# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Burrows, Andrew' _publ_contact_author_name 'Burrows, Andrew' _publ_contact_author_email a.d.burrows@bath.ac.uk _publ_section_title ; Dipyridyl b-diketonate complexes and their use as metalloligands in the formation of mixed-metal coordination networks ; # Attachment '- dppd-strucs.cif' data_compound1_h06adb4 _database_code_depnum_ccdc_archive 'CCDC 853056' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.50 H39 Fe N6 O6' _chemical_formula_weight 869.72 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' Fe Fe 0.3463 0.8444 '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 12.0670(2) _cell_length_b 12.6310(2) _cell_length_c 14.3780(3) _cell_angle_alpha 87.509(1) _cell_angle_beta 82.407(1) _cell_angle_gamma 79.667(1) _cell_volume 2136.59(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23048 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.412 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.858 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36317 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 30.05 _reflns_number_total 12398 _reflns_number_gt 8763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Asymmetric unit consists of one molecule of the iron complex, one full molecule of toluene, and a toluene fragment (1/2 molecule) disordered over 2 sites, and proximate to an inversion centre. The disorder and symmetry associated with this latter fragment precluded location of the hydrogen atoms therein. Hence, these hydrogens were omitted from the final least squares. ; _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^)+(0.0607P)^2^+0.2897P] 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 SHELXL _refine_ls_extinction_coef 0.0075(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12398 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.378256(18) 0.328714(17) 0.754160(15) 0.02143(8) Uani 1 1 d . . . O1 O 0.39334(10) 0.46761(8) 0.68924(8) 0.0258(2) Uani 1 1 d . . . O2 O 0.39349(9) 0.26645(8) 0.62609(7) 0.0239(2) Uani 1 1 d . . . O3 O 0.21032(9) 0.36469(8) 0.75107(8) 0.0249(2) Uani 1 1 d . . . O4 O 0.34836(9) 0.18742(8) 0.80899(8) 0.0240(2) Uani 1 1 d . . . O5 O 0.36702(9) 0.39334(8) 0.87896(7) 0.0235(2) Uani 1 1 d . . . O6 O 0.54195(9) 0.27513(9) 0.76283(7) 0.0235(2) Uani 1 1 d . . . N1 N 0.35632(13) 0.83449(11) 0.54439(11) 0.0347(3) Uani 1 1 d . . . N2 N 0.34075(15) 0.11432(13) 0.32477(11) 0.0419(4) Uani 1 1 d . . . N3 N -0.13807(13) 0.43990(13) 0.59250(11) 0.0383(4) Uani 1 1 d . . . N4 N 0.32432(13) -0.19352(11) 0.88226(11) 0.0329(3) Uani 1 1 d . . . N5 N 0.30521(14) 0.49700(13) 1.21416(11) 0.0369(4) Uani 1 1 d . . . N6 N 0.92154(13) 0.06423(13) 0.80919(12) 0.0386(4) Uani 1 1 d . . . C1 C 0.36189(13) 0.49756(12) 0.60870(11) 0.0238(3) Uani 1 1 d . . . C2 C 0.35732(13) 0.61501(12) 0.58534(11) 0.0239(3) Uani 1 1 d . . . C3 C 0.35103(16) 0.68754(13) 0.65659(12) 0.0309(4) Uani 1 1 d . . . H3 H 0.3467 0.6640 0.7204 0.037 Uiso 1 1 calc R . . C4 C 0.35120(17) 0.79507(14) 0.63255(13) 0.0366(4) Uani 1 1 d . . . H4 H 0.3475 0.8439 0.6818 0.044 Uiso 1 1 calc R . . C5 C 0.36180(15) 0.76372(13) 0.47704(12) 0.0302(4) Uani 1 1 d . . . H5 H 0.3654 0.7897 0.4139 0.036 Uiso 1 1 calc R . . C6 C 0.36261(14) 0.65487(13) 0.49335(12) 0.0270(3) Uani 1 1 d . . . H6 H 0.3667 0.6080 0.4426 0.032 Uiso 1 1 calc R . . C7 C 0.33669(14) 0.42977(12) 0.54387(11) 0.0263(3) Uani 1 1 d . . . H7 H 0.3027 0.4610 0.4909 0.032 Uiso 1 1 calc R . . C8 C 0.35938(13) 0.31684(12) 0.55342(11) 0.0230(3) Uani 1 1 d . . . C9 C 0.34911(14) 0.24861(13) 0.47349(11) 0.0245(3) Uani 1 1 d . . . C10 C 0.36863(16) 0.13748(14) 0.48485(13) 0.0339(4) Uani 1 1 d . . . H10 H 0.3849 0.1049 0.5435 0.041 Uiso 1 1 calc R . . C11 C 0.36395(19) 0.07468(15) 0.40917(14) 0.0425(5) Uani 1 1 d . . . H11 H 0.3781 -0.0013 0.4178 0.051 Uiso 1 1 calc R . . C12 C 0.32125(17) 0.22131(15) 0.31536(13) 0.0363(4) Uani 1 1 d . . . H12 H 0.3043 0.2517 0.2562 0.044 Uiso 1 1 calc R . . C13 C 0.32416(15) 0.29111(14) 0.38656(12) 0.0306(4) Uani 1 1 d . . . H13 H 0.3093 0.3668 0.3759 0.037 Uiso 1 1 calc R . . C14 C 0.14953(13) 0.29782(13) 0.73133(11) 0.0232(3) Uani 1 1 d . . . C15 C 0.04701(13) 0.34512(13) 0.68528(11) 0.0247(3) Uani 1 1 d . . . C16 C 0.03178(17) 0.45216(15) 0.65766(16) 0.0429(5) Uani 1 1 d . . . H16 H 0.0842 0.4961 0.6699 0.051 Uiso 1 1 calc R . . C17 C -0.06111(18) 0.49495(16) 0.61178(16) 0.0466(5) Uani 1 1 d . . . H17 H -0.0698 0.5687 0.5931 0.056 Uiso 1 1 calc R . . C18 C -0.1224(2) 0.33854(19) 0.61991(19) 0.0640(8) Uani 1 1 d . . . H18 H -0.1766 0.2967 0.6073 0.077 Uiso 1 1 calc R . . C19 C -0.03263(18) 0.28782(17) 0.66597(18) 0.0545(6) Uani 1 1 d . . . H19 H -0.0267 0.2139 0.6839 0.065 Uiso 1 1 calc R . . C20 C 0.17432(13) 0.18654(12) 0.74984(11) 0.0256(3) Uani 1 1 d . . . H20 H 0.1244 0.1423 0.7333 0.031 Uiso 1 1 calc R . . C21 C 0.26967(13) 0.13850(12) 0.79168(10) 0.0224(3) Uani 1 1 d . . . C22 C 0.28605(13) 0.02205(12) 0.82062(11) 0.0230(3) Uani 1 1 d . . . C23 C 0.39450(14) -0.03067(13) 0.83450(12) 0.0286(4) Uani 1 1 d . . . H23 H 0.4574 0.0060 0.8240 0.034 Uiso 1 1 calc R . . C24 C 0.40882(15) -0.13768(14) 0.86403(13) 0.0324(4) Uani 1 1 d . . . H24 H 0.4834 -0.1734 0.8717 0.039 Uiso 1 1 calc R . . C25 C 0.22042(15) -0.14154(14) 0.86852(13) 0.0318(4) Uani 1 1 d . . . H25 H 0.1590 -0.1800 0.8806 0.038 Uiso 1 1 calc R . . C26 C 0.19713(14) -0.03538(13) 0.83782(12) 0.0281(4) Uani 1 1 d . . . H26 H 0.1220 -0.0025 0.8287 0.034 Uiso 1 1 calc R . . C27 C 0.43380(13) 0.36721(11) 0.94149(11) 0.0210(3) Uani 1 1 d . . . C28 C 0.39126(13) 0.41174(11) 1.03687(11) 0.0212(3) Uani 1 1 d . . . C29 C 0.27696(14) 0.45458(14) 1.05897(12) 0.0313(4) Uani 1 1 d . . . H29 H 0.2258 0.4562 1.0138 0.038 Uiso 1 1 calc R . . C30 C 0.23866(16) 0.49470(16) 1.14716(13) 0.0397(4) Uani 1 1 d . . . H30 H 0.1600 0.5225 1.1613 0.048 Uiso 1 1 calc R . . C31 C 0.41516(15) 0.45616(13) 1.19187(12) 0.0293(4) Uani 1 1 d . . . H31 H 0.4645 0.4572 1.2380 0.035 Uiso 1 1 calc R . . C32 C 0.46162(14) 0.41267(12) 1.10622(11) 0.0240(3) Uani 1 1 d . . . H32 H 0.5403 0.3838 1.0946 0.029 Uiso 1 1 calc R . . C33 C 0.54051(13) 0.30180(12) 0.92553(11) 0.0235(3) Uani 1 1 d . . . H33 H 0.5823 0.2839 0.9773 0.028 Uiso 1 1 calc R . . C34 C 0.58913(13) 0.26138(12) 0.83844(11) 0.0217(3) Uani 1 1 d . . . C35 C 0.70534(13) 0.19400(12) 0.82929(11) 0.0229(3) Uani 1 1 d . . . C36 C 0.73519(14) 0.11417(13) 0.76226(12) 0.0267(3) Uani 1 1 d . . . H36 H 0.6823 0.1024 0.7221 0.032 Uiso 1 1 calc R . . C37 C 0.84288(15) 0.05198(14) 0.75467(13) 0.0333(4) Uani 1 1 d . . . H37 H 0.8620 -0.0021 0.7085 0.040 Uiso 1 1 calc R . . C38 C 0.89122(15) 0.14053(16) 0.87372(14) 0.0392(4) Uani 1 1 d . . . H38 H 0.9455 0.1498 0.9135 0.047 Uiso 1 1 calc R . . C39 C 0.78619(14) 0.20686(14) 0.88657(13) 0.0311(4) Uani 1 1 d . . . H39 H 0.7696 0.2601 0.9335 0.037 Uiso 1 1 calc R . . C40 C 0.13424(19) 0.22324(16) 1.08134(15) 0.0444(5) Uani 1 1 d . . . C41 C 0.0901(2) 0.28397(18) 1.00718(16) 0.0538(6) Uani 1 1 d . . . H41 H 0.1281 0.2731 0.9452 0.065 Uiso 1 1 calc R . . C42 C -0.0079(2) 0.35956(19) 1.02218(19) 0.0625(7) Uani 1 1 d . . . H42 H -0.0367 0.3998 0.9705 0.075 Uiso 1 1 calc R . . C43 C -0.0643(2) 0.37726(19) 1.1112(2) 0.0620(7) Uani 1 1 d . . . H43 H -0.1312 0.4301 1.1215 0.074 Uiso 1 1 calc R . . C44 C -0.0222(2) 0.31711(18) 1.18547(18) 0.0575(6) Uani 1 1 d . . . H44 H -0.0609 0.3282 1.2472 0.069 Uiso 1 1 calc R . . C45 C 0.0762(2) 0.24059(17) 1.17045(15) 0.0479(5) Uani 1 1 d . . . H45 H 0.1040 0.1996 1.2221 0.057 Uiso 1 1 calc R . . C46 C 0.2420(2) 0.1415(2) 1.06512(17) 0.0599(6) Uani 1 1 d . . . H46A H 0.2711 0.1406 0.9982 0.090 Uiso 1 1 calc R . . H46B H 0.2263 0.0701 1.0856 0.090 Uiso 1 1 calc R . . H46C H 0.2988 0.1608 1.1011 0.090 Uiso 1 1 calc R . . C100 C 0.8958(10) 0.0056(7) 0.4508(12) 0.093(4) Uani 0.50 1 d P . . C101 C 0.932(2) -0.100(4) 0.497(3) 0.47(4) Uani 0.50 1 d P . . C102 C 1.0270(11) -0.0799(7) 0.5347(8) 0.082(3) Uani 0.50 1 d P . . C103 C 1.0568(7) -0.1764(8) 0.5955(6) 0.106(3) Uani 0.50 1 d P . . C200 C 0.9480(11) 0.0987(13) 0.4200(7) 0.136(8) Uani 0.50 1 d P . . C201 C 0.9217(10) -0.024(2) 0.4784(8) 0.127(8) Uani 0.50 1 d P . . C202 C 0.9491(14) -0.0914(7) 0.5277(8) 0.085(3) 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 Fe1 0.02414(13) 0.01979(12) 0.02148(13) 0.00120(8) -0.01039(9) -0.00171(9) O1 0.0331(6) 0.0215(5) 0.0257(6) 0.0025(4) -0.0149(5) -0.0052(5) O2 0.0286(6) 0.0208(5) 0.0227(6) 0.0016(4) -0.0094(5) -0.0015(5) O3 0.0244(6) 0.0217(5) 0.0289(6) -0.0009(5) -0.0098(5) -0.0001(4) O4 0.0247(6) 0.0225(5) 0.0257(6) 0.0036(4) -0.0100(5) -0.0030(4) O5 0.0236(6) 0.0234(5) 0.0236(6) -0.0017(4) -0.0104(4) 0.0015(4) O6 0.0243(6) 0.0258(6) 0.0206(5) 0.0001(4) -0.0078(4) -0.0011(5) N1 0.0408(9) 0.0240(7) 0.0396(9) 0.0061(6) -0.0110(7) -0.0043(6) N2 0.0620(11) 0.0330(8) 0.0349(9) -0.0053(7) -0.0137(8) -0.0134(8) N3 0.0287(8) 0.0487(10) 0.0357(9) 0.0105(7) -0.0125(7) 0.0015(7) N4 0.0355(8) 0.0254(7) 0.0376(8) 0.0065(6) -0.0097(7) -0.0030(6) N5 0.0407(9) 0.0405(9) 0.0274(8) -0.0047(7) -0.0014(7) -0.0027(7) N6 0.0254(8) 0.0374(9) 0.0506(10) -0.0058(7) -0.0076(7) 0.0038(7) C1 0.0244(8) 0.0223(8) 0.0253(8) 0.0022(6) -0.0094(6) -0.0021(6) C2 0.0230(8) 0.0221(7) 0.0274(8) 0.0020(6) -0.0099(6) -0.0017(6) C3 0.0414(10) 0.0241(8) 0.0274(9) 0.0021(7) -0.0100(8) -0.0027(7) C4 0.0532(12) 0.0225(8) 0.0348(10) -0.0025(7) -0.0106(9) -0.0043(8) C5 0.0310(9) 0.0292(9) 0.0313(9) 0.0081(7) -0.0086(7) -0.0065(7) C6 0.0274(8) 0.0266(8) 0.0280(9) 0.0021(7) -0.0100(7) -0.0032(7) C7 0.0311(9) 0.0229(8) 0.0268(8) 0.0017(6) -0.0139(7) -0.0026(7) C8 0.0226(8) 0.0247(8) 0.0229(8) -0.0002(6) -0.0079(6) -0.0034(6) C9 0.0261(8) 0.0242(8) 0.0245(8) -0.0013(6) -0.0071(6) -0.0049(6) C10 0.0484(11) 0.0272(9) 0.0291(9) 0.0029(7) -0.0136(8) -0.0087(8) C11 0.0672(14) 0.0240(9) 0.0396(11) -0.0021(8) -0.0140(10) -0.0110(9) C12 0.0526(12) 0.0341(9) 0.0251(9) -0.0001(7) -0.0127(8) -0.0098(9) C13 0.0412(10) 0.0251(8) 0.0275(9) 0.0008(7) -0.0124(7) -0.0060(7) C14 0.0217(8) 0.0258(8) 0.0210(8) -0.0002(6) -0.0048(6) 0.0000(6) C15 0.0213(8) 0.0282(8) 0.0228(8) 0.0005(6) -0.0051(6) 0.0020(6) C16 0.0378(11) 0.0268(9) 0.0670(14) 0.0025(9) -0.0264(10) 0.0000(8) C17 0.0407(11) 0.0331(10) 0.0644(14) 0.0092(10) -0.0214(10) 0.0063(9) C18 0.0511(14) 0.0522(13) 0.102(2) 0.0307(13) -0.0532(14) -0.0207(11) C19 0.0451(12) 0.0395(11) 0.0888(17) 0.0293(11) -0.0432(12) -0.0156(10) C20 0.0240(8) 0.0233(8) 0.0298(9) 0.0001(6) -0.0087(7) -0.0015(6) C21 0.0235(8) 0.0220(7) 0.0211(8) 0.0000(6) -0.0050(6) -0.0004(6) C22 0.0241(8) 0.0214(7) 0.0225(8) -0.0001(6) -0.0057(6) 0.0003(6) C23 0.0262(8) 0.0250(8) 0.0346(9) 0.0037(7) -0.0076(7) -0.0032(7) C24 0.0280(9) 0.0268(8) 0.0410(10) 0.0055(7) -0.0108(8) 0.0019(7) C25 0.0321(9) 0.0277(9) 0.0375(10) 0.0055(7) -0.0094(8) -0.0084(7) C26 0.0246(8) 0.0256(8) 0.0335(9) 0.0028(7) -0.0068(7) -0.0012(7) C27 0.0247(8) 0.0171(7) 0.0225(8) 0.0016(6) -0.0077(6) -0.0043(6) C28 0.0255(8) 0.0168(7) 0.0219(8) 0.0023(6) -0.0053(6) -0.0040(6) C29 0.0252(8) 0.0371(9) 0.0311(9) -0.0037(7) -0.0076(7) -0.0002(7) C30 0.0294(10) 0.0495(12) 0.0373(11) -0.0074(9) -0.0019(8) 0.0014(8) C31 0.0386(10) 0.0273(8) 0.0239(8) -0.0002(7) -0.0092(7) -0.0076(7) C32 0.0257(8) 0.0206(7) 0.0265(8) 0.0012(6) -0.0070(6) -0.0041(6) C33 0.0239(8) 0.0237(8) 0.0224(8) 0.0006(6) -0.0090(6) 0.0012(6) C34 0.0240(8) 0.0182(7) 0.0240(8) 0.0028(6) -0.0080(6) -0.0039(6) C35 0.0218(8) 0.0225(7) 0.0244(8) 0.0024(6) -0.0056(6) -0.0022(6) C36 0.0258(8) 0.0236(8) 0.0307(9) -0.0008(7) -0.0071(7) -0.0018(7) C37 0.0302(9) 0.0277(9) 0.0406(10) -0.0043(8) -0.0044(8) -0.0009(7) C38 0.0246(9) 0.0465(11) 0.0471(11) -0.0057(9) -0.0138(8) -0.0003(8) C39 0.0248(8) 0.0342(9) 0.0343(9) -0.0070(7) -0.0088(7) -0.0001(7) C40 0.0591(13) 0.0382(11) 0.0411(12) -0.0022(9) -0.0123(10) -0.0176(10) C41 0.0782(17) 0.0485(13) 0.0417(12) 0.0013(10) -0.0204(12) -0.0210(12) C42 0.0846(19) 0.0452(13) 0.0661(17) 0.0084(12) -0.0355(15) -0.0169(13) C43 0.0663(16) 0.0392(12) 0.084(2) -0.0014(12) -0.0231(15) -0.0082(11) C44 0.0694(16) 0.0466(13) 0.0583(15) -0.0084(11) -0.0051(12) -0.0159(12) C45 0.0622(14) 0.0448(12) 0.0409(12) 0.0000(9) -0.0136(10) -0.0156(11) C46 0.0695(17) 0.0632(15) 0.0458(13) 0.0002(11) -0.0050(12) -0.0099(13) C100 0.076(7) 0.049(4) 0.140(11) -0.039(5) 0.026(6) 0.010(4) C101 0.114(14) 0.84(9) 0.47(5) -0.59(7) 0.13(2) -0.11(3) C102 0.078(6) 0.071(5) 0.073(6) -0.008(4) 0.049(5) 0.010(5) C103 0.087(5) 0.113(6) 0.094(6) 0.040(5) 0.017(4) 0.018(5) C200 0.134(10) 0.171(15) 0.046(5) 0.010(6) 0.007(5) 0.114(11) C201 0.036(5) 0.30(2) 0.041(4) -0.007(8) -0.006(3) -0.022(8) C202 0.099(8) 0.058(4) 0.083(7) -0.028(4) 0.038(6) 0.000(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 Fe1 O1 1.9773(11) . ? Fe1 O5 1.9819(11) . ? Fe1 O6 1.9883(11) . ? Fe1 O4 1.9925(11) . ? Fe1 O3 2.0017(11) . ? Fe1 O2 2.0069(11) . ? O1 C1 1.2864(18) . ? O2 C8 1.2760(17) . ? O3 C14 1.2768(18) . ? O4 C21 1.2774(18) . ? O5 C27 1.2794(17) . ? O6 C34 1.2837(17) . ? N1 C5 1.333(2) . ? N1 C4 1.339(2) . ? N2 C12 1.333(2) . ? N2 C11 1.337(2) . ? N3 C18 1.311(3) . ? N3 C17 1.319(3) . ? N4 C24 1.333(2) . ? N4 