Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global #====================================================================== _publ_contact_author K.Dillon _publ_contact_author_email K.B.DILLON@DURHAM.AC.UK _publ_contact_author_address ; Chemistry Department University of Durham South Road Durham DH1 3LE UNITED KINGDOM ; loop_ _publ_author_name _publ_author_address 'Keith B. Dillon' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; 'Goeta, Andres E.' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; 'Judith A. K. Howard' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; 'Philippa K. Monks' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; 'Helena J. Shepherd' ; Department of Chemistry, University of Durham, South Rd., Durham. DH1 3LE ; 'Thompson, Amber L.' ; Department of Chemical Crystallography, Chemistry Research Laboratory, University of Oxford, Oxford. OX1 3TA ; _journal_coden_Cambridge 222 _journal_name_full 'Dalton Transactions' _publ_section_title ; Alkyl and Aryl Dicationic Derivatives of Cyclic Triphosphenium Ions ; #====================================================================== data_1c _database_code_depnum_ccdc_archive 'CCDC 664568' #====================================================================== _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C12 H29 P3, Al Cl4, Cl' _chemical_formula_sum 'C12 H29 Al Cl5 P3' _chemical_formula_weight 470.49 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 Cc _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' _cell_length_a 10.1314(4) _cell_length_b 25.1148(11) _cell_length_c 8.8636(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.9570(10) _cell_angle_gamma 90.00 _cell_volume 2255.01(17) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9201 _cell_measurement_theta_min 2.168 _cell_measurement_theta_max 28.330 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method . _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.879 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0390 before and 0.0288 after correction. The Ratio of minimum to maximum transmission is 0.879. The \l/2 correction factor is 0.0000 ; _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 (20.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.424 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 1K CCD area detector' _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 13735 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5601 _reflns_number_gt 5338 _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, 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. Refinement included an inversion twin, with a batch scale factor of 0.4728 ; _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^)+(0.0317P)^2^+2.1417P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(12) _refine_ls_number_reflns 5601 _refine_ls_number_parameters 196 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P3 P -0.05711(6) -0.10136(3) -0.46758(7) 0.01507(13) Uani 1 1 d . . . P1 P -0.26872(6) -0.07982(3) -0.47202(7) 0.01607(13) Uani 1 1 d . . . Cl1 Cl -0.17460(7) 0.05192(3) -0.29482(7) 0.02312(14) Uani 1 1 d . . . P2 P -0.28078(7) -0.09661(3) -0.22527(7) 0.01624(13) Uani 1 1 d . . . Cl3 Cl -0.63733(7) -0.23383(3) 0.15291(8) 0.02428(14) Uani 1 1 d . . . Cl5 Cl -0.96288(7) -0.21808(3) 0.02560(8) 0.02953(16) Uani 1 1 d . . . Al1 Al -0.76641(9) -0.18882(3) 0.00792(10) 0.02253(18) Uani 1 1 d . . . Cl4 Cl -0.69791(8) -0.19756(4) -0.21663(9) 0.0431(2) Uani 1 1 d . . . Cl2 Cl -0.76235(11) -0.10673(3) 0.07053(13) 0.0488(2) Uani 1 1 d . . . C3 C -0.3456(3) -0.14069(11) -0.5559(3) 0.0230(6) Uani 1 1 d . . . H3A H -0.3118 -0.1466 -0.6562 0.034 Uiso 1 1 calc R . . H3B H -0.3240 -0.1715 -0.4942 0.034 Uiso 1 1 calc R . . C11 C -0.0182(3) -0.15437(11) -0.5984(3) 0.0222(6) Uani 1 1 d . . . H11B H -0.0826 -0.1827 -0.5882 0.033 Uiso 1 1 calc R . . H11A H -0.0254 -0.1408 -0.7006 0.033 Uiso 1 1 calc R . . C7 C -0.3400(3) -0.16186(11) -0.1732(3) 0.0227(6) Uani 1 1 d . . . H7A H -0.4287 -0.1667 -0.2135 0.034 Uiso 1 1 calc R . . H7B H -0.2840 -0.1888 -0.2176 0.034 Uiso 1 1 calc R . . C5 C -0.3796(3) -0.04566(11) -0.1391(3) 0.0228(6) Uani 1 1 d . . . H5A H -0.3827 -0.0522 -0.0313 0.034 Uiso 1 1 calc R . . H5B H -0.3376 -0.0114 -0.1539 0.034 Uiso 1 1 calc R . . C1 C -0.1093(2) -0.09028(10) -0.1668(3) 0.0171(5) Uani 1 1 d . . . H1B H -0.0823 -0.0532 -0.1705 0.026 Uiso 1 1 calc R . . H1A H -0.0973 -0.1030 -0.0641 0.026 Uiso 1 1 calc R . . C9 C 0.0401(3) -0.04195(11) -0.4994(3) 0.0226(6) Uani 1 1 d . . . H9A H 0.0500 -0.0374 -0.6073 0.034 Uiso 1 1 calc R . . H9B H -0.0086 -0.0115 -0.4625 0.034 Uiso 1 1 calc R . . C12 C 0.1185(4) -0.17712(15) -0.5733(4) 0.0373(8) Uani 1 1 d . . . H12A H 0.1283 -0.1886 -0.4704 0.056 Uiso 1 1 calc R . . H12C H 0.1832 -0.1503 -0.5941 0.056 Uiso 1 1 calc R . . H12B H 0.1308 -0.2069 -0.6394 0.056 Uiso 1 1 calc R . . C2 C -0.0254(3) -0.12385(10) -0.2754(3) 0.0179(5) Uani 1 1 d . . . H2A H -0.0483 -0.1612 -0.2662 0.027 Uiso 1 1 calc R . . H2B H 0.0676 -0.1198 -0.2501 0.027 Uiso 1 1 calc R . . C6 C -0.5199(3) -0.04342(14) -0.2027(4) 0.0341(7) Uani 1 1 d . . . H6B H -0.5175 -0.0392 -0.3102 0.051 Uiso 1 1 calc R . . H6C H -0.5655 -0.0138 -0.1593 0.051 Uiso 1 1 calc R . . H6A H -0.5652 -0.0758 -0.1786 0.051 Uiso 1 1 calc R . . C8 C -0.3410(4) -0.16950(14) -0.0027(4) 0.0355(7) Uani 1 1 d . . . H8B H -0.3989 -0.1438 0.0414 0.053 Uiso 1 1 calc R . . H8C H -0.2532 -0.1648 0.0377 0.053 Uiso 1 1 calc R . . H8A H -0.3714 -0.2047 0.0202 0.053 Uiso 1 1 calc R . . C10 C 0.1767(3) -0.04185(15) -0.4252(6) 0.0510(11) Uani 1 1 d . . . H10A H 0.1682 -0.0422 -0.3175 0.076 Uiso 1 1 calc R . . H10C H 0.2236 -0.0104 -0.4550 0.076 Uiso 1 1 calc R . . H10B H 0.2245 -0.0729 -0.4565 0.076 Uiso 1 1 calc R . . C4 C -0.4951(3) -0.13313(14) -0.5641(4) 0.0328(7) Uani 1 1 d . . . H4C H -0.5349 -0.1629 -0.6152 0.049 Uiso 1 1 calc R . . H4A H -0.5155 -0.1010 -0.6185 0.049 Uiso 1 1 calc R . . H4B H -0.5290 -0.1307 -0.4639 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P3 0.0156(3) 0.0143(3) 0.0153(3) 0.0004(2) 0.0020(2) 0.0009(2) P1 0.0164(3) 0.0173(3) 0.0145(3) -0.0002(2) 0.0000(2) 0.0001(2) Cl1 0.0301(3) 0.0235(3) 0.0157(3) 0.0004(2) 0.0005(2) -0.0037(3) P2 0.0173(3) 0.0159(3) 0.0156(3) -0.0011(3) 0.0021(2) -0.0013(2) Cl3 0.0241(3) 0.0213(3) 0.0272(3) 0.0033(3) -0.0037(3) 0.0015(2) Cl5 0.0221(3) 0.0375(4) 0.0290(4) 0.0031(3) -0.0001(3) -0.0007(3) Al1 0.0232(4) 0.0222(4) 0.0222(4) 0.0043(3) 0.0005(3) 0.0025(3) Cl4 0.0277(4) 0.0793(6) 0.0226(4) 0.0065(4) 0.0043(3) 0.0040(4) Cl2 0.0610(6) 0.0186(4) 0.0667(6) 0.0039(4) 0.0005(5) 0.0018(4) C3 0.0256(14) 0.0228(14) 0.0204(13) -0.0035(11) -0.0031(11) -0.0058(11) C11 0.0273(14) 0.0214(13) 0.0180(13) -0.0021(11) 0.0012(10) 0.0054(11) C7 0.0260(14) 0.0157(12) 0.0267(15) 0.0007(11) 0.0050(11) -0.0052(10) C5 0.0270(14) 0.0203(13) 0.0215(14) -0.0064(11) 0.0073(11) 0.0051(11) C1 0.0159(12) 0.0208(13) 0.0146(12) -0.0015(10) -0.0003(9) -0.0022(9) C9 0.0237(13) 0.0183(12) 0.0258(15) 0.0047(11) 0.0032(11) -0.0027(11) C12 0.0423(19) 0.0426(19) 0.0269(17) -0.0098(14) -0.0038(14) 0.0197(15) C2 0.0210(12) 0.0174(12) 0.0154(12) -0.0003(9) 0.0017(10) 0.0023(10) C6 0.0252(15) 0.0352(18) 0.0422(19) -0.0076(14) 0.0060(13) 0.0048(13) C8 0.0404(19) 0.0384(18) 0.0280(16) 0.0103(14) 0.0057(14) -0.0140(15) C10 0.0251(17) 0.0320(18) 0.095(3) 0.013(2) -0.0137(19) -0.0071(14) C4 0.0282(16) 0.0378(18) 0.0323(17) -0.0062(14) -0.0052(13) -0.0067(13) _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 P3 C9 1.812(3) . ? P3 C11 1.813(3) . ? P3 C2 1.818(3) . ? P3 P1 2.2108(9) . ? P1 C3 1.864(3) . ? P1 P2 2.2327(9) . ? P2 C5 1.802(3) . ? P2 C7 1.808(3) . ? P2 C1 1.812(3) . ? Cl3 Al1 2.1410(11) . ? Cl5 Al1 2.1300(11) . ? Al1 Cl4 2.1302(12) . ? Al1 Cl2 2.1351(12) . ? C3 C4 1.527(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C11 C12 1.511(4) . ? C11 H11B 0.9700 . ? C11 H11A 0.9700 . ? C7 C8 1.523(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C5 C6 1.522(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C1 C2 1.545(4) . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C9 C10 1.523(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12C 0.9600 . ? C12 H12B 0.9600 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C6 H6A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8A 0.9600 . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C10 H10B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? 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 C9 P3 C11 112.38(14) . . ? C9 P3 C2 108.28(13) . . ? C11 P3 C2 109.51(12) . . ? C9 P3 P1 108.96(10) . . ? C11 P3 P1 112.91(10) . . ? C2 P3 P1 104.42(9) . . ? C3 P1 P3 101.83(10) . . ? C3 P1 P2 101.90(10) . . ? P3 P1 P2 90.30(3) . . ? C5 P2 C7 110.27(14) . . ? C5 P2 C1 110.67(13) . . ? C7 P2 C1 109.09(13) . . ? C5 P2 P1 108.73(10) . . ? C7 P2 P1 116.45(10) . . ? C1 P2 P1 101.28(9) . . ? Cl5 Al1 Cl4 110.65(5) . . ? Cl5 Al1 Cl2 109.15(5) . . ? Cl4 Al1 Cl2 109.71(5) . . ? Cl5 Al1 Cl3 109.62(5) . . ? Cl4 Al1 Cl3 107.52(5) . . ? Cl2 Al1 Cl3 110.18(5) . . ? C4 C3 P1 108.9(2) . . ? C4 C3 H3A 109.9 . . ? P1 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? P1 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C12 C11 P3 113.1(2) . . ? C12 C11 H11B 109.0 . . ? P3 C11 H11B 109.0 . . ? C12 C11 H11A 109.0 . . ? P3 C11 H11A 109.0 . . ? H11B C11 H11A 107.8 . . ? C8 C7 P2 112.0(2) . . ? C8 C7 H7A 109.2 . . ? P2 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? P2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C6 C5 P2 113.0(2) . . ? C6 C5 H5A 109.0 . . ? P2 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? P2 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C2 C1 P2 107.98(18) . . ? C2 C1 H1B 110.1 . . ? P2 C1 H1B 110.1 . . ? C2 C1 H1A 110.1 . . ? P2 C1 H1A 110.1 . . ? H1B C1 H1A 108.4 . . ? C10 C9 P3 115.2(2) . . ? C10 C9 H9A 108.5 . . ? P3 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? P3 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C1 C2 P3 108.90(18) . . ? C1 C2 H2A 109.9 . . ? P3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? P3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C3 C4 H4C 109.5 . . ? C3 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.418 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.073 #====================================================================== data_1d _database_code_depnum_ccdc_archive 'CCDC 664569' #====================================================================== _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C13 H31 P3, Al Cl4, Cl' _chemical_formula_sum 'C13 H31 Al Cl5 P3' _chemical_formula_weight 484.52 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 Cc _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' _cell_length_a 10.3722(3) _cell_length_b 25.1650(8) _cell_length_c 8.8229(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.5020(10) _cell_angle_gamma 90.00 _cell_volume 2302.83(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8175 _cell_measurement_theta_min 2.820 _cell_measurement_theta_max 31.250 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method . _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0464 before and 0.0311 after correction. The Ratio of minimum to maximum transmission is 0.831035. The \l/2 correction factor is 0.0000 ; _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 (5.00 s exposure) covering -0.300\ degrees in \w. The crystal to detector distance was 4.424 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 1K CCD area detector' _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 19257 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 31.52 _reflns_number_total 7542 _reflns_number_gt 6799 _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 '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. Refinement included an inversion twin, with a batch scale factor of 0.1630 ; _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^)+(0.0275P)^2^+2.6336P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(8) _refine_ls_number_reflns 7542 _refine_ls_number_parameters 205 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P3 P 0.19681(5) 0.39862(2) 0.32708(6) 0.01602(10) Uani 1 1 d . . . P2 P 0.41450(5) 0.39984(2) 0.08174(6) 0.01654(10) Uani 1 1 d . . . P1 P 0.40361(5) 0.41985(2) 0.32754(6) 0.01641(10) Uani 1 1 d . . . Cl1 Cl 0.31113(6) 0.54924(2) 0.14622(6) 0.02354(11) Uani 1 1 d . . . Cl5 Cl 1.09738(6) 0.27676(2) -0.15760(7) 0.02786(12) Uani 1 1 d . . . Cl3 Cl 0.77695(5) 0.27341(2) -0.28590(7) 0.02529(12) Uani 1 1 d . . . Cl2 Cl 0.83874(7) 0.30061(3) 0.08913(7) 0.03519(15) Uani 1 1 d . . . Cl4 Cl 0.92897(7) 0.39417(2) -0.18243(8) 0.03255(14) Uani 1 1 d . . . Al1 Al 0.91094(7) 0.31117(3) -0.13460(8) 0.02024(14) Uani 1 1 d . . . C2 C 0.1661(2) 0.37465(9) 0.1353(2) 0.0190(4) Uani 1 1 d . . . H2A H 0.1887 0.3373 0.1283 0.029 Uiso 1 1 calc R . . H2B H 0.0753 0.3784 0.1104 0.029 Uiso 1 1 calc R . . C1 C 0.2470(2) 0.40704(9) 0.0238(3) 0.0193(4) Uani 1 1 d . . . H1B H 0.2218 0.4441 0.0264 0.029 Uiso 1 1 calc R . . H1A H 0.2347 0.3938 -0.0786 0.029 Uiso 1 1 calc R . . C10 C 0.0999(2) 0.45772(9) 0.3557(3) 0.0222(4) Uani 1 1 d . . . H10A H 0.0813 0.4609 0.4629 0.033 Uiso 1 1 calc R . . H10B H 0.1502 0.4885 0.3268 0.033 Uiso 1 1 calc R . . C6 C 0.5157(2) 0.44805(9) -0.0105(3) 0.0239(5) Uani 1 1 d . . . H6A H 0.5113 0.4426 -0.1193 0.036 Uiso 1 1 calc R . . H6B H 0.4838 0.4835 0.0108 0.036 Uiso 1 1 calc R . . C12 C 0.1589(2) 0.34652(9) 0.4602(3) 0.0226(4) Uani 1 1 d . . . H12A H 0.2172 0.3169 0.4445 0.034 Uiso 1 1 calc R . . H12B H 0.1728 0.3596 0.5624 0.034 Uiso 1 1 calc R . . C4 C 0.6234(3) 0.36351(10) 0.4229(3) 0.0281(5) Uani 1 1 d . . . H4A H 0.6585 0.3309 0.4646 0.042 Uiso 1 1 calc R . . H4B H 0.6562 0.3675 0.3209 0.042 Uiso 1 1 calc R . . C3 C 0.4753(2) 0.35898(9) 0.4152(3) 0.0227(4) Uani 1 1 d . . . H3B H 0.4417 0.3544 0.5167 0.034 Uiso 1 1 calc R . . H3A H 0.4512 0.3281 0.3558 0.034 Uiso 1 1 calc R . . C8 C 0.4683(2) 0.33358(9) 0.0342(3) 0.0232(5) Uani 1 1 d . . . H8B H 0.5557 0.3286 0.0714 0.035 Uiso 1 1 calc R . . H8A H 0.4137 0.3077 0.0840 0.035 Uiso 1 1 calc R . . C9 C 0.4643(3) 0.32395(11) -0.1369(3) 0.0333(6) Uani 1 1 d . . . H9C H 0.5217 0.3483 -0.1860 0.050 Uiso 1 1 calc R . . H9B H 0.3781 0.3294 -0.1743 0.050 Uiso 1 1 calc R . . H9A H 0.4907 0.2881 -0.1578 0.050 Uiso 1 1 calc R . . C13 C 0.0207(3) 0.32697(12) 0.4447(3) 0.0340(6) Uani 1 1 d . . . H13A H 0.0045 0.3163 0.3418 0.051 Uiso 1 1 calc R . . H13C H -0.0374 0.3551 0.4714 0.051 Uiso 1 1 calc R . . H13B H 0.0079 0.2972 0.5110 0.051 Uiso 1 1 calc R . . C11 C -0.0287(2) 0.45850(10) 0.2661(4) 0.0311(6) Uani 1 1 d . . . H11B H -0.0113 0.4583 0.1594 0.047 Uiso 1 1 calc R . . H11C H -0.0761 0.4900 0.2915 0.047 Uiso 1 1 calc R . . H11A H -0.0785 0.4277 0.2918 0.047 Uiso 1 1 calc R . . C5 C 0.6699(3) 0.40997(12) 0.5187(4) 0.0371(6) Uani 1 1 d . . . H5C H 0.7622 0.4091 0.5263 0.056 Uiso 1 1 calc R . . H5A H 0.6336 0.4075 0.6182 0.056 Uiso 1 1 calc R . . H5B H 0.6431 0.4427 0.4722 0.056 Uiso 1 1 calc R . . C7 C 0.6565(3) 0.44373(12) 0.0429(4) 0.0425(8) Uani 1 1 d . . . H7B H 0.6627 0.4538 0.1477 0.064 Uiso 1 1 calc R . . H7C H 0.7092 0.4669 -0.0167 0.064 Uiso 1 1 calc R . . H7A H 0.6856 0.4078 0.0313 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P3 0.0174(3) 0.0150(2) 0.0156(2) -0.00026(18) 0.00098(19) -0.00095(19) P2 0.0179(2) 0.0155(2) 0.0162(2) 0.00064(19) 0.00198(19) 0.0014(2) P1 0.0176(2) 0.0155(2) 0.0161(2) 0.00012(19) -0.00108(19) 0.00045(19) Cl1 0.0299(3) 0.0223(2) 0.0184(2) 0.00084(19) 0.0006(2) 0.0028(2) Cl5 0.0221(3) 0.0258(3) 0.0357(3) -0.0011(2) -0.0009(2) 0.0035(2) Cl3 0.0242(3) 0.0244(3) 0.0272(3) -0.0019(2) -0.0042(2) -0.0023(2) Cl2 0.0320(3) 0.0510(4) 0.0226(3) 0.0012(3) 0.0029(2) -0.0012(3) Cl4 0.0399(4) 0.0174(2) 0.0402(4) 0.0003(2) -0.0086(3) 0.0002(2) Al1 0.0213(3) 0.0177(3) 0.0217(3) -0.0008(2) -0.0014(3) 0.0009(2) C2 0.0188(10) 0.0202(10) 0.0181(10) -0.0018(7) -0.0018(8) -0.0031(8) C1 0.0198(10) 0.0211(10) 0.0168(10) 0.0007(8) -0.0018(8) 0.0021(8) C10 0.0226(11) 0.0179(9) 0.0261(11) -0.0046(8) 0.0001(9) 0.0024(8) C6 0.0262(12) 0.0204(10) 0.0253(12) 0.0032(9) 0.0059(9) -0.0009(9) C12 0.0291(12) 0.0199(10) 0.0188(10) 0.0025(8) 0.0016(8) -0.0049(9) C4 0.0289(13) 0.0286(12) 0.0268(12) -0.0001(9) -0.0070(10) 0.0098(10) C3 0.0274(12) 0.0201(10) 0.0205(10) 0.0026(8) -0.0039(9) 0.0029(8) C8 0.0276(12) 0.0176(9) 0.0244(11) 0.0008(8) 0.0031(9) 0.0032(8) C9 0.0419(16) 0.0320(13) 0.0260(13) -0.0072(10) 0.0029(11) 0.0093(11) C13 0.0359(15) 0.0375(14) 0.0287(14) 0.0082(11) -0.0005(11) -0.0172(12) C11 0.0209(12) 0.0248(11) 0.0474(16) -0.0022(11) -0.0049(11) 0.0033(9) C5 0.0261(13) 0.0384(15) 0.0466(17) -0.0081(13) -0.0095(12) 0.0017(11) C7 0.0215(13) 0.0317(14) 0.074(2) 0.0169(14) 0.0082(13) 0.0017(10) _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 P3 C12 1.806(2) . ? P3 C10 1.814(2) . ? P3 C2 1.822(2) . ? P3 P1 2.2105(8) . ? P2 C6 1.803(2) . ? P2 C8 1.809(2) . ? P2 C1 1.815(2) . ? P2 P1 2.2302(8) . ? P1 C3 1.867(2) . ? Cl5 Al1 2.1302(9) . ? Cl3 Al1 2.1411(9) . ? Cl2 Al1 2.1340(9) . ? Cl4 Al1 2.1393(9) . ? C2 C1 1.533(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C1 H1B 0.9700 . ? C1 H1A 0.9700 . ? C10 C11 1.545(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C6 C7 1.535(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C12 C13 1.520(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C4 C5 1.519(4) . ? C4 C3 1.541(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 H3B 0.9700 . ? C3 H3A 0.9700 . ? C8 C9 1.529(4) . ? C8 H8B 0.9700 . ? C8 H8A 0.9700 . ? C9 H9C 0.9600 . ? C9 H9B 0.9600 . ? C9 H9A 0.9600 . ? C13 H13A 0.9600 . ? C13 H13C 0.9600 . ? C13 H13B 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11 H11A 0.9600 . ? C5 H5C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C7 H7A 0.9600 . ? 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 C12 P3 C10 112.38(12) . . ? C12 P3 C2 109.04(11) . . ? C10 P3 C2 107.97(11) . . ? C12 P3 P1 113.01(9) . . ? C10 P3 P1 109.90(8) . . ? C2 P3 P1 104.09(8) . . ? C6 P2 C8 109.49(11) . . ? C6 P2 C1 111.39(11) . . ? C8 P2 C1 108.83(11) . . ? C6 P2 P1 108.77(8) . . ? C8 P2 P1 116.88(8) . . ? C1 P2 P1 101.25(8) . . ? C3 P1 P3 100.69(8) . . ? C3 P1 P2 101.21(8) . . ? P3 P1 P2 90.06(3) . . ? Cl5 Al1 Cl2 111.33(4) . . ? Cl5 Al1 Cl4 107.29(4) . . ? Cl2 Al1 Cl4 109.64(4) . . ? Cl5 Al1 Cl3 110.18(4) . . ? Cl2 Al1 Cl3 106.87(4) . . ? Cl4 Al1 Cl3 111.58(4) . . ? C1 C2 P3 109.14(15) . . ? C1 C2 H2A 109.9 . . ? P3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? P3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 C1 P2 107.09(15) . . ? C2 C1 H1B 110.3 . . ? P2 C1 H1B 110.3 . . ? C2 C1 H1A 110.3 . . ? P2 C1 H1A 110.3 . . ? H1B C1 H1A 108.6 . . ? C11 C10 P3 114.58(17) . . ? C11 C10 H10A 108.6 . . ? P3 C10 H10A 108.6 . . ? C11 C10 H10B 108.6 . . ? P3 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C7 C6 P2 111.69(18) . . ? C7 C6 H6A 109.3 . . ? P2 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? P2 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C13 C12 P3 112.76(17) . . ? C13 C12 H12A 109.0 . . ? P3 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? P3 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C5 C4 C3 113.1(2) . . ? C5 C4 H4A 109.0 . . ? C3 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C3 P1 110.53(17) . . ? C4 C3 H3B 109.5 . . ? P1 C3 H3B 109.5 . . ? C4 C3 H3A 109.5 . . ? P1 C3 H3A 109.5 . . ? H3B C3 H3A 108.1 . . ? C9 C8 P2 111.69(17) . . ? C9 C8 H8B 109.3 . . ? P2 C8 H8B 109.3 . . ? C9 C8 H8A 109.3 . . ? P2 C8 H8A 109.3 . . ? H8B C8 H8A 107.9 . . ? C8 C9 H9C 109.5 . . ? C8 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? C8 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? C4 C5 H5C 109.5 . . ? C4 C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C7 H7A 109.5 . . ? H7B C7 H7A 109.5 . . ? H7C C7 H7A 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.52 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.445 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.071 #====================================================================== data_6c _database_code_depnum_ccdc_archive 'CCDC 664570' #====================================================================== _audit_creation_date 07-10-09 _audit_creation_method CRYSTALS_ver_12.85 _chemical_name_systematic . _chemical_melting_point 'not measured' _exptl_special_details ; The data collection nominally covered full sphere of reciprocal Space, by a combination of 3 sets of \w scans each set at different \f and/or 2\q angles and each scan (30s exposure) covering 0.3\% in \w. Crystal to detector distance 5.51 cm. ; _cell_length_a 22.8830(16) _cell_length_b 31.806(2) _cell_length_c 9.8121(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7141.4(8) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b a 2' _symmetry_space_group_name_Hall 'P 2 -2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z x+1/2,-y+1/2,z -x,-y,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C28 H29 Al2 Cl8 P3 # Dc = 1.48 Fooo = 3232.00 Mu = 8.35 M = 1592.09 # Found Formula = C28 H29 Al2 Cl8 P3 # Dc = 1.48 FOOO = 3232.00 Mu = 8.35 M = 1592.09 _chemical_formula_sum 'C28 H29 Al2 Cl8 P3' _chemical_formula_moiety 'C28 H29 P3, 2(Al Cl4)' _chemical_formula_weight 796.05 _cell_measurement_reflns_used 5282 _cell_measurement_theta_min 2.600 _cell_measurement_theta_max 27.470 _cell_measurement_temperature 120 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; Gaussian Integration (Busing and Levy, 1957) ; _exptl_absorpt_correction_T_min 0.8039 _exptl_absorpt_correction_T_max 0.9671 _diffrn_measurement_device 'Bruker SMART' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _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 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'Bruker SHELXTL' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 120 _diffrn_reflns_number 51876 _reflns_number_total 15890 _diffrn_reflns_av_R_equivalents 0.098 # Number of reflections with Friedels Law is 8746 # Number of reflections without Friedels Law is 15890 # Theoretical number of reflections is about 7482 _diffrn_reflns_theta_min 2.347 _diffrn_reflns_theta_max 28.298 _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.317 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min 0 _reflns_limit_h_max 29 _reflns_limit_k_min 0 _reflns_limit_k_max 42 _reflns_limit_l_min -12 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 1.58 _oxford_diffrn_Wilson_scale 176.60 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.79 _refine_diff_density_max 0.72 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 14723 _refine_ls_number_restraints 1 _refine_ls_number_parameters 741 _oxford_refine_ls_R_factor_ref 0.1058 _refine_ls_wR_factor_ref 0.1313 _refine_ls_goodness_of_fit_ref 0.9473 _refine_ls_shift/su_max 0.000350 # The values computed from all data _oxford_reflns_number_all 14723 _refine_ls_R_factor_all 0.1058 _refine_ls_wR_factor_all 0.1313 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10238 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_gt 0.1120 _chemical_absolute_configuration unk _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.01P)^2^ +34.25P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Busing, W.R. & Levy, H.A., (1975). Acta Cryst 10, 180. