Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name N.A.Barnes A.K.Brisdon F.R.W Brown W.I.Cross C.J.Herbert R.G.Pritchard G.Sadiq _publ_contact_author_name 'Alan Brisdon' _publ_contact_author_address ; School of Chemistry University of Manchester Oxford Road MANCHESTER M13 9PL UNITED KINGDOM ; _publ_contact_author_email ALAN.BRISDON@MANCHESTER.AC.UK _publ_section_title ; The coordination chemistry of perfluorovinyl substituted phosphine ligands, a crystallographic and spectroscopic study. Co-crystallisation of both cis- and trans- isomers of [PtCl2{PiPr2(CF=CF2)}2] within the same unit cell. ; _publ_requested_category FM data_akb05new _database_code_depnum_ccdc_archive 'CCDC 656532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-[RhCl(CO){PPh2(CF=CF2)}2] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H20 Cl1 F6 O1 P2 Rh1' _chemical_formula_sum 'C29 H20 Cl F6 O P2 Rh' _chemical_formula_weight 698.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.688(2) _cell_length_b 23.638(3) _cell_length_c 11.873(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.83(2) _cell_angle_gamma 90.00 _cell_volume 2976.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8194 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5474 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5211 _reflns_number_gt 2974 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+1.1243P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5211 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1203 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Rh1 Rh 0.33252(6) 0.64384(2) 0.49667(5) 0.0719(2) Uani 1 1 d . . . Cl1 Cl 0.2942(2) 0.54777(8) 0.4434(2) 0.0918(6) Uani 1 1 d . . . P1 P 0.3484(2) 0.62300(9) 0.69224(19) 0.0744(5) Uani 1 1 d . . . P2 P 0.3243(2) 0.66100(9) 0.30301(19) 0.0795(6) Uani 1 1 d . . . O1 O 0.3661(7) 0.7644(3) 0.5583(6) 0.112(2) Uani 1 1 d . . . C1 C 0.3549(7) 0.7191(4) 0.5347(7) 0.081(2) Uani 1 1 d . . . C2 C 0.3723(7) 0.6827(3) 0.7959(7) 0.0728(19) Uani 1 1 d . . . C3 C 0.2757(8) 0.7083(4) 0.8095(8) 0.097(3) Uani 1 1 d . . . H3 H 0.1951 0.6931 0.7698 0.116 Uiso 1 1 calc R . . C4 C 0.2932(10) 0.7562(4) 0.8803(10) 0.115(3) Uani 1 1 d . . . H4 H 0.2248 0.7730 0.8877 0.138 Uiso 1 1 calc R . . C5 C 0.4077(11) 0.7786(4) 0.9386(9) 0.106(3) Uani 1 1 d . . . H5 H 0.4193 0.8108 0.9872 0.127 Uiso 1 1 calc R . . C6 C 0.5072(10) 0.7545(4) 0.9268(9) 0.111(3) Uani 1 1 d . . . H6 H 0.5873 0.7701 0.9674 0.133 Uiso 1 1 calc R . . C7 C 0.4893(8) 0.7063(4) 0.8538(8) 0.095(2) Uani 1 1 d . . . H7 H 0.5573 0.6901 0.8445 0.113 Uiso 1 1 calc R . . C8 C 0.2156(9) 0.5864(3) 0.6998(9) 0.085(2) Uani 1 1 d . . . C9 C 0.1071(9) 0.5816(4) 0.5909(11) 0.114(3) Uani 1 1 d . . . H9 H 0.1030 0.5967 0.5170 0.137 Uiso 1 1 calc R . . C10 C 0.0053(14) 0.5538(6) 0.5953(15) 0.127(5) Uani 1 1 d . . . H10 H -0.0686 0.5514 0.5229 0.153 Uiso 1 1 calc R . . C11 C 0.0077(16) 0.5317(7) 0.692(2) 0.177(8) Uani 1 1 d . . . H11 H -0.0617 0.5108 0.6874 0.212 Uiso 1 1 calc R . . C12 C 0.1075(19) 0.5371(6) 0.8031(18) 0.173(6) Uani 1 1 d . . . H12 H 0.1059 0.5229 0.8755 0.207 Uiso 1 1 calc R . . C13 C 0.2180(11) 0.5661(5) 0.8044(11) 0.126(4) Uani 1 1 d . . . H13 H 0.2897 0.5703 0.8783 0.152 Uiso 1 1 calc R . . C14 C 0.4795(9) 0.5785(4) 0.7808(8) 0.091(2) Uani 1 1 d . . . C15 C 0.5660(11) 0.5563(4) 0.7548(10) 0.102(3) Uani 1 1 d . . . C16 C 0.3171(8) 0.7345(3) 0.2543(7) 0.078(2) Uani 1 1 d . . . C17 C 0.2055(8) 0.7586(4) 0.1719(8) 0.098(3) Uani 1 1 d . . . H17 H 0.1324 0.7370 0.1366 0.118 Uiso 1 1 calc R . . C18 C 0.2042(10) 0.8149(4) 0.1432(10) 0.114(3) Uani 1 1 d . . . H18 H 0.1287 0.8312 0.0890 0.136 Uiso 1 1 calc R . . C19 C 0.3092(11) 0.8476(4) 0.1910(12) 0.119(4) Uani 1 1 d . . . H19 H 0.3066 0.8851 0.1666 0.143 Uiso 1 1 calc R . . C20 C 0.4193(11) 0.8244(4) 0.2761(11) 0.117(3) Uani 1 1 d . . . H20 H 0.4912 0.8467 0.3126 0.140 Uiso 1 1 calc R . . C21 C 0.4234(8) 0.7678(3) 0.3077(9) 0.093(2) Uani 1 1 d . . . H21 H 0.4982 0.7521 0.3651 0.111 Uiso 1 1 calc R . . C22 C 0.4566(8) 0.6326(3) 0.2776(7) 0.084(2) Uani 1 1 d . . . C23 C 0.4852(12) 0.6534(4) 0.1828(9) 0.122(4) Uani 1 1 d . . . H23 H 0.4359 0.6814 0.1296 0.146 Uiso 1 1 calc R . . C24 C 0.5879(13) 0.6316(5) 0.1694(10) 0.141(4) Uani 1 1 d . . . H24 H 0.6076 0.6452 0.1061 0.170 Uiso 1 1 calc R . . C25 C 0.6607(12) 0.5911(4) 0.2456(11) 0.130(4) Uani 1 1 d . . . H25 H 0.7294 0.5769 0.2344 0.157 Uiso 1 1 calc R . . C26 C 0.6338(10) 0.5709(4) 0.3386(9) 0.105(3) Uani 1 1 d . . . H26 H 0.6834 0.5426 0.3906 0.125 Uiso 1 1 calc R . . C27 C 0.5336(9) 0.5923(3) 0.3557(7) 0.085(2) Uani 1 1 d . . . H27 H 0.5174 0.5793 0.4215 0.102 Uiso 1 1 calc R . . C28 C 0.1889(11) 0.6314(4) 0.1781(9) 0.110(3) Uani 1 1 d . . . C29 C 0.0846(13) 0.6188(5) 0.1766(12) 0.125(4) Uani 1 1 d . . . F1 F 0.4938(7) 0.5649(3) 0.8989(6) 0.171(3) Uani 1 1 d . . . F3 F 0.5758(6) 0.5650(3) 0.6537(7) 0.136(2) Uani 1 1 d . . . F2 F 0.6654(7) 0.5235(3) 0.8327(8) 0.179(3) Uani 1 1 d . . . F4 F 0.1992(7) 0.6223(4) 0.0703(6) 0.177(3) Uani 1 1 d . . . F5 F -0.0172(8) 0.5974(4) 0.0793(7) 0.209(4) Uani 1 1 d . . . F6 F 0.0488(6) 0.6254(3) 0.2646(8) 0.162(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0800(4) 0.0614(3) 0.0718(4) -0.0021(3) 0.0295(3) -0.0049(3) Cl1 0.1206(17) 0.0667(11) 0.0924(14) -0.0063(10) 0.0489(13) -0.0133(11) P1 0.0793(13) 0.0709(12) 0.0782(13) -0.0052(10) 0.0382(11) -0.0058(10) P2 0.0910(15) 0.0710(12) 0.0661(12) 0.0045(9) 0.0226(11) -0.0002(10) O1 0.156(6) 0.063(4) 0.129(5) -0.009(3) 0.071(4) -0.010(4) C1 0.081(5) 0.078(6) 0.083(5) 0.004(4) 0.033(4) -0.001(4) C2 0.070(5) 0.074(5) 0.081(5) 0.002(4) 0.038(4) -0.004(4) C3 0.084(6) 0.085(6) 0.124(7) -0.026(5) 0.048(5) -0.010(5) C4 0.097(7) 0.100(7) 0.158(9) -0.031(7) 0.065(7) -0.007(6) C5 0.122(8) 0.087(6) 0.119(7) -0.029(5) 0.061(7) -0.013(6) C6 0.093(7) 0.109(7) 0.118(8) -0.031(6) 0.031(6) -0.027(6) C7 0.087(6) 0.095(6) 0.107(6) -0.016(5) 0.047(5) -0.010(5) C8 0.095(6) 0.069(5) 0.104(6) -0.021(5) 0.056(6) -0.023(4) C9 0.088(7) 0.107(7) 0.172(10) -0.059(7) 0.078(7) -0.030(6) C10 0.107(9) 0.132(11) 0.153(12) -0.040(9) 0.064(9) -0.004(8) C11 0.138(13) 0.121(12) 0.28(2) -0.100(15) 0.093(17) -0.046(10) C12 0.244(18) 0.115(10) 0.230(18) 0.009(10) 0.168(16) -0.033(11) C13 0.151(10) 0.124(8) 0.121(8) -0.010(7) 0.073(7) -0.056(7) C14 0.109(7) 0.096(6) 0.073(5) 0.001(4) 0.044(5) 0.011(5) C15 0.121(8) 0.089(6) 0.103(7) -0.007(6) 0.053(7) 0.000(6) C16 0.080(5) 0.071(5) 0.085(5) 0.008(4) 0.035(5) 0.009(4) C17 0.083(6) 0.086(6) 0.110(7) 0.020(5) 0.025(5) 0.008(5) C18 0.099(7) 0.106(8) 0.128(8) 0.043(6) 0.040(6) 0.034(6) C19 0.102(8) 0.093(7) 0.177(11) 0.039(7) 0.072(8) 0.013(6) C20 0.110(8) 0.085(7) 0.166(10) 0.018(6) 0.068(8) -0.015(6) C21 0.074(5) 0.079(6) 0.116(7) 0.017(5) 0.031(5) 0.001(4) C22 0.109(6) 0.075(5) 0.066(5) 0.000(4) 0.034(5) 0.009(4) C23 0.171(10) 0.119(8) 0.093(7) 0.039(6) 0.073(7) 0.054(7) C24 0.192(12) 0.153(11) 0.115(8) 0.033(8) 0.099(9) 0.057(9) C25 0.186(12) 0.101(7) 0.131(9) 0.024(7) 0.093(9) 0.048(7) C26 0.129(8) 0.076(6) 0.103(7) 0.023(5) 0.043(6) 0.028(5) C27 0.105(7) 0.075(5) 0.077(5) 0.007(4) 0.039(5) 0.007(5) C28 0.109(8) 0.113(8) 0.075(6) 0.001(5) 0.005(6) -0.024(6) C29 0.108(9) 0.137(9) 0.099(8) -0.005(7) 0.013(8) -0.030(8) F1 0.208(7) 0.196(7) 0.120(5) 0.049(5) 0.080(5) 0.070(6) F3 0.121(5) 0.150(5) 0.137(5) 0.000(4) 0.053(4) 0.019(4) F2 0.146(6) 0.149(6) 0.205(7) 0.004(5) 0.037(5) 0.064(5) F4 0.185(7) 0.233(8) 0.082(4) -0.036(5) 0.025(4) -0.044(6) F5 0.178(7) 0.196(8) 0.165(7) 0.001(6) -0.013(6) -0.075(6) F6 0.117(5) 0.188(7) 0.158(6) 0.002(6) 0.035(5) -0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.827(9) . ? Rh1 P2 2.297(2) . ? Rh1 P1 2.304(2) . ? Rh1 Cl1 2.349(2) . ? P1 C14 1.790(9) . ? P1 C8 1.812(8) . ? P1 C2 1.815(8) . ? P2 C28 1.795(10) . ? P2 C16 1.823(8) . ? P2 C22 1.823(9) . ? O1 C1 1.101(9) . ? C2 C3 1.349(10) . ? C2 C7 1.365(11) . ? C3 C4 1.373(12) . ? C4 C5 1.332(13) . ? C5 C6 1.354(12) . ? C6 C7 1.393(12) . ? C8 C13 1.321(12) . ? C8 C9 1.383(13) . ? C9 C10 1.379(15) . ? C10 C11 1.25(2) . ? C11 C12 1.35(2) . ? C12 C13 1.456(17) . ? C14 C15 1.287(12) . ? C14 F1 1.378(9) . ? C15 F3 1.270(11) . ? C15 F2 1.380(14) . ? C16 C21 1.378(10) . ? C16 C17 1.382(10) . ? C17 C18 1.372(12) . ? C18 C19 1.358(13) . ? C19 C20 1.373(13) . ? C20 C21 1.385(12) . ? C22 C27 1.369(10) . ? C22 C23 1.391(12) . ? C23 C24 1.376(14) . ? C24 C25 1.347(13) . ? C25 C26 1.354(13) . ? C26 C27 1.368(12) . ? C28 C29 1.247(15) . ? C28 F4 1.353(12) . ? C29 F6 1.288(14) . ? C29 F5 1.361(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 P2 91.0(3) . . ? C1 Rh1 P1 90.9(3) . . ? P2 Rh1 P1 177.02(8) . . ? C1 Rh1 Cl1 177.5(3) . . ? P2 Rh1 Cl1 88.76(8) . . ? P1 Rh1 Cl1 89.44(8) . . ? C14 P1 C8 103.3(4) . . ? C14 P1 C2 102.0(4) . . ? C8 P1 C2 103.2(4) . . ? C14 P1 Rh1 113.9(3) . . ? C8 P1 Rh1 116.3(3) . . ? C2 P1 Rh1 116.2(3) . . ? C28 P2 C16 101.7(4) . . ? C28 P2 C22 103.6(5) . . ? C16 P2 C22 103.2(4) . . ? C28 P2 Rh1 114.2(4) . . ? C16 P2 Rh1 117.6(3) . . ? C22 P2 Rh1 114.7(3) . . ? O1 C1 Rh1 178.4(8) . . ? C3 C2 C7 117.9(8) . . ? C3 C2 P1 122.1(6) . . ? C7 C2 P1 119.7(6) . . ? C2 C3 C4 121.7(8) . . ? C5 C4 C3 120.4(9) . . ? C4 C5 C6 119.8(9) . . ? C5 C6 C7 119.9(9) . . ? C2 C7 C6 120.3(8) . . ? C13 C8 C9 119.9(9) . . ? C13 C8 P1 122.7(8) . . ? C9 C8 P1 117.4(7) . . ? C10 C9 C8 118.0(12) . . ? C11 C10 C9 123.2(17) . . ? C10 C11 C12 122.2(19) . . ? C11 C12 C13 117.0(15) . . ? C8 C13 C12 119.5(12) . . ? C15 C14 F1 112.1(9) . . ? C15 C14 P1 131.6(8) . . ? F1 C14 P1 116.3(7) . . ? F3 C15 C14 123.5(10) . . ? F2 C15 F3 109.8(10) . . ? C14 C15 F2 126.5(10) . . ? C21 C16 C17 119.5(7) . . ? C21 C16 P2 119.0(6) . . ? C17 C16 P2 121.4(6) . . ? C18 C17 C16 118.9(9) . . ? C19 C18 C17 122.4(9) . . ? C18 C19 C20 118.9(9) . . ? C19 C20 C21 120.0(9) . . ? C16 C21 C20 120.3(8) . . ? C27 C22 C23 118.7(8) . . ? C27 C22 P2 120.4(6) . . ? C23 C22 P2 120.8(7) . . ? C24 C23 C22 118.7(9) . . ? C25 C24 C23 121.5(10) . . ? C24 C25 C26 120.1(11) . . ? C25 C26 C27 119.8(9) . . ? C26 C27 C22 121.1(8) . . ? C29 C28 F4 115.1(10) . . ? C29 C28 P2 128.5(10) . . ? F4 C28 P2 116.4(9) . . ? C28 C29 F6 127.4(12) . . ? C28 C29 F5 127.0(14) . . ? F6 C29 F5 105.5(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.499 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.076 #===END data_PdCliPr2pfv _database_code_depnum_ccdc_archive 'CCDC 656533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-bis(diisopropylperfluorovinylphoshine)palladium(II)chloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl2 F6 P2 Pd1' _chemical_formula_sum 'C16 H28 Cl2 F6 P2 Pd' _chemical_formula_weight 573.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 8.090(2) _cell_length_b 8.3232(14) _cell_length_c 9.2824(13) _cell_angle_alpha 80.593(12) _cell_angle_beta 77.717(16) _cell_angle_gamma 70.897(16) _cell_volume 574.08(19) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 1.227 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.7489 _exptl_absorpt_correction_T_max 0.7914 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2152 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.98 _reflns_number_total 2152 _reflns_number_gt 1994 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1592P)^2^+0.3158P] 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 2152 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.2090 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.0000 0.0225(3) Uani 1 2 d S . . Cl1 Cl 0.3024(2) 0.5082(2) -0.14621(16) 0.0379(5) Uani 1 1 d . . . P1 P 0.6855(2) 0.58602(17) -0.20256(15) 0.0234(4) Uani 1 1 d . . . F1 F 0.6504(6) 0.6929(5) -0.4914(4) 0.0459(10) Uani 1 1 d . . . F2 F 0.3424(7) 0.9370(6) -0.4379(5) 0.0594(13) Uani 1 1 d . . . F3 F 0.3301(6) 0.8873(5) -0.2010(5) 0.0508(11) Uani 1 1 d . . . C1 C 0.5727(9) 0.7200(8) -0.3484(6) 0.0303(13) Uani 1 1 d . . . C2 C 0.4226(10) 0.8415(8) -0.3290(8) 0.0417(16) Uani 1 1 d . . . C3 C 0.8338(8) 0.4018(8) -0.2987(7) 0.0310(13) Uani 1 1 d . . . H3 H 0.9032 0.4445 -0.3892 0.037 Uiso 1 1 calc R . . C4 C 0.7295(10) 0.3031(9) -0.3442(8) 0.0416(16) Uani 1 1 d . . . H4A H 0.8102 0.2118 -0.4009 0.062 Uiso 1 1 calc R . . H4B H 0.6455 0.3794 -0.4045 0.062 Uiso 1 1 calc R . . H4C H 0.6657 0.2549 -0.2564 0.062 Uiso 1 1 calc R . . C5 C 0.9625(11) 0.2875(9) -0.1989(9) 0.0475(18) Uani 1 1 d . . . H5A H 0.8961 0.2527 -0.1059 0.071 Uiso 1 1 calc R . . H5B H 1.0366 0.3501 -0.1799 0.071 Uiso 1 1 calc R . . H5C H 1.0366 0.1872 -0.2474 0.071 Uiso 1 1 calc R . . C6 C 0.8240(9) 0.7077(7) -0.1719(6) 0.0289(13) Uani 1 1 d . . . H6 H 0.9027 0.6343 -0.1030 0.035 Uiso 1 1 calc R . . C7 C 0.9443(9) 0.7549(9) -0.3135(7) 0.0353(14) Uani 1 1 d . . . H7A H 0.8715 0.8298 -0.3830 0.053 Uiso 1 1 calc R . . H7B H 1.0180 0.6517 -0.3582 0.053 Uiso 1 1 calc R . . H7C H 1.0193 0.8128 -0.2887 0.053 Uiso 1 1 calc R . . C8 C 0.7094(10) 0.8664(8) -0.0953(8) 0.0408(16) Uani 1 1 d . . . H8A H 0.7849 0.9275 -0.0764 0.061 Uiso 1 1 calc R . . H8B H 0.6426 0.8323 -0.0022 0.061 Uiso 1 1 calc R . . H8C H 0.6278 0.9403 -0.1587 0.061 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 Pd1 0.0229(4) 0.0220(4) 0.0202(4) -0.0021(3) -0.0030(3) -0.0039(3) Cl1 0.0362(9) 0.0523(10) 0.0291(8) 0.0043(7) -0.0110(7) -0.0192(7) P1 0.0270(8) 0.0186(8) 0.0209(8) -0.0033(6) -0.0026(6) -0.0025(6) F1 0.063(3) 0.051(2) 0.0254(18) 0.0001(16) -0.0077(18) -0.022(2) F2 0.070(3) 0.041(2) 0.072(3) 0.017(2) -0.046(3) -0.012(2) F3 0.044(2) 0.037(2) 0.062(3) -0.0076(18) -0.009(2) 0.0031(18) C1 0.040(4) 0.030(3) 0.026(3) 0.002(2) -0.011(3) -0.016(3) C2 0.051(4) 0.028(3) 0.050(4) 0.008(3) -0.027(3) -0.012(3) C3 0.033(3) 0.024(3) 0.036(3) -0.012(2) 0.007(3) -0.011(2) C4 0.047(4) 0.035(3) 0.049(4) -0.020(3) 0.002(3) -0.021(3) C5 0.043(4) 0.029(3) 0.064(5) -0.016(3) -0.012(4) 0.006(3) C6 0.035(3) 0.024(3) 0.028(3) -0.004(2) -0.004(3) -0.010(3) C7 0.035(3) 0.039(3) 0.035(3) 0.001(3) -0.006(3) -0.018(3) C8 0.047(4) 0.028(3) 0.047(4) -0.011(3) -0.003(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2856(16) . ? Pd1 Cl1 2.2856(16) 2_665 ? Pd1 P1 2.3158(15) 2_665 ? Pd1 P1 2.3158(15) . ? P1 C1 1.810(6) . ? P1 C6 1.826(6) . ? P1 C3 1.837(6) . ? F1 C1 1.363(7) . ? F2 C2 1.324(7) . ? F3 C2 1.303(9) . ? C1 C2 1.301(10) . ? C3 C4 1.511(9) . ? C3 C5 1.523(10) . ? C6 C7 1.538(9) . ? C6 C8 1.528(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl1 180.0 . 