# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- CrystallographicData.cif' #====================================================================== _publ_contact_author 'Keith B. Dillon' _publ_contact_author_name 'Keith B. Dillon' _publ_contact_author_email k.b.dillon@dur.ac.uk _publ_contact_author_address ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; loop_ _publ_author_name _publ_author_address 'Rachel Bashforth' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; A.J.Boyall ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; K.B.Dillon ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; A.E.Goeta ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; J.A.K.Howard ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; ; A.M.Kenwright ; ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; P.K.Monks ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; M.R.Probert ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; H.J.Shepherd ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; A.L.Thompson ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE UK ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? _publ_section_title ; Synthesis of Cyclic Dicationic Derivatives of Diphosphanes with Three (3P) or Four (4P) Linked Phosphorus Atoms: Investigations into the Relative Stabilities of 3P and 4P Systems. ; #====================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 840422' #TrackingRef '- CrystallographicData.cif' #====================================================================== _audit_creation_date 2011-07-07 _audit_creation_method ; Olex2 1.1-beta (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '1(C29 H55 P3), 2(Al2 Cl5 O)' _chemical_formula_sum 'C29 H55 Al4 Cl10 O2 P3' _chemical_formula_weight 991.06 _chemical_melting_point ? 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' 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system Triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.6187(5) _cell_length_b 10.6364(5) _cell_length_c 21.8815(11) _cell_angle_alpha 91.914(2) _cell_angle_beta 94.314(2) _cell_angle_gamma 111.132(2) _cell_volume 2293.80(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 21164 _cell_measurement_temperature 120.0 _cell_measurement_theta_max 25.03 _cell_measurement_theta_min 0.94 _exptl_absorpt_coefficient_mu 0.816 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1024 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_unetI/netI 0.0894 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 21164 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 0.94 _diffrn_ambient_temperature 120.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD area detector diffractometer' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5365 _reflns_number_total 8111 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.763 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_hydrogen_treatment riding _refine_ls_matrix_type full _refine_ls_number_parameters 790 _refine_ls_number_reflns 8111 _refine_ls_number_restraints 1531 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0463 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.1143 _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. The entire structure (both anions and cations) shows orientational whole molecule disorder, a major component with occupancy of 88% and a minor component with occupancy of 12%. SAME restraints have been applied to ensure that the bond lengths and angles (though not torsion angles) for related sets of atoms are consistent. This type of disorder may in some cases indicate twinning or missed symmetry. In this case, despite extensive investigation no twin law or change in symmetry could be identified. Inspection of raw fram data did not indicate any reflections at positions not predicted by the orientation matrix. Thus the current model, including disorder, is somewhat tentatively presented. These limitations have no impact on the conclusions drawn as to chemical connectivity of the species. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 P1A P 0.4939(8) 0.1613(7) 0.1827(3) 0.0166(2) Uani 0.1127(8) 1 d PDU A 1 P2A P 0.5353(7) 0.1715(6) 0.2839(3) 0.0185(2) Uani 0.1127(8) 1 d PDU A 1 P3A P 0.5960(8) 0.3868(6) 0.3099(3) 0.0171(2) Uani 0.1127(8) 1 d PDU A 1 C5A C 0.672(2) 0.4852(15) 0.2488(6) 0.024(3) Uani 0.1127(8) 1 d PDU A 1 H5AA H 0.6796 0.5792 0.2590 0.028 Uiso 0.1127(8) 1 calc PR A 1 H5AB H 0.7655 0.4860 0.2491 0.028 Uiso 0.1127(8) 1 calc PR A 1 C6A C 0.7248(14) 0.4070(18) 0.3746(6) 0.023(2) Uani 0.1127(8) 1 d PDU A 1 H6A H 0.7552 0.5018 0.3928 0.028 Uiso 0.1127(8) 1 calc PR A 1 C7A C 0.8500(18) 0.382(3) 0.3546(8) 0.028(2) Uani 0.1127(8) 1 d PDU A 1 H7AA H 0.8214 0.2905 0.3341 0.033 Uiso 0.1127(8) 1 calc PR A 1 H7AB H 0.8935 0.4483 0.3247 0.033 Uiso 0.1127(8) 1 calc PR A 1 C8A C 0.9521(18) 0.395(3) 0.4095(11) 0.029(3) Uani 0.1127(8) 1 d PDU A 1 H8AA H 0.9893 0.4895 0.4268 0.034 Uiso 0.1127(8) 1 calc PR A 1 H8AB H 1.0282 0.3718 0.3956 0.034 Uiso 0.1127(8) 1 calc PR A 1 C9A C 0.887(2) 0.301(3) 0.4603(11) 0.029(3) Uani 0.1127(8) 1 d PDU A 1 H9AA H 0.8608 0.2054 0.4449 0.035 Uiso 0.1127(8) 1 calc PR A 1 H9AB H 0.9547 0.3174 0.4964 0.035 Uiso 0.1127(8) 1 calc PR A 1 C11A C 0.6622(19) 0.312(4) 0.4240(10) 0.024(3) Uani 0.1127(8) 1 d PDU A 1 H11C H 0.6270 0.2175 0.4062 0.028 Uiso 0.1127(8) 1 calc PR A 1 H11D H 0.5847 0.3321 0.4381 0.028 Uiso 0.1127(8) 1 calc PR A 1 C10A C 0.765(2) 0.325(3) 0.4794(8) 0.030(3) Uani 0.1127(8) 1 d PDU A 1 H10C H 0.7935 0.4167 0.4998 0.036 Uiso 0.1127(8) 1 calc PR A 1 H10D H 0.7215 0.2590 0.5094 0.036 Uiso 0.1127(8) 1 calc PR A 1 C12A C 0.4648(15) 0.4427(18) 0.3373(8) 0.023(3) Uani 0.1127(8) 1 d PDU A 1 H12A H 0.4126 0.3728 0.3646 0.027 Uiso 0.1127(8) 1 calc PR A 1 C17A C 0.362(2) 0.453(3) 0.2865(9) 0.030(3) Uani 0.1127(8) 1 d PDU A 1 H17C H 0.4084 0.5213 0.2580 0.035 Uiso 0.1127(8) 1 calc PR A 1 H17D H 0.3185 0.3647 0.2627 0.035 Uiso 0.1127(8) 1 calc PR A 1 C16A C 0.2550(19) 0.492(3) 0.3156(13) 0.036(3) Uani 0.1127(8) 1 d PDU A 1 H16C H 0.1881 0.4981 0.2829 0.043 Uiso 0.1127(8) 1 calc PR A 1 H16D H 0.2064 0.4208 0.3424 0.043 Uiso 0.1127(8) 1 calc PR A 1 C15A C 0.314(3) 0.624(3) 0.3526(14) 0.033(3) Uani 0.1127(8) 1 d PDU A 1 H15C H 0.2408 0.6440 0.3715 0.039 Uiso 0.1127(8) 1 calc PR A 1 H15D H 0.3560 0.6972 0.3253 0.039 Uiso 0.1127(8) 1 calc PR A 1 C13A C 0.5280(19) 0.576(2) 0.3774(11) 0.023(3) Uani 0.1127(8) 1 d PDU A 1 H13C H 0.5874 0.5644 0.4120 0.028 Uiso 0.1127(8) 1 calc PR A 1 H13D H 0.5849 0.6475 0.3526 0.028 Uiso 0.1127(8) 1 calc PR A 1 C14A C 0.420(2) 0.622(3) 0.4029(11) 0.029(3) Uani 0.1127(8) 1 d PDU A 1 H14C H 0.3756 0.5605 0.4341 0.035 Uiso 0.1127(8) 1 calc PR A 1 H14D H 0.4649 0.7140 0.4233 0.035 Uiso 0.1127(8) 1 calc PR A 1 C1A C 0.3657(17) 0.0902(18) 0.3109(11) 0.020(3) Uani 0.1127(8) 1 d PDU A 1 H1AA H 0.3616 0.1337 0.3511 0.023 Uiso 0.1127(8) 1 calc PR A 1 H1AB H 0.2958 0.1008 0.2812 0.023 Uiso 0.1127(8) 1 calc PR A 1 C2A C 0.338(2) -0.0606(18) 0.3175(13) 0.020(5) Uani 0.1127(8) 1 d PDU A 1 H2AA H 0.3551 -0.1003 0.2793 0.030 Uiso 0.1127(8) 1 calc PR A 1 H2AB H 0.2436 -0.1068 0.3256 0.030 Uiso 0.1127(8) 1 calc PR A 1 H2AC H 0.3983 -0.0708 0.3516 0.030 Uiso 0.1127(8) 1 calc PR A 1 C3A C 0.6147(18) 0.3162(13) 0.1551(7) 0.021(4) Uani 0.1127(8) 1 d PDU A 1 H3AA H 0.7078 0.3175 0.1646 0.026 Uiso 0.1127(8) 1 calc PR A 1 H3AB H 0.5977 0.3138 0.1099 0.026 Uiso 0.1127(8) 1 calc PR A 1 C4A C 0.606(3) 0.4471(17) 0.1832(7) 0.021(3) Uani 0.1127(8) 1 d PDU A 1 H4AA H 0.6511 0.5220 0.1572 0.026 Uiso 0.1127(8) 1 calc PR A 1 H4AB H 0.5098 0.4368 0.1825 0.026 Uiso 0.1127(8) 1 calc PR A 1 C24A C 0.5353(19) 0.0173(16) 0.1589(7) 0.023(2) Uani 0.1127(8) 1 d PDU A 1 H24A H 0.4750 -0.0626 0.1790 0.027 Uiso 0.1127(8) 1 calc PR A 1 C29A C 0.507(2) -0.016(2) 0.0886(8) 0.026(3) Uani 0.1127(8) 1 d PDU A 1 H29C H 0.4107 -0.0308 0.0757 0.031 Uiso 0.1127(8) 1 calc PR A 1 H29D H 0.5646 0.0615 0.0670 0.031 Uiso 0.1127(8) 1 calc PR A 1 C28A C 0.536(2) -0.142(2) 0.0711(11) 0.025(3) Uani 0.1127(8) 1 d PDU A 1 H28C H 0.4726 -0.2209 0.0898 0.030 Uiso 0.1127(8) 1 calc PR A 1 H28D H 0.5222 -0.1600 0.0260 0.030 Uiso 0.1127(8) 1 calc PR A 1 C27A C 0.681(2) -0.123(3) 0.0935(11) 0.031(3) Uani 0.1127(8) 1 d PDU A 1 H27C H 0.7440 -0.0493 0.0720 0.037 Uiso 0.1127(8) 1 calc PR A 1 H27D H 0.6973 -0.2070 0.0831 0.037 Uiso 0.1127(8) 1 calc PR A 1 C25A C 0.683(2) 0.036(3) 0.1808(11) 0.028(3) Uani 0.1127(8) 1 d PDU A 1 H25C H 0.7464 0.1153 0.1620 0.034 Uiso 0.1127(8) 1 calc PR A 1 H25D H 0.6985 0.0539 0.2260 0.034 Uiso 0.1127(8) 1 calc PR A 1 C26A C 0.710(4) -0.090(4) 0.1625(13) 0.030(3) Uani 0.1127(8) 1 d PDU A 1 H26C H 0.6524 -0.1667 0.1843 0.036 Uiso 0.1127(8) 1 calc PR A 1 H26D H 0.8062 -0.0759 0.1750 0.036 Uiso 0.1127(8) 1 calc PR A 1 C18A C 0.3238(11) 0.1446(18) 0.1553(8) 0.022(3) Uani 0.1127(8) 1 d PDU A 1 H18A H 0.3032 0.2111 0.1823 0.026 Uiso 0.1127(8) 1 calc PR A 1 C19A C 0.2127(15) 0.010(2) 0.1636(11) 0.023(3) Uani 0.1127(8) 1 d PDU A 1 H19C H 0.2189 -0.0128 0.2070 0.028 Uiso 0.1127(8) 1 calc PR A 1 H19D H 0.2249 -0.0618 0.1376 0.028 Uiso 0.1127(8) 1 calc PR A 1 C20A C 0.0732(15) 0.016(3) 0.1462(11) 0.024(3) Uani 0.1127(8) 1 d PDU A 1 H20C H 0.0028 -0.0743 0.1486 0.029 Uiso 0.1127(8) 1 calc PR A 1 H20D H 0.0564 0.0793 0.1759 0.029 Uiso 0.1127(8) 1 calc PR A 1 C21A C 0.062(2) 0.063(3) 0.0821(11) 0.026(3) Uani 0.1127(8) 1 d PDU A 1 H21C H -0.0271 0.0728 0.0742 0.031 Uiso 0.1127(8) 1 calc PR A 1 H21D H 0.0646 -0.0076 0.0519 0.031 Uiso 0.1127(8) 1 calc PR A 1 C23A C 0.3148(18) 0.193(3) 0.0904(10) 0.025(3) Uani 0.1127(8) 1 d PDU A 1 H23C H 0.3840 0.2847 0.0887 0.030 Uiso 0.1127(8) 1 calc PR A 1 H23D H 0.3343 0.1318 0.0607 0.030 Uiso 0.1127(8) 1 calc PR A 1 C22A C 0.1745(19) 0.196(2) 0.0724(12) 0.028(2) Uani 0.1127(8) 1 d PDU A 1 H22C H 0.1679 0.2163 0.0287 0.034 Uiso 0.1127(8) 1 calc PR A 1 H22D H 0.1621 0.2697 0.0973 0.034 Uiso 0.1127(8) 1 calc PR A 1 P1 P 0.40664(10) 0.12108(10) 0.19252(4) 0.0171(2) Uani 0.8873(8) 1 d PDU A 2 P2 P 0.46834(10) 0.33892(10) 0.21700(4) 0.0185(2) Uani 0.8873(8) 1 d PDU A 2 P3 P 0.50960(10) 0.35178(10) 0.31768(4) 0.0166(2) Uani 0.8873(8) 1 d PDU A 2 C5 C 0.3846(4) 0.2020(4) 0.34314(17) 0.0197(8) Uani 0.8873(8) 1 d PDU A 2 H5A H 0.3924 0.2078 0.3886 0.024 Uiso 0.8873(8) 1 calc PR A 2 H5B H 0.2933 0.2000 0.3287 0.024 Uiso 0.8873(8) 1 calc PR A 2 C6 C 0.4755(4) 0.5008(4) 0.34258(18) 0.0210(8) Uani 0.8873(8) 1 d PDU A 2 H6 H 0.5479 0.5809 0.3281 0.025 Uiso 0.8873(8) 1 calc PR A 2 C7 C 0.3389(5) 0.5005(5) 0.3134(2) 0.0337(10) Uani 0.8873(8) 1 d PDU A 2 H7A H 0.3354 0.4893 0.2681 0.040 Uiso 0.8873(8) 1 calc PR A 2 H7B H 0.2639 0.4236 0.3273 0.040 Uiso 0.8873(8) 1 calc PR A 2 C8 C 0.3214(5) 0.6329(5) 0.3315(2) 0.0380(12) Uani 0.8873(8) 1 d PDU A 2 H8A H 0.2328 0.6313 0.3131 0.046 Uiso 0.8873(8) 1 calc PR A 2 H8B H 0.3937 0.7094 0.3157 0.046 Uiso 0.8873(8) 1 calc PR A 2 C9 C 0.3287(4) 0.6523(5) 0.4026(2) 0.0352(10) Uani 0.8873(8) 1 d PDU A 2 H9A H 0.3195 0.7392 0.4141 0.042 Uiso 0.8873(8) 1 calc PR A 2 H9B H 0.2530 0.5787 0.4181 0.042 Uiso 0.8873(8) 1 calc PR A 2 C11 C 0.4840(4) 0.5214(4) 0.41224(17) 0.0242(9) Uani 0.8873(8) 1 d PDU A 2 H11A H 0.5742 0.5267 0.4302 0.029 Uiso 0.8873(8) 1 calc PR A 2 H11B H 0.4146 0.4431 0.4285 0.029 Uiso 0.8873(8) 1 calc PR A 2 C10 C 0.4611(4) 0.6515(4) 0.43122(19) 0.0271(9) Uani 0.8873(8) 1 d PDU A 2 H10A H 0.4625 0.6599 0.4765 0.033 Uiso 0.8873(8) 1 calc PR A 2 H10B H 0.5360 0.7304 0.4186 0.033 Uiso 0.8873(8) 1 calc PR A 2 C12 C 0.6780(4) 0.3581(4) 0.34576(17) 0.0189(8) Uani 0.8873(8) 1 d PDU A 2 H12 H 0.6983 0.2914 0.3187 0.023 Uiso 0.8873(8) 1 calc PR A 2 C17 C 0.7911(4) 0.4956(4) 0.34022(19) 0.0240(9) Uani 0.8873(8) 1 d PDU A 2 H17A H 0.7857 0.5243 0.2978 0.029 Uiso 0.8873(8) 1 calc PR A 2 H17B H 0.7802 0.5646 0.3686 0.029 Uiso 0.8873(8) 1 calc PR A 2 C16 C 0.9279(4) 0.4831(4) 0.35604(19) 0.0275(9) Uani 0.8873(8) 1 d PDU A 2 H16A H 0.9399 0.4177 0.3260 0.033 Uiso 0.8873(8) 1 calc PR A 2 H16B H 1.0008 0.5717 0.3528 0.033 Uiso 0.8873(8) 1 calc PR A 2 C15 C 0.9406(4) 0.4376(4) 0.4194(2) 0.0314(11) Uani 0.8873(8) 1 d PDU A 2 H15A H 0.9392 0.5081 0.4498 0.038 Uiso 0.8873(8) 1 calc PR A 2 H15B H 1.0288 0.4260 0.4268 0.038 Uiso 0.8873(8) 1 calc PR A 2 C13 C 0.6873(4) 0.3137(5) 0.41209(19) 0.0263(10) Uani 0.8873(8) 1 d PDU A 2 H13A H 0.6731 0.3796 0.4412 0.032 Uiso 0.8873(8) 1 calc PR A 2 H13B H 0.6154 0.2245 0.4155 0.032 Uiso 0.8873(8) 1 calc PR A 2 C14 C 0.8265(4) 0.3050(4) 0.4287(2) 0.0287(9) Uani 0.8873(8) 1 d PDU A 2 H14A H 0.8335 0.2830 0.4722 0.034 Uiso 0.8873(8) 1 