#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:49:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202697.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_7202697
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            'C48 H52 Au2 N2 O2 P2 S2'
_chemical_formula_weight         1208.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 99.062(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2316(19)
_cell_length_b                   10.341(2)
_cell_length_c                   24.703(5)
_cell_measurement_reflns_used    4381
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      2.2
_cell_volume                     2328.8(8)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.048
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19064
_diffrn_reflns_theta_full        30.1
_diffrn_reflns_theta_max         30.1
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.490
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.59
_refine_diff_density_min         -0.89
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.037
_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)+(0.0429P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.082
_refine_ls_wR_factor_ref         0.097
_reflns_number_gt                5331
_reflns_number_total             6752
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b700295e.txt
_cod_data_source_block           dppb[Au(SC(OEt)=NC6H4Me-p)]2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7202697
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.081884(18) 0.119083(15) 0.056258(7) 0.03069(7) Uani 1 1 d . . .
S1 S -0.11604(14) 0.01776(12) 0.08547(5) 0.0390(3) Uani 1 1 d . . .
P1 P 0.26789(12) 0.24152(10) 0.03408(5) 0.0279(2) Uani 1 1 d . . .
O1 O 0.0303(4) 0.1188(3) 0.17463(16) 0.0452(9) Uani 1 1 d . . .
N1 N -0.1926(4) 0.0403(4) 0.18759(17) 0.0396(9) Uani 1 1 d . . .
C1 C -0.1005(5) 0.0584(4) 0.1555(2) 0.0341(10) Uani 1 1 d . . .
C2 C -0.3264(5) -0.0268(5) 0.17048(19) 0.0343(10) Uani 1 1 d . . .
C3 C -0.4575(6) 0.0373(5) 0.1734(2) 0.0399(11) Uani 1 1 d . . .
H3 H -0.4556 0.1249 0.1837 0.048 Uiso 1 1 calc R . .
C4 C -0.5909(6) -0.0264(5) 0.1611(2) 0.0417(11) Uani 1 1 d . . .
H4 H -0.6783 0.0191 0.1627 0.050 Uiso 1 1 calc R . .
C5 C -0.5973(6) -0.1560(6) 0.1467(2) 0.0459(12) Uani 1 1 d . . .
C6 C -0.4668(6) -0.2200(5) 0.1441(2) 0.0454(12) Uani 1 1 d . . .
H6 H -0.4690 -0.3077 0.1340 0.055 Uiso 1 1 calc R . .
C7 C -0.3318(6) -0.1568(5) 0.1562(2) 0.0415(11) Uani 1 1 d . . .
H7 H -0.2445 -0.2024 0.1547 0.050 Uiso 1 1 calc R . .
C5' C -0.7440(7) -0.2256(7) 0.1333(3) 0.071(2) Uani 1 1 d . . .
H5'1 H -0.8217 -0.1696 0.1417 0.106 Uiso 1 1 calc R . .
H5'2 H -0.7417 -0.3041 0.1549 0.106 Uiso 1 1 calc R . .
H5'3 H -0.7620 -0.2475 0.0946 0.106 Uiso 1 1 calc R . .
C8 C 0.0509(6) 0.1624(6) 0.2314(2) 0.0518(14) Uani 1 1 d . . .
H8A H 0.1560 0.1721 0.2448 0.062 Uiso 1 1 calc R . .
H8B H 0.0120 0.0970 0.2540 0.062 Uiso 1 1 calc R . .
C8A C -0.0249(8) 0.2888(7) 0.2370(3) 0.0682(18) Uani 1 1 d . . .
H8A1 H -0.0087 0.3152 0.2751 0.102 Uiso 1 1 calc R . .
H8A2 H -0.1293 0.2789 0.2245 0.102 Uiso 1 1 calc R . .
H8A3 H 0.0143 0.3540 0.2150 0.102 Uiso 1 1 calc R . .
C9 C 0.3978(5) 0.1648(4) -0.00416(19) 0.0302(9) Uani 1 1 d . . .
H9A H 0.3506 0.1529 -0.0422 0.036 Uiso 1 1 calc R . .
H9B H 0.4817 0.2227 -0.0044 0.036 Uiso 1 1 calc R . .
C10 C 0.4539(5) 0.0335(4) 0.01922(19) 0.0318(9) Uani 1 1 d . . .
H10A H 0.5138 0.0460 0.0553 0.038 Uiso 1 1 calc R . .
H10B H 0.3704 -0.0216 0.0239 0.038 Uiso 1 1 calc R . .
C11 C 0.2023(5) 0.3793(4) -0.0090(2) 0.0312(9) Uani 1 1 d . . .
C12 C 0.1169(6) 0.3543(5) -0.0602(2) 0.0382(11) Uani 1 1 d . . .
H12 H 0.0941 0.2686 -0.0710 0.046 Uiso 1 1 calc R . .
