# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_t63
_database_code_depnum_ccdc_archive 'CCDC 1429227'
_audit_update_record             
;
2015-10-02 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;

_audit_creation_date             2015-10-02T10:33:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            DP172
_chemical_formula_moiety         'C6 H18 Au P2, C36 Au F24 Hg5'
_chemical_formula_sum            'C42 H18 Au2 F24 Hg5 P2'
_chemical_formula_weight         2437.39
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.8022(12)
_cell_length_b                   16.7195(9)
_cell_length_c                   13.2363(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.232(3)
_cell_angle_gamma                90
_cell_volume                     4792.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4241
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      27.45
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    3.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4296
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    22.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  1.54
_exptl_absorpt_correction_T_max  27.45

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.404529E-1
_diffrn_orient_matrix_ub_12      -0.287219E-1
_diffrn_orient_matrix_ub_13      -0.185721E-1
_diffrn_orient_matrix_ub_21      0.213838E-1
_diffrn_orient_matrix_ub_22      -0.516118E-1
_diffrn_orient_matrix_ub_23      -0.37505E-2
_diffrn_orient_matrix_ub_31      0.61874E-2
_diffrn_orient_matrix_ub_32      -0.94105E-2
_diffrn_orient_matrix_ub_33      0.772536E-1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_number            36348
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             5469
_reflns_number_gt                4583
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+981.0213P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5469
_refine_ls_number_parameters     330
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0859
_refine_ls_wR_factor_ref         0.1977
_refine_ls_wR_factor_gt          0.1928
_refine_ls_goodness_of_fit_ref   1.403
_refine_ls_restrained_S_all      1.39
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.414
_refine_diff_density_min         -3.535
_refine_diff_density_rms         0.442

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 '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'