calc PR A 2 H14B H 0.8360 0.2314 0.4028 0.034 Uiso 0.8873(8) 1 calc PR A 2 C1 C 0.6351(4) 0.4151(4) 0.18665(19) 0.0225(10) Uani 0.8873(8) 1 d PDU A 2 H1A H 0.7046 0.3934 0.2122 0.027 Uiso 0.8873(8) 1 calc PR A 2 H1B H 0.6309 0.3780 0.1441 0.027 Uiso 0.8873(8) 1 calc PR A 2 C2 C 0.6736(4) 0.5692(4) 0.18743(19) 0.0279(10) Uani 0.8873(8) 1 d PDU A 2 H2A H 0.6094 0.5903 0.1589 0.042 Uiso 0.8873(8) 1 calc PR A 2 H2B H 0.7655 0.6110 0.1749 0.042 Uiso 0.8873(8) 1 calc PR A 2 H2C H 0.6703 0.6044 0.2290 0.042 Uiso 0.8873(8) 1 calc PR A 2 C3 C 0.3313(4) 0.0192(4) 0.25523(16) 0.0217(9) Uani 0.8873(8) 1 d PDU A 2 H3A H 0.2352 0.0108 0.2539 0.026 Uiso 0.8873(8) 1 calc PR A 2 H3B H 0.3320 -0.0727 0.2471 0.026 Uiso 0.8873(8) 1 calc PR A 2 C4 C 0.3972(4) 0.0692(4) 0.32069(17) 0.0184(9) Uani 0.8873(8) 1 d PDU A 2 H4A H 0.3544 -0.0011 0.3491 0.022 Uiso 0.8873(8) 1 calc PR A 2 H4B H 0.4944 0.0820 0.3222 0.022 Uiso 0.8873(8) 1 calc PR A 2 C24 C 0.2750(4) 0.0950(4) 0.12966(17) 0.0216(8) Uani 0.8873(8) 1 d PDU A 2 H24 H 0.2418 -0.0024 0.1149 0.026 Uiso 0.8873(8) 1 calc PR A 2 C29 C 0.3371(4) 0.1793(4) 0.07557(17) 0.0219(10) Uani 0.8873(8) 1 d PDU A 2 H29A H 0.3739 0.2765 0.0891 0.026 Uiso 0.8873(8) 1 calc PR A 2 H29B H 0.4126 0.1542 0.0625 0.026 Uiso 0.8873(8) 1 calc PR A 2 C28 C 0.2295(4) 0.1539(4) 0.02176(18) 0.0278(9) Uani 0.8873(8) 1 d PDU A 2 H28A H 0.2689 0.2124 -0.0115 0.033 Uiso 0.8873(8) 1 calc PR A 2 H28B H 0.2000 0.0587 0.0055 0.033 Uiso 0.8873(8) 1 calc PR A 2 C27 C 0.1076(4) 0.1828(4) 0.04113(19) 0.0289(10) Uani 0.8873(8) 1 d PDU A 2 H27A H 0.0378 0.1615 0.0058 0.035 Uiso 0.8873(8) 1 calc PR A 2 H27B H 0.1355 0.2800 0.0536 0.035 Uiso 0.8873(8) 1 calc PR A 2 C25 C 0.1521(4) 0.1253(4) 0.14918(18) 0.0254(9) Uani 0.8873(8) 1 d PDU A 2 H25A H 0.1114 0.0668 0.1822 0.030 Uiso 0.8873(8) 1 calc PR A 2 H25B H 0.1815 0.2206 0.1652 0.030 Uiso 0.8873(8) 1 calc PR A 2 C26 C 0.0474(4) 0.0996(5) 0.09428(19) 0.0284(11) Uani 0.8873(8) 1 d PDU A 2 H26A H -0.0298 0.1228 0.1066 0.034 Uiso 0.8873(8) 1 calc PR A 2 H26B H 0.0125 0.0025 0.0807 0.034 Uiso 0.8873(8) 1 calc PR A 2 C18 C 0.5392(4) 0.0708(4) 0.16420(17) 0.0195(8) Uani 0.8873(8) 1 d PDU A 2 H18 H 0.5841 0.1365 0.1337 0.023 Uiso 0.8873(8) 1 calc PR A 2 C19 C 0.6488(4) 0.0756(4) 0.21491(18) 0.0258(9) Uani 0.8873(8) 1 d PDU A 2 H19A H 0.6902 0.1680 0.2348 0.031 Uiso 0.8873(8) 1 calc PR A 2 H19B H 0.6077 0.0130 0.2466 0.031 Uiso 0.8873(8) 1 calc PR A 2 C20 C 0.7578(4) 0.0351(4) 0.1871(2) 0.0304(10) Uani 0.8873(8) 1 d PDU A 2 H20A H 0.8026 0.1013 0.1574 0.036 Uiso 0.8873(8) 1 calc PR A 2 H20B H 0.8276 0.0363 0.2200 0.036 Uiso 0.8873(8) 1 calc PR A 2 C21 C 0.6965(6) -0.1050(6) 0.1547(2) 0.0338(11) Uani 0.8873(8) 1 d PDU A 2 H21A H 0.6569 -0.1720 0.1849 0.041 Uiso 0.8873(8) 1 calc PR A 2 H21B H 0.7685 -0.1282 0.1365 0.041 Uiso 0.8873(8) 1 calc PR A 2 C23 C 0.4766(4) -0.0700(4) 0.1300(2) 0.0287(9) Uani 0.8873(8) 1 d PDU A 2 H23A H 0.4280 -0.1371 0.1586 0.034 Uiso 0.8873(8) 1 calc PR A 2 H23B H 0.4101 -0.0685 0.0960 0.034 Uiso 0.8873(8) 1 calc PR A 2 C22 C 0.5862(4) -0.1117(4) 0.10406(19) 0.0283(9) Uani 0.8873(8) 1 d PDU A 2 H22A H 0.6273 -0.0509 0.0718 0.034 Uiso 0.8873(8) 1 calc PR A 2 H22B H 0.5448 -0.2049 0.0850 0.034 Uiso 0.8873(8) 1 calc PR A 2 Al2 Al 1.09733(16) 0.55344(17) 0.13319(9) 0.0212(4) Uani 0.8873(8) 1 d PDU A 2 Cl3 Cl 1.08063(11) 0.74017(11) 0.16147(5) 0.0354(3) Uani 0.8873(8) 1 d PDU A 2 Cl4 Cl 1.30354(11) 0.56808(12) 0.14164(5) 0.0306(3) Uani 0.8873(8) 1 d PDU A 2 Cl5 Cl 0.97562(17) 0.39527(11) 0.18389(7) 0.0332(3) Uani 0.8873(8) 1 d PDU A 2 O1 O 1.0393(3) 0.5132(4) 0.05446(15) 0.0198(7) Uani 0.8873(8) 1 d PDU . 2 Al1 Al 0.8739(2) 0.4343(2) 0.01328(15) 0.0198(5) Uani 0.8873(8) 1 d PDU . 2 Cl1 Cl 0.78361(14) 0.22222(15) 0.01483(8) 0.0300(3) Uani 0.8873(8) 1 d PDU A 2 Cl2 Cl 0.73492(13) 0.52236(13) 0.03657(6) 0.0332(3) Uani 0.8873(8) 1 d PDU A 2 Al4 Al -0.05550(16) -0.02840(18) 0.36281(10) 0.0224(4) Uani 0.8873(8) 1 d PDU A 2 Cl8 Cl 0.02749(12) 0.16384(11) 0.32516(6) 0.0292(3) Uani 0.8873(8) 1 d PDU A 2 Cl9 Cl 0.03982(13) -0.15679(11) 0.32817(6) 0.0439(3) Uani 0.8873(8) 1 d PDU A 2 Cl10 Cl -0.27010(13) -0.11438(14) 0.34317(6) 0.0448(4) Uani 0.8873(8) 1 d PDU A 2 O2 O -0.0234(3) -0.0058(4) 0.44361(15) 0.0193(7) Uani 0.8873(8) 1 d PDU . 2 Al3 Al 0.1256(3) 0.0799(3) 0.49545(16) 0.0190(5) Uani 0.8873(8) 1 d PDU . 2 Cl6 Cl 0.18677(16) 0.29174(16) 0.49847(7) 0.0283(3) Uani 0.8873(8) 1 d PDU A 2 Cl7 Cl 0.28717(14) 0.01422(13) 0.48114(6) 0.0279(3) Uani 0.8873(8) 1 d PDU A 2 Al2A Al 1.0599(13) 0.5391(15) 0.1395(8) 0.033(3) Uani 0.1127(8) 1 d PDU A 1 Cl3A Cl 0.9585(9) 0.6684(8) 0.1683(4) 0.0354(3) Uani 0.1127(8) 1 d PDU A 1 Cl4A Cl 1.2763(9) 0.6189(10) 0.1550(4) 0.0306(3) Uani 0.1127(8) 1 d PDU A 1 Cl5A Cl 0.9765(16) 0.3501(12) 0.1796(7) 0.0332(3) Uani 0.1127(8) 1 d PDU A 1 O1A O 1.029(2) 0.510(3) 0.0585(9) 0.024(3) Uani 0.1127(8) 1 d PDU . 1 Al1A Al 0.881(2) 0.416(2) 0.0071(13) 0.025(3) Uani 0.1127(8) 1 d PDU . 1 Cl1A Cl 0.8165(14) 0.2056(14) 0.0067(8) 0.0300(3) Uani 0.1127(8) 1 d PDU A 1 Cl2A Cl 0.7169(13) 0.4742(12) 0.0206(6) 0.0332(3) Uani 0.1127(8) 1 d PDU A 1 Al4A Al -0.0920(14) -0.0489(15) 0.3671(8) 0.028(3) Uani 0.1127(8) 1 d PDU A 1 Cl8A Cl 0.0344(12) 0.1131(10) 0.3188(6) 0.0292(3) Uani 0.1127(8) 1 d PDU A 1 Cl9A Cl -0.0660(11) -0.2291(9) 0.3368(4) 0.0439(3) Uani 0.1127(8) 1 d PDU A 1 Cl Cl -0.2945(10) -0.0592(13) 0.3575(5) 0.0448(4) Uani 0.1127(8) 1 d PDU A 1 O2A O -0.036(2) -0.015(3) 0.4464(10) 0.021(3) Uani 0.1127(8) 1 d PDU . 1 Al3A Al 0.127(2) 0.063(2) 0.4898(14) 0.023(3) Uani 0.1127(8) 1 d PDU . 1 Cl6A Cl 0.2097(16) 0.2730(15) 0.4863(8) 0.0283(3) Uani 0.1127(8) 1 d PDU A 1 Cl7A Cl 0.2686(15) -0.0236(14) 0.4674(7) 0.0279(3) Uani 0.1127(8) 1 d PDU A 1 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 P1A 0.0149(5) 0.0186(5) 0.0160(5) 0.0009(4) 0.0013(4) 0.0057(4) P2A 0.0206(5) 0.0176(5) 0.0167(5) 0.0016(4) 0.0010(4) 0.0064(4) P3A 0.0167(5) 0.0168(5) 0.0170(5) 0.0008(4) 0.0012(4) 0.0054(4) C5A 0.023(5) 0.022(5) 0.019(5) 0.003(5) 0.002(5) -0.001(5) C6A 0.020(4) 0.026(4) 0.027(4) 0.003(3) -0.001(4) 0.012(3) C7A 0.023(4) 0.028(4) 0.032(4) 0.003(4) 0.000(4) 0.011(3) C8A 0.025(5) 0.029(5) 0.035(5) 0.005(5) -0.001(4) 0.015(4) C9A 0.027(5) 0.028(5) 0.036(5) 0.003(5) -0.002(5) 0.016(5) C11A 0.022(5) 0.026(4) 0.026(5) 0.004(4) 0.000(4) 0.013(4) C10A 0.028(5) 0.031(5) 0.031(5) 0.003(5) 0.000(5) 0.011(5) C12A 0.022(4) 0.026(4) 0.024(4) -0.003(4) 0.002(4) 0.013(4) C17A 0.030(5) 0.034(5) 0.029(5) -0.005(5) 0.000(5) 0.017(5) C16A 0.035(5) 0.042(5) 0.036(5) -0.008(5) -0.001(5) 0.021(5) C15A 0.033(4) 0.036(4) 0.036(4) -0.005(4) 0.003(4) 0.022(4) C13A 0.025(4) 0.025(4) 0.024(5) -0.002(4) 0.004(4) 0.014(4) C14A 0.030(4) 0.030(4) 0.030(4) -0.003(4) 0.003(4) 0.015(4) C1A 0.017(5) 0.021(5) 0.018(5) 0.006(5) 0.004(5) 0.003(5) C2A 0.020(9) 0.016(9) 0.014(9) 0.006(8) 0.010(8) -0.006(8) C3A 0.023(6) 0.021(6) 0.017(6) -0.001(5) 0.007(5) 0.003(5) C4A 0.023(5) 0.020(5) 0.020(5) 0.000(5) 0.004(5) 0.005(5) C24A 0.021(4) 0.025(4) 0.024(4) 0.001(4) 0.005(3) 0.010(4) C29A 0.024(4) 0.027(5) 0.028(5) 0.001(4) 0.003(4) 0.009(4) C28A 0.025(5) 0.024(5) 0.029(5) 0.002(5) 0.005(5) 0.011(5) C27A 0.031(5) 0.029(5) 0.035(5) 0.004(5) 0.004(5) 0.014(5) C25A 0.028(4) 0.031(4) 0.030(4) 0.005(4) 0.005(4) 0.015(4) C26A 0.031(5) 0.032(5) 0.034(5) 0.005(4) 0.006(4) 0.018(4) C18A 0.020(4) 0.027(4) 0.017(4) 0.001(4) 0.001(4) 0.008(4) C19A 0.023(4) 0.027(4) 0.019(4) -0.001(4) 0.000(4) 0.009(4) C20A 0.022(4) 0.030(5) 0.022(5) -0.002(4) -0.001(4) 0.013(4) C21A 0.021(5) 0.033(5) 0.024(5) -0.004(4) 0.001(4) 0.013(4) C23A 0.023(4) 0.031(4) 0.021(4) 0.000(4) 0.001(4) 0.010(4) C22A 0.026(4) 0.034(4) 0.025(4) -0.001(4) 0.000(4) 0.011(4) P1 0.0167(5) 0.0168(5) 0.0170(5) 0.0008(4) 0.0012(4) 0.0054(4) P2 0.0206(5) 0.0176(5) 0.0167(5) 0.0016(4) 0.0010(4) 0.0064(4) P3 0.0149(5) 0.0186(5) 0.0160(5) 0.0009(4) 0.0013(4) 0.0057(4) C5 0.0129(18) 0.024(2) 0.021(2) 0.0080(16) 0.0025(16) 0.0044(16) C6 0.0214(18) 0.022(2) 0.0216(19) -0.0009(17) 0.0016(16) 0.0106(16) C7 0.032(2) 0.041(2) 0.035(2) -0.0102(19) -0.004(2) 0.024(2) C8 0.039(2) 0.041(2) 0.043(3) -0.003(2) -0.001(2) 0.028(2) C9 0.035(2) 0.033(2) 0.042(2) -0.007(2) 0.008(2) 0.0188(19) C11 0.026(2) 0.025(2) 0.022(2) 0.0015(17) 0.0051(17) 0.0091(17) C10 0.031(2) 0.027(2) 0.026(2) -0.0003(18) 0.0072(18) 0.0125(18) C12 0.0145(17) 0.0208(19) 0.0232(19) 0.0003(16) 0.0012(16) 0.0087(15) C17 0.0194(19) 0.023(2) 0.027(2) 0.0048(17) -0.0011(17) 0.0050(16) C16 0.0203(19) 0.026(2) 0.037(2) 0.0054(18) -0.0028(18) 0.0093(17) C15 0.022(2) 0.032(2) 0.042(2) 0.004(2) -0.0064(19) 0.0141(18) C13 0.026(2) 0.028(2) 0.025(2) 0.0041(19) 0.0027(18) 0.0099(18) C14 0.029(2) 0.031(2) 0.031(2) 0.0070(18) 0.0010(18) 0.0162(17) C1 0.024(2) 0.021(2) 0.021(2) 0.0041(17) 0.0092(17) 0.0041(17) C2 0.032(2) 0.020(2) 0.030(2) 0.0075(18) 0.0033(19) 0.0069(18) C3 0.022(2) 0.020(2) 0.0184(19) 0.0051(16) 0.0040(16) 0.0018(16) C4 0.0181(19) 0.020(2) 0.0148(19) 0.0051(15) 0.0018(16) 0.0039(16) C24 0.0213(19) 0.027(2) 0.0167(18) -0.0017(16) -0.0018(16) 0.0093(16) C29 0.023(2) 0.027(2) 0.018(2) 0.0004(17) 0.0034(17) 0.0115(17) C28 0.029(2) 0.035(2) 0.022(2) 0.0018(18) -0.0003(18) 0.0150(18) C27 0.024(2) 0.036(2) 0.030(2) -0.0021(19) -0.0046(18) 0.0174(18) C25 0.0218(19) 0.034(2) 0.0215(19) 0.0004(17) 0.0049(16) 0.0106(16) C26 0.020(2) 0.038(2) 0.029(2) -0.0028(19) -0.0026(17) 0.0134(18) C18 0.0183(18) 0.0228(19) 0.0197(18) 0.0040(16) 0.0027(15) 0.0099(16) C19 0.025(2) 0.034(2) 0.023(2) 0.0030(18) 0.0040(17) 0.0158(17) C20 0.028(2) 0.042(2) 0.029(2) 0.0026(19) 0.0025(19) 0.0210(19) C21 0.037(2) 0.033(2) 0.040(3) 0.009(2) 0.011(2) 0.020(2) C23 0.025(2) 0.029(2) 0.031(2) -0.0028(18) 0.0023(18) 0.0093(17) C22 0.029(2) 0.024(2) 0.034(2) 0.0013(18) 0.0067(18) 0.0126(17) Al2 0.0213(9) 0.0237(8) 0.0164(8) 0.0027(6) 0.0009(7) 0.0057(7) Cl3 0.0397(6) 0.0256(6) 0.0381(6) -0.0089(5) 0.0046(5) 0.0091(5) Cl4 0.0226(6) 0.0320(7) 0.0379(6) 0.0055(5) -0.0030(5) 0.0115(5) Cl5 0.0395(6) 0.0282(8) 0.0285(6) 0.0087(7) 0.0114(5) 0.0059(7) O1 0.0174(14) 0.0219(14) 0.0176(14) 0.0022(12) -0.0005(12) 0.0046(12) Al1 0.0192(8) 0.0198(9) 0.0194(10) 0.0037(7) 0.0017(7) 0.0057(6) Cl1 0.0264(9) 0.0216(6) 0.0373(8) 0.0056(5) -0.0031(6) 0.0039(5) Cl2 0.0370(7) 0.0389(9) 0.0335(8) 0.0089(6) 0.0142(6) 0.0230(7) Al4 0.0202(9) 0.0265(9) 0.0160(7) 0.0043(6) 0.0023(7) 0.0027(7) Cl8 0.0260(5) 0.0290(7) 0.0338(6) 0.0138(6) 0.0054(5) 0.0098(6) Cl9 0.0601(8) 0.0279(6) 0.0434(7) -0.0019(5) 0.0243(6) 0.0122(6) Cl10 0.0240(6) 0.0597(10) 0.0301(7) 0.0146(6) -0.0053(5) -0.0087(6) O2 0.0171(15) 0.0203(15) 0.0180(14) 0.0030(12) 0.0015(12) 0.0039(12) Al3 0.0174(8) 0.0195(10) 0.0181(10) 0.0027(8) 0.0004(7) 0.0045(7) Cl6 0.0274(8) 0.0187(7) 0.0340(9) 0.0007(6) -0.0038(6) 0.0043(5) Cl7 0.0238(7) 0.0303(9) 0.0307(9) 0.0017(6) 0.0054(6) 0.0107(7) Al2A 0.026(5) 0.034(4) 0.026(4) -0.002(4) 0.007(4) -0.005(4) Cl3A 0.0397(6) 0.0256(6) 0.0381(6) -0.0089(5) 0.0046(5) 0.0091(5) Cl4A 0.0226(6) 0.0320(7) 0.0379(6) 0.0055(5) -0.0030(5) 0.0115(5) Cl5A 0.0395(6) 0.0282(8) 0.0285(6) 0.0087(7) 0.0114(5) 0.0059(7) O1A 0.021(4) 0.025(4) 0.021(4) 0.003(4) 0.001(4) 0.004(4) Al1A 0.020(4) 0.030(5) 0.025(5) 0.001(4) 0.002(4) 0.009(4) Cl1A 0.0264(9) 0.0216(6) 0.0373(8) 0.0056(5) -0.0031(6) 0.0039(5) Cl2A 0.0370(7) 0.0389(9) 0.0335(8) 0.0089(6) 0.0142(6) 0.0230(7) Al4A 0.027(5) 0.028(4) 0.020(4) 0.003(4) 0.005(4) -0.001(4) Cl8A 0.0260(5) 0.0290(7) 0.0338(6) 0.0138(6) 0.0054(5) 0.0098(6) Cl9A 0.0601(8) 0.0279(6) 0.0434(7) -0.0019(5) 0.0243(6) 0.0122(6) Cl 0.0240(6) 0.0597(10) 0.0301(7) 0.0146(6) -0.0053(5) -0.0087(6) O2A 0.020(4) 0.022(4) 0.017(4) 0.002(4) 0.003(4) 0.003(4) Al3A 0.024(5) 0.017(5) 0.021(5) 0.003(4) 0.003(4) -0.002(4) Cl6A 0.0274(8) 0.0187(7) 0.0340(9) 0.0007(6) -0.0038(6) 0.0043(5) Cl7A 0.0238(7) 0.0303(9) 0.0307(9) 0.0017(6) 0.0054(6) 0.0107(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 P1A P2A 2.217(7) . ? P1A C3A 1.839(9) . ? P1A C24A 1.812(9) . ? P1A C18A 1.803(9) . ? P2A P3A 2.186(7) . ? P2A C1A 1.847(10) . ? P3A C5A 1.784(9) . ? P3A C6A 1.843(9) . ? P3A C12A 1.832(9) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? C5A C4A 1.523(11) . ? C6A H6A 1.0000 . ? C6A C7A 1.537(11) . ? C6A C11A 1.528(11) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C7A C8A 1.525(11) . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C8A C9A 1.550(11) . