# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Professor Neil Burford' _publ_contact_author_address ;Department of Chemistry University of Victoria Victoria BC V8W 3V6 Canada ; _publ_contact_author_email nburford@uvic.ca _publ_contact_author_phone '+1 250-721-7150' _publ_contact_author_fax '+1 250-721-7147' loop_ _publ_author_name _publ_author_address N.Burford ;Department of Chemistry University of Victoria Victoria BC V8W 3V6 Canada ; S.S.Chitnis ;Department of Chemistry University of Victoria Victoria BC V8W 3V6 Canada ; R.McDonald ;X-ray Crystallography Laboratory Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; M.J.Ferguson ;X-ray Crystallography Laboratory Department of Chemistry University of Alberta Edmonton Alberta T6G 2G2 Canada ; data_dal1189 _database_code_depnum_ccdc_archive 'CCDC 844313' #TrackingRef '- complete-cif-package 13 Sep.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl P2 Sb, 2(Al2 Cl7)' _chemical_formula_sum 'C26 H24 Al4 Cl15 P2 Sb' _chemical_formula_weight 1159.81 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' 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' Sb Sb -0.5866 1.5461 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2162(7) _cell_length_b 12.2612(7) _cell_length_c 17.8399(11) _cell_angle_alpha 72.2279(7) _cell_angle_beta 73.7807(7) _cell_angle_gamma 63.2388(7) _cell_volume 2240.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8291 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.09 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5462 _exptl_absorpt_correction_T_max 0.7962 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20150 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10237 _reflns_number_gt 8498 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 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^)+(0.0233P)^2^+1.2390P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10237 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _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 Sb Sb 0.503736(15) 0.181029(16) 0.148181(9) 0.02418(5) Uani 1 1 d . . . Cl1 Cl 0.44073(7) 0.38779(6) 0.08024(4) 0.03601(16) Uani 1 1 d . . . P1 P 0.59420(6) 0.21944(6) 0.25006(4) 0.02059(13) Uani 1 1 d . . . P2 P 0.31038(6) 0.22633(6) 0.26127(4) 0.02067(13) Uani 1 1 d . . . C1 C 0.4872(2) 0.2001(2) 0.34233(13) 0.0226(5) Uani 1 1 d . . . H1A H 0.5016 0.1107 0.3612 0.027 Uiso 1 1 calc R . . H1B H 0.5041 0.2263 0.3837 0.027 Uiso 1 1 calc R . . C2 C 0.3518(2) 0.2765(2) 0.33138(14) 0.0225(5) Uani 1 1 d . . . H2A H 0.3377 0.3658 0.3118 0.027 Uiso 1 1 calc R . . H2B H 0.2973 0.2681 0.3837 0.027 Uiso 1 1 calc R . . C11 C 0.7462(2) 0.1044(2) 0.26704(14) 0.0234(5) Uani 1 1 d . . . C12 C 0.7987(2) -0.0063(2) 0.24066(15) 0.0295(6) Uani 1 1 d . . . H12 H 0.7592 -0.0190 0.2071 0.035 Uiso 1 1 calc R . . C13 C 0.9089(3) -0.0983(3) 0.26325(17) 0.0378(7) Uani 1 1 d . . . H13 H 0.9450 -0.1747 0.2455 0.045 Uiso 1 1 calc R . . C14 C 0.9664(3) -0.0797(3) 0.31136(18) 0.0437(7) Uani 1 1 d . . . H14 H 1.0417 -0.1437 0.3274 0.052 Uiso 1 1 calc R . . C15 C 0.9157(3) 0.0312(3) 0.33650(19) 0.0459(8) Uani 1 1 d . . . H15 H 0.9567 0.0438 0.3692 0.055 Uiso 1 1 calc R . . C16 C 0.8058(3) 0.1240(3) 0.31466(17) 0.0367(7) Uani 1 1 d . . . H16 H 0.7711 0.2007 0.3319 0.044 Uiso 1 1 calc R . . C21 C 0.5913(2) 0.3731(2) 0.22735(14) 0.0220(5) Uani 1 1 d . . . C22 C 0.6524(2) 0.4143(2) 0.15263(15) 0.0293(6) Uani 1 1 d . . . H22 H 0.6919 0.3624 0.1146 0.035 Uiso 1 1 calc R . . C23 C 0.6547(3) 0.5309(3) 0.13499(17) 0.0343(6) Uani 1 1 d . . . H23 H 0.6947 0.5601 0.0841 0.041 Uiso 1 1 calc R . . C24 C 0.5993(3) 0.6055(2) 0.19062(17) 0.0345(6) Uani 1 1 d . . . H24 H 0.6011 0.6858 0.1777 0.041 Uiso 1 1 calc R . . C25 C 0.5413(3) 0.5642(2) 0.26474(17) 0.0348(6) Uani 1 1 d . . . H25 H 0.5050 0.6154 0.3032 0.042 Uiso 1 1 calc R . . C26 C 0.5358(2) 0.4483(2) 0.28338(15) 0.0282(6) Uani 1 1 d . . . H26 H 0.4945 0.4205 0.3341 0.034 Uiso 1 1 calc R . . C31 C 0.1631(2) 0.3399(2) 0.23591(14) 0.0234(5) Uani 1 1 d . . . C32 C 0.1464(2) 0.4648(2) 0.20852(15) 0.0295(6) Uani 1 1 d . . . H32 H 0.2128 0.4888 0.2024 0.035 Uiso 1 1 calc R . . C33 C 0.0322(3) 0.5531(3) 0.19039(17) 0.0370(7) Uani 1 1 d . . . H33 H 0.0198 0.6384 0.1715 0.044 Uiso 1 1 calc R . . C34 C -0.0642(3) 0.5179(3) 0.19961(17) 0.0381(7) Uani 1 1 d . . . H34 H -0.1429 0.5792 0.1873 0.046 Uiso 1 1 calc R . . C35 C -0.0468(2) 0.3944(3) 0.22652(16) 0.0344(6) Uani 1 1 d . . . H35 H -0.1136 0.3709 0.2328 0.041 Uiso 1 1 calc R . . C36 C 0.0663(2) 0.3047(2) 0.24446(15) 0.0280(6) Uani 1 1 d . . . H36 H 0.0783 0.2193 0.2625 0.034 Uiso 1 1 calc R . . C41 C 0.3023(2) 0.0773(2) 0.30463(14) 0.0232(5) Uani 1 1 d . . . C42 C 0.3121(3) 0.0044(2) 0.25490(16) 0.0309(6) Uani 1 1 d . . . H42 H 0.3266 0.0321 0.1986 0.037 Uiso 1 1 calc R . . C43 C 0.3006(3) -0.1081(3) 0.28731(18) 0.0376(7) Uani 1 1 d . . . H43 H 0.3062 -0.1575 0.2534 0.045 Uiso 1 1 calc R . . C44 C 0.2812(3) -0.1488(3) 0.36888(18) 0.0391(7) Uani 1 1 d . . . H44 H 0.2741 -0.2267 0.3910 0.047 Uiso 1 1 calc R . . C45 C 0.2720(3) -0.0778(3) 0.41876(17) 0.0363(7) Uani 1 1 d . . . H45 H 0.2585 -0.1067 0.4750 0.044 Uiso 1 1 calc R . . C46 C 0.2822(2) 0.0359(2) 0.38703(15) 0.0294(6) Uani 1 1 d . . . H46 H 0.2756 0.0854 0.4213 0.035 Uiso 1 1 calc R . . Cl2 Cl 0.89542(6) -0.03740(6) -0.10278(4) 0.03303(15) Uani 1 1 d . . . Cl3 Cl 0.57680(6) 0.11809(7) -0.05139(4) 0.03694(16) Uani 1 1 d . . . Cl4 Cl 0.77695(7) 0.16213(7) 0.03331(4) 0.03920(17) Uani 1 1 d . . . Cl5 Cl 0.76419(7) 0.27905(6) -0.17131(4) 0.04016(17) Uani 1 1 d . . . Cl6 Cl 0.73895(7) -0.23648(7) -0.05969(4) 0.03736(16) Uani 1 1 d . . . Cl7 Cl 0.78974(8) -0.15726(7) 0.09428(4) 0.04124(17) Uani 1 1 d . . . Cl8 Cl 1.04393(7) -0.34846(7) -0.02637(5) 0.04497(18) Uani 1 1 d . . . Al1 Al 0.86619(7) -0.20625(7) -0.01769(4) 0.02576(16) Uani 1 1 d . . . Al2 Al 0.74322(7) 0.14154(7) -0.07067(4) 0.02768(17) Uani 1 1 d . . . Cl9 Cl 0.15213(6) 0.39549(6) 0.60145(4) 0.03616(16) Uani 1 1 d . . . Cl10 Cl -0.05258(7) 0.69331(8) 0.54275(5) 0.0507(2) Uani 1 1 d . . . Cl11 Cl 0.20604(7) 0.56594(7) 0.40518(4) 0.03850(16) Uani 1 1 d . . . Cl12 Cl 0.23830(7) 0.64412(7) 0.57087(4) 0.04251(18) Uani 1 1 d . . . Cl13 Cl 0.38303(7) 0.17993(8) 0.71083(4) 0.04260(18) Uani 1 1 d . . . Cl14 Cl 0.34789(7) 0.11268(6) 0.54596(4) 0.03849(16) Uani 1 1 d . . . Cl15 Cl 0.46201(6) 0.34080(7) 0.51643(4) 0.04236(18) Uani 1 1 d . . . Al3 Al 0.13906(7) 0.58434(7) 0.52495(5) 0.02630(17) Uani 1 1 d . . . Al4 Al 0.34876(7) 0.25077(7) 0.59256(4) 0.02822(17) 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 Sb 0.02748(9) 0.02770(10) 0.02190(8) -0.00758(7) -0.00264(6) -0.01422(7) Cl1 0.0425(4) 0.0358(4) 0.0328(3) 0.0062(3) -0.0134(3) -0.0227(3) P1 0.0219(3) 0.0208(3) 0.0216(3) -0.0056(2) -0.0033(2) -0.0100(3) P2 0.0221(3) 0.0181(3) 0.0229(3) -0.0032(2) -0.0040(2) -0.0095(3) C1 0.0255(13) 0.0225(13) 0.0221(12) -0.0037(10) -0.0039(10) -0.0123(11) C2 0.0228(12) 0.0227(13) 0.0248(12) -0.0073(10) -0.0015(10) -0.0114(10) C11 0.0218(12) 0.0228(13) 0.0257(12) -0.0040(10) -0.0034(10) -0.0101(10) C12 0.0311(14) 0.0278(14) 0.0324(14) -0.0104(11) -0.0012(11) -0.0139(12) C13 0.0299(15) 0.0249(15) 0.0470(17) -0.0078(13) -0.0020(13) -0.0034(12) C14 0.0284(15) 0.0415(18) 0.0488(18) -0.0015(15) -0.0101(13) -0.0064(14) C15 0.0378(17) 0.052(2) 0.0538(19) -0.0114(16) -0.0219(15) -0.0142(15) C16 0.0346(15) 0.0347(16) 0.0470(17) -0.0148(13) -0.0151(13) -0.0103(13) C21 0.0242(12) 0.0199(12) 0.0250(12) -0.0023(10) -0.0081(10) -0.0106(10) C22 0.0345(15) 0.0291(14) 0.0280(13) -0.0071(11) -0.0018(11) -0.0173(12) C23 0.0396(16) 0.0329(15) 0.0354(15) 0.0007(12) -0.0069(12) -0.0235(13) C24 0.0382(16) 0.0218(14) 0.0484(17) -0.0011(12) -0.0162(13) -0.0150(12) C25 0.0376(16) 0.0254(14) 0.0454(16) -0.0150(12) -0.0089(13) -0.0099(12) C26 0.0286(13) 0.0255(14) 0.0310(13) -0.0072(11) -0.0032(11) -0.0114(11) C31 0.0240(12) 0.0211(12) 0.0240(12) -0.0033(10) -0.0056(10) -0.0081(10) C32 0.0301(14) 0.0241(14) 0.0364(14) -0.0040(11) -0.0106(11) -0.0113(11) C33 0.0413(16) 0.0226(14) 0.0450(16) -0.0014(12) -0.0165(13) -0.0091(13) C34 0.0312(15) 0.0362(17) 0.0409(16) -0.0044(13) -0.0142(12) -0.0059(13) C35 0.0277(14) 0.0413(17) 0.0366(15) -0.0018(13) -0.0090(12) -0.0177(13) C36 0.0292(14) 0.0265(14) 0.0296(13) -0.0012(11) -0.0065(11) -0.0142(11) C41 0.0226(12) 0.0177(12) 0.0298(13) -0.0018(10) -0.0073(10) -0.0088(10) C42 0.0398(15) 0.0267(14) 0.0290(13) -0.0021(11) -0.0138(11) -0.0134(12) C43 0.0501(18) 0.0281(15) 0.0448(17) -0.0051(13) -0.0198(14) -0.0190(14) C44 0.0455(17) 0.0241(15) 0.0517(18) 0.0035(13) -0.0148(14) -0.0207(13) C45 0.0447(17) 0.0288(15) 0.0318(14) 0.0043(12) -0.0061(12) -0.0185(13) C46 0.0343(14) 0.0236(14) 0.0292(13) -0.0038(11) -0.0050(11) -0.0119(12) Cl2 0.0350(4) 0.0289(3) 0.0319(3) -0.0065(3) 0.0054(3) -0.0161(3) Cl3 0.0316(4) 0.0425(4) 0.0403(4) -0.0073(3) -0.0045(3) -0.0196(3) Cl4 0.0459(4) 0.0471(4) 0.0364(4) -0.0181(3) -0.0044(3) -0.0240(4) Cl5 0.0542(4) 0.0297(4) 0.0402(4) -0.0018(3) -0.0047(3) -0.0251(3) Cl6 0.0412(4) 0.0468(4) 0.0348(3) -0.0062(3) -0.0082(3) -0.0270(3) Cl7 0.0625(5) 0.0344(4) 0.0232(3) -0.0081(3) -0.0032(3) -0.0172(4) Cl8 0.0338(4) 0.0355(4) 0.0596(5) -0.0128(4) -0.0063(3) -0.0077(3) Al1 0.0297(4) 0.0267(4) 0.0236(4) -0.0065(3) -0.0030(3) -0.0136(3) Al2 0.0323(4) 0.0277(4) 0.0268(4) -0.0078(3) -0.0014(3) -0.0158(4) Cl9 0.0284(3) 0.0279(3) 0.0465(4) -0.0069(3) 0.0048(3) -0.0133(3) Cl10 0.0278(4) 0.0519(5) 