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens P11 P 0.74134(10) 0.11225(8) 0.6734(2) 0.0193 1.0000 Uani . . . . . . . P12 P 0.81037(9) 0.15569(7) 0.5980(2) 0.0173 1.0000 Uani . . . . . . . P13 P 0.67465(9) 0.15468(7) 0.5885(2) 0.0165 1.0000 Uani . . . . . . . C101 C 0.7719(3) 0.1962(2) 0.4996(8) 0.0178 1.0000 Uani . . . . . . . H11 H 0.7682 0.2214 0.5576 0.0500 1.0000 Uiso R . . . . . . H229 H 0.7962 0.2035 0.4200 0.0500 1.0000 Uiso R . . . . . . C102 C 0.7118(3) 0.1827(3) 0.4519(8) 0.0203 1.0000 Uani . . . . . . . H12 H 0.7153 0.1642 0.3710 0.0500 1.0000 Uiso R . . . . . . H230 H 0.6886 0.2078 0.4253 0.0500 1.0000 Uiso R . . . . . . C103 C 0.7398(4) 0.0712(3) 0.5402(9) 0.0218 1.0000 Uani . . . . . . . H13 H 0.6995 0.0599 0.5302 0.0500 1.0000 Uiso R . . . . . . H231 H 0.7515 0.0833 0.4510 0.0500 1.0000 Uiso R . . . . . . C104 C 0.7810(4) 0.0359(3) 0.5775(10) 0.0306 1.0000 Uani . . . . . . . H14 H 0.7747 0.0118 0.5158 0.0500 1.0000 Uiso R . . . . . . H232 H 0.7738 0.0269 0.6714 0.0500 1.0000 Uiso R . . . . . . H233 H 0.8216 0.0455 0.5687 0.0500 1.0000 Uiso R . . . . . . C105 C 0.8637(3) 0.1286(3) 0.4985(9) 0.0195 1.0000 Uani . . . . . . . C106 C 0.9129(3) 0.1118(3) 0.5639(9) 0.0214 1.0000 Uani . . . . . . . H106 H 0.9175 0.1151 0.6599 0.0500 1.0000 Uiso R . . . . . . C107 C 0.9544(4) 0.0911(3) 0.4883(10) 0.0272 1.0000 Uani . . . . . . . H107 H 0.9883 0.0804 0.5321 0.0500 1.0000 Uiso R . . . . . . C108 C 0.9474(4) 0.0854(3) 0.3474(10) 0.0333 1.0000 Uani . . . . . . . H108 H 0.9758 0.0706 0.2967 0.0500 1.0000 Uiso R . . . . . . C109 C 0.8988(4) 0.1013(3) 0.2850(10) 0.0339 1.0000 Uani . . . . . . . H109 H 0.8935 0.0973 0.1905 0.0500 1.0000 Uiso R . . . . . . C110 C 0.8569(4) 0.1229(3) 0.3583(9) 0.0268 1.0000 Uani . . . . . . . H110 H 0.8233 0.1340 0.3130 0.0500 1.0000 Uiso R . . . . . . C111 C 0.8467(3) 0.1803(3) 0.7395(8) 0.0182 1.0000 Uani . . . . . . . C112 C 0.8887(3) 0.2103(3) 0.7072(8) 0.0188 1.0000 Uani . . . . . . . H112 H 0.8980 0.2163 0.6149 0.0500 1.0000 Uiso R . . . . . . C113 C 0.9177(4) 0.2306(3) 0.8127(9) 0.0263 1.0000 Uani . . . . . . . H113 H 0.9463 0.2516 0.7934 0.0500 1.0000 Uiso R . . . . . . C114 C 0.9049(4) 0.2208(3) 0.9469(9) 0.0264 1.0000 Uani . . . . . . . H114 H 0.9251 0.2346 1.0173 0.0500 1.0000 Uiso R . . . . . . C115 C 0.8633(4) 0.1916(3) 0.9785(9) 0.0295 1.0000 Uani . . . . . . . H115 H 0.8549 0.1852 1.0714 0.0500 1.0000 Uiso R . . . . . . C116 C 0.8336(4) 0.1708(3) 0.8739(9) 0.0242 1.0000 Uani . . . . . . . H116 H 0.8049 0.1504 0.8942 0.0500 1.0000 Uiso R . . . . . . C117 C 0.6127(3) 0.1267(3) 0.5277(8) 0.0163 1.0000 Uani . . . . . . . C118 C 0.6024(4) 0.1212(3) 0.3886(9) 0.0290 1.0000 Uani . . . . . . . H118 H 0.6298 0.1317 0.3237 0.0500 1.0000 Uiso R . . . . . . C119 C 0.5526(4) 0.0998(3) 0.3438(11) 0.0370 1.0000 Uani . . . . . . . H119 H 0.5463 0.0957 0.2497 0.0500 1.0000 Uiso R . . . . . . C120 C 0.5135(4) 0.0850(3) 0.4392(10) 0.0308 1.0000 Uani . . . . . . . H120 H 0.4790 0.0710 0.4098 0.0500 1.0000 Uiso R . . . . . . C121 C 0.5229(4) 0.0901(3) 0.5753(9) 0.0286 1.0000 Uani . . . . . . . H121 H 0.4961 0.0791 0.6402 0.0500 1.0000 Uiso R . . . . . . C122 C 0.5722(4) 0.1107(3) 0.6210(9) 0.0241 1.0000 Uani . . . . . . . H122 H 0.5784 0.1141 0.7162 0.0500 1.0000 Uiso R . . . . . . C123 C 0.6542(3) 0.1897(3) 0.7242(8) 0.0175 1.0000 Uani . . . . . . . C124 C 0.6254(3) 0.2268(3) 0.6922(9) 0.0214 1.0000 Uani . . . . . . . H124 H 0.6182 0.2342 0.5994 0.0500 1.0000 Uiso R . . . . . . C125 C 0.6070(4) 0.2531(3) 0.7959(9) 0.0241 1.0000 Uani . . . . . . . H125 H 0.5877 0.2786 0.7742 0.0500 1.0000 Uiso R . . . . . . C126 C 0.6168(4) 0.2425(3) 0.9287(9) 0.0269 1.0000 Uani . . . . . . . H126 H 0.6040 0.2607 0.9997 0.0500 1.0000 Uiso R . . . . . . C127 C 0.6445(4) 0.2055(3) 0.9612(10) 0.0379 1.0000 Uani . . . . . . . H127 H 0.6513 0.1986 1.0550 0.0500 1.0000 Uiso R . . . . . . C128 C 0.6637(4) 0.1783(3) 0.8594(9) 0.0270 1.0000 Uani . . . . . . . H128 H 0.6828 0.1531 0.8820 0.0500 1.0000 Uiso R . . . . . . P21 P 0.74878(9) 0.36106(7) 0.7602(2) 0.0162 1.0000 Uani . . . . . . . P22 P 0.68310(9) 0.40716(7) 0.8330(2) 0.0161 1.0000 Uani . . . . . . . P23 P 0.81824(9) 0.39925(7) 0.8542(2) 0.0164 1.0000 Uani . . . . . . . C201 C 0.7234(3) 0.4467(2) 0.9290(8) 0.0167 1.0000 Uani . . . . . . . H21 H 0.7318 0.4709 0.8692 0.0500 1.0000 Uiso R . . . . . . H234 H 0.6991 0.4566 1.0056 0.0500 1.0000 Uiso R . . . . . . C202 C 0.7815(3) 0.4295(2) 0.9856(8) 0.0174 1.0000 Uani . . . . . . . H22 H 0.7735 0.4110 1.0653 0.0500 1.0000 Uiso R . . . . . . H235 H 0.8065 0.4528 1.0153 0.0500 1.0000 Uiso R . . . . . . C203 C 0.7401(4) 0.3192(3) 0.8920(9) 0.0227 1.0000 Uani . . . . . . . H23 H 0.7546 0.3297 0.9813 0.0500 1.0000 Uiso R . . . . . . H236 H 0.6981 0.3122 0.9030 0.0500 1.0000 Uiso R . . . . . . C204 C 0.7747(4) 0.2803(3) 0.8485(9) 0.0310 1.0000 Uani . . . . . . . H24 H 0.7681 0.2577 0.9138 0.0500 1.0000 Uiso R . . . . . . H237 H 0.8163 0.2872 0.8444 0.0500 1.0000 Uiso R . . . . . . H238 H 0.7613 0.2714 0.7576 0.0500 1.0000 Uiso R . . . . . . C205 C 0.6279(3) 0.3815(3) 0.9336(9) 0.0209 1.0000 Uani . . . . . . . C206 C 0.5770(4) 0.3685(3) 0.8698(9) 0.0246 1.0000 Uani . . . . . . . H206 H 0.5720 0.3723 0.7742 0.0500 1.0000 Uiso R . . . . . . C207 C 0.5346(4) 0.3482(3) 0.9463(12) 0.0378 1.0000 Uani . . . . . . . H207 H 0.4996 0.3393 0.9037 0.0500 1.0000 Uiso R . . . . . . C208 C 0.5431(4) 0.3415(3) 1.0838(11) 0.0335 1.0000 Uani . . . . . . . H208 H 0.5135 0.3277 1.1363 0.0500 1.0000 Uiso R . . . . . . C209 C 0.5935(5) 0.3548(3) 1.1465(10) 0.0369 1.0000 Uani . . . . . . . H209 H 0.5992 0.3501 1.2425 0.0500 1.0000 Uiso R . . . . . . C210 C 0.6361(4) 0.3748(3) 1.0731(9) 0.0261 1.0000 Uani . . . . . . . H210 H 0.6709 0.3840 1.1155 0.0500 1.0000 Uiso R . . . . . . C211 C 0.6492(4) 0.4316(3) 0.6888(8) 0.0173 1.0000 Uani . . . . . . . C212 C 0.6541(4) 0.4157(3) 0.5570(9) 0.0292 1.0000 Uani . . . . . . . H212 H 0.6766 0.3909 0.5405 0.0500 1.0000 Uiso R . . . . . . C213 C 0.6256(4) 0.4358(3) 0.4518(9) 0.0327 1.0000 Uani . . . . . . . H213 H 0.6290 0.4254 0.3620 0.0500 1.0000 Uiso R . . . . . . C214 C 0.5922(4) 0.4715(3) 0.4767(9) 0.0266 1.0000 Uani . . . . . . . H214 H 0.5726 0.4850 0.4030 0.0500 1.0000 Uiso R . . . . . . C215 C 0.5875(4) 0.4868(3) 0.6056(9) 0.0262 1.0000 Uani . . . . . . . H215 H 0.5641 0.5111 0.6219 0.0500 1.0000 Uiso R . . . . . . C216 C 0.6158(3) 0.4674(3) 0.7132(9) 0.0201 1.0000 Uani . . . . . . . H216 H 0.6127 0.4784 0.8028 0.0500 1.0000 Uiso R . . . . . . C217 C 0.8783(3) 0.3696(3) 0.9233(8) 0.0183 1.0000 Uani . . . . . . . C218 C 0.9221(4) 0.3553(3) 0.8366(9) 0.0223 1.0000 Uani . . . . . . . H218 H 0.9196 0.3601 0.7418 0.0500 1.0000 Uiso R . . . . . . C219 C 0.9689(4) 0.3341(3) 0.8912(9) 0.0253 1.0000 Uani . . . . . . . H219 H 0.9996 0.3250 0.8329 0.0500 1.0000 Uiso R . . . . . . C220 C 0.9725(4) 0.3261(3) 1.0296(10) 0.0294 1.0000 Uani . . . . . . . H220 H 1.0047 0.3110 1.0652 0.0500 1.0000 Uiso R . . . . . . C221 C 0.9288(4) 0.3406(3) 1.1144(9) 0.0343 1.0000 Uani . . . . . . . H221 H 0.9312 0.3349 1.2091 0.0500 1.0000 Uiso R . . . . . . C222 C 0.8814(4) 0.3619(3) 1.0638(9) 0.0304 1.0000 Uani . . . . . . . H222 H 0.8513 0.3717 1.1219 0.0500 1.0000 Uiso R . . . . . . C223 C 0.8441(3) 0.4341(3) 0.7233(8) 0.0147 1.0000 Uani . . . . . . . C224 C 0.8248(4) 0.4323(3) 0.5901(9) 0.0288 1.0000 Uani . . . . . . . H224 H 0.7968 0.4117 0.5635 0.0500 1.0000 Uiso R . . . . . . C225 C 0.8462(4) 0.4604(3) 0.4941(8) 0.0305 1.0000 Uani . . . . . . . H225 H 0.8327 0.4594 0.4029 0.0500 1.0000 Uiso R . . . . . . C226 C 0.8871(4) 0.4904(3) 0.5330(9) 0.0241 1.0000 Uani . . . . . . . H226 H 0.9015 0.5098 0.4682 0.0500 1.0000 Uiso R . . . . . . C227 C 0.9068(4) 0.4925(3) 0.6653(9) 0.0245 1.0000 Uani . . . . . . . H227 H 0.9353 0.5125 0.6909 0.0500 1.0000 Uiso R . . . . . . C228 C 0.8852(4) 0.4646(3) 0.7621(8) 0.0210 1.0000 Uani . . . . . . . H228 H 0.8979 0.4661 0.8536 0.0500 1.0000 Uiso R . . . . . . Al1 Al 1.00728(10) 0.24244(8) 0.4151(3) 0.0205 1.0000 Uani . . . . . . . Cl11 Cl 0.99135(9) 0.29406(7) 0.5480(2) 0.0287 1.0000 Uani . . . . . . . Cl12 Cl 1.07583(10) 0.26087(8) 0.2801(2) 0.0331 1.0000 Uani . . . . . . . Cl13 Cl 1.03374(9) 0.18812(7) 0.5281(2) 0.0302 1.0000 Uani . . . . . . . Cl14 Cl 0.92947(10) 0.22661(8) 0.3065(2) 0.0330 1.0000 Uani . . . . . . . Al2 Al 0.24551(11) 0.44043(9) 1.0559(3) 0.0217 1.0000 Uani . . . . . . . Cl21 Cl 0.22998(10) 0.37829(7) 1.1354(2) 0.0274 1.0000 Uani . . . . . . . Cl22 Cl 0.32609(9) 0.44017(7) 0.9481(2) 0.0287 1.0000 Uani . . . . . . . Cl23 Cl 0.17799(10) 0.45607(8) 0.9160(2) 0.0340 1.0000 Uani . . . . . . . Cl24 Cl 0.24879(12) 0.48470(8) 1.2181(2) 0.0374 1.0000 Uani . . . . . . . Al3 Al 0.76694(11) 0.31312(9) 0.3798(3) 0.0205 1.0000 Uani . . . . . . . Cl31 Cl 0.77389(13) 0.27047(8) 0.2140(2) 0.0425 1.0000 Uani . . . . . . . Cl32 Cl 0.84120(10) 0.30976(8) 0.5084(3) 0.0359 1.0000 Uani . . . . . . . Cl33 Cl 0.75841(10) 0.37690(7) 0.3086(2) 0.0281 1.0000 Uani . . . . . . . Cl34 Cl 0.69086(10) 0.29880(7) 0.4949(2) 0.0307 1.0000 Uani . . . . . . . Al4 Al 0.5000 0.5000 0.9916(4) 0.0215 1.0000 Uani S T . . . . . Cl41 Cl 0.57177(11) 0.48039(8) 1.1155(2) 0.0344 1.0000 Uani . . . . . . . Cl42 Cl 0.47466(9) 0.44831(7) 0.8666(2) 0.0269 1.0000 Uani . . . . . . . Al5 Al 1.0000 0.5000 0.0644(4) 0.0257 1.0000 Uani S T . . . . . Cl51 Cl 1.01944(10) 0.44645(8) -0.0590(2) 0.0340 1.0000 Uani . . . . . . . Cl52 Cl 1.07462(12) 0.51588(10) 0.1841(3) 0.0473 1.0000 Uani . . . . . . . 