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C9A C10A 1.496(11) . ? C11A H11C 0.9900 . ? C11A H11D 0.9900 . ? C11A C10A 1.536(11) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C12A H12A 1.0000 . ? C12A C17A 1.534(10) . ? C12A C13A 1.544(11) . ? C17A H17C 0.9900 . ? C17A H17D 0.9900 . ? C17A C16A 1.517(11) . ? C16A H16C 0.9900 . ? C16A H16D 0.9900 . ? C16A C15A 1.496(11) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C15A C14A 1.522(11) . ? C13A H13C 0.9900 . ? C13A H13D 0.9900 . ? C13A C14A 1.527(11) . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C1A C2A 1.536(11) . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3A C4A 1.538(11) . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? C24A H24A 1.0000 . ? C24A C29A 1.549(10) . ? C24A C25A 1.545(11) . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C29A C28A 1.528(11) . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? C28A C27A 1.517(11) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C27A C26A 1.522(11) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C25A C26A 1.519(11) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C18A H18A 1.0000 . ? C18A C19A 1.519(10) . ? C18A C23A 1.535(11) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C19A C20A 1.527(11) . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C20A C21A 1.513(11) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C21A C22A 1.526(11) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C23A C22A 1.525(11) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? P1 P2 2.2033(14) . ? P1 C3 1.827(4) . ? P1 C24 1.825(4) . ? P1 C18 1.817(4) . ? P2 P3 2.2036(14) . ? P2 C1 1.847(4) . ? P3 C5 1.804(4) . ? P3 C6 1.824(4) . ? P3 C12 1.824(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C4 1.534(5) . ? C6 H6 1.0000 . ? C6 C7 1.540(6) . ? C6 C11 1.524(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.529(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C9 1.554(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.498(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C10 1.538(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C12 H12 1.0000 . ? C12 C17 1.538(5) . ? C12 C13 1.548(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C16 1.521(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C15 1.497(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C14 1.525(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.531(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.538(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.534(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C24 H24 1.0000 . ? C24 C29 1.549(5) . ? C24 C25 1.539(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C28 1.523(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C27 1.520(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C26 1.522(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.520(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C18 H18 1.0000 . ? C18 C19 1.532(5) . ? C18 C23 1.542(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.532(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.519(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.531(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C22 1.525(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? Al2 Cl3 2.132(2) . ? Al2 Cl4 2.1318(19) . ? Al2 Cl5 2.122(2) . ? Al2 O1 1.770(3) . ? O1 Al1 1.802(3) . ? O1 Al1 1.802(5) 2_765 ? Al1 O1 1.802(5) 2_765 ? Al1 Al1 2.655(5) 2_765 ? Al1 Cl1 2.112(2) . ? Al1 Cl2 2.096(2) . ? Al4 Cl8 2.135(2) . ? Al4 Cl9 2.123(2) . ? Al4 Cl10 2.130(2) . ? Al4 O2 1.767(3) . ? O2 Al3 1.802(5) 2_556 ? O2 Al3 1.801(3) . ? Al3 O2 1.802(5) 2_556 ? Al3 Al3 2.623(6) 2_556 ? Al3 Cl6 2.106(2) . ? Al3 Cl7 2.111(2) . ? Al2A Cl3A 2.136(14) . ? Al2A Cl4A 2.138(14) . ? Al2A Cl5A 2.132(15) . ? Al2A O1A 1.773(16) . ? O1A Al1A 1.82(4) 2_765 ? O1A Al1A 1.803(16) . ? Al1A O1A 1.82(4) 2_765 ? Al1A Al1A 2.56(4) 2_765 ? Al1A Cl1A 2.092(16) . ? Al1A Cl2A 2.088(16) . ? Al4A Cl8A 2.133(14) . ? Al4A Cl9A 2.124(15) . ? Al4A Cl 2.107(14) . ? Al4A O2A 1.774(15) . ? O2A Al3A 1.801(16) . ? O2A Al3A 1.75(4) 2_556 ? Al3A O2A 1.75(4) 2_556 ? Al3A Al3A 2.62(5) 2_556 ? Al3A Cl6A 2.094(17) . ? Al3A Cl7A 2.101(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 C3A P1A P2A 107.4(6) . . ? C24A P1A P2A 102.1(6) . . ? C24A P1A C3A 109.8(8) . . ? C18A P1A P2A 115.3(6) . . ? C18A P1A C3A 109.1(7) . . ? C18A P1A C24A 112.8(8) . . ? P3A P2A P1A 103.2(3) . . ? C1A P2A P1A 103.7(8) . . ? C1A P2A P3A 105.8(7) . . ? C5A P3A P2A 110.4(6) . . ? C5A P3A C6A 110.1(8) . . ? C5A P3A C12A 110.0(8) . . ? C6A P3A P2A 100.9(6) . . ? C12A P3A P2A 116.6(6) . . ? C12A P3A C6A 108.4(7) . . ? P3A C5A H5AA 107.3 . . ? P3A C5A H5AB 107.3 . . ? H5AA C5A H5AB 106.9 . . ? C4A C5A P3A 120.2(12) . . ? C4A C5A H5AA 107.3 . . ? C4A C5A H5AB 107.3 . . ? P3A C6A H6A 108.1 . . ? C7A C6A P3A 112.6(10) . . ? C7A C6A H6A 108.1 . . ? C11A C6A P3A 109.8(9) . . ? C11A C6A H6A 108.1 . . ? C11A C6A C7A 110.0(12) . . ? C6A C7A H7AA 109.4 . . ? C6A C7A H7AB 109.4 . . ? H7AA C7A H7AB 108.0 . . ? C8A C7A C6A 111.2(12) . . ? C8A C7A H7AA 109.4 . . ? C8A C7A H7AB 109.4 . . ? C7A C8A H8AA 109.2 . . ? C7A C8A H8AB 109.2 . . ? C7A C8A C9A 112.0(13) . . ? H8AA C8A H8AB 107.9 . . ? C9A C8A H8AA 109.2 . . ? C9A C8A H8AB 109.2 . . ? C8A C9A H9AA 109.4 . . ? C8A C9A H9AB 109.4 . . ? H9AA C9A H9AB 108.0 . . ? C10A C9A C8A 111.0(12) . . ? C10A C9A H9AA 109.4 . . ? C10A C9A H9AB 109.4 . . ? C6A C11A H11C 109.2 . . ? C6A C11A H11D 109.2 . . ? C6A C11A C10A 112.0(13) . . ? H11C C11A H11D 107.9 . . ? C10A C11A H11C 109.2 . . ? C10A C11A H11D 109.2 . . ? C9A C10A C11A 111.5(13) . . ? C9A C10A H10C 109.3 . . ? C9A C10A H10D 109.3 . . ? C11A C10A H10C 109.3 . . ? C11A C10A H10D 109.3 . . ? H10C C10A H10D 108.0 . . ? P3A C12A H12A 106.6 . . ? C17A C12A P3A 114.4(10) . . ? C17A C12A H12A 106.6 . . ? C17A C12A C13A 110.9(12) . . ? C13A C12A P3A 111.2(10) . . ? C13A C12A H12A 106.6 . . ? C12A C17A H17C 109.9 . . ? C12A C17A H17D 109.9 . . ? H17C C17A H17D 108.3 . . ? C16A C17A C12A 108.9(12) . . ? C16A C17A H17C 109.9 . . ? C16A C17A H17D 109.9 . . ? C17A C16A H16C 109.1 . . ? C17A C16A H16D 109.1 . . ? H16C C16A H16D 107.8 . . ? C15A C16A C17A 112.6(14) . . ? C15A C16A H16C 109.1 . . ? C15A C16A H16D 109.1 . . ? C16A C15A H15C 109.3 . . ? C16A C15A H15D 109.3 . . ? C16A C15A C14A 111.4(13) . . ? H15C C15A H15D 108.0 . . ? C14A C15A H15C 109.3 . . ? C14A C15A H15D 109.3 . . ? C12A C13A H13C 109.2 . . ? C12A C13A H13D 109.2 . . ? H13C C13A H13D 107.9 . . ? C14A C13A C12A 112.2(12) . . ? C14A C13A H13C 109.2 . . ? C14A C13A H13D 109.2 . . ? C15A C14A C13A 111.9(13) . . ? C15A C14A H14C 109.2 . . ? C15A C14A H14D 109.2 . . ? C13A C14A H14C 109.2 . . ? C13A C14A H14D 109.2 . . ? H14C C14A H14D 107.9 . . ? P2A C1A H1AA 109.8 . . ? P2A C1A H1AB 109.8 . . ? H1AA C1A H1AB 108.3 . . ? C2A C1A P2A 109.2(11) . . ? C2A C1A H1AA 109.8 . . ? C2A C1A H1AB 109.8 . . ? P1A C3A H3AA 108.8 . . ? P1A C3A H3AB 108.8 . . ? H3AA C3A H3AB 107.7 . . ? C4A C3A P1A 114.0(11) . . ? C4A C3A H3AA 108.8 . . ? C4A C3A H3AB 108.8 . . ? C5A C4A C3A 114.0(13) . . ? C5A C4A H4AA 108.8 . . ? C5A C4A H4AB 108.8 . . ? C3A C4A H4AA 108.8 . . ? C3A C4A H4AB 108.8 . . ? H4AA C4A H4AB 107.7 . . ? P1A C24A H24A 107.3 . . ? C29A C24A P1A 111.9(9) . . ? C29A C24A H24A 107.3 . . ? C25A C24A P1A 111.7(10) . . ? C25A C24A H24A 107.3 . . ? C25A C24A C29A 111.0(12) . . ? C24A C29A H29C 109.7 . . ? C24A C29A H29D 109.7 . . ? H29C C29A H29D 108.2 . . ? C28A C29A C24A 110.0(11) . . ? C28A C29A H29C 109.7 . . ? C28A C29A H29D 109.7 . . ? C29A C28A H28C 109.6 . . ? C29A C28A H28D 109.6 . . ? H28C C28A H28D 108.1 . . ? C27A C28A C29A 110.3(12) . . ? C27A C28A H28C 109.6 . . ? C27A C28A H28D 109.6 . . ? C28A C27A H27C 109.2 . . ? C28A C27A H27D 109.2 . . ? C28A C27A C26A 112.1(13) . . ? H27C C27A H27D 107.9 . . ? C26A C27A H27C 109.2 . . ? C26A C27A H27D 109.2 . . ? C24A C25A H25C 109.8 . . ? C24A C25A H25D 109.8 . . ? H25C C25A H25D 108.2 . . ? C26A C25A C24A 109.5(13) . . ? C26A C25A H25C 109.8 . . ? C26A C25A H25D 109.8 . . ? C27A C26A H26C 109.4 . . ? C27A C26A H26D 109.4 . . ? C25A C26A C27A 111.0(14) . . ? C25A C26A H26C 109.4 . . ? C25A C26A H26D 109.4 . . ? H26C C26A H26D 108.0 . . ? P1A C18A H18A 104.5 . . ? C19A C18A P1A 116.3(10) . . ? C19A C18A H18A 104.5 . . ? C19A C18A C23A 113.0(12) . . ? C23A C18A P1A 112.7(10) . . ? C23A C18A H18A 104.5 . . ? C18A C19A H19C 109.5 . . ? C18A C19A H19D 109.5 . . ? C18A C19A C20A 110.5(11) . . ? H19C C19A H19D 108.1 . . ? C20A C19A H19C 109.5 . . ? C20A C19A H19D 109.5 . . ? C19A C20A H20C 109.2 . . ? C19A C20A H20D 109.2 . . ? H20C C20A H20D 107.9 . . ? C21A C20A C19A 112.0(13) . . ? C21A C20A H20C 109.2 . . ? C21A C20A H20D 109.2 . . ? C20A C21A H21C 109.0 . . ? C20A C21A H21D 109.0 . . ? C20A C21A C22A 112.8(13) . . ? H21C C21A H21D 107.8 . . ? C22A C21A H21C 109.0 . . ? C22A C21A H21D 109.0 . . ? C18A C23A H23C 109.4 . . ? C18A C23A H23D 109.4 . . ? H23C C23A H23D 108.0 . . ? C22A C23A C18A 111.1(12) . . ? C22A C23A H23C 109.4 . . ? C22A C23A H23D 109.4 . . ? C21A C22A H22C 109.2 . . ? C21A C22A H22D 109.2 . . ? C23A C22A C21A 112.1(13) . . ? C23A C22A H22C 109.2 . . ? C23A C22A H22D 109.2 . . ? H22C C22A H22D 107.9 . . ? C3 P1 P2 111.86(13) . . ? C24 P1 P2 101.85(14) . . ? C24 P1 C3 108.74(18) . . ? C18 P1 P2 114.60(13) . . ? C18 P1 C3 110.84(18) . . ? C18 P1 C24 108.38(17) . . ? P1 P2 P3 102.93(5) . . ? C1 P2 P1 104.37(14) . . ? C1 P2 P3 105.97(14) . . ? C5 P3 P2 105.48(13) . . ? C5 P3 C6 109.95(18) . . ? C5 P3 C12 108.80(17) . . ? C6 P3 P2 103.65(13) . . ? C12 P3 P2 115.39(13) . . ? C12 P3 C6 113.19(18) . . ? P3 C5 H5A 108.6 . . ? P3 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C4 C5 P3 114.5(3) . . ? C4 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? P3 C6 H6 107.0 . . ? C7 C6 P3 112.5(3) . . ? C7 C6 H6 107.0 . . ? C11 C6 P3 112.7(3) . . ? C11 C6 H6 107.0 . . ? C11 C6 C7 110.3(3) . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C8 C7 C6 110.1(4) . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C7 C8 C9 110.0(4) . . ? H8A C8 H8B 108.2 . . ? C9 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C8 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C10 C9 C8 110.2(4) . . ? C10 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C6 C11 H11A 109.4 . . ? C6 C11 H11B 109.4 . . ? C6 C11 C10 111.0(3) . . ? H11A C11 H11B 108.0 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C9 C10 C11 111.8(3) . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? P3 C12 H12 106.3 . . ? C17 C12 P3 113.8(3) . . ? C17 C12 H12 106.3 . . ? C17 C12 C13 109.6(3) . . ? C13 C12 P3 113.9(3) . . ? C13 C12 H12 106.3 . . ? C12 C17 H17A 109.9 . . ? C12 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C16 C17 C12 109.1(3) . . ? C16 C17 H17A 109.9 . . ? C16 C17 H17B 109.9 . . ? C17 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C15 C16 C17 112.1(4) . . ? C15 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C16 C15 H15A 109.2 . . ? C16 C15 H15B 109.2 . . ? C16 C15 C14 111.9(4) . . ? H15A C15 H15B 107.9 . . ? C14 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C12 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C14 C13 C12 110.2(3) . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C15 C14 C13 111.3(4) . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? P2 C1 H1A 109.9 . . ? P2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C2 C1 P2 109.1(3) . . ? C2 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 H3A 107.9 . . ? P1 C3 H3B 107.9 . . ? H3A C3 H3B 107.2 . . ? C4 C3 P1 117.6(3) . . ? C4 C3 H3A 107.9 . . ? C4 C3 H3B 107.9 . . ? C5 C4 C3 113.7(3) . . ? C5 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? P1 C24 H24 107.4 . . ? C29 C24 P1 109.6(3) . . ? C29 C24 H24 107.4 . . ? C25 C24 P1 113.3(3) . . ? C25 C24 H24 107.4 . . ? C25 C24 C29 111.4(3) . . ? C24 C29 H29A 109.6 . . ? C24 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C28 C29 C24 110.2(3) . . ? C28 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C29 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C27 C28 C29 111.1(3) . . ? C27 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C28 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C28 C27 C26 111.3(3) . . ? H27A C27 H27B 108.0 . . ? C26 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C24 C25 H25A 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? C26 C25 C24 109.6(3) . . ? C26 C25 H25A 109.8 . . ? C26 C25 H25B 109.8 . . ? C27 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 C27 111.5(4) . . ? C25 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? P1 C18 H18 107.4 . . ? C19 C18 P1 112.8(3) . . ? C19 C18 H18 107.4 . . ? C19 C18 C23 111.4(3) . . ? C23 C18 P1 110.2(3) . . ? C23 C18 H18 107.4 . . ? C18 C19 H19A 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C20 C19 C18 109.5(3) . . ? C20 C19 H19A 109.8 . . ? C20 C19 H19B 109.8 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C21 C20 C19 110.9(4) . . ? C21 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C20 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C20 C21 C22 111.1(4) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C22 C23 C18 110.8(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 C21 110.9(4) . