#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:49:15 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202695.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_7202695
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            'C49 H54 Au2 N4 O7 P2 S2'
_chemical_formula_weight         1330.95
_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                104.028(5)
_cell_angle_beta                 90.272(5)
_cell_angle_gamma                107.186(5)
_cell_formula_units_Z            1
_cell_length_a                   8.872(2)
_cell_length_b                   12.310(3)
_cell_length_c                   12.717(3)
_cell_measurement_reflns_used    1003
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.9
_cell_volume                     1282.9(5)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.087
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9873
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.907
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.24
_refine_diff_density_min         -1.91
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7227
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.096
_refine_ls_R_factor_gt           0.048
_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)+(0.0662P)²+0.6328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.113
_refine_ls_wR_factor_ref         0.136
_reflns_number_gt                4887
_reflns_number_total             7227
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b700295e.txt
_cod_data_source_block           dppb[Au(SC(OiPr)=NC6H4NO2-p)]2.MeOH
_cod_original_cell_volume        1282.9(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202695
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 0.18861(4) 0.03429(3) 0.25845(2) 0.03527(10) Uani 1 1 d . . .
S1 S 0.2441(3) 0.19674(19) 0.40472(16) 0.0528(6) Uani 1 1 d . . .
P1 P 0.1455(2) -0.11115(16) 0.10389(13) 0.0283(4) Uani 1 1 d . . .
O1 O 0.2463(7) 0.0294(5) 0.4972(4) 0.0466(14) Uani 1 1 d . . .
O2 O 0.1594(10) 0.7007(7) 0.7705(6) 0.077(2) Uani 1 1 d . . .
O3 O 0.4080(11) 0.7529(7) 0.7440(7) 0.091(3) Uani 1 1 d . . .
O4 O 0.067(2) 0.4740(17) 0.4609(15) 0.103(6) Uiso 0.50 1 d PD . .
N1 N 0.2549(9) 0.2024(6) 0.6167(5) 0.0441(16) Uani 1 1 d . . .
N2 N 0.2808(11) 0.6770(7) 0.7436(6) 0.056(2) Uani 1 1 d . . .
C1 C 0.2509(10) 0.1434(7) 0.5205(6) 0.0430(18) Uani 1 1 d . . .
C2 C 0.2635(10) 0.3216(7) 0.6447(6) 0.0409(18) Uani 1 1 d . . .
C3 C 0.1422(11) 0.3544(9) 0.6976(7) 0.053(2) Uani 1 1 d . . .
H3 H 0.0545 0.2964 0.7118 0.064 Uiso 1 1 calc R . .
C4 C 0.1474(12) 0.4702(9) 0.7298(7) 0.057(2) Uani 1 1 d . . .
H4 H 0.0639 0.4919 0.7652 0.068 Uiso 1 1 calc R . .
C5 C 0.2771(11) 0.5538(8) 0.7093(6) 0.048(2) Uani 1 1 d . . .
C6 C 0.4012(10) 0.5255(8) 0.6577(6) 0.048(2) Uani 1 1 d . . .
H6 H 0.4894 0.5841 0.6450 0.058 Uiso 1 1 calc R . .
C7 C 0.3921(10) 0.4080(8) 0.6251(6) 0.0437(19) Uani 1 1 d . . .
H7 H 0.4751 0.3865 0.5890 0.052 Uiso 1 1 calc R . .
C8 C 0.2333(11) -0.0274(8) 0.5868(6) 0.048(2) Uani 1 1 d . . .
H8 H 0.1502 -0.0092 0.6333 0.058 Uiso 1 1 calc R . .
C9 C 0.3884(13) 0.0130(9) 0.6527(9) 0.071(3) Uani 1 1 d . . .
H9A H 0.4128 0.0958 0.6893 0.106 Uiso 1 1 calc R . .
H9B H 0.4707 0.0016 0.6052 0.106 Uiso 1 1 calc R . .
H9C H 0.3825 -0.0320 0.7063 0.106 Uiso 1 1 calc R . .
C10 C 0.1853(15) -0.1565(9) 0.5313(8) 0.075(3) Uani 1 1 d . . .
H10A H 0.0839 -0.1792 0.4899 0.112 Uiso 1 1 calc R . .
H10B H 0.1767 -0.2011 0.5855 0.112 Uiso 1 1 calc R . .
H10C H 0.2645 -0.1726 0.4827 0.112 Uiso 1 1 calc R . .
C11 C 0.2716(8) -0.0636(6) -0.0002(5) 0.0296(14) Uani 1 1 d . . .
H11A H 0.2560 -0.1299 -0.0644 0.036 Uiso 1 1 calc R . .
H11B H 0.2415 -0.0014 -0.0223 0.036 Uiso 1 1 calc R . .
C12 C 0.4459(8) -0.0177(6) 0.0429(5) 0.0313(15) Uani 1 1 d . . .
H12A H 0.4616 0.0504 0.1054 0.038 Uiso 1 1 calc R . .
H12B H 0.4741 -0.0790 0.0680 0.038 Uiso 1 1 calc R . .
