#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/55/7015582.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_7015582
loop_
_publ_author_name
'Oliver, Katie'
'White, Andrew J. P.'
'Hogarth, Graeme'
'Wilton-Ely, James D E T'
_publ_section_title
;
 Multimetallic complexes of group 10 and 11 metals based on polydentate
 dithiocarbamate ligands.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5852
_journal_page_last               5864
_journal_paper_doi               10.1039/c0dt01745k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety
'C54 H48 Au2 N2 P2 S4, 2(C H2 Cl2), 0.5(C2 H6 O)'
_chemical_formula_sum            'C57 H55 Au2 Cl4 N2 O0.5 P2 S4'
_chemical_formula_weight         1501.94
_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                93.738(2)
_cell_angle_beta                 105.979(3)
_cell_angle_gamma                102.402(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0346(3)
_cell_length_b                   12.1805(3)
_cell_length_c                   14.0257(4)
_cell_measurement_reflns_used    8716
_cell_measurement_temperature    173
_cell_measurement_theta_max      32.6893
_cell_measurement_theta_min      3.0413
_cell_volume                     1436.45(8)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 15.9825
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16291
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.75
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.528
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             735
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.746
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0344
_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)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                7186
_reflns_number_total             9388
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01745k.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C57 H55 Au2 Cl4 N2 O0.50 P2 S4'
_cod_database_code               7015582
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
Au1 Au 0.446864(18) 0.912377(13) 0.340038(13) 0.02586(5) Uani 1 1 d . . .
S1 S 0.62133(11) 0.85520(7) 0.47189(7) 0.02345(19) Uani 1 1 d . . .
C2 C 0.5523(4) 0.7090(3) 0.4350(3) 0.0224(7) Uani 1 1 d . . .
S3 S 0.40196(13) 0.65382(9) 0.32894(8) 0.0332(2) Uani 1 1 d . . .
N4 N 0.6251(4) 0.6425(2) 0.4946(2) 0.0234(7) Uani 1 1 d . . .
C5 C 0.5664(5) 0.5179(3) 0.4752(3) 0.0274(8) Uani 1 1 d . . .
H5A H 0.6543 0.4817 0.5030 0.033 Uiso 1 1 calc R . .
H5B H 0.5245 0.4930 0.4022 0.033 Uiso 1 1 calc R . .
C6 C 0.7563(4) 0.6877(3) 0.5862(3) 0.0238(8) Uani 1 1 d . . .
H6A H 0.7615 0.6287 0.6316 0.029 Uiso 1 1 calc R . .
H6B H 0.7340 0.7531 0.6205 0.029 Uiso 1 1 calc R . .
C7 C 0.9161(4) 0.7251(3) 0.5682(3) 0.0239(8) Uani 1 1 d . . .
C8 C 1.0178(5) 0.8266(4) 0.6186(4) 0.0344(10) Uani 1 1 d . . .
H8A H 0.9856 0.8728 0.6625 0.041 Uiso 1 1 calc R . .
C9 C 1.1679(5) 0.8614(4) 0.6053(4) 0.0436(12) Uani 1 1 d . . .
H9A H 1.2375 0.9310 0.6405 0.052 Uiso 1 1 calc R . .
C10 C 1.2154(5) 0.7961(4) 0.5417(4) 0.0404(11) Uani 1 1 d . . .
H10A H 1.3172 0.8200 0.5326 0.049 Uiso 1 1 calc R . .
C11 C 1.1157(5) 0.6973(4) 0.4922(4) 0.0415(11) Uani 1 1 d . . .
H11A H 1.1491 0.6516 0.4486 0.050 Uiso 1 1 calc R . .
C12 C 0.9632(5) 0.6601(4) 0.5035(4) 0.0352(10) Uani 1 1 d . . .
H12A H 0.8939 0.5910 0.4670 0.042 Uiso 1 1 calc R . .
P13 P 0.27302(12) 0.96086(8) 0.21122(8) 0.0242(2) Uani 1 1 d . . .
C14 C 0.2857(5) 0.9041(4) 0.0913(3) 0.0292(8) Uani 1 1 d . . .
C15 C 0.2943(7) 0.7918(4) 0.0783(4) 0.0503(13) Uani 1 1 d . . .
H15A H 0.3004 0.7481 0.1322 0.060 Uiso 1 1 calc R . .
C16 C 0.2940(9) 0.7440(5) -0.0152(5) 0.073(2) Uani 1 1 d . . .
H16A H 0.2941 0.6661 -0.0253 0.088 Uiso 1 1 calc R . .
C17 C 0.2935(6) 0.8066(5) -0.0918(4) 0.0490(13) Uani 1 1 d . . .
H17A H 0.2965 0.7736 -0.1542 0.059 Uiso 1 1 calc R . .
C18 C 0.2886(6) 0.9180(5) -0.0779(4) 0.0451(12) Uani 1 1 d . . .
