Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_contact_author_name 'Kim Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; _publ_contact_author_email dunbar@mail.chem.tamu.edu _publ_contact_author_fax (979)8457177 _publ_contact_author_phone (979)8621485 _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A series of complexes of the phosphorus-based TTF ligand o-P2 with the metal atoms FeII, CoII, NiII, PdII, PtII, and AgI ions. ; loop_ _publ_author_name _publ_author_address 'Calvin E. Uzelmeier' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Bradley W. Smucker' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Eric W. Reinheimer' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; "Amanda W. O'Neal" ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Kim R. Dunbar' ; Department of Chemistry Texas A&M University PO Box 30012 College Station Texas 77842-3012 USA ; 'Marc Fourmigue' ; Labortaire Chimie Ingeniere Moleculaire et Materiaux University of Angers 2 Bd Lavoisier Angers France ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and AgPF6produced the the complex [Ag(o-P2)2][PF6] where the silver metal center displays distorted tetrahedral geometry. The crystal structure is reported. ; data_h:\er044\work\p21n _database_code_depnum_ccdc_archive 'CCDC 615878' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H52 Ag P4 S8), 2(F6 P), 3(C2 H3 N)' _chemical_formula_sum 'C134 H113 Ag2 F12 N3 P10 S16' _chemical_formula_weight 3031.84 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' Ag Ag -0.8971 1.1015 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 25.098(13) _cell_length_b 21.265(11) _cell_length_c 26.793(14) _cell_angle_alpha 90.00 _cell_angle_beta 109.509(11) _cell_angle_gamma 90.00 _cell_volume 13479(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max .10 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6184 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.933 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 110(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 D8 on GADDS' _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 75004 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.1818 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 27550 _reflns_number_gt 14709 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.0600P)^2^+121.1530P] 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 0.00000(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 27550 _refine_ls_number_parameters 1519 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1886 _refine_ls_R_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.2303 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 1.028 _refine_ls_shift/su_mean 0.004 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 Ag1 Ag 0.70105(3) 0.30161(3) 0.15144(3) 0.01717(17) Uani 1 1 d . . . P3 P 0.60139(10) 0.26916(11) 0.12260(9) 0.0168(5) Uiso 1 1 d . . . S6 S 0.54292(10) 0.14214(10) 0.08504(9) 0.0182(5) Uani 1 1 d . . . P2 P 0.75183(10) 0.36250(11) 0.23325(9) 0.0171(5) Uiso 1 1 d . . . S8 S 0.57696(10) -0.06052(10) 0.08673(9) 0.0193(5) Uani 1 1 d . . . S5 S 0.64943(10) 0.06956(10) 0.12022(9) 0.0182(5) Uani 1 1 d . . . S2 S 0.82985(10) 0.47748(10) 0.25320(9) 0.0193(5) Uani 1 1 d . . . S1 S 0.82031(10) 0.49280(10) 0.14115(9) 0.0194(5) Uani 1 1 d . . . P4 P 0.72295(10) 0.18698(10) 0.16168(9) 0.0168(5) Uiso 1 1 d . . . P1 P 0.74051(10) 0.37835(10) 0.10464(9) 0.0162(5) Uiso 1 1 d . . . S7 S 0.47200(10) 0.01304(10) 0.05715(9) 0.0197(5) Uani 1 1 d . . . S4 S 0.94550(11) 0.55743(10) 0.28999(9) 0.0203(5) Uani 1 1 d . . . S3 S 0.93793(11) 0.57561(11) 0.17904(9) 0.0208(5) Uani 1 1 d . . . C10 C 0.6545(4) 0.1514(4) 0.1286(3) 0.017(2) Uani 1 1 d . . . C9 C 0.6056(4) 0.1842(4) 0.1136(3) 0.0142(19) Uani 1 1 d . . . C1 C 0.7871(4) 0.4233(4) 0.2081(4) 0.0152(19) Uani 1 1 d . . . C2 C 0.7828(4) 0.4307(3) 0.1565(3) 0.0112(18) Uani 1 1 d . . . C53 C 0.7700(4) 0.1530(4) 0.1301(4) 0.024(2) Uani 1 1 d . . . C47 C 0.5452(4) 0.2941(4) 0.0636(3) 0.020(2) Uani 1 1 d . . . C21 C 0.8570(5) 0.2867(5) 0.0575(5) 0.043(3) Uani 1 1 d . . . H21 H 0.8781 0.2501 0.0673 0.052 Uiso 1 1 calc R . . C11 C 0.5756(3) 0.0676(4) 0.0933(3) 0.0111(18) Uani 1 1 d . . . C14 C 0.5130(5) -0.1027(4) 0.0631(4) 0.024(2) Uani 1 1 d . . . C3 C 0.8589(4) 0.5098(4) 0.2077(3) 0.017(2) Uani 1 1 d . . . C59 C 0.7417(4) 0.1525(4) 0.2275(4) 0.023(2) Uani 1 1 d . . . C46 C 0.5696(4) 0.2298(4) 0.2097(4) 0.025(2) Uani 1 1 d . . . H46 H 0.5808 0.1893 0.2047 0.031 Uiso 1 1 calc R . . C29 C 0.8108(4) 0.3135(4) 0.2722(4) 0.026(2) Uani 1 1 d . . . C18 C 0.8003(4) 0.3987(5) 0.0321(4) 0.030(2) Uani 1 1 d . . . H18 H 0.7818 0.4372 0.0241 0.036 Uiso 1 1 calc R . . C24 C 0.6644(4) 0.4181(4) 0.0067(4) 0.024(2) Uani 1 1 d . . . H24 H 0.6826 0.3901 -0.0089 0.029 Uiso 1 1 calc R . . C6 C 1.0022(4) 0.5959(4) 0.2282(4) 0.020(2) Uani 1 1 d . . . C13 C 0.4649(4) -0.0695(4) 0.0498(3) 0.022(2) Uani 1 1 d . . . C12 C 0.5452(4) 0.0139(4) 0.0802(3) 0.016(2) Uani 1 1 d . . . C4 C 0.9075(4) 0.5428(4) 0.2230(3) 0.019(2) Uani 1 1 d . . . C5 C 1.0058(4) 0.5884(4) 0.2790(3) 0.017(2) Uani 1 1 d . . . C23 C 0.6860(4) 0.4283(4) 0.0615(4) 0.017(2) Uani 1 1 d . . . C8 C 1.0449(4) 0.6255(4) 0.2072(4) 0.028(2) Uani 1 1 d . . . H8A H 1.0794 0.6329 0.2359 0.043 Uiso 1 1 calc R . . H8B H 1.0305 0.6648 0.1904 0.043 Uiso 1 1 calc R . . H8C H 1.0522 0.5978 0.1819 0.043 Uiso 1 1 calc R . . C40 C 0.6710(5) 0.4231(5) 0.2626(4) 0.034(3) Uani 1 1 d . . . H40 H 0.6470 0.4111 0.2293 0.041 Uiso 1 1 calc R . . C17 C 0.7884(4) 0.3593(4) 0.0690(4) 0.022(2) Uani 1 1 d . . . C52 C 0.4888(5) 0.2959(4) 0.0607(4) 0.035(3) Uani 1 1 d . . . H52 H 0.4788 0.2828 0.0895 0.041 Uiso 1 1 calc R . . C41 C 0.5713(4) 0.2768(4) 0.1757(4) 0.024(2) Uani 1 1 d . . . C54 C 0.7521(5) 0.1344(5) 0.0787(4) 0.034(3) Uani 1 1 d . . . H54 H 0.7137 0.1357 0.0594 0.041 Uiso 1 1 calc R . . C26 C 0.5903(4) 0.4924(5) -0.0008(4) 0.030(2) Uani 1 1 d . . . H26 H 0.5585 0.5143 -0.0217 0.037 Uiso 1 1 calc R . . C39 C 0.6503(6) 0.4596(6) 0.2965(5) 0.049(3) Uani 1 1 d . . . H39 H 0.6129 0.4734 0.2849 0.058 Uiso 1 1 calc R . . C27 C 0.6108(5) 0.5028(5) 0.0523(4) 0.037(3) Uani 1 1 d . . . H27 H 0.5930 0.5316 0.0677 0.045 Uiso 1 1 calc R . . C30 C 0.8498(4) 0.2954(5) 0.2501(5) 0.037(3) Uani 1 1 d . . . H30 H 0.8493 0.3122 0.2179 0.045 Uiso 1 1 calc R . . C56 C 0.8472(6) 0.1125(5) 0.0835(6) 0.049(4) Uani 1 1 d . . . H56 H 0.8731 0.0986 0.0679 0.058 Uiso 1 1 calc R . . C45 C 0.5508(6) 0.2427(5) 0.2522(5) 0.045(3) Uani 1 1 d . . . H45 H 0.5498 0.2107 0.2756 0.054 Uiso 1 1 calc R . . C49 C 0.5166(6) 0.3347(5) -0.0247(4) 0.048(3) Uani 1 1 d . . . H49 H 0.5256 0.3474 -0.0541 0.058 Uiso 1 1 calc R . . C35 C 0.7275(4) 0.4055(4) 0.2796(4) 0.024(2) Uani 1 1 d . . . C48 C 0.5598(5) 0.3138(5) 0.0205(4) 0.043(3) Uani 1 1 d . . . H48 H 0.5972 0.3131 0.0216 0.051 Uiso 1 1 calc R . . C42 C 0.5546(5) 0.3373(5) 0.1843(4) 0.035(3) Uani 1 1 d . . . H42 H 0.5562 0.3699 0.1616 0.042 Uiso 1 1 calc R . . C25 C 0.6167(4) 0.4491(5) -0.0243(4) 0.033(3) Uani 1 1 d . . . H25 H 0.6021 0.4413 -0.0605 0.040 Uiso 1 1 calc R . . C7 C 1.0537(4) 0.6078(4) 0.3271(4) 0.025(2) Uani 1 1 d . . . H7A H 1.0842 0.6235 0.3166 0.037 Uiso 1 1 calc R . . H7B H 1.0665 0.5722 0.3500 0.037 Uiso 1 1 calc R . . H7C H 1.0412 0.6402 0.3455 0.037 Uiso 1 1 calc R . . C64 C 0.7163(5) 0.1779(5) 0.2612(4) 0.036(3) Uani 1 1 d . . . H64 H 0.6913 0.2113 0.2495 0.043 Uiso 1 1 calc R . . C44 C 0.5338(5) 0.3024(5) 0.2595(5) 0.043(3) Uani 1 1 d . . . H44 H 0.5207 0.3104 0.2875 0.052 Uiso 1 1 calc R . . C28 C 0.6579(5) 0.4705(4) 0.0832(4) 0.029(2) Uani 1 1 d . . . H28 H 0.6711 0.4772 0.1196 0.035 Uiso 1 1 calc R . . C19 C 0.8378(5) 0.3826(5) 0.0079(4) 0.032(3) Uani 1 1 d . . . H19 H 0.8444 0.4095 -0.0168 0.039 Uiso 1 1 calc R . . C15 C 0.4057(4) -0.0929(5) 0.0300(4) 0.031(3) Uani 1 1 d . . . H15A H 0.4055 -0.1364 0.0205 0.046 Uiso 1 1 calc R . . H15B H 0.3844 -0.0689 -0.0005 0.046 Uiso 1 1 calc R . . H15C H 0.3891 -0.0884 0.0573 0.046 Uiso 1 1 calc R . . C36 C 0.7621(5) 0.4230(5) 0.3304(4) 0.038(3) Uani 1 1 d . . . H36 H 0.8000 0.4113 0.3423 0.046 Uiso 1 1 calc R . . C60 C 0.7785(5) 0.1022(4) 0.2453(4) 0.031(3) Uani 1 1 d . . . H60 H 0.7941 0.0825 0.2224 0.038 Uiso 1 1 calc R . . C37 C 0.7406(6) 0.4574(6) 0.3632(5) 0.046(3) Uani 1 1 d . . . H37 H 0.7641 0.4687 0.3968 0.055 Uiso 1 1 calc R . . C43 C 0.5358(5) 0.3492(6) 0.2265(5) 0.045(3) Uani 1 1 d . . . H43 H 0.5245 0.3896 0.2319 0.054 Uiso 1 1 calc R . . C16 C 0.5187(5) -0.1726(4) 0.0607(4) 0.034(3) Uani 1 1 d . . . H16A H 0.5331 -0.1891 0.0961 0.051 Uiso 1 1 calc R . . H16B H 0.5442 -0.1826 0.0421 0.051 Uiso 1 1 calc R . . H16C H 0.4823 -0.1907 0.0426 0.051 Uiso 1 1 calc R . . C57 C 0.8655(6) 0.1314(5) 0.1343(6) 0.052(4) Uani 1 1 d . . . H57 H 0.9039 0.1301 0.1536 0.063 Uiso 1 1 calc R . . C50 C 0.4624(5) 0.3366(4) -0.0264(4) 0.039(3) Uani 1 1 d . . . H50 H 0.4347 0.3517 -0.0567 0.047 Uiso 1 1 calc R . . C51 C 0.4473(5) 0.3172(5) 0.0151(5) 0.041(3) Uani 1 1 d . . . H51 H 0.4096 0.3180 0.0132 0.049 Uiso 1 1 calc R . . C61 C 0.7920(5) 0.0814(5) 0.2973(5) 0.045(3) Uani 1 1 d . . . H61 H 0.8188 0.0499 0.3100 0.054 Uiso 1 1 calc R . . C38 C 0.6856(7) 0.4746(5) 0.3466(5) 0.052(4) Uani 1 1 d . . . H38 H 0.6715 0.4968 0.3694 0.062 Uiso 1 1 calc R . . C22 C 0.8162(5) 0.3020(5) 0.0806(5) 0.037(3) Uani 1 1 d . . . H22 H 0.8078 0.2739 0.1035 0.045 Uiso 1 1 calc R . . C58 C 0.8282(5) 0.1524(5) 0.1578(5) 0.036(3) Uani 1 1 d . . . H58 H 0.8416 0.1665 0.1926 0.043 Uiso 1 1 calc R . . C55 C 0.7900(6) 0.1135(5) 0.0539(5) 0.046(3) Uani 1 1 d . . . H55 H 0.7772 0.1006 0.0187 0.055 Uiso 1 1 calc R . . C20 C 0.8659(5) 0.3265(5) 0.0201(5) 0.038(3) Uani 1 1 d . . . H20 H 0.8911 0.3149 0.0031 0.046 Uiso 1 1 calc R . . C63 C 0.7269(6) 0.1553(6) 0.3122(4) 0.045(3) Uani 1 1 d . . . H63 H 0.7084 0.1721 0.3340 0.054 Uiso 1 1 calc R . . C34 C 0.8120(5) 0.2877(5) 0.3207(5) 0.045(3) Uani 1 1 d . . . H34 H 0.7852 0.2992 0.3360 0.054 Uiso 1 1 calc R . . C62 C 0.7656(6) 0.1074(6) 0.3297(5) 0.048(3) Uani 1 1 d . . . H62 H 0.7741 0.0925 0.3641 0.057 Uiso 1 1 calc R . . Ag2 Ag 0.19805(3) 0.21647(3) 0.13847(3) 0.0258(2) Uani 1 1 d . . . P7 P 0.23278(11) 0.12738(11) 0.09935(9) 0.0191(5) Uiso 1 1 d . . . S9 S 0.02571(11) 0.36118(10) 0.07582(10) 0.0237(6) Uani 1 1 d . . . P5 P 0.09589(11) 0.23964(11) 0.11385(9) 0.0179(5) Uiso 1 1 d . . . S16 S 0.43489(11) -0.04868(11) 0.29136(9) 0.0234(6) Uani 1 1 d . . . P8 P 0.24697(12) 0.16385(12) 0.22580(10) 0.0269(6) Uiso 1 1 d . . . S14 S 0.31676(12) 0.03979(12) 0.25539(10) 0.0277(6) Uani 1 1 d . . . P6 P 0.20888(12) 0.33293(12) 0.13687(11) 0.0285(6) Uiso 1 1 d . . . S12 S 0.04616(13) 0.56667(11) 0.07485(11) 0.0332(7) Uani 1 1 d . . . S11 S -0.05433(13) 0.48781(11) 0.05134(10) 0.0306(6) Uani 1 1 d . . . S13 S 0.30455(12) 0.01122(11) 0.14485(10) 0.0282(6) Uani 1 1 d . . . S15 S 0.41735(12) -0.06775(12) 0.17861(10) 0.0305(6) Uani 1 1 d . . . S10 S 0.12553(13) 0.44229(11) 0.09927(11) 0.0333(7) Uani 1 1 d . . . C67 C 0.0917(4) 0.3242(4) 0.1030(4) 0.020(2) Uani 1 1 d . . . C66 C 0.1372(4) 0.3617(4) 0.1134(4) 0.026(2) Uani 1 1 d . . . C69 C 0.0185(5) 0.4899(4) 0.0699(4) 0.031(3) Uani 1 1 d . . . C89 C -0.0141(4) 0.2062(4) 0.0498(4) 0.025(2) Uani 1 1 d . . . H89 H -0.0264 0.2218 0.0765 0.030 Uiso 1 1 calc R . . C79 C 0.4842(4) -0.0867(4) 0.2229(4) 0.026(2) Uani 1 1 d . . . C82 C 0.0651(4) 0.2257(4) 0.1653(3) 0.018(2) Uani 1 1 d . . . C71 C -0.0648(5) 0.5703(4) 0.0508(4) 0.035(3) Uani 1 1 d . . . C75 C 0.2714(4) 0.0801(4) 0.1559(4) 0.022(2) Uani 1 1 d . . . C94 C 0.2408(5) 0.3745(5) 0.0931(4) 0.032(3) Uani 1 1 d . . . C111 C 0.1616(4) 0.0715(4) 0.0054(4) 0.024(2) Uani 1 1 d . . . H111 H 0.1809 0.0950 -0.0123 0.028 Uiso 1 1 calc R . . C90 C -0.0528(4) 0.1814(4) 0.0052(4) 0.028(2) Uani 1 1 d . . . H90 H -0.0908 0.1796 0.0018 0.033 Uiso 1 1 calc R . . C88 C 0.0431(4) 0.2084(4) 0.0561(3) 0.018(2) Uani 1 1 d . . . C78 C 0.4927(4) -0.0787(4) 0.2750(4) 0.024(2) Uani 1 1 d . . . C106 C 0.1788(4) 0.0736(4) 0.0613(4) 0.020(2) Uani 1 1 d . . . C93 C 0.0598(4) 0.1857(4) 0.0136(4) 0.026(2) Uani 1 1 d . . . H93 H 0.0976 0.1879 0.0160 0.031 Uiso 1 1 calc R . . C91 C -0.0347(5) 0.1589(4) -0.0351(4) 0.028(2) Uani 1 1 d . . . H91 H -0.0611 0.1424 -0.0655 0.034 Uiso 1 1 calc R . . C68 C 0.0515(5) 0.4394(4) 0.0805(4) 0.025(2) Uani 1 1 d . . . C83 C 0.0595(4) 0.2722(4) 0.1996(4) 0.028(2) Uani 1 1 d . . . H83 H 0.0688 0.3136 0.1949 0.033 Uiso 1 1 calc R . . C95 C 0.2540(5) 0.4392(5) 0.0985(5) 0.042(3) Uani 1 1 d . . . H95 H 0.2489 0.4622 0.1260 0.050 Uiso 1 1 calc R . . C100 C 0.2375(4) 0.3668(4) 0.2039(4) 0.027(2) Uani 1 1 d . . . C110 C 0.1168(5) 0.0351(5) -0.0226(4) 0.036(3) Uani 1 1 d . . . H110 H 0.1064 0.0328 -0.0593 0.043 Uiso 1 1 calc R . . C118 C 0.3090(4) 0.2036(4) 0.2700(4) 0.027(2) Uani 1 1 d . . . C76 C 0.3451(4) 0.0013(4) 0.2115(4) 0.024(2) Uani 1 1 d . . . C101 C 0.2054(6) 0.3560(5) 0.2367(5) 0.044(3) Uani 1 1 d . . . H101 H 0.1694 0.3384 0.2236 0.053 Uiso 1 1 calc R . . C70 C -0.0192(5) 0.6054(4) 0.0613(4) 0.033(3) Uani 1 1 d . . . C92 C 0.0205(5) 0.1606(4) -0.0311(4) 0.025(2) Uani 1 1 d . . . H92 H 0.0319 0.1449 -0.0583 0.031 Uiso 1 1 calc R . . C87 C 0.0520(4) 0.1641(4) 0.1747(4) 0.026(2) Uani 1 1 d . . . H87 H 0.0566 0.1318 0.1530 0.031 Uiso 1 1 calc R . . C129 C 0.1855(6) 0.0797(5) 0.2639(4) 0.044(3) Uani 1 1 d . . . H129 H 0.1915 0.0512 0.2400 0.052 Uiso 1 1 calc R . . C81 C 0.5253(5) -0.1118(5) 0.1985(4) 0.036(3) Uani 1 1 d . . . H81A H 0.5625 -0.1122 0.2244 0.055 Uiso 1 1 calc R . . H81B H 0.5251 -0.0857 0.1692 0.055 Uiso 1 1 calc R . . H81C H 0.5147 -0.1539 0.1861 0.055 Uiso 1 1 calc R . . C77 C 0.3915(5) -0.0331(5) 0.2256(4) 0.028(2) Uani 1 1 d . . . C109 C 0.0870(5) 0.0016(4) 0.0035(4) 0.032(3) Uani 1 1 d . . . H109 H 0.0566 -0.0230 -0.0159 0.038 Uiso 1 1 calc R . . C105 C 0.2891(5) 0.3939(5) 0.2233(5) 0.037(3) Uani 1 1 d . . . H105 H 0.3099 0.4006 0.2009 0.045 Uiso 1 1 calc R . . C107 C 0.1476(4) 0.0408(4) 0.0869(4) 0.026(2) Uani 1 1 d . . . H107 H 0.1572 0.0431 0.1235 0.031 Uiso 1 1 calc R . . C108 C 0.1012(5) 0.0040(5) 0.0571(4) 0.033(3) Uani 1 1 d . . . H108 H 0.0805 -0.0187 0.0740 0.040 Uiso 1 1 calc R . . C80 C 0.5441(4) -0.0976(5) 0.3199(4) 0.029(2) Uani 1 1 d . . . H80A H 0.5361 -0.1351 0.3361 0.043 Uiso 1 1 calc R . . H80B H 0.5545 -0.0644 0.3456 0.043 Uiso 1 1 calc R . . H80C H 0.5747 -0.1056 0.3068 0.043 Uiso 1 1 calc R . . C84 C 0.0401(5) 0.2569(5) 0.2405(5) 0.040(3) Uani 1 1 d . . . H84 H 0.0365 0.2881 0.2634 0.048 Uiso 1 1 calc R . . C104 C 0.3113(5) 0.4115(5) 0.2751(5) 0.046(3) Uani 1 1 d . . . H104 H 0.3468 0.4302 0.2876 0.055 Uiso 1 1 calc R . . C128 C 0.1522(5) 0.0600(5) 0.2956(4) 0.038(3) Uani 1 1 d . . . H128 H 0.1381 0.0192 0.2933 0.046 Uiso 1 1 calc R . . C112 C 0.2836(4) 0.1350(5) 0.0653(4) 0.028(2) Uani 1 1 d . . . C113 C 0.2954(5) 0.0867(5) 0.0341(4) 0.035(3) Uani 1 1 d . . . H113 H 0.2748 0.0495 0.0278 0.043 Uiso 1 1 calc R . . C117 C 0.3161(5) 0.1878(5) 0.0748(5) 0.040(3) Uani 1 1 d . . . H117 H 0.3095 0.2197 0.0958 0.048 Uiso 1 1 calc R . . C86 C 0.0325(5) 0.1504(5) 0.2152(4) 0.033(3) Uani 1 1 d . . . H86 H 0.0234 0.1091 0.2202 0.039 Uiso 1 1 calc R . . C73 C -0.1247(6) 0.5902(5) 0.0379(4) 0.045(3) Uani 1 1 d . . . H73A H -0.1268 0.6353 0.0374 0.068 Uiso 1 1 calc R . . H73B H -0.1393 0.5742 0.0643 0.068 Uiso 1 1 calc R . . H73C H -0.1467 0.5740 0.0038 0.068 Uiso 1 1 calc R . . C98 C 0.2693(5) 0.3720(5) 0.0174(5) 0.041(3) Uani 1 1 d . . . H98 H 0.2749 0.3483 -0.0096 0.049 Uiso 1 1 calc R . . C96 C 0.2750(5) 0.4687(6) 0.0621(5) 0.047(3) Uani 1 1 d . . . H96 H 0.2836 0.5114 0.0651 0.056 Uiso 1 1 calc R . . C74 C 0.2768(4) 0.0930(4) 0.2067(4) 0.023(2) Uani 1 1 d . . . C122 C 0.3854(5) 0.2753(5) 0.2783(5) 0.045(3) Uani 1 1 d . . . H122 H 0.4053 0.3005 0.2622 0.054 Uiso 1 1 calc R . . C124 C 0.2080(5) 0.1369(5) 0.2673(4) 0.035(3) Uani 1 1 d . . . C99 C 0.2468(5) 0.3432(5) 0.0534(4) 0.039(3) Uani 1 1 d . . . H99 H 0.2361 0.3011 0.0487 0.047 Uiso 1 1 calc R . . C72 C -0.0160(6) 0.6757(5) 0.0620(4) 0.045(3) Uani 1 1 d . . . H72A H -0.0534 0.6929 0.0481 0.068 Uiso 1 1 calc R . . H72B H 0.0058 0.6893 0.0406 0.068 Uiso 1 1 calc R . . H72C H 0.0017 0.6900 0.0977 0.068 Uiso 1 1 calc R . . C126 C 0.1614(7) 0.1634(8) 0.3307(6) 0.073(5) Uani 1 1 d . . . H126 H 0.1530 0.1923 0.3529 0.088 Uiso 1 1 calc R . . C114 C 0.3379(6) 0.0959(6) 0.0134(5) 0.049(3) Uani 1 1 d . . . H114 H 0.3448 0.0647 -0.0080 0.059 Uiso 1 1 calc R . . C97 C 0.2827(5) 0.4336(6) 0.0217(5) 0.045(3) Uani 1 1 d . . . H97 H 0.2972 0.4524 -0.0024 0.054 Uiso 1 1 calc R . . C119 C 0.3274(5) 0.1969(6) 0.3244(4) 0.044(3) Uani 1 1 d . . . H119 H 0.3085 0.1705 0.3406 0.052 Uiso 1 1 calc R . . C103 C 0.2805(5) 0.4013(5) 0.3097(5) 0.047(3) Uani 1 1 d . . . H103 H 0.2949 0.4138 0.3450 0.057 Uiso 1 1 calc R . . C123 C 0.3392(5) 0.2427(5) 0.2485(4) 0.037(3) Uani 1 1 d . . . H123 H 0.3274 0.2471 0.2119 0.044 Uiso 1 1 calc R . . C85 C 0.0261(5) 0.1954(5) 0.2479(4) 0.033(3) Uani 1 1 d . . . H85 H 0.0124 0.1854 0.2752 0.040 Uiso 1 1 calc R . . C115 C 0.3697(6) 0.1471(8) 0.0227(5) 0.057(4) Uani 1 1 d . . . H115 H 0.3988 0.1512 0.0086 0.068 Uiso 1 1 calc R . . C102 C 0.2292(5) 0.3728(5) 0.2905(5) 0.046(3) Uani 1 1 d . . . H102 H 0.2094 0.3642 0.3135 0.055 Uiso 1 1 calc R . . C127 C 0.1424(6) 0.1014(7) 0.3280(5) 0.055(4) Uani 1 1 d . . . H127 H 0.1221 0.0891 0.3498 0.066 Uiso 1 1 calc R . . C116 C 0.3592(5) 0.1942(7) 0.0533(6) 0.059(4) Uani 1 1 d . . . H116 H 0.3810 0.2305 0.0597 0.071 Uiso 1 1 calc R . . C121 C 0.4021(5) 0.2703(5) 0.3315(5) 0.050(4) Uani 1 1 d . . . H121 H 0.4322 0.2943 0.3525 0.060 Uiso 1 1 calc R . . C120 C 0.3747(6) 0.2302(6) 0.3545(5) 0.059(4) Uani 1 1 d . . . H120 H 0.3880 0.2252 0.3911 0.071 Uiso 1 1 calc R . . C125 C 0.1931(6) 0.1808(6) 0.2995(5) 0.055(4) Uani 1 1 d . . . H125 H 0.2047 0.2224 0.2998 0.066 Uiso 1 1 calc R . . P10 P 0.01636(13) 0.95960(13) 0.16755(12) 0.0337(7) Uani 1 1 d . . . P9 P -0.03164(15) 1.05696(16) 0.33328(12) 0.0461(8) Uani 1 1 d . . . F12 F 0.0684(3) 1.0077(3) 0.1843(3) 0.056(2) Uani 1 1 d . . . F9 F -0.0345(3) 0.9116(3) 0.1492(3) 0.061(2) Uani 1 1 d . . . F1 F -0.0653(3) 1.0899(3) 0.2788(3) 0.061(2) Uani 1 1 d . . . F7 F -0.0094(4) 0.9994(5) 0.1160(4) 0.126(5) Uani 1 1 d . . . F10 F 0.0448(3) 0.9217(4) 0.2200(3) 0.067(2) Uani 1 1 d . . . F4 F 0.0012(4) 1.0238(4) 0.3886(3) 0.083(3) Uani 1 1 d . . . F5 F -0.0736(4) 1.0830(3) 0.3602(3) 0.073(2) Uani 1 1 d . . . F3 F -0.0685(4) 0.9952(3) 0.3175(3) 0.087(3) Uani 1 1 d . . . F8 F 0.0514(4) 0.9196(4) 0.1392(3) 0.078(3) Uani 1 1 d . . . F6 F 0.0058(4) 1.1174(4) 0.3513(3) 0.099(3) Uani 1 1 d . . . F11 F -0.0167(4) 0.9996(4) 0.1956(5) 0.116(4) Uani 1 1 d . . . C132 C 0.8450(7) 0.8203(7) 0.1259(6) 0.085(5) Uiso 1 1 d D . . H13A H 0.8806 0.8420 0.1371 0.128 Uiso 1 1 calc R . . H13B H 0.8427 0.7936 0.1540 0.128 Uiso 1 1 calc R . . H13C H 0.8147 0.8504 0.1174 0.128 Uiso 1 1 calc R . . N1 N 0.8341(7) 0.7584(8) 0.0395(6) 0.116(6) Uiso 1 1 d D . . C131 C 0.8403(8) 0.7827(8) 0.0798(6) 0.087(5) Uiso 1 1 d D . . C133 C 0.3972(7) 0.3586(7) 0.1431(7) 0.083(3) Uiso 1 1 d D . . F2 F 0.0114(5) 1.0321(5) 0.3089(4) 0.119(4) Uani 1 1 d . . . C32 C 0.8928(6) 0.2267(6) 0.3232(7) 0.064(5) Uani 1 1 d . . . H32 H 0.9207 0.1977 0.3402 0.077 Uiso 1 1 calc R . . C33 C 0.8544(6) 0.2442(6) 0.3455(6) 0.059(4) Uani 1 1 d . . . H33 H 0.8560 0.2272 0.3779 0.071 Uiso 1 1 calc R . . C31 C 0.8907(6) 0.2510(6) 0.2764(7) 0.062(4) Uani 1 1 d . . . H31 H 0.9171 0.2381 0.2611 0.075 Uiso 1 1 calc R . . N2 N 0.3802(6) 0.3079(6) 0.1457(5) 0.083(3) Uiso 1 1 d D . . C134 C 0.4190(7) 0.4206(6) 0.1398(6) 0.083(3) Uiso 1 1 d D . . H13D H 0.3897 0.4460 0.1162 0.124 Uiso 1 1 calc R . . H13E H 0.4501 0.4176 0.1266 0.124 Uiso 1 1 calc R . . H13F H 0.4316 0.4395 0.1743 0.124 Uiso 1 1 calc R . . N3 N 0.6647(8) 0.2502(8) -0.0313(7) 0.119(6) Uiso 1 1 d D . . C136 C 0.7470(11) 0.2113(14) -0.0684(11) 0.201(13) Uiso 1 1 d D . . H13G H 0.7420 0.1670 -0.0752 0.301 Uiso 1 1 calc R . . H13H H 0.7844 0.2190 -0.0440 0.301 Uiso 1 1 calc R . . H13I H 0.7422 0.2332 -0.1009 0.301 Uiso 1 1 calc R . . C135 C 0.7039(13) 0.2345(17) -0.0446(15) 0.227(16) Uiso 1 1 d 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 Ag1 0.0173(4) 0.0099(3) 0.0233(4) -0.0006(3) 0.0054(3) -0.0035(3) S6 0.0150(13) 0.0115(10) 0.0244(13) -0.0028(9) 0.0016(10) -0.0032(9) S8 0.0236(14) 0.0117(10) 0.0205(12) -0.0011(9) 0.0044(10) 0.0009(10) S5 0.0162(13) 0.0095(10) 0.0254(13) -0.0013(9) 0.0021(10) -0.0017(9) S2 0.0223(14) 0.0165(11) 0.0188(12) -0.0022(9) 0.0065(10) -0.0081(10) S1 0.0223(13) 0.0164(11) 0.0186(12) 0.0011(9) 0.0058(10) -0.0088(10) S7 0.0169(13) 0.0145(11) 0.0270(13) -0.0019(10) 0.0062(10) -0.0032(9) S4 0.0264(14) 0.0173(11) 0.0188(12) -0.0045(9) 0.0096(11) -0.0120(10) S3 0.0269(14) 0.0203(12) 0.0161(12) -0.0029(9) 0.0085(10) -0.0105(10) C10 0.029(6) 0.005(4) 0.014(5) -0.007(3) 0.003(4) 0.001(4) C9 0.015(5) 0.011(4) 0.015(5) -0.002(3) 0.004(4) -0.007(4) C1 0.011(5) 0.008(4) 0.027(5) -0.003(4) 0.007(4) -0.006(3) C2 0.014(5) 0.005(4) 0.014(4) 0.002(3) 0.003(4) -0.004(3) C53 0.017(6) 0.011(4) 0.048(7) -0.002(4) 0.015(5) -0.002(4) C47 0.019(5) 0.015(5) 0.018(5) 0.001(4) -0.006(4) -0.005(4) C21 0.042(8) 0.037(7) 0.062(8) 0.008(6) 0.035(7) 0.008(6) C11 0.004(4) 0.015(4) 0.014(4) 0.000(3) 0.002(3) 0.002(3) C14 0.043(7) 0.009(4) 0.015(5) -0.001(4) 0.002(5) -0.012(4) C3 0.024(5) 0.010(4) 0.015(5) -0.006(4) 0.004(4) -0.010(4) C59 0.023(6) 0.016(5) 0.024(5) -0.001(4) 0.001(4) -0.014(4) C46 0.038(7) 0.018(5) 0.024(5) -0.007(4) 0.016(5) -0.010(4) C29 0.024(6) 0.016(5) 0.028(6) 0.003(4) -0.004(5) -0.012(4) C18 0.031(6) 0.026(5) 0.035(6) -0.007(5) 0.012(5) 0.001(5) C24 0.015(5) 0.027(5) 0.026(5) 0.001(4) 0.002(4) 0.005(4) C6 0.014(5) 0.007(4) 0.036(6) -0.003(4) 0.006(4) -0.001(4) C13 0.035(6) 0.014(4) 0.014(5) 0.000(4) 0.006(4) -0.007(4) C12 0.024(5) 0.012(4) 0.009(4) -0.003(3) 0.002(4) -0.001(4) C4 0.030(6) 0.014(4) 0.019(5) -0.003(4) 0.015(4) -0.009(4) C5 0.021(5) 0.015(4) 0.013(5) 0.001(4) 0.003(4) -0.004(4) C23 0.015(5) 0.007(4) 0.026(5) 0.000(4) 0.004(4) -0.004(4) C8 0.028(6) 0.024(5) 0.033(6) -0.010(4) 0.008(5) -0.015(5) C40 0.036(7) 0.039(6) 0.033(6) 0.003(5) 0.018(5) 0.009(5) C17 0.021(6) 0.023(5) 0.021(5) -0.004(4) 0.005(4) -0.002(4) C52 0.040(7) 0.023(5) 0.035(6) 0.001(5) 0.005(5) 0.000(5) C41 0.017(5) 0.026(5) 0.027(5) -0.007(4) 0.004(4) -0.006(4) C54 0.045(7) 0.025(5) 0.043(7) -0.002(5) 