#------------------------------------------------------------------------------
#$Date: 2025-08-22 00:24:23 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301857 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/05/7110573.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110573
loop_
_publ_author_name
'Seppälä, Emma'
'Ruthe, Frank'
'Jeske, Jörg'
'du Mont, Wolf-W.'
'Jones, Peter G.'
_publ_section_title
;
 Coordination and oxidation of phosphine selenides with iodine: from
 cation pairs [(R3PSe)2I+]2 to (iodoseleno)phosphonium ions [R3PSeI]+
 existing as guests in polyiodide matrices
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1471
_journal_paper_doi               10.1039/a903249e
_journal_year                    1999
_chemical_formula_sum            'C11 H25 I7 P Se'
_chemical_formula_weight         1155.54
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.6693(10)
_cell_length_b                   16.4329(12)
_cell_length_c                   25.2272(18)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     5252.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43866
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    9.714
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   'multiple scans'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.743
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_coef       0.000315(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         15312
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0103P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0368
_refine_ls_wR_factor_ref         0.0380
_reflns_number_gt                12864
_reflns_number_total             15312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903249esup1.cif
_cod_data_source_block           finiki
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7110573
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'
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
I1 I 0.21191(2) 0.024307(19) 0.224641(11) 0.02153(7) Uani 1 1 d .
I2 I 0.45423(2) 0.010418(19) 0.125934(12) 0.02237(7) Uani 1 1 d .
I3 I 0.24601(2) 0.12382(2) 0.112230(11) 0.02232(7) Uani 1 1 d .
I4 I 0.06541(3) 0.23811(2) 0.185120(12) 0.02721(7) Uani 1 1 d .
I5 I -0.08137(2) 0.279712(19) 0.260755(11) 0.02204(7) Uani 1 1 d .
I6 I -0.23672(2) 0.308113(19) 0.363213(12) 0.02389(7) Uani 1 1 d .
I7 I -0.41402(2) 0.275886(19) 0.457562(12) 0.02280(7) Uani 1 1 d .
I8 I -0.55694(2) 0.241158(19) 0.536695(11) 0.02454(7) Uani 1 1 d .
I9 I -0.19583(3) 0.10007(2) 0.352788(13) 0.03245(8) Uani 1 1 d .
I10 I -0.15248(3) -0.06219(2) 0.342804(14) 0.03844(9) Uani 1 1 d .
I11 I -0.44490(2) 0.28560(2) 0.288839(11) 0.02465(7) Uani 1 1 d .
I12 I -0.62104(3) 0.26217(3) 0.227574(15) 0.05103(12) Uani 1 1 d .
I13 I 0.43855(2) 0.224999(19) 0.047840(11) 0.02291(7) Uani 1 1 d .
I14 I 0.58414(2) 0.28785(2) -0.021559(12) 0.02522(7) Uani 1 1 d .
Se2 Se 0.62795(4) -0.06599(3) 0.14212(2) 0.02361(11) Uani 1 1 d .
Se1 Se 0.19240(4) -0.05022(3) 0.313370(18) 0.02273(11) Uani 1 1 d .
P2 P 0.74529(9) 0.01778(7) 0.10453(5) 0.0160(2) Uani 1 1 d .
P1 P 0.28151(9) 0.03104(7) 0.36854(4) 0.0156(2) Uani 1 1 d .
