Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Thomas M. Klapotke' _publ_contact_author_address ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; loop_ _publ_author_name _publ_author_address 'Christoph Aubuauer' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Martin Kaupp' ; Institut fur Anorganische Chemie Universitat Wurzburg Am Hubland D-97074 Wurzburg Bundesrepublik Deutschland ; 'Thomas M. Klapotke' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Heinrich Noth' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Holger Piotrowski' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Wolfgang Schnick' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Jurgen Senker' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; 'Max Suter' ; Department Chemie Ludwig-Maximilians Universitat Butenandtstrase 5-13 (Haus D) D-81377 Munchen Bundesrepublik Deutschland ; _publ_contact_author_email 'tmk@cup.uni-muenchen.de' _publ_contact_author_fax 'Int+ 089-2180-7492' _publ_contact_author_phone 'Int+ 089-2180-7491' _publ_section_title ; Characterisation of the Tetrahalophosphonium Cations PBr~n~I~4-n~ (02sigma(I) _reflns_special_details ? _computing_data_collection 'Stoe IPDS software (Darmstadt, Germany)' _computing_cell_refinement 'Stoe IPDS software (Darmstadt, Germany)' _computing_data_reduction 'Stoe IPDS software (Darmstadt, Germany)' _computing_structure_solution ; SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79) ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0389P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 3879 _refine_ls_number_parameters 91 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_special_details ? 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 P P -0.0464(2) -0.5105(4) 0.2044(2) 0.0256(7) Uani 1 1 d . . . I1 I 0.03737(7) -0.62645(9) 0.08063(6) 0.0306(2) Uani 1 1 d . . . I2 I 0.06505(7) -0.57903(10) 0.33380(6) 0.0334(2) Uani 1 1 d . . . I3 I -0.26105(6) -0.54865(10) 0.22338(6) 0.0319(2) Uani 1 1 d . . . I4 I -0.01725(10) -0.28570(11) 0.18497(8) 0.0513(3) Uani 1 1 d . . . Ga Ga 0.40830(10) -0.50231(14) 0.41342(9) 0.0210(3) Uani 1 1 d . . . I5 I 0.42975(6) -0.56122(9) 0.24958(5) 0.02693(19) Uani 1 1 d . . . I6 I 0.60787(7) -0.50031(10) 0.49336(6) 0.03190(19) Uani 1 1 d . . . I7 I 0.30189(8) -0.28604(9) 0.42190(7) 0.0371(2) Uani 1 1 d . . . I8 I 0.27157(8) -0.67136(11) 0.48364(7) 0.0427(3) 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 P 0.0234(12) 0.0288(19) 0.0245(16) -0.0047(15) 0.0053(12) -0.0064(12) I1 0.0333(4) 0.0347(5) 0.0240(4) -0.0062(4) 0.0047(3) -0.0025(4) I2 0.0313(4) 0.0426(6) 0.0264(4) -0.0046(4) -0.0003(3) -0.0106(4) I3 0.0246(3) 0.0371(5) 0.0339(5) -0.0006(4) 0.0059(3) -0.0042(3) I4 0.0592(6) 0.0307(6) 0.0639(9) 0.0001(5) -0.0007(5) -0.0169(5) Ga 0.0240(5) 0.0208(7) 0.0182(7) -0.0018(6) 0.0014(5) -0.0026(5) I5 0.0280(3) 0.0328(5) 0.0200(4) -0.0062(4) 0.0035(3) -0.0004(3) I6 0.0287(3) 0.0337(5) 0.0333(5) 0.0010(5) -0.0086(3) -0.0019(3) I7 0.0424(4) 0.0302(5) 0.0389(5) -0.0131(5) -0.0120(4) 0.0109(4) I8 0.0409(4) 0.0525(7) 0.0346(5) 0.0174(5) -0.0032(4) -0.0219(4) 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 P I4 2.378(4) . ? P I3 2.414(3) . ? P I1 2.416(4) . ? P I2 2.423(4) . ? Ga I6 2.5103(13) . ? Ga I7 2.5395(17) . ? Ga I8 2.5484(16) . ? Ga I5 2.5728(16) . ? 