0.028(6) -0.003(5) C26 0.020(6) 0.034(6) 0.030(6) 0.006(5) -0.002(5) 0.001(5) C39 0.056(9) 0.050(8) 0.051(8) 0.011(6) 0.032(7) 0.027(7) C27 0.048(8) 0.025(6) 0.037(7) 0.005(5) 0.012(6) 0.018(5) C30 0.022(6) 0.027(6) 0.055(7) -0.007(5) 0.003(5) -0.002(5) C56 0.052(9) 0.020(6) 0.102(12) 0.012(7) 0.064(9) 0.007(6) C45 0.069(10) 0.035(6) 0.040(7) -0.004(5) 0.031(7) -0.021(6) C49 0.072(10) 0.034(6) 0.026(6) 0.014(5) 0.001(6) -0.009(7) C35 0.022(6) 0.028(5) 0.027(6) 0.001(4) 0.014(5) -0.005(4) C48 0.040(7) 0.044(7) 0.039(7) 0.019(6) 0.005(6) -0.011(6) C42 0.051(8) 0.022(5) 0.037(7) -0.007(5) 0.022(6) 0.000(5) C25 0.026(6) 0.048(7) 0.023(6) 0.006(5) 0.006(5) -0.003(5) C7 0.024(6) 0.024(5) 0.023(5) -0.005(4) 0.003(4) -0.008(4) C64 0.045(7) 0.038(6) 0.027(6) 0.006(5) 0.017(5) -0.003(5) C44 0.050(8) 0.043(7) 0.046(7) -0.032(6) 0.031(6) -0.020(6) C28 0.042(7) 0.022(5) 0.023(5) -0.009(4) 0.009(5) 0.006(5) C19 0.033(7) 0.031(6) 0.042(7) -0.002(5) 0.026(6) -0.001(5) C15 0.037(7) 0.028(5) 0.026(6) -0.009(4) 0.008(5) -0.014(5) C36 0.034(7) 0.049(7) 0.031(6) -0.010(5) 0.010(5) -0.021(6) C60 0.034(7) 0.019(5) 0.032(6) 0.009(4) -0.001(5) 0.002(5) C37 0.058(9) 0.052(8) 0.031(7) -0.015(6) 0.020(7) -0.015(7) C43 0.048(8) 0.049(7) 0.051(8) -0.022(6) 0.033(7) -0.004(6) C16 0.047(7) 0.012(5) 0.039(6) -0.002(4) 0.008(6) -0.003(5) C57 0.036(8) 0.033(7) 0.097(12) 0.002(7) 0.034(8) 0.006(6) C50 0.037(7) 0.015(5) 0.038(7) 0.005(5) -0.023(6) 0.000(5) C51 0.031(7) 0.027(6) 0.051(8) 0.006(5) -0.003(6) 0.006(5) C61 0.042(8) 0.027(6) 0.050(8) 0.009(6) -0.004(6) -0.007(5) C38 0.099(13) 0.037(7) 0.038(8) -0.009(6) 0.048(8) -0.006(7) C22 0.041(7) 0.025(5) 0.053(7) 0.000(5) 0.026(6) -0.005(5) C58 0.028(7) 0.023(5) 0.061(8) 0.004(5) 0.022(6) 0.000(5) C55 0.072(10) 0.026(6) 0.054(8) 0.002(5) 0.040(8) -0.006(6) C20 0.030(7) 0.042(7) 0.052(7) -0.028(6) 0.025(6) -0.009(5) C63 0.059(9) 0.049(7) 0.029(7) 0.001(6) 0.018(6) -0.018(7) C34 0.029(7) 0.043(7) 0.053(8) 0.016(6) -0.001(6) -0.018(6) C62 0.054(9) 0.040(7) 0.036(7) 0.007(6) -0.003(6) -0.025(7) Ag2 0.0193(4) 0.0219(4) 0.0350(5) -0.0093(3) 0.0075(3) 0.0020(3) S9 0.0333(16) 0.0108(11) 0.0287(14) 0.0006(10) 0.0125(12) 0.0005(10) S16 0.0277(15) 0.0214(12) 0.0198(13) 0.0054(10) 0.0062(11) 0.0027(11) S14 0.0321(16) 0.0301(14) 0.0190(13) 0.0033(11) 0.0061(11) -0.0007(12) S12 0.057(2) 0.0140(12) 0.0324(15) -0.0006(11) 0.0201(14) -0.0023(12) S11 0.0489(19) 0.0147(12) 0.0288(14) 0.0008(10) 0.0140(13) 0.0021(12) S13 0.0382(17) 0.0186(12) 0.0219(13) 0.0013(10) 0.0022(12) 0.0048(11) S15 0.0434(18) 0.0253(13) 0.0191(13) 0.0025(11) 0.0057(12) 0.0042(12) S10 0.0443(18) 0.0152(12) 0.0490(18) -0.0048(12) 0.0268(15) -0.0067(12) C67 0.023(6) 0.022(5) 0.020(5) -0.007(4) 0.013(4) -0.006(4) C66 0.034(6) 0.018(5) 0.033(6) -0.003(4) 0.022(5) 0.000(4) C69 0.078(9) 0.006(4) 0.017(5) -0.002(4) 0.025(5) -0.001(5) C89 0.025(6) 0.020(5) 0.031(6) 0.001(4) 0.010(5) 0.001(4) C79 0.034(6) 0.017(5) 0.029(6) 0.008(4) 0.015(5) 0.000(4) C82 0.012(5) 0.020(5) 0.020(5) -0.001(4) 0.002(4) 0.002(4) C71 0.066(9) 0.013(5) 0.020(5) 0.003(4) 0.007(5) 0.008(5) C75 0.022(6) 0.019(5) 0.017(5) -0.002(4) -0.002(4) -0.002(4) C94 0.027(6) 0.026(5) 0.042(7) -0.004(5) 0.011(5) -0.004(5) C111 0.024(6) 0.018(5) 0.027(6) 0.002(4) 0.006(4) 0.001(4) C90 0.014(5) 0.031(6) 0.033(6) 0.001(5) 0.001(5) -0.009(4) C88 0.028(6) 0.004(4) 0.019(5) -0.002(3) 0.005(4) 0.005(4) C78 0.034(6) 0.012(4) 0.027(6) 0.002(4) 0.013(5) -0.001(4) C106 0.014(5) 0.012(4) 0.030(6) -0.002(4) 0.003(4) 0.004(4) C93 0.025(6) 0.020(5) 0.030(6) 0.002(4) 0.004(5) 0.007(4) C91 0.041(7) 0.014(5) 0.024(6) -0.002(4) 0.003(5) -0.002(5) C68 0.043(7) 0.015(5) 0.022(5) -0.004(4) 0.019(5) -0.007(5) C83 0.032(6) 0.009(4) 0.049(7) 0.001(4) 0.022(5) -0.006(4) C95 0.034(7) 0.034(6) 0.055(8) 0.019(6) 0.011(6) 0.010(5) C100 0.015(5) 0.015(5) 0.049(7) -0.005(5) 0.007(5) -0.007(4) C110 0.045(8) 0.023(5) 0.033(6) -0.003(5) 0.005(6) -0.002(5) C118 0.025(6) 0.015(5) 0.039(6) -0.006(4) 0.006(5) 0.008(4) C76 0.031(6) 0.020(5) 0.016(5) 0.003(4) 0.000(4) -0.002(4) C101 0.052(8) 0.031(6) 0.049(8) -0.011(5) 0.017(7) -0.011(6) C70 0.073(9) 0.009(4) 0.018(5) 0.002(4) 0.017(6) 0.001(5) C92 0.037(7) 0.015(5) 0.027(6) -0.006(4) 0.014(5) 0.002(4) C87 0.042(7) 0.010(4) 0.025(5) -0.004(4) 0.010(5) -0.004(4) C129 0.069(9) 0.028(6) 0.033(7) -0.010(5) 0.016(6) -0.011(6) C81 0.046(8) 0.025(5) 0.040(7) -0.002(5) 0.016(6) -0.002(5) C77 0.042(7) 0.027(5) 0.013(5) 0.007(4) 0.007(5) -0.004(5) C109 0.027(6) 0.022(5) 0.043(7) -0.015(5) 0.007(5) -0.009(5) C105 0.034(7) 0.024(5) 0.041(7) 0.008(5) -0.005(5) -0.002(5) C107 0.028(6) 0.031(5) 0.023(5) -0.001(4) 0.013(5) -0.002(5) C108 0.035(7) 0.029(6) 0.035(6) 0.011(5) 0.011(5) -0.008(5) C80 0.024(6) 0.031(6) 0.033(6) 0.001(5) 0.012(5) -0.001(5) C84 0.058(9) 0.017(5) 0.060(8) -0.004(5) 0.039(7) 0.003(5) C104 0.023(7) 0.020(6) 0.081(10) 0.011(6) 0.000(7) 0.002(5) C128 0.045(8) 0.033(6) 0.040(7) 0.005(5) 0.018(6) 0.007(5) C112 0.020(6) 0.028(5) 0.032(6) 0.004(5) 0.003(5) 0.008(5) C113 0.036(7) 0.043(7) 0.034(6) 0.012(5) 0.019(5) 0.026(5) C117 0.033(7) 0.038(7) 0.045(7) 0.005(5) 0.010(6) -0.004(5) C86 0.034(7) 0.019(5) 0.040(7) 0.008(5) 0.005(5) -0.002(5) C73 0.079(10) 0.020(5) 0.032(7) 0.007(5) 0.012(6) 0.014(6) C98 0.042(8) 0.031(6) 0.055(8) 0.008(6) 0.023(6) 0.005(5) C96 0.040(8) 0.044(7) 0.048(8) 0.015(6) 0.005(6) -0.007(6) C74 0.019(5) 0.020(5) 0.026(6) 0.003(4) 0.000(4) -0.004(4) C122 0.025(7) 0.025(6) 0.072(9) 0.022(6) -0.001(6) 0.009(5) C124 0.038(7) 0.044(7) 0.025(6) -0.009(5) 0.012(5) -0.009(6) C99 0.038(7) 0.030(6) 0.044(7) 0.011(5) 0.006(6) 0.001(5) C72 0.074(10) 0.021(5) 0.032(6) 0.001(5) 0.006(6) 0.001(6) C126 0.101(14) 0.079(11) 0.051(9) -0.014(8) 0.042(9) -0.010(10) C114 0.047(9) 0.063(9) 0.041(8) 0.006(6) 0.020(7) 0.027(7) C97 0.033(7) 0.060(8) 0.041(7) 0.010(6) 0.010(6) 0.003(6) C119 0.048(8) 0.049(7) 0.025(6) -0.013(5) 0.002(5) -0.007(6) C103 0.031(7) 0.040(7) 0.053(8) -0.012(6) -0.007(6) 0.014(6) C123 0.034(7) 0.035(6) 0.031(6) 0.005(5) -0.003(5) -0.004(5) C85 0.041(7) 0.027(5) 0.041(7) 0.022(5) 0.025(6) 0.007(5) C115 0.037(8) 0.092(11) 0.055(9) 0.024(8) 0.033(7) 0.012(8) C102 0.045(8) 0.050(7) 0.039(7) -0.004(6) 0.010(6) 0.004(6) C127 0.050(9) 0.072(10) 0.055(9) 0.013(7) 0.035(7) 0.003(7) C116 0.031(8) 0.071(10) 0.081(10) 0.025(8) 0.026(7) -0.006(7) C121 0.037(8) 0.022(6) 0.072(10) -0.015(6) -0.008(7) 0.000(5) C120 0.065(10) 0.058(9) 0.040(8) -0.028(7) -0.002(7) -0.015(8) C125 0.062(10) 0.061(9) 0.056(9) -0.014(7) 0.036(8) 0.000(7) P10 0.0324(17) 0.0293(15) 0.0355(17) -0.0033(13) 0.0060(14) -0.0018(13) P9 0.050(2) 0.057(2) 0.0319(17) -0.0064(15) 0.0138(16) -0.0094(17) F12 0.041(4) 0.033(4) 0.084(5) -0.010(4) 0.009(4) -0.007(3) F9 0.063(5) 0.055(4) 0.052(4) 0.004(3) 0.002(4) -0.035(4) F1 0.092(6) 0.054(4) 0.033(4) 0.008(3) 0.014(4) -0.012(4) F7 0.067(7) 0.125(8) 0.132(9) 0.090(7) -0.038(6) -0.053(6) F10 0.060(5) 0.087(6) 0.051(5) 0.024(4) 0.013(4) -0.012(4) F4 0.068(6) 0.115(7) 0.055(5) 0.021(5) 0.005(4) -0.003(5) F5 0.105(7) 0.057(5) 0.077(6) 0.010(4) 0.056(5) 0.005(5) F3 0.113(8) 0.043(4) 0.079(6) -0.011(4) -0.006(5) -0.029(5) F8 0.108(7) 0.066(5) 0.081(6) -0.038(4) 0.060(5) -0.022(5) F6 0.125(9) 0.113(7) 0.054(5) -0.007(5) 0.024(5) -0.074(7) F11 0.074(7) 0.070(6) 0.239(13) -0.065(7) 0.100(8) -0.017(5) F2 0.109(9) 0.146(10) 0.121(9) 0.048(7) 0.063(7) 0.064(8) C32 0.037(9) 0.022(6) 0.098(12) 0.011(7) -0.024(8) -0.006(6) C33 0.045(9) 0.049(8) 0.061(9) 0.036(7) -0.012(7) -0.011(7) C31 0.037(9) 0.029(7) 0.104(13) -0.014(8) 0.003(8) 0.008(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 Ag1 P3 2.457(3) . ? Ag1 P1 2.459(3) . ? Ag1 P4 2.494(3) . ? Ag1 P2 2.498(3) . ? P3 C47 1.812(9) . ? P3 C41 1.828(10) . ? P3 C9 1.831(8) . ? S6 C9 1.748(9) . ? S6 C11 1.763(8) . ? P2 C35 1.805(10) . ? P2 C1 1.818(9) . ? P2 C29 1.826(10) . ? S8 C12 1.754(9) . ? S8 C14 1.763(10) . ? S5 C11 1.751(8) . ? S5 C10 1.754(8) . ? S2 C1 1.753(8) . ? S2 C3 1.755(9) . ? S1 C2 1.750(8) . ? S1 C3 1.759(9) . ? P4 C10 1.814(9) . ? P4 C53 1.817(10) . ? P4 C59 1.821(10) . ? P1 C23 1.810(9) . ? P1 C17 1.814(10) . ? P1 C2 1.819(8) . ? S7 C12 1.733(10) . ? S7 C13 1.768(9) . ? S4 C4 1.757(9) . ? S4 C5 1.763(9) . ? S3 C4 1.749(9) . ? S3 C6 1.761(9) . ? C10 C9 1.352(12) . ? C1 C2 1.358(12) . ? C53 C54 1.356(14) . ? C53 C58 1.400(14) . ? C47 C48 1.386(14) . ? C47 C52 1.393(14) . ? C21 C20 1.386(15) . ? C21 C22 1.398(15) . ? C11 C12 1.353(11) . ? C14 C13 1.340(14) . ? C14 C16 1.495(12) . ? C3 C4 1.347(12) . ? C59 C64 1.377(14) . ? C59 C60 1.389(13) . ? C46 C41 1.363(13) . ? C46 C45 1.395(14) . ? C29 C30 1.359(15) . ? C29 C34 1.400(14) . ? C18 C19 1.356(14) . ? C18 C17 1.401(13) . ? C24 C25 1.376(13) . ? C24 C23 1.401(12) . ? C6 C5 1.345(12) . ? C6 C8 1.505(13) . ? C13 C15 1.486(14) . ? C5 C7 1.497(12) . ? C23 C28 1.386(13) . ? C40 C35 1.389(14) . ? C40 C39 1.420(15) . ? C17 C22 1.387(14) . ? C52 C51 1.390(14) . ? C41 C42 1.397(13) . ? C54 C55 1.402(15) . ? C26 C27 1.358(14) . ? C26 C25 1.401(14) . ? C39 C38 1.377(17) . ? C27 C28 1.380(14) . ? C30 C31 1.399(16) . ? C56 C57 1.345(18) . ? C56 C55 1.390(18) . ? C45 C44 1.374(15) . ? C49 C50 1.348(17) . ? C49 C48 1.400(15) . ? C35 C36 1.398(14) . ? C42 C43 1.387(15) . ? C64 C63 1.386(14) . ? C44 C43 1.344(16) . ? C19 C20 1.369(15) . ? C36 C37 1.384(16) . ? C60 C61 1.392(15) . ? C37 C38 1.351(18) . ? C57 C58 1.368(16) . ? C50 C51 1.353(16) . ? C61 C62 1.371(17) . ? C63 C62 1.378(17) . ? C34 C33 1.398(17) . ? Ag2 P7 2.461(3) . ? Ag2 P5 2.474(3) . ? Ag2 P6 2.493(3) . ? Ag2 P8 2.513(3) . ? P7 C112 1.805(11) . ? P7 C106 1.806(9) . ? P7 C75 1.807(9) . ? S9 C67 1.757(10) . ? S9 C68 1.773(9) . ? P5 C88 1.796(9) . ? P5 C82 1.817(9) . ? P5 C67 1.818(9) . ? S16 C77 1.766(10) . ? S16 C78 1.768(10) . ? P8 C124 1.802(11) . ? P8 C118 1.821(10) . ? P8 C74 1.830(10) . ? S14 C76 1.765(10) . ? S14 C74 1.765(9) . ? P6 C66 1.804(11) . ? P6 C100 1.843(11) . ? P6 C94 1.850(11) . ? S12 C70 1.762(12) . ? S12 C69 1.762(9) . ? S11 C69 1.728(13) . ? S11 C71 1.773(10) . ? S13 C76 1.749(9) . ? S13 C75 1.756(10) . ? S15 C79 1.748(11) . ? S15 C77 1.758(11) . ? S10 C68 1.757(11) . ? S10 C66 1.759(9) . ? C67 C66 1.343(13) . ? C69 C68 1.327(14) . ? C89 C90 1.369(13) . ? C89 C88 1.389(13) . ? C79 C78 1.353(13) . ? C79 C81 1.491(14) . ? C82 C83 1.388(12) . ? C82 C87 1.394(12) . ? C71 C70 1.317(16) . ? C71 C73 1.488(16) . ? C75 C74 1.351(13) . ? C94 C99 1.307(15) . ? C94 C95 1.413(14) . ? C111 C110 1.365(14) . ? C111 C106 1.412(13) . ? C90 C91 1.387(14) . ? C88 C93 1.421(13) . ? C78 C80 1.496(13) . ? C106 C107 1.390(13) . ? C93 C92 1.380(13) . ? C91 C92 1.354(14) . ? C83 C84 1.381(14) . ? C95 C96 1.400(16) . ? C100 C105 1.352(14) . ? C100 C101 1.397(15) . ? C110 C109 1.380(15) . ? C118 C123 1.373(14) . ? C118 C119 1.382(14) . ? C76 C77 1.320(14) . ? C101 C102 1.410(15) . ? C70 C72 1.496(13) . ? C87 C86 1.361(14) . ? C129 C124 1.332(15) . ? C129 C128 1.437(16) . ? C109 C108 1.361(14) . ? C105 C104 1.364(16) . ? C107 C108 1.408(14) . ? C84 C85 1.385(13) . ? C104 C103 1.408(17) . ? C128 C127 1.318(16) . ? C112 C117 1.361(14) . ? C112 C113 1.417(14) . ? C113 C114 1.370(16) . ? C117 C116 1.391(16) . ? C86 C85 1.344(14) . ? C98 C97 1.348(16) . ? C98 C99 1.409(15) . ? C96 C97 1.381(17) . ? C122 C121 1.350(17) . ? C122 C123 1.358(15) . ? C124 C125 1.404(15) . ? C126 C125 1.383(18) . ? C126 C127 1.395(19) . ? C114 C115 1.324(18) . ? C119 C120 1.386(16) . ? C103 C102 1.358(16) . ? C115 C116 1.375(19) . ? C121 C120 1.364(18) . ? P10 F11 1.546(8) . ? P10 F7 1.564(8) . ? P10 F10 1.570(7) . ? P10 F9 1.580(7) . ? P10 F8 1.587(8) . ? P10 F12 1.601(7) . ? P9 F2 1.531(10) . ? P9 F5 1.561(8) . ? P9 F6 1.570(9) . ? P9 F3 1.579(8) . ? P9 F1 1.585(7) . ? P9 F4 1.599(8) . ? C132 C131 1.443(13) . ? N1 C131 1.161(13) . ? C133 N2 1.169(12) . ? C133 C134 1.442(13) . ? C32 C31 1.34(2) . ? C32 C33 1.35(2) . ? N3 C135 1.200(16) . ? C136 C135 1.509(16) . ? 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 P3 Ag1 P1 124.54(8) . . ? P3 Ag1 P4 85.64(8) . . ? P1 Ag1 P4 126.39(9) . . ? P3 Ag1 P2 126.09(9) . . ? P1 Ag1 P2 85.93(9) . . ? P4 Ag1 P2 112.40(8) . . ? C47 P3 C41 104.5(5) . . ? C47 P3 C9 103.7(4) . . ? C41 P3 C9 104.3(4) . . ? C47 P3 Ag1 127.3(3) . . ? C41 P3 Ag1 111.8(3) . . ? C9 P3 Ag1 102.8(3) . . ? C9 S6 C11 95.3(4) . . ? C35 P2 C1 102.3(4) . . ? C35 P2 C29 106.9(5) . . ? C1 P2 C29 102.5(4) . . ? C35 P2 Ag1 132.5(3) . . ? C1 P2 Ag1 102.3(3) . . ? C29 P2 Ag1 106.6(3) . . ? C12 S8 C14 95.4(4) . . ? C11 S5 C10 95.6(4) . . ? C1 S2 C3 94.5(4) . . ? C2 S1 C3 94.2(4) . . ? C10 P4 C53 105.2(4) . . ? C10 P4 C59 101.6(4) . . ? C53 P4 C59 107.1(5) . . ? C10 P4 Ag1 102.5(3) . . ? C53 P4 Ag1 119.4(3) . . ? C59 P4 Ag1 118.4(3) . . ? C23 P1 C17 106.6(4) . . ? C23 P1 C2 104.7(4) . . ? C17 P1 C2 102.7(4) . . ? C23 P1 Ag1 111.6(3) . . ? C17 P1 Ag1 124.8(3) . . ? C2 P1 Ag1 104.3(3) . . ? C12 S7 C13 96.1(4) . . ? C4 S4 C5 95.7(4) . . ? C4 S3 C6 95.3(5) . . ? C9 C10 S5 116.9(7) . . ? C9 C10 P4 123.3(6) . . ? S5 C10 P4 119.5(5) . . ? C10 C9 S6 117.5(6) . . ? C10 C9 P3 123.8(6) . . ? S6 C9 P3 118.7(5) . . ? C2 C1 S2 116.6(6) . . ? C2 C1 P2 125.1(6) . . ? S2 C1 P2 118.3(5) . . ? C1 C2 S1 117.4(6) . . ? C1 C2 P1 122.3(6) . . ? S1 C2 P1 120.3(5) . . ? C54 C53 C58 118.0(10) . . ? C54 C53 P4 122.9(8) . . ? C58 C53 P4 118.7(8) . . ? C48 C47 C52 119.5(9) . . ? C48 C47 P3 118.1(8) . . ? C52 C47 P3 122.4(8) . . ? C20 C21 C22 119.8(11) . . ? C12 C11 S5 123.6(7) . . ? C12 C11 S6 121.9(7) . . ? S5 C11 S6 114.5(5) . . ? C13 C14 C16 127.1(9) . . ? C13 C14 S8 117.3(7) . . ? C16 C14 S8 115.6(8) . . ? C4 C3 S2 122.5(7) . . ? C4 C3 S1 123.4(7) . . ? S2 C3 S1 114.1(5) . . ? C64 C59 C60 118.5(9) . . ? C64 C59 P4 116.8(8) . . ? C60 C59 P4 124.6(8) . . ? C41 C46 C45 119.7(9) . . ? C30 C29 C34 119.8(10) . . ? C30 C29 P2 118.4(8) . . ? C34 C29 P2 121.1(9) . . ? C19 C18 C17 122.2(10) . . ? C25 C24 C23 120.9(9) . . ? C5 C6 C8 127.7(9) . . ? C5 C6 S3 117.6(7) . . ? C8 C6 S3 114.4(7) . . ? C14 C13 C15 128.5(8) . . ? C14 C13 S7 116.5(7) . . ? C15 C13 S7 115.1(7) . . ? C11 C12 S7 122.6(7) . . ? C11 C12 S8 122.6(7) . . ? S7 C12 S8 114.7(5) . . ? C3 C4 S3 123.9(7) . . ? C3 C4 S4 122.1(7) . . ? S3 C4 S4 114.0(5) . . ? C6 C5 C7 127.1(9) . . ? C6 C5 S4 116.2(7) . . ? C7 C5 S4 116.6(7) . . ? C28 C23 C24 117.8(8) . . ? C28 C23 P1 119.6(7) . . ? C24 C23 P1 121.7(7) . . ? C35 C40 C39 119.4(11) . . ? C22 C17 C18 118.3(9) . . ? C22 C17 P1 116.8(8) . . ? C18 C17 P1 124.9(7) . . ? C51 C52 C47 120.4(11) . . ? C46 C41 C42 119.2(9) . . ? C46 C41 P3 124.7(8) . . ? C42 C41 P3 115.7(8) . . ? C53 C54 C55 121.8(12) . . ? C27 C26 C25 120.4(10) . . ? C38 C39 C40 119.7(12) . . ? C26 C27 C28 119.8(10) . . ? C29 C30 C31 119.0(12) . . ? C57 C56 C55 120.7(11) . . ? C44 C45 C46 120.3(10) . . ? C50 C49 C48 121.3(12) . . ? C40 C35 C36 118.8(10) . . ? C40 C35 P2 117.0(8) . . ? C36 C35 P2 124.2(8) . . ? C47 C48 C49 118.2(12) . . ? C43 C42 C41 120.3(10) . . ? C24 C25 C26 119.4(10) . . ? C59 C64 C63 122.1(11) . . ? C43 C44 C45 120.6(11) . . ? C27 C28 C23 121.7(9) . . ? C18 C19 C20 119.3(10) . . ? C37 C36 C35 120.7(11) . . ? C59 C60 C61 120.0(11) . . ? C38 C37 C36 120.5(11) . . ? C44 C43 C42 120.0(11) . . ? C56 C57 C58 120.6(13) . . ? C49 C50 C51 121.2(10) . . ? C50 C51 C52 119.3(11) . . ? C62 C61 C60 119.8(11) . . ? C37 C38 C39 120.8(11) . . ? C17 C22 C21 119.5(10) . . ? C57 C58 C53 120.8(12) . . ? C56 C55 C54 118.1(12) . . ? C19 C20 C21 120.7(10) . . ? C62 C63 C64 118.2(12) . . ? C33 C34 C29 118.6(13) . . ? C61 C62 C63 121.2(11) . . ? P7 Ag2 P5 121.51(9) . . ? P7 Ag2 P6 134.50(10) . . ? P5 Ag2 P6 84.66(9) . . ? P7 Ag2 P8 85.50(9) . . ? P5 Ag2 P8 118.52(9) . . ? P6 Ag2 P8 115.86(9) . . ? C112 P7 C106 107.1(5) . . ? C112 P7 C75 101.6(5) . . ? C106 P7 C75 102.3(4) . . ? C112 P7 Ag2 123.8(3) . . ? C106 P7 Ag2 115.0(3) . . ? C75 P7 Ag2 103.8(3) . . ? C67 S9 C68 96.9(5) . . ? C88 P5 C82 102.4(4) . . ? C88 P5 C67 104.0(4) . . ? C82 P5 C67 105.4(4) . . ? C88 P5 Ag2 123.9(3) . . ? C82 P5 Ag2 115.5(3) . . ? C67 P5 Ag2 103.8(3) . . ? C77 S16 C78 96.0(5) . . ? C124 P8 C118 105.6(5) . . ? C124 P8 C74 105.6(5) . . ? C118 P8 C74 102.9(4) . . ? C124 P8 Ag2 121.2(4) . . ? C118 P8 Ag2 116.4(3) . . ? C74 P8 Ag2 103.0(3) . . ? C76 S14 C74 93.5(5) . . ? C66 P6 C100 103.1(4) . . ? C66 P6 C94 102.1(5) . . ? C100 P6 C94 108.7(5) . . ? C66 P6 Ag2 103.9(3) . . ? C100 P6 Ag2 112.4(3) . . ? C94 P6 Ag2 123.9(3) . . ? C70 S12 C69 95.9(5) . . ? C69 S11 C71 96.7(5) . . ? C76 S13 C75 94.3(4) . . ? C79 S15 C77 96.4(5) . . ? C68 S10 C66 96.4(5) . . ? C66 C67 S9 116.0(7) . . ? C66 C67 P5 123.6(8) . . ? S9 C67 P5 120.4(5) . . ? C67 C66 S10 117.8(8) . . ? C67 C66 P6 123.5(7) . . ? S10 C66 P6 118.7(6) . . ? C68 C69 S11 124.4(8) . . ? C68 C69 S12 122.1(9) . . ? S11 C69 S12 113.4(6) . . ? C90 C89 C88 121.4(9) . . ? C78 C79 C81 127.2(10) . . ? C78 C79 S15 117.1(8) . . ? C81 C79 S15 115.6(8) . . ? C83 C82 C87 118.0(9) . . ? C83 C82 P5 123.2(7) . . ? C87 C82 P5 118.5(7) . . ? C70 C71 C73 128.9(9) . . ? C70 C71 S11 116.4(9) . . ? C73 C71 S11 114.8(8) . . ? C74 C75 S13 116.5(7) . . ? C74 C75 P7 125.2(7) . . ? S13 C75 P7 118.4(5) . . ? C99 C94 C95 119.4(11) . . ? C99 C94 P6 117.8(8) . . ? C95 C94 P6 122.6(9) . . ? C110 C111 C106 120.4(9) . . ? C89 C90 C91 119.5(10) . . ? C89 C88 C93 117.4(8) . . ? C89 C88 P5 123.6(7) . . ? C93 C88 P5 119.0(7) . . ? C79 C78 C80 126.3(9) . . ? C79 C78 S16 116.2(8) . . ? C80 C78 S16 117.2(7) . . ? C107 C106 C111 119.0(9) . . ? C107 C106 P7 118.6(7) . . ? C111 C106 P7 121.6(7) . . ? C92 C93 C88 120.6(10) . . ? C92 C91 C90 121.4(9) . . ? C69 C68 S10 123.9(8) . . ? C69 C68 S9 123.8(9) . . ? S10 C68 S9 112.3(5) . . ? C84 C83 C82 119.8(9) . . ? C96 C95 C94 119.8(12) . . ? C105 C100 C101 120.4(11) . . ? C105 C100 P6 123.6(9) . . ? C101 C100 P6 115.5(8) . . ? C111 C110 C109 119.9(10) . . ? C123 C118 C119 118.0(10) . . ? C123 C118 P8 118.7(8) . . ? C119 C118 P8 123.4(9) . . ? C77 C76 S13 121.0(8) . . ? C77 C76 S14 125.5(7) . . ? S13 C76 S14 113.4(6) . . ? C100 C101 C102 117.7(11) . . ? C71 C70 C72 127.6(11) . . ? C71 C70 S12 117.5(7) . . ? C72 C70 S12 115.0(9) . . ? C91 C92 C93 119.6(9) . . ? C86 C87 C82 120.9(9) . . ? C124 C129 C128 123.0(11) . . ? C76 C77 S15 122.0(7) . . ? C76 C77 S16 125.4(8) . . ? S15 C77 S16 112.6(6) . . ? C108 C109 C110 121.4(10) . . ? C100 C105 C104 121.5(12) . . ? C106 C107 C108 119.6(9) . . ? C109 C108 C107 119.6(9) . . ? C83 C84 C85 120.8(10) . . ? C105 C104 C103 120.0(11) . . ? C127 C128 C129 117.8(11) . . ? C117 C112 C113 118.5(10) . . ? C117 C112 P7 117.3(8) . . ? C113 C112 P7 123.8(8) . . ? C114 C113 C112 118.7(12) . . ? C112 C117 C116 120.2(12) . . ? C85 C86 C87 121.5(9) . . ? C97 C98 C99 120.7(12) . . ? C97 C96 C95 119.2(12) . . ? C75 C74 S14 117.1(7) . . ? C75 C74 P8 122.5(7) . . ? S14 C74 P8 120.4(5) . . ? C121 C122 C123 118.8(12) . . ? C129 C124 C125 117.0(11) . . ? C129 C124 P8 123.7(9) . . ? C125 C124 P8 118.6(9) . . ? C94 C99 C98 121.2(11) . . ? C125 C126 C127 118.6(13) . . ? C115 C114 C113 122.9(12) . . ? C98 C97 C96 119.7(12) . . ? C118 C119 C120 118.6(12) . . ? C102 C103 C104 118.5(12) . . ? C122 C123 C118 123.1(11) . . ? C86 C85 C84 119.1(10) . . ? C114 C115 C116 119.1(12) . . ? C103 C102 C101 121.7(13) . . ? C128 C127 C126 122.0(12) . . ? C115 C116 C117 120.5(13) . . ? C122 C121 C120 120.1(11) . . ? C121 C120 C119 121.4(12) . . ? C126 C125 C124 121.2(13) . . ? F11 P10 F7 90.0(7) . . ? F11 P10 F10 90.3(6) . . ? F7 P10 F10 177.3(5) . . ? F11 P10 F9 89.9(5) . . ? F7 P10 F9 91.3(4) . . ? F10 P10 F9 91.4(4) . . ? F11 P10 F8 178.8(5) . . ? F7 P10 F8 89.9(6) . . ? F10 P10 F8 89.7(5) . . ? F9 P10 F8 91.4(4) . . ? F11 P10 F12 91.8(4) . . ? F7 P10 F12 87.6(4) . . ? F10 P10 F12 89.7(4) . . ? F9 P10 F12 178.0(5) . . ? F8 P10 F12 86.9(4) . . ? F2 P9 F5 177.8(6) . . ? F2 P9 F6 88.8(7) . . ? F5 P9 F6 89.7(5) . . ? F2 P9 F3 91.8(6) . . ? F5 P9 F3 89.7(5) . . ? F6 P9 F3 177.8(5) . . ? F2 P9 F1 89.7(5) . . ? F5 P9 F1 92.0(5) . . ? F6 P9 F1 90.1(5) . . ? F3 P9 F1 92.1(4) . . ? F2 P9 F4 91.4(5) . . ? F5 P9 F4 86.9(5) . . ? F6 P9 F4 90.3(5) . . ? F3 P9 F4 87.5(5) . . ? F1 P9 F4 178.8(5) . . ? N1 C131 C132 172(2) . . ? N2 C133 C134 179(2) . . ? C31 C32 C33 119.9(13) . . ? C32 C33 C34 121.0(13) . . ? C32 C31 C30 121.6(14) . . ? N3 C135 C136 172(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.205 _refine_diff_density_min -1.843 _refine_diff_density_rms 0.154 # Attachment 'cop22.txt' data_final _database_code_depnum_ccdc_archive 'CCDC 615879' _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and [Co(MeCN)6][BF4]2 produced the the complex [Co(o-P2)2(MECN)][BF4]2 where the cobalt metal center displays five-coordinate geometry. The complex was analyzed by several physical methods including x-ray crystallography, NMR, IR, magnetism, and cyclic voltammetry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H67 B2 Co F8 N5 P4 S8' _chemical_formula_weight 1639.24 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 '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_Hall '-P 2ybc' _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 17.420(4) _cell_length_b 19.241(4) _cell_length_c 23.198(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.12(3) _cell_angle_gamma 90.00 _cell_volume 7630(3) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Brown _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.194 _exptl_crystal_size_min 0.185 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3372 _exptl_absorpt_coefficient_mu 0.594 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _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 'Bruker SMART 1000' _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 72641 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 24.71 _reflns_number_total 13022 _reflns_number_gt 6264 _reflns_threshold_expression I>2s(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.1809P)^2^+0.0000P] 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 13022 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1703 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2951 _refine_ls_wR_factor_gt 0.2260 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 5.123 _refine_ls_shift/su_mean 0.334 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 Co1 Co 0.22674(7) 0.22482(5) 0.21718(4) 0.0407(3) Uani 1 1 d . . . S6 S 0.18343(12) 0.10906(10) 0.39950(8) 0.0388(5) Uani 1 1 d . . . S5 S 0.18194(13) -0.00053(10) 0.30979(9) 0.0409(5) Uani 1 1 d . . . P3 P 0.22908(14) 