data_[PCl2N]3_[HAlBr4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cl6 H N3 P3, Al Br4' _chemical_formula_sum 'Al Br4 Cl6 H N3 P3' _chemical_formula_weight 695.27 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' 'Al' 'Al' 0.0645 0.0514 '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' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6721(9) _cell_length_b 9.9263(12) _cell_length_c 12.3245(14) _cell_angle_alpha 84.643(2) _cell_angle_beta 85.055(2) _cell_angle_gamma 73.178(2) _cell_volume 892.77(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2643 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.07 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 10.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4283 _exptl_absorpt_correction_T_max 0.7492 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7222 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.30 _reflns_number_total 3598 _reflns_number_gt 3078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.2688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3598 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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 _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.31450(5) 0.52324(4) 0.39479(3) 0.01713(11) Uani 1 1 d . . . Br2 Br 0.00541(6) 0.87531(5) 0.30409(4) 0.02286(12) Uani 1 1 d . . . Br3 Br 0.47310(6) 0.74444(5) 0.16211(3) 0.02072(11) Uani 1 1 d . . . Br4 Br 0.42671(7) 0.84950(5) 0.45091(4) 0.02542(12) Uani 1 1 d . . . Cl1 Cl 0.85699(14) 0.54418(11) 0.32196(8) 0.0187(2) Uani 1 1 d . . . Cl2 Cl 1.03815(14) 0.23421(11) 0.40722(8) 0.0216(2) Uani 1 1 d . . . Cl3 Cl 0.43673(14) 0.38182(11) 0.11952(8) 0.0221(2) Uani 1 1 d . . . Cl4 Cl 0.54343(14) 0.09330(11) 0.25415(9) 0.0226(2) Uani 1 1 d . . . Cl5 Cl 0.97657(15) 0.35097(12) -0.05991(8) 0.0244(2) Uani 1 1 d . . . Cl6 Cl 1.19503(14) 0.07086(11) 0.05708(9) 0.0247(2) Uani 1 1 d . . . P1 P 0.90849(14) 0.34868(12) 0.28472(8) 0.0144(2) Uani 1 1 d . . . P2 P 0.64559(14) 0.24190(11) 0.18548(9) 0.0146(2) Uani 1 1 d . . . P3 P 0.98380(14) 0.23591(11) 0.08046(9) 0.0145(2) Uani 1 1 d . . . Al1 Al 0.30481(17) 0.75088(13) 0.32590(10) 0.0160(3) Uani 1 1 d . . . N1 N 0.7080(5) 0.3170(4) 0.2838(3) 0.0210(9) Uani 1 1 d . . . H1 H 0.630(7) 0.347(6) 0.330(4) 0.049(18) Uiso 1 1 d . . . N2 N 0.8066(4) 0.1847(4) 0.1008(3) 0.0166(8) Uani 1 1 d . . . N3 N 1.0191(4) 0.3232(4) 0.1731(3) 0.0178(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0153(2) 0.0151(2) 0.0196(2) 0.00007(16) 0.00123(16) -0.00321(17) Br2 0.0183(2) 0.0215(2) 0.0235(2) 0.00100(18) -0.00119(18) 0.00186(18) Br3 0.0202(2) 0.0225(2) 0.0160(2) 0.00109(17) 0.00162(17) -0.00216(18) Br4 0.0373(3) 0.0270(3) 0.0185(2) -0.00125(19) -0.0050(2) -0.0186(2) Cl1 0.0206(5) 0.0164(5) 0.0193(5) -0.0030(4) -0.0013(4) -0.0050(4) Cl2 0.0229(6) 0.0216(6) 0.0185(5) 0.0027(4) -0.0046(4) -0.0041(5) Cl3 0.0187(5) 0.0227(6) 0.0223(6) -0.0003(4) -0.0032(4) -0.0019(4) Cl4 0.0219(6) 0.0238(6) 0.0249(6) 0.0041(5) -0.0010(4) -0.0131(5) Cl5 0.0320(6) 0.0258(6) 0.0155(5) 0.0031(4) -0.0001(5) -0.0101(5) Cl6 0.0181(5) 0.0187(6) 0.0337(6) -0.0049(5) 0.0030(5) 0.0000(4) P1 0.0131(5) 0.0182(6) 0.0134(5) -0.0019(4) -0.0006(4) -0.0066(4) P2 0.0132(5) 0.0167(6) 0.0149(5) -0.0011(4) -0.0013(4) -0.0061(4) P3 0.0140(5) 0.0159(6) 0.0132(5) -0.0009(4) 0.0010(4) -0.0043(4) Al1 0.0174(7) 0.0154(6) 0.0146(6) -0.0006(5) -0.0017(5) -0.0036(5) N1 0.0148(19) 0.036(2) 0.017(2) -0.0087(17) 0.0057(16) -0.0134(18) N2 0.0153(18) 0.0195(19) 0.0154(18) -0.0055(15) 0.0013(14) -0.0049(15) N3 0.0150(18) 0.023(2) 0.0176(19) -0.0045(15) 0.0032(15) -0.0099(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Al1 2.3212(13) . ? Br2 Al1 2.2971(13) . ? Br3 Al1 2.2963(13) . ? Br4 Al1 2.2949(13) . ? Cl1 P1 1.9555(15) . ? Cl2 P1 1.9607(15) . ? Cl3 P2 1.9706(15) . ? Cl4 P2 1.9565(15) . ? Cl5 P3 1.9777(15) . ? Cl6 P3 1.9658(15) . ? P1 N3 1.554(3) . ? P1 N1 1.658(4) . ? P2 N2 1.555(3) . ? P2 N1 1.652(4) . ? P3 N2 1.577(3) . ? P3 N3 1.582(3) . ? 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_3 _geom_angle_publ_flag N3 P1 N1 111.71(18) . . ? N3 P1 Cl1 111.86(14) . . ? N1 P1 Cl1 106.34(15) . . ? N3 P1 Cl2 113.07(15) . . ? N1 P1 Cl2 108.24(15) . . ? Cl1 P1 Cl2 105.18(6) . . ? N2 P2 N1 111.94(18) . . ? N2 P2 Cl4 112.26(14) . . ? N1 P2 Cl4 107.59(14) . . ? N2 P2 Cl3 112.93(14) . . ? N1 P2 Cl3 107.36(15) . . ? Cl4 P2 Cl3 104.30(7) . . ? N2 P3 N3 115.27(18) . . ? N2 P3 Cl6 108.67(14) . . ? N3 P3 Cl6 110.26(14) . . ? N2 P3 Cl5 110.06(14) . . ? N3 P3 Cl5 108.44(14) . . ? Cl6 P3 Cl5 103.50(7) . . ? Br4 Al1 Br3 109.99(5) . . ? Br4 Al1 Br2 110.47(5) . . ? Br3 Al1 Br2 110.64(5) . . ? Br4 Al1 Br1 107.41(5) . . ? Br3 Al1 Br1 109.93(5) . . ? Br2 Al1 Br1 108.32(5) . . ? P2 N1 P1 124.7(2) . . ? P2 N2 P3 125.5(2) . . ? P1 N3 P3 126.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 Br1 0.80(5) 2.65(5) 3.378(4) 151(5) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.892 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.133