Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Daniel Reger' 'Radu F. Semeniuc' 'Mark D. Smith' _publ_contact_author_name 'Daniel Reger' _publ_contact_author_address ; Department of Chemistry University of South Carolina 730 S. Main Columbia SC 29208 UNITED STATES OF AMERICA ; _publ_contact_author_email REGER@SC.EDU _publ_section_title ; Supramolecular networks of Silver(I) and Iron(II) Complexes of the Third Generation Tris(pyrazolyl)-methane Ligand Ph2(O)POCH2C(pz)3 (pz = pyrazolyl ring) ; data_rs4001s _database_code_depnum_ccdc_archive 'CCDC 272227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C46 H42 Ag2 N12 O4 P2, 2(C4 H8 O), 2(B F4) ; _chemical_formula_sum 'C54 H58 Ag2 B2 F8 N12 O6 P2' _chemical_formula_weight 1422.42 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9754(8) _cell_length_b 11.4045(8) _cell_length_c 12.9314(9) _cell_angle_alpha 109.1080(10) _cell_angle_beta 98.4090(10) _cell_angle_gamma 102.7470(10) _cell_volume 1449.22(18) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8191 _cell_measurement_theta_min 2.347 _cell_measurement_theta_max 26.352 _exptl_crystal_description parallelipiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8619 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(SADABS, Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13216 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.36 _reflns_number_total 5923 _reflns_number_gt 5283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0502P)^2^+1.3895P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5923 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.01038(2) 0.61081(2) 0.439324(18) 0.03641(10) Uani 1 1 d . . . P1 P 0.24883(7) 0.14220(7) 0.09866(6) 0.02744(17) Uani 1 1 d . . . C1 C 0.0132(2) 0.2717(2) 0.2750(2) 0.0212(5) Uani 1 1 d . . . C2 C 0.0548(3) 0.2193(3) 0.1643(2) 0.0248(6) Uani 1 1 d . . . H2A H -0.0147 0.1447 0.1082 0.030 Uiso 1 1 calc R . . H2B H 0.0749 0.2875 0.1326 0.030 Uiso 1 1 calc R . . C11 C 0.2172(3) 0.3706(3) 0.4270(2) 0.0288(6) Uani 1 1 d . . . H11 H 0.2200 0.2989 0.4484 0.035 Uiso 1 1 calc R . . C12 C 0.3115(3) 0.4850(3) 0.4618(3) 0.0378(7) Uani 1 1 d . . . H12 H 0.3923 0.5099 0.5133 0.045 Uiso 1 1 calc R . . C13 C 0.2646(3) 0.5576(3) 0.4060(3) 0.0378(7) Uani 1 1 d . . . H13 H 0.3104 0.6426 0.4146 0.045 Uiso 1 1 calc R . . C21 C -0.2021(3) 0.2461(3) 0.1602(2) 0.0315(6) Uani 1 1 d . . . H21 H -0.2075 0.1696 0.0990 0.038 Uiso 1 1 calc R . . C22 C -0.2956(3) 0.3068(3) 0.1754(3) 0.0335(7) Uani 1 1 d . . . H22 H -0.3781 0.2826 0.1267 0.040 Uiso 1 1 calc R . . C23 C -0.2451(3) 0.4109(3) 0.2764(3) 0.0323(6) Uani 1 1 d . . . H23 H -0.2898 0.4710 0.3084 0.039 Uiso 1 1 calc R . . C31 C -0.0410(3) 0.0427(3) 0.2706(2) 0.0278(6) Uani 1 1 d . . . H31 H -0.0293 -0.0012 0.1981 0.033 Uiso 1 1 calc R . . C32 C -0.0838(3) -0.0134(3) 0.3414(3) 0.0328(6) Uani 1 1 d . . . H32 H -0.1068 -0.1030 0.3294 0.039 Uiso 1 1 calc R . . C33 C -0.0867(3) 0.0890(3) 0.4359(2) 0.0299(6) Uani 1 1 d . . . H33 H -0.1131 0.0790 0.5000 0.036 Uiso 1 1 calc R . . C41 C 0.3030(3) 0.2873(3) 0.0721(2) 0.0313(6) Uani 1 1 d . . . C42 C 0.2806(3) 0.2829(4) -0.0383(3) 0.0414(8) Uani 1 1 d . . . H42 H 0.2440 0.2021 -0.0994 0.050 Uiso 1 1 calc R . . C43 C 0.3115(4) 0.3960(4) -0.0584(3) 0.0538(10) Uani 1 1 d . . . H43 H 0.2969 0.3930 -0.1335 0.065 Uiso 1 1 calc R . . C44 C 0.3638(4) 0.5141(4) 0.0309(3) 0.0529(9) Uani 1 1 d . . . H44 H 0.3828 0.5920 0.0166 0.064 Uiso 1 1 calc R . . C45 C 0.3886(3) 0.5192(4) 0.1407(3) 0.0459(8) Uani 1 1 d . . . H45 H 0.4261 0.6001 0.2016 0.055 Uiso 1 1 calc R . . C46 C 0.3587(3) 0.4064(3) 0.1612(3) 0.0344(7) Uani 1 1 d . . . H46 H 0.3761 0.4096 0.2363 0.041 Uiso 1 1 calc R . . C51 C 0.3765(3) 0.1109(3) 0.1785(3) 0.0319(6) Uani 1 1 d . . . C52 C 0.4345(3) 0.0217(3) 0.1201(3) 0.0450(8) Uani 1 1 d . . . H52 H 0.4073 -0.0183 0.0403 0.054 Uiso 1 1 calc R . . C53 C 0.5314(3) -0.0089(4) 0.1775(4) 0.0575(11) Uani 1 1 d . . . H53 H 0.5720 -0.0685 0.1371 0.069 Uiso 1 1 calc R . . C54 C 0.5695(3) 0.0478(4) 0.2945(4) 0.0567(11) Uani 1 1 d . . . H54 H 0.6353 0.0259 0.3343 0.068 Uiso 1 1 calc R . . C55 C 0.5118(3) 0.1354(4) 0.3525(3) 0.0524(9) Uani 1 1 d . . . H55 H 0.5376 0.1738 0.4324 0.063 Uiso 1 1 calc R . . C56 C 0.4159(3) 0.1679(3) 0.2949(3) 0.0423(8) Uani 1 1 d . . . H56 H 0.3772 0.2295 0.3353 0.051 Uiso 1 1 calc R . . N11 N 0.1477(2) 0.4934(2) 0.3389(2) 0.0318(5) Uani 1 1 d . . . N12 N 0.1183(2) 0.3790(2) 0.35582(19) 0.0240(5) Uani 1 1 d . . . N21 N -0.1269(2) 0.4172(2) 0.3236(2) 0.0292(5) Uani 1 1 d . . . N22 N -0.0994(2) 0.3155(2) 0.24931(18) 0.0233(5) Uani 1 1 d . . . N31 N -0.0481(2) 0.2019(2) 0.42484(19) 0.0250(5) Uani 1 1 d . . . N32 N -0.0180(2) 0.1727(2) 0.32210(18) 0.0219(4) Uani 1 1 d . . . O1 O 0.16698(17) 0.18014(18) 0.19128(15) 0.0255(4) Uani 1 1 d . . . O2 O 0.1775(2) 0.0312(2) -0.00628(18) 0.0369(5) Uani 1 1 d . . . B1 B -0.3393(5) 0.7587(4) 0.3868(4) 0.0533(11) Uani 1 1 d . . . F1 F -0.2436(3) 0.7021(2) 0.3493(2) 0.0714(7) Uani 1 1 d . . . F2 F -0.4276(2) 0.6668(3) 0.4062(2) 0.0769(8) Uani 1 1 d . . . F3 F -0.2767(2) 0.8613(2) 0.48579(19) 0.0641(6) Uani 1 1 d . . . F4 F -0.3886(3) 0.7949(3) 0.3035(3) 0.0917(10) Uani 1 1 d . . . O3 O 0.0937(3) 0.7421(3) 0.3025(3) 0.0689(8) Uani 1 1 d . . . C61 C 0.0219(5) 0.6598(6) 0.1972(5) 0.0852(17) Uani 1 1 d . . . H61B H -0.0673 0.6660 0.1897 0.102 Uiso 1 1 calc R . . H61A H 0.0192 0.5697 0.1887 0.102 Uiso 1 1 calc R . . C62 C 0.0718(8) 0.6878(9) 0.1091(6) 0.140(3) Uani 1 1 d . . . H62B H 0.0095 0.7139 0.0642 0.169 Uiso 1 1 calc R . . H62A H 0.0906 0.6112 0.0585 0.169 Uiso 1 1 calc R . . C63 C 0.1871(7) 0.7920(7) 0.1653(6) 0.112(2) Uani 1 1 d . . . H63B H 0.1796 0.8696 0.1494 0.134 Uiso 1 1 calc R . . H63A H 0.2613 0.7672 0.1390 0.134 Uiso 1 1 calc R . . C64 C 0.2054(6) 0.8200(6) 0.2883(5) 0.0892(16) Uani 1 1 d . . . H64B H 0.2828 0.7985 0.3170 0.107 Uiso 1 1 calc R . . H64A H 0.2159 0.9130 0.3300 0.107 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 0.05242(17) 0.02578(14) 0.02764(14) 0.00039(9) 0.01356(11) 0.01660(11) P1 0.0212(3) 0.0289(4) 0.0229(3) -0.0025(3) 0.0072(3) 0.0066(3) C1 0.0210(12) 0.0188(12) 0.0207(12) 0.0033(10) 0.0051(10) 0.0058(10) C2 0.0210(13) 0.0268(14) 0.0222(13) 0.0025(11) 0.0072(10) 0.0075(11) C11 0.0249(14) 0.0324(15) 0.0214(13) 0.0006(11) 0.0057(11) 0.0075(12) C12 0.0253(15) 0.0403(18) 0.0288(15) -0.0056(13) 0.0070(12) 0.0004(13) C13 0.0372(17) 0.0269(15) 0.0358(16) -0.0011(13) 0.0163(14) -0.0026(13) C21 0.0268(14) 0.0289(15) 0.0295(15) 0.0000(12) 0.0037(12) 0.0086(12) C22 0.0281(15) 0.0368(17) 0.0354(16) 0.0103(13) 0.0071(12) 0.0138(13) C23 0.0338(16) 0.0350(16) 0.0341(16) 0.0117(13) 0.0144(13) 0.0193(13) C31 0.0305(14) 0.0189(13) 0.0266(14) 0.0006(11) 0.0038(11) 0.0066(11) C32 0.0376(16) 0.0214(14) 0.0370(16) 0.0097(12) 0.0063(13) 0.0073(12) C33 0.0306(15) 0.0299(15) 0.0294(15) 0.0125(12) 0.0074(12) 0.0069(12) C41 0.0239(14) 0.0381(16) 0.0258(14) 0.0047(12) 0.0095(11) 0.0058(12) C42 0.0320(16) 0.055(2) 0.0257(15) 0.0069(14) 0.0065(13) 0.0034(15) C43 0.052(2) 0.072(3) 0.0357(19) 0.0244(19) 0.0117(16) 0.0077(19) C44 0.051(2) 0.056(2) 0.054(2) 0.028(2) 0.0166(18) 0.0059(18) C45 0.047(2) 0.0412(19) 0.0410(19) 0.0105(15) 0.0109(16) 0.0028(15) C46 0.0318(16) 0.0381(17) 0.0269(15) 0.0065(13) 0.0079(12) 0.0055(13) C51 0.0228(14) 0.0301(15) 0.0355(16) 0.0029(12) 0.0075(12) 0.0074(12) C52 0.0308(17) 0.0391(18) 0.054(2) 0.0000(16) 0.0136(15) 0.0118(14) C53 0.0350(19) 0.044(2) 0.086(3) 0.006(2) 0.0152(19) 0.0224(16) C54 0.0332(19) 0.048(2) 0.085(3) 0.022(2) 0.0004(19) 0.0149(16) C55 0.0395(19) 0.056(2) 0.053(2) 0.0141(18) -0.0026(16) 0.0155(17) C56 0.0363(17) 0.0431(19) 0.0390(18) 0.0024(15) 0.0042(14) 0.0176(15) N11 0.0340(13) 0.0204(12) 0.0368(14) 0.0051(10) 0.0141(11) 0.0042(10) N12 0.0245(11) 0.0169(11) 0.0245(11) 0.0009(9) 0.0071(9) 0.0038(9) N21 0.0354(13) 0.0257(12) 0.0268(12) 0.0034(10) 0.0128(10) 0.0154(10) N22 0.0256(11) 0.0205(11) 0.0237(11) 0.0045(9) 0.0100(9) 0.0095(9) N31 0.0270(12) 0.0255(12) 0.0223(11) 