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 P11 0.0208(11) 0.0179(12) 0.0191(11) 0.0015(9) 0.0003(8) 0.0010(9) P12 0.0181(10) 0.0161(11) 0.0177(10) -0.0006(9) 0.0003(8) 0.0004(9) P13 0.0171(10) 0.0170(10) 0.0154(10) -0.0001(8) 0.0011(8) 0.0025(8) C101 0.016(4) 0.013(4) 0.024(4) 0.001(3) -0.003(3) 0.002(3) C102 0.019(4) 0.024(4) 0.018(4) 0.001(3) 0.001(3) 0.010(3) C103 0.027(5) 0.017(4) 0.022(4) 0.004(4) -0.006(4) 0.000(3) C104 0.031(5) 0.022(5) 0.039(5) -0.002(4) -0.004(4) 0.002(4) C105 0.015(4) 0.014(4) 0.029(5) 0.006(4) -0.001(3) -0.003(3) C106 0.022(4) 0.023(5) 0.019(4) 0.001(4) 0.001(3) -0.005(4) C107 0.020(4) 0.021(5) 0.041(6) 0.004(4) 0.002(4) 0.000(4) C108 0.037(5) 0.026(5) 0.037(6) -0.011(4) 0.016(5) 0.001(4) C109 0.040(6) 0.032(6) 0.029(5) -0.011(4) 0.006(4) -0.004(5) C110 0.030(5) 0.032(5) 0.019(4) -0.003(4) -0.001(4) -0.004(4) C111 0.016(4) 0.019(4) 0.020(4) -0.004(4) -0.004(3) 0.003(3) C112 0.021(4) 0.022(5) 0.014(4) 0.002(3) 0.005(3) -0.001(3) C113 0.024(4) 0.020(5) 0.035(5) -0.002(4) -0.010(4) 0.000(4) C114 0.029(5) 0.025(5) 0.025(5) -0.007(4) -0.007(4) 0.002(4) C115 0.042(5) 0.026(5) 0.020(5) 0.001(4) 0.004(4) 0.005(4) C116 0.030(5) 0.023(4) 0.020(4) -0.002(4) 0.000(4) -0.006(4) C117 0.017(4) 0.016(4) 0.016(4) 0.001(3) 0.000(3) 0.008(3) C118 0.022(4) 0.043(6) 0.022(5) -0.001(4) -0.004(3) -0.005(4) C119 0.041(6) 0.035(6) 0.036(6) -0.001(5) -0.012(5) -0.012(5) C120 0.023(5) 0.025(5) 0.044(6) -0.002(4) -0.012(4) 0.002(4) C121 0.031(5) 0.020(4) 0.035(5) 0.004(4) 0.007(4) -0.001(4) C122 0.026(4) 0.019(4) 0.028(5) 0.006(4) 0.002(4) 0.001(4) C123 0.019(4) 0.018(4) 0.015(4) 0.001(3) 0.003(3) 0.002(3) C124 0.018(4) 0.025(5) 0.022(4) 0.002(4) 0.005(3) -0.004(3) C125 0.030(5) 0.014(4) 0.028(5) -0.002(4) -0.002(4) 0.007(4) C126 0.034(5) 0.024(5) 0.023(5) -0.008(4) 0.000(4) 0.005(4) C127 0.047(6) 0.041(6) 0.025(5) -0.002(4) -0.001(4) 0.015(5) C128 0.036(5) 0.026(5) 0.019(4) -0.002(4) 0.003(4) 0.019(4) P21 0.0170(10) 0.0130(11) 0.0184(11) -0.0003(9) 0.0008(8) 0.0020(8) P22 0.0168(10) 0.0153(11) 0.0162(11) -0.0001(8) 0.0007(8) -0.0004(8) P23 0.0186(10) 0.0163(10) 0.0143(10) 0.0023(8) 0.0001(8) 0.0000(8) C201 0.013(4) 0.019(4) 0.018(4) -0.001(3) 0.001(3) -0.003(3) C202 0.018(4) 0.018(4) 0.016(4) -0.005(3) -0.001(3) 0.002(3) C203 0.025(4) 0.017(4) 0.026(5) 0.007(4) 0.006(4) -0.002(3) C204 0.049(6) 0.018(4) 0.025(5) 0.002(4) 0.003(4) 0.015(4) C205 0.019(4) 0.016(4) 0.028(5) -0.004(4) 0.004(3) 0.001(3) C206 0.024(4) 0.019(4) 0.031(5) 0.005(4) 0.000(4) 0.002(3) C207 0.016(4) 0.029(5) 0.068(8) 0.012(5) -0.002(5) -0.004(4) C208 0.024(5) 0.023(5) 0.054(7) 0.010(5) 0.018(4) 0.003(4) C209 0.050(6) 0.033(6) 0.028(5) 0.007(4) 0.010(4) -0.003(5) C210 0.027(5) 0.025(5) 0.026(5) 0.002(4) 0.002(4) -0.004(4) C211 0.023(4) 0.015(4) 0.013(4) 0.003(3) 0.004(3) 0.004(3) C212 0.029(5) 0.032(5) 0.026(5) -0.005(4) 0.002(4) 0.014(4) C213 0.039(5) 0.038(6) 0.021(5) -0.008(4) -0.009(4) 0.014(4) C214 0.027(5) 0.031(5) 0.021(4) 0.004(4) -0.005(4) 0.003(4) C215 0.024(5) 0.024(5) 0.030(5) 0.009(4) 0.002(4) 0.005(4) C216 0.022(4) 0.023(5) 0.015(4) -0.006(4) 0.004(3) -0.004(4) C217 0.021(4) 0.016(4) 0.018(4) 0.003(3) -0.001(3) -0.002(3) C218 0.027(4) 0.018(4) 0.022(4) 0.001(4) 0.002(4) 0.004(3) C219 0.023(4) 0.022(5) 0.032(5) -0.008(4) -0.002(4) 0.000(4) C220 0.025(5) 0.025(5) 0.038(5) -0.001(4) -0.008(4) -0.001(4) C221 0.042(6) 0.047(6) 0.014(4) 0.010(4) -0.010(4) 0.018(5) C222 0.031(5) 0.039(6) 0.021(5) 0.004(4) -0.001(4) 0.005(4) C223 0.018(4) 0.016(4) 0.010(4) -0.002(3) 0.001(3) -0.001(3) C224 0.033(5) 0.029(5) 0.025(5) 0.003(4) 0.003(4) -0.008(4) C225 0.038(5) 0.047(6) 0.006(4) 0.008(4) -0.002(3) -0.010(5) C226 0.029(5) 0.018(5) 0.026(5) 0.008(4) 0.010(4) 0.007(4) C227 0.022(4) 0.021(5) 0.030(5) 0.003(4) 0.008(4) 0.002(4) C228 0.023(4) 0.022(5) 0.018(4) -0.001(3) 0.003(3) 0.000(4) Al1 0.0215(12) 0.0235(13) 0.0164(12) -0.0023(11) 0.0016(10) -0.0027(10) Cl11 0.0252(11) 0.0302(12) 0.0307(11) -0.0088(10) 0.0009(9) 0.0011(9) Cl12 0.0331(12) 0.0422(15) 0.0240(11) 0.0037(10) 0.0090(9) -0.0026(11) Cl13 0.0286(11) 0.0253(11) 0.0366(13) 0.0056(10) -0.0023(9) -0.0031(9) Cl14 0.0269(11) 0.0445(15) 0.0277(12) -0.0102(11) -0.0081(9) -0.0024(10) Al2 0.0245(13) 0.0210(14) 0.0196(13) 0.0011(11) -0.0004(10) 0.0022(10) Cl21 0.0353(12) 0.0254(12) 0.0216(11) 0.0048(9) 0.0014(9) -0.0064(10) Cl22 0.0222(10) 0.0310(12) 0.0330(12) 0.0031(10) 0.0033(9) -0.0035(9) Cl23 0.0306(12) 0.0415(14) 0.0299(12) -0.0010(10) -0.0057(10) 0.0131(11) Cl24 0.0639(16) 0.0285(12) 0.0198(11) -0.0041(9) 0.0013(11) 0.0013(11) Al3 0.0235(13) 0.0235(14) 0.0146(12) 0.0014(11) 0.0005(10) 0.0037(11) Cl31 0.0696(18) 0.0350(14) 0.0229(12) -0.0063(10) -0.0002(12) 0.0144(13) Cl32 0.0256(11) 0.0493(15) 0.0328(13) -0.0035(11) -0.0046(9) 0.0116(11) Cl33 0.0406(13) 0.0255(12) 0.0180(10) 0.0048(9) 0.0016(9) -0.0003(10) Cl34 0.0265(11) 0.0284(12) 0.0371(13) -0.0017(10) 0.0052(9) -0.0088(9) Al4 0.0238(18) 0.0235(19) 0.0173(17) 0.0000 0.0000 0.0031(15) Cl41 0.0334(12) 0.0438(15) 0.0259(12) 0.0087(11) -0.0091(10) 0.0082(11) Cl42 0.0264(11) 0.0229(11) 0.0314(11) -0.0058(9) 0.0013(9) 0.0008(9) Al5 0.0231(19) 0.038(2) 0.0155(18) 0.0000 0.0000 -0.0028(16) Cl51 0.0302(12) 0.0370(13) 0.0350(13) -0.0051(10) -0.0015(10) 0.0027(10) Cl52 0.0394(14) 0.069(2) 0.0331(14) -0.0170(13) -0.0169(11) 0.0025(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.080761(12) loop_ _oxford_twin_element_scale_factors 0.59(11) 0.41(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P11 . P12 . 2.225(3) yes P11 . P13 . 2.201(3) yes P11 . C103 . 1.848(10) yes P12 . C101 . 1.833(8) yes P12 . C105 . 1.785(9) yes P12 . C111 . 1.797(8) yes P13 . C102 . 1.821(8) yes P13 . C117 . 1.777(8) yes P13 . C123 . 1.797(8) yes C101 . H11 . 0.988 no C101 . H229 . 0.987 no C101 . C102 . 1.514(11) yes C102 . H12 . 0.992 no C102 . H230 . 0.992 no C103 . H13 . 0.995 no C103 . H231 . 0.994 no C103 . C104 . 1.509(11) yes C104 . H14 . 0.987 no C104 . H232 . 0.979 no C104 . H233 . 0.981 no C105 . C106 . 1.402(11) yes C105 . C110 . 1.397(13) yes C106 . H106 . 0.953 no C106 . C107 . 1.373(12) yes C107 . H107 . 0.950 no C107 . C108 . 1.404(14) yes C108 . H108 . 0.944 no C108 . C109 . 1.368(14) yes C109 . H109 . 0.944 no C109 . C110 . 1.380(13) yes C110 . H110 . 0.956 no C111 . C112 . 1.391(12) yes C111 . C116 . 1.385(12) yes C112 . H112 . 0.950 no C112 . C113 . 1.389(12) yes C113 . H113 . 0.954 no C113 . C114 . 1.384(13) yes C114 . H114 . 0.940 no C114 . C115 . 1.366(13) yes C115 . H115 . 0.954 no C115 . C116 . 1.397(12) yes C116 . H116 . 0.944 no C117 . C118 . 1.397(12) yes C117 . C122 . 1.397(11) yes C118 . H118 . 0.954 no C118 . C119 . 1.399(12) yes C119 . H119 . 0.944 no C119 . C120 . 1.378(14) yes C120 . H120 . 0.952 no C120 . C121 . 1.362(13) yes C121 . H121 . 0.951 no C121 . C122 . 1.379(12) yes C122 . H122 . 0.951 no C123 . C124 . 1.388(12) yes C123 . C128 . 1.392(12) yes C124 . H124 . 0.955 no C124 . C125 . 1.384(12) yes C125 . H125 . 0.947 no C125 . C126 . 1.364(12) yes C126 . H126 . 0.954 no C126 . C127 . 1.373(13) yes C127 . H127 . 0.959 no C127 . C128 . 1.393(12) yes C128 . H128 . 0.941 no P21 . P22 . 2.218(3) yes P21 . P23 . 2.203(3) yes P21 . C203 . 1.867(9) yes P22 . C201 . 1.822(8) yes P22 . C205 . 1.799(9) yes P22 . C211 . 1.791(8) yes P23 . C202 . 1.815(8) yes P23 . C217 . 1.800(8) yes P23 . C223 . 1.796(8) yes C201 . H21 . 0.989 no C201 . H234 . 0.988 no C201 . C202 . 1.540(10) yes C202 . H22 . 0.994 no C202 . H235 . 0.981 no C203 . H23 . 0.995 no C203 . H236 . 0.992 no C203 . C204 . 1.529(11) yes C204 . H24 . 0.975 no C204 . H237 . 0.977 no C204 . H238 . 0.985 no C205 . C206 . 1.386(12) yes C205 . C210 . 1.398(12) yes C206 . H206 . 0.953 no C206 . C207 . 1.386(12) yes C207 . H207 . 0.946 no C207 . C208 . 1.379(16) yes C208 . H208 . 0.958 no C208 . C209 . 1.375(14) yes C209 . H209 . 0.961 no C209 . C210 . 1.369(12) yes C210 . H210 . 0.944 no C211 . C212 . 1.393(12) yes C211 . C216 . 1.392(12) yes C212 . H212 . 0.955 no C212 . C213 . 1.378(12) yes C213 . H213 . 0.944 no C213 . C214 . 1.390(12) yes C214 . H214 . 0.953 no C214 . C215 . 1.359(13) yes C215 . H215 . 0.953 no C215 . C216 . 1.384(12) yes C216 . H216 . 0.949 no C217 . C218 . 1.390(11) yes C217 . C222 . 1.402(12) yes C218 . H218 . 0.944 no C218 . C219 . 1.376(11) yes C219 . H219 . 0.951 no C219 . C220 . 1.384(13) yes C220 . H220 . 0.946 no C220 . C221 . 1.381(13) yes C221 . H221 . 0.949 no C221 . C222 . 1.372(12) yes C222 . H222 . 0.946 no C223 . C224 . 1.382(12) yes C223 . C228 . 1.403(11) yes C224 . H224 . 0.952 no C224 . C225 . 1.387(12) yes C225 . H225 . 0.947 no C225 . C226 . 1.390(12) yes C226 . H226 . 0.946 no C226 . C227 . 1.376(12) yes C227 . H227 . 0.947 no C227 . C228 . 1.390(12) yes C228 . H228 . 0.946 no Al1 . Cl11 . 2.128(3) yes Al1 . Cl12 . 2.135(3) yes Al1 . Cl13 . 2.140(3) yes Al1 . Cl14 . 2.135(3) yes Al2 . Cl21 . 2.154(4) yes Al2 . Cl22 . 2.126(3) yes Al2 . Cl23 . 2.125(3) yes Al2 . Cl24 . 2.126(4) yes Al3 . Cl31 . 2.125(4) yes Al3 . Cl32 . 2.119(3) yes Al3 . Cl33 . 2.154(4) yes Al3 . Cl34 . 2.124(3) yes Al4 . Cl41 4_665 2.136(3) yes Al4 . Cl42 4_665 2.132(3) yes Al4 . Cl41 . 2.136(3) yes Al4 . Cl42 . 2.132(3) yes Al5 . Cl51 4_765 2.137(3) yes Al5 . Cl52 4_765 2.133(3) yes Al5 . Cl51 . 2.137(3) yes Al5 . Cl52 . 2.133(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P12 . P11 . P13 . 89.17(12) yes P12 . P11 . C103 . 102.5(3) yes P13 . P11 . C103 . 98.8(3) yes P11 . P12 . C101 . 105.7(3) yes P11 . P12 . C105 . 111.6(3) yes C101 . P12 . C105 . 112.3(4) yes P11 . P12 . C111 . 110.0(3) yes C101 . P12 . C111 . 108.8(4) yes C105 . P12 . C111 . 108.4(4) yes P11 . P13 . C102 . 104.8(3) yes P11 . P13 . C117 . 112.0(3) yes C102 . P13 . C117 . 111.8(4) yes P11 . P13 . C123 . 106.3(3) yes C102 . P13 . C123 . 111.3(4) yes C117 . P13 . C123 . 110.5(4) yes P12 . C101 . H11 . 108.0 no P12 . C101 . H229 . 108.2 no H11 . C101 . H229 . 108.1 no P12 . C101 . C102 . 113.6(5) yes H11 . C101 . C102 . 109.2 no H229 . C101 . C102 . 109.5 no C101 . C102 . P13 . 109.6(6) yes C101 . C102 . H12 . 110.0 no P13 . C102 . H12 . 109.7 no C101 . C102 . H230 . 109.9 no P13 . C102 . H230 . 109.7 no H12 . C102 . H230 . 108.0 no P11 . C103 . H13 . 110.0 no P11 . C103 . H231 . 110.0 no H13 . C103 . H231 . 107.5 no P11 . C103 . C104 . 110.0(6) yes H13 . C103 . C104 . 109.6 no H231 . C103 . C104 . 109.6 no C103 . C104 . H14 . 109.7 no C103 . C104 . H232 . 109.9 no H14 . C104 . H232 . 109.0 no C103 . C104 . H233 . 109.9 no H14 . C104 . H233 . 108.8 no H232 . C104 . H233 . 109.5 no P12 . C105 . C106 . 118.9(7) yes P12 . C105 . C110 . 121.7(7) yes C106 . C105 . C110 . 119.4(8) yes C105 . C106 . H106 . 119.9 no C105 . C106 . C107 . 119.4(8) yes H106 . C106 . C107 . 120.7 no C106 . C107 . H107 . 119.5 no C106 . C107 . C108 . 121.0(9) yes H107 . C107 . C108 . 119.5 no C107 . C108 . H108 . 120.3 no C107 . C108 . C109 . 119.1(9) yes H108 . C108 . C109 . 120.6 no C108 . C109 . H109 . 119.5 no C108 . C109 . C110 . 121.0(9) yes H109 . C109 . C110 . 119.5 no C105 . C110 . C109 . 120.1(9) yes C105 . C110 . H110 . 120.0 no C109 . C110 . H110 . 119.9 no P12 . C111 . C112 . 116.2(6) yes P12 . C111 . C116 . 122.8(7) yes C112 . C111 . C116 . 121.0(8) yes C111 . C112 . H112 . 120.7 no C111 . C112 . C113 . 118.6(8) yes H112 . C112 . C113 . 120.6 no C112 . C113 . H113 . 120.4 no C112 . C113 . C114 . 120.2(8) yes H113 . C113 . C114 . 119.4 no C113 . C114 . H114 . 119.3 no C113 . C114 . C115 . 121.1(8) yes H114 . C114 . C115 . 119.6 no C114 . C115 . H115 . 120.2 no C114 . C115 . C116 . 119.6(8) yes H115 . C115 . C116 . 120.2 no C115 . C116 . C111 . 119.5(8) yes C115 . C116 . H116 . 120.5 no C111 . C116 . H116 . 120.0 no P13 . C117 . C118 . 121.7(6) yes P13 . C117 . C122 . 119.4(6) yes C118 . C117 . C122 . 118.9(8) yes C117 . C118 . H118 . 119.9 no C117 . C118 . C119 . 120.4(9) yes H118 . C118 . C119 . 119.7 no C118 . C119 . H119 . 119.9 no C118 . C119 . C120 . 118.8(9) yes H119 . C119 . C120 . 121.3 no C119 . C120 . H120 . 119.5 no C119 . C120 . C121 . 121.5(9) yes H120 . C120 . C121 . 119.0 no C120 . C121 . H121 . 120.6 no C120 . C121 . C122 . 120.3(9) yes H121 . C121 . C122 . 119.1 no C117 . C122 . C121 . 120.2(9) yes C117 . C122 . H122 . 120.2 no C121 . C122 . H122 . 119.6 no P13 . C123 . C124 . 118.9(6) yes P13 . C123 . C128 . 120.3(6) yes C124 . C123 . C128 . 120.7(8) yes C123 . C124 . H124 . 120.5 no C123 . C124 . C125 . 119.5(8) yes H124 . C124 . C125 . 