#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012954.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # 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_2012954 loop_ _publ_author_name 'Rivard, Eric' 'McWilliams, Andrew R.' 'Lough, Alan J.' 'Manners, Ian' _publ_section_title ; Bis(trichlorophosphine)iminium salts, [Cl~3~P=N=PCl~3~]^+^, with transition metal halide counter-ions ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first i114 _journal_page_last i118 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '(Cl6 N P2) [Ta1 Cl6]' _chemical_formula_moiety 'Cl6 N P2 1+, Cl6 Ta 1-' _chemical_formula_sum 'Cl12 N P2 Ta' _chemical_formula_weight 682.30 _chemical_name_systematic ; Bis(trichlorophosphino)iminium hexachlorotantalate ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 103.855(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.3957(5) _cell_length_b 8.5165(4) _cell_length_c 15.0937(5) _cell_measurement_reflns_used 10506 _cell_measurement_temperature 150.0(10) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.5 _cell_volume 1671.86(12) _computing_cell_refinement 'DENZO--SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius BV, 2001)' _computing_data_reduction DENZO--SMN _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1999)' _diffrn_ambient_temperature 150.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _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 0.043 _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 6759 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.86 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.655 _exptl_absorpt_correction_T_max 0.271 _exptl_absorpt_correction_T_min 0.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO--SMN; Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.292 _refine_diff_density_min -1.348 _refine_ls_extinction_coef 0.00092(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 1917 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.078 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0272 _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/[\s^2^(Fo^2^)+(0.0322P)^2^+1.5713P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.0694 _reflns_number_gt 1675 _reflns_number_total 1917 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1570.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_original_cell_volume 1671.86(11) _cod_database_code 2012954 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Ta1 0.5000 0.5000 0.5000 0.01880(11) Uani d S 1 . . Ta Cl1 0.43104(9) 0.52079(12) 0.34243(7) 0.0296(2) Uani d . 1 . . Cl Cl2 0.33754(7) 0.55757(14) 0.52638(7) 0.0298(2) Uani d . 1 . . Cl Cl3 0.46034(8) 0.23099(12) 0.49147(7) 0.0295(2) Uani d . 1 . . Cl Cl4 0.36758(8) -0.13868(14) 0.67504(9) 0.0427(3) Uani d . 1 . . Cl Cl5 0.33272(8) 0.06577(15) 0.83807(7) 0.0348(3) Uani d . 1 . . Cl Cl6 0.29916(8) 0.21558(13) 0.64515(7) 0.0321(2) Uani d . 1 . . Cl P1 0.38721(7) 0.07149(12) 0.72910(7) 0.0225(2) Uani d . 1 . . P N1 0.5000 0.1287(6) 0.7500 0.0370(13) Uani d S 1 . . N loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ta1 0.02090(15) 0.01762(16) 0.01829(16) -0.00047(7) 0.00553(10) -0.00070(7) Cl1 0.0359(6) 0.0331(6) 0.0183(5) -0.0020(4) 0.0038(4) 0.0012(4) Cl2 0.0248(5) 0.0325(6) 0.0340(5) 0.0014(4) 0.0111(4) -0.0050(5) Cl3 0.0342(5) 0.0196(5) 0.0342(5) -0.0025(4) 0.0070(4) -0.0014(4) Cl4 0.0365(6) 0.0271(6) 0.0625(8) -0.0012(5) 0.0079(5) -0.0178(5) Cl5 0.0380(6) 0.0379(7) 0.0311(5) -0.0031(5) 0.0134(4) 0.0057(5) Cl6 0.0295(5) 0.0343(6) 0.0312(5) 0.0045(4) 0.0044(4) 0.0079(4) P1 0.0185(4) 0.0185(6) 0.0311(5) -0.0004(4) 0.0070(4) 0.0000(4) N1 0.020(2) 0.026(3) 0.064(4) 0.000 0.009(2) 0.000 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ta1 Cl1 . 2.3428(11) y Ta1 Cl3 . 2.3484(10) y Ta1 Cl2 . 2.3559(9) y Cl4 P1 . 1.9586(15) ? Cl5 P1 . 1.9532(14) ? Cl6 P1 . 1.9460(14) ? P1 N1 . 1.546(2) y loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Ta1 Cl1 . 5_666 180.0 ? Cl1 Ta1 Cl3 . . 89.37(4) y Cl1 Ta1 Cl3 5_666 . 90.63(4) y Cl1 Ta1 Cl3 . 5_666 90.63(4) ? Cl1 Ta1 Cl3 5_666 5_666 89.37(4) ? Cl3 Ta1 Cl3 . 5_666 180.0 ? Cl1 Ta1 Cl2 . . 90.01(4) ? Cl1 Ta1 Cl2 5_666 . 89.99(4) ? Cl3 Ta1 Cl2 . . 90.36(4) ? Cl3 Ta1 Cl2 5_666 . 89.64(4) ? Cl1 Ta1 Cl2 . 5_666 89.99(4) ? Cl1 Ta1 Cl2 5_666 5_666 90.01(4) ? Cl3 Ta1 Cl2 . 5_666 89.64(4) ? Cl3 Ta1 Cl2 5_666 5_666 90.36(4) ? Cl2 Ta1 Cl2 . 5_666 180.0 ? N1 P1 Cl6 . . 110.14(17) y N1 P1 Cl5 . . 112.33(7) y Cl6 P1 Cl5 . . 105.88(6) y N1 P1 Cl4 . . 113.59(18) y Cl6 P1 Cl4 . . 107.76(7) y Cl5 P1 Cl4 . . 106.74(7) y P1 N1 P1 . 2_656 143.3(4) y 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl6 P1 N1 P1 2_656 -146.05(8) y Cl5 P1 N1 P1 2_656 96.20(10) ? Cl4 P1 N1 P1 2_656 -25.08(7) ? _cod_database_fobs_code 2012954