The Gilded Edge in Acetylenic Scaffolding: Pd-Catalyzed Cross-Coupling Reactions of Phosphine-Gold(I) Oligoynyl Complexes.
Mazzanti, Virginia; Jiang, Huixin; Gotfredsen, Henrik; Morsing, Thorbjørn J; Parker, Christian R.; Nielsen, Mogens Brøndsted; Organic letters 16 (2014) 3736–; doi:10.1021/ol5015587

data_1517022
_publ_section_title
;
 The Gilded Edge in Acetylenic Scaffolding: Pd-Catalyzed Cross-Coupling
 Reactions of Phosphine-Gold(I) Oligoynyl Complexes.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3736
_journal_paper_doi               10.1021/ol5015587
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C32 H36 Au P Si, 2(C3 H3)'
_chemical_formula_sum            'C38 H42 Au P Si'
_chemical_formula_weight         754.78
_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'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date             2014-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.278(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9774(15)
_cell_length_b                   25.2649(15)
_cell_length_c                   11.2161(6)
_cell_measurement_reflns_used    9766
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.55
_cell_volume                     6762.1(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            115500
_diffrn_reflns_theta_full        26.3714
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.458
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0994 before and 0.0685 after correction.
The Ratio of minimum to maximum transmission is 0.7529.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.4827
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3024.0
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.6385
_refine_diff_density_min         -1.1245
_refine_diff_density_rms         0.1622
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             8.6740
_refine_ls_goodness_of_fit_ref   1.0753
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0751
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+12.2719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              29
_reflns_limit_h_min              -32
_reflns_limit_k_max              31
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5824
_reflns_number_total             6907
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ol5015587_si_002.cif
_cod_data_source_block           mo_D8V512_0m-1
_cod_depositor_comments
'Adding full bibliography for 1517022--1517023.cif.'
_cod_database_code               1517022
_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
 C35-C34 = C36-C35 = C36-C34_$1
 1.395 with sigma of 0.005
3.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C31(H31)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39)
3.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C29(H29a,H29b,H29c), C30(H30a,H30b,
 H30c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c)
;