#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:49:15 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180357 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/26/7202691.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_7202691
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 Cl4 N2 O2 P2 S2'
_chemical_formula_weight         1322.66
_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                114.135(1)
_cell_angle_beta                 98.032(1)
_cell_angle_gamma                92.760(1)
_cell_formula_units_Z            1
_cell_length_a                   9.9628(6)
_cell_length_b                   10.6131(7)
_cell_length_c                   12.7053(8)
_cell_measurement_reflns_used    4879
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      2.5
_cell_volume                     1205.68(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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.020
_diffrn_reflns_av_sigmaI/netI    0.045
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10047
_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    6.491
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 2000 & Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             642
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.06
_refine_diff_density_min         -1.07
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.00
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.00
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.027
_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)+(0.0234P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.057
_refine_ls_wR_factor_ref         0.059
_reflns_number_gt                6183
_reflns_number_total             6865
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b700295e.txt
_cod_data_source_block           dppb[Au(SC(OMe)=NC6H5)]2.2CH2Cl2(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7202691
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 0.091194(11) 0.404745(12) 0.076744(10) 0.02137(4) Uani 1 1 d . . .
Cl1 Cl 0.7888(2) 0.1187(2) 0.66240(15) 0.1094(6) Uani 1 1 d . . .
Cl2 Cl 0.71550(16) 0.1935(2) 0.8928(2) 0.1101(6) Uani 1 1 d . . .
S1 S -0.07033(9) 0.53598(10) 0.17095(7) 0.03190(18) Uani 1 1 d . . .
P1 P 0.25024(7) 0.26465(8) 0.00259(7) 0.01872(14) Uani 1 1 d . . .
O1 O 0.1273(2) 0.5490(3) 0.3341(2) 0.0373(6) Uani 1 1 d . . .
N1 N -0.0624(3) 0.6332(3) 0.4053(2) 0.0339(7) Uani 1 1 d . . .
C1 C -0.0032(3) 0.5778(4) 0.3184(3) 0.0283(7) Uani 1 1 d . . .
C2 C -0.2008(3) 0.6570(4) 0.3883(3) 0.0309(7) Uani 1 1 d . . .
C3 C -0.3054(4) 0.5473(5) 0.3456(3) 0.0404(9) Uani 1 1 d . . .
H3 H -0.2836 0.4557 0.3226 0.048 Uiso 1 1 calc R . .
C4 C -0.4398(4) 0.5713(5) 0.3365(3) 0.0495(11) Uani 1 1 d . . .
H4 H -0.5093 0.4964 0.3075 0.059 Uiso 1 1 calc R . .
C5 C -0.4726(4) 0.7042(6) 0.3698(4) 0.0565(13) Uani 1 1 d . . .
H5 H -0.5646 0.7206 0.3636 0.068 Uiso 1 1 calc R . .
C6 C -0.3709(4) 0.8139(5) 0.4124(4) 0.0527(11) Uani 1 1 d . . .
H6 H -0.3935 0.9050 0.4338 0.063 Uiso 1 1 calc R . .
C7 C -0.2343(4) 0.7902(4) 0.4240(3) 0.0405(9) Uani 1 1 d . . .
H7 H -0.1652 0.8657 0.4564 0.049 Uiso 1 1 calc R . .
C8 C 0.1883(4) 0.5791(5) 0.4524(3) 0.0481(11) Uani 1 1 d . . .
H8A H 0.1931 0.6781 0.5005 0.072 Uiso 1 1 calc R . .
H8B H 0.2796 0.5512 0.4536 0.072 Uiso 1 1 calc R . .
H8C H 0.1334 0.5284 0.4829 0.072 Uiso 1 1 calc R . .
C9 C 0.3729(3) 0.3311(3) -0.0608(3) 0.0214(6) Uani 1 1 d . . .
H9A H 0.4346 0.2610 -0.0925 0.026 Uiso 1 1 calc R . .
H9B H 0.3243 0.3474 -0.1259 0.026 Uiso 1 1 calc R . .
C10 C 0.4572(3) 0.4664(3) 0.0284(3) 0.0244(6) Uani 1 1 d . . .
H10A H 0.5172 0.4470 0.0866 0.029 Uiso 1 1 calc R . .
H10B H 0.3956 0.5314 0.0694 0.029 Uiso 1 1 calc R . .
C11 C 0.3470(3) 0.2303(3) 0.1180(3) 0.0216(6) Uani 1 1 d . . .
C12 C 0.2959(3) 0.2576(4) 0.2210(3) 0.0308(7) Uani 1 1 d . . .
H12 H 0.2125 0.2952 0.2305 0.037 Uiso 1 1 calc R . .