C25 1.342(2) . ? N5 C31 1.336(2) . ? N5 C30 1.337(2) . ? N6 C38 1.336(2) . ? N6 C37 1.341(2) . ? C1 C7 1.390(2) . ? C1 C2 1.500(2) . ? C2 C3 1.389(2) . ? C2 C6 1.392(2) . ? C3 C4 1.387(2) . ? C5 C6 1.383(2) . ? C7 C8 1.408(2) . ? C8 C9 1.497(2) . ? C9 C10 1.387(2) . ? C9 C13 1.387(2) . ? C10 C11 1.387(2) . ? C12 C13 1.388(2) . ? C14 C20 1.405(2) . ? C14 C15 1.498(2) . ? C15 C19 1.364(2) . ? C15 C16 1.380(2) . ? C16 C17 1.390(3) . ? C18 C19 1.388(3) . ? C20 C21 1.398(2) . ? C21 C22 1.497(2) . ? C22 C26 1.390(2) . ? C22 C23 1.393(2) . ? C23 C24 1.387(2) . ? C25 C26 1.385(2) . ? C27 C33 1.397(2) . ? C27 C28 1.496(2) . ? C28 C29 1.388(2) . ? C28 C32 1.394(2) . ? C29 C30 1.377(3) . ? C31 C32 1.378(2) . ? C33 C34 1.388(2) . ? C34 C35 1.497(2) . ? C35 C39 1.392(2) . ? C35 C36 1.392(2) . ? C36 C37 1.386(2) . ? C38 C39 1.383(2) . ? C40 C45 1.383(3) . ? C40 C41 1.393(3) . ? C40 C46 1.507(3) . ? C41 C42 1.379(3) . ? C42 C43 1.375(4) . ? C43 C44 1.382(3) . ? C44 C45 1.389(3) . ? C100 C201 0.610(17) . ? C100 C101 1.48(6) . ? C100 C200 1.46(2) . ? C100 C102 1.474(19) 2_756 ? C100 C202 1.710(17) . ? C101 C202 0.54(4) . ? C101 C201 0.97(6) . ? C101 C102 1.40(3) . ? C101 C200 2.00(4) 2_756 ? C102 C200 0.765(12) 2_756 ? C102 C202 0.995(14) . ? C102 C100 1.474(19) 2_756 ? C102 C103 1.488(12) . ? C102 C201 1.54(2) 2_756 ? C102 C201 1.634(18) . ? C103 C200 0.990(16) 2_756 ? C103 C202 1.880(17) . ? C200 C102 0.765(12) 2_756 ? C200 C103 0.990(16) 2_756 ? C200 C202 1.52(2) 2_756 ? C200 C201 1.79(3) . ? C200 C101 2.00(4) 2_756 ? C201 C202 1.117(18) . ? C201 C102 1.54(2) 2_756 ? C202 C200 1.52(2) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O5 91.76(4) . . ? O1 Fe1 O6 98.02(5) . . ? O5 Fe1 O6 88.16(4) . . ? O1 Fe1 O4 172.76(4) . . ? O5 Fe1 O4 93.10(4) . . ? O6 Fe1 O4 87.51(4) . . ? O1 Fe1 O3 88.93(5) . . ? O5 Fe1 O3 92.71(4) . . ? O6 Fe1 O3 172.97(4) . . ? O4 Fe1 O3 85.48(4) . . ? O1 Fe1 O2 86.69(4) . . ? O5 Fe1 O2 178.06(4) . . ? O6 Fe1 O2 90.90(4) . . ? O4 Fe1 O2 88.56(4) . . ? O3 Fe1 O2 88.43(4) . . ? C1 O1 Fe1 125.68(10) . . ? C8 O2 Fe1 125.48(10) . . ? C14 O3 Fe1 124.26(10) . . ? C21 O4 Fe1 126.23(9) . . ? C27 O5 Fe1 127.45(10) . . ? C34 O6 Fe1 126.19(10) . . ? C5 N1 C4 116.31(14) . . ? C12 N2 C11 116.16(15) . . ? C18 N3 C17 115.46(16) . . ? C24 N4 C25 116.52(14) . . ? C31 N5 C30 116.13(15) . . ? C38 N6 C37 116.53(15) . . ? O1 C1 C7 125.16(14) . . ? O1 C1 C2 114.87(13) . . ? C7 C1 C2 119.94(14) . . ? C3 C2 C6 117.83(15) . . ? C3 C2 C1 119.90(14) . . ? C6 C2 C1 122.24(14) . . ? C4 C3 C2 118.59(16) . . ? N1 C4 C3 124.21(16) . . ? N1 C5 C6 124.11(16) . . ? C5 C6 C2 118.95(15) . . ? C1 C7 C8 122.78(14) . . ? O2 C8 C7 124.00(14) . . ? O2 C8 C9 116.07(13) . . ? C7 C8 C9 119.87(14) . . ? C10 C9 C13 117.73(15) . . ? C10 C9 C8 119.21(14) . . ? C13 C9 C8 123.03(14) . . ? C11 C10 C9 118.87(16) . . ? N2 C11 C10 124.15(17) . . ? N2 C12 C13 124.14(16) . . ? C9 C13 C12 118.95(15) . . ? O3 C14 C20 123.97(14) . . ? O3 C14 C15 115.63(13) . . ? C20 C14 C15 120.40(14) . . ? C19 C15 C16 116.76(15) . . ? C19 C15 C14 123.94(15) . . ? C16 C15 C14 119.27(15) . . ? C15 C16 C17 119.22(18) . . ? N3 C17 C16 124.32(18) . . ? N3 C18 C19 124.87(19) . . ? C15 C19 C18 119.36(18) . . ? C21 C20 C14 122.49(14) . . ? O4 C21 C20 124.61(14) . . ? O4 C21 C22 114.48(13) . . ? C20 C21 C22 120.90(14) . . ? C26 C22 C23 118.12(14) . . ? C26 C22 C21 123.02(14) . . ? C23 C22 C21 118.81(14) . . ? C24 C23 C22 118.68(15) . . ? N4 C24 C23 124.02(16) . . ? N4 C25 C26 124.09(16) . . ? C25 C26 C22 118.55(15) . . ? O5 C27 C33 124.34(14) . . ? O5 C27 C28 115.79(13) . . ? C33 C27 C28 119.87(13) . . ? C29 C28 C32 117.41(15) . . ? C29 C28 C27 119.66(14) . . ? C32 C28 C27 122.94(14) . . ? C30 C29 C28 119.14(16) . . ? N5 C30 C29 124.18(18) . . ? N5 C31 C32 124.20(16) . . ? C31 C32 C28 118.94(15) . . ? C34 C33 C27 123.82(14) . . ? O6 C34 C33 125.46(14) . . ? O6 C34 C35 115.42(14) . . ? C33 C34 C35 119.11(13) . . ? C39 C35 C36 117.68(15) . . ? C39 C35 C34 122.45(14) . . ? C36 C35 C34 119.87(13) . . ? C37 C36 C35 119.37(15) . . ? N6 C37 C36 123.36(16) . . ? N6 C38 C39 124.46(16) . . ? C38 C39 C35 118.60(16) . . ? C45 C40 C41 117.9(2) . . ? C45 C40 C46 121.0(2) . . ? C41 C40 C46 121.1(2) . . ? C42 C41 C40 121.1(2) . . ? C43 C42 C41 120.6(2) . . ? C42 C43 C44 119.0(2) . . ? C43 C44 C45 120.4(2) . . ? C40 C45 C44 120.9(2) . . ? C201 C100 C101 27(3) . . ? C201 C100 C200 113(3) . . ? C101 C100 C200 136.3(17) . . ? C201 C100 C102 85(3) . 2_756 ? C101 C100 C102 110.2(18) . 2_756 ? C200 C100 C102 30.2(5) . 2_756 ? C201 C100 C202 11(2) . . ? C101 C100 C202 17.7(12) . . ? C200 C100 C202 124.0(10) . . ? C102 C100 C202 95.2(10) 2_756 . ? C202 C101 C201 90(5) . . ? C202 C101 C102 33(3) . . ? C201 C101 C102 85(2) . . ? C202 C101 C100 106(6) . . ? C201 C101 C100 16.4(14) . . ? C102 C101 C100 100(3) . . ? C202 C101 C200 23(3) . 2_756 ? C201 C101 C200 97(2) . 2_756 ? C102 C101 C200 16.3(9) . 2_756 ? C100 C101 C200 113(2) . 2_756 ? C200 C102 C202 119(2) 2_756 . ? C200 C102 C101 133(3) 2_756 . ? C202 C102 C101 17.2(16) . . ? C200 C102 C100 74(2) 2_756 2_756 ? C202 C102 C100 149.1(11) . 2_756 ? C101 C102 C100 149(3) . 2_756 ? C200 C102 C103 36.9(17) 2_756 . ? C202 C102 C103 96.4(10) . . ? C101 C102 C103 104(2) . . ? C100 C102 C103 106.7(13) 2_756 . ? C200 C102 C201 96(2) 2_756 2_756 ? C202 C102 C201 129.7(12) . 2_756 ? C101 C102 C201 126(3) . 2_756 ? C100 C102 C201 23.2(6) 2_756 2_756 ? C103 C102 C201 129.8(13) . 2_756 ? C200 C102 C201 151.7(14) 2_756 . ? C202 C102 C201 42.1(10) . . ? C101 C102 C201 36(3) . . ? C100 C102 C201 113.1(11) 2_756 . ? C103 C102 C201 138.4(13) . . ? C201 C102 C201 90.3(8) 2_756 . ? C200 C103 C102 27.7(10) 2_756 . ? C200 C103 C202 53.8(11) 2_756 . ? C102 C103 C202 31.7(5) . . ? C102 C200 C103 115(3) 2_756 2_756 ? C102 C200 C100 76.1(18) 2_756 . ? C103 C200 C100 151.7(13) 2_756 . ? C102 C200 C202 34.9(13) 2_756 2_756 ? C103 C200 C202 94.6(16) 2_756 2_756 ? C100 C200 C202 106.3(9) . 2_756 ? C102 C200 C201 59.0(17) 2_756 . ? C103 C200 C201 161.1(11) 2_756 . ? C100 C200 C201 18.2(7) . . ? C202 C200 C201 88.0(7) 2_756 . ? C102 C200 C101 30.9(19) 2_756 2_756 ? C103 C200 C101 92(2) 2_756 2_756 ? C100 C200 C101 105.6(19) . 2_756 ? C202 C200 C101 8.0(8) 2_756 2_756 ? C201 C200 C101 87.6(16) . 2_756 ? C100 C201 C101 137(4) . . ? C100 C201 C202 163(3) . . ? C101 C201 C202 29(2) . . ? C100 C201 C102 72(3) . 2_756 ? C101 C201 C102 148(3) . 2_756 ? C202 C201 C102 124.1(10) . 2_756 ? C100 C201 C102 159(3) . . ? C101 C201 C102 59(2) . . ? C202 C201 C102 36.7(8) . . ? C102 C201 C102 89.7(8) 2_756 . ? C100 C201 C200 48(2) . . ? C101 C201 C200 160(2) . . ? C202 C201 C200 148.1(13) . . ? C102 C201 C200 25.2(8) 2_756 . ? C102 C201 C200 111.8(11) . . ? C101 C202 C102 130(4) . . ? C101 C202 C201 61(6) . . ? C102 C202 C201 101.2(14) . . ? C101 C202 C200 149(4) . 2_756 ? C102 C202 C200 26.1(9) . 2_756 ? C201 C202 C200 123.9(15) . 2_756 ? C101 C202 C100 56(6) . . ? C102 C202 C100 106.9(11) . . ? C201 C202 C100 5.8(11) . . ? C200 C202 C100 129.7(11) 2_756 . ? C101 C202 C103 131(5) . . ? C102 C202 C103 51.9(9) . . ? C201 C202 C103 152.9(14) . . ? C200 C202 C103 31.7(7) 2_756 . ? C100 C202 C103 158.4(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.446 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.080 #===end data_compound4_k05cr1 _database_code_depnum_ccdc_archive 'CCDC 853057' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H31 Al Cl12 N6 O6' _chemical_formula_weight 1180.12 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' Al Al 0.0645 0.0514 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2070(2) _cell_length_b 15.0570(2) _cell_length_c 33.3180(5) _cell_angle_alpha 92.341(1) _cell_angle_beta 90.772(1) _cell_angle_gamma 96.535(1) _cell_volume 5082.17(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 123953 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.373 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52542 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16879 _reflns_number_gt 12637 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Asymmetric unit consists of two aluminium complex molecules, in addition to eight molecules of dichloromethane. Slightly higher than expected R1 values reflects the residual electron density maxima in the region of the solvent chlorines, and a fall off on diffracting power of the crystal at Bragg angles greater than 20o. ; _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^)+(0.1105P)^2^+29.2607P] 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 16879 _refine_ls_number_parameters 1226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2540 _refine_ls_wR_factor_gt 0.2327 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Cl1 Cl 0.1972(3) 0.6151(2) 0.43556(9) 0.0939(10) Uani 1 1 d . . . Cl2 Cl 0.4315(3) 0.66914(17) 0.48302(6) 0.0739(7) Uani 1 1 d . . . Cl3 Cl 0.3953(3) 0.49629(18) 0.44236(8) 0.0791(7) Uani 1 1 d . . . Cl4 Cl 0.0214(3) 0.3333(2) 0.44021(8) 0.1029(10) Uani 1 1 d . . . Cl5 Cl 0.1065(2) 0.39310(17) 0.36112(7) 0.0692(6) Uani 1 1 d . . . Cl6 Cl -0.0591(3) 0.22427(16) 0.36822(8) 0.0757(7) Uani 1 1 d . . . Cl7 Cl 0.60459(18) 0.31732(12) 0.40802(5) 0.0430(4) Uani 1 1 d . . . Cl8 Cl 0.3626(4) 0.2354(3) 0.43983(12) 0.162(2) Uani 1 1 d . . . Cl9 Cl 0.5374(3) 0.12610(15) 0.39863(10) 0.0870(9) Uani 1 1 d . . . Cl10 Cl 0.3217(2) 0.59500(19) 0.33501(6) 0.0657(6) Uani 1 1 d . . . Cl11 Cl 0.6054(2) 0.60961(14) 0.33291(7) 0.0583(6) Uani 1 1 d . . . Cl12 Cl 0.4503(2) 0.52771(13) 0.26550(6) 0.0586(6) Uani 1 1 d . . . Cl13 Cl 0.3561(3) 0.35469(19) 0.18479(8) 0.0862(8) Uani 1 1 d . . . Cl14 Cl 0.4780(3) 0.49349(18) 0.13694(8) 0.0733(7) Uani 1 1 d . . . Cl15 Cl 0.6334(4) 0.3860(5) 0.1773(2) 0.247(4) Uani 1 1 d . . . Cl16 Cl 1.0275(2) 0.75882(14) 0.12929(6) 0.0561(5) Uani 1 1 d . . . Cl17 Cl 0.8471(2) 0.59646(15) 0.12945(7) 0.0635(6) Uani 1 1 d . . . Cl18 Cl 0.9243(3) 0.67589(17) 0.05436(7) 0.0847(8) Uani 1 1 d . . . Cl19 Cl 0.6066(4) 0.4672(4) 0.03456(11) 0.160(2) Uani 1 1 d . . . Cl20 Cl 0.8626(2) 0.41156(18) 0.02572(8) 0.0737(7) Uani 1 1 d . . . Cl21 Cl 0.6830(7) 0.3077(2) 0.0720(2) 0.272(5) Uani 1 1 d . . . Cl22 Cl 0.5511(4) 0.7746(3) 0.03907(11) 0.1337(15) Uani 1 1 d . . . Cl23 Cl 0.3558(2) 0.67348(15) 0.08653(7) 0.0660(6) Uani 1 1 d . . . Cl24 Cl 0.4358(3) 0.85955(15) 0.10375(9) 0.0797(8) Uani 1 1 d . . . Al1 Al 0.06233(16) 0.87267(10) 0.35169(5) 0.0173(4) Uani 1 1 d . . . Al2 Al 0.92265(16) 0.10025(10) 0.15419(5) 0.0171(4) Uani 1 1 d . . . O1 O -0.1060(4) 0.8761(2) 0.32771(11) 0.0194(8) Uani 1 1 d . . . O2 O 0.1280(4) 0.9743(2) 0.32380(11) 0.0182(8) Uani 1 1 d . . . O3 O 0.0125(4) 0.9480(2) 0.39402(11) 0.0194(8) Uani 1 1 d . . . O4 O 0.2276(4) 0.8673(2) 0.37608(11) 0.0208(8) Uani 1 1 d . . . O5 O 0.1099(4) 0.7986(2) 0.30853(10) 0.0192(8) Uani 1 1 d . . . O6 O -0.0114(4) 0.7731(2) 0.37862(11) 0.0209(8) Uani 1 1 d . . . O7 O 0.7600(4) 0.1113(2) 0.12910(11) 0.0218(9) Uani 1 1 d . . . O8 O 0.9737(4) 0.0288(2) 0.11029(11) 0.0211(8) Uani 1 1 d . . . O9 O 0.8459(4) -0.0036(2) 0.17863(11) 0.0194(8) Uani 1 1 d . . . O10 O 1.0867(4) 0.0883(2) 0.17949(11) 0.0197(8) Uani 1 1 d . . . O11 O 0.8718(4) 0.1721(2) 0.19762(10) 0.0185(8) Uani 1 1 d . . . O12 O 1.0040(4) 0.2006(2) 0.12924(11) 0.0221(9) Uani 1 1 d . . . N1 N -0.4981(5) 0.8345(3) 0.29679(15) 0.0286(12) Uani 1 1 d . . . N2 N 0.0346(5) 1.1567(3) 0.50588(14) 0.0286(12) Uani 1 1 d . . . N3 N 0.3315(5) 1.2243(3) 0.31783(15) 0.0285(12) Uani 1 1 d . . . N4 N 0.6010(5) 0.9148(4) 0.46524(16) 0.0344(13) Uani 1 1 d . . . N5 N 0.0998(5) 0.5589(3) 0.21095(15) 0.0326(13) Uani 1 1 d . . . N6 N -0.2049(6) 0.4842(3) 0.41011(16) 0.0368(14) Uani 1 1 d . . . N7 N 0.3915(5) 0.0771(4) 0.03864(15) 0.0316(12) Uani 1 1 d . . . N8 N 0.9625(5) -0.1469(3) -0.01208(15) 0.0287(12) Uani 1 1 d . . . N9 N 0.6348(5) -0.2524(3) 0.17423(17) 0.0326(12) Uani 1 1 d . . . N10 N 1.4791(5) 0.1048(4) 0.21503(16) 0.0356(13) Uani 1 1 d . . . N11 N 0.8346(5) 0.4186(3) 0.28868(15) 0.0300(12) Uani 1 1 d . . . N12 N 1.1563(6) 0.4958(3) 0.09325(15) 0.0327(13) Uani 1 1 d . . . C1 C -0.1530(5) 0.9443(4) 0.31441(16) 0.0196(12) Uani 1 1 d . . . C2 C -0.0753(5) 1.0241(4) 0.30603(17) 0.0221(12) Uani 1 1 d . . . H2 H -0.1176 1.0728 0.2969 0.026 Uiso 1 1 calc R . . C3 C 0.0600(5) 1.0345(3) 0.31053(15) 0.0175(12) Uani 1 1 d . . . C4 C -0.2991(6) 0.9355(4) 0.30845(16) 0.0223(12) Uani 1 1 d . . . C5 C -0.3673(6) 0.8506(4) 0.30183(17) 0.0251(13) Uani 1 1 d . . . H5 H -0.3177 0.8009 0.3008 0.030 Uiso 1 1 calc R . . C6 C -0.5659(6) 0.9062(4) 0.29966(19) 0.0319(15) Uani 1 1 d . . . H6 H -0.6593 0.8965 0.2970 0.038 Uiso 1 1 calc R . . C7 C -0.5078(6) 0.9924(5) 0.3062(2) 0.0363(16) Uani 1 1 d . . . H7 H -0.5600 1.0407 0.3079 0.044 Uiso 1 1 calc R . . C8 C -0.3714(6) 1.0079(4) 0.3103(2) 0.0324(15) Uani 1 1 d . . . H8 H -0.3285 1.0671 0.3144 0.039 Uiso 1 1 calc R . . C9 C 0.1391(5) 1.1208(4) 0.30131(16) 0.0191(12) Uani 1 1 d . . . C10 C 0.2547(5) 1.1478(4) 0.32328(16) 0.0210(12) Uani 1 1 d . . . H10 H 0.2805 1.1098 0.3433 0.025 Uiso 1 1 calc R . . C11 C 0.2928(6) 1.2777(4) 0.28984(19) 0.0295(14) Uani 1 1 d . . . H11 H 0.3464 1.3321 0.2855 0.035 Uiso 1 1 calc R . . C12 C 0.1792(6) 