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
Hg1 Hg 0.11993(4) 0.98248(6) 0.12850(8) 0.0290(2) Uani 1 1 d . . .
Hg2 Hg 0.01347(5) 0.82458(7) 0.12287(8) 0.0312(2) Uani 1 1 d . . .
Hg3 Hg -0.03346(5) 1.02771(7) 0.12859(8) 0.0362(3) Uani 0.5 1 d P . 1
Au3 Au -0.03346(5) 1.02771(7) 0.12859(8) 0.0362(3) Uani 0.5 1 d P . 2
Au1 Au 0.5 0.00617(9) 0.25 0.0366(4) Uani 1 2 d S . .
P P 0.4033(3) -0.0042(4) 0.1270(6) 0.0343(16) Uani 1 1 d . . .
C1 C 0.1440(11) 0.8608(18) 0.126(2) 0.032(5) Uani 1 1 d U . .
C2 C 0.2044(12) 0.8457(15) 0.1247(19) 0.027(4) Uani 1 1 d U . .
C3 C 0.2228(13) 0.7666(18) 0.131(2) 0.040(6) Uani 1 1 d U . .
C4 C 0.1838(12) 0.7038(16) 0.129(2) 0.031(5) Uani 1 1 d U . .
C5 C 0.1220(12) 0.7211(18) 0.130(2) 0.033(5) Uani 1 1 d U . .
C6 C 0.1028(13) 0.8029(17) 0.1243(19) 0.031(5) Uani 1 1 d U . .
F1 F 0.2446(7) 0.9023(10) 0.1245(14) 0.043(4) Uani 1 1 d U . .
F2 F 0.2812(7) 0.7457(10) 0.1284(14) 0.040(4) Uani 1 1 d U . .
F3 F 0.2024(8) 0.6272(10) 0.1367(14) 0.047(4) Uani 1 1 d U . .
F4 F 0.0845(8) 0.6603(11) 0.1294(14) 0.046(4) Uani 1 1 d U . .
C11 C -0.0773(12) 0.8491(17) 0.124(2) 0.037(6) Uani 1 1 d U . .
C12 C -0.1185(13) 0.7937(19) 0.113(3) 0.045(7) Uani 1 1 d U . .
C13 C -0.1786(12) 0.8068(18) 0.108(2) 0.034(5) Uani 1 1 d U . .
C14 C -0.1964(12) 0.8855(19) 0.103(2) 0.039(5) Uani 1 1 d U . .
C15 C -0.1568(12) 0.9464(18) 0.1108(19) 0.032(4) Uani 1 1 d U . .
C16 C -0.0943(11) 0.9346(17) 0.1218(19) 0.029(5) Uani 1 1 d U . .
F5 F -0.0999(8) 0.7161(11) 0.1167(14) 0.047(4) Uani 1 1 d U . .
F6 F -0.2177(7) 0.7500(11) 0.1074(13) 0.044(4) Uani 1 1 d U . .
F7 F -0.2552(7) 0.8997(11) 0.1020(15) 0.048(4) Uani 1 1 d U . .
F8 F -0.1795(8) 1.0201(12) 0.1075(15) 0.052(4) Uani 1 1 d U . .
C21 C 0.0310(11) 1.1139(15) 0.1323(19) 0.027(4) Uani 1 1 d U . .
C22 C 0.0133(12) 1.1917(15) 0.132(2) 0.030(4) Uani 1 1 d U . .
C23 C 0.0544(12) 1.2588(15) 0.1356(19) 0.029(4) Uani 1 1 d U . .
C24 C 0.1147(12) 1.2397(16) 0.144(2) 0.030(4) Uani 1 1 d U . .
C25 C 0.1328(12) 1.1616(16) 0.145(2) 0.032(5) Uani 1 1 d U . .
C26 C 0.0914(12) 1.1015(16) 0.138(2) 0.030(4) Uani 1 1 d U . .
F9 F -0.0442(7) 1.2165(9) 0.1268(13) 0.037(4) Uani 1 1 d U . .
F10 F 0.0363(8) 1.3359(9) 0.1356(13) 0.041(4) Uani 1 1 d U . .
F11 F 0.1550(8) 1.3005(10) 0.1490(13) 0.040(4) Uani 1 1 d U . .
F12 F 0.1922(7) 1.1449(10) 0.1508(13) 0.039(4) Uani 1 1 d U . .
C31 C 0.3817(14) -0.1078(16) 0.112(3) 0.042(4) Uani 1 1 d . . .
H31A H 0.3409 -0.1129 0.063 0.063 Uiso 1 1 calc R . .
H31B H 0.3824 -0.1291 0.1802 0.063 Uiso 1 1 calc R . .
H31C H 0.4103 -0.1369 0.0864 0.063 Uiso 1 1 calc R . .
C32 C 0.3408(14) 0.0467(17) 0.155(3) 0.042(4) Uani 1 1 d . . .
H32A H 0.3449 0.1033 0.1469 0.063 Uiso 1 1 calc R . .
H32B H 0.3418 0.0352 0.2265 0.063 Uiso 1 1 calc R . .
H32C H 0.3023 0.0289 0.1063 0.063 Uiso 1 1 calc R . .
C33 C 0.3982(14) 0.0266(17) -0.003(2) 0.042(4) Uani 1 1 d . . .
H33A H 0.4152 -0.0141 -0.0363 0.063 Uiso 1 1 calc R . .
H33B H 0.421 0.0754 0.0008 0.063 Uiso 1 1 calc R . .
H33C H 0.3557 0.0354 -0.0429 0.063 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
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
Hg1 C26 2.11(3) . ?
Hg1 C1 2.11(3) . ?
Hg1 Au3 3.3613(14) 5_575 ?
Hg1 Hg3 3.3613(14) 5_575 ?
Hg2 C6 2.06(3) . ?
Hg2 C11 2.12(3) . ?
Hg3 C21 2.05(3) . ?
Hg3 C16 2.07(3) . ?
Hg3 Hg3 3.097(2) 2 ?
Hg3 Hg1 3.3613(14) 5_575 ?
Au1 P 2.302(7) . ?
Au1 P 2.302(7) 2_655 ?
P C33 1.76(3) . ?
P C32 1.79(3) . ?
P C31 1.79(3) . ?
C1 C6 1.35(4) . ?
C1 C2 1.40(4) . ?
C2 F1 1.32(3) . ?
C2 C3 1.38(4) . ?
C3 C4 1.37(4) . ?
C3 F2 1.39(3) . ?
C4 F3 1.34(3) . ?
C4 C5 1.44(4) . ?
C5 F4 1.33(3) . ?
C5 C6 1.43(4) . ?
C11 C12 1.30(4) . ?
C11 C16 1.48(4) . ?
C12 F5 1.36(4) . ?
C12 C13 1.37(4) . ?
C13 F6 1.30(3) . ?
C13 C14 1.37(4) . ?
C14 C15 1.34(4) . ?
C14 F7 1.36(3) . ?
C15 F8 1.33(3) . ?
C15 C16 1.40(3) . ?
C21 C22 1.36(3) . ?
C21 C26 1.37(4) . ?
C22 F9 1.36(3) . ?
C22 C23 1.45(4) . ?
C23 F10 1.35(3) . ?
C23 C24 1.38(4) . ?
C24 F11 1.36(3) . ?
C24 C25 1.37(4) . ?
C25 F12 1.36(3) . ?
C25 C26 1.36(4) . ?
C31 H31A 0.96 . ?
C31 H31B 0.96 . ?
C31 H31C 0.96 . ?
C32 H32A 0.96 . ?
C32 H32B 0.96 . ?
C32 H32C 0.96 . ?
C33 H33A 0.96 . ?
C33 H33B 0.96 . ?
C33 H33C 0.96 . ?

