#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:49:15 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202692.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_7202692
loop_
_publ_author_name
'Ho, Soo Yei'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Supramolecular aggregation patterns in the crystal structures of the
 dinuclear phosphinegold(i) thiolates,
 [(Ph2P(CH2)4PPh2){AuSC(OR)?NC6H4Y-4}2] for R = Me, Et or iPr and Y =
 H, NO2 or Me: the influence on intermolecular interactions exerted by
 R and Y
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              368
_journal_paper_doi               10.1039/b700295e
_journal_volume                  9
_journal_year                    2007
_chemical_formula_sum            'C46 H48 Au2 N2 O2 P2 S2'
_chemical_formula_weight         1180.86
_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                105.973(1)
_cell_angle_beta                 99.485(1)
_cell_angle_gamma                106.821(1)
_cell_formula_units_Z            1
_cell_length_a                   8.4818(6)
_cell_length_b                   11.9828(8)
_cell_length_c                   12.1684(8)
_cell_measurement_reflns_used    5728
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.6
_cell_volume                     1097.24(13)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SHELXTL (Bruker, 2000)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'Bruker SHEXLTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'PATTY in DIRDIF92 (Beurskens et al., 1992)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker AXS SMART CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9225
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.8
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.885
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             574
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.77
_refine_diff_density_min         -0.96
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.16
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         6265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.16
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.035
_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)+(0.0424P)²+0.2837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.090
_reflns_number_gt                5960
_reflns_number_total             6265
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b700295e.txt
_cod_data_source_block           dppb[Au(SC(OEt)=NC6H5)]2(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202692
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au 0.198667(19) 0.057701(13) 0.260308(13) 0.03209(6) Uani 1 1 d . . .
S1 S 0.22430(19) 0.24270(11) 0.39730(10) 0.0435(3) Uani 1 1 d . . .
P1 P 0.15975(13) -0.11539(10) 0.11005(9) 0.02880(19) Uani 1 1 d . . .
O1 O 0.2337(4) 0.0979(3) 0.5199(3) 0.0404(7) Uani 1 1 d . . .
N1 N 0.2118(5) 0.2794(3) 0.6255(3) 0.0361(7) Uani 1 1 d . . .
C1 C 0.2232(5) 0.2107(4) 0.5293(4) 0.0344(8) Uani 1 1 d . . .
C2 C 0.2023(5) 0.3975(4) 0.6375(4) 0.0356(8) Uani 1 1 d . . .
C3 C 0.0728(7) 0.4259(5) 0.6827(6) 0.0563(14) Uani 1 1 d . . .
H3 H -0.0026 0.3680 0.7061 0.068 Uiso 1 1 calc R . .
C4 C 0.0552(9) 0.5387(6) 0.6932(8) 0.073(2) Uani 1 1 d . . .
H4 H -0.0367 0.5549 0.7196 0.087 Uiso 1 1 calc R . .
C5 C 0.1683(8) 0.6280(5) 0.6662(6) 0.0634(16) Uani 1 1 d . . .
H5 H 0.1557 0.7051 0.6752 0.076 Uiso 1 1 calc R . .
C6 C 0.3007(7) 0.6028(5) 0.6257(5) 0.0483(11) Uani 1 1 d . . .
H6 H 0.3795 0.6634 0.6071 0.058 Uiso 1 1 calc R . .
C7 C 0.3190(6) 0.4895(5) 0.6120(4) 0.0418(10) Uani 1 1 d . . .
H7 H 0.4111 0.4740 0.5853 0.050 Uiso 1 1 calc R . .
C8 C 0.2206(7) 0.0588(5) 0.6205(4) 0.0442(10) Uani 1 1 d . . .
H8A H 0.1070 0.0480 0.6337 0.053 Uiso 1 1 calc R . .
H8B H 0.3065 0.1206 0.6920 0.053 Uiso 1 1 calc R . .
C8A C 0.2507(9) -0.0638(5) 0.5917(6) 0.0595(15) Uani 1 1 d . . .
H8A1 H 0.2431 -0.0943 0.6574 0.089 Uiso 1 1 calc R . .
H8A2 H 0.3633 -0.0516 0.5787 0.089 Uiso 1 1 calc R . .
H8A3 H 0.1649 -0.1237 0.5207 0.089 Uiso 1 1 calc R . .
C9 C 0.2654(5) -0.0844(4) -0.0033(4) 0.0348(8) Uani 1 1 d . . .
H9A H 0.2462 -0.1634 -0.0646 0.042 Uiso 1 1 calc R . .
H9B H 0.2140 -0.0361 -0.0408 0.042 Uiso 1 1 calc R . .
C10 C 0.4563(5) -0.0140(4) 0.0468(4) 0.0334(8) Uani 1 1 d . . .
H10A H 0.5080 -0.0632 0.0829 0.040 Uiso 1 1 calc R . .
H10B H 0.4755 0.0641 0.1093 0.040 Uiso 1 1 calc R . .