2_665 ? Cl1 Pd1 P1 88.77(6) . 2_665 ? Cl1 Pd1 P1 91.23(6) 2_665 2_665 ? Cl1 Pd1 P1 91.23(6) . . ? Cl1 Pd1 P1 88.77(6) 2_665 . ? P1 Pd1 P1 180.00(7) 2_665 . ? C1 P1 C6 102.6(3) . . ? C1 P1 C3 102.1(3) . . ? C6 P1 C3 107.1(3) . . ? C1 P1 Pd1 114.5(2) . . ? C6 P1 Pd1 118.17(19) . . ? C3 P1 Pd1 110.8(2) . . ? C8 C6 C7 111.2(5) . . ? C8 C6 P1 110.4(5) . . ? C7 C6 P1 113.6(4) . . ? C4 C3 C5 111.0(6) . . ? C4 C3 P1 111.2(5) . . ? C5 C3 P1 109.4(4) . . ? C2 C1 F1 116.6(5) . . ? C2 C1 P1 125.6(5) . . ? F1 C1 P1 117.8(5) . . ? C1 C2 F3 125.4(6) . . ? C1 C2 F2 124.3(7) . . ? F3 C2 F2 110.3(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.722 _refine_diff_density_min -2.198 _refine_diff_density_rms 0.239 #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2003-07-02 at 11:13:03 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : a dreduc sortav struct data_akb01df _database_code_depnum_ccdc_archive 'CCDC 656534' _audit_creation_date 2003-07-02T11:13:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; trans-bis(diisopropylperfluorovinyl)palladiumdibromide ; _chemical_formula_moiety 'C16 H28 Br2 F6 P2 Pd1' _chemical_formula_sum 'C16 H28 Br2 F6 P2 Pd' _chemical_formula_weight 662.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.7399(2) _cell_length_b 11.6112(3) _cell_length_c 10.7920(3) _cell_angle_alpha 90 _cell_angle_beta 93.6970(10) _cell_angle_gamma 90 _cell_volume 1217.95(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15716 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.448 _exptl_absorpt_correction_T_max 0.748 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.596806E-1 _diffrn_orient_matrix_ub_12 0.36349E-2 _diffrn_orient_matrix_ub_13 0.719045E-1 _diffrn_orient_matrix_ub_21 -0.836888E-1 _diffrn_orient_matrix_ub_22 -0.71332E-2 _diffrn_orient_matrix_ub_23 -0.582186E-1 _diffrn_orient_matrix_ub_31 0.44319E-2 _diffrn_orient_matrix_ub_32 -0.857508E-1 _diffrn_orient_matrix_ub_33 0.7891E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_number 19675 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2786 _reflns_number_gt 2083 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+0.9399P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0067(9) _refine_ls_number_reflns 2786 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.087 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.893 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' 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 C1 C 1.1818(4) 0.0741(3) 0.2375(3) 0.0580(9) Uani 1 1 d . . . C2 C 1.3000(5) 0.0937(4) 0.2920(5) 0.0755(12) Uani 1 1 d . . . C3 C 0.9045(5) 0.0072(4) 0.1852(4) 0.0690(12) Uani 1 1 d . . . C4 C 0.7526(6) 0.0350(9) 0.2042(7) 0.105(2) Uani 1 1 d . . . C5 C 0.9341(9) -0.1214(5) 0.1865(6) 0.098(2) Uani 1 1 d . . . C6 C 0.9739(5) 0.2375(4) 0.2886(4) 0.0626(10) Uani 1 1 d . . . C7 C 0.9723(7) 0.2800(6) 0.1542(6) 0.0874(16) Uani 1 1 d . . . C8 C 1.0718(7) 0.3076(5) 0.3752(7) 0.0937(17) Uani 1 1 d . . . F1 F 1.1824(3) 0.0473(3) 0.1133(2) 0.0838(7) Uani 1 1 d . . . F3 F 1.3184(3) 0.1212(3) 0.4078(3) 0.1089(11) Uani 1 1 d . . . F2 F 1.4184(3) 0.0901(3) 0.2369(4) 0.1076(10) Uani 1 1 d . . . Br1 Br 1.17885(5) -0.13680(4) 0.45766(4) 0.0865(2) Uani 1 1 d . . . Pd1 Pd 1 0 0.5 0.04655(16) Uani 1 2 d S . . P1 P 1.01499(9) 0.08277(8) 0.30434(8) 0.0472(2) Uani 1 1 d . . . H3 H 0.927(4) 0.043(4) 0.107(4) 0.073(12) Uiso 1 1 d . . . H4A H 0.719(8) 0.003(6) 0.282(8) 0.15(3) Uiso 1 1 d . . . H4B H 0.697(8) 0.004(6) 0.135(7) 0.14(3) Uiso 1 1 d . . . H4C H 0.744(9) 0.117(7) 0.205(8) 0.17(4) Uiso 1 1 d . . . H5A H 0.912(4) -0.165(4) 0.262(4) 0.070(13) Uiso 1 1 d . . . H5B H 0.886(7) -0.155(6) 0.117(7) 0.14(2) Uiso 1 1 d . . . H5C H 1.030(8) -0.132(6) 0.175(7) 0.14(3) Uiso 1 1 d . . . H6 H 0.878(4) 0.240(3) 0.309(4) 0.066(11) Uiso 1 1 d . . . H7A H 0.899(5) 0.235(4) 0.104(4) 0.077(15) Uiso 1 1 d . . . H7B H 0.963(7) 0.361(6) 0.154(6) 0.13(2) Uiso 1 1 d . . . H7C H 1.054(6) 0.264(5) 0.118(5) 0.11(2) Uiso 1 1 d . . . H8A H 1.167(6) 0.304(5) 0.348(5) 0.104(19) Uiso 1 1 d . . . H8B H 1.045(6) 0.382(6) 0.375(5) 0.11(2) Uiso 1 1 d . . . H8C H 1.081(6) 0.271(5) 0.468(6) 0.12(2) Uiso 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 C1 0.060(2) 0.065(2) 0.050(2) 0.0001(18) 0.0119(17) -0.0027(19) C2 0.058(3) 0.076(3) 0.093(3) -0.011(3) 0.006(2) 0.001(2) C3 0.067(3) 0.090(3) 0.049(2) 0.006(2) -0.0012(19) -0.015(2) C4 0.064(3) 0.155(7) 0.096(4) 0.005(5) -0.005(3) -0.027(4) C5 0.137(6) 0.078(4) 0.077(4) -0.011(3) -0.009(4) -0.028(4) C6 0.058(2) 0.061(2) 0.069(3) 0.018(2) 0.011(2) 0.0094(19) C7 0.092(4) 0.087(4) 0.085(4) 0.040(3) 0.022(3) 0.018(3) C8 0.100(4) 0.057(3) 0.123(5) -0.007(3) 0.000(4) -0.003(3) F1 0.0843(17) 0.119(2) 0.0500(13) -0.0063(14) 0.0187(12) 0.0031(16) F2 0.085(2) 0.144(3) 0.095(2) -0.037(2) -0.0201(16) -0.0080(18) F3 0.0560(16) 0.101(2) 0.169(3) -0.013(2) 0.0306(18) -0.0013(14) Br1 0.0988(4) 0.0927(4) 0.0720(3) 0.0233(2) 0.0370(3) 0.0509(3) Pd1 0.0514(2) 0.0516(2) 0.0374(2) 0.00465(15) 0.00907(15) 0.01231(16) P1 0.0471(5) 0.0551(5) 0.0398(5) 0.0057(4) 0.0053(4) 0.0014(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.279(6) . ? C1 F1 1.377(4) . ? C1 P1 1.822(4) . ? C2 F3 1.291(6) . ? C2 F2 1.331(5) . ? C3 C5 1.520(8) . ? C3 C4 1.541(8) . ? C3 P1 1.845(4) . ? C3 H3 0.98(5) . ? C4 H4A 0.99(8) . ? C4 H4B 0.96(7) . ? C4 H4C 0.96(8) . ? C5 H5A 1.00(5) . ? C5 H5B 0.94(7) . ? C5 H5C 0.96(8) . ? C6 C8 1.526(7) . ? C6 C7 1.532(6) . ? C6 P1 1.846(4) . ? C6 H6 0.97(4) . ? C7 H7A 1.01(5) . ? C7 H7B 0.95(7) . ? C7 H7C 0.93(6) . ? C8 H8A 0.99(6) . ? C8 H8B 0.90(6) . ? C8 H8C 1.08(6) . ? Br1 Pd1 2.4226(4) . ? Pd1 P1 2.3331(8) . ? Pd1 P1 2.3331(8) 3_756 ? Pd1 Br1 2.4226(4) 3_756 ? 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 C2 C1 F1 115.3(4) . . ? C2 C1 P1 127.4(3) . . ? F1 C1 P1 117.2(3) . . ? C1 C2 F3 123.6(4) . . ? C1 C2 F2 124.7(5) . . ? F3 C2 F2 111.7(4) . . ? C5 C3 C4 112.8(6) . . ? C5 C3 P1 111.0(4) . . ? C4 C3 P1 109.2(4) . . ? C5 C3 H3 112(3) . . ? C4 C3 H3 107(3) . . ? P1 C3 H3 104(3) . . ? C3 C4 H4A 114(5) . . ? C3 C4 H4B 108(5) . . ? H4A C4 H4B 108(6) . . ? C3 C4 H4C 107(5) . . ? H4A C4 H4C 109(7) . . ? H4B C4 H4C 110(7) . . ? C3 C5 H5A 117(3) . . ? C3 C5 H5B 108(4) . . ? H5A C5 H5B 109(5) . . ? C3 C5 H5C 108(4) . . ? H5A C5 H5C 108(5) . . ? H5B C5 H5C 106(6) . . ? C8 C6 C7 112.1(5) . . ? C8 C6 P1 109.8(3) . . ? C7 C6 P1 112.9(4) . . ? C8 C6 H6 115(2) . . ? C7 C6 H6 105(2) . . ? P1 C6 H6 102(2) . . ? C6 C7 H7A 107(3) . . ? C6 C7 H7B 108(4) . . ? H7A C7 H7B 117(5) . . ? C6 C7 H7C 112(4) . . ? H7A C7 H7C 106(5) . . ? H7B C7 H7C 106(6) . . ? C6 C8 H8A 111(3) . . ? C6 C8 H8B 110(4) . . ? H8A C8 H8B 109(5) . . ? C6 C8 H8C 111(3) . . ? H8A C8 H8C 103(5) . . ? H8B C8 H8C 113(5) . . ? P1 Pd1 P1 180 . 3_756 ? P1 Pd1 Br1 89.33(2) . 3_756 ? P1 Pd1 Br1 90.67(2) 3_756 3_756 ? P1 Pd1 Br1 90.67(2) . . ? P1 Pd1 Br1 89.33(2) 3_756 . ? Br1 Pd1 Br1 180 3_756 . ? C1 P1 C3 101.1(2) . . ? C1 P1 C6 102.19(19) . . ? C3 P1 C6 106.6(2) . . ? C1 P1 Pd1 116.40(13) . . ? C3 P1 Pd1 111.54(14) . . ? C6 P1 Pd1 117.27(14) . . ? 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 F1 C1 C2 F3 179.1(4) . . . . ? P1 C1 C2 F3 1.6(7) . . . . ? F1 C1 C2 F2 0.3(7) . . . . ? P1 C1 C2 F2 -177.3(3) . . . . ? C2 C1 P1 C3 -165.7(4) . . . . ? F1 C1 P1 C3 16.8(3) . . . . ? C2 C1 P1 C6 84.4(5) . . . . ? F1 C1 P1 C6 -93.1(3) . . . . ? C2 C1 P1 Pd1 -44.7(5) . . . . ? F1 C1 P1 Pd1 137.8(3) . . . . ? C5 C3 P1 C1 71.3(5) . . . . ? C4 C3 P1 C1 -163.6(4) . . . . ? C5 C3 P1 C6 177.8(4) . . . . ? C4 C3 P1 C6 -57.2(5) . . . . ? C5 C3 P1 Pd1 -53.1(5) . . . . ? C4 C3 P1 Pd1 72.0(5) . . . . ? C8 C6 P1 C1 -68.5(4) . . . . ? C7 C6 P1 C1 57.4(4) . . . . ? C8 C6 P1 C3 -174.1(4) . . . . ? C7 C6 P1 C3 -48.2(4) . . . . ? C8 C6 P1 Pd1 60.1(4) . . . . ? C7 C6 P1 Pd1 -174.0(3) . . . . ? P1 Pd1 P1 C1 -7E1(10) 3_756 . . . ? Br1 Pd1 P1 C1 151.42(15) 3_756 . . . ? Br1 Pd1 P1 C1 -28.58(15) . . . . ? P1 Pd1 P1 C3 5E1(10) 3_756 . . . ? Br1 Pd1 P1 C3 -93.30(17) 3_756 . . . ? Br1 Pd1 P1 C3 86.70(17) . . . . ? P1 Pd1 P1 C6 17E1(10) 3_756 . . . ? Br1 Pd1 P1 C6 30.00(16) 3_756 . . . ? Br1 Pd1 P1 C6 -150.00(16) . . . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-04-24 at 13:22:33 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : a dreduc sortav struct data_a _database_code_depnum_ccdc_archive 'CCDC 656535' _audit_creation_date 2007-04-24T13:22:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl2 F6 P2 Pd1' _chemical_formula_sum 'C28 H44 Cl2 F6 P2 Pd' _chemical_formula_weight 733.87 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2691(6) _cell_length_b 11.6674(6) _cell_length_c 14.9514(9) _cell_angle_alpha 74.405(2) _cell_angle_beta 70.092(3) _cell_angle_gamma 63.955(3) _cell_volume 1644.00(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4142 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.8214 _exptl_absorpt_correction_T_max 0.9919 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.905955E-1 _diffrn_orient_matrix_ub_12 -0.89265E-2 _diffrn_orient_matrix_ub_13 -0.466181E-1 _diffrn_orient_matrix_ub_21 0.443332E-1 _diffrn_orient_matrix_ub_22 -0.335313E-1 _diffrn_orient_matrix_ub_23 0.544681E-1 _diffrn_orient_matrix_ub_31 0.165087E-1 _diffrn_orient_matrix_ub_32 -0.898982E-1 _diffrn_orient_matrix_ub_33 -0.48078E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0915 _diffrn_reflns_av_unetI/netI 0.0802 _diffrn_reflns_number 22106 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.25 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 5820 _reflns_number_gt 4101 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+10.9855P] 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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0075(16) _refine_ls_number_reflns 5820 _refine_ls_number_parameters 357 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1758 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.313 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.145 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' Cl Cl 0.1495 0.1591 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1026 0.0946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9739 1.