#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:52:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178795 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/49/4104938.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4104938
loop_
_publ_author_name
'Haifeng Duan'
'Sujata Sengupta'
'Jeffrey L. Petersen'
'Novruz G. Akhmedov'
'Xiaodong Shi'
_publ_section_title
;
 Triazole-Au(I) Complexes: A New Class of Catalysts with Improved Thermal
 Stability and Reactivity for Intermolecular Alkyne Hydroamination
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12100
_journal_page_last               12102
_journal_paper_doi               10.1021/ja9041093
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C28 H27 Au F3 N3 O3 P S'
_chemical_formula_weight         770.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.107(1)
_cell_angle_beta                 104.804(1)
_cell_angle_gamma                100.656(1)
_cell_formula_units_Z            2
_cell_length_a                   9.2800(6)
_cell_length_b                   13.2256(8)
_cell_length_c                   14.1159(9)
_cell_measurement_reflns_used    8471
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.37
_cell_volume                     1500.24(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10340
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    5.078
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0586P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                5822
_reflns_number_total             6574
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9041093_si_004.cif
_cod_data_source_block           ms62plt
_cod_database_code               4104938
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Au1 Au 0.146229(18) 0.336889(10) 0.074408(12) 0.05943(8) Uani 1 1 d .
P1 P 0.26317(12) 0.52077(8) 0.17923(9) 0.0506(2) Uani 1 1 d .
S1 S 0.83788(14) 0.23684(9) 0.25857(10) 0.0657(3) Uani 1 1 d .
F1 F 0.9855(6) 0.2222(4) 0.4358(4) 0.1255(15) Uani 1 1 d .
F2 F 0.7626(6) 0.2468(5) 0.4258(4) 0.1255(15) Uani 1 1 d .
F3 F 0.9570(6) 0.3837(4) 0.4562(4) 0.1314(17) Uani 1 1 d .
O1 O 0.7687(5) 0.1167(3) 0.2116(4) 0.0907(12) Uani 1 1 d .
O2 O 0.7328(6) 0.2990(4) 0.2393(4) 0.0982(13) Uani 1 1 d .
O3 O 0.9868(6) 0.2699(4) 0.2469(4) 0.1014(13) Uani 1 1 d .
N1 N 0.0488(4) 0.1677(3) -0.0264(3) 0.0581(8) Uani 1 1 d .
N2 N 0.1411(5) 0.1142(3) -0.0636(3) 0.0656(9) Uani 1 1 d .
N3 N 0.0562(5) 0.0084(3) -0.1273(3) 0.0635(8) Uani 1 1 d .
H3N H 0.0923 -0.0428 -0.1607 0.076 Uiso 1 1 calc R
C1 C -0.1010(5) 0.0951(3) -0.0675(3) 0.0574(9) Uani 1 1 d .
C2 C -0.2413(6) 0.1118(5) -0.0531(5) 0.0757(12) Uani 1 1 d .
H2 H -0.2467 0.1816 -0.0106 0.091 Uiso 1 1 calc R
C3 C -0.3687(7) 0.0177(5) -0.1065(5) 0.0873(15) Uani 1 1 d .
H3 H -0.4638 0.0231 -0.0985 0.105 Uiso 1 1 calc R
C4 C -0.3612(6) -0.0874(5) -0.1733(6) 0.0903(17) Uani 1 1 d .
H4 H -0.4525 -0.1478 -0.2084 0.108 Uiso 1 1 calc R
C5 C -0.2291(6) -0.1049(4) -0.1890(4) 0.0776(13) Uani 1 1 d .
H5 H -0.2257 -0.1746 -0.2331 0.093 Uiso 1 1 calc R
C6 C -0.0961(5) -0.0088(3) -0.1329(3) 0.0596(9) Uani 1 1 d .
C7 C 0.1266(5) 0.5956(3) 0.2160(3) 0.0532(8) Uani 1 1 d .
C8 C 0.0245(6) 0.5502(4) 0.2578(4) 0.0698(11) Uani 1 1 d .
H8 H 0.0225 0.4814 0.2619 0.084 Uiso 1 1 calc R
C9 C -0.0739(6) 0.6080(6) 0.2930(5) 0.0894(16) Uani 1 1 d .
H9 H -0.1412 0.5775 0.3217 0.107 Uiso 1 1 calc R
C10 C -0.0754(7) 0.7073(7) 0.2873(5) 0.0928(18) Uani 1 1 d .
H10 H -0.1428 0.7450 0.3117 0.111 Uiso 1 1 calc R
C11 C 0.0250(9) 0.7525(6) 0.2444(6) 0.0962(18) Uani 1 1 d .
H11 H 0.0241 0.8207 0.2392 0.115 Uiso 1 1 calc R
C12 C 0.1268(6) 0.6971(4) 0.2092(4) 0.0730(12) Uani 1 1 d .
H12 H 0.1947 0.7282 0.1812 0.088 Uiso 1 1 calc R
C13 C 0.4102(5) 0.5495(3) 0.3055(3) 0.0523(8) Uani 1 1 d .
C14 C 0.4338(6) 0.6437(4) 0.3989(4) 0.0681(11) Uani 1 1 d .
H14 H 0.3691 0.6896 0.3985 0.082 Uiso 1 1 calc R
C15 C 0.5554(7) 0.6676(5) 0.4924(4) 0.0828(14) Uani 1 1 d .
H15 H 0.5733 0.7309 0.5544 0.099 Uiso 1 1 calc R
C16 C 0.6488(6) 0.5992(6) 0.4944(5) 0.0816(14) Uani 1 1 d .