C11 C 0.2312(5) -0.2271(4) 0.1565(4) 0.0305(8) Uani 1 1 d . . .
C12 C 0.3129(6) -0.1975(5) 0.2758(4) 0.0391(9) Uani 1 1 d . . .
H12 H 0.3338 -0.1190 0.3311 0.047 Uiso 1 1 calc R . .
C13 C 0.3626(7) -0.2853(6) 0.3113(5) 0.0524(13) Uani 1 1 d . . .
H13 H 0.4196 -0.2657 0.3910 0.063 Uiso 1 1 calc R . .
C14 C 0.3293(7) -0.4008(5) 0.2310(6) 0.0531(13) Uani 1 1 d . . .
H14 H 0.3636 -0.4595 0.2564 0.064 Uiso 1 1 calc R . .
C15 C 0.2470(6) -0.4313(5) 0.1147(5) 0.0479(12) Uani 1 1 d . . .
H15 H 0.2246 -0.5108 0.0610 0.057 Uiso 1 1 calc R . .
C16 C 0.1958(6) -0.3454(4) 0.0753(4) 0.0392(9) Uani 1 1 d . . .
H16 H 0.1385 -0.3665 -0.0047 0.047 Uiso 1 1 calc R . .
C17 C -0.0660(5) -0.1988(4) 0.0379(4) 0.0298(7) Uani 1 1 d . . .
C18 C -0.1683(6) -0.2360(5) 0.1098(4) 0.0406(10) Uani 1 1 d . . .
H18 H -0.1190 -0.2211 0.1899 0.049 Uiso 1 1 calc R . .
C19 C -0.3438(6) -0.2954(5) 0.0615(5) 0.0488(12) Uani 1 1 d . . .
H19 H -0.4132 -0.3189 0.1099 0.059 Uiso 1 1 calc R . .
C20 C -0.4172(6) -0.3202(5) -0.0565(5) 0.0462(11) Uani 1 1 d . . .
H20 H -0.5358 -0.3608 -0.0886 0.055 Uiso 1 1 calc R . .
C21 C -0.3151(6) -0.2850(5) -0.1267(4) 0.0412(10) Uani 1 1 d . . .
H21 H -0.3649 -0.3010 -0.2070 0.049 Uiso 1 1 calc R . .
C22 C -0.1389(6) -0.2258(4) -0.0808(4) 0.0361(8) Uani 1 1 d . . .
H22 H -0.0701 -0.2045 -0.1303 0.043 Uiso 1 1 calc R . .
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'
Au Au -2.0133 8.8022 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Au S1 173.23(4) . . ?
C1 S1 Au 104.29(15) . . ?
C17 P1 C11 103.92(18) . . ?
C17 P1 C9 107.68(19) . . ?
C11 P1 C9 107.0(2) . . ?
C17 P1 Au 110.58(13) . . ?
C11 P1 Au 113.82(14) . . ?
C9 P1 Au 113.24(15) . . ?
C1 O1 C8 116.6(4) . . ?
C1 N1 C2 121.4(4) . . ?
N1 C1 O1 120.5(4) . . ?
N1 C1 S1 127.2(4) . . ?
O1 C1 S1 112.3(3) . . ?
C3 C2 C7 118.0(5) . . ?
C3 C2 N1 117.8(4) . . ?
C7 C2 N1 124.1(4) . . ?
C4 C3 C2 120.1(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.6(6) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 120.6(5) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 120.7(5) . . ?
C6 C7 H7 119.7 . . ?
C2 C7 H7 119.7 . . ?
O1 C8 C8A 106.2(4) . . ?
O1 C8 H8A 110.5 . . ?
C8A C8 H8A 110.5 . . ?
O1 C8 H8B 110.5 . . ?
C8A C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C8 C8A H8A1 109.5 . . ?
C8 C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C8 C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10 C9 P1 112.6(3) . . ?
C10 C9 H9A 109.1 . . ?
P1 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
P1 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 C10 112.7(4) . 2_655 ?
C9 C10 H10A 109.1 . . ?
C10 C10 H10A 109.1 2_655 . ?
C9 C10 H10B 109.1 . . ?
C10 C10 H10B 109.1 2_655 . ?
H10A C10 H10B 107.8 . . ?
C12 C11 C16 120.2(4) . . ?
C12 C11 P1 119.5(3) . . ?
C16 C11 P1 120.2(3) . . ?
C13 C12 C11 119.1(5) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C14 C13 C12 120.5(5) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 120.8(5) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 118.9(5) . . ?
C15 C16 H16 120.5 . . ?
C11 C16 H16 120.5 . . ?
C22 C17 C18 119.8(4) . . ?
C22 C17 P1 123.9(3) . . ?
C18 C17 P1 116.3(3) . . ?
C17 C18 C19 119.3(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 120.9(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 119.2(4) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C20 C21 C22 121.1(5) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
C17 C22 C21 119.5(4) . . ?
C17 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au P1 2.2520(10) . ?