1.2572(4) 0.26720(18) 0.0295(14) Uani 1 1 d . . . H12 H 0.1554 1.2971 0.2477 0.035 Uiso 1 1 calc R . . C13 C 0.0995(6) 1.1782(4) 0.27288(17) 0.0238(13) Uani 1 1 d . . . H13 H 0.0198 1.1635 0.2578 0.029 Uiso 1 1 calc R . . C14 C 0.0849(5) 0.9888(3) 0.42200(15) 0.0178(11) Uani 1 1 d . . . C15 C 0.2164(6) 0.9751(4) 0.42875(17) 0.0261(13) Uani 1 1 d . . . H15 H 0.2655 1.0106 0.4492 0.031 Uiso 1 1 calc R . . C16 C 0.2789(5) 0.9116(4) 0.40681(15) 0.0184(12) Uani 1 1 d . . . C17 C 0.0213(6) 1.0518(4) 0.44882(16) 0.0212(12) Uani 1 1 d . . . C18 C 0.0890(6) 1.1011(4) 0.48065(16) 0.0231(13) Uani 1 1 d . . . H18 H 0.1797 1.0947 0.4845 0.028 Uiso 1 1 calc R . . C19 C -0.0928(7) 1.1650(4) 0.50017(19) 0.0349(16) Uani 1 1 d . . . H19 H -0.1331 1.2039 0.5181 0.042 Uiso 1 1 calc R . . C20 C -0.1702(7) 1.1196(5) 0.4692(2) 0.0388(17) Uani 1 1 d . . . H20 H -0.2606 1.1278 0.4660 0.047 Uiso 1 1 calc R . . C21 C -0.1110(6) 1.0623(4) 0.44344(19) 0.0305(14) Uani 1 1 d . . . H21 H -0.1609 1.0303 0.4221 0.037 Uiso 1 1 calc R . . C22 C 0.4136(6) 0.8913(4) 0.41905(16) 0.0215(12) Uani 1 1 d . . . C23 C 0.4797(6) 0.9287(4) 0.45397(18) 0.0283(14) Uani 1 1 d . . . H23 H 0.4344 0.9669 0.4709 0.034 Uiso 1 1 calc R . . C24 C 0.6621(6) 0.8596(5) 0.4409(2) 0.0350(15) Uani 1 1 d . . . H24 H 0.7491 0.8487 0.4480 0.042 Uiso 1 1 calc R . . C25 C 0.6053(7) 0.8179(5) 0.40621(19) 0.0363(16) Uani 1 1 d . . . H25 H 0.6523 0.7795 0.3900 0.044 Uiso 1 1 calc R . . C26 C 0.4789(6) 0.8332(4) 0.39562(17) 0.0285(14) Uani 1 1 d . . . H26 H 0.4369 0.8039 0.3723 0.034 Uiso 1 1 calc R . . C27 C 0.0729(5) 0.7146(3) 0.30159(15) 0.0175(11) Uani 1 1 d . . . C28 C -0.0017(6) 0.6611(4) 0.32749(16) 0.0215(12) Uani 1 1 d . . . H28 H -0.0302 0.6009 0.3191 0.026 Uiso 1 1 calc R . . C29 C -0.0372(5) 0.6921(3) 0.36579(15) 0.0176(11) Uani 1 1 d . . . C30 C 0.1191(5) 0.6764(4) 0.26286(16) 0.0195(12) Uani 1 1 d . . . C31 C 0.0603(6) 0.5957(4) 0.24521(17) 0.0248(13) Uani 1 1 d . . . H31 H -0.0123 0.5650 0.2584 0.030 Uiso 1 1 calc R . . C32 C 0.2020(7) 0.6029(4) 0.19290(18) 0.0319(15) Uani 1 1 d . . . H32 H 0.2319 0.5774 0.1686 0.038 Uiso 1 1 calc R . . C33 C 0.2671(6) 0.6836(4) 0.20767(17) 0.0254(13) Uani 1 1 d . . . H33 H 0.3395 0.7125 0.1938 0.030 Uiso 1 1 calc R . . C34 C 0.2245(6) 0.7211(4) 0.24294(17) 0.0241(13) Uani 1 1 d . . . H34 H 0.2666 0.7768 0.2535 0.029 Uiso 1 1 calc R . . C35 C -0.1067(5) 0.6308(4) 0.39468(16) 0.0199(12) Uani 1 1 d . . . C36 C -0.1446(6) 0.5409(4) 0.38474(17) 0.0260(13) Uani 1 1 d . . . H36 H -0.1267 0.5188 0.3585 0.031 Uiso 1 1 calc R . . C37 C -0.2307(7) 0.5159(5) 0.4468(2) 0.0397(17) Uani 1 1 d . . . H37 H -0.2738 0.4760 0.4651 0.048 Uiso 1 1 calc R . . C38 C -0.1973(7) 0.6049(4) 0.45944(18) 0.0338(15) Uani 1 1 d . . . H38 H -0.2179 0.6256 0.4857 0.041 Uiso 1 1 calc R . . C39 C -0.1335(6) 0.6629(4) 0.43289(17) 0.0250(13) Uani 1 1 d . . . H39 H -0.1084 0.7238 0.4408 0.030 Uiso 1 1 calc R . . C40 C 0.7078(6) 0.0683(4) 0.09792(16) 0.0206(12) Uani 1 1 d . . . C41 C 0.7714(6) 0.0082(4) 0.07457(18) 0.0261(13) Uani 1 1 d . . . H41 H 0.7225 -0.0252 0.0534 0.031 Uiso 1 1 calc R . . C42 C 0.9024(6) -0.0058(3) 0.08050(16) 0.0192(12) Uani 1 1 d . . . C43 C 0.5723(6) 0.0869(4) 0.08682(17) 0.0211(12) Uani 1 1 d . . . C44 C 0.5151(6) 0.0647(4) 0.04881(17) 0.0281(14) Uani 1 1 d . . . H44 H 0.5673 0.0391 0.0290 0.034 Uiso 1 1 calc R . . C45 C 0.3199(6) 0.1135(4) 0.06689(19) 0.0332(15) Uani 1 1 d . . . H45 H 0.2314 0.1219 0.0603 0.040 Uiso 1 1 calc R . . C46 C 0.3677(6) 0.1396(4) 0.10512(19) 0.0331(15) Uani 1 1 d . . . H46 H 0.3137 0.1660 0.1242 0.040 Uiso 1 1 calc R . . C47 C 0.4965(6) 0.1264(4) 0.11505(17) 0.0276(14) Uani 1 1 d . . . H47 H 0.5322 0.1442 0.1410 0.033 Uiso 1 1 calc R . . C48 C 0.9699(6) -0.0620(4) 0.05121(16) 0.0200(12) Uani 1 1 d . . . C49 C 0.9060(6) -0.0998(4) 0.01611(16) 0.0252(13) Uani 1 1 d . . . H49 H 0.8161 -0.0912 0.0121 0.030 Uiso 1 1 calc R . . C50 C 1.0882(7) -0.1588(4) -0.00577(19) 0.0351(16) Uani 1 1 d . . . H50 H 1.1309 -0.1916 -0.0257 0.042 Uiso 1 1 calc R . . C51 C 1.1607(6) -0.1257(4) 0.0285(2) 0.0344(15) Uani 1 1 d . . . H51 H 1.2500 -0.1364 0.0321 0.041 Uiso 1 1 calc R . . C52 C 1.0989(6) -0.0770(4) 0.05719(18) 0.0276(14) Uani 1 1 d . . . H52 H 1.1455 -0.0541 0.0810 0.033 Uiso 1 1 calc R . . C53 C 0.9057(5) -0.0660(4) 0.19256(15) 0.0187(12) Uani 1 1 d . . . C54 C 1.0403(6) -0.0598(4) 0.20014(17) 0.0215(12) Uani 1 1 d . . . H54 H 1.0763 -0.1095 0.2108 0.026 Uiso 1 1 calc R . . C55 C 1.1251(5) 0.0173(4) 0.19259(16) 0.0201(12) Uani 1 1 d . . . C56 C 0.8205(5) -0.1522(4) 0.19891(16) 0.0211(12) Uani 1 1 d . . . C57 C 0.7154(6) -0.1763(4) 0.17245(18) 0.0244(13) Uani 1 1 d . . . H57 H 0.6998 -0.1366 0.1519 0.029 Uiso 1 1 calc R . . C58 C 0.6606(6) -0.3072(4) 0.2028(2) 0.0329(15) Uani 1 1 d . . . H58 H 0.6045 -0.3617 0.2045 0.040 Uiso 1 1 calc R . . C59 C 0.7631(6) -0.2901(4) 0.23007(18) 0.0294(14) Uani 1 1 d . . . H59 H 0.7772 -0.3319 0.2499 0.035 Uiso 1 1 calc R . . C60 C 0.8465(6) -0.2102(4) 0.22817(17) 0.0263(13) Uani 1 1 d . . . H60 H 0.9188 -0.1963 0.2465 0.032 Uiso 1 1 calc R . . C61 C 1.2697(5) 0.0179(4) 0.19992(16) 0.0211(12) Uani 1 1 d . . . C62 C 1.3479(6) 0.0984(4) 0.20948(17) 0.0273(13) Uani 1 1 d . . . H62 H 1.3060 0.1515 0.2122 0.033 Uiso 1 1 calc R . . C63 C 1.5362(6) 0.0304(5) 0.2104(2) 0.0391(17) Uani 1 1 d . . . H63 H 1.6294 0.0342 0.2135 0.047 Uiso 1 1 calc R . . C64 C 1.4676(7) -0.0517(5) 0.2014(2) 0.0407(17) Uani 1 1 d . . . H64 H 1.5128 -0.1034 0.1989 0.049 Uiso 1 1 calc R . . C65 C 1.3317(6) -0.0589(4) 0.1960(2) 0.0339(15) Uani 1 1 d . . . H65 H 1.2825 -0.1153 0.1898 0.041 Uiso 1 1 calc R . . C66 C 0.8903(5) 0.2584(4) 0.20254(16) 0.0182(11) Uani 1 1 d . . . C67 C 0.9582(6) 0.3148(4) 0.17549(17) 0.0243(13) Uani 1 1 d . . . H67 H 0.9683 0.3774 0.1816 0.029 Uiso 1 1 calc R . . C68 C 1.0117(5) 0.2836(3) 0.13995(15) 0.0178(11) Uani 1 1 d . . . C69 C 0.8339(5) 0.2962(4) 0.23952(16) 0.0184(11) Uani 1 1 d . . . C70 C 0.8850(6) 0.3795(4) 0.25667(17) 0.0258(13) Uani 1 1 d . . . H70 H 0.9603 0.4101 0.2448 0.031 Uiso 1 1 calc R . . C71 C 0.7290(6) 0.3739(4) 0.30497(18) 0.0311(14) Uani 1 1 d . . . H71 H 0.6906 0.4010 0.3275 0.037 Uiso 1 1 calc R . . C72 C 0.6730(6) 0.2907(4) 0.29082(18) 0.0295(14) Uani 1 1 d . . . H72 H 0.5988 0.2612 0.3037 0.035 Uiso 1 1 calc R . . C73 C 0.7261(6) 0.2505(4) 0.25757(17) 0.0233(12) Uani 1 1 d . . . H73 H 0.6895 0.1930 0.2474 0.028 Uiso 1 1 calc R . . C74 C 1.0795(6) 0.3459(4) 0.11164(16) 0.0204(12) Uani 1 1 d . . . C75 C 1.0923(6) 0.4382(4) 0.11802(17) 0.0273(13) Uani 1 1 d . . . H75 H 1.0534 0.4620 0.1413 0.033 Uiso 1 1 calc R . . C76 C 1.2105(7) 0.4614(4) 0.06110(18) 0.0311(15) Uani 1 1 d . . . H76 H 1.2563 0.5013 0.0433 0.037 Uiso 1 1 calc R . . C77 C 1.2041(6) 0.3702(4) 0.05205(17) 0.0306(14) Uani 1 1 d . . . H77 H 1.2458 0.3484 0.0289 0.037 Uiso 1 1 calc R . . C78 C 1.1360(6) 0.3118(4) 0.07730(17) 0.0281(14) Uani 1 1 d . . . H78 H 1.1278 0.2492 0.0714 0.034 Uiso 1 1 calc R . . C79 C 0.3648(8) 0.6064(6) 0.4403(2) 0.053(2) Uani 1 1 d . . . H79 H 0.4091 0.6321 0.4161 0.064 Uiso 1 1 calc R . . C80 C -0.0156(9) 0.3321(5) 0.3894(2) 0.052(2) Uani 1 1 d . . . H80 H -0.0963 0.3636 0.3870 0.063 Uiso 1 1 calc R . . C81 C 0.4770(7) 0.2285(5) 0.4025(2) 0.0419(17) Uani 1 1 d . . . H81 H 0.4304 0.2361 0.3765 0.050 Uiso 1 1 calc R . . C82 C 0.4591(7) 0.6105(5) 0.3040(2) 0.0359(15) Uani 1 1 d . . . H82 H 0.4605 0.6701 0.2917 0.043 Uiso 1 1 calc R . . C83 C 0.4868(9) 0.3881(6) 0.1535(3) 0.061(2) Uani 1 1 d . . . H83 H 0.4824 0.3454 0.1296 0.073 Uiso 1 1 calc R . . C84 C 0.9742(8) 0.6567(5) 0.1032(2) 0.0438(18) Uani 1 1 d . . . H84 H 1.0504 0.6205 0.1016 0.053 Uiso 1 1 calc R . . C85 C 0.7232(10) 0.4115(6) 0.0553(2) 0.065(2) Uani 1 1 d . . . H85 H 0.7541 0.4486 0.0799 0.077 Uiso 1 1 calc R . . C86 C 0.4891(8) 0.7559(5) 0.0867(2) 0.053(2) Uani 1 1 d . . . H86 H 0.5605 0.7399 0.1050 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0640(16) 0.128(2) 0.0936(19) -0.0361(18) -0.0232(14) 0.0477(16) Cl2 0.0911(18) 0.0800(16) 0.0442(11) 0.0030(11) -0.0109(11) -0.0161(14) Cl3 0.0795(17) 0.0735(16) 0.0884(18) -0.0015(14) -0.0080(14) 0.0301(14) Cl4 0.121(3) 0.129(3) 0.0554(15) 0.0168(16) -0.0124(15) -0.004(2) Cl5 0.0653(15) 0.0845(16) 0.0589(13) 0.0050(12) 0.0167(11) 0.0112(12) Cl6 0.0837(17) 0.0641(14) 0.0799(16) -0.0231(12) 0.0169(13) 0.0182(13) Cl7 0.0443(10) 0.0430(10) 0.0367(9) -0.0066(7) 0.0055(7) -0.0146(8) Cl8 0.144(3) 0.161(3) 0.148(3) -0.089(3) 0.106(3) -0.111(3) Cl9 0.0741(17) 0.0381(12) 0.146(3) -0.0003(13) -0.0483(17) 0.0000(11) Cl10 0.0420(12) 0.115(2) 0.0428(11) 0.0169(11) 0.0033(9) 0.0157(12) Cl11 0.0425(11) 0.0515(12) 0.0810(15) -0.0031(10) -0.0224(10) 0.0099(9) Cl12 0.0953(17) 0.0379(10) 0.0397(10) -0.0018(8) 0.0017(10) -0.0036(10) Cl13 0.097(2) 0.0918(19) 0.0612(14) 0.0002(13) 0.0272(14) -0.0274(15) Cl14 0.0685(15) 0.0804(16) 0.0748(15) 0.0265(13) 0.0074(12) 0.0160(13) Cl15 0.072(2) 0.395(9) 0.305(7) 0.250(7) -0.017(3) 0.070(4) Cl16 0.0623(13) 0.0547(12) 0.0515(11) -0.0126(9) 0.0019(10) 0.0127(10) Cl17 0.0641(14) 0.0678(14) 0.0587(13) 0.0009(10) 0.0270(11) 0.0063(11) Cl18 0.134(2) 0.0699(16) 0.0442(12) 0.0059(11) -0.0124(13) -0.0127(16) Cl19 0.079(2) 0.327(7) 0.092(2) 0.048(3) 0.0307(19) 0.080(3) Cl20 0.0531(14) 0.0865(17) 0.0858(17) 0.0412(14) 0.0020(12) 0.0140(12) Cl21 0.407(9) 0.063(2) 0.363(8) 0.057(3) 0.337(8) 0.048(3) Cl22 0.123(3) 0.176(4) 0.090(2) 0.003(2) 0.049(2) -0.040(3) Cl23 0.0606(14) 0.0537(12) 0.0782(15) 0.0005(11) 0.0003(11) -0.0165(11) Cl24 0.0919(19) 0.0444(12) 0.0995(19) -0.0066(12) -0.0446(15) 0.0021(12) Al1 0.0202(9) 0.0142(8) 0.0171(8) -0.0040(6) -0.0029(6) 0.0023(7) Al2 0.0214(9) 0.0143(8) 0.0154(8) -0.0028(6) -0.0041(6) 0.0026(7) O1 0.019(2) 0.0158(19) 0.0221(19) -0.0060(15) -0.0033(15) -0.0003(16) O2 0.016(2) 0.0162(19) 0.0220(19) -0.0014(15) -0.0036(15) 0.0027(16) O3 0.020(2) 0.0190(19) 0.0182(19) -0.0059(15) -0.0024(15) 0.0007(16) O4 0.022(2) 0.020(2) 0.0199(19) -0.0067(16) -0.0054(16) 0.0059(16) O5 0.023(2) 0.0174(19) 0.0169(18) -0.0037(15) -0.0023(15) 0.0007(16) O6 0.028(2) 0.0161(19) 0.0177(19) -0.0038(15) 0.0020(16) 0.0005(17) O7 0.022(2) 0.022(2) 0.022(2) -0.0078(16) -0.0083(16) 0.0083(17) O8 0.021(2) 0.021(2) 0.0213(19) -0.0062(16) -0.0057(16) 0.0036(16) O9 0.018(2) 0.0145(19) 0.026(2) -0.0012(16) -0.0024(16) 0.0030(16) O10 0.019(2) 0.0166(19) 0.0231(19) -0.0032(15) -0.0031(16) 0.0014(16) O11 0.023(2) 0.0179(19) 0.0138(18) -0.0028(15) -0.0031(15) 0.0026(16) O12 0.030(2) 0.021(2) 0.0158(18) -0.0018(15) 0.0002(16) 0.0040(17) N1 0.016(3) 0.033(3) 0.034(3) -0.009(2) 0.000(2) -0.003(2) N2 0.031(3) 0.031(3) 0.024(3) -0.008(2) -0.001(2) 0.007(2) N3 0.021(3) 0.026(3) 0.036(3) 0.001(2) -0.002(2) -0.006(2) N4 0.029(3) 0.039(3) 0.035(3) -0.010(2) -0.012(2) 0.008(2) N5 0.039(3) 0.026(3) 0.031(3) -0.012(2) 0.009(2) -0.002(2) N6 0.051(4) 0.023(3) 0.033(3) -0.007(2) 0.014(3) -0.011(3) N7 0.024(3) 0.045(3) 0.026(3) -0.010(2) -0.007(2) 0.010(2) N8 0.030(3) 0.028(3) 0.028(3) -0.010(2) -0.004(2) 0.008(2) N9 0.026(3) 0.024(3) 0.046(3) -0.001(2) -0.004(2) -0.003(2) N10 0.019(3) 0.049(4) 0.037(3) -0.002(3) 0.003(2) -0.005(3) N11 0.033(3) 0.026(3) 0.029(3) -0.010(2) 0.007(2) 0.001(2) N12 0.047(3) 0.021(3) 0.029(3) 0.003(2) 0.006(2) 0.000(2) C1 0.017(3) 0.024(3) 0.017(3) -0.006(2) 0.000(2) 0.005(2) C2 0.018(3) 0.019(3) 0.029(3) 0.001(2) -0.003(2) 0.002(2) C3 0.024(3) 0.017(3) 0.011(2) -0.003(2) 0.001(2) 0.003(2) C4 0.021(3) 0.024(3) 0.020(3) -0.007(2) -0.003(2) 0.000(2) C5 0.020(3) 0.028(3) 0.026(3) -0.004(2) 0.003(2) 0.001(3) C6 0.014(3) 0.046(4) 0.033(3) -0.006(3) 0.000(3) -0.001(3) C7 0.019(3) 0.042(4) 0.050(4) -0.005(3) 0.000(3) 0.015(3) C8 0.024(3) 0.028(3) 0.045(4) -0.003(3) 0.001(3) 0.007(3) C9 0.016(3) 0.020(3) 0.022(3) -0.004(2) -0.001(2) 0.004(2) C10 0.018(3) 0.024(3) 0.021(3) 0.002(2) -0.001(2) 0.005(2) C11 0.030(4) 0.021(3) 0.036(3) 0.008(3) 0.003(3) -0.001(3) C12 0.035(4) 0.029(3) 0.026(3) 0.008(3) 0.002(3) 0.005(3) C13 0.019(3) 0.029(3) 0.023(3) 0.000(2) -0.004(2) 0.001(3) C14 0.021(3) 0.016(3) 0.016(3) -0.003(2) -0.001(2) 0.000(2) C15 0.028(3) 0.026(3) 0.023(3) -0.012(2) -0.004(2) 0.002(3) C16 0.021(3) 0.020(3) 0.013(3) 0.000(2) -0.002(2) -0.001(2) C17 0.026(3) 0.018(3) 0.018(3) 0.000(2) 0.002(2) -0.001(2) C18 0.027(3) 0.021(3) 0.020(3) -0.004(2) -0.001(2) 0.003(3) C19 0.039(4) 0.033(4) 0.033(3) -0.012(3) 0.008(3) 0.010(3) C20 0.026(4) 0.046(4) 0.045(4) -0.017(3) -0.002(3) 0.012(3) C21 0.025(3) 0.036(4) 0.031(3) -0.012(3) -0.001(3) 0.006(3) C22 0.022(3) 0.024(3) 0.018(3) -0.003(2) -0.003(2) 0.000(2) C23 0.027(3) 0.031(3) 0.027(3) -0.010(3) -0.007(3) 0.009(3) C24 0.026(3) 0.043(4) 0.037(4) -0.008(3) -0.011(3) 0.015(3) C25 0.036(4) 0.047(4) 0.029(3) -0.012(3) -0.005(3) 0.024(3) C26 0.034(4) 0.032(3) 0.021(3) -0.008(3) -0.007(3) 0.011(3) C27 0.021(3) 0.012(3) 0.019(3) -0.004(2) -0.006(2) 0.005(2) C28 0.023(3) 0.015(3) 0.025(3) -0.004(2) 0.005(2) -0.001(2) C29 0.015(3) 0.018(3) 0.019(3) -0.005(2) -0.004(2) 0.003(2) C30 0.020(3) 0.021(3) 0.019(3) 0.001(2) -0.001(2) 0.007(2) C31 0.026(3) 0.024(3) 0.023(3) -0.006(2) 0.004(2) -0.001(3) C32 0.040(4) 0.032(3) 0.022(3) -0.006(3) 0.007(3) 0.004(3) C33 0.027(3) 0.022(3) 