#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:00:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179088 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/50/4305080.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_4305080
loop_
_publ_author_name
'Eamonn Conrad'
'Neil Burford'
'Robert McDonald'
'Michael J. Ferguson'
_publ_section_title
;
Phosphinoarsonium and Diarsonium Cations from Chloride-Abstraction-Induced
Pnictogen Coupling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2952
_journal_page_last               2954
_journal_paper_doi               10.1021/ic800287e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C16 H19 As F3 O3 P S'
_chemical_formula_weight         454.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.4800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7585(8)
_cell_length_b                   12.8289(9)
_cell_length_c                   12.9423(9)
_cell_measurement_reflns_used    7932
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      2.24
_cell_volume                     1939.9(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16071
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  0.6429
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4449
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0335
_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)+(0.0496P)²+0.7515P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0889
_reflns_number_gt                3723
_reflns_number_total             4449
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic800287e-file003_3.cif
_cod_data_source_block           dal0793
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4305080
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
As As 0.373769(19) 0.214706(18) 0.478341(18) 0.03811(9) Uani 1 1 d . . .
P P 0.22375(5) 0.24447(5) 0.34881(5) 0.03971(14) Uani 1 1 d . . .
C1 C 0.3444(2) 0.0940(2) 0.5574(2) 0.0569(7) Uani 1 1 d . . .
H1A H 0.4085 0.0825 0.6115 0.068 Uiso 1 1 calc R . .
H1B H 0.3356 0.0332 0.5115 0.068 Uiso 1 1 calc R . .
H1C H 0.2739 0.1044 0.5900 0.068 Uiso 1 1 calc R . .
C2 C 0.4011(3) 0.3278(2) 0.5743(3) 0.0712(9) Uani 1 1 d . . .
H2A H 0.4654 0.3103 0.6264 0.085 Uiso 1 1 calc R . .
H2B H 0.3325 0.3402 0.6090 0.085 Uiso 1 1 calc R . .
H2C H 0.4196 0.3907 0.5368 0.085 Uiso 1 1 calc R . .
C3 C 0.5103(2) 0.1928(3) 0.4153(3) 0.0681(9) Uani 1 1 d . . .
H3A H 0.5741 0.1802 0.4694 0.082 Uiso 1 1 calc R . .
H3B H 0.5266 0.2547 0.3751 0.082 Uiso 1 1 calc R . .
H3C H 0.5005 0.1323 0.3690 0.082 Uiso 1 1 calc R . .
C11 C 0.10572(19) 0.19921(17) 0.41709(19) 0.0395(5) Uani 1 1 d . . .
C12 C 0.0879(2) 0.2271(2) 0.5189(2) 0.0485(6) Uani 1 1 d . . .
H12 H 0.1405 0.2722 0.5579 0.058 Uiso 1 1 calc R . .
C13 C -0.0053(2) 0.1896(2) 0.5625(3) 0.0568(7) Uani 1 1 d . . .
H13 H -0.0160 0.2081 0.6318 0.068 Uiso 1 1 calc R . .
C14 C -0.0832(2) 0.1253(2) 0.5062(3) 0.0648(8) Uani 1 1 d . . .
H14 H -0.1481 0.1005 0.5363 0.078 Uiso 1 1 calc R . .
C15 C -0.0670(2) 0.0970(2) 0.4062(3) 0.0652(8) Uani 1 1 d . . .
H15 H -0.1207 0.0527 0.3674 0.078 Uiso 1 1 calc R . .
C16 C 0.0276(2) 0.1332(2) 0.3620(2) 0.0499(6) Uani 1 1 d . . .
H16 H 0.0390 0.1125 0.2934 0.060 Uiso 1 1 calc R . .
C21 C 0.21716(19) 0.38671(19) 0.35941(17) 0.0391(5) Uani 1 1 d . . .
C22 C 0.1231(2) 0.4411(2) 0.38712(19) 0.0441(5) Uani 1 1 d . . .
H22 H 0.0588 0.4039 0.4062 0.053 Uiso 1 1 calc R . .
C23 C 0.1223(3) 0.5487(2) 0.3872(2) 0.0535(6) Uani 1 1 d . . .
H23 H 0.0577 0.5848 0.4072 0.064 Uiso 1 1 calc R . .
C24 C 0.2135(3) 0.6043(2) 0.3585(2) 0.0583(7) Uani 1 1 d . . .
H24 H 0.2125 0.6783 0.3591 0.070 Uiso 1 1 calc R . .
