#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:25:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179919 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/14/7021489.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_7021489
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 Cl P Se'
_chemical_formula_weight         485.63
_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                 92.389(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2215(2)
_cell_length_b                   11.3519(3)
_cell_length_c                   15.2400(4)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6703
_cell_measurement_theta_min      2.2333
_cell_volume                     1421.11(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36734
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    13.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.736
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.00065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         4103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0129P)²+2.1815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0402
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                3360
_reflns_number_total             4103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50777g.txt
_cod_data_source_block           rudi
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7021489
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
Au Au 0.984242(12) 0.001438(10) 0.706909(7) 0.01254(4) Uani 1 1 d .
Se Se 0.80002(4) 0.00672(2) 0.58319(2) 0.01569(6) Uani 1 1 d .
Cl Cl 1.16671(9) -0.01630(6) 0.82363(5) 0.01805(14) Uani 1 1 d .
P P 0.70380(8) 0.18698(6) 0.58570(5) 0.00985(14) Uani 1 1 d .
C1 C 0.8636(3) 0.3032(2) 0.59398(19) 0.0133(5) Uani 1 1 d .
C2 C 0.5568(3) 0.2041(3) 0.67300(19) 0.0146(6) Uani 1 1 d .
H2 H 0.5246 0.2889 0.6751 0.018 Uiso 1 1 calc R
C3 C 0.5831(3) 0.1950(3) 0.48104(18) 0.0148(6) Uani 1 1 d .
H3 H 0.5146 0.1221 0.4795 0.018 Uiso 1 1 calc R
C11 C 0.7903(4) 0.4209(3) 0.5622(2) 0.0178(6) Uani 1 1 d .
H11A H 0.8709 0.4838 0.5716 0.027 Uiso 1 1 calc R
H11B H 0.6936 0.4387 0.5953 0.027 Uiso 1 1 calc R
H11C H 0.7596 0.4154 0.4995 0.027 Uiso 1 1 calc R
C12 C 1.0073(3) 0.2699(3) 0.5373(2) 0.0204(6) Uani 1 1 d .
H12A H 1.0894 0.3325 0.5408 0.031 Uiso 1 1 calc R
H12B H 0.9683 0.2600 0.4761 0.031 Uiso 1 1 calc R
H12C H 1.0558 0.1960 0.5589 0.031 Uiso 1 1 calc R
C13 C 0.9279(4) 0.3178(3) 0.68885(19) 0.0173(6) Uani 1 1 d .
H13A H 0.9572 0.2405 0.7133 0.026 Uiso 1 1 calc R
H13B H 0.8435 0.3536 0.7237 0.026 Uiso 1 1 calc R
H13C H 1.0243 0.3687 0.6903 0.026 Uiso 1 1 calc R
C21 C 0.4034(4) 0.1316(3) 0.6518(2) 0.0277(8) Uani 1 1 d .
H21A H 0.4316 0.0478 0.6500 0.041 Uiso 1 1 calc R
H21B H 0.3557 0.1558 0.5946 0.041 Uiso 1 1 calc R
H21C H 0.3244 0.1448 0.6972 0.041 Uiso 1 1 calc R
C22 C 0.6215(4) 0.1686(3) 0.76448(19) 0.0200(6) Uani 1 1 d .
H22A H 0.5349 0.1770 0.8063 0.030 Uiso 1 1 calc R
H22B H 0.7132 0.2196 0.7824 0.030 Uiso 1 1 calc R
H22C H 0.6580 0.0865 0.7635 0.030 Uiso 1 1 calc R
C31 C 0.6862(4) 0.1870(3) 0.39964(19) 0.0204(6) Uani 1 1 d .
H31A H 0.6152 0.1717 0.3476 0.031 Uiso 1 1 calc R
H31B H 0.7652 0.1228 0.4073 0.031 Uiso 1 1 calc R
H31C H 0.7442 0.2615 0.3920 0.031 Uiso 1 1 calc R
C32 C 0.4615(3) 0.2976(3) 0.4722(2) 0.0181(6) Uani 1 1 d .
H32A H 0.5161 0.3668 0.4486 0.027 Uiso 1 1 calc R
H32B H 0.4207 0.3166 0.5301 0.027 Uiso 1 1 calc R
H32C H 0.3702 0.2750 0.4324 0.027 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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl Au Se 176.13(2)
P Se Au 103.22(2)
C2 P C3 105.86(13)
C2 P C1 110.98(13)
C3 P C1 112.10(13)
C2 P Se 110.99(10)
C3 P Se 102.24(10)
C1 P Se 114.08(9)
C13 C1 C11 108.7(2)
C13 C1 C12 108.3(2)
C11 C1 C12 109.7(2)
C13 C1 P 110.86(19)
C11 C1 P 109.17(19)
C12 C1 P 110.1(2)
C22 C2 C21 107.7(2)
C22 C2 P 114.7(2)
C21 C2 P 110.5(2)
C31 C3 C32 110.7(2)
C31 C3 P 113.6(2)
C32 C3 P 115.9(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Au Cl 2.2876(7)
Au Se 2.3695(3)
Se P 2.1948(7)
P C2 1.844(3)
P C3 1.845(3)
P C1 1.863(3)
C1 C13 1.528(4)
C1 C11 1.536(4)
C1 C12 1.540(4)
C2 C22 1.525(4)
C2 C21 1.529(4)
C3 C31 1.534(4)
C3 C32 1.538(4)