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? Cl4 Al2 Cl3 111.11(9) . . ? Cl5 Al2 Cl3 110.33(9) . . ? Cl5 Al2 Cl4 111.34(10) . . ? O1 Al2 Cl3 109.56(17) . . ? O1 Al2 Cl4 106.29(15) . . ? O1 Al2 Cl5 108.07(15) . . ? Al2 O1 Al1 133.8(2) . . ? Al2 O1 Al1 130.6(2) . 2_765 ? Al1 O1 Al1 94.89(19) 2_765 . ? O1 Al1 O1 85.11(19) 2_765 . ? O1 Al1 Al1 42.56(13) 2_765 2_765 ? O1 Al1 Al1 42.55(13) . 2_765 ? O1 Al1 Cl1 116.53(19) . . ? O1 Al1 Cl1 112.75(19) 2_765 . ? O1 Al1 Cl2 118.0(2) 2_765 . ? O1 Al1 Cl2 113.45(18) . . ? Cl1 Al1 Al1 124.45(15) . 2_765 ? Cl2 Al1 Al1 126.04(15) . 2_765 ? Cl2 Al1 Cl1 109.51(12) . . ? Cl9 Al4 Cl8 108.80(9) . . ? Cl9 Al4 Cl10 111.53(10) . . ? Cl10 Al4 Cl8 111.44(10) . . ? O2 Al4 Cl8 108.60(17) . . ? O2 Al4 Cl9 109.82(17) . . ? O2 Al4 Cl10 106.60(14) . . ? Al4 O2 Al3 132.1(2) . 2_556 ? Al4 O2 Al3 134.1(2) . . ? Al3 O2 Al3 93.4(2) . 2_556 ? O2 Al3 O2 86.6(2) . 2_556 ? O2 Al3 Al3 43.31(13) . 2_556 ? O2 Al3 Al3 43.26(15) 2_556 2_556 ? O2 Al3 Cl6 113.0(2) 2_556 . ? O2 Al3 Cl6 113.4(2) . . ? O2 Al3 Cl7 112.99(19) . . ? O2 Al3 Cl7 116.4(2) 2_556 . ? Cl6 Al3 Al3 122.78(16) . 2_556 ? Cl6 Al3 Cl7 112.19(13) . . ? Cl7 Al3 Al3 125.00(16) . 2_556 ? Cl3A Al2A Cl4A 116.2(8) . . ? Cl5A Al2A Cl3A 109.0(7) . . ? Cl5A Al2A Cl4A 111.1(9) . . ? O1A Al2A Cl3A 108.3(13) . . ? O1A Al2A Cl4A 103.7(10) . . ? O1A Al2A Cl5A 108.2(13) . . ? Al2A O1A Al1A 135.5(18) . 2_765 ? Al2A O1A Al1A 133.9(18) . . ? Al1A O1A Al1A 89.7(14) . 2_765 ? O1A Al1A O1A 90.3(14) . 2_765 ? O1A Al1A Al1A 45.5(10) . 2_765 ? O1A Al1A Al1A 44.8(10) 2_765 2_765 ? O1A Al1A Cl1A 115.2(16) 2_765 . ? O1A Al1A Cl1A 116.1(15) . . ? O1A Al1A Cl2A 112.3(14) . . ? O1A Al1A Cl2A 113.4(17) 2_765 . ? Cl1A Al1A Al1A 127.9(12) . 2_765 ? Cl2A Al1A Al1A 123.4(12) . 2_765 ? Cl2A Al1A Cl1A 108.7(11) . . ? Cl9A Al4A Cl8A 108.2(8) . . ? Cl Al4A Cl8A 111.0(8) . . ? Cl Al4A Cl9A 114.2(8) . . ? O2A Al4A Cl8A 107.9(12) . . ? O2A Al4A Cl9A 108.4(13) . . ? O2A Al4A Cl 106.9(11) . . ? Al4A O2A Al3A 134.9(18) . . ? Al3A O2A Al4A 129.5(19) 2_556 . ? Al3A O2A Al3A 95.4(15) 2_556 . ? O2A Al3A O2A 84.6(15) 2_556 . ? O2A Al3A Al3A 43.1(11) 2_556 2_556 ? O2A Al3A Al3A 41.5(10) . 2_556 ? O2A Al3A Cl6A 113.6(15) . . ? O2A Al3A Cl6A 111.9(17) 2_556 . ? O2A Al3A Cl7A 120.8(19) 2_556 . ? O2A Al3A Cl7A 113.3(14) . . ? Cl6A Al3A Al3A 121.5(13) . 2_556 ? Cl6A Al3A Cl7A 110.5(12) . . ? Cl7A Al3A Al3A 127.8(13) . 2_556 ? #====================================================================== data_6 _database_code_depnum_ccdc_archive 'CCDC 840423' #TrackingRef '- CrystallographicData.cif' #====================================================================== _audit_creation_method SHELXL-97 _chemical_formula_moiety '2(C39 H59 P3), Cl6 Sn, 7.982(C H Cl3), 2(Cl3 Sn)' _chemical_formula_sum 'C85.982 H125.982 Cl35.946 P6 Sn3' _chemical_formula_weight 2975.87 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? 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' 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' Sn Sn -0.6537 1.4246 '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_angle_alpha 72.928(2) _cell_angle_beta 87.477(2) _cell_angle_gamma 72.386(2) _cell_formula_units_Z 1 _cell_length_a 10.5087(6) _cell_length_b 15.1261(8) _cell_length_c 20.8450(10) _cell_measurement_reflns_used 4030 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 24.914 _cell_measurement_theta_min 2.233 _cell_volume 3015.3(3) _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.771354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. ; _exptl_crystal_F_000 1490 _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 5 sets of \w scans each set at different \f and/or 2\q angles and each scan (30.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_ambient_temperature 120(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 8.0 _diffrn_detector_type 'Bruker SMART CCD 1K area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.081221 _diffrn_orient_matrix_UB_12 0.022212 _diffrn_orient_matrix_UB_13 -0.005989 _diffrn_orient_matrix_UB_21 0.010465 _diffrn_orient_matrix_UB_22 -0.011287 _diffrn_orient_matrix_UB_23 -0.045044 _diffrn_orient_matrix_UB_31 -0.056988 _diffrn_orient_matrix_UB_32 0.068133 _diffrn_orient_matrix_UB_33 -0.021247 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_refln_scan_width 0.3 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.1089 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 35805 _diffrn_reflns_theta_full 26.42 _diffrn_reflns_theta_max 26.42 _diffrn_reflns_theta_min 1.02 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7439 _reflns_number_total 12391 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; Olex2, Durham University (compiled Feb 15 2009 13:03:59) ; _computing_publication_material ; Olex2, Durham University (compiled Feb 15 2009 13:03:59) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.415 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.135 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0520 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 607 _refine_ls_number_reflns 12391 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.1090 _refine_ls_wR_factor_ref 0.1301 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Sn1 Sn 0.5000 0.5000 -1.0000 0.01792(14) Uani 1 2 d S . . Sn2 Sn 0.55518(4) 0.61341(3) -0.49722(2) 0.02513(12) Uani 1 1 d . . . P2 P 0.91881(14) 0.43824(11) -0.69574(7) 0.0163(3) Uani 1 1 d . . . P1 P 0.74533(14) 0.66132(11) -0.78776(7) 0.0161(3) Uani 1 1 d . . . P3 P 0.70969(14) 0.53766(11) -0.70959(7) 0.0167(3) Uani 1 1 d . . . Cl6 Cl 0.78466(15) 0.56879(12) -0.53776(8) 0.0299(4) Uani 1 1 d . . . Cl11 Cl 0.62326(15) 0.60203(11) -1.06798(7) 0.0269(3) Uani 1 1 d . . . Cl16 Cl 0.62721(18) -0.00801(12) -0.56035(9) 0.0362(4) Uani 1 1 d . . . Cl17 Cl 0.86211(18) 0.05591(13) -0.59115(10) 0.0431(5) Uani 1 1 d . . . Cl7 Cl 0.44132(15) 0.66229(12) -0.60858(8) 0.0310(4) Uani 1 1 d . . . Cl12 Cl 0.7135(2) 1.05666(14) -0.91733(10) 0.0482(6) Uani 0.991(4) 1 d P A 1 Cl8 Cl 0.54601(16) 0.78144(12) -0.50703(9) 0.0359(4) Uani 1 1 d . . . Cl9 Cl 0.69297(14) 0.41531(11) -0.92176(7) 0.0269(4) Uani 1 1 d . . . Cl10 Cl 0.57808(15) 0.38216(11) -1.06387(8) 0.0281(4) Uani 1 1 d . . . Cl20 Cl 0.40712(17) 0.99373(14) -0.70606(10) 0.0451(5) Uani 1 1 d . . . Cl3N Cl 0.8333(2) 0.86396(16) -1.01915(12) 0.0452(6) Uani 0.848(2) 1 d PD B 1 Cl18 Cl 0.6100(2) 0.17199(14) -0.66228(10) 0.0557(6) Uani 1 1 d . . . Cl19 Cl 0.18867(19) 0.91268(14) -0.69293(9) 0.0460(5) Uani 1 1 d . . . Cl2N Cl 1.1083(2) 0.76642(15) -1.03761(11) 0.0397(5) Uani 0.848(2) 1 d PD B 1 Cl22 Cl 0.4309(2) 1.13865(17) -0.90882(12) 0.0590(7) Uani 0.991(4) 1 d P A 1 Cl1N Cl 1.0441(3) 0.87206(19) -0.94023(11) 0.0526(6) Uani 0.848(2) 1 d PD B 1 Cl21 Cl 0.6141(3) 1.15819(16) -0.81919(11) 0.0779(9) Uani 0.991(4) 1 d P A 1 C4 C 0.8598(6) 0.6191(4) -0.8474(3) 0.0181(12) Uani 1 1 d . . . C5 C 0.9987(6) 0.5784(4) -0.8313(3) 0.0186(13) Uani 1 1 d . . . C14 C 0.8956(6) 0.6010(4) -0.9584(3) 0.0239(14) Uani 1 1 d . . . H14 H 0.8608 0.6062 -1.0001 0.036 Uiso 1 1 calc R . . C15 C 0.8113(6) 0.6280(4) -0.9101(3) 0.0204(13) Uani 1 1 d . . . H15 H 0.7197 0.6529 -0.9201 0.031 Uiso 1 1 calc R . . C12 C 1.0841(6) 0.5541(4) -0.8809(3) 0.0233(14) Uani 1 1 d . . . H12 H 1.1760 0.5298 -0.8715 0.035 Uiso 1 1 calc R . . C9 C 1.1731(6) 0.5680(4) -0.6453(3) 0.0244(14) Uani 1 1 d . . . H9 H 1.2069 0.5708 -0.6058 0.037 Uiso 1 1 calc R . . C8 C 1.0848(6) 0.5131(4) -0.6432(3) 0.0221(13) Uani 1 1 d . . . H8 H 1.0639 0.4769 -0.6020 0.033 Uiso 1 1 calc R . . C34 C 0.9297(5) 0.3652(4) -0.6079(3) 0.0154(12) Uani 1 1 d . . . H34 H 0.9229 0.4108 -0.5819 0.023 Uiso 1 1 calc R . . C6 C 1.0610(5) 0.5668(4) -0.7651(3) 0.0167(12) Uani 1 1 d . . . C39 C 0.8135(6) 0.3231(4) -0.5861(3) 0.0199(13) Uani 1 1 d . . . H39B H 0.8166 0.2742 -0.6081 0.030 Uiso 1 1 calc R . . H39A H 0.7291 0.3741 -0.5993 0.030 Uiso 1 1 calc R . . C22 C 0.8097(6) 0.7310(4) -0.7458(3) 0.0187(13) Uani 1 1 d . . . H22 H 0.8838 0.6839 -0.7152 0.028 Uiso 1 1 calc R . . C23 C 0.8691(6) 0.8047(4) -0.7937(3) 0.0230(14) Uani 1 1 d . . . H23B H 0.9360 0.7723 -0.8196 0.035 Uiso 1 1 calc R . . H23A H 0.7993 0.8540 -0.8247 0.035 Uiso 1 1 calc R . . C7 C 1.0290(5) 0.5128(4) -0.7023(3) 0.0163(12) Uani 1 1 d . . . C13 C 1.0322(6) 0.5661(4) -0.9442(3) 0.0240(14) Uani 1 1 d . . . H13 H 1.0897 0.5506 -0.9772 0.036 Uiso 1 1 calc R . . C27 C 0.7078(6) 0.7781(5) -0.7018(3) 0.0244(14) Uani 1 1 d . . . H27A H 0.6726 0.7298 -0.6714 0.037 Uiso 1 1 calc R . . H27B H 0.6339 0.8283 -0.7296 0.037 Uiso 1 1 calc R . . C33 C 0.9086(6) 0.2786(4) -0.7370(3) 0.0230(14) Uani 1 1 d . . . H33A H 0.9444 0.2347 -0.6931 0.035 Uiso 1 1 calc R . . H33B H 0.8122 0.3026 -0.7351 0.035 Uiso 1 1 calc R . . C11 C 1.1540(6) 0.6154(4) -0.7653(3) 0.0240(14) Uani 1 1 d . . . H11 H 1.1807 0.6479 -0.8063 0.036 Uiso 1 1 calc R . . C36 C 1.0729(6) 0.2460(4) -0.5092(3) 0.0259(14) Uani 1 1 d . . . H36B H 1.1576 0.1956 -0.4951 0.039 Uiso 1 1 calc R . . H36A H 1.0693 0.2965 -0.4888 0.039 Uiso 1 1 calc R . . C16 C 0.5812(5) 0.7322(4) -0.8315(3) 0.0163(12) Uani 1 1 d . . . H16 H 0.5640 0.6957 -0.8602 0.025 Uiso 1 1 calc R . . C28 C 0.9670(5) 0.3648(4) -0.7544(3) 0.0203(13) Uani 1 1 d . . . H28 H 0.9295 0.4070 -0.7990 0.031 Uiso 1 1 calc R . . C21 C 0.4652(5) 0.7430(4) -0.7849(3) 0.0200(13) Uani 1 1 d . . . H21A H 0.4634 0.6794 -0.7573 0.030 Uiso 1 1 calc R . . H21B H 0.4766 0.7795 -0.7555 0.030 Uiso 1 1 calc R . . C10 C 1.2083(6) 0.6171(4) -0.7065(3) 0.0229(14) Uani 1 1 d . . . H10 H 1.2688 0.6516 -0.7084 0.034 Uiso 1 1 calc R . . C32 C 0.9429(6) 0.2244(5) -0.7890(3) 0.0316(16) Uani 1 1 d . . . H32A H 0.9099 0.1686 -0.7758 0.047 Uiso 1 1 calc R . . H32B H 0.8988 0.2665 -0.8319 0.047 Uiso 1 1 calc R . . C29 C 1.1190(6) 0.3282(4) -0.7594(3) 0.0257(14) Uani 1 1 d . . . H29A H 1.1601 0.2847 -0.7163 0.039 Uiso 1 1 calc R . . H29B H 1.1550 0.3826 -0.7714 0.039 Uiso 1 1 calc R . . C18 C 0.4516(6) 0.8802(5) -0.9194(3) 0.0278(15) Uani 1 1 d . . . H18B H 0.4524 0.9430 -0.9488 0.042 Uiso 1 1 calc R . . H18A H 0.4412 0.8413 -0.9473 0.042 Uiso 1 1 calc R . . C26 C 0.7766(7) 0.8221(5) -0.6614(3) 0.0311(16) Uani 1 1 d . . . H26A H 0.7121 0.8534 -0.6340 0.047 Uiso 1 1 calc R . . H26B H 0.8468 0.7709 -0.6317 0.047 Uiso 1 1 calc R . . C35 C 1.0656(6) 0.2883(4) -0.5855(3) 0.0204(13) Uani 1 1 d . . . H35A H 1.0766 0.2372 -0.6065 0.031 Uiso 1 1 calc R . . H35B H 1.1367 0.3174 -0.5992 0.031 Uiso 1 1 calc R . . C2 C 0.5377(6) 0.4327(5) -0.7200(3) 0.0269(14) Uani 1 1 d . . . H2B H 0.5955 0.3746 -0.6888 0.040 Uiso 1 1 calc R . . H2A H 0.4787 0.4707 -0.6942 0.040 Uiso 1 1 calc R . . C30 C 1.1507(6) 0.2741(5) -0.8135(3) 0.0318(16) Uani 1 1 d . . . H30A H 1.1142 0.3190 -0.8569 0.048 Uiso 1 1 calc R . . H30B H 1.2468 0.2495 -0.8160 0.048 Uiso 1 1 calc R . . C19 C 0.3349(6) 0.8934(5) -0.8743(3) 0.0298(15) Uani 1 1 d . . . H19B H 0.2518 0.9232 -0.9014 0.045 Uiso 1 1 calc R . . H19A H 0.3416 0.9360 -0.8485 0.045 Uiso 1 1 calc R . . C38 C 0.6862(7) 0.0930(5) -0.5850(3) 0.0335(16) Uani 1 1 d . . . H38 H 0.6643 0.1276 -0.5510 0.050 Uiso 1 1 calc R . . C1 C 0.6226(6) 0.4919(4) -0.7627(3) 0.0225(13) Uani 1 1 d . . . H1A H 0.5658 0.5462 -0.7971 0.034 Uiso 1 1 calc R . . H1B H 0.6881 0.4516 -0.7848 0.034 Uiso 1 1 calc R . . C37 C 0.9596(6) 0.2034(5) -0.4844(3) 0.0277(15) Uani 1 1 d . . . H37B H 0.9643 0.1820 -0.4357 0.041 Uiso 1 1 calc R . . H37A H 0.9698 0.1473 -0.5000 0.041 Uiso 1 1 calc R . . C17 C 0.5829(6) 0.8310(4) -0.8786(3) 0.0221(13) Uani 1 1 d . . . H17A H 0.5961 0.8713 -0.8524 0.033 Uiso 1 1 calc R . . H17B H 0.6562 0.8221 -0.9084 0.033 Uiso 1 1 calc R . . C24 C 0.9322(6) 0.8522(5) -0.7549(3) 0.0270(15) Uani 1 1 d . . . H24B H 0.9616 0.9028 -0.7863 0.041 Uiso 1 1 calc R . . H24A H 1.0103 0.8043 -0.7289 0.041 Uiso 1 1 calc R . . C3 C 0.4549(6) 0.4044(5) -0.7645(3) 0.0302(15) Uani 1 1 d . . . H3C H 0.5129 0.3708 -0.7923 0.045 Uiso 1 1 calc R . . H3B H 0.3917 0.4618 -0.7923 0.045 Uiso 1 1 calc R . . H3A H 0.4080 0.3629 -0.7367 0.045 Uiso 1 1 calc R . . C20 C 0.3346(6) 0.7955(4) -0.8267(3) 0.0243(14) Uani 1 1 d . . . H20B