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
C26 Hg1 C1 175.7(11) . . ?
C26 Hg1 Au3 90.8(7) . 5_575 ?
C1 Hg1 Au3 90.4(6) . 5_575 ?
C26 Hg1 Hg3 90.8(7) . 5_575 ?
C1 Hg1 Hg3 90.4(6) . 5_575 ?
Au3 Hg1 Hg3 0.00(6) 5_575 5_575 ?
C6 Hg2 C11 178.5(12) . . ?
C21 Hg3 C16 175.7(11) . . ?
C21 Hg3 Hg3 81.8(7) . 2 ?
C16 Hg3 Hg3 98.7(6) . 2 ?
C21 Hg3 Hg1 104.4(6) . 5_575 ?
C16 Hg3 Hg1 75.2(6) . 5_575 ?
Hg3 Hg3 Hg1 173.33(5) 2 5_575 ?
P Au1 P 171.4(4) . 2_655 ?
C33 P C32 104.4(14) . . ?
C33 P C31 104.2(15) . . ?
C32 P C31 105.8(14) . . ?
C33 P Au1 115.0(11) . . ?
C32 P Au1 117.7(11) . . ?
C31 P Au1 108.5(11) . . ?
C6 C1 C2 124(3) . . ?
C6 C1 Hg1 121(2) . . ?
C2 C1 Hg1 115.8(19) . . ?
F1 C2 C3 119(2) . . ?
F1 C2 C1 124(2) . . ?
C3 C2 C1 117(3) . . ?
C4 C3 C2 123(3) . . ?
C4 C3 F2 115(2) . . ?
C2 C3 F2 121(3) . . ?
F3 C4 C3 123(2) . . ?
F3 C4 C5 119(2) . . ?
C3 C4 C5 118(2) . . ?
F4 C5 C6 123(2) . . ?
F4 C5 C4 118(2) . . ?
C6 C5 C4 118(3) . . ?
C1 C6 C5 119(3) . . ?
C1 C6 Hg2 124(2) . . ?
C5 C6 Hg2 117(2) . . ?
C12 C11 C16 121(3) . . ?
C12 C11 Hg2 123(2) . . ?
C16 C11 Hg2 116.0(18) . . ?
C11 C12 F5 118(3) . . ?
C11 C12 C13 125(3) . . ?
F5 C12 C13 117(3) . . ?
F6 C13 C12 124(3) . . ?
F6 C13 C14 121(3) . . ?
C12 C13 C14 115(3) . . ?
C15 C14 F7 120(3) . . ?
C15 C14 C13 123(3) . . ?
F7 C14 C13 116(2) . . ?
F8 C15 C14 117(2) . . ?
F8 C15 C16 120(2) . . ?
C14 C15 C16 123(3) . . ?
C15 C16 C11 113(2) . . ?
C15 C16 Hg3 123(2) . . ?
C11 C16 Hg3 123.9(18) . . ?
C22 C21 C26 116(2) . . ?
C22 C21 Hg3 117.5(19) . . ?
C26 C21 Hg3 126.6(19) . . ?
F9 C22 C21 125(2) . . ?
F9 C22 C23 112(2) . . ?
C21 C22 C23 123(3) . . ?
F10 C23 C24 121(2) . . ?
F10 C23 C22 123(2) . . ?
C24 C23 C22 116(2) . . ?
F11 C24 C25 121(2) . . ?
F11 C24 C23 118(2) . . ?
C25 C24 C23 121(2) . . ?
F12 C25 C26 121(2) . . ?
F12 C25 C24 119(2) . . ?
C26 C25 C24 120(3) . . ?
C25 C26 C21 124(3) . . ?
C25 C26 Hg1 119(2) . . ?
C21 C26 Hg1 117.5(19) . . ?
P C31 H31A 109.5 . . ?
P C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
P C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
P C32 H32A 109.5 . . ?
P C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P C33 H33A 109.5 . . ?
P C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
P C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