C13 C 0.3669(4) 0.2297(5) 0.3095(3) 0.0439(9) Uani 1 1 d . . .
H13 H 0.3312 0.2473 0.3783 0.053 Uiso 1 1 calc R . .
C14 C 0.4894(4) 0.1762(4) 0.2966(3) 0.0416(9) Uani 1 1 d . . .
H14 H 0.5380 0.1588 0.3572 0.050 Uiso 1 1 calc R . .
C15 C 0.5416(3) 0.1478(4) 0.1950(3) 0.0397(9) Uani 1 1 d . . .
H15 H 0.6250 0.1101 0.1863 0.048 Uiso 1 1 calc R . .
C16 C 0.4704(3) 0.1751(4) 0.1053(3) 0.0305(7) Uani 1 1 d . . .
H16 H 0.5061 0.1561 0.0364 0.037 Uiso 1 1 calc R . .
C17 C 0.1797(3) 0.0941(3) -0.1101(3) 0.0216(6) Uani 1 1 d . . .
C18 C 0.1415(4) -0.0124(4) -0.0799(3) 0.0345(8) Uani 1 1 d . . .
H18 H 0.1549 0.0033 -0.0006 0.041 Uiso 1 1 calc R . .
C19 C 0.0839(4) -0.1416(4) -0.1653(4) 0.0426(9) Uani 1 1 d . . .
H19 H 0.0594 -0.2134 -0.1439 0.051 Uiso 1 1 calc R . .
C20 C 0.0629(4) -0.1644(4) -0.2811(4) 0.0412(9) Uani 1 1 d . . .
H20 H 0.0228 -0.2516 -0.3391 0.049 Uiso 1 1 calc R . .
C21 C 0.1000(4) -0.0607(4) -0.3122(3) 0.0410(9) Uani 1 1 d . . .
H21 H 0.0865 -0.0773 -0.3918 0.049 Uiso 1 1 calc R . .
C22 C 0.1575(4) 0.0695(4) -0.2271(3) 0.0347(8) Uani 1 1 d . . .
H22 H 0.1814 0.1409 -0.2491 0.042 Uiso 1 1 calc R . .
C23 C 0.8330(6) 0.1613(9) 0.8075(6) 0.118(3) Uani 1 1 d . . .
H23A H 0.8798 0.0855 0.8152 0.141 Uiso 1 1 calc R . .
H23B H 0.9006 0.2438 0.8403 0.141 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'
Cl Cl 0.1484 0.1585 '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 172.37(3) . . ?
C1 S1 Au 101.31(11) . . ?
C17 P1 C11 104.73(14) . . ?
C17 P1 C9 105.29(14) . . ?
C11 P1 C9 106.88(13) . . ?
C17 P1 Au 114.04(9) . . ?
C11 P1 Au 109.05(10) . . ?
C9 P1 Au 116.04(10) . . ?
C1 O1 C8 116.0(3) . . ?
C1 N1 C2 120.3(3) . . ?
N1 C1 O1 120.3(3) . . ?
N1 C1 S1 126.7(3) . . ?
O1 C1 S1 113.0(2) . . ?
C7 C2 N1 120.1(3) . . ?
C7 C2 C3 118.8(3) . . ?
N1 C2 C3 120.9(3) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.1(4) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C2 C7 C6 120.1(4) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 112.4(2) . . ?
C10 C9 H9A 109.1 . . ?
P1 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
P1 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 C10 112.2(3) . 2_665 ?
C9 C10 H10A 109.2 . . ?
C10 C10 H10A 109.2 2_665 . ?
C9 C10 H10B 109.2 . . ?
C10 C10 H10B 109.2 2_665 . ?
H10A C10 H10B 107.9 . . ?
C16 C11 C12 119.1(3) . . ?
C16 C11 P1 121.3(2) . . ?
C12 C11 P1 119.6(2) . . ?
C13 C12 C11 120.6(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 120.0(3) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C22 C17 C18 118.7(3) . . ?
C22 C17 P1 120.8(2) . . ?
C18 C17 P1 120.5(2) . . ?
C17 C18 C19 120.8(3) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C20 C19 C18 119.8(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.2(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C20 C21 C22 120.4(4) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C17 C22 C21 120.1(3) . . ?
C17 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
Cl2 C23 Cl1 120.6(4) . . ?
Cl2 C23 H23A 107.2 . . ?
Cl1 C23 H23A 107.2 . . ?
Cl2 C23 H23B 107.2 . . ?
Cl1 C23 H23B 107.2 . . ?
H23A C23 H23B 106.8 . . ?
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 2.2601(8) . ?
Au S1 2.3137(8) . ?