C25 C 0.3068(3) 0.5512(2) 0.3288(2) 0.0589(7) Uani 1 1 d . . .
H25 H 0.3699 0.5891 0.3082 0.071 Uiso 1 1 calc R . .
C26 C 0.3093(2) 0.4435(2) 0.32889(19) 0.0486(6) Uani 1 1 d . . .
H26 H 0.3738 0.4079 0.3081 0.058 Uiso 1 1 calc R . .
S1A S 0.3512(3) 0.5801(2) 0.7762(2) 0.0443(7) Uani 0.70 1 d PD A 1
F1A F 0.2418(4) 0.6629(4) 0.6131(3) 0.0992(14) Uani 0.70 1 d PD A 1
F2A F 0.1876(3) 0.5086(3) 0.6433(3) 0.0717(12) Uani 0.70 1 d PD A 1
F3A F 0.1388(2) 0.6383(3) 0.7320(3) 0.0967(12) Uani 0.70 1 d PD A 1
O1A O 0.3096(3) 0.5086(3) 0.8513(3) 0.0915(12) Uani 0.70 1 d PD A 1
O2A O 0.3743(4) 0.6799(3) 0.8187(3) 0.0874(15) Uani 0.70 1 d PD A 1
O3A O 0.4307(2) 0.5396(3) 0.7185(3) 0.0858(11) Uani 0.70 1 d PD A 1
C10A C 0.2227(4) 0.5996(5) 0.6870(3) 0.0491(11) Uani 0.70 1 d PD A 1
S1B S 0.3546(6) 0.5859(5) 0.7908(4) 0.0426(17) Uani 0.30 1 d PD B 2
F1B F 0.1944(9) 0.5124(10) 0.6590(8) 0.200(10) Uani 0.30 1 d PD B 2
F2B F 0.2047(10) 0.6780(8) 0.6589(8) 0.135(6) Uani 0.30 1 d PD B 2
F3B F 0.3251(8) 0.5840(7) 0.5884(4) 0.126(4) Uani 0.30 1 d PD B 2
O1B O 0.4355(6) 0.6699(5) 0.7775(6) 0.085(3) Uani 0.30 1 d PD B 2
O2B O 0.4053(7) 0.4867(4) 0.7925(5) 0.082(3) Uani 0.30 1 d PD B 2
O3B O 0.2827(8) 0.6048(8) 0.8644(5) 0.133(5) Uani 0.30 1 d PD B 2
C10B C 0.2657(6) 0.5894(7) 0.6670(5) 0.076(5) Uani 0.30 1 d PD B 2
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'
O O 0.0106 0.0060 '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'
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'
As As 0.0499 2.0058 '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
C3 As C1 108.84(14) . . ?
C3 As C2 107.59(16) . . ?
C1 As C2 107.09(15) . . ?
C3 As P 108.88(10) . . ?
C1 As P 110.58(9) . . ?
C2 As P 113.72(10) . . ?
C11 P C21 103.89(10) . . ?
C11 P As 98.94(8) . . ?
C21 P As 98.32(7) . . ?
C16 C11 C12 118.5(2) . . ?
C16 C11 P 116.2(2) . . ?
C12 C11 P 125.23(19) . . ?
C13 C12 C11 120.5(3) . . ?
C12 C13 C14 120.3(3) . . ?
C13 C14 C15 120.0(3) . . ?
C14 C15 C16 120.1(3) . . ?
C11 C16 C15 120.5(3) . . ?
C22 C21 C26 118.4(2) . . ?
C22 C21 P 124.15(18) . . ?
C26 C21 P 117.20(19) . . ?
C23 C22 C21 120.6(2) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 119.3(3) . . ?
C24 C25 C26 120.6(3) . . ?
C25 C26 C21 120.3(3) . . ?
O3A S1A O2A 116.5(4) . . ?
O3A S1A O1A 115.3(3) . . ?
O2A S1A O1A 112.1(4) . . ?
O3A S1A C10A 106.1(3) . . ?
O2A S1A C10A 103.5(3) . . ?
O1A S1A C10A 101.2(3) . . ?
F1A C10A F3A 107.2(5) . . ?
F1A C10A F2A 107.8(4) . . ?
F3A C10A F2A 107.9(4) . . ?
F1A C10A S1A 110.9(4) . . ?
F3A C10A S1A 112.8(3) . . ?
F2A C10A S1A 110.0(4) . . ?
O3B S1B O2B 116.5(5) . . ?