0.10655(11) 0.22133(9) 0.0437(6) Uani 1 1 d . . . P1 P 0.23639(14) 0.23084(10) 0.11970(9) 0.0419(6) Uani 1 1 d . . . P2 P 0.24371(13) 0.34336(10) 0.21494(9) 0.0385(5) Uani 1 1 d . . . P4 P 0.23079(15) 0.22156(10) 0.31598(9) 0.0432(6) Uani 1 1 d . . . S8 S 0.18303(13) -0.01344(10) 0.49859(9) 0.0432(5) Uani 1 1 d . . . S2 S 0.35412(13) 0.43112(11) 0.15019(9) 0.0448(6) Uani 1 1 d . . . S1 S 0.34846(14) 0.32113(11) 0.06042(9) 0.0485(6) Uani 1 1 d . . . S7 S 0.18710(13) -0.11891(10) 0.40811(9) 0.0449(6) Uani 1 1 d . . . S3 S 0.39120(13) 0.43049(13) -0.03190(9) 0.0513(6) Uani 1 1 d . . . S4 S 0.39962(14) 0.54351(12) 0.05366(10) 0.0540(6) Uani 1 1 d . . . N1S N 0.1106(5) 0.2303(3) 0.2004(3) 0.0438(18) Uani 1 1 d . . . C111 C 0.1445(5) 0.2469(4) 0.0691(3) 0.043(2) Uani 1 1 d . . . C401 C 0.3243(6) 0.2359(4) 0.3634(4) 0.048(2) Uani 1 1 d . . . C101 C 0.2853(6) 0.1656(4) 0.0823(4) 0.055(3) Uani 1 1 d . . . C411 C 0.1565(6) 0.2706(4) 0.3430(3) 0.046(2) Uani 1 1 d . . . C1 C 0.2959(5) 0.3078(4) 0.1161(3) 0.044(2) Uani 1 1 d . . . C11 C 0.2047(5) 0.0843(4) 0.2911(3) 0.041(2) Uani 1 1 d . . . C10 C 0.2048(5) 0.1334(4) 0.3318(3) 0.042(2) Uani 1 1 d . . . C2 C 0.2976(5) 0.3564(4) 0.1572(3) 0.0387(19) Uani 1 1 d . . . C201 C 0.3036(5) 0.3905(4) 0.2761(3) 0.043(2) Uani 1 1 d . . . C212 C 0.1414(5) 0.4295(4) 0.1392(4) 0.045(2) Uani 1 1 d . . . H21A H 0.1786 0.4289 0.1153 0.054 Uiso 1 1 calc R . . C16 C 0.2023(6) -0.1116(5) 0.5873(4) 0.064(3) Uani 1 1 d . . . H16A H 0.2104 -0.1600 0.5965 0.096 Uiso 1 1 calc R . . H16B H 0.1547 -0.0964 0.5984 0.096 Uiso 1 1 calc R . . H16C H 0.2455 -0.0852 0.6085 0.096 Uiso 1 1 calc R . . C106 C 0.2454(6) 0.1292(4) 0.0329(4) 0.058(3) Uani 1 1 d . . . H10A H 0.1932 0.1392 0.0178 0.069 Uiso 1 1 calc R . . C14 C 0.1966(5) -0.1008(4) 0.5220(4) 0.049(2) Uani 1 1 d . . . C3 C 0.3662(5) 0.4095(4) 0.0785(4) 0.044(2) Uani 1 1 d . . . C12 C 0.1863(4) -0.0307(4) 0.4246(3) 0.0385(19) Uani 1 1 d . . . C15 C 0.2060(6) -0.2259(4) 0.4878(4) 0.059(3) Uani 1 1 d . . . H15A H 0.2115 -0.2381 0.5285 0.088 Uiso 1 1 calc R . . H15B H 0.2515 -0.2409 0.4735 0.088 Uiso 1 1 calc R . . H15C H 0.1604 -0.2482 0.4656 0.088 Uiso 1 1 calc R . . C117 C 0.1857(4) 0.0186(4) 0.3846(3) 0.0369(19) Uani 1 1 d . . . C1S C 0.0441(7) 0.2416(4) 0.1866(4) 0.047(2) Uani 1 1 d . . . C311 C 0.1540(6) 0.0628(4) 0.1699(4) 0.050(2) Uani 1 1 d . . . C413 C 0.1063(8) 0.3718(5) 0.3849(4) 0.066(3) Uani 1 1 d . . . H41A H 0.1146 0.4150 0.4029 0.080 Uiso 1 1 calc R . . C211 C 0.1557(5) 0.3935(4) 0.1918(3) 0.0395(19) Uani 1 1 d . . . C116 C 0.0846(5) 0.1998(4) 0.0658(4) 0.047(2) Uani 1 1 d . . . H11A H 0.0915 0.1603 0.0894 0.057 Uiso 1 1 calc R . . C112 C 0.1327(6) 0.3058(4) 0.0334(4) 0.050(2) Uani 1 1 d . . . H11B H 0.1728 0.3380 0.0348 0.060 Uiso 1 1 calc R . . C406 C 0.3344(6) 0.2611(4) 0.4207(4) 0.054(2) Uani 1 1 d . . . H40A H 0.2911 0.2706 0.4373 0.065 Uiso 1 1 calc R . . C215 C 0.0312(5) 0.4338(4) 0.2104(4) 0.049(2) Uani 1 1 d . . . H21B H -0.0058 0.4350 0.2344 0.059 Uiso 1 1 calc R . . C415 C 0.0186(6) 0.2815(4) 0.3452(4) 0.054(2) Uani 1 1 d . . . H41B H -0.0319 0.2637 0.3361 0.065 Uiso 1 1 calc R . . C13 C 0.1975(5) -0.1485(4) 0.4811(4) 0.049(2) Uani 1 1 d . . . C204 C 0.3996(6) 0.4553(6) 0.3700(4) 0.064(3) Uani 1 1 d . . . H20A H 0.4316 0.4771 0.4015 0.077 Uiso 1 1 calc R . . C206 C 0.2739(6) 0.4438(4) 0.3055(4) 0.056(2) Uani 1 1 d . . . H20B H 0.2222 0.4581 0.2943 0.067 Uiso 1 1 calc R . . C216 C 0.0986(5) 0.3962(4) 0.2272(4) 0.046(2) Uani 1 1 d . . . H21C H 0.1068 0.3720 0.2625 0.055 Uiso 1 1 calc R . . C214 C 0.0182(5) 0.4701(4) 0.1579(4) 0.049(2) Uani 1 1 d . . . H21D H -0.0268 0.4968 0.1472 0.059 Uiso 1 1 calc R . . C203 C 0.4288(6) 0.4016(5) 0.3400(4) 0.063(3) Uani 1 1 d . . . H20C H 0.4806 0.3876 0.3513 0.075 Uiso 1 1 calc R . . C213 C 0.0724(5) 0.4664(4) 0.1214(4) 0.050(2) Uani 1 1 d . . . H21E H 0.0626 0.4886 0.0851 0.059 Uiso 1 1 calc R . . C205 C 0.3242(7) 0.4755(5) 0.3526(4) 0.068(3) Uani 1 1 d . . . H20D H 0.3051 0.5115 0.3726 0.082 Uiso 1 1 calc R . . C416 C 0.0809(6) 0.2444(4) 0.3314(4) 0.055(3) Uani 1 1 d . . . H41C H 0.0718 0.2009 0.3139 0.066 Uiso 1 1 calc R . . C301 C 0.3168(6) 0.0563(5) 0.2231(4) 0.058(3) Uani 1 1 d . . . C115 C 0.0141(6) 0.2103(5) 0.0277(4) 0.055(2) Uani 1 1 d . . . H11C H -0.0257 0.1775 0.0252 0.066 Uiso 1 1 calc R . . C5 C 0.3984(5) 0.5158(5) -0.0576(4) 0.053(2) Uani 1 1 d . . . C6 C 0.4022(5) 0.5667(5) -0.0194(4) 0.056(2) Uani 1 1 d . . . C4 C 0.3835(5) 0.4551(4) 0.0393(3) 0.044(2) Uani 1 1 d . . . C407 C 0.4085(7) 0.2720(5) 0.4527(4) 0.064(3) Uani 1 1 d . . . H40B H 0.4148 0.2902 0.4905 0.077 Uiso 1 1 calc R . . C2S C -0.0386(5) 0.2552(5) 0.1699(4) 0.059(2) Uani 1 1 d . . . H2S1 H -0.0599 0.2639 0.2044 0.089 Uiso 1 1 calc R . . H2S2 H -0.0641 0.2157 0.1494 0.089 Uiso 1 1 calc R . . H2S3 H -0.0468 0.2952 0.1447 0.089 Uiso 1 1 calc R . . C316 C 0.0778(6) 0.0660(4) 0.1778(4) 0.055(2) Uani 1 1 d . . . H31A H 0.0666 0.0867 0.2115 0.065 Uiso 1 1 calc R . . C114 C 0.0026(6) 0.2695(5) -0.0065(4) 0.055(2) Uani 1 1 d . . . H11D H -0.0455 0.2772 -0.0312 0.066 Uiso 1 1 calc R . . C202 C 0.3807(5) 0.3695(5) 0.2937(4) 0.050(2) Uani 1 1 d . . . H20E H 0.4001 0.3335 0.2739 0.059 Uiso 1 1 calc R . . C105 C 0.2830(8) 0.0791(5) 0.0067(5) 0.074(3) Uani 1 1 d . . . H10B H 0.2572 0.0566 -0.0269 0.089 Uiso 1 1 calc R . . C104 C 0.3575(10) 0.0629(5) 0.0301(5) 0.089(4) Uani 1 1 d . . . H10C H 0.3815 0.0266 0.0139 0.107 Uiso 1 1 calc R . . C8 C 0.4101(6) 0.6424(5) -0.0317(5) 0.076(3) Uani 1 1 d . . . H8A H 0.4111 0.6488 -0.0726 0.114 Uiso 1 1 calc R . . H8B H 0.4578 0.6597 -0.0083 0.114 Uiso 1 1 calc R . . H8C H 0.3665 0.6672 -0.0220 0.114 Uiso 1 1 calc R . . C302 C 0.3889(7) 0.0882(6) 0.2318(4) 0.065(3) Uani 1 1 d . . . H30A H 0.3918 0.1364 0.2320 0.078 Uiso 1 1 calc R . . C7 C 0.4016(6) 0.5207(6) -0.1218(4) 0.071(3) Uani 1 1 d . . . H7A H 0.4056 0.5686 -0.1324 0.106 Uiso 1 1 calc R . . H7B H 0.3549 0.5010 -0.1447 0.106 Uiso 1 1 calc R . . H7C H 0.4464 0.4958 -0.1292 0.106 Uiso 1 1 calc R . . C113 C 0.0614(6) 0.3167(5) -0.0043(4) 0.059(3) Uani 1 1 d . . . H11E H 0.0539 0.3562 -0.0279 0.070 Uiso 1 1 calc R . . C405 C 0.3899(6) 0.2185(5) 0.3415(4) 0.060(3) Uani 1 1 d . . . H40C H 0.3836 0.2005 0.3037 0.072 Uiso 1 1 calc R . . C315 C 0.0174(7) 0.0385(5) 0.1358(4) 0.074(3) Uani 1 1 d . . . H31B H -0.0342 0.0400 0.1411 0.088 Uiso 1 1 calc R . . C305 C 0.3789(10) -0.0546(7) 0.2303(5) 0.096(4) Uani 1 1 d . . . H30B H 0.3758 -0.1028 0.2298 0.115 Uiso 1 1 calc R . . C412 C 0.1706(6) 0.3352(4) 0.3708(4) 0.055(2) Uani 1 1 d . . . H41D H 0.2209 0.3535 0.3798 0.066 Uiso 1 1 calc R . . C404 C 0.4647(7) 0.2269(5) 0.3738(4) 0.069(3) Uani 1 1 d . . . H40D H 0.5081 0.2133 0.3586 0.083 Uiso 1 1 calc R . . C313 C 0.1123(9) 0.0043(5) 0.0780(4) 0.076(4) Uani 1 1 d . . . H31C H 0.1239 -0.0168 0.0447 0.092 Uiso 1 1 calc R . . C414 C 0.0326(7) 0.3455(5) 0.3727(4) 0.064(3) Uani 1 1 d . . . H41F H -0.0086 0.3705 0.3828 0.077 Uiso 1 1 calc R . . C314 C 0.0366(10) 0.0085(5) 0.0852(5) 0.091(5) Uani 1 1 d . . . H31D H -0.0031 -0.0088 0.0560 0.110 Uiso 1 1 calc R . . C312 C 0.1708(7) 0.0309(4) 0.1193(4) 0.064(3) Uani 1 1 d . . . H31E H 0.2223 0.0279 0.1141 0.077 Uiso 1 1 calc R . . C304 C 0.4489(9) -0.0242(8) 0.2400(5) 0.090(4) Uani 1 1 d . . . H30C H 0.4933 -0.0521 0.2468 0.107 Uiso 1 1 calc R . . C103 C 0.3998(8) 0.0993(6) 0.0782(5) 0.092(4) Uani 1 1 d . . . H10D H 0.4522 0.0891 0.0926 0.110 Uiso 1 1 calc R . . C306 C 0.3122(7) -0.0168(5) 0.2210(4) 0.070(3) Uani 1 1 d . . . H30D H 0.2637 -0.0388 0.2133 0.084 Uiso 1 1 calc R . . C102 C 0.3625(7) 0.1507(5) 0.1040(4) 0.068(3) Uani 1 1 d . . . H10E H 0.3897 0.1751 0.1361 0.082 Uiso 1 1 calc R . . C403 C 0.4734(6) 0.2562(5) 0.4294(4) 0.064(3) Uani 1 1 d . . . H40E H 0.5232 0.2652 0.4509 0.077 Uiso 1 1 calc R . . C303 C 0.4585(8) 0.0488(8) 0.2404(4) 0.091(4) Uani 1 1 d . . . H30E H 0.5076 0.0696 0.2460 0.109 Uiso 1 1 calc R . . F24 F 0.2657(5) 0.5964(3) 0.4485(3) 0.106(2) Uani 1 1 d . . . F23 F 0.1766(6) 0.6490(4) 0.3829(3) 0.133(3) Uani 1 1 d . . . F14 F 0.5520(6) 0.7526(4) 0.2871(4) 0.128(3) Uani 1 1 d . . . F22 F 0.1430(5) 0.6093(4) 0.4630(5) 0.162(4) Uani 1 1 d . . . F21 F 0.1719(4) 0.5343(4) 0.3950(5) 0.165(5) Uani 1 1 d . . . F13 F 0.4399(7) 0.7820(5) 0.2367(4) 0.172(4) Uani 1 1 d . . . C9S C 0.1083(12) 0.6211(7) 0.2368(5) 0.089(5) Uani 1 1 d . . . F12 F 0.4625(7) 0.7992(7) 0.3316(5) 0.207(6) Uani 1 1 d . . . F11 F 0.4502(6) 0.6942(5) 0.2977(8) 0.232(7) Uani 1 1 d . . . B2 B 0.1880(10) 0.5969(8) 0.4218(9) 0.088(5) Uani 1 1 d . . . C10S C 0.1901(11) 0.6042(9) 0.2418(6) 0.143(6) Uani 1 1 d . . . H10F H 0.2201 0.6463 0.2443 0.215 Uiso 1 1 calc R . . H10G H 0.1973 0.5783 0.2079 0.215 Uiso 1 1 calc R . . H10H H 0.2073 0.5769 0.2765 0.215 Uiso 1 1 calc R . . N5S N 0.0468(10) 0.6308(7) 0.2318(6) 0.126(6) Uani 1 1 d . . . B1 B 0.4780(14) 0.7543(10) 0.2875(8) 0.113(6) Uani 1 1 d . . . C8S C 0.4484(8) -0.0935(8) -0.0024(8) 0.140(6) Uani 1 1 d . . . H8SA H 0.4737 -0.1185 0.0319 0.210 Uiso 1 1 calc R . . H8SB H 0.4049 -0.0678 0.0066 0.210 Uiso 1 1 calc R . . H8SC H 0.4850 -0.0619 -0.0144 0.210 Uiso 1 1 calc R . . N4S N 0.3968(9) -0.1815(9) -0.0778(8) 0.202(8) Uani 1 1 d . . . C7S C 0.4219(12) -0.140(2) -0.0472(12) 0.27(2) Uani 1 1 d . . . C4S C -0.3014(9) 0.3756(8) 0.4104(6) 0.134(5) Uani 1 1 d . . . H4S1 H -0.2726 0.3776 0.4500 0.202 Uiso 1 1 calc R . . H4S2 H -0.3493 0.4012 0.4075 0.202 Uiso 1 1 calc R . . H4S3 H -0.2707 0.3954 0.3844 0.202 Uiso 1 1 calc R . . C5S C -0.2039(11) 0.3121(8) 0.2468(10) 0.170(7) Uani 1 1 d . . . C6S C -0.2687(11) 0.2752(11) 0.2013(14) 0.37(2) Uani 1 1 d . . . H6SA H -0.3054 0.2532 0.2215 0.553 Uiso 1 1 calc R . . H6SB H -0.2452 0.2407 0.1803 0.553 Uiso 1 1 calc R . . H6SC H -0.2954 0.3088 0.1741 0.553 Uiso 1 1 calc R . . N3S N -0.1589(9) 0.3427(17) 0.2788(14) 0.39(2) Uani 1 1 d . . . N2S N -0.3398(11) 0.2682(12) 0.3910(8) 0.227(8) Uani 1 1 d . . . C3S C -0.3142(17) 0.3240(12) 0.3988(12) 0.309(16) 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 Co1 0.0631(8) 0.0293(6) 0.0326(6) 0.0004(5) 0.0162(5) 0.0050(5) S6 0.0545(14) 0.0292(10) 0.0346(11) 0.0002(8) 0.0133(10) 0.0052(9) S5 0.0587(14) 0.0307(11) 0.0342(11) -0.0021(9) 0.0111(10) 0.0009(9) P3 0.0735(17) 0.0294(11) 0.0303(11) -0.0005(9) 0.0156(11) 0.0086(11) P1 0.0647(15) 0.0313(12) 0.0333(11) -0.0005(9) 0.0183(11) 0.0039(10) P2 0.0563(14) 0.0295(11) 0.0322(11) -0.0015(9) 0.0149(10) 0.0032(10) P4 0.0726(16) 0.0275(11) 0.0321(11) -0.0011(9) 0.0168(11) 0.0040(10) S8 0.0600(14) 0.0347(11) 0.0366(11) -0.0013(9) 0.0134(10) 0.0034(10) S2 0.0527(14) 0.0459(13) 0.0390(12) 0.0003(10) 0.0167(10) -0.0045(10) S1 0.0631(15) 0.0483(13) 0.0398(12) -0.0001(10) 0.0238(11) 0.0042(11) S7 0.0650(15) 0.0319(11) 0.0376(11) -0.0004(9) 0.0094(10) 0.0035(10) S3 0.0487(14) 0.0698(16) 0.0376(12) 0.0031(11) 0.0135(10) -0.0091(11) S4 0.0554(15) 0.0578(15) 0.0493(14) 0.0038(11) 0.0114(11) -0.0152(11) N1S 0.072(5) 0.030(4) 0.032(4) 0.001(3) 0.017(4) 0.000(4) C111 0.066(6) 0.033(4) 0.036(5) -0.003(4) 0.023(4) -0.003(4) C401 0.082(7) 0.032(5) 0.035(5) 0.006(4) 0.019(5) 0.002(4) C101 0.098(8) 0.038(5) 0.034(5) 0.009(4) 0.029(5) 0.013(5) C411 0.086(7) 0.021(4) 0.035(5) 0.000(3) 0.022(5) 0.005(4) C1 0.053(5) 0.040(5) 0.041(5) 0.005(4) 0.018(4) 0.008(4) C11 0.060(6) 0.033(4) 0.032(4) 0.004(3) 0.017(4) 0.005(4) C10 0.057(6) 0.031(4) 0.041(5) 0.009(4) 0.016(4) 0.006(4) C2 0.048(5) 0.034(4) 0.038(5) 0.003(4) 0.019(4) 0.005(4) C201 0.051(6) 0.040(5) 0.042(5) -0.001(4) 0.019(4) -0.006(4) C212 0.054(6) 0.036(5) 0.048(5) 0.007(4) 0.019(4) 0.000(4) C16 0.106(8) 0.049(6) 0.036(5) 0.011(4) 0.015(5) 0.021(5) C106 0.104(8) 0.037(5) 0.039(5) -0.003(4) 0.032(5) -0.003(5) C14 0.067(6) 0.041(5) 0.045(5) 0.015(4) 0.022(5) 0.009(4) C3 0.037(5) 0.055(5) 0.040(5) -0.003(4) 0.008(4) 0.003(4) C12 0.042(5) 0.033(4) 0.042(5) -0.004(4) 0.010(4) 0.003(4) C15 0.094(8) 0.039(5) 0.048(5) 0.014(4) 0.025(5) 0.011(5) C117 0.039(5) 0.034(4) 0.039(4) -0.011(4) 0.010(4) 0.001(3) C1S 0.084(8) 0.029(5) 0.033(5) 0.007(4) 0.020(5) -0.001(5) C311 0.089(8) 0.022(4) 0.041(5) 0.006(4) 0.013(5) 0.009(4) C413 0.134(11) 0.027(5) 0.046(6) 0.003(4) 0.037(6) 0.022(6) C211 0.049(5) 0.027(4) 0.045(5) -0.004(4) 0.015(4) -0.001(4) C116 0.071(6) 0.033(5) 0.040(5) 0.001(4) 0.015(5) -0.006(4) C112 0.067(7) 0.040(5) 0.045(5) 0.008(4) 0.016(5) -0.012(4) C406 0.080(7) 0.048(5) 0.041(5) -0.007(4) 0.029(5) -0.022(5) C215 0.057(6) 0.043(5) 0.053(5) 0.002(4) 0.025(5) 0.003(4) C415 0.084(7) 0.040(5) 0.046(5) 0.005(4) 0.030(5) 0.021(5) C13 0.073(6) 0.033(5) 0.042(5) 0.009(4) 0.017(5) 0.006(4) C204 0.072(7) 0.079(7) 0.048(6) -0.017(5) 0.028(5) -0.033(6) C206 0.076(7) 0.045(5) 0.056(6) -0.022(5) 0.033(5) -0.015(5) C216 0.061(6) 0.036(5) 0.048(5) 0.006(4) 0.028(5) 0.002(4) C214 0.046(5) 0.038(5) 0.064(6) 0.004(4) 0.010(5) 0.005(4) C203 0.066(7) 0.082(7) 0.044(5) 0.014(5) 0.022(5) -0.015(6) C213 0.058(6) 0.046(5) 0.048(5) 0.013(4) 0.019(5) 0.003(4) C205 0.095(9) 0.060(6) 0.059(7) -0.019(5) 0.040(6) -0.024(6) C416 0.097(8) 0.034(5) 0.036(5) 0.004(4) 0.019(5) 0.016(5) C301 0.086(8) 0.059(6) 0.034(5) 0.001(4) 0.026(5) 0.020(6) C115 0.077(7) 0.051(6) 0.039(5) -0.001(4) 0.018(5) -0.012(5) C5 0.039(5) 0.081(7) 0.040(5) 0.017(5) 0.005(4) -0.010(5) C6 0.041(5) 0.066(6) 0.057(6) 0.019(5) 0.002(5) -0.013(5) C4 0.037(5) 0.057(5) 0.039(5) 0.005(4) 0.010(4) -0.005(4) C407 0.096(8) 0.060(6) 0.038(5) 0.000(5) 0.018(6) -0.027(6) C2S 0.060(6) 0.058(6) 0.058(6) 0.015(5) 0.011(5) 0.005(5) C316 0.086(8) 0.028(5) 0.043(5) 0.004(4) -0.003(5) -0.007(5) C114 0.056(6) 0.062(6) 0.049(6) 0.002(5) 0.014(5) -0.008(5) C202 0.064(6) 0.055(6) 0.035(5) -0.002(4) 0.020(5) -0.013(5) C105 0.129(11) 0.048(6) 0.056(7) -0.002(5) 0.044(7) 0.017(6) C104 0.177(14) 0.048(6) 0.055(7) 0.011(5) 0.055(8) 0.032(8) C8 0.079(8) 0.079(7) 0.066(7) 0.017(6) 0.004(6) -0.032(6) C302 0.089(8) 0.067(7) 0.045(6) 0.000(5) 0.031(6) 0.023(6) C7 0.056(6) 0.117(9) 0.037(5) 0.020(5) 0.002(5) -0.022(6) C113 0.069(7) 0.061(6) 0.043(5) 0.019(5) 0.005(5) -0.004(5) C405 0.078(7) 0.063(6) 0.037(5) 0.000(4) 0.007(5) 0.013(5) C315 0.112(9) 0.048(6) 0.051(6) 0.020(5) -0.010(6) -0.024(6) C305 0.149(13) 0.095(10) 0.051(7) 0.014(7) 0.037(8) 0.058(10) C412 0.091(8) 0.033(5) 0.044(5) 0.002(4) 0.022(5) 0.005(5) C404 0.084(8) 0.078(7) 0.047(6) 0.003(5) 0.017(6) 0.009(6) C313 0.147(12) 0.047(6) 0.036(6) 0.004(5) 0.020(7) -0.025(7) C414 0.087(8) 0.056(7) 0.058(6) 0.006(5) 0.033(6) 0.027(6) C314 0.170(14) 0.049(7) 0.037(6) 0.018(5) -0.026(8) -0.050(8) C312 0.120(9) 0.032(5) 0.038(5) 0.005(4) 0.012(6) -0.002(5) C304 0.114(11) 0.117(12) 0.040(6) -0.002(7) 0.021(7) 0.074(9) C103 0.137(11) 0.087(8) 0.057(7) 0.005(6) 0.030(7) 0.066(8) C306 0.119(9) 0.050(6) 0.049(6) 0.009(5) 0.039(6) 0.038(6) C102 0.097(9) 0.068(7) 0.043(6) 0.010(5) 0.023(6) 0.039(6) C403 0.071(7) 0.062(6) 0.060(7) 0.010(5) 0.013(6) -0.009(5) C303 0.102(9) 0.126(12) 0.048(6) -0.015(7) 0.026(6) 0.030(9) F24 0.122(6) 0.082(5) 0.118(6) -0.005(4) 0.038(5) 0.002(4) F23 0.232(10) 0.077(5) 0.085(5) -0.007(4) 0.015(6) 0.029(5) F14 0.186(9) 0.112(6) 0.113(6) 0.037(5) 0.097(6) 0.026(6) F22 0.154(8) 0.115(7) 0.258(12) -0.007(7) 0.140(8) 0.018(5) F21 0.107(6) 0.059(4) 0.340(15) -0.064(6) 0.072(7) -0.003(4) F13 0.236(12) 0.146(8) 0.137(8) 0.007(7) 0.040(8) 0.076(8) C9S 0.162(16) 0.057(7) 0.042(6) 0.019(5) 0.009(10) 0.039(10) F12 0.211(12) 0.270(15) 0.175(10) -0.057(10) 0.125(9) 0.012(10) F11 0.165(10) 0.102(7) 0.43(2) 0.075(10) 0.070(11) -0.025(7) B2 0.080(11) 0.064(10) 0.130(14) -0.016(10) 0.044(10) 0.004(8) C10S 0.197(18) 0.173(17) 0.064(9) 0.011(10) 0.036(11) 0.034(15) N5S 0.203(17) 0.079(9) 0.087(9) -0.008(6) 0.004(11) 0.041(10) B1 0.161(19) 0.103(14) 0.089(13) 0.059(11) 0.058(13) 0.040(13) C8S 0.069(9) 0.144(11) 0.221(17) 0.124(12) 0.060(10) 0.050(8) N4S 0.128(12) 0.222(14) 0.231(16) -0.132(12) -0.025(10) 0.053(10) C7S 0.110(15) 0.50(6) 0.19(3) 0.19(3) 0.005(17) 0.04(3) C4S 0.171(14) 0.131(11) 0.108(10) 0.034(9) 0.045(9) 0.044(10) C5S 0.090(11) 0.116(11) 0.30(2) 0.022(13) 0.029(14) 0.010(9) C6S 0.126(17) 0.26(2) 0.74(6) 0.33(3) 0.13(3) 0.029(15) N3S 0.083(10) 0.54(4) 0.51(4) 0.33(3) -0.053(15) -0.011(15) N2S 0.192(16) 0.25(2) 0.198(16) 0.010(15) -0.054(12) 0.049(15) C3S 0.44(3) 0.092(15) 0.30(2) -0.037(17) -0.18(2) -0.014(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1S 1.988(9) . ? Co1 P3 2.278(2) . ? Co1 P4 2.280(2) . ? Co1 P2 2.302(2) . ? Co1 P1 2.303(2) . ? S6 C10 1.746(8) . ? S6 C117 1.776(7) . ? S5 C11 1.754(8) . ? S5 C117 1.763(8) . ? P3 C11 1.801(8) . ? P3 C301 1.802(10) . ? P3 C311 1.801(10) . ? P1 C1 1.819(8) . ? P1 C111 1.819(9) . ? P1 C101 1.826(9) . ? P2 C2 1.795(8) . ? P2 C211 1.803(8) . ? P2 C201 1.832(8) . ? P4 C401 1.803(10) . ? P4 C411 1.809(9) . ? P4 C10 1.812(8) . ? S8 C12 1.760(8) . ? S8 C14 1.769(8) . ? S2 C3 1.766(8) . ? S2 C2 1.768(8) . ? S1 C1 1.741(8) . ? S1 C3 1.765(9) . ? S7 C12 1.740(8) . ? S7 C13 1.762(8) . ? S3 C4 1.748(8) . ? S3 C5 1.759(10) . ? S4 C4 1.746(9) . ? S4 C6 1.762(9) . ? N1S C1S 1.162(11) . ? C111 C116 1.374(11) . ? C111 C112 1.396(11) . ? C401 C405 1.379(12) . ? C401 C406 1.394(11) . ? C101 C102 1.374(13) . ? C101 C106 1.407(12) . ? C411 C416 1.386(12) . ? C411 C412 1.400(11) . ? C1 C2 1.331(11) . ? C11 C10 1.336(10) . ? C201 C206 1.385(11) . ? C201 C202 1.387(12) . ? C212 C211 1.383(11) . ? C212 C213 1.389(11) . ? C16 C14 1.514(11) . ? C106 C105 1.371(12) . ? C14 C13 1.322(11) . ? C3 C4 1.338(11) . ? C12 C117 1.326(10) . ? C15 C13 1.501(11) . ? C1S C2S 1.441(14) . ? C311 C316 1.376(12) . ? C311 C312 1.404(12) . ? C413 C414 1.358(14) . ? C413 C412 1.413(13) . ? C211 C216 1.407(10) . ? C116 C115 1.383(12) . ? C112 C113 1.389(12) . ? C406 C407 1.374(13) . ? C215 C216 1.370(11) . ? C215 C214 1.383(12) . ? C415 C414 1.385(13) . ? C415 C416 1.388(12) . ? C204 C205 1.354(14) . ? C204 C203 1.395(13) . ? C206 C205 1.402(13) . ? C214 C213 1.387(11) . ? C203 C202 1.375(12) . ? C301 C302 1.377(13) . ? C301 C306 1.409(13) . ? C115 C114 1.381(12) . ? C5 C6 1.314(13) . ? C5 C7 1.504(12) . ? C6 C8 1.495(13) . ? C407 C403 1.379(13) . ? C316 C315 1.394(13) . ? C114 C113 1.363(12) . ? C105 C104 1.342(16) . ? C104 C103 1.402(17) . ? C302 C303 1.410(15) . ? C405 C404 1.381(13) . ? C315 C314 1.406(17) . ? C305 C304 1.332(17) . ? C305 C306 1.353(15) . ? C404 C403 1.389(14) . ? C313 C312 1.357(15) . ? C313 C314 1.363(17) . ? C304 C303 1.415(18) . ? C103 C102 1.380(13) . ? F24 B2 1.376(17) . ? F23 B2 1.337(18) . ? F14 B1 1.29(2) . ? F22 B2 1.368(16) . ? F21 B2 1.360(16) . ? F13 B1 1.348(18) . ? C9S N5S 1.071(19) . ? C9S C10S 1.44(2) . ? F12 B1 1.40(2) . ? F11 B1 1.29(2) . ? C8S C7S 1.38(4) . ? N4S C7S 1.10(4) . ? C4S C3S 1.04(2) . ? C5S N3S 1.14(3) . ? C5S C6S 1.56(3) . ? N2S C3S 1.16(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 N1S Co1 P3 94.05(19) . . ? N1S Co1 P4 91.8(2) . . ? P3 Co1 P4 86.17(8) . . ? N1S Co1 P2 94.20(19) . . ? P3 Co1 P2 171.74(10) . . ? P4 Co1 P2 94.06(8) . . ? N1S Co1 P1 94.0(2) . . ? P3 Co1 P1 95.03(8) . . ? P4 Co1 P1 174.00(10) . . ? P2 Co1 P1 83.91(8) . . ? C10 S6 C117 94.1(4) . . ? C11 S5 C117 94.7(4) . . ? C11 P3 C301 101.4(4) . . ? C11 P3 C311 102.6(4) . . ? C301 P3 C311 105.6(5) . . ? C11 P3 Co1 105.7(3) . . ? C301 P3 Co1 123.0(4) . . ? C311 P3 Co1 115.7(3) . . ? C1 P1 C111 105.7(4) . . ? C1 P1 C101 102.5(4) . . ? C111 P1 C101 104.1(4) . . ? C1 P1 Co1 103.6(3) . . ? C111 P1 Co1 114.8(3) . . ? C101 P1 Co1 124.1(3) . . ? C2 P2 C211 103.9(4) . . ? C2 P2 C201 102.0(4) . . ? C211 P2 C201 106.9(4) . . ? C2 P2 Co1 104.1(3) . . ? C211 P2 Co1 115.6(3) . . ? C201 P2 Co1 122.0(3) . . ? C401 P4 C411 109.3(4) . . ? C401 P4 C10 104.5(4) . . ? C411 P4 C10 101.2(4) . . ? C401 P4 Co1 117.3(3) . . ? C411 P4 Co1 116.7(3) . . ? C10 P4 Co1 105.6(3) . . ? C12 S8 C14 95.3(4) . . ? C3 S2 C2 93.7(4) . . ? C1 S1 C3 93.4(4) . . ? C12 S7 C13 96.2(4) . . ? C4 S3 C5 95.2(4) . . ? C4 S4 C6 95.5(4) . . ? C1S N1S Co1 170.8(7) . . ? C116 C111 C112 118.6(8) . . ? C116 C111 P1 119.3(6) . . ? C112 C111 P1 122.1(7) . . ? C405 C401 C406 118.3(9) . . ? C405 C401 P4 117.0(7) . . ? C406 C401 P4 124.7(8) . . ? C102 C101 C106 119.3(9) . . ? C102 C101 P1 118.9(7) . . ? C106 C101 P1 121.8(8) . . ? C416 C411 C412 119.2(8) . . ? C416 C411 P4 117.3(6) . . ? C412 C411 P4 123.3(8) . . ? C2 C1 S1 119.1(6) . . ? C2 C1 P1 118.3(6) . . ? S1 C1 P1 122.6(5) . . ? C10 C11 S5 116.9(6) . . ? C10 C11 P3 119.9(6) . . ? S5 C11 P3 123.2(4) . . ? C11 C10 S6 118.4(6) . . ? C11 C10 P4 119.0(6) . . ? S6 C10 P4 122.6(5) . . ? C1 C2 S2 116.2(6) . . ? C1 C2 P2 119.5(6) . . ? S2 C2 P2 124.3(4) . . ? C206 C201 C202 120.3(8) . . ? C206 C201 P2 122.5(7) . . ? C202 C201 P2 117.3(6) . . ? C211 C212 C213 121.1(8) . . ? C105 C106 C101 120.5(11) . . ? C13 C14 C16 128.0(7) . . ? C13 C14 S8 117.3(6) . . ? C16 C14 S8 114.6(6) . . ? C4 C3 S1 121.5(6) . . ? C4 C3 S2 124.7(7) . . ? S1 C3 S2 113.8(5) . . ? C117 C12 S7 122.9(6) . . ? C117 C12 S8 123.4(6) . . ? S7 C12 S8 113.7(4) . . ? C12 C117 S5 122.2(6) . . ? C12 C117 S6 124.2(6) . . ? S5 C117 S6 113.5(4) . . ? N1S C1S C2S 179.5(10) . . ? C316 C311 C312 119.5(9) . . ? C316 C311 P3 119.1(7) . . ? C312 C311 P3 121.1(8) . . ? C414 C413 C412 121.7(9) . . ? C212 C211 C216 118.0(8) . . ? C212 C211 P2 121.9(6) . . ? C216 C211 P2 120.1(6) . . ? C111 C116 C115 120.7(8) . . ? C113 C112 C111 120.5(8) . . ? C407 C406 C401 120.1(9) . . ? C216 C215 C214 120.2(8) . . ? C414 C415 C416 119.1(10) . . ? C14 C13 C15 129.0(8) . . ? C14 C13 S7 116.9(6) . . ? C15 C13 S7 114.2(6) . . ? C205 C204 C203 119.4(9) . . ? C201 C206 C205 118.0(9) . . ? C215 C216 C211 121.1(8) . . ? C213 C214 C215 119.8(8) . . ? C202 C203 C204 119.8(10) . . ? C214 C213 C212 119.8(8) . . ? C204 C205 C206 122.1(10) . . ? C411 C416 C415 121.6(8) . . ? C302 C301 C306 119.6(10) . . ? C302 C301 P3 120.7(8) . . ? C306 C301 P3 119.4(9) . . ? C116 C115 C114 120.1(9) . . ? C6 C5 C7 127.9(9) . . ? C6 C5 S3 117.7(7) . . ? C7 C5 S3 114.4(8) . . ? C5 C6 C8 126.3(9) . . ? C5 C6 S4 116.9(7) . . ? C8 C6 S4 116.8(8) . . ? C3 C4 S3 122.2(7) . . ? C3 C4 S4 123.9(7) . . ? S3 C4 S4 113.9(5) . . ? C406 C407 C403 120.7(9) . . ? C311 C316 C315 120.5(10) . . ? C113 C114 C115 120.2(9) . . ? C203 C202 C201 120.5(9) . . ? C104 C105 C106 119.5(11) . . ? C105 C104 C103 121.6(11) . . ? C301 C302 C303 121.1(11) . . ? C114 C113 C112 119.8(9) . . ? C401 C405 C404 122.3(9) . . ? C314 C315 C316 118.1(12) . . ? C304 C305 C306 121.4(14) . . ? C411 C412 C413 118.2(10) . . ? C403 C404 C405 118.2(10) . . ? C312 C313 C314 120.3(11) . . ? C413 C414 C415 120.1(9) . . ? C313 C314 C315 121.2(11) . . ? C313 C312 C311 120.4(11) . . ? C305 C304 C303 122.7(12) . . ? C102 C103 C104 119.0(12) . . ? C305 C306 C301 119.3(13) . . ? C101 C102 C103 120.0(11) . . ? C407 C403 C404 120.2(10) . . ? C302 C303 C304 115.8(12) . . ? N5S C9S C10S 176.8(19) . . ? F23 B2 F21 111.4(15) . . ? F23 B2 F22 108.1(12) . . ? F21 B2 F22 112.2(13) . . ? F23 B2 F24 108.3(12) . . ? F21 B2 F24 107.3(11) . . ? F22 B2 F24 109.5(15) . . ? F14 B1 F11 112.8(16) . . ? F14 B1 F13 109.2(15) . . ? F11 B1 F13 112(2) . . ? F14 B1 F12 110.7(19) . . ? F11 B1 F12 106.6(15) . . ? F13 B1 F12 105.3(15) . . ? N4S C7S C8S 171(3) . . ? N3S C5S C6S 176(2) . . ? C4S C3S N2S 167(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.828 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.188 # Attachment 'er043_1.txt' data_er043_1 _database_code_depnum_ccdc_archive 'CCDC 615880' _audit_creation_method ; SHELXL-97, PLATON,and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and AgSbF6 produced the the complex [Ag(o-P2)2][SbF6] where the silver metal center displayed distorted tetrahedral geometry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H52 Ag P4 S8), 2(F6 Sb), 11(C2 H3 N)' _chemical_formula_sum 'C150 H137 Ag2 F12 N11 P8 S16 Sb2' _chemical_formula_weight 3541.