Au S1 2.3040(11) . ?
S1 C1 1.752(4) . ?
P1 C17 1.814(4) . ?
P1 C11 1.803(4) . ?
P1 C9 1.827(4) . ?
O1 C1 1.355(5) . ?
O1 C8 1.435(6) . ?
N1 C1 1.269(5) . ?
N1 C2 1.409(6) . ?
C2 C3 1.391(7) . ?
C2 C7 1.397(6) . ?
C3 C4 1.377(8) . ?
C3 H3 0.9400 . ?
C4 C5 1.369(9) . ?
C4 H4 0.9400 . ?
C5 C6 1.376(8) . ?
C5 H5 0.9400 . ?
C6 C7 1.379(7) . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?
C8 C8A 1.520(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8A H8A3 0.9700 . ?
C9 C10 1.518(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C10 1.518(8) 2_655 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.398(6) . ?
C11 C16 1.401(6) . ?
C12 C13 1.385(7) . ?
C12 H12 0.9400 . ?
C13 C14 1.374(9) . ?
C13 H13 0.9400 . ?
C14 C15 1.365(8) . ?
C14 H14 0.9400 . ?
C15 C16 1.393(7) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 C22 1.380(6) . ?
C17 C18 1.399(6) . ?
C18 C19 1.391(7) . ?
C18 H18 0.9400 . ?
C19 C20 1.378(8) . ?
C19 H19 0.9400 . ?
C20 C21 1.374(7) . ?
C20 H20 0.9400 . ?
C21 C22 1.393(6) . ?
C21 H21 0.9400 . ?
C22 H22 0.9400 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 Au S1 C1 153.9(3) . . . . ?
S1 Au P1 C17 -63.3(4) . . . . ?
S1 Au P1 C11 -179.9(3) . . . . ?
S1 Au P1 C9 57.6(4) . . . . ?
C2 N1 C1 O1 179.5(4) . . . . ?
C2 N1 C1 S1 -1.6(7) . . . . ?
C8 O1 C1 N1 3.7(6) . . . . ?
C8 O1 C1 S1 -175.4(3) . . . . ?
Au S1 C1 N1 -169.9(4) . . . . ?
Au S1 C1 O1 9.1(3) . . . . ?
C1 N1 C2 C3 130.1(5) . . . . ?
C1 N1 C2 C7 -52.9(6) . . . . ?
C7 C2 C3 C4 4.6(9) . . . . ?
N1 C2 C3 C4 -178.3(6) . . . . ?
C2 C3 C4 C5 -3.6(12) . . . . ?
C3 C4 C5 C6 1.1(12) . . . . ?
C4 C5 C6 C7 0.2(10) . . . . ?
C5 C6 C7 C2 0.9(8) . . . . ?
C3 C2 C7 C6 -3.3(7) . . . . ?
N1 C2 C7 C6 179.8(4) . . . . ?
C1 O1 C8 C8A -175.4(4) . . . . ?
C17 P1 C9 C10 179.8(3) . . . . ?
C11 P1 C9 C10 -69.0(3) . . . . ?
Au P1 C9 C10 57.2(3) . . . . ?
P1 C9 C10 C10 -178.8(4) . . . 2_655 ?
C17 P1 C11 C12 -124.6(3) . . . . ?
C9 P1 C11 C12 121.7(3) . . . . ?
Au P1 C11 C12 -4.2(4) . . . . ?
C17 P1 C11 C16 51.6(4) . . . . ?
C9 P1 C11 C16 -62.2(4) . . . . ?
Au P1 C11 C16 171.9(3) . . . . ?
C16 C11 C12 C13 1.9(6) . . . . ?
P1 C11 C12 C13 178.0(4) . . . . ?
C11 C12 C13 C14 -1.2(7) . . . . ?
C12 C13 C14 C15 0.1(8) . . . . ?
C13 C14 C15 C16 0.3(8) . . . . ?
C14 C15 C16 C11 0.4(7) . . . . ?
C12 C11 C16 C15 -1.5(6) . . . . ?
P1 C11 C16 C15 -177.6(3) . . . . ?
C11 P1 C17 C22 -116.2(4) . . . . ?
C9 P1 C17 C22 -2.9(4) . . . . ?
Au P1 C17 C22 121.3(3) . . . . ?
C11 P1 C17 C18 64.0(4) . . . . ?
C9 P1 C17 C18 177.3(3) . . . . ?
Au P1 C17 C18 -58.5(4) . . . . ?
C22 C17 C18 C19 -2.7(7) . . . . ?
P1 C17 C18 C19 177.1(4) . . . . ?
C17 C18 C19 C20 1.4(8) . . . . ?
C18 C19 C20 C21 -0.4(8) . . . . ?
C19 C20 C21 C22 0.6(8) . . . . ?
C18 C17 C22 C21 3.0(7) . . . . ?
P1 C17 C22 C21 -176.8(3) . . . . ?
C20 C21 C22 C17 -1.9(7) . . . . ?