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.4434(11) 0.3224(9) 0.4801(6) 0.044(2) Uani 1 1 d . . . C2 C 0.5705(13) 0.3064(12) 0.4454(8) 0.058(3) Uani 1 1 d . . . C3 C 0.2031(9) 0.2691(8) 0.5408(6) 0.039(2) Uani 1 1 d . . . H3 H 0.1597 0.3601 0.5544 0.047 Uiso 1 1 calc R . . C4 C 0.1989(10) 0.2709(10) 0.4392(7) 0.047(2) Uani 1 1 d . . . H4A H 0.2413 0.1818 0.4238 0.056 Uiso 1 1 calc R . . H4B H 0.2516 0.3205 0.3921 0.056 Uiso 1 1 calc R . . C5 C 0.0485(12) 0.3336(11) 0.4324(9) 0.062(3) Uani 1 1 d . . . H5A H 0.0084 0.4245 0.4436 0.075 Uiso 1 1 calc R . . H5B H 0.0459 0.3326 0.3671 0.075 Uiso 1 1 calc R . . C6 C -0.0356(12) 0.2611(12) 0.5064(9) 0.069(3) Uani 1 1 d . . . H6A H -0.1318 0.304 0.5023 0.083 Uiso 1 1 calc R . . H6B H 0.0003 0.172 0.4923 0.083 Uiso 1 1 calc R . . C7 C -0.0298(10) 0.2579(12) 0.6072(8) 0.061(3) Uani 1 1 d . . . H7A H -0.0811 0.2071 0.6541 0.074 Uiso 1 1 calc R . . H7B H -0.0731 0.3467 0.6234 0.074 Uiso 1 1 calc R . . C8 C 0.1232(10) 0.1959(10) 0.6135(7) 0.050(3) Uani 1 1 d . . . H8A H 0.1261 0.1968 0.6787 0.06 Uiso 1 1 calc R . . H8B H 0.1645 0.1051 0.6018 0.06 Uiso 1 1 calc R . . C9 C 0.3649(9) 0.2137(9) 0.6761(6) 0.039(2) Uani 1 1 d . . . H9 H 0.3198 0.155 0.7205 0.047 Uiso 1 1 calc R . . C10 C 0.2742(10) 0.3515(9) 0.7017(7) 0.044(2) Uani 1 1 d . . . H10A H 0.3129 0.4134 0.6566 0.053 Uiso 1 1 calc R . . H10B H 0.1811 0.3764 0.6953 0.053 Uiso 1 1 calc R . . C11 C 0.2667(12) 0.3568(10) 0.8044(7) 0.055(3) Uani 1 1 d . . . H11A H 0.217 0.3035 0.8495 0.066 Uiso 1 1 calc R . . H11B H 0.2145 0.4467 0.818 0.066 Uiso 1 1 calc R . . C12 C 0.4082(14) 0.3085(12) 0.8213(8) 0.067(3) Uani 1 1 d . . . H12A H 0.4562 0.3653 0.78 0.08 Uiso 1 1 calc R . . H12B H 0.3992 0.3103 0.8892 0.08 Uiso 1 1 calc R . . C13 C 0.4885(13) 0.1740(11) 0.7983(8) 0.065(3) Uani 1 1 d . . . H13A H 0.4413 0.1173 0.8411 0.078 Uiso 1 1 calc R . . H13B H 0.5798 0.142 0.8102 0.078 Uiso 1 1 calc R . . C14 C 0.5056(10) 0.1676(10) 0.6933(7) 0.046(2) Uani 1 1 d . . . H14A H 0.5543 0.2228 0.6499 0.055 Uiso 1 1 calc R . . H14B H 0.5602 0.078 0.6794 0.055 Uiso 1 1 calc R . . C15 C 0.9011(13) 0.3323(10) 0.9643(9) 0.067(4) Uani 1 1 d . . . C16 C 0.8997(16) 0.3490(14) 0.8757(10) 0.095(5) Uani 1 1 d . . . C17 C 0.6938(8) 0.2436(8) 1.1056(6) 0.0273(17) Uani 1 1 d U . . H17 H 0.6809 0.1773 1.1623 0.033 Uiso 1 1 calc R . . C18 C 0.6263(10) 0.3753(9) 1.1438(7) 0.046(2) Uani 1 1 d . . . H18A H 0.67 0.3722 1.1922 0.055 Uiso 1 1 calc R . . H18B H 0.6375 0.4445 1.0904 0.055 Uiso 1 1 calc R . . C19 C 0.4754(11) 0.4019(10) 1.1890(9) 0.064(3) Uani 1 1 d . . . H19A H 0.4274 0.4921 1.2025 0.077 Uiso 1 1 calc R . . H19B H 0.4651 0.3447 1.251 0.077 Uiso 1 1 calc R . . C20 C 0.4081(14) 0.3810(17) 1.1249(11) 0.099(6) Uani 1 1 d . . . H20A H 0.3144 0.3875 1.1619 0.118 Uiso 1 1 calc R . . H20B H 0.4003 0.4508 1.0696 0.118 Uiso 1 1 calc R . . C21 C 0.4827(15) 0.2564(17) 1.0887(10) 0.086(5) Uani 1 1 d . . . H21A H 0.4376 0.2522 1.0439 0.103 Uiso 1 1 calc R . . H21B H 0.4802 0.1861 1.143 0.103 Uiso 1 1 calc R . . C22 C 0.6309(14) 0.2374(14) 1.0369(8) 0.073(4) Uani 1 1 d . . . H22A H 0.6801 0.1528 1.0133 0.087 Uiso 1 1 calc R . . H22B H 0.6347 0.3058 0.9811 0.087 Uiso 1 1 calc R . . C23 C 0.9547(9) 0.2044(10) 1.1458(8) 0.051(3) Uani 1 1 d . . . H23 H 0.91 0.2944 1.1617 0.061 Uiso 1 1 calc R . . C24 C 0.9210(10) 0.1148(10) 1.2369(7) 0.048(2) Uani 1 1 d . . . H24A H 0.8205 0.1416 1.2608 0.058 Uiso 1 1 calc R . . H24B H 0.9598 0.0258 1.2219 0.058 Uiso 1 1 calc R . . C25 C 0.9780(10) 0.1173(12) 1.3145(9) 0.063(3) Uani 1 1 d . . . H25A H 0.9581 0.0556 1.3717 0.075 Uiso 1 1 calc R . . H25B H 0.9331 0.2045 1.3337 0.075 Uiso 1 1 calc R . . C26 C 1.1321(12) 0.0817(14) 1.2783(12) 0.083(4) Uani 1 1 d . . . H26A H 1.1668 0.0869 1.3291 0.1 Uiso 1 1 calc R . . H26B H 1.1775 -0.0082 1.2642 0.1 Uiso 1 1 calc R . . C27 C 1.1677(14) 0.1709(15) 1.1883(11) 0.087(4) Uani 1 1 d . . . H27A H 1.2683 0.142 1.164 0.104 Uiso 1 1 calc R . . H27B H 1.1313 0.2594 1.2039 0.104 Uiso 1 1 calc R . . C28 C 1.1064(11) 0.1715(12) 1.1093(10) 0.075(4) Uani 1 1 d . . . H28A H 1.1244 0.2353 1.0532 0.09 Uiso 1 1 calc R . . H28B H 1.1519 0.0856 1.0879 0.09 Uiso 1 1 calc R . . Cl1 Cl 0.5577(2) 0.0914(2) 0.34382(14) 0.0425(6) Uani 1 1 d . . . Cl2 Cl 0.8420(3) -0.0726(3) 1.11464(19) 0.0667(9) Uani 1 1 d . . . F1 F 0.3492(7) 0.4455(5) 0.4594(4) 0.0625(16) Uani 1 1 d . . . F3 F 0.6718(7) 0.1998(7) 0.4600(5) 0.0671(18) Uani 1 1 d . . . F2 F 0.6163(9) 0.3972(8) 0.3923(5) 0.088(2) Uani 1 1 d . . . F4 F 0.9146(8) 0.4305(7) 0.9930(6) 0.099(3) Uani 1 1 d . . . F6 F 0.8798(10) 0.2754(8) 0.8389(5) 0.105(3) Uani 1 1 d . . . F5 F 0.9216(9) 0.4483(8) 0.8107(6) 0.132(4) Uani 1 1 d . . . P1 P 0.3783(2) 0.2010(2) 0.55274(15) 0.0307(5) Uani 1 1 d . . . P2 P 0.8824(3) 0.1983(2) 1.05478(18) 0.0478(7) Uani 1 1 d . . . Pd1 Pd 0.5 0 0.5 0.0285(3) Uani 1 2 d S . . Pd2 Pd 1 0 1 0.0522(4) Uani 1 2 d S . . 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 C1 0.059(6) 0.034(5) 0.034(5) -0.007(4) -0.003(5) -0.019(5) C2 0.070(8) 0.063(7) 0.049(6) -0.015(5) 0.006(6) -0.044(7) C3 0.038(5) 0.031(5) 0.045(5) -0.010(4) -0.008(4) -0.010(4) C4 0.057(6) 0.042(6) 0.047(6) -0.006(4) -0.019(5) -0.020(5) C5 0.066(7) 0.045(6) 0.081(8) -0.016(6) -0.032(7) -0.012(6) C6 0.043(6) 0.071(8) 0.102(10) -0.032(7) -0.027(7) -0.012(6) C7 0.037(6) 0.078(8) 0.073(8) -0.036(6) -0.001(5) -0.021(5) C8 0.045(6) 0.046(6) 0.043(6) -0.022(5) -0.012(5) 0.006(5) C9 0.040(5) 0.040(5) 0.034(5) -0.007(4) -0.001(4) -0.019(4) C10 0.048(6) 0.036(5) 0.044(5) -0.016(4) -0.003(5) -0.013(4) C11 0.075(8) 0.041(6) 0.042(5) -0.016(5) -0.002(5) -0.018(5) C12 0.090(9) 0.065(8) 0.043(6) -0.022(5) -0.019(6) -0.018(7) C13 0.071(8) 0.062(7) 0.059(7) -0.021(6) -0.030(6) -0.008(6) C14 0.047(6) 0.045(6) 0.047(6) -0.017(4) -0.016(5) -0.011(5) C15 0.077(8) 0.035(6) 0.063(7) -0.013(5) 0.024(6) -0.027(6) C16 0.098(11) 0.066(9) 0.062(9) -0.011(7) 0.042(8) -0.026(8) C17 0.0268(19) 0.0270(19) 0.0256(19) -0.0020(10) -0.0067(10) -0.0091(11) C18 0.041(5) 0.037(5) 0.053(6) -0.004(4) -0.010(5) -0.013(4) C19 0.046(6) 0.032(5) 0.086(8) 0.025(5) -0.013(6) -0.012(5) C20 0.064(9) 0.128(14) 0.096(11) 0.076(11) -0.046(8) -0.064(10) C21 0.091(11) 0.126(14) 0.067(8) 0.037(9) -0.048(8) -0.073(11) C22 0.100(10) 0.093(10) 0.048(6) -0.001(6) -0.010(7) -0.068(9) C23 0.032(5) 0.047(6) 0.074(7) -0.022(5) 0.001(5) -0.018(4) C24 0.031(5) 0.056(6) 0.064(6) -0.016(5) -0.008(5) -0.022(5) C25 0.037(6) 0.060(7) 0.096(9) -0.026(6) -0.017(6) -0.016(5) C26 0.043(7) 0.083(9) 0.143(13) -0.047(9) -0.037(8) -0.014(7) C27 0.055(8) 0.091(10) 0.127(13) -0.046(9) -0.001(8) -0.037(8) C28 0.047(6) 0.070(8) 0.106(10) -0.043(7) 0.025(7) -0.036(6) Cl1 0.0576(14) 0.0316(11) 0.0258(10) -0.0003(8) -0.0019(10) -0.0149(10) Cl2 0.081(2) 0.0488(15) 0.0508(15) -0.0210(12) 0.0368(14) -0.0395(14) F1 0.085(5) 0.036(3) 0.061(4) 0.001(3) -0.015(3) -0.025(3) F3 0.054(4) 0.077(5) 0.070(4) -0.019(4) 0.002(3) -0.034(4) F2 0.110(6) 0.092(5) 0.075(5) -0.008(4) 0.010(4) -0.079(5) F4 0.099(6) 0.047(4) 0.118(6) -0.017(4) 0.030(5) -0.040(4) F6 0.141(8) 0.070(5) 0.052(4) -0.003(4) 0.013(5) -0.026(5) F5 0.104(6) 0.070(5) 0.104(6) 0.030(5) 0.051(5) -0.011(5) P1 0.0333(12) 0.0254(11) 0.0294(11) -0.0057(9) -0.0019(9) -0.0111(9) P2 0.0557(16) 0.0402(15) 0.0383(13) -0.0183(11) 0.0197(12) -0.0266(13) Pd1 0.0295(5) 0.0240(5) 0.0235(5) -0.0030(3) -0.0012(4) -0.0073(4) Pd2 0.0670(8) 0.0406(6) 0.0360(6) -0.0163(5) 0.0240(5) -0.0305(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.292(15) . ? C1 F1 1.390(11) . ? C1 P1 1.807(9) . ? C2 F3 1.294(14) . ? C2 F2 1.330(12) . ? C3 C8 1.493(14) . ? C3 C4 1.530(13) . ? C3 P1 1.830(9) . ? C3 H3 1 . ? C4 C5 1.552(15) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.524(17) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.521(16) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.576(14) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C14 1.524(13) . ? C9 C10 1.549(12) . ? C9 P1 1.839(9) . ? C9 H9 1 . ? C10 C11 1.525(13) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.528(16) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.495(15) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.534(13) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.29(2) . ? C15 F4 1.408(14) . ? C15 P2 1.810(11) . ? C16 F6 1.265(19) . ? C16 F5 1.354(15) . ? C17 C22 1.465(14) . ? C17 C18 1.554(12) . ? C17 P2 1.872(8) . ? C17 H17 1 . ? C18 C19 1.521(14) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.527(19) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.47(2) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.524(18) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C28 1.507(14) . ? C23 C24 1.525(14) . ? C23 P2 1.838(11) . ? C23 H23 1 . ? C24 C25 1.517(15) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.526(15) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.52(2) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.555(19) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? Cl1 Pd1 2.2911(19) . ? Cl2 Pd2 2.300(2) . ? P1 Pd1 2.332(2) . ? P2 Pd2 2.317(2) . ? Pd1 Cl1 2.2911(19) 2_656 ? Pd1 P1 2.332(2) 2_656 ? Pd2 Cl2 2.300(2) 2_757 ? Pd2 P2 2.317(2) 2_757 ? 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 C2 C1 F1 115.9(9) . . ? C2 C1 P1 126.2(9) . . ? F1 C1 P1 117.9(7) . . ? C1 C2 F3 124.4(10) . . ? C1 C2 F2 125.3(12) . . ? F2 C2 F3 110.3(10) . . ? C8 C3 C4 110.9(8) . . ? C8 C3 P1 109.9(6) . . ? C4 C3 P1 111.9(6) . . ? C8 C3 H3 108 . . ? C4 C3 H3 108 . . ? P1 C3 H3 108 . . ? C3 C4 C5 109.6(9) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 110.7(9) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 110.5(9) . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C6 C7 C8 110.2(9) . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C3 C8 C7 110.3(8) . . ? C3 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C3 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C14 C9 C10 111.2(8) . . ? C14 C9 P1 111.3(6) . . ? C10 C9 P1 112.2(6) . . ? C14 C9 H9 107.3 . . ? C10 C9 H9 107.3 . . ? P1 C9 H9 107.3 . . ? C11 C10 C9 110.1(8) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C10 C11 C12 112.3(9) . . ? C10 C11 H11A 109.2 . . ? C12 C11 H11A 109.2 . . ? C10 C11 H11B 109.2 . . ? C12 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 109.2(9) . . ? C13 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C12 C13 C14 111.3(9) . . ? C12 C13 H13A 109.4 . . ? C14 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? C14 C13 H13B 109.4 . . ? H13A C13 H13B 108 . . ? C9 C14 C13 109.1(8) . . ? C9 C14 H14A 109.9 . . ? C13 C14 H14A 109.9 . . ? C9 C14 H14B 109.9 . . ? C13 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C16 C15 F4 116.1(11) . . ? C16 C15 P2 126.4(11) . . ? F4 C15 P2 117.5(9) . . ? F6 C16 C15 124.9(12) . . ? F5 C16 F6 112.0(14) . . ? C15 C16 F5 123.1(16) . . ? C22 C17 C18 113.9(9) . . ? C22 C17 P2 111.2(7) . . ? C18 C17 P2 110.9(6) . . ? C22 C17 H17 106.8 . . ? C18 C17 H17 106.8 . . ? P2 C17 H17 106.8 . . ? C19 C18 C17 107.9(8) . . ? C19 C18 H18A 110.1 . . ? C17 C18 H18A 110.1 . . ? C19 C18 H18B 110.1 . . ? C17 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? C18 C19 C20 112.8(11) . . ? C18 C19 H19A 109 . . ? C20 C19 H19A 109 . . ? C18 C19 H19B 109 . . ? C20 C19 H19B 109 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C19 113.8(11) . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 111.0(12) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C17 C22 C21 107.6(9) . . ? C17 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? C17 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C28 C23 C24 111.3(10) . . ? C28 C23 P2 111.9(8) . . ? C24 C23 P2 109.4(6) . . ? C28 C23 H23 108 . . ? C24 C23 H23 108 . . ? P2 C23 H23 108 . . ? C25 C24 C23 111.3(8) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108 . . ? C24 C25 C26 110.6(10) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 111.4(12) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108 . . ? C26 C27 C28 110.5(10) . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C23 C28 C27 111.5(10) . . ? C23 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? C23 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108 . . ? C1 P1 C3 102.5(4) . . ? C1 P1 C9 103.5(4) . . ? C3 P1 C9 106.2(4) . . ? C1 P1 Pd1 113.5(3) . . ? C3 P1 Pd1 111.0(3) . . ? C9 P1 Pd1 118.7(3) . . ? C15 P2 C23 102.6(6) . . ? C15 P2 C17 105.4(5) . . ? C23 P2 C17 108.7(4) . . ? C15 P2 Pd2 114.0(4) . . ? C23 P2 Pd2 110.1(3) . . ? C17 P2 Pd2 115.2(3) . . ? Cl1 Pd1 Cl1 180.0000(10) 2_656 . ? Cl1 Pd1 P1 88.02(7) 2_656 . ? Cl1 Pd1 P1 91.98(7) . . ? Cl1 Pd1 P1 91.98(7) 2_656 2_656 ? Cl1 Pd1 P1 88.02(7) . 2_656 ? P1 Pd1 P1 180.00(10) . 2_656 ? Cl2 Pd2 Cl2 180.0000(10) . 2_757 ? Cl2 Pd2 P2 91.04(9) . 2_757 ? Cl2 Pd2 P2 88.96(9) 2_757 2_757 ? Cl2 Pd2 P2 88.96(9) . . ? Cl2 Pd2 P2 91.04(9) 2_757 . ? P2 Pd2 P2 180.00(12) 2_757 . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-07-03 at 23:36:53 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : b psi_scan struct data_PdBrPhpfv2 _database_code_depnum_ccdc_archive 'CCDC 656536' _audit_creation_date 2007-07-03T23:36:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(phenylbisperfluorovinylphosphine)palladium(II) bromide ; _chemical_formula_moiety 'C20 H10 Br2 F12 P2 Pd1' _chemical_formula_sum 'C20 H10 Br2 F12 P2 Pd' _chemical_formula_weight 806.