C13 C 0.1951(8) -0.2382(6) 0.1226(6) 0.0340(15) Uani 1 1 d . . .
C14 C 0.1724(10) -0.3371(7) 0.0363(7) 0.0432(18) Uani 1 1 d . . .
H14 H 0.1285 -0.3395 -0.0320 0.052 Uiso 1 1 calc R . .
C15 C 0.2153(11) -0.4326(8) 0.0516(9) 0.056(2) Uani 1 1 d . . .
H15 H 0.2022 -0.4991 -0.0068 0.067 Uiso 1 1 calc R . .
C16 C 0.2782(11) -0.4296(9) 0.1543(9) 0.058(2) Uani 1 1 d . . .
H16 H 0.3045 -0.4947 0.1657 0.070 Uiso 1 1 calc R . .
C17 C 0.3009(12) -0.3293(9) 0.2385(8) 0.059(2) Uani 1 1 d . . .
H17 H 0.3469 -0.3248 0.3068 0.071 Uiso 1 1 calc R . .
C18 C 0.2566(10) -0.2366(8) 0.2225(7) 0.0464(19) Uani 1 1 d . . .
H18 H 0.2684 -0.1705 0.2811 0.056 Uiso 1 1 calc R . .
C19 C -0.0585(8) -0.1698(6) 0.0440(5) 0.0308(14) Uani 1 1 d . . .
C20 C -0.1769(9) -0.1900(7) 0.1126(6) 0.0385(17) Uani 1 1 d . . .
H20 H -0.1512 -0.1681 0.1882 0.046 Uiso 1 1 calc R . .
C21 C -0.3322(9) -0.2416(8) 0.0725(7) 0.047(2) Uani 1 1 d . . .
H21 H -0.4123 -0.2557 0.1201 0.056 Uiso 1 1 calc R . .
C22 C -0.3708(10) -0.2736(8) -0.0412(7) 0.047(2) Uani 1 1 d . . .
H22 H -0.4767 -0.3100 -0.0695 0.057 Uiso 1 1 calc R . .
C23 C -0.2532(10) -0.2513(7) -0.1100(6) 0.0439(19) Uani 1 1 d . . .
H23 H -0.2794 -0.2708 -0.1853 0.053 Uiso 1 1 calc R . .
C24 C -0.0977(9) -0.2009(7) -0.0697(5) 0.0361(16) Uani 1 1 d . . .
H24 H -0.0177 -0.1870 -0.1174 0.043 Uiso 1 1 calc R . .
C25 C 0.194(2) 0.5393(17) 0.4269(16) 0.058(5) Uiso 0.50 1 d PD . .
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 173.73(7) . . ?
C1 S1 Au 105.7(3) . . ?
C13 P1 C19 104.6(3) . . ?
C13 P1 C11 104.5(3) . . ?
C19 P1 C11 107.8(3) . . ?
C13 P1 Au 112.8(2) . . ?
C19 P1 Au 115.2(2) . . ?
C11 P1 Au 111.2(2) . . ?
C1 O1 C8 118.1(6) . . ?
C25 O4 O4 125(2) . 2_566 ?
C1 N1 C2 123.6(7) . . ?
O3 N2 O2 122.8(9) . . ?
O3 N2 C5 117.7(9) . . ?
O2 N2 C5 119.4(9) . . ?
N1 C1 O1 121.7(8) . . ?
N1 C1 S1 124.6(7) . . ?
O1 C1 S1 113.7(5) . . ?
C7 C2 N1 122.3(8) . . ?
C7 C2 C3 118.8(8) . . ?
N1 C2 C3 118.9(8) . . ?
C4 C3 C2 121.2(9) . . ?
C3 C4 C5 118.6(8) . . ?
C6 C5 C4 122.4(8) . . ?
C6 C5 N2 119.6(9) . . ?
C4 C5 N2 118.1(8) . . ?
C5 C6 C7 117.9(9) . . ?
C2 C7 C6 121.3(8) . . ?
O1 C8 C9 110.0(8) . . ?
O1 C8 C10 104.1(7) . . ?
C9 C8 C10 112.2(9) . . ?
C12 C11 P1 110.7(4) . . ?
C12 C12 C11 112.1(7) 2_655 . ?
C18 C13 C14 119.7(7) . . ?
C18 C13 P1 119.8(6) . . ?
C14 C13 P1 120.4(6) . . ?
C13 C14 C15 119.5(8) . . ?
C16 C15 C14 120.1(9) . . ?
C17 C16 C15 119.0(8) . . ?
C16 C17 C18 120.2(9) . . ?
C13 C18 C17 121.4(9) . . ?
C20 C19 C24 119.5(7) . . ?
C20 C19 P1 117.8(5) . . ?
C24 C19 P1 122.6(5) . . ?
C19 C20 C21 120.9(7) . . ?
C20 C21 C22 119.4(7) . . ?
C23 C22 C21 119.9(8) . . ?
C22 C23 C24 120.6(7) . . ?
C23 C24 C19 119.7(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 2.2576(17) . ?
Au S1 2.304(2) . ?
S1 C1 1.759(8) . ?
P1 C13 1.812(8) . ?
P1 C19 1.823(7) . ?