H 0.2614 0.8052 -0.7969 0.036 Uiso 1 1 calc R . . H20A H 0.3197 0.7555 -0.8526 0.036 Uiso 1 1 calc R . . C1AA C 0.8238(6) 0.2774(5) -0.5095(3) 0.0273(15) Uani 1 1 d . . . H1AB H 0.8078 0.3283 -0.4880 0.041 Uiso 1 1 calc R . . H1AA H 0.7548 0.2459 -0.4967 0.041 Uiso 1 1 calc R . . C25 C 0.8361(7) 0.8959(5) -0.7079(3) 0.0345(17) Uani 1 1 d . . . H25A H 0.7647 0.9504 -0.7342 0.052 Uiso 1 1 calc R . . H25B H 0.8831 0.9201 -0.6811 0.052 Uiso 1 1 calc R . . C31 C 1.0920(6) 0.1907(5) -0.7971(3) 0.0302(15) Uani 1 1 d . . . H31B H 1.1096 0.1600 -0.8327 0.045 Uiso 1 1 calc R . . H31A H 1.1351 0.1428 -0.7558 0.045 Uiso 1 1 calc R . . C0AA C 0.5869(8) 1.1526(5) -0.9000(3) 0.0399(18) Uani 0.991(4) 1 d P A 1 H0AA H 0.5898 1.2137 -0.9326 0.048 Uiso 0.991(4) 1 calc PR A 1 C1M C 0.9975(7) 0.8660(6) -1.0196(4) 0.034(2) Uani 0.848(2) 1 d PD B 1 H1M H 1.0029 0.9246 -1.0541 0.041 Uiso 0.848(2) 1 calc PR B 1 C45 C 0.3100(7) 0.9349(5) -0.6493(3) 0.0357(17) Uani 1 1 d . . . H45 H 0.3689 0.8722 -0.6224 0.054 Uiso 1 1 calc R . . Cl24 Cl 0.2338(2) 1.00066(15) -0.59476(9) 0.0533(5) Uani 1 1 d . . . Cl3P Cl 1.1432(11) 0.7843(8) -0.9828(6) 0.0397(5) Uani 0.152(2) 1 d PD B 2 Cl2P Cl 1.0072(14) 0.9349(10) -1.1013(6) 0.0526(6) Uani 0.152(2) 1 d PD B 2 Cl1P Cl 0.8649(12) 0.8862(9) -0.9825(7) 0.0452(6) Uani 0.152(2) 1 d PD B 2 C1O C 1.019(2) 0.896(2) -1.0138(11) 0.034(2) Uani 0.152(2) 1 d PD B 2 H1O H 1.0417 0.9448 -0.9980 0.041 Uiso 0.152(2) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0179(3) 0.0180(3) 0.0188(3) -0.0076(2) -0.0031(2) -0.0042(2) Sn2 0.0285(2) 0.0247(2) 0.0217(2) -0.00573(19) 0.00028(18) -0.00836(19) P2 0.0155(7) 0.0178(8) 0.0165(8) -0.0059(6) -0.0013(6) -0.0052(6) P1 0.0173(8) 0.0173(8) 0.0155(7) -0.0069(6) 0.0004(6) -0.0058(6) P3 0.0179(8) 0.0167(8) 0.0164(8) -0.0053(6) -0.0005(6) -0.0061(6) Cl6 0.0261(8) 0.0320(9) 0.0327(9) -0.0155(7) -0.0016(7) -0.0042(7) Cl11 0.0263(8) 0.0307(9) 0.0255(8) -0.0062(7) -0.0007(6) -0.0128(7) Cl16 0.0454(10) 0.0296(9) 0.0382(10) -0.0129(8) 0.0039(8) -0.0153(8) Cl17 0.0422(11) 0.0372(11) 0.0581(12) -0.0229(9) 0.0036(9) -0.0152(8) Cl7 0.0283(8) 0.0437(10) 0.0268(8) -0.0153(7) 0.0003(6) -0.0144(7) Cl12 0.0565(13) 0.0367(11) 0.0451(12) -0.0053(9) -0.0089(9) -0.0103(9) Cl8 0.0323(9) 0.0319(9) 0.0521(11) -0.0249(8) 0.0023(8) -0.0100(7) Cl9 0.0225(8) 0.0306(9) 0.0248(8) -0.0082(7) -0.0064(6) -0.0031(7) Cl10 0.0296(8) 0.0267(9) 0.0299(8) -0.0162(7) -0.0029(7) -0.0029(7) Cl20 0.0300(9) 0.0452(11) 0.0584(12) -0.0156(9) -0.0010(8) -0.0080(8) Cl3N 0.0279(11) 0.0395(13) 0.0614(16) -0.0048(11) 0.0019(10) -0.0104(9) Cl18 0.0758(15) 0.0408(12) 0.0420(11) 0.0046(9) -0.0195(10) -0.0188(11) Cl19 0.0502(11) 0.0507(12) 0.0451(11) -0.0164(9) -0.0065(9) -0.0233(10) Cl2N 0.0373(11) 0.0345(12) 0.0479(13) -0.0148(10) 0.0052(9) -0.0094(9) Cl22 0.0605(14) 0.0626(15) 0.0798(16) -0.0458(13) 0.0240(12) -0.0348(12) Cl1N 0.0708(16) 0.0597(16) 0.0359(12) -0.0182(11) 0.0014(11) -0.0282(13) Cl21 0.143(3) 0.0402(13) 0.0447(13) -0.0130(10) -0.0346(14) -0.0141(14) C4 0.022(3) 0.016(3) 0.020(3) -0.006(2) -0.001(2) -0.010(2) C5 0.026(3) 0.014(3) 0.021(3) -0.008(2) 0.004(2) -0.010(3) C14 0.028(3) 0.028(4) 0.017(3) -0.008(3) -0.004(3) -0.010(3) C15 0.019(3) 0.019(3) 0.023(3) -0.006(3) -0.006(2) -0.004(3) C12 0.025(3) 0.025(3) 0.022(3) -0.007(3) 0.002(3) -0.012(3) C9 0.025(3) 0.023(3) 0.028(3) -0.008(3) -0.008(3) -0.008(3) C8 0.024(3) 0.022(3) 0.021(3) -0.005(3) -0.005(2) -0.008(3) C34 0.017(3) 0.015(3) 0.016(3) -0.004(2) -0.004(2) -0.008(2) C6 0.015(3) 0.022(3) 0.017(3) -0.012(3) 0.006(2) -0.005(2) C39 0.024(3) 0.018(3) 0.017(3) -0.002(2) 0.001(2) -0.007(3) C22 0.022(3) 0.021(3) 0.015(3) -0.006(2) -0.005(2) -0.006(3) C23 0.027(3) 0.023(3) 0.025(3) -0.009(3) 0.001(3) -0.013(3) C7 0.010(3) 0.023(3) 0.016(3) -0.006(2) -0.001(2) -0.005(2) C13 0.027(3) 0.029(4) 0.022(3) -0.014(3) 0.009(3) -0.012(3) C27 0.028(3) 0.029(4) 0.020(3) -0.012(3) -0.002(3) -0.011(3) C33 0.022(3) 0.024(3) 0.026(3) -0.009(3) -0.005(3) -0.008(3) C11 0.022(3) 0.022(3) 0.027(3) -0.005(3) 0.001(3) -0.009(3) C36 0.027(3) 0.022(3) 0.023(3) -0.002(3) -0.006(3) -0.004(3) C16 0.020(3) 0.016(3) 0.013(3) -0.004(2) -0.005(2) -0.006(2) C28 0.019(3) 0.018(3) 0.024(3) -0.005(3) -0.002(2) -0.006(3) C21 0.018(3) 0.022(3) 0.018(3) -0.004(3) 0.004(2) -0.007(3) C10 0.021(3) 0.026(3) 0.023(3) -0.008(3) -0.002(2) -0.010(3) C32 0.034(4) 0.025(4) 0.040(4) -0.018(3) -0.007(3) -0.007(3) C29 0.024(3) 0.021(3) 0.030(4) -0.006(3) 0.001(3) -0.004(3) C18 0.033(4) 0.023(3) 0.021(3) 0.003(3) -0.008(3) -0.007(3) C26 0.034(4) 0.037(4) 0.030(4) -0.026(3) -0.003(3) -0.006(3) C35 0.021(3) 0.016(3) 0.021(3) -0.001(2) -0.003(2) -0.006(3) C2 0.024(3) 0.032(4) 0.031(4) -0.014(3) -0.001(3) -0.014(3) C30 0.026(4) 0.029(4) 0.038(4) -0.014(3) 0.003(3) -0.001(3) C19 0.023(3) 0.025(4) 0.035(4) -0.002(3) -0.007(3) -0.004(3) C38 0.050(4) 0.023(4) 0.025(4) -0.007(3) 0.000(3) -0.008(3) C1 0.022(3) 0.024(3) 0.024(3) -0.007(3) -0.005(2) -0.010(3) C37 0.034(4) 0.025(4) 0.021(3) -0.002(3) -0.008(3) -0.008(3) C17 0.022(3) 0.023(3) 0.023(3) -0.007(3) 0.000(2) -0.009(3) C24 0.031(4) 0.022(3) 0.031(4) -0.005(3) -0.009(3) -0.014(3) C3 0.028(4) 0.033(4) 0.034(4) -0.009(3) -0.010(3) -0.015(3) C20 0.019(3) 0.025(3) 0.029(3) -0.006(3) -0.006(3) -0.008(3) C1AA 0.035(4) 0.030(4) 0.021(3) -0.004(3) 0.002(3) -0.018(3) C25 0.040(4) 0.031(4) 0.040(4) -0.018(3) -0.008(3) -0.013(3) C31 0.035(4) 0.023(4) 0.036(4) -0.021(3) 0.000(3) -0.001(3) C0AA 0.064(5) 0.032(4) 0.028(4) -0.006(3) -0.007(3) -0.022(4) C1M 0.032(4) 0.043(5) 0.030(4) -0.008(4) 0.000(3) -0.016(4) C45 0.035(4) 0.040(4) 0.031(4) -0.014(3) -0.005(3) -0.005(3) Cl24 0.0620(13) 0.0582(13) 0.0383(11) -0.0258(10) -0.0028(9) -0.0044(11) Cl3P 0.0373(11) 0.0345(12) 0.0479(13) -0.0148(10) 0.0052(9) -0.0094(9) Cl2P 0.0708(16) 0.0597(16) 0.0359(12) -0.0182(11) 0.0014(11) -0.0282(13) Cl1P 0.0279(11) 0.0395(13) 0.0614(16) -0.0048(11) 0.0019(10) -0.0104(9) C1O 0.032(4) 0.043(5) 0.030(4) -0.008(4) 0.000(3) -0.016(4) _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 Sn1 Cl11 2.4149(15) 2_663 ? Sn1 Cl11 2.4149(15) . ? Sn1 Cl9 2.4301(14) 2_663 ? Sn1 Cl9 2.4301(14) . ? Sn1 Cl10 2.4566(15) 2_663 ? Sn1 Cl10 2.4566(15) . ? Sn2 Cl8 2.4616(17) . ? Sn2 Cl7 2.4633(16) . ? Sn2 Cl6 2.4810(16) . ? P2 C7 1.822(6) . ? P2 C34 1.829(5) . ? P2 C28 1.840(6) . ? P2 P3 2.230(2) . ? P1 C4 1.808(6) . ? P1 C22 1.833(6) . ? P1 C16 1.844(5) . ? P1 P3 2.208(2) . ? P3 C1 1.862(6) . ? Cl16 C38 1.751(7) . ? Cl17 C38 1.773(7) . ? Cl12 C0AA 1.762(8) . ? Cl20 C45 1.749(7) . ? Cl3N C1M 1.734(7) . ? Cl18 C38 1.752(6) . ? Cl19 C45 1.763(7) . ? Cl2N C1M 1.731(8) . ? Cl22 C0AA 1.740(8) . ? Cl1N C1M 1.781(7) . ? Cl21 C0AA 1.751(7) . ? C4 C15 1.378(8) . ? C4 C5 1.414(8) . ? C5 C12 1.396(8) . ? C5 C6 1.493(8) . ? C14 C15 1.383(8) . ? C14 C13 1.383(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C12 C13 1.392(8) . ? C12 H12 0.9300 . ? C9 C10 1.372(8) . ? C9 C8 1.411(8) . ? C9 H9 0.9300 . ? C8 C7 1.390(8) . ? C8 H8 0.9300 . ? C34 C35 1.531(7) . ? C34 C39 1.535(7) . ? C34 H34 0.9800 . ? C6 C11 1.389(8) . ? C6 C7 1.412(8) . ? C39 C1AA 1.535(8) . ? C39 H39B 0.9700 . ? C39 H39A 0.9700 . ? C22 C27 1.528(8) . ? C22 C23 1.530(8) . ? C22 H22 0.9800 . ? C23 C24 1.512(8) . ? C23 H23B 0.9700 . ? C23 H23A 0.9700 . ? C13 H13 0.9300 . ? C27 C26 1.533(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C33 C32 1.513(8) . ? C33 C28 1.548(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C11 C10 1.386(8) . ? C11 H11 0.9300 . ? C36 C37 1.521(8) . ? C36 C35 1.526(8) . ? C36 H36B 0.9700 . ? C36 H36A 0.9700 . ? C16 C21 1.524(7) . ? C16 C17 1.533(8) . ? C16 H16 0.9800 . ? C28 C29 1.533(8) . ? C28 H28 0.9800 . ? C21 C20 1.521(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C10 H10 0.9300 . ? C32 C31 1.512(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C29 C30 1.548(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C18 C19 1.514(9) . ? C18 C17 1.514(8) . ? C18 H18B 0.9700 . ? C18 H18A 0.9700 . ? C26 C25 1.520(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C2 C3 1.526(8) . ? C2 C1 1.527(8) . ? C2 H2B 0.9700 . ? C2 H2A 0.9700 . ? C30 C31 1.512(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C19 C20 1.521(8) . ? C19 H19B 0.9700 . ? C19 H19A 0.9700 . ? C38 H38 0.9800 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C37 C1AA 1.522(8) . ? C37 H37B 0.9700 . ? C37 H37A 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C24 C25 1.518(9) . ? C24 H24B 0.9700 . ? C24 H24A 0.9700 . ? C3 H3C 0.9600 . ? C3 H3B 0.9600 . ? C3 H3A 0.9600 . ? C20 H20B 0.9700 . ? C20 H20A 0.9700 . ? C1AA H1AB 0.9700 . ? C1AA H1AA 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C31 H31B 0.9700 . ? C31 H31A 0.9700 . ? C0AA H0AA 0.9800 . ? C1M H1M 0.9800 . ? C45 Cl24 1.739(7) . ? C45 H45 0.9800 . ? Cl3P C1O 1.756(19) . ? Cl2P C1O 1.743(19) . ? Cl1P C1O 1.750(19) . ? C1O H1O 0.9800 . ? 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 Cl11 Sn1 Cl11 179.999(1) 2_663 . ? Cl11 Sn1 Cl9 89.78(5) 2_663 2_663 ? Cl11 Sn1 Cl9 90.21(5) . 2_663 ? Cl11 Sn1 Cl9 90.22(5) 2_663 . ? Cl11 Sn1 Cl9 89.79(5) . . ? Cl9 Sn1 Cl9 179.999(1) 2_663 . ? Cl11 Sn1 Cl10 91.02(5) 2_663 2_663 ? Cl11 Sn1 Cl10 88.98(5) . 2_663 ? Cl9 Sn1 Cl10 90.47(5) 2_663 2_663 ? Cl9 Sn1 Cl10 89.54(5) . 2_663 ? Cl11 Sn1 Cl10 88.97(5) 2_663 . ? Cl11 Sn1 Cl10 91.02(5) . . ? Cl9 Sn1 Cl10 89.53(5) 2_663 . ? Cl9 Sn1 Cl10 90.46(5) . . ? Cl10 Sn1 Cl10 179.998(1) 2_663 . ? Cl8 Sn2 Cl7 92.16(6) . . ? Cl8 Sn2 Cl6 94.78(6) . . ? Cl7 Sn2 Cl6 95.30(5) . . ? C7 P2 C34 106.9(2) . . ? C7 P2 C28 109.9(3) . . ? C34 P2 C28 113.2(3) . . ? C7 P2 P3 107.02(19) . . ? C34 P2 P3 103.19(18) . . ? C28 P2 P3 115.94(19) . . ? C4 P1 C22 111.8(3) . . ? C4 P1 C16 108.9(3) . . ? C22 P1 C16 112.0(3) . . ? C4 P1 P3 110.61(19) . . ? C22 P1 P3 107.91(19) . . ? C16 P1 P3 105.45(18) . . ? C1 P3 P1 99.25(19) . . ? C1 P3 P2 104.3(2) . . ? P1 P3 P2 97.72(8) . . ? C15 C4 C5 119.3(5) . . ? C15 C4 P1 119.5(4) . . ? C5 C4 P1 121.3(4) . . ? C12 C5 C4 119.0(5) . . ? C12 C5 C6 117.5(5) . . ? C4 C5 C6 123.3(5) . . ? C15 C14 C13 119.4(5) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C4 C15 C14 121.6(5) . . ? C4 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C13 C12 C5 120.2(6) . . ? C13 C12 H12 119.9 . . ? C5 C12 H12 119.9 . . ? C10 C9 C8 119.3(5) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C7 C8 C9 120.3(5) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C35 C34 C39 111.9(4) . . ? C35 C34 P2 113.7(4) . . ? C39 C34 P2 115.2(4) . . ? C35 C34 H34 104.9 . . ? C39 C34 H34 104.9 . . ? P2 C34 H34 104.9 . . ? C11 C6 C7 117.6(5) . . ? C11 C6 C5 117.5(5) . . ? C7 C6 C5 124.8(5) . . ? C34 C39 C1AA 109.7(5) . . ? C34 C39 H39B 109.7 . . ? C1AA C39 H39B 109.7 . . ? C34 C39 H39A 109.7 . . ? C1AA C39 H39A 109.7 . . ? H39B C39 H39A 108.2 . . ? C27 C22 C23 111.4(5) . . ? C27 C22 P1 112.8(4) . . ? C23 C22 P1 113.6(4) . . ? C27 C22 H22 106.1 . . ? C23 C22 H22 106.1 . . ? P1 C22 H22 106.1 . . ? C24 C23 C22 110.6(5) . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? H23B C23 H23A 108.1 . . ? C8 C7 C6 120.3(5) . . ? C8 C7 P2 117.9(4) . . ? C6 C7 P2 121.8(4) . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C22 C27 C26 108.8(5) . . ? C22 C27 H27A 109.9 . . ? C26 C27 H27A 109.9 . . ? C22 C27 H27B 109.9 . . ? C26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? C32 C33 C28 110.7(5) . . ? C32 C33 H33A 109.5 . . ? C28 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C10 C11 C6 122.1(5) . . ? C10 C11 H11 118.9 . . ? C6 C11 H11 118.9 . . ? C37 C36 C35 112.3(5) . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? H36B C36 H36A 107.9 . . ? C21 C16 C17 111.3(5) . . ? C21 C16 P1 114.1(4) . . ? C17 C16 P1 111.9(4) . . ? C21 C16 H16 106.3 . . ? C17 C16 H16 106.3 . . ? P1 C16 H16 106.3 . . ? C29 C28 C33 110.1(5) . . ? C29 C28 P2 112.4(4) . . ? C33 C28 P2 112.5(4) . . ? C29 C28 H28 107.2 . . ? C33 C28 H28 107.2 . . ? P2 C28 H28 107.2 . . ? C20 C21 C16 109.4(5) . . ? C20 C21 H21A 109.8 . . ? C16 C21 H21A 109.8 . . ? C20 C21 H21B 109.8 . . ? C16 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C9 C10 C11 120.2(6) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C31 C32 C33 111.7(5) . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C28 C29 C30 109.1(5) . . ? C28 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? C19 C18 C17 111.1(5) . . ? C19 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? H18B C18 H18A 108.0 . . ? C25 C26 C27 110.9(5) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.0 . . ? C36 C35 C34 109.1(5) . . ? C36 C35 H35A 109.9 . . ? C34 C35 H35A 109.9 . . ? C36 C35 H35B 109.9 . . ? C34 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? C3 C2 C1 110.6(5) . