# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1273 data_fg2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 Al4 Cl4 F8' _chemical_formula_weight 605.98 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' '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 9.832(2) _cell_length_b 9.8549(16) _cell_length_c 25.692(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.40(2) _cell_angle_gamma 90.00 _cell_volume 2484.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irreg. plat' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.681 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13194 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.23 _reflns_number_total 3549 _reflns_number_gt 2505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0401P)^2^+0.8610P] 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 3549 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Al1 Al 0.27647(12) -0.01973(11) 0.32917(4) 0.0421(3) Uani 1 1 d . . . Al2 Al 0.19767(11) 0.28821(11) 0.27129(4) 0.0393(3) Uani 1 1 d . . . Al3 Al 0.22845(11) 0.14895(11) 0.46680(4) 0.0372(3) Uani 1 1 d . . . Al4 Al 0.13106(10) 0.45269(10) 0.40723(4) 0.0352(3) Uani 1 1 d . . . Cl12 Cl 0.08925(9) 0.09939(9) 0.29888(4) 0.0433(3) Uani 1 1 d . . . Cl13 Cl 0.23870(10) -0.04042(9) 0.41556(4) 0.0473(3) Uani 1 1 d . . . Cl24 Cl 0.09188(9) 0.44905(9) 0.31808(3) 0.0421(3) Uani 1 1 d . . . Cl34 Cl 0.03811(8) 0.25100(9) 0.42909(4) 0.0391(2) Uani 1 1 d . . . C1 C 0.2635(4) -0.2013(4) 0.30108(16) 0.0602(12) Uani 1 1 d . . . H1A H 0.3551 -0.2398 0.2995 0.090 Uiso 1 1 calc R . . H1B H 0.2192 -0.1983 0.2659 0.090 Uiso 1 1 calc R . . H1C H 0.2096 -0.2578 0.3235 0.090 Uiso 1 1 calc R . . C2 C 0.1493(4) 0.3147(4) 0.19819(14) 0.0561(11) Uani 1 1 d . . . H2A H 0.1997 0.2500 0.1777 0.084 Uiso 1 1 calc R . . H2B H 0.1725 0.4074 0.1882 0.084 Uiso 1 1 calc R . . H2C H 0.0512 0.3000 0.1915 0.084 Uiso 1 1 calc R . . C3 C 0.1906(4) 0.0811(4) 0.53451(14) 0.0520(11) Uani 1 1 d . . . H3A H 0.1663 0.1568 0.5569 0.078 Uiso 1 1 calc R . . H3B H 0.2715 0.0350 0.5500 0.078 Uiso 1 1 calc R . . H3C H 0.1145 0.0168 0.5311 0.078 Uiso 1 1 calc R . . C4 C 0.0218(4) 0.6013(4) 0.42860(15) 0.0489(10) Uani 1 1 d . . . H4A H 0.0302 0.6094 0.4667 0.073 Uiso 1 1 calc R . . H4B H -0.0737 0.5851 0.4172 0.073 Uiso 1 1 calc R . . H4C H 0.0531 0.6854 0.4129 0.073 Uiso 1 1 calc R . . C11 C 0.4142(4) 0.1214(4) 0.32298(13) 0.0399(9) Uani 1 1 d . . . C12 C 0.3802(4) 0.2525(4) 0.30274(14) 0.0396(9) Uani 1 1 d . . . C13 C 0.4820(4) 0.3480(4) 0.30277(16) 0.0531(11) Uani 1 1 d . . . C14 C 0.6152(4) 0.3200(5) 0.32247(18) 0.0644(14) Uani 1 1 d . . . C15 C 0.6457(4) 0.1932(6) 0.34055(18) 0.0656(13) Uani 1 1 d . . . C16 C 0.5470(4) 0.0984(5) 0.34070(16) 0.0554(11) Uani 1 1 d . . . C21 C 0.3626(3) 0.2863(3) 0.44954(13) 0.0355(9) Uani 1 1 d . . . C22 C 0.3232(3) 0.4140(3) 0.42726(13) 