C1 C 0.2579(4) 0.1388(3) 0.35141(17) 0.0189(10) Uani 1 1 d U
H1 H 0.3029 0.1500 0.3197 0.023 Uiso 1 1 calc R
C2 C 0.1458(4) 0.1604(3) 0.33501(19) 0.0289(12) Uani 1 1 d U
H2A H 0.1025 0.1686 0.3667 0.035 Uiso 1 1 calc R
H2B H 0.1161 0.1159 0.3138 0.035 Uiso 1 1 calc R
H2C H 0.1467 0.2104 0.3139 0.035 Uiso 1 1 calc R
C3 C 0.2950(4) 0.1989(3) 0.39431(19) 0.0312(12) Uani 1 1 d U
H3A H 0.2920 0.2545 0.3803 0.037 Uiso 1 1 calc R
H3B H 0.3677 0.1859 0.4045 0.037 Uiso 1 1 calc R
H3C H 0.2489 0.1945 0.4254 0.037 Uiso 1 1 calc R
C4 C 0.2232(4) 0.0015(3) 0.43423(17) 0.0230(11) Uani 1 1 d U
C5 C 0.2052(4) -0.0901(3) 0.43706(19) 0.0332(13) Uani 1 1 d U
H5A H 0.2708 -0.1185 0.4281 0.040 Uiso 1 1 calc R
H5B H 0.1499 -0.1056 0.4118 0.040 Uiso 1 1 calc R
H5C H 0.1833 -0.1050 0.4730 0.040 Uiso 1 1 calc R
C6 C 0.1146(4) 0.0421(3) 0.4390(2) 0.0368(13) Uani 1 1 d U
H6A H 0.0812 0.0254 0.4724 0.044 Uiso 1 1 calc R
H6B H 0.0701 0.0254 0.4092 0.044 Uiso 1 1 calc R
H6C H 0.1230 0.1014 0.4387 0.044 Uiso 1 1 calc R
C7 C 0.2932(4) 0.0294(3) 0.48031(17) 0.0302(12) Uani 1 1 d U
H7A H 0.3022 0.0886 0.4787 0.036 Uiso 1 1 calc R
H7B H 0.3623 0.0030 0.4777 0.036 Uiso 1 1 calc R
H7C H 0.2598 0.0145 0.5140 0.036 Uiso 1 1 calc R
C8 C 0.4256(4) 0.0073(3) 0.36088(18) 0.0233(10) Uani 1 1 d U
C9 C 0.4959(4) 0.0670(3) 0.3922(2) 0.0357(13) Uani 1 1 d U
H9A H 0.5696 0.0492 0.3902 0.043 Uiso 1 1 calc R
H9B H 0.4734 0.0681 0.4294 0.043 Uiso 1 1 calc R
H9C H 0.4894 0.1216 0.3770 0.043 Uiso 1 1 calc R
C10 C 0.4562(4) 0.0158(3) 0.30275(18) 0.0299(12) Uani 1 1 d U
H10A H 0.5323 0.0071 0.2988 0.036 Uiso 1 1 calc R
H10B H 0.4380 0.0705 0.2903 0.036 Uiso 1 1 calc R
H10C H 0.4179 -0.0247 0.2817 0.036 Uiso 1 1 calc R
C11 C 0.4485(4) -0.0792(3) 0.37977(19) 0.0334(12) Uani 1 1 d U
H11A H 0.4019 -0.1174 0.3612 0.040 Uiso 1 1 calc R
H11B H 0.4360 -0.0829 0.4180 0.040 Uiso 1 1 calc R
H11C H 0.5222 -0.0929 0.3721 0.040 Uiso 1 1 calc R
C21 C 0.7066(4) 0.1245(3) 0.11695(17) 0.0203(10) Uani 1 1 d U
H21 H 0.6458 0.1350 0.0926 0.024 Uiso 1 1 calc R
C22 C 0.7898(4) 0.1878(3) 0.1023(2) 0.0327(12) Uani 1 1 d U
H22A H 0.7574 0.2420 0.1019 0.039 Uiso 1 1 calc R
H22B H 0.8184 0.1754 0.0672 0.039 Uiso 1 1 calc R
H22C H 0.8468 0.1866 0.1285 0.039 Uiso 1 1 calc R
C23 C 0.6642(4) 0.1424(3) 0.17363(19) 0.0321(13) Uani 1 1 d U
H23A H 0.7237 0.1524 0.1976 0.039 Uiso 1 1 calc R
H23B H 0.6236 0.0955 0.1864 0.039 Uiso 1 1 calc R
H23C H 0.6186 0.1905 0.1726 0.039 Uiso 1 1 calc R
C24 C 0.8718(3) -0.0119(3) 0.13835(18) 0.0225(10) Uani 1 1 d U
C25 C 0.9676(4) 0.0155(3) 0.1066(2) 0.0312(12) Uani 1 1 d U
H25A H 0.9647 0.0745 0.1014 0.037 Uiso 1 1 calc R
H25B H 0.9676 -0.0118 0.0720 0.037 Uiso 1 1 calc R
H25C H 1.0321 0.0013 0.1259 0.037 Uiso 1 1 calc R