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? H2B C2 H2A 108.1 . . ? C31 C30 C29 111.0(5) . . ? C31 C30 H30A 109.4 . . ? C29 C30 H30A 109.4 . . ? C31 C30 H30B 109.4 . . ? C29 C30 H30B 109.4 . . ? H30A C30 H30B 108.0 . . ? C18 C19 C20 109.9(5) . . ? C18 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? C18 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? H19B C19 H19A 108.2 . . ? Cl16 C38 Cl18 110.7(4) . . ? Cl16 C38 Cl17 110.5(4) . . ? Cl18 C38 Cl17 109.7(4) . . ? Cl16 C38 H38 108.7 . . ? Cl18 C38 H38 108.7 . . ? Cl17 C38 H38 108.7 . . ? C2 C1 P3 110.7(4) . . ? C2 C1 H1A 109.5 . . ? P3 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? P3 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? C36 C37 C1AA 111.4(5) . . ? C36 C37 H37B 109.3 . . ? C1AA C37 H37B 109.3 . . ? C36 C37 H37A 109.3 . . ? C1AA C37 H37A 109.3 . . ? H37B C37 H37A 108.0 . . ? C18 C17 C16 109.5(5) . . ? C18 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? C18 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? C23 C24 C25 112.2(5) . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? H24B C24 H24A 107.9 . . ? C2 C3 H3C 109.5 . . ? C2 C3 H3B 109.5 . . ? H3C C3 H3B 109.5 . . ? C2 C3 H3A 109.5 . . ? H3C C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? C21 C20 C19 112.2(5) . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? H20B C20 H20A 107.9 . . ? C37 C1AA C39 112.6(5) . . ? C37 C1AA H1AB 109.1 . . ? C39 C1AA H1AB 109.1 . . ? C37 C1AA H1AA 109.1 . . ? C39 C1AA H1AA 109.1 . . ? H1AB C1AA H1AA 107.8 . . ? C24 C25 C26 111.7(5) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C32 C31 C30 111.7(5) . . ? C32 C31 H31B 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31A 109.3 . . ? H31B C31 H31A 107.9 . . ? Cl22 C0AA Cl21 110.9(4) . . ? Cl22 C0AA Cl12 110.2(4) . . ? Cl21 C0AA Cl12 110.4(4) . . ? Cl22 C0AA H0AA 108.4 . . ? Cl21 C0AA H0AA 108.4 . . ? Cl12 C0AA H0AA 108.4 . . ? Cl2N C1M Cl3N 112.8(4) . . ? Cl2N C1M Cl1N 109.8(4) . . ? Cl3N C1M Cl1N 109.4(4) . . ? Cl2N C1M H1M 108.2 . . ? Cl3N C1M H1M 108.2 . . ? Cl1N C1M H1M 108.2 . . ? Cl24 C45 Cl20 112.1(4) . . ? Cl24 C45 Cl19 110.2(4) . . ? Cl20 C45 Cl19 110.2(4) . . ? Cl24 C45 H45 108.1 . . ? Cl20 C45 H45 108.1 . . ? Cl19 C45 H45 108.1 . . ? Cl2P C1O Cl1P 109.9(15) . . ? Cl2P C1O Cl3P 111.5(15) . . ? Cl1P C1O Cl3P 109.5(14) . . ? Cl2P C1O H1O 108.6 . . ? Cl1P C1O H1O 108.6 . . ? Cl3P C1O H1O 108.6 . . ? #=================================================== data_16b _database_code_depnum_ccdc_archive 'CCDC 840424' #TrackingRef '- CrystallographicData.cif' #=================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H56 P4, C H Cl3, 2(Al Cl4)' _chemical_formula_sum 'C30 H57 Al2 Cl11 P4' _chemical_formula_weight 985.55 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' _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 38.5425(12) _cell_length_b 11.8925(4) _cell_length_c 26.5378(9) _cell_angle_alpha 90.00 _cell_angle_beta 130.3910(10) _cell_angle_gamma 90.00 _cell_volume 9264.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8098 _cell_measurement_theta_min 4.717 _cell_measurement_theta_max 58.234 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.9199 _exptl_absorpt_process_details 'XPREP (SHELXTL,1997)' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.1400 0.00 -1.00 0.00 0.1400 0.00 0.00 1.00 0.2500 0.00 0.00 -1.00 0.3000 -2.00 0.00 1.00 0.0500 2.00 0.00 -1.00 0.0500 -4.00 -2.00 -5.00 0.5000 -4.00 -2.00 -5.00 0.2400 _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of \w scans each set at different \f and/or 2\q angles and each frame covering 0.3\% in \w. Crystal to detector distance was 5.81 cm. ; _diffrn_ambient_temperature 120(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 SMART-6000 CCD Diffractometer' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 55926 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 29.14 _reflns_number_total 12468 _reflns_number_gt 10076 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V6.1 (Bruker, 2000)' _computing_cell_refinement 'SMART-NT V6.1 (Bruker, 2000)' _computing_data_reduction 'SAINT-NT V6.45A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+10.8889P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12468 _refine_ls_number_parameters 432 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 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 P1 P 0.645170(14) 0.47757(3) 0.22327(2) 0.01526(8) Uani 1 1 d . . . P2 P 0.706962(15) 0.42066(4) 0.32037(2) 0.01830(9) Uani 1 1 d . . . P3 P 0.702387(14) 0.55931(4) 0.37265(2) 0.01767(9) Uani 1 1 d . . . P4 P 0.631755(14) 0.51683(3) 0.32487(2) 0.01479(8) Uani 1 1 d . . . C1 C 0.60537(5) 0.49958(14) 0.23813(8) 0.0176(3) Uani 1 1 d . . . H1A H 0.5869 0.5673 0.2135 0.021 Uiso 1 1 calc R . . H1B H 0.5843 0.4347 0.2198 0.021 Uiso 1 1 calc R . . C2 C 0.75456(6) 0.47184(17) 0.32525(10) 0.0257(4) Uani 1 1 d . . . H2A H 0.7542 0.4331 0.2919 0.031 Uiso 1 1 calc R . . H2B H 0.7514 0.5537 0.3163 0.031 Uiso 1 1 calc R . . C3 C 0.79920(7) 0.4474(2) 0.39467(11) 0.0373(5) Uani 1 1 d . . . H3A H 0.8248 0.4737 0.3983 0.056 Uiso 1 1 calc R . . H3B H 0.8020 0.3662 0.4030 0.056 Uiso 1 1 calc R . . H3C H 0.7994 0.4866 0.4273 0.056 Uiso 1 1 calc R . . C4 C 0.73525(6) 0.50126(16) 0.45791(8) 0.0228(3) Uani 1 1 d . . . H4A H 0.7146 0.4885 0.4674 0.027 Uiso 1 1 calc R . . H4B H 0.7490 0.4283 0.4614 0.027 Uiso 1 1 calc R . . C5 C 0.77246(7) 0.58395(19) 0.50770(10) 0.0362(5) Uani 1 1 d . . . H5A H 0.7898 0.5536 0.5525 0.054 Uiso 1 1 calc R . . H5B H 0.7586 0.6558 0.5044 0.054 Uiso 1 1 calc R . . H5C H 0.7930 0.5957 0.4983 0.054 Uiso 1 1 calc R . . C11 C 0.62460(6) 0.36246(14) 0.16477(8) 0.0180(3) Uani 1 1 d . . . H11A H 0.5944 0.3851 0.1222 0.022 Uiso 1 1 calc R . . C12 C 0.61790(6) 0.25276(14) 0.18796(9) 0.0207(3) Uani 1 1 d . . . H12A H 0.6475 0.2271 0.2296 0.025 Uiso 1 1 calc R . . H12B H 0.5968 0.2656 0.1966 0.025 Uiso 1 1 calc R . . C13 C 0.59834(6) 0.16290(15) 0.13446(10) 0.0245(4) Uani 1 1 d . . . H13A H 0.5945 0.0917 0.1497 0.029 Uiso 1 1 calc R . . H13B H 0.5680 0.1870 0.0938 0.029 Uiso 1 1 calc R . . C14 C 0.62956(6) 0.14301(15) 0.11869(9) 0.0247(4) Uani 1 1 d . . . H14A H 0.6587 0.1104 0.1579 0.030 Uiso 1 1 calc R . . H14B H 0.6151 0.0881 0.0821 0.030 Uiso 1 1 calc R . . C15 C 0.63915(7) 0.25126(15) 0.09915(10) 0.0259(4) Uani 1 1 d . . . H15A H 0.6107 0.2775 0.0561 0.031 Uiso 1 1 calc R . . H15B H 0.6617 0.2361 0.0935 0.031 Uiso 1 1 calc R . . C16 C 0.65741(7) 0.34405(15) 0.15094(10) 0.0243(4) Uani 1 1 d . . . H16A H 0.6606 0.4149 0.1347 0.029 Uiso 1 1 calc R . . H16B H 0.6879 0.3226 0.1924 0.029 Uiso 1 1 calc R . . C21 C 0.64728(6) 0.60493(14) 0.18692(8) 0.0183(3) Uani 1 1 d . . . H21A H 0.6679 0.5893 0.1772 0.022 Uiso 1 1 calc R . . C22 C 0.66631(6) 0.70808(14) 0.23251(9) 0.0217(3) Uani 1 1 d . . . H22A H 0.6479 0.7230 0.2457 0.026 Uiso 1 1 calc R . . H22B H 0.6981 0.6931 0.2731 0.026 Uiso 1 1 calc R . . C23 C 0.66517(7) 0.81094(15) 0.19685(10) 0.0261(4) Uani 1 1 d . . . H23A H 0.6767 0.8773 0.2262 0.031 Uiso 1 1 calc R . . H23B H 0.6853 0.7979 0.1865 0.031 Uiso 1 1 calc R . . C24 C 0.61698(7) 0.83416(16) 0.13312(10) 0.0310(4) Uani 1 1 d . . . H24A H 0.5970 0.8503 0.1435 0.037 Uiso 1 1 calc R . . H24B H 0.6170 0.9011 0.1110 0.037 Uiso 1 1 calc R . . C25 C 0.59859(8) 0.73340(17) 0.08704(10) 0.0360(5) Uani 1 1 d . . . H25A H 0.6172 0.7211 0.0740 0.043 Uiso 1 1 calc R . . H25B H 0.5669 0.7489 0.0464 0.043 Uiso 1 1 calc R . . C26 C 0.59943(7) 0.62761(16) 0.12034(10) 0.0316(4) Uani 1 1 d . . . H26A H 0.5897 0.5624 0.0907 0.038 Uiso 1 1 calc R . . H26B H 0.5775 0.6362 0.1279 0.038 Uiso 1 1 calc R . . C31 C 0.62181(6) 0.39186(13) 0.35421(9) 0.0178(3) Uani 1 1 d . . . H31A H 0.6310 0.4119 0.3980 0.021 Uiso 1 1 calc R . . C32 C 0.64997(6) 0.28846(14) 0.36575(9) 0.0219(3) Uani 1 1 d . . . H32A H 0.6420 0.2653 0.3235 0.026 Uiso 1 1 calc R . . H32B H 0.6828 0.3074 0.3974 0.026 Uiso 1 1 calc R . . C33 C 0.64037(7) 0.19166(15) 0.39321(10) 0.0265(4) Uani 1 1 d . . . H33A H 0.6578 0.1245 0.3991 0.032 Uiso 1 1 calc R . . H33B H 0.6506 0.2130 0.4371 0.032 Uiso 1 1 calc R . . C34 C 0.58984(7) 0.16345(15) 0.34681(11) 0.0294(4) Uani 1 1 d . . . H34A H 0.5800 0.1378 0.3038 0.035 Uiso 1 1 calc R . . H34B H 0.5844 0.1016 0.3659 0.035 Uiso 1 1 calc R . . C35 C 0.56222(7) 0.26601(17) 0.33626(12) 0.0316(4) Uani 1 1 d . . . H35A H 0.5709 0.2890 0.3790 0.038 Uiso 1 1 calc R . . H35B H 0.5294 0.2466 0.3056 0.038 Uiso 1 1 calc R . . C36 C 0.57040(6) 0.36390(16) 0.30762(11) 0.0279(4) Uani 1 1 d . . . H36A H 0.5531 0.4307 0.3027 0.034 Uiso 1 1 calc R . . H36B H 0.5596 0.3433 0.2633 0.034 Uiso 1 1 calc R . . C41 C 0.60729(6) 0.63577(13) 0.33601(8) 0.0170(3) Uani 1 1 d . . . H41A H 0.5775 0.6101 0.3223 0.020 Uiso 1 1 calc R . . C42 C 0.63849(6) 0.66541(14) 0.41009(9) 0.0210(3) Uani 1 1 d . . . H42A H 0.6445 0.5971 0.4360 0.025 Uiso 1 1 calc R . . H42B H 0.6680 0.6941 0.4251 0.025 Uiso 1 1 calc R . . C43 C 0.61578(7) 0.75482(16) 0.42180(10) 0.0266(4) Uani 1 1 d . . . H43A H 0.5884 0.7221 0.4122 0.032 Uiso 1 1 calc R . . H43B H 0.6371 0.7774 0.4689 0.032 Uiso 1 1 calc R . . C44 C 0.60196(7) 0.85828(15) 0.37883(10) 0.0278(4) Uani 1 1 d . . . H44A H 0.6297 0.8988 0.3939 0.033 Uiso 1 1 calc R . . H44B H 0.5842 0.9094 0.3841 0.033 Uiso 1 1 calc R . . C45 C 0.57344(7) 0.82793(16) 0.30586(10) 0.0287(4) Uani 1 1 d . . . H45A H 0.5674 0.8967 0.2803 0.034 Uiso 1 1 calc R . . H45B H 0.5438 0.7971 0.2891 0.034 Uiso 1 1 calc R . . C46 C 0.59768(6) 0.74131(14) 0.29545(9) 0.0231(3) Uani 1 1 d . . . H46A H 0.6266 0.7730 0.3099 0.028 Uiso 1 1 calc R . . H46B H 0.5783 0.7218 0.2480 0.028 Uiso 1 1 calc R . . Al1 Al 0.967217(18) 0.99641(5) 0.57721(3) 0.02241(11) Uani 1 1 d . . . Al2 Al 0.739370(19) 0.04847(5) 0.36262(3) 0.02490(12) Uani 1 1 d . . . Cl1 Cl 1.003832(16) 1.15035(4) 0.60066(2) 0.02931(10) Uani 1 1 d . . . Cl2 Cl 0.994296(15) 0.92044(4) 0.67002(2) 0.02977(10) Uani 1 1 d . . . Cl3 Cl 0.978725(17) 0.88643(4) 0.52622(3) 0.03328(11) Uani 1 1 d . . . Cl4 Cl 0.896297(15) 1.02822(5) 0.51877(2) 0.03176(11) Uani 1 1 d . . . Cl5 Cl 0.77349(2) -0.10846(5) 0.40270(3) 0.04405(14) Uani 1 1 d . . . Cl6 Cl 0.668241(16) 0.02148(4) 0.30859(2) 0.02855(10) Uani 1 1 d . . . Cl7 Cl 0.748917(18) 0.11685(5) 0.29753(3) 0.03886(13) Uani 1 1 d . . . Cl8 Cl 0.765674(18) 0.16923(4) 0.43962(2) 0.03276(11) Uani 1 1 d . . . Cl1S Cl 0.92726(2) 0.42695(5) 0.53606(3) 0.04172(13) Uani 1 1 d D . . Cl2S Cl 1.01633(3) 0.44743(7) 0.66462(3) 0.0644(2) Uani 1 1 d D . . Cl3S Cl 0.98581(14) 0.6078(3) 0.5644(2) 0.0792(9) Uani 0.50 1 d PD A 1 C1S C 0.9838(2) 0.4683(6) 0.5804(3) 0.066(4) Uiso 0.50 1 d PD A 1 H1SA H 0.9970 0.4220 0.5650 0.079 Uiso 0.50 1 calc PR A 1 Cl3A Cl 0.99252(13) 0.5722(3) 0.5494(2) 0.1074(16) Uani 0.50 1 d PD A 2 C1SA C 0.98469(14) 0.4532(6) 0.5783(2) 0.0302(17) Uiso 0.50 1 d PD A 2 H1SB H 0.9957 0.3888 0.5677 0.036 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.01932(19) 0.01389(18) 0.01437(19) 0.00036(14) 0.01172(17) 0.00011(14) P2 0.01926(19) 0.0201(2) 0.0171(2) 0.00276(16) 0.01251(18) 0.00210(15) P3 0.01881(19) 0.0186(2) 0.0144(2) 0.00067(15) 0.01020(17) -0.00143(15) P4 0.01880(19) 0.01303(18) 0.01412(19) -0.00004(14) 0.01137(17) -0.00043(14) C1 0.0187(7) 0.0201(8) 0.0156(8) -0.0017(6) 0.0118(7) -0.0005(6) C2 0.0231(8) 0.0323(10) 0.0268(10) 0.0041(8) 0.0185(8) 0.0013(7) C3 0.0233(9) 0.0573(14) 0.0307(11) 0.0039(10) 0.0172(9) -0.0026(9) C4 0.0233(8) 0.0274(9) 0.0133(8) 0.0027(6) 0.0099(7) 0.0017(7) C5 0.0323(10) 0.0389(12) 0.0191(9) -0.0016(8) 0.0084(9) -0.0072(9) C11 0.0237(8) 0.0153(7) 0.0168(8) -0.0015(6) 0.0139(7) -0.0011(6) C12 0.0269(8) 0.0162(8) 0.0203(8) 0.0009(6) 0.0159(7) -0.0001(6) C13 0.0308(9) 0.0161(8) 0.0256(9) -0.0028(7) 0.0178(8) -0.0032(7) C14 0.0300(9) 0.0180(8) 0.0234(9) -0.0040(7) 0.0161(8) 0.0004(7) C15 0.0362(10) 0.0221(9) 0.0278(10) -0.0054(7) 0.0245(9) -0.0009(7) C16 0.0338(9) 0.0193(8) 0.0298(10) -0.0052(7) 0.0250(9) -0.0039(7) C21 0.0269(8) 0.0152(7) 0.0167(8) 0.0003(6) 0.0159(7) -0.0012(6) C22 0.0300(9) 0.0175(8) 0.0193(8) -0.0025(6) 0.0167(8) -0.0048(6) C23 0.0393(10) 0.0163(8) 0.0265(9) -0.0019(7) 0.0230(9) -0.0062(7) C24 0.0450(11) 0.0176(8) 0.0293(10) 0.0051(7) 0.0236(10) 0.0021(8) C25 0.0489(12) 0.0231(9) 0.0204(9) 0.0052(7) 0.0154(9) -0.0049(9) C26 0.0367(10) 0.0204(9) 0.0180(9) 0.0044(7) 0.0089(8) -0.0056(8) C31 0.0253(8) 0.0137(7) 0.0199(8) 0.0009(6) 0.0171(7) -0.0007(6) C32 0.0297(9) 0.0154(8) 0.0280(9) 0.0022(6) 0.0221(8) 0.0019(6) C33 0.0389(10) 