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.105(2) _cell_length_b 10.0130(10) _cell_length_c 7.8700(10) _cell_angle_alpha 109.062(10) _cell_angle_beta 102.91(2) _cell_angle_gamma 99.26(2) _cell_volume 639.34(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 25 _cell_measurement_theta_max 36 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.628 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.1091 _exptl_absorpt_correction_T_max 0.2744 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.0577 _diffrn_reflns_number 2191 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 6.81 _diffrn_reflns_theta_max 64.99 _diffrn_reflns_theta_full 64.99 _diffrn_measured_fraction_theta_full 0.938 _diffrn_measured_fraction_theta_max 0.938 _reflns_number_total 2048 _reflns_number_gt 1474 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+0.9402P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 2048 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1562 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.775 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.14 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pd1 Pd 0.5 0 0 0.0541(3) Uani 1 2 d S . . Br1 Br 0.40193(13) 0.02317(13) 0.26525(16) 0.0805(4) Uani 1 1 d . . . P1 P 0.6937(3) 0.2101(3) 0.1866(4) 0.0610(6) Uani 1 1 d . . . C1 C 0.7998(11) 0.2087(12) 0.4083(15) 0.071(3) Uani 1 1 d . . . C2 C 0.8205(12) 0.0938(17) 0.4415(19) 0.084(3) Uani 1 1 d . . . C3 C 0.8539(13) 0.2514(14) 0.0925(19) 0.084(3) Uani 1 1 d . . . C4 C 0.9721(16) 0.207(2) 0.098(2) 0.122(6) Uani 1 1 d . . . C5 C 0.6289(11) 0.3767(10) 0.2419(15) 0.066(2) Uani 1 1 d . . . C6 C 0.4726(13) 0.3669(12) 0.1798(18) 0.079(3) Uani 1 1 d . . . H6 H 0.401 0.2764 0.1149 0.095 Uiso 1 1 calc R . . C7 C 0.4243(16) 0.4945(15) 0.216(2) 0.101(4) Uani 1 1 d . . . H7 H 0.3188 0.4891 0.1738 0.121 Uiso 1 1 calc R . . C8 C 0.5254(19) 0.6260(15) 0.311(2) 0.105(4) Uani 1 1 d . . . H8 H 0.4901 0.7104 0.3343 0.126 Uiso 1 1 calc R . . C9 C 0.678(2) 0.6346(15) 0.371(2) 0.118(5) Uani 1 1 d . . . H9 H 0.7489 0.7255 0.438 0.142 Uiso 1 1 calc R . . C10 C 0.7314(16) 0.5096(13) 0.334(2) 0.099(4) Uani 1 1 d . . . H10 H 0.8375 0.5165 0.3734 0.118 Uiso 1 1 calc R . . F1 F 0.8693(8) 0.3399(8) 0.5516(11) 0.109(2) Uani 1 1 d . . . F2 F 0.9056(9) 0.0972(11) 0.6046(12) 0.119(3) Uani 1 1 d . . . F3 F 0.7662(10) -0.0371(9) 0.3270(13) 0.114(3) Uani 1 1 d . . . F4 F 0.8301(12) 0.3447(12) -0.0128(16) 0.141(3) Uani 1 1 d . . . F5 F 1.0765(10) 0.2488(15) 0.0115(15) 0.183(6) Uani 1 1 d . . . F6 F 1.0051(13) 0.1264(17) 0.1831(17) 0.166(5) 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 Pd1 0.0515(5) 0.0515(5) 0.0624(6) 0.0225(4) 0.0178(4) 0.0179(4) Br1 0.0809(7) 0.0867(8) 0.0704(7) 0.0236(6) 0.0316(6) 0.0120(6) P1 0.0526(11) 0.0607(14) 0.0697(15) 0.0250(12) 0.0164(10) 0.0156(10) C1 0.062(5) 0.073(7) 0.070(6) 0.030(5) 0.004(5) 0.013(5) C2 0.064(5) 0.114(10) 0.091(8) 0.060(8) 0.019(6) 0.028(6) C3 0.069(6) 0.080(7) 0.095(8) 0.028(6) 0.025(6) 0.006(5) C4 0.081(8) 0.164(17) 0.111(12) 0.027(11) 0.039(8) 0.042(10) C5 0.067(5) 0.045(5) 0.077(6) 0.015(4) 0.015(5) 0.013(4) C6 0.078(6) 0.060(6) 0.095(8) 0.028(6) 0.016(6) 0.025(5) C7 0.087(7) 0.085(9) 0.140(12) 0.046(8) 0.032(8) 0.040(7) C8 0.126(11) 0.075(8) 0.121(11) 0.040(8) 0.030(9) 0.043(8) C9 0.122(11) 0.060(8) 0.134(12) 0.025(8) -0.002(10) 0.004(7) C10 0.095(8) 0.055(7) 0.127(11) 0.031(7) 0.005(8) 0.014(6) F1 0.098(5) 0.102(5) 0.093(5) 0.025(4) -0.010(4) 0.014(4) F2 0.090(4) 0.190(9) 0.114(6) 0.097(6) 0.026(4) 0.054(5) F3 0.113(5) 0.094(6) 0.145(7) 0.066(5) 0.021(5) 0.037(5) F4 0.146(7) 0.160(9) 0.187(10) 0.112(8) 0.096(7) 0.066(7) F5 0.081(5) 0.277(15) 0.146(8) 0.031(9) 0.059(5) -0.012(7) F6 0.154(9) 0.272(16) 0.159(9) 0.127(11) 0.085(8) 0.132(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pd1 P1 2.307(2) 2_655 ? Pd1 P1 2.307(2) . ? Pd1 Br1 2.4067(11) . ? Pd1 Br1 2.4067(11) 2_655 ? P1 C1 1.802(10) . ? P1 C5 1.810(10) . ? P1 C3 1.826(11) . ? C5 C10 1.355(15) . ? C5 C6 1.374(14) . ? C6 C7 1.380(16) . ? C6 H6 0.93 . ? C7 C8 1.34(2) . ? C7 H7 0.93 . ? C8 C9 1.35(2) . ? C8 H8 0.93 . ? C9 C10 1.380(19) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? C1 C2 1.293(17) . ? C1 F1 1.357(13) . ? C2 F3 1.263(16) . ? C2 F2 1.329(13) . ? C3 C4 1.226(19) . ? C3 F4 1.448(15) . ? C4 F6 1.24(2) . ? C4 F5 1.375(18) . ? 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 P1 Pd1 P1 180.00(11) 2_655 . ? P1 Pd1 Br1 91.44(7) 2_655 . ? P1 Pd1 Br1 88.56(7) . . ? P1 Pd1 Br1 88.56(7) 2_655 2_655 ? P1 Pd1 Br1 91.44(7) . 2_655 ? Br1 Pd1 Br1 180.00(5) . 2_655 ? C1 P1 C5 106.1(5) . . ? C1 P1 C3 100.5(5) . . ? C5 P1 C3 103.0(5) . . ? C1 P1 Pd1 114.4(4) . . ? C5 P1 Pd1 114.9(3) . . ? C3 P1 Pd1 116.3(4) . . ? C6 C5 C10 119.8(10) . . ? C10 C5 P1 121.5(9) . . ? C6 C5 P1 118.6(7) . . ? C5 C6 C7 118.4(11) . . ? C5 C6 H6 120.8 . . ? C6 C6 H6 120.8 . . ? C8 C7 C6 121.8(13) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C9 119.4(13) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 120.4(13) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C5 C10 C9 120.1(13) . . ? C5 C10 H10 120 . . ? C9 C10 H10 120 . . ? C2 C1 F1 116.8(10) . . ? C2 C1 P1 125.7(10) . . ? F1 C1 P1 117.4(8) . . ? F3 C2 C1 126.3(11) . . ? F3 C2 F2 109.6(11) . . ? C1 C2 F2 124.1(14) . . ? C4 C3 F4 116.6(14) . . ? C4 C3 P1 129.9(14) . . ? F4 C3 P1 113.4(8) . . ? C3 C4 F6 122.7(16) . . ? C3 C4 F5 120(2) . . ? F6 C4 F5 117.0(14) . . ? 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 P1 Pd1 P1 C1 -14E1(10) 2_655 . . . ? Br1 Pd1 P1 C1 51.3(4) . . . . ? Br1 Pd1 P1 C1 -128.7(4) 2_655 . . . ? P1 Pd1 P1 C5 10E1(10) 2_655 . . . ? Br1 Pd1 P1 C5 -71.8(4) . . . . ? Br1 Pd1 P1 C5 108.2(4) 2_655 . . . ? P1 Pd1 P1 C3 -2E1(10) 2_655 . . . ? Br1 Pd1 P1 C3 167.8(5) . . . . ? Br1 Pd1 P1 C3 -12.2(5) 2_655 . . . ? C1 P1 C5 C10 59.1(12) . . . . ? C3 P1 C5 C10 -46.0(12) . . . . ? Pd1 P1 C5 C10 -173.5(10) . . . . ? C1 P1 C5 C6 -124.1(10) . . . . ? C3 P1 C5 C6 130.8(10) . . . . ? Pd1 P1 C5 C6 3.3(11) . . . . ? C10 C5 C6 C7 -0.7(19) . . . . ? P1 C5 C6 C7 -177.6(10) . . . . ? C5 C6 C7 C8 0(2) . . . . ? C6 C7 C8 C9 0(3) . . . . ? C7 C8 C9 C10 1(3) . . . . ? C6 C5 C10 C9 2(2) . . . . ? P1 C5 C10 C9 178.7(12) . . . . ? C8 C9 C10 C5 -2(3) . . . . ? C5 P1 C1 C2 155.4(10) . . . . ? C3 P1 C1 C2 -97.7(11) . . . . ? Pd1 P1 C1 C2 27.6(11) . . . . ? C5 P1 C1 F1 -27.3(9) . . . . ? C3 P1 C1 F1 79.6(9) . . . . ? Pd1 P1 C1 F1 -155.0(7) . . . . ? F1 C1 C2 F3 -179.8(10) . . . . ? P1 C1 C2 F3 -2.4(18) . . . . ? F1 C1 C2 F2 -0.6(17) . . . . ? P1 C1 C2 F2 176.8(8) . . . . ? C1 P1 C3 C4 40.0(16) . . . . ? C5 P1 C3 C4 149.4(15) . . . . ? Pd1 P1 C3 C4 -84.1(16) . . . . ? C1 P1 C3 F4 -143.8(9) . . . . ? C5 P1 C3 F4 -34.3(10) . . . . ? Pd1 P1 C3 F4 92.2(9) . . . . ? F4 C3 C4 F6 -179.8(15) . . . . ? P1 C3 C4 F6 -4(3) . . . . ? F4 C3 C4 F5 2(2) . . . . ? P1 C3 C4 F5 177.7(11) . . . . ? #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-07-03 at 17:22:10 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : akb02 dreduc psi_scan struct data_PdIPPhpfv2 _database_code_depnum_ccdc_archive 'CCDC 656537' _audit_creation_date 2007-07-03T17:22:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H10 F12 I2 P2 Pd1' _chemical_formula_sum 'C20 H10 F12 I2 P2 Pd' _chemical_formula_weight 900.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9798(10) _cell_length_b 11.4305(10) _cell_length_c 12.382(2) _cell_angle_alpha 106.783(10) _cell_angle_beta 94.101(10) _cell_angle_gamma 102.413(10) _cell_volume 1307.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.5 _cell_measurement_theta_max 19.9 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.289 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 4 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.4936 _exptl_absorpt_correction_T_max 0.7345 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.052601 _diffrn_orient_matrix_ub_12 0.0555 _diffrn_orient_matrix_ub_13 0.075721 _diffrn_orient_matrix_ub_21 0.087036 _diffrn_orient_matrix_ub_22 0.011569 _diffrn_orient_matrix_ub_23 -0.035203 _diffrn_orient_matrix_ub_31 -0.020102 _diffrn_orient_matrix_ub_32 0.075346 _diffrn_orient_matrix_ub_33 -0.017071 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 5 -2 2 3 -8 7 -3 -3 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_unetI/netI 0.0203 _diffrn_reflns_number 4874 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4583 _reflns_number_gt 3784 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+1.9751P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 4583 _refine_ls_number_parameters 334 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.894 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.112 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.5091(6) 0.2162(5) 0.5532(5) 0.0491(14) Uani 1 1 d . . . C2 C 0.3787(7) 0.1861(6) 0.5575(7) 0.0636(18) Uani 1 1 d . . . C3 C 0.6248(6) 0.2306(5) 0.3602(5) 0.0442(13) Uani 1 1 d . . . C4 C 0.5501(8) 0.1219(6) 0.2997(6) 0.0586(16) Uani 1 1 d . . . C5 C 0.7746(5) 0.3874(5) 0.5706(5) 0.0419(12) Uani 1 1 d . . . C6 C 0.8273(6) 0.5121(6) 0.6313(6) 0.0550(15) Uani 1 1 d . . . H6 H 0.7716 0.5685 0.6361 0.066 Uiso 1 1 calc R . . C7 C 0.9619(7) 0.5546(7) 0.6853(7) 0.073(2) Uani 1 1 d . . . H7 H 0.9973 0.6395 0.7257 0.087 Uiso 1 1 calc R . . C8 C 1.0439(7) 0.4713(7) 0.6794(7) 0.0675(19) Uani 1 1 d . . . H8 H 1.1346 0.4995 0.7167 0.081 Uiso 1 1 calc R . . C9 C 0.9928(6) 0.3481(7) 0.6193(6) 0.0630(18) Uani 1 1 d . . . H9 H 1.0491 0.2923 0.6152 0.076 Uiso 1 1 calc R . . C10 C 0.8588(6) 0.3041(6) 0.5641(5) 0.0510(14) Uani 1 1 d . . . H10 H 0.8249 0.2193 0.5227 0.061 Uiso 1 1 calc R . . C11 C 0.9422(6) 0.0438(6) 0.7391(5) 0.0506(14) Uani 1 1 d . . . C12 C 1.0118(8) -0.0352(7) 0.6922(7) 0.0702(19) Uani 1 1 d . . . C15 C 0.8015(6) 0.1804(5) 0.9096(5) 0.0478(13) Uani 1 1 d . . . C16 C 0.7643(8) 0.2557(7) 0.8486(6) 0.0674(19) Uani 1 1 d . . . H16 H 0.8181 0.2762 0.7953 0.081 Uiso 1 1 calc R . . C17 C 0.6470(9) 0.3000(8) 0.8675(7) 0.084(2) Uani 1 1 d . . . H17 H 0.6214 0.3496 0.8258 0.101 Uiso 1 1 calc R . . C18 C 0.5694(9) 0.2724(8) 0.9453(7) 0.082(2) Uani 1 1 d . . . H18 H 0.4907 0.303 0.9571 0.099 Uiso 1 1 calc R . . C19 C 0.6059(8) 0.1992(8) 1.0076(7) 0.078(2) Uani 1 1 d . . . H19 H 0.5526 0.1811 1.062 0.094 Uiso 1 1 calc R . . C20 C 0.7215(7) 0.1527(7) 0.9890(6) 0.0619(17) Uani 1 1 d . . . H20 H 0.7455 0.1023 1.0305 0.074 Uiso 1 1 calc R . . F1 F 0.5857(4) 0.1461(4) 0.5873(4) 0.0709(11) Uani 1 1 d . . . F2 F 0.3169(5) 0.0964(4) 0.5960(5) 0.1019(17) Uani 1 1 d . . . F3 F 0.2887(4) 0.2407(4) 0.5241(5) 0.0979(16) Uani 1 1 d . . . F4 F 0.7398(4) 0.2749(4) 0.3191(3) 0.0655(10) Uani 1 1 d . . . F5 F 0.5812(5) 0.0532(4) 0.2035(4) 0.0862(13) Uani 1 1 d . . . F6 F 0.4331(5) 0.0631(4) 0.3215(4) 0.0853(13) Uani 1 1 d . . . F7 F 0.8554(5) 0.0714(5) 0.6671(3) 0.0814(13) Uani 1 1 d . . . F8 F 1.0055(6) -0.0867(5) 0.5828(4) 0.1014(16) Uani 1 1 d . . . F9 F 1.0996(6) -0.0721(6) 0.7489(5) 0.120(2) Uani 1 1 d . . . F10 F 1.0470(7) 0.3918(6) 1.0211(6) 0.1215(19) Uani 1 1 d . . . F11A F 1.2161(12) 0.4633(11) 0.9531(10) 0.105(3) Uiso 0.5 1 d PD . . F12 F 1.2000(6) 0.2285(6) 0.8083(5) 0.121(2) Uani 1 1 d . . . P1 P 0.59941(13) 0.33455(12) 0.49564(12) 0.0369(3) Uani 1 1 d . . . P2 P 0.95504(15) 0.12272(14) 0.89041(13) 0.0440(3) Uani 1 1 d . . . Pd1 Pd 0.5 0.5 0.5 0.03544(14) Uani 1 2 d S . . Pd2 Pd 1 0 1 0.04057(15) Uani 1 2 d S . . I1 I 0.47474(4) 0.52845(4) 0.71296(3) 0.04918(12) Uani 1 1 d . . . I2 I 1.21546(4) 0.17180(4) 1.12069(4) 0.05642(14) Uani 1 1 d . . . C14A C 1.1185(16) 0.3640(13) 0.9503(13) 0.067(4) Uiso 0.5 1 d PD . . C14B C 1.1767(18) 0.3081(17) 0.8797(17) 0.089(5) Uiso 0.5 1 d PD . . C13B C 1.0684(14) 0.2771(16) 0.9225(14) 0.060(4) Uiso 0.5 1 d PD . . C13A C 1.0954(14) 0.2515(11) 0.8866(12) 0.047(3) Uiso 0.5 1 d PD . . F11B F 1.2675(11) 0.4250(10) 0.9152(10) 0.094(3) Uiso 0.5 1 d PD . . 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 C1 0.051(3) 0.042(3) 0.059(4) 0.019(3) 0.013(3) 0.016(3) C2 0.056(4) 0.050(4) 0.081(5) 0.016(3) 0.025(3) 0.007(3) C3 0.048(3) 0.040(3) 0.050(3) 0.015(3) 0.007(3) 0.020(2) C4 0.078(5) 0.050(4) 0.049(4) 0.016(3) 0.004(3) 0.018(3) C5 0.032(3) 0.044(3) 0.053(3) 0.017(3) 0.008(2) 0.012(2) C6 0.038(3) 0.052(3) 0.074(4) 0.012(3) 0.007(3) 0.019(3) C7 0.043(3) 0.055(4) 0.107(6) 0.010(4) 0.003(4) 0.008(3) C8 0.039(3) 0.083(5) 0.079(5) 0.025(4) 0.000(3) 0.016(3) C9 0.045(3) 0.084(5) 0.075(5) 0.032(4) 0.014(3) 0.036(3) C10 0.045(3) 0.053(3) 0.061(4) 0.017(3) 0.009(3) 0.024(3) C11 0.053(3) 0.057(4) 0.048(3) 0.019(3) 0.009(3) 0.022(3) C12 0.067(4) 0.072(5) 0.078(5) 0.017(4) 0.018(4) 0.034(4) C15 0.060(3) 0.046(3) 0.043(3) 0.012(3) 0.007(3) 0.028(3) C16 0.090(5) 0.079(5) 0.057(4) 0.033(4) 0.018(4) 0.051(4) C17 0.113(6) 0.094(6) 0.070(5) 0.028(4) 0.008(5) 0.074(5) C18 0.085(5) 0.100(6) 0.073(5) 0.017(5) 0.012(4) 0.061(5) C19 0.086(5) 0.092(6) 0.076(5) 0.028(4) 0.033(4) 0.051(5) C20 0.077(4) 0.066(4) 0.059(4) 0.025(3) 0.015(3) 0.041(4) F1 0.076(2) 0.063(2) 0.096(3) 0.052(2) 0.019(2) 0.0250(19) F2 0.101(3) 0.073(3) 0.131(4) 0.040(3) 0.058(3) -0.003(3) F3 0.043(2) 0.083(3) 0.165(5) 0.035(3) 0.017(3) 0.013(2) F4 0.059(2) 0.073(2) 0.067(2) 0.018(2) 0.0276(18) 0.0209(19) F5 0.132(4) 0.061(2) 0.056(2) -0.001(2) 0.010(2) 0.031(3) F6 0.096(3) 0.071(3) 0.067(3) 0.019(2) -0.002(2) -0.016(2) F7 0.109(3) 0.102(3) 0.051(2) 0.026(2) 0.008(2) 0.061(3) F8 0.116(4) 0.114(4) 0.074(3) 0.006(3) 0.038(3) 0.053(3) F9 0.113(4) 0.155(5) 0.110(4) 0.019(4) 0.013(3) 0.103(4) F10 0.123(5) 0.098(4) 0.122(5) 0.015(4) 0.005(4) 0.013(3) F12 0.104(4) 0.104(4) 0.121(5) 0.005(4) 0.025(3) -0.006(3) P1 0.0338(6) 0.0339(7) 0.0480(8) 0.0152(6) 0.0075(6) 0.0149(5) P2 0.0448(8) 0.0412(8) 0.0498(9) 0.0184(7) 0.0019(6) 0.0146(6) Pd1 0.0317(3) 0.0346(3) 0.0437(3) 0.0135(2) 0.0051(2) 0.0143(2) Pd2 0.0368(3) 0.0359(3) 0.0498(4) 0.0153(3) -0.0024(2) 0.0107(2) I1 0.0558(2) 0.0534(2) 0.0462(2) 0.01859(18) 0.01079(17) 0.02441(17) I2 0.0484(2) 0.0462(2) 0.0666(3) 0.01542(19) -0.01053(18) 0.00384(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.282(9) . ? C1 F1 1.349(7) . ? C1 P1 1.810(6) . ? C2 F3 1.306(8) . ? C2 F2 1.307(8) . ? C3 C4 1.283(9) . ? C3 F4 1.346(7) . ? C3 P1 1.825(6) . ? C4 F6 1.304(8) . ? C4 F5 1.322(8) . ? C5 C6 1.370(8) . ? C5 C10 1.389(8) . ? C5 P1 1.809(5) . ? C6 C7 1.374(9) . ? C6 H6 0.93 . ? C7 C8 1.373(10) . ? C7 H7 0.93 . ? C8 C9 1.352(10) . ? C8 H8 0.93 . ? C9 C10 1.374(9) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? C11 C12 1.288(9) . ? C11 F7 1.346(7) . ? C11 P2 1.811(6) . ? C12 F9 1.297(9) . ? C12 F8 1.303(9) . ? C15 C20 1.375(9) . ? C15 C16 1.386(8) . ? C15 P2 1.798(6) . ? C16 C17 1.382(10) . ? C16 H16 0.93 . ? C17 C18 1.343(12) . ? C17 H17 0.93 . ? C18 C19 1.375(11) . ? C18 H18 0.93 . ? C19 C20 1.377(9) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? F10 C14A 1.185(15) . ? F10 C13B 1.577(19) . ? F11A F11B 0.829(13) . ? F11A C14A 1.318(15) . ? F11A C14B 1.69(2) . ? F12 C14B 1.148(19) . ? F12 C13A 1.488(16) . ? P1 Pd1 2.3063(13) . ? P2 C13B 1.796(15) . ? P2 C13A 1.815(13) . ? P2 Pd2 2.3007(14) . ? Pd1 P1 2.3064(13) 2_666 ? Pd1 I1 2.5995(6) . ? Pd1 I1 2.5995(6) 2_666 ? Pd2 P2 2.3007(14) 2_757 ? Pd2 I2 2.5968(6) . ? Pd2 I2 2.5968(6) 2_757 ? 