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_4519384
_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         'C31 H49 Au P, F6 Sb'
_chemical_formula_sum            'C31 H49 Au F6 P Sb'
_chemical_formula_weight         885.39
_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     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                86.489(3)
_cell_angle_beta                 89.678(3)
_cell_angle_gamma                77.831(3)
_cell_formula_units_Z            4
_cell_length_a                   8.7636(7)
_cell_length_b                   13.6876(12)
_cell_length_c                   28.412(2)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.754
_cell_measurement_theta_min      2.377
_cell_volume                     3325.2(5)
_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 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  0.1226
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            95123
_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         26.000
_diffrn_reflns_theta_min         2.030
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.320
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1722 before and 0.0934 after correction.
The Ratio of minimum to maximum transmission is 0.5864.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       prysm
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.576
_refine_diff_density_min         -2.644
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         13023
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0247P)^2^+58.1331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10098
_reflns_number_total             13023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c05823_si_003.cif
_cod_data_source_block           jcm04221a_0m
_cod_original_cell_volume        3325.1(5)
_cod_database_code               4519384
_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
 C62, C63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Au1, C30, C31
 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 C30 \\sim C31: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C19(H19), C45(H45), C48(H48), C51(H51)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C62(H62A,H62B), C63(H63A,H63B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C43(H43)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
;
_shelx_res_checksum              36459
_shelx_hkl_checksum              65592
_olex2_submission_special_instructions 'No special instructions were received'