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_4519391
_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         'C66 H90 Au N P, F6 Sb'
_chemical_formula_sum            'C66 H90 Au F6 N P Sb'
_chemical_formula_weight         1361.07
_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     iterative
_audit_creation_date             2021-11-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                95.2651(17)
_cell_angle_beta                 103.1408(17)
_cell_angle_gamma                117.9130(18)
_cell_formula_units_Z            2
_cell_length_a                   15.3509(9)
_cell_length_b                   15.4730(9)
_cell_length_c                   19.0096(10)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.33
_cell_volume                     3781.0(4)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0946
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            124627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.745
_diffrn_reflns_theta_min         1.993
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.363
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1308 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.7887.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       prysm
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.471
_refine_diff_density_min         -2.140
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         16058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0350P)^2^+5.4926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12771
_reflns_number_total             16058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c05823_si_010.cif
_cod_data_source_block           jcm03621_sq
_cod_database_code               4519391
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=
 Sof(H16F)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C14A)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 N1(H1), C64(H64), C61(H61)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C31(H31), C22(H22), C32(H32), C42(H42), C8(H8), C4(H4), C12(H12),
 C11(H11), C49(H49), C9(H9), C52(H52), C48(H48), C51(H51), C5(H5), C45(H45),
 C44(H44), C28(H28), C24(H24), C25(H25), C29(H29)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C18(H18A,H18B,H18C), C60(H60A,H60B,H60C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C19(H19A,H19B,H19C), C65(H65A,H65B,H65C), C62(H62A,
 H62B,H62C), C66(H66A,H66B,H66C), C38(H38A,H38B,H38C), C63(H63A,H63B,H63C),
 C59(H59A,H59B,H59C), C58(H58A,H58B,H58C), C56(H56A,H56B,H56C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C36A(H36A,H36B,H36C), C34A(H34A,H34B,H34C),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C34B(H34D,H34E,H34F), C36B(H36D,
 H36E,H36F), C16A(H16A,H16B,H16C), C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C),
 C15B(H15D,H15E,H15F), C16B(H16D,H16E,H16F), C14B(H14D,H14E,H14F)
;
_shelx_res_checksum              69861
_shelx_hkl_checksum              57582
_shelx_fab_checksum              26327
_olex2_submission_special_instructions 'No special instructions were received'