0.0066(9) 0.0093(9) 0.0084(9) N32 0.0224(11) 0.0207(11) 0.0212(11) 0.0049(9) 0.0074(9) 0.0067(9) O1 0.0221(9) 0.0286(10) 0.0232(9) 0.0031(8) 0.0082(8) 0.0102(8) O2 0.0300(11) 0.0356(12) 0.0298(11) -0.0053(9) 0.0073(9) 0.0064(9) B1 0.067(3) 0.035(2) 0.046(2) 0.0160(18) -0.001(2) 0.000(2) F1 0.112(2) 0.0491(14) 0.0564(14) 0.0211(12) 0.0303(14) 0.0208(14) F2 0.0592(15) 0.0772(18) 0.0768(17) 0.0419(15) -0.0076(13) -0.0192(13) F3 0.0675(15) 0.0503(13) 0.0507(13) 0.0000(11) 0.0160(11) -0.0017(11) F4 0.106(2) 0.0616(17) 0.090(2) 0.0452(16) -0.0226(17) -0.0050(15) O3 0.098(2) 0.0596(18) 0.066(2) 0.0308(16) 0.0357(18) 0.0335(18) C61 0.067(3) 0.120(5) 0.085(4) 0.072(4) 0.008(3) 0.011(3) C62 0.137(6) 0.176(8) 0.080(4) 0.041(5) 0.050(4) -0.015(6) C63 0.136(6) 0.092(4) 0.121(5) 0.050(4) 0.074(5) 0.016(4) C64 0.091(4) 0.071(3) 0.101(4) 0.025(3) 0.030(3) 0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N31 2.182(2) 2_566 ? Ag1 N21 2.257(2) . ? Ag1 N11 2.464(2) . ? Ag1 O3 2.795(3) . ? Ag1 F1 3.366(3) . ? Ag1 Ag1 3.3690(5) 2_566 ? P1 O2 1.478(2) . ? P1 O1 1.6048(19) . ? P1 C51 1.788(3) . ? P1 C41 1.791(3) . ? C1 N32 1.450(3) . ? C1 N12 1.452(3) . ? C1 N22 1.466(3) . ? C1 C2 1.540(3) . ? C2 O1 1.434(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 N12 1.358(4) . ? C11 C12 1.363(4) . ? C11 H11 0.9500 . ? C12 C13 1.394(5) . ? C12 H12 0.9500 . ? C13 N11 1.334(4) . ? C13 H13 0.9500 . ? C21 N22 1.361(4) . ? C21 C22 1.362(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 N21 1.326(4) . ? C23 H23 0.9500 . ? C31 N32 1.359(3) . ? C31 C32 1.359(4) . ? C31 H31 0.9500 . ? C32 C33 1.396(4) . ? C32 H32 0.9500 . ? C33 N31 1.325(4) . ? C33 H33 0.9500 . ? C41 C42 1.394(4) . ? C41 C46 1.395(4) . ? C42 C43 1.378(5) . ? C42 H42 0.9500 . ? C43 C44 1.387(6) . ? C43 H43 0.9500 . ? C44 C45 1.386(5) . ? C44 H44 0.9500 . ? C45 C46 1.377(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.386(5) . ? C51 C52 1.390(4) . ? C52 C53 1.381(5) . ? C52 H52 0.9500 . ? C53 C54 1.393(6) . ? C53 H53 0.9500 . ? C54 C55 1.375(6) . ? C54 H54 0.9500 . ? C55 C56 1.387(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N11 N12 1.369(3) . ? N21 N22 1.367(3) . ? N31 N32 1.368(3) . ? N31 Ag1 2.182(2) 2_566 ? B1 F4 1.357(5) . ? B1 F3 1.374(5) . ? B1 F2 1.377(5) . ? B1 F1 1.414(6) . ? O3 C61 1.371(6) . ? O3 C64 1.420(6) . ? C61 C62 1.429(7) . ? C61 H61B 0.9900 . ? C61 H61A 0.9900 . ? C62 C63 1.430(9) . ? C62 H62B 0.9900 . ? C62 H62A 0.9900 . ? C63 C64 1.489(8) . ? C63 H63B 0.9900 . ? C63 H63A 0.9900 . ? C64 H64B 0.9900 . ? C64 H64A 0.9900 . ? 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 N31 Ag1 N21 149.94(9) 2_566 . ? N31 Ag1 N11 134.01(8) 2_566 . ? N21 Ag1 N11 75.79(8) . . ? N31 Ag1 O3 88.60(9) 2_566 . ? N21 Ag1 O3 106.87(10) . . ? N11 Ag1 O3 74.28(9) . . ? N31 Ag1 F1 80.23(7) 2_566 . ? N21 Ag1 F1 79.12(7) . . ? N11 Ag1 F1 132.39(8) . . ? O3 Ag1 F1 75.30(8) . . ? N31 Ag1 Ag1 106.42(6) 2_566 2_566 ? N21 Ag1 Ag1 68.25(6) . 2_566 ? N11 Ag1 Ag1 83.07(6) . 2_566 ? O3 Ag1 Ag1 157.29(6) . 2_566 ? F1 Ag1 Ag1 123.27(4) . 2_566 ? O2 P1 O1 114.91(11) . . ? O2 P1 C51 113.42(14) . . ? O1 P1 C51 100.00(12) . . ? O2 P1 C41 111.51(14) . . ? O1 P1 C41 104.25(12) . . ? C51 P1 C41 111.92(14) . . ? N32 C1 N12 108.6(2) . . ? N32 C1 N22 110.5(2) . . ? N12 C1 N22 110.6(2) . . ? N32 C1 C2 111.2(2) . . ? N12 C1 C2 108.8(2) . . ? N22 C1 C2 107.2(2) . . ? O1 C2 C1 106.6(2) . . ? O1 C2 H2A 110.4 . . ? C1 C2 H2A 110.4 . . ? O1 C2 H2B 110.4 . . ? C1 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N12 C11 C12 106.7(3) . . ? N12 C11 H11 126.6 . . ? C12 C11 H11 126.6 . . ? C11 C12 C13 105.6(3) . . ? C11 C12 H12 127.2 . . ? C13 C12 H12 127.2 . . ? N11 C13 C12 111.9(3) . . ? N11 C13 H13 124.1 . . ? C12 C13 H13 124.1 . . ? N22 C21 C22 107.2(3) . . ? N22 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? C21 C22 C23 105.5(3) . . ? C21 C22 H22 127.3 . . ? C23 C22 H22 127.3 . . ? N21 C23 C22 112.1(3) . . ? N21 C23 H23 124.0 . . ? C22 C23 H23 124.0 . . ? N32 C31 C32 107.7(3) . . ? N32 C31 H31 126.2 . . ? C32 C31 H31 126.2 . . ? C31 C32 C33 105.2(3) . . ? C31 C32 H32 127.4 . . ? C33 C32 H32 127.4 . . ? N31 C33 C32 111.6(3) . . ? N31 C33 H33 124.2 . . ? C32 C33 H33 124.2 . . ? C42 C41 C46 119.5(3) . . ? C42 C41 P1 119.7(2) . . ? C46 C41 P1 120.6(2) . . ? C43 C42 C41 119.8(3) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.4(4) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 119.7(3) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C41 120.4(3) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C56 C51 C52 119.5(3) . . ? C56 C51 P1 122.8(2) . . ? C52 C51 P1 117.7(3) . . ? C53 C52 C51 120.3(4) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C53 C54 119.9(3) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 119.9(3) . . ? C55 C54 H54 120.1 . . ? C53 C54 H54 120.1 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.1(3) . . ? C51 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C13 N11 N12 103.9(3) . . ? C13 N11 Ag1 102.43(19) . . ? N12 N11 Ag1 102.83(16) . . ? C11 N12 N11 111.8(2) . . ? C11 N12 C1 126.4(2) . . ? N11 N12 C1 118.6(2) . . ? C23 N21 N22 104.6(2) . . ? C23 N21 Ag1 119.55(19) . . ? N22 N21 Ag1 127.89(18) . . ? C21 N22 N21 110.6(2) . . ? C21 N22 C1 124.4(2) . . ? N21 N22 C1 123.7(2) . . ? C33 N31 N32 105.1(2) . . ? C33 N31 Ag1 124.01(19) . 2_566 ? N32 N31 Ag1 129.99(17) . 2_566 ? C31 N32 N31 110.5(2) . . ? C31 N32 C1 128.2(2) . . ? N31 N32 C1 120.6(2) . . ? C2 O1 P1 119.43(16) . . ? F4 B1 F3 113.4(4) . . ? F4 B1 F2 113.7(4) . . ? F3 B1 F2 110.5(4) . . ? F4 B1 F1 105.8(4) . . ? F3 B1 F1 105.5(4) . . ? F2 B1 F1 107.3(3) . . ? B1 F1 Ag1 142.5(2) . . ? C61 O3 C64 107.3(4) . . ? C61 O3 Ag1 102.6(3) . . ? C64 O3 Ag1 142.2(3) . . ? O3 C61 C62 112.8(5) . . ? O3 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? O3 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? H61B C61 H61A 107.8 . . ? C61 C62 C63 105.1(6) . . ? C61 C62 H62B 110.7 . . ? C63 C62 H62B 110.7 . . ? C61 C62 H62A 110.7 . . ? C63 C62 H62A 110.7 . . ? H62B C62 H62A 108.8 . . ? C62 C63 C64 107.4(5) . . ? C62 C63 H63B 110.2 . . ? C64 C63 H63B 110.2 . . ? C62 C63 H63A 110.2 . . ? C64 C63 H63A 110.2 . . ? H63B C63 H63A 108.5 . . ? O3 C64 C63 106.8(5) . . ? O3 C64 H64B 110.4 . . ? C63 C64 H64B 110.4 . . ? O3 C64 H64A 110.4 . . ? C63 C64 H64A 110.4 . . ? H64B C64 H64A 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N32 C1 C2 O1 -60.7(3) . . . . ? N12 C1 C2 O1 58.8(3) . . . . ? N22 C1 C2 O1 178.4(2) . . . . ? N12 C11 C12 C13 -1.5(3) . . . . ? C11 C12 C13 N11 -0.4(4) . . . . ? N22 C21 C22 C23 -1.3(3) . . . . ? C21 C22 C23 N21 0.0(4) . . . . ? N32 C31 C32 C33 0.8(3) . . . . ? C31 C32 C33 N31 -0.1(3) . . . . ? O2 P1 C41 C42 -2.9(3) . . . . ? O1 P1 C41 C42 -127.4(2) . . . . ? C51 P1 C41 C42 125.4(3) . . . . ? O2 P1 C41 C46 172.2(2) . . . . ? O1 P1 C41 C46 47.7(3) . . . . ? C51 P1 C41 C46 -59.5(3) . . . . ? C46 C41 C42 C43 -1.1(5) . . . . ? P1 C41 C42 C43 174.1(3) . . . . ? C41 C42 C43 C44 -0.5(6) . . . . ? C42 C43 C44 C45 1.7(6) . . . . ? C43 C44 C45 C46 -1.3(6) . . . . ? C44 C45 C46 C41 -0.4(5) . . . . ? C42 C41 C46 C45 1.5(5) . . . . ? P1 C41 C46 C45 -173.6(3) . . . . ? O2 P1 C51 C56 -149.4(3) . . . . ? O1 P1 C51 C56 -26.6(3) . . . . ? C41 P1 C51 C56 83.3(3) . . . . ? O2 P1 C51 C52 28.2(3) . . . . ? O1 P1 C51 C52 151.1(3) . . . . ? C41 P1 C51 C52 -99.0(3) . . . . ? C56 C51 C52 C53 -0.6(5) . . . . ? P1 C51 C52 C53 -178.4(3) . . . . ? C51 C52 C53 C54 1.3(6) . . . . ? C52 C53 C54 C55 -0.9(6) . . . . ? C53 C54 C55 C56 -0.2(6) . . . . ? C52 C51 C56 C55 -0.5(5) . . . . ? P1 C51 C56 C55 177.1(3) . . . . ? C54 C55 C56 C51 0.9(6) . . . . ? C12 C13 N11 N12 2.0(3) . . . . ? C12 C13 N11 Ag1 108.8(2) . . . . ? N31 Ag1 N11 C13 15.2(3) 2_566 . . . ? N21 Ag1 N11 C13 -160.2(2) . . . . ? O3 Ag1 N11 C13 87.3(2) . . . . ? F1 Ag1 N11 C13 139.46(19) . . . . ? Ag1 Ag1 N11 C13 -91.0(2) 2_566 . . . ? N31 Ag1 N11 N12 122.89(16) 2_566 . . . ? N21 Ag1 N11 N12 -52.54(16) . . . . ? O3 Ag1 N11 N12 -165.01(19) . . . . ? F1 