H18A H 0.2880 0.9623 -0.1312 0.054 Uiso 1 1 calc R . .
C19 C 0.2843(5) 0.9668(4) 0.0133(3) 0.0355(10) Uani 1 1 d . . .
H19A H 0.2805 1.0441 0.0218 0.043 Uiso 1 1 calc R . .
C20 C 0.0707(5) 0.9003(3) 0.2128(3) 0.0270(8) Uani 1 1 d . . .
C21 C -0.0518(5) 0.8518(4) 0.1265(3) 0.0353(10) Uani 1 1 d . . .
H21A H -0.0319 0.8479 0.0635 0.042 Uiso 1 1 calc R . .
C22 C -0.2041(5) 0.8090(4) 0.1330(4) 0.0408(11) Uani 1 1 d . . .
H22A H -0.2888 0.7763 0.0743 0.049 Uiso 1 1 calc R . .
C23 C -0.2318(6) 0.8143(4) 0.2257(4) 0.0452(12) Uani 1 1 d . . .
H23A H -0.3358 0.7862 0.2302 0.054 Uiso 1 1 calc R . .
C24 C -0.1104(6) 0.8594(4) 0.3097(4) 0.0437(12) Uani 1 1 d . . .
H24A H -0.1302 0.8615 0.3728 0.052 Uiso 1 1 calc R . .
C25 C 0.0415(5) 0.9025(4) 0.3050(3) 0.0344(9) Uani 1 1 d . . .
H25A H 0.1256 0.9334 0.3645 0.041 Uiso 1 1 calc R . .
C26 C 0.2860(5) 1.1109(3) 0.2042(3) 0.0263(8) Uani 1 1 d . . .
C27 C 0.1525(5) 1.1503(4) 0.1589(3) 0.0329(9) Uani 1 1 d . . .
H27A H 0.0508 1.0991 0.1357 0.040 Uiso 1 1 calc R . .
C28 C 0.1690(6) 1.2640(4) 0.1480(4) 0.0415(11) Uani 1 1 d . . .
H28A H 0.0787 1.2909 0.1165 0.050 Uiso 1 1 calc R . .
C29 C 0.3180(7) 1.3390(4) 0.1832(4) 0.0484(14) Uani 1 1 d . . .
H29A H 0.3293 1.4171 0.1759 0.058 Uiso 1 1 calc R . .
C30 C 0.4468(6) 1.3009(4) 0.2279(4) 0.0424(12) Uani 1 1 d . . .
H30A H 0.5479 1.3529 0.2514 0.051 Uiso 1 1 calc R . .
C31 C 0.4343(5) 1.1869(4) 0.2401(3) 0.0343(9) Uani 1 1 d . . .
H31A H 0.5255 1.1615 0.2725 0.041 Uiso 1 1 calc R . .
C40 C 0.9654(9) 0.5816(5) 0.2206(5) 0.0544(17) Uani 0.875(4) 1 d PDU A 1
H40A H 0.8743 0.6169 0.2111 0.065 Uiso 0.875(4) 1 calc PR A 1
H40B H 1.0607 0.6367 0.2648 0.065 Uiso 0.875(4) 1 calc PR A 1
Cl1 Cl 0.9944(4) 0.55108(19) 0.10656(18) 0.0856(8) Uani 0.875(4) 1 d PDU A 1
Cl2 Cl 0.9286(2) 0.45868(13) 0.27756(14) 0.0640(6) Uani 0.875(4) 1 d PDU A 1
C40' C 0.961(4) 0.527(5) 0.207(2) 0.062(6) Uiso 0.125(4) 1 d PDU A 2
H40C H 1.0435 0.5926 0.2485 0.075 Uiso 0.125(4) 1 calc PR A 2
H40D H 1.0051 0.4597 0.2088 0.075 Uiso 0.125(4) 1 calc PR A 2
Cl1' Cl 0.898(3) 0.5557(17) 0.0849(13) 0.089(4) Uiso 0.125(4) 1 d PDU A 2
Cl2' Cl 0.795(2) 0.5028(16) 0.2503(14) 0.103(4) Uiso 0.125(4) 1 d PDU A 2
O50 O 0.576(4) 0.550(2) 0.162(2) 0.134(10) Uiso 0.25 1 d P B -1
C51 C 0.469(5) 0.572(3) 0.076(3) 0.111(12) Uiso 0.25 1 d P B -1
H51A H 0.4938 0.6517 0.0631 0.133 Uiso 0.25 1 calc PR B -1
H51B H 0.3563 0.5466 0.0745 0.133 Uiso 0.25 1 calc PR B -1
C52 C 0.522(9) 0.488(7) 0.008(6) 0.132(15) Uiso 0.25 1 d P B -1
H52A H 0.4578 0.4823 -0.0622 0.198 Uiso 0.25 1 calc PR B -1
H52B H 0.5060 0.4128 0.0297 0.198 Uiso 0.25 1 calc PR B -1
H52C H 0.6341 0.5171 0.0133 0.198 Uiso 0.25 1 calc PR B -1
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'
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'
Cl Cl 0.1484 0.1585 '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'
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
P13 Au1 S1 177.86(3) . . ?
