(H01T),
 C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C022(H022), C023(H023),
 C024(H024), C025(H025), C026(H026), C027(H027), C028(H028), C029(H029),
 C02A(H02A), C02C(H02C), C02D(H02D), C03S(H03S), C26(H26), C051(H051), C42(H42),
  C37(H37), C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02J), C02L(H02L),
 C02M(H02M), C02N(H02N), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02Y(H02Y), C02Z(H02Z),
 C030(H030), C031(H031), C033(H033), C034(H034), C035(H035), C037(H037),
 C038(H038), C039(H039), C03A(H03A), C03B(H03B), C03C(H03C), C03D(H03D),
 C03E(H03E), C03F(H03F), C03G(H03G), C03H(H03H), C03I(H03I), C03K(H03K),
 C03L(H03L), C03M(H03M), C03N(H03N), C03O(H03O), C03Q(H03Q), C03R(H03R),
 C03T(H03T), C03U(H03U), C03V(H03V), C03W(H03W), C03X(H03X), C03Y(H03Y),
 C040(H040), C041(H041), C042(H042), C043(H043), C044(H044), C045(H045),
 C046(H046), C047(H047), C048(H048), C049(H049), C04A(H04A), C04B(H04B),
 C04C(H04C), C04D(H04D), C04E(H04E), C04F(H04F), C04G(H04G), C04H(H04H),
 C04J(H04J), C04L(H04L), C04M(H04M), C04N(H04N), C04O(H04O), C04Q(H04Q),
 C04R(H04R), C04T(H04T), C04U(H04U), C04V(H04V), C04W(H04W), C04X(H04X),
 C04Y(H04Y), C050(H050), C052(H052), C053(H053), C054(H054), C16(H16), C19(H19),
  C41(H41), C33(H33), C032(H032), C04I(H04I), C23(H23)
3.c Fitted hexagon refined as free rotating group:
 C02E(C03S,C26,C051,C42,C37), C41(C33,C032,C03J,C04I,C23)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 1142 electrons were 
found in a volume of 6036\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
7[CH2Cl2] per Asymmetric Unit 
which account for 1176 electrons 
per unit cell.
;
_shelx_res_checksum              35005
_shelx_fab_checksum              27896
_olex2_submission_special_instructions 'No special instructions were received'