Dicoordinate Au(I)–Ethylene Complexes as Hydroamination Catalysts
Navarro, Miquel; Alférez, Macarena G.; de Sousa, Morgane; Miranda-Pizarro, Juan; Campos, Jesús; ACS Catalysis 12 (2022) 4227–4241; doi:10.1021/acscatal.1c05823

data_4519387
_publ_section_title
;
 Dicoordinate Au(I)--Ethylene Complexes as Hydroamination Catalysts
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              4227
_journal_page_last               4241
_journal_paper_doi               10.1021/acscatal.1c05823
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C48 H71 Au P, F6 Sb, 2(C H2 Cl2), C3 H7'
_chemical_formula_sum            'C53 H82 Au Cl4 F6 P Sb'
_chemical_formula_weight         1324.67
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2021-12-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.079(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.253(3)
_cell_length_b                   13.3849(11)
_cell_length_c                   26.020(2)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.058
_cell_measurement_theta_min      2.247
_cell_volume                     11564.5(17)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0988
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            100015
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.938
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.266
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1519 before and 0.0948 after correction.
The Ratio of minimum to maximum transmission is 0.5830.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       prysm
_exptl_crystal_F_000             5336
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.185
_refine_diff_density_min         -2.479
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         11354
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0691P)^2^+161.8453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9089
_reflns_number_total             11354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c05823_si_004.cif
_cod_data_source_block           jcm04321a_0m
_cod_database_code               4519387
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Au1, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C51, C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Au1 \\sim C47 \\sim C48: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
C27 \\sim C30: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C51 \\sim C52 \\sim C53: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C17A, C18A, C19A, C20A, C17B, C18B, C19B, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C17B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C35(H35), C41(H41)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,
 H40B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
  C51(H51A,H51B), C52(H52A,H52B)
6.c Me refined with riding coordinates:
 C53(H53A,H53B,H53C)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C22(H22), C24(H24),
 C26(H26)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C),
 C20A(H20A,H20B,H20C), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F), C20B(H20D,
 H20E,H20F)
;
_shelx_res_checksum              41895
_shelx_hkl_checksum              16679
_olex2_submission_special_instructions 'No special instructions were received'