119.9 no C124 . C125 . H125 . 119.6 no C124 . C125 . C126 . 120.1(8) yes H125 . C125 . C126 . 120.2 no C125 . C126 . H126 . 119.8 no C125 . C126 . C127 . 120.7(8) yes H126 . C126 . C127 . 119.5 no C126 . C127 . H127 . 119.6 no C126 . C127 . C128 . 120.7(9) yes H127 . C127 . C128 . 119.7 no C127 . C128 . C123 . 118.2(8) yes C127 . C128 . H128 . 120.5 no C123 . C128 . H128 . 121.2 no P22 . P21 . P23 . 89.41(11) yes P22 . P21 . C203 . 100.2(3) yes P23 . P21 . C203 . 100.4(3) yes P21 . P22 . C201 . 106.2(3) yes P21 . P22 . C205 . 110.7(3) yes C201 . P22 . C205 . 112.6(4) yes P21 . P22 . C211 . 109.0(3) yes C201 . P22 . C211 . 109.2(4) yes C205 . P22 . C211 . 109.0(4) yes P21 . P23 . C202 . 104.8(3) yes P21 . P23 . C217 . 114.8(3) yes C202 . P23 . C217 . 111.3(4) yes P21 . P23 . C223 . 106.2(3) yes C202 . P23 . C223 . 109.6(4) yes C217 . P23 . C223 . 109.9(4) yes P22 . C201 . H21 . 109.2 no P22 . C201 . H234 . 109.2 no H21 . C201 . H234 . 108.2 no P22 . C201 . C202 . 112.2(5) yes H21 . C201 . C202 . 108.9 no H234 . C201 . C202 . 109.0 no C201 . C202 . P23 . 109.4(5) yes C201 . C202 . H22 . 109.6 no P23 . C202 . H22 . 109.4 no C201 . C202 . H235 . 109.9 no P23 . C202 . H235 . 109.9 no H22 . C202 . H235 . 108.6 no P21 . C203 . H23 . 109.4 no P21 . C203 . H236 . 109.7 no H23 . C203 . H236 . 107.7 no P21 . C203 . C204 . 109.2(6) yes H23 . C203 . C204 . 110.2 no H236 . C203 . C204 . 110.7 no C203 . C204 . H24 . 109.4 no C203 . C204 . H237 . 109.5 no H24 . C204 . H237 . 110.2 no C203 . C204 . H238 . 108.9 no H24 . C204 . H238 . 109.5 no H237 . C204 . H238 . 109.3 no P22 . C205 . C206 . 118.5(7) yes P22 . C205 . C210 . 120.8(7) yes C206 . C205 . C210 . 120.6(8) yes C205 . C206 . H206 . 120.5 no C205 . C206 . C207 . 118.9(9) yes H206 . C206 . C207 . 120.6 no C206 . C207 . H207 . 119.4 no C206 . C207 . C208 . 120.1(9) yes H207 . C207 . C208 . 120.4 no C207 . C208 . H208 . 119.8 no C207 . C208 . C209 . 120.7(9) yes H208 . C208 . C209 . 119.6 no C208 . C209 . H209 . 120.3 no C208 . C209 . C210 . 120.3(9) yes H209 . C209 . C210 . 119.4 no C205 . C210 . C209 . 119.4(9) yes C205 . C210 . H210 . 119.8 no C209 . C210 . H210 . 120.8 no P22 . C211 . C212 . 122.8(6) yes P22 . C211 . C216 . 117.2(6) yes C212 . C211 . C216 . 120.0(8) yes C211 . C212 . H212 . 119.9 no C211 . C212 . C213 . 119.3(8) yes H212 . C212 . C213 . 120.7 no C212 . C213 . H213 . 119.9 no C212 . C213 . C214 . 120.5(9) yes H213 . C213 . C214 . 119.6 no C213 . C214 . H214 . 119.6 no C213 . C214 . C215 . 120.0(8) yes H214 . C214 . C215 . 120.4 no C214 . C215 . H215 . 119.5 no C214 . C215 . C216 . 120.9(8) yes H215 . C215 . C216 . 119.7 no C211 . C216 . C215 . 119.4(8) yes C211 . C216 . H216 . 120.2 no C215 . C216 . H216 . 120.5 no P23 . C217 . C218 . 119.4(6) yes P23 . C217 . C222 . 120.0(7) yes C218 . C217 . C222 . 120.6(8) yes C217 . C218 . H218 . 120.5 no C217 . C218 . C219 . 118.9(8) yes H218 . C218 . C219 . 120.7 no C218 . C219 . H219 . 119.3 no C218 . C219 . C220 . 121.3(8) yes H219 . C219 . C220 . 119.4 no C219 . C220 . H220 . 120.1 no C219 . C220 . C221 . 119.1(8) yes H220 . C220 . C221 . 120.8 no C220 . C221 . H221 . 118.9 no C220 . C221 . C222 . 121.3(9) yes H221 . C221 . C222 . 119.7 no C217 . C222 . C221 . 118.8(9) yes C217 . C222 . H222 . 119.9 no C221 . C222 . H222 . 121.3 no P23 . C223 . C224 . 123.1(6) yes P23 . C223 . C228 . 117.0(6) yes C224 . C223 . C228 . 119.9(8) yes C223 . C224 . H224 . 120.1 no C223 . C224 . C225 . 120.2(8) yes H224 . C224 . C225 . 119.6 no C224 . C225 . H225 . 120.4 no C224 . C225 . C226 . 119.5(8) yes H225 . C225 . C226 . 120.1 no C225 . C226 . H226 . 119.9 no C225 . C226 . C227 . 120.8(8) yes H226 . C226 . C227 . 119.3 no C226 . C227 . H227 . 120.6 no C226 . C227 . C228 . 119.8(8) yes H227 . C227 . C228 . 119.6 no C223 . C228 . C227 . 119.6(8) yes C223 . C228 . H228 . 119.9 no C227 . C228 . H228 . 120.4 no Cl11 . Al1 . Cl12 . 107.11(14) yes Cl11 . Al1 . Cl13 . 110.72(14) yes Cl12 . Al1 . Cl13 . 109.57(14) yes Cl11 . Al1 . Cl14 . 110.17(14) yes Cl12 . Al1 . Cl14 . 111.59(14) yes Cl13 . Al1 . Cl14 . 107.70(14) yes Cl21 . Al2 . Cl22 . 108.64(15) yes Cl21 . Al2 . Cl23 . 109.18(15) yes Cl22 . Al2 . Cl23 . 108.07(15) yes Cl21 . Al2 . Cl24 . 110.01(15) yes Cl22 . Al2 . Cl24 . 110.14(15) yes Cl23 . Al2 . Cl24 . 110.74(15) yes Cl31 . Al3 . Cl32 . 111.34(15) yes Cl31 . Al3 . Cl33 . 111.08(14) yes Cl32 . Al3 . Cl33 . 108.25(15) yes Cl31 . Al3 . Cl34 . 109.37(16) yes Cl32 . Al3 . Cl34 . 109.26(14) yes Cl33 . Al3 . Cl34 . 107.45(14) yes Cl41 4_665 Al4 . Cl42 4_665 108.14(9) yes Cl41 4_665 Al4 . Cl41 . 110.6(2) yes Cl42 4_665 Al4 . Cl41 . 110.09(9) yes Cl41 4_665 Al4 . Cl42 . 110.09(9) yes Cl42 4_665 Al4 . Cl42 . 109.7(2) yes Cl41 . Al4 . Cl42 . 108.14(9) yes Cl51 4_765 Al5 . Cl52 4_765 109.52(10) yes Cl51 4_765 Al5 . Cl51 . 110.9(2) yes Cl52 4_765 Al5 . Cl51 . 106.85(11) yes Cl51 4_765 Al5 . Cl52 . 106.85(11) yes Cl52 4_765 Al5 . Cl52 . 113.2(2) yes Cl51 . Al5 . Cl52 . 109.52(10) yes #====================================================================== data_6e _database_code_depnum_ccdc_archive 'CCDC 664571' #====================================================================== _chemical_name_systematic . _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C29 H31 P3, Cl6 Sn, 2(C H Cl3)' _chemical_formula_sum 'C31 H33 Cl12 P3 Sn' _chemical_formula_weight 1042.57 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 Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7862(8) _cell_length_b 21.2600(14) _cell_length_c 15.2904(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.6610(10) _cell_angle_gamma 90.00 _cell_volume 4142.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6891 _cell_measurement_theta_min 2.216 _cell_measurement_theta_max 27.892 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method . _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0651 before and 0.0520 after correction. The Ratio of minimum to maximum transmission is 0.758. The \l/2 correction factor is 0.0000 ; _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 1K CCD area detector' _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 29989 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8451 _reflns_number_gt 5869 _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 '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. Some restraints were used in the refinement of one of the PPh2 groups and one of the carbons of the ethane linking two PPh2 groups. This latter carbon, the P atom coordinated to it and one of the phenyl rings attached to this P atom were disordered over two positions (refined occupancies of 89.2(7) and 10.8(7)% respectively). Each pair of disordered atoms were contrained to have the same displacement parameters (EADP instruction in SHELXL). Distances between equivalents atoms in the disordered part with lowest occupancy were restrained to be the same as those from the fragment with highest occupancy (SAME instruction).In addition, the anisotropic displacement parameters of all carbons belonging to the phenyl rings were subject to a 'rigid body' restraint (DELU instruction). The distance between P1 and the minor component P32 was constrained to a sensible distance (DFIX instruction). ; _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^)+(0.0466P)^2^+27.8776P] 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 7314 _refine_ls_number_parameters 442 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.45897(4) 0.13785(3) -0.28605(3) 0.01842(15) Uani 1 1 d . . . Cl1 Cl 0.3658(2) 0.06553(15) -0.20208(16) 0.0608(8) Uani 1 1 d . . . Cl2 Cl 0.48120(18) 0.20876(11) -0.16219(12) 0.0368(5) Uani 1 1 d . . . Cl3 Cl 0.29898(18) 0.19158(14) -0.33824(15) 0.0530(7) Uani 1 1 d . . . Cl4 Cl 0.56169(18) 0.20964(11) -0.36855(12) 0.0361(5) Uani 1 1 d . . . Cl5 Cl 0.43641(16) 0.06928(10) -0.41521(12) 0.0289(5) Uani 1 1 d . . . Cl6 Cl 0.62191(18) 0.08422(11) -0.23897(14) 0.0382(5) Uani 1 1 d . . . P1 P 0.30142(15) -0.22114(10) -0.35364(12) 0.0190(4) Uani 1 1 d D . . P2 P 0.44409(15) -0.16277(10) -0.32004(12) 0.0199(4) Uani 1 1 d . A . C6 C 0.5609(6) -0.2053(4) -0.3387(5) 0.0223(17) Uani 1 1 d U . . C11 C 0.5883(6) -0.2130(4) -0.4247(5) 0.0261(18) Uani 1 1 d U A . H11 H 0.5505 -0.1918 -0.4719 0.039 Uiso 1 1 calc R . . C10 C 0.6703(7) -0.2517(5) -0.4399(5) 0.036(2) Uani 1 1 d U . . H10 H 0.6873 -0.2585 -0.4985 0.054 Uiso 1 1 calc R A . C9 C 0.7291(7) -0.2811(4) -0.3716(6) 0.035(2) Uani 1 1 d U A . H9 H 0.7867 -0.3072 -0.3832 0.053 Uiso 1 1 calc R . . C8 C 0.7030(6) -0.2720(4) -0.2862(5) 0.0312(19) Uani 1 1 d U . . H8 H 0.7437 -0.2913 -0.2389 0.047 Uiso 1 1 calc R A . C7 C 0.6181(6) -0.2349(4) -0.2696(5) 0.0257(18) Uani 1 1 d U A . H7 H 0.5991 -0.2297 -0.2112 0.039 Uiso 1 1 calc R . . C12 C 0.4463(6) -0.1415(4) -0.2058(5) 0.0230(16) Uani 1 1 d U . . C13 C 0.4999(8) -0.0866(5) -0.1787(6) 0.047(3) Uani 1 1 d U A . H13 H 0.5289 -0.0596 -0.2200 0.071 Uiso 1 1 calc R . . C14 C 0.5094(8) -0.0725(5) -0.0896(7) 0.053(3) Uani 1 1 d U . . H14 H 0.5478 -0.0363 -0.0697 0.080 Uiso 1 1 calc R A . C15 C 0.4652(7) -0.1092(5) -0.0309(6) 0.040(2) Uani 1 1 d U A . H15 H 0.4712 -0.0985 0.0296 0.060 Uiso 1 1 calc R . . C16 C 0.4120(9) -0.1616(5) -0.0593(6) 0.053(3) Uani 1 1 d U . . H16 H 0.3835 -0.1883 -0.0175 0.079 Uiso 1 1 calc R A . C17 C 0.3980(8) -0.1775(5) -0.1480(5) 0.043(2) Uani 1 1 d U A . H17 H 0.3560 -0.2125 -0.1673 0.064 Uiso 1 1 calc R . . C18 C 0.1379(6) -0.1458(4) -0.5104(5) 0.0266(18) Uani 1 1 d U . . C19 C 0.1543(7) -0.1254(4) -0.5953(6) 0.037(2) Uani 1 1 d U A . H19 H 0.2209 -0.1094 -0.6076 0.055 Uiso 1 1 calc R . . C20 C 0.0754(7) -0.1283(4) -0.6599(5) 0.035(2) Uani 1 1 d U . . H20 H 0.0872 -0.1144 -0.7173 0.052 Uiso 1 1 calc R A . C21 C -0.0217(7) -0.1511(4) -0.6433(5) 0.037(2) Uani 1 1 d U A . H21 H -0.0763 -0.1529 -0.6892 0.055 Uiso 1 1 calc R . . C22 C -0.0398(7) -0.1714(4) -0.5605(5) 0.034(2) Uani 1 1 d U . . H22 H -0.1069 -0.1874 -0.5495 0.051 Uiso 1 1 calc R A . C23 C 0.0392(6) -0.1686(4) -0.4926(5) 0.0264(18) Uani 1 1 d U A . H23 H 0.0265 -0.1819 -0.4351 0.040 Uiso 1 1 calc R . . P3 P 0.23513(18) -0.13645(12) -0.4226(2) 0.0188(6) Uani 0.898(7) 1 d P A 1 C24 C 0.1797(7) -0.0960(5) -0.3348(7) 0.0234(19) Uani 0.898(7) 1 d PU A 1 C25 C 0.1848(8) -0.0306(5) -0.3296(7) 0.036(2) Uani 0.898(7) 1 d PU A 1 H25 H 0.2216 -0.0071 -0.3701 0.043 Uiso 0.898(7) 1 calc PR A 1 C26 C 0.1348(8) -0.0004(6) -0.2637(7) 0.045(3) Uani 0.898(7) 1 d PU A 1 H26 H 0.1383 0.0441 -0.2592 0.054 Uiso 0.898(7) 1 calc PR A 1 C27 C 0.0809(13) -0.0334(10) -0.2054(8) 0.046(3) Uani 0.898(7) 1 d PU A 1 H27 H 0.0451 -0.0118 -0.1624 0.055 Uiso 0.898(7) 1 calc PR A 1 C28 C 0.0786(8) -0.0967(6) -0.2091(7) 0.044(3) Uani 0.898(7) 1 d PU A 1 H28 H 0.0427 -0.1194 -0.1672 0.052 Uiso 0.898(7) 1 calc PR A 1 C29 C 0.1283(8) -0.1300(6) -0.2737(7) 0.031(2) Uani 0.898(7) 1 d PU A 1 H29 H 0.1268 -0.1746 -0.2754 0.037 Uiso 0.898(7) 1 calc PR A 1 C2 C 0.3466(7) -0.0955(4) -0.4602(5) 0.023(2) Uani 0.898(7) 1 d P A 1 H2B H 0.3726 -0.1181 -0.5106 0.027 Uiso 0.898(7) 1 calc PR A 1 H2A H 0.3254 -0.0526 -0.4798 0.027 Uiso 0.898(7) 1 calc PR A 1 P3A P 0.2221(17) -0.1294(7) -0.3849(19) 0.0188(6) Uani 0.102(7) 1 d PD A 2 C24A C 0.162(9) -0.111(5) -0.292(8) 0.0234(19) Uani 0.102(7) 1 d PU A 2 C25A C 0.128(7) -0.046(5) -0.296(6) 0.036(2) Uani 0.102(7) 1 d PU A 