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 C2 C1 F1 116.6(6) . . ? C2 C1 P1 126.9(5) . . ? F1 C1 P1 116.3(4) . . ? C1 C2 F3 124.8(6) . . ? C1 C2 F2 124.9(7) . . ? F3 C2 F2 110.3(6) . . ? C4 C3 F4 115.9(6) . . ? C4 C3 P1 129.4(5) . . ? F4 C3 P1 114.7(4) . . ? C3 C4 F6 126.2(6) . . ? C3 C4 F5 124.0(7) . . ? F6 C4 F5 109.8(6) . . ? C6 C5 C10 119.2(5) . . ? C6 C5 P1 119.8(4) . . ? C10 C5 P1 120.9(4) . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 119.9(7) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 119.9(6) . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C8 C9 C10 121.0(6) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C5 119.4(6) . . ? C9 C10 H10 120.3 . . ? C5 C10 H10 120.3 . . ? C12 C11 F7 115.9(6) . . ? C12 C11 P2 125.9(5) . . ? F7 C11 P2 118.2(4) . . ? C11 C12 F9 123.9(7) . . ? C11 C12 F8 125.0(7) . . ? F9 C12 F8 111.1(6) . . ? C20 C15 C16 119.1(6) . . ? C20 C15 P2 119.4(4) . . ? C16 C15 P2 121.4(5) . . ? C17 C16 C15 119.6(7) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 120.8(7) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.3(7) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 120.3(6) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C5 P1 C1 105.9(3) . . ? C5 P1 C3 100.7(3) . . ? C1 P1 C3 98.8(3) . . ? C5 P1 Pd1 112.27(18) . . ? C1 P1 Pd1 116.50(19) . . ? C3 P1 Pd1 120.43(18) . . ? C13B P2 C15 94.0(6) . . ? C13B P2 C11 107.9(6) . . ? C15 P2 C11 106.2(3) . . ? C15 P2 C13A 108.2(5) . . ? C11 P2 C13A 92.4(5) . . ? C13B P2 Pd2 117.6(5) . . ? C15 P2 Pd2 116.3(2) . . ? C11 P2 Pd2 112.9(2) . . ? C13A P2 Pd2 117.8(4) . . ? P1 Pd1 P1 180 . 2_666 ? P1 Pd1 I1 89.26(4) . . ? P1 Pd1 I1 90.74(4) 2_666 . ? P1 Pd1 I1 90.74(4) . 2_666 ? P1 Pd1 I1 89.26(4) 2_666 2_666 ? I1 Pd1 I1 180 . 2_666 ? P2 Pd2 P2 180.0000(10) 2_757 . ? P2 Pd2 I2 87.35(4) 2_757 . ? P2 Pd2 I2 92.65(4) . . ? P2 Pd2 I2 92.65(4) 2_757 2_757 ? P2 Pd2 I2 87.35(4) . 2_757 ? I2 Pd2 I2 180 . 2_757 ? F10 C14A C13A 119.9(15) . . ? F10 C14A F11A 110.5(13) . . ? C13A C14A F11A 129.6(16) . . ? F12 C14B F11B 119.5(15) . . ? C13B C14B F11B 125.2(18) . . ? C14B C13B F10 111.4(14) . . ? C14B C13B P2 127.5(15) . . ? F10 C13B P2 120.9(9) . . ? C14A C13A F12 113.9(12) . . ? C14A C13A P2 125.3(13) . . ? F12 C13A P2 120.7(8) . . ? 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 F1 C1 C2 F3 -177.5(6) . . . . ? P1 C1 C2 F3 -2.7(11) . . . . ? F1 C1 C2 F2 2.5(11) . . . . ? P1 C1 C2 F2 177.2(5) . . . . ? F4 C3 C4 F6 -177.9(6) . . . . ? P1 C3 C4 F6 2.7(10) . . . . ? F4 C3 C4 F5 1.2(9) . . . . ? P1 C3 C4 F5 -178.1(5) . . . . ? C10 C5 C6 C7 0.0(10) . . . . ? P1 C5 C6 C7 -177.6(6) . . . . ? C5 C6 C7 C8 -0.7(12) . . . . ? C6 C7 C8 C9 0.9(12) . . . . ? C7 C8 C9 C10 -0.4(12) . . . . ? C8 C9 C10 C5 -0.3(10) . . . . ? C6 C5 C10 C9 0.5(9) . . . . ? P1 C5 C10 C9 178.1(5) . . . . ? F7 C11 C12 F9 -179.9(7) . . . . ? P2 C11 C12 F9 2.0(12) . . . . ? F7 C11 C12 F8 1.3(11) . . . . ? P2 C11 C12 F8 -176.8(6) . . . . ? C20 C15 C16 C17 -0.8(11) . . . . ? P2 C15 C16 C17 -178.8(6) . . . . ? C15 C16 C17 C18 0.9(13) . . . . ? C16 C17 C18 C19 0.0(14) . . . . ? C17 C18 C19 C20 -0.8(14) . . . . ? C16 C15 C20 C19 0.0(11) . . . . ? P2 C15 C20 C19 178.0(6) . . . . ? C18 C19 C20 C15 0.8(12) . . . . ? C6 C5 P1 C1 -121.4(5) . . . . ? C10 C5 P1 C1 61.0(5) . . . . ? C6 C5 P1 C3 136.2(5) . . . . ? C10 C5 P1 C3 -41.4(5) . . . . ? C6 C5 P1 Pd1 6.8(6) . . . . ? C10 C5 P1 Pd1 -170.8(4) . . . . ? C2 C1 P1 C5 153.1(6) . . . . ? F1 C1 P1 C5 -32.1(5) . . . . ? C2 C1 P1 C3 -103.0(7) . . . . ? F1 C1 P1 C3 71.7(5) . . . . ? C2 C1 P1 Pd1 27.5(7) . . . . ? F1 C1 P1 Pd1 -157.8(4) . . . . ? C4 C3 P1 C5 137.8(6) . . . . ? F4 C3 P1 C5 -41.5(4) . . . . ? C4 C3 P1 C1 29.7(6) . . . . ? F4 C3 P1 C1 -149.6(4) . . . . ? C4 C3 P1 Pd1 -98.2(6) . . . . ? F4 C3 P1 Pd1 82.5(4) . . . . ? C20 C15 P2 C13B -121.8(7) . . . . ? C16 C15 P2 C13B 56.1(8) . . . . ? C20 C15 P2 C11 128.3(5) . . . . ? C16 C15 P2 C11 -53.8(6) . . . . ? C20 C15 P2 C13A -133.6(7) . . . . ? C16 C15 P2 C13A 44.3(7) . . . . ? C20 C15 P2 Pd2 1.8(6) . . . . ? C16 C15 P2 Pd2 179.7(5) . . . . ? C12 C11 P2 C13B 97.7(8) . . . . ? F7 C11 P2 C13B -80.4(7) . . . . ? C12 C11 P2 C15 -162.5(6) . . . . ? F7 C11 P2 C15 19.4(6) . . . . ? C12 C11 P2 C13A 87.7(8) . . . . ? F7 C11 P2 C13A -90.3(6) . . . . ? C12 C11 P2 Pd2 -33.9(7) . . . . ? F7 C11 P2 Pd2 148.0(4) . . . . ? C5 P1 Pd1 P1 7E1(9) . . . 2_666 ? C1 P1 Pd1 P1 -17E1(9) . . . 2_666 ? C3 P1 Pd1 P1 -5E1(9) . . . 2_666 ? C5 P1 Pd1 I1 -73.6(2) . . . . ? C1 P1 Pd1 I1 48.8(2) . . . . ? C3 P1 Pd1 I1 168.2(2) . . . . ? C5 P1 Pd1 I1 106.4(2) . . . 2_666 ? C1 P1 Pd1 I1 -131.2(2) . . . 2_666 ? C3 P1 Pd1 I1 -11.8(2) . . . 2_666 ? C13B P2 Pd2 P2 11E1(10) . . . 2_757 ? C15 P2 Pd2 P2 0E1(10) . . . 2_757 ? C11 P2 Pd2 P2 -12E1(10) . . . 2_757 ? C13A P2 Pd2 P2 13E1(10) . . . 2_757 ? C13B P2 Pd2 I2 -0.7(6) . . . . ? C15 P2 Pd2 I2 -111.0(2) . . . . ? C11 P2 Pd2 I2 125.9(2) . . . . ? C13A P2 Pd2 I2 20.0(5) . . . . ? C13B P2 Pd2 I2 179.3(6) . . . 2_757 ? C15 P2 Pd2 I2 69.0(2) . . . 2_757 ? C11 P2 Pd2 I2 -54.1(2) . . . 2_757 ? C13A P2 Pd2 I2 -160.0(5) . . . 2_757 ? F12 C14B C13B F10 178.9(14) . . . . ? F12 C14B C13B P2 4(3) . . . . ? F11B C14B C13B P2 -173.1(13) . . . . ? C15 P2 C13B C14B -145.7(16) . . . . ? C11 P2 C13B C14B -37.3(18) . . . . ? Pd2 P2 C13B C14B 91.7(17) . . . . ? C15 P2 C13B F10 40.0(10) . . . . ? C11 P2 C13B F10 148.4(9) . . . . ? Pd2 P2 C13B F10 -82.6(10) . . . . ? F10 C14A C13A F12 -175.4(12) . . . . ? F11A C14A C13A F12 4(2) . . . . ? F10 C14A C13A P2 2(2) . . . . ? F11A C14A C13A P2 -179.2(13) . . . . ? C15 P2 C13A C14A 41.0(14) . . . . ? C11 P2 C13A C14A 148.8(13) . . . . ? Pd2 P2 C13A C14A -93.7(13) . . . . ? C15 P2 C13A F12 -142.4(8) . . . . ? C11 P2 C13A F12 -34.5(9) . . . . ? Pd2 P2 C13A F12 83.0(9) . . . . ? #===END data_nb2b _database_code_depnum_ccdc_archive 'CCDC 656538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis and trans -bis(diisopropylperfluorovinylphosphine)platinum(II) chloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 Cl2 F6 P2 Pt1' _chemical_formula_sum 'C16 H28 Cl2 F6 P2 Pt' _chemical_formula_weight 662.3 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1294(9) _cell_length_b 16.184(7) _cell_length_c 25.965(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.315(15) _cell_angle_gamma 90.00 _cell_volume 3410.4(18) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 6.595 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.3522 _exptl_absorpt_correction_T_max 0.4379 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6444 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5986 _reflns_number_gt 4824 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+19.9058P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5986 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.128 _refine_ls_shift/su_mean 0.003 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 Pt1 Pt 0.48334(6) 0.06482(2) 0.296421(16) 0.02690(18) Uani 1 1 d . . . Pt2 Pt 0.0000 0.0000 0.0000 0.0273(2) Uani 1 2 d S . . Cl1 Cl 0.6094(5) 0.1610(2) 0.24438(14) 0.0557(11) Uani 1 1 d . . . Cl2 Cl 0.5275(6) -0.0310(2) 0.23189(13) 0.0634(12) Uani 1 1 d . . . Cl3 Cl -0.0298(5) -0.10277(19) 0.05945(12) 0.0454(8) Uani 1 1 d . . . P1 P 0.4710(4) 0.16948(17) 0.35272(11) 0.0270(6) Uani 1 1 d . . . P2 P 0.3588(4) -0.03984(18) 0.33555(12) 0.0307(7) Uani 1 1 d . . . P3 P 0.0766(4) 0.0884(2) 0.06593(12) 0.0349(7) Uani 1 1 d . . . F1 F 0.1753(9) 0.1477(5) 0.3866(3) 0.051(2) Uani 1 1 d . . . F2 F 0.2338(13) 0.1530(6) 0.4861(4) 0.073(3) Uani 1 1 d . . . F3 F 0.4953(14) 0.1677(7) 0.4821(3) 0.076(3) Uani 1 1 d . . . F4 F 0.4674(11) -0.0191(5) 0.4325(3) 0.049(2) Uani 1 1 d . . . F5 F 0.1970(13) -0.0220(5) 0.4808(4) 0.067(3) Uani 1 1 d . . . F6 F 0.0412(11) -0.0407(6) 0.4110(3) 0.058(2) Uani 1 1 d . . . F7 F 0.1359(15) 0.2529(5) 0.0727(4) 0.081(3) Uani 1 1 d . . . F8 F -0.1339(15) 0.3049(5) 0.0225(4) 0.076(3) Uani 1 1 d . . . F9 F -0.2265(11) 0.1816(6) 0.0100(4) 0.061(2) Uani 1 1 d . . . C1 C 0.3341(16) 0.1580(7) 0.4049(5) 0.033(3) Uani 1 1 d . . . C2 C 0.353(2) 0.1608(8) 0.4545(5) 0.048(4) Uani 1 1 d . . . C3 C 0.6740(17) 0.1940(9) 0.3870(5) 0.041(3) Uani 1 1 d . . . H3 H 0.6529 0.2260 0.4180 0.050 Uiso 1 1 calc R . . C4 C 0.7604(19) 0.1159(11) 0.4036(6) 0.059(4) Uani 1 1 d . . . H4A H 0.7865 0.0847 0.3737 0.088 Uiso 1 1 calc R . . H4B H 0.6899 0.0838 0.4243 0.088 Uiso 1 1 calc R . . H4C H 0.8601 0.1292 0.4235 0.088 Uiso 1 1 calc R . . C5 C 0.780(2) 0.2464(11) 0.3531(7) 0.070(5) Uani 1 1 d . . . H5A H 0.8819 0.2596 0.3718 0.105 Uiso 1 1 calc R . . H5B H 0.7224 0.2965 0.3438 0.105 Uiso 1 1 calc R . . H5C H 0.8021 0.2162 0.3225 0.105 Uiso 1 1 calc R . . C6 C 0.3912(18) 0.2655(7) 0.3241(5) 0.040(3) Uani 1 1 d . . . H6 H 0.4774 0.2870 0.3029 0.048 Uiso 1 1 calc R . . C7 C 0.246(2) 0.2540(11) 0.2895(8) 0.077(6) Uani 1 1 d . . . H7A H 0.1595 0.2295 0.3081 0.115 Uiso 1 1 calc R . . H7B H 0.2723 0.2183 0.2616 0.115 Uiso 1 1 calc R . . H7C H 0.2096 0.3065 0.2759 0.115 Uiso 1 1 calc R . . C8 C 0.363(2) 0.3321(8) 0.3653(6) 0.061(5) Uani 1 1 d . . . H8A H 0.3416 0.3843 0.3486 0.091 Uiso 1 1 calc R . . H8B H 0.4601 0.3366 0.3881 0.091 Uiso 1 1 calc R . . H8C H 0.2710 0.3168 0.3846 0.091 Uiso 1 1 calc R . . C9 C 0.3229(18) -0.0292(7) 0.4031(5) 0.039(3) Uani 1 1 d . . . C10 C 0.194(2) -0.0305(8) 0.4313(4) 0.044(4) Uani 1 1 d . . . C11 C 0.155(2) -0.0656(9) 0.3065(6) 0.052(4) Uani 1 1 d . . . H11 H 0.0987 -0.1005 0.3309 0.062 Uiso 1 1 calc R . . C12 C 0.0499(19) 0.0124(10) 0.2968(6) 0.054(4) Uani 1 1 d . . . H12A H 0.0826 0.0394 0.2660 0.081 Uiso 1 1 calc R . . H12B H 0.0662 0.0493 0.3256 0.081 Uiso 1 1 calc R . . H12C H -0.0643 -0.0026 0.2926 0.081 Uiso 1 1 calc R . . C13 C 0.163(3) -0.1155(13) 0.2540(8) 0.091(7) Uani 1 1 d . . . H13A H 0.0550 -0.1339 0.2427 0.136 Uiso 1 1 calc R . . H13B H 0.2346 -0.1624 0.2594 0.136 Uiso 1 1 calc R . . H13C H 0.2060 -0.0802 0.2282 0.136 Uiso 1 1 calc R . . C14 C 0.4836(18) -0.1357(7) 0.3386(6) 0.044(3) Uani 1 1 d . . . H14 H 0.4785 -0.1568 0.3032 0.053 Uiso 1 1 calc R . . C15 C 0.661(2) -0.1215(10) 0.3517(7) 0.064(5) Uani 1 1 d . . . H15A H 0.6775 -0.1092 0.3878 0.096 Uiso 1 1 calc R . . H15B H 0.6989 -0.0759 0.3319 0.096 Uiso 1 1 calc R . . H15C H 0.7224 -0.1702 0.3439 0.096 Uiso 1 1 calc R . . C16 C 0.409(2) -0.2039(9) 0.3701(6) 0.061(4) Uani 1 1 d . . . H16A H 0.4714 -0.2538 0.3669 0.092 Uiso 1 1 calc R . . H16B H 0.2970 -0.2133 0.3577 0.092 Uiso 1 1 calc R . . H16C H 0.4113 -0.1877 0.4057 0.092 Uiso 1 1 calc R . . C17 C 0.0248(19) 0.1961(8) 0.0534(5) 0.041(3) Uani 1 1 d . . . C18 C -0.106(2) 0.2255(8) 0.0302(6) 0.050(4) Uani 1 1 d . . . C19 C 0.298(2) 0.0900(11) 0.0763(7) 0.062(5) Uani 1 1 d . . . H19 H 0.3266 0.1315 0.1028 0.075 Uiso 1 1 calc R . . C20 C 0.360(2) 0.0055(12) 0.0966(8) 0.079(6) Uani 1 1 d . . . H20A H 0.3353 -0.0361 0.0710 0.119 Uiso 1 1 calc R . . H20B H 0.3071 -0.0080 0.1276 0.119 Uiso 1 1 calc R . . H20C H 0.4773 0.0079 0.1039 0.119 Uiso 1 1 calc R . . C21 C 0.382(2) 0.1145(14) 0.0273(8) 0.080(6) Uani 1 1 d . . . H21A H 0.4974 0.1221 0.0352 0.121 Uiso 1 1 calc R . . H21B H 0.3343 0.1651 0.0140 0.121 Uiso 1 1 calc R . . H21C H 0.3654 0.0716 0.0020 0.121 Uiso 1 1 calc R . . C22 C -0.011(2) 0.0706(8) 0.1298(5) 0.047(4) Uani 1 1 d . . . H22 H 0.0237 0.0156 0.1418 0.057 Uiso 1 1 calc R . . C23 C 0.052(3) 0.1328(12) 0.1700(6) 0.078(6) Uani 1 1 d . . . H23A H 0.0337 0.1878 0.1569 0.118 Uiso 1 1 calc R . . H23B H 0.1677 0.1243 0.1775 0.118 Uiso 1 1 calc R . . H23C H -0.0058 0.1257 0.2009 0.118 Uiso 1 1 calc R . . C24 C -0.197(2) 0.0705(9) 0.1229(6) 0.051(4) Uani 1 1 d . . . H24A H -0.2427 0.0506 0.1539 0.077 Uiso 1 1 calc R . . H24B H -0.2311 0.0352 0.0946 0.077 Uiso 1 1 calc R . . H24C H -0.2355 0.1257 0.1159 0.077 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 Pt1 0.0425(3) 0.0163(3) 0.0224(3) -0.00139(15) 0.00633(19) 0.00028(17) Pt2 0.0356(4) 0.0202(3) 0.0269(4) 0.0051(2) 0.0071(3) -0.0013(2) Cl1 0.096(3) 0.0269(15) 0.049(2) -0.0008(14) 0.042(2) -0.0088(17) Cl2 0.132(4) 0.0261(16) 0.0351(18) -0.0091(14) 0.030(2) -0.005(2) Cl3 0.076(2) 0.0279(15) 0.0337(17) 0.0090(13) 0.0154(16) -0.0030(15) P1 0.0341(16) 0.0202(14) 0.0273(15) -0.0063(11) 0.0077(12) -0.0020(12) P2 0.0447(18) 0.0157(13) 0.0317(16) 0.0003(12) 0.0023(14) -0.0012(13) P3 0.046(2) 0.0282(16) 0.0307(16) 0.0052(13) 0.0018(14) -0.0075(14) F1 0.041(4) 0.047(5) 0.066(5) 0.003(4) 0.017(4) -0.007(4) F2 0.105(8) 0.057(6) 0.064(6) -0.007(5) 0.058(6) -0.012(5) F3 0.114(9) 0.088(7) 0.025(4) -0.014(4) 0.006(5) -0.028(6) F4 0.072(6) 0.049(5) 0.025(4) 0.006(3) -0.001(4) 0.002(4) F5 0.104(8) 0.041(5) 0.061(6) 0.006(4) 0.040(5) 0.001(5) F6 0.050(5) 0.078(6) 0.046(5) 0.015(4) 0.011(4) -0.008(5) F7 0.126(9) 0.037(5) 0.075(7) 0.004(4) -0.028(6) -0.042(5) F8 0.120(9) 0.033(5) 0.076(7) 0.014(4) 0.028(6) 0.025(5) F9 0.053(5) 0.054(5) 0.078(6) 0.010(5) 0.009(5) 0.011(4) C1 0.047(8) 0.021(6) 0.034(7) 0.000(5) 0.015(6) 0.000(5) C2 0.086(11) 0.029(7) 0.032(7) -0.015(6) 0.024(8) -0.002(7) C3 0.052(8) 0.049(8) 