0.0568(5) -0.0185(4) -0.0034(3) -0.0003(3) Cl11 0.0462(4) 0.0378(4) 0.0317(3) -0.0138(3) -0.0002(3) -0.0164(3) Cl12 0.0530(5) 0.0506(5) 0.0412(4) -0.0133(3) -0.0047(3) -0.0350(4) Cl13 0.0496(4) 0.0617(5) 0.0259(3) -0.0039(3) -0.0078(3) -0.0327(4) Cl14 0.0517(4) 0.0283(4) 0.0316(3) -0.0080(3) -0.0125(3) -0.0083(3) Cl15 0.0310(4) 0.0441(4) 0.0412(4) 0.0017(3) 0.0014(3) -0.0168(3) Al3 0.0254(4) 0.0244(4) 0.0298(4) -0.0091(3) -0.0013(3) -0.0103(3) Al4 0.0297(4) 0.0282(4) 0.0230(4) -0.0035(3) -0.0018(3) -0.0111(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 Sb Cl1 2.3187(7) . ? Sb P2 2.6074(6) . ? Sb P1 2.6191(6) . ? Sb Cl4 3.3415(7) . ? Sb Cl6 3.4479(7) 2_655 ? Sb Cl3 3.6538(7) . ? P1 C21 1.788(2) . ? P1 C11 1.795(2) . ? P1 C1 1.820(2) . ? P2 C31 1.787(2) . ? P2 C41 1.790(2) . ? P2 C2 1.818(2) . ? C1 C2 1.524(3) . ? C11 C12 1.384(3) . ? C11 C16 1.392(3) . ? C12 C13 1.380(4) . ? C13 C14 1.373(4) . ? C14 C15 1.375(4) . ? C15 C16 1.376(4) . ? C21 C26 1.389(3) . ? C21 C22 1.401(3) . ? C22 C23 1.378(4) . ? C23 C24 1.379(4) . ? C24 C25 1.377(4) . ? C25 C26 1.385(4) . ? C31 C36 1.388(3) . ? C31 C32 1.393(3) . ? C32 C33 1.379(4) . ? C33 C34 1.380(4) . ? C34 C35 1.376(4) . ? C35 C36 1.373(4) . ? C41 C42 1.389(3) . ? C41 C46 1.391(3) . ? C42 C43 1.378(4) . ? C43 C44 1.376(4) . ? C44 C45 1.375(4) . ? C45 C46 1.384(4) . ? Cl2 Al2 2.2578(10) . ? Cl2 Al1 2.2721(10) . ? Cl3 Al2 2.1000(10) . ? Cl4 Al2 2.1167(10) . ? Cl5 Al2 2.1015(10) . ? Cl6 Al1 2.1104(10) . ? Cl7 Al1 2.0997(10) . ? Cl8 Al1 2.0848(11) . ? Cl9 Al4 2.2504(10) . ? Cl9 Al3 2.2604(10) . ? Cl10 Al3 2.0962(11) . ? Cl11 Al3 2.1065(10) . ? Cl12 Al3 2.0974(10) . ? Cl13 Al4 2.1044(10) . ? Cl14 Al4 2.1067(11) . ? Cl15 Al4 2.0946(10) . ? 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 Cl1 Sb P2 93.66(2) . . ? Cl1 Sb P1 92.77(2) . . ? P2 Sb P1 80.60(2) . . ? Cl1 Sb Cl4 82.37(2) . . ? P2 Sb Cl4 162.800(19) . . ? P1 Sb Cl4 82.874(18) . . ? Cl1 Sb Cl6 74.26(2) . 2_655 ? P2 Sb Cl6 75.487(19) . 2_655 ? P1 Sb Cl6 151.790(19) . 2_655 ? Cl4 Sb Cl6 118.937(17) . 2_655 ? Cl1 Sb Cl3 83.55(2) . . ? P2 Sb Cl3 136.431(18) . . ? P1 Sb Cl3 142.862(18) . . ? Cl4 Sb Cl3 59.993(16) . . ? Cl6 Sb Cl3 61.862(16) 2_655 . ? C21 P1 C11 110.29(11) . . ? C21 P1 C1 109.07(11) . . ? C11 P1 C1 106.89(11) . . ? C21 P1 Sb 113.74(8) . . ? C11 P1 Sb 114.19(8) . . ? C1 P1 Sb 102.00(8) . . ? C31 P2 C41 110.02(11) . . ? C31 P2 C2 108.79(11) . . ? C41 P2 C2 110.28(11) . . ? C31 P2 Sb 118.80(8) . . ? C41 P2 Sb 104.10(8) . . ? C2 P2 Sb 104.57(8) . . ? C2 C1 P1 111.99(16) . . ? C1 C2 P2 111.93(16) . . ? C12 C11 C16 120.0(2) . . ? C12 C11 P1 121.82(19) . . ? C16 C11 P1 117.87(19) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C16 120.4(3) . . ? C15 C16 C11 119.3(3) . . ? C26 C21 C22 120.1(2) . . ? C26 C21 P1 121.42(18) . . ? C22 C21 P1 118.36(18) . . ? C23 C22 C21 119.2(2) . . ? C22 C23 C24 120.5(2) . . ? C25 C24 C23 120.4(2) . . ? C24 C25 C26 120.2(2) . . ? C25 C26 C21 119.5(2) . . ? C36 C31 C32 120.5(2) . . ? C36 C31 P2 120.55(19) . . ? C32 C31 P2 118.92(19) . . ? C33 C32 C31 119.1(2) . . ? C32 C33 C34 120.3(3) . . ? C35 C34 C33 120.2(3) . . ? C36 C35 C34 120.6(3) . . ? C35 C36 C31 119.3(2) . . ? C42 C41 C46 119.9(2) . . ? C42 C41 P2 119.14(19) . . ? C46 C41 P2 120.96(19) . . ? C43 C42 C41 120.0(2) . . ? C44 C43 C42 119.9(3) . . ? C45 C44 C43 120.7(3) . . ? C44 C45 C46 120.0(3) . . ? C45 C46 C41 119.6(2) . . ? Al2 Cl2 Al1 110.77(4) . . ? Al2 Cl3 Sb 89.15(3) . . ? Al2 Cl4 Sb 97.67(3) . . ? Cl8 Al1 Cl7 115.78(5) . . ? Cl8 Al1 Cl6 113.09(5) . . ? Cl7 Al1 Cl6 110.71(4) . . ? Cl8 Al1 Cl2 103.20(4) . . ? Cl7 Al1 Cl2 106.02(4) . . ? Cl6 Al1 Cl2 107.11(4) . . ? Cl3 Al2 Cl5 114.37(5) . . ? Cl3 Al2 Cl4 112.58(4) . . ? Cl5 Al2 Cl4 112.68(4) . . ? Cl3 Al2 Cl2 105.34(4) . . ? Cl5 Al2 Cl2 103.42(4) . . ? Cl4 Al2 Cl2 107.47(4) . . ? Al4 Cl9 Al3 112.24(4) . . ? Cl10 Al3 Cl12 112.26(5) . . ? Cl10 Al3 Cl11 111.09(5) . . ? Cl12 Al3 Cl11 114.72(4) . . ? Cl10 Al3 Cl9 102.72(4) . . ? Cl12 Al3 Cl9 106.83(4) . . ? Cl11 Al3 Cl9 108.35(4) . . ? Cl15 Al4 Cl13 114.83(5) . . ? Cl15 Al4 Cl14 112.80(4) . . ? Cl13 Al4 Cl14 110.83(5) . . ? Cl15 Al4 Cl9 107.00(4) . . ? Cl13 Al4 Cl9 105.11(4) . . ? Cl14 Al4 Cl9 105.45(4) . . ? 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 Cl1 Sb P1 C21 -5.86(9) . . . . ? P2 Sb P1 C21 -99.11(9) . . . . ? Cl4 Sb P1 C21 76.10(9) . . . . ? Cl6 Sb P1 C21 -66.89(10) 2_655 . . . ? Cl3 Sb P1 C21 77.12(9) . . . . ? Cl1 Sb P1 C11 -133.66(9) . . . . ? P2 Sb P1 C11 133.08(9) . . . . ? Cl4 Sb P1 C11 -51.71(9) . . . . ? Cl6 Sb P1 C11 165.30(8) 2_655 . . . ? Cl3 Sb P1 C11 -50.69(9) . . . . ? Cl1 Sb P1 C1 111.43(8) . . . . ? P2 Sb P1 C1 18.18(8) . . . . ? Cl4 Sb P1 C1 -166.61(8) . . . . ? Cl6 Sb P1 C1 50.40(9) 2_655 . . . ? Cl3 Sb P1 C1 -165.59(8) . . . . ? Cl1 Sb P2 C31 36.95(9) . . . . ? P1 Sb P2 C31 129.16(9) . . . . ? Cl4 Sb P2 C31 112.90(11) . . . . ? Cl6 Sb P2 C31 -35.75(9) 2_655 . . . ? Cl3 Sb P2 C31 -47.54(10) . . . . ? Cl1 Sb P2 C41 159.70(8) . . . . ? P1 Sb P2 C41 -108.09(8) . . . . ? Cl4 Sb P2 C41 -124.36(10) . . . . ? Cl6 Sb P2 C41 87.00(8) 2_655 . . . ? Cl3 Sb P2 C41 75.21(9) . . . . ? Cl1 Sb P2 C2 -84.55(8) . . . . ? P1 Sb P2 C2 7.66(8) . . . . ? Cl4 Sb P2 C2 -8.61(12) . . . . ? Cl6 Sb P2 C2 -157.25(8) 2_655 . . . ? Cl3 Sb P2 C2 -169.04(8) . . . . ? C21 P1 C1 C2 70.96(19) . . . . ? C11 P1 C1 C2 -169.80(16) . . . . ? Sb P1 C1 C2 -49.64(17) . . . . ? P1 C1 C2 P2 63.0(2) . . . . ? C31 P2 C2 C1 -167.82(16) . . . . ? C41 P2 C2 C1 71.44(18) . . . . ? Sb P2 C2 C1 -39.93(17) . . . . ? C21 P1 C11 C12 -141.5(2) . . . . ? C1 P1 C11 C12 100.1(2) . . . . ? Sb P1 C11 C12 -11.9(2) . . . . ? C21 P1 C11 C16 44.7(2) . . . . ? C1 P1 C11 C16 -73.8(2) . . . . ? Sb P1 C11 C16 174.21(18) . . . . ? C16 C11 C12 C13 1.5(4) . . . . ? P1 C11 C12 C13 -172.2(2) . . . . ? C11 C12 C13 C14 -0.4(4) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C14 C15 C16 C11 0.2(5) . . . . ? C12 C11 C16 C15 -1.5(4) . . . . ? P1 C11 C16 C15 172.5(2) . . . . ? C11 P1 C21 C26 -104.1(2) . . . . ? C1 P1 C21 C26 13.0(2) . . . . ? Sb P1 C21 C26 126.09(19) . . . . ? C11 P1 C21 C22 72.5(2) . . . . ? C1 P1 C21 C22 -170.44(19) . . . . ? Sb P1 C21 C22 -57.3(2) . . . . ? C26 C21 C22 C23 -1.3(4) . . . . ? P1 C21 C22 C23 -177.9(2) . . . . ? C21 C22 C23 C24 1.1(4) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C26 -1.4(4) . . . . ? C24 C25 C26 C21 1.2(4) . . . . ? C22 C21 C26 C25 0.1(4) . . . . ? P1 C21 C26 C25 176.7(2) . . . . ? C41 P2 C31 C36 -5.3(2) . . . . ? C2 P2 C31 C36 -126.2(2) . . . . ? Sb P2 C31 C36 114.44(19) . . . . ? C41 P2 C31 C32 173.77(19) . . . . ? C2 P2 C31 C32 52.9(2) . . . . ? Sb P2 C31 C32 -66.5(2) . . . . ? C36 C31 C32 C33 0.3(4) . . . . ? P2 C31 C32 C33 -178.7(2) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C32 C33 C34 C35 -0.4(4) . . . . ? C33 C34 C35 C36 0.0(4) . . . . ? C34 C35 C36 C31 0.6(4) . . . . ? C32 C31 C36 C35 -0.8(4) . . . . ? P2 C31 C36 C35 178.3(2) . . . . ? C31 P2 C41 C42 80.6(2) . . . . ? C2 P2 C41 C42 -159.4(2) . . . . ? Sb P2 C41 C42 -47.7(2) . . . . ? C31 P2 C41 C46 -97.1(2) . . . . ? C2 P2 C41 C46 22.9(2) . . . . ? Sb P2 C41 C46 134.6(2) . . . . ? C46 C41 C42 C43 0.6(4) . . . . ? P2 C41 C42 C43 -177.2(2) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? C42 C43 C44 C45 0.5(5) . . . . ? C43 C44 C45 C46 0.0(5) . . . . ? C44 C45 C46 C41 -0.2(4) . . . . ? C42 C41 C46 C45 -0.1(4) . . . . ? P2 C41 C46 C45 177.6(2) . . . . ? Cl1 Sb Cl3 Al2 80.20(3) . . . . ? P2 Sb Cl3 Al2 168.74(3) . . . . ? P1 Sb Cl3 Al2 -5.86(5) . . . . ? Cl4 Sb Cl3 Al2 -4.70(3) . . . . ? Cl6 Sb Cl3 Al2 155.77(4) 2_655 . . . ? Cl1 Sb Cl4 Al2 -82.23(4) . . . . ? P2 Sb Cl4 Al2 -159.84(6) . . . . ? P1 Sb Cl4 Al2 -176.01(4) . . . . ? Cl6 Sb Cl4 Al2 -14.98(4) 2_655 . . . ? Cl3 Sb Cl4 Al2 4.70(3) . . . . ? Al2 Cl2 Al1 Cl8 -157.07(4) . . . . ? Al2 Cl2 Al1 Cl7 -34.91(6) . . . . ? Al2 Cl2 Al1 Cl6 83.35(5) . . . . ? Sb Cl3 Al2 Cl5 -123.34(4) . . . . ? Sb Cl3 Al2 Cl4 6.96(4) . . . . ? Sb Cl3 Al2 Cl2 123.79(3) . . . . ? Sb Cl4 Al2 Cl3 -7.69(5) . . . . ? Sb Cl4 Al2 Cl5 123.47(4) . . . . ? Sb Cl4 Al2 Cl2 -123.24(3) . . . . ? Al1 Cl2 Al2 Cl3 -46.06(5) . . . . ? Al1 Cl2 Al2 Cl5 -166.41(4) . . . . ? Al1 Cl2 Al2 Cl4 74.20(5) . . . . ? Al4 Cl9 Al3 Cl10 177.81(4) . . . . ? Al4 Cl9 Al3 Cl12 -63.90(5) . . . . ? Al4 Cl9 Al3 Cl11 60.20(6) . . . . ? Al3 Cl9 Al4 Cl15 1.70(6) . . . . ? Al3 Cl9 Al4 Cl13 124.21(5) . . . . ? Al3 Cl9 Al4 Cl14 -118.62(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.614 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.078 data_dal1188 _database_code_depnum_ccdc_archive 'CCDC 844314' #TrackingRef '- complete-cif-package 13 Sep.cif' _vrf_CHEMW03_dal1188 ; RESPONSE: The reported formula, molecular weights, etc, include contributions from disordered solvent pentane and dichloromethane molecules that were removed by the SQUEEZE procedure as implemented in PLATON. See _platon_squeeze_details in this CIF for more information. ; _vrf_PLAT043_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_PLAT051_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_PLAT041_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_PLAT068_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_FORMU01_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_CELLZ01_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_PLAT606_dal1188 ; RESPONSE: see response to CHEMW03. ; _vrf_PLAT869_dal1188 ; RESPONSE: see response to CHEMW03. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H36 Al4 Cl11 P2 Sb' _chemical_formula_weight 1090.16 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' 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' Sb Sb -0.5866 1.5461 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.299(2) _cell_length_b 10.3844(15) _cell_length_c 25.251(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.272(2) _cell_angle_gamma 90.00 _cell_volume 4229.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9140 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.39 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 1.532 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4647 _exptl_absorpt_correction_T_max 0.7638 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32771 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.55 _reflns_number_total 8740 _reflns_number_gt 7200 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0648P)^2^+6.7150P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8740 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1216 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _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 Sb Sb 0.442657(15) 0.20766(3) 0.766462(11) 0.02770(9) Uani 1 1 d . . . Cl1 Cl 0.30905(6) 0.18434(11) 0.78884(5) 0.0415(3) Uani 1 1 d . . . P1 P 0.47495(6) -0.02587(10) 0.80374(4) 0.0269(2) Uani 1 1 d . . . P2 P 0.41395(6) 0.02631(10) 0.69461(4) 0.0256(2) Uani 1 1 d . . . C1 C 0.4099(2) -0.0966(4) 0.74559(16) 0.0289(8) Uani 1 1 d . . . H1A H 0.4330 -0.1794 0.7350 0.035 Uiso 1 1 calc R . . H1B H 0.3524 -0.1106 0.7528 0.035 Uiso 1 1 calc R . . C11 C 0.5805(2) -0.0723(4) 0.80148(16) 0.0287(8) Uani 1 1 d . . . C12 C 0.6407(3) 0.0199(5) 0.79681(18) 0.0365(10) Uani 1 1 d . . . H12 H 0.6267 0.1088 0.7959 0.044 Uiso 1 1 calc R . . C13 C 0.7217(3) -0.0182(5) 0.7934(2) 0.0481(12) Uani 1 1 d . . . H13 H 0.7631 0.0443 0.7898 0.058 Uiso 1 1 calc R . . C14 C 0.7411(3) -0.1468(5) 0.7953(2) 0.0470(12) Uani 1 1 d . . . H14 H 0.7963 -0.1727 0.7929 0.056 Uiso 1 1 calc R . . C15 C 0.6820(3) -0.2396(5) 0.8005(2) 0.0433(11) Uani 1 1 d . . . H15 H 0.6965 -0.3283 0.8019 0.052 Uiso 1 1 calc R . . C16 C 0.6014(3) -0.2021(4) 0.80377(18) 0.0370(10) Uani 1 1 d . . . H16 H 0.5604 -0.2651 0.8076 0.044 Uiso 1 1 calc R . . C21 C 0.4442(3) -0.0814(4) 0.86485(16) 0.0310(9) Uani 1 1 d . . . C22 C 0.5048(3) -0.0968(5) 0.90908(18) 0.0445(12) Uani 1 1 d . . . H22 H 0.5612 -0.0797 0.9061 0.053 Uiso 1 1 calc R . . C23 C 0.4832(3) -0.1367(6) 0.9573(2) 0.0537(13) Uani 1 1 d . . . H23 H 0.5245 -0.1460 0.9877 0.064 Uiso 1 1 calc R . . C24 C 0.4016(4) -0.1632(6) 0.9611(2) 0.0598(15) Uani 1 1 d . . . H24 H 0.3866 -0.1924 0.9940 0.072 Uiso 1 1 calc R . . C25 C 0.3425(4) -0.1476(7) 0.9179(2) 0.0635(16) Uani 1 1 d . . . H25 H 0.2863 -0.1655 0.9212 0.076 Uiso 1 1 calc R . . C26 C 0.3620(3) -0.1065(6) 0.8694(2) 0.0495(13) Uani 1 1 d . . . H26 H 0.3198 -0.0955 0.8396 0.059 Uiso 1 1 calc R . . C31 C 0.3267(2) 0.0197(4) 0.64344(16) 0.0294(8) Uani 1 1 d . . . C32 C 0.3372(3) 0.0225(5) 0.59002(18) 0.0446(11) Uani 1 1 d . . . H32 H 0.3912 0.0279 0.5803 0.054 Uiso 1 1 calc R . . C33 C 0.2687(4) 0.0173(6) 0.5509(2) 0.0608(15) Uani 1 1 d . . . H33 H 0.2758 0.0197 0.5142 0.073 Uiso 1 1 calc R . . C34 C 0.1909(3) 0.0088(6) 0.5645(2) 0.0557(14) Uani 1 1 d . . . H34 H 0.1442 0.0038 0.5373 0.067 Uiso 1 1 calc R . . C35 C 0.1798(3) 0.0074(6) 0.6177(2) 0.0503(13) Uani 1 1 d . . . H35 H 0.1254 0.0021 0.6269 0.060 Uiso 1 1 calc R . . C36 C 0.2464(3) 0.0136(5) 0.65709(18) 0.0384(10) Uani 1 1 d . . . H36 H 0.2384 0.0138 0.6936 0.046 Uiso 1 1 calc R . . C41 C 0.5099(2) 0.0156(4) 0.66756(16) 0.0300(8) Uani 1 1 d . . . C42 C 0.5540(3) -0.1005(4) 0.66693(18) 0.0373(10) Uani 1 1 d . . . H42 H 0.5330 -0.1777 0.6801 0.045 Uiso 1 1 calc R . . C43 C 0.6280(3) -0.0999(5) 0.6469(2) 0.0441(11) Uani 1 1 d . . . H43 H 0.6589 -0.1774 0.6466 0.053 Uiso 1 1 calc R . . C44 C 0.6582(3) 0.0126(6) 0.6272(2) 0.0490(12) Uani 1 1 d . . . H44 H 0.7091 0.0111 0.6130 0.059 Uiso 1 1 calc R . . C45 C 0.6152(3) 0.1253(5) 0.6280(2) 0.0459(12) Uani 1 1 d . . . H45 H 0.6367 0.2018 0.6146 0.055 Uiso 1 1 calc R . . C46 C 0.5405(3) 0.1291(4) 0.64812(18) 0.0362(10) Uani 1 1 d . . . H46 H 0.5106 0.2076 0.6487 0.043 Uiso 1 1 calc R . . Cl2 Cl 0.35855(7) 0.35095(11) 0.66291(5) 0.0414(3) Uani 1 1 d . . . Cl3 Cl 0.36354(8) 0.68063(11) 0.63456(5) 0.0490(3) Uani 1 1 d . . . Cl4 Cl 0.54781(7) 0.51044(15) 0.66595(6) 0.0540(3) Uani 1 1 d . . . Cl5 Cl 0.42046(8) 0.56266(11) 0.76420(5) 0.0426(3) Uani 1 1 d . . . Cl6 Cl 0.62872(7) 0.38644(12) 0.80455(4) 0.0438(3) Uani 1 1 d . . . Cl7 Cl 0.59256(13) 0.55150(14) 0.91898(6) 0.0761(5) Uani 1 1 d . . . Cl8 Cl 0.70950(8) 0.26642(16) 0.92870(6) 0.0594(4) Uani 1 1 d . . . Cl9 Cl 0.49724(7) 0.25622(12) 0.88696(5) 0.0436(3) Uani 1 1 d . . . Al1 Al 0.42414(8) 0.52920(12) 0.68091(5) 0.0324(3) Uani 1 1 d . . . Al2 Al 0.60843(8) 0.36929(13) 0.88584(5) 0.0343(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 Sb 0.02295(14) 0.02452(14) 0.03441(16) -0.00192(10) -0.00004(10) -0.00057(10) Cl1 0.0255(5) 0.0461(7) 0.0535(7) -0.0071(5) 0.0080(4) 0.0017(4) P1 0.0217(5) 0.0284(5) 0.0295(5) 0.0024(4) 0.0000(4) -0.0008(4) P2 0.0235(5) 0.0238(5) 0.0286(5) 0.0006(4) 0.0010(4) 0.0006(4) C1 0.0273(19) 0.027(2) 0.031(2) 0.0005(16) 0.0009(15) -0.0003(16) C11 0.0230(18) 0.032(2) 0.030(2) 0.0031(16) -0.0012(15) -0.0005(16) C12 0.029(2) 0.035(2) 0.044(3) 0.0057(19) 0.0009(18) -0.0020(18) C13 0.024(2) 0.056(3) 0.063(3) 0.013(2) 0.005(2) -0.004(2) C14 0.025(2) 0.063(3) 0.053(3) 0.013(2) 0.0071(19) 0.007(2) C15 0.036(2) 0.042(3) 0.051(3) 0.008(2) 0.003(2) 0.011(2) C16 0.034(2) 0.032(2) 0.044(3) 0.0071(18) 0.0021(18) 0.0014(18) C21 0.032(2) 0.028(2) 0.033(2) 0.0018(16) 0.0058(16) 0.0002(17) C22 0.032(2) 0.066(3) 0.034(2) 0.007(2) -0.0001(18) 0.001(2) C23 0.055(3) 0.068(4) 0.036(3) 0.013(2) -0.001(2) 0.002(3) C24 0.059(3) 0.081(4) 0.042(3) 0.018(3) 0.016(2) -0.006(3) C25 0.047(3) 0.096(5) 0.051(3) 0.014(3) 0.015(2) -0.015(3) C26 0.034(2) 0.071(4) 0.042(3) 0.012(2) 0.001(2) -0.006(2) C31 0.0266(19) 0.029(2) 0.031(2) -0.0008(16) 0.0003(15) 0.0021(16) C32 0.038(2) 0.056(3) 0.037(2) 0.004(2) -0.0014(19) 0.004(2) C33 0.064(4) 0.082(4) 0.032(3) 0.002(3) -0.008(2) 0.004(3) C34 0.038(3) 0.074(4) 0.049(3) 0.001(3) -0.017(2) -0.002(3) C35 0.032(2) 0.064(3) 0.051(3) 0.000(2) -0.007(2) -0.008(2) C36 0.033(2) 0.043(3) 0.038(2) 0.0031(19) 0.0009(18) -0.0054(19) C41 0.0259(19) 0.034(2) 0.029(2) -0.0025(16) -0.0007(15) 0.0033(16) C42 0.037(2) 0.036(2) 0.038(2) -0.0018(18) 0.0047(18) 0.0053(19) C43 0.034(2) 0.048(3) 0.051(3) -0.002(2) 0.008(2) 0.013(2) C44 0.029(2) 0.070(4) 0.049(3) -0.003(3) 0.008(2) 0.003(2) C45 0.033(2) 0.055(3) 0.052(3) 0.005(2) 0.011(2) -0.009(2) C46 0.034(2) 0.026(2) 0.048(3) 0.0052(18) 0.0064(19) 0.0030(17) Cl2 0.0370(6) 0.0299(5) 0.0532(7) 0.0013(5) -0.0076(5) -0.0007(4) Cl3 0.0600(7) 0.0326(6) 0.0516(7) 0.0093(5) -0.0018(6) 0.0114(5) Cl4 0.0300(6) 0.0689(9) 0.0639(8) 0.0048(7) 0.0094(5) 0.0027(6) Cl5 0.0495(6) 0.0365(6) 0.0416(6) 0.0002(5) 0.0056(5) 0.0010(5) Cl6 0.0423(6) 0.0538(7) 0.0354(6) 0.0050(5) 0.0056(4) -0.0108(5) Cl7 0.1279(15) 0.0405(7) 0.0585(9) -0.0127(6) 0.0090(9) -0.0061(8) Cl8 0.0375(6) 0.0806(10) 0.0589(8) 0.0296(7) 0.0031(5) 0.0005(6) Cl9 0.0363(6) 0.0540(7) 0.0415(6) -0.0051(5) 0.0091(5) -0.0144(5) Al1 0.0301(6) 0.0261(6) 0.0400(7) 0.0017(5) 0.0019(5) 0.0033(5) Al2 0.0340(7) 0.0350(7) 0.0326(7) 0.0005(5) 0.0003(5) -0.0077(5) _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 Sb Cl1 2.3397(11) . ? Sb P2 2.6101(11) . ? Sb P1 2.6270(11) . ? P1 C21 1.785(4) . ? P1 C11 1.795(4) . ? P1 C1 1.836(4) . ? P2 C31 1.780(4) . ? P2 C41 1.798(4) . ? P2 C1 1.821(4) . ? C11 C12 1.388(6) . ? C11 C16 1.390(6) . ? C12 C13 1.393(6) . ? C13 C14 1.372(8) . ? C14 C15 1.382(7) . ? C15 C16 1.383(6) . ? C21 C26 1.387(6) . ? C21 C22 1.389(6) . ? C22 C23 1.378(7) . ? C23 C24 1.375(8) . ? C24 C25 1.356(8) . ? C25 C26 1.376(7) . ? C31 C32 1.384(6) . ? C31 C36 1.402(6) . ? C32 C33 1.381(7) . ? C33 C34 1.364(8) . ? C34 C35 1.380(7) . ? C35 C36 1.366(6) . ? C41 C46 1.396(6) . ? C41 C42 1.404(6) . ? C42 C43 1.373(6) . ? C43 C44 1.388(8) . ? C44 C45 1.366(7) . ? C45 C46 1.386(6) . ? Cl2 Al1 2.1531(17) . ? Cl3 Al1 2.1179(17) . ? Cl4 Al1 2.1125(18) . ? Cl5 Al1 2.1409(18) . ? Cl6 Al2 2.1330(17) . ? Cl7 Al2 2.100(2) . ? Cl8 Al2 2.1243(19) . ? Cl9 Al2 2.1629(17) . ? 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 Cl1 Sb P2 90.75(4) . . ? Cl1 Sb P1 87.90(4) . . ? P2 Sb P1 65.77(3) . . ? C21 P1 C11 109.26(19) . . ? C21 P1 C1 111.13(19) . . ? C11 P1 C1 108.24(19) . . ? C21 P1 Sb 122.76(14) . . ? C11 P1 Sb 112.34(14) . . ? C1 P1 Sb 91.14(13) . . ? C31 P2 C41 111.70(19) . . ? C31 P2 C1 112.31(19) . . ? C41 P2 C1 110.33(19) . . ? C31 P2 Sb 125.24(14) . . ? C41 P2 Sb 103.28(14) . . ? C1 P2 Sb 92.04(13) . . ? P2 C1 P1 102.1(2) . . ? C12 C11 C16 120.0(4) . . ? C12 C11 P1 120.6(3) . . ? C16 C11 P1 119.3(3) . . ? C11 C12 C13 119.8(4) . . ? C14 C13 C12 119.3(5) . . ? C13 C14 C15 121.5(4) . . ? C14 C15 C16 119.3(5) . . ? C15 C16 C11 120.0(4) . . ? C26 C21 C22 119.7(4) . . ? C26 C21 P1 121.8(3) . . ? C22 C21 P1 118.5(3) . . ? C23 C22 C21 120.2(5) . . ? C24 C23 C22 119.6(5) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 121.6(5) . . ? C25 C26 C21 118.8(5) . . ? C32 C31 C36 119.4(4) . . ? C32 C31 P2 120.6(3) . . ? C36 C31 P2 120.0(3) . . ? C33 C32 C31 119.8(5) . . ? C34 C33 C32 120.4(5) . . ? C33 C34 C35 120.2(4) . . ? C36 C35 C34 120.4(5) . . ? C35 C36 C31 119.7(4) . . ? C46 C41 C42 120.8(4) . . ? C46 C41 P2 117.1(3) . . ? C42 C41 P2 122.1(3) . . ? C43 C42 C41 118.6(4) . . ? C42 C43 C44 120.7(5) . . ? C45 C44 C43 120.5(4) . . ? C44 C45 C46 120.6(5) . . ? C45 C46 C41 118.8(4) . . ? Cl4 Al1 Cl3 110.53(8) . . ? Cl4 Al1 Cl5 110.66(7) . . ? Cl3 Al1 Cl5 110.22(7) . . ? Cl4 Al1 Cl2 109.91(8) . . ? Cl3 Al1 Cl2 110.10(7) . . ? Cl5 Al1 Cl2 105.29(7) . . ? Cl7 Al2 Cl8 112.40(9) . . ? Cl7 Al2 Cl6 110.69(8) . . ? Cl8 Al2 Cl6 108.42(8) . . ? Cl7 Al2 Cl9 109.42(9) . . ? Cl8 Al2 Cl9 108.07(8) . . ? Cl6 Al2 Cl9 107.71(7) . . ? 