#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:25:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179919 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/14/7021490.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_7021490
loop_
_publ_author_name
'Upmann, Daniel'
'Jones, Peter G.'
_publ_section_title
;
 Synthesis and X-ray structural characterization of the
 (chlorochalcogeno)phosphonium cations R2R'PSCl(+) and R2R'PSeCl(+) as
 their AuCl4(-) salts.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7526
_journal_page_last               7528
_journal_paper_doi               10.1039/c3dt50777g
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C11 H25 Au Cl3 P S'
_chemical_formula_weight         523.66
_chemical_name_systematic
;
?
;
_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                78.876(3)
_cell_angle_beta                 71.456(4)
_cell_angle_gamma                72.702(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6034(4)
_cell_length_b                   9.7779(4)
_cell_length_c                   11.4231(4)
_cell_measurement_reflns_used    31596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7543
_cell_measurement_theta_min      2.1901
_cell_volume                     864.70(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scan'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0166
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            68815
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.82
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    9.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.560
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0158
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0168P)²+0.7671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0360
_reflns_number_gt                4939
_reflns_number_total             5155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50777g.txt
_cod_data_source_block           eing
_cod_original_cell_volume        864.69(6)
_cod_database_code               7021490
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
Au1 Au 0.964760(9) 0.850143(7) 0.740716(6) 0.01311(3) Uani 1 1 d .
Cl1 Cl 1.23243(7) 0.87150(6) 0.71221(5) 0.02010(10) Uani 1 1 d .
Cl2 Cl 1.03637(8) 0.62179(5) 0.84126(5) 0.02352(11) Uani 1 1 d .
Cl3 Cl 0.70542(7) 0.81734(5) 0.75814(5) 0.02176(10) Uani 1 1 d .
S1 S 0.90625(6) 1.08036(5) 0.63464(4) 0.01338(9) Uani 1 1 d .
P1 P 0.71575(6) 1.22282(5) 0.74712(4) 0.00948(8) Uani 1 1 d .
C1 C 0.7568(2) 1.2093(2) 0.90129(16) 0.0120(3) Uani 1 1 d .
C2 C 0.7277(3) 1.3996(2) 0.65054(17) 0.0128(3) Uani 1 1 d .
C3 C 0.5119(2) 1.1799(2) 0.77290(18) 0.0143(4) Uani 1 1 d .
H3 H 0.5285 1.0777 0.8116 0.017 Uiso 1 1 calc R
C11 C 0.7023(3) 1.0771(2) 0.98235(17) 0.0154(4) Uani 1 1 d .
H11A H 0.7616 0.9913 0.9385 0.023 Uiso 1 1 calc R
H11B H 0.5797 1.0924 0.9991 0.023 Uiso 1 1 calc R
H11C H 0.7309 1.0635 1.0610 0.023 Uiso 1 1 calc R
C12 C 0.9458(2) 1.1884(2) 0.88626(18) 0.0159(4) Uani 1 1 d .
H12A H 0.9649 1.1743 0.9684 0.024 Uiso 1 1 calc R
H12B H 0.9814 1.2739 0.8385 0.024 Uiso 1 1 calc R
H12C H 1.0118 1.1036 0.8423 0.024 Uiso 1 1 calc R
C13 C 0.6566(3) 1.3445(2) 0.96903(18) 0.0165(4) Uani 1 1 d .
H13A H 0.6755 1.3304 1.0512 0.025 Uiso 1 1 calc R
H13B H 0.5355 1.3606 0.9784 0.025 Uiso 1 1 calc R
H13C H 0.6953 1.4284 0.9205 0.025 Uiso 1 1 calc R
C21 C 0.8769(3) 1.4485(2) 0.65963(19) 0.0178(4) Uani 1 1 d .
H21A H 0.9819 1.3731 0.6353 0.027 Uiso 1 1 calc R
H21B H 0.8575 1.4663 0.7453 0.027 Uiso 1 1 calc R
H21C H 0.8864 1.5373 0.6041 0.027 Uiso 1 1 calc R
C22 C 0.5615(3) 1.5154(2) 0.69360(19) 0.0171(4) Uani 1 1 d .
H22A H 0.5739 1.6092 0.6482 0.026 Uiso 1 1 calc R
H22B H 0.5362 1.5203 0.7828 0.026 Uiso 1 1 calc R
H22C H 0.4688 1.4904 0.6772 0.026 Uiso 1 1 calc R
C23 C 0.7572(3) 1.3834(2) 0.51298(18) 0.0186(4) Uani 1 1 d .
H23A H 0.7493 1.4783 0.4645 0.028 Uiso 1 1 calc R
H23B H 0.6711 1.3413 0.5056 0.028 Uiso 1 1 calc R
H23C H 0.8701 1.3203 0.4813 0.028 Uiso 1 1 calc R
C31 C 0.4719(3) 1.1790(2) 0.6513(2) 0.0230(4) Uani 1 1 d .
H31A H 0.3837 1.1278 0.6681 0.035 Uiso 1 1 calc R
H31B H 0.5746 1.1302 0.5920 0.035 Uiso 1 1 calc R
H31C H 0.4320 1.2784 0.6163 0.035 Uiso 1 1 calc R
C32 C 0.3569(3) 1.2650(2) 0.8650(2) 0.0203(4) Uani 1 1 d .
H32A H 0.3337 1.3673 0.8332 0.031 Uiso 1 1 calc R
H32B H 0.3800 1.2531 0.9455 0.031 Uiso 1 1 calc R
H32C H 0.2582 1.2288 0.8750 0.031 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'
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'
Au Au -2.0133 8.8022 '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
Cl1 Au1 Cl3 175.765(18)
Cl1 Au1 Cl2 89.44(2)
Cl3 Au1 Cl2 89.35(2)
Cl1 Au1 S1 87.963(19)
Cl3 Au1 S1 93.176(19)
Cl2 Au1 S1 177.233(19)
P1 S1 Au1 111.35(2)
C3 P1 C2 112.67(9)
C3 P1 C1 108.88(9)
C2 P1 C1 113.60(8)
C3 P1 S1 109.17(7)
C2 P1 S1 101.47(6)
C1 P1 S1 110.81(6)
C12 C1 C11 108.33(16)
C12 C1 C13 108.22(16)
C11 C1 C13 108.84(15)
C12 C1 P1 111.17(13)
C11 C1 P1 108.08(13)
C13 C1 P1 112.11(13)
C21 C2 C22 109.54(16)
C21 C2 C23 107.67(16)
C22 C2 C23 108.82(16)
C21 C2 P1 110.44(13)
C22 C2 P1 110.44(13)
C23 C2 P1 109.86(13)
C31 C3 C32 110.93(17)
C31 C3 P1 112.86(14)
C32 C3 P1 116.89(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au1 Cl1 2.2881(5)
Au1 Cl3 2.2889(5)
Au1 Cl2 2.3080(5)
Au1 S1 2.3346(5)
S1 P1 2.0666(7)
P1 C3 1.844(2)
P1 C2 1.8741(19)
P1 C1 1.8766(18)
C1 C12 1.534(3)
C1 C11 1.540(3)
C1 C13 1.543(3)
C2 C21 1.535(3)
C2 C22 1.541(3)
C2 C23 1.542(3)
C3 C31 1.535(3)
C3 C32 1.537(3)