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.5270(11) _cell_length_b 20.6653(15) _cell_length_c 24.6469(18) _cell_angle_alpha 83.414(4) _cell_angle_beta 87.686(4) _cell_angle_gamma 72.710(4) _cell_volume 7984.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red-orange _exptl_crystal_size_max .27 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3588 _exptl_absorpt_coefficient_mu 7.849 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.240 _exptl_absorpt_correction_T_max 0.534 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 on GADDS' _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 37903 _diffrn_reflns_av_R_equivalents 0.1354 _diffrn_reflns_av_sigmaI/netI 0.2484 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 55.57 _reflns_number_total 19495 _reflns_number_gt 12146 _reflns_threshold_expression I>2s(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.0802P)^2^+0.0000P] 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 19495 _refine_ls_number_parameters 1769 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1812 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.86434(7) 0.23496(6) 0.26043(5) 0.0297(4) Uani 1 1 d . . . Ag2 Ag 0.18786(7) 0.62875(6) 0.23737(5) 0.0313(4) Uani 1 1 d . . . Sb2 Sb 0.42168(7) 0.92711(7) 0.38343(5) 0.0514(4) Uani 1 1 d . . . P3 P 1.0030(2) 0.1977(2) 0.21072(18) 0.0310(12) Uani 1 1 d . . . S1 S 0.7199(2) 0.4752(2) 0.30840(17) 0.0327(12) Uani 1 1 d . . . S2 S 0.8294(2) 0.4044(2) 0.40186(17) 0.0323(12) Uani 1 1 d . . . S10 S -0.0846(2) 0.8159(2) 0.18199(17) 0.0382(13) Uani 1 1 d . . . P7 P 0.3470(2) 0.6040(2) 0.24408(18) 0.0303(12) Uani 1 1 d . . . S13 S 0.3557(2) 0.4337(2) 0.37153(17) 0.0353(12) Uani 1 1 d . . . S16 S 0.5920(2) 0.4492(2) 0.43653(18) 0.0363(12) Uani 1 1 d . . . S15 S 0.4722(2) 0.3765(2) 0.48041(18) 0.0372(12) Uani 1 1 d . . . S3 S 0.6794(3) 0.6169(2) 0.36022(18) 0.0409(13) Uani 1 1 d . . . S14 S 0.4751(2) 0.5088(2) 0.32831(17) 0.0345(12) Uani 1 1 d . . . P4 P 0.8463(2) 0.1242(2) 0.23815(19) 0.0339(13) Uani 1 1 d . . . S11 S -0.2541(2) 0.9067(2) 0.11063(18) 0.0417(13) Uani 1 1 d . . . S6 S 1.0838(2) 0.0792(2) 0.14132(18) 0.0362(12) Uani 1 1 d . . . P2 P 0.8690(2) 0.2631(2) 0.35779(17) 0.0277(12) Uani 1 1 d . . . P1 P 0.7483(2) 0.3458(2) 0.25121(18) 0.0287(12) Uani 1 1 d . . . S9 S -0.0160(2) 0.7502(2) 0.08299(17) 0.0359(12) Uani 1 1 d . . . P8 P 0.2158(2) 0.5149(2) 0.28833(18) 0.0317(12) Uani 1 1 d . . . P6 P 0.1508(2) 0.6637(2) 0.13958(18) 0.0325(13) Uani 1 1 d . . . P5 P 0.0708(2) 0.7327(2) 0.25249(18) 0.0319(13) Uani 1 1 d . . . S7 S 1.0242(3) -0.0826(2) 0.06517(18) 0.0402(13) Uani 1 1 d . . . S4 S 0.7829(2) 0.5494(2) 0.45615(18) 0.0396(13) Uani 1 1 d . . . S8 S 1.1574(3) -0.0156(2) 0.04597(19) 0.0433(13) Uani 1 1 d . . . S12 S -0.1795(3) 0.8365(2) 0.01531(19) 0.0463(14) Uani 1 1 d . . . S5 S 0.9459(3) 0.0159(2) 0.16395(19) 0.0421(13) Uani 1 1 d . . . F10 F 0.4205(7) 1.0148(6) 0.3686(6) 0.113(5) Uani 1 1 d . . . C73 C 0.3732(8) 0.5353(7) 0.2999(6) 0.020(4) Uani 1 1 d . . . C9 C 0.9985(9) 0.1197(8) 0.1826(6) 0.023(4) Uiso 1 1 d . . . C77 C 0.5510(9) 0.3798(8) 0.5245(6) 0.026(4) Uani 1 1 d . . . C6 C 0.7298(10) 0.6363(8) 0.4550(6) 0.030(4) Uani 1 1 d . . . C22 C 0.5934(9) 0.3316(8) 0.2242(7) 0.032(5) Uani 1 1 d . . . H24 H 0.6104 0.3400 0.1875 0.038 Uiso 1 1 calc R . . C120 C 0.0844(13) 0.5345(11) 0.4316(8) 0.068(7) Uani 1 1 d . . . H93 H 0.0841 0.5571 0.4631 0.081 Uiso 1 1 calc R . . F12 F 0.4187(8) 0.8360(5) 0.3981(5) 0.112(5) Uani 1 1 d . . . F11 F 0.5236(7) 0.8925(6) 0.3492(6) 0.132(6) Uani 1 1 d . . . C5 C 0.6800(10) 0.6682(8) 0.4113(7) 0.031(4) Uani 1 1 d . . . N2 N 0.6533(10) 0.7636(8) 0.6224(7) 0.063(5) Uani 1 1 d . . . N11 N -0.0028(11) 0.5833(9) 0.2104(8) 0.075(6) Uani 1 1 d . . . C74 C 0.3177(9) 0.4999(8) 0.3192(6) 0.027(5) Uani 1 1 d . . . C18 C 0.6185(9) 0.3226(7) 0.3211(7) 0.030(5) Uani 1 1 d . . . H20 H 0.6519 0.3256 0.3507 0.036 Uiso 1 1 calc R . . C104 C 0.4060(10) 0.6630(8) 0.2565(6) 0.026(4) Uiso 1 1 d . . . C57 C 0.6323(12) 0.1866(11) 0.1455(8) 0.071(7) Uani 1 1 d . . . H53 H 0.5993 0.2288 0.1274 0.085 Uiso 1 1 calc R . . C59 C 0.8625(11) 0.0551(8) 0.2922(6) 0.033(5) Uani 1 1 d . . . C14 C 1.0849(10) -0.0980(8) 0.0059(7) 0.035(5) Uani 1 1 d . . . C101 C 0.3103(10) 0.7993(10) 0.0623(10) 0.053(6) Uani 1 1 d . . . H77 H 0.3452 0.8264 0.0478 0.064 Uiso 1 1 calc R . . C116 C 0.1463(9) 0.5043(8) 0.3456(6) 0.022(4) Uiso 1 1 d . . . N4 N 0.9635(12) 0.4055(13) 0.2574(7) 0.099(9) Uani 1 1 d . . . C24 C 0.6557(8) 0.4685(8) 0.1897(6) 0.024(4) Uani 1 1 d . . . H25 H 0.6094 0.4694 0.2140 0.029 Uiso 1 1 calc R . . C21 C 0.5154(10) 0.3161(9) 0.2358(8) 0.042(5) Uani 1 1 d . . . H23 H 0.4794 0.3152 0.2070 0.051 Uiso 1 1 calc R . . C113 C 0.4528(9) 0.5115(11) 0.0857(8) 0.041(5) Uani 1 1 d . . . H87 H 0.4691 0.4936 0.0517 0.049 Uiso 1 1 calc R . . C70 C -0.3118(9) 0.9309(8) 0.0491(7) 0.031(5) Uani 1 1 d . . . C122 C 0.2331(8) 0.4405(8) 0.2509(7) 0.019(4) Uani 1 1 d . . . C4 C 0.7442(8) 0.5417(8) 0.3931(6) 0.025(4) Uani 1 1 d . . . C112 C 0.4424(8) 0.5802(11) 0.0912(7) 0.041(5) Uani 1 1 d . . . H86 H 0.4534 0.6096 0.0611 0.049 Uiso 1 1 calc R . . C114 C 0.4391(10) 0.4711(9) 0.1303(8) 0.036(5) Uani 1 1 d . . . H88 H 0.4487 0.4239 0.1277 0.043 Uiso 1 1 calc R . . C110 C 0.3985(8) 0.5649(8) 0.1850(6) 0.021(4) Uiso 1 1 d . . . C12 C 1.0675(10) -0.0228(8) 0.0834(7) 0.030(5) Uani 1 1 d . . . C26 C 0.7147(12) 0.5187(8) 0.1135(7) 0.042(5) Uani 1 1 d . . . H27 H 0.7083 0.5544 0.0846 0.051 Uiso 1 1 calc R . . C96 C 0.1565(11) 0.4978(8) 0.0281(7) 0.040(5) Uani 1 1 d . . . H72 H 0.1588 0.4628 0.0057 0.048 Uiso 1 1 calc R . . F8 F 0.3660(8) 0.9347(6) 0.3204(6) 0.135(6) Uani 1 1 d . . . C69 C -0.2770(9) 0.9003(8) 0.0068(7) 0.029(5) Uani 1 1 d . . . C72 C -0.3939(9) 0.9866(9) 0.0510(7) 0.053(6) Uani 1 1 d . . . H17A H -0.4164 1.0013 0.0140 0.079 Uiso 1 1 calc R . . H17B H -0.3843 1.0254 0.0664 0.079 Uiso 1 1 calc R . . H17C H -0.4347 0.9697 0.0739 0.079 Uiso 1 1 calc R . . C67 C -0.1001(9) 0.8127(8) 0.1138(7) 0.034(5) Uani 1 1 d . . . C91 C 0.1714(12) 0.8587(15) 0.3208(11) 0.081(9) Uani 1 1 d . . . H68 H 0.1904 0.8614 0.3561 0.097 Uiso 1 1 calc R . . C78 C 0.6048(10) 0.4156(8) 0.5045(7) 0.034(5) Uani 1 1 d . . . C60 C 0.7920(12) 0.0465(9) 0.3225(7) 0.041(5) Uani 1 1 d . . . H55 H 0.7363 0.0728 0.3118 0.049 Uiso 1 1 calc R . . C16 C 1.0668(10) -0.1456(7) -0.0291(6) 0.036(5) Uani 1 1 d . . . H15A H 1.0891 -0.1380 -0.0660 0.054 Uiso 1 1 calc R . . H15B H 1.0054 -0.1376 -0.0308 0.054 Uiso 1 1 calc R . . H15C H 1.0939 -0.1926 -0.0137 0.054 Uiso 1 1 calc R . . C50 C 0.2261(11) 0.5669(9) 0.0705(7) 0.045(5) Uani 1 1 d . . . H74 H 0.2762 0.5781 0.0773 0.054 Uiso 1 1 calc R . . C10 C 0.9377(9) 0.0914(8) 0.1925(6) 0.035(5) Uani 1 1 d . . . C40 C 0.7599(11) 0.1901(9) 0.3955(8) 0.052(6) Uani 1 1 d . . . H39 H 0.7673 0.1748 0.3602 0.062 Uiso 1 1 calc R . . C2 C 0.8178(9) 0.3551(8) 0.3508(7) 0.027(4) Uani 1 1 d . . . C64 C 0.9434(12) 0.0129(9) 0.3083(8) 0.054(6) Uani 1 1 d . . . H59 H 0.9922 0.0166 0.2880 0.065 Uiso 1 1 calc R . . C42 C 1.1283(12) 0.1025(11) 0.2765(8) 0.063(6) Uani 1 1 d . . . H44 H 1.1048 0.0687 0.2668 0.076 Uiso 1 1 calc R . . C68 C -0.1674(10) 0.8472(8) 0.0836(6) 0.033(5) Uani 1 1 d . . . C17 C 0.6447(8) 0.3346(7) 0.2671(7) 0.021(4) Uani 1 1 d . . . C118 C 0.0192(11) 0.4798(10) 0.3770(12) 0.069(7) Uani 1 1 d . . . H91 H -0.0275 0.4637 0.3707 0.083 Uiso 1 1 calc R . . C23 C 0.7317(9) 0.4131(8) 0.1961(6) 0.028(4) Uani 1 1 d . . . C35 C 0.8030(10) 0.2331(8) 0.4087(7) 0.033(5) Uiso 1 1 d . . . C95 C 0.0804(11) 0.5323(9) 0.0500(7) 0.042(5) Uani 1 1 d . . . H71 H 0.0313 0.5195 0.0436 0.051 Uiso 1 1 calc R . . C76 C 0.4990(8) 0.4304(7) 0.4271(6) 0.021(4) Uani 1 1 d . . . C80 C 0.6781(9) 0.4238(8) 0.5345(6) 0.037(5) Uani 1 1 d . . . H19A H 0.6750 0.4069 0.5731 0.056 Uiso 1 1 calc R . . H19B H 0.6754 0.4721 0.5313 0.056 Uiso 1 1 calc R . . H19C H 0.7315 0.3977 0.5186 0.056 Uiso 1 1 calc R . . C3 C 0.7603(8) 0.4824(9) 0.3713(6) 0.024(4) Uani 1 1 d . . . C126 C 0.2547(10) 0.3947(9) 0.1646(7) 0.038(5) Uani 1 1 d . . . H98 H 0.2560 0.4020 0.1259 0.046 Uiso 1 1 calc R . . C11 C 1.0375(9) 0.0169(8) 0.1231(8) 0.038(5) Uani 1 1 d . . . C115 C 0.4113(9) 0.4966(9) 0.1801(7) 0.036(5) Uani 1 1 d . . . H89 H 0.4013 0.4671 0.2104 0.044 Uiso 1 1 calc R . . C124 C 0.2773(9) 0.3175(10) 0.2461(8) 0.045(5) Uani 1 1 d . . . H96 H 0.2949 0.2722 0.2635 0.054 Uiso 1 1 calc R . . C66 C 0.0128(8) 0.7533(7) 0.1874(6) 0.022(4) Uani 1 1 d . . . C19 C 0.5441(9) 0.3064(8) 0.3311(7) 0.036(5) Uani 1 1 d . . . H21 H 0.5268 0.2977 0.3677 0.043 Uiso 1 1 calc R . . C75 C 0.4523(9) 0.4532(7) 0.3825(6) 0.025(4) Uiso 1 1 d . . . C29 C 0.9674(10) 0.2533(9) 0.3933(8) 0.044(5) Uani 1 1 d . . . C100 C 0.2932(11) 0.7928(9) 0.1172(9) 0.046(5) Uani 1 1 d . . . H76 H 0.3139 0.8173 0.1409 0.055 Uiso 1 1 calc R . . C90 C 0.1819(12) 0.9038(13) 0.2786(15) 0.084(11) Uani 1 1 d . . . H67 H 0.2102 0.9360 0.2851 0.101 Uiso 1 1 calc R . . C1 C 0.7681(9) 0.3889(8) 0.3090(6) 0.029(5) Uani 1 1 d . . . C30 C 1.0139(10) 0.2992(10) 0.3789(8) 0.054(6) Uani 1 1 d . . . H30 H 0.9960 0.3350 0.3501 0.065 Uiso 1 1 calc R . . C54 C 0.7302(10) 0.0642(9) 0.2001(7) 0.040(5) Uani 1 1 d . . . H50 H 0.7637 0.0219 0.2177 0.048 Uiso 1 1 calc R . . C31 C 1.0887(12) 0.2906(10) 0.4085(10) 0.081(8) Uani 1 1 d . . . H31 H 1.1193 0.3231 0.4020 0.098 Uiso 1 1 calc R . . N1 N 1.2753(10) 0.1420(9) 0.5386(8) 0.069(6) Uani 1 1 d . . . C34 C 0.9996(12) 0.1975(10) 0.4315(9) 0.082(8) Uani 1 1 d . . . H34 H 0.9675 0.1665 0.4406 0.098 Uiso 1 1 calc R . . C111 C 0.4163(9) 0.6043(8) 0.1399(7) 0.030(4) Uiso 1 1 d . . . H85 H 0.4101 0.6509 0.1430 0.036 Uiso 1 1 calc R . . C7 C 0.6310(10) 0.7409(8) 0.4019(7) 0.048(5) Uani 1 1 d . . . H13A H 0.6422 0.7652 0.4313 0.072 Uiso 1 1 calc R . . H13B H 0.5704 0.7452 0.4012 0.072 Uiso 1 1 calc R . . H13C H 0.6480 0.7608 0.3668 0.072 Uiso 1 1 calc R . . C32 C 1.1162(13) 0.2360(12) 0.4462(11) 0.111(11) Uani 1 1 d . . . H32 H 1.1654 0.2319 0.4666 0.133 Uiso 1 1 calc R . . C13 C 1.1482(10) -0.0683(8) -0.0017(7) 0.034(5) Uani 1 1 d . . . C65 C 0.0447(8) 0.7229(8) 0.1429(7) 0.028(4) Uani 1 1 d . . . C58 C 0.7063(11) 0.1826(10) 0.1746(7) 0.059(6) Uani 1 1 d . . . H54 H 0.7238 0.2224 0.1752 0.070 Uiso 1 1 calc R . . C61 C 0.8049(15) -0.0013(11) 0.3687(9) 0.067(7) Uani 1 1 d . . . H56 H 0.7572 -0.0071 0.3893 0.080 Uiso 1 1 calc R . . C41 C 1.0963(11) 0.1623(11) 0.2531(8) 0.051(6) Uani 1 1 d . . . C102 C 0.2758(10) 0.7657(10) 0.0284(7) 0.047(5) Uani 1 1 d . . . H78 H 0.2860 0.7706 -0.0099 0.056 Uiso 1 1 calc R . . C85 C -0.0946(13) 0.6760(9) 0.3591(8) 0.052(6) Uani 1 1 d . . . H63 H -0.1053 0.6343 0.3725 0.062 Uiso 1 1 calc R . . C47 C 1.0325(11) 0.2442(8) 0.1507(6) 0.036(5) Uani 1 1 d . . . C125 C 0.2750(10) 0.3298(9) 0.1903(7) 0.039(5) Uiso 1 1 d . . . H97 H 0.2879 0.2925 0.1690 0.047 Uiso 1 1 calc R . . C33 C 1.0759(13) 0.1855(12) 0.4565(10) 0.116(11) Uani 1 1 d . . . H33 H 1.1001 0.1447 0.4796 0.139 Uiso 1 1 calc R . . C37 C 0.7359(15) 0.2330(12) 0.4980(9) 0.073(7) Uani 1 1 d . . . H36 H 0.7287 0.2476 0.5336 0.087 Uiso 1 1 calc R . . C43 C 1.1921(12) 0.0807(11) 0.3134(8) 0.064(7) Uani 1 1 d . . . H43 H 1.2140 0.0336 0.3255 0.077 Uiso 1 1 calc R . . C82 C -0.0648(10) 0.7990(10) 0.3191(7) 0.046(5) Uani 1 1 d . . . H60 H -0.0542 0.8406 0.3055 0.055 Uiso 1 1 calc R . . C83 C -0.1304(10) 0.7976(11) 0.3570(7) 0.046(5) Uani 1 1 d . . . H61 H -0.1654 0.8386 0.3695 0.055 Uiso 1 1 calc R . . C109 C 0.3583(10) 0.7226(9) 0.2763(7) 0.044(6) Uani 1 1 d . . . H84 H 0.2999 0.7302 0.2849 0.053 Uiso 1 1 calc R . . C93 C 0.1483(9) 0.6038(8) 0.0926(6) 0.028(4) Uani 1 1 d . . . F7 F 0.4741(11) 0.9148(7) 0.4444(6) 0.208(10) Uani 1 1 d . . . C127 C 0.2316(9) 0.4511(9) 0.1955(7) 0.041(5) Uani 1 1 d . . . H99 H 0.2151 0.4962 0.1776 0.049 Uiso 1 1 calc R . . C45 C 1.1905(12) 0.1937(11) 0.3143(8) 0.057(6) Uani 1 1 d . . . H41 H 1.2109 0.2272 0.3277 0.068 Uiso 1 1 calc R . . C27 C 0.7897(11) 0.4679(9) 0.1180(7) 0.042(5) Uani 1 1 d . . . H28 H 0.8351 0.4690 0.0933 0.050 Uiso 1 1 calc R . . C8 C 0.7434(10) 0.6671(8) 0.5048(6) 0.042(5) Uani 1 1 d . . . H12A H 0.8042 0.6597 0.5096 0.063 Uiso 1 1 calc R . . H12B H 0.7208 0.6456 0.5370 0.063 Uiso 1 1 calc R . . H12C H 0.7142 0.7161 0.5005 0.063 Uiso 1 1 calc R . . C86 C -0.0292(11) 0.6758(9) 0.3226(8) 0.042(5) Uani 1 1 d . . . H64 H 0.0059 0.6338 0.3118 0.050 Uiso 1 1 calc R . . C135 C 1.0175(12) 0.4323(11) 0.1578(8) 0.080(7) Uani 1 1 d . . . H9A H 1.0324 0.3920 0.1378 0.120 Uiso 1 1 calc R . . H9B H 1.0675 0.4481 0.1603 0.120 Uiso 1 1 calc R . . H9C H 0.9723 0.4686 0.1385 0.120 Uiso 1 1 calc R . . C36 C 0.7897(12) 0.2542(9) 0.4613(8) 0.051(5) Uani 1 1 d . . . H35 H 0.8189 0.2840 0.4717 0.061 Uiso 1 1 calc R . . C25 C 0.6491(9) 0.5205(9) 0.1484(7) 0.035(5) Uani 1 1 d . . . H26 H 0.5986 0.5576 0.1445 0.042 Uiso 1 1 calc R . . C97 C 0.2309(10) 0.5136(9) 0.0384(7) 0.043(5) Uani 1 1 d . . . H73 H 0.2838 0.4889 0.0240 0.051 Uiso 1 1 calc R . . C98 C 0.2119(8) 0.7171(8) 0.1053(8) 0.026(4) Uani 1 1 d . . . C79 C 0.5508(10) 0.3428(9) 0.5807(6) 0.051(6) Uani 1 1 d . . . H18A H 0.5577 0.2946 0.5777 0.077 Uiso 1 1 calc R . . H18B H 0.4969 0.3628 0.5990 0.077 Uiso 1 1 calc R . . H18C H 0.5976 0.3469 0.6019 0.077 Uiso 1 1 calc R . . C81 C -0.0146(9) 0.7353(11) 0.3018(7) 0.038(5) Uani 1 1 d . . . C99 C 0.2476(10) 0.7521(9) 0.1373(7) 0.036(5) Uani 1 1 d . . . H75 H 0.2391 0.7468 0.1757 0.044 Uiso 1 1 calc R . . C119 C 0.0210(12) 0.5040(13) 0.4238(10) 0.071(8) Uani 1 1 d . . . H92 H -0.0195 0.5009 0.4517 0.085 Uiso 1 1 calc R . . C53 C 0.7529(9) 0.1224(9) 0.2017(6) 0.027(4) Uiso 1 1 d . . . C87 C 0.1039(10) 0.8062(9) 0.2627(8) 0.037(5) Uiso 1 1 d . . . C123 C 0.2526(9) 0.3742(10) 0.2772(7) 0.039(5) Uani 1 1 d . . . H95 H 0.2494 0.3669 0.3159 0.047 Uiso 1 1 calc R . . C106 C 0.5295(11) 0.7003(12) 0.2548(7) 0.052(6) Uani 1 1 d . . . H81 H 0.5881 0.6937 0.2473 0.063 Uiso 1 1 calc R . . C28 C 0.7987(10) 0.4150(8) 0.1590(7) 0.030(5) Uani 1 1 d . . . H29 H 0.8506 0.3793 0.1623 0.036 Uiso 1 1 calc R . . C144 C 1.3180(14) 0.0909(13) 0.5345(8) 0.064(7) Uani 1 1 d . . . C103 C 0.2261(10) 0.7246(9) 0.0499(7) 0.043(5) Uani 1 1 d . . . H79 H 0.2022 0.7020 0.0263 0.051 Uiso 1 1 calc R . . C52 C 0.9768(11) 0.2748(9) 0.1088(8) 0.047(6) Uani 1 1 d . . . H45 H 0.9211 0.2706 0.1133 0.056 Uiso 1 1 calc R . . C84 C -0.1436(11) 0.7351(12) 0.3761(8) 0.057(6) Uani 1 1 d . . . H62 H -0.1880 0.7342 0.4016 0.068 Uiso 1 1 calc R . . C94 C 0.0735(9) 0.5849(8) 0.0810(7) 0.028(5) Uani 1 1 d . . . H70 H 0.0198 0.6088 0.0949 0.034 Uiso 1 1 calc R . . C89 C 0.1536(12) 0.9048(11) 0.2274(11) 0.074(8) Uani 1 1 d . . . H66 H 0.1604 0.9369 0.1981 0.089 Uiso 1 1 calc R . . C55 C 0.6569(11) 0.0681(10) 0.1720(8) 0.052(6) Uani 1 1 d . . . H51 H 0.6391 0.0285 0.1720 0.062 Uiso 1 1 calc R . . C148 C 1.0747(14) 0.3128(10) 0.0538(9) 0.065(6) Uani 1 1 d . . . H47 H 1.0885 0.3371 0.0214 0.078 Uiso 1 1 calc R . . C20 C 0.4937(10) 0.3024(8) 0.2887(8) 0.038(5) Uani 1 1 d . . . H22 H 0.4432 0.2901 0.2968 0.046 Uiso 1 1 calc R . . C108 C 0.3988(11) 0.7711(10) 0.2830(7) 0.053(6) Uani 1 1 d . . . H83 H 0.3667 0.8136 0.2945 0.064 Uiso 1 1 calc R . . C134 C 0.9867(14) 0.4138(10) 0.2158(10) 0.060(7) Uani 1 1 d . . . C62 C 0.8844(17) -0.0399(11) 0.3851(9) 0.072(7) Uani 1 1 d . . . H57 H 0.8932 -0.0706 0.4176 0.087 Uiso 1 1 calc R . . C51 C 0.9925(11) 0.3104(9) 0.0614(7) 0.038(5) Uani 1 1 d . . . H46 H 0.9495 0.3321 0.0353 0.045 Uiso 1 1 calc R . . C49 C 1.1385(13) 0.2812(10) 0.0918(9) 0.067(7) Uani 1 1 d . . . H48 H 1.1947 0.2829 0.0842 0.080 Uiso 1 1 calc R . . C71 C -0.3142(10) 0.9097(9) -0.0512(7) 0.055(6) Uani 1 1 d . . . H16A H -0.3705 0.9431 -0.0523 0.082 Uiso 1 1 calc R . . H16B H -0.3188 0.8659 -0.0603 0.082 Uiso 1 1 calc R . . H16C H -0.2769 0.9258 -0.0778 0.082 Uiso 1 1 calc R . . C63 C 0.9510(14) -0.0323(11) 0.3525(10) 0.066(7) Uani 1 1 d . . . H58 H 1.0061 -0.0612 0.3620 0.080 Uiso 1 1 calc R . . C88 C 0.1124(9) 0.8537(9) 0.2207(8) 0.042(5) Uani 1 1 d . . . H65 H 0.0904 0.8528 0.1859 0.051 Uiso 1 1 calc R . . C117 C 0.0792(10) 0.4759(8) 0.3364(8) 0.046(5) Uani 1 1 d . . . H90 H 0.0766 0.4555 0.3041 0.055 Uiso 1 1 calc R . . C44 C 1.2236(14) 0.1256(13) 0.3326(10) 0.086(8) Uani 1 1 d . . . H42 H 1.2682 0.1110 0.3585 0.103 Uiso 1 1 calc R . . C56 C 0.6097(12) 0.1288(12) 0.1443(8) 0.064(7) Uani 1 1 d . . . H52 H 0.5612 0.1300 0.1243 0.077 Uiso 1 1 calc R . . C146 C 0.9046(19) 0.066(3) 0.5313(12) 0.15(2) Uani 1 1 d . . . C39 C 0.7059(12) 0.1686(11) 0.4324(11) 0.068(7) Uani 1 1 d . . . H38 H 0.6774 0.1381 0.4223 0.082 Uiso 1 1 calc R . . C46 C 1.1230(12) 0.2127(12) 0.2737(8) 0.074(7) Uani 1 1 d . . . H40 H 1.0973 0.2593 0.2613 0.088 Uiso 1 1 calc R . . C48 C 1.1207(12) 0.2473(10) 0.1403(9) 0.065(6) Uani 1 1 d . . . H49 H 1.1638 0.2265 0.1666 0.078 Uiso 1 1 calc R . . N3 N 0.941(2) 0.102(3) 0.5302(17) 0.30(3) Uani 1 1 d . . . C105 C 0.4934(9) 0.6491(10) 0.2458(6) 0.042(5) Uani 1 1 d . . . H80 H 0.5261 0.6073 0.2333 0.051 Uiso 1 1 calc R . . C92 C 0.1330(10) 0.8081(10) 0.3136(8) 0.056(6) Uani 1 1 d . . . H69 H 0.1273 0.7760 0.3432 0.068 Uiso 1 1 calc R . . C133 C -0.1526(12) 0.5867(11) 0.2448(9) 0.094(8) Uani 1 1 d . . . H4A H -0.1721 0.5548 0.2260 0.142 Uiso 1 1 calc R . . H4B H -0.1916 0.6327 0.2373 0.142 Uiso 1 1 calc R . . H4C H -0.1511 0.5729 0.2843 0.142 Uiso 1 1 calc R . . C38 C 0.6923(14) 0.1902(13) 0.4832(10) 0.074(8) Uani 1 1 d . . . H37 H 0.6536 0.1761 0.5079 0.089 Uiso 1 1 calc R . . C132 C -0.0679(16) 0.5861(14) 0.2255(11) 0.104(10) Uani 1 1 d . . . C107 C 0.4824(12) 0.7592(10) 0.2738(8) 0.056(6) Uani 1 1 d . . . H82 H 0.5089 0.7925 0.2806 0.068 Uiso 1 1 calc R . . C15 C 1.2110(10) -0.0730(9) -0.0487(7) 0.053(6) Uani 1 1 d . . . H14C H 1.2043 -0.1061 -0.0723 0.080 Uiso 1 1 calc R . . H14B H 1.2688 -0.0877 -0.0343 0.080 Uiso 1 1 calc R . . H14A H 1.2005 -0.0282 -0.0699 0.080 Uiso 1 1 calc R . . Sb1 Sb 0.42016(8) 0.30050(8) 0.02205(6) 0.0632(5) Uani 1 1 d . . . N10 N 0.1277(9) 0.4018(8) -0.0791(6) 0.060(5) Uani 1 1 d . . . F5 F 0.4354(8) 0.3884(7) 0.0230(5) 0.119(5) Uani 1 1 d . . . F1 F 0.4181(8) 0.3194(6) -0.0513(4) 0.097(4) Uani 1 1 d . . . F4 F 0.5340(7) 0.2673(9) 0.0198(6) 0.182(8) Uani 1 1 d . . . N8 N 0.7717(10) 0.2900(9) 0.0895(7) 0.073(6) Uani 1 1 d . . . C131 C 0.6402(11) 0.3861(10) 0.0541(8) 0.079(7) Uani 1 1 d . . . H8C H 0.6542 0.4292 0.0469 0.118 Uiso 1 1 calc R . . H8B H 0.5939 0.3911 0.0809 0.118 Uiso 1 1 calc R . . H8A H 0.6224 0.3742 0.0200 0.118 Uiso 1 1 calc R . . F3 F 0.4046(11) 0.2221(7) 0.0185(7) 0.187(8) Uani 1 1 d . . . C130 C 0.7134(13) 0.3332(10) 0.0751(8) 0.052(6) Uani 1 1 d . . . F6 F 0.3061(6) 0.3420(7) 0.0264(6) 0.130(5) Uani 1 1 d . . . F2 F 0.4263(10) 0.2828(9) 0.0949(6) 0.199(9) Uani 1 1 d . . . C129 C 0.2432(11) 0.3002(9) -0.1106(8) 0.068(6) Uani 1 1 d . . . H5B H 0.2913 0.3162 -0.1239 0.102 Uiso 1 1 calc R . . H5A H 0.2230 0.2808 -0.1399 0.102 Uiso 1 1 calc R . . H5C H 0.2611 0.2652 -0.0795 0.102 Uiso 1 1 calc R . . N5 N 0.7063(13) 0.7626(11) 0.2407(9) 0.089(7) Uani 1 1 d . . . C137 C 0.6886(11) 0.8834(11) 0.2715(9) 0.081(7) Uani 1 1 d . . . H1B H 0.6708 0.8822 0.3099 0.122 Uiso 1 1 calc R . . H1C H 0.6460 0.9192 0.2497 0.122 Uiso 1 1 calc R . . H1A H 0.7432 0.8931 0.2679 0.122 Uiso 1 1 calc R . . C136 C 0.6972(13) 0.8156(14) 0.2516(9) 0.064(8) Uani 1 1 d . . . C138 C 0.4791(14) 0.8736(11) 0.0964(9) 0.072(7) Uani 1 1 d . . . N6 N 0.4195(12) 0.9141(10) 0.0784(9) 0.104(8) Uani 1 1 d . . . C139 C 0.5515(12) 0.8220(10) 0.1199(8) 0.085(8) Uani 1 1 d . . . H3B H 0.5981 0.8141 0.0932 0.127 Uiso 1 1 calc R . . H3C H 0.5367 0.7796 0.1299 0.127 Uiso 1 1 calc R . . H3A H 0.5690 0.8370 0.1526 0.127 Uiso 1 1 calc R . . C149 C 0.5327(15) 0.1047(13) 0.3150(12) 0.086(9) Uani 1 1 d . . . C141 C 0.4687(12) 0.1229(12) 0.2732(8) 0.087(8) Uani 1 1 d . . . H6A H 0.4129 0.1275 0.2902 0.130 Uiso 1 1 calc R . . H6C H 0.4808 0.0873 0.2484 0.130 Uiso 1 1 calc R . . H6B H 0.4689 0.1663 0.2525 0.130 Uiso 1 1 calc R . . N9 N 0.5815(12) 0.0959(12) 0.3503(9) 0.105(8) Uani 1 1 d . . . C150 C 0.4952(12) 0.9780(10) 0.1914(9) 0.076(7) Uiso 1 1 d . . . H2A H 0.5075 0.9945 0.2249 0.114 Uiso 1 1 calc R . . H2B H 0.5098 1.0057 0.1596 0.114 Uiso 1 1 calc R . . H2C H 0.5289 0.9303 0.1904 0.114 Uiso 1 1 calc R . . C140 C 0.417(2) 0.9827(14) 0.1901(10) 0.121(10) Uani 1 1 d . . . F9 F 0.3163(9) 0.9566(7) 0.4140(8) 0.191(8) Uani 1 1 d . . . C142 C 0.6030(12) 0.7875(11) 0.5917(8) 0.048(6) Uani 1 1 d . . . C143 C 0.5368(11) 0.8163(10) 0.5474(8) 0.085(8) Uani 1 1 d . . . H10A H 0.5643 0.8121 0.5115 0.128 Uiso 1 1 calc R . . H10B H 0.5084 0.8645 0.5512 0.128 Uiso 1 1 calc R . . H10C H 0.4949 0.7910 0.5510 0.128 Uiso 1 1 calc R . . C128 C 0.1759(12) 0.3565(10) -0.0936(8) 0.044(6) Uiso 1 1 d . . . N7 N 0.3328(13) 0.9856(15) 0.1919(11) 0.188(13) Uani 1 1 d . . . C145 C 1.3742(16) 0.0259(12) 0.5251(12) 0.155(14) Uani 1 1 d . . . H7A H 1.3758 0.0208 0.4860 0.232 Uiso 1 1 calc R . . H7B H 1.3542 -0.0100 0.5455 0.232 Uiso 1 1 calc R . . H7C H 1.4312 0.0224 0.5373 0.232 Uiso 1 1 calc R . . C147 C 0.8624(18) 0.0153(19) 0.5335(13) 