0.0159(8) 0.0311(10) 0.0053(7) 0.0256(9) 0.0037(7) C34 0.0455(11) 0.0157(8) 0.0360(11) -0.0018(7) 0.0305(10) -0.0059(8) C35 0.0332(10) 0.0250(9) 0.0441(12) 0.0051(8) 0.0284(10) -0.0031(8) C36 0.0239(8) 0.0227(9) 0.0352(11) 0.0072(8) 0.0182(8) -0.0008(7) C41 0.0207(7) 0.0150(7) 0.0165(8) -0.0006(6) 0.0126(7) 0.0001(6) C42 0.0282(8) 0.0170(8) 0.0182(8) -0.0015(6) 0.0152(7) 0.0003(6) C43 0.0368(10) 0.0213(9) 0.0291(10) -0.0052(7) 0.0247(9) -0.0013(7) C44 0.0344(10) 0.0175(8) 0.0331(10) -0.0043(7) 0.0227(9) 0.0013(7) C45 0.0322(10) 0.0185(8) 0.0286(10) 0.0016(7) 0.0165(8) 0.0070(7) C46 0.0306(9) 0.0170(8) 0.0196(8) 0.0018(6) 0.0154(8) 0.0019(7) Al1 0.0210(2) 0.0267(3) 0.0188(3) 0.0012(2) 0.0125(2) -0.0018(2) Al2 0.0257(3) 0.0300(3) 0.0197(3) 0.0007(2) 0.0150(2) 0.0039(2) Cl1 0.0271(2) 0.0263(2) 0.0292(2) 0.00208(17) 0.0159(2) -0.00323(17) Cl2 0.0248(2) 0.0405(3) 0.0207(2) 0.00625(18) 0.01328(19) -0.00232(18) Cl3 0.0345(2) 0.0368(3) 0.0303(3) -0.0061(2) 0.0217(2) -0.0019(2) Cl4 0.0213(2) 0.0427(3) 0.0267(2) 0.0045(2) 0.01354(19) 0.00072(18) Cl5 0.0404(3) 0.0389(3) 0.0465(3) 0.0067(2) 0.0253(3) 0.0170(2) Cl6 0.0273(2) 0.0320(2) 0.0271(2) 0.00074(18) 0.0180(2) 0.00300(17) Cl7 0.0347(3) 0.0633(4) 0.0270(3) 0.0005(2) 0.0238(2) -0.0009(2) Cl8 0.0440(3) 0.0305(2) 0.0209(2) -0.00052(17) 0.0198(2) -0.0027(2) Cl1S 0.0487(3) 0.0454(3) 0.0286(3) -0.0039(2) 0.0239(3) -0.0009(2) Cl2S 0.0656(4) 0.0620(4) 0.0312(3) -0.0047(3) 0.0159(3) -0.0043(3) Cl3S 0.0593(14) 0.0610(14) 0.090(2) 0.0324(12) 0.0363(12) -0.0025(10) Cl3A 0.0523(14) 0.119(3) 0.092(3) 0.068(2) 0.0208(13) -0.0114(18) _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 P1 C11 1.8214(17) . ? P1 C21 1.8257(17) . ? P1 C1 1.8333(16) . ? P1 P2 2.1946(6) . ? P2 C2 1.8560(18) . ? P2 P3 2.2343(6) . ? P3 C4 1.8672(18) . ? P3 P4 2.1910(6) . ? P4 C41 1.8272(16) . ? P4 C1 1.8279(17) . ? P4 C31 1.8300(16) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.527(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.521(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C11 C12 1.534(2) . ? C11 C16 1.544(2) . ? C11 H11A 1.0000 . ? C12 C13 1.529(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.527(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.520(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.532(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C21 C22 1.535(2) . ? C21 C26 1.540(3) . ? C21 H21A 1.0000 . ? C22 C23 1.530(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.520(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.526(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C31 C32 1.534(2) . ? C31 C36 1.546(2) . ? C31 H31A 1.0000 . ? C32 C33 1.531(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.521(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.521(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.531(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C41 C46 1.534(2) . ? C41 C42 1.540(2) . ? C41 H41A 1.0000 . ? C42 C43 1.532(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.520(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.526(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.531(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? Al1 Cl3 2.1251(8) . ? Al1 Cl4 2.1274(7) . ? Al1 Cl1 2.1429(7) . ? Al1 Cl2 2.1542(7) . ? Al2 Cl5 2.1286(8) . ? Al2 Cl6 2.1401(7) . ? Al2 Cl8 2.1404(8) . ? Al2 Cl7 2.1457(8) . ? Cl1S C1SA 1.743(4) . ? Cl1S C1S 1.746(6) . ? Cl2S C1S 1.731(6) . ? Cl2S C1SA 1.765(4) . ? Cl3S C1S 1.726(6) . ? C1S H1SA 1.0000 . ? Cl3A C1SA 1.727(5) . ? C1SA H1SB 1.0000 . ? 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 C11 P1 C21 108.48(8) . . ? C11 P1 C1 109.14(8) . . ? C21 P1 C1 108.98(8) . . ? C11 P1 P2 108.11(6) . . ? C21 P1 P2 119.35(6) . . ? C1 P1 P2 102.37(6) . . ? C2 P2 P1 104.62(6) . . ? C2 P2 P3 100.77(7) . . ? P1 P2 P3 92.25(2) . . ? C4 P3 P4 103.22(6) . . ? C4 P3 P2 102.42(6) . . ? P4 P3 P2 92.23(2) . . ? C41 P4 C1 111.49(8) . . ? C41 P4 C31 106.71(8) . . ? C1 P4 C31 110.22(8) . . ? C41 P4 P3 107.81(6) . . ? C1 P4 P3 102.90(5) . . ? C31 P4 P3 117.74(6) . . ? P4 C1 P1 115.26(9) . . ? P4 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? P4 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 P2 108.17(13) . . ? C3 C2 H2A 110.1 . . ? P2 C2 H2A 110.1 . . ? C3 C2 H2B 110.1 . . ? P2 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 P3 109.32(13) . . ? C5 C4 H4A 109.8 . . ? P3 C4 H4A 109.8 . . ? C5 C4 H4B 109.8 . . ? P3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C11 C16 110.58(14) . . ? C12 C11 P1 113.00(12) . . ? C16 C11 P1 109.76(11) . . ? C12 C11 H11A 107.8 . . ? C16 C11 H11A 107.8 . . ? P1 C11 H11A 107.8 . . ? C13 C12 C11 109.38(14) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C12 111.15(15) . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 111.79(15) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 112.08(15) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C11 110.14(15) . . ? C15 C16 H16A 109.6 . . ? C11 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? C11 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C22 C21 C26 111.68(15) . . ? C22 C21 P1 114.12(12) . . ? C26 C21 P1 108.73(12) . . ? C22 C21 H21A 107.3 . . ? C26 C21 H21A 107.3 . . ? P1 C21 H21A 107.3 . . ? C23 C22 C21 110.13(14) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 110.97(15) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 110.38(16) . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 111.11(17) . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25B 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C25 C26 C21 111.65(16) . . ? C25 C26 H26A 109.3 . . ? C21 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C21 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C32 C31 C36 111.21(14) . . ? C32 C31 P4 114.82(11) . . ? C36 C31 P4 110.35(12) . . ? C32 C31 H31A 106.7 . . ? C36 C31 H31A 106.7 . . ? P4 C31 H31A 106.7 . . ? C33 C32 C31 109.86(14) . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 110.99(16) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.38(16) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 110.90(16) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 109.64(16) . . ? C35 C36 H36A 109.7 . . ? C31 C36 H36A 109.7 . . ? C35 C36 H36B 109.7 . . ? C31 C36 H36B 109.7 . . ? H36A C36 H36B 108.2 . . ? C46 C41 C42 110.01(14) . . ? C46 C41 P4 115.79(12) . . ? C42 C41 P4 109.01(11) . . ? C46 C41 H41A 107.2 . . ? C42 C41 H41A 107.2 . . ? P4 C41 H41A 107.2 . . ? C43 C42 C41 109.97(14) . . ? C43 C42 H42A 109.7 . . ? C41 C42 H42A 109.7 . . ? C43 C42 H42B 109.7 . . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C44 C43 C42 112.23(15) . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43B 109.2 . . ? C42 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C43 C44 C45 111.99(15) . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C45 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 111.46(15) . . ? C44 C45 H45A 109.3 . . ? C46 C45 H45A 109.3 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C41 108.78(15) . . ? C45 C46 H46A 109.9 . . ? C41 C46 H46A 109.9 . . ? C45 C46 H46B 109.9 . . ? C41 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? Cl3 Al1 Cl4 110.18(3) . . ? Cl3 Al1 Cl1 109.93(3) . . ? Cl4 Al1 Cl1 110.67(3) . . ? Cl3 Al1 Cl2 108.87(3) . . ? Cl4 Al1 Cl2 110.47(3) . . ? Cl1 Al1 Cl2 106.64(3) . . ? Cl5 Al2 Cl6 108.16(3) . . ? Cl5 Al2 Cl8 110.74(3) . . ? Cl6 Al2 Cl8 110.42(3) . . ? Cl5 Al2 Cl7 111.21(3) . . ? Cl6 Al2 Cl7 109.32(3) . . ? Cl8 Al2 Cl7 106.98(3) . . ? Cl3S C1S Cl2S 110.1(4) . . ? Cl3S C1S Cl1S 109.9(4) . . ? Cl2S C1S Cl1S 112.0(4) . . ? Cl3S C1S H1SA 108.2 . . ? Cl2S C1S H1SA 108.2 . . ? Cl1S C1S H1SA 108.2 . . ? Cl3A C1SA Cl1S 112.1(3) . . ? Cl3A C1SA Cl2S 115.8(3) . . ? Cl1S C1SA Cl2S 110.5(3) . . ? Cl3A C1SA H1SB 105.9 . . ? Cl1S C1SA H1SB 105.9 . . ? Cl2S C1SA H1SB 105.9 . . ? 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 C11 P1 P2 C2 95.75(9) . . . . ? C21 P1 P2 C2 -28.76(9) . . . . ? C1 P1 P2 C2 -149.11(9) . . . . ? C11 P1 P2 P3 -162.51(6) . . . . ? C21 P1 P2 P3 72.98(7) . . . . ? C1 P1 P2 P3 -47.37(6) . . . . ? C2 P2 P3 C4 -97.96(9) . . . . ? P1 P2 P3 C4 156.69(6) . . . . ? C2 P2 P3 P4 157.98(6) . . . . ? P1 P2 P3 P4 52.64(2) . . . . ? C4 P3 P4 C41 92.24(8) . . . . ? P2 P3 P4 C41 -164.45(6) . . . . ? C4 P3 P4 C1 -149.84(8) . . . . ? P2 P3 P4 C1 -46.53(6) . . . . ? C4 P3 P4 C31 -28.43(9) . . . . ? P2 P3 P4 C31 74.88(7) . . . . ? C41 P4 C1 P1 133.62(9) . . . . ? C31 P4 C1 P1 -108.07(10) . . . . ? P3 P4 C1 P1 18.31(10) . . . . ? C11 P1 C1 P4 134.37(9) . . . . ? C21 P1 C1 P4 -107.32(10) . . . . ? P2 P1 C1 P4 19.98(10) . . . . ? P1 P2 C2 C3 173.70(14) . . . . ? P3 P2 C2 C3 78.49(15) . . . . ? P4 P3 C4 C5 -139.13(13) . . . . ? P2 P3 C4 C5 125.55(14) . . . . ? C21 P1 C11 C12 -175.53(12) . . . . ? C1 P1 C11 C12 -56.91(14) . . . . ? P2 P1 C11 C12 53.70(13) . . . . ? C21 P1 C11 C16 60.54(14) . . . . ? C1 P1 C11 C16 179.16(12) . . . . ? P2 P1 C11 C16 -70.23(12) . . . . ? C16 C11 C12 C13 -59.41(19) . . . . ? P1 C11 C12 C13 177.11(12) . . . . ? C11 C12 C13 C14 58.08(19) . . . . ? C12 C13 C14 C15 -55.4(2) . . . . ? C13 C14 C15 C16 53.5(2) . . . . ? C14 C15 C16 C11 -54.3(2) . . . . ? C12 C11 C16 C15 57.5(2) . . . . ? P1 C11 C16 C15 -177.20(13) . . . . ? C11 P1 C21 C22 -177.21(12) . . . . ? C1 P1 C21 C22 64.07(14) . . . . ? P2 P1 C21 C22 -52.89(14) . . . . ? C11 P1 C21 C26 57.39(15) . . . . ? C1 P1 C21 C26 -61.34(15) . . . . ? P2 P1 C21 C26 -178.29(11) . . . . ? C26 C21 C22 C23 -54.2(2) . . . . ? P1 C21 C22 C23 -178.07(12) . . . . ? C21 C22 C23 C24 57.6(2) . . . . ? C22 C23 C24 C25 -59.4(2) . . . . ? C23 C24 C25 C26 57.4(3) . . . . ? C24 C25 C26 C21 -54.4(3) . . . . ? C22 C21 C26 C25 53.1(2) . . . . ? P1 C21 C26 C25 179.90(15) . . . . ? C41 P4 C31 C32 -165.11(13) . . . . ? C1 P4 C31 C32 73.68(14) . . . . ? P3 P4 C31 C32 -43.87(15) . . . . ? C41 P4 C31 C36 68.27(14) . . . . ? C1 P4 C31 C36 -52.94(14) . . . . ? P3 P4 C31 C36 -170.49(11) . . . . ? C36 C31 C32 C33 -56.5(2) . . . . ? P4 C31 C32 C33 177.32(13) . . . . ? C31 C32 C33 C34 57.2(2) . . . . ? C32 C33 C34 C35 -58.4(2) . . . . ? C33 C34 C35 C36 58.5(2) . . . . ? C34 C35 C36 C31 -57.2(2) . . . . ? C32 C31 C36 C35 56.6(2) . . . . ? P4 C31 C36 C35 -174.81(14) . . . . ? C1 P4 C41 C46 -40.68(15) . . . . ? C31 P4 C41 C46 -161.08(13) . . . . ? P3 P4 C41 C46 71.56(13) . . . . ? C1 P4 C41 C42 -165.32(11) . . . . ? C31 P4 C41 C42 74.28(13) . . . . ? P3 P4 C41 C42 -53.08(12) . . . . ? C46 C41 C42 C43 59.18(18) . . . . ? P4 C41 C42 C43 -172.85(12) . . . . ? C41 C42 C43 C44 -54.5(2) . . . . ? C42 C43 C44 C45 52.2(2) . . . . ? C43 C44 C45 C46 -54.2(2) . . . . ? C44 C45 C46 C41 58.4(2) . . . . ? C42 C41 C46 C45 -61.00(19) . . . . ? P4 C41 C46 C45 174.89(12) . . . . ? C1SA Cl2S C1S Cl3S -149(3) . . . . ? C1SA Cl2S C1S Cl1S 88(3) . . . . ? C1SA Cl1S C1S Cl3S 142(3) . . . . ? C1SA Cl1S C1S Cl2S -96(3) . . . . ? C1S Cl1S C1SA Cl3A -56(3) . . . . ? C1S Cl1S C1SA Cl2S 75(3) . . . . ? C1S Cl2S C1SA Cl3A 46(3) . . . . ? C1S Cl2S C1SA Cl1S -82(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.966 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.068 #=================================================== data_19a _database_code_depnum_ccdc_archive 'CCDC 840425' #TrackingRef '- CrystallographicData.cif' #=================================================== _audit_creation_date 2011-08-10 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H32 P4, Cl6 Sn' _chemical_formula_sum 'C29 H32 Cl6 P4 Sn' _chemical_formula_weight 835.82 _chemical_melting_point ? 