2 H25A H 0.1452 -0.0163 -0.3398 0.043 Uiso 0.102(7) 1 calc PR A 2 C26A C 0.069(16) -0.032(10) -0.228(10) 0.045(3) Uani 0.102(7) 1 d PU A 2 H26A H 0.0354 0.0074 -0.2331 0.054 Uiso 0.102(7) 1 calc PR A 2 C27A C 0.046(7) -0.067(5) -0.151(6) 0.046(3) Uani 0.102(7) 1 d PU A 2 H27A H 0.0141 -0.0520 -0.1012 0.055 Uiso 0.102(7) 1 calc PR A 2 C28A C 0.085(7) -0.132(6) -0.166(7) 0.044(3) Uani 0.102(7) 1 d PU A 2 H28A H 0.0630 -0.1624 -0.1251 0.052 Uiso 0.102(7) 1 calc PR A 2 C29A C 0.137(6) -0.153(5) -0.217(6) 0.031(2) Uani 0.102(7) 1 d PU A 2 H29A H 0.1632 -0.1951 -0.2125 0.037 Uiso 0.102(7) 1 calc PR A 2 C2A C 0.350(6) -0.076(4) -0.401(5) 0.023(2) Uani 0.102(7) 1 d P A 2 H2AC H 0.3441 -0.0625 -0.4628 0.027 Uiso 0.102(7) 1 calc PR A 2 H2AA H 0.3423 -0.0377 -0.3653 0.027 Uiso 0.102(7) 1 calc PR A 2 C1 C 0.4329(6) -0.0913(4) -0.3865(5) 0.0287(19) Uani 1 1 d . . . H2AB H 0.4187 -0.0552 -0.3483 0.043 Uiso 1 1 calc R A 1 H1B H 0.5005 -0.0834 -0.4118 0.043 Uiso 1 1 calc R A 1 C3 C 0.3417(6) -0.2755(4) -0.4419(5) 0.0234(17) Uani 1 1 d . A . H3 H 0.3923 -0.2541 -0.4786 0.028 Uiso 1 1 calc R . . C5 C 0.2420(7) -0.2953(4) -0.4986(6) 0.036(2) Uani 1 1 d . . . H5A H 0.1897 -0.3110 -0.4606 0.054 Uiso 1 1 calc R A . H5C H 0.2596 -0.3285 -0.5393 0.054 Uiso 1 1 calc R . . H5B H 0.2134 -0.2589 -0.5319 0.054 Uiso 1 1 calc R . . C4 C 0.3919(6) -0.3320(4) -0.3962(6) 0.030(2) Uani 1 1 d . . . H4B H 0.4549 -0.3188 -0.3600 0.045 Uiso 1 1 calc R A . H4C H 0.4114 -0.3625 -0.4400 0.045 Uiso 1 1 calc R . . H4A H 0.3422 -0.3514 -0.3588 0.045 Uiso 1 1 calc R . . C30 C -0.2067(7) -0.0780(4) -0.4156(6) 0.030(2) Uani 1 1 d . . . H30 H -0.2444 -0.0991 -0.4674 0.045 Uiso 1 1 calc R . . Cl7 Cl -0.15709(18) -0.13571(12) -0.34320(16) 0.0456(6) Uani 1 1 d . . . Cl8 Cl -0.1054(2) -0.03186(12) -0.4527(2) 0.0598(8) Uani 1 1 d . . . Cl9 Cl -0.29629(16) -0.02895(10) -0.36650(13) 0.0314(5) Uani 1 1 d . . . C31 C 0.21619(12) -0.01556(8) 0.07218(9) 0.039(2) Uani 1 1 d . . . H31 H 0.2764 -0.0391 0.1025 0.059 Uiso 1 1 calc R . . Cl10 Cl 0.25243(12) 0.01087(8) -0.02996(9) 0.0439(6) Uani 1 1 d R . . Cl11 Cl 0.18584(12) 0.04923(8) 0.13754(9) 0.0604(8) Uani 1 1 d R . . Cl12 Cl 0.10692(12) -0.06589(8) 0.05895(9) 0.0694(9) Uani 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0191(3) 0.0221(3) 0.0143(2) 0.0002(2) 0.00283(18) 0.0022(2) Cl1 0.0741(19) 0.074(2) 0.0369(13) 0.0104(13) 0.0187(13) -0.0361(16) Cl2 0.0496(14) 0.0377(13) 0.0221(10) -0.0125(9) -0.0030(9) 0.0141(11) Cl3 0.0336(13) 0.083(2) 0.0405(13) -0.0119(13) -0.0092(10) 0.0316(14) Cl4 0.0474(13) 0.0359(13) 0.0238(10) 0.0060(9) -0.0038(9) -0.0198(11) Cl5 0.0385(12) 0.0256(11) 0.0226(9) -0.0042(8) 0.0026(8) -0.0084(9) Cl6 0.0395(13) 0.0354(13) 0.0378(12) -0.0071(10) -0.0092(10) 0.0158(11) P1 0.0199(10) 0.0172(11) 0.0203(9) -0.0001(8) 0.0034(8) -0.0012(9) P2 0.0184(10) 0.0203(11) 0.0204(9) 0.0034(8) -0.0010(8) -0.0037(9) C6 0.018(4) 0.026(5) 0.023(4) 0.004(3) -0.002(3) -0.002(3) C11 0.020(4) 0.038(5) 0.020(3) 0.003(4) 0.001(3) -0.003(3) C10 0.028(5) 0.052(6) 0.027(4) -0.002(4) 0.005(3) 0.000(4) C9 0.026(5) 0.033(5) 0.047(5) 0.003(4) 0.009(4) 0.008(4) C8 0.021(4) 0.039(5) 0.033(4) 0.013(4) -0.005(3) 0.004(4) C7 0.026(4) 0.033(5) 0.017(4) 0.008(3) -0.003(3) 0.003(4) C12 0.020(4) 0.030(5) 0.019(3) -0.002(3) -0.004(3) 0.002(4) C13 0.051(6) 0.046(6) 0.045(5) -0.019(5) 0.010(5) -0.026(5) C14 0.059(7) 0.052(7) 0.048(5) -0.031(5) 0.006(5) -0.019(5) C15 0.047(6) 0.042(6) 0.027(4) -0.012(4) -0.010(4) 0.008(4) C16 0.086(8) 0.049(6) 0.025(4) 0.002(4) 0.008(5) -0.023(6) C17 0.068(7) 0.035(6) 0.025(4) 0.000(4) 0.004(4) -0.023(5) C18 0.021(4) 0.023(5) 0.035(4) 0.000(4) -0.003(3) 0.007(4) C19 0.040(5) 0.026(5) 0.046(5) 0.001(4) 0.017(4) -0.005(4) C20 0.053(5) 0.025(5) 0.025(4) -0.005(4) -0.007(3) 0.010(4) C21 0.045(5) 0.033(6) 0.031(4) -0.011(4) -0.008(4) 0.017(4) C22 0.028(4) 0.037(6) 0.035(4) -0.006(4) -0.006(3) 0.009(4) C23 0.018(4) 0.028(5) 0.033(4) 0.004(4) 0.002(3) 0.009(4) P3 0.0176(11) 0.0172(12) 0.0213(15) -0.0035(11) 0.0007(10) 0.0029(10) C24 0.016(5) 0.026(5) 0.027(5) -0.005(4) -0.007(4) 0.005(4) C25 0.032(6) 0.034(5) 0.039(5) -0.008(4) -0.006(4) 0.010(5) C26 0.037(6) 0.047(6) 0.049(6) -0.024(4) -0.012(4) 0.016(5) C27 0.027(7) 0.070(7) 0.041(8) -0.041(7) 0.003(6) 0.002(6) C28 0.029(5) 0.062(6) 0.041(6) -0.028(5) 0.008(4) -0.006(5) C29 0.018(5) 0.045(6) 0.029(6) -0.013(4) 0.002(4) -0.001(4) C2 0.029(5) 0.014(5) 0.024(5) 0.005(4) -0.001(4) -0.003(4) P3A 0.0176(11) 0.0172(12) 0.0213(15) -0.0035(11) 0.0007(10) 0.0029(10) C24A 0.016(5) 0.026(5) 0.027(5) -0.005(4) -0.007(4) 0.005(4) C25A 0.032(6) 0.034(5) 0.039(5) -0.008(4) -0.006(4) 0.010(5) C26A 0.037(6) 0.047(6) 0.049(6) -0.024(4) -0.012(4) 0.016(5) C27A 0.027(7) 0.070(7) 0.041(8) -0.041(7) 0.003(6) 0.002(6) C28A 0.029(5) 0.062(6) 0.041(6) -0.028(5) 0.008(4) -0.006(5) C29A 0.018(5) 0.045(6) 0.029(6) -0.013(4) 0.002(4) -0.001(4) C2A 0.029(5) 0.014(5) 0.024(5) 0.005(4) -0.001(4) -0.003(4) C1 0.020(4) 0.028(5) 0.037(5) 0.011(4) 0.002(4) -0.004(4) C3 0.028(4) 0.018(4) 0.024(4) -0.003(3) 0.003(3) 0.004(4) C5 0.044(6) 0.023(5) 0.039(5) -0.003(4) -0.007(4) 0.003(4) C4 0.023(4) 0.020(5) 0.045(5) -0.006(4) -0.005(4) 0.008(4) C30 0.035(5) 0.017(5) 0.038(5) -0.004(4) 0.007(4) -0.001(4) Cl7 0.0396(13) 0.0416(14) 0.0560(14) 0.0097(12) 0.0070(11) 0.0090(12) Cl8 0.0576(17) 0.0271(14) 0.102(2) 0.0047(14) 0.0511(16) 0.0001(12) Cl9 0.0269(11) 0.0321(12) 0.0356(11) -0.0005(9) 0.0057(9) 0.0037(9) C31 0.040(5) 0.046(6) 0.031(5) 0.009(4) 0.001(4) 0.004(5) Cl10 0.0409(13) 0.0626(17) 0.0281(11) 0.0080(11) 0.0033(10) 0.0015(12) Cl11 0.0730(19) 0.071(2) 0.0395(13) -0.0083(13) 0.0159(13) -0.0139(16) Cl12 0.0653(19) 0.0462(18) 0.100(2) -0.0012(16) 0.0290(17) -0.0156(15) _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 Cl1 2.383(2) . ? Sn1 Cl2 2.419(2) . ? Sn1 Cl3 2.421(2) . ? Sn1 Cl6 2.432(2) . ? Sn1 Cl4 2.432(2) . ? Sn1 Cl5 2.4528(19) . ? P1 C3 1.880(8) . ? P1 P3 2.220(3) . ? P1 P2 2.231(3) . ? P1 P3A 2.232(9) . ? P2 C6 1.788(8) . ? P2 C12 1.802(7) . ? P2 C1 1.827(8) . ? C6 C7 1.387(10) . ? C6 C11 1.397(10) . ? C11 C10 1.367(12) . ? C11 H11 0.9500 . ? C10 C9 1.385(12) . ? C10 H10 0.9500 . ? C9 C8 1.388(11) . ? C9 H9 0.9500 . ? C8 C7 1.382(11) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C12 C17 1.356(11) . ? C12 C13 1.400(12) . ? C13 C14 1.390(13) . ? C13 H13 0.9500 . ? C14 C15 1.347(14) . ? C14 H14 0.9500 . ? C15 C16 1.359(13) . ? C15 H15 0.9500 . ? C16 C17 1.395(12) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.399(11) . ? C18 C19 1.401(11) . ? C18 P3 1.764(8) . ? C18 P3A 2.15(3) . ? C19 C20 1.355(12) . ? C19 H19 0.9500 . ? C20 C21 1.375(13) . ? C20 H20 0.9500 . ? C21 C22 1.375(12) . ? C21 H21 0.9500 . ? C22 C23 1.390(11) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? P3 C24 1.789(10) . ? P3 C2 1.803(9) . ? C24 C29 1.388(14) . ? C24 C25 1.395(14) . ? C25 C26 1.393(14) . ? C25 H25 0.9500 . ? C26 C27 1.36(2) . ? C26 H26 0.9500 . ? C27 C28 1.35(2) . ? C27 H27 0.9500 . ? C28 C29 1.407(13) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C2 C1 1.514(11) . ? C2 H2B 0.9900 . ? C2 H2A 0.9900 . ? P3A C24A 1.72(12) . ? P3A C2A 2.02(8) . ? C24A C25A 1.45(14) . ? C24A C29A 1.51(14) . ? C25A C26A 1.4(2) . ? C25A H25A 0.9500 . ? C26A C27A 1.4(2) . ? C26A H26A 0.9500 . ? C27A C28A 1.49(15) . ? C27A H27A 0.9500 . ? C28A C29A 1.16(11) . ? C28A H28A 0.9500 . ? C29A H29A 0.9500 . ? C2A C1 1.11(8) . ? C2A H2AC 0.9900 . ? C2A H2AA 0.9900 . ? C1 H2AB 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.508(11) . ? C3 C5 1.540(11) . ? C3 H3 1.0000 . ? C5 H5A 0.9800 . ? C5 H5C 0.9800 . ? C5 H5B 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4 H4A 0.9800 . ? C30 Cl7 1.738(9) . ? C30 Cl8 1.755(8) . ? C30 Cl9 1.761(8) . ? C30 H30 1.0000 . ? C31 Cl10 1.7570 . ? C31 Cl12 1.7584 . ? C31 Cl11 1.7634 . ? C31 H31 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 Cl1 Sn1 Cl2 90.71(9) . . ? Cl1 Sn1 Cl3 92.06(11) . . ? Cl2 Sn1 Cl3 90.36(8) . . ? Cl1 Sn1 Cl6 89.53(10) . . ? Cl2 Sn1 Cl6 90.98(7) . . ? Cl3 Sn1 Cl6 177.90(8) . . ? Cl1 Sn1 Cl4 177.32(10) . . ? Cl2 Sn1 Cl4 88.91(8) . . ? Cl3 Sn1 Cl4 90.59(9) . . ? Cl6 Sn1 Cl4 87.82(8) . . ? Cl1 Sn1 Cl5 91.09(8) . . ? Cl2 Sn1 Cl5 177.91(8) . . ? Cl3 Sn1 Cl5 88.52(8) . . ? Cl6 Sn1 Cl5 90.09(7) . . ? Cl4 Sn1 Cl5 89.34(7) . . ? C3 P1 P3 105.9(3) . . ? C3 P1 P2 103.9(3) . . ? P3 P1 P2 86.09(11) . . ? C3 P1 P3A 122.0(8) . . ? P3 P1 P3A 16.3(7) . . ? P2 P1 P3A 85.0(6) . . ? C6 P2 C12 109.6(3) . . ? C6 P2 C1 111.1(4) . . ? C12 P2 C1 108.9(4) . . ? C6 P2 P1 111.1(3) . . ? C12 P2 P1 108.1(3) . . ? C1 P2 P1 108.0(3) . . ? C7 C6 C11 120.4(7) . . ? C7 C6 P2 120.2(6) . . ? C11 C6 P2 119.1(6) . . ? C10 C11 C6 119.1(7) . . ? C10 C11 H11 120.5 . . ? C6 C11 H11 120.5 . . ? C11 C10 C9 121.3(8) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C9 C8 119.3(8) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C7 C8 C9 120.3(7) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C7 C6 119.5(7) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C17 C12 C13 121.1(7) . . ? C17 C12 P2 121.2(6) . . ? C13 C12 P2 117.7(6) . . ? C14 C13 C12 118.1(9) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C15 C14 C13 121.4(9) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.2(8) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 122.1(9) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C12 C17 C16 117.9(9) . . ? C12 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? C23 C18 C19 119.5(7) . . ? C23 C18 P3 118.8(6) . . ? C19 C18 P3 121.4(6) . . ? C23 C18 P3A 106.1(9) . . ? C19 C18 P3A 132.5(9) . . ? P3 C18 P3A 14.7(6) . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.8(8) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 120.2(8) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.4(9) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 118.9(8) . . ? C22 C23 H23 120.6 . . ? C18 C23 H23 120.6 . . ? C18 P3 C24 109.1(4) . . ? C18 P3 C2 109.8(4) . . ? C24 P3 C2 112.2(5) . . ? C18 P3 P1 119.2(3) . . ? C24 P3 P1 101.1(3) . . ? C2 P3 P1 105.2(3) . . ? C29 C24 C25 120.2(10) . . ? C29 C24 P3 119.6(7) . . ? C25 C24 P3 120.2(9) . . ? C26 C25 C24 118.5(11) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 121.5(13) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C28 C27 C26 119.7(13) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 121.5(13) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C24 C29 C28 118.4(11) . . ? C24 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? C1 C2 P3 109.8(6) . . ? C1 C2 H2B 109.7 . . ? P3 C2 H2B 109.7 . . ? C1 C2 H2A 109.7 . . ? P3 C2 H2A 109.7 . . ? H2B C2 H2A 108.2 . . ? C24A P3A C2A 113(5) . . ? C24A P3A C18 123(4) . . ? C2A P3A C18 110(3) . . ? C24A P3A P1 105(4) . . ? C2A P3A P1 99(2) . . ? C18 P3A P1 103.6(10) . . ? C25A C24A C29A 122(10) . . ? C25A C24A P3A 110(9) . . ? C29A C24A P3A 129(8) . . ? C26A C25A C24A 110(10) . . ? C26A C25A H25A 125.0 . . ? C24A C25A H25A 125.0 . . ? C25A C26A C27A 133(10) . . ? C25A C26A H26A 113.6 . . ? C27A C26A H26A 113.6 . . ? C26A C27A C28A 105(10) . . ? C26A C27A H27A 127.5 . . ? C28A C27A H27A 127.5 . . ? C29A C28A C27A 132(10) . . ? C29A C28A H28A 113.8 . . ? C27A C28A H28A 113.8 . . ? C28A C29A C24A 117(10) . . ? C28A C29A H29A 121.6 . . ? C24A C29A H29A 121.6 . . ? C1 C2A P3A 126(5) . . ? C1 C2A H2AC 105.9 . . ? P3A C2A H2AC 105.9 . . ? C1 C2A H2AA 105.9 . . ? P3A C2A H2AA 105.9 . . ? H2AC C2A H2AA 106.3 . . ? C2A C1 C2 41(4) . . ? C2A C1 P2 112(4) . . ? C2 C1 P2 112.6(6) . . ? C2A C1 H2AB 70.8 . . ? C2 C1 H2AB 109.1 . . ? P2 C1 H2AB 109.1 . . ? C2A C1 H1B 136.2 . . ? C2 C1 H1B 109.1 . . ? P2 C1 H1B 109.1 . . ? H2AB C1 H1B 107.8 . . ? C4 C3 C5 110.2(7) . . ? C4 C3 P1 106.8(5) . . ? C5 C3 P1 108.0(5) . . ? C4 C3 H3 110.6 . . ? C5 C3 H3 110.6 . . ? P1 C3 H3 110.6 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? Cl7 C30 Cl8 111.1(5) . . ? Cl7 C30 Cl9 111.3(5) . . ? Cl8 C30 Cl9 109.3(4) . . ? Cl7 C30 H30 108.4 . . ? Cl8 C30 H30 108.4 . . ? Cl9 C30 H30 108.4 . . ? Cl10 C31 Cl12 110.9 . . ? Cl10 C31 Cl11 109.9 . . ? Cl12 C31 Cl11 109.3 . . ? Cl10 C31 H31 108.9 . . ? Cl12 C31 H31 108.9 . . ? Cl11 C31 H31 108.