Ag1 N11 N12 -112.88(16) . . . . ? Ag1 Ag1 N11 N12 16.71(15) 2_566 . . . ? C12 C11 N12 N11 2.8(3) . . . . ? C12 C11 N12 C1 162.0(2) . . . . ? C13 N11 N12 C11 -3.0(3) . . . . ? Ag1 N11 N12 C11 -109.5(2) . . . . ? C13 N11 N12 C1 -164.0(2) . . . . ? Ag1 N11 N12 C1 89.5(2) . . . . ? N32 C1 N12 C11 34.3(3) . . . . ? N22 C1 N12 C11 155.7(2) . . . . ? C2 C1 N12 C11 -86.8(3) . . . . ? N32 C1 N12 N11 -167.7(2) . . . . ? N22 C1 N12 N11 -46.4(3) . . . . ? C2 C1 N12 N11 71.1(3) . . . . ? C22 C23 N21 N22 1.4(3) . . . . ? C22 C23 N21 Ag1 152.8(2) . . . . ? N31 Ag1 N21 C23 42.6(3) 2_566 . . . ? N11 Ag1 N21 C23 -144.0(2) . . . . ? O3 Ag1 N21 C23 -75.7(2) . . . . ? F1 Ag1 N21 C23 -4.8(2) . . . . ? Ag1 Ag1 N21 C23 127.9(2) 2_566 . . . ? N31 Ag1 N21 N22 -173.39(19) 2_566 . . . ? N11 Ag1 N21 N22 0.0(2) . . . . ? O3 Ag1 N21 N22 68.4(2) . . . . ? F1 Ag1 N21 N22 139.2(2) . . . . ? Ag1 Ag1 N21 N22 -88.1(2) 2_566 . . . ? C22 C21 N22 N21 2.2(3) . . . . ? C22 C21 N22 C1 169.4(3) . . . . ? C23 N21 N22 C21 -2.2(3) . . . . ? Ag1 N21 N22 C21 -150.4(2) . . . . ? C23 N21 N22 C1 -169.5(2) . . . . ? Ag1 N21 N22 C1 42.3(3) . . . . ? N32 C1 N22 C21 -74.7(3) . . . . ? N12 C1 N22 C21 165.1(2) . . . . ? C2 C1 N22 C21 46.7(3) . . . . ? N32 C1 N22 N21 90.9(3) . . . . ? N12 C1 N22 N21 -29.3(3) . . . . ? C2 C1 N22 N21 -147.7(2) . . . . ? C32 C33 N31 N32 -0.7(3) . . . . ? C32 C33 N31 Ag1 -170.64(19) . . . 2_566 ? C32 C31 N32 N31 -1.3(3) . . . . ? C32 C31 N32 C1 -171.6(2) . . . . ? C33 N31 N32 C31 1.3(3) . . . . ? Ag1 N31 N32 C31 170.35(19) 2_566 . . . ? C33 N31 N32 C1 172.3(2) . . . . ? Ag1 N31 N32 C1 -18.6(3) 2_566 . . . ? N12 C1 N32 C31 -135.2(3) . . . . ? N22 C1 N32 C31 103.4(3) . . . . ? C2 C1 N32 C31 -15.6(4) . . . . ? N12 C1 N32 N31 55.4(3) . . . . ? N22 C1 N32 N31 -66.0(3) . . . . ? C2 C1 N32 N31 175.1(2) . . . . ? C1 C2 O1 P1 -170.14(16) . . . . ? O2 P1 O1 C2 -60.9(2) . . . . ? C51 P1 O1 C2 177.3(2) . . . . ? C41 P1 O1 C2 61.4(2) . . . . ? F4 B1 F1 Ag1 164.3(2) . . . . ? F3 B1 F1 Ag1 43.8(5) . . . . ? F2 B1 F1 Ag1 -74.0(4) . . . . ? N31 Ag1 F1 B1 -43.3(4) 2_566 . . . ? N21 Ag1 F1 B1 114.7(4) . . . . ? N11 Ag1 F1 B1 173.8(3) . . . . ? O3 Ag1 F1 B1 -134.4(4) . . . . ? Ag1 Ag1 F1 B1 60.0(4) 2_566 . . . ? N31 Ag1 O3 C61 -149.2(3) 2_566 . . . ? N21 Ag1 O3 C61 4.7(3) . . . . ? N11 Ag1 O3 C61 74.0(3) . . . . ? F1 Ag1 O3 C61 -68.9(3) . . . . ? Ag1 Ag1 O3 C61 78.5(4) 2_566 . . . ? N31 Ag1 O3 C64 69.1(5) 2_566 . . . ? N21 Ag1 O3 C64 -137.1(5) . . . . ? N11 Ag1 O3 C64 -67.7(5) . . . . ? F1 Ag1 O3 C64 149.3(5) . . . . ? Ag1 Ag1 O3 C64 -63.3(6) 2_566 . . . ? C64 O3 C61 C62 -7.0(8) . . . . ? Ag1 O3 C61 C62 -163.7(6) . . . . ? O3 C61 C62 C63 2.9(10) . . . . ? C61 C62 C63 C64 2.2(9) . . . . ? C61 O3 C64 C63 8.0(6) . . . . ? Ag1 O3 C64 C63 148.8(4) . . . . ? C62 C63 C64 O3 -6.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.052 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.083 ### END ### Compound 7 data_7 _database_code_depnum_ccdc_archive 'CCDC 625866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 Ag2 F6 N12 O6 S2' _chemical_formula_weight 942.36 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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6922(6) _cell_length_b 9.4966(7) _cell_length_c 10.3316(8) _cell_angle_alpha 71.5870(10) _cell_angle_beta 68.4530(10) _cell_angle_gamma 81.8470(10) _cell_volume 752.30(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5799 _cell_measurement_theta_min 2.212 _cell_measurement_theta_max 26.360 _exptl_crystal_description 'flat bar' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8685 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(SADABS, Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8993 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.40 _reflns_number_total 3066 _reflns_number_gt 2904 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0258P)^2^+0.6529P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3066 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0611 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.56022(2) 0.36646(2) 0.458674(19) 0.02649(8) Uani 1 1 d . . . C1 C 0.6400(3) 0.3494(2) 0.7838(2) 0.0171(4) Uani 1 1 d . . . H1 H 0.6686 0.3249 0.8740 0.021 Uiso 1 1 calc R . . C11 C 0.8005(3) 0.1119(3) 0.7764(3) 0.0238(5) Uani 1 1 d . . . H11 H 0.8349 0.1012 0.8564 0.029 Uiso 1 1 calc R . . C12 C 0.8370(3) 0.0164(3) 0.6938(3) 0.0261(5) Uani 1 1 d . . . H12 H 0.9014 -0.0734 0.7038 0.031 Uiso 1 1 calc R . . C13 C 0.7587(3) 0.0797(3) 0.5907(3) 0.0226(5) Uani 1 1 d . . . H13 H 0.7616 0.0370 0.5181 0.027 Uiso 1 1 calc R . . C21 C 0.3608(3) 0.3144(3) 0.9712(3) 0.0243(5) Uani 1 1 d . . . H21 H 0.3933 0.2773 1.0544 0.029 Uiso 1 1 calc R . . C22 C 0.2030(3) 0.3308(3) 0.9699(3) 0.0281(5) Uani 1 1 d . . . H22 H 0.1034 0.3082 1.0509 0.034 Uiso 1 1 calc R . . C23 C 0.2197(3) 0.3882(3) 0.8234(3) 0.0258(5) Uani 1 1 d . . . H23 H 0.1291 0.4113 0.7890 0.031 Uiso 1 1 calc R . . C31 C 0.8391(3) 0.5425(3) 0.7157(3) 0.0234(5) Uani 1 1 d . . . H31 H 0.8696 0.5084 0.8001 0.028 Uiso 1 1 calc R . . C32 C 0.9053(3) 0.6586(3) 0.5963(3) 0.0283(5) Uani 1 1 d . . . H32 H 0.9902 0.7217 0.5803 0.034 Uiso 1 1 calc R . . C33 C 0.8209(3) 0.6642(3) 0.5032(3) 0.0288(5) Uani 1 1 d . . . H33 H 0.8404 0.7351 0.4107 0.035 Uiso 1 1 calc R . . N11 N 0.6800(2) 0.2067(2) 0.6076(2) 0.0191(4) Uani 1 1 d . . . N12 N 0.7061(2) 0.2246(2) 0.7231(2) 0.0179(4) Uani 1 1 d . . . N21 N 0.3767(2) 0.4066(2) 0.7379(2) 0.0237(4) Uani 1 1 d . . . N22 N 0.4626(2) 0.3613(2) 0.8312(2) 0.0182(4) Uani 1 1 d . . . N31 N 0.7096(3) 0.5586(2) 0.5588(2) 0.0247(4) Uani 1 1 d . . . N32 N 0.7223(2) 0.4856(2) 0.6911(2) 0.0188(4) Uani 1 1 d . . . S1 S 0.72923(7) 0.22760(6) 0.16901(6) 0.02131(13) Uani 1 1 d . . . O1 O 0.5622(2) 0.2833(2) 0.2190(3) 0.0447(5) Uani 1 1 d . . . O2 O 0.8289(2) 0.2331(2) 0.25200(19) 0.0300(4) Uani 1 1 d . . . O3 O 0.8115(2) 0.2732(2) 0.01403(19) 0.0309(4) Uani 1 1 d . . . C41 C 0.7038(3) 0.0299(3) 0.2073(3) 0.0274(5) Uani 1 1 d . . . F1 F 0.8480(2) -0.04010(18) 0.1632(2) 0.0474(5) Uani 1 1 d . . . F2 F 0.6089(2) 0.00593(18) 0.14056(17) 0.0357(4) Uani 1 1 d . . . F3 F 0.6325(2) -0.03300(19) 0.34975(18) 0.0446(4) 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 Ag1 0.03581(12) 0.02418(11) 0.02378(11) -0.00706(8) -0.01858(8) 0.00921(8) C1 0.0206(11) 0.0170(10) 0.0145(10) -0.0031(8) -0.0086(8) 0.0014(8) C11 0.0268(12) 0.0237(12) 0.0203(11) -0.0041(9) -0.0117(10) 0.0058(10) C12 0.0305(13) 0.0228(12) 0.0229(12) -0.0050(10) -0.0112(10) 0.0079(10) C13 0.0254(12) 0.0218(12) 0.0194(11) -0.0051(9) -0.0075(9) 0.0010(9) C21 0.0256(12) 0.0262(12) 0.0182(11) -0.0049(9) -0.0060(9) 0.0003(10) C22 0.0214(12) 0.0314(13) 0.0278(13) -0.0097(11) -0.0026(10) -0.0027(10) C23 0.0201(12) 0.0272(13) 0.0340(13) -0.0115(11) -0.0124(10) 0.0025(10) C31 0.0217(11) 0.0260(12) 0.0268(12) -0.0116(10) -0.0110(10) 0.0025(9) C32 0.0269(13) 0.0218(12) 0.0356(14) -0.0106(11) -0.0071(11) -0.0031(10) C33 0.0314(13) 0.0211(12) 0.0256(12) -0.0018(10) -0.0048(10) -0.0003(10) N11 0.0215(9) 0.0198(9) 0.0169(9) -0.0043(7) -0.0085(8) -0.0003(7) N12 0.0199(9) 0.0179(9) 0.0167(9) -0.0042(7) -0.0086(7) 0.0012(7) N21 0.0224(10) 0.0273(11) 0.0236(10) -0.0049(8) -0.0136(8) 0.0028(8) N22 0.0188(9) 0.0201(9) 0.0166(9) -0.0054(7) -0.0077(7) 0.0019(7) N31 0.0297(11) 0.0223(10) 0.0199(10) -0.0011(8) -0.0109(8) 0.0009(8) N32 0.0204(9) 0.0180(9) 0.0184(9) -0.0031(7) -0.0092(8) 0.0006(7) S1 0.0243(3) 0.0203(3) 0.0213(3) -0.0068(2) -0.0104(2) 0.0021(2) O1 0.0294(10) 0.0417(12) 0.0676(15) -0.0291(11) -0.0151(10) 0.0114(9) O2 0.0400(10) 0.0337(10) 0.0217(9) -0.0054(7) -0.0163(8) -0.0076(8) O3 0.0427(11) 0.0314(10) 0.0199(9) 0.0001(7) -0.0152(8) -0.0102(8) C41 0.0305(13) 0.0243(12) 0.0275(13) -0.0037(10) -0.0127(11) -0.0021(10) F1 0.0401(9) 0.0279(9) 0.0754(13) -0.0191(9) -0.0225(9) 0.0123(7) F2 0.0427(9) 0.0356(9) 0.0375(9) -0.0116(7) -0.0194(7) -0.0099(7) F3 0.0607(11) 0.0410(9) 0.0292(8) 0.0072(7) -0.0190(8) -0.0236(8) _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 N11 2.2375(19) . ? Ag1 N31 2.407(2) 2_666 ? Ag1 N21 2.413(2) 2_666 ? Ag1 O1 2.821(2) . ? Ag1 N21 2.856(2) . ? Ag1 Ag1 2.8664(4) 2_666 ? Ag1 O2 2.9710(19) . ? Ag1 N31 2.989(2) . ? C1 N22 1.436(3) . ? C1 N32 1.442(3) . ? C1 N12 1.462(3) . ? C1 H1 1.0000 . ? C11 N12 1.354(3) . ? C11 C12 1.364(3) . ? C11 H11 0.9500 . ? C12 C13 1.404(3) . ? C12 H12 0.9500 . ? C13 N11 1.328(3) . ? C13 H13 0.9500 . ? C21 N22 1.356(3) . ? C21 C22 1.363(4) . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 H22 0.9500 . ? C23 N21 1.326(3) . ? C23 H23 0.9500 . ? C31 N32 1.349(3) . ? C31 C32 1.367(4) . ? C31 H31 0.9500 . ? C32 C33 1.393(4) . ? C32 H32 0.9500 . ? C33 N31 1.332(3) . ? C33 H33 0.9500 . ? N11 N12 1.358(3) . ? N21 N22 1.359(3) . ? N21 Ag1 2.413(2) 2_666 ? N31 N32 1.361(3) . ? N31 Ag1 2.407(2) 2_666 ? S1 O1 1.435(2) . ? S1 O3 1.4393(18) . ? S1 O2 1.4408(18) . ? S1 C41 1.821(3) . ? C41 F1 1.326(3) . ? C41 F2 1.333(3) . ? C41 F3 1.337(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag1 N31 140.42(7) . 2_666 ? N11 Ag1 N21 138.91(7) . 2_666 ? N31 Ag1 N21 79.21(7) 2_666 2_666 ? N11 Ag1 O1 116.83(7) . . ? N31 Ag1 O1 75.24(6) 2_666 . ? N21 Ag1 O1 76.48(7) 2_666 . ? N11 Ag1 N21 75.47(6) . . ? N31 Ag1 N21 77.81(6) 2_666 . ? N21 Ag1 N21 114.72(5) 2_666 . ? O1 Ag1 N21 148.14(6) . . ? N11 Ag1 Ag1 112.62(5) . 2_666 ? N31 Ag1 Ag1 68.42(5) 2_666 2_666 ? N21 Ag1 Ag1 64.83(5) 2_666 2_666 ? O1 Ag1 Ag1 130.50(4) . 2_666 ? N21 Ag1 Ag1 49.88(4) . 2_666 ? N11 Ag1 O2 78.81(6) . . ? N31 Ag1 O2 124.59(6) 2_666 . ? N21 Ag1 O2 84.48(6) 2_666 . ? O1 Ag1 O2 49.44(5) . . ? N21 Ag1 O2 154.26(5) . . ? Ag1 Ag1 O2 144.73(4) 2_666 . ? N11 Ag1 N31 75.41(6) . . ? N31 Ag1 N31 116.91(5) 2_666 . ? N21 Ag1 N31 75.10(6) 2_666 . ? O1 Ag1 N31 145.89(6) . . ? N21 Ag1 N31 63.39(6) . . ? Ag1 Ag1 N31 48.49(4) 2_666 . ? O2 Ag1 N31 109.01(5) . . ? N22 C1 N32 114.56(18) . . ? N22 C1 N12 112.55(18) . . ? N32 C1 N12 112.31(18) . . ? N22 C1 H1 105.5 . . ? N32 C1 H1 105.5 . . ? N12 C1 H1 105.5 . . ? N12 C11 C12 107.2(2) . . ? N12 C11 H11 126.4 . . ? C12 C11 H11 126.4 . . ? C11 C12 C13 105.0(2) . . ? C11 C12 H12 127.5 . . ? C13 C12 H12 127.5 . . ? N11 C13 C12 111.5(2) . . ? N11 C13 H13 124.3 . . ? C12 C13 H13 124.3 . . ? N22 C21 C22 107.0(2) . . ? N22 C21 H21 126.5 . . ? C22 C21 H21 126.5 . . ? C21 C22 C23 104.9(2) . . ? C21 C22 H22 127.6 . . ? C23 C22 H22 127.6 . . ? N21 C23 C22 112.2(2) . . ? N21 C23 H23 123.9 . . ? C22 C23 H23 123.9 . . ? N32 C31 C32 107.1(2) . . ? N32 C31 H31 126.5 . . ? C32 C31 H31 126.5 . . ? C31 C32 C33 104.8(2) . . ? C31 C32 H32 127.6 . . ? C33 C32 H32 127.6 . . ? N31 C33 C32 112.2(2) . . ? N31 C33 H33 123.9 . . ? C32 C33 H33 123.9 . . ? C13 N11 N12 104.74(18) . . ? C13 N11 Ag1 126.47(15) . . ? N12 N11 Ag1 128.38(14) . . ? C11 N12 N11 111.64(19) . . ? C11 N12 C1 123.85(19) . . ? N11 N12 C1 124.51(18) . . ? C23 N21 N22 104.20(19) . . ? C23 N21 Ag1 116.77(16) . 2_666 ? N22 N21 Ag1 121.46(14) . 2_666 ? C23 N21 Ag1 133.53(16) . . ? N22 N21 Ag1 112.94(13) . . ? Ag1 N21 Ag1 65.28(5) 2_666 . ? C21 N22 N21 111.75(19) . . ? C21 N22 C1 124.77(19) . . ? N21 N22 C1 123.12(18) . . ? C33 N31 N32 103.8(2) . . ? C33 N31 Ag1 116.73(16) . 2_666 ? N32 N31 Ag1 119.17(14) . 2_666 ? C33 N31 Ag1 139.24(17) . . ? N32 N31 Ag1 110.87(13) . . ? Ag1 N31 Ag1 63.09(5) 2_666 . ? C31 N32 N31 112.13(19) . . ? C31 N32 C1 123.50(19) . . ? N31 N32 C1 123.69(19) . . ? O1 S1 O3 115.19(13) . . ? O1 S1 O2 115.06(13) . . ? O3 S1 O2 114.66(11) . . ? O1 S1 C41 103.06(12) . . ? O3 S1 C41 102.59(11) . . ? O2 S1 C41 103.86(11) . . ? S1 O1 Ag1 101.04(11) . . ? S1 O2 Ag1 94.46(9) . . ? F1 C41 F2 107.6(2) . . ? F1 C41 F3 107.7(2) . . ? F2 C41 F3 107.7(2) . . ? F1 C41 S1 111.47(17) . . ? F2 C41 S1 111.29(17) . . ? F3 C41 S1 110.87(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 N11 0.5(3) . . . . ? N22 C21 C22 C23 0.3(3) . . . . ? C21 C22 C23 N21 0.1(3) . . . . ? N32 C31 C32 C33 -0.2(3) . . . . ? C31 C32 C33 N31 -0.4(3) . . . . ? C12 C13 N11 N12 -0.7(3) . . . . ? C12 C13 N11 Ag1 172.39(16) . . . . ? N31 Ag1 N11 C13 102.7(2) 2_666 . . . ? N21 Ag1 N11 C13 -97.1(2) 2_666 . . . ? O1 Ag1 N11 C13 3.3(2) . . . . ? N21 Ag1 N11 C13 151.8(2) . . . . ? Ag1 Ag1 N11 C13 -174.23(17) 2_666 . . . ? O2 Ag1 N11 C13 -29.23(18) . . . . ? N31 Ag1 N11 C13 -142.5(2) . . . . ? N31 Ag1 N11 N12 -85.8(2) 2_666 . . . ? N21 Ag1 N11 N12 74.3(2) 2_666 . . . ? O1 Ag1 N11 N12 174.76(16) . . . . ? N21 Ag1 N11 N12 -36.80(17) . . . . ? Ag1 Ag1 N11 N12 -2.80(19) 2_666 . . . ? O2 Ag1 N11 N12 142.20(18) . . . . ? N31 Ag1 N11 N12 28.96(17) . . . . ? C12 C11 N12 N11 -0.3(3) . . . . ? C12 C11 N12 C1 179.3(2) . . . . ? C13 N11 N12 C11 0.6(2) . . . . ? Ag1 N11 N12 C11 -172.28(15) . . . . ? C13 N11 N12 C1 -179.0(2) . . . . ? Ag1 N11 N12 C1 8.1(3) . . . . ? N22 C1 N12 C11 -120.8(2) . . . . ? N32 C1 N12 C11 108.1(2) . . . . ? N22 C1 N12 N11 58.7(3) . . . . ? N32 C1 N12 N11 -72.3(3) . . . . ? C22 C23 N21 N22 -0.4(3) . . . . ? C22 C23 N21 Ag1 -137.38(18) . . . 2_666 ? C22 C23 N21 Ag1 142.22(19) . . . . ? N11 Ag1 N21 C23 -118.2(2) . . . . ? N31 Ag1 N21 C23 32.3(2) 2_666 . . . ? N21 Ag1 N21 C23 104.3(2) 2_666 . . . ? O1 Ag1 N21 C23 -0.4(3) . . . . ? Ag1 Ag1 N21 C23 104.3(2) 2_666 . . . ? O2 Ag1 N21 C23 -120.4(2) . . . . ? N31 Ag1 N21 C23 161.1(2) . . . . ? N11 Ag1 N21 N22 22.13(14) . . . . ? N31 Ag1 N21 N22 172.65(16) 2_666 . . . ? N21 Ag1 N21 N22 -115.41(16) 2_666 . . . ? O1 Ag1 N21 N22 139.93(14) . . . . ? Ag1 Ag1 N21 N22 -115.41(16) 2_666 . . . ? O2 Ag1 N21 N22 19.9(2) . . . . ? N31 Ag1 N21 N22 -58.58(14) . . . . ? N11 Ag1 N21 Ag1 137.55(7) . . . 2_666 ? N31 Ag1 N21 Ag1 -71.93(6) 2_666 . . 2_666 ? N21 Ag1 N21 Ag1 0.0 2_666 . . 2_666 ? O1 Ag1 N21 Ag1 -104.66(11) . . . 2_666 ? O2 Ag1 N21 Ag1 135.28(11) . . . 2_666 ? N31 Ag1 N21 Ag1 56.83(5) . . . 2_666 ? C22 C21 N22 N21 -0.6(3) . . . . ? C22 C21 N22 C1 -173.8(2) . . . . ? C23 N21 N22 C21 0.6(3) . . . . ? Ag1 N21 N22 C21 135.00(17) 2_666 . . . ? Ag1 N21 N22 C21 -150.86(16) . . . . ? C23 N21 N22 C1 174.0(2) . . . . ? Ag1 N21 N22 C1 -51.6(3) 2_666 . . . ? Ag1 N21 N22 C1 22.5(2) . . . . ? N32 C1 N22 C21 -129.1(2) . . . . ? N12 C1 N22 C21 101.0(2) . . . . ? N32 C1 N22 N21 58.4(3) . . . . ? N12 C1 N22 N21 -71.6(3) . . . . ? C32 C33 N31 N32 0.8(3) . . . . ? C32 C33 N31 Ag1 134.03(18) . . . 2_666 ? C32 C33 N31 Ag1 -147.03(19) . . . . ? N11 Ag1 N31 C33 119.9(3) . . . . ? N31 Ag1 N31 C33 -100.6(3) 2_666 . . . ? N21 Ag1 N31 C33 -31.2(2) 2_666 . . . ? O1 Ag1 N31 C33 3.3(3) . . . . ? N21 Ag1 N31 C33 -159.3(3) . . . . ? Ag1 Ag1 N31 C33 -100.6(3) 2_666 . . . ? O2 Ag1 N31 C33 47.4(3) . . . . ? N11 Ag1 N31 N32 -26.51(14) . . . . ? N31 Ag1 N31 N32 113.04(15) 2_666 . . . ? N21 Ag1 N31 N32 -177.58(15) 2_666 . . . ? O1 Ag1 N31 N32 -143.08(13) . . . . ? N21 Ag1 N31 N32 54.31(14) . . . . ? Ag1 Ag1 N31 N32 113.04(15) 2_666 . . . ? O2 Ag1 N31 N32 -98.94(14) . . . . ? N11 Ag1 N31 Ag1 -139.55(7) . . . 2_666 ? N31 Ag1 N31 Ag1 0.0 2_666 . . 2_666 ? N21 Ag1 N31 Ag1 69.38(6) 2_666 . . 2_666 ? O1 Ag1 N31 Ag1 103.88(10) . . . 2_666 ? N21 Ag1 N31 Ag1 -58.73(5) . . . 2_666 ? O2 Ag1 N31 Ag1 148.02(4) . . . 2_666 ? C32 C31 N32 N31 0.7(3) . . . . ? C32 C31 N32 C1 171.5(2) . . . . ? C33 N31 N32 C31 -0.9(3) . . . . ? Ag1 N31 N32 C31 -132.74(17) 2_666 . . . ? Ag1 N31 N32 C31 157.25(15) . . . . ? C33 N31 N32 C1 -171.6(2) . . . . ? Ag1 N31 N32 C1 56.5(2) 2_666 . . . ? Ag1 N31 N32 C1 -13.5(2) . . . . ? N22 C1 N32 C31 128.1(2) . . . . ? N12 C1 N32 C31 -101.9(2) . . . . ? N22 C1 N32 N31 -62.2(3) . . . . ? N12 C1 N32 N31 67.9(3) . . . . ? O3 S1 O1 Ag1 -136.72(10) . . . . ? O2 S1 O1 Ag1 0.07(14) . . . . ? C41 S1 O1 Ag1 112.40(10) . . . . ? N11 Ag1 O1 S1 -44.05(14) . . . . ? N31 Ag1 O1 S1 176.49(13) 2_666 . . . ? N21 Ag1 O1 S1 94.29(12) 2_666 . . . ? N21 Ag1 O1 S1 -150.38(9) . . . . ? Ag1 Ag1 O1 S1 132.98(8) 2_666 . . . ? O2 Ag1 O1 S1 -0.04(8) . . . . ? N31 Ag1 O1 S1 60.03(16) . . . . ? O1 S1 O2 Ag1 -0.06(13) . . . . ? O3 S1 O2 Ag1 136.96(9) . . . . ? C41 S1 O2 Ag1 -111.93(10) . . . . ? N11 Ag1 O2 S1 140.84(10) . . . . ? N31 Ag1 O2 S1 -4.04(12) 2_666 . . . ? N21 Ag1 O2 S1 -76.88(9) 2_666 . . . ? O1 Ag1 O2 S1 0.04(8) . . . . ? N21 Ag1 O2 S1 143.07(11) . . . . ? Ag1 Ag1 O2 S1 -105.64(8) 2_666 . . . ? N31 Ag1 O2 S1 -149.03(8) . . . . ? O1 S1 C41 F1 178.0(2) . . . . ? O3 S1 C41 F1 58.1(2) . . . . ? O2 S1 C41 F1 -61.6(2) . . . . ? O1 S1 C41 F2 57.9(2) . . . . ? O3 S1 C41 F2 -62.0(2) . . . . ? O2 S1 C41 F2 178.26(17) . . . . ? O1 S1 C41 F3 -62.0(2) . . . . ? O3 S1 C41 F3 178.06(17) . . . . ? O2 S1 C41 F3 58.