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' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.5532(8) _cell_length_b 11.0978(8) _cell_length_c 16.1102(12) _cell_angle_alpha 104.3190(10) _cell_angle_beta 92.3670(10) _cell_angle_gamma 100.4550(10) _cell_volume 1790.4(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8576 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 28.265 _cell_measurement_theta_min 2.265 _exptl_absorpt_coefficient_mu 1.360 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 836 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 19382 _diffrn_reflns_theta_full 28.30 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_theta_min 1.31 _diffrn_ambient_temperature 120.15 _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_detector_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 35.0 _diffrn_source_power 1.75 _diffrn_source_voltage 50.0 _reflns_number_gt 6804 _reflns_number_total 8782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v5.630 (Bruker, 2003)' _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _refine_diff_density_max 3.757 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.125 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 375 _refine_ls_number_reflns 8782 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0466 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+4.6641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1085 _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. The terminal carbon atoms of both ethyl substituents show minor positional disorder, with the major orientational component representing approximately 84% There is a relatively large residual peak of electron density (3.76 e/A3) close to one of the (SnCl)6 ions which most likely indicates slight disorder of this moiety which breaks the inversion symmetry. Modelling of this disorder requires heavy restraints and constraints and does not result in a chemically sensible model. as such the current structural model was deemed most suitable ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Sn2 Sn 0.0000 0.0000 0.0000 0.01669(9) Uani 1 2 d S . . Cl5 Cl -0.16330(10) 0.10503(9) 0.07120(7) 0.0217(2) Uani 1 1 d . . . Cl6 Cl 0.14054(10) 0.20662(9) 0.01393(7) 0.0228(2) Uani 1 1 d . . . Cl4 Cl 0.09570(10) -0.00994(10) 0.13722(7) 0.0232(2) Uani 1 1 d . . . Sn1 Sn 0.5000 0.5000 0.5000 0.01749(10) Uani 1 2 d S . . Cl2 Cl 0.68512(10) 0.51158(9) 0.41492(7) 0.0214(2) Uani 1 1 d . . . Cl1 Cl 0.35538(10) 0.49324(10) 0.37657(7) 0.0264(2) Uani 1 1 d . . . Cl3 Cl 0.47236(11) 0.26924(9) 0.45890(7) 0.0261(2) Uani 1 1 d . . . P4 P 0.69828(10) 0.74969(9) 0.21763(7) 0.0144(2) Uani 1 1 d . . . P1 P 0.69920(10) 1.03005(9) 0.27471(6) 0.0148(2) Uani 1 1 d . . . P3 P 0.65548(11) 0.77199(10) 0.35188(7) 0.0187(2) Uani 1 1 d . A . P2 P 0.58552(11) 0.95111(10) 0.36765(7) 0.0208(2) Uani 1 1 d . A . C19 C 0.5355(4) 0.6941(4) 0.0669(3) 0.0175(8) Uani 1 1 d . . . H19 H 0.6024 0.7454 0.0463 0.021 Uiso 1 1 calc R . . C1 C 0.7632(4) 0.9055(3) 0.2019(2) 0.0153(7) Uani 1 1 d . . . H1A H 0.7406 0.9055 0.1417 0.018 Uiso 1 1 calc R . . H1B H 0.8587 0.9233 0.2122 0.018 Uiso 1 1 calc R . . C23 C 0.4527(4) 0.5995(4) 0.1795(3) 0.0202(8) Uani 1 1 d . . . H23 H 0.4627 0.5883 0.2358 0.024 Uiso 1 1 calc R . . C29 C 0.7734(4) 0.5234(4) 0.2017(3) 0.0218(9) Uani 1 1 d . . . H29 H 0.6943 0.5009 0.2255 0.026 Uiso 1 1 calc R . . C24 C 0.8107(4) 0.6460(4) 0.1907(3) 0.0185(8) Uani 1 1 d . . . C18 C 0.5499(4) 0.6788(3) 0.1500(3) 0.0161(8) Uani 1 1 d . . . C25 C 0.9267(4) 0.6797(4) 0.1573(3) 0.0316(11) Uani 1 1 d . . . H25 H 0.9538 0.7631 0.1508 0.038 Uiso 1 1 calc R . . C6 C 0.5982(4) 1.0989(3) 0.2154(3) 0.0155(7) Uani 1 1 d . . . C21 C 0.3264(4) 0.5552(4) 0.0439(3) 0.0254(9) Uani 1 1 d . . . H21 H 0.2495 0.5135 0.0078 0.030 Uiso 1 1 calc R . . C7 C 0.5218(4) 1.0287(4) 0.1411(3) 0.0212(8) Uani 1 1 d . . . H7 H 0.5311 0.9443 0.1153 0.025 Uiso 1 1 calc R . . C11 C 0.5860(4) 1.2233(4) 0.2544(3) 0.0197(8) Uani 1 1 d . . . H11 H 0.6383 1.2713 0.3053 0.024 Uiso 1 1 calc R . . C12 C 0.8311(4) 1.1485(4) 0.3368(3) 0.0190(8) Uani 1 1 d . . . C26 C 1.0026(5) 0.5892(5) 0.1334(4) 0.0456(15) Uani 1 1 d . . . H26 H 1.0818 0.6111 0.1097 0.055 Uiso 1 1 calc R . . C8 C 0.4321(4) 1.0816(4) 0.1046(3) 0.0276(10) Uani 1 1 d . . . H8 H 0.3797 1.0340 0.0535 0.033 Uiso 1 1 calc R . . C22 C 0.3421(4) 0.5377(4) 0.1256(3) 0.0256(9) Uani 1 1 d . . . H22 H 0.2766 0.4828 0.1449 0.031 Uiso 1 1 calc R . . C27 C 0.9658(5) 0.4686(5) 0.1433(4) 0.0407(13) Uani 1 1 d . . . H27 H 1.0191 0.4079 0.1263 0.049 Uiso 1 1 calc R . . C13 C 0.9453(4) 1.1776(4) 0.2997(3) 0.0248(9) Uani 1 1 d . . . H13 H 0.9549 1.1330 0.2426 0.030 Uiso 1 1 calc R . . C15 C 1.0295(5) 1.3386(4) 0.4292(4) 0.0381(12) Uani 1 1 d . . . H15 H 1.0982 1.4028 0.4616 0.046 Uiso 1 1 calc R . . C17 C 0.8135(5) 1.2163(4) 0.4191(3) 0.0275(10) Uani 1 1 d . . . H17 H 0.7342 1.1976 0.4436 0.033 Uiso 1 1 calc R . . C10 C 0.4958(4) 1.2744(4) 0.2168(3) 0.0258(9) Uani 1 1 d . . . H10 H 0.4865 1.3589 0.2421 0.031 Uiso 1 1 calc R . . C16 C 0.9140(6) 1.3117(5) 0.4647(3) 0.0393(13) Uani 1 1 d . . . H16 H 0.9033 1.3588 0.5210 0.047 Uiso 1 1 calc R . . C9 C 0.4191(4) 1.2043(4) 0.1430(3) 0.0276(10) Uani 1 1 d . . . H9 H 0.3570 1.2406 0.1184 0.033 Uiso 1 1 calc R . . C20 C 0.4219(4) 0.6332(4) 0.0145(3) 0.0238(9) Uani 1 1 d . . . H20 H 0.4101 0.6453 -0.0414 0.029 Uiso 1 1 calc R . . C28 C 0.8505(5) 0.4358(4) 0.1783(3) 0.0294(10) Uani 1 1 d . . . H28 H 0.8251 0.3530 0.1861 0.035 Uiso 1 1 calc R . . C14 C 1.0454(5) 1.2725(4) 0.3466(3) 0.0328(11) Uani 1 1 d . . . H14 H 1.1245 1.2920 0.3221 0.039 Uiso 1 1 calc R . . C2 C 0.4206(4) 0.9030(4) 0.3110(3) 0.0268(10) Uani 1 1 d . . . H2AA H 0.3869 0.9791 0.3068 0.032 Uiso 0.842(6) 1 calc PR A 1 H2AB H 0.4233 0.8502 0.2520 0.032 Uiso 0.842(6) 1 calc PR A 1 H2BC H 0.4302 0.8602 0.2506 0.032 Uiso 0.158(6) 1 calc PR A 2 H2BD H 0.3725 0.8372 0.3361 0.032 Uiso 0.158(6) 1 calc PR A 2 C4 C 0.8260(4) 0.8326(5) 0.4014(3) 0.0304(10) Uani 1 1 d . . . H4AA H 0.8731 0.7616 0.3919 0.037 Uiso 0.842(6) 1 calc PR A 1 H4AB H 0.8700 0.8961 0.3730 0.037 Uiso 0.842(6) 1 calc PR A 1 H4BC H 0.8500 0.9190 0.3931 0.037 Uiso 0.158(6) 1 calc PR A 2 H4BD H 0.8205 0.8442 0.4640 0.037 Uiso 0.158(6) 1 calc PR A 2 C5 C 0.8309(5) 0.8931(5) 0.4975(3) 0.0226(11) Uani 0.842(6) 1 d P A 1 H5A H 0.7910 0.9680 0.5069 0.034 Uiso 0.842(6) 1 calc PR A 1 H5B H 0.9211 0.9185 0.5221 0.034 Uiso 0.842(6) 1 calc PR A 1 H5C H 0.7835 0.8318 0.5254 0.034 Uiso 0.842(6) 1 calc PR A 1 C3 C 0.3325(5) 0.8278(6) 0.3607(4) 0.0336(14) Uani 0.842(6) 1 d P A 1 H3A H 0.3582 0.7462 0.3569 0.050 Uiso 0.842(6) 1 calc PR A 1 H3B H 0.2428 0.8130 0.3361 0.050 Uiso 0.842(6) 1 calc PR A 1 H3C H 0.3396 0.8758 0.4211 0.050 Uiso 0.842(6) 1 calc PR A 1 C4A C 0.336(3) 0.993(3) 0.308(2) 0.0336(14) Uani 0.158(6) 1 d P A 2 H4AC H 0.3291 1.0418 0.3666 0.050 Uiso 0.158(6) 1 calc PR A 2 H4AD H 0.2501 0.9459 0.2817 0.050 Uiso 0.158(6) 1 calc PR A 2 H4AE H 0.3724 1.0500 0.2739 0.050 Uiso 0.158(6) 1 calc PR A 2 C5A C 0.935(2) 0.778(3) 0.3832(17) 0.0226(11) Uani 0.158(6) 1 d P A 2 H5AA H 0.9161 0.6897 0.3865 0.034 Uiso 0.158(6) 1 calc PR A 2 H5AB H 1.0082 0.8256 0.4251 0.034 Uiso 0.158(6) 1 calc PR A 2 H5AC H 0.9578 0.7808 0.3252 0.034 Uiso 0.158(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn2 0.01338(19) 0.01585(18) 0.0191(2) 0.00305(15) 0.00460(15) -0.00020(14) Cl5 0.0187(5) 0.0207(5) 0.0253(5) 0.0038(4) 0.0070(4) 0.0044(4) Cl6 0.0186(5) 0.0181(4) 0.0291(5) 0.0046(4) 0.0040(4) -0.0019(4) Cl4 0.0186(5) 0.0273(5) 0.0229(5) 0.0073(4) 0.0030(4) 0.0011(4) Sn1 0.0170(2) 0.01639(18) 0.0188(2) 0.00567(15) 0.00249(15) 0.00088(14) Cl2 0.0210(5) 0.0194(4) 0.0234(5) 0.0054(4) 0.0063(4) 0.0019(4) Cl1 0.0213(5) 0.0331(5) 0.0251(5) 0.0111(4) -0.0002(4) 0.0014(4) Cl3 0.0297(6) 0.0174(4) 0.0299(6) 0.0058(4) 0.0085(5) 0.0004(4) P4 0.0147(5) 0.0112(4) 0.0175(5) 0.0038(4) 0.0027(4) 0.0025(3) P1 0.0166(5) 0.0117(4) 0.0156(5) 0.0022(4) 0.0014(4) 0.0032(4) P3 0.0223(5) 0.0180(5) 0.0174(5) 0.0071(4) 0.0024(4) 0.0045(4) P2 0.0271(6) 0.0185(5) 0.0193(5) 0.0061(4) 0.0088(4) 0.0080(4) C19 0.0183(19) 0.0156(17) 0.0166(19) 0.0009(15) 0.0038(16) 0.0020(15) C1 0.0173(19) 0.0126(16) 0.0159(19) 0.0030(14) 0.0019(15) 0.0036(14) C23 0.018(2) 0.0188(19) 0.026(2) 0.0070(16) 0.0051(17) 0.0060(15) C29 0.024(2) 0.0134(18) 0.027(2) 0.0028(16) 0.0053(18) 0.0036(15) C24 0.0158(19) 0.0150(18) 0.025(2) 0.0031(16) 0.0018(16) 0.0062(15) C18 0.0130(18) 0.0144(17) 0.020(2) 0.0023(15) 0.0040(15) 0.0031(14) C25 0.018(2) 0.027(2) 0.053(3) 0.013(2) 0.011(2) 0.0091(18) C6 0.0133(18) 0.0140(17) 0.020(2) 0.0057(15) 0.0040(15) 0.0021(14) C21 0.016(2) 0.022(2) 0.033(2) -0.0040(18) -0.0009(18) 0.0044(16) C7 0.021(2) 0.023(2) 0.018(2) 0.0013(16) 0.0017(17) 0.0039(16) C11 0.023(2) 0.0139(17) 0.021(2) 0.0027(15) 0.0023(17) 0.0030(15) C12 0.023(2) 0.0146(17) 0.019(2) 0.0029(15) -0.0042(16) 0.0046(15) C26 0.026(3) 0.045(3) 0.078(4) 0.025(3) 0.025(3) 0.020(2) C8 0.022(2) 0.035(2) 0.023(2) 0.0062(19) -0.0024(18) 0.0029(18) C22 0.017(2) 0.020(2) 0.039(3) 0.0069(18) 0.0082(19) 0.0013(16) C27 0.031(3) 0.033(3) 0.065(4) 0.015(3) 0.014(3) 0.022(2) C13 0.026(2) 0.020(2) 0.023(2) 0.0008(17) -0.0027(18) -0.0015(17) C15 0.037(3) 0.020(2) 0.047(3) 0.000(2) -0.016(2) -0.002(2) C17 0.035(3) 0.019(2) 0.024(2) -0.0020(17) 0.000(2) 0.0061(18) C10 0.029(2) 0.021(2) 0.032(2) 0.0107(18) 0.009(2) 0.0096(18) C16 0.053(3) 0.028(2) 0.027(3) -0.010(2) -0.012(2) 0.009(2) C9 0.021(2) 0.037(2) 0.031(3) 0.015(2) 0.0029(19) 0.0108(19) C20 0.024(2) 0.025(2) 0.020(2) 0.0007(17) 0.0006(17) 0.0064(17) C28 0.034(3) 0.017(2) 0.040(3) 0.0082(19) 0.007(2) 0.0109(18) C14 0.025(2) 0.025(2) 0.041(3) 0.003(2) -0.005(2) -0.0043(18) C2 0.025(2) 0.035(2) 0.027(2) 0.014(2) 0.0116(19) 0.0147(19) C4 0.019(2) 0.044(3) 0.029(3) 0.011(2) 0.0022(19) 0.008(2) C5 0.016(2) 0.034(3) 0.014(2) 0.002(2) -0.0038(18) 0.000(2) C3 0.016(3) 0.052(4) 0.039(3) 0.024(3) 0.011(2) 0.004(2) C4A 0.016(3) 0.052(4) 0.039(3) 0.024(3) 0.011(2) 0.004(2) C5A 0.016(2) 0.034(3) 0.014(2) 0.002(2) -0.0038(18) 0.000(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 Sn2 Cl5 2.4238(10) . ? Sn2 Cl5 2.4238(10) 2 ? Sn2 Cl6 2.4478(9) 2 ? Sn2 Cl6 2.4478(9) . ? Sn2 Cl4 2.4281(11) . ? Sn2 Cl4 2.4282(11) 2 ? Sn1 Cl2 2.4349(10) . ? Sn1 Cl2 2.4349(10) 2_666 ? Sn1 Cl1 2.4336(11) 2_666 ? Sn1 Cl1 2.4337(11) . ? Sn1 Cl3 2.4405(10) . ? Sn1 Cl3 2.4405(10) 2_666 ? P4 P3 2.1907(15) . ? P4 C1 1.823(4) . ? P4 C24 1.792(4) . ? P4 C18 1.801(4) . ? P1 P2 2.2056(14) . ? P1 C1 1.829(4) . ? P1 C6 1.791(4) . ? P1 C12 1.800(4) . ? P3 P2 2.2044(15) . ? P3 C4 1.872(5) . ? P2 C2 1.854(5) . ? C19 C18 1.396(6) . ? C19 C20 1.395(6) . ? C23 C18 1.405(5) . ? C23 C22 1.385(6) . ? C29 C24 1.403(5) . ? C29 C28 1.370(6) . ? C24 C25 1.385(6) . ? C25 C26 1.387(7) . ? C6 C7 1.386(6) . ? C6 C11 1.399(5) . ? C21 C22 1.385(7) . ? C21 C20 1.383(6) . ? C7 C8 1.384(6) . ? C11 C10 1.383(6) . ? C12 C13 1.388(6) . ? C12 C17 1.391(6) . ? C26 C27 1.375(7) . ? C8 C9 1.383(6) . ? C27 C28 1.390(7) . ? C13 C14 1.391(6) . ? C15 C16 1.383(8) . ? C15 C14 1.385(7) . ? C17 C16 1.389(6) . ? C10 C9 1.382(7) . ? C2 C3 1.520(6) . ? C2 C4A 1.46(3) . ? C4 C5 1.522(7) . ? C4 C5A 1.41(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl5 Sn2 Cl5 180.0 2 . ? Cl5 Sn2 Cl6 89.92(3) 2 2 ? Cl5 Sn2 Cl6 89.92(3) . . ? Cl5 Sn2 Cl6 90.08(3) . 2 ? Cl5 Sn2 Cl6 90.08(3) 2 . ? Cl5 Sn2 Cl4 89.24(4) 2 . ? Cl5 Sn2 Cl4 90.76(4) . . ? Cl5 Sn2 Cl4 90.76(4) 2 2 ? Cl5 Sn2 Cl4 89.24(4) . 2 ? Cl6 Sn2 Cl6 180.0 2 . ? Cl4 Sn2 Cl6 89.60(3) 2 . ? Cl4 Sn2 Cl6 90.40(3) . . ? Cl4 Sn2 Cl6 90.40(3) 2 2 ? Cl4 Sn2 Cl6 89.60(3) . 2 ? Cl4 Sn2 Cl4 180.0 . 2 ? Cl2 Sn1 Cl2 180.0 . 2_666 ? Cl2 Sn1 Cl3 91.09(3) 2_666 . ? Cl2 Sn1 Cl3 88.91(3) . . ? Cl2 Sn1 Cl3 91.09(3) . 2_666 ? Cl2 Sn1 Cl3 88.91(3) 2_666 2_666 ? Cl1 Sn1 Cl2 89.11(4) 2_666 . ? Cl1 Sn1 Cl2 90.89(4) . . ? Cl1 Sn1 Cl2 89.11(4) . 2_666 ? Cl1 Sn1 Cl2 90.89(4) 2_666 2_666 ? Cl1 Sn1 Cl1 180.0 2_666 . ? Cl1 Sn1 Cl3 90.93(4) . . ? Cl1 Sn1 Cl3 90.93(4) 2_666 2_666 ? Cl1 Sn1 Cl3 89.07(4) . 2_666 ? Cl1 Sn1 Cl3 89.07(4) 2_666 . ? Cl3 Sn1 Cl3 180.000(1) 2_666 . ? C1 P4 P3 108.88(13) . . ? C24 P4 P3 110.55(15) . . ? C24 P4 C1 110.77(18) . . ? C24 P4 C18 108.17(18) . . ? C18 P4 P3 108.17(13) . . ? C18 P4 C1 110.26(18) . . ? C1 P1 P2 110.15(13) . . ? C6 P1 P2 109.16(13) . . ? C6 P1 C1 110.52(18) . . ? C6 P1 C12 110.97(18) . . ? C12 P1 P2 106.44(14) . . ? C12 P1 C1 109.51(19) . . ? P4 P3 P2 96.69(5) . . ? C4 P3 P4 96.99(16) . . ? C4 P3 P2 100.84(17) . . ? P3 P2 P1 99.27(6) . . ? C2 P2 P1 102.14(15) . . ? C2 P2 P3 104.45(15) . . ? C20 C19 C18 119.4(4) . . ? P4 C1 P1 111.4(2) . . ? C22 C23 C18 119.3(4) . . ? C28 C29 C24 120.3(4) . . ? C29 C24 P4 116.5(3) . . ? C25 C24 P4 123.4(3) . . ? C25 C24 C29 120.0(4) . . ? C19 C18 P4 120.6(3) . . ? C19 C18 C23 120.2(4) . . ? C23 C18 P4 119.0(3) . . ? C24 C25 C26 118.6(4) . . ? C7 C6 P1 122.3(3) . . ? C7 C6 C11 120.9(4) . . ? C11 C6 P1 116.2(3) . . ? C20 C21 C22 120.4(4) . . ? C8 C7 C6 119.9(4) . . ? C10 C11 C6 118.3(4) . . ? C13 C12 P1 119.6(3) . . ? C13 C12 C17 120.9(4) . . ? C17 C12 P1 119.3(3) . . ? C27 C26 C25 121.5(5) . . ? C9 C8 C7 119.5(4) . . ? C23 C22 C21 120.4(4) . . ? C26 C27 C28 119.7(4) . . ? C12 C13 C14 119.6(4) . . ? C16 C15 C14 120.3(4) . . ? C16 C17 C12 118.7(5) . . ? C9 C10 C11 120.9(4) . . ? C15 C16 C17 120.7(5) . . ? C10 C9 C8 120.5(4) . . ? C21 C20 C19 120.1(4) . . ? C29 C28 C27 119.8(4) . . ? C15 C14 C13 119.7(5) . . ? C3 C2 P2 109.1(3) . . ? C4A C2 P2 123.0(13) . . ? C4A C2 C3 94.8(11) . . ? C5 C4 P3 111.5(3) . . ? C5A C4 P3 128.6(11) . . ? C5A C4 C5 109.9(11) . . ?