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#$Date: 2025-08-21 02:27:06 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/03/4340378.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_4340378
loop_
_publ_author_name
'Burford, Neil'
'Ragogna, Paul J.'
'Sharp, Kendall'
'McDonald, Robert'
'Ferguson, Michael J.'
_publ_section_title
;
 Arsinophosphonium cations from arsenium-phosphine and -bisphosphine
 coordination chemistry.
;
_journal_issue                   25
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9453
_journal_page_last               9460
_journal_paper_doi               10.1021/ic050989w
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C16 H18 As F3 N O3 P S'
_chemical_formula_weight         467.26
_space_group_IT_number           61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.4041(11)
_cell_length_b                   14.4224(13)
_cell_length_c                   21.608(2)
_cell_measurement_temperature    193(2)
_cell_volume                     3865.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0847
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22726
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.5592
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0468
_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)+(0.0415P)²+2.3411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                2580
_reflns_number_total             3942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050989wsi20050616_040139.cif
_cod_data_source_block           dal0449_[AN-PMe3]9a[OTf]
_cod_original_cell_volume        3865.5(6)
_cod_database_code               4340378
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
As1 As 0.04217(3) 0.17498(3) 0.423916(18) 0.03736(13) Uani 1 1 d .
P1 P -0.07041(8) 0.24314(7) 0.34974(5) 0.0404(3) Uani 1 1 d .
N1 N -0.1459(3) 0.1550(2) 0.52789(15) 0.0414(8) Uani 1 1 d .
H1N H -0.2015 0.1526 0.5531 0.050 Uiso 1 1 calc R
C1 C -0.2083(3) 0.2086(3) 0.3591(2) 0.0500(11) Uani 1 1 d .
H1A H -0.2135 0.1409 0.3565 0.060 Uiso 1 1 calc R
H1B H -0.2522 0.2367 0.3264 0.060 Uiso 1 1 calc R
H1C H -0.2345 0.2292 0.3996 0.060 Uiso 1 1 calc R
C2 C -0.0632(4) 0.3673(3) 0.3544(2) 0.0519(11) Uani 1 1 d .
H2A H -0.0881 0.3876 0.3953 0.062 Uiso 1 1 calc R
H2B H -0.1092 0.3947 0.3224 0.062 Uiso 1 1 calc R
H2C H 0.0115 0.3873 0.3482 0.062 Uiso 1 1 calc R
C3 C -0.0216(4) 0.2077(3) 0.27548(19) 0.0576(12) Uani 1 1 d .
H3A H -0.0249 0.1400 0.2723 0.069 Uiso 1 1 calc R
H3B H 0.0532 0.2282 0.2705 0.069 Uiso 1 1 calc R
H3C H -0.0663 0.2355 0.2430 0.069 Uiso 1 1 calc R
C11 C -0.0003(3) 0.2553(3) 0.49151(17) 0.0354(9) Uani 1 1 d .
C12 C -0.0836(3) 0.2345(3) 0.53183(18) 0.0368(9) Uani 1 1 d .
C13 C -0.1071(4) 0.2970(3) 0.57953(19) 0.0470(10) Uani 1 1 d .
H13 H -0.1648 0.2844 0.6072 0.056 Uiso 1 1 calc R
C14 C -0.0473(4) 0.3767(3) 0.5867(2) 0.0588(13) Uani 1 1 d .
H14 H -0.0646 0.4188 0.6190 0.071 Uiso 1 1 calc R
C15 C 0.0377(4) 0.3962(3) 0.5476(2) 0.0583(12) Uani 1 1 d .
H15 H 0.0800 0.4504 0.5535 0.070 Uiso 1 1 calc R
C16 C 0.0601(3) 0.3363(3) 0.5001(2) 0.0465(10) Uani 1 1 d .
H16 H 0.1175 0.3500 0.4725 0.056 Uiso 1 1 calc R
C21 C -0.0569(3) 0.0753(2) 0.44197(18) 0.0365(9) Uani 1 1 d .
C22 C -0.1325(3) 0.0786(3) 0.48956(19) 0.0382(9) Uani 1 1 d .
C23 C -0.1997(3) 0.0020(3) 0.4995(2) 0.0440(10) Uani 1 1 d .
H23 H -0.2517 0.0036 0.5318 0.053 Uiso 1 1 calc R
C24 C -0.1910(4) -0.0758(3) 0.4626(2) 0.0531(12) Uani 1 1 d .
H24 H -0.2371 -0.1272 0.4699 0.064 Uiso 1 1 calc R
C25 C -0.1163(4) -0.0799(3) 0.4155(2) 0.0524(12) Uani 1 1 d .
H25 H -0.1114 -0.1334 0.3900 0.063 Uiso 1 1 calc R
C26 C -0.0490(3) -0.0056(3) 0.40584(19) 0.0458(10) Uani 1 1 d .
H26 H 0.0039 -0.0090 0.3741 0.055 Uiso 1 1 calc R
S S 0.26148(10) 0.38653(8) 0.30662(5) 0.0516(3) Uani 1 1 d .
F1 F 0.2722(4) 0.5132(3) 0.22181(18) 0.1484(19) Uani 1 1 d .
F2 F 0.2606(4) 0.5655(2) 0.3137(2) 0.1400(17) Uani 1 1 d .
F3 F 0.1204(3) 0.5063(3) 0.27032(17) 0.1173(14) Uani 1 1 d .