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 Cl1 Sb P1 C21 -43.57(17) . . . . ? P2 Sb P1 C21 -135.34(17) . . . . ? Cl1 Sb P1 C11 -177.08(15) . . . . ? P2 Sb P1 C11 91.15(15) . . . . ? Cl1 Sb P1 C1 72.64(14) . . . . ? P2 Sb P1 C1 -19.14(13) . . . . ? Cl1 Sb P2 C31 51.32(18) . . . . ? P1 Sb P2 C31 138.68(18) . . . . ? Cl1 Sb P2 C41 -179.49(14) . . . . ? P1 Sb P2 C41 -92.13(14) . . . . ? Cl1 Sb P2 C1 -68.05(13) . . . . ? P1 Sb P2 C1 19.32(13) . . . . ? C31 P2 C1 P1 -155.88(19) . . . . ? C41 P2 C1 P1 78.8(2) . . . . ? Sb P2 C1 P1 -26.18(17) . . . . ? C21 P1 C1 P2 152.00(19) . . . . ? C11 P1 C1 P2 -88.0(2) . . . . ? Sb P1 C1 P2 25.99(17) . . . . ? C21 P1 C11 C12 -120.9(4) . . . . ? C1 P1 C11 C12 117.9(4) . . . . ? Sb P1 C11 C12 18.8(4) . . . . ? C21 P1 C11 C16 59.9(4) . . . . ? C1 P1 C11 C16 -61.3(4) . . . . ? Sb P1 C11 C16 -160.4(3) . . . . ? C16 C11 C12 C13 1.2(7) . . . . ? P1 C11 C12 C13 -177.9(4) . . . . ? C11 C12 C13 C14 -0.7(7) . . . . ? C12 C13 C14 C15 -0.1(8) . . . . ? C13 C14 C15 C16 0.2(8) . . . . ? C14 C15 C16 C11 0.3(7) . . . . ? C12 C11 C16 C15 -1.0(7) . . . . ? P1 C11 C16 C15 178.1(4) . . . . ? C11 P1 C21 C26 -153.9(4) . . . . ? C1 P1 C21 C26 -34.5(5) . . . . ? Sb P1 C21 C26 71.4(4) . . . . ? C11 P1 C21 C22 27.5(4) . . . . ? C1 P1 C21 C22 146.9(4) . . . . ? Sb P1 C21 C22 -107.2(4) . . . . ? C26 C21 C22 C23 0.0(8) . . . . ? P1 C21 C22 C23 178.6(4) . . . . ? C21 C22 C23 C24 1.0(9) . . . . ? C22 C23 C24 C25 -1.3(10) . . . . ? C23 C24 C25 C26 0.6(11) . . . . ? C24 C25 C26 C21 0.4(10) . . . . ? C22 C21 C26 C25 -0.7(8) . . . . ? P1 C21 C26 C25 -179.2(5) . . . . ? C41 P2 C31 C32 -7.4(4) . . . . ? C1 P2 C31 C32 -131.9(4) . . . . ? Sb P2 C31 C32 118.4(4) . . . . ? C41 P2 C31 C36 173.6(3) . . . . ? C1 P2 C31 C36 49.0(4) . . . . ? Sb P2 C31 C36 -60.7(4) . . . . ? C36 C31 C32 C33 -0.9(7) . . . . ? P2 C31 C32 C33 -180.0(4) . . . . ? C31 C32 C33 C34 -0.4(9) . . . . ? C32 C33 C34 C35 1.1(10) . . . . ? C33 C34 C35 C36 -0.5(9) . . . . ? C34 C35 C36 C31 -0.9(8) . . . . ? C32 C31 C36 C35 1.6(7) . . . . ? P2 C31 C36 C35 -179.4(4) . . . . ? C31 P2 C41 C46 82.8(4) . . . . ? C1 P2 C41 C46 -151.5(3) . . . . ? Sb P2 C41 C46 -54.2(3) . . . . ? C31 P2 C41 C42 -98.7(4) . . . . ? C1 P2 C41 C42 27.0(4) . . . . ? Sb P2 C41 C42 124.3(3) . . . . ? C46 C41 C42 C43 0.2(6) . . . . ? P2 C41 C42 C43 -178.2(3) . . . . ? C41 C42 C43 C44 -0.7(7) . . . . ? C42 C43 C44 C45 0.9(8) . . . . ? C43 C44 C45 C46 -0.5(8) . . . . ? C44 C45 C46 C41 -0.1(7) . . . . ? C42 C41 C46 C45 0.2(7) . . . . ? P2 C41 C46 C45 178.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.867 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.006 0.000 466 176 ' ' 2 0.500 -0.042 0.500 466 176 ' ' _platon_squeeze_details ; Attempts to refine peaks of residual electron density as disordered or partial-occupancy solvent pentane or dichloromethane chlorine or carbon atoms were unsuccessful. The data were corrected for disordered electron density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194201) as implemented in PLATON (Spek, A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. Cryst. 2003, 36, 713. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). A total solvent-accessible void volume of 932 \%A3 with a total electron count of 352 (consistent with 4 molecules each of solvent dichloromethane and pentane, or 1 molecule of dichloromethane and 1 molecule of pentane per formula unit of the [(dppm)SbCl][AlCl4]2 compound) was found in the unit cell. ; data_dal1137 _database_code_depnum_ccdc_archive 'CCDC 844315' #TrackingRef '- complete-cif-package 13 Sep.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 Cl2 P2 Sb, C F3 O3 S' _chemical_formula_sum 'C7 H16 Cl2 F3 O3 P2 S Sb' _chemical_formula_weight 491.85 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' O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.1129(3) _cell_length_b 11.3226(3) _cell_length_c 13.0683(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1644.34(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 2.352 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4485 _exptl_absorpt_correction_T_max 0.5788 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14741 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3781 _reflns_number_gt 3758 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 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^)+(0.0179P)^2^+0.3004P] 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 constr _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 0.008(9) _refine_ls_number_reflns 3781 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0132 _refine_ls_R_factor_gt 0.0131 _refine_ls_wR_factor_ref 0.0329 _refine_ls_wR_factor_gt 0.0329 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.001 _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 Sb Sb 0.365049(8) 0.347820(8) 0.247797(8) 0.01720(3) Uani 1 1 d . . . Cl1 Cl 0.34410(4) 0.37973(4) 0.05368(3) 0.02632(9) Uani 1 1 d . . . Cl2 Cl 0.34829(4) 0.35932(4) 0.44230(3) 0.02634(9) Uani 1 1 d . . . P1 P 0.34459(3) 0.57316(3) 0.25863(3) 0.01721(7) Uani 1 1 d . . . P2 P 0.13483(3) 0.36303(3) 0.24082(3) 0.01667(7) Uani 1 1 d . . . C1 C 0.18429(14) 0.59921(14) 0.27700(12) 0.0219(3) Uani 1 1 d . . . H1A H 0.1638 0.5866 0.3499 0.026 Uiso 1 1 calc R . . H1B H 0.1657 0.6824 0.2598 0.026 Uiso 1 1 calc R . . C2 C 0.10675(14) 0.51727(13) 0.21037(13) 0.0205(3) Uani 1 1 d . . . H2A H 0.1251 0.5315 0.1373 0.025 Uiso 1 1 calc R . . H2B H 0.0206 0.5354 0.2217 0.025 Uiso 1 1 calc R . . C3 C 0.42244(17) 0.63461(15) 0.36662(12) 0.0250(4) Uani 1 1 d . . . H3A H 0.4021 0.5896 0.4283 0.030 Uiso 1 1 calc R . . H3B H 0.3983 0.7172 0.3757 0.030 Uiso 1 1 calc R . . H3C H 0.5094 0.6306 0.3548 0.030 Uiso 1 1 calc R . . C4 C 0.38665(16) 0.65353(16) 0.14562(12) 0.0238(3) Uani 1 1 d . . . H4A H 0.3454 0.6198 0.0861 0.029 Uiso 1 1 calc R . . H4B H 0.4739 0.6480 0.1358 0.029 Uiso 1 1 calc R . . H4C H 0.3636 0.7366 0.1533 0.029 Uiso 1 1 calc R . . C5 C 0.06125(16) 0.33105(17) 0.36013(12) 0.0262(4) Uani 1 1 d . . . H5A H 0.0949 0.3813 0.4141 0.031 Uiso 1 1 calc R . . H5B H 0.0739 0.2479 0.3779 0.031 Uiso 1 1 calc R . . H5C H -0.0252 0.3465 0.3535 0.031 Uiso 1 1 calc R . . C6 C 0.06811(16) 0.27416(15) 0.14225(13) 0.0244(3) Uani 1 1 d . . . H6A H 0.1071 0.2914 0.0767 0.029 Uiso 1 1 calc R . . H6B H -0.0180 0.2922 0.1374 0.029 Uiso 1 1 calc R . . H6C H 0.0787 0.1904 0.1589 0.029 Uiso 1 1 calc R . . S S 0.72627(3) 0.49043(3) 0.20259(3) 0.02213(8) Uani 1 1 d . . . F1 F 0.84984(14) 0.52559(16) 0.03607(11) 0.0672(4) Uani 1 1 d . . . F2 F 0.72723(18) 0.38195(12) 0.02678(11) 0.0684(5) Uani 1 1 d . . . F3 F 0.66214(15) 0.55923(14) 0.01908(11) 0.0624(4) Uani 1 1 d . . . O1 O 0.60360(12) 0.45595(16) 0.21939(12) 0.0468(4) Uani 1 1 d . . . O2 O 0.75324(15) 0.61053(11) 0.22969(10) 0.0462(4) Uani 1 1 d . . . O3 O 0.81344(13) 0.40556(13) 0.23528(13) 0.0450(4) Uani 1 1 d . . . C7 C 0.74194(18) 0.48919(16) 0.06355(14) 0.0332(4) 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 Sb 0.01578(5) 0.01801(5) 0.01782(5) -0.00100(5) 0.00033(5) 0.00427(3) Cl1 0.0296(2) 0.0316(2) 0.01775(17) -0.00315(15) 0.00139(15) -0.00148(18) Cl2 0.0305(2) 0.02926(19) 0.01925(17) 0.00118(15) -0.00107(15) 0.00092(19) P1 0.01701(15) 0.01692(15) 0.01770(18) -0.00168(15) 0.00077(16) -0.00211(13) P2 0.01527(16) 0.01736(16) 0.01740(18) 0.00041(15) 0.00105(18) -0.00085(12) C1 0.0177(7) 0.0177(7) 0.0302(9) -0.0032(6) 0.0048(6) 0.0025(6) C2 0.0174(7) 0.0178(7) 0.0263(7) 0.0021(6) -0.0008(6) 0.0042(6) C3 0.0291(9) 0.0258(9) 0.0202(8) -0.0037(6) -0.0024(6) -0.0088(7) C4 0.0255(8) 0.0247(8) 0.0212(7) 0.0026(6) -0.0001(6) -0.0046(7) C5 0.0219(8) 0.0344(9) 0.0223(8) 0.0037(7) 0.0032(6) -0.0022(8) C6 0.0240(8) 0.0245(8) 0.0249(8) -0.0037(7) -0.0024(7) -0.0059(7) S 0.01680(17) 0.01814(17) 0.03144(19) -0.00240(15) -0.00143(14) -0.00032(15) F1 0.0528(9) 0.0969(12) 0.0519(8) -0.0017(8) 0.0221(7) -0.0196(9) F2 0.1097(13) 0.0422(8) 0.0533(8) -0.0268(6) 0.0012(9) -0.0083(8) F3 0.0764(10) 0.0716(10) 0.0392(7) 0.0058(7) -0.0105(7) 0.0270(9) O1 0.0204(6) 0.0732(11) 0.0467(9) 0.0017(7) 0.0026(6) -0.0089(7) O2 0.0756(11) 0.0232(6) 0.0398(8) -0.0089(5) -0.0043(8) -0.0097(6) O3 0.0375(7) 0.0442(7) 0.0532(10) 0.0034(8) -0.0052(7) 0.0187(6) C7 0.0347(10) 0.0286(9) 0.0364(9) -0.0061(8) 0.0018(8) -0.0007(8) _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 Sb Cl2 2.5520(4) . ? Sb P1 2.5655(4) . ? Sb P2 2.5658(4) . ? Sb Cl1 2.5729(4) . ? Sb O1 2.9436(14) . ? Sb O2 3.0055(14) 3_645 ? P1 C3 1.7956(17) . ? P1 C4 1.7965(17) . ? P1 C1 1.8216(16) . ? P2 C6 1.7949(16) . ? P2 C5 1.7974(16) . ? P2 C2 1.8181(15) . ? C1 C2 1.537(2) . ? S O3 1.4298(13) . ? S O1 1.4348(14) . ? S O2 1.4369(13) . ? S C7 1.8253(19) . ? F1 C7 1.318(2) . ? F2 C7 1.316(2) . ? F3 C7 1.324(2) . ? 