Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Greg Grant' _publ_contact_author_address ; Department of Chemistry The University of Tennessee at Chattanooga Dept. #2252 Chattanooga TN 37403-2598 UNITED STATES OF AMERICA ; _publ_contact_author_email GREG-GRANT@UTC.EDU _publ_section_title ; Cadmium-113 NMR studies on homoleptic complexes containing thioether ligands: the crystal structures of [Cd([12]aneS4)2](ClO4)2[, Cd([18]aneS4N2)](PF6)2, and [Cd([9]aneS3)2](PF6)2 ; loop_ _publ_author_name 'Greg Grant' 'Monte L. Helm' 'Lensey L. Hill' 'John P. Lee' 'D.G.Van Derveer' # Attachment 'CCDC295721.doc' data_grant41 _database_code_depnum_ccdc_archive 'CCDC 295721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(12S4)2)(ClO4)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 Cd Cl2 N2 O12 S8' _chemical_formula_weight 914.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.323(3) _cell_length_b 8.4702(13) _cell_length_c 21.334(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.441(2) _cell_angle_gamma 90.00 _cell_volume 3507.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6907 _exptl_absorpt_correction_T_max 0.8424 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17616 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6238 _reflns_number_gt 4758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+4.5051P] 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 6238 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1258 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.246629(17) 0.98496(4) 0.501717(17) 0.02071(14) Uani 1 1 d . . . S1 S 0.10279(6) 1.02728(14) 0.43313(7) 0.0237(3) Uani 1 1 d . . . C2 C 0.0820(2) 1.1586(6) 0.4888(3) 0.0259(11) Uani 1 1 d . . . H2A H 0.0347 1.1908 0.4661 0.041(11) Uiso 1 1 calc R . . H2B H 0.0878 1.1038 0.5302 0.041(11) Uiso 1 1 calc R . . C3 C 0.1288(2) 1.3050(6) 0.5069(3) 0.0259(11) Uani 1 1 d . . . H3A H 0.1141 1.3758 0.5333 0.029(10) Uiso 1 1 calc R . . H3B H 0.1225 1.3580 0.4650 0.029(10) Uiso 1 1 calc R . . S4 S 0.21980(6) 1.26611(14) 0.55489(6) 0.0238(3) Uani 1 1 d . . . C5 C 0.2241(3) 1.2036(6) 0.6377(3) 0.0270(11) Uani 1 1 d . . . H5A H 0.2181 1.2933 0.6621 0.044(12) Uiso 1 1 calc R . . H5B H 0.1876 1.1302 0.6310 0.044(12) Uiso 1 1 calc R . . C6 C 0.2928(3) 1.1263(6) 0.6798(3) 0.0290(12) Uani 1 1 d . . . H6A H 0.2957 1.1064 0.7252 0.029(10) Uiso 1 1 calc R . . H6B H 0.3288 1.1993 0.6841 0.029(10) Uiso 1 1 calc R . . S7 S 0.30815(6) 0.94267(14) 0.64472(6) 0.0242(3) Uani 1 1 d . . . C8 C 0.2515(3) 0.8092(6) 0.6625(3) 0.0301(12) Uani 1 1 d . . . H8A H 0.2730 0.7760 0.7098 0.035(10) Uiso 1 1 calc R . . H8B H 0.2095 0.8629 0.6557 0.035(10) Uiso 1 1 calc R . . C9 C 0.2351(3) 0.6648(6) 0.6157(3) 0.0274(12) Uani 1 1 d . . . H9A H 0.2079 0.5933 0.6292 0.031(10) Uiso 1 1 calc R . . H9B H 0.2776 0.6122 0.6235 0.031(10) Uiso 1 1 calc R . . S10 S 0.18973(6) 0.70300(14) 0.52442(6) 0.0241(3) Uani 1 1 d . . . C11 C 0.1045(2) 0.7648(6) 0.5153(3) 0.0281(12) Uani 1 1 d . . . H11A H 0.0791 0.6749 0.5194 0.039(11) Uiso 1 1 calc R . . H11B H 0.1088 0.8384 0.5511 0.039(11) Uiso 1 1 calc R . . C12 C 0.0669(2) 0.8415(6) 0.4456(3) 0.0291(12) Uani 1 1 d . . . H12A H 0.0200 0.8595 0.4386 0.029(10) Uiso 1 1 calc R . . H12B H 0.0662 0.7688 0.4108 0.029(10) Uiso 1 1 calc R . . S13 S 0.20518(6) 0.81627(16) 0.37416(7) 0.0287(3) Uani 1 1 d . . . C14 C 0.2700(3) 0.6645(6) 0.3910(3) 0.0324(12) Uani 1 1 d . . . H14A H 0.2577 0.5759 0.4117 0.034(10) Uiso 1 1 calc R . . H14B H 0.2690 0.6297 0.3478 0.034(10) Uiso 1 1 calc R . . C15 C 0.3431(3) 0.7132(7) 0.4372(3) 0.0310(12) Uani 1 1 d . . . H15A H 0.3554 0.8055 0.4187 0.038(11) Uiso 1 1 calc R . . H15B H 0.3744 0.6300 0.4391 0.038(11) Uiso 1 1 calc R . . S16 S 0.35019(6) 0.75476(15) 0.52351(7) 0.0287(3) Uani 1 1 d . . . C17 C 0.4324(2) 0.8539(6) 0.5620(3) 0.0331(13) Uani 1 1 d . . . H17A H 0.4448 0.8644 0.6105 0.045(12) Uiso 1 1 calc R . . H17B H 0.4664 0.7884 0.5564 0.045(12) Uiso 1 1 calc R . . C18 C 0.4348(3) 1.0190(6) 0.5323(3) 0.0366(14) Uani 1 1 d . . . H18A H 0.4211 1.0113 0.4835 0.056(14) Uiso 1 1 calc R . . H18B H 0.4810 1.0591 0.5528 0.056(14) Uiso 1 1 calc R . . S19 S 0.37757(6) 1.15263(16) 0.54967(7) 0.0295(3) Uani 1 1 d . . . C20 C 0.3656(3) 1.3031(6) 0.4855(3) 0.0326(13) Uani 1 1 d . . . H20A H 0.3447 1.3937 0.4960 0.036(11) Uiso 1 1 calc R . . H20B H 0.4101 1.3348 0.4886 0.036(11) Uiso 1 1 calc R . . C21 C 0.3216(3) 1.2524(7) 0.4117(3) 0.0358(13) Uani 1 1 d . . . H21A H 0.3406 1.1587 0.4011 0.036(11) Uiso 1 1 calc R . . H21B H 0.3218 1.3341 