0.027(3) -0.002(2) 0.008(2) -0.001(3) C34 0.029(3) 0.020(3) 0.023(3) -0.005(2) -0.002(2) 0.001(3) C35 0.016(3) 0.023(3) 0.021(3) 0.000(2) -0.001(2) 0.005(2) C36 0.033(3) 0.021(3) 0.023(3) -0.004(2) 0.007(3) -0.006(3) C37 0.046(4) 0.035(4) 0.037(4) 0.002(3) 0.021(3) -0.005(3) C38 0.044(4) 0.033(3) 0.024(3) -0.005(3) 0.011(3) 0.000(3) C39 0.029(3) 0.021(3) 0.024(3) -0.005(2) 0.003(2) 0.001(3) C40 0.021(3) 0.022(3) 0.018(3) 0.001(2) 0.000(2) 0.002(2) C41 0.019(3) 0.030(3) 0.028(3) -0.014(3) -0.010(2) 0.004(3) C42 0.024(3) 0.015(3) 0.019(3) 0.000(2) -0.001(2) 0.002(2) C43 0.020(3) 0.017(3) 0.025(3) 0.001(2) -0.002(2) 0.001(2) C44 0.025(3) 0.036(3) 0.023(3) -0.009(3) -0.004(2) 0.006(3) C45 0.023(3) 0.042(4) 0.035(3) -0.008(3) -0.007(3) 0.012(3) C46 0.028(4) 0.043(4) 0.029(3) -0.009(3) -0.004(3) 0.013(3) C47 0.029(3) 0.032(3) 0.022(3) -0.004(3) -0.005(2) 0.007(3) C48 0.022(3) 0.019(3) 0.019(3) -0.001(2) -0.001(2) 0.004(2) C49 0.027(3) 0.028(3) 0.021(3) -0.006(2) 0.001(2) 0.010(3) C50 0.042(4) 0.034(4) 0.030(3) -0.010(3) 0.007(3) 0.011(3) C51 0.023(3) 0.040(4) 0.042(4) -0.007(3) 0.001(3) 0.013(3) C52 0.024(3) 0.033(3) 0.026(3) -0.005(3) -0.003(3) 0.005(3) C53 0.022(3) 0.016(3) 0.017(3) -0.005(2) 0.000(2) -0.001(2) C54 0.022(3) 0.017(3) 0.027(3) 0.002(2) -0.001(2) 0.005(2) C55 0.020(3) 0.023(3) 0.017(3) -0.004(2) -0.004(2) 0.006(2) C56 0.017(3) 0.023(3) 0.024(3) -0.002(2) 0.002(2) 0.005(2) C57 0.020(3) 0.019(3) 0.034(3) 0.005(2) 0.000(2) 0.002(2) C58 0.032(4) 0.020(3) 0.046(4) 0.002(3) 0.009(3) -0.003(3) C59 0.035(4) 0.023(3) 0.031(3) 0.007(3) 0.011(3) 0.006(3) C60 0.027(3) 0.029(3) 0.024(3) -0.001(2) -0.001(2) 0.007(3) C61 0.019(3) 0.025(3) 0.019(3) 0.004(2) 0.000(2) 0.001(2) C62 0.018(3) 0.035(3) 0.028(3) -0.004(3) 0.004(2) 0.002(3) C63 0.018(3) 0.062(5) 0.038(4) 0.003(3) 0.003(3) 0.007(3) C64 0.024(4) 0.045(4) 0.058(5) 0.009(3) 0.004(3) 0.020(3) C65 0.026(4) 0.028(3) 0.049(4) 0.004(3) 0.000(3) 0.006(3) C66 0.019(3) 0.017(3) 0.019(3) -0.004(2) -0.007(2) 0.007(2) C67 0.031(3) 0.019(3) 0.023(3) -0.003(2) 0.006(2) 0.001(3) C68 0.022(3) 0.016(3) 0.016(3) -0.003(2) -0.004(2) 0.004(2) C69 0.016(3) 0.021(3) 0.019(3) 0.002(2) -0.002(2) 0.005(2) C70 0.028(3) 0.023(3) 0.025(3) -0.004(2) 0.008(3) -0.001(3) C71 0.034(4) 0.032(3) 0.028(3) -0.007(3) 0.010(3) 0.005(3) C72 0.026(3) 0.035(3) 0.028(3) -0.001(3) 0.007(3) 0.002(3) C73 0.024(3) 0.020(3) 0.025(3) -0.002(2) -0.001(2) 0.000(2) C74 0.024(3) 0.020(3) 0.017(3) 0.000(2) 0.000(2) 0.004(2) C75 0.037(4) 0.023(3) 0.022(3) -0.003(2) 0.007(3) 0.006(3) C76 0.042(4) 0.026(3) 0.024(3) 0.003(3) 0.007(3) -0.002(3) C77 0.036(4) 0.036(4) 0.019(3) -0.001(3) 0.009(3) 0.001(3) C78 0.037(4) 0.023(3) 0.025(3) -0.004(2) 0.002(3) 0.005(3) C79 0.057(5) 0.071(6) 0.035(4) 0.003(4) -0.002(4) 0.016(4) C80 0.078(6) 0.047(4) 0.034(4) 0.009(3) 0.002(4) 0.015(4) C81 0.039(4) 0.045(4) 0.038(4) -0.007(3) -0.001(3) -0.012(3) C82 0.034(4) 0.033(4) 0.040(4) 0.004(3) -0.006(3) 0.005(3) C83 0.059(5) 0.076(6) 0.053(5) 0.012(4) 0.011(4) 0.026(5) C84 0.055(5) 0.042(4) 0.038(4) 0.004(3) 0.011(3) 0.018(4) C85 0.098(7) 0.055(5) 0.040(4) 0.004(4) 0.003(5) 0.003(5) C86 0.051(5) 0.053(5) 0.054(5) 0.006(4) -0.009(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C79 1.736(9) . ? Cl2 C79 1.760(8) . ? Cl3 C79 1.726(9) . ? Cl4 C80 1.727(8) . ? Cl5 C80 1.769(9) . ? Cl6 C80 1.751(8) . ? Cl7 C81 1.759(7) . ? Cl8 C81 1.725(8) . ? Cl9 C81 1.725(8) . ? Cl10 C82 1.754(7) . ? Cl11 C82 1.769(7) . ? Cl12 C82 1.745(7) . ? Cl13 C83 1.746(9) . ? Cl14 C83 1.713(9) . ? Cl15 C83 1.689(10) . ? Cl16 C84 1.761(8) . ? Cl17 C84 1.761(8) . ? Cl18 C84 1.743(8) . ? Cl19 C85 1.688(10) . ? Cl20 C85 1.743(10) . ? Cl21 C85 1.689(9) . ? Cl22 C86 1.740(9) . ? Cl23 C86 1.733(8) . ? Cl24 C86 1.784(9) . ? Al1 O6 1.868(4) . ? Al1 O4 1.874(4) . ? Al1 O3 1.885(4) . ? Al1 O2 1.885(4) . ? Al1 O5 1.886(4) . ? Al1 O1 1.892(4) . ? Al2 O12 1.871(4) . ? Al2 O7 1.876(4) . ? Al2 O11 1.885(4) . ? Al2 O9 1.888(4) . ? Al2 O8 1.894(4) . ? Al2 O10 1.894(4) . ? O1 C1 1.274(7) . ? O2 C3 1.291(6) . ? O3 C14 1.274(6) . ? O4 C16 1.272(6) . ? O5 C27 1.289(6) . ? O6 C29 1.274(6) . ? O7 C40 1.278(6) . ? O8 C42 1.280(6) . ? O9 C53 1.276(7) . ? O10 C55 1.271(7) . ? O11 C66 1.294(6) . ? O12 C68 1.278(6) . ? N1 C5 1.336(7) . ? N1 C6 1.348(8) . ? N2 C18 1.332(7) . ? N2 C19 1.332(8) . ? N3 C10 1.338(7) . ? N3 C11 1.340(8) . ? N4 C23 1.331(8) . ? N4 C24 1.347(8) . ? N5 C32 1.334(8) . ? N5 C31 1.335(7) . ? N6 C36 1.332(8) . ? N6 C37 1.336(8) . ? N7 C45 1.337(8) . ? N7 C44 1.337(8) . ? N8 C50 1.330(8) . ? N8 C49 1.332(7) . ? N9 C58 1.328(8) . ? N9 C57 1.336(7) . ? N10 C63 1.326(9) . ? N10 C62 1.341(8) . ? N11 C70 1.335(7) . ? N11 C71 1.337(8) . ? N12 C76 1.327(8) . ? N12 C75 1.343(8) . ? C1 C2 1.404(8) . ? C1 C4 1.493(8) . ? C2 C3 1.377(8) . ? C3 C9 1.495(8) . ? C4 C8 1.384(8) . ? C4 C5 1.392(8) . ? C6 C7 1.371(9) . ? C7 C8 1.390(9) . ? C9 C10 1.391(8) . ? C9 C13 1.394(8) . ? C11 C12 1.373(9) . ? C12 C13 1.384(8) . ? C14 C15 1.397(8) . ? C14 C17 1.486(7) . ? C15 C16 1.396(8) . ? C16 C22 1.497(8) . ? C17 C21 1.388(9) . ? C17 C18 1.397(8) . ? C19 C20 1.397(9) . ? C20 C21 1.386(8) . ? C22 C26 1.382(8) . ? C22 C23 1.402(8) . ? C24 C25 1.380(9) . ? C25 C26 1.380(9) . ? C27 C28 1.381(8) . ? C27 C30 1.495(7) . ? C28 C29 1.407(7) . ? C29 C35 1.492(8) . ? C30 C34 1.393(8) . ? C30 C31 1.397(8) . ? C32 C33 1.385(8) . ? C33 C34 1.380(8) . ? C35 C39 1.385(8) . ? C35 C36 1.390(8) . ? C37 C38 1.391(9) . ? C38 C39 1.385(8) . ? C40 C41 1.391(8) . ? C40 C43 1.488(8) . ? C41 C42 1.390(8) . ? C42 C48 1.492(7) . ? C43 C47 1.384(8) . ? C43 C44 1.399(8) . ? C45 C46 1.383(9) . ? C46 C47 1.390(9) . ? C48 C52 1.375(8) . ? C48 C49 1.399(8) . ? C50 C51 1.396(9) . ? C51 C52 1.382(8) . ? C53 C54 1.386(8) . ? C53 C56 1.502(8) . ? C54 C55 1.400(8) . ? C55 C61 1.492(8) . ? C56 C60 1.378(8) . ? C56 C57 1.386(8) . ? C58 C59 1.371(9) . ? C59 C60 1.396(9) . ? C61 C65 1.382(8) . ? C61 C62 1.397(8) . ? C63 C64 1.369(10) . ? C64 C65 1.388(9) . ? C66 C67 1.400(8) . ? C66 C69 1.487(7) . ? C67 C68 1.397(8) . ? C68 C74 1.480(8) . ? C69 C73 1.388(8) . ? C69 C70 1.398(8) . ? C71 C72 1.379(9) . ? C72 C73 1.387(8) . ? C74 C75 1.388(8) . ? C74 C78 1.394(8) . ? C76 C77 1.388(9) . ? C77 C78 1.379(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 O6 Al1 O4 91.59(18) . . ? O6 Al1 O3 89.62(17) . . ? O4 Al1 O3 91.42(17) . . ? O6 Al1 O2 177.10(19) . . ? O4 Al1 O2 91.24(18) . . ? O3 Al1 O2 89.64(17) . . ? O6 Al1 O5 91.06(17) . . ? O4 Al1 O5 89.68(17) . . ? O3 Al1 O5 178.70(19) . . ? O2 Al1 O5 89.63(17) . . ? O6 Al1 O1 87.23(18) . . ? O4 Al1 O1 178.8(2) . . ? O3 Al1 O1 88.52(17) . . ? O2 Al1 O1 89.94(17) . . ? O5 Al1 O1 90.41(17) . . ? O12 Al2 O7 91.86(18) . . ? O12 Al2 O11 91.41(17) . . ? O7 Al2 O11 88.38(17) . . ? O12 Al2 O9 177.75(19) . . ? O7 Al2 O9 89.52(18) . . ? O11 Al2 O9 90.41(17) . . ? O12 Al2 O8 88.20(17) . . ? O7 Al2 O8 91.41(17) . . ? O11 Al2 O8 179.54(19) . . ? O9 Al2 O8 90.00(17) . . ? O12 Al2 O10 88.44(18) . . ? O7 Al2 O10 179.62(19) . . ? O11 Al2 O10 91.85(17) . . ? O9 Al2 O10 90.17(17) . . ? O8 Al2 O10 88.36(17) . . ? C1 O1 Al1 127.1(3) . . ? C3 O2 Al1 126.3(3) . . ? C14 O3 Al1 128.3(4) . . ? C16 O4 Al1 128.7(4) . . ? C27 O5 Al1 127.8(3) . . ? C29 O6 Al1 129.5(3) . . ? C40 O7 Al2 128.4(4) . . ? C42 O8 Al2 128.0(4) . . ? C53 O9 Al2 127.1(3) . . ? C55 O10 Al2 127.2(3) . . ? C66 O11 Al2 128.3(3) . . ? C68 O12 Al2 130.1(3) . . ? C5 N1 C6 116.4(5) . . ? C18 N2 C19 117.3(5) . . ? C10 N3 C11 117.4(5) . . ? C23 N4 C24 116.1(5) . . ? C32 N5 C31 117.2(5) . . ? C36 N6 C37 118.0(5) . . ? C45 N7 C44 117.0(5) . . ? C50 N8 C49 116.8(5) . . ? C58 N9 C57 116.8(5) . . ? C63 N10 C62 117.5(6) . . ? C70 N11 C71 116.9(5) . . ? C76 N12 C75 117.3(5) . . ? O1 C1 C2 123.5(5) . . ? O1 C1 C4 115.9(5) . . ? C2 C1 C4 120.6(5) . . ? C3 C2 C1 122.4(5) . . ? O2 C3 C2 124.5(5) . . ? O2 C3 C9 114.8(5) . . ? C2 C3 C9 120.7(5) . . ? C8 C4 C5 118.0(5) . . ? C8 C4 C1 123.0(5) . . ? C5 C4 C1 118.9(5) . . ? N1 C5 C4 124.2(6) . . ? N1 C6 C7 123.7(6) . . ? C6 C7 C8 119.0(6) . . ? C4 C8 C7 118.7(6) . . ? C10 C9 C13 117.9(5) . . ? C10 C9 C3 119.0(5) . . ? C13 C9 C3 123.1(5) . . ? N3 C10 C9 123.7(5) . . ? N3 C11 C12 123.0(6) . . ? C11 C12 C13 119.7(6) . . ? C12 C13 C9 118.3(5) . . ? O3 C14 C15 123.5(5) . . ? O3 C14 C17 116.4(5) . . ? C15 C14 C17 120.1(5) . . ? C16 C15 C14 123.0(5) . . ? O4 C16 C15 123.8(5) . . ? O4 C16 C22 115.7(5) . . ? C15 C16 C22 120.5(5) . . ? C21 C17 C18 117.1(5) . . ? C21 C17 C14 120.3(5) . . ? C18 C17 C14 122.6(5) . . ? N2 C18 C17 124.3(6) . . ? N2 C19 C20 123.5(6) . . ? C21 C20 C19 117.9(6) . . ? C20 C21 C17 119.9(6) . . ? C26 C22 C23 116.7(5) . . ? C26 C22 C16 120.2(5) . . ? C23 C22 C16 123.1(5) . . ? N4 C23 C22 125.0(6) . . ? N4 C24 C25 123.7(6) . . ? C24 C25 C26 118.6(6) . . ? C25 C26 C22 119.8(5) . . ? O5 C27 C28 124.2(5) . . ? O5 C27 C30 114.9(5) . . ? C28 C27 C30 120.8(5) . . ? C27 C28 C29 122.8(5) . . ? O6 C29 C28 123.2(5) . . ? O6 C29 C35 115.2(4) . . ? C28 C29 C35 121.6(5) . . ? C34 C30 C31 117.3(5) . . ? C34 C30 C27 120.4(5) . . ? C31 C30 C27 122.3(5) . . ? N5 C31 C30 124.0(5) . . ? N5 C32 C33 123.5(5) . . ? C34 C33 C32 118.7(5) . . ? C33 C34 C30 119.3(5) . . ? C39 C35 C36 118.2(5) . . ? C39 C35 C29 119.8(5) . . ? C36 C35 C29 122.0(5) . . ? N6 C36 C35 123.3(5) . . ? N6 C37 C38 122.8(6) . . ? C39 C38 C37 118.6(5) . . ? C38 C39 C35 119.1(5) . . ? O7 C40 C41 123.7(5) . . ? O7 C40 C43 116.0(5) . . ? C41 C40 C43 120.3(5) . . ? C42 C41 C40 123.6(5) . . ? O8 C42 C41 123.5(5) . . ? O8 C42 C48 115.5(5) . . ? C41 C42 C48 121.0(5) . . ? C47 C43 C44 117.4(5) . . ? C47 C43 C40 119.7(5) . . ? C44 C43 C40 122.9(5) . . ? N7 C44 C43 124.1(5) . . ? N7 C45 C46 123.6(6) . . ? C45 C46 C47 118.5(6) . . ? C43 C47 C46 119.4(5) . . ? C52 C48 C49 117.2(5) . . ? C52 C48 C42 121.2(5) . . ? C49 C48 C42 121.6(5) . . ? N8 C49 C48 124.5(6) . . ? N8 C50 C51 123.5(6) . . ? C52 C51 C50 118.2(6) . . ? C48 C52 C51 119.8(6) . . ? O9 C53 C54 124.7(5) . . ? O9 C53 C56 115.4(5) . . ? C54 C53 C56 119.9(5) . . ? C53 C54 C55 122.2(5) . . ? O10 C55 C54 123.9(5) . . ? O10 C55 C61 116.8(5) . . ? C54 C55 C61 119.2(5) . . ? C60 C56 C57 118.8(5) . . ? C60 C56 C53 123.2(5) . . ? C57 C56 C53 117.9(5) . . ? N9 C57 C56 123.6(6) . . ? N9 C58 C59 124.2(6) . . ? C58 C59 C60 118.7(6) . . ? C56 C60 C59 117.9(6) . . ? C65 C61 C62 117.8(5) . . ? C65 C61 C55 122.2(5) . . ? C62 C61 C55 120.0(5) . . ? N10 C62 C61 123.4(6) . . ? N10 C63 C64 123.2(6) . . ? C63 C64 C65 119.6(6) . . ? C61 C65 C64 118.5(6) . . ? O11 C66 C67 123.9(5) . . ? O11 C66 C69 115.7(5) . . ? C67 C66 C69 120.4(5) . . ? C68 C67 C66 123.2(5) . . ? O12 C68 C67 123.1(5) . . ? O12 C68 C74 115.5(5) . . ? C67 C68 C74 121.4(5) . . ? C73 C69 C70 117.8(5) . . ? C73 C69 C66 120.7(5) . . ? C70 C69 C66 121.5(5) . . ? N11 C70 C69 124.1(5) . . ? N11 C71 C72 123.5(5) . . ? C71 C72 C73 119.3(6) . . ? C72 C73 C69 118.4(5) . . ? C75 C74 C78 117.5(5) . . ? C75 C74 C68 122.9(5) . . ? C78 C74 C68 119.6(5) . . ? N12 C75 C74 123.8(5) . . ? N12 C76 C77 123.5(5) . . ? C78 C77 C76 118.7(5) . . ? C77 C78 C74 119.2(5) . . ? Cl3 C79 Cl1 111.4(5) . . ? Cl3 C79 Cl2 110.7(4) . . ? Cl1 C79 Cl2 110.3(5) . . ? Cl4 C80 Cl6 113.3(4) . . ? Cl4 C80 Cl5 113.9(5) . . ? Cl6 C80 Cl5 111.4(4) . . ? Cl8 C81 Cl9 113.5(5) . . ? Cl8 C81 Cl7 110.9(4) . . ? Cl9 C81 Cl7 111.8(4) . . ? Cl12 C82 Cl10 110.9(4) . . ? Cl12 C82 Cl11 110.2(4) . . ? Cl10 C82 Cl11 109.7(4) . . ? Cl15 C83 Cl14 108.8(6) . . ? Cl15 C83 Cl13 111.0(5) . . ? Cl14 C83 Cl13 111.7(5) . . ? Cl18 C84 Cl17 111.6(5) . . ? Cl18 C84 Cl16 110.3(4) . . ? Cl17 C84 Cl16 110.2(4) . . ? Cl19 C85 Cl21 120.3(7) . . ? Cl19 C85 Cl20 112.3(5) . . ? Cl21 C85 Cl20 109.1(5) . . ? Cl23 C86 Cl22 113.0(5) . . ? Cl23 C86 Cl24 108.8(5) . . ? Cl22 C86 Cl24 105.4(5) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 2.788 _refine_diff_density_min -2.172 _refine_diff_density_rms 0.193 #===end data_compound5_k08clr1 _database_code_depnum_ccdc_archive 'CCDC 853058' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Cu N4 O5 S' _chemical_formula_weight 592.11 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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.5630(4) _cell_length_b 11.4730(3) _cell_length_c 16.3770(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.2890(10) _cell_angle_gamma 90.00 _cell_volume 2692.29(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 121216 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Yellow-green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51590 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6155 _reflns_number_gt 3620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0974P)^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 6155 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1697 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 Cu1 Cu 0.26412(3) -0.00035(3) 0.16657(3) 0.02370(16) Uani 1 1 d . . . S1 S -0.03763(10) -0.20628(12) 0.50274(10) 0.0664(4) Uani 1 1 d . . . O1 O 0.24446(16) -0.02178(19) 0.04650(15) 0.0261(6) Uani 1 1 d . . . O2 O 0.37254(16) 0.1018(2) 0.16677(15) 0.0271(6) Uani 1 1 d . . . O3 O 0.28600(17) 0.01748(19) 0.28717(16) 0.0279(6) Uani 1 1 d . . . O4 O 0.15472(16) -0.1009(2) 0.16496(15) 