0.179(17) Uani 1 1 d . . . H11A H 0.8957 -0.0262 0.5551 0.269 Uiso 1 1 calc R . . H11C H 0.8556 0.0051 0.4964 0.269 Uiso 1 1 calc R . . H11B H 0.8065 0.0320 0.5505 0.269 Uiso 1 1 calc R . . C121 C 0.1474(11) 0.5311(9) 0.3924(7) 0.051(6) Uani 1 1 d . . . H94 H 0.1929 0.5483 0.3989 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 Ag1 0.0246(7) 0.0300(8) 0.0351(8) -0.0092(7) 0.0033(6) -0.0073(6) Ag2 0.0237(7) 0.0352(9) 0.0354(9) -0.0028(7) -0.0032(6) -0.0091(6) Sb2 0.0402(8) 0.0532(10) 0.0500(9) -0.0002(8) -0.0053(7) 0.0013(7) P3 0.027(3) 0.028(3) 0.039(3) -0.005(2) 0.001(2) -0.009(2) S1 0.029(2) 0.028(3) 0.041(3) -0.010(2) -0.007(2) -0.005(2) S2 0.029(2) 0.036(3) 0.033(3) -0.013(2) -0.007(2) -0.006(2) S10 0.025(2) 0.051(3) 0.034(3) -0.011(2) -0.005(2) -0.002(2) P7 0.022(2) 0.036(3) 0.035(3) -0.002(2) -0.005(2) -0.011(2) S13 0.022(2) 0.047(3) 0.039(3) -0.007(3) 0.002(2) -0.012(2) S16 0.023(2) 0.046(3) 0.040(3) -0.001(3) 0.000(2) -0.012(2) S15 0.029(2) 0.047(3) 0.039(3) 0.002(3) -0.004(2) -0.018(2) S3 0.038(3) 0.034(3) 0.048(3) -0.015(3) -0.006(2) -0.002(2) S14 0.020(2) 0.043(3) 0.041(3) 0.000(2) -0.004(2) -0.011(2) P4 0.025(3) 0.039(3) 0.043(3) -0.013(3) 0.001(2) -0.015(2) S11 0.031(3) 0.041(3) 0.050(3) -0.008(3) -0.007(2) -0.003(2) S6 0.028(2) 0.040(3) 0.048(3) -0.020(3) 0.009(2) -0.016(2) P2 0.025(2) 0.029(3) 0.030(3) -0.006(2) 0.000(2) -0.008(2) P1 0.021(2) 0.030(3) 0.034(3) -0.006(2) 0.003(2) -0.005(2) S9 0.030(2) 0.037(3) 0.038(3) -0.006(2) -0.007(2) -0.005(2) P8 0.021(2) 0.040(3) 0.037(3) 0.001(3) -0.006(2) -0.014(2) P6 0.022(2) 0.038(3) 0.036(3) -0.007(3) 0.002(2) -0.006(2) P5 0.024(2) 0.033(3) 0.040(3) -0.009(2) -0.005(2) -0.007(2) S7 0.043(3) 0.039(3) 0.049(3) -0.021(3) 0.013(3) -0.022(2) S4 0.032(3) 0.042(3) 0.045(3) -0.016(3) -0.003(2) -0.007(2) S8 0.040(3) 0.044(3) 0.052(3) -0.022(3) 0.012(3) -0.017(2) S12 0.040(3) 0.048(3) 0.047(3) -0.011(3) -0.008(3) -0.005(2) S5 0.040(3) 0.039(3) 0.057(3) -0.021(3) 0.013(3) -0.021(2) F10 0.077(8) 0.053(9) 0.210(15) 0.014(9) -0.028(9) -0.029(7) C73 0.012(9) 0.014(11) 0.033(11) -0.003(8) -0.015(8) 0.001(7) C77 0.029(10) 0.033(12) 0.009(10) 0.012(9) 0.000(9) -0.005(9) C6 0.052(12) 0.029(12) 0.016(11) -0.006(9) 0.013(10) -0.021(9) C22 0.035(11) 0.040(12) 0.027(11) -0.020(9) -0.005(10) -0.013(9) C120 0.029(12) 0.12(2) 0.038(15) -0.020(13) -0.009(12) 0.013(13) F12 0.140(11) 0.045(8) 0.140(12) 0.023(8) 0.034(9) -0.028(8) F11 0.072(9) 0.086(10) 0.207(15) 0.020(10) 0.072(10) 0.001(7) C5 0.040(11) 0.027(12) 0.032(12) -0.001(10) 0.003(10) -0.022(9) N2 0.056(12) 0.065(13) 0.078(15) -0.029(11) 0.009(10) -0.025(10) N11 0.063(12) 0.070(13) 0.110(17) -0.046(12) -0.002(13) -0.034(11) C74 0.025(10) 0.024(11) 0.027(11) -0.015(9) -0.017(9) 0.005(8) C18 0.020(10) 0.019(11) 0.048(14) -0.008(10) 0.001(10) -0.003(8) C57 0.062(14) 0.046(16) 0.095(19) -0.040(14) -0.029(13) 0.013(12) C59 0.042(11) 0.042(13) 0.019(11) 0.000(9) 0.007(10) -0.019(10) C14 0.042(11) 0.024(12) 0.042(12) -0.023(10) -0.007(10) -0.008(9) C101 0.024(11) 0.061(15) 0.083(18) -0.044(15) 0.014(13) -0.013(10) N4 0.075(14) 0.22(3) 0.029(12) 0.001(15) -0.024(12) -0.078(14) C24 0.012(9) 0.043(12) 0.011(10) 0.002(9) -0.011(8) 0.001(8) C21 0.032(12) 0.050(14) 0.053(15) -0.010(12) -0.003(11) -0.022(10) C113 0.026(11) 0.060(16) 0.032(13) -0.020(13) 0.015(10) -0.001(11) C70 0.015(10) 0.041(12) 0.028(11) -0.001(10) -0.009(9) 0.004(8) C122 0.016(9) 0.021(11) 0.022(11) -0.003(9) 0.004(8) -0.010(8) C4 0.016(9) 0.021(11) 0.031(11) -0.003(9) -0.005(8) 0.003(8) C112 0.009(9) 0.082(17) 0.031(13) 0.002(12) -0.012(9) -0.016(10) C114 0.038(11) 0.044(14) 0.040(13) -0.005(12) -0.009(11) -0.031(10) C12 0.039(11) 0.030(12) 0.031(11) -0.013(10) 0.022(10) -0.024(9) C26 0.050(13) 0.029(12) 0.042(13) -0.011(10) -0.023(12) 0.004(10) C96 0.051(13) 0.027(12) 0.042(13) 0.001(10) 0.005(11) -0.013(10) F8 0.148(12) 0.071(9) 0.159(13) -0.040(9) -0.107(11) 0.031(8) C69 0.026(10) 0.025(11) 0.036(12) 0.013(10) -0.011(10) -0.011(8) C72 0.019(10) 0.090(16) 0.048(13) -0.017(12) 0.008(10) -0.012(10) C67 0.031(10) 0.033(11) 0.036(12) 0.007(9) 0.002(9) -0.011(9) C91 0.034(13) 0.12(3) 0.11(2) -0.08(2) 0.023(15) -0.033(15) C78 0.031(10) 0.017(12) 0.051(13) -0.013(10) -0.007(10) 0.000(8) C60 0.071(14) 0.042(14) 0.023(12) 0.001(11) 0.018(11) -0.040(11) C16 0.069(12) 0.005(10) 0.031(11) -0.005(9) 0.004(10) -0.005(9) C50 0.037(12) 0.034(13) 0.062(15) 0.007(11) -0.009(11) -0.011(10) C10 0.026(10) 0.035(12) 0.046(12) -0.034(10) 0.017(9) -0.004(8) C40 0.059(13) 0.062(16) 0.051(14) -0.020(12) 0.006(12) -0.038(12) C2 0.020(9) 0.028(11) 0.037(12) -0.011(9) 0.010(9) -0.012(8) C64 0.052(14) 0.041(14) 0.053(15) 0.004(12) 0.017(12) 0.006(11) C42 0.062(14) 0.068(18) 0.061(16) 0.030(13) -0.022(13) -0.032(13) C68 0.038(11) 0.031(11) 0.016(10) 0.002(9) -0.002(9) 0.009(9) C17 0.017(9) 0.011(10) 0.037(12) -0.012(9) -0.011(9) -0.004(7) C118 0.016(12) 0.064(17) 0.13(2) 0.016(17) 0.002(16) -0.026(11) C23 0.021(10) 0.039(12) 0.029(11) -0.004(9) -0.005(9) -0.017(9) C95 0.029(11) 0.062(15) 0.041(13) -0.029(11) 0.007(10) -0.014(10) C76 0.017(8) 0.033(11) 0.013(9) 0.011(8) 0.000(8) -0.011(8) C80 0.027(10) 0.052(13) 0.032(11) -0.022(10) 0.000(9) -0.004(9) C3 0.016(9) 0.042(12) 0.016(10) 0.014(9) 0.001(8) -0.016(8) C126 0.055(12) 0.047(14) 0.025(11) -0.019(11) -0.005(10) -0.029(10) C11 0.027(10) 0.020(11) 0.073(15) 0.002(11) 0.000(11) -0.019(8) C115 0.036(11) 0.043(13) 0.030(12) 0.004(10) 0.008(10) -0.015(9) C124 0.032(11) 0.042(13) 0.067(16) -0.006(12) -0.014(11) -0.017(10) C66 0.015(9) 0.025(10) 0.020(10) -0.010(8) 0.001(8) 0.007(7) C19 0.012(9) 0.043(13) 0.040(13) 0.005(10) 0.017(10) 0.005(9) C29 0.034(11) 0.016(13) 0.074(15) 0.000(11) -0.019(11) 0.005(9) C100 0.049(13) 0.035(15) 0.055(16) 0.008(12) 0.009(12) -0.021(10) C90 0.017(12) 0.06(2) 0.19(4) -0.07(2) 0.022(18) -0.017(12) C1 0.023(9) 0.047(12) 0.026(11) -0.028(10) 0.011(9) -0.017(9) C30 0.034(11) 0.040(15) 0.081(16) 0.007(12) -0.023(12) -0.003(10) C54 0.032(11) 0.056(15) 0.041(13) -0.022(10) 0.008(10) -0.023(10) C31 0.070(15) 0.036(15) 0.15(2) 0.015(15) -0.042(16) -0.031(12) N1 0.043(12) 0.066(14) 0.094(15) -0.006(12) 0.006(11) -0.013(10) C34 0.061(15) 0.034(15) 0.16(2) 0.020(16) -0.027(16) -0.031(12) C7 0.058(13) 0.039(13) 0.046(13) -0.006(11) 0.002(11) -0.015(10) C32 0.073(16) 0.050(18) 0.22(3) 0.049(19) -0.093(19) -0.040(14) C13 0.034(11) 0.031(12) 0.044(13) -0.033(10) 0.008(10) -0.011(9) C65 0.010(9) 0.027(11) 0.054(13) -0.011(10) -0.001(9) -0.014(7) C58 0.041(12) 0.066(16) 0.072(16) -0.024(13) 0.003(12) -0.016(11) C61 0.078(18) 0.073(18) 0.056(17) -0.018(14) 0.041(14) -0.034(14) C41 0.052(12) 0.029(14) 0.080(17) -0.023(13) -0.044(12) -0.010(10) C102 0.048(12) 0.067(16) 0.029(12) 0.014(12) 0.001(11) -0.030(11) C85 0.068(15) 0.011(12) 0.077(16) -0.006(11) 0.020(13) -0.014(11) C47 0.073(14) 0.037(13) 0.016(11) -0.007(9) 0.011(11) -0.041(11) C33 0.074(16) 0.09(2) 0.18(3) 0.095(19) -0.086(18) -0.044(15) C37 0.10(2) 0.07(2) 0.049(16) -0.003(14) 0.033(15) -0.032(15) C43 0.079(16) 0.035(16) 0.068(16) 0.026(13) -0.051(13) -0.007(12) C82 0.034(12) 0.068(16) 0.044(13) -0.009(12) 0.019(11) -0.029(11) C83 0.021(11) 0.062(16) 0.040(13) 0.005(12) 0.009(10) 0.005(10) C109 0.032(11) 0.065(16) 0.041(13) 0.007(11) -0.023(10) -0.025(11) C93 0.013(9) 0.029(11) 0.033(11) 0.003(9) 0.009(9) 0.002(8) F7 0.280(19) 0.131(13) 0.121(13) -0.058(11) -0.133(13) 0.111(13) C127 0.040(11) 0.039(13) 0.035(13) -0.002(11) -0.017(10) 0.003(9) C45 0.062(14) 0.060(17) 0.065(16) -0.032(13) 0.012(13) -0.037(13) C27 0.058(14) 0.043(13) 0.027(12) 0.001(11) 0.006(10) -0.021(11) C8 0.052(12) 0.048(13) 0.033(12) -0.015(10) 0.019(10) -0.025(10) C86 0.032(12) 0.024(13) 0.059(15) 0.001(11) -0.001(11) 0.006(9) C135 0.088(17) 0.094(19) 0.065(17) 0.027(15) -0.016(14) -0.048(14) C36 0.082(15) 0.035(13) 0.043(14) -0.014(11) 0.009(12) -0.026(11) C25 0.003(9) 0.071(15) 0.034(12) -0.016(12) -0.002(10) -0.009(9) C97 0.018(10) 0.036(13) 0.061(14) -0.009(11) 0.005(10) 0.012(9) C98 0.012(9) 0.014(11) 0.057(14) -0.008(10) 0.014(10) -0.009(7) C79 0.036(11) 0.082(16) 0.042(13) -0.017(12) -0.010(10) -0.022(10) C81 0.015(10) 0.057(15) 0.036(12) -0.008(12) 0.006(9) -0.004(10) C99 0.048(12) 0.026(13) 0.045(13) -0.008(11) -0.012(10) -0.022(10) C119 0.023(13) 0.12(2) 0.051(17) 0.007(16) 0.018(13) -0.003(13) C123 0.028(10) 0.061(15) 0.031(12) 0.005(12) -0.004(9) -0.020(10) C106 0.026(11) 0.11(2) 0.035(13) 0.003(13) -0.012(10) -0.041(13) C28 0.036(11) 0.020(12) 0.042(12) -0.014(10) 0.003(10) -0.016(9) C144 0.071(19) 0.08(2) 0.044(14) -0.036(15) 0.031(13) -0.024(15) C103 0.041(12) 0.055(15) 0.025(13) 0.013(11) 0.018(10) -0.011(10) C52 0.041(12) 0.051(14) 0.034(13) -0.017(11) -0.012(11) 0.012(10) C84 0.040(13) 0.072(17) 0.054(15) 0.026(15) -0.001(11) -0.023(13) C94 0.012(9) 0.029(12) 0.040(12) 0.013(10) -0.001(9) -0.006(8) C89 0.048(15) 0.049(18) 0.13(2) 0.003(17) 0.015(15) -0.023(12) C55 0.045(13) 0.027(13) 0.091(18) -0.032(12) 0.018(12) -0.014(10) C148 0.085(17) 0.054(16) 0.062(17) -0.021(13) 0.003(15) -0.024(14) C20 0.024(10) 0.036(13) 0.055(14) -0.010(11) 0.001(12) -0.009(9) C108 0.030(12) 0.064(16) 0.064(15) -0.011(12) -0.007(11) -0.008(11) C134 0.064(16) 0.044(14) 0.064(18) -0.019(15) -0.038(16) 0.005(12) C62 0.11(2) 0.050(16) 0.065(18) -0.007(13) 0.013(18) -0.029(16) C51 0.040(12) 0.048(14) 0.014(12) -0.002(10) 0.001(10) 0.005(10) C49 0.056(14) 0.078(18) 0.067(17) 0.028(14) 0.018(14) -0.036(13) C71 0.048(12) 0.064(15) 0.047(14) 0.004(11) -0.008(11) -0.011(10) C63 0.069(16) 0.065(18) 0.069(18) -0.007(15) 0.009(15) -0.027(14) C88 0.021(10) 0.041(14) 0.060(14) -0.009(12) -0.003(10) 0.000(9) C117 0.020(10) 0.055(14) 0.069(15) -0.012(11) 0.006(11) -0.021(9) C44 0.069(17) 0.06(2) 0.11(2) 0.016(18) -0.010(15) -0.013(15) C56 0.047(13) 0.069(18) 0.081(17) -0.059(16) 0.008(12) -0.008(13) C146 0.06(2) 0.30(7) 0.07(2) 0.09(3) -0.018(18) -0.05(2) C39 0.051(14) 0.071(18) 0.10(2) 0.002(17) 0.006(15) -0.046(13) C46 0.055(14) 0.09(2) 0.050(15) 0.021(14) -0.008(13) 0.007(13) C48 0.055(14) 0.058(16) 0.088(18) 0.020(14) -0.005(13) -0.036(12) N3 0.15(3) 0.43(6) 0.30(5) 0.31(4) -0.12(3) -0.17(3) C105 0.016(10) 0.073(16) 0.039(13) -0.013(11) 0.005(9) -0.012(10) C92 0.029(11) 0.080(17) 0.070(16) -0.045(13) 0.007(11) -0.018(11) C133 0.067(16) 0.094(19) 0.11(2) 0.006(16) -0.002(15) -0.014(14) C38 0.073(17) 0.08(2) 0.055(18) -0.010(16) 0.034(15) -0.010(15) C132 0.056(17) 0.14(3) 0.13(3) -0.054(19) 0.02(2) -0.037(19) C107 0.042(14) 0.056(15) 0.078(17) -0.041(13) -0.023(12) -0.011(11) C15 0.050(12) 0.052(14) 0.063(14) -0.017(11) 0.014(12) -0.020(10) Sb1 0.0392(8) 0.0896(13) 0.0601(11) -0.0128(9) 0.0052(8) -0.0167(8) N10 0.050(10) 0.064(12) 0.078(13) -0.014(10) -0.002(9) -0.035(9) F5 0.155(12) 0.138(13) 0.124(12) -0.082(10) 0.058(9) -0.115(10) F1 0.147(11) 0.098(10) 0.052(8) -0.008(7) -0.010(8) -0.046(9) F4 0.053(9) 0.31(2) 0.123(13) -0.057(14) -0.013(8) 0.042(11) N8 0.056(12) 0.075(14) 0.084(15) -0.017(12) -0.005(11) -0.011(10) C131 0.065(15) 0.069(16) 0.091(18) -0.009(14) -0.014(14) 0.000(13) F3 0.255(19) 0.053(10) 0.25(2) -0.005(11) 0.136(16) -0.061(11) C130 0.053(14) 0.056(15) 0.047(15) -0.018(12) 0.005(12) -0.014(12) F6 0.032(7) 0.147(12) 0.195(15) -0.044(11) 0.000(8) 0.008(7) F2 0.161(15) 0.26(2) 0.082(12) 0.036(12) 0.017(10) 0.053(14) C129 0.076(15) 0.044(14) 0.089(17) 0.002(13) 0.027(13) -0.033(12) N5 0.090(15) 0.082(17) 0.105(18) -0.010(16) -0.002(13) -0.040(15) C137 0.050(14) 0.10(2) 0.095(19) -0.008(17) 0.015(13) -0.024(14) C136 0.054(14) 0.08(2) 0.053(16) -0.001(17) -0.034(12) -0.007(16) C138 0.071(17) 0.068(18) 0.086(19) 0.006(15) -0.023(15) -0.036(14) N6 0.083(15) 0.074(15) 0.16(2) -0.009(15) -0.057(15) -0.029(12) C139 0.086(16) 0.073(16) 0.089(18) 0.032(14) -0.041(14) -0.024(14) C149 0.055(17) 0.11(2) 0.12(3) -0.06(2) 0.054(17) -0.054(17) C141 0.063(15) 0.14(2) 0.064(17) -0.034(16) -0.013(13) -0.033(15) N9 0.062(14) 0.15(2) 0.13(2) -0.064(17) 0.013(13) -0.060(14) C140 0.12(3) 0.15(3) 0.10(2) -0.037(19) 0.01(2) -0.05(2) F9 0.122(12) 0.113(12) 0.27(2) 0.020(13) 0.113(14) 0.036(10) C142 0.043(13) 0.081(18) 0.036(15) -0.016(13) 0.010(11) -0.041(13) C143 0.048(13) 0.087(17) 0.100(19) -0.006(15) 0.013(14) 0.008(12) N7 0.058(15) 0.28(3) 0.19(3) 0.05(2) 0.068(17) -0.025(18) C145 0.14(3) 0.09(2) 0.24(4) -0.08(2) 0.15(3) -0.050(19) C147 0.10(3) 0.28(5) 0.16(3) -0.08(3) 0.06(2) -0.05(3) C121 0.023(11) 0.082(16) 0.041(13) -0.027(12) -0.005(11) 0.002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 P3 2.507(4) . ? Ag1 P1 2.507(4) . ? Ag1 P4 2.517(5) . ? Ag1 P2 2.543(4) . ? Ag2 P8 2.459(5) . ? Ag2 P5 2.481(4) . ? Ag2 P6 2.483(5) . ? Ag2 P7 2.535(4) . ? Sb2 F7 1.719(12) . ? Sb2 F10 1.801(11) . ? Sb2 F8 1.806(11) . ? Sb2 F9 1.828(12) . ? Sb2 F11 1.835(11) . ? Sb2 F12 1.892(11) . ? P3 C47 1.800(16) . ? P3 C41 1.814(17) . ? P3 C9 1.850(16) . ? S1 C1 1.722(16) . ? S1 C3 1.751(15) . ? S2 C2 1.757(16) . ? S2 C3 1.779(15) . ? S10 C67 1.722(16) . ? S10 C66 1.739(13) . ? P7 C110 1.805(15) . ? P7 C73 1.823(15) . ? P7 C104 1.829(16) . ? S13 C74 1.755(15) . ? S13 C75 1.796(15) . ? S16 C76 1.725(14) . ? S16 C78 1.733(17) . ? S15 C77 1.752(15) . ? S15 C76 1.754(14) . ? S3 C4 1.734(14) . ? S3 C5 1.739(16) . ? S14 C73 1.757(13) . ? S14 C75 1.764(16) . ? P4 C59 1.802(16) . ? P4 C53 1.828(16) . ? P4 C10 1.855(15) . ? S11 C68 1.753(15) . ? S11 C70 1.766(15) . ? S6 C9 1.761(15) . ? S6 C11 1.786(17) . ? P2 C35 1.806(17) . ? P2 C29 1.824(17) . ? P2 C2 1.827(15) . ? P1 C23 1.796(16) . ? P1 C17 1.815(15) . ? P1 C1 1.853(15) . ? S9 C65 1.761(15) . ? S9 C67 1.803(16) . ? P8 C74 1.804(14) . ? P8 C116 1.819(16) . ? P8 C122 1.828(15) . ? P6 C93 1.799(17) . ? P6 C65 1.820(14) . ? P6 C98 1.824(16) . ? P5 C87 1.807(19) . ? P5 C81 1.818(17) . ? P5 C66 1.844(14) . ? S7 C12 1.709(17) . ? S7 C14 1.744(17) . ? S4 C4 1.746(16) . ? S4 C6 1.746(16) . ? S8 C13 1.731(16) . ? S8 C12 1.753(16) . ? S12 C68 1.750(15) . ? S12 C69 1.755(15) . ? S5 C10 1.751(15) . ? S5 C11 1.789(17) . ? C73 C74 1.373(19) . ? C9 C10 1.307(19) . ? C77 C78 1.36(2) . ? C77 C79 1.503(19) . ? C6 C5 1.363(19) . ? C6 C8 1.50(2) . ? C22 C17 1.399(19) . ? C22 C21 1.43(2) . ? C120 C121 1.38(2) . ? C120 C119 1.40(3) . ? C5 C7 1.48(2) . ? N2 C142 1.11(2) . ? N11 C132 1.11(2) . ? C18 C19 1.37(2) . ? C18 C17 1.40(2) . ? C104 C109 1.38(2) . ? C104 C105 1.407(19) . ? C57 C56 1.36(2) . ? C57 C58 1.42(2) . ? C59 C60 1.40(2) . ? C59 C64 1.41(2) . ? C14 C13 1.36(2) . ? C14 C16 1.480(19) . ? C101 C100 1.37(2) . ? C101 C102 1.38(2) . ? C116 C121 1.337(19) . ? C116 C117 1.44(2) . ? N4 C134 1.09(2) . ? C24 C25 1.38(2) . ? C24 C23 1.425(18) . ? C21 C20 1.36(2) . ? C113 C114 1.36(2) . ? C113 C112 1.40(2) . ? C70 C69 1.305(19) . ? C70 C72 1.500(19) . ? C122 C127 1.357(19) . ? C122 C123 1.40(2) . ? C4 C3 1.345(19) . ? C112 C111 1.36(2) . ? C114 C115 1.40(2) . ? C110 C111 1.376(19) . ? C110 C115 1.381(19) . ? C12 C11 1.33(2) . ? C26 C25 1.35(2) . ? C26 C27 1.37(2) . ? C96 C95 1.37(2) . ? C96 C97 1.40(2) . ? C69 C71 1.55(2) . ? C67 C68 1.331(18) . ? C91 C90 1.36(3) . ? C91 C92 1.40(3) . ? C78 C80 1.505(19) . ? C60 C61 1.40(2) . ? C50 C97 1.41(2) . ? C50 C93 1.41(2) . ? C40 C35 1.36(2) . ? C40 C39 1.38(2) . ? C2 C1 1.335(19) . ? C64 C63 1.33(2) . ? C42 C41 1.27(2) . ? C42 C43 1.36(2) . ? C118 C119 1.32(3) . ? C118 C117 1.37(2) . ? C23 C28 1.414(19) . ? C35 C36 1.40(2) . ? C95 C94 1.38(2) . ? C76 C75 1.326(17) . ? C126 C125 1.37(2) . ? C126 C127 1.41(2) . ? C124 C125 1.37(2) . ? C124 C123 1.42(2) . ? C66 C65 1.336(18) . ? C19 C20 1.39(2) . ? C29 C34 1.39(2) . ? C29 C30 1.40(2) . ? C100 C99 1.33(2) . ? C90 C89 1.36(3) . ? C30 C31 1.42(2) . ? C54 C53 1.37(2) . ? C54 C55 1.40(2) . ? C31 C32 1.35(2) . ? N1 C144 1.10(2) . ? C34 C33 1.37(2) . ? C32 C33 1.39(3) . ? C13 C15 1.51(2) . ? C58 C53 1.37(2) . ? C61 C62 1.37(2) . ? C41 C46 1.40(2) . ? C102 C103 1.40(2) . ? C85 C84 1.35(2) . ? C85 C86 1.38(2) . ? C47 C52 1.38(2) . ? C47 C48 1.49(2) . ? C37 C36 1.37(2) . ? C37 C38 1.38(3) . ? C43 C44 1.33(2) . ? C82 C83 1.41(2) . ? C82 C81 1.43(2) . ? C83 C84 1.40(2) . ? C109 C108 1.39(2) . ? C93 C94 1.451(19) . ? C45 C44 1.38(2) . ? C45 C46 1.46(2) . ? C27 C28 1.38(2) . ? C86 C81 1.36(2) . ? C135 C134 1.54(3) . ? C98 C103 1.38(2) . ? C98 C99 1.38(2) . ? C87 C92 1.37(2) . ? C87 C88 1.38(2) . ? C106 C107 1.36(2) . ? C106 C105 1.40(2) . ? C144 C145 1.42(3) . ? C52 C51 1.37(2) . ? C89 C88 1.44(2) . ? C55 C56 1.38(2) . ? C148 C51 1.38(2) . ? C148 C49 1.39(2) . ? C108 C107 1.34(2) . ? C62 C63 1.37(2) . ? C49 C48 1.38(2) . ? C146 N3 1.10(5) . ? C146 C147 1.41(5) . ? C39 C38 1.37(3) . ? C133 C132 1.46(3) . ? Sb1 F3 1.726(15) . ? Sb1 F2 1.791(14) . ? Sb1 F4 1.801(11) . ? Sb1 F1 1.806(10) . ? Sb1 F6 1.829(10) . ? Sb1 F5 1.910(12) . ? N10 C128 1.117(19) . ? N8 C130 1.14(2) . ? C131 C130 1.44(2) . ? C129 C128 1.44(2) . ? N5 C136 1.12(2) . ? C137 C136 1.50(3) . ? C138 N6 1.15(2) . ? C138 C139 1.43(3) . ? C149 N9 1.17(3) . ? C149 C141 1.45(3) . ? C150 C140 1.27(3) . ? C140 N7 1.37(3) . ? C142 C143 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 P3 Ag1 P1 130.83(15) . . ? P3 Ag1 P4 84.62(14) . . ? P1 Ag1 P4 123.50(14) . . ? P3 Ag1 P2 117.13(14) . . ? P1 Ag1 P2 82.88(13) . . ? P4 Ag1 P2 122.88(15) . . ? P8 Ag2 P5 127.49(15) . . ? P8 Ag2 P6 128.53(16) . . ? P5 Ag2 P6 83.95(14) . . ? P8 Ag2 P7 83.24(14) . . ? P5 Ag2 P7 130.80(15) . . ? P6 Ag2 P7 106.89(14) . . ? F7 Sb2 F10 94.6(7) . . ? F7 Sb2 F8 176.4(8) . . ? F10 Sb2 F8 89.0(6) . . ? F7 Sb2 F9 94.4(9) . . ? F10 Sb2 F9 88.7(6) . . ? F8 Sb2 F9 85.4(8) . . ? F7 Sb2 F11 89.3(8) . . ? F10 Sb2 F11 94.8(6) . . ? F8 Sb2 F11 90.7(7) . . ? F9 Sb2 F11 174.7(8) . . ? F7 Sb2 F12 86.9(7) . . ? F10 Sb2 F12 177.9(5) . . ? F8 Sb2 F12 89.5(6) . . ? F9 Sb2 F12 89.8(6) . . ? F11 Sb2 F12 86.6(5) . . ? C47 P3 C41 107.8(9) . . ? C47 P3 C9 100.8(7) . . ? C41 P3 C9 99.6(8) . . ? C47 P3 Ag1 124.7(6) . . ? C41 P3 Ag1 116.0(7) . . ? C9 P3 Ag1 103.3(5) . . ? C1 S1 C3 95.6(8) . . ? C2 S2 C3 95.5(8) . . ? C67 S10 C66 96.6(7) . . ? C110 P7 C73 104.4(7) . . ? C110 P7 C104 104.2(7) . . ? C73 P7 C104 106.4(7) . . ? C110 P7 Ag2 110.0(5) . . ? C73 P7 Ag2 102.0(5) . . ? C104 P7 Ag2 127.7(5) . . ? C74 S13 C75 96.0(7) . . ? C76 S16 C78 96.1(8) . . ? C77 S15 C76 94.8(7) . . ? C4 S3 C5 96.8(8) . . ? C73 S14 C75 96.0(7) . . ? C59 P4 C53 105.0(8) . . ? C59 P4 C10 101.5(8) . . ? C53 P4 C10 105.6(7) . . ? C59 P4 Ag1 117.9(5) . . ? C53 P4 Ag1 121.1(6) . . ? C10 P4 Ag1 103.3(5) . . ? C68 S11 C70 95.5(8) . . ? C9 S6 C11 95.5(8) . . ? C35 P2 C29 104.7(9) . . ? C35 P2 C2 102.0(7) . . ? C29 P2 C2 103.7(8) . . ? C35 P2 Ag1 118.2(6) . . ? C29 P2 Ag1 123.3(6) . . ? C2 P2 Ag1 101.8(5) . . ? C23 P1 C17 105.8(7) . . ? C23 P1 C1 101.6(7) . . ? C17 P1 C1 103.3(7) . . ? C23 P1 Ag1 127.7(6) . . ? C17 P1 Ag1 112.3(5) . . ? C1 P1 Ag1 102.9(5) . . ? C65 S9 C67 94.8(7) . . ? C74 P8 C116 104.2(7) . . ? C74 P8 C122 102.1(7) . . ? C116 P8 C122 106.7(7) . . ? C74 P8 Ag2 104.2(6) . . ? C116 P8 Ag2 117.8(5) . . ? C122 P8 Ag2 119.4(6) . . ? C93 P6 C65 107.8(7) . . ? C93 P6 C98 105.6(8) . . ? C65 P6 C98 102.9(7) . . ? C93 P6 Ag2 122.8(5) . . ? C65 P6 Ag2 102.7(6) . . ? C98 P6 Ag2 113.1(6) . . ? C87 P5 C81 103.8(9) . . ? C87 P5 C66 106.8(8) . . ? C81 P5 C66 101.6(7) . . ? C87 P5 Ag2 115.0(5) . . ? C81 P5 Ag2 124.5(7) . . ? C66 P5 Ag2 103.2(5) . . ? C12 S7 C14 95.4(8) . . ? C4 S4 C6 94.6(8) . . ? C13 S8 C12 94.6(8) . . ? C68 S12 C69 95.1(8) . . ? C10 S5 C11 95.6(8) . . ? C74 C73 S14 117.3(11) . . ? C74 C73 P7 122.7(10) . . ? S14 C73 P7 119.8(9) . . ? C10 C9 S6 117.7(13) . . ? C10 C9 P3 124.6(12) . . ? S6 C9 P3 117.6(9) . . ? C78 C77 C79 127.5(15) . . ? C78 C77 S15 116.9(12) . . ? C79 C77 S15 115.6(12) . . ? C5 C6 C8 127.2(14) . . ? C5 C6 S4 118.6(12) . . ? C8 C6 S4 114.2(12) . . ? C17 C22 C21 120.0(16) . . ? C121 C120 C119 119(2) . . ? C6 C5 C7 127.4(15) . . ? C6 C5 S3 114.9(12) . . ? C7 C5 S3 117.6(12) . . ? C73 C74 S13 116.1(10) . . ? C73 C74 P8 122.0(11) . . ? S13 C74 P8 121.6(10) . . ? C19 C18 C17 119.5(16) . . ? C109 C104 C105 122.4(17) . . ? C109 C104 P7 115.2(13) . . ? C105 C104 P7 122.4(13) . . ? C56 C57 C58 118.3(19) . . ? C60 C59 C64 118.3(16) . . ? C60 C59 P4 118.6(13) . . ? C64 C59 P4 122.9(15) . . ? C13 C14 C16 126.2(16) . . ? C13 C14 S7 116.3(13) . . ? C16 C14 S7 117.3(13) . . ? C100 C101 C102 119(2) . . ? C121 C116 C117 119.1(16) . . ? C121 C116 P8 122.4(14) . . ? C117 C116 P8 117.7(13) . . ? C25 C24 C23 120.3(15) . . ? C20 C21 C22 118.9(17) . . ? C114 C113 C112 118.0(17) . . ? C69 C70 C72 127.4(14) . . ? C69 C70 S11 116.8(11) . . ? C72 C70 S11 115.8(12) . . ? C127 C122 C123 120.1(16) . . ? C127 C122 P8 117.6(13) . . ? C123 C122 P8 122.3(13) . . ? C3 C4 S3 121.2(12) . . ? C3 C4 S4 123.8(11) . . ? S3 C4 S4 115.0(9) . . ? C111 C112 C113 119.2(17) . . ? C113 C114 C115 122.2(18) . . ? C111 C110 C115 117.1(15) . . ? C111 C110 P7 120.4(13) . . ? C115 C110 P7 121.9(13) . . ? C11 C12 S7 124.5(13) . . ? C11 C12 S8 120.0(14) . . ? S7 C12 S8 115.4(10) . . ? C25 C26 C27 122.9(18) . . ? C95 C96 C97 120.8(17) . . ? C70 C69 C71 127.7(14) . . ? C70 C69 S12 118.5(12) . . ? C71 C69 S12 113.7(13) . . ? C68 C67 S10 127.8(12) . . ? C68 C67 S9 118.4(12) . . ? S10 C67 S9 113.7(9) . . ? C90 C91 C92 122(3) . . ? C77 C78 C80 125.9(15) . . ? C77 C78 S16 116.5(12) . . ? C80 C78 S16 117.4(13) . . ? C61 C60 C59 119.2(18) . . ? C97 C50 C93 121.3(16) . . ? C9 C10 S5 118.2(12) . . ? C9 C10 P4 123.5(13) . . ? S5 C10 P4 118.2(9) . . ? C35 C40 C39 121.2(19) . . ? C1 C2 S2 115.7(11) . . ? C1 C2 P2 124.0(12) . . ? S2 C2 P2 120.3(9) . . ? C63 C64 C59 119.4(19) . . ? C41 C42 C43 128(2) . . ? C67 C68 S12 124.2(12) . . ? C67 C68 S11 121.8(12) . . ? S12 C68 S11 114.0(8) . . ? C22 C17 C18 119.3(15) . . ? C22 C17 P1 118.8(13) . . ? C18 C17 P1 121.6(12) . . ? C119 C118 C117 125(2) . . ? C28 C23 C24 117.2(15) . . ? C28 C23 P1 119.3(12) . . ? C24 C23 P1 123.3(13) . . ? C40 C35 C36 117.0(17) . . ? C40 C35 P2 119.5(15) . . ? C36 C35 P2 123.4(15) . . ? C96 C95 C94 121.6(16) . . ? C75 C76 S16 123.0(12) . . ? C75 C76 S15 122.4(12) . . ? S16 C76 S15 114.6(8) . . ? C4 C3 S1 123.3(11) . . ? C4 C3 S2 123.1(11) . . ? S1 C3 S2 113.5(10) . . ? C125 C126 C127 120.3(16) . . ? C12 C11 S6 123.7(13) . . ? C12 C11 S5 124.9(13) . . ? S6 C11 S5 111.5(10) . . ? C110 C115 C114 119.7(16) . . ? C125 C124 C123 118.4(18) . . ? C65 C66 S10 118.2(11) . . ? C65 C66 P5 121.9(10) . . ? S10 C66 P5 119.9(8) . . ? C18 C19 C20 121.3(17) . . ? C76 C75 S14 124.2(12) . . ? C76 C75 S13 123.7(12) . . ? S14 C75 S13 112.0(8) . . ? C34 C29 C30 119.7(16) . . ? C34 C29 P2 120.3(16) . . ? C30 C29 P2 119.8(14) . . ? C99 C100 C101 120(2) . . ? C91 C90 C89 123(3) . . ? C2 C1 S1 119.7(11) . . ? C2 C1 P1 122.1(12) . . ? S1 C1 P1 118.2(9) . . ? C29 C30 C31 117.8(17) . . ? C53 C54 C55 118.6(17) . . ? C32 C31 C30 120(2) . . ? C33 C34 C29 122.5(19) . . ? C112 C111 C110 123.6(17) . . ? C31 C32 C33 123.0(19) . . ? C14 C13 C15 128.0(16) . . ? C14 C13 S8 117.3(14) . . ? C15 C13 S8 114.7(13) . . ? C66 C65 S9 116.7(11) . . ? C66 C65 P6 123.6(11) . . ? S9 C65 P6 119.3(10) . . ? C53 C58 C57 121.0(19) . . ? C62 C61 C60 122(2) . . ? C42 C41 C46 114.8(19) . . ? C42 C41 P3 130.8(18) . . ? C46 C41 P3 112.2(15) . . ? C101 C102 C103 120.6(18) . . ? C84 C85 C86 120.5(19) . . ? C52 C47 C48 114.8(16) . . ? C52 C47 P3 122.4(15) . . ? C48 C47 P3 122.6(14) . . ? C126 C125 C124 121.4(18) . . ? C34 C33 C32 116.6(18) . . ? C36 C37 C38 120(2) . . ? C44 C43 C42 120(2) . . ? C83 C82 C81 117.6(18) . . ? C84 C83 C82 119.3(18) . . ? C104 C109 C108 117.5(16) . . ? C50 C93 C94 117.4(15) . . ? C50 C93 P6 117.7(13) . . ? C94 C93 P6 124.4(12) . . ? C122 C127 C126 119.7(16) . . ? C44 C45 C46 118(2) . . ? C26 C27 C28 119.0(17) . . ? C81 C86 C85 120.5(17) . . ? C37 C36 C35 122(2) . . ? C26 C25 C24 119.7(15) . . ? C96 C97 C50 118.9(16) . . ? C103 C98 C99 117.3(16) . . ? C103 C98 P6 124.8(14) . . ? C99 C98 P6 117.9(15) . . ? C86 C81 C82 120.6(16) . . ? C86 C81 P5 119.0(15) . . ? C82 C81 P5 120.4(16) . . ? C100 C99 C98 123.6(19) . . ? C118 C119 C120 118(2) . . ? C58 C53 C54 120.4(16) . . ? C58 C53 P4 116.7(14) . . ? C54 C53 P4 122.8(13) . . ? C92 C87 C88 119.5(19) . . ? C92 C87 P5 116.8(16) . . ? C88 C87 P5 123.0(15) . . ? C122 C123 C124 120.0(16) . . ? C107 C106 C105 121.3(17) . . ? C27 C28 C23 120.9(15) . . ? N1 C144 C145 176(3) . . ? C98 C103 C102 119.7(18) . . ? C51 C52 C47 127.4(18) . . ? C85 C84 C83 121.5(19) . . ? C95 C94 C93 119.9(15) . . ? C90 C89 C88 115(2) . . ? C56 C55 C54 121.2(19) . . ? C51 C148 C49 123(2) . . ? C21 C20 C19 120.9(17) . . ? C107 C108 C109 121.6(18) . . ? N4 C134 C135 175(3) . . ? C61 C62 C63 117(2) . . ? C52 C51 C148 115.8(18) . . ? C48 C49 C148 120.5(19) . . ? C64 C63 C62 124(2) . . ? C87 C88 C89 122.6(19) . . ? C118 C117 C116 116.1(17) . . ? C43 C44 C45 119(2) . . ? C57 C56 C55 120.3(19) . . ? N3 C146 C147 176(5) . . ? C38 C39 C40 121(2) . . ? C41 C46 C45 120.0(19) . . ? C49 C48 C47 118.7(18) . . ? C106 C105 C104 116.2(16) . . ? C87 C92 C91 118(2) . . ? C39 C38 C37 119(2) . . ? N11 C132 C133 177(3) . . ? C108 C107 C106 120.8(19) . . ? F3 Sb1 F2 89.2(9) . . ? F3 Sb1 F4 93.8(8) . . ? F2 Sb1 F4 88.0(7) . . ? F3 Sb1 F1 92.4(7) . . ? F2 Sb1 F1 177.5(8) . . ? F4 Sb1 F1 90.1(6) . . ? F3 Sb1 F6 91.8(7) . . ? F2 Sb1 F6 90.8(6) . . ? F4 Sb1 F6 174.3(7) . . ? F1 Sb1 F6 91.0(6) . . ? F3 Sb1 F5 177.7(8) . . ? F2 Sb1 F5 92.9(8) . . ? F4 Sb1 F5 87.0(8) . . ? F1 Sb1 F5 85.5(5) . . ? F6 Sb1 F5 87.4(6) . . ? N8 C130 C131 177(2) . . ? N5 C136 C137 174(3) . . ? N6 C138 C139 178(3) . . ? N9 C149 C141 174(3) . . ? C150 C140 N7 177(3) . . ? N2 C142 C143 176(2) . . ? N10 C128 C129 175(2) . . ? C116 C121 C120 122.3(18) . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 55.57 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 1.758 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.130 # Attachment 'fep22.txt' data_fep22_final _database_code_depnum_ccdc_archive 'CCDC 615881' _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and [Fe(MeCN)6][BF4]2 produced the the complex [Fe(o-P2)2(MECN)2][BF4]2 where the iron metal center displays distorted octahedral geometry. The complex was analyzed by several physical methods including x-ray crystallography, NMR, IR, magnetism, and cyclic voltammetry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H58 B2 F8 Fe N2 P4 S8' _chemical_formula_weight 1512.99 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.440(5) _cell_length_b 13.500(5) _cell_length_c 21.500(5) _cell_angle_alpha 89.000(5) _cell_angle_beta 89.000(5) _cell_angle_gamma 79.000(5) _cell_volume 3259(2) _cell_formula_units_Z 2 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.427 _exptl_crystal_size_mid 0.227 _exptl_crystal_size_min 0.023 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 293(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 'Bruker SMART 1000' _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 21119 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.2739 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.46 _reflns_number_total 13403 _reflns_number_gt 5342 _reflns_threshold_expression I>2s(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.0235P)^2^+0.0000P] 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 13403 _refine_ls_number_parameters 1070 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1672 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 0.759 _refine_ls_restrained_S_all 0.759 _refine_ls_shift/su_max 2.322 _refine_ls_shift/su_mean 0.018 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 S6 S 1.36197(13) -0.25945(12) 1.04220(7) 0.0188(4) Uani 1 1 d . . . S2 S 0.86184(13) 0.24036(13) 0.45776(7) 0.0203(4) Uani 1 1 d . . . P1 P 0.62918(13) 0.44439(13) 0.58326(7) 0.0154(4) Uani 1 1 d . . . S1 S 0.81593(13) 0.24039(13) 0.59369(7) 0.0206(4) Uani 1 1 d . . . S4 S 1.11884(13) 0.07983(13) 0.48437(7) 0.0220(4) Uani 1 1 d . . . P4 P 1.15786(13) -0.07085(13) 1.06118(7) 0.0154(4) Uani 1 1 d . . . S8 S 1.61885(13) -0.42034(13) 1.01541(7) 0.0213(4) Uani 1 1 d . . . P3 P 1.12895(13) -0.05519(13) 0.91661(7) 0.0148(4) Uani 1 1 d . . . S7 S 1.55422(13) -0.41751(13) 0.88264(7) 0.0236(4) Uani 1 1 d . . . P2 P 0.65821(13) 0.42919(13) 0.43878(7) 0.0158(4) Uani 1 1 d . . . S5 S 1.31619(13) -0.25915(12) 0.90626(7) 0.0196(4) Uani 1 1 d . . . S3 S 1.05442(13) 0.08249(13) 0.61725(7) 0.0246(4) Uani 1 1 d . . . C2 C 0.7501(5) 0.3357(4) 0.4879(3) 0.0147(14) Uani 1 1 d . . . C10 C 1.2489(5) -0.1653(5) 1.0125(3) 0.0147(14) Uani 1 1 d . . . C14 C 1.7228(5) -0.4900(5) 0.9634(3) 0.0187(15) Uani 1 1 d . . . C11 C 1.4146(5) -0.3035(4) 0.9683(3) 0.0164(15) Uani 1 1 d . . . C4 C 1.0152(5) 0.1278(5) 0.5422(3) 0.0193(16) Uani 1 1 d . . . C201 C 0.6365(5) 0.3583(5) 0.3694(3) 0.0170(15) Uani 1 1 d . . . C411 C 1.2575(5) 0.0127(5) 1.0847(3) 0.0169(15) Uani 1 1 d . . . C1 C 0.7282(5) 0.3370(4) 0.5501(3) 0.0173(15) Uani 1 1 d . . . C12 C 1.5149(5) -0.3713(5) 0.9576(3) 0.0174(15) Uani 1 1 d . . . C102 C 0.5484(5) 0.2931(5) 0.6541(3) 0.0192(16) Uani 1 1 d . . . F1 F 0.8790(3) 0.5575(3) 0.21028(17) 0.0578(14) Uani 1 1 d . . . C13 C 1.6943(5) -0.4875(5) 0.9033(3) 0.0218(16) Uani 1 1 d . . . C316 C 1.0489(5) -0.2073(5) 0.8467(3) 0.0194(16) Uani 1 1 d . . . C213 C 0.9160(6) 0.6019(6) 0.4425(3) 0.034(2) Uani 1 1 d . . . C311 C 1.0660(5) -0.1067(5) 0.8478(3) 0.0166(15) Uani 1 1 d . . . C101 C 0.5677(5) 0.3931(5) 0.6515(3) 0.0172(15) Uani 1 1 d . . . C6 C 1.2230(5) 0.0096(5) 0.5365(3) 0.0215(16) Uani 1 1 d . . . C9 C 1.2308(4) -0.1624(5) 0.9499(3) 0.0174(15) Uani 1 1 d . . . C8 C 1.3344(6) -0.0513(6) 0.5086(3) 0.0297(19) Uani 1 1 d . . . C111 C 0.7353(5) 0.5132(5) 0.6197(3) 0.0175(15) Uani 1 1 d . . . C211 C 0.7576(5) 0.5128(5) 0.4160(3) 0.0197(15) Uani 1 1 d . . . C3 C 0.9136(5) 0.1959(5) 0.5321(3) 0.0185(15) Uani 1 1 d . . . C412 C 1.3487(5) 0.0284(5) 1.0440(3) 0.0229(16) Uani 1 1 d . . . C401 C 1.1362(5) -0.1415(5) 1.1308(3) 0.0181(15) Uani 1 1 d . . . C205 C 0.6855(6) 0.3054(5) 0.2632(3) 0.0264(18) Uani 1 1 d . . . C5 C 1.1938(5) 0.0125(5) 0.5970(3) 0.0213(16) Uani 1 1 d . . . C206 C 0.7103(6) 0.3526(5) 0.3179(3) 0.0210(16) Uani 1 1 d . . . C405 C 1.1858(6) -0.1957(5) 1.2361(3) 0.0261(18) Uani 1 1 d . . . C315 C 0.9938(5) -0.2421(6) 0.7952(3) 0.0242(17) Uani 1 1 d . . . F3 F 0.8614(4) 0.6138(3) 0.11081(19) 0.0626(14) Uani 1 1 d . . . C16 C 1.8358(7) -0.5525(7) 0.9906(4) 0.030(2) Uani 1 1 d . . . C301 C 1.2359(5) 0.0115(5) 0.8810(2) 0.0157(15) Uani 1 1 d . . . C212 C 0.8487(6) 0.5290(6) 0.4556(3) 0.0286(18) Uani 1 1 d . . . F2 F 0.7649(4) 0.4912(4) 0.14215(19) 0.0703(16) Uani 1 1 d . . . C406 C 1.2120(6) -0.1488(5) 1.1831(3) 0.0207(16) Uani 1 1 d . . . C106 C 0.5347(5) 0.4535(5) 0.7043(3) 0.0187(16) Uani 1 1 d . . . C204 C 0.5835(6) 0.2622(5) 0.2610(3) 0.0220(17) Uani 1 1 d . . . C313 C 0.9820(6) -0.0827(6) 0.7452(3) 0.0244(18) Uani 1 1 d . . . C203 C 0.5119(5) 0.2621(5) 0.3115(3) 0.0210(16) Uani 1 1 d . . . B1 B 0.8660(7) 0.5284(7) 0.1509(4) 0.033(2) Uani 1 1 d . . . F4 F 0.9654(4) 0.4592(3) 0.13257(19) 0.0633(14) Uani 1 1 d . . . C312 C 1.0361(5) -0.0460(5) 0.7960(3) 0.0207(16) Uani 1 1 d . . . N2 N 0.9561(4) -0.1298(4) 0.9888(2) 0.0147(12) Uani 1 1 d . . . N1 N 0.4572(4) 0.3705(4) 0.5108(2) 0.0119(12) Uani 1 1 d . . . C1A C 0.4270(5) 0.2964(5) 0.5212(3) 0.0158(15) Uani 1 1 d . . . C116 C 0.7640(5) 0.6005(5) 0.5943(3) 0.0233(17) Uani 1 1 d . . . C416 C 1.2397(6) 0.0682(6) 1.1389(3) 0.0255(18) Uani 1 1 d . . . C415 C 1.3117(6) 0.1407(5) 1.1526(3) 0.0253(18) Uani 1 1 d . . . C216 C 0.7403(6) 0.5688(6) 0.3615(3) 0.0297(19) Uani 1 1 d . . . C113 C 0.8937(6) 0.5103(6) 0.6946(3) 0.0276(18) Uani 1 1 d . . . C112 C 0.8014(5) 0.4691(6) 0.6705(3) 0.0253(17) Uani 1 1 d . . . C314 C 0.9583(6) -0.1775(6) 0.7451(3) 0.0270(18) Uani 1 1 d . . . C215 C 0.8120(6) 0.6408(6) 0.3470(3) 0.0297(19) Uani 1 1 d . . . C414 C 1.3976(7) 0.1551(6) 1.1117(4) 0.032(2) Uani 1 1 d . . . C302 C 1.2643(6) 0.1004(5) 0.9064(3) 0.0230(17) Uani 1 1 d . . . C2A C 0.9268(5) -0.2042(5) 0.9784(3) 0.0146(15) Uani 1 1 d . . . C1B C 0.3819(6) 0.2020(6) 0.5316(4) 0.0258(18) Uani 1 1 d . . . C115 C 0.8557(6) 0.6442(5) 0.6187(3) 0.0279(18) Uani 1 1 d . . . C305 C 1.3948(6) 0.0116(6) 0.8059(3) 0.0267(18) Uani 1 1 d . . . C105 C 0.4818(6) 0.4179(5) 0.7551(3) 0.0235(16) Uani 1 1 d . . . C2B C 0.8822(6) -0.2977(5) 0.9694(4) 0.0230(17) Uani 1 1 d . . . C304 C 1.4202(6) 0.0973(6) 0.8333(3) 0.0293(19) Uani 1 1 d . . . C114 C 0.9201(6) 0.5957(6) 0.6675(3) 0.031(2) Uani 1 1 d . . . C214 C 0.8961(7) 0.6548(6) 0.3890(4) 0.031(2) Uani 1 1 d . . . C202 C 0.5369(5) 0.3105(5) 0.3661(3) 0.0202(16) Uani 1 1 d . . . C306 C 1.3021(6) -0.0320(5) 0.8295(3) 0.0226(17) Uani 1 1 d . . . C104 C 0.4610(6) 0.3241(6) 0.7544(3) 0.0269(18) Uani 1 1 d . . . C404 C 1.0849(6) -0.2381(5) 1.2393(3) 0.0250(18) Uani 1 1 d . . . C413 C 1.4156(7) 0.1012(6) 1.0580(4) 0.033(2) Uani 1 1 d . . . C402 C 1.0392(5) -0.1899(5) 1.1346(3) 0.0180(15) Uani 1 1 d . . . C103 C 0.4943(6) 0.2570(6) 0.7053(3) 0.0275(19) Uani 1 1 d . . . C7 C 1.2636(7) -0.0419(6) 0.6498(4) 0.038(2) Uani 1 1 d . . . C403 C 1.0123(6) -0.2387(5) 1.1884(3) 0.0211(16) Uani 1 1 d . . . C303 C 1.3550(6) 0.1431(6) 0.8816(4) 0.031(2) Uani 1 1 d . . . C15 C 1.7657(7) -0.5424(7) 0.8506(4) 0.037(2) Uani 1 1 d . . . Fe2 Fe 1.0000 0.0000 1.0000 0.0121(3) Uani 1 2 d S . . Fe1 Fe 0.5000 0.5000 0.5000 0.0129(3) Uani 1 2 d S . . F8 F 0.5353(3) 0.0420(3) -0.36712(19) 0.0609(14) Uani 1 1 d . . . F7 F 0.6382(4) -0.1132(4) -0.38922(19) 0.0680(14) Uani 1 1 d . . . F6 F 0.6218(3) -0.0563(4) -0.28911(18) 0.0620(14) Uani 1 1 d . . . F5 F 0.7345(4) 0.0082(4) -0.35710(19) 0.0718(16) Uani 1 1 d . . . B2 B 0.6328(8) -0.0307(8) -0.3495(4) 0.041(3) Uani 1 1 d . . . H203 H 0.429(4) 0.244(3) 0.3090(19) 0.000(13) Uiso 1 1 d . . . H204 H 0.568(4) 0.230(4) 0.226(2) 0.000(13) Uiso 1 1 d . . . H15A H 1.727(4) -0.601(4) 0.828(2) 0.017(15) Uiso 1 1 d . . . H102 H 0.581(4) 0.244(4) 0.618(2) 0.000(13) Uiso 1 1 d . . . H216 H 0.679(4) 0.572(4) 0.334(2) 0.000(13) Uiso 1 1 d . . . H302 H 1.222(4) 0.140(4) 0.940(2) 0.020(17) Uiso 1 1 d . . . H16A H 1.814(5) -0.578(4) 1.019(2) 0.000(18) Uiso 1 1 d . . . H206 H 0.779(4) 0.381(4) 0.319(2) 0.003(14) Uiso 1 1 d . . . H404 H 1.065(4) -0.270(4) 1.273(2) 0.000(14) Uiso 1 1 d . . . H405 H 1.236(4) -0.185(4) 1.273(2) 0.017(15) Uiso 1 1 d . . . H306 H 1.284(5) -0.088(5) 0.804(3) 0.06(2) Uiso 1 1 d . . . H312 H 1.051(4) 0.025(4) 0.799(2) 0.008(14) Uiso 1 1 d . . . H7A H 1.259(6) 0.029(6) 0.689(3) 0.10(3) Uiso 1 1 d . . . H105 H 0.441(4) 0.468(4) 0.792(2) 0.016(15) Uiso 1 1 d . . . H212 H 0.862(4) 0.491(4) 0.501(2) 0.012(14) Uiso 1 1 d . . . H112 H 0.771(4) 0.411(4) 0.689(2) 0.023(18) Uiso 1 1 d . . . H316 H 1.074(4) -0.255(4) 0.885(2) 0.003(13) Uiso 1 1 d . . . H113 H 0.946(4) 0.473(4) 0.728(2) 0.013(15) Uiso 1 1 d . . . H202 H 0.483(4) 0.314(4) 0.403(2) 0.002(14) Uiso 1 1 d . . . H103 H 0.502(5) 0.192(4) 0.708(3) 0.022(19) Uiso 1 1 d . . . H16B H 1.883(4) -0.501(5) 1.023(2) 0.036(18) Uiso 1 1 d . . . H305 H 1.435(5) -0.017(5) 0.774(2) 0.03(2) Uiso 1 1 d . . . H205 H 0.727(5) 0.305(5) 0.223(3) 0.04(2) Uiso 1 1 d . . . H402 H 0.980(4) -0.183(4) 1.101(2) 0.023(16) Uiso 1 1 d . . . H2BC H 0.935(4) -0.336(4) 0.936(2) 0.000(13) Uiso 1 1 d . . . H2BB H 0.884(5) -0.331(5) 1.014(3) 0.05(2) Uiso 1 1 d . . . H2BA H 0.814(5) -0.284(5) 0.952(3) 0.05(2) Uiso 1 1 d . . . H1BB H 0.442(5) 0.166(5) 0.558(2) 0.032(18) Uiso 1 1 d . . . H1BA H 0.382(4) 0.170(4) 0.486(2) 0.021(16) Uiso 1 1 d . . . H106 H 0.552(4) 0.512(4) 0.705(2) 0.010(16) Uiso 1 1 d . . . H8A H 1.331(5) -0.094(5) 0.467(3) 0.04(2) Uiso 1 1 d . . . H115 H 0.882(4) 0.695(4) 0.589(2) 0.006(14) Uiso 1 1 d . . . H104 H 0.417(4) 0.311(4) 0.786(2) 0.004(16) Uiso 1 1 d . . . H15B H 1.844(4) -0.566(4) 0.866(2) 0.014(15) Uiso 1 1 d . . . H304 H 1.475(4) 0.123(4) 0.817(2) 0.001(15) Uiso 1 1 d . . . H114 H 0.977(4) 0.623(4) 0.681(2) 0.004(14) Uiso 1 1 d . . . H313 H 0.947(4) -0.043(4) 0.719(2) 0.013(16) Uiso 1 1 d . . . H403 H 0.930(5) -0.248(5) 1.197(3) 0.05(2) Uiso 1 1 d . . . H415 H 1.294(5) 0.174(5) 1.188(3) 0.03(2) Uiso 1 1 d . . . H315 H 1.000(4) -0.317(4) 0.792(2) 0.018(16) Uiso 1 1 d . . . H412 H 1.368(5) -0.017(5) 0.997(3) 0.07(2) Uiso 1 1 d . . . H116 H 0.715(6) 0.645(5) 0.563(3) 0.08(2) Uiso 1 1 d . . . H7B H 1.343(5) -0.067(5) 0.639(3) 0.04(2) Uiso 1 1 d . . . H213 H 0.965(5) 0.623(5) 0.471(3) 0.05(2) Uiso 1 1 d . . . H413 H 1.470(5) 0.110(5) 1.035(3) 0.03(2) Uiso 1 1 d . . . H16C H 1.879(5) -0.590(5) 0.961(2) 0.023(19) Uiso 1 1 d . . . H8B H 1.383(5) -0.089(5) 0.540(3) 0.034(19) Uiso 1 1 d . . . H214 H 0.941(5) 0.690(5) 0.377(3) 0.02(2) Uiso 1 1 d . . . H303 H 1.364(5) 0.181(5) 0.909(3) 0.03(2) Uiso 1 1 d . . . H414 H 1.427(7) 0.194(6) 1.126(4) 0.09(4) Uiso 1 1 d . . . H314 H 0.916(6) -0.183(6) 0.712(3) 0.10(3) Uiso 1 1 d . . . H215 H 0.803(5) 0.675(5) 0.312(3) 0.05(2) Uiso 1 1 d . . . H406 H 1.279(5) -0.123(5) 1.173(3) 0.03(2) Uiso 1 1 d . . . H15C H 1.764(6) -0.502(6) 0.817(3) 0.07(3) Uiso 1 1 d . . . H416 H 1.175(7) 0.087(7) 1.158(4) 0.10(4) Uiso 1 1 d . . . H1BC H 0.320(7) 0.220(8) 0.539(4) 0.123 Uiso 1 1 d . . . H7C H 1.243(8) -0.100(7) 0.668(4) 0.123 Uiso 1 1 d . . . H8C H 1.385(7) 0.002(7) 0.480(4) 0.123 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 S6 0.0189(8) 0.0186(10) 0.0178(9) 0.0023(7) -0.0014(7) -0.0011(7) S2 0.0207(9) 0.0194(10) 0.0199(9) 0.0004(8) -0.0033(7) -0.0012(7) P1 0.0160(8) 0.0135(10) 0.0175(9) 0.0023(7) -0.0012(7) -0.0048(7) S1 0.0222(9) 0.0210(10) 0.0179(9) 0.0067(8) -0.0028(7) -0.0023(8) S4 0.0228(9) 0.0200(11) 0.0233(9) 0.0016(8) -0.0007(7) -0.0042(8) P4 0.0168(8) 0.0152(10) 0.0146(9) 0.0006(7) 0.0003(7) -0.0044(7) S8 0.0205(9) 0.0195(10) 0.0229(9) 0.0011(8) -0.0029(7) -0.0009(7) P3 0.0150(8) 0.0128(10) 0.0174(9) 0.0007(7) -0.0021(7) -0.0045(7) S7 0.0218(9) 0.0228(11) 0.0234(9) -0.0042(8) -0.0015(7) 0.0029(8) P2 0.0167(8) 0.0149(10) 0.0169(9) 0.0045(7) -0.0021(7) -0.0060(7) S5 0.0199(8) 0.0183(10) 0.0195(9) -0.0025(8) -0.0023(7) -0.0002(7) S3 0.0244(9) 0.0234(11) 0.0234(9) 0.0061(8) -0.0033(8) 0.0019(8) C2 0.013(3) 0.013(4) 0.019(3) 0.006(3) -0.005(3) -0.006(3) C10 0.012(3) 0.016(4) 0.019(3) 0.002(3) 0.005(3) -0.009(3) C14 0.017(3) 0.010(4) 0.029(4) -0.001(3) 0.000(3) -0.002(3) C11 0.017(3) 0.010(4) 0.023(4) 0.003(3) 0.001(3) -0.004(3) C4 0.015(3) 0.024(4) 0.020(4) 0.000(3) -0.002(3) -0.007(3) C201 0.022(3) 0.015(4) 0.013(3) 0.002(3) 0.003(3) -0.002(3) C411 0.020(3) 0.015(4) 0.016(3) 0.002(3) -0.001(3) -0.002(3) C1 0.015(3) 0.013(4) 0.026(4) 0.000(3) -0.003(3) -0.010(3) C12 0.017(3) 0.014(4) 0.021(4) 0.001(3) 0.004(3) -0.003(3) C102 0.024(4) 0.019(4) 0.014(4) -0.001(3) 0.002(3) -0.004(3) F1 0.066(3) 0.074(4) 0.035(3) -0.007(2) -0.015(2) -0.016(3) C13 0.020(3) 0.019(4) 0.025(4) -0.003(3) 0.004(3) 0.000(3) C316 0.016(3) 0.020(4) 0.020(4) -0.002(3) -0.002(3) 0.001(3) C213 0.033(4) 0.042(5) 0.033(5) 0.004(4) -0.003(4) -0.021(4) C311 0.014(3) 0.021(4) 0.016(3) -0.002(3) 0.001(3) -0.003(3) C101 0.010(3) 0.020(4) 0.022(4) 0.004(3) -0.007(3) -0.005(3) C6 0.024(4) 0.007(4) 0.032(4) 0.004(3) -0.009(3) -0.001(3) C9 0.011(3) 0.020(4) 0.024(4) 0.001(3) 0.002(3) -0.013(3) C8 0.024(4) 0.031(5) 0.031(5) 0.005(4) 0.003(3) 0.000(3) C111 0.018(3) 0.017(4) 0.018(3) -0.002(3) 0.000(3) -0.006(3) C211 0.022(3) 0.019(4) 0.020(4) 0.007(3) 0.000(3) -0.009(3) C3 0.018(3) 0.022(4) 0.019(3) 0.005(3) -0.004(3) -0.010(3) C412 0.022(4) 0.022(4) 0.027(4) 0.003(3) -0.001(3) -0.011(3) C401 0.022(3) 0.018(4) 0.014(3) -0.002(3) 0.004(3) -0.004(3) C205 0.031(4) 0.033(5) 0.018(4) -0.004(4) 0.010(3) -0.010(4) C5 0.021(3) 0.019(4) 0.022(4) 0.004(3) -0.003(3) 0.000(3) C206 0.024(4) 0.024(4) 0.017(4) 0.002(3) 0.000(3) -0.010(3) C405 0.027(4) 0.041(5) 0.013(4) 0.011(3) 0.002(3) -0.014(4) C315 0.029(4) 0.028(5) 0.013(4) -0.006(3) -0.002(3) 0.000(3) F3 0.099(4) 0.037(3) 0.056(3) 0.010(2) -0.024(3) -0.021(3) C16 0.026(5) 0.033(6) 0.028(5) 0.007(4) -0.002(4) 0.003(4) C301 0.017(3) 0.019(4) 0.011(3) 0.005(3) -0.001(3) -0.004(3) C212 0.027(4) 0.030(5) 0.030(4) 0.008(4) -0.001(3) -0.008(3) F2 0.059(3) 0.109(5) 0.054(3) -0.004(3) -0.004(2) -0.043(3) C406 0.021(4) 0.029(4) 0.014(4) 0.005(3) -0.001(3) -0.010(3) C106 0.019(4) 0.021(4) 0.018(4) -0.004(3) -0.001(3) -0.008(3) C204 0.033(4) 0.023(4) 0.011(4) -0.002(3) 0.001(3) -0.008(3) C313 0.035(4) 0.024(4) 0.011(4) 0.003(3) -0.010(3) 0.002(3) C203 0.022(4) 0.017(4) 0.025(4) 0.006(3) -0.008(3) -0.005(3) B1 0.036(5) 0.029(6) 0.034(5) -0.002(4) -0.013(4) -0.006(4) F4 0.067(3) 0.050(4) 0.064(3) 0.000(3) -0.001(2) 0.010(3) C312 0.025(4) 0.012(4) 0.026(4) 0.006(3) -0.006(3) -0.007(3) N2 0.017(3) 0.013(3) 0.012(3) -0.002(2) 0.001(2) 0.000(2) N1 0.011(3) 0.015(3) 0.010(3) 0.003(2) 0.002(2) -0.005(2) C1A 0.014(3) 0.020(4) 0.014(3) 0.000(3) 0.003(3) -0.006(3) C116 0.023(4) 0.028(5) 0.024(4) 0.013(3) -0.009(3) -0.018(3) C416 0.026(4) 0.023(5) 0.028(4) -0.004(3) -0.003(3) -0.005(3) C415 0.032(4) 0.019(4) 0.027(4) 0.000(3) -0.003(4) -0.011(3) C216 0.025(4) 0.033(5) 0.032(4) 0.006(4) -0.002(3) -0.007(4) C113 0.026(4) 0.038(5) 0.021(4) -0.004(4) -0.006(3) -0.009(4) C112 0.023(4) 0.031(5) 0.024(4) 0.008(3) -0.008(3) -0.011(3) C314 0.031(4) 0.027(5) 0.023(4) -0.010(3) -0.004(3) -0.005(3) C215 0.032(4) 0.030(5) 0.026(4) 0.009(4) 0.004(4) -0.004(4) C414 0.036(5) 0.038(5) 0.025(4) 0.014(4) -0.014(4) -0.014(4) C302 0.023(4) 0.022(4) 0.028(4) -0.004(3) 0.005(3) -0.012(3) C2A 0.012(3) 0.018(4) 0.014(3) 0.002(3) 0.004(3) -0.002(3) C1B 0.031(4) 0.016(4) 0.034(4) 0.008(3) -0.008(4) -0.013(4) C115 0.028(4) 0.024(5) 0.037(5) 0.007(4) -0.005(3) -0.018(3) C305 0.027(4) 0.031(5) 0.022(4) 0.004(4) 0.005(3) -0.007(4) C105 0.036(4) 0.021(4) 0.014(4) -0.007(3) 0.007(3) -0.007(3) C2B 0.024(4) 0.016(4) 0.032(5) -0.005(4) 0.004(4) -0.010(3) C304 0.021(4) 0.034(5) 0.035(5) 0.015(4) 0.010(4) -0.012(4) C114 0.027(4) 0.027(5) 0.043(5) -0.012(4) -0.010(4) -0.012(4) C214 0.030(5) 0.037(5) 0.029(5) 0.003(4) 0.016(4) -0.016(4) C202 0.026(4) 0.014(4) 0.022(4) 0.006(3) -0.005(3) -0.008(3) C306 0.020(4) 0.027(5) 0.020(4) 0.002(3) 0.002(3) -0.004(3) C104 0.028(4) 0.039(5) 0.016(4) 0.005(4) 0.002(3) -0.013(4) C404 0.041(4) 0.022(4) 0.013(4) 0.013(3) 0.007(4) -0.009(3) C413 0.023(4) 0.032(5) 0.049(6) 0.002(4) -0.001(4) -0.018(4) C402 0.023(4) 0.022(4) 0.012(3) 0.002(3) -0.001(3) -0.010(3) C103 0.031(4) 0.024(5) 0.026(4) 0.000(4) -0.004(3) -0.001(4) C7 0.027(4) 0.040(6) 0.041(5) 0.007(4) 0.000(4) 0.009(4) C403 0.025(4) 0.016(4) 0.023(4) 0.000(3) 0.006(3) -0.007(3) C303 0.031(4) 0.027(5) 0.037(5) -0.003(4) 0.009(4) -0.009(4) C15 0.035(5) 0.043(6) 0.029(5) -0.003(4) -0.001(4) 0.003(4) Fe2 0.0115(6) 0.0103(8) 0.0149(7) 0.0009(6) 0.0007(5) -0.0030(5) Fe1 0.0125(6) 0.0109(8) 0.0159(7) 0.0027(6) -0.0022(5) -0.0038(6) F8 0.059(3) 0.058(4) 0.062(3) 0.007(3) -0.014(2) -0.001(3) F7 0.112(4) 0.045(4) 0.047(3) -0.004(3) 0.026(3) -0.019(3) F6 0.070(3) 0.081(4) 0.036(3) 0.018(3) 0.004(2) -0.018(3) F5 0.057(3) 0.114(5) 0.055(3) 0.012(3) -0.004(2) -0.043(3) B2 0.036(5) 0.056(7) 0.038(6) 0.004(5) -0.006(5) -0.025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S6 C10 1.752(6) . ? S6 C11 1.762(6) . ? S2 C2 1.756(6) . ? S2 C3 1.770(5) . ? P1 C101 1.800(6) . ? P1 C1 1.809(6) . ? P1 C111 1.855(6) . ? P1 Fe1 2.3610(15) . ? S1 C3 1.755(6) . ? S1 C1 1.754(6) . ? S4 C4 1.748(6) . ? S4 C6 1.776(5) . ? P4 C401 1.800(6) . ? P4 C10 1.819(6) . ? P4 C411 1.832(6) . ? P4 Fe2 2.2992(15) . ? S8 C14 1.764(6) . ? S8 C12 1.766(5) . ? P3 C301 1.804(6) . ? P3 C9 1.820(6) . ? P3 C311 1.859(5) . ? P3 Fe2 2.3410(16) . ? S7 C12 1.758(6) . ? S7 C13 1.758(6) . ? P2 C211 1.804(7) . ? P2 C2 1.816(5) . ? P2 C201 1.833(6) . ? P2 Fe1 2.2854(17) . ? S5 C9 1.750(6) . ? S5 C11 1.781(5) . ? S3 C5 1.743(6) . ? S3 C4 1.750(6) . ? C2 C1 1.356(7) . ? C10 C9 1.365(7) . ? C14 C13 1.336(7) . ? C14 C16 1.523(8) . ? C11 C12 1.344(7) . ? C4 C3 1.355(7) . ? C201 C206 1.374(8) . ? C201 C202 1.416(8) . ? C411 C412 1.394(8) . ? C411 C416 1.388(8) . ? C102 C103 1.380(9) . ? C102 C101 1.409(8) . ? F1 B1 1.362(8) . ? C13 C15 1.507(9) . ? C316 C311 1.410(8) . ? C316 C315 1.413(7) . ? C213 C214 1.344(10) . ? C213 C212 1.383(10) . ? C311 C312 1.381(8) . ? C101 C106 1.414(8) . ? C6 C5 1.336(8) . ? C6 C8 1.501(8) . ? C111 C116 1.383(8) . ? C111 C112 1.397(8) . ? C211 C216 1.381(8) . ? C211 C212 1.408(7) . ? C412 C413 1.396(9) . ? C401 C402 1.392(8) . ? C401 C406 1.423(7) . ? C205 C204 1.402(8) . ? C205 C206 1.405(8) . ? C5 C7 1.498(8) . ? C405 C406 1.352(9) . ? C405 C404 1.382(9) . ? C315 C314 1.392(9) . ? F3 B1 1.420(9) . ? C301 C306 1.404(8) . ? C301 C302 1.422(8) . ? F2 B1 1.363(9) . ? C106 C105 1.364(9) . ? C204 C203 1.349(8) . ? C313 C314 1.358(10) . ? C313 C312 1.406(8) . ? C203 C202 1.412(8) . ? B1 F4 1.383(8) . ? N2 C2A 1.144(7) . ? N2 Fe2 1.933(5) . ? N1 C1A 1.137(7) . ? N1 Fe1 1.912(5) . ? C1A C1B 1.475(10) . ? C116 C115 1.411(8) . ? C416 C415 1.431(9) . ? C415 C414 1.348(10) . ? C216 C215 1.414(10) . ? C113 C114 1.365(9) . ? C113 C112 1.395(8) . ? C215 C214 1.371(9) . ? C414 C413 1.366(10) . ? C302 C303 1.375(9) . ? C2A C2B 1.466(9) . ? C115 C114 1.376(9) . ? C305 C306 1.392(9) . ? C305 C304 1.390(10) . ? C105 C104 1.333(9) . ? C304 C303 1.355(9) . ? C104 C103 1.403(9) . ? C404 C403 1.386(8) . ? C402 C403 1.381(8) . ? Fe2 N2 1.933(5) 2_757 ? Fe2 P4 2.2992(15) 2_757 ? Fe2 P3 2.3410(16) 2_757 ? Fe1 N1 1.912(5) 2_666 ? Fe1 P2 2.2854(17) 2_666 ? Fe1 P1 2.3610(15) 2_666 ? F8 B2 1.392(9) . ? F7 B2 1.407(10) . ? F6 B2 1.347(9) . ? F5 B2 1.370(9) . ? 