#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:25:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179919 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/14/7021493.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_7021493
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            'C10 H23 Au Cl3 P Se'
_chemical_formula_weight         556.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.285(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9388(2)
_cell_length_b                   14.5821(3)
_cell_length_c                   14.3875(4)
_cell_measurement_reflns_used    29528
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8049
_cell_measurement_theta_min      2.5654
_cell_volume                     1665.14(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5908
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    11.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24584
_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    2.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.233
_refine_diff_density_min         -2.063
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0439
_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)+(0.0351P)²+10.4358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                4433
_reflns_number_total             5925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50777g.txt
_cod_data_source_block           sandra2_hklf5
_cod_original_cell_volume        1665.16(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7021493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.04080(3) 0.066206(16) 0.184109(18) 0.01808(8) Uani 1 1 d .
Cl1 Cl 0.3261(2) 0.08727(12) 0.18017(13) 0.0299(4) Uani 1 1 d .
Cl2 Cl 0.0688(2) 0.01284(12) 0.33642(12) 0.0286(4) Uani 1 1 d .
Cl3 Cl -0.24127(19) 0.03578(11) 0.18382(12) 0.0246(3) Uani 1 1 d .
Se1 Se 0.02969(8) 0.12096(4) 0.02360(5) 0.02006(14) Uani 1 1 d .
P1 P -0.14953(19) 0.23730(10) 0.01490(11) 0.0150(3) Uani 1 1 d .
C1 C -0.1074(9) 0.3271(4) 0.1053(5) 0.0243(15) Uani 1 1 d .
C2 C -0.1089(8) 0.2816(4) -0.1032(4) 0.0206(13) Uani 1 1 d .
H2 H -0.1936 0.3306 -0.1178 0.025 Uiso 1 1 calc R
C3 C -0.3685(8) 0.1986(4) 0.0235(5) 0.0243(15) Uani 1 1 d .
H3 H -0.3833 0.1808 0.0899 0.029 Uiso 1 1 calc R
C11 C -0.1695(10) 0.4212(4) 0.0691(5) 0.0282(16) Uani 1 1 d .
H11A H -0.1511 0.4676 0.1175 0.042 Uiso 1 1 calc R
H11B H -0.2900 0.4175 0.0532 0.042 Uiso 1 1 calc R
H11C H -0.1069 0.4381 0.0138 0.042 Uiso 1 1 calc R
C12 C -0.2032(12) 0.3016(5) 0.1944(5) 0.041(2) Uani 1 1 d .
H12A H -0.1636 0.2419 0.2174 0.061 Uiso 1 1 calc R
H12B H -0.3243 0.2982 0.1799 0.061 Uiso 1 1 calc R
H12C H -0.1823 0.3484 0.2421 0.061 Uiso 1 1 calc R
C13 C 0.0802(11) 0.3335(5) 0.1298(6) 0.039(2) Uani 1 1 d .
H13A H 0.1426 0.3491 0.0740 0.058 Uiso 1 1 calc R
H13B H 0.1199 0.2744 0.1542 0.058 Uiso 1 1 calc R
H13C H 0.0987 0.3811 0.1770 0.058 Uiso 1 1 calc R
C21 C -0.1273(12) 0.2060(5) -0.1777(5) 0.041(2) Uani 1 1 d .
H21A H -0.0917 0.2300 -0.2378 0.061 Uiso 1 1 calc R
H21B H -0.2453 0.1866 -0.1827 0.061 Uiso 1 1 calc R
H21C H -0.0566 0.1535 -0.1601 0.061 Uiso 1 1 calc R
C22 C 0.0671(9) 0.3227(5) -0.1133(5) 0.0285(16) Uani 1 1 d .
H22A H 0.1520 0.2744 -0.1049 0.043 Uiso 1 1 calc R
H22B H 0.0854 0.3704 -0.0662 0.043 Uiso 1 1 calc R
H22C H 0.0768 0.3496 -0.1754 0.043 Uiso 1 1 calc R
C31 C -0.4126(10) 0.1136(6) -0.0339(5) 0.040(2) Uani 1 1 d .
H31A H -0.5139 0.0848 -0.0094 0.061 Uiso 1 1 calc R
H31B H -0.3186 0.0701 -0.0303 0.061 Uiso 1 1 calc R
H31C H -0.4335 0.1314 -0.0988 0.061 Uiso 1 1 calc R
C32 C -0.4990(10) 0.2758(6) 0.0032(8) 0.054(3) Uani 1 1 d .
H32A H -0.4885 0.2968 -0.0611 0.081 Uiso 1 1 calc R
H32B H -0.4780 0.3272 0.0457 0.081 Uiso 1 1 calc R
H32C H -0.6130 0.2520 0.0121 0.081 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
P P 0.1023 0.0942 '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
Cl3 Au1 Cl1 176.19(6)
Cl3 Au1 Cl2 90.55(6)
Cl1 Au1 Cl2 89.69(6)
Cl3 Au1 Se1 92.70(5)
Cl1 Au1 Se1 86.99(5)
Cl2 Au1 Se1 176.57(5)
P1 Se1 Au1 108.25(5)
C3 P1 C2 110.7(3)
C3 P1 C1 108.9(3)
C2 P1 C1 111.2(3)
C3 P1 Se1 111.7(2)
C2 P1 Se1 101.2(2)
C1 P1 Se1 113.1(2)
C13 C1 C11 109.0(6)
C13 C1 C12 108.5(7)
C11 C1 C12 109.5(6)
C13 C1 P1 111.2(5)
C11 C1 P1 109.7(5)
C12 C1 P1 108.9(5)
C22 C2 C21 106.6(6)
C22 C2 P1 113.7(5)
C21 C2 P1 111.9(4)
C31 C3 C32 110.1(7)
C31 C3 P1 114.8(5)
C32 C3 P1 113.2(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au1 Cl3 2.2827(15)
Au1 Cl1 2.2875(16)
Au1 Cl2 2.3314(17)
Au1 Se1 2.4432(7)
Se1 P1 2.2159(16)
P1 C3 1.835(6)
P1 C2 1.853(6)
P1 C1 1.870(7)
C1 C13 1.526(11)
C1 C11 1.545(9)
C1 C12 1.550(9)
C2 C22 1.531(9)
C2 C21 1.542(9)
C3 C31 1.526(10)
C3 C32 1.553(10)