O1 O 0.2091(2) 0.3855(2) 0.36530(14) 0.0688(10) Uani 1 1 d .
O2 O 0.2183(3) 0.3254(2) 0.26226(17) 0.0806(11) Uani 1 1 d .
O3 O 0.3770(3) 0.3876(3) 0.30867(17) 0.0798(11) Uani 1 1 d .
C30 C 0.2274(6) 0.4987(4) 0.2765(3) 0.0847(18) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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
C21 As1 C11 96.87(16)
C21 As1 P1 94.09(11)
C11 As1 P1 95.90(11)
C3 P1 C1 110.2(2)
C3 P1 C2 108.6(2)
C1 P1 C2 108.5(2)
C3 P1 As1 106.97(15)
C1 P1 As1 112.00(14)
C2 P1 As1 110.50(15)
C12 N1 C22 128.8(3)
C12 C11 C16 119.7(4)
C12 C11 As1 123.3(3)
C16 C11 As1 117.0(3)
C11 C12 N1 123.8(4)
C11 C12 C13 118.7(4)
N1 C12 C13 117.5(4)
C14 C13 C12 120.5(4)
C13 C14 C15 120.8(4)
C16 C15 C14 119.0(4)
C15 C16 C11 121.1(4)
C22 C21 C26 119.0(4)
C22 C21 As1 123.5(3)
C26 C21 As1 117.5(3)
N1 C22 C21 123.2(3)
N1 C22 C23 117.6(4)
C21 C22 C23 119.2(4)
C24 C23 C22 120.4(4)
C25 C24 C23 121.0(4)
C26 C25 C24 119.1(4)
C25 C26 C21 121.4(4)
O2 S O1 115.2(2)
O2 S O3 114.1(2)
O1 S O3 115.4(2)
O2 S C30 103.2(3)
O1 S C30 103.0(2)
O3 S C30 103.7(3)
F2 C30 F1 107.3(6)
F2 C30 F3 108.1(5)
F1 C30 F3 108.4(5)
F2 C30 S 111.3(5)
F1 C30 S 111.5(4)
F3 C30 S 110.1(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
As1 C21 1.931(4)
As1 C11 1.937(4)
As1 P1 2.3421(11)
P1 C3 1.790(4)
P1 C1 1.793(4)
P1 C2 1.795(4)
N1 C12 1.386(5)
N1 C22 1.388(5)
C11 C12 1.384(5)
C11 C16 1.401(5)
C12 C13 1.400(5)
C13 C14 1.377(6)
C14 C15 1.380(6)
C15 C16 1.370(6)
C21 C22 1.393(5)
C21 C26 1.408(5)
C22 C23 1.401(5)
C23 C24 1.380(6)
C24 C25 1.379(6)
C25 C26 1.374(6)
S O2 1.408(3)
S O1 1.425(3)
S O3 1.434(3)
S C30 1.795(6)
F1 C30 1.323(6)
F2 C30 1.320(7)
F3 C30 1.338(7)
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
C21 As1 P1 C3 -99.9(2)
C11 As1 P1 C3 162.80(19)
C21 As1 P1 C1 20.97(19)
C11 As1 P1 C1 -76.38(19)
C21 As1 P1 C2 142.1(2)
C11 As1 P1 C2 44.8(2)
C21 As1 C11 C12 -3.5(3)
P1 As1 C11 C12 91.4(3)
C21 As1 C11 C16 174.3(3)
P1 As1 C11 C16 -90.8(3)
C16 C11 C12 N1 -178.4(4)
As1 C11 C12 N1 -0.6(5)
C16 C11 C12 C13 1.7(6)
As1 C11 C12 C13 179.4(3)
C22 N1 C12 C11 7.3(6)
C22 N1 C12 C13 -172.8(4)
C11 C12 C13 C14 -1.1(6)
N1 C12 C13 C14 178.9(4)
C12 C13 C14 C15 -0.7(7)
C13 C14 C15 C16 1.8(7)
C14 C15 C16 C11 -1.2(7)
C12 C11 C16 C15 -0.5(6)
As1 C11 C16 C15 -178.4(4)
C11 As1 C21 C22 3.0(3)
P1 As1 C21 C22 -93.4(3)
C11 As1 C21 C26 -175.0(3)
P1 As1 C21 C26 88.5(3)
C12 N1 C22 C21 -7.7(6)
C12 N1 C22 C23 172.8(4)
C26 C21 C22 N1 179.6(3)
As1 C21 C22 N1 1.5(5)
C26 C21 C22 C23 -1.0(5)
As1 C21 C22 C23 -179.0(3)
N1 C22 C23 C24 179.5(3)
C21 C22 C23 C24 0.1(6)
C22 C23 C24 C25 0.0(6)
C23 C24 C25 C26 0.8(6)
C24 C25 C26 C21 -1.8(6)
C22 C21 C26 C25 1.9(6)
As1 C21 C26 C25 -179.9(3)
O2 S C30 F2 178.7(4)
O1 S C30 F2 58.6(5)
O3 S C30 F2 -62.0(5)
O2 S C30 F1 -61.5(6)
O1 S C30 F1 178.4(5)
O3 S C30 F1 57.8(6)
O2 S C30 F3 58.9(4)
O1 S C30 F3 -61.3(5)
O3 S C30 F3 178.1(4)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139141955