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.725 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.075 ### END ### END OF COMBINED CIF # Attachment 'rs4001bt.cif' data_rs4001bt _database_code_depnum_ccdc_archive 'CCDC 670349' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H42 Ag N12 O4 P2, B F4' _chemical_formula_sum 'C46 H42 Ag B F4 N12 O4 P2' _chemical_formula_weight 1083.54 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0846(7) _cell_length_b 10.9600(9) _cell_length_c 13.9140(12) _cell_angle_alpha 67.246(2) _cell_angle_beta 73.530(2) _cell_angle_gamma 71.977(2) _cell_volume 1193.48(17) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 8191 _cell_measurement_theta_min 2.347 _cell_measurement_theta_max 26.352 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 9146 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4197 _reflns_number_gt 3120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _refine_special_details ; BF4 disordered over inversion center 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^)+(0.0244P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4197 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 Ag1 Ag 0.0000 0.0000 0.5000 0.04506(16) Uani 1 2 d S . . P1 P 0.04017(11) 0.64020(8) 0.11315(7) 0.0262(2) Uani 1 1 d . . . C1 C 0.0554(4) 0.2573(3) 0.2726(2) 0.0247(8) Uani 1 1 d . . . C2 C 0.0958(4) 0.3775(3) 0.1740(2) 0.0243(8) Uani 1 1 d . . . H2A H 0.2110 0.3707 0.1554 0.029 Uiso 1 1 calc R . . H2B H 0.0601 0.3786 0.1127 0.029 Uiso 1 1 calc R . . C11 C 0.2012(4) 0.1075(3) 0.1595(3) 0.0297(8) Uani 1 1 d . . . H11 H 0.1914 0.1722 0.0912 0.036 Uiso 1 1 calc R . . C12 C 0.2687(4) -0.0274(3) 0.1820(3) 0.0384(9) Uani 1 1 d . . . H12 H 0.3180 -0.0756 0.1331 0.046 Uiso 1 1 calc R . . C13 C 0.2500(4) -0.0796(3) 0.2916(3) 0.0421(10) Uani 1 1 d . . . H13 H 0.2852 -0.1728 0.3300 0.051 Uiso 1 1 calc R . . C21 C -0.2238(4) 0.3312(3) 0.2362(3) 0.0288(8) Uani 1 1 d . . . H21 H -0.2127 0.4031 0.1708 0.035 Uiso 1 1 calc R . . C22 C -0.3554(4) 0.2835(3) 0.2871(3) 0.0357(9) Uani 1 1 d . . . H22 H -0.4547 0.3148 0.2657 0.043 Uiso 1 1 calc R . . C23 C -0.3135(5) 0.1786(3) 0.3776(3) 0.0396(9) Uani 1 1 d . . . H23 H -0.3837 0.1259 0.4291 0.047 Uiso 1 1 calc R . . C31 C -0.0024(5) 0.3140(3) 0.4421(3) 0.0360(9) Uani 1 1 d . . . H31 H -0.1143 0.3337 0.4568 0.043 Uiso 1 1 calc R . . C32 C 0.0921(5) 0.3272(4) 0.4951(3) 0.0480(11) Uani 1 1 d . . . H32 H 0.0606 0.3558 0.5557 0.058 Uiso 1 1 calc R . . C33 C 0.2456(5) 0.2901(4) 0.4427(3) 0.0447(10) Uani 1 1 d . . . H33 H 0.3368 0.2904 0.4630 0.054 Uiso 1 1 calc R . . C41 C -0.0900(4) 0.7555(3) 0.1778(3) 0.0281(8) Uani 1 1 d . . . C42 C -0.2253(4) 0.7263(3) 0.2485(3) 0.0373(9) Uani 1 1 d . . . H42 H -0.2437 0.6379 0.2701 0.045 Uiso 1 1 calc R . . C43 C -0.3347(5) 0.8226(4) 0.2886(3) 0.0507(11) Uani 1 1 d . . . H43 H -0.4279 0.8009 0.3369 0.061 Uiso 1 1 calc R . . C44 C -0.3076(6) 0.9502(4) 0.2579(4) 0.0627(13) Uani 1 1 d . . . H44 H -0.3835 1.0178 0.2836 0.075 Uiso 1 1 calc R . . C45 C -0.1708(6) 0.9801(4) 0.1901(4) 0.0682(14) Uani 1 1 d . . . H45 H -0.1505 1.0671 0.1714 0.082 Uiso 1 1 calc R . . C46 C -0.0633(5) 0.8842(3) 0.1491(3) 0.0498(11) Uani 1 1 d . . . H46 H 0.0297 0.9063 0.1008 0.060 Uiso 1 1 calc R . . C51 C 0.2374(4) 0.6467(3) 0.1038(3) 0.0282(8) Uani 1 1 d . . . C52 C 0.3276(5) 0.6932(3) 0.0047(3) 0.0413(10) Uani 1 1 d . . . H52 H 0.2856 0.7166 -0.0570 0.050 Uiso 1 1 calc R . . C53 C 0.4790(5) 0.7061(4) -0.0057(3) 0.0525(11) Uani 1 1 d . . . H53 H 0.5396 0.7393 -0.0742 0.063 Uiso 1 1 calc R . . C54 C 0.5410(5) 0.6713(3) 0.0824(4) 0.0505(11) Uani 1 1 d . . . H54 H 0.6447 0.6802 0.0750 0.061 Uiso 1 1 calc R . . C55 C 0.4536(5) 0.6230(3) 0.1824(3) 0.0420(10) Uani 1 1 d . . . H55 H 0.4974 0.5982 0.2436 0.050 Uiso 1 1 calc R . . C56 C 0.3021(4) 0.6110(3) 0.1931(3) 0.0335(9) Uani 1 1 d . . . H56 H 0.2418 0.5783 0.2618 0.040 Uiso 1 1 calc R . . N11 N 0.1775(4) 0.0152(3) 0.3369(2) 0.0416(8) Uani 1 1 d . . . N12 N 0.1509(3) 0.1321(2) 0.25293(19) 0.0269(7) Uani 1 1 d . . . N21 N -0.1666(4) 0.1605(3) 0.3840(2) 0.0377(8) Uani 1 1 d . . . N22 N -0.1102(3) 0.2577(2) 0.29540(19) 0.0242(6) Uani 1 1 d . . . N31 N 0.2493(4) 0.2545(3) 0.3612(2) 0.0392(8) Uani 1 1 d . . . N32 N 0.0942(3) 0.2672(2) 0.3635(2) 0.0286(7) Uani 1 1 d . . . O1 O 0.0085(3) 0.6596(2) 0.00939(16) 0.0344(6) Uani 1 1 d . . . O2 O 0.0152(3) 0.49810(18) 0.20108(15) 0.0267(5) Uani 1 1 d . . . B1 B 0.5000 0.5000 0.5000 0.0442(17) Uani 1 2 d S . . F1 F 0.5410(8) 0.3590(5) 0.5192(5) 0.097(2) Uani 0.50 1 d P . . F2 F 0.3828(8) 0.5156(6) 0.5843(4) 0.0876(18) Uani 0.50 1 d P . . F3 F 0.6206(10) 0.5299(10) 0.5081(11) 0.162(4) Uani 0.50 1 d P . . F4 F 0.4415(16) 0.5630(8) 0.4153(6) 0.151(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0545(3) 0.0344(2) 0.0282(2) 0.00927(16) -0.0087(2) -0.0098(2) P1 0.0330(6) 0.0210(4) 0.0259(5) -0.0045(3) -0.0097(4) -0.0084(4) C1 0.025(2) 0.0218(16) 0.0228(18) -0.0030(13) -0.0056(16) -0.0034(15) C2 0.029(2) 0.0207(16) 0.0236(18) -0.0071(13) -0.0040(16) -0.0069(15) C11 0.031(2) 0.0285(18) 0.030(2) -0.0109(14) -0.0048(17) -0.0061(16) C12 0.035(2) 0.0270(18) 0.049(2) -0.0168(17) -0.003(2) -0.0001(17) C13 0.037(3) 0.0209(17) 0.054(3) -0.0020(17) -0.009(2) 0.0001(17) C21 0.029(2) 0.0253(17) 0.030(2) -0.0075(14) -0.0112(18) -0.0001(16) C22 0.027(2) 0.0362(19) 0.047(2) -0.0156(17) -0.0106(19) -0.0044(17) C23 0.028(2) 0.037(2) 0.047(2) -0.0096(17) 0.003(2) -0.0134(18) C31 0.037(2) 0.0382(19) 0.029(2) -0.0132(16) -0.0064(19) 0.0002(18) C32 0.058(3) 0.054(2) 0.040(2) -0.0253(19) -0.016(2) -0.004(2) C33 0.042(3) 0.056(2) 0.045(3) -0.0174(19) -0.020(2) -0.009(2) C41 0.029(2) 0.0243(17) 0.035(2) -0.0107(14) -0.0154(18) -0.0019(16) C42 0.039(3) 0.038(2) 0.043(2) -0.0191(17) -0.013(2) -0.0082(19) C43 0.040(3) 0.063(3) 0.058(3) -0.032(2) -0.017(2) 0.001(2) C44 0.052(3) 0.053(3) 0.097(4) -0.051(3) -0.026(3) 0.013(2) C45 0.067(4) 0.035(2) 0.111(4) -0.036(2) -0.025(3) -0.001(2) C46 0.044(3) 0.032(2) 0.072(3) -0.0176(19) -0.010(2) -0.0084(19) C51 0.031(2) 0.0193(16) 0.036(2) -0.0076(14) -0.0069(18) -0.0082(15) C52 0.038(3) 0.047(2) 0.041(2) -0.0152(17) -0.004(2) -0.014(2) C53 0.040(3) 0.061(3) 0.051(3) -0.019(2) 0.005(2) -0.016(2) C54 0.030(3) 0.041(2) 0.081(3) -0.019(2) -0.013(2) -0.0081(19) C55 0.041(3) 0.0294(19) 0.057(3) -0.0097(17) -0.024(2) -0.0017(18) C56 0.034(2) 0.0245(17) 0.040(2) -0.0047(15) -0.0133(19) -0.0056(16) N11 0.050(2) 0.0233(15) 0.0328(18) 0.0041(13) -0.0091(16) 0.0018(14) N12 0.0307(18) 0.0187(13) 0.0250(16) -0.0016(11) -0.0072(14) -0.0026(12) N21 0.038(2) 0.0319(15) 0.0317(18) 0.0011(12) 0.0000(15) -0.0126(15) N22 0.0231(17) 0.0221(13) 0.0235(15) -0.0018(11) -0.0033(13) -0.0082(12) N31 0.027(2) 0.0555(19) 0.0365(18) -0.0133(15) -0.0121(15) -0.0073(16) N32 0.0311(19) 0.0300(14) 0.0209(15) -0.0047(12) -0.0061(14) -0.0052(13) O1 0.0443(17) 0.0308(12) 0.0314(13) -0.0060(10) -0.0147(12) -0.0115(11) O2 0.0330(15) 0.0203(11) 0.0257(12) -0.0053(9) -0.0056(11) -0.0075(10) B1 0.057(5) 0.051(4) 0.035(4) -0.021(3) -0.010(4) -0.016(4) F1 0.125(6) 0.056(3) 0.119(5) -0.031(3) -0.043(4) -0.010(4) F2 0.083(5) 0.088(4) 0.049(4) -0.017(3) 0.010(3) 0.010(4) F3 0.094(7) 0.168(9) 0.277(14) -0.105(9) 0.000(8) -0.093(7) F4 0.249(13) 0.119(6) 0.064(5) 0.008(4) -0.070(7) -0.024(8) _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 N21 2.352(3) . ? Ag1 N21 2.352(3) 2_556 ? Ag1 N11 2.362(3) . ? Ag1 N11 2.362(3) 2_556 ? P1 O1 1.474(2) . ? P1 O2 1.600(2) . ? P1 C41 1.777(3) . ? P1 C51 1.781(4) . ? C1 