C26 C 0.8745(4) 0.0279(3) 0.19302(18) 0.0310(12) Uani 1 1 d U
H26A H 0.9366 0.0086 0.2125 0.037 Uiso 1 1 calc R
H26B H 0.8104 0.0135 0.2126 0.037 Uiso 1 1 calc R
H26C H 0.8784 0.0871 0.1890 0.037 Uiso 1 1 calc R
C27 C 0.8761(4) -0.1047(3) 0.1461(2) 0.0334(13) Uani 1 1 d U
H27A H 0.8649 -0.1319 0.1120 0.040 Uiso 1 1 calc R
H27B H 0.8209 -0.1214 0.1711 0.040 Uiso 1 1 calc R
H27C H 0.9453 -0.1201 0.1603 0.040 Uiso 1 1 calc R
C28 C 0.7439(4) -0.0018(3) 0.03056(17) 0.0205(10) Uani 1 1 d U
C29 C 0.7848(4) -0.0877(3) 0.01951(19) 0.0301(12) Uani 1 1 d U
H29A H 0.7489 -0.1265 0.0429 0.036 Uiso 1 1 calc R
H29B H 0.8610 -0.0897 0.0261 0.036 Uiso 1 1 calc R
H29C H 0.7707 -0.1020 -0.0175 0.036 Uiso 1 1 calc R
C30 C 0.8076(4) 0.0618(3) -0.00065(19) 0.0351(13) Uani 1 1 d U
H30A H 0.8104 0.0461 -0.0381 0.042 Uiso 1 1 calc R
H30B H 0.8794 0.0648 0.0136 0.042 Uiso 1 1 calc R
H30C H 0.7735 0.1151 0.0026 0.042 Uiso 1 1 calc R
C31 C 0.6296(4) 0.0015(3) 0.01092(18) 0.0291(12) Uani 1 1 d U
H31A H 0.5992 0.0548 0.0193 0.035 Uiso 1 1 calc R
H31B H 0.5883 -0.0411 0.0284 0.035 Uiso 1 1 calc R
H31C H 0.6281 -0.0070 -0.0275 0.035 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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
P2 Se2 I2 101.62(4)
P1 Se1 I1 102.10(3)
C21 P2 C24 113.3(2)
C21 P2 C28 109.0(2)
C24 P2 C28 114.3(2)
C21 P2 Se2 109.61(15)
C24 P2 Se2 102.39(15)
C28 P2 Se2 107.89(15)
C1 P1 C8 109.4(2)
C1 P1 C4 113.0(2)
C8 P1 C4 114.8(2)
C1 P1 Se1 110.19(14)
C8 P1 Se1 107.66(15)
C4 P1 Se1 101.34(15)
C2 C1 C3 109.1(4)
C2 C1 P1 116.0(3)
C3 C1 P1 113.6(3)
C5 C4 C7 110.3(4)
C5 C4 C6 106.9(4)
C7 C4 C6 109.2(4)
C5 C4 P1 110.8(3)
C7 C4 P1 111.4(3)
C6 C4 P1 108.1(3)
C10 C8 C11 109.7(4)
C10 C8 C9 106.8(4)
C11 C8 C9 108.8(4)
C10 C8 P1 109.1(3)
C11 C8 P1 110.2(3)
C9 C8 P1 112.2(3)
C22 C21 C23 109.4(4)
C22 C21 P2 115.0(3)
C23 C21 P2 115.3(3)
C25 C24 C26 109.3(4)
C25 C24 C27 109.4(4)
C26 C24 C27 108.0(4)
C25 C24 P2 111.4(3)
C26 C24 P2 108.6(3)
C27 C24 P2 110.2(3)
C29 C28 C31 107.1(4)
C29 C28 C30 110.9(4)
C31 C28 C30 107.8(4)
C29 C28 P2 109.5(3)
C31 C28 P2 108.7(3)
C30 C28 P2 112.6(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 Se1 2.5635(6)
I2 Se2 2.5666(6)
I4 I5 2.7507(5)
I7 I8 2.7549(4)
I9 I10 2.7339(6)
I11 I12 2.7417(5)
I13 I14 2.7449(5)
Se2 P2 2.2370(12)
Se1 P1 2.2349(12)
P2 C21 1.847(4)
P2 C24 1.880(4)
P2 C28 1.894(4)
P1 C1 1.847(4)
P1 C8 1.877(5)
P1 C4 1.878(4)
C1 C2 1.520(6)
C1 C3 1.539(6)
C4 C5 1.525(6)
C4 C7 1.532(6)
C4 C6 1.534(7)
C8 C10 1.523(6)
C8 C11 1.528(6)
C8 C9 1.542(6)
C21 C22 1.526(6)
C21 C23 1.555(6)
C24 C25 1.522(6)
C24 C26 1.527(6)
C24 C27 1.539(6)
C28 C29 1.530(6)
C28 C31 1.532(6)
C28 C30 1.537(7)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139183767