0.0337(9) Uani 1 1 d . . . C23 C 0.4222(4) 0.5097(4) 0.42117(14) 0.0417(10) Uani 1 1 d . . . C24 C 0.5584(4) 0.4882(4) 0.43512(15) 0.0509(11) Uani 1 1 d . . . C25 C 0.5976(4) 0.3661(5) 0.45608(16) 0.0509(11) Uani 1 1 d . . . C26 C 0.5003(4) 0.2681(4) 0.46321(15) 0.0463(10) Uani 1 1 d . . . F13 F 0.4527(3) 0.4748(2) 0.28429(10) 0.0779(8) Uani 1 1 d . . . F14 F 0.7096(3) 0.4199(3) 0.32216(11) 0.1012(11) Uani 1 1 d . . . F15 F 0.7756(2) 0.1668(3) 0.35791(11) 0.1058(11) Uani 1 1 d . . . F16 F 0.5810(2) -0.0278(3) 0.35946(10) 0.0837(8) Uani 1 1 d . . . F23 F 0.3873(2) 0.6338(2) 0.40108(9) 0.0625(7) Uani 1 1 d . . . F24 F 0.6520(2) 0.5852(2) 0.42791(10) 0.0719(8) Uani 1 1 d . . . F25 F 0.7295(2) 0.3424(3) 0.46978(10) 0.0793(8) Uani 1 1 d . . . F26 F 0.5423(2) 0.1484(2) 0.48443(10) 0.0717(7) 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 Al1 0.0515(8) 0.0362(7) 0.0386(7) 0.0019(5) 0.0033(6) 0.0085(5) Al2 0.0432(7) 0.0360(6) 0.0386(7) 0.0041(5) 0.0019(5) 0.0012(5) Al3 0.0399(7) 0.0351(6) 0.0359(7) 0.0024(5) -0.0031(5) 0.0063(5) Al4 0.0342(6) 0.0335(6) 0.0371(6) 0.0014(5) -0.0044(5) 0.0029(5) Cl12 0.0419(6) 0.0381(5) 0.0491(6) 0.0020(5) -0.0057(5) -0.0057(4) Cl13 0.0705(7) 0.0336(5) 0.0381(6) 0.0028(4) 0.0055(5) 0.0043(5) Cl24 0.0497(6) 0.0384(5) 0.0373(5) 0.0032(4) -0.0059(4) 0.0091(4) Cl34 0.0319(5) 0.0398(5) 0.0450(6) 0.0048(4) -0.0016(4) -0.0008(4) C1 0.087(3) 0.046(3) 0.049(3) -0.001(2) 0.015(2) 0.008(2) C2 0.066(3) 0.059(3) 0.044(3) 0.005(2) 0.001(2) 0.010(2) C3 0.061(3) 0.052(3) 0.043(2) 0.004(2) 0.000(2) 0.013(2) C4 0.047(2) 0.048(2) 0.050(3) -0.003(2) -0.002(2) 0.0065(19) C11 0.036(2) 0.055(3) 0.029(2) -0.0060(19) 0.0027(18) 0.0107(18) C12 0.037(2) 0.048(2) 0.035(2) -0.0077(19) 0.0073(18) -0.0005(19) C13 0.058(3) 0.051(3) 0.052(3) -0.012(2) 0.019(2) -0.009(2) C14 0.043(3) 0.091(4) 0.061(3) -0.039(3) 0.019(2) -0.028(3) C15 0.033(3) 0.103(4) 0.059(3) -0.025(3) -0.007(2) -0.001(3) C16 0.048(3) 0.075(3) 0.043(3) -0.003(2) 0.002(2) 0.016(3) C21 0.031(2) 0.044(2) 0.031(2) -0.0062(18) -0.0041(16) 0.0051(17) C22 0.031(2) 0.042(2) 0.028(2) -0.0058(17) -0.0024(16) -0.0026(17) C23 0.042(2) 0.045(2) 0.037(2) -0.0038(19) -0.0024(19) -0.0031(19) C24 0.039(3) 0.068(3) 0.047(3) -0.022(2) 0.010(2) -0.015(2) C25 0.023(2) 0.075(3) 0.053(3) -0.025(2) -0.0084(19) 0.002(2) C26 0.043(3) 0.048(3) 0.047(3) -0.010(2) -0.007(2) 0.013(2) F13 0.0813(19) 0.0569(17) 0.099(2) -0.0033(15) 0.0305(16) -0.0251(14) F14 0.0671(18) 0.131(3) 0.109(2) -0.062(2) 0.0302(17) -0.0552(18) F15 0.0392(16) 0.177(3) 0.099(2) -0.030(2) -0.0176(15) 0.0034(17) F16 0.0581(17) 0.105(2) 0.086(2) 0.0144(17) -0.0123(14) 0.0350(15) F23 0.0660(16) 0.0497(14) 0.0711(16) 0.0098(13) -0.0018(13) -0.0193(12) F24 0.0489(15) 0.0890(18) 0.0791(18) -0.0228(14) 0.0141(13) -0.0318(14) F25 0.0285(13) 0.109(2) 0.099(2) -0.0297(17) -0.0109(13) 0.0075(13) F26 0.0514(15) 