0.3805 0.036(11) Uiso 1 1 calc R . . S22 S 0.23397(7) 1.21454(15) 0.40038(7) 0.0284(3) Uani 1 1 d . . . C23 C 0.1980(3) 1.1120(6) 0.3180(3) 0.0328(13) Uani 1 1 d . . . H23A H 0.1490 1.1047 0.3032 0.039(11) Uiso 1 1 calc R . . H23B H 0.2064 1.1747 0.2848 0.039(11) Uiso 1 1 calc R . . C24 C 0.2260(3) 0.9477(6) 0.3182(3) 0.0339(13) Uani 1 1 d . . . H24A H 0.2751 0.9529 0.3335 0.041(11) Uiso 1 1 calc R . . H24B H 0.2068 0.9064 0.2721 0.041(11) Uiso 1 1 calc R . . Cl1 Cl 0.05142(7) 1.00116(15) 0.15172(8) 0.0361(3) Uani 1 1 d . . . O1 O -0.0053(5) 0.9816(10) 0.0927(7) 0.115(5) Uani 0.67 1 d P . . O1' O 0.0047(11) 0.879(3) 0.1579(12) 0.104(6) Uiso 0.33 1 d P . . O2 O 0.0433(3) 1.1330(7) 0.1879(3) 0.100(2) Uani 1 1 d . . . O3 O 0.1148(8) 1.019(2) 0.1489(8) 0.042(4) Uiso 0.33 1 d P . . O3' O 0.1031(11) 1.107(3) 0.1491(12) 0.109(7) Uiso 0.33 1 d P . . O3" O 0.0210(9) 1.026(2) 0.0761(9) 0.051(5) Uiso 0.33 1 d P . . O4 O 0.1115(8) 0.916(3) 0.1626(8) 0.072(5) Uani 0.33 1 d P . . O4' O 0.0831(12) 0.861(3) 0.1794(13) 0.095(7) Uiso 0.33 1 d P . . O4" O 0.0587(7) 0.8849(15) 0.2058(7) 0.048(3) Uiso 0.33 1 d P . . Cl2 Cl 0.39719(8) 1.48535(15) 0.78712(8) 0.0346(3) Uani 1 1 d . . . O5 O 0.4065(3) 1.5387(8) 0.8525(3) 0.088(2) Uani 1 1 d . . . O6 O 0.3255(2) 1.4571(6) 0.7487(3) 0.0688(15) Uani 1 1 d . . . O7 O 0.4074(5) 1.6074(9) 0.7436(5) 0.070(2) Uani 0.67 1 d P . . O7' O 0.4499(12) 1.585(3) 0.7863(12) 0.106(7) Uiso 0.33 1 d P . . O8 O 0.4345(2) 1.3467(6) 0.7887(3) 0.0803(18) Uani 1 1 d . . . N1 N 0.4460(2) 0.9725(5) 0.8553(3) 0.0321(11) Uani 1 1 d . . . O9 O 0.3840(2) 0.9674(5) 0.8279(2) 0.0448(11) Uani 1 1 d . . . O10 O 0.4783(2) 0.9917(6) 0.9170(2) 0.0598(14) Uani 1 1 d . . . C25 C 0.4848(3) 0.9565(8) 0.8118(3) 0.0495(17) Uani 1 1 d . . . H25A H 0.4614 0.8837 0.7750 0.080(14) Uiso 1 1 calc R . . H25B H 0.5303 0.9178 0.8393 0.080(14) Uiso 1 1 calc R . . H25C H 0.4879 1.0576 0.7929 0.080(14) Uiso 1 1 calc R . . N2 N -0.1080(2) 1.0041(5) 0.2912(2) 0.0302(10) Uani 1 1 d . . . O11 O -0.1693(2) 0.9855(5) 0.2544(2) 0.0492(12) Uani 1 1 d . . . O12 O -0.0853(2) 1.0135(4) 0.3538(2) 0.0395(10) Uani 1 1 d . . . C26 C -0.0597(3) 1.0154(8) 0.2580(4) 0.0528(18) Uani 1 1 d . . . H26A H -0.0417 0.9125 0.2560 0.13(2) Uiso 1 1 calc R . . H26B H -0.0224 1.0848 0.2842 0.13(2) Uiso 1 1 calc R . . H26C H -0.0834 1.0562 0.2122 0.13(2) 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 Cd1 0.0230(2) 0.0192(2) 0.0212(2) 0.00006(14) 0.01034(17) 0.00096(14) S1 0.0252(6) 0.0218(6) 0.0261(7) 0.0001(5) 0.0128(5) 0.0011(5) C2 0.024(2) 0.025(3) 0.031(3) 0.002(2) 0.014(2) 0.004(2) C3 0.026(2) 0.020(2) 0.029(3) 0.003(2) 0.008(2) 0.007(2) S4 0.0282(6) 0.0191(6) 0.0248(7) 0.0013(5) 0.0118(5) 0.0002(5) C5 0.038(3) 0.022(3) 0.025(3) -0.001(2) 0.018(2) 0.002(2) C6 0.040(3) 0.021(3) 0.024(3) 0.000(2) 0.012(2) 0.003(2) S7 0.0293(6) 0.0199(6) 0.0238(7) 0.0004(5) 0.0114(5) 0.0024(5) C8 0.043(3) 0.028(3) 0.024(3) -0.001(2) 0.018(3) 0.000(2) C9 0.032(3) 0.021(3) 0.026(3) 0.001(2) 0.010(2) 0.004(2) S10 0.0279(6) 0.0190(6) 0.0265(7) 0.0003(5) 0.0122(6) 0.0017(5) C11 0.026(3) 0.021(3) 0.035(3) 0.004(2) 0.011(2) -0.003(2) C12 0.026(3) 0.025(3) 0.039(3) -0.001(2) 0.015(2) -0.003(2) S13 0.0295(7) 0.0313(7) 0.0271(7) -0.0010(6) 0.0136(6) 0.0035(6) C14 0.039(3) 0.031(3) 0.028(3) -0.005(2) 0.015(3) 0.005(2) C15 0.031(3) 0.039(3) 0.027(3) -0.004(2) 0.015(2) 0.009(2) S16 0.0301(7) 0.0307(7) 0.0275(7) -0.0026(6) 0.0141(6) 0.0045(6) C17 0.019(2) 0.044(3) 0.032(3) -0.005(3) 0.007(2) 0.006(2) C18 0.028(3) 0.046(3) 0.039(3) -0.001(3) 0.017(3) 0.001(3) S19 0.0281(6) 0.0322(7) 0.0301(7) -0.0008(6) 0.0138(6) -0.0009(6) C20 0.030(3) 0.034(3) 0.035(3) 0.002(2) 0.015(3) -0.008(2) C21 0.032(3) 0.044(3) 0.040(3) 0.004(3) 0.022(3) -0.005(3) S22 0.0311(7) 0.0309(7) 0.0254(7) 0.0022(6) 0.0138(6) -0.0023(6) C23 0.037(3) 0.040(3) 0.018(3) 0.006(2) 0.008(2) 0.000(3) C24 0.043(3) 0.037(3) 0.025(3) -0.004(2) 0.017(3) -0.005(3) Cl1 0.0332(7) 0.0322(7) 0.0415(8) 0.0044(6) 0.0142(7) 0.0042(6) O1 0.071(7) 0.048(5) 0.124(10) -0.033(6) -0.061(7) 0.010(5) O2 0.113(5) 0.095(4) 0.065(4) -0.024(3) 0.009(4) 0.033(4) O4 0.048(9) 0.110(15) 0.061(10) 0.004(11) 0.027(8) 0.055(11) Cl2 0.0401(8) 0.0321(7) 0.0373(8) -0.0084(6) 0.0218(7) -0.0052(6) O5 0.046(3) 0.171(6) 0.043(3) -0.046(4) 0.014(2) -0.007(3) O6 0.049(3) 0.082(3) 0.052(3) -0.027(3) -0.003(2) 0.020(3) O7 0.088(6) 0.053(5) 0.100(7) 0.026(5) 0.068(6) 0.009(4) O8 0.049(3) 0.063(3) 0.096(4) -0.009(3) -0.002(3) 0.025(2) N1 0.029(3) 0.039(3) 0.029(3) 0.005(2) 0.013(2) -0.002(2) O9 