Pd-Promoted cross coupling of iodobenzene with vinylgold via an unprecedented phenyl transmetalation from Pd to Au.
Wang, Jiwei; Zhan, Licheng; Wang, Gendi; Wei, Yin; Shi, Min; Zhang, Jun; Chemical communications (Cambridge, England) 56 (2020) 6213–6216; doi:10.1039/d0cc02645j

data_7126406
_publ_section_title
;
 Pd-Promoted cross coupling of iodobenzene with vinylgold via an
 unprecedented phenyl transmetalation from Pd to Au.
;
_journal_issue                   46
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6213
_journal_page_last               6216
_journal_paper_doi               10.1039/d0cc02645j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C63 H78 Au N5 Pd, 2(B F4)'
_chemical_formula_sum            'C63 H78 Au B2 F8 N5 Pd'
_chemical_formula_weight         1382.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-06-26 deposited with the CCDC.	2020-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.7160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3922(2)
_cell_length_b                   14.4465(2)
_cell_length_c                   16.7191(2)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.883
_cell_measurement_theta_min      2.840
_cell_volume                     3349.50(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36285
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        52.980
_diffrn_reflns_theta_max         52.980
_diffrn_reflns_theta_min         2.839
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.657
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1513 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.6961. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.343
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6170
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0347P)^2^+12.5930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5599
_reflns_number_total             6170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02645j2.cif
_cod_data_source_block           wmj18009_0m
_cod_depositor_comments
'Adding full bibliography for 7126403--7126408.cif.'
_cod_database_code               7126406
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F4-B2 = F5_$1-B2 = F5-B2 = F6-B2
 1.34 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim B1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
F4 \\sim F5 \\sim F5 \\sim F6 \\sim B2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H40A(0.5) H40B(0.5) H40C(0.5)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C22(H22), C33(H33), C36(H36)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C13(H13), C14(H14), C20(H20),
 C21(H21), C26(H26), C29(H29), C30(H30), C31(H31)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              40365
_shelx_hkl_checksum              86620
_shelx_fab_checksum              95602
_olex2_submission_special_instructions 'No special instructions were received'