0.0672(17) 0.094(2) 0.0012(15) -0.0219(14) 0.0267(12) _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 Al1 C1 1.930(4) . ? Al1 C11 1.954(4) . ? Al1 Cl12 2.2808(15) . ? Al1 Cl13 2.2812(16) . ? Al2 C2 1.927(4) . ? Al2 C12 1.955(4) . ? Al2 Cl24 2.2778(14) . ? Al2 Cl12 2.2784(14) . ? Al3 C3 1.921(4) . ? Al3 C21 1.959(4) . ? Al3 Cl34 2.2884(14) . ? Al3 Cl13 2.2894(14) . ? Al4 C4 1.915(4) . ? Al4 C22 1.966(3) . ? Al4 Cl34 2.2720(14) . ? Al4 Cl24 2.3003(15) . ? C11 C16 1.376(5) . ? C11 C12 1.425(5) . ? C12 C13 1.374(5) . ? C13 F13 1.362(5) . ? C13 C14 1.403(6) . ? C14 F14 1.354(5) . ? C14 C15 1.360(6) . ? C15 C16 1.348(6) . ? C15 F15 1.352(5) . ? C16 F16 1.368(5) . ? C21 C26 1.391(5) . ? C21 C22 1.426(5) . ? C22 C23 1.371(5) . ? C23 F23 1.363(4) . ? C23 C24 1.382(5) . ? C24 F24 1.347(4) . ? C24 C25 1.365(6) . ? C25 F25 1.344(4) . ? C25 C26 1.379(5) . ? C26 F26 1.353(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_3 _geom_angle_publ_flag C1 Al1 C11 131.30(17) . . ? C1 Al1 Cl12 108.38(14) . . ? C11 Al1 Cl12 98.90(12) . . ? C1 Al1 Cl13 105.66(13) . . ? C11 Al1 Cl13 107.24(11) . . ? Cl12 Al1 Cl13 101.73(6) . . ? C2 Al2 C12 126.45(17) . . ? C2 Al2 Cl24 109.04(13) . . ? C12 Al2 Cl24 110.09(12) . . ? C2 Al2 Cl12 108.71(13) . . ? C12 Al2 Cl12 99.17(12) . . ? Cl24 Al2 Cl12 99.63(6) . . ? C3 Al3 C21 127.95(16) . . ? C3 Al3 Cl34 109.80(13) . . ? C21 Al3 Cl34 98.33(11) . . ? C3 Al3 Cl13 104.74(13) . . ? C21 Al3 Cl13 112.34(11) . . ? Cl34 Al3 Cl13 100.23(5) . . ? C4 Al4 C22 128.31(16) . . ? C4 Al4 Cl34 110.94(13) . . ? C22 Al4 Cl34 99.20(11) . . ? C4 Al4 Cl24 103.52(12) . . ? C22 Al4 Cl24 111.05(11) . . ? Cl34 Al4 Cl24 100.75(5) . . ? Al2 Cl12 Al1 98.25(5) . . ? Al1 Cl13 Al3 120.12(6) . . ? Al2 Cl24 Al4 118.79(5) . . ? Al4 Cl34 Al3 99.11(5) . . ? C16 C11 C12 117.9(4) . . ? C16 C11 Al1 120.3(3) . . ? C12 C11 Al1 121.8(3) . . ? C13 C12 C11 117.7(4) . . ? C13 C12 Al2 121.9(3) . . ? C11 C12 Al2 120.2(3) . . ? F13 C13 C12 119.3(4) . . ? F13 C13 C14 118.7(4) . . ? C12 C13 C14 122.0(4) . . ? F14 C14 C15 122.2(5) . . ? F14 C14 C13 118.7(5) . . ? C15 C14 C13 119.1(4) . . ? C16 C15 F15 122.1(5) . . ? C16 C15 C14 119.6(4) . . ? F15 C15 C14 118.3(5) . . ? C15 C16 F16 118.1(4) . . ? C15 C16 C11 123.6(4) . . ? F16 C16 C11 118.3(4) . . ? C26 C21 C22 116.9(3) . . ? C26 C21 Al3 120.8(3) . . ? C22 C21 Al3 122.0(2) . . ? C23 C22 C21 118.4(3) . . ? C23 C22 Al4 120.9(3) . . ? C21 C22 Al4 120.7(3) . . ? F23 C23 C22 119.8(3) . . ? F23 C23 C24 117.0(3) . . ? C22 C23 C24 123.2(4) . . ? F24 C24 C25 120.1(4) . . ? F24 C24 C23 121.0(4) . . ? C25 C24 C23 119.0(4) . . ? F25 C25 C24 120.1(4) . . ? F25 C25 C26 120.7(4) . . ? C24 C25 C26 119.2(3) . . ? F26 C26 C25 117.8(3) . . ? F26 C26 C21 118.9(4) . . ? C25 C26 C21 123.3(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.345 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.054