0.040(2) 0.062(3) 0.036(2) 0.012(2) 0.019(2) 0.008(2) O10 0.050(3) 0.093(4) 0.034(3) -0.007(2) 0.015(2) -0.014(2) C25 0.050(4) 0.066(4) 0.044(4) 0.002(3) 0.030(3) 0.007(3) N2 0.034(3) 0.030(2) 0.028(3) 0.0027(19) 0.014(2) 0.007(2) O11 0.035(2) 0.072(3) 0.040(3) -0.001(2) 0.015(2) 0.004(2) O12 0.044(2) 0.044(2) 0.031(2) -0.0003(18) 0.017(2) 0.0030(18) C26 0.042(4) 0.083(5) 0.047(4) 0.008(4) 0.032(3) 0.006(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 Cd1 S4 2.7968(13) . ? Cd1 S7 2.8010(14) . ? Cd1 S10 2.8101(13) . ? Cd1 S1 2.8219(13) . ? Cd1 S16 2.8363(13) . ? Cd1 S22 2.8364(14) . ? Cd1 S13 2.8702(14) . ? Cd1 S19 2.9147(14) . ? S1 C2 1.810(5) . ? S1 C12 1.817(5) . ? C2 C3 1.537(7) . ? C3 S4 1.810(5) . ? S4 C5 1.809(5) . ? C5 C6 1.513(7) . ? C6 S7 1.813(5) . ? S7 C8 1.806(5) . ? C8 C9 1.525(7) . ? C9 S10 1.810(5) . ? S10 C11 1.822(5) . ? C11 C12 1.514(7) . ? S13 C14 1.811(5) . ? S13 C24 1.817(5) . ? C14 C15 1.518(7) . ? C15 S16 1.818(5) . ? S16 C17 1.805(5) . ? C17 C18 1.545(8) . ? C18 S19 1.812(5) . ? S19 C20 1.810(5) . ? C20 C21 1.524(8) . ? C21 S22 1.810(5) . ? S22 C23 1.820(5) . ? C23 C24 1.514(8) . ? Cl1 O1 1.347(8) . ? Cl1 O4' 1.37(2) . ? Cl1 O3 1.385(15) . ? Cl1 O4 1.404(12) . ? Cl1 O2 1.409(6) . ? Cl1 O3' 1.44(2) . ? Cl1 O4" 1.476(14) . ? Cl1 O1' 1.48(2) . ? Cl1 O3" 1.484(18) . ? O1 O3" 0.864(19) . ? O1 O1' 1.57(2) . ? O1' O4" 1.18(2) . ? O1' O4' 1.55(3) . ? O2 O3' 1.80(2) . ? O3 O3' 0.79(2) . ? O3 O4 0.93(2) . ? O3 O4' 1.74(3) . ? O3' O4 1.64(3) . ? O4 O4' 0.94(2) . ? O4 O4" 1.75(2) . ? O4' O4" 0.93(2) . ? Cl2 O5 1.400(5) . ? Cl2 O7' 1.41(2) . ? Cl2 O8 1.411(5) . ? Cl2 O6 1.425(5) . ? Cl2 O7 1.465(7) . ? O7 O7' 1.00(2) . ? N1 O9 1.206(6) . ? N1 O10 1.218(6) . ? N1 C25 1.483(8) . ? N2 O12 1.220(6) . ? N2 O11 1.224(6) . ? N2 C26 1.476(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 S4 Cd1 S7 75.48(4) . . ? S4 Cd1 S10 118.58(4) . . ? S7 Cd1 S10 75.20(4) . . ? S4 Cd1 S1 75.01(4) . . ? S7 Cd1 S1 119.99(4) . . ? S10 Cd1 S1 75.12(4) . . ? S4 Cd1 S16 142.64(4) . . ? S7 Cd1 S16 75.61(4) . . ? S10 Cd1 S16 75.51(4) . . ? S1 Cd1 S16 141.06(4) . . ? S4 Cd1 S22 75.79(4) . . ? S7 Cd1 S22 140.52(4) . . ? S10 Cd1 S22 143.35(4) . . ? S1 Cd1 S22 77.14(4) . . ? S16 Cd1 S22 114.73(4) . . ? S4 Cd1 S13 140.72(4) . . ? S7 Cd1 S13 142.26(4) . . ? S10 Cd1 S13 75.81(4) . . ? S1 Cd1 S13 74.29(4) . . ? S16 Cd1 S13 74.13(4) . . ? S22 Cd1 S13 73.97(4) . . ? S4 Cd1 S19 76.69(4) . . ? S7 Cd1 S19 74.40(4) . . ? S10 Cd1 S19 140.61(4) . . ? S1 Cd1 S19 142.93(4) . . ? S16 Cd1 S19 73.12(4) . . ? S22 Cd1 S19 73.06(4) . . ? S13 Cd1 S19 116.73(4) . . ? C2 S1 C12 101.7(2) . . ? C2 S1 Cd1 104.25(16) . . ? C12 S1 Cd1 104.35(16) . . ? C3 C2 S1 110.6(3) . . ? C2 C3 S4 115.3(3) . . ? C5 S4 C3 102.4(2) . . ? C5 S4 Cd1 102.14(16) . . ? C3 S4 Cd1 106.07(17) . . ? C6 C5 S4 110.6(4) . . ? C5 C6 S7 114.9(4) . . ? C8 S7 C6 101.5(2) . . ? C8 S7 Cd1 104.88(18) . . ? C6 S7 Cd1 104.85(17) . . ? C9 C8 S7 110.9(4) . . ? C8 C9 S10 115.9(3) . . ? C9 S10 C11 103.4(2) . . ? C9 S10 Cd1 105.13(17) . . ? C11 S10 Cd1 102.71(16) . . ? C12 C11 S10 109.2(4) . . ? C11 C12 S1 115.5(4) . . ? C14 S13 C24 101.0(3) . . ? C14 S13 Cd1 104.78(18) . . ? C24 S13 Cd1 104.78(18) . . ? C15 C14 S13 115.5(4) . . ? C14 C15 S16 110.1(4) . . ? C17 S16 C15 102.0(3) . . ? C17 S16 Cd1 107.35(18) . . ? C15 S16 Cd1 103.56(17) . . ? C18 C17 S16 115.2(4) . . ? C17 C18 S19 110.0(4) . . ? C20 S19 C18 100.4(3) . . ? C20 S19 Cd1 105.26(17) . . ? C18 S19 Cd1 104.61(19) . . ? C21 C20 S19 114.7(4) . . ? C20 C21 S22 110.4(4) . . ? C21 S22 C23 102.3(3) . . ? C21 S22 Cd1 104.64(19) . . ? C23 S22 Cd1 106.12(18) . . ? C24 C23 S22 115.4(4) . . ? C23 C24 S13 111.2(4) . . ? O1 Cl1 O4' 112.9(10) . . ? O1 Cl1 O3 119.2(10) . . ? O4' Cl1 O3 78.2(11) . . ? O1 Cl1 O4 119.8(9) . . ? O4' Cl1 O4 39.7(10) . . ? O3 Cl1 O4 38.9(9) . . ? O1 Cl1 O2 110.1(5) . . ? O4' Cl1 O2 126.8(11) . . ? O3 Cl1 O2 106.4(7) . . ? O4 Cl1 O2 128.9(8) . . ? O1 Cl1 O3' 116.5(11) . . ? O4' Cl1 O3' 107.9(13) . . ? O3 Cl1 O3' 32.5(9) . . ? O4 Cl1 O3' 70.5(13) . . ? O2 Cl1 O3' 78.2(10) . . ? O1 Cl1 O4" 114.3(8) . . ? O4' Cl1 O4" 38.1(10) . . ? O3 Cl1 O4" 108.5(9) . . ? O4 Cl1 O4" 74.6(10) . . ? O2 Cl1 O4" 95.6(6) . . ? O3' Cl1 O4" 127.8(11) . . ? O1 Cl1 O1' 67.6(10) . . ? O4' Cl1 O1' 65.7(12) . . ? O3 Cl1 O1' 141.7(11) . . ? O4 Cl1 O1' 103.3(13) . . ? O2 Cl1 O1' 105.3(9) . . ? O3' Cl1 O1' 173.6(13) . . ? O4" Cl1 O1' 47.2(9) . . ? O1 Cl1 O3" 35.1(7) . . ? O4' Cl1 O3" 120.4(13) . . ? O3 Cl1 O3" 86.1(9) . . ? O4 Cl1 O3" 102.2(10) . . ? O2 Cl1 O3" 