N22 1.446(4) . ? C1 N32 1.455(4) . ? C1 N12 1.459(4) . ? C1 C2 1.539(4) . ? C2 O2 1.433(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 N12 1.352(4) . ? C11 C12 1.361(4) . ? C11 H11 0.9500 . ? C12 C13 1.385(4) . ? C12 H12 0.9500 . ? C13 N11 1.326(4) . ? C13 H13 0.9500 . ? C21 C22 1.350(4) . ? C21 N22 1.359(4) . ? C21 H21 0.9500 . ? C22 C23 1.390(4) . ? C22 H22 0.9500 . ? C23 N21 1.311(4) . ? C23 H23 0.9500 . ? C31 C32 1.350(5) . ? C31 N32 1.356(4) . ? C31 H31 0.9500 . ? C32 C33 1.394(5) . ? C32 H32 0.9500 . ? C33 N31 1.323(4) . ? C33 H33 0.9500 . ? C41 C42 1.377(5) . ? C41 C46 1.388(4) . ? C42 C43 1.381(5) . ? C42 H42 0.9500 . ? C43 C44 1.375(5) . ? C43 H43 0.9500 . ? C44 C45 1.375(6) . ? C44 H44 0.9500 . ? C45 C46 1.377(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.381(5) . ? C51 C56 1.392(4) . ? C52 C53 1.387(5) . ? C52 H52 0.9500 . ? C53 C54 1.365(5) . ? C53 H53 0.9500 . ? C54 C55 1.382(5) . ? C54 H54 0.9500 . ? C55 C56 1.384(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N11 N12 1.370(3) . ? N21 N22 1.372(3) . ? N31 N32 1.365(4) . ? B1 F3 1.281(8) 2_666 ? B1 F3 1.281(8) . ? B1 F4 1.283(7) . ? B1 F4 1.283(7) 2_666 ? B1 F2 1.368(5) 2_666 ? B1 F2 1.368(5) . ? B1 F1 1.406(5) 2_666 ? B1 F1 1.406(5) . ? 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 N21 Ag1 N21 180.00(12) . 2_556 ? N21 Ag1 N11 80.63(10) . . ? N21 Ag1 N11 99.37(10) 2_556 . ? N21 Ag1 N11 99.37(10) . 2_556 ? N21 Ag1 N11 80.63(10) 2_556 2_556 ? N11 Ag1 N11 180.0 . 2_556 ? O1 P1 O2 113.63(12) . . ? O1 P1 C41 114.87(14) . . ? O2 P1 C41 100.75(14) . . ? O1 P1 C51 111.79(15) . . ? O2 P1 C51 106.37(13) . . ? C41 P1 C51 108.59(15) . . ? N22 C1 N32 108.6(3) . . ? N22 C1 N12 110.3(2) . . ? N32 C1 N12 109.5(2) . . ? N22 C1 C2 111.5(2) . . ? N32 C1 C2 108.9(2) . . ? N12 C1 C2 108.0(2) . . ? O2 C2 C1 106.4(2) . . ? O2 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O2 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.6 . . ? N12 C11 C12 107.0(3) . . ? N12 C11 H11 126.5 . . ? C12 C11 H11 126.5 . . ? C11 C12 C13 105.3(3) . . ? C11 C12 H12 127.4 . . ? C13 C12 H12 127.4 . . ? N11 C13 C12 112.3(3) . . ? N11 C13 H13 123.8 . . ? C12 C13 H13 123.8 . . ? C22 C21 N22 107.7(3) . . ? C22 C21 H21 126.1 . . ? N22 C21 H21 126.1 . . ? C21 C22 C23 104.9(3) . . ? C21 C22 H22 127.6 . . ? C23 C22 H22 127.6 . . ? N21 C23 C22 112.6(3) . . ? N21 C23 H23 123.7 . . ? C22 C23 H23 123.7 . . ? C32 C31 N32 106.3(3) . . ? C32 C31 H31 126.8 . . ? N32 C31 H31 126.8 . . ? C31 C32 C33 105.8(3) . . ? C31 C32 H32 127.1 . . ? C33 C32 H32 127.1 . . ? N31 C33 C32 112.1(3) . . ? N31 C33 H33 123.9 . . ? C32 C33 H33 123.9 . . ? C42 C41 C46 118.5(3) . . ? C42 C41 P1 122.0(2) . . ? C46 C41 P1 119.3(3) . . ? C41 C42 C43 121.4(3) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C44 C43 C42 119.3(4) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 120.2(4) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.2(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.4(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C52 C51 C56 118.8(3) . . ? C52 C51 P1 118.9(3) . . ? C56 C51 P1 122.3(3) . . ? C51 C52 C53 120.6(4) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 120.1(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.4(4) . . ? C53 C54 H54 119.8 . . ? C55 C54 H54 119.8 . . ? C54 C55 C56 119.7(4) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C55 C56 C51 120.5(3) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C13 N11 N12 103.8(3) . . ? C13 N11 Ag1 129.6(2) . . ? N12 N11 Ag1 118.1(2) . . ? C11 N12 N11 111.5(2) . . ? C11 N12 C1 128.2(2) . . ? N11 N12 C1 119.5(3) . . ? C23 N21 N22 104.5(3) . . ? C23 N21 Ag1 134.4(2) . . ? N22 N21 Ag1 121.0(2) . . ? C21 N22 N21 110.4(3) . . ? C21 N22 C1 130.5(3) . . ? N21 N22 C1 118.7(2) . . ? C33 N31 N32 103.4(3) . . ? C31 N32 N31 112.3(3) . . ? C31 N32 C1 129.2(3) . . ? N31 N32 C1 117.1(3) . . ? C2 O2 P1 117.25(18) . . ? F3 B1 F4 119.6(5) . . ? F3 B1 F2 108.0(5) . . ? F4 B1 F2 107.9(5) . . ? F3 B1 F1 105.8(5) . . ? F4 B1 F1 110.6(4) . . ? F2 B1 F1 103.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 C1 C2 O2 65.7(3) . . . . ? N32 C1 C2 O2 -54.1(3) . . . . ? N12 C1 C2 O2 -173.0(2) . . . . ? N12 C11 C12 C13 2.0(4) . . . . ? C11 C12 C13 N11 -0.8(4) . . . . ? N22 C21 C22 C23 -0.6(4) . . . . ? C21 C22 C23 N21 -0.1(4) . . . . ? N32 C31 C32 C33 1.7(4) . . . . ? C31 C32 C33 N31 -0.4(4) . . . . ? O1 P1 C41 C42 91.9(3) . . . . ? O2 P1 C41 C42 -30.6(3) . . . . ? C51 P1 C41 C42 -142.1(3) . . . . ? O1 P1 C41 C46 -81.8(3) . . . . ? O2 P1 C41 C46 155.7(3) . . . . ? C51 P1 C41 C46 44.2(3) . . . . ? C46 C41 C42 C43 1.5(5) . . . . ? P1 C41 C42 C43 -172.2(3) . . . . ? C41 C42 C43 C44 -0.5(5) . . . . ? C42 C43 C44 C45 -1.6(6) . . . . ? C43 C44 C45 C46 2.7(7) . . . . ? C44 C45 C46 C41 -1.6(6) . . . . ? C42 C41 C46 C45 -0.5(5) . . . . ? P1 C41 C46 C45 173.4(3) . . . . ? O1 P1 C51 C52 12.2(3) . . . . ? O2 P1 C51 C52 136.8(2) . . . . ? C41 P1 C51 C52 -115.6(3) . . . . ? O1 P1 C51 C56 -170.2(2) . . . . ? O2 P1 C51 C56 -45.6(3) . . . . ? C41 P1 C51 C56 62.1(3) . . . . ? C56 C51 C52 C53 -1.0(5) . . . . ? P1 C51 C52 C53 176.8(3) . . . . ? C51 C52 C53 C54 0.8(5) . . . . ? C52 C53 C54 C55 -0.1(6) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? C54 C55 C56 C51 0.3(5) . . . . ? C52 C51 C56 C55 0.4(5) . . . . ? P1 C51 C56 C55 -177.2(2) . . . . ? C12 C13 N11 N12 -0.8(4) . . . . ? C12 C13 N11 Ag1 145.6(3) . . . . ? N21 Ag1 N11 C13 -117.5(3) . . . . ? N21 Ag1 N11 C13 62.5(3) 2_556 . . . ? N21 Ag1 N11 N12 24.8(2) . . . . ? N21 Ag1 N11 N12 -155.2(2) 2_556 . . . ? C12 C11 N12 N11 -2.7(4) . . . . ? C12 C11 N12 C1 -172.3(3) . . . . ? C13 N11 N12 C11 2.1(4) . . . . ? Ag1 N11 N12 C11 -148.9(2) . . . . ? C13 N11 N12 C1 172.8(3) . . . . ? Ag1 N11 N12 C1 21.8(4) . . . . ? N22 C1 N12 C11 89.8(4) . . . . ? N32 C1 N12 C11 -150.7(3) . . . . ? C2 C1 N12 C11 -32.3(4) . . . . ? N22 C1 N12 N11 -79.1(3) . . . . ? N32 C1 N12 N11 40.3(4) . . . . ? C2 C1 N12 N11 158.8(3) . . . . ? C22 C23 N21 N22 0.7(4) . . . . ? C22 C23 N21 Ag1 -174.5(2) . . . . ? N11 Ag1 N21 C23 137.2(3) . . . . ? N11 Ag1 N21 C23 -42.8(3) 2_556 . . . ? N11 Ag1 N21 N22 -37.3(2) . . . . ? N11 Ag1 N21 N22 142.7(2) 2_556 . . . ? C22 C21 N22 N21 1.1(4) . . . . ? C22 C21 N22 C1 172.9(3) . . . . ? C23 N21 N22 C21 -1.1(4) . . . . ? Ag1 N21 N22 C21 174.88(19) . . . . ? C23 N21 N22 C1 -174.0(3) . . . . ? Ag1 N21 N22 C1 1.9(4) . . . . ? N32 C1 N22 C21 131.7(3) . . . . ? N12 C1 N22 C21 -108.2(3) . . . . ? C2 C1 N22 C21 11.7(4) . . . . ? N32 C1 N22 N21 -57.0(3) . . . . ? N12 C1 N22 N21 63.0(3) . . . . ? C2 C1 N22 N21 -177.0(3) . . . . ? C32 C33 N31 N32 -1.0(4) . . . . ? C32 C31 N32 N31 -2.4(4) . . . . ? C32 C31 N32 C1 -168.3(3) . . . . ? C33 N31 N32 C31 2.1(4) . . . . ? C33 N31 N32 C1 169.8(3) . . . . ? N22 C1 N32 C31 -21.2(4) . . . . ? N12 C1 N32 C31 -141.7(3) . . . . ? C2 C1 N32 C31 100.4(4) . . . . ? N22 C1 N32 N31 173.6(2) . . . . ? N12 C1 N32 N31 53.0(3) . . . . ? C2 C1 N32 N31 -64.8(3) . . . . ? C1 C2 O2 P1 178.3(2) . . . . ? O1 P1 O2 C2 52.7(2) . . . . ? C41 P1 O2 C2 176.1(2) . . . . ? C51 P1 O2 C2 -70.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.550 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.063 # Attachment 'rspofcm.cif' data_rspofcm _database_code_depnum_ccdc_archive 'CCDC 670350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C46 H42 Fe N12 O4 P2, 2(C3 H6 O), 2(B F4) ; _chemical_formula_sum 'C52 H54 B2 F8 Fe N12 O6 P2' _chemical_formula_weight 1234.48 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3175(7) _cell_length_b 18.4056(10) _cell_length_c 12.3750(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.8390(10) _cell_angle_gamma 90.00 _cell_volume 2785.