P13 Au1 S3 111.96(3) . . ?
S1 Au1 S3 65.96(3) . . ?
C2 S1 Au1 97.67(14) . . ?
N4 C2 S3 121.6(3) . . ?
N4 C2 S1 116.6(3) . . ?
S3 C2 S1 121.8(2) . . ?
C2 S3 Au1 74.60(13) . . ?
C2 N4 C6 122.9(3) . . ?
C2 N4 C5 120.8(3) . . ?
C6 N4 C5 116.1(3) . . ?
N4 C5 C5 108.9(4) . 2_666 ?
N4 C6 C7 113.8(3) . . ?
C12 C7 C8 119.3(4) . . ?
C12 C7 C6 121.5(4) . . ?
C8 C7 C6 119.2(4) . . ?
C7 C8 C9 120.2(4) . . ?
C10 C9 C8 120.5(4) . . ?
C11 C10 C9 119.2(4) . . ?
C10 C11 C12 121.6(5) . . ?
C7 C12 C11 119.1(4) . . ?
C26 P13 C14 105.04(19) . . ?
C26 P13 C20 105.52(18) . . ?
C14 P13 C20 106.03(19) . . ?
C26 P13 Au1 117.87(14) . . ?
C14 P13 Au1 111.76(14) . . ?
C20 P13 Au1 109.81(13) . . ?
C19 C14 C15 119.1(4) . . ?
C19 C14 P13 122.8(3) . . ?
C15 C14 P13 118.1(4) . . ?
C14 C15 C16 119.3(5) . . ?
C17 C16 C15 121.3(6) . . ?
C16 C17 C18 119.2(5) . . ?
C17 C18 C19 120.7(5) . . ?
C14 C19 C18 120.4(5) . . ?
C21 C20 C25 119.8(4) . . ?
C21 C20 P13 122.6(3) . . ?
C25 C20 P13 117.6(3) . . ?
C20 C21 C22 119.6(4) . . ?
C23 C22 C21 119.8(5) . . ?
C24 C23 C22 120.1(4) . . ?
C23 C24 C25 121.1(5) . . ?
C24 C25 C20 119.6(5) . . ?
C31 C26 C27 119.7(4) . . ?
C31 C26 P13 118.7(3) . . ?
C27 C26 P13 121.5(3) . . ?
C28 C27 C26 119.9(4) . . ?
C27 C28 C29 119.9(5) . . ?
C30 C29 C28 120.2(4) . . ?
C29 C30 C31 121.4(5) . . ?
C26 C31 C30 119.0(4) . . ?
Cl1 C40 Cl2 111.2(4) . . ?
Cl1' C40' Cl2' 107.2(15) . . ?
O50 C51 C52 90(4) . . ?
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
Au1 P13 2.2483(10) . ?
Au1 S1 2.3290(10) . ?
Au1 S3 3.0756(10) . ?
S1 C2 1.747(4) . ?
C2 N4 1.343(5) . ?
C2 S3 1.695(4) . ?
N4 C6 1.465(5) . ?
N4 C5 1.476(5) . ?
C5 C5 1.545(8) 2_666 ?
C6 C7 1.513(5) . ?
C7 C12 1.377(6) . ?
C7 C8 1.383(6) . ?
C8 C9 1.399(6) . ?
C9 C10 1.370(7) . ?
C10 C11 1.351(7) . ?
C11 C12 1.411(6) . ?
P13 C26 1.817(4) . ?
P13 C14 1.819(4) . ?
P13 C20 1.826(4) . ?
C14 C19 1.373(6) . ?
C14 C15 1.390(6) . ?
C15 C16 1.398(8) . ?
C16 C17 1.357(8) . ?
C17 C18 1.370(8) . ?
C18 C19 1.389(7) . ?
C20 C21 1.387(6) . ?
C20 C25 1.388(6) . ?
C21 C22 1.394(6) . ?
C22 C23 1.389(7) . ?
C23 C24 1.356(8) . ?
C24 C25 1.382(7) . ?
C26 C31 1.393(6) . ?
C26 C27 1.398(6) . ?
C27 C28 1.385(6) . ?
C28 C29 1.392(7) . ?
C29 C30 1.353(8) . ?
C30 C31 1.394(6) . ?
C40 Cl1 1.720(7) . ?
C40 Cl2 1.755(6) . ?
C40' Cl1' 1.726(17) . ?
C40' Cl2' 1.741(17) . ?
O50 C51 1.40(5) . ?
C51 C52 1.59(9) . ?