112.8(7) . . ? O3' Cl1 O3" 82.4(11) . . ? O4" Cl1 O3" 143.3(8) . . ? O1' Cl1 O3" 100.8(10) . . ? O3" O1 Cl1 81.2(14) . . ? O3" O1 O1' 136.7(19) . . ? Cl1 O1 O1' 60.1(9) . . ? O4" O1' Cl1 66.4(12) . . ? O4" O1' O4' 37.1(12) . . ? Cl1 O1' O4' 53.8(11) . . ? O4" O1' O1 118.1(17) . . ? Cl1 O1' O1 52.3(8) . . ? O4' O1' O1 93.0(15) . . ? Cl1 O2 O3' 51.7(8) . . ? O3' O3 O4 145(3) . . ? O3' O3 Cl1 78(2) . . ? O4 O3 Cl1 71.6(13) . . ? O3' O3 O4' 124(3) . . ? O4 O3 O4' 22.0(13) . . ? Cl1 O3 O4' 50.5(9) . . ? O3 O3' Cl1 70(2) . . ? O3 O3' O4 18.8(18) . . ? Cl1 O3' O4 53.7(9) . . ? O3 O3' O2 114(3) . . ? Cl1 O3' O2 50.1(7) . . ? O4 O3' O2 94.9(12) . . ? O1 O3" Cl1 63.7(14) . . ? O3 O4 O4' 136(3) . . ? O3 O4 Cl1 69.5(13) . . ? O4' O4 Cl1 68.2(17) . . ? O3 O4 O3' 16.0(15) . . ? O4' O4 O3' 121(2) . . ? Cl1 O4 O3' 55.8(10) . . ? O3 O4 O4" 117.1(16) . . ? O4' O4 O4" 21.4(17) . . ? Cl1 O4 O4" 54.5(7) . . ? O3' O4 O4" 101.2(11) . . ? O4" O4' O4 137(3) . . ? O4" O4' Cl1 77.1(19) . . ? O4 O4' Cl1 72.1(17) . . ? O4" O4' O1' 49.7(16) . . ? O4 O4' O1' 129(3) . . ? Cl1 O4' O1' 60.4(12) . . ? O4" O4' O3 118(2) . . ? O4 O4' O3 21.7(14) . . ? Cl1 O4' O3 51.3(9) . . ? O1' O4' O3 110.6(16) . . ? O4' O4" O1' 93(2) . . ? O4' O4" Cl1 64.8(17) . . ? O1' O4" Cl1 66.4(12) . . ? O4' O4" O4 21.6(17) . . ? O1' O4" O4 99.1(15) . . ? Cl1 O4" O4 50.8(7) . . ? O5 Cl2 O7' 91.9(10) . . ? O5 Cl2 O8 113.5(4) . . ? O7' Cl2 O8 93.2(10) . . ? O5 Cl2 O6 107.6(3) . . ? O7' Cl2 O6 139.8(10) . . ? O8 Cl2 O6 109.5(3) . . ? O5 Cl2 O7 114.0(5) . . ? O7' Cl2 O7 40.7(9) . . ? O8 Cl2 O7 111.8(4) . . ? O6 Cl2 O7 99.2(5) . . ? O7' O7 Cl2 66.7(15) . . ? O7 O7' Cl2 72.6(15) . . ? O9 N1 O10 123.0(5) . . ? O9 N1 C25 118.5(5) . . ? O10 N1 C25 118.5(5) . . ? O12 N2 O11 123.1(5) . . ? O12 N2 C26 118.8(5) . . ? O11 N2 C26 118.2(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.771 _refine_diff_density_min -1.752 _refine_diff_density_rms 0.139 # Attachment 'CCDC295722.doc' data_grant31 _database_code_depnum_ccdc_archive 'CCDC 295722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(9S3)2)(PF6)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H30 Cd F12 N2 O4 P2 S6' _chemical_formula_weight 885.10 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.180(3) _cell_length_b 10.089(3) _cell_length_c 10.129(4) _cell_angle_alpha 82.599(5) _cell_angle_beta 66.620(5) _cell_angle_gamma 89.569(5) _cell_volume 760.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 1.337 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7415 _exptl_absorpt_correction_T_max 0.7432 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6350 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.62 _reflns_number_total 3433 _reflns_number_gt 3191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.3041P] 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_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3433 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 Cd1 Cd 0.0000 0.0000 0.0000 0.02285(13) Uani 1 2 d S . . S1 S -0.12063(8) 0.12121(6) -0.18761(7) 0.02222(17) Uani 1 1 d . . . C2 C 0.0385(4) 0.0588(3) -0.3476(3) 0.0313(6) Uani 1 1 d . . . H2A H 0.0083 -0.0343 -0.3407 0.048(8) Uiso 1 1 calc R . . H2B H 0.0225 0.1042 -0.4307 0.048(8) Uiso 1 1 calc R . . C3 C 0.2360(4) 0.0722(3) -0.3774(3) 0.0293(6) Uani 1 1 d . . . H3A H 0.2702 0.1656 -0.3927 0.042(7) Uiso 1 1 calc R . . H3B H 0.3032 0.0367 -0.4658 0.042(7) Uiso 1 1 calc R . . S4 S 0.29713(9) -0.01121(7) -0.23485(8) 0.02634(18) Uani 1 1 d . . . C5 C 0.4238(4) 0.1176(3) -0.2012(3) 0.0269(5) Uani 1 1 d . . . H5A H 0.4476 0.0831 -0.1181 0.035(7) Uiso 1 1 calc R . . H5B H 0.5366 0.1325 -0.2827 0.035(7) Uiso 1 1 calc R . . C6 C 0.3421(3) 0.2524(3) -0.1751(3) 0.0247(5) Uani 1 1 d . . . H6A H 0.3211 0.2894 -0.2589 0.030(6) Uiso 1 1 calc R . . H6B H 0.4265 0.3117 -0.1653 0.030(6) Uiso 1 1 calc R . . S7 S 0.13399(9) 0.24664(6) -0.01565(7) 0.02305(17) Uani 1 1 d . . . C8 C -0.0170(4) 0.3376(3) -0.0820(3) 0.0268(5) Uani 1 1 d . . . H8A H -0.1320 0.3327 -0.0029 0.038(7) Uiso 1 1 calc R . . H8B H 0.0239 0.4300 -0.1071 0.038(7) Uiso 1 1 calc R . . C9 C -0.0418(4) 0.2937(3) -0.2114(3) 0.0261(5) Uani 1 1 d . . . H9A H 0.0701 0.3074 -0.2940 0.039(7) Uiso 1 1 calc R . . H9B H -0.1250 0.3507 -0.2332 0.039(7) Uiso 1 1 calc R . . P1 P -0.23341(10) -0.64903(7) 0.42532(8) 0.02589(18) Uani 1 1 d . . . F1 F -0.4286(3) -0.7136(3) 0.4738(3) 0.0544(6) Uani 1 1 d . . . F2 F -0.0393(3) -0.5848(3) 0.3757(3) 0.0608(7) Uani 1 1 d . . . F3 F -0.2836(5) -0.6255(4) 0.5880(3) 0.0844(10) Uani 1 1 