Dispersion, solvent and metal effects in the binding of gold cations to alkynyl ligands: implications for Au(I) catalysis
Luisa Ciano; Natalie Fey; Connor J. V. Halliday; Jason M. Lynam; Lucy M. Milner; Nimesh Mistry; Natalie E. Pridmore; Nell S. Townsend; Adrian C. Whitwood; Chem.Commun. 51 (2015) 9702–; doi:10.1039/C5cc02629F

data_7117238
_publ_section_title
;
 Dispersion, solvent and metal effects in the binding of gold cations to
 alkynyl ligands: implications for Au(I) catalysis
;
_journal_name_full               Chem.Commun.
_journal_page_first              9702
_journal_paper_doi               10.1039/C5cc02629F
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C51 H47 Au2 N P, F6 Sb, 1(C7 H8)'
_chemical_formula_sum            'C58.01 H55.02 Au2 F6 N P Sb'
_chemical_formula_weight         1426.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-11-04 deposited with the CCDC.
2015-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.291(3)
_cell_length_b                   17.933(2)
_cell_length_c                   24.334(3)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    150
_cell_measurement_theta_max      66.79
_cell_measurement_theta_min      3.06
_cell_volume                     10600(2)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_laue_measured_fraction_full 0.977
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            167357
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.881
_diffrn_reflns_theta_min         3.063
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.988
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0984 before and 0.0702 after correction. The Ratio of minimum to maximum transmission is 0.7348. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             5504.8
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         9391
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.295
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0293P)^2^+72.8034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                9156
_reflns_number_total             9391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02629f2.cif
_cod_data_source_block           '[5]SbF6.C6H5Ch3'
_cod_database_code               7117238
_shelxl_version_number           2013-4
_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
 C30-C31 = C30-C32 = C30-C33
 1.53 with sigma of 0.02
 C30-C31A = C30-C32A = C30-C33A
 1.53 with sigma of 0.02
 C52-C58
 1.49 with sigma of 0.02
 C52A-C58A
 1.49 with sigma of 0.02
 C52B-C58B
 1.49 with sigma of 0.02
 F2-F3 = F3-F4 = F4-F5 = F5-F2
 2.22 with sigma of 0.04
 F1-F2 = F1-F3 = F1-F4 = F1-F5
 2.22 with sigma of 0.04
 F2A-F3A = F3A-F4A = F4A-F5A = F5A-F2A
 2.22 with sigma of 0.04
 F1A-F2A = F1A-F3A = F1A-F4A = F1A-F5A
 2.22 with sigma of 0.04
 F6A-F2A = F6A-F3A = F6A-F4A = F6A-F5A
 2.22 with sigma of 0.04
 F6-F2 = F6-F3 = F6-F4 = F6-F5
 2.22 with sigma of 0.04
 C31-C32 = C32-C33 = C33-C31
 2.5 with sigma of 0.04
 C31A-C32A = C32A-C33A = C33A-C31A
 2.5 with sigma of 0.04
 C58-C53
 2.5 with sigma of 0.005
 C58-C57
 2.5 with sigma of 0.005
 C58A-C53A
 2.5 with sigma of 0.005
 C58A-C57A
 2.5 with sigma of 0.005
 C58B-C53B
 2.5 with sigma of 0.005
 C58B-C57B
 2.5 with sigma of 0.005
 Sb1-F1 \\sim Sb1A-F1A \\sim Sb1-F2 \\sim Sb1A-F2A \\sim Sb1-F3 \\sim Sb1A-F3A
\\sim Sb1-F4 \\sim Sb1A-F4A
 \\sim Sb1-F5 \\sim Sb1A-F5A \\sim Sb1-F6 \\sim Sb1A-F6A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C52A) \\sim Ueq, Uanis(C53A) \\sim Ueq, Uanis(C54A) \\sim Ueq,
Uanis(C55A) \\sim Ueq, Uanis(C56A) \\sim Ueq, Uanis(C57A) \\sim Ueq,
Uanis(C58A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C52B) \\sim Ueq, Uanis(C53B) \\sim Ueq, Uanis(C54B) \\sim Ueq,
Uanis(C55B) \\sim Ueq, Uanis(C56B) \\sim Ueq, Uanis(C57B) \\sim Ueq,
Uanis(C58B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Sb1) = Uanis(Sb1A)
Uanis(C31) = Uanis(C32A)
Uanis(C32) = Uanis(C33A)
Uanis(F2) = Uanis(F4A)
Uanis(F4) = Uanis(F2A)
Uanis(F1) = Uanis(F6A)
Uanis(F3) = Uanis(F5A)
Uanis(F5) = Uanis(F3A)
Uanis(F6) = Uanis(F1A)
Uanis(C33) = Uanis(C31A)
4. Others
 1*[Sof(C52)+Sof(C57)+Sof(H57)+Sof(C56)+Sof(H56)+Sof(C55)+Sof(H55)+Sof(C54)+
 Sof(H54)+Sof(C53)+Sof(H53)+Sof(C58)+Sof(H58A)+Sof(H58B)+Sof(H58C)]+1*
 [Sof(C52A)+Sof(C57A)+Sof(H57A)+Sof(C56A)+Sof(H56A)+Sof(C55A)+Sof(H55A)+
 Sof(C54A)+Sof(H54A)+Sof(C53A)+Sof(H53A)+Sof(C58A)+Sof(H58G)+Sof(H58H)+
 Sof(H58I)]+1*[Sof(C52B)+Sof(C53B)+Sof(H53B)+Sof(C54B)+Sof(H54B)+Sof(C55B)+
 Sof(H55B)+Sof(C56B)+Sof(H56B)+Sof(C57B)+Sof(H57B)+Sof(C58B)+Sof(H58D)+
 Sof(H58E)+Sof(H58F)]=1 with esd of 0.005
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=
 Sof(H32F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(1)
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(Sb1A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(Sb1)=FVAR(2)
 Sof(C52)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56)=Sof(C55)=Sof(H55)=Sof(C54)=
 Sof(H54)=Sof(C53)=Sof(H53)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=FVAR(3)
 Sof(C52A)=Sof(C57A)=Sof(H57A)=Sof(C56A)=Sof(H56A)=Sof(C55A)=Sof(H55A)=
 Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(H53A)=Sof(C58A)=Sof(H58G)=Sof(H58H)=
 Sof(H58I)=FVAR(4)
 Sof(C52B)=Sof(C53B)=Sof(H53B)=Sof(C54B)=Sof(H54B)=Sof(C55B)=Sof(H55B)=
 Sof(C56B)=Sof(H56B)=Sof(C57B)=Sof(H57B)=Sof(C58B)=Sof(H58D)=Sof(H58E)=
 Sof(H58F)=FVAR(5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C24(H24), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C57(H57), C56(H56),
  C55(H55), C54(H54), C53(H53), C53B(H53B), C54B(H54B), C55B(H55B), C56B(H56B),
 C57B(H57B), C57A(H57A), C56A(H56A), C55A(H55A), C54A(H54A), C53A(H53A)
5.b Fitted hexagon refined as free rotating group:
 C52(C57,C56,C55,C54,C53), C52B(C53B,C54B,C55B,C56B,C57B), C52A(C57A,C56A,C55A,
 C54A,C53A)
5.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F),
 C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F), C58(H58A,H58B,H58C), C58B(H58D,H58E,
 H58F), C58A(H58G,H58H,H58I)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'