0.023(6) -0.014(6) -0.001(6) -0.005(7) C4 0.049(9) 0.077(12) 0.049(9) -0.006(8) -0.018(7) 0.003(8) C5 0.059(11) 0.078(12) 0.073(12) 0.000(10) 0.008(9) -0.032(10) C6 0.055(8) 0.021(6) 0.048(8) 0.004(5) 0.031(7) 0.009(6) C7 0.078(13) 0.055(11) 0.098(15) 0.041(10) 0.014(11) 0.016(9) C8 0.108(14) 0.026(7) 0.053(9) 0.000(6) 0.045(9) 0.007(8) C9 0.060(9) 0.016(6) 0.039(7) 0.006(5) 0.002(7) 0.002(6) C10 0.087(12) 0.031(7) 0.014(6) 0.012(5) 0.011(6) 0.001(7) C11 0.059(10) 0.044(8) 0.050(9) -0.005(6) -0.007(7) -0.017(7) C12 0.049(9) 0.070(11) 0.043(8) 0.010(7) -0.012(7) -0.013(8) C13 0.084(14) 0.094(16) 0.091(15) -0.052(13) -0.023(11) -0.009(12) C14 0.063(9) 0.021(6) 0.049(8) 0.014(6) 0.010(7) 0.014(6) C15 0.080(12) 0.045(9) 0.066(11) 0.001(8) -0.012(9) 0.026(8) C16 0.096(13) 0.027(7) 0.061(10) 0.007(7) 0.011(9) 0.006(8) C17 0.068(10) 0.024(6) 0.030(7) 0.001(5) 0.002(6) -0.010(6) C18 0.075(11) 0.029(7) 0.048(8) -0.002(6) 0.016(8) 0.010(7) C19 0.057(10) 0.068(11) 0.060(10) 0.022(9) -0.016(8) -0.020(8) C20 0.037(9) 0.102(15) 0.095(14) 0.036(12) -0.031(9) -0.007(9) C21 0.052(10) 0.099(16) 0.090(14) 0.026(12) 0.002(10) -0.005(10) C22 0.081(11) 0.036(7) 0.024(6) -0.001(5) -0.001(7) -0.011(7) C23 0.123(17) 0.077(12) 0.036(9) -0.004(8) 0.003(9) -0.018(12) C24 0.066(10) 0.045(8) 0.045(8) -0.003(6) 0.017(7) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.243(3) . ? Pt1 P2 2.246(3) . ? Pt1 Cl2 2.326(3) . ? Pt1 Cl1 2.336(3) . ? Pt2 P3 2.290(3) . ? Pt2 P3 2.290(3) 3 ? Pt2 Cl3 2.292(3) 3 ? Pt2 Cl3 2.292(3) . ? P1 C1 1.813(12) . ? P1 C6 1.826(13) . ? P1 C3 1.871(14) . ? P2 C9 1.802(13) . ? P2 C11 1.832(15) . ? P2 C14 1.853(12) . ? P3 C19 1.805(16) . ? P3 C17 1.818(13) . ? P3 C22 1.865(14) . ? F1 C1 1.360(15) . ? F2 C2 1.311(16) . ? F3 C2 1.330(19) . ? F4 C9 1.373(16) . ? F5 C10 1.291(15) . ? F6 C10 1.332(18) . ? F7 C17 1.364(15) . ? F8 C18 1.317(16) . ? F9 C18 1.296(18) . ? C1 C2 1.289(19) . ? C3 C4 1.50(2) . ? C3 C5 1.52(2) . ? C6 C7 1.45(2) . ? C6 C8 1.543(18) . ? C9 C10 1.31(2) . ? C11 C12 1.54(2) . ? C11 C13 1.59(2) . ? C14 C15 1.48(2) . ? C14 C16 1.521(19) . ? C17 C18 1.28(2) . ? C19 C21 1.53(2) . ? C19 C20 1.54(2) . ? C22 C24 1.51(2) . ? C22 C23 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 103.68(11) . . ? P1 Pt1 Cl2 170.86(13) . . ? P2 Pt1 Cl2 85.14(12) . . ? P1 Pt1 Cl1 84.93(12) . . ? P2 Pt1 Cl1 171.18(12) . . ? Cl2 Pt1 Cl1 86.35(13) . . ? P3 Pt2 P3 180.00(17) . 3 ? P3 Pt2 Cl3 90.88(12) . 3 ? P3 Pt2 Cl3 89.12(12) 3 3 ? P3 Pt2 Cl3 89.12(12) . . ? P3 Pt2 Cl3 90.88(12) 3 . ? Cl3 Pt2 Cl3 180.00(15) 3 . ? C1 P1 C6 99.9(6) . . ? C1 P1 C3 103.2(6) . . ? C6 P1 C3 107.2(7) . . ? C1 P1 Pt1 117.5(4) . . ? C6 P1 Pt1 113.9(4) . . ? C3 P1 Pt1 113.5(4) . . ? C9 P2 C11 103.2(7) . . ? C9 P2 C14 99.1(6) . . ? C11 P2 C14 107.9(7) . . ? C9 P2 Pt1 118.1(4) . . ? C11 P2 Pt1 114.0(5) . . ? C14 P2 Pt1 113.0(4) . . ? C19 P3 C17 103.4(7) . . ? C19 P3 C22 107.4(8) . . ? C17 P3 C22 102.1(6) . . ? C19 P3 Pt2 110.3(7) . . ? C17 P3 Pt2 114.5(4) . . ? C22 P3 Pt2 117.8(4) . . ? C2 C1 F1 114.2(12) . . ? C2 C1 P1 134.5(12) . . ? F1 C1 P1 111.3(8) . . ? C1 C2 F2 124.8(16) . . ? C1 C2 F3 126.2(14) . . ? F2 C2 F3 108.8(12) . . ? C4 C3 C5 111.4(14) . . ? C4 C3 P1 110.2(9) . . ? C5 C3 P1 110.8(10) . . ? C7 C6 C8 111.8(14) . . ? C7 C6 P1 113.5(10) . . ? C8 C6 P1 112.0(10) . . ? C10 C9 F4 112.0(12) . . ? C10 C9 P2 136.2(12) . . ? F4 C9 P2 111.8(9) . . ? F5 C10 C9 125.8(15) . . ? F5 C10 F6 111.7(13) . . ? C9 C10 F6 122.5(11) . . ? C12 C11 C13 109.2(14) . . ? C12 C11 P2 111.1(9) . . ? C13 C11 P2 112.6(12) . . ? C15 C14 C16 113.8(13) . . ? C15 C14 P2 113.8(10) . . ? C16 C14 P2 113.3(10) . . ? C18 C17 F7 115.8(12) . . ? C18 C17 P3 128.1(11) . . ? F7 C17 P3 116.0(10) . . ? C17 C18 F9 124.9(13) . . ? C17 C18 F8 124.3(16) . . ? F9 C18 F8 110.7(14) . . ? C21 C19 C20 111.2(17) . . ? C21 C19 P3 111.5(11) . . ? C20 C19 P3 110.1(11) . . ? C24 C22 C23 112.2(14) . . ? C24 C22 P3 109.0(10) . . ? C23 C22 P3 112.2(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.402 _refine_diff_density_min -4.298 _refine_diff_density_rms 0.339 #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2003-07-02 at 11:26:07 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : a dreduc sortav struct data_PtBrPiPr2pfv _database_code_depnum_ccdc_archive 'CCDC 656539' _audit_creation_date 2003-07-02T11:26:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(diisopropylperfluorovinylphosphine)platinum(II) dibromide ; _chemical_formula_moiety 'C16 H28 Br2 F6 P2 Pt1' _chemical_formula_sum 'C16 H28 Br2 F6 P2 Pt' _chemical_formula_weight 751.23 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.7227(3) _cell_length_b 11.5780(4) _cell_length_c 10.7417(4) _cell_angle_alpha 90 _cell_angle_beta 93.241(2) _cell_angle_gamma 90 _cell_volume 1207.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12646 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_T_max 1.027 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.437585E-1 _diffrn_orient_matrix_ub_12 0.210939E-1 _diffrn_orient_matrix_ub_13 -0.833937E-1 _diffrn_orient_matrix_ub_21 -0.753129E-1 _diffrn_orient_matrix_ub_22 0.410604E-1 _diffrn_orient_matrix_ub_23 0.417082E-1 _diffrn_orient_matrix_ub_31 0.550057E-1 _diffrn_orient_matrix_ub_32 0.729999E-1 _diffrn_orient_matrix_ub_33 0.6376E-3 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_unetI/netI 0.026 _diffrn_reflns_number 10256 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 2117 _reflns_number_gt 1842 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+2.6881P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0046(7) _refine_ls_number_reflns 2117 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.287 _refine_diff_density_min -1.46 _refine_diff_density_rms 0.12 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' 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 C1 C 0.3168(6) 0.5736(5) 0.7616(6) 0.0548(14) Uani 1 1 d . . . C2 C 0.1980(7) 0.5939(6) 0.7068(8) 0.0710(19) Uani 1 1 d . . . C3 C 0.5253(7) 0.7371(5) 0.7095(6) 0.0586(15) Uani 1 1 d . . . H3 H 0.6185 0.7477 0.6811 0.07 Uiso 1 1 calc R . . C4 C 0.4277(9) 0.8079(6) 0.6225(9) 0.085(2) Uani 1 1 d . . . H4A H 0.4304 0.7788 0.539 0.128 Uiso 1 1 calc R . . H4B H 0.4559 0.8873 0.6245 0.128 Uiso 1 1 calc R . . H4C H 0.3355 0.8019 0.6496 0.128 Uiso 1 1 calc R . . C5 C 0.5265(9) 0.7799(7) 0.8445(7) 0.082(2) Uani 1 1 d . . . H5A H 0.5893 0.7339 0.8957 0.122 Uiso 1 1 calc R . . H5B H 0.4356 0.7735 0.8744 0.122 Uiso 1 1 calc R . . H5C H 0.5554 0.8592 0.848 0.122 Uiso 1 1 calc R . . C6 C 0.5939(8) 0.5071(5) 0.8156(7) 0.0617(18) Uani 1 1 d . . . H6 H 0.5724 0.5382 0.8971 0.074 Uiso 1 1 calc R . . C7 C 0.5636(11) 0.3774(7) 0.8156(8) 0.091(3) Uani 1 1 d . . . H7A H 0.468 0.3652 0.8295 0.137 Uiso 1 1 calc R . . H7B H 0.6194 0.3407 0.8807 0.137 Uiso 1 1 calc R . . H7C H 0.5843 0.3451 0.7365 0.137 Uiso 1 1 calc R . . C8 C 0.7464(9) 0.5336(11) 0.7952(10) 0.103(3) Uani 1 1 d . . . H8A H 0.7604 0.6157 0.7959 0.154 Uiso 1 1 calc R . . H8B H 0.7702 0.5028 0.7163 0.154 Uiso 1 1 calc R . . H8C H 0.8035 0.4989 0.8608 0.154 Uiso 1 1 calc R . . Br1 Br 0.67903(10) 0.63692(8) 0.45606(8) 0.0908(3) Uani 1 1 d . . . F1 F 0.3149(4) 0.5489(5) 0.8869(4) 0.0786(11) Uani 1 1 d . . . F2 F 0.0790(4) 0.5904(4) 0.7627(5) 0.0997(15) Uani 1 1 d . . . F3 F 0.1797(5) 0.6200(5) 0.5895(5) 0.1012(16) Uani 1 1 d . . . Pt1 Pt 0.5 0.5 0.5 0.04399(18) Uani 1 2 d S . . P1 P 0.48444(15) 0.58227(13) 0.69505(13) 0.0444(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(4) 0.059(4) 0.050(3) -0.001(3) 0.007(3) -0.002(3) C2 0.060(4) 0.068(4) 0.086(5) 0.006(4) 0.008(4) -0.005(3) C3 0.057(4) 0.055(4) 0.064(4) -0.013(3) 0.007(3) -0.006(3) C4 0.100(6) 0.051(4) 0.105(6) 0.003(4) -0.002(5) -0.001(4) C5 0.099(6) 0.071(5) 0.077(5) -0.034(4) 0.019(4) -0.016(4) C6 0.065(4) 0.077(5) 0.043(4) -0.006(3) -0.001(3) 0.010(3) C7 0.128(7) 0.069(5) 0.076(5) 0.008(4) -0.010(5) 0.024(5) C8 0.057(5) 0.151(8) 0.100(7) -0.009(7) -0.010(5) 0.029(5) Br1 0.1046(6) 0.0948(6) 0.0764(5) -0.0222(4) 0.0354(4) -0.0492(5) F1 0.079(3) 0.110(3) 0.049(2) 0.005(2) 0.0165(19) -0.001(3) F2 0.052(2) 0.099(3) 0.150(5) 0.009(3) 0.026(3) 0.001(2) F3 0.083(3) 0.134(4) 0.084(3) 0.036(3) -0.020(2) 0.008(3) Pt1 0.0497(2) 0.0475(2) 0.0353(2) -0.00359(11) 0.00721(13) -0.01103(12) P1 0.0457(8) 0.0502(8) 0.0375(7) -0.0049(6) 0.0047(6) -0.0022(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.288(9) . ? C1 F1 1.377(7) . ? C1 P1 1.820(6) . ? C2 F3 1.298(9) . ? C2 F2 1.334(8) . ? C3 C4 1.531(10) . ? C3 C5 1.532(9) . ? C3 P1 1.840(6) . ? C3 H3 0.98 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 C7 1.530(10) . ? C6 C8 1.541(13) . ? C6 P1 1.847(7) . ? C6 H6 0.98 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? Br1 Pt1 2.4205(7) . ? Pt1 P1 2.3142(13) 3_666 ? Pt1 P1 2.3142(13) . ? Pt1 Br1 2.4205(7) 3_666 ? 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 C2 C1 F1 115.1(6) . . ? C2 C1 P1 127.6(5) . . ? F1 C1 P1 117.2(4) . . ? C1 C2 F3 123.8(7) . . ? C1 C2 F2 124.5(7) . . ? F3 C2 F2 111.7(6) . . ? C4 C3 C5 112.1(6) . . ? C4 C3 P1 110.3(5) . . ? C5 C3 P1 112.7(5) . . ? C4 C3 H3 107.2 . . ? C5 C3 H3 107.2 . . ? P1 C3 H3 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C8 112.5(8) . . ? C7 C6 P1 111.0(5) . . ? C8 C6 P1 109.1(6) . . ? C7 C6 H6 108 . . ? C8 C6 H6 108 . . ? P1 C6 H6 108 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 Pt1 P1 180 3_666 . ? P1 Pt1 Br1 89.51(4) 3_666 3_666 ? P1 Pt1 Br1 90.49(4) . 3_666 ? P1 Pt1 Br1 90.49(4) 3_666 . ? P1 Pt1 Br1 89.51(4) . . ? Br1 Pt1 Br1 180.00(3) 3_666 . ? C1 P1 C3 102.4(3) . . ? C1 P1 C6 101.1(3) . . ? C3 P1 C6 106.7(3) . . ? C1 P1 Pt1 116.0(2) . . ? C3 P1 Pt1 116.9(2) . . ? C6 P1 Pt1 112.1(2) . . ? 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 F1 C1 C2 F3 179.2(7) . . . . ? P1 C1 C2 F3 3.1(11) . . . . ? F1 C1 C2 F2 -1.1(11) . . . . ? P1 C1 C2 F2 -177.2(5) . . . . ? C2 C1 P1 C3 83.6(7) . . . . ? F1 C1 P1 C3 -92.4(5) . . . . ? C2 C1 P1 C6 -166.4(7) . . . . ? F1 C1 P1 C6 17.6(6) . . . . ? C2 C1 P1 Pt1 -44.9(7) . . . . ? F1 C1 P1 Pt1 139.1(4) . . . . ? C4 C3 P1 C1 -68.0(6) . . . . ? C5 C3 P1 C1 58.0(6) . . . . ? C4 C3 P1 C6 -173.7(5) . . . . ? C5 C3 P1 C6 -47.7(6) . . . . ? C4 C3 P1 Pt1 60.0(6) . . . . ? C5 C3 P1 Pt1 -174.0(4) . . . . ? C7 C6 P1 C1 70.9(6) . . . . ? C8 C6 P1 C1 -164.6(6) . . . . ? C7 C6 P1 C3 177.6(6) . . . . ? C8 C6 P1 C3 -57.9(6) . . . . ? C7 C6 P1 Pt1 -53.3(7) . . . . ? C8 C6 P1 Pt1 71.2(6) . . . . ? P1 Pt1 P1 C1 16E1(10) 3_666 . . . ? Br1 Pt1 P1 C1 -28.9(2) 3_666 . . . ? Br1 Pt1 P1 C1 151.1(2) . . . . ? P1 Pt1 P1 C3 4E1(10) 3_666 . . . ? Br1 Pt1 P1 C3 -149.9(2) 3_666 . . . ? Br1 Pt1 P1 C3 30.1(2) . . . . ? P1 Pt1 P1 C6 -9E1(10) 3_666 . . . ? Br1 Pt1 P1 C6 86.5(3) 3_666 . . . ? Br1 Pt1 P1 C6 -93.5(3) . . . . ? #===END data_nb7b _database_code_depnum_ccdc_archive 'CCDC 656540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(diiospropylperfluorovinylphospine)platium(II) diioide ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 F6 I2 P2 Pt1' _chemical_formula_sum 'C16 H28 F6 I2 P2 Pt' _chemical_formula_weight 845.2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6437(16) _cell_length_b 12.9891(18) _cell_length_c 14.5673(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2392.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 8.626 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.2217 _exptl_absorpt_correction_T_max 0.2773 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2102 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2102 _reflns_number_gt 1713 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+8.0313P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2102 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.190 _refine_ls_shift/su_mean 0.002 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 Pt1 Pt 0.5000 0.0000 0.5000 0.02059(18) Uani 1 2 d S . . I1 I 0.64054(5) 0.05094(6) 0.62272(4) 0.0435(2) Uani 1 1 d . . . P1 P 0.42559(16) -0.11903(16) 0.59889(13) 0.0202(4) Uani 1 1 d . . . F1 F 0.4750(5) -0.1745(4) 0.7738(3) 0.0394(13) Uani 1 1 d . . . F2 F 0.4436(5) 0.0065(5) 0.8527(4) 0.0467(15) Uani 1 1 d . . . F3 F 0.3970(5) 0.0778(4) 0.7256(4) 0.0473(15) Uani 1 1 d . . . C1 C 0.4449(6) -0.0937(7) 0.7205(5) 0.0259(18) Uani 1 1 d . . . C2 C 0.4283(8) -0.0085(7) 0.7647(6) 0.036(2) Uani 1 1 d . . . C3 C 0.2823(6) -0.1437(7) 0.5938(6) 0.0287(19) Uani 1 1 d . . . H3 H 0.2657 -0.1692 0.5314 0.034 Uiso 1 1 calc R . . C4 C 0.2207(7) -0.0436(8) 0.6084(8) 0.044(2) Uani 1 1 d . . . H4A H 0.1472 -0.0541 0.5918 0.066 Uiso 1 1 calc R . . H4B H 0.2508 0.0102 0.5703 0.066 Uiso 1 1 calc R . . H4C H 0.2251 -0.0235 0.6724 0.066 Uiso 1 1 calc R . . C5 C 0.2488(7) -0.2267(9) 0.6622(8) 0.044(2) Uani 1 1 d . . . H5A H 0.2744 -0.2088 0.7229 0.066 Uiso 1 1 calc R . . H5B H 0.2783 -0.2924 0.6438 0.066 Uiso 1 1 calc R . . H5C H 0.1722 -0.2314 0.6634 0.066 Uiso 1 1 calc R . . C6 C 0.4880(8) -0.2465(7) 0.5876(6) 0.033(2) Uani 1 1 d . . . H6 H 0.462(5) -0.288(6) 0.628(5) 0.000(16) Uiso 1 1 d . . . C7 C 0.6071(8) -0.2389(8) 0.5925(7) 0.046(3) Uani 1 1 d . . . H7A H 0.6373 -0.3075 0.5937 0.069 Uiso 1 1 calc R . . H7B H 0.6272 -0.2021 0.6477 0.069 Uiso 1 1 calc R . . H7C H 0.6332 -0.2021 0.5391 0.069 Uiso 1 1 calc R . . C8 C 0.4504(10) -0.3005(8) 0.5010(6) 0.044(3) Uani 1 1 d . . . H8A H 0.4705 -0.2602 0.4477 0.066 Uiso 1 1 calc R . . H8B H 0.3741 -0.3076 0.5028 0.066 Uiso 1 1 calc R . . H8C H 0.4827 -0.3681 0.4973 0.066 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 Pt1 0.0211(3) 0.0185(3) 0.0222(3) 0.00564(17) -0.00293(16) -0.00447(18) I1 0.0402(4) 0.0574(5) 0.0328(3) 0.0144(3) -0.0129(3) -0.0251(3) P1 0.0246(11) 0.0129(10) 0.0232(10) 0.0029(8) 0.0011(8) -0.0022(8) F1 0.065(4) 0.025(3) 0.029(3) 0.009(2) -0.003(2) 0.007(3) F2 0.055(4) 0.054(4) 0.031(3) -0.018(3) -0.004(3) 0.007(3) F3 0.066(4) 0.026(3) 0.050(3) -0.001(2) -0.008(3) 0.013(3) C1 0.026(4) 0.024(5) 0.027(4) 0.004(3) 0.003(3) -0.002(4) C2 0.041(5) 0.035(6) 0.031(5) -0.002(4) -0.003(4) 0.012(4) C3 0.022(4) 0.029(5) 0.035(4) -0.008(4) 0.001(3) -0.008(4) C4 0.023(5) 0.047(6) 0.062(7) 0.000(5) 0.001(4) 0.001(4) C5 0.034(5) 0.046(6) 0.051(6) 0.008(5) 0.008(5) -0.017(5) C6 0.055(6) 0.016(4) 0.027(4) 0.003(4) 0.011(4) 0.003(4) C7 0.056(6) 0.037(6) 0.046(5) 0.002(5) 0.008(5) 0.024(5) C8 0.069(8) 0.029(5) 0.034(5) -0.012(4) 0.002(5) 0.010(6) _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 Pt1 P1 2.3131(19) . ? Pt1 P1 2.3131(19) 5_656 ? Pt1 I1 2.6060(6) 5_656 ? Pt1 I1 2.6060(6) . ? P1 C1 1.818(8) . ? P1 C6 1.841(9) . ? P1 C3 1.842(8) . ? F1 C1 1.361(10) . ? F2 C2 1.312(11) . ? F3 C2 1.318(10) . ? C1 C2 1.297(13) . ? C3 C5 1.527(13) . ? C3 C4 1.531(13) . ? C6 C7 1.510(14) . ? C6 C8 1.519(13) . ? 