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 C10 S6 C11 94.2(3) . . ? C2 S2 C3 93.7(3) . . ? C101 P1 C1 104.0(3) . . ? C101 P1 C111 100.3(3) . . ? C1 P1 C111 102.0(2) . . ? C101 P1 Fe1 117.86(17) . . ? C1 P1 Fe1 102.11(18) . . ? C111 P1 Fe1 127.5(2) . . ? C3 S1 C1 95.4(3) . . ? C4 S4 C6 95.1(3) . . ? C401 P4 C10 102.7(3) . . ? C401 P4 C411 104.3(3) . . ? C10 P4 C411 105.2(3) . . ? C401 P4 Fe2 121.21(19) . . ? C10 P4 Fe2 104.89(18) . . ? C411 P4 Fe2 116.58(19) . . ? C14 S8 C12 95.1(3) . . ? C301 P3 C9 99.3(3) . . ? C301 P3 C311 102.0(3) . . ? C9 P3 C311 104.7(3) . . ? C301 P3 Fe2 126.4(2) . . ? C9 P3 Fe2 103.0(2) . . ? C311 P3 Fe2 117.94(19) . . ? C12 S7 C13 95.6(3) . . ? C211 P2 C2 103.2(3) . . ? C211 P2 C201 106.6(3) . . ? C2 P2 C201 103.5(3) . . ? C211 P2 Fe1 115.1(2) . . ? C2 P2 Fe1 105.5(2) . . ? C201 P2 Fe1 120.9(2) . . ? C9 S5 C11 94.1(3) . . ? C5 S3 C4 96.4(3) . . ? C1 C2 S2 118.7(4) . . ? C1 C2 P2 118.6(4) . . ? S2 C2 P2 122.6(3) . . ? C9 C10 S6 117.9(4) . . ? C9 C10 P4 119.2(4) . . ? S6 C10 P4 122.9(3) . . ? C13 C14 C16 124.7(6) . . ? C13 C14 S8 117.6(4) . . ? C16 C14 S8 117.7(5) . . ? C12 C11 S6 125.0(4) . . ? C12 C11 S5 120.4(4) . . ? S6 C11 S5 114.4(3) . . ? C3 C4 S3 121.1(4) . . ? C3 C4 S4 124.7(4) . . ? S3 C4 S4 114.2(3) . . ? C206 C201 C202 117.2(6) . . ? C206 C201 P2 122.9(5) . . ? C202 C201 P2 119.9(5) . . ? C412 C411 C416 118.3(6) . . ? C412 C411 P4 118.9(4) . . ? C416 C411 P4 122.6(5) . . ? C2 C1 S1 115.7(4) . . ? C2 C1 P1 119.1(4) . . ? S1 C1 P1 124.5(3) . . ? C11 C12 S7 121.6(4) . . ? C11 C12 S8 124.2(4) . . ? S7 C12 S8 114.2(3) . . ? C103 C102 C101 121.2(6) . . ? C14 C13 C15 127.7(6) . . ? C14 C13 S7 117.3(5) . . ? C15 C13 S7 115.0(5) . . ? C311 C316 C315 120.1(6) . . ? C214 C213 C212 118.1(7) . . ? C312 C311 C316 118.6(5) . . ? C312 C311 P3 119.8(5) . . ? C316 C311 P3 121.6(5) . . ? C102 C101 C106 117.6(6) . . ? C102 C101 P1 121.9(5) . . ? C106 C101 P1 120.5(5) . . ? C5 C6 C8 125.5(5) . . ? C5 C6 S4 117.4(4) . . ? C8 C6 S4 117.1(5) . . ? C10 C9 S5 116.8(4) . . ? C10 C9 P3 118.6(4) . . ? S5 C9 P3 124.4(3) . . ? C116 C111 C112 117.4(6) . . ? C116 C111 P1 123.0(4) . . ? C112 C111 P1 119.1(5) . . ? C216 C211 C212 118.0(6) . . ? C216 C211 P2 120.7(5) . . ? C212 C211 P2 121.0(5) . . ? C4 C3 S1 121.2(4) . . ? C4 C3 S2 124.4(4) . . ? S1 C3 S2 114.2(3) . . ? C411 C412 C413 119.2(7) . . ? C402 C401 C406 117.9(6) . . ? C402 C401 P4 118.8(4) . . ? C406 C401 P4 123.3(5) . . ? C204 C205 C206 119.4(6) . . ? C6 C5 C7 127.9(6) . . ? C6 C5 S3 116.7(4) . . ? C7 C5 S3 115.3(5) . . ? C201 C206 C205 121.6(6) . . ? C406 C405 C404 119.6(6) . . ? C314 C315 C316 120.0(7) . . ? C306 C301 C302 118.5(6) . . ? C306 C301 P3 118.2(5) . . ? C302 C301 P3 123.0(5) . . ? C213 C212 C211 121.8(7) . . ? C405 C406 C401 120.7(6) . . ? C105 C106 C101 121.4(7) . . ? C203 C204 C205 120.6(6) . . ? C314 C313 C312 122.0(6) . . ? C204 C203 C202 119.5(6) . . ? F2 B1 F1 113.8(7) . . ? F2 B1 F4 110.6(7) . . ? F1 B1 F4 109.9(6) . . ? F2 B1 F3 107.6(6) . . ? F1 B1 F3 108.4(6) . . ? F4 B1 F3 106.3(7) . . ? C311 C312 C313 120.0(6) . . ? C2A N2 Fe2 175.3(5) . . ? C1A N1 Fe1 174.7(5) . . ? N1 C1A C1B 176.3(6) . . ? C111 C116 C115 121.7(6) . . ? C411 C416 C415 121.1(7) . . ? C414 C415 C416 119.0(8) . . ? C211 C216 C215 120.1(6) . . ? C114 C113 C112 118.9(6) . . ? C113 C112 C111 121.7(7) . . ? C313 C314 C315 119.1(6) . . ? C214 C215 C216 118.4(7) . . ? C415 C414 C413 120.4(8) . . ? C303 C302 C301 121.2(6) . . ? N2 C2A C2B 175.2(7) . . ? C114 C115 C116 118.2(7) . . ? C306 C305 C304 119.8(7) . . ? C104 C105 C106 118.8(7) . . ? C303 C304 C305 122.3(7) . . ? C113 C114 C115 121.9(6) . . ? C213 C214 C215 123.4(8) . . ? C203 C202 C201 121.5(6) . . ? C305 C306 C301 119.2(7) . . ? C105 C104 C103 124.2(8) . . ? C405 C404 C403 122.0(7) . . ? C414 C413 C412 122.0(8) . . ? C403 C402 C401 121.5(5) . . ? C102 C103 C104 116.8(7) . . ? C402 C403 C404 118.0(7) . . ? C304 C303 C302 118.9(7) . . ? N2 Fe2 N2 180.000(1) 2_757 . ? N2 Fe2 P4 88.53(13) 2_757 . ? N2 Fe2 P4 91.47(13) . . ? N2 Fe2 P4 91.47(13) 2_757 2_757 ? N2 Fe2 P4 88.53(13) . 2_757 ? P4 Fe2 P4 180.0 . 2_757 ? N2 Fe2 P3 81.86(14) 2_757 2_757 ? N2 Fe2 P3 98.14(14) . 2_757 ? P4 Fe2 P3 95.14(6) . 2_757 ? P4 Fe2 P3 84.86(6) 2_757 2_757 ? N2 Fe2 P3 98.14(14) 2_757 . ? N2 Fe2 P3 81.86(14) . . ? P4 Fe2 P3 84.86(6) . . ? P4 Fe2 P3 95.14(6) 2_757 . ? P3 Fe2 P3 180.000(1) 2_757 . ? N1 Fe1 N1 180.000(1) 2_666 . ? N1 Fe1 P2 89.75(14) 2_666 2_666 ? N1 Fe1 P2 90.25(14) . 2_666 ? N1 Fe1 P2 90.25(14) 2_666 . ? N1 Fe1 P2 89.75(14) . . ? P2 Fe1 P2 180.00(6) 2_666 . ? N1 Fe1 P1 96.53(13) 2_666 . ? N1 Fe1 P1 83.47(13) . . ? P2 Fe1 P1 95.50(6) 2_666 . ? P2 Fe1 P1 84.50(6) . . ? N1 Fe1 P1 83.47(13) 2_666 2_666 ? N1 Fe1 P1 96.53(13) . 2_666 ? P2 Fe1 P1 84.50(6) 2_666 2_666 ? P2 Fe1 P1 95.50(6) . 2_666 ? P1 Fe1 P1 180.0 . 2_666 ? F6 B2 F5 108.7(6) . . ? F6 B2 F8 110.0(7) . . ? F5 B2 F8 109.1(8) . . ? F6 B2 F7 112.5(8) . . ? F5 B2 F7 109.2(7) . . ? F8 B2 F7 107.2(6) . . ? _diffrn_measured_fraction_theta_max 0.813 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.813 _refine_diff_density_max 0.696 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.103 # Attachment 'nip22_new.txt' data_nip22 _database_code_depnum_ccdc_archive 'CCDC 615882' _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and [Ni(MeCN)6][BF4]2 produced the the complex [Ni(o-P2)2][BF4]2 where the nickel metal center displays square planar geometry. The complex was analyzed by several physical methods including x-ray crystallography, NMR, IR, magnetism, and cyclic voltammetry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H52 Ni P4 S8), 4(C7 H8), C14 H16, 4(B F4)' _chemical_formula_sum 'C170 H152 B4 F16 Ni2 P8 S16' _chemical_formula_weight 3420.42 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' B B 0.0013 0.0007 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.677(2) _cell_length_b 14.3220(13) _cell_length_c 15.4465(13) _cell_angle_alpha 90.00 _cell_angle_beta 127.169(10) _cell_angle_gamma 90.00 _cell_volume 4350.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Platelet _exptl_crystal_colour Brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9223 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. Two independent toluene molecules were located and refined isotropically with restraints on bond distances and angles. Hydrogen atoms were not included in the disordered solvent molecules. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _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 21449 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4411 _reflns_number_gt 2767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.1181P)^2^+0.0000P] 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 4411 _refine_ls_number_parameters 309 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1048 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.007 _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 Ni1 Ni 0.5000 0.0000 0.0000 0.0231(3) Uani 1 4 d S . . S1 S 0.51212(6) -0.10254(9) 0.31713(9) 0.0396(3) Uani 1 1 d . . . S2 S 0.59216(6) -0.10251(10) 0.57949(9) 0.0461(4) Uani 1 1 d . . . P1 P 0.52266(5) -0.10760(7) 0.12451(8) 0.0268(3) Uani 1 1 d . . . F1 F 0.7890(3) 0.0000 1.2056(4) 0.102(2) Uani 1 2 d S . . F2 F 0.6885(3) 0.0000 1.0426(5) 0.0940(18) Uani 1 2 d S . . F3 F 0.7824(4) 0.0280(13) 1.0586(6) 0.137(10) Uani 0.50 1 d P . . F4 F 0.7651(5) -0.1195(7) 1.0877(8) 0.088(3) Uani 0.50 1 d P . . C1 C 0.5159(2) -0.0467(3) 0.2200(3) 0.0324(9) Uani 1 1 d . . . C2 C 0.5349(3) 0.0000 0.3948(4) 0.0351(14) Uani 1 2 d S . . C3 C 0.5683(3) 0.0000 0.5030(5) 0.0380(15) Uani 1 2 d S . . C4 C 0.6446(2) -0.0458(4) 0.7067(3) 0.0505(14) Uani 1 1 d . . . C5 C 0.6830(3) -0.1115(6) 0.8023(4) 0.073(2) Uani 1 1 d . . . H5A H 0.7191 -0.1425 0.8040 0.109 Uiso 1 1 calc R . . H5B H 0.6518 -0.1585 0.7954 0.109 Uiso 1 1 calc R . . H5C H 0.7033 -0.0761 0.8697 0.109 Uiso 1 1 calc R . . C6 C 0.6075(2) -0.1565(3) 0.2060(3) 0.0336(10) Uani 1 1 d . . . C7 C 0.6270(2) -0.2213(3) 0.2886(3) 0.0426(11) Uani 1 1 d . . . H7 H 0.5952 -0.2405 0.3005 0.051 Uiso 1 1 calc R . . C8 C 0.6922(3) -0.2569(4) 0.3524(4) 0.0536(14) Uani 1 1 d . . . H8 H 0.7053 -0.3000 0.4087 0.064 Uiso 1 1 calc R . . C9 C 0.7384(3) -0.2297(5) 0.3344(4) 0.0626(16) Uani 1 1 d . . . H9 H 0.7831 -0.2547 0.3775 0.075 Uiso 1 1 calc R . . C10 C 0.7193(3) -0.1663(5) 0.2538(4) 0.0640(17) Uani 1 1 d . . . H10 H 0.7513 -0.1474 0.2422 0.077 Uiso 1 1 calc R . . C11 C 0.6544(2) -0.1297(4) 0.1895(4) 0.0445(12) Uani 1 1 d . . . H11 H 0.6419 -0.0861 0.1339 0.053 Uiso 1 1 calc R . . C12 C 0.4651(2) -0.2040(3) 0.0856(3) 0.0360(10) Uani 1 1 d . . . C13 C 0.4011(3) -0.1865(5) 0.0571(4) 0.0528(14) Uani 1 1 d . . . H13 H 0.3871 -0.1244 0.0558 0.063 Uiso 1 1 calc R . . C14 C 0.3569(3) -0.2622(7) 0.0301(5) 0.079(2) Uani 1 1 d . . . H14 H 0.3129 -0.2511 0.0111 0.094 Uiso 1 1 calc R . . C15 C 0.3767(5) -0.3509(6) 0.0311(6) 0.099(3) Uani 1 1 d . . . H15 H 0.3468 -0.4017 0.0134 0.119 Uiso 1 1 calc R . . C16 C 0.4388(5) -0.3666(5) 0.0573(7) 0.114(4) Uani 1 1 d . . . H16 H 0.4518 -0.4287 0.0559 0.137 Uiso 1 1 calc R . . C17 C 0.4832(3) -0.2958(4) 0.0855(5) 0.072(2) Uani 1 1 d . . . H17 H 0.5271 -0.3091 0.1054 0.086 Uiso 1 1 calc R . . C1P C 0.2899(9) 0.0000 0.5460(13) 0.072(9) Uani 0.50 2 d SPD A 1 H1P1 H 0.3035 -0.0645 0.5712 0.108 Uiso 0.25 1 calc PR A 1 H1P2 H 0.2791 0.0317 0.5901 0.108 Uiso 0.25 1 calc PR A 1 H1P3 H 0.3272 0.0328 0.5529 0.108 Uiso 0.25 1 calc PR A 1 C2P C 0.2299(9) 0.0000 0.4322(13) 0.053(5) Uani 0.50 2 d SPRD A 1 C3P C 0.2346(9) 0.0001(12) 0.3470(13) 0.070(9) Uani 0.50 2 d SPRD A 1 H3P H 0.2780 0.0001 0.3617 0.084 Uiso 0.50 2 calc SPR A 1 C4P C 0.1754(16) 0.0000 0.239(2) 0.068(6) Uani 0.50 2 d SPD A 1 H4P H 0.1785 0.0000 0.1808 0.081 Uiso 0.50 2 calc SPR A 1 C5P C 0.1124(11) 0.0000 0.218(2) 0.090(8) Uani 0.50 2 d SPD A 1 H5P H 0.0718 0.0000 0.1456 0.107 Uiso 0.50 2 calc SPR A 1 C6P C 0.110(3) 0.0000 0.308(5) 0.101(12) Uani 0.50 2 d SPD A 1 H6P H 0.0679 0.0000 0.2974 0.121 Uiso 0.50 2 calc SPR A 1 C7P C 0.1640(18) 0.0000 0.400(4) 0.076(9) Uani 0.50 2 d SPD A 1 H7P H 0.1599 0.0000 0.4573 0.091 Uiso 0.50 2 calc SPR A 1 C1Q C 0.1493(11) 0.0000 0.2035(14) 0.17(3) Uani 0.50 2 d SPD B 2 H1Q1 H 0.1579 0.0602 0.1837 0.256 Uiso 0.25 1 calc PR B 2 H1Q2 H 0.1002 -0.0099 0.1612 0.256 Uiso 0.25 1 calc PR B 2 H1Q3 H 0.1693 -0.0502 0.1881 0.256 Uiso 0.25 1 calc PR B 2 C2Q C 0.1810(11) 0.0000 0.3233(14) 0.061(4) Uani 0.50 2 d SPRD B 2 C3Q C 0.1340(11) 0.0000(12) 0.3468(14) 0.17(5) Uani 0.50 2 d SPRD B 2 H3Q H 0.0858 0.0001 0.2950 0.206 Uiso 0.50 2 calc SPR B 2 C4Q C 0.173(2) 0.0000 0.467(4) 0.110(13) Uani 0.50 2 d SPD B 2 H4Q H 0.1483 0.0000 0.4958 0.132 Uiso 0.50 2 calc SPR B 2 C5Q C 0.242(2) 0.0000 0.538(2) 0.105(10) Uani 0.50 2 d SPD B 2 H5Q H 0.2642 0.0000 0.6135 0.126 Uiso 0.50 2 calc SPR B 2 C6Q C 0.280(2) 0.0000 0.500(4) 0.106(15) Uani 0.50 2 d SPD B 2 H6Q H 0.3279 0.0000 0.5484 0.127 Uiso 0.50 2 calc SPR B 2 C7Q C 0.246(2) 0.0000 0.392(4) 0.090(10) Uani 0.50 2 d SPD B 2 H7Q H 0.2713 0.0000 0.3644 0.108 Uiso 0.50 2 calc SPR B 2 C1S C 0.4821(14) 0.355(2) 0.3633(16) 0.071(4) Uiso 0.25 1 d PD . . H1S1 H 0.5201 0.3321 0.3650 0.107 Uiso 0.25 1 calc PR . . H1S2 H 0.4671 0.4159 0.3263 0.107 Uiso 0.25 1 calc PR . . H1S3 H 0.4443 0.3108 0.3241 0.107 Uiso 0.25 1 calc PR . . C2S C 0.5030(9) 0.3656(10) 0.4691(10) 0.138(16) Uiso 0.25 1 d PGD . . C3S C 0.5668(8) 0.3708(10) 0.5691(12) 0.086(5) Uiso 0.25 1 d PG . . H3S H 0.6062 0.3788 0.5722 0.104 Uiso 0.25 1 calc PR . . C4S C 0.5730(6) 0.3644(7) 0.6645(9) 0.051(5) Uiso 0.25 1 d PG . . H4S H 0.6166 0.3680 0.7328 0.061 Uiso 0.25 1 calc PR . . C5S C 0.5154(7) 0.3527(9) 0.6599(10) 0.071(4) Uiso 0.25 1 d PG . . H5S H 0.5196 0.3482 0.7251 0.086 Uiso 0.25 1 calc PR . . C6S C 0.4516(6) 0.3474(11) 0.5599(12) 0.064(6) Uiso 0.25 1 d PG . . H6S H 0.4122 0.3394 0.5568 0.077 Uiso 0.25 1 calc PR . . C7S C 0.4454(7) 0.3539(9) 0.4645(9) 0.086(5) Uiso 0.25 1 d PG . . H7S H 0.4018 0.3503 0.3961 0.104 Uiso 0.25 1 calc PR . . B1 B 0.7575(6) -0.0260(9) 1.0973(8) 0.062(6) Uani 0.50 1 d PG . . 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 Ni1 0.0268(5) 0.0253(6) 0.0184(5) 0.000 0.0143(4) 0.000 S1 0.0539(7) 0.0432(7) 0.0313(5) 0.0014(5) 0.0308(5) -0.0038(6) S2 0.0443(7) 0.0655(9) 0.0303(6) 0.0086(5) 0.0236(5) 0.0075(6) P1 0.0327(6) 0.0272(6) 0.0220(5) 0.0016(4) 0.0173(4) -0.0007(5) F1 0.116(5) 0.133(6) 0.055(3) 0.000 0.051(3) 0.000 F2 0.063(3) 0.114(5) 0.107(4) 0.000 0.052(3) 0.000 F3 0.083(5) 0.25(3) 0.076(4) 0.031(8) 0.049(4) -0.065(10) F4 0.089(6) 0.096(7) 0.102(6) -0.007(5) 0.069(5) 0.001(5) C1 0.032(2) 0.040(2) 0.0241(18) 0.0019(17) 0.0167(17) 0.0003(19) C2 0.039(3) 0.051(4) 0.023(3) 0.000 0.023(3) 0.000 C3 0.036(3) 0.058(4) 0.026(3) 0.000 0.022(3) 0.000 C4 0.033(2) 0.090(4) 0.028(2) 0.005(2) 0.0182(19) 0.007(2) C5 0.058(4) 0.117(6) 0.036(3) 0.021(3) 0.025(3) 0.018(4) C6 0.040(2) 0.033(2) 0.028(2) -0.0021(17) 0.0202(19) -0.002(2) C7 0.042(3) 0.041(3) 0.035(2) 0.007(2) 0.019(2) -0.001(2) C8 0.052(3) 0.053(3) 0.035(2) 0.010(2) 0.016(2) 0.013(3) C9 0.046(3) 0.076(4) 0.052(3) 0.015(3) 0.022(3) 0.025(3) C10 0.040(3) 0.097(5) 0.056(3) 0.020(3) 0.030(3) 0.019(3) C11 0.043(3) 0.057(3) 0.038(2) 0.012(2) 0.027(2) 0.011(2) C12 0.043(3) 0.037(3) 0.0248(19) 0.0012(17) 0.0189(19) -0.005(2) C13 0.048(3) 0.074(4) 0.041(3) -0.018(3) 0.029(2) -0.018(3) C14 0.061(4) 0.133(7) 0.047(3) -0.022(4) 0.035(3) -0.045(5) C15 0.099(6) 0.081(6) 0.082(5) -0.006(4) 0.036(5) -0.058(5) C16 0.083(6) 0.046(4) 0.131(7) 0.000(4) 0.021(5) -0.034(4) C17 0.056(4) 0.038(3) 0.072(4) -0.002(3) 0.012(3) -0.008(3) C1P 0.081(18) 0.065(14) 0.053(14) 0.000 0.033(14) 0.000 C2P 0.052(11) 0.038(9) 0.046(10) 0.000 0.017(9) 0.000 C3P 0.069(16) 0.080(18) 0.081(16) 0.000 0.057(14) 0.000 C4P 0.095(18) 0.059(12) 0.043(11) 0.000 0.038(12) 0.000 C5P 0.048(12) 0.078(15) 0.091(17) 0.000 0.015(12) 0.000 C6P 0.09(2) 0.11(3) 0.15(3) 0.000 0.10(2) 0.000 C7P 0.08(2) 0.073(17) 0.13(3) 0.000 0.10(2) 0.000 C1Q 0.13(5) 0.26(6) 0.11(4) 0.000 0.06(4) 0.000 C2Q 0.057(11) 0.064(12) 0.055(10) 0.000 0.029(9) 0.000 C3Q 0.13(7) 0.07(3) 0.28(12) 0.000 0.11(7) 0.000 C4Q 0.13(3) 0.081(17) 0.21(4) 0.000 0.15(4) 0.000 C5Q 0.14(3) 0.066(15) 0.068(14) 0.000 0.042(18) 0.000 C6Q 0.16(5) 0.09(2) 0.13(4) 0.000 0.12(4) 0.000 C7Q 0.14(3) 0.050(15) 0.16(3) 0.000 0.13(3) 0.000 B1 0.053(7) 0.09(2) 0.044(6) 0.001(6) 0.031(5) -0.006(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 Ni1 P1 2.2555(10) 6 ? Ni1 P1 2.2555(10) 2_655 ? Ni1 P1 2.2555(10) . ? Ni1 P1 2.2555(10) 5_655 ? S1 C1 1.753(4) . ? S1 C2 1.760(3) . ? S2 C3 1.749(3) . ? S2 C4 1.767(5) . ? P1 C12 1.804(5) . ? P1 C1 1.806(4) . ? P1 C6 1.810(5) . ? F1 B1 1.403(13) . ? F1 B1 1.403(12) 6 ? F2 B1 1.419(13) 6 ? F2 B1 1.419(13) . ? F3 F3 0.80(4) 6 ? F3 B1 1.086(15) 6 ? F3 B1 1.332(16) . ? F3 F4 1.529(19) 6 ? F4 B1 1.372(16) . ? F4 F3 1.529(19) 6 ? C1 C1 1.337(9) 6 ? C2 C3 1.344(8) . ? C2 S1 1.760(3) 6 ? C3 S2 1.749(3) 6 ? C4 C4 1.312(12) 6 ? C4 C5 1.507(7) . ? C6 C11 1.380(6) . ? C6 C7 1.406(6) . ? C7 C8 1.379(7) . ? C8 C9 1.383(8) . ? C9 C10 1.372(8) . ? C10 C11 1.381(7) . ? C12 C13 1.382(7) . ? C12 C17 1.388(8) . ? C13 C14 1.412(9) . ? C14 C15 1.357(12) . ? C15 C16 1.347(13) . ? C16 C17 1.358(9) . ? C1P C2P 1.4620 . ? C2P C3P 1.3891 . ? C2P C7P 1.38(3) . ? C3P C4P 1.40(3) . ? C4P C5P 1.38(4) . ? C5P C6P 1.43(6) . ? C6P C7P 1.22(8) . ? C1Q C2Q 1.5118 . ? C2Q C7Q 1.27(4) . ? C2Q C3Q 1.4101 . ? C3Q C4Q 1.49(5) . ? C4Q C5Q 1.36(5) . ? C5Q C6Q 1.35(5) . ? C6Q C7Q 1.35(5) . ? C1S C2S 1.392(16) . ? C2S C3S 1.3900 . ? C2S C7S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C7S 1.3900 . ? B1 B1 0.75(3) 6 ? B1 F3 1.086(15) 6 ? 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 Ni1 P1 180.00(7) 6 2_655 ? P1 Ni1 P1 86.20(5) 6 . ? P1 Ni1 P1 93.80(5) 2_655 . ? P1 Ni1 P1 93.80(5) 6 5_655 ? P1 Ni1 P1 86.20(5) 2_655 5_655 ? P1 Ni1 P1 180.00(7) . 5_655 ? C1 S1 C2 92.4(2) . . ? C3 S2 C4 95.0(2) . . ? C12 P1 C1 101.5(2) . . ? C12 P1 C6 106.5(2) . . ? C1 P1 C6 104.96(19) . . ? C12 P1 Ni1 119.94(14) . . ? C1 P1 Ni1 105.57(14) . . ? C6 P1 Ni1 116.35(15) . . ? B1 F1 B1 30.8(10) . 6 ? B1 F2 B1 30.4(11) 6 . ? F3 F3 B1 88.5(12) 6 6 ? F3 F3 B1 54.5(9) 6 . ? B1 F3 B1 34.0(13) 6 . ? F3 F3 F4 149.1(5) 6 6 ? B1 F3 F4 60.5(11) 6 6 ? B1 F3 F4 94.5(9) . 6 ? B1 F4 F3 43.5(8) . 6 ? C1 C1 S1 117.16(15) 6 . ? C1 C1 P1 118.90(14) 6 . ? S1 C1 P1 123.9(3) . . ? C3 C2 S1 123.42(15) . . ? C3 C2 S1 123.42(15) . 6 ? S1 C2 S1 113.1(3) . 6 ? C2 C3 S2 122.92(16) . 6 ? C2 C3 S2 122.92(16) . . ? S2 C3 S2 114.2(3) 6 . ? C4 C4 C5 128.6(4) 6 . ? C4 C4 S2 117.37(19) 6 . ? C5 C4 S2 114.0(5) . . ? C11 C6 C7 119.1(4) . . ? C11 C6 P1 120.7(3) . . ? C7 C6 P1 120.2(4) . . ? C8 C7 C6 120.3(5) . . ? C7 C8 C9 119.9(5) . . ? C10 C9 C8 119.7(5) . . ? C9 C10 C11 121.2(5) . . ? C6 C11 C10 119.9(5) . . ? C13 C12 C17 118.5(5) . . ? C13 C12 P1 119.0(4) . . ? C17 C12 P1 122.4(4) . . ? C12 C13 C14 119.0(6) . . ? C15 C14 C13 120.5(7) . . ? C16 C15 C14 119.7(7) . . ? C15 C16 C17 121.5(8) . . ? C16 C17 C12 120.7(7) . . ? C3P C2P C7P 114(2) . . ? C3P C2P C1P 122.4 . . ? C7P C2P C1P 123(2) . . ? C2P C3P C4P 120.1(15) . . ? C5P C4P C3P 120(2) . . ? C4P C5P C6P 118(3) . . ? C7P C6P C5P 118(4) . . ? C6P C7P C2P 129(4) . . ? C7Q C2Q C3Q 127(2) . . ? C7Q C2Q C1Q 119(2) . . ? C3Q C2Q C1Q 114.7 . . ? C2Q C3Q C4Q 107.9(15) . . ? C5Q C4Q C3Q 124(3) . . ? C6Q C5Q C4Q 120(3) . . ? C5Q C6Q C7Q 117(4) . . ? C2Q C7Q C6Q 124(4) . . ? C3S C2S C7S 120.0 . . ? C3S C2S C1S 132.7(16) . . ? C7S C2S C1S 106.6(17) . . ? C4S C3S C2S 120.0 . . ? C3S C4S C5S 120.0 . . ? C6S C5S C4S 120.0 . . ? C7S C6S C5S 120.0 . . ? C6S C7S C2S 120.0 . . ? B1 B1 F3 91.5(13) 6 6 ? B1 B1 F3 54.5(10) 6 . ? F3 B1 F3 36.9(17) 6 . ? B1 B1 F4 167.4(9) 6 . ? F3 B1 F4 76.0(14) 6 . ? F3 B1 F4 112.9(13) . . ? B1 B1 F1 74.6(6) 6 . ? F3 B1 F1 125.0(12) 6 . ? F3 B1 F1 107.9(11) . . ? F4 B1 F1 112.0(8) . . ? B1 B1 F2 74.8(6) 6 . ? F3 B1 F2 123.6(9) 6 . ? F3 B1 F2 107.0(8) . . ? F4 B1 F2 112.6(10) . . ? F1 B1 F2 104.0(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.880 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.098 # Attachment 'pdp22_new.txt' data_pdp2 _database_code_depnum_ccdc_archive 'CCDC 615883' _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and [Pd(MeCN)4][BF4]2 produced the the complex [Pd(o-P2)2][BF4]2 where the nickel metal center displays square planar geometry. The complex was analyzed by several physical methods including x-ray crystallography, NMR, IR, magnetism, and cyclic voltammetry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H52 P4 Pd S8), 4(C8.18 H8.41), C14 H16, 4(B F4)' _chemical_formula_sum 'C174.72 H153.64 B4 F16 P8 Pd2 S16' _chemical_formula_weight 3572.56 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.549(5) _cell_length_b 14.287(5) _cell_length_c 15.527(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 127.400(5) _cell_angle_gamma 90.000(5) _cell_volume 4326(2) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rectangular _exptl_crystal_colour Brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832.3 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. Two independent toluene molecules were located and refined isotropically with restraints on bond distances and angles. Hydrogen atoms were not included in the disordered solvent molecules. ; _diffrn_ambient_temperature 173(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 'Bruker SMART 1000' _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 24743 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.54 _reflns_number_total 5530 _reflns_number_gt 3479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.1326P)^2^+3.6259P] 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 0.0041(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5530 _refine_ls_number_parameters 249 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.2440 _refine_ls_wR_factor_gt 0.2248 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.025 _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 Pd1 Pd 0.0000 0.0000 -1.0000 0.02240(9) Uani 1 4 d S . . S1 S 0.01285(3) -0.10292(4) -0.67930(4) 0.03335(16) Uani 1 1 d . . . S2 S 0.09256(3) -0.10247(5) -0.41870(4) 0.03878(18) Uani 1 1 d . . . P1 P 0.02408(2) -0.11046(4) -0.86945(4) 0.02498(15) Uani 1 1 d . . . C1 C 0.01704(8) -0.04708(15) -0.77640(13) 0.0267(6) Uani 1 1 d . . . C2 C 0.03476(13) 0.0000 -0.6023(2) 0.0324(9) Uani 1 2 d S . . C3 C 0.06973(12) 0.0000 -0.4945(2) 0.0306(9) Uani 1 2 d S . . C4 C 0.14514(10) -0.04659(19) -0.29142(16) 0.0435(8) Uani 1 1 d . . . C5 C 0.18472(13) -0.1108(3) -0.19649(19) 0.0700(12) Uani 1 1 d . . . H5A H 0.2126 -0.0739 -0.1296 0.105 Uiso 1 1 calc R . . H5B H 0.2147 -0.1504 -0.2030 0.105 Uiso 1 1 calc R . . H5C H 0.1529 -0.1503 -0.1944 0.105 Uiso 1 1 calc R . . C101 C -0.03346(10) -0.20733(16) -0.90855(15) 0.0332(7) Uani 1 1 d . . . C102 C -0.01444(15) -0.29722(19) -0.9123(3) 0.0874(17) Uani 1 1 d . . . H10C H 0.0292 -0.3095 -0.8951 0.105 Uiso 1 1 calc R . . C103 C -0.06051(18) -0.3689(3) -0.9416(4) 0.140(3) Uani 1 1 d . . . H10E H -0.0471 -0.4309 -0.9434 0.168 Uiso 1 1 calc R . . C104 C -0.12258(17) -0.3562(2) -0.9675(3) 0.0933(17) Uani 1 1 d . . . H10B H -0.1524 -0.4078 -0.9868 0.112 Uiso 1 1 calc R . . C105 C -0.14265(12) -0.2676(2) -0.96589(19) 0.0641(10) Uani 1 1 d . . . H10D H -0.1868 -0.2571 -0.9844 0.077 Uiso 1 1 calc R . . C106 C -0.09785(10) -0.1919(2) -0.93670(17) 0.0483(8) Uani 1 1 d . . . H10A H -0.1120 -0.1301 -0.9364 0.058 Uiso 1 1 calc R . . C111 C 0.10923(9) -0.15988(15) -0.78953(14) 0.0294(6) Uani 1 1 d . . . C112 C 0.15457(10) -0.13492(19) -0.81062(16) 0.0428(7) Uani 1 1 d . . . H11C H 0.1406 -0.0923 -0.8676 0.051 Uiso 1 1 calc R . . C113 C 0.21989(11) -0.1718(2) -0.7492(2) 0.0609(10) Uani 1 1 d . . . H11E H 0.2512 -0.1544 -0.7632 0.073 Uiso 1 1 calc R . . C114 C 0.23931(12) -0.2339(2) -0.6673(2) 0.0586(10) Uani 1 1 d . . . H11D H 