C13 C 0.0667(5) 0.4553(5) -0.0945(2) 0.0417(12) Uani 1 1 d . . .
H13 H 0.0122 0.4382 -0.1292 0.050 Uiso 1 1 calc R . .
C14 C 0.0960(6) 0.5809(5) -0.0782(2) 0.0447(12) Uani 1 1 d . . .
H14 H 0.0617 0.6495 -0.1018 0.054 Uiso 1 1 calc R . .
C15 C 0.1750(6) 0.6062(4) -0.0276(3) 0.0443(13) Uani 1 1 d . . .
H15 H 0.1929 0.6924 -0.0164 0.053 Uiso 1 1 calc R . .
C16 C 0.2290(5) 0.5066(4) 0.0073(2) 0.0378(11) Uani 1 1 d . . .
H16 H 0.2836 0.5252 0.0418 0.045 Uiso 1 1 calc R . .
C17 C 0.3714(5) 0.3117(4) 0.09570(18) 0.0297(9) Uani 1 1 d . . .
C18 C 0.3038(6) 0.3263(5) 0.1420(2) 0.0446(12) Uani 1 1 d . . .
H18 H 0.2074 0.2964 0.1414 0.054 Uiso 1 1 calc R . .
C19 C 0.3785(7) 0.3849(5) 0.1889(2) 0.0549(15) Uani 1 1 d . . .
H19 H 0.3314 0.3973 0.2195 0.066 Uiso 1 1 calc R . .
C20 C 0.5209(7) 0.4244(6) 0.1904(2) 0.0550(15) Uani 1 1 d . . .
H20 H 0.5719 0.4626 0.2223 0.066 Uiso 1 1 calc R . .
C21 C 0.5887(7) 0.4084(6) 0.1454(2) 0.0527(15) Uani 1 1 d . . .
H21 H 0.6862 0.4360 0.1467 0.063 Uiso 1 1 calc R . .
C22 C 0.5160(6) 0.3525(5) 0.0985(2) 0.0450(12) Uani 1 1 d . . .
H22 H 0.5642 0.3417 0.0680 0.054 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 172.35(4) . . ?
C1 S1 Au 104.54(16) . . ?
C17 P1 C11 105.0(2) . . ?
C17 P1 C9 107.8(2) . . ?
C11 P1 C9 102.9(2) . . ?
C17 P1 Au 109.81(15) . . ?
C11 P1 Au 112.48(15) . . ?
C9 P1 Au 117.87(15) . . ?
C1 O1 C8 116.5(4) . . ?
C1 N1 C2 121.6(4) . . ?
N1 C1 O1 119.5(4) . . ?
N1 C1 S1 128.4(4) . . ?
O1 C1 S1 112.2(4) . . ?
C3 C2 C7 118.6(4) . . ?
C3 C2 N1 118.3(4) . . ?
C7 C2 N1 122.9(4) . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 121.0(5) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 118.2(5) . . ?
C4 C5 C5' 120.9(5) . . ?
C6 C5 C5' 120.9(5) . . ?
C7 C6 C5 121.3(5) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C2 120.2(5) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C5 C5' H5'1 109.5 . . ?
C5 C5' H5'2 109.5 . . ?
H5'1 C5' H5'2 109.5 . . ?
C5 C5' H5'3 109.5 . . ?
H5'1 C5' H5'3 109.5 . . ?
H5'2 C5' H5'3 109.5 . . ?
O1 C8 C8A 111.6(5) . . ?
O1 C8 H8A 109.3 . . ?
C8A C8 H8A 109.3 . . ?
O1 C8 H8B 109.3 . . ?
C8A C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
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 113.7(3) . . ?
C10 C9 H9A 108.8 . . ?
P1 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
P1 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C10 C10 C9 110.7(5) 3_655 . ?
C10 C10 H10A 109.5 3_655 . ?
C9 C10 H10A 109.5 . . ?
C10 C10 H10B 109.5 3_655 . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C16 C11 C12 119.0(4) . . ?
C16 C11 P1 123.1(4) . . ?
C12 C11 P1 118.0(3) . . ?
C11 C12 C13 120.0(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.2(5) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.9(5) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 119.8(5) . . ?
C11 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C22 C17 C18 118.4(4) . . ?
C22 C17 P1 122.5(4) . . ?
C18 C17 P1 119.1(4) . . ?
C19 C18 C17 120.2(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 120.0(6) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.0(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.7(6) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C17 120.5(5) . . ?
C21 C22 H22 119.7 . . ?
C17 C22 H22 119.7 . . ?
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 2.2689(12) . ?
Au S1 2.3179(13) . ?
S1 C1 1.763(5) . ?
P1 C17 1.816(4) . ?
P1 C11 1.823(4) . ?
P1 C9 1.821(4) . ?
O1 C1 1.375(5) . ?
O1 C8 1.456(7) . ?
N1 C1 1.265(6) . ?