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 P1 Pt1 P1 180.0 . 5_656 ? P1 Pt1 I1 88.86(5) . 5_656 ? P1 Pt1 I1 91.14(5) 5_656 5_656 ? P1 Pt1 I1 91.14(5) . . ? P1 Pt1 I1 88.86(5) 5_656 . ? I1 Pt1 I1 180.0 5_656 . ? C1 P1 C6 101.1(4) . . ? C1 P1 C3 101.7(4) . . ? C6 P1 C3 105.2(4) . . ? C1 P1 Pt1 115.5(3) . . ? C6 P1 Pt1 111.8(3) . . ? C3 P1 Pt1 119.5(3) . . ? C2 C1 F1 114.9(7) . . ? C2 C1 P1 128.0(7) . . ? F1 C1 P1 117.0(6) . . ? C1 C2 F2 126.0(9) . . ? C1 C2 F3 124.1(8) . . ? F2 C2 F3 109.9(8) . . ? C5 C3 C4 111.6(8) . . ? C5 C3 P1 111.7(6) . . ? C4 C3 P1 110.3(6) . . ? C7 C6 C8 112.4(8) . . ? C7 C6 P1 111.4(7) . . ? C8 C6 P1 110.8(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.139 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.258 #===END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2007-06-06 at 09:11:22 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : al dreduc sortav struct data_al _database_code_depnum_ccdc_archive 'CCDC 656541' _audit_creation_date 2007-06-06T09:11:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H44 Cl2 F6 P2 Pt1' _chemical_formula_sum 'C28 H44 Cl2 F6 P2 Pt' _chemical_formula_weight 822.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2760(2) _cell_length_b 11.6583(2) _cell_length_c 14.9767(3) _cell_angle_alpha 74.5780(10) _cell_angle_beta 70.0010(10) _cell_angle_gamma 63.9810(10) _cell_volume 1646.86(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7578 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.57 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.4934 _exptl_absorpt_correction_T_max 0.7403 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.425283E-1 _diffrn_orient_matrix_ub_12 -0.693133E-1 _diffrn_orient_matrix_ub_13 0.486639E-1 _diffrn_orient_matrix_ub_21 0.880612E-1 _diffrn_orient_matrix_ub_22 0.127141E-1 _diffrn_orient_matrix_ub_23 -0.30713E-1 _diffrn_orient_matrix_ub_31 -0.297042E-1 _diffrn_orient_matrix_ub_32 0.657233E-1 _diffrn_orient_matrix_ub_33 0.428289E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.085 _diffrn_reflns_av_unetI/netI 0.04 _diffrn_reflns_number 7530 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7530 _reflns_number_gt 5104 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with SORTAV R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+5.3673P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 7530 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.042 _refine_diff_density_min -3.02 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.017 0.01 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.703 8.391 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.9417(9) 0.3231(8) -0.0221(5) 0.0421(18) Uani 1 1 d . . . C2 C 1.0704(11) 0.3076(9) -0.0555(6) 0.057(2) Uani 1 1 d . . . C3 C 0.8644(8) 0.2146(7) 0.1748(5) 0.0377(16) Uani 1 1 d . . . H3 H 0.8194 0.1561 0.2194 0.045 Uiso 1 1 calc R . . C4 C 1.0064(8) 0.1675(9) 0.1911(6) 0.0468(19) Uani 1 1 d . . . H4A H 1.0553 0.2222 0.1474 0.056 Uiso 1 1 calc R . . H4B H 1.0602 0.0778 0.1769 0.056 Uiso 1 1 calc R . . C5 C 0.9924(11) 0.1733(10) 0.2961(7) 0.064(3) Uani 1 1 d . . . H5A H 0.948 0.1148 0.3397 0.077 Uiso 1 1 calc R . . H5B H 1.0841 0.1444 0.3061 0.077 Uiso 1 1 calc R . . C6 C 0.9086(11) 0.3084(9) 0.3190(7) 0.066(3) Uani 1 1 d . . . H6A H 0.9554 0.3659 0.2774 0.079 Uiso 1 1 calc R . . H6B H 0.9 0.311 0.3865 0.079 Uiso 1 1 calc R . . C7 C 0.7669(9) 0.3563(8) 0.3037(6) 0.051(2) Uani 1 1 d . . . H7A H 0.7147 0.4462 0.3178 0.061 Uiso 1 1 calc R . . H7B H 0.7177 0.3027 0.3489 0.061 Uiso 1 1 calc R . . C8 C 0.7743(8) 0.3510(7) 0.2003(5) 0.0431(17) Uani 1 1 d . . . H8A H 0.6812 0.3755 0.1942 0.052 Uiso 1 1 calc R . . H8B H 0.8127 0.413 0.1554 0.052 Uiso 1 1 calc R . . C9 C 0.7018(8) 0.2691(7) 0.0414(5) 0.0401(17) Uani 1 1 d . . . H9 H 0.6588 0.3595 0.0564 0.048 Uiso 1 1 calc R . . C10 C 0.6954(8) 0.2737(7) -0.0609(6) 0.0443(18) Uani 1 1 d . . . H10A H 0.7462 0.3253 -0.1073 0.053 Uiso 1 1 calc R . . H10B H 0.7393 0.1853 -0.0781 0.053 Uiso 1 1 calc R . . C11 C 0.5471(9) 0.3334(9) -0.0667(7) 0.060(2) Uani 1 1 d . . . H11A H 0.5063 0.4245 -0.0557 0.073 Uiso 1 1 calc R . . H11B H 0.5448 0.3318 -0.1319 0.073 Uiso 1 1 calc R . . C12 C 0.4634(9) 0.2620(10) 0.0063(7) 0.065(3) Uani 1 1 d . . . H12A H 0.4978 0.1736 -0.0091 0.078 Uiso 1 1 calc R . . H12B H 0.367 0.3064 0.0032 0.078 Uiso 1 1 calc R . . C13 C 0.4706(8) 0.2551(10) 0.1068(7) 0.055(2) Uani 1 1 d . . . H13A H 0.4191 0.2037 0.1525 0.066 Uiso 1 1 calc R . . H13B H 0.4271 0.3431 0.1247 0.066 Uiso 1 1 calc R . . C14 C 0.6196(7) 0.1934(8) 0.1145(6) 0.0458(19) Uani 1 1 d . . . H14A H 0.6212 0.1939 0.1801 0.055 Uiso 1 1 calc R . . H14B H 0.6612 0.1028 0.1021 0.055 Uiso 1 1 calc R . . C15 C 0.4012(10) 0.3333(9) 0.4640(7) 0.061(3) Uani 1 1 d . . . C16 C 0.4009(11) 0.3481(10) 0.3761(9) 0.084(4) Uani 1 1 d . . . C17 C 0.4539(8) 0.2067(8) 0.6453(6) 0.049(2) Uani 1 1 d . . . H17 H 0.4083 0.2967 0.6614 0.059 Uiso 1 1 calc R . . C18 C 0.6091(9) 0.1724(10) 0.6084(7) 0.065(3) Uani 1 1 d . . . H18A H 0.6548 0.0857 0.588 0.078 Uiso 1 1 calc R . . H18B H 0.6282 0.2352 0.5521 0.078 Uiso 1 1 calc R . . C19 C 0.6659(10) 0.1740(13) 0.6870(9) 0.087(4) Uani 1 1 d . . . H19A H 0.6266 0.2628 0.7028 0.105 Uiso 1 1 calc R . . H19B H 0.7663 0.1478 0.663 0.105 Uiso 1 1 calc R . . C20 C 0.6326(10) 0.0832(11) 0.7779(8) 0.074(3) Uani 1 1 d . . . H20A H 0.6781 -0.0068 0.7638 0.089 Uiso 1 1 calc R . . H20B H 0.6674 0.0891 0.8282 0.089 Uiso 1 1 calc R . . C21 C 0.4784(9) 0.1197(11) 0.8137(7) 0.059(2) Uani 1 1 d . . . H21A H 0.4337 0.208 0.8312 0.071 Uiso 1 1 calc R . . H21B H 0.4577 0.06 0.8719 0.071 Uiso 1 1 calc R . . C22 C 0.4211(8) 0.1138(9) 0.7368(6) 0.051(2) Uani 1 1 d . . . H22A H 0.321 0.1386 0.7612 0.061 Uiso 1 1 calc R . . H22B H 0.4623 0.0247 0.7213 0.061 Uiso 1 1 calc R . . C23 C 0.2006(8) 0.2431(8) 0.6070(5) 0.0416(17) Uani 1 1 d . . . H23 H 0.1886 0.1768 0.6636 0.05 Uiso 1 1 calc R . . C24 C 0.1274(8) 0.3738(8) 0.6438(6) 0.0465(19) Uani 1 1 d . . . H24A H 0.1369 0.4424 0.5897 0.056 Uiso 1 1 calc R . . H24B H 0.1707 0.3744 0.691 0.056 Uiso 1 1 calc R . . C25 C -0.0251(9) 0.4017(9) 0.6913(7) 0.062(3) Uani 1 1 d . . . H25A H -0.0351 0.3426 0.7521 0.075 Uiso 1 1 calc R . . H25B H -0.0722 0.4911 0.7067 0.075 Uiso 1 1 calc R . . C26 C -0.0916(10) 0.3842(11) 0.6251(8) 0.080(4) Uani 1 1 d . . . H26A H -0.1863 0.3925 0.6604 0.096 Uiso 1 1 calc R . . H26B H -0.0965 0.4539 0.5699 0.096 Uiso 1 1 calc R . . C27 C -0.0155(10) 0.2560(12) 0.5879(7) 0.066(3) Uani 1 1 d . . . H27A H -0.061 0.2516 0.5436 0.079 Uiso 1 1 calc R . . H27B H -0.0179 0.1859 0.6422 0.079 Uiso 1 1 calc R . . C28 C 0.1317(10) 0.2368(11) 0.5358(6) 0.060(2) Uani 1 1 d . . . H28A H 0.1352 0.305 0.4802 0.072 Uiso 1 1 calc R . . H28B H 0.1804 0.1522 0.512 0.072 Uiso 1 1 calc R . . Cl1 Cl 1.0563(2) 0.09154(18) -0.15681(12) 0.0437(4) Uani 1 1 d . . . Cl2 Cl 0.6592(2) 0.0725(2) 0.38530(15) 0.0560(6) Uani 1 1 d . . . F1 F 0.8486(6) 0.4438(5) -0.0411(4) 0.0643(15) Uani 1 1 d . . . F2 F 1.1721(5) 0.2015(6) -0.0430(4) 0.0675(14) Uani 1 1 d . . . F3 F 1.1122(7) 0.4006(6) -0.1089(4) 0.091(2) Uani 1 1 d . . . F4 F 0.4158(7) 0.4293(6) 0.4920(5) 0.090(2) Uani 1 1 d . . . F5 F 0.3809(7) 0.2739(7) 0.3386(4) 0.093(2) Uani 1 1 d . . . F6 F 0.4231(7) 0.4481(6) 0.3106(5) 0.124(3) Uani 1 1 d . . . P1 P 0.87833(17) 0.19974(15) 0.05165(11) 0.0246(3) Uani 1 1 d . . . P2 P 0.38376(19) 0.19728(18) 0.55407(13) 0.0342(4) Uani 1 1 d . . . Pt1 Pt 1 0 0 0.02908(13) Uani 1 2 d S . . Pt2 Pt 0.5 0 0.5 0.04041(14) Uani 1 2 d S . . 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 C1 0.052(5) 0.040(4) 0.035(4) -0.007(3) -0.004(3) -0.023(4) C2 0.081(7) 0.053(6) 0.049(5) -0.014(4) 0.002(5) -0.047(5) C3 0.047(4) 0.037(4) 0.031(4) -0.004(3) -0.008(3) -0.020(3) C4 0.040(4) 0.052(5) 0.049(5) -0.012(4) -0.018(4) -0.012(4) C5 0.070(6) 0.074(7) 0.048(5) -0.022(5) -0.030(5) -0.010(5) C6 0.087(7) 0.062(6) 0.060(6) -0.025(5) -0.034(5) -0.018(5) C7 0.069(6) 0.040(5) 0.045(4) -0.018(4) -0.007(4) -0.021(4) C8 0.046(4) 0.040(4) 0.044(4) -0.015(3) -0.008(3) -0.016(4) C9 0.041(4) 0.033(4) 0.045(4) -0.007(3) -0.011(3) -0.012(3) C10 0.047(4) 0.034(4) 0.053(5) -0.010(3) -0.021(4) -0.008(3) C11 0.059(5) 0.048(5) 0.075(6) -0.010(5) -0.036(5) -0.006(4) C12 0.048(5) 0.069(6) 0.086(7) -0.024(5) -0.033(5) -0.010(5) C13 0.033(4) 0.063(6) 0.070(6) -0.023(5) 0.000(4) -0.021(4) C14 0.032(4) 0.057(5) 0.053(5) -0.011(4) -0.013(3) -0.017(4) C15 0.061(6) 0.038(5) 0.051(5) -0.003(4) 0.023(4) -0.019(4) C16 0.069(7) 0.042(6) 0.083(8) 0.003(6) 0.016(6) -0.002(5) C17 0.039(4) 0.044(5) 0.065(6) -0.022(4) 0.004(4) -0.020(4) C18 0.046(5) 0.076(7) 0.084(7) -0.028(5) 0.007(5) -0.041(5) C19 0.039(5) 0.109(9) 0.133(11) -0.057(8) -0.003(6) -0.037(6) C20 0.050(6) 0.087(8) 0.099(8) -0.040(7) -0.028(6) -0.015(5) C21 0.044(5) 0.079(7) 0.063(6) -0.025(5) -0.014(4) -0.022(5) C22 0.036(4) 0.062(5) 0.063(5) -0.009(4) -0.017(4) -0.023(4) C23 0.041(4) 0.045(4) 0.034(4) 0.007(3) -0.005(3) -0.023(4) C24 0.038(4) 0.044(5) 0.050(5) -0.002(4) -0.012(4) -0.011(4) C25 0.042(5) 0.041(5) 0.082(7) 0.006(4) -0.007(5) -0.011(4) C26 0.042(5) 0.096(9) 0.076(7) 0.043(6) -0.027(5) -0.026(5) C27 0.062(6) 0.094(8) 0.057(6) 0.013(5) -0.031(5) -0.045(6) C28 0.062(6) 0.084(7) 0.045(5) 0.006(5) -0.020(4) -0.041(5) Cl1 0.0604(12) 0.0356(10) 0.0262(8) 0.0004(7) -0.0040(8) -0.0187(9) Cl2 0.0605(13) 0.0460(12) 0.0498(11) -0.0145(9) 0.0192(10) -0.0308(10) F1 0.091(4) 0.029(3) 0.067(3) 0.001(2) -0.023(3) -0.020(3) F2 0.056(3) 0.069(4) 0.077(4) -0.020(3) -0.003(3) -0.029(3) F3 0.125(5) 0.098(5) 0.078(4) -0.005(3) 0.001(4) -0.092(5) F4 0.082(4) 0.044(3) 0.116(5) -0.010(3) 0.020(4) -0.034(3) F5 0.107(5) 0.078(5) 0.064(4) -0.003(3) -0.008(4) -0.024(4) F6 0.077(4) 0.074(4) 0.117(6) 0.049(4) 0.021(4) -0.006(3) P1 0.0290(8) 0.0209(8) 0.0226(7) -0.0061(6) -0.0012(6) -0.0109(7) P2 0.0410(10) 0.0309(10) 0.0283(9) -0.0105(7) 0.0097(7) -0.0221(8) Pt1 0.0334(2) 0.0266(2) 0.02502(19) -0.00478(14) -0.00167(14) -0.01334(16) Pt2 0.0481(3) 0.0358(2) 0.0319(2) -0.01199(17) 0.01101(18) -0.0233(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.307(12) . ? C1 F1 1.363(10) . ? C1 P1 1.822(8) . ? C2 F2 1.288(11) . ? C2 F3 1.328(9) . ? C3 C8 1.532(10) . ? C3 C4 1.532(11) . ? C3 P1 1.845(7) . ? C3 H3 1 . ? C4 C5 1.542(11) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.500(13) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.521(13) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.539(10) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C14 1.532(11) . ? C9 C10 1.544(10) . ? C9 P1 1.836(8) . ? C9 H9 1 . ? C10 C11 1.528(11) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.509(14) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.514(13) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.542(11) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.283(17) . ? C15 F4 1.384(12) . ? C15 P2 1.824(9) . ? C16 F5 1.276(15) . ? C16 F6 1.365(11) . ? C17 C18 1.539(11) . ? C17 C22 1.551(12) . ? C17 P2 1.843(9) . ? C17 H17 1 . ? C18 C19 1.528(15) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.532(16) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.526(13) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.528(11) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.529(11) . ? C23 C28 1.549(12) . ? C23 P2 1.821(8) . ? C23 H23 1 . ? C24 C25 1.537(11) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.530(15) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.507(17) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.516(13) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? Cl1 Pt1 2.3020(16) . ? Cl2 Pt2 2.3101(18) . ? P1 Pt1 2.3092(16) . ? P2 Pt2 2.2986(18) . ? Pt1 Cl1 2.3020(16) 2_755 ? Pt1 P1 2.3092(16) 2_755 ? Pt2 P2 2.2986(18) 2_656 ? Pt2 Cl2 2.3101(18) 2_656 ? 