0.2841 -0.2600 -0.6256 0.070 Uiso 1 1 calc R . . C115 C 0.19464(12) -0.25884(19) -0.64484(18) 0.0477(9) Uani 1 1 d . . . H11B H 0.2090 -0.3012 -0.5875 0.057 Uiso 1 1 calc R . . C116 C 0.12908(10) -0.22201(16) -0.70605(16) 0.0375(7) Uani 1 1 d . . . H11A H 0.0980 -0.2389 -0.6913 0.045 Uiso 1 1 calc R . . C1P C 0.3437(5) 0.0059(3) -0.2125(8) 0.117(3) Uiso 0.2949(19) 1 d PD A -1 H1P1 H 0.3193 -0.0415 -0.2020 0.175 Uiso 0.2949(19) 1 calc PR A -1 H1P2 H 0.3350 0.0680 -0.1962 0.175 Uiso 0.2949(19) 1 calc PR A -1 H1P3 H 0.3930 -0.0071 -0.1638 0.175 Uiso 0.2949(19) 1 calc PR A -1 C2P C 0.31861(14) 0.0034(2) -0.3285(2) 0.0428(15) Uiso 0.590(4) 2 d SPGD A -1 C3P C 0.24786(14) -0.0041(4) -0.4048(3) 0.0501(17) Uiso 0.2949(19) 1 d PGD A -1 H3P H 0.2198 -0.0072 -0.3819 0.060 Uiso 0.2949(19) 1 calc PR A -1 C4P C 0.21822(18) -0.0071(3) -0.5146(2) 0.0950(19) Uiso 0.2949(19) 1 d PGD A -1 H4P H 0.1699 -0.0122 -0.5667 0.114 Uiso 0.2949(19) 1 calc PR A -1 C5P C 0.2593(3) -0.0026(4) -0.5482(2) 0.067(2) Uiso 0.590(4) 2 d SPGD A -1 H5P H 0.2391 -0.0047 -0.6232 0.081 Uiso 0.2949(19) 1 calc PR A -1 C6P C 0.3301(2) 0.0049(6) -0.4719(3) 0.084(3) Uiso 0.2949(19) 1 d PGD A -1 H6P H 0.3582 0.0080 -0.4948 0.101 Uiso 0.2949(19) 1 calc PR A -1 C7P C 0.35972(16) 0.0079(5) -0.3620(3) 0.0520(18) Uiso 0.2949(19) 1 d PGD A -1 H7P H 0.4081 0.0130 -0.3099 0.062 Uiso 0.2949(19) 1 calc PR A -1 C1Q C 0.21376(18) -0.0076(4) -0.5268(2) 0.0950(19) Uiso 0.2051(19) 1 d PGD A -2 H1Q1 H 0.1858 0.0453 -0.5343 0.142 Uiso 0.2051(19) 1 calc PR A -2 H1Q2 H 0.1880 -0.0659 -0.5439 0.142 Uiso 0.2051(19) 1 calc PR A -2 H1Q3 H 0.2252 0.0005 -0.5769 0.142 Uiso 0.410(4) 2 calc SPR A -2 C2Q C 0.2684(2) -0.0110(2) -0.4305(3) 0.087(4) Uiso 0.2051(19) 1 d PGD A -2 C3Q C 0.2619(2) -0.0137(2) -0.3476(4) 0.050(3) Uiso 0.2051(19) 1 d PGD A -2 H3Q H 0.2177 -0.0134 -0.3644 0.060 Uiso 0.2051(19) 1 calc PR A -2 C4Q C 0.3202(3) -0.0169(3) -0.2402(3) 0.117(3) Uiso 0.2051(19) 1 d PGD A -2 H4Q H 0.3158 -0.0187 -0.1835 0.140 Uiso 0.2051(19) 1 calc PR A -2 C5Q C 0.3849(2) -0.0173(3) -0.2156(4) 0.080(5) Uiso 0.2051(19) 1 d PGD A -2 H5Q H 0.4247 -0.0195 -0.1422 0.096 Uiso 0.2051(19) 1 calc PR A -2 C6Q C 0.3913(2) -0.0146(3) -0.2986(4) 0.095(5) Uiso 0.2051(19) 1 d PGD A -2 H6Q H 0.4355 -0.0149 -0.2818 0.114 Uiso 0.2051(19) 1 calc PR A -2 C7Q C 0.3331(2) -0.0114(2) -0.4060(4) 0.102(5) Uiso 0.2051(19) 1 d PGD A -2 H7Q H 0.3375 -0.0095 -0.4627 0.123 Uiso 0.2051(19) 1 calc PR A -2 C1S C 0.0488(3) -0.3722(3) -0.5896(7) 0.137(8) Uiso 0.25 1 d PGDU A -3 H1S1 H 0.0858 -0.3297 -0.5711 0.206 Uiso 0.25 1 calc PR A -3 H1S2 H 0.0068 -0.3556 -0.6610 0.206 Uiso 0.25 1 calc PR A -3 H1S3 H 0.0618 -0.4367 -0.5913 0.206 Uiso 0.25 1 calc PR A -3 C2S C 0.03743(8) -0.36464(15) -0.51123(11) 0.096(3) Uiso 0.25 1 d PGDU A -3 C3S C -0.02914(8) -0.35090(15) -0.54576(11) 0.103(5) Uiso 0.25 1 d PGDU A -3 H3S H -0.0661 -0.3485 -0.6210 0.124 Uiso 0.25 1 calc PR A -3 C4S C -0.04164(8) -0.34068(16) -0.47013(12) 0.096(3) Uiso 0.25 1 d PGDU A -3 H4S H -0.0871 -0.3313 -0.4937 0.115 Uiso 0.25 1 calc PR A -3 C5S C 0.01243(8) -0.34420(16) -0.35997(12) 0.0293(18) Uiso 0.25 1 d PGDU A -3 H5S H 0.0039 -0.3372 -0.3083 0.035 Uiso 0.25 1 calc PR A -3 C6S C 0.07900(8) -0.35795(15) -0.32544(11) 0.039(2) Uiso 0.25 1 d PGDU A -3 H6S H 0.1159 -0.3604 -0.2501 0.046 Uiso 0.25 1 calc PR A -3 C7S C 0.09150(8) -0.36817(15) -0.40106(11) 0.089(4) Uiso 0.25 1 d PGDU A -3 H7S H 0.1370 -0.3776 -0.3775 0.107 Uiso 0.25 1 calc PR A -3 B1 B 0.24760(12) -0.01307(19) 0.09312(14) 0.097(3) Uani 0.50 1 d PG . . F1 F 0.28134(12) -0.0001(2) 0.20370(14) 0.0954(12) Uani 1 2 d SG . . F2 F 0.18187(12) -0.00008(19) 0.03859(15) 0.0837(11) Uani 1 2 d SG . . F3 F 0.27591(12) 0.03722(18) 0.04913(15) 0.0997(18) Uani 0.50 1 d PG . . F4 F 0.26067(10) -0.11270(19) 0.07778(12) 0.0762(13) Uani 0.50 1 d PG . . 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 0.02089(9) 0.02300(14) 0.02141(10) 0.000 0.01186(7) 0.000 S1 0.04550(19) 0.0302(3) 0.02957(18) -0.00035(18) 0.02548(13) -0.0028(2) S2 0.0381(2) 0.0488(3) 0.02937(19) 0.0079(2) 0.02042(14) 0.0090(2) P1 0.02559(16) 0.0244(3) 0.02287(17) 0.00024(17) 0.01363(12) 0.00021(18) C1 0.0243(6) 0.0335(10) 0.0218(6) 0.0019(7) 0.0138(5) 0.0010(7) C2 0.0371(10) 0.0380(17) 0.0305(10) 0.000 0.0249(7) 0.000 C3 0.0210(9) 0.0450(18) 0.0241(10) 0.000 0.0128(7) 0.000 C4 0.0277(7) 0.0734(17) 0.0246(8) 0.0046(9) 0.0133(5) 0.0058(9) C5 0.0552(12) 0.115(3) 0.0300(10) 0.0222(13) 0.0209(8) 0.0270(15) C101 0.0347(8) 0.0325(11) 0.0235(7) 0.0026(8) 0.0130(6) -0.0038(9) C102 0.0431(13) 0.0294(14) 0.121(2) -0.0178(16) 0.0138(15) -0.0067(12) C103 0.0522(18) 0.0395(18) 0.215(5) -0.015(3) 0.021(2) -0.0142(16) C104 0.0807(18) 0.0424(16) 0.107(2) -0.0038(17) 0.0308(16) -0.0319(15) C105 0.0454(9) 0.104(2) 0.0440(10) -0.0140(13) 0.0277(7) -0.0329(13) C106 0.0437(8) 0.0644(16) 0.0454(9) -0.0180(10) 0.0316(6) -0.0189(10) C111 0.0312(7) 0.0265(10) 0.0261(7) -0.0019(7) 0.0151(5) 0.0033(8) C112 0.0377(8) 0.0581(15) 0.0371(8) 0.0145(10) 0.0250(6) 0.0157(10) C113 0.0392(8) 0.081(2) 0.0658(12) 0.0236(13) 0.0338(7) 0.0171(12) C114 0.0365(10) 0.0687(18) 0.0508(12) 0.0135(13) 0.0163(8) 0.0208(12) C115 0.0419(10) 0.0449(14) 0.0338(10) 0.0083(10) 0.0112(8) 0.0138(11) C116 0.0412(8) 0.0295(11) 0.0381(9) 0.0022(8) 0.0221(6) 0.0016(9) B1 0.053(2) 0.198(9) 0.0387(19) 0.014(7) 0.0280(14) 0.011(8) F1 0.1186(15) 0.108(2) 0.0630(11) 0.000 0.0567(9) 0.000 F2 0.0544(10) 0.0924(19) 0.0934(14) 0.000 0.0392(9) 0.000 F3 0.0841(14) 0.145(5) 0.0733(15) 0.0036(18) 0.0498(10) -0.0383(18) F4 0.0635(12) 0.111(3) 0.0665(13) -0.0146(16) 0.0457(9) 0.0103(17) _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 2.3438(8) 2_553 ? Pd1 P1 2.3438(8) 6 ? Pd1 P1 2.3438(8) 5_553 ? Pd1 P1 2.3438(8) . ? S1 C2 1.7604(18) . ? S1 C1 1.763(2) . ? S2 C3 1.7440(17) . ? S2 C4 1.764(2) . ? P1 C101 1.799(2) . ? P1 C1 1.800(2) . ? P1 C111 1.8046(19) . ? C1 C1 1.345(4) 6 ? C2 C3 1.339(4) . ? C2 S1 1.7604(17) 6 ? C3 S2 1.7440(17) 6 ? C4 C4 1.331(6) 6 ? C4 C5 1.489(4) . ? C101 C106 1.378(4) . ? C101 C102 1.380(4) . ? C102 C103 1.382(5) . ? C103 C104 1.331(6) . ? C104 C105 1.363(5) . ? C105 C106 1.407(4) . ? C111 C112 1.384(4) . ? C111 C116 1.392(3) . ? C112 C113 1.378(3) . ? C113 C114 1.377(4) . ? C114 C115 1.384(5) . ? C115 C116 1.383(3) . ? C1P C2P 1.509(13) . ? C2P C3P 1.3900 . ? C2P C7P 1.3900 . ? C3P C4P 1.3900 . ? C4P C5P 1.3900 . ? C5P C6P 1.3900 . ? C6P C7P 1.3900 . ? C1Q C2Q 1.265(4) . ? C2Q C3Q 1.3900 . ? C2Q C7Q 1.3900 . ? C3Q C4Q 1.3900 . ? C4Q C5Q 1.3900 . ? C5Q C6Q 1.3900 . ? C6Q C7Q 1.3900 . ? C1S C2S 1.410(10) . ? C2S C3S 1.3900 . ? C2S C7S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C7S 1.3900 . ? B1 B1 0.373(5) 6 ? B1 F3 1.2826(14) 6 ? B1 F2 1.3022 . ? B1 F1 1.3932 . ? B1 F3 1.4290 . ? B1 F4 1.5096 . ? B1 F4 1.866(5) 6 ? F1 B1 1.3935 6 ? F2 B1 1.3025 6 ? F3 F3 1.064(5) 6 ? F3 B1 1.2826(15) 6 ? F3 F4 1.305(4) 6 ? F4 F3 1.305(4) 6 ? F4 B1 1.866(5) 6 ? 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 180.0 2_553 6 ? P1 Pd1 P1 84.65(4) 2_553 5_553 ? P1 Pd1 P1 95.35(4) 6 5_553 ? P1 Pd1 P1 95.35(4) 2_553 . ? P1 Pd1 P1 84.65(4) 6 . ? P1 Pd1 P1 180.0 5_553 . ? C2 S1 C1 92.88(13) . . ? C3 S2 C4 95.33(12) . . ? C101 P1 C1 102.67(12) . . ? C101 P1 C111 105.97(10) . . ? C1 P1 C111 106.30(9) . . ? C101 P1 Pd1 119.48(6) . . ? C1 P1 Pd1 104.99(8) . . ? C111 P1 Pd1 115.88(9) . . ? C1 C1 S1 116.90(8) 6 . ? C1 C1 P1 120.20(7) 6 . ? S1 C1 P1 122.86(13) . . ? C3 C2 S1 123.25(7) . . ? C3 C2 S1 123.25(7) . 6 ? S1 C2 S1 113.28(16) . 6 ? C2 C3 S2 122.88(8) . 6 ? C2 C3 S2 122.88(8) . . ? S2 C3 S2 114.16(16) 6 . ? C4 C4 C5 128.02(16) 6 . ? C4 C4 S2 116.91(9) 6 . ? C5 C4 S2 115.1(2) . . ? C106 C101 C102 119.2(3) . . ? C106 C101 P1 119.88(19) . . ? C102 C101 P1 120.9(2) . . ? C101 C102 C103 118.3(4) . . ? C104 C103 C102 123.7(4) . . ? C103 C104 C105 118.8(3) . . ? C104 C105 C106 119.9(3) . . ? C101 C106 C105 120.0(3) . . ? C112 C111 C116 120.50(19) . . ? C112 C111 P1 119.90(16) . . ? C116 C111 P1 119.6(2) . . ? C113 C112 C111 120.2(2) . . ? C114 C113 C112 119.3(3) . . ? C113 C114 C115 121.1(2) . . ? C116 C115 C114 119.9(2) . . ? C115 C116 C111 119.0(3) . . ? C3P C2P C7P 120.0 . . ? C3P C2P C1P 114.3(5) . . ? C7P C2P C1P 125.7(5) . . ? C4P C3P C2P 120.0 . . ? C3P C4P C5P 120.0 . . ? C6P C5P C4P 120.0 . . ? C7P C6P C5P 120.0 . . ? C6P C7P C2P 120.0 . . ? C1Q C2Q C3Q 117.4(4) . . ? C1Q C2Q C7Q 122.6(4) . . ? C3Q C2Q C7Q 120.0 . . ? C4Q C3Q C2Q 120.0 . . ? C3Q C4Q C5Q 120.0 . . ? C6Q C5Q C4Q 120.0 . . ? C5Q C6Q C7Q 120.0 . . ? C6Q C7Q C2Q 120.0 . . ? C3S C2S C7S 120.0 . . ? C3S C2S C1S 118.8(3) . . ? C7S C2S C1S 121.2(3) . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C7S C6S C5S 120.0 . . ? C6S C7S C2S 120.0 . . ? B1 B1 F3 105.6(2) 6 6 ? B1 B1 F2 81.8 6 . ? F3 B1 F2 123.4 6 . ? B1 B1 F1 82.3 6 . ? F3 B1 F1 125.7 6 . ? F2 B1 F1 110.9 . . ? B1 B1 F3 59.8 6 . ? F3 B1 F3 45.8(2) 6 . ? F2 B1 F3 112.8 . . ? F1 B1 F3 115.1 . . ? B1 B1 F4 160.6 6 . ? F3 B1 F4 55.0(2) 6 . ? F2 B1 F4 109.3 . . ? F1 B1 F4 107.2 . . ? F3 B1 F4 100.8 . . ? B1 B1 F4 15.6 6 6 ? F3 B1 F4 90.02(18) 6 6 ? F2 B1 F4 91.2 . 6 ? F1 B1 F4 90.5 . 6 ? F3 B1 F4 44.2 . 6 ? F4 B1 F4 144.9 . 6 ? B1 F1 B1 15.4(2) . 6 ? B1 F2 B1 16.5(2) . 6 ? F3 F3 B1 74.4(2) 6 6 ? F3 F3 F4 145.73(13) 6 6 ? B1 F3 F4 71.37(10) 6 6 ? F3 F3 B1 59.8 6 . ? B1 F3 B1 14.6(2) 6 . ? F4 F3 B1 85.94(13) 6 . ? F3 F4 B1 53.62(13) 6 . ? F3 F4 B1 49.82(17) 6 6 ? B1 F4 B1 3.8 . 6 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.54 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.702 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.169 # Attachment 'ptp22_new.txt' data_ptp22 _database_code_depnum_ccdc_archive 'CCDC 615884' _audit_creation_method ; SHELXL-97, PLATON, and text editor. ; _publ_section_abstract ; The reaction between 3,4-dimethyl-3',4'-bis(diphenylphosphino)tetrathia- fulvalene and [Pt(MeCN)4][BF4]2 produced the the complex [Pt(o-P2)2][BF4]2 where the nickel metal center displays square planar geometry. The complex was analyzed by several physical methods including x-ray crystallography, NMR, IR, magnetism, and cyclic voltammetry. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C64 H52 P4 Pt S8), 4(C7 H8.75), C14 H19, 4(B F4)' _chemical_formula_sum 'C170 H158 B4 F16 P8 Pt2 S16' _chemical_formula_weight 3693.20 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' B B 0.0013 0.0007 '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' 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_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 24.617(2) _cell_length_b 14.3476(13) _cell_length_c 15.5292(13) _cell_angle_alpha 90.00 _cell_angle_beta 127.072(10) _cell_angle_gamma 90.00 _cell_volume 4376.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Platelet _exptl_crystal_colour Red-Orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1868 _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6550 _exptl_absorpt_correction_T_max 0.8612 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (432 frames), and at phi = 180 deg (230 frames). A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. Two independent toluene molecules were located and refined isotropically with restraints on bond distances and angles. Hydrogen atoms were not included in the disordered solvent molecules. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _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 21317 _diffrn_reflns_av_R_equivalents 0.2221 _diffrn_reflns_av_sigmaI/netI 0.2498 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4402 _reflns_number_gt 2424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _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^)+(0.0002P)^2^+0.0000P] 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 4402 _refine_ls_number_parameters 258 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 0.765 _refine_ls_restrained_S_all 0.764 _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 Pt1 Pt 0.5000 0.0000 0.0000 0.0204(2) Uani 1 4 d S . . S1 S 0.51392(11) -0.10241(16) 0.32093(16) 0.0374(6) Uani 1 1 d . . . S2 S 0.59262(10) -0.10238(17) 0.58135(16) 0.0422(6) Uani 1 1 d . . . P1 P 0.52445(10) -0.11015(14) 0.13015(15) 0.0249(5) Uani 1 1 d . . . F1 F 0.7853(5) 0.0000 1.2019(7) 0.102(3) Uani 1 2 d S . . F2 F 0.6855(4) 0.0000 1.0377(8) 0.099(3) Uani 1 2 d S . . F3 F 0.7808(6) 0.0306(11) 1.0573(10) 0.093(8) Uani 0.50 1 d P . . F4 F 0.7635(6) -0.1126(12) 1.0831(11) 0.084(4) Uani 0.50 1 d P . . C1 C 0.5181(3) -0.0473(5) 0.2252(5) 0.0261(18) Uani 1 1 d . . . C2 C 0.5363(5) 0.0000 0.3982(8) 0.026(3) Uani 1 2 d S . . C3 C 0.5691(5) 0.0000 0.5054(8) 0.032(3) Uani 1 2 d S . . C4 C 0.6450(4) -0.0459(7) 0.7075(6) 0.050(3) Uani 1 1 d . . . C5 C 0.6830(4) -0.1126(8) 0.8027(7) 0.065(3) Uani 1 1 d . . . H5A H 0.7159 -0.1486 0.8003 0.097 Uiso 1 1 calc R . . H5B H 0.6505 -0.1551 0.7990 0.097 Uiso 1 1 calc R . . H5C H 0.7071 -0.0770 0.8701 0.097 Uiso 1 1 calc R . . C11 C 0.4661(4) -0.2068(6) 0.0899(6) 0.036(2) Uani 1 1 d . . . C12 C 0.4022(4) -0.1885(8) 0.0605(6) 0.052(3) Uani 1 1 d . . . H13 H 0.3887 -0.1262 0.0592 0.062 Uiso 1 1 calc R . . C13 C 0.3577(5) -0.2613(10) 0.0330(8) 0.070(3) Uani 1 1 d . . . H14 H 0.3139 -0.2497 0.0148 0.084 Uiso 1 1 calc R . . C14 C 0.3776(7) -0.3504(11) 0.0323(9) 0.091(5) Uani 1 1 d . . . H15 H 0.3475 -0.4010 0.0140 0.109 Uiso 1 1 calc R . . C15 C 0.4404(7) -0.3668(8) 0.0577(11) 0.120(6) Uani 1 1 d . . . H16 H 0.4529 -0.4285 0.0543 0.144 Uiso 1 1 calc R . . C16 C 0.4850(5) -0.2962(7) 0.0876(8) 0.072(4) Uani 1 1 d . . . H17 H 0.5290 -0.3084 0.1068 0.086 Uiso 1 1 calc R . . C21 C 0.6087(4) -0.1585(5) 0.2093(6) 0.0285(18) Uani 1 1 d . . . C22 C 0.6290(4) -0.2222(6) 0.2924(6) 0.041(2) Uani 1 1 d . . . H7 H 0.5978 -0.2403 0.3063 0.050 Uiso 1 1 calc R . . C23 C 0.6940(4) -0.2586(6) 0.3539(6) 0.044(2) Uani 1 1 d . . . H8 H 0.7073 -0.3018 0.4098 0.053 Uiso 1 1 calc R . . C24 C 0.7393(5) -0.2330(7) 0.3350(8) 0.060(3) Uani 1 1 d . . . H9 H 0.7841 -0.2577 0.3783 0.072 Uiso 1 1 calc R . . C25 C 0.7200(4) -0.1711(8) 0.2529(8) 0.064(3) Uani 1 1 d . . . H10 H 0.7512 -0.1548 0.2385 0.076 Uiso 1 1 calc R . . C26 C 0.6555(4) -0.1329(6) 0.1919(6) 0.044(2) Uani 1 1 d . . . H11 H 0.6432 -0.0887 0.1374 0.053 Uiso 1 1 calc R . . C1P C 0.155(2) 0.0000 0.209(2) 0.104(15) Uiso 0.50 2 d SPD A 1 H1P1 H 0.1893 0.0288 0.2046 0.157 Uiso 0.25 1 calc PR A 1 H1P2 H 0.1123 0.0354 0.1641 0.157 Uiso 0.25 1 calc PR A 1 H1P3 H 0.1468 -0.0643 0.1823 0.157 Uiso 0.25 1 calc PR A 1 C2P C 0.1791(8) 0.0000 0.3222(10) 0.032(5) Uiso 0.50 2 d SPGD A 1 C3P C 0.2497(7) 0.000(5) 0.3963(14) 0.054(8) Uiso 0.50 2 d SPGD A 1 H3P H 0.2769 0.0000 0.3717 0.065 Uiso 0.50 2 calc SPR A 1 C4P C 0.2804(6) 0.000(4) 0.5063(13) 0.052(8) Uiso 0.50 2 d SPGD A 1 H4P H 0.3286 0.0000 0.5569 0.062 Uiso 0.50 2 calc SPR A 1 C5P C 0.2406(8) 0.000(4) 0.5422(10) 0.067(9) Uiso 0.50 2 d SPGD A 1 H5P H 0.2616 0.0000 0.6173 0.081 Uiso 0.50 2 calc SPR A 1 C6P C 0.1700(8) 0.000(8) 0.4681(14) 0.076(9) Uiso 0.50 2 d SPGD A 1 H6P H 0.1427 0.0000 0.4926 0.091 Uiso 0.50 2 calc SPR A 1 C7P C 0.1393(5) 0.000(6) 0.3581(13) 0.066(8) Uiso 0.50 2 d SPGD A 1 H7P H 0.0910 0.0000 0.3074 0.079 Uiso 0.50 2 calc SPR A 1 C1Q C 0.2876(6) 0.000(4) 0.5488(12) 0.084(11) Uiso 0.50 2 d SPGD A 2 H1Q1 H 0.2937 0.0627 0.5783 0.126 Uiso 0.25 1 calc PR A 2 H1Q2 H 0.3291 -0.0189 0.5580 0.126 Uiso 0.25 1 calc PR A 2 H1Q3 H 0.2785 -0.0439 0.5870 0.126 Uiso 0.25 1 calc PR A 2 C2Q C 0.2305(9) 0.0000 0.4343(16) 0.068(9) Uiso 0.50 2 d SPGD A 2 C3Q C 0.1667(12) 0.0001(7) 0.4121(18) 0.116(14) Uiso 0.50 2 d SPGD A 2 H3Q H 0.1630 0.0000 0.4696 0.139 Uiso 0.50 2 calc SPR A 2 C4Q C 0.1082(9) 0.000(3) 0.306(2) 0.138(17) Uiso 0.50 2 d SPGD A 2 H4Q H 0.0646 0.0004 0.2906 0.166 Uiso 0.50 2 calc SPR A 2 C5Q C 0.1136(11) 0.000(4) 0.2216(16) 0.082(10) Uiso 0.50 2 d SPGD A 2 H5Q H 0.0737 0.0006 0.1490 0.098 Uiso 0.50 2 calc SPR A 2 C6Q C 0.1774(14) 0.000(4) 0.2439(18) 0.110(18) Uiso 0.50 2 d SPGD A 2 H6Q H 0.1811 0.0005 0.1864 0.132 Uiso 0.50 2 calc SPR A 2 C7Q C 0.2358(10) 0.0002(16) 0.350(2) 0.101(13) Uiso 0.50 2 d SPGD A 2 H7Q H 0.2794 0.0001 0.3654 0.121 Uiso 0.50 2 calc SPR A 2 C1S C 0.5139(18) 0.348(2) 0.376(3) 0.064(12) Uiso 0.25 1 d PGD . . H1S1 H 0.5432 0.3943 0.3760 0.096 Uiso 0.25 1 calc PR . . H1S2 H 0.4677 0.3525 0.3085 0.096 Uiso 0.25 1 calc PR . . H1S3 H 0.5320 0.2856 0.3836 0.096 Uiso 0.25 1 calc PR . . C2S C 0.5120(14) 0.3666(14) 0.4656(14) 0.18(3) Uiso 0.25 1 d PGD . . C3S C 0.5739(11) 0.3686(15) 0.5680(17) 0.072(13) Uiso 0.25 1 d PG . . H3S H 0.6151 0.3752 0.5760 0.086 Uiso 0.25 1 calc PR . . C4S C 0.5755(9) 0.3609(9) 0.6587(13) 0.027(7) Uiso 0.25 1 d PG . . H4S H 0.6178 0.3623 0.7288 0.033 Uiso 0.25 1 calc PR . . C5S C 0.5151(9) 0.3513(12) 0.6470(13) 0.034(9) Uiso 0.25 1 d PG . . H5S H 0.5162 0.3460 0.7090 0.041 Uiso 0.25 1 calc PR . . C6S C 0.4532(8) 0.3493(15) 0.5446(16) 0.051(10) Uiso 0.25 1 d PG . . H6S H 0.4120 0.3427 0.5365 0.061 Uiso 0.25 1 calc PR . . C7S C 0.4516(11) 0.3569(12) 0.4538(12) 0.082(15) Uiso 0.25 1 d PG . . H7S H 0.4093 0.3555 0.3838 0.099 Uiso 0.25 1 calc PR . . B1 B 0.7543(10) -0.0231(12) 1.0952(13) 0.039(7) Uani 0.50 1 d PG . . 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 0.0235(4) 0.0233(4) 0.0158(4) 0.000 0.0126(3) 0.000 S1 0.0574(14) 0.0374(14) 0.0287(11) 0.0000(10) 0.0319(11) -0.0049(11) S2 0.0442(14) 0.0557(17) 0.0282(12) 0.0079(11) 0.0226(11) 0.0089(11) P1 0.0322(12) 0.0240(14) 0.0209(11) 0.0012(9) 0.0172(10) -0.0003(9) F1 0.148(9) 0.102(8) 0.062(6) 0.000 0.067(6) 0.000 F2 0.066(6) 0.111(8) 0.117(7) 0.000 0.053(6) 0.000 F3 0.092(8) 0.12(3) 0.081(8) 0.015(9) 0.058(7) -0.024(9) F4 0.067(8) 0.109(13) 0.090(10) -0.011(9) 0.054(7) 0.005(8) C1 0.031(4) 0.028(4) 0.018(4) -0.004(3) 0.014(3) -0.008(3) C2 0.029(6) 0.035(7) 0.021(6) 0.000 0.018(5) 0.000 C3 0.038(7) 0.034(7) 0.025(6) 0.000 0.020(5) 0.000 C4 0.030(4) 0.101(9) 0.020(4) 0.010(4) 0.016(4) 0.005(4) C5 0.053(6) 0.098(9) 0.037(5) 0.022(6) 0.024(5) 0.019(6) C11 0.041(5) 0.045(6) 0.021(4) 0.006(4) 0.018(4) -0.003(4) C12 0.050(6) 0.076(8) 0.035(5) -0.017(5) 0.029(5) -0.021(5) C13 0.053(7) 0.104(11) 0.047(6) -0.027(7) 0.028(5) -0.039(7) C14 0.097(10) 0.090(11) 0.065(8) -0.006(8) 0.038(8) -0.057(9) C15 0.095(10) 0.036(8) 0.147(13) -0.002(8) 0.029(9) -0.019(7) C16 0.053(6) 0.026(6) 0.084(8) -0.005(6) 0.013(6) -0.011(5) C21 0.040(5) 0.021(5) 0.029(4) -0.006(4) 0.022(4) -0.005(4) C22 0.040(5) 0.044(6) 0.033(5) 0.011(4) 0.018(4) 0.007(4) C23 0.060(6) 0.041(6) 0.033(5) 0.011(4) 0.028(5) 0.010(5) C24 0.052(6) 0.068(8) 0.050(6) 0.012(6) 0.025(5) 0.026(6) C25 0.044(6) 0.094(9) 0.061(7) 0.025(6) 0.036(5) 0.027(6) C26 0.043(5) 0.052(6) 0.033(5) 0.014(4) 0.020(4) 0.012(4) B1 0.061(13) 0.02(2) 0.052(12) 0.002(10) 0.041(11) -0.006(9) _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 2.341(2) 6 ? Pt1 P1 2.341(2) 2_655 ? Pt1 P1 2.341(2) . ? Pt1 P1 2.341(2) 5_655 ? S1 C1 1.741(7) . ? S1 C2 1.762(6) . ? S2 C3 1.749(6) . ? S2 C4 1.764(8) . ? P1 C21 1.795(8) . ? P1 C1 1.815(7) . ? P1 C11 1.815(9) . ? F1 B1 1.383(19) . ? F1 B1 1.383(18) 6 ? F2 B1 1.397(19) 6 ? F2 B1 1.397(19) . ? F3 F3 0.88(3) 6 ? F3 B1 1.12(2) 6 ? F3 B1 1.35(2) . ? F3 F4 1.39(2) 6 ? F4 B1 1.34(2) . ? F4 F3 1.39(2) 6 ? C1 C1 1.357(14) 6 ? C2 C3 1.343(13) . ? C2 S1 1.762(6) 6 ? C3 S2 1.749(6) 6 ? C4 C4 1.317(19) 6 ? C4 C5 1.519(11) . ? C11 C16 1.371(12) . ? C11 C12 1.375(11) . ? C12 C13 1.380(13) . ? C13 C14 1.371(16) . ? C14 C15 1.365(17) . ? C15 C16 1.355(14) . ? C21 C26 1.382(11) . ? C21 C22 1.405(10) . ? C22 C23 1.380(11) . ? C23 C24 1.363(12) . ? C24 C25 1.381(12) . ? C25 C26 1.380(11) . ? C1P C2P 1.481(19) . ? C2P C3P 1.3900 . ? C2P C7P 1.3900 . ? C3P C4P 1.3900 . ? C4P C5P 1.3900 . ? C5P C6P 1.3900 . ? C6P C7P 1.3900 . ? C1Q C2Q 1.458(19) . ? C2Q C3Q 1.3900 . ? C2Q C7Q 1.3900 . ? C3Q C4Q 1.3900 . ? C4Q C5Q 1.3900 . ? C5Q C6Q 1.3900 . ? C6Q C7Q 1.3900 . ? C1S C2S 1.439(18) . ? C2S C3S 1.3900 . ? C2S C7S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C7S 1.3900 . ? B1 B1 0.66(3) 6 ? B1 F3 1.12(2) 6 ? 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 180.00(10) 6 2_655 ? P1 Pt1 P1 84.94(10) 6 . ? P1 Pt1 P1 95.06(10) 2_655 . ? P1 Pt1 P1 95.06(10) 6 5_655 ? P1 Pt1 P1 84.94(10) 2_655 5_655 ? P1 Pt1 P1 180.00(12) . 5_655 ? C1 S1 C2 92.7(4) . . ? C3 S2 C4 94.9(4) . . ? C21 P1 C1 105.4(3) . . ? C21 P1 C11 106.8(4) . . ? C1 P1 C11 102.8(4) . . ? C21 P1 Pt1 116.2(3) . . ? C1 P1 Pt1 105.3(2) . . ? C11 P1 Pt1 118.7(2) . . ? B1 F1 B1 27.7(13) . 6 ? B1 F2 B1 27.4(14) 6 . ? F3 F3 B1 84.5(13) 6 6 ? F3 F3 B1 55.3(10) 6 . ? B1 F3 B1 29.2(16) 6 . ? F3 F3 F4 147.8(8) 6 6 ? B1 F3 F4 63.3(13) 6 6 ? B1 F3 F4 92.5(13) . 6 ? B1 F4 F3 48.3(13) . 6 ? C1 C1 S1 117.0(2) 6 . ? C1 C1 P1 119.8(2) 6 . ? S1 C1 P1 123.2(4) . . ? C3 C2 S1 123.5(3) . . ? C3 C2 S1 123.5(3) . 6 ? S1 C2 S1 113.0(5) . 6 ? C2 C3 S2 122.9(3) . 6 ? C2 C3 S2 122.9(3) . . ? S2 C3 S2 114.2(6) 6 . ? C4 C4 C5 129.0(5) 6 . ? C4 C4 S2 117.3(3) 6 . ? C5 C4 S2 113.6(7) . . ? C16 C11 C12 120.6(9) . . ? C16 C11 P1 120.9(7) . . ? C12 C11 P1 118.5(7) . . ? C11 C12 C13 119.6(11) . . ? C14 C13 C12 119.2(11) . . ? C15 C14 C13 120.3(11) . . ? C16 C15 C14 120.9(13) . . ? C15 C16 C11 119.3(11) . . ? C26 C21 C22 118.5(7) . . ? C26 C21 P1 121.3(6) . . ? C22 C21 P1 120.3(6) . . ? C23 C22 C21 120.2(8) . . ? C24 C23 C22 120.5(9) . . ? C23 C24 C25 120.1(9) . . ? C26 C25 C24 120.1(9) . . ? C25 C26 C21 120.7(8) . . ? C3P C2P C7P 120.0 . . ? C3P C2P C1P 113(2) . . ? C7P C2P C1P 127(2) . . ? C4P C3P C2P 120.0 . . ? C3P C4P C5P 120.0 . . ? C4P C5P C6P 120.0 . . ? C7P C6P C5P 120.0 . . ? C6P C7P C2P 120.0 . . ? C3Q C2Q C7Q 120.0 . . ? C3Q C2Q C1Q 114.7(17) . . ? C7Q C2Q C1Q 125.3(17) . . ? C2Q C3Q C4Q 120.0 . . ? C5Q C4Q C3Q 120.0 . . ? C6Q C5Q C4Q 120.0 . . ? C5Q C6Q C7Q 120.0 . . ? C6Q C7Q C2Q 120.0 . . ? C3S C2S C7S 120.0 . . ? C3S C2S C1S 117(2) . . ? C7S C2S C1S 121(2) . . ? C4S C3S C2S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C7S C6S C5S 120.0 . . ? C6S C7S C2S 120.0 . . ? B1 B1 F3 95.5(14) 6 6 ? B1 B1 F4 163.9(15) 6 . ? F3 B1 F4 68.4(16) 6 . ? B1 B1 F3 55.3(12) 6 . ? F3 B1 F3 40.3(17) 6 . ? F4 B1 F3 109(2) . . ? B1 B1 F1 76.1(8) 6 . ? F3 B1 F1 125.4(18) 6 . ? F4 B1 F1 112.3(11) . . ? F3 B1 F1 108.8(15) . . ? B1 B1 F2 76.3(8) 6 . ? F3 B1 F2 123.7(15) 6 . ? F4 B1 F2 112.3(15) . . ? F3 B1 F2 107.7(11) . . ? F1 B1 F2 106.8(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.153 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.141