N1 C2 1.423(6) . ?
C2 C3 1.391(7) . ?
C2 C7 1.389(7) . ?
C3 C4 1.387(7) . ?
C3 H3 0.9400 . ?
C4 C5 1.386(7) . ?
C4 H4 0.9400 . ?
C5 C6 1.386(8) . ?
C5 C5' 1.523(7) . ?
C6 C7 1.397(7) . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?
C5' H5'1 0.9700 . ?
C5' H5'2 0.9700 . ?
C5' H5'3 0.9700 . ?
C8 C8A 1.499(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8A H8A3 0.9700 . ?
C9 C10 1.533(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C10 1.536(8) 3_655 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C16 1.387(6) . ?
C11 C12 1.405(7) . ?
C12 C13 1.380(7) . ?
C12 H12 0.9400 . ?
C13 C14 1.374(7) . ?
C13 H13 0.9400 . ?
C14 C15 1.370(8) . ?
C14 H14 0.9400 . ?
C15 C16 1.384(7) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 C22 1.391(7) . ?
C17 C18 1.394(7) . ?
C18 C19 1.390(8) . ?
C18 H18 0.9400 . ?
C19 C20 1.372(9) . ?
C19 H19 0.9400 . ?
C20 C21 1.368(9) . ?
C20 H20 0.9400 . ?
C21 C22 1.372(8) . ?
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 -43.8(4) . . . . ?
S1 Au P1 C17 50.5(4) . . . . ?
S1 Au P1 C11 -66.1(4) . . . . ?
S1 Au P1 C9 174.4(3) . . . . ?
C2 N1 C1 O1 -177.1(4) . . . . ?
C2 N1 C1 S1 3.9(7) . . . . ?
C8 O1 C1 N1 -2.2(7) . . . . ?
C8 O1 C1 S1 177.0(4) . . . . ?
Au S1 C1 N1 169.9(4) . . . . ?
Au S1 C1 O1 -9.1(4) . . . . ?
C1 N1 C2 C3 -121.2(5) . . . . ?
C1 N1 C2 C7 65.2(7) . . . . ?
C7 C2 C3 C4 -1.3(7) . . . . ?
N1 C2 C3 C4 -175.1(4) . . . . ?
C2 C3 C4 C5 1.1(8) . . . . ?
C3 C4 C5 C6 -0.8(8) . . . . ?
C3 C4 C5 C5' -179.9(5) . . . . ?
C4 C5 C6 C7 0.7(8) . . . . ?
C5' C5 C6 C7 179.8(6) . . . . ?
C5 C6 C7 C2 -0.9(8) . . . . ?
C3 C2 C7 C6 1.2(7) . . . . ?
N1 C2 C7 C6 174.7(5) . . . . ?
C1 O1 C8 C8A -80.8(6) . . . . ?
C17 P1 C9 C10 77.6(4) . . . . ?
C11 P1 C9 C10 -171.7(3) . . . . ?
Au P1 C9 C10 -47.3(4) . . . . ?
P1 C9 C10 C10 172.4(4) . . . 3_655 ?
C17 P1 C11 C16 -1.8(5) . . . . ?
C9 P1 C11 C16 -114.6(4) . . . . ?
Au P1 C11 C16 117.6(4) . . . . ?
C17 P1 C11 C12 -179.8(4) . . . . ?
C9 P1 C11 C12 67.5(4) . . . . ?
Au P1 C11 C12 -60.4(4) . . . . ?
C16 C11 C12 C13 2.9(8) . . . . ?
P1 C11 C12 C13 -179.0(4) . . . . ?
C11 C12 C13 C14 -2.0(8) . . . . ?
C12 C13 C14 C15 -0.2(8) . . . . ?
C13 C14 C15 C16 1.3(9) . . . . ?
C12 C11 C16 C15 -1.8(7) . . . . ?
P1 C11 C16 C15 -179.7(4) . . . . ?
C14 C15 C16 C11 -0.4(8) . . . . ?
C11 P1 C17 C22 -81.6(4) . . . . ?
C9 P1 C17 C22 27.6(5) . . . . ?
Au P1 C17 C22 157.2(4) . . . . ?
C11 P1 C17 C18 98.0(4) . . . . ?
C9 P1 C17 C18 -152.8(4) . . . . ?
Au P1 C17 C18 -23.2(4) . . . . ?
C22 C17 C18 C19 2.4(8) . . . . ?
P1 C17 C18 C19 -177.2(4) . . . . ?
C17 C18 C19 C20 -2.3(9) . . . . ?
C18 C19 C20 C21 1.2(10) . . . . ?
C19 C20 C21 C22 -0.2(10) . . . . ?
C20 C21 C22 C17 0.4(10) . . . . ?
C18 C17 C22 C21 -1.5(8) . . . . ?
P1 C17 C22 C21 178.2(5) . . . . ?