0.0284(6) Uani 1 1 d . . . N1 N 0.1919(2) -0.0501(3) -0.2604(2) 0.0431(9) Uani 1 1 d . . . N2 N 0.6500(2) 0.3454(3) 0.1479(2) 0.0306(7) Uani 1 1 d . . . N3 N 0.3718(3) -0.0123(3) 0.5957(2) 0.0566(11) Uani 1 1 d . . . N4 N -0.1203(2) -0.3468(3) 0.1880(2) 0.0303(7) Uani 1 1 d . . . C1 C 0.2973(3) 0.0165(3) -0.0018(2) 0.0274(8) Uani 1 1 d . . . C2 C 0.2645(3) -0.0075(3) -0.0921(2) 0.0278(8) Uani 1 1 d . . . C3 C 0.2013(3) -0.0973(3) -0.1168(2) 0.0341(9) Uani 1 1 d . . . H3 H 0.1817 -0.1464 -0.0765 0.041 Uiso 1 1 calc R . . C4 C 0.1680(3) -0.1146(3) -0.1985(3) 0.0403(10) Uani 1 1 d . . . H4A H 0.1248 -0.1764 -0.2133 0.048 Uiso 1 1 calc R . . C5 C 0.2523(3) 0.0346(4) -0.2364(3) 0.0469(11) Uani 1 1 d . . . H5 H 0.2711 0.0815 -0.2783 0.056 Uiso 1 1 calc R . . C6 C 0.2901(3) 0.0601(4) -0.1551(2) 0.0384(10) Uani 1 1 d . . . H6 H 0.3330 0.1227 -0.1422 0.046 Uiso 1 1 calc R . . C7 C 0.3791(3) 0.0809(3) 0.0228(2) 0.0335(9) Uani 1 1 d . . . H7 H 0.4160 0.0984 -0.0179 0.040 Uiso 1 1 calc R . . C8 C 0.4101(2) 0.1212(3) 0.1038(2) 0.0260(8) Uani 1 1 d . . . C9 C 0.4954(2) 0.1975(3) 0.1193(2) 0.0290(8) Uani 1 1 d . . . C10 C 0.5112(3) 0.2788(3) 0.0598(2) 0.0354(9) Uani 1 1 d . . . H10 H 0.4700 0.2844 0.0080 0.042 Uiso 1 1 calc R . . C11 C 0.5888(3) 0.3513(3) 0.0783(3) 0.0366(9) Uani 1 1 d . . . H11 H 0.5981 0.4083 0.0384 0.044 Uiso 1 1 calc R . . C12 C 0.6344(2) 0.2673(3) 0.2047(2) 0.0314(9) Uani 1 1 d . . . H12 H 0.6776 0.2628 0.2555 0.038 Uiso 1 1 calc R . . C13 C 0.5582(2) 0.1931(3) 0.1932(2) 0.0312(9) Uani 1 1 d . . . H13 H 0.5493 0.1398 0.2354 0.037 Uiso 1 1 calc R . . C14 C 0.2451(2) -0.0410(3) 0.3368(2) 0.0290(8) Uani 1 1 d . . . C15 C 0.2865(3) -0.0307(3) 0.4271(2) 0.0345(9) Uani 1 1 d . . . C16 C 0.3607(3) 0.0437(4) 0.4523(3) 0.0482(11) Uani 1 1 d . . . H16 H 0.3840 0.0903 0.4126 0.058 Uiso 1 1 calc R . . C17 C 0.40096(17) 0.0504(2) 0.53518(16) 0.0617(14) Uani 1 1 d . . . H17 H 0.4521 0.1020 0.5506 0.074 Uiso 1 1 calc R . . O5 O 0.04468(17) -0.1685(2) 0.47410(16) 0.0727(11) Uani 1 1 d R . . C28 C -0.04671(17) -0.1216(2) 0.59249(16) 0.0876(19) Uani 1 1 d R . . H28A H 0.0081 -0.1357 0.6356 0.131 Uiso 1 1 calc R . . H28B H -0.1033 -0.1440 0.6133 0.131 Uiso 1 1 calc R . . H28C H -0.0499 -0.0387 0.5778 0.131 Uiso 1 1 calc R . . C27 C -0.13452(17) -0.1479(2) 0.43309(16) 0.095(2) Uani 1 1 d R . . H27A H -0.1281 -0.0631 0.4302 0.142 Uiso 1 1 calc R . . H27B H -0.1923 -0.1670 0.4529 0.142 Uiso 1 1 calc R . . H27C H -0.1365 -0.1815 0.3778 0.142 Uiso 1 1 calc R . . C18 C 0.3015(3) -0.0841(4) 0.5711(3) 0.0532(12) Uani 1 1 d . . . H18 H 0.2797 -0.1298 0.6121 0.064 Uiso 1 1 calc R . . C19 C 0.2571(3) -0.0972(4) 0.4892(3) 0.0473(11) Uani 1 1 d . . . H19 H 0.2071 -0.1509 0.4755 0.057 Uiso 1 1 calc R . . C20 C 0.1678(3) -0.1116(3) 0.3124(2) 0.0339(9) Uani 1 1 d . . . H20 H 0.1408 -0.1472 0.3548 0.041 Uiso 1 1 calc R . . C21 C 0.1264(2) -0.1344(3) 0.2298(2) 0.0256(8) Uani 1 1 d . . . C22 C 0.0397(2) -0.2077(3) 0.2157(2) 0.0248(8) Uani 1 1 d . . . C23 C 0.0308(2) -0.3027(3) 0.2665(2) 0.0306(8) Uani 1 1 d . . . H23 H 0.0790 -0.3216 0.3116 0.037 Uiso 1 1 calc R . . C24 C -0.0499(2) -0.3694(3) 0.2500(2) 0.0317(9) Uani 1 1 d . . . H24 H -0.0553 -0.4346 0.2846 0.038 Uiso 1 1 calc R . . C25 C -0.1112(2) -0.2562(3) 0.1394(2) 0.0324(9) Uani 1 1 d . . . H25 H -0.1606 -0.2399 0.0946 0.039 Uiso 1 1 calc R . . C26 C -0.0338(2) -0.1843(3) 0.1505(2) 0.0296(8) Uani 1 1 d . . . H26 H -0.0307 -0.1202 0.1144 0.035 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 Cu1 0.0202(2) 0.0268(2) 0.0247(3) 0.00051(18) 0.00553(17) -0.00218(16) S1 0.0619(8) 0.0597(8) 0.0811(11) 0.0045(7) 0.0219(7) 0.0032(7) O1 0.0224(13) 0.0306(13) 0.0271(14) 0.0003(10) 0.0092(11) -0.0058(10) O2 0.0237(13) 0.0307(13) 0.0276(15) 0.0015(11) 0.0061(11) -0.0018(10) O3 0.0229(13) 0.0314(14) 0.0298(15) -0.0010(11) 0.0059(11) -0.0032(10) O4 0.0240(13) 0.0331(13) 0.0287(15) 0.0035(11) 0.0064(11) -0.0014(11) N1 0.051(2) 0.050(2) 0.028(2) -0.0013(16) 0.0064(17) -0.0085(18) N2 0.0236(16) 0.0359(17) 0.0325(19) -0.0007(14) 0.0053(14) -0.0038(13) N3 0.057(3) 0.078(3) 0.034(2) -0.010(2) 0.0070(19) -0.017(2) N4 0.0278(17) 0.0308(17) 0.0314(19) 0.0017(13) 0.0030(14) 0.0001(13) C1 0.0266(19) 0.0284(19) 0.028(2) -0.0001(15) 0.0083(16) 0.0039(15) C2 0.0258(19) 0.0279(19) 0.030(2) 0.0007(16) 0.0071(16) -0.0007(15) C3 0.035(2) 0.035(2) 0.032(2) -0.0003(17) 0.0058(18) -0.0074(17) C4 0.043(2) 0.039(2) 0.038(3) -0.0033(19) 0.004(2) -0.0137(18) C5 0.055(3) 0.055(3) 0.033(3) 0.006(2) 0.012(2) -0.015(2) C6 0.042(2) 0.043(2) 0.031(2) -0.0012(18) 0.0096(19) -0.0151(18) C7 0.031(2) 0.042(2) 0.030(2) -0.0059(17) 0.0122(17) -0.0098(17) C8 0.0208(18) 0.0243(18) 0.034(2) 0.0016(15) 0.0066(16) -0.0034(14) C9 0.0226(19) 0.0302(19) 0.035(2) -0.0042(16) 0.0070(17) -0.0044(15) C10 0.030(2) 0.046(2) 0.029(2) 0.0017(17) 0.0024(17) -0.0085(17) C11 0.031(2) 0.041(2) 0.037(2) 0.0071(18) 0.0034(19) -0.0096(17) C12 0.026(2) 0.035(2) 0.032(2) 0.0006(17) 0.0037(16) -0.0019(16) C13 0.033(2) 0.0271(19) 0.036(2) 0.0050(16) 0.0125(18) -0.0028(15) C14 0.028(2) 0.0334(18) 0.027(2) -0.0030(16) 0.0090(17) 0.0000(16) C15 0.032(2) 0.042(2) 0.030(2) -0.0072(17) 0.0088(18) -0.0087(17) C16 0.050(3) 0.063(3) 0.033(3) -0.007(2) 0.010(2) -0.024(2) C17 0.065(3) 0.085(3) 0.034(3) -0.009(2) 0.005(2) -0.040(3) O5 0.064(2) 0.073(2) 0.087(3) -0.003(2) 0.030(2) -0.0053(18) C28 0.106(5) 0.088(4) 0.077(4) -0.008(3) 0.039(4) -0.001(4) C27 0.089(5) 0.089(4) 0.103(6) 0.006(4) 0.009(4) 0.014(4) C18 0.058(3) 0.068(3) 0.033(3) 0.001(2) 0.005(2) -0.013(3) C19 0.043(3) 0.062(3) 0.036(3) -0.001(2) 0.005(2) -0.015(2) C20 0.036(2) 0.044(2) 0.024(2) -0.0041(17) 0.0106(17) -0.0112(18) C21 0.0235(19) 0.0245(18) 0.030(2) -0.0001(15) 0.0080(16) -0.0007(14) C22 0.0218(18) 0.0267(18) 0.028(2) -0.0032(15) 0.0101(16) -0.0013(14) C23 0.0262(19) 0.034(2) 0.029(2) 0.0054(16) -0.0010(16) -0.0017(16) C24 0.032(2) 0.030(2) 0.034(2) 0.0072(16) 0.0062(18) -0.0043(15) C25 0.0255(19) 0.033(2) 0.036(2) 0.0014(17) -0.0015(17) -0.0014(16) C26 0.028(2) 0.0283(19) 0.032(2) 0.0033(16) 0.0041(16) -0.0024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.951(2) . ? Cu1 O3 1.954(3) . ? Cu1 O4 1.963(2) . ? Cu1 O2 1.966(2) . ? Cu1 N4 2.413(3) 4_655 ? Cu1 N2 2.415(3) 4_565 ? S1 O5 1.430(3) . ? S1 C27 1.779(3) . ? S1 C28 1.786(3) . ? O1 C1 1.276(4) . ? O2 C8 1.270(4) . ? O3 C14 1.280(4) . ? O4 C21 1.266(4) . ? N1 C5 1.323(5) . ? N1 C4 1.351(5) . ? N2 C11 1.317(5) . ? N2 C12 1.341(5) . ? N2 Cu1 2.415(3) 4_665 ? N3 C18 1.320(6) . ? N3 C17 1.353(5) . ? N4 C25 1.330(5) . ? N4 C24 1.333(5) . ? N4 Cu1 2.413(3) 4 ? C1 C7 1.398(5) . ? C1 C2 1.496(5) . ? C2 C6 1.393(5) . ? C2 C3 1.393(5) . ? C3 C4 1.354(5) . ? C3 H3 0.9500 . ? C4 H4A 0.9500 . ? C5 C6 1.378(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.400(5) . ? C7 H7 0.9500 . ? C8 C9 1.504(4) . ? C9 C13 1.381(5) . ? C9 C10 1.396(5) . ? C10 C11 1.392(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.384(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C20 1.387(5) . ? C14 C15 1.499(5) . ? C15 C16 1.381(6) . ? C15 C19 1.398(6) . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C18 C19 1.389(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.404(5) . ? C20 H20 0.9500 . ? C21 C22 1.500(4) . ? C22 C23 1.392(5) . ? C22 C26 1.397(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? 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 O1 Cu1 O3 178.48(10) . . ? O1 Cu1 O4 86.55(10) . . ? O3 Cu1 O4 93.47(10) . . ? O1 Cu1 O2 92.87(10) . . ? O3 Cu1 O2 87.13(10) . . ? O4 Cu1 O2 179.09(10) . . ? O1 Cu1 N4 91.59(10) . 4_655 ? O3 Cu1 N4 86.89(10) . 4_655 ? O4 Cu1 N4 96.81(10) . 4_655 ? O2 Cu1 N4 83.91(10) . 4_655 ? O1 Cu1 N2 89.49(10) . 4_565 ? O3 Cu1 N2 92.03(10) . 4_565 ? O4 Cu1 N2 83.83(10) . 4_565 ? O2 Cu1 N2 95.47(10) . 4_565 ? N4 Cu1 N2 178.78(11) 4_655 4_565 ? O5 S1 C27 106.91(17) . . ? O5 S1 C28 107.15(17) . . ? C27 S1 C28 98.99(14) . . ? C1 O1 Cu1 125.8(2) . . ? C8 O2 Cu1 124.4(2) . . ? C14 O3 Cu1 125.2(2) . . ? C21 O4 Cu1 123.5(2) . . ? C5 N1 C4 115.2(4) . . ? C11 N2 C12 117.5(3) . . ? C11 N2 Cu1 114.6(2) . 4_665 ? C12 N2 Cu1 127.0(2) . 4_665 ? C18 N3 C17 115.8(4) . . ? C25 N4 C24 117.6(3) . . ? C25 N4 Cu1 128.5(2) . 4 ? C24 N4 Cu1 113.0(2) . 4 ? O1 C1 C7 125.4(3) . . ? O1 C1 C2 115.4(3) . . ? C7 C1 C2 119.2(3) . . ? C6 C2 C3 116.5(4) . . ? C6 C2 C1 123.3(3) . . ? C3 C2 C1 120.1(3) . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? N1 C4 C3 124.5(4) . . ? N1 C4 H4A 117.7 . . ? C3 C4 H4A 117.7 . . ? N1 C5 C6 125.0(4) . . ? N1 C5 H5 117.5 . . ? C6 C5 H5 117.5 . . ? C5 C6 C2 118.9(4) . . ? C5 C6 H6 120.5 . . ? C2 C6 H6 120.5 . . ? C1 C7 C8 124.2(3) . . ? C1 C7 H7 117.9 . . ? C8 C7 H7 117.9 . . ? O2 C8 C7 126.7(3) . . ? O2 C8 C9 115.3(3) . . ? C7 C8 C9 117.9(3) . . ? C13 C9 C10 118.0(3) . . ? C13 C9 C8 121.6(3) . . ? C10 C9 C8 120.4(3) . . ? C11 C10 C9 118.5(4) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N2 C11 C10 123.7(4) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N2 C12 C13 123.2(3) . . ? N2 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C9 C13 C12 119.1(3) . . ? C9 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? O3 C14 C20 124.6(3) . . ? O3 C14 C15 115.8(3) . . ? C20 C14 C15 119.6(3) . . ? C16 C15 C19 116.5(4) . . ? C16 C15 C14 119.9(4) . . ? C19 C15 C14 123.6(3) . . ? C15 C16 C17 119.9(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? N3 C17 C16 123.9(3) . . ? N3 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C18 C19 124.4(4) . . ? N3 C18 H18 117.8 . . ? C19 C18 H18 117.8 . . ? C18 C19 C15 119.5(4) . . ? C18 C19 H19 120.3 . . ? C15 C19 H19 120.3 . . ? C14 C20 C21 125.0(3) . . ? C14 C20 H20 117.5 . . ? C21 C20 H20 117.5 . . ? O4 C21 C20 127.1(3) . . ? O4 C21 C22 115.6(3) . . ? C20 C21 C22 117.3(3) . . ? C23 C22 C26 117.8(3) . . ? C23 C22 C21 120.9(3) . . ? C26 C22 C21 121.3(3) . . ? C24 C23 C22 118.9(3) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? N4 C24 C23 123.3(3) . . ? N4 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? N4 C25 C26 123.6(3) . . ? N4 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C22 118.8(3) . . ? C25 C26 H26 120.6 . . ? C22 C26 H26 120.6 . . ? 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 O3 Cu1 O1 C1 -85(4) . . . . ? O4 Cu1 O1 C1 -175.5(3) . . . . ? O2 Cu1 O1 C1 5.2(3) . . . . ? N4 Cu1 O1 C1 -78.7(3) 4_655 . . . ? N2 Cu1 O1 C1 100.7(3) 4_565 . . . ? O1 Cu1 O2 C8 -7.3(3) . . . . ? O3 Cu1 O2 C8 171.2(3) . . . . ? O4 Cu1 O2 C8 -58(7) . . . . ? N4 Cu1 O2 C8 84.0(3) 4_655 . . . ? N2 Cu1 O2 C8 -97.1(3) 4_565 . . . ? O1 Cu1 O3 C14 -80(4) . . . . ? O4 Cu1 O3 C14 10.2(3) . . . . ? O2 Cu1 O3 C14 -170.5(3) . . . . ? N4 Cu1 O3 C14 -86.5(3) 4_655 . . . ? N2 Cu1 O3 C14 94.1(3) 4_565 . . . ? O1 Cu1 O4 C21 175.4(3) . . . . ? O3 Cu1 O4 C21 -3.1(3) . . . . ? O2 Cu1 O4 C21 -134(6) . . . . ? N4 Cu1 O4 C21 84.2(3) 4_655 . . . ? N2 Cu1 O4 C21 -94.8(3) 4_565 . . . ? Cu1 O1 C1 C7 0.1(5) . . . . ? Cu1 O1 C1 C2 -177.5(2) . . . . ? O1 C1 C2 C6 155.3(3) . . . . ? C7 C1 C2 C6 -22.4(5) . . . . ? O1 C1 C2 C3 -21.2(5) . . . . ? C7 C1 C2 C3 161.1(3) . . . . ? C6 C2 C3 C4 -0.3(6) . . . . ? C1 C2 C3 C4 176.4(3) . . . . ? C5 N1 C4 C3 0.0(6) . . . . ? C2 C3 C4 N1 0.3(6) . . . . ? C4 N1 C5 C6 -0.4(7) . . . . ? N1 C5 C6 C2 0.4(7) . . . . ? C3 C2 C6 C5 0.0(6) . . . . ? C1 C2 C6 C5 -176.6(4) . . . . ? O1 C1 C7 C8 -5.9(6) . . . . ? C2 C1 C7 C8 171.6(3) . . . . ? Cu1 O2 C8 C7 4.4(5) . . . . ? Cu1 O2 C8 C9 -177.0(2) . . . . ? C1 C7 C8 O2 3.4(6) . . . . ? C1 C7 C8 C9 -175.2(3) . . . . ? O2 C8 C9 C13 35.4(5) . . . . ? C7 C8 C9 C13 -145.9(4) . . . . ? O2 C8 C9 C10 -142.0(3) . . . . ? C7 C8 C9 C10 36.7(5) . . . . ? C13 C9 C10 C11 -0.4(5) . . . . ? C8 C9 C10 C11 177.1(3) . . . . ? C12 N2 C11 C10 -2.3(6) . . . . ? Cu1 N2 C11 C10 -172.4(3) 4_665 . . . ? C9 C10 C11 N2 2.1(6) . . . . ? C11 N2 C12 C13 0.7(5) . . . . ? Cu1 N2 C12 C13 169.5(3) 4_665 . . . ? C10 C9 C13 C12 -1.0(5) . . . . ? C8 C9 C13 C12 -178.5(3) . . . . ? N2 C12 C13 C9 0.9(5) . . . . ? Cu1 O3 C14 C20 -11.7(5) . . . . ? Cu1 O3 C14 C15 167.8(2) . . . . ? O3 C14 C15 C16 3.6(6) . . . . ? C20 C14 C15 C16 -176.9(4) . . . . ? O3 C14 C15 C19 -173.3(4) . . . . ? C20 C14 C15 C19 6.2(6) . . . . ? C19 C15 C16 C17 -0.7(6) . . . . ? C14 C15 C16 C17 -177.8(4) . . . . ? C18 N3 C17 C16 1.0(6) . . . . ? C15 C16 C17 N3 -0.4(6) . . . . ? C17 N3 C18 C19 -0.5(7) . . . . ? N3 C18 C19 C15 -0.5(8) . . . . ? C16 C15 C19 C18 1.1(7) . . . . ? C14 C15 C19 C18 178.1(4) . . . . ? O3 C14 C20 C21 3.8(6) . . . . ? C15 C14 C20 C21 -175.7(4) . . . . ? Cu1 O4 C21 C20 -2.8(5) . . . . ? Cu1 O4 C21 C22 178.1(2) . . . . ? C14 C20 C21 O4 4.3(6) . . . . ? C14 C20 C21 C22 -176.6(3) . . . . ? O4 C21 C22 C23 140.5(3) . . . . ? C20 C21 C22 C23 -38.7(5) . . . . ? O4 C21 C22 C26 -38.4(5) . . . . ? C20 C21 C22 C26 142.4(4) . . . . ? C26 C22 C23 C24 0.2(5) . . . . ? C21 C22 C23 C24 -178.7(3) . . . . ? C25 N4 C24 C23 0.8(5) . . . . ? Cu1 N4 C24 C23 170.7(3) 4 . . . ? C22 C23 C24 N4 -0.5(6) . . . . ? C24 N4 C25 C26 -0.8(5) . . . . ? Cu1 N4 C25 C26 -168.9(3) 4 . . . ? N4 C25 C26 C22 0.5(6) . . . . ? C23 C22 C26 C25 -0.2(5) . . . . ? C21 C22 C26 C25 178.