#------------------------------------------------------------------------------ #$Date: 2020-01-31 12:37:04 +0200 (Fri, 31 Jan 2020) $ #$Revision: 247409 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/71/1557199.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_1557199 loop_ _publ_author_name 'Rudd, Martin D.' 'Lindeman, Sergey V.' 'Husebye, Steinar' _publ_section_title ; Three-Center, Four-Electron Bonding and Structural Characteristics of Two-Coordinate Iodine(I) Complexes with Halogen and Chalcogen Ligands. Synthesis, Spectroscopic Characterization and X-Ray Structural Studies of (Triiodo)[tris(dimethylamino)phosphaneselenide]iodine(I) and Bis{(triiodo)[tri(N-morpholyl)phosphaneselenide]iodine(I)}/Diiodine Molecular Complex ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 689 _journal_page_last 708 _journal_paper_doi 10.3891/acta.chem.scand.51-0689 _journal_volume 51 _journal_year 1997 _chemical_formula_sum 'C6 H18 I4 N3 P Se' _chemical_formula_weight 749.76 _chemical_name_common ; (Triiodo)[tris(dimethylamino)phosphaneselenide]iodine(I) ; _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 14.003(4) _cell_length_b 10.958(2) _cell_length_c 11.801(2) _cell_volume 1810.8(7) _diffrn_ambient_temperature 103 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 8.964 _exptl_crystal_density_diffrn 2.750 _exptl_crystal_F_000 1344 _refine_ls_goodness_of_fit_ref 0.617 _refine_ls_number_parameters 148 _refine_ls_number_reflns 2745 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_gt 9.0729 _refine_ls_wR_factor_ref 0.0870 _cod_data_source_file Acta-Chem-Scand-1997-51-689-1.cif _cod_data_source_block 1 _cod_database_code 1557199 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,1/2+y,1/2+z 4 1/2+x,1/2-y,z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I Uiso -0.64188(3) 0.10099(4) 0.01841(4) 1.000 0.0195(1) . . . . I2 I Uiso -0.72872(3) 0.03441(4) -0.22610(4) 1.000 0.0211(1) . . . . I3 I Uiso -0.91838(3) 0.02151(4) -0.07922(4) 1.000 0.0187(1) . . . . I4 I Uiso -1.07083(3) 0.00829(4) 0.07086(5) 1.000 0.0222(1) . . . . Se1 Se Uiso -0.57932(6) 0.17397(8) 0.21410(7) 1.000 0.0273(2) . . . . P1 P Uiso -0.67120(10) 0.06690(10) 0.33110(10) 1.000 0.0152(3) . . . . N1 N Uiso -0.6243(4) -0.0651(5) 0.3572(5) 1.000 0.0190(10) . . . . N2 N Uiso -0.6710(4) 0.1412(5) 0.4522(5) 1.000 0.0170(10) . . . . N3 N Uiso -0.7781(4) 0.0562(5) 0.2803(6) 1.000 0.0200(10) . . . . C11 C Uiso -0.6501(5) -0.1344(6) 0.4598(6) 1.000 0.0220(10) . . . . C12 C Uiso -0.5731(5) -0.1381(7) 0.2713(8) 1.000 0.0270(10) . . . . C21 C Uiso -0.5778(5) 0.1633(7) 0.5063(7) 1.000 0.0250(10) . . . . C22 C Uiso -0.7442(6) 0.2278(5) 0.4850(6) 1.000 0.0220(10) . . . . C31 C Uiso -0.8233(5) -0.0618(7) 0.2562(6) 1.000 0.0240(10) . . . . C32 C Uiso -0.8311(6) 0.1600(6) 0.2375(6) 1.000 0.0240(10) . . . . 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' I I -0.4742 1.8119 ' 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' 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' 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I2 I3 I4 173.44(2) . . . yes I1 Se1 P1 101.23(5) . . . yes Se1 P1 N2 106.1(2) . . . yes Se1 P1 N3 110.1(2) . . . yes N1 P1 N2 106.1(3) . . . yes N1 P1 N3 112.4(3) . . . yes N2 P1 N3 111.1(3) . . . yes Se1 P1 N1 110.8(2) . . . yes P1 N1 C11 121.2(5) . . . yes P1 N1 C12 123.4(5) . . . yes C11 N1 C12 113.8(5) . . . yes P1 N2 C22 123.7(5) . . . yes C21 N2 C22 113.8(6) . . . yes P1 N2 C21 117.4(5) . . . yes P1 N3 C32 123.1(5) . . . yes C31 N3 C32 113.8(6) . . . yes P1 N3 C31 122.4(5) . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Se1 2.5962(12) . . yes I2 I3 3.1746(11) . . yes I3 I4 2.7776(10) . . yes Se1 P1 2.2222(16) . . yes P1 N2 1.645(6) . . yes P1 N1 1.618(6) . . yes P1 N3 1.617(6) . . yes N1 C12 1.477(10) . . yes N1 C11 1.474(9) . . yes N2 C21 1.473(9) . . yes N2 C22 1.450(9) . . yes N3 C32 1.449(9) . . yes N3 C31 1.468(9) . . yes 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 I1 Se1 P1 N1 87.6(2) . . . . no I1 Se1 P1 N2 -157.7(2) . . . . no I1 Se1 P1 N3 -37.4(2) . . . . no Se1 P1 N1 C11 157.8(4) . . . . no Se1 P1 N1 C12 -37.8(6) . . . . no N2 P1 N1 C11 43.0(6) . . . . no N2 P1 N1 C12 -152.5(5) . . . . no N3 P1 N1 C11 -78.6(6) . . . . no N3 P1 N1 C12 86.0(6) . . . . no Se1 P1 N2 C21 -57.5(5) . . . . no Se1 P1 N2 C22 95.4(5) . . . . no N1 P1 N2 C21 60.4(6) . . . . no N1 P1 N2 C22 -146.7(5) . . . . no N3 P1 N2 C21 -177.2(5) . . . . no N3 P1 N2 C22 -24.2(6) . . . . no Se1 P1 N3 C31 121.2(5) . . . . no Se1 P1 N3 C32 -48.4(6) . . . . no N1 P1 N3 C31 -2.9(7) . . . . no N1 P1 N3 C32 -172.5(6) . . . . no N2 P1 N3 C31 -121.6(6) . . . . no N2 P1 N3 C32 68.9(7) . . . . no