Cl1 C23 1.694(7) . ?
Cl2 C23 1.659(6) . ?
S1 C1 1.759(3) . ?
P1 C17 1.816(3) . ?
P1 C11 1.813(3) . ?
P1 C9 1.816(3) . ?
O1 C1 1.357(4) . ?
O1 C8 1.436(4) . ?
N1 C1 1.264(4) . ?
N1 C2 1.416(4) . ?
C2 C7 1.372(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.374(5) . ?
C3 H3 0.9400 . ?
C4 C5 1.367(7) . ?
C4 H4 0.9400 . ?
C5 C6 1.376(7) . ?
C5 H5 0.9400 . ?
C6 C7 1.394(5) . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 C10 1.529(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C10 1.514(5) 2_665 ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C16 1.389(4) . ?
C11 C12 1.395(4) . ?
C12 C13 1.387(5) . ?
C12 H12 0.9400 . ?
C13 C14 1.373(5) . ?
C13 H13 0.9400 . ?
C14 C15 1.384(5) . ?
C14 H14 0.9400 . ?
C15 C16 1.396(5) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 C22 1.383(4) . ?
C17 C18 1.387(4) . ?
C18 C19 1.386(5) . ?
C18 H18 0.9400 . ?
C19 C20 1.373(6) . ?
C19 H19 0.9400 . ?
C20 C21 1.365(5) . ?
C20 H20 0.9400 . ?
C21 C22 1.392(5) . ?
C21 H21 0.9400 . ?
C22 H22 0.9400 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
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 38.4(3) . . . . ?
S1 Au P1 C17 90.5(2) . . . . ?
S1 Au P1 C11 -26.2(3) . . . . ?
S1 Au P1 C9 -146.9(2) . . . . ?
C2 N1 C1 O1 -176.9(3) . . . . ?
C2 N1 C1 S1 5.6(5) . . . . ?
C8 O1 C1 N1 2.8(5) . . . . ?
C8 O1 C1 S1 -179.3(3) . . . . ?
Au S1 C1 N1 -169.8(3) . . . . ?
Au S1 C1 O1 12.5(3) . . . . ?
C1 N1 C2 C7 -111.9(4) . . . . ?
C1 N1 C2 C3 74.2(5) . . . . ?
C7 C2 C3 C4 1.5(5) . . . . ?
N1 C2 C3 C4 175.6(3) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C5 C6 C7 -1.3(6) . . . . ?
N1 C2 C7 C6 -177.0(3) . . . . ?
C3 C2 C7 C6 -2.9(5) . . . . ?
C5 C6 C7 C2 2.8(6) . . . . ?
C17 P1 C9 C10 -172.1(2) . . . . ?
C11 P1 C9 C10 -61.0(2) . . . . ?
Au P1 C9 C10 60.8(2) . . . . ?
P1 C9 C10 C10 -170.8(3) . . . 2_665 ?
C17 P1 C11 C16 72.8(3) . . . . ?
C9 P1 C11 C16 -38.6(3) . . . . ?
Au P1 C11 C16 -164.8(2) . . . . ?
C17 P1 C11 C12 -106.1(3) . . . . ?
C9 P1 C11 C12 142.5(3) . . . . ?
Au P1 C11 C12 16.3(3) . . . . ?
C16 C11 C12 C13 -0.2(5) . . . . ?
P1 C11 C12 C13 178.8(3) . . . . ?
C11 C12 C13 C14 0.8(6) . . . . ?
C12 C13 C14 C15 -1.1(6) . . . . ?
C13 C14 C15 C16 0.8(6) . . . . ?
C12 C11 C16 C15 -0.1(5) . . . . ?
P1 C11 C16 C15 -179.0(3) . . . . ?
C14 C15 C16 C11 -0.2(6) . . . . ?
C11 P1 C17 C22 -148.9(3) . . . . ?
C9 P1 C17 C22 -36.3(3) . . . . ?
Au P1 C17 C22 92.0(3) . . . . ?
C11 P1 C17 C18 34.0(3) . . . . ?
C9 P1 C17 C18 146.5(3) . . . . ?
Au P1 C17 C18 -85.1(3) . . . . ?
C22 C17 C18 C19 0.9(5) . . . . ?
P1 C17 C18 C19 178.1(3) . . . . ?
C17 C18 C19 C20 -0.7(6) . . . . ?
C18 C19 C20 C21 0.8(6) . . . . ?
C19 C20 C21 C22 -0.9(6) . . . . ?
C18 C17 C22 C21 -1.0(5) . . . . ?
P1 C17 C22 C21 -178.2(3) . . . . ?
C20 C21 C22 C17 1.1(6) . . . . ?
