#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012956.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_2012956 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)2 [Zr2 Cl10]' _chemical_formula_moiety '(Cl6 N P2 2+)2, Cl10 Zr2 2-' _chemical_formula_sum 'Cl22 N2 P4 Zr2' _chemical_formula_weight 1114.24 _chemical_name_systematic ;Bis[bis(trichlorophosphino)iminium] di-\m-chloro-bis[tetrachlorozirconium(IV)] ; _space_group_IT_number 64 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2ac 2' _symmetry_space_group_name_H-M 'C m c a' _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 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.0456(4) _cell_length_b 11.4295(6) _cell_length_c 15.7039(5) _cell_measurement_reflns_used 7047 _cell_measurement_temperature 250.0(10) _cell_measurement_theta_max 26.5 _cell_measurement_theta_min 3.3 _cell_volume 3239.0(2) _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 250.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _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 0.051 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7407 _diffrn_reflns_theta_full 26.51 _diffrn_reflns_theta_max 26.51 _diffrn_reflns_theta_min 3.34 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.660 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_correction_T_min 0.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO--SMN; Otwinowski & Minor, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2112 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.398 _refine_diff_density_min -0.403 _refine_ls_extinction_coef 0.00067(9) _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 1.063 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 76 _refine_ls_number_reflns 1725 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0299 _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^)+(0.0297P)^2^+3.2260P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.0739 _reflns_number_gt 1386 _reflns_number_total 1725 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sk1570.cif _[local]_cod_data_source_block IV _[local]_cod_cif_authors_sg_Hall '-C 2bc 2' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012956 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' 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 Zr1 0.0000 0.15039(3) 0.56964(2) 0.03063(15) Uani d S 1 . . Zr Cl1 0.0000 0.07877(9) 0.41179(7) 0.0422(3) Uani d S 1 . . Cl Cl2 0.0000 0.17037(11) 0.72136(7) 0.0470(3) Uani d S 1 . . Cl Cl3 0.13433(5) 0.14417(8) 0.56419(6) 0.0552(3) Uani d . 1 . . Cl Cl4 0.0000 0.34968(10) 0.52937(9) 0.0537(3) Uani d S 1 . . Cl Cl5 0.11584(6) 0.40936(9) 0.73073(7) 0.0635(3) Uani d . 1 . . Cl Cl6 0.14964(6) 0.63068(9) 0.61942(6) 0.0614(3) Uani d . 1 . . Cl Cl7 0.24468(6) 0.40472(8) 0.59714(6) 0.0588(3) Uani d . 1 . . Cl P1 0.19578(5) 0.50311(8) 0.68220(5) 0.0385(2) Uani d . 1 . . P N1 0.2500 0.5532(3) 0.7500 0.0401(9) 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 Zr1 0.0313(3) 0.0286(2) 0.0319(2) 0.000 0.000 -0.00253(16) Cl1 0.0650(8) 0.0310(5) 0.0306(5) 0.000 0.000 -0.0006(4) Cl2 0.0627(8) 0.0454(7) 0.0329(6) 0.000 0.000 -0.0031(5) Cl3 0.0321(5) 0.0592(6) 0.0743(6) 0.0003(4) 0.0017(4) -0.0189(5) Cl4 0.0711(9) 0.0328(6) 0.0570(7) 0.000 0.000 0.0092(5) Cl5 0.0547(6) 0.0701(7) 0.0656(6) -0.0202(5) 0.0057(5) 0.0059(5) Cl6 0.0643(6) 0.0631(6) 0.0567(5) 0.0129(5) -0.0102(5) 0.0139(5) Cl7 0.0741(7) 0.0578(6) 0.0446(5) 0.0040(5) 0.0047(4) -0.0150(4) P1 0.0428(5) 0.0395(5) 0.0332(4) -0.0012(4) 0.0001(3) 0.0004(3) N1 0.047(2) 0.040(2) 0.0335(19) 0.000 -0.0014(16) 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 Zr1 Cl4 . 2.3640(12) y Zr1 Cl2 . 2.3935(11) ? Zr1 Cl3 . 2.4266(9) y Zr1 Cl1 . 2.6106(11) y Zr1 Cl1 9_556 2.6354(12) y Cl5 P1 . 1.9520(12) ? Cl6 P1 . 1.9471(12) ? Cl7 P1 . 1.9565(12) ? P1 N1 . 1.5554(16) 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' Zr Zr -2.9673 0.5597 '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 Cl4 Zr1 Cl2 . . 100.04(5) y Cl4 Zr1 Cl3 . . 91.08(3) ? Cl2 Zr1 Cl3 . . 92.17(2) ? Cl4 Zr1 Cl3 . 12 91.08(3) ? Cl2 Zr1 Cl3 . 12 92.17(2) ? Cl3 Zr1 Cl3 . 12 174.74(5) y Cl4 Zr1 Cl1 . . 92.76(4) ? Cl2 Zr1 Cl1 . . 167.20(4) y Cl3 Zr1 Cl1 . . 87.55(2) ? Cl3 Zr1 Cl1 12 . 87.55(2) ? Cl4 Zr1 Cl1 . 9_556 170.84(4) y Cl2 Zr1 Cl1 . 9_556 89.12(4) ? Cl3 Zr1 Cl1 . 9_556 88.55(2) ? Cl3 Zr1 Cl1 12 9_556 88.55(2) ? Cl1 Zr1 Cl1 . 9_556 78.08(4) y Zr1 Cl1 Zr1 . 9_556 101.92(4) y N1 P1 Cl6 . . 109.86(14) y N1 P1 Cl5 . . 113.57(8) y Cl6 P1 Cl5 . . 107.02(6) ? N1 P1 Cl7 . . 113.29(9) y Cl6 P1 Cl7 . . 106.12(6) ? Cl5 P1 Cl7 . . 106.52(6) ? P1 N1 P1 . 7_546 136.8(3) 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_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cl4 Zr1 Cl1 Zr1 . 9_556 180.0 ? Cl2 Zr1 Cl1 Zr1 . 9_556 0.0 ? Cl3 Zr1 Cl1 Zr1 . 9_556 89.04(3) ? Cl3 Zr1 Cl1 Zr1 12 9_556 -89.04(3) ? Cl1 Zr1 Cl1 Zr1 9_556 9_556 0.0 ? Cl6 P1 N1 P1 . 7_546 -178.31(6) y Cl5 P1 N1 P1 . 7_546 61.88(7) y Cl7 P1 N1 P1 . 7_546 -59.83(7) y _cod_database_fobs_code 2012956 _journal_paper_doi 10.1107/S0108270102012532