H16 H 0.7295 0.6163 0.5576 0.098 Uiso 1 1 calc R
C17 C 0.6244(6) 0.5058(5) 0.4042(5) 0.0783(14) Uani 1 1 d .
H17 H 0.6882 0.4595 0.4066 0.094 Uiso 1 1 calc R
C18 C 0.5056(6) 0.4796(4) 0.3094(4) 0.0654(10) Uani 1 1 d .
H18 H 0.4892 0.4156 0.2484 0.078 Uiso 1 1 calc R
C19 C 0.3608(5) 0.5908(3) 0.1126(3) 0.0525(8) Uani 1 1 d .
C20 C 0.4948(6) 0.6812(5) 0.1703(4) 0.0776(13) Uani 1 1 d .
H20 H 0.5390 0.7049 0.2442 0.093 Uiso 1 1 calc R
C21 C 0.5650(7) 0.7383(5) 0.1176(5) 0.0836(14) Uani 1 1 d .
H21 H 0.6549 0.7996 0.1567 0.100 Uiso 1 1 calc R
C22 C 0.4998(6) 0.7026(4) 0.0091(4) 0.0687(11) Uani 1 1 d .
H22 H 0.5456 0.7397 -0.0261 0.082 Uiso 1 1 calc R
C23 C 0.3664(7) 0.6118(5) -0.0489(4) 0.0772(12) Uani 1 1 d .
H23 H 0.3221 0.5885 -0.1228 0.093 Uiso 1 1 calc R
C24 C 0.2977(6) 0.5549(4) 0.0027(4) 0.0682(10) Uani 1 1 d .
H24 H 0.2091 0.4927 -0.0370 0.082 Uiso 1 1 calc R
C25 C 0.8858(7) 0.2723(5) 0.4010(5) 0.0834(14) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 Au1 P1 176.52(10)
C13 P1 C19 106.15(18)
C13 P1 C7 105.28(18)
C19 P1 C7 106.56(18)
C13 P1 Au1 114.13(12)
C19 P1 Au1 111.45(14)
C7 P1 Au1 112.69(14)
O2 S1 O1 115.0(3)
O2 S1 O3 117.1(3)
O1 S1 O3 112.7(2)
O2 S1 C25 102.8(3)
O1 S1 C25 102.7(3)
O3 S1 C25 104.1(3)
N2 N1 C1 109.8(3)
N2 N1 Au1 117.2(3)
C1 N1 Au1 133.0(3)
N1 N2 N3 107.7(4)
N2 N3 C6 111.3(3)
N1 C1 C6 106.6(4)
N1 C1 C2 131.7(4)
C6 C1 C2 121.7(4)
C3 C2 C1 114.9(5)
C2 C3 C4 122.4(5)
C5 C4 C3 123.6(5)
C4 C5 C6 114.5(5)
N3 C6 C1 104.6(4)
N3 C6 C5 132.6(4)
C1 C6 C5 122.8(5)
C12 C7 C8 119.5(4)
C12 C7 P1 122.7(3)
C8 C7 P1 117.6(3)
C9 C8 C7 119.5(5)
C10 C9 C8 122.0(5)
C9 C10 C11 118.9(5)
C12 C11 C10 120.6(5)
C7 C12 C11 119.5(5)
C18 C13 C14 119.3(4)
C18 C13 P1 119.9(3)
C14 C13 P1 120.7(3)
C15 C14 C13 119.0(4)
C16 C15 C14 120.9(5)
C17 C16 C15 120.4(5)
C16 C17 C18 120.5(4)
C17 C18 C13 119.8(5)
C20 C19 C24 119.4(4)
C20 C19 P1 121.1(3)
C24 C19 P1 119.4(3)
C19 C20 C21 120.3(5)
C22 C21 C20 119.4(5)
C21 C22 C23 120.3(4)
C22 C23 C24 120.3(5)
C19 C24 C23 120.1(4)
F2 C25 F1 108.5(5)
F2 C25 F3 108.3(5)
F1 C25 F3 106.0(5)
F2 C25 S1 112.2(5)
F1 C25 S1 112.3(4)
F3 C25 S1 109.3(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au1 N1 2.063(3)
Au1 P1 2.2384(10)
P1 C13 1.812(4)
P1 C19 1.813(4)
P1 C7 1.817(4)
S1 O2 1.421(4)
S1 O1 1.435(4)
S1 O3 1.439(4)
S1 C25 1.810(6)
F1 C25 1.325(6)
F2 C25 1.299(7)
F3 C25 1.342(8)
N1 N2 1.307(5)
N1 C1 1.379(6)
N2 N3 1.323(5)
N3 C6 1.366(6)
C1 C6 1.384(6)
C1 C2 1.413(7)
C2 C3 1.368(8)
C3 C4 1.412(9)
C4 C5 1.347(8)
C5 C6 1.412(6)
C7 C12 1.378(6)
C7 C8 1.387(6)
C8 C9 1.376(8)
C9 C10 1.345(10)
C10 C11 1.388(9)
C11 C12 1.386(7)
C13 C18 1.398(5)
C13 C14 1.401(6)
C14 C15 1.391(7)
C15 C16 1.366(8)
C16 C17 1.366(9)
C17 C18 1.383(8)
C19 C20 1.379(6)
C19 C24 1.380(6)
C20 C21 1.414(7)
C21 C22 1.364(8)
C22 C23 1.379(8)
C23 C24 1.392(7)