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.824 _refine_diff_density_min -1.271 _refine_diff_density_rms 0.146 #====================================================================== data_11c _database_code_depnum_ccdc_archive 'CCDC 664572' #====================================================================== _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C38 H33 P3, Sn Cl6, 2(C H Cl3)' _chemical_formula_sum 'C40 H35 Cl12 P3 Sn' _chemical_formula_weight 1152.68 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_length_a 10.7742(10) _cell_length_b 11.4878(10) _cell_length_c 19.2490(17) _cell_angle_alpha 89.558(2) _cell_angle_beta 82.088(2) _cell_angle_gamma 82.033(2) _cell_volume 2336.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2596 _cell_measurement_theta_min 2.442 _cell_measurement_theta_max 27.009 _exptl_crystal_description block _exptl_crystal_colour clear_pale_colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 1.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (G.M.Sheldrick, 1998)' _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 4.51 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 CCD 1K area detector' _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 16252 _diffrn_reflns_av_R_equivalents 0.1124 _diffrn_reflns_av_sigmaI/netI 0.1900 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9111 _reflns_number_gt 5008 _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. Althouth the data is weak and noisy (hence the low quality and poorly defined thermal ellipsoids which were restrained to sensible sizes and shapes using SIMU/DELU in SHELXTL), the crystal and molecular structure is in no doubt. Efforts were made to examine the possibility of disorder, twinning etc., but there was no evidence to support these. ; _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^)+(0.0000P)^2^+20.8628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9111 _refine_ls_number_parameters 509 _refine_ls_number_restraints 299 _refine_ls_R_factor_all 0.1822 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.7437(2) 0.2961(2) 0.79281(13) 0.0145(6) Uani 1 1 d . . . P2 P 0.6437(2) 0.1812(2) 0.73476(13) 0.0159(6) Uani 1 1 d . . . P3 P 0.9137(2) 0.1684(2) 0.79837(13) 0.0134(5) Uani 1 1 d . . . C1 C 0.7452(10) 0.0664(8) 0.6832(5) 0.018(2) Uani 1 1 d U . . C2 C 0.8102(9) -0.0303(8) 0.7166(6) 0.019(2) Uani 1 1 d U . . C3 C 0.8054(9) -0.0397(8) 0.7945(6) 0.020(2) Uani 1 1 d U . . C4 C 0.8505(9) 0.0401(8) 0.8354(5) 0.015(2) Uani 1 1 d U . . C5 C 0.7971(9) 0.4095(8) 0.7300(5) 0.018(2) Uani 1 1 d . . . H5A H 0.8790 0.4299 0.7403 0.022 Uiso 1 1 calc R . . H5B H 0.8096 0.3775 0.6815 0.022 Uiso 1 1 calc R . . C6 C 0.6995(10) 0.5192(9) 0.7357(6) 0.027(3) Uani 1 1 d . . . H6A H 0.7280 0.5773 0.7018 0.040 Uiso 1 1 calc R . . H6B H 0.6893 0.5522 0.7833 0.040 Uiso 1 1 calc R . . H6C H 0.6183 0.4987 0.7258 0.040 Uiso 1 1 calc R . . C7 C 0.7591(10) 0.0698(9) 0.6093(6) 0.029(2) Uani 1 1 d U . . H7A H 0.7192 0.1354 0.5864 0.035 Uiso 1 1 calc R . . C8 C 0.8314(10) -0.0228(11) 0.5698(6) 0.035(3) Uani 1 1 d U . . H8A H 0.8416 -0.0195 0.5201 0.042 Uiso 1 1 calc R . . C9 C 0.8879(11) -0.1185(11) 0.6019(6) 0.037(3) Uani 1 1 d U . . H9A H 0.9343 -0.1825 0.5744 0.044 Uiso 1 1 calc R . . C10 C 0.8777(11) -0.1228(10) 0.6754(6) 0.033(3) Uani 1 1 d U . . H10A H 0.9174 -0.1897 0.6971 0.040 Uiso 1 1 calc R . . C11 C 0.7570(10) -0.1345(9) 0.8284(6) 0.025(2) Uani 1 1 d U . . H11A H 0.7241 -0.1892 0.8016 0.031 Uiso 1 1 calc R . . C12 C 0.7549(10) -0.1517(9) 0.8990(6) 0.030(2) Uani 1 1 d U . . H12A H 0.7223 -0.2183 0.9200 0.036 Uiso 1 1 calc R . . C13 C 0.7997(10) -0.0732(9) 0.9395(6) 0.028(2) Uani 1 1 d U . . H13A H 0.7977 -0.0845 0.9886 0.033 Uiso 1 1 calc R . . C14 C 0.8478(9) 0.0227(8) 0.9075(5) 0.019(2) Uani 1 1 d U . . H14A H 0.8793 0.0773 0.9350 0.023 Uiso 1 1 calc R . . C15 C 0.5438(9) 0.2764(8) 0.6853(5) 0.017(2) Uani 1 1 d U . . C16 C 0.4139(10) 0.2987(8) 0.7107(6) 0.025(2) Uani 1 1 d U . . H16A H 0.3807 0.2609 0.7518 0.030 Uiso 1 1 calc R . . C17 C 0.3362(10) 0.3747(9) 0.6763(6) 0.024(2) Uani 1 1 d U . . H17A H 0.2483 0.3885 0.6932 0.028 Uiso 1 1 calc R . . C18 C 0.3833(11) 0.4329(9) 0.6165(6) 0.031(3) Uani 1 1 d U . . H18A H 0.3277 0.4841 0.5920 0.038 Uiso 1 1 calc R . . C19 C 0.5103(10) 0.4153(9) 0.5936(5) 0.023(2) Uani 1 1 d U . . H19A H 0.5433 0.4571 0.5541 0.028 Uiso 1 1 calc R . . C20 C 0.5918(10) 0.3373(9) 0.6274(5) 0.022(2) Uani 1 1 d U . . H20A H 0.6800 0.3255 0.6110 0.027 Uiso 1 1 calc R . . C21 C 0.5451(9) 0.1063(8) 0.7995(5) 0.016(2) Uani 1 1 d U . . C22 C 0.5305(8) 0.1322(8) 0.8703(5) 0.016(2) Uani 1 1 d U . . H22A H 0.5696 0.1938 0.8867 0.019 Uiso 1 1 calc R . . C23 C 0.4581(10) 0.0676(9) 0.9177(5) 0.024(2) Uani 1 1 d U . . H23A H 0.4477 0.0858 0.9664 0.029 Uiso 1 1 calc R . . C24 C 0.4020(10) -0.0218(9) 0.8945(6) 0.027(2) Uani 1 1 d U . . H24A H 0.3542 -0.0666 0.9270 0.033 Uiso 1 1 calc R . . C25 C 0.4156(9) -0.0469(8) 0.8223(6) 0.024(2) Uani 1 1 d U . . H25A H 0.3755 -0.1081 0.8062 0.029 Uiso 1 1 calc R . . C26 C 0.4873(10) 0.0170(9) 0.7742(6) 0.026(2) Uani 1 1 d U . . H26A H 0.4965 0.0001 0.7254 0.031 Uiso 1 1 calc R . . C27 C 1.0304(9) 0.1237(8) 0.7241(5) 0.018(2) Uani 1 1 d U . . C28 C 1.0602(9) 0.1992(8) 0.6708(5) 0.019(2) Uani 1 1 d U . . H28A H 1.0117 0.2746 0.6691 0.023 Uiso 1 1 calc R . . C29 C 1.1647(10) 0.1635(10) 0.6180(6) 0.029(3) Uani 1 1 d U . . H29A H 1.1872 0.2141 0.5805 0.035 Uiso 1 1 calc R . . C30 C 1.2326(10) 0.0525(9) 0.6229(5) 0.026(2) Uani 1 1 d U . . H30A H 1.3020 0.0275 0.5878 0.031 Uiso 1 1 calc R . . C31 C 1.2030(10) -0.0223(9) 0.6768(6) 0.029(3) Uani 1 1 d U . . H31A H 1.2529 -0.0968 0.6792 0.035 Uiso 1 1 calc R . . C32 C 1.1018(10) 0.0106(9) 0.7268(5) 0.027(3) Uani 1 1 d U . . H32A H 1.0792 -0.0419 0.7633 0.032 Uiso 1 1 calc R . . C33 C 0.9905(10) 0.2371(9) 0.8621(5) 0.020(2) Uani 1 1 d U . . C34 C 1.1240(10) 0.2214(9) 0.8530(6) 0.026(2) Uani 1 1 d U . . H34A H 1.1718 0.1753 0.8152 0.032 Uiso 1 1 calc R . . C35 C 1.1825(11) 0.2745(9) 0.9002(6) 0.026(2) Uani 1 1 d U . . H35A H 1.2723 0.2672 0.8945 0.031 Uiso 1 1 calc R . . C36 C 1.1115(11) 0.3395(9) 0.9566(6) 0.031(3) Uani 1 1 d U . . H36A H 1.1531 0.3740 0.9900 0.038 Uiso 1 1 calc R . . C37 C 0.9828(10) 0.3535(8) 0.9640(6) 0.022(2) Uani 1 1 d U . . H37A H 0.9351 0.3993 1.0019 0.026 Uiso 1 1 calc R . . C38 C 0.9199(10) 0.3008(8) 0.9158(5) 0.017(2) Uani 1 1 d U . . H38A H 0.8301 0.3099 0.9210 0.021 Uiso 1 1 calc R . . Sn1 Sn 0.5000 0.5000 0.0000 0.0156(3) Uani 1 2 d S . . Cl1 Cl -0.0842(2) 0.3175(2) 0.53273(13) 0.0225(6) Uani 1 1 d . . . Cl2 Cl 0.2111(2) 0.3922(2) 0.46978(14) 0.0252(6) Uani 1 1 d . . . Cl3 Cl 0.0394(2) 0.5270(2) 0.61992(14) 0.0245(6) Uani 1 1 d . . . Sn2 Sn 0.0000 0.5000 0.5000 0.0144(2) Uani 1 2 d S . . Cl4 Cl 0.5729(3) 0.5548(2) 0.10800(14) 0.0233(6) Uani 1 1 d . . . Cl5 Cl 0.3076(2) 0.4538(2) 0.06960(13) 0.0223(6) Uani 1 1 d . . . Cl6 Cl 0.6009(2) 0.2992(2) 0.01355(14) 0.0242(6) Uani 1 1 d . . . C1S C 0.8249(12) 0.3404(10) 0.1571(6) 0.043(3) Uani 1 1 d . . . H1S H 0.7681 0.3853 0.1263 0.051 Uiso 1 1 calc R . . Cl1S Cl 0.7399(5) 0.3293(3) 0.2398(2) 0.0911(16) Uani 1 1 d . . . Cl2S Cl 0.8762(3) 0.1992(2) 0.12046(16) 0.0370(7) Uani 1 1 d . . . Cl3S Cl 0.9562(4) 0.4143(3) 0.1604(2) 0.0718(13) Uani 1 1 d . . . C2S C 0.5101(10) 0.2538(9) 0.4343(5) 0.025(3) Uani 1 1 d . . . H2S H 0.4568 0.3283 0.4526 0.030 Uiso 1 1 calc R . . Cl4S Cl 0.4843(3) 0.2328(3) 0.34817(19) 0.0553(10) Uani 1 1 d . . . Cl5S Cl 0.4668(3) 0.1394(3) 0.4883(2) 0.0674(12) Uani 1 1 d . . . Cl6S Cl 0.6687(3) 0.2686(2) 0.43824(15) 0.0313(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0122(14) 0.0148(13) 0.0172(14) -0.0011(11) -0.0040(11) -0.0025(10) P2 0.0163(15) 0.0194(14) 0.0138(14) -0.0013(11) -0.0069(11) -0.0038(11) P3 0.0111(14) 0.0140(13) 0.0144(14) 0.0000(11) -0.0009(11) -0.0006(10) C1 0.024(6) 0.014(5) 0.019(5) -0.009(4) -0.002(4) -0.011(4) C2 0.015(6) 0.011(5) 0.035(5) -0.010(4) -0.008(4) -0.007(4) C3 0.012(5) 0.015(5) 0.031(5) -0.001(4) 0.000(4) -0.004(4) C4 0.014(5) 0.009(4) 0.019(5) 0.000(4) 0.006(4) 0.002(4) C5 0.025(6) 0.013(5) 0.017(6) -0.001(4) -0.002(5) -0.004(4) C6 0.024(7) 0.022(6) 0.029(7) 0.007(5) 0.004(5) 0.006(5) C7 0.026(7) 0.030(6) 0.031(5) -0.008(5) 0.000(5) -0.005(4) C8 0.021(7) 0.062(7) 0.019(6) -0.021(5) 0.001(5) 0.004(5) C9 0.021(7) 0.046(6) 0.039(6) -0.022(5) 0.003(5) 0.006(5) C10 0.029(7) 0.027(6) 0.045(6) -0.020(5) -0.012(5) -0.002(4) C11 0.026(6) 0.018(5) 0.036(5) -0.004(4) -0.016(5) -0.006(4) C12 0.023(6) 0.022(5) 0.044(6) 0.007(5) -0.002(5) -0.005(5) C13 0.026(6) 0.036(6) 0.020(5) 0.005(4) 0.002(5) -0.005(5) C14 0.012(6) 0.019(5) 0.026(5) -0.005(4) -0.003(5) 0.003(4) C15 0.011(5) 0.019(5) 0.019(5) -0.001(4) -0.005(4) 0.006(4) C16 0.019(5) 0.018(5) 0.039(7) 0.011(5) -0.004(4) -0.003(4) C17 0.013(5) 0.025(6) 0.032(6) -0.003(5) -0.005(4) 0.000(4) C18 0.032(6) 0.020(6) 0.045(7) 0.007(5) -0.018(5) 0.001(5) C19 0.038(6) 0.031(6) 0.002(5) 0.001(4) -0.005(4) -0.009(5) C20 0.016(5) 0.033(6) 0.021(6) -0.009(4) -0.008(4) -0.009(4) C21 0.009(5) 0.018(5) 0.020(5) -0.005(4) -0.002(4) 0.000(4) C22 0.005(5) 0.022(5) 0.019(5) -0.003(4) -0.002(4) 0.004(4) C23 0.024(6) 0.033(6) 0.016(5) 0.008(4) -0.005(4) -0.005(5) C24 0.025(6) 0.023(5) 0.031(5) 0.007(5) 0.003(5) 0.002(4) C25 0.015(6) 0.016(5) 0.038(6) -0.003(4) 0.003(5) 0.002(4) C26 0.032(7) 0.026(6) 0.019(5) -0.009(4) -0.003(5) -0.004(5) C27 0.020(6) 0.024(5) 0.011(5) 0.002(4) -0.003(4) -0.002(4) C28 0.018(6) 0.019(5) 0.020(5) 0.000(4) -0.008(4) 0.006(4) C29 0.020(6) 0.038(6) 0.024(6) 0.007(5) 0.009(4) 0.000(5) C30 0.016(6) 0.040(6) 0.017(5) -0.003(4) 0.008(4) 0.002(4) C31 0.016(6) 0.025(5) 0.043(7) 0.006(5) 0.001(5) 0.008(4) C32 0.030(7) 0.027(5) 0.019(6) 0.013(5) 0.008(4) 0.000(5) C33 0.024(5) 0.027(6) 0.013(5) 0.001(4) -0.008(4) -0.013(5) C34 0.023(5) 0.020(5) 0.037(6) -0.010(5) -0.007(5) 0.002(4) C35 0.024(6) 0.020(6) 0.035(7) -0.001(5) -0.012(5) -0.003(4) C36 0.031(6) 0.027(6) 0.042(7) -0.007(5) -0.018(5) -0.008(5) C37 0.027(5) 0.011(5) 0.030(6) -0.007(4) -0.015(5) -0.002(4) C38 0.020(5) 0.018(5) 0.018(5) -0.005(4) -0.013(4) -0.006(4) Sn1 0.0140(6) 0.0148(5) 0.0190(6) -0.0012(4) -0.0046(5) -0.0031(4) Cl1 0.0198(15) 0.0227(13) 0.0245(15) 0.0003(11) 0.0006(11) -0.0053(11) Cl2 0.0132(14) 0.0303(15) 0.0300(16) 0.0002(12) -0.0021(12) 0.0037(11) Cl3 0.0216(16) 0.0325(15) 0.0213(15) -0.0003(12) -0.0066(12) -0.0066(12) Sn2 0.0112(6) 0.0181(5) 0.0132(6) -0.0020(4) -0.0001(4) -0.0010(4) Cl4 0.0224(15) 0.0267(14) 0.0232(15) -0.0040(12) -0.0075(12) -0.0073(11) Cl5 