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.628 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.135 #===end data_compound6_bath155 _database_code_depnum_ccdc_archive 'CCDC 853059' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H7 N2 O2 Zn0.50' _chemical_formula_weight 255.89 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0820(16) _cell_length_b 9.9551(17) _cell_length_c 13.093(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.136(3) _cell_angle_gamma 90.00 _cell_volume 1118.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1479 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 28.57 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_process_details ; SADABS - Bruker software ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8460 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7824 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.62 _diffrn_reflns_theta_max 31.84 _reflns_number_total 2259 _reflns_number_gt 1779 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0641P)^2^+0.4936P] 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 2259 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Zn1 Zn 0.0000 0.0000 0.0000 0.01785(18) Uani 1 2 d S . . O1 O 0.0938(3) 0.1541(2) -0.06391(17) 0.0239(5) Uani 1 1 d . . . O2 O 0.0286(3) 0.1159(2) 0.13643(17) 0.0236(5) Uani 1 1 d . . . N1 N 0.1409(4) 0.4210(3) -0.2834(2) 0.0326(7) Uani 1 1 d . . . N2 N 0.2743(3) 0.4111(3) 0.4185(2) 0.0228(6) Uani 1 1 d . . . C1 C 0.1665(4) 0.3688(3) -0.0984(3) 0.0214(7) Uani 1 1 d . . . C2 C 0.1055(4) 0.3454(3) -0.2094(3) 0.0248(7) Uani 1 1 d . . . C3 C 0.2388(5) 0.5238(3) -0.2471(3) 0.0324(9) Uani 1 1 d . . . H3 H 0.2665 0.5753 -0.2972 0.039 Uiso 1 1 calc R . . C4 C 0.3007(5) 0.5574(4) -0.1394(3) 0.0354(9) Uani 1 1 d . . . H4 H 0.3656 0.6317 -0.1180 0.042 Uiso 1 1 calc R . . C5 C 0.2650(5) 0.4788(3) -0.0633(3) 0.0314(9) Uani 1 1 d . . . H5 H 0.3061 0.4991 0.0099 0.038 Uiso 1 1 calc R . . C6 C 0.1274(4) 0.2697(3) -0.0245(2) 0.0196(7) Uani 1 1 d . . . C7 C 0.1312(4) 0.3108(3) 0.0784(2) 0.0236(7) Uani 1 1 d . . . H7 H 0.1641 0.3981 0.0989 0.028 Uiso 1 1 calc R . . C8 C 0.0895(4) 0.2313(3) 0.1538(2) 0.0202(7) Uani 1 1 d . . . C9 C 0.1164(4) 0.2861(3) 0.2648(2) 0.0208(7) Uani 1 1 d . . . C10 C 0.2432(4) 0.3685(3) 0.3157(2) 0.0226(7) Uani 1 1 d . . . C11 C 0.1773(4) 0.3774(4) 0.4708(3) 0.0280(8) Uani 1 1 d . . . H11 H 0.1977 0.4087 0.5410 0.034 Uiso 1 1 calc R . . C12 C 0.0469(4) 0.2978(4) 0.4260(3) 0.0298(8) Uani 1 1 d . . . H12 H -0.0205 0.2781 0.4642 0.036 Uiso 1 1 calc R . . C13 C 0.0198(4) 0.2487(4) 0.3233(3) 0.0269(8) Uani 1 1 d . . . H13 H -0.0631 0.1904 0.2930 0.032 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 Zn1 0.0283(3) 0.0143(3) 0.0077(3) 0.00038(19) 0.0016(2) -0.0005(2) O1 0.0367(14) 0.0180(12) 0.0169(11) -0.0008(9) 0.0089(10) -0.0019(10) O2 0.0336(13) 0.0198(12) 0.0148(11) -0.0022(9) 0.0044(9) -0.0029(10) N1 0.0482(19) 0.0295(17) 0.0203(15) 0.0008(13) 0.0115(14) -0.0023(15) N2 0.0330(16) 0.0224(15) 0.0114(13) -0.0029(11) 0.0052(12) -0.0027(12) C1 0.0305(18) 0.0173(16) 0.0171(16) -0.0004(13) 0.0087(14) 0.0026(13) C2 0.038(2) 0.0246(18) 0.0148(16) 0.0016(13) 0.0123(14) 0.0011(15) C3 0.052(2) 0.0228(19) 0.0272(19) 0.0055(14) 0.0190(17) -0.0006(16) C4 0.055(2) 0.0266(19) 0.0273(19) -0.0029(16) 0.0174(18) -0.0111(18) C5 0.046(2) 0.031(2) 0.0185(17) -0.0030(14) 0.0116(16) -0.0087(16) C6 0.0220(16) 0.0204(16) 0.0149(15) -0.0003(13) 0.0039(13) -0.0003(13) C7 0.0332(19) 0.0216(17) 0.0152(16) -0.0008(13) 0.0067(14) -0.0030(14) C8 0.0222(16) 0.0216(17) 0.0131(15) -0.0002(12) 0.0006(13) 0.0013(13) C9 0.0245(17) 0.0212(17) 0.0149(15) 0.0009(13) 0.0038(13) -0.0003(13) C10 0.0313(18) 0.0238(17) 0.0096(15) -0.0044(13) 0.0026(13) -0.0006(14) C11 0.037(2) 0.035(2) 0.0112(16) -0.0041(14) 0.0072(14) -0.0016(16) C12 0.037(2) 0.035(2) 0.0202(17) -0.0003(15) 0.0143(15) -0.0083(16) C13 0.0299(18) 0.0304(19) 0.0189(17) -0.0031(14) 0.0059(14) -0.0074(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 2.061(2) 3 ? Zn1 O1 2.061(2) . ? Zn1 O2 2.070(2) . ? Zn1 O2 2.070(2) 3 ? Zn1 N2 2.166(3) 4_565 ? Zn1 N2 2.166(3) 2_545 ? O1 C6 1.257(4) . ? O2 C8 1.263(4) . ? N1 C3 1.336(5) . ? N1 C2 1.346(4) . ? N2 C11 1.324(4) . ? N2 C10 1.350(4) . ? N2 Zn1 2.166(3) 2 ? C1 C5 1.393(5) . ? C1 C2 1.395(4) . ? C1 C6 1.504(4) . ? C3 C4 1.377(5) . ? C4 C5 1.387(5) . ? C6 C7 1.397(4) . ? C7 C8 1.411(4) . ? C8 C9 1.496(4) . ? C9 C13 1.391(4) . ? C9 C10 1.393(4) . ? C11 C12 1.386(5) . ? C12 C13 1.374(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 O1 Zn1 O1 180.00(13) 3 . ? O1 Zn1 O2 90.93(8) 3 . ? O1 Zn1 O2 89.07(8) . . ? O1 Zn1 O2 89.07(8) 3 3 ? O1 Zn1 O2 90.93(8) . 3 ? O2 Zn1 O2 180.00(13) . 3 ? O1 Zn1 N2 93.07(9) 3 4_565 ? O1 Zn1 N2 86.93(9) . 4_565 ? O2 Zn1 N2 91.62(9) . 4_565 ? O2 Zn1 N2 88.38(9) 3 4_565 ? O1 Zn1 N2 86.93(9) 3 2_545 ? O1 Zn1 N2 93.07(9) . 2_545 ? O2 Zn1 N2 88.38(9) . 2_545 ? O2 Zn1 N2 91.62(9) 3 2_545 ? N2 Zn1 N2 180.0(2) 4_565 2_545 ? C6 O1 Zn1 126.3(2) . . ? C8 O2 Zn1 125.9(2) . . ? C3 N1 C2 117.4(3) . . ? C11 N2 C10 118.6(3) . . ? C11 N2 Zn1 122.1(2) . 2 ? C10 N2 Zn1 118.3(2) . 2 ? C5 C1 C2 117.9(3) . . ? C5 C1 C6 124.4(3) . . ? C2 C1 C6 117.6(3) . . ? N1 C2 C1 123.3(3) . . ? N1 C3 C4 123.5(3) . . ? C3 C4 C5 119.0(3) . . ? C4 C5 C1 118.9(3) . . ? O1 C6 C7 126.2(3) . . ? O1 C6 C1 114.4(3) . . ? C7 C6 C1 119.4(3) . . ? C6 C7 C8 125.7(3) . . ? O2 C8 C7 125.9(3) . . ? O2 C8 C9 115.4(3) . . ? C7 C8 C9 118.7(3) . . ? C13 C9 C10 117.8(3) . . ? C13 C9 C8 120.4(3) . . ? C10 C9 C8 121.7(3) . . ? N2 C10 C9 122.1(3) . . ? N2 C11 C12 123.2(3) . . ? C13 C12 C11 118.2(3) . . ? C12 C13 C9 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 31.84 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.736 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.087 #===end data_compound7_k08adb24 _database_code_depnum_ccdc_archive 'CCDC 853060' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 Cl Eu N4 O10.50' _chemical_formula_weight 811.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8170(3) _cell_length_b 12.8910(4) _cell_length_c 13.8310(6) _cell_angle_alpha 87.802(1) _cell_angle_beta 79.328(1) _cell_angle_gamma 79.802(2) _cell_volume 1692.85(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14912 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 1.993 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7615 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.36 _reflns_number_total 5673 _reflns_number_gt 4758 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. The asymmetric unit in this structure is best formulated as [Eu(L)2(H2O)4][Cl]?(EtOH)2(H2O)0.5. The chloride anion was seen to be disordered over 2 sites in a 60:40 ratio, while the solvent ethanols presented as fractional molecules (75%,75% and 50% for the moieties based on O9, O10 and O11 respectively). The solvent portion based on O11 is in the same region of the electron density map as the 40% occupancy chloride. Similarly, the 1/2 occupancy water molecule (O12) is shares its region in space with the fractional ethanol based on O10. Oxygen bound hydrogens in the lattice solvent could not be reliably located and hence were omitted from the refinement. Those attached to the ligated waters were located readily however, and refined subject to distance restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.3615P] 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 0.0031(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5673 _refine_ls_number_parameters 485 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.123 _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 Eu1 Eu 0.25068(3) 0.74611(2) 0.74727(2) 0.02094(14) Uani 1 1 d D . . Cl1A Cl 0.2945(4) 0.5142(3) 0.4607(4) 0.0569(9) Uani 0.60 1 d P A 1 Cl1B Cl 0.0303(12) 0.9840(7) 1.0025(7) 0.063(2) Uani 0.40 1 d P . . O1 O 0.3794(4) 0.5891(3) 0.8075(3) 0.0284(9) Uani 1 1 d . . . O2 O 0.1195(4) 0.6911(3) 0.8963(4) 0.0353(11) Uani 1 1 d . . . O3 O 0.3358(4) 0.9034(3) 0.6873(3) 0.0290(10) Uani 1 1 d . . . O4 O 0.1670(4) 0.8021(3) 0.5990(3) 0.0284(10) Uani 1 1 d . . . O5 O 0.4606(4) 0.6860(3) 0.6320(4) 0.0350(10) Uani 1 1 d D . . O6 O 0.3618(6) 0.8146(4) 0.8667(4) 0.0408(12) Uani 1 1 d D . . O7 O 0.1413(6) 0.6125(4) 0.6913(5) 0.0514(15) Uani 1 1 d D . . O8 O 0.0473(5) 0.8809(3) 0.8034(4) 0.0327(10) Uani 1 1 d D . . O9 O 0.2974(10) 1.0197(5) 0.9302(6) 0.060(2) Uani 0.75 1 d PU B 1 O10 O 0.7438(13) 0.6974(12) 0.7866(10) 0.124(5) Uani 0.75 1 d PU C 1 O11 O 0.4472(11) 0.5123(7) 0.4284(8) 0.043(2) Uani 0.50 1 d PU D 2 O12 O 0.8825(13) 0.6354(11) 0.6232(11) 0.072(4) Uani 0.50 1 d P E 2 N1 N 0.5958(5) 0.2815(4) 0.9577(4) 0.0269(12) Uani 1 1 d . . . N2 N -0.0987(5) 0.5666(4) 1.2025(4) 0.0265(11) Uani 1 1 d . . . N3 N 0.4687(5) 1.2199(4) 0.5447(4) 0.0256(11) Uani 1 1 d . . . N4 N 0.0403(5) 0.9381(4) 0.2975(4) 0.0292(12) Uani 1 1 d . . . C1 C 0.3644(6) 0.5283(4) 0.8795(5) 0.0224(12) Uani 1 1 d . . . C2 C 0.2490(6) 0.5414(4) 0.9578(5) 0.0232(12) Uani 1 1 d . . . H2 H 0.2495 0.4921 1.0107 0.028 Uiso 1 1 calc R . . C3 C 0.1343(6) 0.6226(4) 0.9619(4) 0.0210(12) Uani 1 1 d . . . C4 C 0.0167(6) 0.6313(4) 1.0491(5) 0.0232(13) Uani 1 1 d . . . C5 C 0.0078(6) 0.5590(5) 1.1254(5) 0.0263(14) Uani 1 1 d . . . H5 H 0.0819 0.5003 1.1231 0.032 Uiso 1 1 calc R . . C6 C -0.2023(6) 0.6485(5) 1.2062(5) 0.0300(14) Uani 1 1 d . . . H6 H -0.2788 0.6540 1.2601 0.036 Uiso 1 1 calc R . . C7 C -0.2030(7) 0.7256(5) 1.1349(5) 0.0327(15) Uani 1 1 d . . . H7 H -0.2780 0.7840 1.1403 0.039 Uiso 1 1 calc R . . C8 C -0.0930(6) 0.7176(5) 1.0547(5) 0.0271(13) Uani 1 1 d . . . H8 H -0.0923 0.7700 1.0045 0.033 Uiso 1 1 calc R . . C9 C 0.4839(6) 0.4366(4) 0.8808(4) 0.0194(12) Uani 1 1 d . . . C10 C 0.4878(6) 0.3619(4) 0.9565(5) 0.0256(13) Uani 1 1 d . . . H10 H 0.4105 0.3681 1.0099 0.031 Uiso 1 1 calc R . . C11 C 0.7029(6) 0.2723(5) 0.8821(5) 0.0270(14) Uani 1 1 d . . . H11 H 0.7792 0.2156 0.8824 0.032 Uiso 1 1 calc R . . C12 C 0.7081(6) 0.3408(5) 0.8038(5) 0.0291(14) Uani 1 1 d . . . H12 H 0.7866 0.3318 0.7513 0.035 Uiso 1 1 calc R . . C13 C 0.5959(6) 0.4245(5) 0.8025(5) 0.0247(13) Uani 1 1 d . . . H13 H 0.5966 0.4723 0.7484 0.030 Uiso 1 1 calc R . . C14 C 0.3222(5) 0.9679(4) 0.6187(4) 0.0170(11) Uani 1 1 d . . . C15 C 0.2474(6) 0.9588(4) 0.5424(4) 0.0215(12) Uani 1 1 d . . . H15 H 0.2448 1.0118 0.4929 0.026 Uiso 1 1 calc R . . C16 C 0.1772(5) 0.8749(4) 0.5371(4) 0.0182(11) Uani 1 1 d . . . C17 C 0.1054(5) 0.8690(4) 0.4501(4) 0.0197(12) Uani 1 1 d . . . C18 C 0.0339(6) 0.7855(5) 0.4451(5) 0.0272(13) Uani 1 1 d . . . H18 H 0.0306 0.7332 0.4954 0.033 Uiso 1 1 calc R . . C19 C -0.0326(6) 0.7801(5) 0.3652(5) 0.0321(15) Uani 1 1 d . . . H19 H -0.0811 0.7237 0.3596 0.039 Uiso 1 1 calc R . . C20 C -0.0266(6) 0.8574(5) 0.2948(5) 0.0315(15) Uani 1 1 d . . . H1 H -0.0729 0.8533 0.2409 0.038 Uiso 1 1 calc R . . C21 C 0.1054(6) 0.9420(5) 0.3747(5) 0.0279(13) Uani 1 1 d . . . H21 H 0.1545 0.9989 0.3773 0.033 Uiso 1 1 calc R . . C22 C 0.3948(5) 1.0620(4) 0.6190(4) 0.0199(12) Uani 1 1 d . . . C23 C 0.4595(6) 1.0744(5) 0.6992(5) 0.0248(13) Uani 1 1 d . . . H23 H 0.4570 1.0254 0.7523 0.030 Uiso 1 1 calc R . . C24 C 0.5274(6) 1.1604(5) 0.6990(5) 0.0304(14) Uani 1 1 d . . . H24 H 0.5725 1.1707 0.7521 0.036 Uiso 1 1 calc R . . C25 C 0.5288(6) 1.2299(5) 0.6221(5) 0.0279(14) Uani 1 1 d . . . H25 H 0.5750 1.2885 0.6237 0.034 Uiso 1 1 calc R . . C26 C 0.4024(6) 1.1366(4) 0.5442(5) 0.0238(12) Uani 1 1 d . . . H26 H 0.3586 1.1288 0.4898 0.029 Uiso 1 1 calc R . . C27 C 0.365(3) 1.052(2) 1.0096(17) 0.153(9) Uani 0.75 1 d PDU B 1 H27A H 0.3434 1.1296 1.0146 0.183 Uiso 0.75 1 calc PR B 1 H27B H 0.4687 1.0322 0.9888 0.183 Uiso 0.75 1 calc PR B 1 C28 C 0.324(2) 1.0043(14) 1.1151(17) 0.138(10) Uani 0.75 1 d PDU B 1 H28A H 0.3768 1.0298 1.1601 0.207 Uiso 0.75 1 calc PR B 1 H28B H 0.3463 0.9272 1.1121 0.207 Uiso 0.75 1 calc PR B 1 H28C H 0.2228 1.0263 1.1389 0.207 Uiso 0.75 1 calc PR B 1 C29 C 0.7793(15) 0.7566(16) 0.6894(14) 0.103(6) Uani 0.75 1 d PDU C 1 H29A H 0.8771 0.7703 0.6774 0.123 Uiso 0.75 1 calc PR C 1 H29B H 0.7635 0.7187 0.6326 0.123 Uiso 0.75 1 calc PR C 1 C30 C 0.6728(18) 0.8563(13) 0.7122(15) 0.112(7) Uani 0.75 1 d PDU C 1 H30A H 0.6810 0.9043 0.6555 0.169 Uiso 0.75 1 calc PR C 1 H30B H 0.6905 0.8904 0.7697 0.169 Uiso 0.75 1 calc PR C 1 H30C H 0.5778 0.8391 0.7262 0.169 Uiso 0.75 1 calc PR C 1 C31 C 0.319(2) 0.521(2) 0.5121(18) 0.092(9) Uani 0.50 1 d PDU D 2 H31A H 0.2887 0.5940 0.5356 0.111 Uiso 0.50 1 calc PR D 2 H31B H 0.3410 0.4743 0.5680 0.111 Uiso 0.50 1 calc PR D 2 C32 C 0.202(2) 0.483(2) 0.4632(19) 0.089(8) Uani 0.50 1 d PDU D 2 H32A H 0.1154 0.4864 0.5119 0.134 Uiso 0.50 1 calc PR D 2 H32B H 0.2353 0.4101 0.4405 0.134 Uiso 0.50 1 calc PR D 2 H32C H 0.1846 0.5288 0.4072 0.134 Uiso 0.50 1 calc PR D 2 H5A H 0.539(4) 0.647(7) 0.6482(17) 0.107 Uiso 1 1 d D . . H6A H 0.345(11) 0.8854(6) 0.871(7) 0.107 Uiso 1 1 d D . . H7A H 0.092(10) 0.617(8) 0.642(5) 0.107 Uiso 1 1 d D . . H8A H 0.026(11) 0.936(5) 0.763(6) 0.107 Uiso 1 1 d D . . H5B H 0.474(4) 0.704(7) 0.5679(18) 0.107 Uiso 1 1 d D . . H6B H 0.369(12) 0.782(6) 0.925(3) 0.107 Uiso 1 1 d D . . H7B H 0.128(11) 0.557(6) 0.732(7) 0.107 Uiso 1 1 d D . . H8B H 0.020(11) 0.898(7) 0.8675(17) 