d . . . F4 F -0.2943(16) -0.4964(9) 0.4217(10) 0.062(2) Uani 0.50 1 d P . . F5 F -0.1685(13) -0.7834(9) 0.4927(9) 0.063(2) Uani 0.50 1 d P . . F6 F -0.2147(9) -0.6463(10) 0.2628(7) 0.073(2) Uani 0.50 1 d P . . F4' F -0.2965(13) -0.5218(9) 0.3629(11) 0.072(3) Uani 0.50 1 d P . . F5' F -0.1721(17) -0.7931(9) 0.4311(13) 0.088(4) Uani 0.50 1 d P . . F6' F -0.1553(11) -0.7087(10) 0.2743(8) 0.077(2) Uani 0.50 1 d P . . N1 N 0.5864(5) -0.2576(4) -0.1766(4) 0.0492(9) Uani 1 1 d . . . O1 O 0.656(3) -0.1552(17) -0.2050(18) 0.112(7) Uani 0.50 1 d P . . O1' O 0.6868(15) -0.1583(13) -0.2665(11) 0.049(2) Uani 0.50 1 d P . . O2 O 0.4815(19) -0.2454(11) -0.0698(12) 0.051(2) Uani 0.50 1 d P . . O2' O 0.459(3) -0.2979(18) -0.0424(18) 0.109(7) Uani 0.50 1 d P . . C10 C 0.6243(6) -0.3745(5) -0.2516(5) 0.0549(10) Uani 1 1 d . . . H10A H 0.6106 -0.4532 -0.1830 0.120(15) Uiso 1 1 calc R . . H10B H 0.7443 -0.3658 -0.3237 0.120(15) Uiso 1 1 calc R . . H10C H 0.5430 -0.3820 -0.2976 0.120(15) 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 Cd1 0.02147(18) 0.02121(17) 0.02238(18) 0.00701(11) -0.00796(12) -0.00669(10) S1 0.0219(3) 0.0243(3) 0.0222(3) -0.0003(2) -0.0114(3) -0.0037(2) C2 0.0315(14) 0.0407(15) 0.0249(14) -0.0113(12) -0.0125(12) -0.0048(12) C3 0.0271(13) 0.0389(15) 0.0215(13) -0.0091(11) -0.0076(11) -0.0048(11) S4 0.0206(3) 0.0243(3) 0.0309(4) -0.0044(3) -0.0066(3) -0.0014(2) C5 0.0196(11) 0.0308(13) 0.0288(14) 0.0000(11) -0.0091(11) -0.0058(10) C6 0.0218(12) 0.0286(13) 0.0210(12) 0.0019(10) -0.0071(10) -0.0107(10) S7 0.0265(3) 0.0247(3) 0.0175(3) -0.0010(2) -0.0087(3) -0.0069(2) C8 0.0326(14) 0.0196(11) 0.0274(14) -0.0037(10) -0.0108(11) -0.0006(10) C9 0.0325(14) 0.0205(11) 0.0267(14) 0.0026(10) -0.0150(12) -0.0011(10) P1 0.0241(3) 0.0245(3) 0.0259(4) -0.0007(3) -0.0075(3) -0.0011(3) F1 0.0389(11) 0.0780(16) 0.0400(12) 0.0161(11) -0.0159(9) -0.0297(11) F2 0.0289(10) 0.0619(14) 0.0864(19) 0.0004(13) -0.0206(11) -0.0106(10) F3 0.102(2) 0.103(2) 0.0404(14) -0.0157(14) -0.0179(14) -0.0498(18) F4 0.060(4) 0.034(3) 0.076(6) 0.004(3) -0.014(4) 0.012(3) F5 0.056(4) 0.049(5) 0.067(4) 0.020(3) -0.016(3) 0.015(3) F6 0.049(4) 0.136(8) 0.023(2) -0.014(4) -0.002(3) -0.020(4) F4' 0.041(3) 0.043(4) 0.114(8) 0.047(5) -0.030(5) -0.009(3) F5' 0.090(5) 0.028(3) 0.169(12) -0.037(6) -0.070(8) 0.028(3) F6' 0.068(5) 0.117(7) 0.034(3) -0.032(4) -0.001(3) -0.008(4) N1 0.0433(17) 0.058(2) 0.069(2) -0.0274(18) -0.0404(19) 0.0169(16) O1 0.132(14) 0.056(6) 0.21(2) -0.043(12) -0.131(15) 0.021(8) O1' 0.038(3) 0.039(4) 0.065(5) 0.001(4) -0.017(3) -0.011(3) O2 0.052(5) 0.076(5) 0.024(4) -0.023(4) -0.010(4) 0.022(4) O2' 0.060(6) 0.22(2) 0.050(7) -0.027(10) -0.024(6) 0.020(12) C10 0.048(2) 0.060(2) 0.068(3) -0.028(2) -0.029(2) 0.0136(19) _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 Cd1 S1 2.6366(9) 2 ? Cd1 S1 2.6366(9) . ? Cd1 S4 2.6563(9) 2 ? Cd1 S4 2.6563(9) . ? Cd1 S7 2.6869(10) . ? Cd1 S7 2.6869(10) 2 ? S1 C9 1.813(3) . ? S1 C2 1.815(3) . ? C2 C3 1.525(4) . ? C3 S4 1.816(3) . ? S4 C5 1.815(3) . ? C5 C6 1.518(4) . ? C6 S7 1.818(3) . ? S7 C8 1.817(3) . ? C8 C9 1.523(4) . ? P1 F4' 1.534(8) . ? P1 F5' 1.536(8) . ? P1 F2 1.579(2) . ? P1 F3 1.582(3) . ? P1 F6 1.588(7) . ? P1 F1 1.589(2) . ? P1 F6' 1.602(7) . ? P1 F4 1.615(9) . ? P1 F5 1.620(8) . ? F4 F4' 0.684(12) . ? F5 F5' 0.656(12) . ? F6 F6' 0.816(10) . ? F6 F4' 1.683(13) . ? F5' F6' 1.657(14) . ? N1 O2 1.103(12) . ? N1 O1 1.130(18) . ? N1 O1' 1.300(12) . ? N1 O2' 1.357(17) . ? N1 C10 1.450(5) . ? O1 O1' 0.58(2) . ? O1 O2 1.70(2) . ? O2 O2' 0.56(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 S1 Cd1 S1 180.0 2 . ? S1 Cd1 S4 83.78(3) 2 2 ? S1 Cd1 S4 96.22(3) . 2 ? S1 Cd1 S4 96.22(3) 2 . ? S1 Cd1 S4 83.78(3) . . ? S4 Cd1 S4 180.00(4) 2 . ? S1 Cd1 S7 96.94(3) 2 . ? S1 Cd1 S7 83.06(3) . . ? S4 Cd1 S7 96.89(2) 2 . ? S4 Cd1 S7 83.11(2) . . ? S1 Cd1 S7 83.06(3) 2 2 ? S1 Cd1 S7 96.94(3) . 2 ? S4 Cd1 S7 83.11(2) 2 2 ? S4 Cd1 S7 96.89(2) . 2 ? S7 Cd1 S7 180.000(10) . 