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 Cl2 Sb P1 83.560(14) . . ? Cl2 Sb P2 87.663(15) . . ? P1 Sb P2 81.190(11) . . ? Cl2 Sb Cl1 165.527(14) . . ? P1 Sb Cl1 84.647(14) . . ? P2 Sb Cl1 82.259(15) . . ? Cl2 Sb O1 99.79(3) . . ? P1 Sb O1 70.92(4) . . ? P2 Sb O1 149.95(4) . . ? Cl1 Sb O1 84.19(3) . . ? Cl2 Sb O2 85.19(3) . 3_645 ? P1 Sb O2 147.66(3) . 3_645 ? P2 Sb O2 68.12(3) . 3_645 ? Cl1 Sb O2 100.51(3) . 3_645 ? O1 Sb O2 141.08(5) . 3_645 ? C3 P1 C4 108.93(8) . . ? C3 P1 C1 107.75(8) . . ? C4 P1 C1 106.31(8) . . ? C3 P1 Sb 112.71(6) . . ? C4 P1 Sb 115.81(6) . . ? C1 P1 Sb 104.77(5) . . ? C6 P2 C5 108.76(8) . . ? C6 P2 C2 108.09(8) . . ? C5 P2 C2 107.77(8) . . ? C6 P2 Sb 113.57(6) . . ? C5 P2 Sb 114.16(6) . . ? C2 P2 Sb 104.09(5) . . ? C2 C1 P1 112.08(10) . . ? C1 C2 P2 111.08(11) . . ? O3 S O1 114.52(10) . . ? O3 S O2 114.90(10) . . ? O1 S O2 114.71(10) . . ? O3 S C7 103.16(9) . . ? O1 S C7 103.94(9) . . ? O2 S C7 103.46(8) . . ? S O1 Sb 171.14(11) . . ? F2 C7 F1 107.58(18) . . ? F2 C7 F3 108.01(17) . . ? F1 C7 F3 107.60(18) . . ? F2 C7 S 111.02(14) . . ? F1 C7 S 110.83(14) . . ? F3 C7 S 111.62(13) . . ? 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 Cl2 Sb P1 C3 37.82(7) . . . . ? P2 Sb P1 C3 126.44(7) . . . . ? Cl1 Sb P1 C3 -150.59(7) . . . . ? O1 Sb P1 C3 -64.90(7) . . . . ? O2 Sb P1 C3 108.19(8) 3_645 . . . ? Cl2 Sb P1 C4 164.19(6) . . . . ? P2 Sb P1 C4 -107.19(6) . . . . ? Cl1 Sb P1 C4 -24.22(6) . . . . ? O1 Sb P1 C4 61.47(7) . . . . ? O2 Sb P1 C4 -125.44(8) 3_645 . . . ? Cl2 Sb P1 C1 -79.06(6) . . . . ? P2 Sb P1 C1 9.56(6) . . . . ? Cl1 Sb P1 C1 92.53(6) . . . . ? O1 Sb P1 C1 178.22(6) . . . . ? O2 Sb P1 C1 -8.69(8) 3_645 . . . ? Cl2 Sb P2 C6 -142.81(6) . . . . ? P1 Sb P2 C6 133.35(6) . . . . ? Cl1 Sb P2 C6 47.60(6) . . . . ? O1 Sb P2 C6 111.56(9) . . . . ? O2 Sb P2 C6 -57.05(7) 3_645 . . . ? Cl2 Sb P2 C5 -17.34(7) . . . . ? P1 Sb P2 C5 -101.18(7) . . . . ? Cl1 Sb P2 C5 173.07(7) . . . . ? O1 Sb P2 C5 -122.97(9) . . . . ? O2 Sb P2 C5 68.42(7) 3_645 . . . ? Cl2 Sb P2 C2 99.89(6) . . . . ? P1 Sb P2 C2 16.04(6) . . . . ? Cl1 Sb P2 C2 -69.70(6) . . . . ? O1 Sb P2 C2 -5.75(9) . . . . ? O2 Sb P2 C2 -174.36(6) 3_645 . . . ? C3 P1 C1 C2 -161.08(11) . . . . ? C4 P1 C1 C2 82.27(12) . . . . ? Sb P1 C1 C2 -40.84(12) . . . . ? P1 C1 C2 P2 60.19(13) . . . . ? C6 P2 C2 C1 -167.25(11) . . . . ? C5 P2 C2 C1 75.36(12) . . . . ? Sb P2 C2 C1 -46.21(11) . . . . ? O3 S O1 Sb -33.2(6) . . . . ? O2 S O1 Sb -169.2(6) . . . . ? C7 S O1 Sb 78.5(6) . . . . ? Cl2 Sb O1 S 105.2(6) . . . . ? P1 Sb O1 S -175.2(6) . . . . ? P2 Sb O1 S -152.4(6) . . . . ? Cl1 Sb O1 S -88.9(6) . . . . ? O2 Sb O1 S 10.7(6) 3_645 . . . ? O3 S C7 F2 55.98(18) . . . . ? O1 S C7 F2 -63.83(18) . . . . ? O2 S C7 F2 176.02(16) . . . . ? O3 S C7 F1 -63.52(17) . . . . ? O1 S C7 F1 176.67(15) . . . . ? O2 S C7 F1 56.52(17) . . . . ? O3 S C7 F3 176.55(14) . . . . ? O1 S C7 F3 56.74(17) . . . . ? O2 S C7 F3 -63.41(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.278 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.109 data_dal1166 _database_code_depnum_ccdc_archive 'CCDC 844316' #TrackingRef '- complete-cif-package 13 Sep.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Cl2 P2 Sb, C H2 Cl2, Al Cl4' _chemical_formula_sum 'C27 H26 Al Cl8 P2 Sb' _chemical_formula_weight 844.75 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' 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' Sb Sb -0.5866 1.5461 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5270(3) _cell_length_b 12.8155(3) _cell_length_c 14.0046(3) _cell_angle_alpha 74.3015(3) _cell_angle_beta 71.3838(3) _cell_angle_gamma 87.5567(3) _cell_volume 1721.72(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9547 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.45 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.559 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7060 _exptl_absorpt_correction_T_max 0.7930 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15558 _diffrn_reflns_av_R_equivalents 0.0142 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7895 _reflns_number_gt 7215 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 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^)+(0.0252P)^2^+1.3868P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7895 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0564 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _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 Sb Sb 0.338661(12) 0.034308(10) 0.435504(10) 0.02087(4) Uani 1 1 d . . . Cl1 Cl 0.59898(5) -0.00045(4) 0.35470(4) 0.02557(10) Uani 1 1 d . . . Cl2 Cl 0.12063(5) 0.12007(5) 0.46646(4) 0.03479(12) Uani 1 1 d . . . P1 P 0.44784(5) 0.22577(4) 0.40123(4) 0.01958(10) Uani 1 1 d . . . P2 P 0.35165(5) 0.11447(4) 0.23964(4) 0.02198(10) Uani 1 1 d . . . C1 C 0.50035(19) 0.27858(16) 0.25920(15) 0.0240(4) Uani 1 1 d . . . H1A H 0.5206 0.3577 0.2404 0.029 Uiso 1 1 calc R . . H1B H 0.5841 0.2445 0.2285 0.029 Uiso 1 1 calc R . . C2 C 0.3951(2) 0.25841(16) 0.21064(15) 0.0249(4) Uani 1 1 d . . . H2A H 0.4303 0.2895 0.1338 0.030 Uiso 1 1 calc R . . H2B H 0.3131 0.2963 0.2377 0.030 Uiso 1 1 calc R . . C11 C 0.59456(19) 0.23458(15) 0.44016(15) 0.0224(4) Uani 1 1 d . . . C12 C 0.7238(2) 0.22642(16) 0.37370(17) 0.0268(4) Uani 1 1 d . . . H12 H 0.7357 0.2140 0.3076 0.032 Uiso 1 1 calc R . . C13 C 0.8347(2) 0.23656(18) 0.40460(19) 0.0340(5) Uani 1 1 d . . . H13 H 0.9223 0.2310 0.3595 0.041 Uiso 1 1 calc R . . C14 C 0.8179(2) 0.25463(19) 0.5007(2) 0.0365(5) Uani 1 1 d . . . H14 H 0.8940 0.2616 0.5214 0.044 Uiso 1 1 calc R . . C15 C 0.6905(2) 0.26267(19) 0.56685(19) 0.0345(5) Uani 1 1 d . . . H15 H 0.6794 0.2748 0.6330 0.041 Uiso 1 1 calc R . . C16 C 0.5785(2) 0.25301(17) 0.53700(17) 0.0278(4) Uani 1 1 d . . . H16 H 0.4912 0.2589 0.5825 0.033 Uiso 1 1 calc R . . C21 C 0.32378(19) 0.30947(16) 0.46094(15) 0.0228(4) Uani 1 1 d . . . C22 C 0.2503(2) 0.27105(18) 0.56706(16) 0.0280(4) Uani 1 1 d . . . H22 H 0.2664 0.2018 0.6064 0.034 Uiso 1 1 calc R . . C23 C 0.1539(2) 0.3340(2) 0.61481(19) 0.0365(5) Uani 1 1 d . . . H23 H 0.1045 0.3084 0.6872 0.044 Uiso 1 1 calc R . . C24 C 0.1297(2) 0.4345(2) 0.5567(2) 0.0421(6) Uani 1 1 d . . . H24 H 0.0637 0.4778 0.5896 0.051 Uiso 1 1 calc R . . C25 C 0.2004(2) 0.4719(2) 0.4520(2) 0.0384(5) Uani 1 1 d . . . H25 H 0.1822 0.5405 0.4128 0.046 Uiso 1 1 calc R . . C26 C 0.2983(2) 0.41028(17) 0.40291(17) 0.0288(4) Uani 1 1 d . . . H26 H 0.3473 0.4366 0.3306 0.035 Uiso 1 1 calc R . . C31 C 0.1938(2) 0.10199(18) 0.21821(16) 0.0264(4) Uani 1 1 d . . . C32 C 0.1181(2) 0.0045(2) 0.2630(2) 0.0403(5) Uani 1 1 d . . . H32 H 0.1479 -0.0547 0.3069 0.048 Uiso 1 1 calc R . . C33 C -0.0009(3) -0.0061(3) 0.2433(2) 0.0511(7) Uani 1 1 d . . . H33 H -0.0517 -0.0732 0.2727 0.061 Uiso 1 1 calc R . . C34 C -0.0461(2) 0.0798(3) 0.1815(2) 0.0473(7) Uani 1 1 d . . . H34 H -0.1279 0.0720 0.1686 0.057 Uiso 1 1 calc R . . C35 C 0.0271(2) 0.1771(2) 0.13842(19) 0.0421(6) Uani 1 1 d . . . H35 H -0.0048 0.2363 0.0961 0.051 Uiso 1 1 calc R . . C36 C 0.1478(2) 0.18938(19) 0.15629(17) 0.0316(5) Uani 1 1 d . . . H36 H 0.1981 0.2567 0.1265 0.038 Uiso 1 1 calc R . . C41 C 0.4783(2) 0.05075(17) 0.15624(15) 0.0266(4) Uani 1 1 d . . . C42 C 0.4585(3) -0.0585(2) 0.1656(2) 0.0403(5) Uani 1 1 d . . . H42 H 0.3753 -0.0956 0.2091 0.048 Uiso 1 1 calc R . . C43 C 0.5600(3) -0.1134(2) 0.1116(2) 0.0517(7) Uani 1 1 d . . . H43 H 0.5468 -0.1883 0.1184 0.062 Uiso 1 1 calc R . . C44 C 0.6801(3) -0.0591(2) 0.0480(2) 0.0486(7) Uani 1 1 d . . . H44 H 0.7502 -0.0971 0.0118 0.058 Uiso 1 1 calc R . . C45 C 0.6997(3) 0.0497(2) 0.03635(19) 0.0442(6) Uani 1 1 d . . . H45 H 0.7824 0.0866 -0.0086 0.053 Uiso 1 1 calc R . . C46 C 0.5986(2) 0.1053(2) 0.09030(17) 0.0341(5) Uani 1 1 d . . . H46 H 0.6117 0.1805 0.0821 0.041 Uiso 1 1 calc R . . Cl3 Cl 0.11350(6) 0.45328(5) 0.21668(5) 0.04119(13) Uani 1 1 d . . . Cl4 Cl 0.21037(7) 0.64235(5) -0.02645(5) 0.04374(14) Uani 1 1 d . . . Cl5 Cl 0.18195(7) 0.72189(5) 0.20148(5) 0.04553(15) Uani 1 1 d . . . Cl6 Cl 0.44317(6) 0.56788(6) 0.10663(5) 0.05110(17) Uani 1 1 d . . . Al Al 0.23709(7) 0.59620(5) 0.12440(5) 0.02976(14) Uani 1 1 d . . . Cl1S Cl 0.62023(9) 0.52944(7) 0.31385(7) 0.0702(2) Uani 1 1 d . . . Cl2S Cl 0.81053(12) 0.66896(10) 0.12822(8) 0.0996(4) Uani 1 1 d . . . C1S C 0.7619(4) 0.5335(3) 0.2102(4) 0.0823(12) Uani 1 1 d . . . H1SA H 0.7460 0.4877 0.1682 0.099 Uiso 1 1 calc R . . H1SB H 0.8361 0.5032 0.2367 0.099 Uiso 1 1 calc R . . 