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6633 _cell_measurement_theta_min 2.205 _cell_measurement_theta_max 26.389 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23898 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5718 _reflns_number_gt 4897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0617P)^2^+0.3691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5718 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.5000 0.01585(11) Uani 1 2 d S . . P1 P 0.18984(4) 0.26645(3) 0.65644(4) 0.02146(13) Uani 1 1 d . . . C1 C 0.37732(14) 0.14209(9) 0.51129(15) 0.0180(4) Uani 1 1 d . . . C2 C 0.31708(15) 0.21461(10) 0.51537(16) 0.0202(4) Uani 1 1 d . . . H2A H 0.3619 0.2545 0.4903 0.024 Uiso 1 1 calc R . . H2B H 0.2468 0.2129 0.4675 0.024 Uiso 1 1 calc R . . C11 C 0.20077(15) 0.07873(10) 0.55152(16) 0.0212(4) Uani 1 1 d . . . H11 H 0.1533 0.1191 0.5551 0.025 Uiso 1 1 calc R . . C12 C 0.17469(16) 0.00728(10) 0.56249(17) 0.0252(4) Uani 1 1 d . . . H12 H 0.1061 -0.0120 0.5762 0.030 Uiso 1 1 calc R . . C13 C 0.26933(15) -0.03146(10) 0.54953(16) 0.0225(4) Uani 1 1 d . . . H13 H 0.2752 -0.0829 0.5528 0.027 Uiso 1 1 calc R . . C21 C 0.38898(15) 0.17222(10) 0.31055(16) 0.0213(4) Uani 1 1 d . . . H21 H 0.3482 0.2161 0.3025 0.026 Uiso 1 1 calc R . . C22 C 0.43819(16) 0.13739(10) 0.23149(16) 0.0228(4) Uani 1 1 d . . . H22 H 0.4392 0.1524 0.1582 0.027 Uiso 1 1 calc R . . C23 C 0.48651(15) 0.07541(10) 0.28083(16) 0.0212(4) Uani 1 1 d . . . H23 H 0.5267 0.0407 0.2451 0.025 Uiso 1 1 calc R . . C31 C 0.51987(15) 0.19287(10) 0.66172(16) 0.0225(4) Uani 1 1 d . . . H31 H 0.4919 0.2402 0.6713 0.027 Uiso 1 1 calc R . . C32 C 0.61185(15) 0.16332(10) 0.71720(17) 0.0255(4) Uani 1 1 d . . . H32 H 0.6603 0.1858 0.7728 0.031 Uiso 1 1 calc R . . C33 C 0.62018(15) 0.09325(10) 0.67539(16) 0.0228(4) Uani 1 1 d . . . H33 H 0.6767 0.0597 0.6991 0.027 Uiso 1 1 calc R . . C41 C 0.19471(16) 0.35921(11) 0.61112(17) 0.0266(4) Uani 1 1 d . . . C42 C 0.25898(19) 0.41185(12) 0.6682(2) 0.0366(5) Uani 1 1 d . . . H42 H 0.3060 0.3989 0.7318 0.044 Uiso 1 1 calc R . . C43 C 0.2544(2) 0.48357(13) 0.6321(3) 0.0515(7) Uani 1 1 d . . . H43 H 0.2967 0.5199 0.6722 0.062 Uiso 1 1 calc R . . C44 C 0.1887(3) 0.50169(14) 0.5386(3) 0.0590(8) Uani 1 1 d . . . H44 H 0.1863 0.5505 0.5137 0.071 Uiso 1 1 calc R . . C45 C 0.1258(3) 0.44930(15) 0.4802(2) 0.0576(8) Uani 1 1 d . . . H45 H 0.0816 0.4621 0.4148 0.069 Uiso 1 1 calc R . . C46 C 0.1274(2) 0.37811(13) 0.5173(2) 0.0405(6) Uani 1 1 d . . . H46 H 0.0825 0.3424 0.4786 0.049 Uiso 1 1 calc R . . C51 C 0.21838(16) 0.25961(10) 0.80085(17) 0.0240(4) Uani 1 1 d . . . C52 C 0.13471(17) 0.23394(11) 0.85744(18) 0.0310(5) Uani 1 1 d . . . H52 H 0.0648 0.2238 0.8193 0.037 Uiso 1 1 calc R . . C53 C 0.1530(2) 0.22327(14) 0.9682(2) 0.0445(6) Uani 1 1 d . . . H53 H 0.0962 0.2051 1.0063 0.053 Uiso 1 1 calc R . . C54 C 0.2543(2) 0.23902(16) 1.0240(2) 0.0521(7) Uani 1 1 d . . . H54 H 0.2662 0.2326 1.1007 0.062 Uiso 1 1 calc R . . C55 C 0.3383(2) 0.26393(14) 0.9695(2) 0.0439(6) Uani 1 1 d . . . H55 H 0.4077 0.2745 1.0085 0.053 Uiso 1 1 calc R . . C56 C 0.32137(17) 0.27356(12) 0.85721(18) 0.0315(5) Uani 1 1 d . . . H56 H 0.3795 0.2895 0.8191 0.038 Uiso 1 1 calc R . . N11 N 0.35012(12) 0.01288(8) 0.53196(13) 0.0184(3) Uani 1 1 d . . . N12 N 0.30752(12) 0.08117(8) 0.53445(13) 0.0175(3) Uani 1 1 d . . . N21 N 0.46894(12) 0.07137(8) 0.38439(13) 0.0184(3) Uani 1 1 d . . . N22 N 0.40973(12) 0.13203(8) 0.40258(12) 0.0175(3) Uani 1 1 d . . . N31 N 0.53859(12) 0.07993(8) 0.59822(13) 0.0185(3) Uani 1 1 d . . . N32 N 0.47576(12) 0.14150(8) 0.59002(12) 0.0179(3) Uani 1 1 d . . . O1 O 0.29810(10) 0.22658(7) 0.62535(11) 0.0224(3) Uani 1 1 d . . . O2 O 0.08807(11) 0.23067(7) 0.61004(12) 0.0286(3) Uani 1 1 d . . . B1 B 0.0893(2) 0.11874(13) 0.2761(2) 0.0328(6) Uani 1 1 d . . . F1 F 0.04591(15) 0.13400(8) 0.17042(12) 0.0638(5) Uani 1 1 d . . . F2 F 0.17775(11) 0.07199(8) 0.27937(14) 0.0548(4) Uani 1 1 d . . . F3 F 0.00977(11) 0.08741(8) 0.32985(14) 0.0524(4) Uani 1 1 d . . . F4 F 0.12331(12) 0.18371(7) 0.32695(12) 0.0493(4) Uani 1 1 d . . . C61 C 0.4308(2) 0.40583(13) 0.2034(2) 0.0467(6) Uani 1 1 d . . . H61A H 0.5087 0.3973 0.1989 0.070 Uiso 1 1 calc R . . H61B H 0.4128 0.4564 0.1842 0.070 Uiso 1 1 calc R . . H61C H 0.3871 0.3733 0.1527 0.070 Uiso 1 1 calc R . . C62 C 0.40639(16) 0.39120(10) 0.31644(19) 0.0291(5) Uani 1 1 d . . . C63 C 0.4464(3) 0.44428(15) 0.4025(2) 0.0614(8) Uani 1 1 d . . . H63A H 0.4103 0.4912 0.3868 0.092 Uiso 1 1 calc R . . H63B H 0.5257 0.4502 0.4042 0.092 Uiso 1 1 calc R . . H63C H 0.4296 0.4265 0.4733 0.092 Uiso 1 1 calc R . . O3 O 0.35583(13) 0.33802(8) 0.33844(15) 0.0411(4) 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 Fe1 0.01661(19) 0.01524(18) 0.0161(2) 0.00016(14) 0.00368(15) 0.00034(13) P1 0.0191(2) 0.0257(3) 0.0198(3) -0.0026(2) 0.0031(2) 0.00379(19) C1 0.0192(9) 0.0199(9) 0.0154(10) 0.0001(7) 0.0037(7) -0.0005(7) C2 0.0224(9) 0.0201(9) 0.0186(10) -0.0001(7) 0.0040(8) 0.0036(7) C11 0.0183(9) 0.0256(9) 0.0207(11) -0.0008(8) 0.0061(8) 0.0007(7) C12 0.0206(9) 0.0291(10) 0.0269(12) 0.0006(8) 0.0069(8) -0.0035(8) C13 0.0244(10) 0.0210(9) 0.0225(11) 0.0006(8) 0.0043(8) -0.0038(7) C21 0.0218(9) 0.0214(9) 0.0205(11) 0.0043(8) 0.0016(8) -0.0003(7) C22 0.0270(10) 0.0263(9) 0.0157(10) 0.0020(8) 0.0048(8) -0.0016(8) C23 0.0219(9) 0.0244(9) 0.0183(10) -0.0022(8) 0.0067(8) -0.0016(7) C31 0.0232(9) 0.0208(9) 0.0239(11) -0.0044(8) 0.0042(8) -0.0020(7) C32 0.0238(10) 0.0282(10) 0.0237(11) -0.0066(8) 0.0002(8) -0.0025(8) C33 0.0205(9) 0.0257(9) 0.0219(11) 0.0002(8) 0.0008(8) 0.0001(7) C41 0.0259(10) 0.0283(10) 0.0272(12) 0.0021(8) 0.0106(9) 0.0077(8) C42 0.0360(12) 0.0337(11) 0.0402(14) 0.0029(10) 0.0051(10) 0.0001(9) C43 0.0570(17) 0.0335(13) 0.064(2) 0.0039(12) 0.0094(15) -0.0038(11) C44 0.069(2) 0.0362(14) 0.073(2) 0.0188(14) 0.0133(17) 0.0086(13) C45 0.0695(19) 0.0550(17) 0.0476(18) 0.0208(14) 0.0032(15) 0.0190(15) C46 0.0443(14) 0.0431(13) 0.0334(14) 0.0057(10) 0.0024(11) 0.0105(11) C51 0.0243(10) 0.0271(10) 0.0204(11) -0.0019(8) 0.0020(8) 0.0073(8) C52 0.0279(11) 0.0371(11) 0.0291(13) 0.0023(9) 0.0077(9) 0.0085(9) C53 0.0447(14) 0.0576(15) 0.0339(15) 0.0115(12) 0.0161(12) 0.0192(12) C54 0.0596(17) 0.0759(19) 0.0207(13) 0.0039(12) 0.0046(12) 0.0340(15) C55 0.0380(13) 0.0617(16) 0.0290(14) -0.0109(11) -0.0080(11) 0.0211(12) C56 0.0266(11) 0.0387(12) 0.0288(13) -0.0056(9) 0.0018(9) 0.0084(9) N11 0.0204(8) 0.0170(7) 0.0184(9) 0.0007(6) 0.0040(6) 0.0001(6) N12 0.0178(7) 0.0170(7) 0.0181(9) 0.0002(6) 0.0036(6) 0.0007(6) N21 0.0195(8) 0.0175(7) 0.0187(9) -0.0004(6) 0.0051(6) 0.0011(6) N22 0.0183(7) 0.0183(7) 0.0164(9) 0.0013(6) 0.0041(6) 0.0011(6) N31 0.0184(7) 0.0180(7) 0.0195(9) 0.0005(6) 0.0033(6) 0.0018(6) N32 0.0173(7) 0.0177(7) 0.0188(9) -0.0008(6) 0.0021(6) 0.0004(6) O1 0.0228(7) 0.0264(7) 0.0183(7) -0.0026(5) 0.0034(6) 0.0060(5) O2 0.0229(7) 0.0347(8) 0.0280(9) -0.0058(6) 0.0018(6) 0.0021(6) B1 0.0354(13) 0.0269(12) 0.0352(15) 0.0056(10) 0.0002(11) -0.0076(10) F1 0.1102(14) 0.0417(8) 0.0347(9) 0.0064(7) -0.0121(9) -0.0158(8) F2 0.0391(8) 0.0472(8) 0.0806(12) 0.0003(8) 0.0173(8) -0.0028(6) F3 0.0369(8) 0.0472(8) 0.0749(12) 0.0208(7) 0.0137(7) -0.0041(6) F4 0.0606(9) 0.0351(7) 0.0472(9) 0.0002(6) -0.0135(7) -0.0118(6) C61 0.0641(17) 0.0362(12) 0.0423(16) 0.0012(11) 0.0157(13) 0.0104(12) C62 0.0269(10) 0.0236(10) 0.0367(13) 0.0015(9) 0.0036(9) 0.0014(8) C63 0.092(2) 0.0467(15) 0.0441(18) -0.0083(13) 0.0016(16) -0.0210(15) O3 0.0376(9) 0.0281(8) 0.0571(12) 0.0072(7) 0.0033(8) -0.0037(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 Fe1 N31 1.9313(15) . ? Fe1 N31 1.9313(15) 3_656 ? Fe1 N21 1.9464(15) . ? Fe1 N21 1.9464(15) 3_656 ? Fe1 N11 1.9480(15) 3_656 ? Fe1 N11 1.9480(15) . ? P1 O2 1.4708(14) . ? P1 O1 1.6084(13) . ? P1 C51 1.784(2) . ? P1 C41 1.800(2) . ? C1 N22 1.460(2) . ? C1 N12 1.462(2) . ? C1 N32 1.462(2) . ? C1 C2 1.531(2) . ? C2 O1 1.425(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 N12 1.357(2) . ? C11 C12 1.364(3) . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C13 N11 1.325(2) . ? C13 H13 0.9500 . ? C21 N22 1.357(2) . ? C21 C22 1.370(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 H22 0.9500 . ? C23 N21 1.327(2) . ? C23 H23 0.9500 . ? C31 N32 1.364(2) . ? C31 C32 1.366(3) . ? C31 H31 0.9500 . ? C32 C33 1.398(3) . ? C32 H32 0.9500 . ? C33 N31 1.324(2) . ? C33 H33 0.9500 . ? C41 C46 1.388(3) . ? C41 C42 1.390(3) . ? C42 C43 1.392(3) . ? C42 H42 0.9500 . ? C43 C44 1.372(4) . ? C43 H43 0.9500 . ? C44 C45 1.385(4) . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.396(3) . ? C51 C56 1.397(3) . ? C52 C53 1.376(3) . ? C52 H52 0.9500 . ? C53 C54 1.383(4) . ? C53 H53 0.9500 . ? C54 C55 1.380(4) . ? C54 H54 0.9500 . ? C55 C56 1.391(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? N11 N12 1.364(2) . ? N21 N22 1.367(2) . ? N31 N32 1.369(2) . ? B1 F3 1.375(3) . ? B1 F1 1.381(3) . ? B1 F2 1.385(3) . ? B1 F4 1.392(3) . ? C61 C62 1.490(3) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 O3 1.209(2) . ? C62 C63 1.485(3) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Fe1 N31 180.00(5) . 3_656 ? N31 Fe1 N21 87.74(6) . . ? N31 Fe1 N21 92.26(6) 3_656 . ? N31 Fe1 N21 92.26(6) . 3_656 ? N31 Fe1 N21 87.74(6) 3_656 3_656 ? N21 Fe1 N21 180.00(6) . 3_656 ? N31 Fe1 N11 93.00(6) . 3_656 ? N31 Fe1 N11 87.00(6) 3_656 3_656 ? N21 Fe1 N11 92.35(6) . 3_656 ? N21 Fe1 N11 87.65(6) 3_656 3_656 ? N31 Fe1 N11 87.00(6) . . ? N31 Fe1 N11 93.00(6) 3_656 . ? N21 Fe1 N11 87.65(6) . . ? N21 Fe1 N11 92.35(6) 3_656 . ? N11 Fe1 N11 180.0 3_656 . ? O2 P1 O1 113.25(8) . . ? O2 P1 C51 114.61(9) . . ? O1 P1 C51 97.89(8) . . ? O2 P1 C41 111.19(9) . . ? O1 P1 C41 107.39(8) . . ? C51 P1 C41 111.65(10) . . ? N22 C1 N12 108.37(14) . . ? N22 C1 N32 108.47(14) . . ? N12 C1 N32 108.91(14) . . ? N22 C1 C2 109.13(14) . . ? N12 C1 C2 111.32(14) . . ? N32 C1 C2 110.56(15) . . ? O1 C2 C1 107.55(14) . . ? O1 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? O1 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? N12 C11 C12 106.94(16) . . ? N12 C11 H11 126.5 . . ? C12 C11 H11 126.5 . . ? C11 C12 C13 105.78(17) . . ? C11 C12 H12 127.1 . . ? C13 C12 H12 127.1 . . ? N11 C13 C12 111.05(16) . . ? N11 C13 H13 124.5 . . ? C12 C13 H13 124.5 . . ? N22 C21 C22 106.81(16) . . ? N22 C21 H21 126.6 . . ? C22 C21 H21 126.6 . . ? C21 C22 C23 105.80(17) . . ? C21 C22 H22 127.1 . . ? C23 C22 H22 127.1 . . ? N21 C23 C22 111.03(16) . . ? N21 C23 H23 124.5 . . ? C22 C23 H23 124.5 . . ? N32 C31 C32 107.05(16) . . ? N32 C31 H31 126.5 . . ? C32 C31 H31 126.5 . . ? C31 C32 C33 105.92(17) . . ? C31 C32 H32 127.0 . . ? C33 C32 H32 127.0 . . ? N31 C33 C32 110.78(17) . . ? N31 C33 H33 124.6 . . ? C32 C33 H33 124.6 . . ? C46 C41 C42 119.9(2) . . ? C46 C41 P1 117.34(17) . . ? C42 C41 P1 122.75(17) . . ? C41 C42 C43 120.0(2) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.5(2) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 120.0(3) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 119.8(2) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? C52 C51 C56 119.5(2) . . ? C52 C51 P1 117.22(16) . . ? C56 C51 P1 123.10(16) . . ? C53 C52 C51 120.3(2) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C52 C53 C54 119.9(2) . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.7(2) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C54 C55 C56 119.9(2) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 119.7(2) . . ? C55 C56 H56 120.2 . . ? C51 C56 H56 120.2 . . ? C13 N11 N12 105.39(14) . . ? C13 N11 Fe1 134.98(13) . . ? N12 N11 Fe1 119.56(11) . . ? C11 N12 N11 110.83(14) . . ? C11 N12 C1 131.24(15) . . ? N11 N12 C1 117.75(14) . . ? C23 N21 N22 105.36(14) . . ? C23 N21 Fe1 135.02(13) . . ? N22 N21 Fe1 119.49(11) . . ? C21 N22 N21 110.98(14) . . ? C21 N22 C1 131.26(15) . . ? N21 N22 C1 117.72(14) . . ? C33 N31 N32 105.90(14) . . ? C33 N31 Fe1 134.72(12) . . ? N32 N31 Fe1 119.29(11) . . ? C31 N32 N31 110.33(15) . . ? C31 N32 C1 131.50(15) . . ? N31 N32 C1 118.17(14) . . ? C2 O1 P1 122.26(11) . . ? F3 B1 F1 109.0(2) . . ? F3 B1 F2 109.19(18) . . ? F1 B1 F2 111.6(2) . . ? F3 B1 F4 109.6(2) . . ? F1 B1 F4 108.35(18) . . ? F2 B1 F4 109.09(19) . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O3 C62 C63 120.5(2) . . ? O3 C62 C61 121.7(2) . . ? C63 C62 C61 117.9(2) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22 C1 C2 O1 -173.32(14) . . . . ? N12 C1 C2 O1 67.11(19) . . . . ? N32 C1 C2 O1 -54.09(18) . . . . ? N12 C11 C12 C13 -0.9(2) . . . . ? C11 C12 C13 N11 0.3(2) . . . . ? N22 C21 C22 C23 0.8(2) . . . . ? C21 C22 C23 N21 0.0(2) . . . . ? N32 C31 C32 C33 0.2(2) . . . . ? C31 C32 C33 N31 0.2(2) . . . . ? O2 P1 C41 C46 -20.29(19) . . . . ? O1 P1 C41 C46 104.12(17) . . . . ? C51 P1 C41 C46 -149.68(17) . . . . ? O2 P1 C41 C42 157.13(17) . . . . ? O1 P1 C41 C42 -78.47(19) . . . . ? C51 P1 C41 C42 27.7(2) . . . . ? C46 C41 C42 C43 1.0(3) . . . . ? P1 C41 C42 C43 -176.35(19) . . . . ? C41 C42 C43 C44 -1.8(4) . . . . ? C42 C43 C44 C45 0.7(5) . . . . ? C43 C44 C45 C46 1.2(5) . . . . ? C44 C45 C46 C41 -2.0(4) . . . . ? C42 C41 C46 C45 0.9(3) . . . . ? P1 C41 C46 C45 178.4(2) . . . . ? O2 P1 C51 C52 -11.55(18) . . . . ? O1 P1 C51 C52 -131.67(16) . . . . ? C41 P1 C51 C52 116.02(16) . . . . ? O2 P1 C51 C56 163.68(16) . . . . ? O1 P1 C51 C56 43.56(18) . . . . ? C41 P1 C51 C56 -68.75(18) . . . . ? C56 C51 C52 C53 0.8(3) . . . . ? P1 C51 C52 C53 176.21(17) . . . . ? C51 C52 C53 C54 0.9(3) . . . . ? C52 C53 C54 C55 -1.4(4) . . . . ? C53 C54 C55 C56 0.1(4) . . . . ? C54 C55 C56 C51 1.6(3) . . . . ? C52 C51 C56 C55 -2.0(3) . . . . ? P1 C51 C56 C55 -177.17(17) . . . . ? C12 C13 N11 N12 0.5(2) . . . . ? C12 C13 N11 Fe1 -176.37(15) . . . . ? N31 Fe1 N11 C13 -139.40(19) . . . . ? N31 Fe1 N11 C13 40.60(19) 3_656 . . . ? N21 Fe1 N11 C13 132.74(19) . . . . ? N21 Fe1 N11 C13 -47.26(19) 3_656 . . . ? N31 Fe1 N11 N12 44.09(13) . . . . ? N31 Fe1 N11 N12 -135.91(13) 3_656 . . . ? N21 Fe1 N11 N12 -43.77(13) . . . . ? N21 Fe1 N11 N12 136.23(13) 3_656 . . . ? C12 C11 N12 N11 1.3(2) . . . . ? C12 C11 N12 C1 176.09(18) . . . . ? C13 N11 N12 C11 -1.1(2) . . . . ? Fe1 N11 N12 C11 176.36(12) . . . . y C13 N11 N12 C1 -176.69(15) . . . . ? Fe1 N11 N12 C1 0.8(2) . . . . ? N22 C1 N12 C11 -115.5(2) . . . . ? N32 C1 N12 C11 126.6(2) . . . . ? C2 C1 N12 C11 4.5(3) . . . . ? N22 C1 N12 N11 59.00(19) . . . . ? N32 C1 N12 N11 -58.83(19) . . . . ? C2 C1 N12 N11 179.02(15) . . . . ? C22 C23 N21 N22 -0.8(2) . . . . ? C22 C23 N21 Fe1 174.79(13) . . . . ? N31 Fe1 N21 C23 139.46(18) . . . . ? N31 Fe1 N21 C23 -40.54(18) 3_656 . . . ? N11 Fe1 N21 C23 46.55(18) 3_656 . . . ? N11 Fe1 N21 C23 -133.45(18) . . . . ? N31 Fe1 N21 N22 -45.44(12) . . . . ? N31 Fe1 N21 N22 134.56(12) 3_656 . . . ? N11 Fe1 N21 N22 -138.35(13) 3_656 . . . ? N11 Fe1 N21 N22 41.65(13) . . . . ? C22 C21 N22 N21 -1.3(2) . . . . ? C22 C21 N22 C1 -179.31(17) . . . . ? C23 N21 N22 C21 1.33(19) . . . . ? Fe1 N21 N22 C21 -175.09(12) . . . . y C23 N21 N22 C1 179.60(15) . . . . ? Fe1 N21 N22 C1 3.19(19) . . . . ? N12 C1 N22 C21 116.52(19) . . . . ? N32 C1 N22 C21 -125.38(19) . . . . ? C2 C1 N22 C21 -4.9(3) . . . . ? N12 C1 N22 N21 -61.33(19) . . . . ? N32 C1 N22 N21 56.77(19) . . . . ? C2 C1 N22 N21 177.28(14) . . . . ? C32 C33 N31 N32 -0.5(2) . . . . ? C32 C33 N31 Fe1 175.88(14) . . . . ? N21 Fe1 N31 C33 -134.63(19) . . . . ? N21 Fe1 N31 C33 45.37(19) 3_656 . . . ? N11 Fe1 N31 C33 -42.39(19) 3_656 . . . ? N11 Fe1 N31 C33 137.61(19) . . . . ? N21 Fe1 N31 N32 41.40(13) . . . . ? N21 Fe1 N31 N32 -138.60(13) 3_656 . . . ? N11 Fe1 N31 N32 133.63(13) 3_656 . . . ? N11 Fe1 N31 N32 -46.37(13) . . . . ? C32 C31 N32 N31 -0.5(2) . . . . ? C32 C31 N32 C1 179.00(18) . . . . ? C33 N31 N32 C31 0.6(2) . . . . ? Fe1 N31 N32 C31 -176.43(12) . . . . y C33 N31 N32 C1 -178.95(15) . . . . ? Fe1 N31 N32 C1 4.0(2) . . . . ? N22 C1 N32 C31 119.1(2) . . . . ? N12 C1 N32 C31 -123.12(19) . . . . ? C2 C1 N32 C31 -0.5(3) . . . . ? N22 C1 N32 N31 -61.39(19) . . . . ? N12 C1 N32 N31 56.37(19) . . . . ? C2 C1 N32 N31 178.98(14) . . . . ? C1 C2 O1 P1 -145.40(12) . . . . ? O2 P1 O1 C2 56.96(15) . . . . ? C51 P1 O1 C2 178.10(14) . . . . ? C41 P1 O1 C2 -66.19(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.444 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.064