2 ? C9 S1 C2 102.89(14) . . ? C9 S1 Cd1 103.16(9) . . ? C2 S1 Cd1 97.13(10) . . ? C3 C2 S1 118.08(19) . . ? C2 C3 S4 115.0(2) . . ? C5 S4 C3 103.71(14) . . ? C5 S4 Cd1 96.31(10) . . ? C3 S4 Cd1 101.76(10) . . ? C6 C5 S4 117.94(19) . . ? C5 C6 S7 114.44(19) . . ? C8 S7 C6 104.21(13) . . ? C8 S7 Cd1 96.72(9) . . ? C6 S7 Cd1 101.46(9) . . ? C9 C8 S7 118.25(18) . . ? C8 C9 S1 115.41(19) . . ? F4' P1 F5' 156.5(5) . . ? F4' P1 F2 92.1(4) . . ? F5' P1 F2 93.6(5) . . ? F4' P1 F3 102.2(4) . . ? F5' P1 F3 100.4(4) . . ? F2 P1 F3 91.91(17) . . ? F4' P1 F6 65.2(5) . . ? F5' P1 F6 91.8(5) . . ? F2 P1 F6 92.7(3) . . ? F3 P1 F6 166.7(3) . . ? F4' P1 F1 87.7(4) . . ? F5' P1 F1 86.4(5) . . ? F2 P1 F1 179.50(15) . . ? F3 P1 F1 88.58(15) . . ? F6 P1 F1 86.8(3) . . ? F4' P1 F6' 94.1(5) . . ? F5' P1 F6' 63.7(5) . . ? F2 P1 F6' 85.3(3) . . ? F3 P1 F6' 163.5(4) . . ? F6 P1 F6' 29.7(3) . . ? F1 P1 F6' 94.3(3) . . ? F4' P1 F4 24.9(4) . . ? F5' P1 F4 178.3(5) . . ? F2 P1 F4 85.2(4) . . ? F3 P1 F4 78.5(4) . . ? F6 P1 F4 89.5(5) . . ? F1 P1 F4 94.8(4) . . ? F6' P1 F4 117.3(5) . . ? F4' P1 F5 179.4(5) . . ? F5' P1 F5 23.8(4) . . ? F2 P1 F5 88.3(4) . . ? F3 P1 F5 77.4(3) . . ? F6 P1 F5 115.2(5) . . ? F1 P1 F5 91.9(4) . . ? F6' P1 F5 86.3(4) . . ? F4 P1 F5 154.7(4) . . ? F4' F4 P1 71.0(13) . . ? F5' F5 P1 70.9(13) . . ? F6' F6 P1 76.1(9) . . ? F6' F6 F4' 130.3(11) . . ? P1 F6 F4' 55.9(4) . . ? F4 F4' P1 84.1(15) . . ? F4 F4' F6 140.6(17) . . ? P1 F4' F6 58.9(4) . . ? F5 F5' P1 85.3(14) . . ? F5 F5' F6' 140.5(17) . . ? P1 F5' F6' 60.1(5) . . ? F6 F6' P1 74.2(9) . . ? F6 F6' F5' 126.8(11) . . ? P1 F6' F5' 56.2(4) . . ? O2 N1 O1 99.1(11) . . ? O2 N1 O1' 123.1(8) . . ? O1 N1 O1' 26.3(10) . . ? O2 N1 O2' 23.6(11) . . ? O1 N1 O2' 121.2(12) . . ? O1' N1 O2' 146.4(10) . . ? O2 N1 C10 129.1(7) . . ? O1 N1 C10 131.8(10) . . ? O1' N1 C10 107.3(6) . . ? O2' N1 C10 106.3(9) . . ? O1' O1 N1 94(3) . . ? O1' O1 O2 130(3) . . ? N1 O1 O2 39.9(8) . . ? O1 O1' N1 60(3) . . ? O2' O2 N1 104(3) . . ? O2' O2 O1 142(3) . . ? N1 O2 O1 41.0(7) . . ? O2 O2' N1 52(2) . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 28.62 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 1.250 _refine_diff_density_min -1.532 _refine_diff_density_rms 0.143 # Attachment 'CCDC295723.doc' data_grant24 _database_code_depnum_ccdc_archive 'CCDC 295723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cd(18S4N2))(PF6)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12.50 H25.50 Cd F12 N2.50 O P2 S4' _chemical_formula_weight 757.43 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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 ? _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.635(4) _cell_length_b 10.0366(17) _cell_length_c 23.850(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.377(3) _cell_angle_gamma 90.00 _cell_volume 5045.5(15) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5716 _exptl_absorpt_correction_T_max 0.6696 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 13191 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.05 _reflns_number_total 4975 _reflns_number_gt 4458 _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^)+(0.0654P)^2^+18.1998P] 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 4975 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.142674(11) 0.03819(2) 0.125250(11) 0.02376(11) Uani 1 1 d . . . S1 S 0.10080(4) -0.12889(9) 0.19076(4) 0.0287(2) Uani 1 1 d . . . C2 C 0.01623(18) -0.0998(4) 0.16412(19) 0.0339(8) Uani 1 1 d . . . H2A H -0.0035 -0.1792 0.1715 0.037(8) Uiso 1 1 calc R . . H2B H 0.0086 -0.0305 0.1884 0.037(8) Uiso 1 1 calc R . . C3 C -0.01782(18) -0.0613(4) 0.09800(19) 0.0324(8) Uani 1 1 d . . . H3A H -0.0610 -0.0394 0.0921 0.040(9) Uiso 1 1 calc R . . H3B H -0.0188 -0.1381 0.0737 0.040(9) Uiso 1 1 calc R . . S4 S 0.01559(4) 0.07599(9) 0.07031(4) 0.0266(2) Uani 1 1 d . . . C5 C 0.01250(17) 0.2127(4) 0.11940(17) 0.0290(8) Uani 1 1 d . . . H5A H -0.0273 0.2586 0.1022 0.034(8) Uiso 1 1 calc R . . H5B H 0.0156 0.1782 0.1579 0.034(8) Uiso 1 1 calc R . . C6 C 0.06611(17) 0.3082(4) 0.12720(17) 0.0298(8) Uani 1 1 d . . . H6A H 0.0663 0.3328 0.0884 0.031(8) Uiso 1 1 calc R . . H6B H 0.0598 0.3876 0.1468 0.031(8) Uiso 1 1 calc R . . N7 N 0.12799(13) 0.2479(3) 0.16348(13) 0.0235(6) Uani 1 1 d . . . C8 C 0.18136(17) 0.3375(4) 0.16853(17) 0.0295(8) Uani 1 1 d . . . H8A H 0.1743 0.4225 0.1834 0.038(8) Uiso 1 1 calc R . . H8B H 0.1832 0.3509 0.1293 0.038(8) Uiso 1 1 calc R . . C9 C 0.24394(18) 0.2817(4) 0.21019(17) 0.0311(8) Uani 1 1 d . . . H9A H 0.2444 0.2846 0.2506 0.046(10) Uiso 1 1 calc R . . H9B H 0.2772 0.3392 0.2087 0.046(10) Uiso 1 1 calc R . . S10 S 0.26230(4) 0.11275(9) 0.19476(4) 0.0259(2) Uani 1 1 d . . . C11 C 0.29962(17) 0.1379(5) 0.14053(17) 0.0333(9) Uani 1 1 d . . . H11A H 0.3346 0.1978 0.1579 0.028(7) Uiso 1 1 calc R . . H11B H 0.3170 0.0541 0.1346 0.028(7) Uiso 1 1 calc R . . C12 C 0.25877(18) 0.1922(4) 0.07867(18) 0.0337(9) Uani 1 1 d . . . H12A H 0.2840 0.1927 0.0539 0.038(9) Uiso 1 1 calc R . . H12B H 0.2485 0.2832 0.0836 0.038(9) Uiso 1 1 calc R . . S13 S 