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 Sb 0.01982(7) 0.02098(7) 0.02266(7) -0.00478(5) -0.00894(5) 0.00114(5) Cl1 0.0245(2) 0.0276(2) 0.0267(2) -0.00900(19) -0.01022(18) 0.00538(18) Cl2 0.0184(2) 0.0476(3) 0.0437(3) -0.0220(3) -0.0097(2) 0.0050(2) P1 0.0171(2) 0.0211(2) 0.0213(2) -0.00638(18) -0.00673(18) 0.00238(17) P2 0.0217(2) 0.0247(2) 0.0220(2) -0.00686(19) -0.01025(19) 0.00333(19) C1 0.0234(9) 0.0257(10) 0.0215(9) -0.0052(8) -0.0060(7) 0.0000(7) C2 0.0283(10) 0.0234(10) 0.0242(9) -0.0059(8) -0.0106(8) 0.0027(8) C11 0.0205(9) 0.0197(9) 0.0286(10) -0.0067(8) -0.0100(8) 0.0018(7) C12 0.0218(9) 0.0264(10) 0.0320(11) -0.0078(8) -0.0088(8) 0.0019(8) C13 0.0209(10) 0.0339(12) 0.0470(13) -0.0105(10) -0.0110(9) 0.0015(8) C14 0.0291(11) 0.0370(12) 0.0538(14) -0.0156(11) -0.0246(10) 0.0022(9) C15 0.0375(12) 0.0352(12) 0.0399(12) -0.0149(10) -0.0209(10) 0.0024(9) C16 0.0258(10) 0.0285(10) 0.0333(11) -0.0115(9) -0.0127(8) 0.0027(8) C21 0.0193(9) 0.0245(9) 0.0276(10) -0.0105(8) -0.0089(7) 0.0038(7) C22 0.0241(10) 0.0318(11) 0.0295(10) -0.0110(9) -0.0087(8) 0.0038(8) C23 0.0272(11) 0.0511(14) 0.0344(12) -0.0218(11) -0.0060(9) 0.0055(10) C24 0.0332(12) 0.0531(15) 0.0554(15) -0.0362(13) -0.0194(11) 0.0205(11) C25 0.0410(13) 0.0338(12) 0.0507(14) -0.0187(11) -0.0244(11) 0.0165(10) C26 0.0309(11) 0.0264(10) 0.0330(11) -0.0100(9) -0.0144(9) 0.0057(8) C31 0.0224(9) 0.0357(11) 0.0245(10) -0.0103(8) -0.0108(8) 0.0036(8) C32 0.0352(12) 0.0449(14) 0.0420(13) -0.0041(11) -0.0196(11) -0.0048(10) C33 0.0359(13) 0.0669(19) 0.0503(16) -0.0089(14) -0.0169(12) -0.0176(13) C34 0.0244(11) 0.086(2) 0.0391(13) -0.0237(14) -0.0148(10) 0.0038(12) C35 0.0317(12) 0.0662(17) 0.0374(13) -0.0196(12) -0.0207(10) 0.0188(12) C36 0.0300(11) 0.0392(12) 0.0292(11) -0.0115(9) -0.0135(9) 0.0093(9) C41 0.0287(10) 0.0338(11) 0.0238(10) -0.0123(8) -0.0140(8) 0.0077(8) C42 0.0412(13) 0.0369(13) 0.0485(14) -0.0206(11) -0.0145(11) 0.0034(10) C43 0.0628(18) 0.0438(15) 0.0630(18) -0.0343(14) -0.0249(15) 0.0150(13) C44 0.0504(16) 0.0650(18) 0.0402(14) -0.0315(13) -0.0165(12) 0.0258(14) C45 0.0366(13) 0.0650(18) 0.0292(12) -0.0171(12) -0.0055(10) 0.0116(12) C46 0.0345(12) 0.0399(13) 0.0268(11) -0.0096(9) -0.0083(9) 0.0053(10) Cl3 0.0409(3) 0.0323(3) 0.0445(3) -0.0045(2) -0.0105(3) -0.0002(2) Cl4 0.0488(3) 0.0511(4) 0.0331(3) -0.0063(3) -0.0196(3) 0.0005(3) Cl5 0.0483(3) 0.0420(3) 0.0452(3) -0.0203(3) -0.0059(3) -0.0009(3) Cl6 0.0311(3) 0.0669(4) 0.0507(4) -0.0087(3) -0.0139(3) 0.0100(3) Al 0.0287(3) 0.0324(3) 0.0273(3) -0.0068(3) -0.0091(3) 0.0034(3) Cl1S 0.0684(5) 0.0717(5) 0.0726(5) -0.0159(4) -0.0250(4) -0.0236(4) Cl2S 0.0922(7) 0.1140(9) 0.0669(6) 0.0174(6) -0.0225(5) -0.0187(6) C1S 0.069(2) 0.081(3) 0.129(4) -0.063(3) -0.049(2) 0.027(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 Sb Cl2 2.4640(5) . ? Sb P1 2.6121(5) . ? Sb P2 2.6164(5) . ? Sb Cl1 2.6791(5) . ? Sb Cl1 3.1255(5) 2_656 ? P1 C21 1.7956(19) . ? P1 C11 1.811(2) . ? P1 C1 1.822(2) . ? P2 C41 1.799(2) . ? P2 C31 1.801(2) . ? P2 C2 1.824(2) . ? C1 C2 1.535(3) . ? C11 C16 1.395(3) . ? C11 C12 1.400(3) . ? C12 C13 1.390(3) . ? C13 C14 1.382(3) . ? C14 C15 1.384(3) . ? C15 C16 1.390(3) . ? C21 C26 1.394(3) . ? C21 C22 1.397(3) . ? C22 C23 1.384(3) . ? C23 C24 1.387(4) . ? C24 C25 1.375(4) . ? C25 C26 1.390(3) . ? C31 C32 1.390(3) . ? C31 C36 1.392(3) . ? C32 C33 1.386(3) . ? C33 C34 1.374(4) . ? C34 C35 1.374(4) . ? C35 C36 1.394(3) . ? C41 C46 1.387(3) . ? C41 C42 1.389(3) . ? C42 C43 1.384(4) . ? C43 C44 1.378(4) . ? C44 C45 1.375(4) . ? C45 C46 1.388(3) . ? Cl3 Al 2.1368(9) . ? Cl4 Al 2.1403(9) . ? Cl5 Al 2.1350(9) . ? Cl6 Al 2.1300(9) . ? Cl1S C1S 1.708(4) . ? Cl2S C1S 1.793(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 Cl2 Sb P1 87.147(17) . . ? Cl2 Sb P2 82.286(18) . . ? P1 Sb P2 80.933(16) . . ? Cl2 Sb Cl1 162.004(19) . . ? P1 Sb Cl1 78.995(15) . . ? P2 Sb Cl1 84.222(15) . . ? Cl2 Sb Cl1 104.095(16) . 2_656 ? P1 Sb Cl1 80.755(14) . 2_656 ? P2 Sb Cl1 160.254(15) . 2_656 ? Cl1 Sb Cl1 85.096(14) . 2_656 ? C21 P1 C11 108.04(9) . . ? C21 P1 C1 110.00(9) . . ? C11 P1 C1 106.77(9) . . ? C21 P1 Sb 109.54(7) . . ? C11 P1 Sb 118.64(6) . . ? C1 P1 Sb 103.59(7) . . ? C41 P2 C31 109.41(9) . . ? C41 P2 C2 110.89(10) . . ? C31 P2 C2 108.24(10) . . ? C41 P2 Sb 110.70(7) . . ? C31 P2 Sb 112.92(7) . . ? C2 P2 Sb 104.59(7) . . ? C2 C1 P1 113.72(14) . . ? C1 C2 P2 112.40(14) . . ? C16 C11 C12 119.46(18) . . ? C16 C11 P1 119.27(15) . . ? C12 C11 P1 121.25(15) . . ? C13 C12 C11 119.9(2) . . ? C14 C13 C12 120.3(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.3(2) . . ? C15 C16 C11 119.9(2) . . ? C26 C21 C22 119.94(18) . . ? C26 C21 P1 121.18(16) . . ? C22 C21 P1 118.87(15) . . ? C23 C22 C21 119.9(2) . . ? C22 C23 C24 119.8(2) . . ? C25 C24 C23 120.4(2) . . ? C24 C25 C26 120.6(2) . . ? C25 C26 C21 119.3(2) . . ? C32 C31 C36 119.9(2) . . ? C32 C31 P2 119.89(17) . . ? C36 C31 P2 120.25(17) . . ? C33 C32 C31 119.8(2) . . ? C34 C33 C32 120.5(3) . . ? C35 C34 C33 120.1(2) . . ? C34 C35 C36 120.5(2) . . ? C31 C36 C35 119.3(2) . . ? C46 C41 C42 119.8(2) . . ? C46 C41 P2 121.63(17) . . ? C42 C41 P2 118.37(17) . . ? C43 C42 C41 120.0(2) . . ? C44 C43 C42 119.8(3) . . ? C45 C44 C43 120.7(2) . . ? C44 C45 C46 120.0(2) . . ? C41 C46 C45 119.8(2) . . ? Cl6 Al Cl5 107.60(4) . . ? Cl6 Al Cl3 111.04(4) . . ? Cl5 Al Cl3 109.24(4) . . ? Cl6 Al Cl4 109.38(4) . . ? Cl5 Al Cl4 111.19(4) . . ? Cl3 Al Cl4 108.39(4) . . ? Cl1S C1S Cl2S 112.08(19) . . ? 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 Cl2 Sb P1 C21 21.29(7) . . . . ? P2 Sb P1 C21 103.93(7) . . . . ? Cl1 Sb P1 C21 -170.25(7) . . . . ? Cl1 Sb P1 C21 -83.49(7) 2_656 . . . ? Cl2 Sb P1 C11 145.92(8) . . . . ? P2 Sb P1 C11 -131.45(8) . . . . ? Cl1 Sb P1 C11 -45.62(7) . . . . ? Cl1 Sb P1 C11 41.13(7) 2_656 . . . ? Cl2 Sb P1 C1 -96.04(7) . . . . ? P2 Sb P1 C1 -13.40(7) . . . . ? Cl1 Sb P1 C1 72.43(7) . . . . ? Cl1 Sb P1 C1 159.18(7) 2_656 . . . ? Cl2 Sb P2 C41 -163.21(8) . . . . ? P1 Sb P2 C41 108.47(8) . . . . ? Cl1 Sb P2 C41 28.73(8) . . . . ? Cl1 Sb P2 C41 86.30(9) 2_656 . . . ? Cl2 Sb P2 C31 -40.15(8) . . . . ? P1 Sb P2 C31 -128.48(8) . . . . ? Cl1 Sb P2 C31 151.78(8) . . . . ? Cl1 Sb P2 C31 -150.64(8) 2_656 . . . ? Cl2 Sb P2 C2 77.31(7) . . . . ? P1 Sb P2 C2 -11.01(7) . . . . ? Cl1 Sb P2 C2 -90.75(7) . . . . ? Cl1 Sb P2 C2 -33.18(9) 2_656 . . . ? C21 P1 C1 C2 -73.45(16) . . . . ? C11 P1 C1 C2 169.56(14) . . . . ? Sb P1 C1 C2 43.55(15) . . . . ? P1 C1 C2 P2 -59.08(17) . . . . ? C41 P2 C2 C1 -78.71(16) . . . . ? C31 P2 C2 C1 161.28(14) . . . . ? Sb P2 C2 C1 40.64(15) . . . . ? C21 P1 C11 C16 29.85(19) . . . . ? C1 P1 C11 C16 148.13(16) . . . . ? Sb P1 C11 C16 -95.50(16) . . . . ? C21 P1 C11 C12 -148.26(16) . . . . ? C1 P1 C11 C12 -29.99(19) . . . . ? Sb P1 C11 C12 86.39(17) . . . . ? C16 C11 C12 C13 0.1(3) . . . . ? P1 C11 C12 C13 178.18(16) . . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C11 0.3(3) . . . . ? C12 C11 C16 C15 -0.2(3) . . . . ? P1 C11 C16 C15 -178.40(17) . . . . ? C11 P1 C21 C26 104.23(17) . . . . ? C1 P1 C21 C26 -12.0(2) . . . . ? Sb P1 C21 C26 -125.20(16) . . . . ? C11 P1 C21 C22 -77.05(18) . . . . ? C1 P1 C21 C22 166.76(16) . . . . ? Sb P1 C21 C22 53.52(17) . . . . ? C26 C21 C22 C23 -1.2(3) . . . . ? P1 C21 C22 C23 -179.89(17) . . . . ? C21 C22 C23 C24 0.7(3) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C26 -0.8(4) . . . . ? C24 C25 C26 C21 0.4(3) . . . . ? C22 C21 C26 C25 0.6(3) . . . . ? P1 C21 C26 C25 179.30(17) . . . . ? C41 P2 C31 C32 78.2(2) . . . . ? C2 P2 C31 C32 -160.82(18) . . . . ? Sb P2 C31 C32 -45.5(2) . . . . ? C41 P2 C31 C36 -101.26(18) . . . . ? C2 P2 C31 C36 19.7(2) . . . . ? Sb P2 C31 C36 134.97(15) . . . . ? C36 C31 C32 C33 1.8(4) . . . . ? P2 C31 C32 C33 -177.7(2) . . . . ? C31 C32 C33 C34 -1.3(4) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C36 0.4(4) . . . . ? C32 C31 C36 C35 -1.2(3) . . . . ? P2 C31 C36 C35 178.29(17) . . . . ? C34 C35 C36 C31 0.1(3) . . . . ? C31 P2 C41 C46 127.07(18) . . . . ? C2 P2 C41 C46 7.8(2) . . . . ? Sb P2 C41 C46 -107.86(17) . . . . ? C31 P2 C41 C42 -58.5(2) . . . . ? C2 P2 C41 C42 -177.84(17) . . . . ? Sb P2 C41 C42 66.54(18) . . . . ? C46 C41 C42 C43 1.8(4) . . . . ? P2 C41 C42 C43 -172.7(2) . . . . ? C41 C42 C43 C44 -0.5(4) . . . . ? C42 C43 C44 C45 -1.0(4) . . . . ? C43 C44 C45 C46 1.0(4) . . . . ? C42 C41 C46 C45 -1.8(3) . . . . ? P2 C41 C46 C45 172.57(18) . . . . ? C44 C45 C46 C41 0.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.346 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.063 data_dal1163 _database_code_depnum_ccdc_archive 'CCDC 844317' #TrackingRef '- complete-cif-package 13 Sep.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H22 Al Cl6 P2 Sb' _chemical_formula_weight 745.80 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' 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' Sb Sb -0.5866 1.5461 '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 '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3131(2) _cell_length_b 11.7645(3) _cell_length_c 13.2776(3) _cell_angle_alpha 81.5321(3) _cell_angle_beta 73.3679(3) _cell_angle_gamma 86.3619(3) _cell_volume 1526.34(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.51 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.577 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5530 _exptl_absorpt_correction_T_max 0.7864 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50402 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.53 _reflns_number_total 7012 _reflns_number_gt 6592 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 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^)+(0.0200P)^2^+1.0451P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7012 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0217 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _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 Sb Sb 0.565480(11) 0.465580(9) 0.151304(9) 0.02627(4) Uani 1 1 d . . . Cl1 Cl 0.76982(5) 0.46261(4) 0.20524(4) 0.04014(10) Uani 1 1 d . . . Cl2 Cl 0.66081(5) 0.37518(4) -0.00250(3) 0.03489(9) Uani 1 1 d . . . P1 P 0.53005(4) 0.25968(3) 0.25611(3) 0.02401(8) Uani 1 1 d . . . P2 P 0.31497(4) 0.33836(3) 0.16151(3) 0.02409(8) Uani 1 1 d . . . C1 C 0.40999(16) 0.20789(14) 0.19774(13) 0.0268(3) Uani 1 1 d . . . H1A H 0.3488 0.1516 0.2495 0.032 Uiso 1 1 calc R . . H1B H 0.4574 0.1712 0.1343 0.032 Uiso 1 1 calc R . . C11 C 0.67803(17) 0.16816(14) 0.23880(15) 0.0322(4) Uani 1 1 d . . . C12 C 0.7243(2) 0.11570(17) 0.14730(17) 