O3B S1B O1B 114.5(4) . . ?
O2B S1B O1B 112.9(4) . . ?
O3B S1B C10B 105.8(3) . . ?
O2B S1B C10B 103.7(4) . . ?
O1B S1B C10B 101.3(4) . . ?
F1B C10B F3B 107.3(6) . . ?
F1B C10B F2B 107.7(4) . . ?
F3B C10B F2B 108.3(5) . . ?
F1B C10B S1B 110.9(5) . . ?
F3B C10B S1B 112.6(4) . . ?
F2B C10B S1B 109.8(5) . . ?
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
As C3 1.902(3) . ?
As C1 1.909(3) . ?
As C2 1.913(3) . ?
As P 2.3239(7) . ?
P C11 1.822(2) . ?
P C21 1.832(3) . ?
C11 C16 1.386(3) . ?
C11 C12 1.403(4) . ?
C12 C13 1.374(4) . ?
C13 C14 1.378(5) . ?
C14 C15 1.379(5) . ?
C15 C16 1.387(4) . ?
C21 C22 1.388(3) . ?
C21 C26 1.399(3) . ?
C22 C23 1.381(4) . ?
C23 C24 1.374(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.382(4) . ?
S1A O3A 1.363(5) . ?
S1A O2A 1.408(4) . ?
S1A O1A 1.460(5) . ?
S1A C10A 1.813(4) . ?
F1A C10A 1.293(8) . ?
F2A C10A 1.342(7) . ?
F3A C10A 1.300(5) . ?
S1B O3B 1.365(6) . ?
S1B O2B 1.406(5) . ?
S1B O1B 1.460(5) . ?
S1B C10B 1.812(4) . ?
F1B C10B 1.293(8) . ?
F2B C10B 1.342(7) . ?
F3B C10B 1.299(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 As P C11 153.50(14) . . . . ?
C1 As P C11 33.97(13) . . . . ?
C2 As P C11 -86.55(15) . . . . ?
C3 As P C21 -100.92(14) . . . . ?
C1 As P C21 139.54(12) . . . . ?
C2 As P C21 19.02(15) . . . . ?
C21 P C11 C16 125.85(19) . . . . ?
As P C11 C16 -133.21(17) . . . . ?
C21 P C11 C12 -53.2(2) . . . . ?
As P C11 C12 47.7(2) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
P C11 C12 C13 179.0(2) . . . . ?
C11 C12 C13 C14 -0.9(4) . . . . ?
C12 C13 C14 C15 1.0(4) . . . . ?
C13 C14 C15 C16 0.0(4) . . . . ?
C12 C11 C16 C15 1.1(4) . . . . ?
P C11 C16 C15 -178.1(2) . . . . ?
C14 C15 C16 C11 -1.0(4) . . . . ?
C11 P C21 C22 -16.0(2) . . . . ?
As P C21 C22 -117.40(19) . . . . ?
C11 P C21 C26 169.70(18) . . . . ?
As P C21 C26 68.28(18) . . . . ?
C26 C21 C22 C23 -1.7(4) . . . . ?
P C21 C22 C23 -176.0(2) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C24 C25 C26 C21 -0.2(4) . . . . ?
C22 C21 C26 C25 1.4(4) . . . . ?
P C21 C26 C25 176.1(2) . . . . ?
O3A S1A C10A F1A -59.8(5) . . . . ?
O2A S1A C10A F1A 63.4(5) . . . . ?
O1A S1A C10A F1A 179.5(4) . . . . ?
O3A S1A C10A F3A 180.0(5) . . . . ?
O2A S1A C10A F3A -56.9(6) . . . . ?
O1A S1A C10A F3A 59.3(6) . . . . ?
O3A S1A C10A F2A 59.4(5) . . . . ?
O2A S1A C10A F2A -177.5(4) . . . . ?
O1A S1A C10A F2A -61.3(5) . . . . ?
O3B S1B C10B F1B -66.9(9) . . . . ?
O2B S1B C10B F1B 56.2(9) . . . . ?
O1B S1B C10B F1B 173.4(8) . . . . ?
O3B S1B C10B F3B 172.9(7) . . . . ?
O2B S1B C10B F3B -64.0(8) . . . . ?
O1B S1B C10B F3B 53.1(8) . . . . ?
O3B S1B C10B F2B 52.0(7) . . . . ?
O2B S1B C10B F2B 175.1(7) . . . . ?
O1B S1B C10B F2B -67.7(7) . . . . ?