0.18569(4) 0.10512(11) 0.03832(4) 0.0318(2) Uani 1 1 d . . . C14 C 0.2133(2) -0.0614(5) 0.02960(19) 0.0391(10) Uani 1 1 d . . . H14A H 0.2200 -0.0669 -0.0078 0.067(12) Uiso 1 1 calc R . . H14B H 0.2530 -0.0786 0.0616 0.067(12) Uiso 1 1 calc R . . C15 C 0.1652(2) -0.1649(5) 0.03063(17) 0.0373(9) Uani 1 1 d . . . H15A H 0.1243 -0.1419 0.0016 0.038(8) Uiso 1 1 calc R . . H15B H 0.1770 -0.2501 0.0197 0.038(8) Uiso 1 1 calc R . . N16 N 0.16148(15) -0.1734(3) 0.09113(14) 0.0305(7) Uani 1 1 d . . . C17 C 0.1120(2) -0.2678(4) 0.09239(19) 0.0367(9) Uani 1 1 d . . . H17A H 0.1205 -0.3536 0.0792 0.053(10) Uiso 1 1 calc R . . H17B H 0.0716 -0.2381 0.0647 0.053(10) Uiso 1 1 calc R . . C18 C 0.10877(19) -0.2811(4) 0.15368(18) 0.0332(8) Uani 1 1 d . . . H18A H 0.1465 -0.3259 0.1791 0.038(9) Uiso 1 1 calc R . . H18B H 0.0734 -0.3376 0.1504 0.038(9) Uiso 1 1 calc R . . P1 P 0.08353(4) -0.56051(10) -0.04994(4) 0.0265(2) Uani 1 1 d . . . F1 F 0.10511(11) -0.6875(2) -0.07779(11) 0.0387(5) Uani 1 1 d . . . F2 F 0.06048(13) -0.4343(3) -0.02387(13) 0.0495(7) Uani 1 1 d . . . F3 F 0.1246(2) -0.4676(3) -0.0737(2) 0.0915(14) Uani 1 1 d . . . F4 F 0.02515(18) -0.5462(4) -0.11110(17) 0.0910(15) Uani 1 1 d . . . F5 F 0.0430(2) -0.6570(4) -0.0253(2) 0.0892(14) Uani 1 1 d . . . F6 F 0.1410(2) -0.5791(4) 0.01189(16) 0.0942(14) Uani 1 1 d . . . P2 P 0.33546(5) 0.62981(10) 0.16349(4) 0.0311(2) Uani 1 1 d . . . F7 F 0.31795(17) 0.7808(3) 0.17318(15) 0.0627(8) Uani 1 1 d . . . F8 F 0.30316(17) 0.5838(3) 0.20989(14) 0.0611(8) Uani 1 1 d . . . F9 F 0.35102(16) 0.4797(3) 0.15465(15) 0.0597(8) Uani 1 1 d . . . F10 F 0.26957(15) 0.6157(4) 0.10981(15) 0.0773(11) Uani 1 1 d . . . F11 F 0.36823(17) 0.6753(4) 0.11916(16) 0.0723(10) Uani 1 1 d . . . F12 F 0.40053(15) 0.6448(4) 0.21914(15) 0.0755(10) Uani 1 1 d . . . C1 C 0.008(2) -0.4050(19) -0.245(2) 0.049(7) Uiso 0.25 1 d P . . C1' C -0.0294(10) -0.418(2) -0.2655(11) 0.042(6) Uiso 0.25 1 d P . . N1 N 0.0000 -0.5481(7) -0.2500 0.073(2) Uani 1 2 d S . . O1 O -0.0585(5) -0.5625(11) -0.2472(5) 0.091(3) Uiso 0.50 1 d P . . O1' O -0.0276(4) -0.6411(10) -0.2541(4) 0.073(2) Uiso 0.50 1 d P . . 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 Cd1 0.02180(15) 0.01944(16) 0.03143(17) -0.00271(9) 0.01134(12) -0.00026(9) S1 0.0307(4) 0.0252(5) 0.0264(4) 0.0015(3) 0.0060(4) -0.0032(4) C2 0.0310(19) 0.032(2) 0.043(2) 0.0040(17) 0.0185(17) -0.0019(17) C3 0.0221(17) 0.0268(19) 0.045(2) -0.0008(16) 0.0078(16) -0.0032(15) S4 0.0228(4) 0.0274(5) 0.0255(4) -0.0002(3) 0.0039(3) -0.0006(4) C5 0.0235(16) 0.0277(19) 0.036(2) 0.0008(15) 0.0107(15) 0.0042(15) C6 0.0265(17) 0.0252(18) 0.0333(19) 0.0037(15) 0.0057(15) 0.0054(15) N7 0.0213(13) 0.0196(14) 0.0284(15) -0.0016(12) 0.0075(12) -0.0001(11) C8 0.0314(18) 0.0187(17) 0.035(2) -0.0024(14) 0.0086(16) -0.0034(15) C9 0.0279(18) 0.031(2) 0.0309(19) -0.0031(15) 0.0067(15) -0.0063(15) S10 0.0218(4) 0.0295(5) 0.0247(4) 0.0042(3) 0.0066(3) 0.0004(3) C11 0.0204(16) 0.048(2) 0.033(2) 0.0040(17) 0.0120(15) -0.0001(16) C12 0.0273(18) 0.041(2) 0.036(2) 0.0111(17) 0.0154(16) 0.0007(16) S13 0.0260(4) 0.0435(6) 0.0247(4) 0.0083(4) 0.0076(4) 0.0058(4) C14 0.034(2) 0.054(3) 0.032(2) -0.0072(19) 0.0155(17) 0.0076(19) C15 0.039(2) 0.043(2) 0.0278(19) -0.0071(17) 0.0095(17) 0.0087(19) N16 0.0299(15) 0.0279(16) 0.0310(16) -0.0055(13) 0.0081(13) 0.0034(13) C17 0.036(2) 0.028(2) 0.040(2) -0.0097(17) 0.0059(17) -0.0020(17) C18 0.035(2) 0.0213(18) 0.039(2) 0.0008(16) 0.0084(17) -0.0004(15) P1 0.0223(4) 0.0263(5) 0.0295(5) -0.0012(4) 0.0080(4) -0.0001(4) F1 0.0381(12) 0.0306(12) 0.0533(15) -0.0031(11) 0.0234(11) 0.0020(10) F2 0.0534(16) 0.0450(15) 0.0507(16) -0.0167(12) 0.0195(13) 0.0054(13) F3 0.132(3) 0.0388(17) 0.159(4) -0.010(2) 0.119(3) -0.0198(19) F4 0.075(2) 0.089(3) 0.065(2) -0.0312(19) -0.0272(18) 0.046(2) F5 0.133(3) 0.060(2) 0.123(3) -0.034(2) 0.105(3) -0.040(2) F6 0.097(3) 0.073(2) 0.061(2) -0.0120(19) -0.033(2) 0.028(2) P2 0.0365(5) 0.0317(5) 0.0272(5) 0.0007(4) 0.0143(4) -0.0009(4) F7 0.097(2) 0.0314(14) 0.075(2) 0.0060(13) 0.0491(19) 0.0074(15) F8 0.100(2) 0.0453(16) 0.0640(19) -0.0007(14) 0.0610(19) -0.0095(16) F9 0.079(2) 0.0408(16) 0.073(2) -0.0115(14) 0.0432(18) 0.0030(14) F10 0.0502(17) 0.111(3) 0.0532(18) -0.0171(19) -0.0024(15) 0.0120(19) F11 0.089(2) 0.078(2) 0.075(2) 0.0148(18) 0.060(2) -0.0037(19) F12 0.0586(19) 0.085(3) 0.0581(19) -0.0116(18) -0.0076(15) -0.0023(18) N1 0.104(6) 0.054(4) 0.040(4) 0.000 0.001(4) 0.000 _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 Cd1 N7 2.365(3) . ? Cd1 