0.0171(15) 0.0278(14) 0.0237(15) 0.0001(11) -0.0037(11) -0.0080(11) Cl6 0.0274(16) 0.0176(13) 0.0263(15) 0.0025(11) -0.0026(12) -0.0001(11) C1S 0.050(9) 0.040(8) 0.032(8) 0.012(6) 0.003(6) 0.007(6) Cl1S 0.150(5) 0.047(2) 0.056(3) 0.004(2) 0.048(3) -0.006(3) Cl2S 0.0373(19) 0.0318(16) 0.0394(18) 0.0049(14) -0.0003(14) -0.0009(13) Cl3S 0.108(4) 0.053(2) 0.067(3) 0.013(2) -0.032(3) -0.039(2) C2S 0.023(6) 0.021(6) 0.030(7) 0.004(5) -0.001(5) -0.001(5) Cl4S 0.030(2) 0.082(3) 0.050(2) -0.028(2) -0.0141(17) 0.0168(18) Cl5S 0.038(2) 0.046(2) 0.110(3) 0.034(2) 0.015(2) -0.0032(16) Cl6S 0.0216(16) 0.0346(16) 0.0371(18) -0.0062(14) -0.0034(13) -0.0024(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C5 1.867(9) . ? P1 P3 2.197(4) . ? P1 P2 2.214(3) . ? P2 C15 1.789(9) . ? P2 C1 1.800(10) . ? P2 C21 1.815(10) . ? P3 C27 1.796(10) . ? P3 C4 1.809(9) . ? P3 C33 1.813(10) . ? C1 C7 1.412(14) . ? C1 C2 1.426(13) . ? C2 C10 1.388(14) . ? C2 C3 1.496(14) . ? C3 C4 1.392(13) . ? C3 C11 1.392(13) . ? C4 C14 1.397(13) . ? C5 C6 1.519(13) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.391(15) . ? C7 H7A 0.9500 . ? C8 C9 1.368(16) . ? C8 H8A 0.9500 . ? C9 C10 1.404(16) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.368(15) . ? C11 H11A 0.9500 . ? C12 C13 1.375(14) . ? C12 H12A 0.9500 . ? C13 C14 1.386(13) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.389(13) . ? C15 C16 1.406(13) . ? C16 C17 1.358(13) . ? C16 H16A 0.9500 . ? C17 C18 1.397(14) . ? C17 H17A 0.9500 . ? C18 C19 1.366(15) . ? C18 H18A 0.9500 . ? C19 C20 1.389(14) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.381(13) . ? C21 C26 1.394(13) . ? C22 C23 1.394(13) . ? C22 H22A 0.9500 . ? C23 C24 1.368(14) . ? C23 H23A 0.9500 . ? C24 C25 1.404(14) . ? C24 H24A 0.9500 . ? C25 C26 1.394(14) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.372(13) . ? C27 C32 1.419(13) . ? C28 C29 1.426(14) . ? C28 H28A 0.9500 . ? C29 C30 1.389(14) . ? C29 H29A 0.9500 . ? C30 C31 1.373(14) . ? C30 H30A 0.9500 . ? C31 C32 1.365(14) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.351(14) . ? C33 C34 1.411(14) . ? C34 C35 1.367(14) . ? C34 H34A 0.9500 . ? C35 C36 1.395(15) . ? C35 H35A 0.9500 . ? C36 C37 1.361(14) . ? C36 H36A 0.9500 . ? C37 C38 1.407(12) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? Sn1 Cl5 2.430(2) . ? Sn1 Cl5 2.430(2) 2_665 ? Sn1 Cl4 2.437(2) 2_665 ? Sn1 Cl4 2.437(3) . ? Sn1 Cl6 2.438(2) 2_665 ? Sn1 Cl6 2.438(2) . ? Cl1 Sn2 2.443(2) . ? Cl2 Sn2 2.431(3) . ? Cl3 Sn2 2.434(3) . ? Sn2 Cl2 2.431(3) 2_566 ? Sn2 Cl3 2.434(3) 2_566 ? Sn2 Cl1 2.443(2) 2_566 ? C1S Cl1S 1.737(12) . ? C1S Cl3S 1.756(13) . ? C1S Cl2S 1.759(12) . ? C1S H1S 1.0000 . ? C2S Cl4S 1.742(11) . ? C2S Cl5S 1.744(10) . ? C2S Cl6S 1.752(10) . ? C2S H2S 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 C5 P1 P3 104.9(3) . . ? C5 P1 P2 106.8(3) . . ? P3 P1 P2 96.59(13) . . ? C15 P2 C1 114.0(5) . . ? C15 P2 C21 108.8(5) . . ? C1 P2 C21 105.5(4) . . ? C15 P2 P1 106.4(3) . . ? C1 P2 P1 114.8(3) . . ? C21 P2 P1 107.2(3) . . ? C27 P3 C4 109.0(4) . . ? C27 P3 C33 107.9(5) . . ? C4 P3 C33 110.3(5) . . ? C27 P3 P1 123.8(3) . . ? C4 P3 P1 103.3(3) . . ? C33 P3 P1 102.0(4) . . ? C7 C1 C2 119.3(9) . . ? C7 C1 P2 120.3(8) . . ? C2 C1 P2 120.4(8) . . ? C10 C2 C1 118.8(10) . . ? C10 C2 C3 117.9(9) . . ? C1 C2 C3 123.3(9) . . ? C4 C3 C11 117.4(10) . . ? C4 C3 C2 123.4(8) . . ? C11 C3 C2 119.1(9) . . ? C3 C4 C14 120.1(9) . . ? C3 C4 P3 122.1(7) . . ? C14 C4 P3 117.8(7) . . ? C6 C5 P1 110.4(7) . . ? C6 C5 H5A 109.6 . . ? P1 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? P1 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C1 120.0(11) . . ? C8 C7 H7A 120.0 . . ? C1 C7 H7A 120.0 . . ? C9 C8 C7 120.7(11) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 120.4(11) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C2 C10 C9 120.7(11) . . ? C2 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C12 C11 C3 122.4(10) . . ? C12 C11 H11A 118.8 . . ? C3 C11 H11A 118.8 . . ? C11 C12 C13 120.3(10) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C12 C13 C14 118.8(10) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C13 C14 C4 121.0(9) . . ? C13 C14 H14A 119.5 . . ? C4 C14 H14A 119.5 . . ? C20 C15 C16 119.3(9) . . ? C20 C15 P2 122.3(8) . . ? C16 C15 P2 118.1(7) . . ? C17 C16 C15 119.7(10) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 121.1(10) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 119.2(10) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 120.9(10) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C15 119.7(10) . . ? C19 C20 H20A 120.2 . . ? C15 C20 H20A 120.2 . . ? C22 C21 C26 121.0(9) . . ? C22 C21 P2 122.6(7) . . ? C26 C21 P2 116.3(8) . . ? C21 C22 C23 119.8(9) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 120.4(10) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 119.6(10) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C26 C25 C24 120.7(10) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C21 118.4(10) . . ? C25 C26 H26A 120.8 . . ? C21 C26 H26A 120.8 . . ? C28 C27 C32 120.7(9) . . ? C28 C27 P3 122.0(8) . . ? C32 C27 P3 116.9(7) . . ? C27 C28 C29 119.3(9) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C30 C29 C28 118.1(9) . . ? C30 C29 H29A 121.0 . . ? C28 C29 H29A 121.0 . . ? C31 C30 C29 122.4(10) . . ? C31 C30 H30A 118.8 . . ? C29 C30 H30A 118.8 . . ? C32 C31 C30 119.8(10) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C27 119.7(9) . . ? C31 C32 H32A 120.1 . . ? C27 C32 H32A 120.1 . . ? C38 C33 C34 122.4(9) . . ? C38 C33 P3 119.9(8) . . ? C34 C33 P3 117.7(8) . . ? C35 C34 C33 118.0(10) . . ? C35 C34 H34A 121.0 . . ? C33 C34 H34A 121.0 . . ? C34 C35 C36 120.5(11) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C37 C36 C35 120.2(10) . . ? C37 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C36 C37 C38 120.6(10) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? C33 C38 C37 118.3(10) . . ? C33 C38 H38A 120.9 . . ? C37 C38 H38A 120.9 . . ? Cl5 Sn1 Cl5 180.00(15) . 2_665 ? Cl5 Sn1 Cl4 91.30(8) . 2_665 ? Cl5 Sn1 Cl4 88.70(8) 2_665 2_665 ? Cl5 Sn1 Cl4 88.70(8) . . ? Cl5 Sn1 Cl4 91.30(8) 2_665 . ? Cl4 Sn1 Cl4 180.00(5) 2_665 . ? Cl5 Sn1 Cl6 90.05(8) . 2_665 ? Cl5 Sn1 Cl6 89.95(8) 2_665 2_665 ? Cl4 Sn1 Cl6 89.12(9) 2_665 2_665 ? Cl4 Sn1 Cl6 90.88(9) . 2_665 ? Cl5 Sn1 Cl6 89.95(8) . . ? Cl5 Sn1 Cl6 90.05(8) 2_665 . ? Cl4 Sn1 Cl6 90.88(9) 2_665 . ? Cl4 Sn1 Cl6 89.12(9) . . ? Cl6 Sn1 Cl6 180.00(12) 2_665 . ? Cl2 Sn2 Cl2 180.00(13) 2_566 . ? Cl2 Sn2 Cl3 89.30(9) 2_566 . ? Cl2 Sn2 Cl3 90.70(9) . . ? Cl2 Sn2 Cl3 90.70(9) 2_566 2_566 ? Cl2 Sn2 Cl3 89.30(9) . 2_566 ? Cl3 Sn2 Cl3 180.0 . 2_566 ? Cl2 Sn2 Cl1 89.36(9) 2_566 . ? Cl2 Sn2 Cl1 90.64(9) . . ? Cl3 Sn2 Cl1 90.30(8) . . ? Cl3 Sn2 Cl1 89.70(8) 2_566 . ? Cl2 Sn2 Cl1 90.64(9) 2_566 2_566 ? Cl2 Sn2 Cl1 89.36(9) . 2_566 ? Cl3 Sn2 Cl1 89.70(8) . 2_566 ? Cl3 Sn2 Cl1 90.30(8) 2_566 2_566 ? Cl1 Sn2 Cl1 180.0 . 2_566 ? Cl1S C1S Cl3S 111.6(7) . . ? Cl1S C1S Cl2S 109.8(6) . . ? Cl3S C1S Cl2S 109.5(7) . . ? Cl1S C1S H1S 108.6 . . ? Cl3S C1S H1S 108.6 . . ? Cl2S C1S H1S 108.6 . . ? Cl4S C2S Cl5S 111.8(6) . . ? Cl4S C2S Cl6S 111.2(6) . . ? Cl5S C2S Cl6S 109.6(6) . . ? Cl4S C2S H2S 108.1 . . ? Cl5S C2S H2S 108.1 . . ? Cl6S C2S H2S 108.1 . . ? 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 C5 P1 P2 C15 -43.9(5) . . . . ? P3 P1 P2 C15 -151.7(4) . . . . ? C5 P1 P2 C1 83.1(5) . . . . ? P3 P1 P2 C1 -24.7(4) . . . . ? C5 P1 P2 C21 -160.2(5) . . . . ? P3 P1 P2 C21 92.0(3) . . . . ? C5 P1 P3 C27 -38.2(5) . . . . ? P2 P1 P3 C27 71.2(4) . . . . ? C5 P1 P3 C4 -162.3(5) . . . . ? P2 P1 P3 C4 -52.9(4) . . . . ? C5 P1 P3 C33 83.2(5) . . . . ? P2 P1 P3 C33 -167.4(3) . . . . ? C15 P2 C1 C7 11.9(10) . . . . ? C21 P2 C1 C7 131.1(8) . . . . ? P1 P2 C1 C7 -111.2(8) . . . . ? C15 P2 C1 C2 -166.8(7) . . . . ? C21 P2 C1 C2 -47.5(9) . . . . ? P1 P2 C1 C2 70.2(8) . . . . ? C7 C1 C2 C10 -4.9(14) . . . . ? P2 C1 C2 C10 173.8(8) . . . . ? C7 C1 C2 C3 177.6(9) . . . . ? P2 C1 C2 C3 -3.7(13) . . . . ? C10 C2 C3 C4 120.0(11) . . . . ? C1 C2 C3 C4 -62.5(13) . . . . ? C10 C2 C3 C11 -58.0(13) . . . . ? C1 C2 C3 C11 119.5(11) . . . . ? C11 C3 C4 C14 0.9(14) . . . . ? C2 C3 C4 C14 -177.2(9) . . . . ? C11 C3 C4 P3 -179.0(8) . . . . ? C2 C3 C4 P3 2.9(14) . . . . ? C27 P3 C4 C3 -50.9(9) . . . . ? C33 P3 C4 C3 -169.2(8) . . . . ? P1 P3 C4 C3 82.3(8) . . . . ? C27 P3 C4 C14 129.2(8) . . . . ? C33 P3 C4 C14 10.9(9) . . . . ? P1 P3 C4 C14 -97.5(7) . . . . ? P3 P1 C5 C6 -164.8(6) . . . . ? P2 P1 C5 C6 93.4(7) . . . . ? C2 C1 C7 C8 2.7(15) . . . . ? P2 C1 C7 C8 -176.0(8) . . . . ? C1 C7 C8 C9 1.0(17) . . . . ? C7 C8 C9 C10 -2.4(18) . . . . ? C1 C2 C10 C9 3.6(15) . . . . ? C3 C2 C10 C9 -178.8(9) . . . . ? C8 C9 C10 C2 0.0(17) . . . . ? C4 C3 C11 C12 -1.2(16) . . . . ? C2 C3 C11 C12 177.0(10) . . . . ? C3 C11 C12 C13 1.1(17) . . . . ? C11 C12 C13 C14 -0.6(16) . . . . ? C12 C13 C14 C4 0.2(16) . . . . ? C3 C4 C14 C13 -0.4(15) . . . . ? P3 C4 C14 C13 179.5(8) . . . . ? C1 P2 C15 C20 -56.4(10) . . . . ? C21 P2 C15 C20 -173.7(8) . . . . ? P1 P2 C15 C20 71.1(9) . . . . ? C1 P2 C15 C16 130.2(8) . . . . ? C21 P2 C15 C16 12.8(9) . . . . ? P1 P2 C15 C16 -102.3(8) . . . . ? C20 C15 C16 C17 3.4(15) . . . . ? P2 C15 C16 C17 177.0(8) . . . . ? C15 C16 C17 C18 -1.1(16) . . . . ? C16 C17 C18 C19 -1.9(16) . . . . ? C17 C18 C19 C20 2.5(16) . . . . ? C18 C19 C20 C15 -0.2(15) . . . . ? C16 C15 C20 C19 -2.8(15) . . . . ? P2 C15 C20 C19 -176.1(7) . . . . ? C15 P2 C21 C22 -108.2(8) . . . . ? C1 P2 C21 C22 129.2(8) . . . . ? P1 P2 C21 C22 6.5(9) . . . . ? C15 P2 C21 C26 74.0(9) . . . . ? C1 P2 C21 C26 -48.6(9) . . . . ? P1 P2 C21 C26 -171.3(7) . . . . ? C26 C21 C22 C23 0.7(14) . . . . ? P2 C21 C22 C23 -177.0(7) . . . . ? C21 C22 C23 C24 0.4(15) . . . . ? C22 C23 C24 C25 -1.2(16) . . . . ? C23 C24 C25 C26 1.0(15) . . . . ? C24 C25 C26 C21 0.0(15) . . . . ? C22 C21 C26 C25 -0.9(15) . . . . ? P2 C21 C26 C25 176.9(8) . . . . ? C4 P3 C27 C28 155.1(8) . . . . ? C33 P3 C27 C28 -85.1(9) . . . . ? P1 P3 C27 C28 33.6(10) . . . . ? C4 P3 C27 C32 -32.2(9) . . . . ? C33 P3 C27 C32 87.6(9) . . . . ? P1 P3 C27 C32 -153.7(7) . . . . ? C32 C27 C28 C29 -0.4(15) . . . . ? P3 C27 C28 C29 172.0(8) . . . . ? C27 C28 C29 C30 -0.1(15) . . . . ? C28 C29 C30 C31 -0.5(16) . . . . ? C29 C30 C31 C32 1.7(17) . . . . ? C30 C31 C32 C27 -2.2(17) . . . . ? C28 C27 C32 C31 1.6(16) . . . . ? P3 C27 C32 C31 -171.2(9) . . . . ? C27 P3 C33 C38 165.8(8) . . . . ? C4 P3 C33 C38 -75.3(9) . . . . ? P1 P3 C33 C38 34.0(8) . . . . ? C27 P3 C33 C34 -14.0(9) . . . . ? C4 P3 C33 C34 104.9(8) . . . . ? P1 P3 C33 C34 -145.8(7) . . . . ? C38 C33 C34 C35 -0.8(15) . . . . ? P3 C33 C34 C35 178.9(8) . . . . ? C33 C34 C35 C36 1.7(15) . . . . ? C34 C35 C36 C37 -2.0(16) . . . . ? C35 C36 C37 C38 1.4(15) . . . . ? C34 C33 C38 C37 0.2(15) . . . . ? P3 C33 C38 C37 -179.6(7) . . . . ? C36 C37 C38 C33 -0.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.821 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.182 #====================================================================== _vrf_PLAT213_11c ; PROBLEM: Atom C2 & C19 have ADP max/min Ratio ............. 6.00 prola RESPONSE: The data is weak and noisy (hence the general low quality and poorly defined thermal ellipsoids). ; #======================================================================