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 I4 P I3 107.97(14) . . ? I4 P I1 110.04(14) . . ? I3 P I1 112.62(14) . . ? I4 P I2 108.75(14) . . ? I3 P I2 110.53(14) . . ? I1 P I2 106.89(13) . . ? I6 Ga I7 111.83(6) . . ? I6 Ga I8 108.69(6) . . ? I7 Ga I8 108.50(6) . . ? I6 Ga I5 112.90(5) . . ? I7 Ga I5 107.60(6) . . ? I8 Ga I5 107.12(6) . . ? 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 ? ? ? ? ? ? ? ? ? ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? data_d:\auba7\work\auba7 _database_code_CSD 158051 _publ_manuscript_creation 'RTF-File by CIFRTF (H.Schwenk 1996)' _audit_creation_method 'SHELXL-CIF-file updated by CIFRTF' _chemical_name_systematic ; Tetraiodophosphonium tetrachloroaluminate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al Cl4 I4 P' _chemical_formula_weight 707.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.523(6) _cell_length_b 15.808(14) _cell_length_c 14.339(13) _cell_angle_alpha 90 _cell_angle_beta 92.092(14) _cell_angle_gamma 90 _cell_volume 1478(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 348 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 9.277 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.04927 _exptl_absorpt_correction_T_max 0.09772 _exptl_absorpt_process_details ? _exptl_special_details ; Diffractometer operator M. Suter scanspeed_seconds/frame 10 1200 frames measured in phi (0-360) with chi=0 and om=2th=25 65 frames measured in om (15-35) with chi=280, 2th=29 and phi=0 Crystal mounted in perfluorpolyetheroil ; _diffrn_ambient_temperature 193(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 'Siemens SMART Area-detector' _diffrn_measurement_method Hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5309 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 21.26 _reflns_number_total 1627 _reflns_number_gt 1292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (V4.C50)' _computing_cell_refinement 'SMART (V4.C50)' _computing_data_reduction 'SAINT (V4.D50)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (SHELXTL-Ver.5)' _computing_publication_material 'SHELXL (Sheldrick 1997)' _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^)+(0.0491P)^2^+18.0112P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy-atom-method _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometrically _refine_ls_hydrogen_treatment 'mixed ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1627 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _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 I1 I 0.2734(2) 0.82862(8) 0.42735(9) 0.0795(5) Uani 1 1 d . . . I2 I 0.73321(18) 0.78727(8) 0.60100(8) 0.0678(4) Uani 1 1 d . . . I3 I 0.64522(17) 0.64162(7) 0.38689(7) 0.0555(4) Uani 1 1 d . . . I4 I 0.2693(2) 0.63285(7) 0.58626(10) 0.0853(5) Uani 1 1 d . . . Cl1 Cl 1.1607(7) 0.6446(3) 0.2134(3) 0.0790(15) Uani 1 1 d . A . Cl2 Cl 0.7575(6) 0.5058(2) 0.2201(3) 0.0508(10) Uani 1 1 d . A . Cl3B Cl 1.166(8) 0.485(3) 0.376(3) 0.057(9) Uani 0.36(8) 1 d P A 1 Cl4B Cl 1.208(3) 0.410(4) 0.155(5) 0.082(16) Uani 0.36(8) 1 d P A 1 Cl3A Cl 1.188(7) 0.467(3) 0.356(3) 0.110(12) Uani 0.64(8) 1 d P A 2 Cl4A Cl 