P1 C11 1.830(7) . ?
O1 C1 1.350(9) . ?
O1 C8 1.464(10) . ?
O2 N2 1.226(10) . ?
O3 N2 1.233(11) . ?
O4 C25 1.315(10) . ?
O4 O4 1.73(4) 2_566 ?
N1 C1 1.256(10) . ?
N1 C2 1.402(10) . ?
N2 C5 1.463(11) . ?
C2 C7 1.382(12) . ?
C2 C3 1.381(12) . ?
C3 C4 1.371(13) . ?
C4 C5 1.373(14) . ?
C5 C6 1.374(12) . ?
C6 C7 1.382(12) . ?
C8 C9 1.491(12) . ?
C8 C10 1.503(13) . ?
C11 C12 1.528(10) . ?
C12 C12 1.516(13) 2_655 ?
C13 C18 1.373(11) . ?
C13 C14 1.390(10) . ?
C14 C15 1.393(12) . ?
C15 C16 1.406(14) . ?
C16 C17 1.387(14) . ?
C17 C18 1.369(12) . ?
C19 C20 1.374(10) . ?
C19 C24 1.417(9) . ?
C20 C21 1.372(11) . ?
C21 C22 1.414(12) . ?
C22 C23 1.373(12) . ?
C23 C24 1.372(11) . ?
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 -158.8(7) . . . . ?
S1 Au P1 C13 137.6(8) . . . . ?
S1 Au P1 C19 -102.5(8) . . . . ?
S1 Au P1 C11 20.5(8) . . . . ?
C2 N1 C1 O1 178.4(7) . . . . ?
C2 N1 C1 S1 -3.8(13) . . . . ?
C8 O1 C1 N1 4.8(12) . . . . ?
C8 O1 C1 S1 -173.2(6) . . . . ?
Au S1 C1 N1 -168.9(7) . . . . ?
Au S1 C1 O1 9.0(7) . . . . ?
C1 N1 C2 C7 -63.9(12) . . . . ?
C1 N1 C2 C3 118.8(10) . . . . ?
C7 C2 C3 C4 0.5(13) . . . . ?
N1 C2 C3 C4 177.9(8) . . . . ?
C2 C3 C4 C5 -0.6(15) . . . . ?
C3 C4 C5 C6 0.1(14) . . . . ?
C3 C4 C5 N2 179.7(8) . . . . ?
O3 N2 C5 C6 -13.8(12) . . . . ?
O2 N2 C5 C6 166.3(8) . . . . ?
O3 N2 C5 C4 166.6(9) . . . . ?
O2 N2 C5 C4 -13.3(12) . . . . ?
C4 C5 C6 C7 0.6(13) . . . . ?
N2 C5 C6 C7 -179.0(7) . . . . ?
N1 C2 C7 C6 -177.1(7) . . . . ?
C3 C2 C7 C6 0.2(12) . . . . ?
C5 C6 C7 C2 -0.7(12) . . . . ?
C1 O1 C8 C9 -75.2(10) . . . . ?
C1 O1 C8 C10 164.5(8) . . . . ?
C13 P1 C11 C12 -66.8(5) . . . . ?
C19 P1 C11 C12 -177.7(5) . . . . ?
Au P1 C11 C12 55.1(5) . . . . ?
P1 C11 C12 C12 177.7(7) . . . 2_655 ?
C19 P1 C13 C18 -127.8(6) . . . . ?
C11 P1 C13 C18 119.0(6) . . . . ?
Au P1 C13 C18 -1.9(7) . . . . ?
C19 P1 C13 C14 52.7(7) . . . . ?
C11 P1 C13 C14 -60.5(7) . . . . ?
Au P1 C13 C14 178.5(5) . . . . ?
C18 C13 C14 C15 -1.3(12) . . . . ?
P1 C13 C14 C15 178.3(7) . . . . ?
C13 C14 C15 C16 1.2(13) . . . . ?
C14 C15 C16 C17 -1.9(15) . . . . ?
C15 C16 C17 C18 2.6(15) . . . . ?
C14 C13 C18 C17 2.0(13) . . . . ?
P1 C13 C18 C17 -177.5(7) . . . . ?
C16 C17 C18 C13 -2.7(15) . . . . ?
C13 P1 C19 C20 81.4(6) . . . . ?
C11 P1 C19 C20 -167.8(6) . . . . ?
Au P1 C19 C20 -42.9(7) . . . . ?
C13 P1 C19 C24 -95.1(7) . . . . ?
C11 P1 C19 C24 15.8(7) . . . . ?
Au P1 C19 C24 140.6(6) . . . . ?
C24 C19 C20 C21 1.2(12) . . . . ?
P1 C19 C20 C21 -175.4(7) . . . . ?
C19 C20 C21 C22 -0.5(13) . . . . ?
C20 C21 C22 C23 -0.9(14) . . . . ?
C21 C22 C23 C24 1.6(13) . . . . ?
C22 C23 C24 C19 -1.0(12) . . . . ?
C20 C19 C24 C23 -0.4(11) . . . . ?
P1 C19 C24 C23 176.0(6) . . . . ?