0.0415(4) Uani 1 1 d . . . H12 H 0.6733 0.1227 0.0973 0.050 Uiso 1 1 calc R . . C13 C 0.8452(2) 0.05320(19) 0.1298(2) 0.0574(6) Uani 1 1 d . . . H13 H 0.8780 0.0179 0.0672 0.069 Uiso 1 1 calc R . . C14 C 0.9182(2) 0.0422(2) 0.2032(3) 0.0663(8) Uani 1 1 d . . . H14 H 1.0011 -0.0007 0.1908 0.080 Uiso 1 1 calc R . . C15 C 0.8720(2) 0.0927(2) 0.2939(3) 0.0640(7) Uani 1 1 d . . . H15 H 0.9224 0.0833 0.3444 0.077 Uiso 1 1 calc R . . C16 C 0.7522(2) 0.15733(18) 0.3128(2) 0.0463(5) Uani 1 1 d . . . H16 H 0.7212 0.1936 0.3750 0.056 Uiso 1 1 calc R . . C21 C 0.45037(17) 0.26951(15) 0.39389(13) 0.0296(3) Uani 1 1 d . . . C22 C 0.4212(2) 0.37649(17) 0.42852(15) 0.0377(4) Uani 1 1 d . . . H22 H 0.4499 0.4442 0.3803 0.045 Uiso 1 1 calc R . . C23 C 0.3503(2) 0.3850(2) 0.53290(17) 0.0488(5) Uani 1 1 d . . . H23 H 0.3311 0.4583 0.5563 0.059 Uiso 1 1 calc R . . C24 C 0.3081(2) 0.2879(2) 0.60221(17) 0.0561(6) Uani 1 1 d . . . H24 H 0.2582 0.2940 0.6735 0.067 Uiso 1 1 calc R . . C25 C 0.3375(3) 0.1812(2) 0.56933(18) 0.0642(7) Uani 1 1 d . . . H25 H 0.3085 0.1141 0.6183 0.077 Uiso 1 1 calc R . . C26 C 0.4091(2) 0.17078(19) 0.46516(16) 0.0488(5) Uani 1 1 d . . . H26 H 0.4297 0.0970 0.4428 0.059 Uiso 1 1 calc R . . C31 C 0.17348(16) 0.35348(14) 0.27667(13) 0.0278(3) Uani 1 1 d . . . C32 C 0.11405(19) 0.46228(16) 0.28584(15) 0.0354(4) Uani 1 1 d . . . H32 H 0.1524 0.5261 0.2358 0.042 Uiso 1 1 calc R . . C33 C -0.0013(2) 0.47769(19) 0.36801(17) 0.0448(5) Uani 1 1 d . . . H33 H -0.0433 0.5517 0.3730 0.054 Uiso 1 1 calc R . . C34 C -0.0548(2) 0.3861(2) 0.44218(17) 0.0497(5) Uani 1 1 d . . . H34 H -0.1336 0.3969 0.4985 0.060 Uiso 1 1 calc R . . C35 C 0.0054(2) 0.2788(2) 0.43516(18) 0.0547(6) Uani 1 1 d . . . H35 H -0.0310 0.2161 0.4875 0.066 Uiso 1 1 calc R . . C36 C 0.1189(2) 0.26156(17) 0.35213(16) 0.0426(4) Uani 1 1 d . . . H36 H 0.1592 0.1870 0.3470 0.051 Uiso 1 1 calc R . . C41 C 0.23990(16) 0.29979(14) 0.06337(13) 0.0273(3) Uani 1 1 d . . . C42 C 0.32118(19) 0.25003(16) -0.02286(14) 0.0344(4) Uani 1 1 d . . . H42 H 0.4147 0.2357 -0.0294 0.041 Uiso 1 1 calc R . . C43 C 0.2657(2) 0.22138(19) -0.09911(16) 0.0432(5) Uani 1 1 d . . . H43 H 0.3207 0.1856 -0.1569 0.052 Uiso 1 1 calc R . . C44 C 0.1305(2) 0.24470(19) -0.09122(16) 0.0452(5) Uani 1 1 d . . . H44 H 0.0926 0.2247 -0.1434 0.054 Uiso 1 1 calc R . . C45 C 0.0503(2) 0.2970(2) -0.00776(17) 0.0448(5) Uani 1 1 d . . . H45 H -0.0422 0.3143 -0.0035 0.054 Uiso 1 1 calc R . . C46 C 0.10406(18) 0.32446(18) 0.06991(15) 0.0375(4) Uani 1 1 d . . . H46 H 0.0483 0.3601 0.1275 0.045 Uiso 1 1 calc R . . Cl3 Cl 0.39846(6) 0.68593(5) 0.30184(5) 0.05506(14) Uani 1 1 d . . . Cl4 Cl 0.24984(7) 0.94114(5) 0.38554(4) 0.05990(16) Uani 1 1 d . . . Cl5 Cl 0.37302(8) 0.92773(5) 0.11629(4) 0.06407(18) Uani 1 1 d . . . Cl6 Cl 0.08849(7) 0.77436(5) 0.26519(7) 0.0696(2) Uani 1 1 d . . . Al Al 0.27849(6) 0.83234(4) 0.26574(4) 0.03185(11) 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 Sb 0.02835(6) 0.02183(6) 0.02899(6) -0.00232(4) -0.00924(4) -0.00034(4) Cl1 0.0326(2) 0.0408(2) 0.0521(3) -0.0054(2) -0.0192(2) -0.00612(18) Cl2 0.0387(2) 0.0375(2) 0.02592(19) -0.00342(16) -0.00601(16) 0.00156(17) P1 0.02499(19) 0.02183(18) 0.0265(2) -0.00272(15) -0.00984(16) 0.00095(15) P2 0.02132(18) 0.02438(19) 0.0269(2) -0.00310(15) -0.00744(15) -0.00103(15) C1 0.0273(8) 0.0237(7) 0.0316(8) -0.0055(6) -0.0108(6) -0.0009(6) C11 0.0281(8) 0.0226(8) 0.0456(10) 0.0002(7) -0.0130(7) 0.0021(6) C12 0.0365(10) 0.0338(10) 0.0510(12) -0.0064(8) -0.0089(9) 0.0072(8) C13 0.0405(12) 0.0369(11) 0.0835(18) -0.0096(11) -0.0011(11) 0.0114(9) C14 0.0341(11) 0.0363(12) 0.121(2) 0.0018(13) -0.0194(13) 0.0114(9) C15 0.0455(13) 0.0466(13) 0.109(2) 0.0042(14) -0.0448(14) 0.0055(10) C16 0.0419(11) 0.0369(10) 0.0668(14) -0.0008(9) -0.0298(10) 0.0018(8) C21 0.0299(8) 0.0350(9) 0.0256(8) -0.0013(7) -0.0112(7) -0.0040(7) C22 0.0421(10) 0.0386(10) 0.0306(9) -0.0056(7) -0.0078(8) 0.0035(8) C23 0.0482(12) 0.0625(14) 0.0360(10) -0.0165(10) -0.0094(9) 0.0086(10) C24 0.0500(13) 0.0884(19) 0.0285(10) -0.0090(11) -0.0068(9) -0.0083(12) C25 0.0781(18) 0.0751(17) 0.0338(11) 0.0142(11) -0.0108(11) -0.0324(14) C26 0.0685(15) 0.0424(11) 0.0359(10) 0.0046(8) -0.0168(10) -0.0172(10) C31 0.0253(8) 0.0311(8) 0.0277(8) -0.0066(6) -0.0070(6) -0.0018(6) C32 0.0358(9) 0.0337(9) 0.0350(9) -0.0076(7) -0.0068(7) 0.0024(7) C33 0.0412(11) 0.0474(11) 0.0446(11) -0.0187(9) -0.0056(9) 0.0080(9) C34 0.0386(11) 0.0653(14) 0.0400(11) -0.0198(10) 0.0042(9) -0.0034(10) C35 0.0517(13) 0.0538(13) 0.0440(12) -0.0012(10) 0.0095(10) -0.0129(10) C36 0.0425(11) 0.0353(10) 0.0417(11) -0.0031(8) 0.0008(8) -0.0041(8) C41 0.0267(8) 0.0294(8) 0.0263(8) -0.0005(6) -0.0090(6) -0.0043(6) C42 0.0313(9) 0.0416(10) 0.0313(9) -0.0072(7) -0.0091(7) -0.0009(7) C43 0.0483(11) 0.0523(12) 0.0321(9) -0.0110(8) -0.0123(8) -0.0054(9) C44 0.0502(12) 0.0563(13) 0.0360(10) -0.0010(9) -0.0222(9) -0.0163(10) C45 0.0310(9) 0.0627(13) 0.0440(11) 0.0013(10) -0.0189(8) -0.0079(9) C46 0.0265(8) 0.0514(11) 0.0358(9) -0.0056(8) -0.0105(7) -0.0007(8) Cl3 0.0479(3) 0.0402(3) 0.0746(4) -0.0017(2) -0.0191(3) 0.0125(2) Cl4 0.0964(5) 0.0364(3) 0.0388(3) -0.0113(2) 0.0004(3) -0.0168(3) Cl5 0.0997(5) 0.0400(3) 0.0361(3) -0.0018(2) 0.0057(3) -0.0033(3) Cl6 0.0625(4) 0.0503(3) 0.1113(6) 0.0115(3) -0.0578(4) -0.0105(3) Al 0.0374(3) 0.0235(2) 0.0340(3) -0.0038(2) -0.0092(2) 0.0000(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 Sb Cl2 2.3718(4) . ? Sb Cl1 2.4088(4) . ? Sb P1 2.6011(4) . ? Sb P2 3.0272(4) . ? Sb Cl3 3.5596(6) . ? Sb Cl2 3.7221(5) 2_665 ? P1 C11 1.7902(17) . ? P1 C21 1.7959(17) . ? P1 C1 1.8135(16) . ? P2 C31 1.8079(17) . ? P2 C41 1.8165(17) . ? P2 C1 1.8465(17) . ? C11 C12 1.391(3) . ? C11 C16 1.395(3) . ? C12 C13 1.385(3) . ? C13 C14 1.379(4) . ? C14 C15 1.369(4) . ? C15 C16 1.388(3) . ? C21 C22 1.389(3) . ? C21 C26 1.391(3) . ? C22 C23 1.384(3) . ? C23 C24 1.366(3) . ? C24 C25 1.377(4) . ? C25 C26 1.388(3) . ? C31 C36 1.388(3) . ? C31 C32 1.390(2) . ? C32 C33 1.388(3) . ? C33 C34 1.374(3) . ? C34 C35 1.374(3) . ? C35 C36 1.387(3) . ? C41 C46 1.393(2) . ? C41 C42 1.393(2) . ? C42 C43 1.387(3) . ? C43 C44 1.380(3) . ? C44 C45 1.379(3) . ? C45 C46 1.387(3) . ? Cl3 Al 2.1338(7) . ? Cl4 Al 2.1305(7) . ? Cl5 Al 2.1267(8) . ? Cl6 Al 2.1176(8) . ? 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 Cl2 Sb Cl1 96.328(17) . . ? Cl2 Sb P1 86.614(14) . . ? Cl1 Sb P1 85.517(15) . . ? Cl2 Sb P2 83.337(14) . . ? Cl1 Sb P2 146.721(15) . . ? P1 Sb P2 61.215(12) . . ? Cl2 Sb Cl3 157.104(15) . . ? Cl1 Sb Cl3 95.507(16) . . ? P1 Sb Cl3 113.830(14) . . ? P2 Sb Cl3 97.219(13) . . ? Cl2 Sb Cl2 86.255(14) . 2_665 ? Cl1 Sb Cl2 148.020(14) . 2_665 ? P1 Sb Cl2 126.459(12) . 2_665 ? P2 Sb Cl2 65.258(11) . 2_665 ? Cl3 Sb Cl2 73.448(12) . 2_665 ? C11 P1 C21 111.39(9) . . ? C11 P1 C1 110.62(8) . . ? C21 P1 C1 109.58(8) . . ? C11 P1 Sb 115.63(6) . . ? C21 P1 Sb 109.28(6) . . ? C1 P1 Sb 99.69(5) . . ? C31 P2 C41 104.84(8) . . ? C31 P2 C1 105.98(8) . . ? C41 P2 C1 104.71(7) . . ? C31 P2 Sb 114.85(5) . . ? C41 P2 Sb 134.62(5) . . ? C1 P2 Sb 85.22(5) . . ? P1 C1 P2 104.25(8) . . ? C12 C11 C16 120.40(18) . . ? C12 C11 P1 119.60(14) . . ? C16 C11 P1 119.80(15) . . ? C13 C12 C11 119.4(2) . . ? C14 C13 C12 120.1(2) . . ? C15 C14 C13 120.5(2) . . ? C14 C15 C16 120.7(2) . . ? C15 C16 C11 118.9(2) . . ? C22 C21 C26 119.49(17) . . ? C22 C21 P1 120.01(14) . . ? C26 C21 P1 120.35(15) . . ? C23 C22 C21 120.32(19) . . ? C24 C23 C22 120.0(2) . . ? C23 C24 C25 120.4(2) . . ? C24 C25 C26 120.5(2) . . ? C25 C26 C21 119.3(2) . . ? C36 C31 C32 119.40(16) . . ? C36 C31 P2 123.17(14) . . ? C32 C31 P2 117.36(13) . . ? C33 C32 C31 120.06(18) . . ? C34 C33 C32 120.09(19) . . ? C33 C34 C35 120.18(19) . . ? C34 C35 C36 120.4(2) . . ? C35 C36 C31 119.83(19) . . ? C46 C41 C42 119.40(16) . . ? C46 C41 P2 121.11(13) . . ? C42 C41 P2 119.41(13) . . ? C43 C42 C41 120.07(17) . . ? C44 C43 C42 120.10(19) . . ? C45 C44 C43 120.16(18) . . ? C44 C45 C46 120.31(18) . . ? C45 C46 C41 119.91(18) . . ? Al Cl3 Sb 132.17(3) . . ? Cl6 Al Cl5 109.91(4) . . ? Cl6 Al Cl4 109.48(4) . . ? Cl5 Al Cl4 108.65(3) . . ? Cl6 Al Cl3 108.19(3) . . ? Cl5 Al Cl3 111.77(4) . . ? Cl4 Al Cl3 108.80(4) . . ? 