1.195(2) 0.452(3) 0.110(3) 0.093(8) Uani 0.64(8) 1 d P A 2 P5 P 0.4806(6) 0.7234(2) 0.5009(3) 0.0435(10) Uani 1 1 d . . . Al1 Al 1.0856(7) 0.5145(3) 0.2301(3) 0.0538(12) 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 I1 0.1032(11) 0.0561(8) 0.0778(8) 0.0096(6) -0.0138(7) 0.0281(7) I2 0.0701(8) 0.0719(8) 0.0611(7) -0.0194(6) -0.0031(6) -0.0066(6) I3 0.0614(7) 0.0559(7) 0.0497(6) -0.0077(5) 0.0088(5) 0.0052(6) I4 0.1046(11) 0.0387(7) 0.1169(11) 0.0076(6) 0.0626(8) -0.0017(7) Cl1 0.073(3) 0.067(3) 0.095(3) 0.037(3) -0.028(3) -0.027(3) Cl2 0.045(2) 0.044(2) 0.063(2) -0.0020(18) 0.0008(18) -0.0050(18) Cl3B 0.063(14) 0.049(15) 0.057(14) 0.027(11) -0.018(8) -0.023(12) Cl4B 0.037(10) 0.09(3) 0.11(3) -0.05(2) 0.016(10) 0.003(10) Cl3A 0.105(15) 0.083(17) 0.14(2) 0.043(14) -0.046(15) -0.018(11) Cl4A 0.080(7) 0.093(16) 0.107(16) -0.049(13) 0.028(7) 0.006(7) P5 0.048(2) 0.035(2) 0.047(2) 0.0020(17) 0.0045(18) 0.0003(18) Al1 0.052(3) 0.046(3) 0.064(3) -0.009(2) 0.002(2) -0.004(2) _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 I1 P5 2.367(4) . ? I2 P5 2.372(4) . ? I3 P5 2.371(4) . ? I4 P5 2.361(4) . ? Cl1 Al1 2.129(6) . ? Cl2 Al1 2.144(6) . ? Cl3B Al1 2.18(4) . ? Cl4B Al1 2.14(3) . ? Cl3A Al1 2.05(4) . ? Cl4A Al1 2.134(16) . ? 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 I4 P5 I1 108.79(17) . . ? I4 P5 I3 108.36(16) . . ? I1 P5 I3 109.99(16) . . ? I4 P5 I2 110.50(16) . . ? I1 P5 I2 110.07(16) . . ? I3 P5 I2 109.12(17) . . ? Cl3A Al1 Cl1 112.5(12) . . ? Cl3A Al1 Cl4A 115.8(11) . . ? Cl1 Al1 Cl4A 105.9(13) . . ? Cl3A Al1 Cl4B 92.8(15) . . ? Cl1 Al1 Cl4B 127(2) . . ? Cl4A Al1 Cl4B 24.9(11) . . ? Cl3A Al1 Cl2 109.1(12) . . ? Cl1 Al1 Cl2 106.8(3) . . ? Cl4A Al1 Cl2 106.3(5) . . ? Cl4B Al1 Cl2 107.8(6) . . ? Cl3A Al1 Cl3B 11(2) . . ? Cl1 Al1 Cl3B 105.2(13) . . ? Cl4A Al1 Cl3B 126.7(18) . . ? Cl4B Al1 Cl3B 104(2) . . ? Cl2 Al1 Cl3B 104.8(13) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 21.26 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.299 _refine_diff_density_min -1.587 _refine_diff_density_rms 0.167 data_d:\r?ntgen\auba5\auba5 _database_code_CSD 158052 _publ_manuscript_creation 'RTF-File by CIFRTF (H.Schwenk 1996)' _audit_creation_method 'SHELXL-CIF-file updated by CIFRTF' _chemical_name_systematic 'tetraiodophosphonium-tetrabromoaluminate' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al Br4 I4 P' _chemical_formula_weight 885.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.6475(8) _cell_length_b 16.471(2) _cell_length_c 14.5339(19) _cell_angle_alpha 90 _cell_angle_beta 91.832(2) _cell_angle_gamma 90 _cell_volume 1590.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needls _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 17.996 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.0298 _exptl_absorpt_correction_T_max 0.0666 _exptl_absorpt_process_details ? _exptl_special_details ; Diffractometer operator M. Suter scanspeed_seconds/frame 5 1200 frames measured in phi (0-360) with chi=0 and om=2th=25 65 frames measured in om (15-35) with chi=280, 2th=29 and phi=0 Crystal mounted in perfluorpolyetheroil ; _diffrn_ambient_temperature 188(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 'Siemens SMART Area-detector' _diffrn_measurement_method Hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 6541 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 22.71 _reflns_number_total 2056 _reflns_number_gt 1673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (V4.C50)' _computing_cell_refinement 'SMART (V4.C50)' _computing_data_reduction 'SAINT (V4.D50)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (SHELXTL-Ver.5)' _computing_publication_material 'SHELXL (Sheldrick 1997)' _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^)+(0.0585P)^2^+14.9708P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometrically _refine_ls_hydrogen_treatment 'mixed ' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2056 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _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 I1 I 0.27343(15) 0.27773(6) 0.39943(7) 0.0574(3) Uani 1 1 d . . . I2 I 0.36822(15) 0.14141(6) 0.61508(6) 0.0580(3) Uani 1 1 d . . . I3 I 0.74647(18) 0.13331(6) 0.42088(9) 0.0721(4) Uani 1 1 d . . . I4 I 0.72084(19) 0.32640(6) 0.56889(8) 0.0763(4) Uani 1 1 d . . . Br1 Br -0.1744(3) 0.52900(11) 0.13675(14) 0.0796(6) Uani 1 1 d . A . Br3 Br -0.1456(2) 0.34510(9) 0.28582(11) 0.0646(5) Uani 1 1 d . A . Br4 Br 0.2804(2) 0.49213(8) 0.28698(10) 0.0505(4) Uani 1 1 d . A . P1 P 0.5250(5) 0.2206(2) 0.5000(2) 0.0426(8) Uani 1 1 d . . . Al1 Al -0.0664(6) 0.4817(2) 0.2780(3) 0.0495(11) Uani 1 1 d . . . Br2A Br -0.191(3) 0.575(5) 0.375(6) 0.100(16) Uani 0.33(9) 1 d P A 1 Br2B Br -0.1942(17) 0.5449(15) 0.4046(10) 0.083(2) Uani 0.67(9) 1 d P A 2 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 I1 0.0630(7) 0.0514(6) 0.0571(6) 0.0087(4) -0.0117(5) 0.0023(5) I2 0.0613(7) 0.0604(7) 0.0522(6) 0.0084(4) -0.0009(5) -0.0066(5) I3 0.0820(8) 0.0395(6) 0.0963(9) -0.0027(5) 0.0291(6) 0.0050(5) I4 0.1024(10) 0.0488(6) 0.0759(7) -0.0030(5) -0.0273(7) -0.0205(6) Br1 0.0732(12) 0.0653(11) 0.0979(13) 0.0369(10) -0.0339(10) -0.0220(9) Br3 0.0623(10) 0.0504(9) 0.0794(11) 0.0205(8) -0.0239(8) -0.0148(8) Br4 0.0438(9) 0.0429(8) 0.0643(9) -0.0050(6) -0.0042(7) -0.0023(6) P1 0.047(2) 0.0336(19) 0.0469(19) 0.0006(15) -0.0033(16) -0.0014(16) Al1 0.049(3) 0.040(2) 0.059(3) -0.0085(19) -0.009(2) 0.0011(19) Br2A 0.045(5) 0.12(2) 0.14(3) -0.09(2) 0.011(7) -0.006(7) Br2B 0.073(4) 0.089(6) 0.089(5) -0.040(4) 0.009(2) 0.000(3) _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 I1 P1 2.380(4) . ? I2 P1 2.387(4) . ? I3 P1 2.381(4) . ? I4 P1 2.376(3) . ? Br1 Al1 2.290(5) . ? Br3 Al1 2.314(4) . ? Br4 Al1 2.312(5) . ? Al1 Br2A 2.259(18) . ? Al1 Br2B 2.299(11) . ? 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 I4 P1 I1 109.51(13) . . ? I4 P1 I3 107.90(15) . . ? I1 P1 I3 112.03(14) . . ? I4 P1 I2 110.58(14) . . ? I1 P1 I2 109.42(15) . . ? I3 P1 I2 107.38(13) . . ? Br2A Al1 Br1 102(3) . . ? Br2A Al1 Br2B 17(2) . . ? Br1 Al1 Br2B 116.8(5) . . ? Br2A Al1 Br4 107.4(5) . . ? Br1 Al1 Br4 108.0(2) . . ? Br2B Al1 Br4 108.3(3) . . ? Br2A Al1 Br3 123(3) . . ? Br1 Al1 Br3 108.02(17) . . ? Br2B Al1 Br3 108.1(7) . . ? Br4 Al1 Br3 107.30(17) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 22.71 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.873 _refine_diff_density_min -1.840 _refine_diff_density_rms 0.225