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 C2 C1 F1 116.4(8) . . ? C2 C1 P1 125.4(7) . . ? F1 C1 P1 118.1(6) . . ? F2 C2 C1 125.1(8) . . ? F2 C2 F3 111.5(8) . . ? C1 C2 F3 123.4(10) . . ? C8 C3 C4 111.9(6) . . ? C8 C3 P1 112.7(5) . . ? C4 C3 P1 110.8(5) . . ? C8 C3 H3 107.1 . . ? C4 C3 H3 107.1 . . ? P1 C3 H3 107.1 . . ? C3 C4 C5 109.8(7) . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 110.1(8) . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 111.0(7) . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108 . . ? C6 C7 C8 111.6(7) . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108 . . ? C3 C8 C7 109.9(6) . . ? C3 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C3 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C14 C9 C10 110.2(6) . . ? C14 C9 P1 110.4(5) . . ? C10 C9 P1 112.1(5) . . ? C14 C9 H9 108 . . ? C10 C9 H9 108 . . ? P1 C9 H9 108 . . ? C11 C10 C9 110.4(7) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 111.6(7) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108 . . ? C11 C12 C13 111.3(8) . . ? C11 C12 H12A 109.4 . . ? C13 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C13 C12 H12B 109.4 . . ? H12A C12 H12B 108 . . ? C12 C13 C14 111.6(7) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108 . . ? C9 C14 C13 109.7(7) . . ? C9 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C9 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 F4 116.7(9) . . ? C16 C15 P2 125.5(9) . . ? F4 C15 P2 117.9(7) . . ? F5 C16 C15 125.6(10) . . ? F5 C16 F6 111.8(12) . . ? C15 C16 F6 122.6(13) . . ? C18 C17 C22 110.4(8) . . ? C18 C17 P2 111.5(6) . . ? C22 C17 P2 108.6(5) . . ? C18 C17 H17 108.8 . . ? C22 C17 H17 108.8 . . ? P2 C17 H17 108.8 . . ? C19 C18 C17 110.5(8) . . ? C19 C18 H18A 109.6 . . ? C17 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 C20 111.6(8) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108 . . ? C21 C20 C19 109.8(9) . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C20 C21 C22 111.0(8) . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C21 C22 C17 109.7(7) . . ? C21 C22 H22A 109.7 . . ? C17 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? C17 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C28 110.7(7) . . ? C24 C23 P2 114.8(5) . . ? C28 C23 P2 110.3(6) . . ? C24 C23 H23 106.9 . . ? C28 C23 H23 106.9 . . ? P2 C23 H23 106.9 . . ? C23 C24 C25 111.2(7) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108 . . ? C26 C25 C24 111.0(8) . . ? C26 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108 . . ? C27 C26 C25 113.1(8) . . ? C27 C26 H26A 109 . . ? C25 C26 H26A 109 . . ? C27 C26 H26B 109 . . ? C25 C26 H26B 109 . . ? H26A C26 H26B 107.8 . . ? C26 C27 C28 111.0(9) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108 . . ? C27 C28 C23 108.3(7) . . ? C27 C28 H28A 110 . . ? C23 C28 H28A 110 . . ? C27 C28 H28B 110 . . ? C23 C28 H28B 110 . . ? H28A C28 H28B 108.4 . . ? C1 P1 C9 101.6(4) . . ? C1 P1 C3 103.4(3) . . ? C9 P1 C3 105.4(3) . . ? C1 P1 Pt1 113.8(3) . . ? C9 P1 Pt1 112.1(3) . . ? C3 P1 Pt1 118.8(2) . . ? C23 P2 C15 105.2(4) . . ? C23 P2 C17 106.3(4) . . ? C15 P2 C17 101.8(5) . . ? C23 P2 Pt2 116.4(3) . . ? C15 P2 Pt2 114.8(3) . . ? C17 P2 Pt2 111.1(3) . . ? Cl1 Pt1 Cl1 180.00(14) 2_755 . ? Cl1 Pt1 P1 88.26(6) 2_755 . ? Cl1 Pt1 P1 91.74(6) . . ? Cl1 Pt1 P1 91.74(6) 2_755 2_755 ? Cl1 Pt1 P1 88.26(6) . 2_755 ? P1 Pt1 P1 180.00(15) . 2_755 ? P2 Pt2 P2 180.00(9) 2_656 . ? P2 Pt2 Cl2 89.18(7) 2_656 . ? P2 Pt2 Cl2 90.82(7) . . ? P2 Pt2 Cl2 90.82(7) 2_656 2_656 ? P2 Pt2 Cl2 89.18(7) . 2_656 ? Cl2 Pt2 Cl2 180.00(10) . 2_656 ? #===END # CIF produced by WinGX routine CIF_UPDATE # Created on 2000-04-14 at 17:15:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.1beta5 # Request file : C:\chem\wingx\files\archive.dat # CIF files read : nb10 psi_scan struct dreduc data_akbn10 _database_code_depnum_ccdc_archive 'CCDC 656542' _audit_creation_date 2000-04-14T17:15:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(phenylbisperfluorovinyl)phosphine)platinum(II)dibromide ; _chemical_formula_moiety 'C20 H10 Br2 F12 P2 Pt1' _chemical_formula_structural 'C20 H10 BR2 F12 P2 PT1' _chemical_formula_sum 'C20 H10 Br2 F12 P2 Pt' _chemical_formula_weight 895.13 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3236(3) _cell_length_b 13.3972(2) _cell_length_c 16.7449(2) _cell_angle_alpha 90 _cell_angle_beta 106.182(2) _cell_angle_gamma 90 _cell_volume 2439.63(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.259 _exptl_absorpt_factor_muR 0.926 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 5 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.3052 _exptl_absorpt_correction_T_max 0.3946 _exptl_absorpt_correction_T_ave 0.3425 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.58708E-1 _diffrn_orient_matrix_ub_12 0.57316E-1 _diffrn_orient_matrix_ub_13 -0.8088E-2 _diffrn_orient_matrix_ub_21 -0.15401E-1 _diffrn_orient_matrix_ub_22 -0.5682E-2 _diffrn_orient_matrix_ub_23 -0.61606E-1 _diffrn_orient_matrix_ub_31 -0.69078E-1 _diffrn_orient_matrix_ub_32 -0.47477E-1 _diffrn_orient_matrix_ub_33 -0.00246 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.026 _diffrn_standards_decay_corr_min 0.99 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -3 -10 7 -3 -8 1 6 -10 _diffrn_reflns_number 4507 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.063 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4276 _reflns_number_gt 3115 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.9090P] 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 fixed _refine_ls_extinction_method none _refine_ls_number_reflns 4276 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.947 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.171 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.26880(3) -0.08677(2) 0.327724(19) 0.01957(9) Uani 1 d . . . Br1 Br 0.42252(9) -0.19640(7) 0.41528(6) 0.0437(3) Uani 1 d . . . Br2 Br 0.11476(8) -0.18411(6) 0.37253(5) 0.0321(2) Uani 1 d . . . P1 P 0.41524(19) -0.00813(15) 0.28583(13) 0.0215(5) Uani 1 d . . . P2 P 0.10384(19) -0.00299(15) 0.25198(12) 0.0209(5) Uani 1 d . . . F1 F 0.5798(5) -0.1379(4) 0.2612(3) 0.0555(16) Uani 1 d . . . F2 F 0.7614(4) -0.1003(4) 0.3970(4) 0.0602(16) Uani 1 d . . . F3 F 0.6561(5) 0.0122(4) 0.4390(3) 0.0532(15) Uani 1 d . . . F4 F 0.5499(4) 0.1597(4) 0.3048(3) 0.0374(12) Uani 1 d . . . F5 F 0.4370(4) 0.2593(3) 0.3961(3) 0.0355(12) Uani 1 d . . . F6 F 0.3161(4) 0.1375(3) 0.4028(3) 0.0364(12) Uani 1 d . . . F7 F 0.2088(4) 0.1641(4) 0.2243(3) 0.0445(14) Uani 1 d . . . F8 F 0.0981(5) 0.1931(4) 0.0661(3) 0.0490(15) Uani 1 d . . . F9 F -0.0201(6) 0.0648(4) 0.0585(3) 0.0591(16) Uani 1 d . . . F10 F 0.0608(4) -0.1195(4) 0.1196(3) 0.0396(13) Uani 1 d . . . F11 F -0.1531(5) -0.1939(4) 0.1207(4) 0.0641(17) Uani 1 d . . . F12 F -0.1631(5) -0.1074(4) 0.2267(4) 0.0595(17) Uani 1 d . . . C1 C 0.5659(7) -0.0667(6) 0.3132(5) 0.028(2) Uani 1 d . . . C2 C 0.6579(8) -0.0511(7) 0.3798(6) 0.037(2) Uani 1 d . . . C3 C 0.3836(7) -0.0004(6) 0.1737(5) 0.0227(18) Uani 1 d . . . C4 C 0.3392(7) -0.0891(7) 0.1310(5) 0.0293(19) Uani 1 d . . . H4 H 0.3251 -0.1453 0.1595 0.035 Uiso 1 calc R . . C5 C 0.3168(8) -0.0907(7) 0.0455(5) 0.037(2) Uani 1 d . . . H5 H 0.2895 -0.1489 0.0159 0.045 Uiso 1 calc R . . C6 C 0.3352(8) -0.0066(8) 0.0050(6) 0.047(3) Uani 1 d . . . H6 H 0.3191 -0.0077 -0.0526 0.057 Uiso 1 calc R . . C7 C 0.3767(9) 0.0793(9) 0.0472(6) 0.053(3) Uani 1 d . . . H7 H 0.3883 0.1359 0.0181 0.064 Uiso 1 calc R . . C8 C 0.4016(8) 0.0831(7) 0.1324(5) 0.038(2) Uani 1 d . . . H8 H 0.4301 0.1416 0.1612 0.045 Uiso 1 calc R . . C9 C 0.4555(7) 0.1147(6) 0.3262(5) 0.0262(19) Uani 1 d . . . C10 C 0.4063(7) 0.1681(6) 0.3735(5) 0.0258(19) Uani 1 d . . . C11 C 0.1258(7) 0.0958(6) 0.1837(5) 0.0248(18) Uani 1 d . . . C12 C 0.0734(8) 0.1164(6) 0.1059(6) 0.035(2) Uani 1 d . . . C13 C 0.0059(7) -0.0858(6) 0.1778(5) 0.0275(18) Uani 1 d . . . C14 C -0.0990(9) -0.1262(7) 0.1768(6) 0.043(2) Uani 1 d . . . C15 C 0.0081(7) 0.0585(5) 0.3074(5) 0.0222(18) Uani 1 d . . . C16 C -0.0984(7) 0.1063(6) 0.2634(5) 0.031(2) Uani 1 d . . . H16 H -0.1221 0.1054 0.2055 0.037 Uiso 1 calc R . . C17 C -0.1685(8) 0.1549(7) 0.3058(6) 0.038(2) Uani 1 d . . . H17 H -0.2403 0.187 0.2764 0.046 Uiso 1 calc R . . C18 C -0.1338(8) 0.1567(6) 0.3917(6) 0.037(2) Uani 1 d . . . H18 H -0.1832 0.189 0.4197 0.045 Uiso 1 calc R . . C19 C -0.0274(7) 0.1115(6) 0.4359(5) 0.029(2) Uani 1 d . . . H19 H -0.0036 0.114 0.4937 0.035 Uiso 1 calc R . . C20 C 0.0445(7) 0.0619(5) 0.3941(5) 0.0249(19) Uani 1 d . . . H20 H 0.1169 0.0309 0.4238 0.03 Uiso 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 Pt1 0.02372(16) 0.01905(15) 0.01696(15) 0.00101(16) 0.00735(11) 0.00187(17) Br1 0.0395(5) 0.0438(6) 0.0460(6) 0.0231(5) 0.0089(5) 0.0130(5) Br2 0.0411(5) 0.0272(5) 0.0340(5) 0.0025(4) 0.0202(4) -0.0040(4) P1 0.0211(11) 0.0231(11) 0.0207(11) 0.0003(9) 0.0064(9) 0.0004(9) P2 0.0221(11) 0.0221(11) 0.0187(11) 0.0017(9) 0.0060(9) 0.0012(9) F1 0.047(3) 0.057(4) 0.060(4) -0.026(3) 0.010(3) 0.024(3) F2 0.029(3) 0.073(4) 0.068(4) -0.004(4) -0.004(3) 0.015(3) F3 0.052(4) 0.062(4) 0.035(3) -0.012(3) -0.005(3) 0.012(3) F4 0.035(3) 0.041(3) 0.039(3) -0.005(2) 0.016(2) -0.013(2) F5 0.052(3) 0.026(3) 0.029(3) -0.007(2) 0.011(2) -0.004(2) F6 0.039(3) 0.033(3) 0.044(3) -0.007(2) 0.025(3) -0.005(2) F7 0.039(3) 0.040(3) 0.045(3) 0.010(3) -0.004(3) -0.012(3) F8 0.066(4) 0.047(3) 0.041(3) 0.026(3) 0.027(3) 0.016(3) F9 0.078(4) 0.056(4) 0.030(3) 0.002(3) -0.007(3) -0.004(3) F10 0.043(3) 0.043(3) 0.033(3) -0.012(2) 0.011(2) 0.000(2) F11 0.056(4) 0.047(3) 0.077(4) -0.019(3) -0.003(3) -0.021(3) F12 0.039(3) 0.070(4) 0.076(4) -0.011(3) 0.026(3) -0.028(3) C1 0.021(4) 0.025(5) 0.036(5) -0.005(4) 0.004(4) 0.007(4) C2 0.021(5) 0.048(6) 0.039(6) 0.002(5) 0.004(4) 0.008(4) C3 0.018(4) 0.029(5) 0.023(4) 0.001(4) 0.009(4) 0.006(4) C4 0.039(5) 0.026(4) 0.024(4) 0.004(4) 0.011(4) 0.006(4) C5 0.044(5) 0.037(5) 0.032(5) 0.000(5) 0.013(4) 0.003(5) C6 0.042(6) 0.072(7) 0.028(5) -0.007(5) 0.010(5) -0.010(6) C7 0.055(6) 0.068(7) 0.034(6) 0.004(6) 0.007(5) -0.029(6) C8 0.052(6) 0.038(5) 0.023(4) -0.001(5) 0.012(4) -0.012(5) C9 0.034(5) 0.020(4) 0.026(4) -0.002(4) 0.011(4) -0.002(4) C10 0.031(5) 0.016(4) 0.028(5) -0.002(4) 0.006(4) -0.005(4) C11 0.022(4) 0.030(5) 0.025(4) 0.004(4) 0.010(4) 0.001(4) C12 0.042(6) 0.035(5) 0.030(5) 0.011(4) 0.017(5) 0.010(4) C13 0.038(5) 0.021(4) 0.022(4) -0.005(4) 0.007(4) 0.005(5) C14 0.042(6) 0.039(6) 0.043(6) -0.001(5) 0.006(5) -0.009(5) C15 0.025(4) 0.016(4) 0.029(5) 0.008(3) 0.015(4) -0.001(3) C16 0.031(5) 0.039(5) 0.027(5) 0.011(4) 0.012(4) 0.007(4) C17 0.031(5) 0.039(5) 0.050(6) 0.010(5) 0.021(5) -0.001(4) C18 0.034(5) 0.032(5) 0.052(7) 0.011(5) 0.025(5) 0.009(4) C19 0.038(5) 0.025(5) 0.031(5) -0.004(4) 0.022(4) -0.001(4) C20 0.028(4) 0.020(5) 0.027(4) 0.000(3) 0.007(4) -0.002(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pt1 P1 2.236(2) . ? Pt1 P2 2.244(2) . ? Pt1 Br1 2.4319(9) . ? Pt1 Br2 2.4567(9) . ? P1 C9 1.790(8) . ? P1 C3 1.813(8) . ? P1 C1 1.817(8) . ? P2 C13 1.798(8) . ? P2 C15 1.810(8) . ? P2 C11 1.812(8) . ? F1 C1 1.330(9) . ? F2 C2 1.306(9) . ? F3 C2 1.308(10) . ? F4 C9 1.359(8) . ? F5 C10 1.297(8) . ? F6 C10 1.316(9) . ? F7 C11 1.351(9) . ? F8 C12 1.297(9) . ? F9 C12 1.327(10) . ? F10 C13 1.370(8) . ? F11 C14 1.326(10) . ? F12 C14 1.276(11) . ? C1 C2 1.313(11) . ? C3 C8 1.360(11) . ? C3 C4 1.406(11) . ? C4 C5 1.382(11) . ? C5 C6 1.361(12) . ? C6 C7 1.364(13) . ? C7 C8 1.376(12) . ? C9 C10 1.301(10) . ? C11 C12 1.301(11) . ? C13 C14 1.301(12) . ? C15 C16 1.383(10) . ? C15 C20 1.395(11) . ? C16 C17 1.368(11) . ? C17 C18 1.382(12) . ? C18 C19 1.367(11) . ? C19 C20 1.382(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 99.22(7) . . ? P1 Pt1 Br1 90.28(6) . . ? P2 Pt1 Br1 170.36(6) . . ? P1 Pt1 Br2 176.04(6) . . ? P2 Pt1 Br2 83.58(6) . . ? Br1 Pt1 Br2 86.85(3) . . ? C9 P1 C3 107.2(4) . . ? C9 P1 C1 100.3(4) . . ? C3 P1 C1 100.8(4) . . ? C9 P1 Pt1 116.6(3) . . ? C3 P1 Pt1 113.7(3) . . ? C1 P1 Pt1 116.3(3) . . ? C13 P2 C15 107.0(4) . . ? C13 P2 C11 100.5(4) . . ? C15 P2 C11 101.4(3) . . ? C13 P2 Pt1 109.7(3) . . ? C15 P2 Pt1 117.4(3) . . ? C11 P2 Pt1 118.9(3) . . ? C2 C1 F1 117.4(7) . . ? C2 C1 P1 127.7(7) . . ? F1 C1 P1 114.7(6) . . ? F2 C2 F3 111.3(7) . . ? F2 C2 C1 123.9(9) . . ? F3 C2 C1 124.8(8) . . ? C8 C3 C4 121.3(7) . . ? C8 C3 P1 124.0(6) . . ? C4 C3 P1 114.7(6) . . ? C5 C4 C3 118.5(8) . . ? C6 C5 C4 119.6(9) . . ? C5 C6 C7 121.3(9) . . ? C6 C7 C8 120.6(10) . . ? C3 C8 C7 118.7(9) . . ? C10 C9 F4 114.7(7) . . ? C10 C9 P1 128.9(6) . . ? F4 C9 P1 116.4(5) . . ? F5 C10 C9 124.8(8) . . ? F5 C10 F6 110.9(7) . . ? C9 C10 F6 124.4(7) . . ? C12 C11 F7 114.8(8) . . ? C12 C11 P2 133.0(7) . . ? F7 C11 P2 112.0(5) . . ? F8 C12 C11 125.4(9) . . ? F8 C12 F9 110.8(7) . . ? C11 C12 F9 123.6(8) . . ? C14 C13 F10 116.5(8) . . ? C14 C13 P2 130.6(7) . . ? F10 C13 P2 112.3(6) . . ? F12 C14 C13 126.4(9) . . ? F12 C14 F11 111.3(8) . . ? C13 C14 F11 122.3(9) . . ? C16 C15 C20 120.0(7) . . ? C16 C15 P2 119.7(6) . . ? C20 C15 P2 120.2(6) . . ? C17 C16 C15 119.3(8) . . ? C16 C17 C18 120.8(9) . . ? C19 C18 C17 120.5(8) . . ? C18 C19 C20 119.6(8) . . ? C19 C20 C15 119.8(8) . . ?