N16 2.368(3) . ? Cd1 S13 2.6775(10) . ? Cd1 S1 2.6890(10) . ? Cd1 S10 2.7142(10) . ? Cd1 S4 2.7179(10) . ? S1 C18 1.807(4) . ? S1 C2 1.808(4) . ? C2 C3 1.531(6) . ? C3 S4 1.809(4) . ? S4 C5 1.822(4) . ? C5 C6 1.504(5) . ? C6 N7 1.481(4) . ? N7 C8 1.475(5) . ? C8 C9 1.511(5) . ? C9 S10 1.815(4) . ? S10 C11 1.802(4) . ? C11 C12 1.528(5) . ? C12 S13 1.807(4) . ? S13 C14 1.823(5) . ? C14 C15 1.511(6) . ? C15 N16 1.478(5) . ? N16 C17 1.475(5) . ? C17 C18 1.496(6) . ? P1 F3 1.562(3) . ? P1 F4 1.578(3) . ? P1 F2 1.581(3) . ? P1 F6 1.582(3) . ? P1 F5 1.588(3) . ? P1 F1 1.594(2) . ? P2 F11 1.565(3) . ? P2 F9 1.578(3) . ? P2 F10 1.578(3) . ? P2 F12 1.590(3) . ? P2 F8 1.601(3) . ? P2 F7 1.605(3) . ? C1 C1 0.33(10) 2_554 ? C1 C1' 0.49(5) 2_554 ? C1 C1' 0.81(6) . ? C1 N1 1.45(2) . ? C1' C1 0.49(5) 2_554 ? C1' C1' 1.26(4) 2_554 ? C1' N1 1.45(2) . ? C1' O1 1.71(3) . ? N1 O1' 1.108(10) . ? N1 O1' 1.108(10) 2_554 ? N1 O1 1.359(12) . ? N1 O1 1.359(12) 2_554 ? N1 C1 1.45(2) 2_554 ? N1 C1' 1.45(2) 2_554 ? O1 O1' 1.106(13) . ? O1' O1' 1.193(17) 2_554 ? 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 N7 Cd1 N16 177.35(10) . . ? N7 Cd1 S13 102.54(8) . . ? N16 Cd1 S13 78.30(9) . . ? N7 Cd1 S1 101.66(8) . . ? N16 Cd1 S1 77.63(9) . . ? S13 Cd1 S1 155.64(3) . . ? N7 Cd1 S10 76.60(7) . . ? N16 Cd1 S10 101.12(8) . . ? S13 Cd1 S10 80.82(3) . . ? S1 Cd1 S10 107.54(3) . . ? N7 Cd1 S4 77.81(7) . . ? N16 Cd1 S4 104.52(8) . . ? S13 Cd1 S4 102.20(3) . . ? S1 Cd1 S4 80.33(3) . . ? S10 Cd1 S4 154.27(3) . . ? C18 S1 C2 104.26(19) . . ? C18 S1 Cd1 97.12(14) . . ? C2 S1 Cd1 104.33(13) . . ? C3 C2 S1 118.3(3) . . ? C2 C3 S4 116.6(3) . . ? C3 S4 C5 102.71(19) . . ? C3 S4 Cd1 103.15(13) . . ? C5 S4 Cd1 94.42(12) . . ? C6 C5 S4 110.0(3) . . ? N7 C6 C5 111.1(3) . . ? C8 N7 C6 111.7(3) . . ? C8 N7 Cd1 110.4(2) . . ? C6 N7 Cd1 112.0(2) . . ? N7 C8 C9 111.8(3) . . ? C8 C9 S10 116.2(3) . . ? C11 S10 C9 102.5(2) . . ? C11 S10 Cd1 102.98(13) . . ? C9 S10 Cd1 97.48(12) . . ? C12 C11 S10 117.8(3) . . ? C11 C12 S13 117.1(3) . . ? C12 S13 C14 102.7(2) . . ? C12 S13 Cd1 103.27(13) . . ? C14 S13 Cd1 95.43(15) . . ? C15 C14 S13 110.5(3) . . ? N16 C15 C14 110.7(3) . . ? C17 N16 C15 111.8(3) . . ? C17 N16 Cd1 109.6(2) . . ? C15 N16 Cd1 111.4(2) . . ? N16 C17 C18 112.7(3) . . ? C17 C18 S1 116.9(3) . . ? F3 P1 F4 91.1(3) . . ? F3 P1 F2 89.44(17) . . ? F4 P1 F2 90.31(16) . . ? F3 P1 F6 90.7(3) . . ? F4 P1 F6 178.1(3) . . ? F2 P1 F6 90.28(18) . . ? F3 P1 F5 178.8(3) . . ? F4 P1 F5 89.7(3) . . ? F2 P1 F5 91.42(18) . . ? F6 P1 F5 88.4(3) . . ? F3 P1 F1 90.70(16) . . ? F4 P1 F1 88.18(16) . . ? F2 P1 F1 178.48(16) . . ? F6 P1 F1 91.23(18) . . ? F5 P1 F1 88.46(16) . . ? F11 P2 F9 90.24(19) . . ? F11 P2 F10 91.1(2) . . ? F9 P2 F10 89.8(2) . . ? F11 P2 F12 90.8(2) . . ? F9 P2 F12 91.0(2) . . ? F10 P2 F12 178.0(2) . . ? F11 P2 F8 178.9(2) . . ? F9 P2 F8 89.84(17) . . ? F10 P2 F8 90.0(2) . . ? F12 P2 F8 88.2(2) . . ? F11 P2 F7 91.41(19) . . ? F9 P2 F7 178.23(18) . . ? F10 P2 F7 89.5(2) . . ? F12 P2 F7 89.6(2) . . ? F8 P2 F7 88.51(16) . . ? C1 C1 C1' 162(10) 2_554 2_554 ? C1 C1 C1' 10(7) 2_554 . ? C1' C1 C1' 154(7) 2_554 . ? C1 C1 N1 83(2) 2_554 . ? C1' C1 N1 80(4) 2_554 . ? C1' C1 N1 74(3) . . ? C1 C1' C1 7(6) 2_554 . ? C1 C1' C1' 16(5) 2_554 2_554 ? C1 C1' C1' 10(2) . 2_554 ? C1 C1' N1 80(5) 2_554 . ? C1 C1' N1 74(2) . . ? C1' C1' N1 64.1(9) 2_554 . ? C1 C1' O1 121(6) 2_554 . ? C1 C1' O1 114(3) . . ? C1' C1' O1 105.8(15) 2_554 . ? N1 C1' O1 50.1(9) . . ? O1' N1 O1' 65.1(10) . 2_554 ? O1' N1 O1 52.1(6) . . ? O1' N1 O1 115.7(9) 2_554 . ? O1' N1 O1 115.7(9) . 2_554 ? O1' N1 O1 52.1(6) 2_554 2_554 ? O1 N1 O1 167.7(12) . 2_554 ? O1' N1 C1 153(2) . . ? O1' N1 C1 142(2) 2_554 . ? O1 N1 C1 101(2) . . ? O1 N1 C1 91(2) 2_554 . ? O1' N1 C1 142(2) . 2_554 ? O1' N1 C1 153(2) 2_554 2_554 ? O1 N1 C1 91(2) . 2_554 ? O1 N1 C1 101(2) 2_554 2_554 ? C1 N1 C1 13(4) . 2_554 ? O1' N1 C1' 166.6(11) . 2_554 ? O1' N1 C1' 122.9(10) 2_554 2_554 ? O1 N1 C1' 116.7(11) . 2_554 ? O1 N1 C1' 75.1(11) 2_554 2_554 ? C1 N1 C1' 19.4(19) . 2_554 ? C1 N1 C1' 32(3) 2_554 2_554 ? O1' N1 C1' 122.9(10) . . ? O1' N1 C1' 166.6(11) 2_554 . ? O1 N1 C1' 75.1(11) . . ? O1 N1 C1' 116.7(11) 2_554 . ? C1 N1 C1' 32(2) . . ? C1 N1 C1' 19.4(19) 2_554 . ? C1' N1 C1' 51.8(18) 2_554 . ? O1' O1 N1 52.2(7) . . ? O1' O1 C1' 103.9(12) . . ? N1 O1 C1' 54.8(9) . . ? O1 O1' N1 75.7(9) . . ? O1 O1' O1' 131.1(9) . 2_554 ? N1 O1' O1' 57.4(5) . 2_554 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.538 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.117