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 Cl2 Sb P1 C11 54.13(7) . . . . ? Cl1 Sb P1 C11 -42.50(7) . . . . ? P2 Sb P1 C11 138.38(7) . . . . ? Cl3 Sb P1 C11 -136.55(7) . . . . ? Cl2 Sb P1 C11 136.94(7) 2_665 . . . ? Cl2 Sb P1 C21 -179.27(6) . . . . ? Cl1 Sb P1 C21 84.11(6) . . . . ? P2 Sb P1 C21 -95.01(6) . . . . ? Cl3 Sb P1 C21 -9.94(6) . . . . ? Cl2 Sb P1 C21 -96.45(6) 2_665 . . . ? Cl2 Sb P1 C1 -64.44(6) . . . . ? Cl1 Sb P1 C1 -161.07(6) . . . . ? P2 Sb P1 C1 19.81(5) . . . . ? Cl3 Sb P1 C1 104.89(6) . . . . ? Cl2 Sb P1 C1 18.38(6) 2_665 . . . ? Cl2 Sb P2 C31 175.97(6) . . . . ? Cl1 Sb P2 C31 84.59(7) . . . . ? P1 Sb P2 C31 86.18(6) . . . . ? Cl3 Sb P2 C31 -27.09(6) . . . . ? Cl2 Sb P2 C31 -95.09(6) 2_665 . . . ? Cl2 Sb P2 C41 -35.43(8) . . . . ? Cl1 Sb P2 C41 -126.82(8) . . . . ? P1 Sb P2 C41 -125.22(8) . . . . ? Cl3 Sb P2 C41 121.51(8) . . . . ? Cl2 Sb P2 C41 53.50(8) 2_665 . . . ? Cl2 Sb P2 C1 70.56(5) . . . . ? Cl1 Sb P2 C1 -20.83(6) . . . . ? P1 Sb P2 C1 -19.23(5) . . . . ? Cl3 Sb P2 C1 -132.50(5) . . . . ? Cl2 Sb P2 C1 159.50(5) 2_665 . . . ? C11 P1 C1 P2 -152.39(8) . . . . ? C21 P1 C1 P2 84.43(10) . . . . ? Sb P1 C1 P2 -30.17(8) . . . . ? C31 P2 C1 P1 -89.21(9) . . . . ? C41 P2 C1 P1 160.26(8) . . . . ? Sb P2 C1 P1 25.29(7) . . . . ? C21 P1 C11 C12 156.23(15) . . . . ? C1 P1 C11 C12 34.09(17) . . . . ? Sb P1 C11 C12 -78.24(15) . . . . ? C21 P1 C11 C16 -28.93(18) . . . . ? C1 P1 C11 C16 -151.06(15) . . . . ? Sb P1 C11 C16 96.60(16) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? P1 C11 C12 C13 174.34(16) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C14 C15 C16 C11 1.3(4) . . . . ? C12 C11 C16 C15 -0.5(3) . . . . ? P1 C11 C16 C15 -175.33(17) . . . . ? C11 P1 C21 C22 127.46(15) . . . . ? C1 P1 C21 C22 -109.80(15) . . . . ? Sb P1 C21 C22 -1.52(16) . . . . ? C11 P1 C21 C26 -57.01(18) . . . . ? C1 P1 C21 C26 65.73(18) . . . . ? Sb P1 C21 C26 174.01(15) . . . . ? C26 C21 C22 C23 -0.6(3) . . . . ? P1 C21 C22 C23 174.93(16) . . . . ? C21 C22 C23 C24 -0.4(3) . . . . ? C22 C23 C24 C25 1.1(4) . . . . ? C23 C24 C25 C26 -0.7(4) . . . . ? C24 C25 C26 C21 -0.4(4) . . . . ? C22 C21 C26 C25 1.0(3) . . . . ? P1 C21 C26 C25 -174.53(18) . . . . ? C41 P2 C31 C36 85.18(17) . . . . ? C1 P2 C31 C36 -25.26(18) . . . . ? Sb P2 C31 C36 -117.39(15) . . . . ? C41 P2 C31 C32 -91.72(15) . . . . ? C1 P2 C31 C32 157.84(14) . . . . ? Sb P2 C31 C32 65.71(15) . . . . ? C36 C31 C32 C33 -2.0(3) . . . . ? P2 C31 C32 C33 175.02(15) . . . . ? C31 C32 C33 C34 1.8(3) . . . . ? C32 C33 C34 C35 -0.2(3) . . . . ? C33 C34 C35 C36 -1.3(4) . . . . ? C34 C35 C36 C31 1.1(4) . . . . ? C32 C31 C36 C35 0.6(3) . . . . ? P2 C31 C36 C35 -176.28(18) . . . . ? C31 P2 C41 C46 21.64(17) . . . . ? C1 P2 C41 C46 132.98(15) . . . . ? Sb P2 C41 C46 -129.07(13) . . . . ? C31 P2 C41 C42 -161.69(14) . . . . ? C1 P2 C41 C42 -50.34(16) . . . . ? Sb P2 C41 C42 47.60(18) . . . . ? C46 C41 C42 C43 -2.5(3) . . . . ? P2 C41 C42 C43 -179.23(15) . . . . ? C41 C42 C43 C44 1.6(3) . . . . ? C42 C43 C44 C45 0.3(3) . . . . ? C43 C44 C45 C46 -1.3(3) . . . . ? C44 C45 C46 C41 0.4(3) . . . . ? C42 C41 C46 C45 1.5(3) . . . . ? P2 C41 C46 C45 178.17(15) . . . . ? Cl2 Sb Cl3 Al 16.85(6) . . . . ? Cl1 Sb Cl3 Al 137.71(4) . . . . ? P1 Sb Cl3 Al -134.77(4) . . . . ? P2 Sb Cl3 Al -73.10(4) . . . . ? Cl2 Sb Cl3 Al -11.64(3) 2_665 . . . ? Sb Cl3 Al Cl6 72.96(5) . . . . ? Sb Cl3 Al Cl5 -48.19(5) . . . . ? Sb Cl3 Al Cl4 -168.18(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.011 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.049 data_dal1195 _database_code_depnum_ccdc_archive 'CCDC 844318' #TrackingRef '- complete-cif-package 13 Sep.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H18 Cl2 P2 Sb, C F3 O3 S' _chemical_formula_sum 'C7 H18 Cl2 F3 O3 P2 S Sb' _chemical_formula_weight 493.86 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' O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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' _cell_length_a 25.4181(11) _cell_length_b 6.4530(3) _cell_length_c 22.8805(10) _cell_angle_alpha 90.00 _cell_angle_beta 113.8889(4) _cell_angle_gamma 90.00 _cell_volume 3431.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 2.255 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3400 _exptl_absorpt_correction_T_max 0.5648 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14812 _diffrn_reflns_av_R_equivalents 0.0093 _diffrn_reflns_av_sigmaI/netI 0.0085 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3931 _reflns_number_gt 3845 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0185P)^2^+4.3640P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3931 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0149 _refine_ls_wR_factor_ref 0.0387 _refine_ls_wR_factor_gt 0.0385 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _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 Sb Sb 0.093610(4) 0.346593(15) 0.034452(4) 0.01861(4) Uani 1 1 d . . . Cl1 Cl 0.161858(18) 0.08280(6) 0.00816(2) 0.03012(8) Uani 1 1 d . . . Cl2 Cl 0.052923(17) 0.68663(6) 0.04907(2) 0.02987(8) Uani 1 1 d . . . P1 P 0.083588(16) 0.48353(6) -0.075743(17) 0.02019(8) Uani 1 1 d . . . P2 P 0.193145(16) 0.48834(6) 0.108612(18) 0.02136(8) Uani 1 1 d . . . C1 C 0.04360(8) 0.7197(3) -0.09914(8) 0.0320(4) Uani 1 1 d . . . H1A H 0.0416 0.7629 -0.1411 0.038 Uiso 1 1 calc R . . H1B H 0.0627 0.8277 -0.0675 0.038 Uiso 1 1 calc R . . H1C H 0.0046 0.6978 -0.1016 0.038 Uiso 1 1 calc R . . C2 C 0.14954(7) 0.5231(3) -0.08525(9) 0.0374(4) Uani 1 1 d . . . H2A H 0.1410 0.5745 -0.1285 0.045 Uiso 1 1 calc R . . H2B H 0.1704 0.3916 -0.0787 0.045 Uiso 1 1 calc R . . H2C H 0.1732 0.6248 -0.0538 0.045 Uiso 1 1 calc R . . C3 C 0.04278(8) 0.2919(3) -0.13260(8) 0.0305(3) Uani 1 1 d . . . H3A H 0.0376 0.3356 -0.1756 0.037 Uiso 1 1 calc R . . H3B H 0.0051 0.2758 -0.1310 0.037 Uiso 1 1 calc R . . H3C H 0.0633 0.1593 -0.1223 0.037 Uiso 1 1 calc R . . C4 C 0.18756(8) 0.7010(3) 0.15616(8) 0.0334(4) Uani 1 1 d . . . H4A H 0.2262 0.7504 0.1836 0.040 Uiso 1 1 calc R . . H4B H 0.1677 0.6552 0.1828 0.040 Uiso 1 1 calc R . . H4C H 0.1657 0.8136 0.1281 0.040 Uiso 1 1 calc R . . C5 C 0.23968(7) 0.5763(3) 0.07190(8) 0.0308(3) Uani 1 1 d . . . H5A H 0.2759 0.6261 0.1050 0.037 Uiso 1 1 calc R . . H5B H 0.2209 0.6892 0.0421 0.037 Uiso 1 1 calc R . . H5C H 0.2475 0.4613 0.0486 0.037 Uiso 1 1 calc R . . C6 C 0.23056(7) 0.2811(3) 0.16169(8) 0.0337(4) Uani 1 1 d . . . H6A H 0.2688 0.3290 0.1909 0.040 Uiso 1 1 calc R . . H6B H 0.2345 0.1635 0.1367 0.040 Uiso 1 1 calc R . . H6C H 0.2087 0.2380 0.1864 0.040 Uiso 1 1 calc R . . S S 0.114491(18) 0.31992(7) 0.235809(19) 0.02988(9) Uani 1 1 d . . . F1 F 0.11556(6) 0.0301(2) 0.31546(6) 0.0534(3) Uani 1 1 d . . . F2 F 0.13129(8) -0.0789(3) 0.23631(8) 0.0779(5) Uani 1 1 d . . . F3 F 0.04600(5) 0.0050(2) 0.22361(7) 0.0604(4) Uani 1 1 d . . . O1 O 0.10299(6) 0.3129(3) 0.16873(6) 0.0506(4) Uani 1 1 d . . . O2 O 0.07460(7) 0.4374(2) 0.25173(7) 0.0473(3) Uani 1 1 d . . . O3 O 0.17414(6) 0.3487(3) 0.27753(7) 0.0487(4) Uani 1 1 d . . . C7 C 0.10062(8) 0.0553(3) 0.25278(9) 0.0342(4) 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 Sb 0.01591(5) 0.02383(6) 0.01615(5) 0.00009(3) 0.00657(4) -0.00214(3) Cl1 0.03227(19) 0.02719(18) 0.0318(2) -0.00024(15) 0.01387(16) 0.00620(15) Cl2 0.02311(17) 0.0351(2) 0.03044(19) -0.00827(16) 0.00982(15) 0.00311(15) P1 0.02067(17) 0.02247(18) 0.01655(16) 0.00119(14) 0.00663(14) -0.00183(14) P2 0.01603(16) 0.02872(19) 0.01828(17) -0.00026(14) 0.00584(14) -0.00278(14) C1 0.0371(9) 0.0250(8) 0.0279(8) 0.0056(6) 0.0069(7) 0.0035(7) C2 0.0261(8) 0.0605(12) 0.0270(8) 0.0124(8) 0.0123(7) -0.0028(8) C3 0.0398(9) 0.0303(8) 0.0210(7) -0.0062(6) 0.0119(7) -0.0074(7) C4 0.0309(8) 0.0386(9) 0.0293(8) -0.0128(7) 0.0108(7) -0.0102(7) C5 0.0221(7) 0.0431(10) 0.0286(8) 0.0044(7) 0.0117(6) -0.0050(7) C6 0.0255(8) 0.0428(10) 0.0264(8) 0.0107(7) 0.0039(6) 0.0012(7) S 0.02409(19) 0.0442(2) 0.01952(18) 0.00080(16) 0.00689(15) -0.00733(16) F1 0.0586(8) 0.0601(8) 0.0361(6) 0.0140(6) 0.0136(6) -0.0128(6) F2 0.0901(12) 0.0605(9) 0.0851(11) -0.0108(9) 0.0374(10) 0.0331(9) F3 0.0403(7) 0.0530(8) 0.0652(9) 0.0029(7) -0.0022(6) -0.0198(6) O1 0.0386(8) 0.0911(12) 0.0207(6) 0.0056(7) 0.0104(6) -0.0151(8) O2 0.0495(8) 0.0410(8) 0.0496(8) -0.0034(7) 0.0181(7) 0.0091(7) O3 0.0275(7) 0.0824(12) 0.0300(7) 0.0004(7) 0.0053(5) -0.0206(7) C7 0.0309(8) 0.0372(9) 0.0310(9) -0.0033(7) 0.0089(7) 0.0015(7) _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 Sb Cl2 2.5052(4) . ? Sb P2 2.5768(4) . ? Sb P1 2.5851(4) . ? Sb Cl1 2.6673(4) . ? P1 C1 1.7892(17) . ? P1 C3 1.7902(17) . ? P1 C2 1.7940(17) . ? P2 C4 1.7921(18) . ? P2 C5 1.7974(16) . ? P2 C6 1.7977(18) . ? S O2 1.4265(15) . ? S O3 1.4396(13) . ? S O1 1.4422(13) . ? S C7 1.817(2) . ? F1 C7 1.337(2) . ? F2 C7 1.318(2) . ? F3 C7 1.314(2) . ? 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 Cl2 Sb P2 87.105(13) . . ? Cl2 Sb P1 87.010(14) . . ? P2 Sb P1 101.747(12) . . ? Cl2 Sb Cl1 158.503(14) . . ? P2 Sb Cl1 79.646(13) . . ? P1 Sb Cl1 79.302(13) . . ? C1 P1 C3 106.21(9) . . ? C1 P1 C2 106.74(9) . . ? C3 P1 C2 107.76(9) . . ? C1 P1 Sb 113.74(6) . . ? C3 P1 Sb 105.78(6) . . ? C2 P1 Sb 116.05(6) . . ? C4 P2 C5 105.72(9) . . ? C4 P2 C6 108.04(9) . . ? C5 P2 C6 106.39(8) . . ? C4 P2 Sb 111.93(6) . . ? C5 P2 Sb 117.43(6) . . ? C6 P2 Sb 106.89(6) . . ? O2 S O3 115.39(10) . . ? O2 S O1 115.45(10) . . ? O3 S O1 114.51(9) . . ? O2 S C7 103.03(9) . . ? O3 S C7 102.88(9) . . ? O1 S C7 102.98(9) . . ? F3 C7 F2 108.56(17) . . ? F3 C7 F1 107.31(16) . . ? F2 C7 F1 106.42(16) . . ? F3 C7 S 112.32(13) . . ? F2 C7 S 111.58(14) . . ? F1 C7 S 110.38(13) . . ? 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 Cl2 Sb P1 C1 -10.00(7) . . . . ? P2 Sb P1 C1 -96.41(7) . . . . ? Cl1 Sb P1 C1 -173.34(7) . . . . ? Cl2 Sb P1 C3 -126.17(7) . . . . ? P2 Sb P1 C3 147.41(7) . . . . ? Cl1 Sb P1 C3 70.48(7) . . . . ? Cl2 Sb P1 C2 114.43(8) . . . . ? P2 Sb P1 C2 28.01(8) . . . . ? Cl1 Sb P1 C2 -48.92(8) . . . . ? Cl2 Sb P2 C4 19.88(7) . . . . ? P1 Sb P2 C4 106.21(7) . . . . ? Cl1 Sb P2 C4 -177.13(7) . . . . ? Cl2 Sb P2 C5 -102.68(7) . . . . ? P1 Sb P2 C5 -16.34(7) . . . . ? Cl1 Sb P2 C5 60.32(7) . . . . ? Cl2 Sb P2 C6 137.99(7) . . . . ? P1 Sb P2 C6 -135.67(7) . . . . ? Cl1 Sb P2 C6 -59.01(7) . . . . ? O2 S C7 F3 53.29(16) . . . . ? O3 S C7 F3 173.58(14) . . . . ? O1 S C7 F3 -67.11(15) . . . . ? O2 S C7 F2 175.46(14) . . . . ? O3 S C7 F2 -64.25(15) . . . . ? O1 S C7 F2 55.06(16) . . . . ? O2 S C7 F1 -66.42(14) . . . . ? O3 S C7 F1 53.87(15) . . . . ? O1 S C7 F1 173.18(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.396 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.056