0.107 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 Eu1 0.02609(18) 0.0186(2) 0.0191(2) 0.00624(11) -0.00458(13) -0.00737(11) Cl1A 0.056(2) 0.059(2) 0.049(3) 0.0047(18) 0.000(2) -0.0033(16) Cl1B 0.124(9) 0.021(6) 0.041(3) -0.019(3) -0.027(4) 0.012(4) O1 0.030(2) 0.024(2) 0.026(3) 0.0112(18) 0.0020(19) -0.0016(16) O2 0.035(2) 0.031(3) 0.031(3) 0.015(2) 0.007(2) 0.0001(18) O3 0.041(2) 0.028(2) 0.025(3) 0.0108(18) -0.015(2) -0.0181(18) O4 0.034(2) 0.031(2) 0.025(3) 0.0054(18) -0.0116(19) -0.0148(18) O5 0.038(2) 0.029(3) 0.033(3) 0.0094(19) 0.002(2) -0.0044(18) O6 0.066(3) 0.031(3) 0.035(3) 0.012(2) -0.029(3) -0.018(2) O7 0.075(4) 0.035(3) 0.062(4) 0.021(2) -0.042(3) -0.032(3) O8 0.037(2) 0.032(3) 0.027(3) 0.0032(18) -0.010(2) 0.0017(18) O9 0.110(6) 0.025(4) 0.051(5) 0.001(3) -0.034(5) -0.010(4) O10 0.106(9) 0.177(13) 0.072(9) 0.051(9) -0.017(7) 0.015(8) O11 0.054(6) 0.036(6) 0.034(7) 0.001(4) 0.006(5) -0.007(4) O12 0.058(8) 0.098(10) 0.063(10) 0.014(7) -0.016(7) -0.021(7) N1 0.035(3) 0.019(3) 0.029(3) 0.006(2) -0.012(3) -0.005(2) N2 0.034(3) 0.026(3) 0.023(3) 0.002(2) -0.005(2) -0.015(2) N3 0.028(3) 0.019(3) 0.028(3) 0.002(2) 0.001(2) -0.0060(19) N4 0.033(3) 0.032(3) 0.024(3) 0.003(2) -0.011(2) -0.002(2) C1 0.029(3) 0.016(3) 0.025(4) 0.005(2) -0.008(3) -0.009(2) C2 0.025(3) 0.025(3) 0.024(3) 0.006(2) -0.009(3) -0.011(2) C3 0.026(3) 0.021(3) 0.017(3) 0.002(2) 0.001(2) -0.013(2) C4 0.024(3) 0.018(3) 0.032(4) 0.000(2) -0.009(3) -0.011(2) C5 0.030(3) 0.022(3) 0.030(4) 0.000(2) -0.004(3) -0.012(2) C6 0.031(3) 0.034(4) 0.026(4) -0.007(3) 0.005(3) -0.018(3) C7 0.032(3) 0.026(4) 0.038(4) -0.006(3) 0.004(3) -0.009(2) C8 0.029(3) 0.021(3) 0.030(4) 0.001(2) 0.001(3) -0.008(2) C9 0.023(3) 0.019(3) 0.019(3) 0.000(2) -0.004(2) -0.009(2) C10 0.030(3) 0.022(3) 0.027(4) 0.004(2) -0.006(3) -0.009(2) C11 0.026(3) 0.023(3) 0.034(4) -0.001(2) -0.013(3) -0.003(2) C12 0.026(3) 0.031(4) 0.028(4) 0.000(3) -0.002(3) -0.004(2) C13 0.026(3) 0.029(3) 0.020(3) 0.007(2) -0.004(3) -0.009(2) C14 0.016(2) 0.018(3) 0.016(3) -0.001(2) 0.000(2) -0.0034(19) C15 0.028(3) 0.017(3) 0.021(3) 0.006(2) -0.006(2) -0.004(2) C16 0.017(2) 0.018(3) 0.018(3) 0.002(2) -0.005(2) 0.0006(19) C17 0.015(2) 0.021(3) 0.021(3) 0.000(2) 0.000(2) -0.0012(19) C18 0.031(3) 0.021(3) 0.028(4) 0.000(2) -0.008(3) 0.000(2) C19 0.028(3) 0.031(4) 0.040(4) -0.010(3) -0.010(3) -0.006(2) C20 0.030(3) 0.033(4) 0.032(4) -0.008(3) -0.016(3) 0.004(2) C21 0.028(3) 0.032(4) 0.025(4) 0.001(3) -0.009(3) -0.004(2) C22 0.015(2) 0.021(3) 0.023(3) 0.000(2) 0.000(2) -0.006(2) C23 0.026(3) 0.027(3) 0.022(4) 0.004(2) -0.006(3) -0.008(2) C24 0.032(3) 0.032(4) 0.030(4) 0.000(3) -0.005(3) -0.015(3) C25 0.029(3) 0.023(3) 0.032(4) 0.001(3) 0.003(3) -0.013(2) C26 0.026(3) 0.021(3) 0.024(4) 0.001(2) -0.003(3) -0.004(2) C27 0.22(2) 0.16(2) 0.091(19) -0.007(15) -0.042(17) -0.067(18) C28 0.19(2) 0.080(12) 0.19(2) 0.010(12) -0.14(2) -0.015(12) C29 0.056(8) 0.180(18) 0.075(12) 0.048(12) -0.024(8) -0.023(10) C30 0.120(14) 0.109(13) 0.105(16) -0.036(11) 0.043(11) -0.071(12) C31 0.075(15) 0.17(2) 0.035(13) -0.053(14) -0.006(12) -0.013(14) C32 0.052(11) 0.128(19) 0.10(2) -0.022(15) -0.006(11) -0.059(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O2 2.374(5) . ? Eu1 O5 2.388(4) . ? Eu1 O4 2.388(4) . ? Eu1 O3 2.390(4) . ? Eu1 O1 2.396(4) . ? Eu1 O7 2.405(4) . ? Eu1 O6 2.413(4) . ? Eu1 O8 2.430(4) . ? Cl1B Cl1B 0.676(12) 2_577 ? O1 C1 1.247(7) . ? O2 C3 1.251(7) . ? O3 C14 1.248(7) . ? O4 C16 1.250(7) . ? O9 C27 1.49(2) . ? O10 C29 1.53(2) . ? O11 C31 1.53(3) . ? N1 C11 1.331(9) . ? N1 C10 1.346(8) . ? N2 C6 1.325(8) . ? N2 C5 1.341(9) . ? N3 C25 1.335(8) . ? N3 C26 1.351(7) . ? N4 C20 1.330(8) . ? N4 C21 1.350(8) . ? C1 C2 1.406(9) . ? C1 C9 1.513(8) . ? C2 C3 1.390(8) . ? C3 C4 1.500(9) . ? C4 C5 1.381(9) . ? C4 C8 1.398(8) . ? C6 C7 1.374(10) . ? C7 C8 1.390(10) . ? C9 C13 1.384(9) . ? C9 C10 1.397(8) . ? C11 C12 1.370(9) . ? C12 C13 1.401(8) . ? C14 C15 1.411(7) . ? C14 C22 1.513(7) . ? C15 C16 1.392(7) . ? C16 C17 1.514(7) . ? C17 C21 1.378(9) . ? C17 C18 1.395(8) . ? C18 C19 1.394(9) . ? C19 C20 1.367(10) . ? C22 C26 1.386(8) . ? C22 C23 1.404(8) . ? C23 C24 1.390(8) . ? C24 C25 1.364(9) . ? C27 C28 1.57(2) . ? C29 C30 1.510(18) . ? C31 C32 1.587(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Eu1 O5 139.70(15) . . ? O2 Eu1 O4 127.51(15) . . ? O5 Eu1 O4 81.22(16) . . ? O2 Eu1 O3 136.15(16) . . ? O5 Eu1 O3 75.42(15) . . ? O4 Eu1 O3 70.38(13) . . ? O2 Eu1 O1 70.18(15) . . ? O5 Eu1 O1 69.81(15) . . ? O4 Eu1 O1 136.87(15) . . ? O3 Eu1 O1 127.94(14) . . ? O2 Eu1 O7 77.9(2) . . ? O5 Eu1 O7 89.8(2) . . ? O4 Eu1 O7 69.82(16) . . ? O3 Eu1 O7 139.14(17) . . ? O1 Eu1 O7 78.58(16) . . ? O2 Eu1 O6 79.12(18) . . ? O5 Eu1 O6 96.90(18) . . ? O4 Eu1 O6 138.66(14) . . ? O3 Eu1 O6 69.25(15) . . ? O1 Eu1 O6 77.72(15) . . ? O7 Eu1 O6 151.38(17) . . ? O2 Eu1 O8 70.12(15) . . ? O5 Eu1 O8 150.14(16) . . ? O4 Eu1 O8 76.86(15) . . ? O3 Eu1 O8 78.25(16) . . ? O1 Eu1 O8 139.35(16) . . ? O7 Eu1 O8 101.27(19) . . ? O6 Eu1 O8 86.62(17) . . ? C1 O1 Eu1 137.9(4) . . ? C3 O2 Eu1 138.8(4) . . ? C14 O3 Eu1 137.8(3) . . ? C16 O4 Eu1 138.1(3) . . ? C11 N1 C10 118.1(5) . . ? C6 N2 C5 118.2(6) . . ? C25 N3 C26 117.4(5) . . ? C20 N4 C21 116.9(6) . . ? O1 C1 C2 124.8(5) . . ? O1 C1 C9 115.4(5) . . ? C2 C1 C9 119.7(5) . . ? C3 C2 C1 123.4(6) . . ? O2 C3 C2 124.6(6) . . ? O2 C3 C4 115.7(5) . . ? C2 C3 C4 119.8(5) . . ? C5 C4 C8 116.8(6) . . ? C5 C4 C3 124.5(5) . . ? C8 C4 C3 118.7(5) . . ? N2 C5 C4 124.2(6) . . ? N2 C6 C7 122.3(6) . . ? C6 C7 C8 119.5(6) . . ? C7 C8 C4 119.0(6) . . ? C13 C9 C10 117.4(5) . . ? C13 C9 C1 118.8(5) . . ? C10 C9 C1 123.7(5) . . ? N1 C10 C9 123.3(6) . . ? N1 C11 C12 123.0(5) . . ? C11 C12 C13 119.0(6) . . ? C9 C13 C12 119.2(6) . . ? O3 C14 C15 125.4(5) . . ? O3 C14 C22 115.6(5) . . ? C15 C14 C22 119.0(5) . . ? C16 C15 C14 122.5(5) . . ? O4 C16 C15 125.6(5) . . ? O4 C16 C17 115.6(5) . . ? C15 C16 C17 118.7(5) . . ? C21 C17 C18 117.4(5) . . ? C21 C17 C16 123.8(5) . . ? C18 C17 C16 118.8(5) . . ? C19 C18 C17 118.9(6) . . ? C20 C19 C18 118.8(5) . . ? N4 C20 C19 123.8(6) . . ? N4 C21 C17 124.2(6) . . ? C26 C22 C23 117.8(5) . . ? C26 C22 C14 123.9(5) . . ? C23 C22 C14 118.3(5) . . ? C24 C23 C22 118.2(6) . . ? C25 C24 C23 119.6(6) . . ? N3 C25 C24 123.4(5) . . ? N3 C26 C22 123.5(5) . . ? O9 C27 C28 117.1(17) . . ? C30 C29 O10 98.8(15) . . ? O11 C31 C32 103.8(16) . . ? _diffrn_measured_fraction_theta_max 0.740 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.740 _refine_diff_density_max 1.959 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.121 #===end data_compound8_h08adb09 _database_code_depnum_ccdc_archive 'CCDC 853061' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 La N6 O9' _chemical_formula_weight 868.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21ca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, -z' 'x+1/2, y, -z+1/2' 'x, -y, z+1/2' _cell_length_a 9.7470(2) _cell_length_b 12.7120(2) _cell_length_c 31.1260(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3856.63(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57513 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description Irregular _exptl_crystal_colour straw _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34837 _diffrn_reflns_av_R_equivalents 0.1384 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6696 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Asymmetric unit contains one lanthanum chelated to 3 acac ligands and one water molecule, plus lattice solvent which was successfully modeled as 2 water oxygens. This was a very small crystal, and the quality was not ideal, necessitating a data collection time of 38 hours. Water hydrogens could not be realiably located and hence were omitted from the refinement. Similarity restrains were applied to the ADPs for carbons 37-39 during the final least-squares cycles. ; _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^)+(0.0335P)^2^+3.5057P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_number_reflns 6696 _refine_ls_number_parameters 496 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0962 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _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 La1 La 0.13720(7) 0.37616(3) 0.123601(10) 0.01997(11) Uani 1 1 d . . . O1 O 0.0362(5) 0.4735(4) 0.06144(15) 0.0282(13) Uani 1 1 d . . . O2 O -0.0017(5) 0.2594(4) 0.07706(16) 0.0277(13) Uani 1 1 d . . . O3 O 0.1085(5) 0.4650(4) 0.19443(15) 0.0351(16) Uani 1 1 d . . . O4 O 0.0300(5) 0.2602(4) 0.17733(16) 0.0288(12) Uani 1 1 d . . . O5 O 0.3824(6) 0.3960(5) 0.14300(19) 0.0286(15) Uani 1 1 d . . . O6 O 0.2647(5) 0.2039(4) 0.12674(16) 0.0271(12) Uani 1 1 d . . . O7 O 0.2200(6) 0.5737(4) 0.12065(17) 0.0340(13) Uani 1 1 d . . . O8 O 0.0852(6) 0.7591(5) 0.1055(2) 0.068(2) Uani 1 1 d . . . O9 O -0.1411(11) 0.8634(7) 0.1328(3) 0.070(3) Uani 1 1 d . . . N1 N -0.2118(7) 0.6396(5) -0.05023(19) 0.0296(16) Uani 1 1 d . . . N2 N -0.2152(9) -0.0081(6) 0.0596(3) 0.055(2) Uani 1 1 d . . . N3 N -0.1366(8) 0.6513(6) 0.3023(2) 0.0370(19) Uani 1 1 d . . . N4 N -0.1893(9) 0.0008(6) 0.2056(3) 0.050(2) Uani 1 1 d . . . N5 N 0.3073(9) -0.1059(7) 0.1005(3) 0.064(2) Uani 1 1 d . . . N6 N 0.8635(7) 0.4412(6) 0.1352(2) 0.0294(19) Uani 1 1 d . . . C1 C -0.0513(11) 0.4590(9) 0.0340(3) 0.034(3) Uani 1 1 d . . . C2 C -0.1152(9) 0.3611(7) 0.0242(2) 0.032(2) Uani 1 1 d . . . H2 H -0.1783 0.3583 0.0009 0.038 Uiso 1 1 calc R . . C3 C -0.0890(9) 0.2687(7) 0.0474(3) 0.030(2) Uani 1 1 d . . . C4 C -0.1730(8) 0.1711(7) 0.0378(2) 0.033(2) Uani 1 1 d . . . C5 C -0.2761(10) 0.1628(8) 0.0082(3) 0.051(3) Uani 1 1 d . . . H5 H -0.2995 0.2213 -0.0093 0.061 Uiso 1 1 calc R . . C6 C -0.3460(15) 0.0691(8) 0.0040(3) 0.062(3) Uani 1 1 d . . . H6 H -0.4155 0.0618 -0.0171 0.075 Uiso 1 1 calc R . . C7 C -0.3154(10) -0.0115(8) 0.0300(3) 0.053(3) Uani 1 1 d . . . H7 H -0.3673 -0.0745 0.0273 0.063 Uiso 1 1 calc R . . C8 C -0.1467(9) 0.0850(7) 0.0625(3) 0.044(2) Uani 1 1 d . . . H8 H -0.0755 0.0903 0.0833 0.052 Uiso 1 1 calc R . . C9 C -0.1014(8) 0.5528(7) 0.0095(2) 0.027(2) Uani 1 1 d . . . C10 C -0.1633(9) 0.5518(9) -0.0302(3) 0.024(3) Uani 1 1 d . . . H10 H -0.1727 0.4862 -0.0445 0.028 Uiso 1 1 calc R . . C11 C -0.1992(9) 0.7306(8) -0.0298(3) 0.035(2) Uani 1 1 d . . . H11 H -0.2353 0.7921 -0.0429 0.041 Uiso 1 1 calc R . . C12 C -0.1346(9) 0.7401(8) 0.0105(3) 0.042(2) Uani 1 1 d . . . H12 H -0.1259 0.8067 0.0241 0.050 Uiso 1 1 calc R . . C13 C -0.0853(9) 0.6522(7) 0.0294(3) 0.036(2) Uani 1 1 d . . . H13 H -0.0395 0.6570 0.0563 0.043 Uiso 1 1 calc R . . C14 C 0.0172(9) 0.4585(7) 0.2231(2) 0.034(2) Uani 1 1 d . . . C15 C -0.0512(8) 0.3669(7) 0.2339(3) 0.037(2) Uani 1 1 d . . . H15 H -0.1109 0.3691 0.2580 0.044 Uiso 1 1 calc R . . C16 C -0.0392(8) 0.2727(7) 0.2123(2) 0.027(2) Uani 1 1 d . . . C17 C -0.1190(10) 0.1782(7) 0.2258(3) 0.031(2) Uani 1 1 d . . . C18 C -0.1906(10) 0.1686(8) 0.2636(3) 0.042(3) Uani 1 1 d . . . H18 H -0.1926 0.2250 0.2836 0.050 Uiso 1 1 calc R . . C19 C -0.2597(10) 0.0764(8) 0.2722(3) 0.044(3) Uani 1 1 d . . . H19 H -0.3092 0.0687 0.2983 0.053 Uiso 1 1 calc R . . C20 C -0.2568(11) -0.0047(9) 0.2428(4) 0.057(3) Uani 1 1 d . . . H20 H -0.3052 -0.0675 0.2494 0.069 Uiso 1 1 calc R . . C21 C -0.1231(10) 0.0892(7) 0.1984(3) 0.040(2) Uani 1 1 d . . . H21 H -0.0732 0.0939 0.1723 0.048 Uiso 1 1 calc R . . C22 C -0.0203(9) 0.5598(7) 0.2451(3) 0.035(2) Uani 1 1 d . . . C23 C -0.0959(10) 0.5654(8) 0.2818(3) 0.040(2) Uani 1 1 d . . . H23 H -0.1225 0.5002 0.2942 0.048 Uiso 1 1 calc R . . C24 C -0.1029(11) 0.7401(9) 0.2839(3) 0.048(3) Uani 1 1 d . . . H24 H -0.1265 0.8037 0.2981 0.058 Uiso 1 1 calc R . . C25 C -0.0348(11) 0.7467(9) 0.2450(3) 0.056(3) Uani 1 1 d . . . H25 H -0.0200 0.8129 0.2316 0.068 Uiso 1 1 calc R . . C26 C 0.0115(10) 0.6540(8) 0.2260(3) 0.048(3) Uani 1 1 d . . . H26 H 0.0641 0.6559 0.2003 0.058 Uiso 1 1 calc R . . C27 C 0.4972(10) 0.3474(9) 0.1347(4) 0.029(3) Uani 1 1 d . . . C28 C 0.5030(7) 0.2397(7) 0.1270(3) 0.0313(19) Uani 1 1 d . . . H28 H 0.5905 0.2085 0.1228 0.038 Uiso 1 1 calc R . . C29 C 0.3884(8) 0.1755(7) 0.1252(3) 0.0300(18) Uani 1 1 d . . . C30 C 0.4072(8) 0.0590(7) 0.1217(3) 0.039(2) Uani 1 1 d . . . C31 C 0.3031(12) -0.0020(8) 0.1061(3) 0.056(3) Uani 1 1 d . . . H31 H 0.2202 0.0328 0.0986 0.067 Uiso 1 1 calc R . . C32 C 0.4203(15) -0.1552(11) 0.1117(4) 0.064(4) Uani 1 1 d . . . H32 H 0.4248 -0.2292 0.1077 0.076 Uiso 1 1 calc R . . C33 C 0.5319(13) -0.1047(9) 0.1289(5) 0.091(5) Uani 1 1 d . . . H33 H 0.6110 -0.1429 0.1376 0.109 Uiso 1 1 calc R . . C34 C 0.5256(10) 0.0041(9) 0.1333(4) 0.071(4) Uani 1 1 d . . . H34 H 0.6025 0.0413 0.1442 0.086 Uiso 1 1 calc R . . C35 C 0.6186(11) 0.4168(6) 0.1341(2) 0.028(2) Uani 1 1 d . . . C36 C 0.7516(12) 0.3803(8) 0.1355(3) 0.027(3) Uani 1 1 d . . . H36 H 0.7648 0.3063 0.1368 0.032 Uiso 1 1 calc R . . C37 C 0.8435(8) 0.5434(8) 0.1338(3) 0.0376(17) Uani 1 1 d U . . H37 H 0.9217 0.5881 0.1343 0.045 Uiso 1 1 calc R . . C38 C 0.7161(8) 0.5895(7) 0.1315(3) 0.0396(15) Uani 1 1 d U . . H38 H 0.7064 0.6638 0.1304 0.047 Uiso 1 1 calc R . . C39 C 0.6035(7) 0.5248(7) 0.1308(3) 0.0382(18) Uani 1 1 d U . . H39 H 0.5144 0.5544 0.1281 0.046 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 La1 0.01540(16) 0.02604(19) 0.01847(16) 0.00132(19) 0.0001(4) 0.0004(4) O1 0.022(3) 0.040(4) 0.023(3) 0.001(3) -0.011(2) -0.004(3) O2 0.025(3) 0.031(3) 0.027(3) 0.004(3) -0.010(2) 0.000(3) O3 0.030(4) 0.047(3) 0.028(3) -0.006(2) 0.014(3) -0.016(3) O4 0.028(3) 0.027(3) 0.032(3) 0.003(3) 0.008(2) 0.004(3) O5 0.018(3) 0.033(4) 0.035(3) -0.007(3) -0.003(3) -0.001(3) O6 0.019(3) 0.033(3) 0.029(3) 0.006(3) 0.002(2) 0.003(2) O7 0.042(3) 0.027(3) 0.032(3) 0.005(3) -0.005(3) -0.003(3) O8 0.050(4) 0.046(4) 0.109(5) -0.009(4) -0.042(4) 0.003(3) O9 0.081(7) 0.057(6) 0.072(5) 0.001(5) -0.007(5) 0.003(5) N1 0.035(4) 0.029(5) 0.025(4) 0.004(3) -0.005(3) 0.005(3) N2 0.052(6) 0.035(6) 0.078(6) 0.001(4) -0.013(5) -0.003(4) N3 0.046(5) 0.031(5) 0.034(4) -0.003(4) 0.012(4) 0.001(4) N4 0.067(6) 0.029(6) 0.054(5) 0.004(4) -0.003(5) -0.018(4) N5 0.067(6) 0.039(6) 0.086(7) -0.004(5) -0.004(5) 0.000(5) N6 0.013(4) 0.037(5) 0.038(4) 0.008(4) -0.002(3) 0.000(4) C1 0.032(6) 0.042(8) 0.029(7) 0.002(5) -0.008(5) 0.006(6) C2 0.038(5) 0.033(6) 0.026(4) 0.006(4) -0.012(4) -0.003(4) C3 0.035(5) 0.023(5) 0.033(5) -0.002(4) 0.008(4) -0.009(4) C4 0.039(5) 0.034(5) 0.026(4) -0.001(4) -0.004(4) -0.001(4) C5 0.053(6) 0.045(6) 0.054(6) 0.001(5) -0.031(5) -0.007(5) C6 0.059(8) 0.055(6) 0.072(6) 0.000(5) -0.033(7) -0.024(8) C7 0.039(6) 0.044(7) 0.075(7) -0.010(5) -0.011(5) -0.008(4) C8 0.041(5) 0.028(6) 0.062(6) -0.005(5) -0.014(5) -0.001(4) C9 0.029(5) 0.030(6) 0.023(4) 0.000(4) -0.010(4) -0.006(4) C10 0.024(6) 0.026(6) 0.021(6) -0.008(5) -0.003(4) -0.003(5) C11 0.034(5) 0.033(6) 0.037(5) 0.001(5) -0.013(4) 0.005(5) C12 0.049(5) 0.040(6) 0.037(5) -0.013(5) -0.022(4) 0.013(5) C13 0.044(5) 0.033(6) 0.031(5) 0.000(4) -0.008(4) 0.013(4) C14 0.040(5) 0.038(6) 0.024(4) 0.004(4) 0.007(4) -0.001(5) C15 0.037(5) 0.045(6) 0.030(5) -0.011(5) 0.011(4) -0.006(5) C16 0.029(5) 0.030(6) 0.023(4) -0.001(4) -0.001(4) 0.001(4) C17 0.027(5) 0.028(6) 0.039(5) -0.002(4) 0.002(4) -0.004(5) C18 0.041(6) 0.044(7) 0.041(6) 0.002(5) 0.020(5) 0.005(5) C19 0.039(6) 0.043(6) 0.052(6) 0.006(5) 0.008(5) -0.011(5) C20 0.050(7) 0.053(8) 0.068(8) 0.019(6) -0.005(6) -0.020(5) C21 0.048(6) 0.039(7) 0.033(5) 0.009(4) 0.003(4) -0.007(5) C22 0.036(5) 0.026(6) 0.043(5) 0.002(4) 0.010(4) -0.016(4) C23 0.053(7) 0.032(6) 0.034(5) 0.005(4) 0.012(5) 0.008(5) C24 0.065(7) 0.042(7) 0.038(5) -0.006(5) 0.013(5) 0.008(6) C25 0.074(7) 0.039(6) 0.056(7) 0.001(6) 0.010(6) -0.002(6) C26 0.053(7) 0.047(8) 0.046(6) -0.009(5) 0.010(5) 0.001(5) C27 0.006(4) 0.041(7) 0.040(6) -0.002(5) 0.000(4) 0.006(5) C28 0.007(4) 0.031(5) 0.055(5) -0.006(5) -0.003(4) 0.001(3) C29 0.026(5) 0.038(5) 0.026(4) 0.002(4) -0.005(4) 0.010(4) C30 0.031(5) 0.030(5) 0.056(6) 0.001(5) 0.004(5) -0.002(4) C31 0.054(7) 0.037(7) 0.078(8) -0.002(5) -0.006(6) 0.007(5) C32 0.061(9) 0.037(7) 0.093(10) -0.004(7) 0.015(8) 0.003(7) C33 0.049(7) 0.038(8) 0.185(15) 0.021(9) 0.020(9) 0.011(6) C34 0.030(6) 0.051(7) 0.133(11) 0.010(7) -0.007(7) 0.008(5) C35 0.010(6) 0.032(4) 0.041(4) 0.002(3) -0.001(4) 0.000(4) C36 0.037(7) 0.031(6) 0.014(5) 0.002(4) 0.005(4) -0.006(5) C37 0.024(4) 0.034(4) 0.055(4) 0.003(3) 0.005(3) 0.000(3) C38 0.025(3) 0.036(4) 0.057(3) 0.001(3) 0.005(3) 0.002(3) C39 0.020(4) 0.037(4) 0.057(4) 0.000(3) 0.005(3) 0.007(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 La1 O4 2.462(5) . ? La1 O2 2.477(5) . ? La1 O5 2.478(6) . ? La1 O3 2.493(5) . ? La1 O1 2.499(5) . ? La1 O6 2.520(5) . ? La1 O7 2.640(5) . ? La1 N1 2.725(6) 2_565 ? La1 N6 2.816(7) 1_455 ? O1 C1 1.222(11) . ? O2 C3 1.262(10) . ? O3 C14 1.264(9) . ? O4 C16 1.291(9) . ? O5 C27 1.304(12) . ? O6 C29 1.260(9) . ? N1 C11 1.326(11) . ? N1 C10 1.361(12) . ? N1 La1 2.725(6) 2_465 ? N2 C7 1.344(12) . ? N2 C8 1.362(11) . ? N3 C24 1.307(12) . ? N3 C23 1.326(11) . ? N4 C21 1.316(11) . ? N4 C20 1.333(13) . ? N5 C32 1.314(16) . ? N5 C31 1.333(12) . ? N6 C37 1.315(12) . ? N6 C36 1.337(13) . ? N6 La1 2.816(7) 1_655 ? C1 C2 1.425(14) . ? C1 C9 1.497(14) . ? C2 C3 1.402(12) . ? C2 H2 0.9500 . ? C3 C4 1.516(11) . ? C4 C8 1.363(12) . ? C4 C5 1.366(11) . ? C5 C6 1.379(13) . ? C5 H5 0.9500 . ? C6 C7 1.338(13) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.376(11) . ? C9 C13 1.415(12) . ? C10 H10 0.9500 . ? C11 C12 1.409(11) . ? C11 H11 0.9500 . ? C12 C13 1.352(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.383(12) . ? C14 C22 1.503(12) . ? C15 C16 1.379(11) . ? C15 H15 0.9500 . ? C16 C17 1.492(12) . ? C17 C18 1.374(11) . ? C17 C21 1.417(12) . ? C18 C19 1.378(13) . ? C18 H18 0.9500 . ? C19 C20 1.378(14) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.362(12) . ? C22 C26 1.372(12) . ? C23 H23 0.9500 . ? C24 C25 1.383(13) . ? C24 H24 0.9500 . ? C25 C26 1.395(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.390(13) . ? C27 C35 1.476(15) . ? C28 C29 1.385(11) . ? C28 H28 0.9500 . ? C29 C30 1.496(11) . ? C30 C31 1.366(13) . ? C30 C34 1.396(13) . ? C31 H31 0.9500 . ? C32 C33 1.372(19) . ? C32 H32 0.9500 . ? C33 C34 1.391(15) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.377(16) . ? C35 C39 1.386(11) . ? C36 H36 0.9500 . ? C37 C38 1.375(11) . ? C37 H37 0.9500 . ? C38 C39 1.371(11) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? 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 O4 La1 O2 78.84(17) . . ? O4 La1 O5 107.74(18) . . ? O2 La1 O5 136.95(18) . . ? O4 La1 O3 67.86(18) . . ? O2 La1 O3 136.68(17) . . ? O5 La1 O3 81.17(18) . . ? O4 La1 O1 130.95(17) . . ? O2 La1 O1 68.19(17) . . ? O5 La1 O1 121.21(19) . . ? O3 La1 O1 114.60(18) . . ? O4 La1 O6 70.26(16) . . ? O2 La1 O6 76.78(17) . . ? O5 La1 O6 66.64(17) . . ? O3 La1 O6 114.51(17) . . ? O1 La1 O6 130.89(16) . . ? O4 La1 O7 136.32(17) . . ? O2 La1 O7 135.81(17) . . ? O5 La1 O7 67.46(18) . . ? O3 La1 O7 68.53(17) . . ? O1 La1 O7 67.81(17) . . ? O6 La1 O7 132.66(17) . . ? O4 La1 N1 139.00(19) . 2_565 ? O2 La1 N1 76.18(18) . 2_565 ? O5 La1 N1 71.98(19) . 2_565 ? O3 La1 N1 146.63(18) . 2_565 ? O1 La1 N1 66.43(18) . 2_565 ? O6 La1 N1 72.68(18) . 2_565 ? O7 La1 N1 82.84(19) . 2_565 ? O4 La1 N6 71.73(19) . 1_455 ? O2 La1 N6 74.5(2) . 1_455 ? O5 La1 N6 148.48(18) . 1_455 ? O3 La1 N6 69.3(2) . 1_455 ? O1 La1 N6 65.23(18) . 1_455 ? O6 La1 N6 135.82(19) . 1_455 ? O7 La1 N6 90.9(2) . 1_455 ? N1 La1 N6 129.9(2) 2_565 1_455 ? C1 O1 La1 137.9(7) . . ? C3 O2 La1 137.8(5) . . ? C14 O3 La1 132.4(5) . . ? C16 O4 La1 136.1(5) . . ? C27 O5 La1 137.0(6) . . ? C29 O6 La1 136.0(5) . . ? C11 N1 C10 117.6(7) . . ? C11 N1 La1 121.1(5) . 2_465 ? C10 N1 La1 120.7(6) . 2_465 ? C7 N2 C8 115.4(8) . . ? C24 N3 C23 115.1(8) . . ? C21 N4 C20 115.8(8) . . ? C32 N5 C31 117.6(11) . . ? C37 N6 C36 116.8(8) . . ? C37 N6 La1 115.2(5) . 1_655 ? C36 N6 La1 127.1(6) . 1_655 ? O1 C1 C2 125.9(10) . . ? O1 C1 C9 117.6(10) . . ? C2 C1 C9 116.4(8) . . ? C3 C2 C1 122.8(8) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? O2 C3 C2 125.4(8) . . ? O2 C3 C4 115.6(7) . . ? C2 C3 C4 119.0(8) . . ? C8 C4 C5 117.2(8) . . ? C8 C4 C3 116.4(7) . . ? C5 C4 C3 126.4(8) . . ? C4 C5 C6 119.6(9) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 119.6(10) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 N2 123.5(9) . . ? C6 C7 H7 118.3 . . ? N2 C7 H7 118.3 . . ? N2 C8 C4 124.7(8) . . ? N2 C8 H8 117.7 . . ? C4 C8 H8 117.7 . . ? C10 C9 C13 116.8(8) . . ? C10 C9 C1 126.4(9) . . ? C13 C9 C1 116.8(7) . . ? N1 C10 C9 123.7(9) . . ? N1 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? N1 C11 C12 122.9(8) . . ? N1 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 118.4(9) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C9 120.5(8) . . ? C12 C13 H13 119.8 . . ? C9 C13 H13 119.8 . . ? O3 C14 C15 124.5(8) . . ? O3 C14 C22 115.9(8) . . ? C15 C14 C22 119.6(7) . . ? C16 C15 C14 124.9(8) . . ? C16 C15 H15 117.6 . . ? C14 C15 H15 117.6 . . ? O4 C16 C15 124.3(8) . . ? O4 C16 C17 114.2(7) . . ? C15 C16 C17 121.2(8) . . ? C18 C17 C21 115.5(9) . . ? C18 C17 C16 125.3(9) . . ? C21 C17 C16 119.2(8) . . ? C17 C18 C19 119.3(10) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 119.8(9) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N4 C20 C19 123.2(9) . . ? N4 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? N4 C21 C17 126.4(8) . . ? N4 C21 H21 116.8 . . ? C17 C21 H21 116.8 . . ? C23 C22 C26 116.2(9) . . ? C23 C22 C14 123.9(8) . . ? C26 C22 C14 119.7(8) . . ? N3 C23 C22 127.5(9) . . ? N3 C23 H23 116.2 . . ? C22 C23 H23 116.2 . . ? N3 C24 C25 123.9(10) . . ? N3 C24 H24 118.1 . . ? C25 C24 H24 118.1 . . ? C24 C25 C26 118.4(10) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C22 C26 C25 118.6(9) . . ? C22 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? O5 C27 C28 122.4(9) . . ? O5 C27 C35 114.1(9) . . ? C28 C27 C35 123.6(9) . . ? C29 C28 C27 123.7(7) . . ? C29 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? O6 C29 C28 127.0(7) . . ? O6 C29 C30 113.8(7) . . ? C28 C29 C30 119.2(7) . . ? C31 C30 C34 114.9(9) . . ? C31 C30 C29 119.8(8) . . ? C34 C30 C29 125.3(9) . . ? N5 C31 C30 125.9(10) . . ? N5 C31 H31 117.0 . . ? C30 C31 H31 117.0 . . ? N5 C32 C33 123.0(12) . . ? N5 C32 H32 118.5 . . ? C33 C32 H32 118.5 . . ? C32 C33 C34 117.9(12) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C33 C34 C30 120.6(11) . . ? C33 C34 H34 119.7 . . ? C30 C34 H34 119.7 . . ? C36 C35 C39 115.8(9) . . ? C36 C35 C27 123.6(8) . . ? C39 C35 C27 120.5(9) . . ? N6 C36 C35 125.0(9) . . ? N6 C36 H36 117.5 . . ? C35 C36 H36 117.5 . . ? N6 C37 C38 123.8(8) . . ? N6 C37 H37 118.1 . . ? C38 C37 H37 118.1 . . ? C39 C38 C37 118.0(8) . . ? C39 C38 H38 121.0 . . ? C37 C38 H38 121.0 . . ? C38 C39 C35 120.6(8) . . ? C38 C39 H39 119.7 . . ? C35 C39 H39 119.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.767 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.118 #===end data_compound9_bath330 _database_code_depnum_ccdc_archive 'CCDC 853062' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H43 Ag B F4 Fe N6 O10 S2' _chemical_formula_weight 1118.48 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' 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' Fe Fe 0.3463 0.8444 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 23.5252(4) _cell_length_b 23.5252(4) _cell_length_c 17.8727(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8566.2(4) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3414 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9436 _exptl_absorpt_correction_T_max 0.9712 _exptl_absorpt_process_details ? _exptl_special_details ; SADABS ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6907 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69715 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 29.75 _reflns_number_total 8830 _reflns_number_gt 7827 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Fe, Ag on special positions. BF4 region of electron density map is subject to substantial smearing. Given that this ion is not present at full occupancy, it is possible that the site is shared with some solvent. Unfortunately, this could not be resolved. This structure refined successfully after accounting for pseudo-merohedral twinning twinning on c. R factor by 10% when twinning was accounted for. There are an apparent void channels in this structure along the c direction. PLATON suggest that the electron density approximates to the equivalent of one water molecule pre asymmetric unti. However, this has not been additionally included as it is clear that the BF4 counter ion electron density is smeared. It is highly probable, after scrutiny of the structure that this counter-ion is along the structural channels, and that the modelled fragment represents the highest concentration of same. In short, the occupancy of the BF4 as presented is simplistic, as there is more disorder in this region than can be adequately modelled. ; _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^)+(0.1065P)^2^+0.8695P] 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 8830 _refine_ls_number_parameters 334 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.095 _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 0.349438(12) -0.2500 0.02267(9) Uani 1 2 d S . . Fe1 Fe 0.0000 0.41762(2) 0.2500 0.01779(11) Uani 1 2 d S . . S1 S -0.20614(6) 0.54500(6) -0.02355(8) 0.0498(3) Uani 1 1 d . . . F1 F 0.0777(5) 0.2897(5) 0.0510(6) 0.110(3) Uani 0.50 1 d PDU . . F2 F 0.1224(10) 0.2516(13) -0.0178(16) 0.57(4) Uani 0.50 1 d PDU . . F4 F 0.0495(10) 0.1842(7) 0.0557(9) 0.179(7) Uani 0.50 1 d PDU . . F3 F 0.0223(8) 0.2232(6) -0.0326(9) 0.182(6) Uani 0.50 1 d PDU . . O1 O 0.06688(9) 0.38946(9) 0.25498(18) 0.0242(4) Uani 1 1 d . . . O3 O 0.00578(13) 0.42323(11) 0.13917(12) 0.0222(4) Uani 1 1 d . . . O2 O -0.07231(10) 0.43813(10) 0.24148(15) 0.0214(4) Uani 1 1 d . . . O4 O -0.26195(17) 0.47420(16) -0.0230(2) 0.0502(8) Uani 1 1 d . . . O5 O -0.19901(15) 0.39821(17) -0.03816(19) 0.0452(7) Uani 1 1 d . . . N1 N -0.00300(19) 0.38502(15) -0.13365(13) 0.0275(5) Uani 1 1 d . . . N2 N -0.27764(15) 0.44867(16) 0.23347(18) 0.0339(7) Uani 1 1 d . . . N3 N 0.24273(13) 0.33396(15) 0.2604(2) 0.0356(8) Uani 1 1 d . . . C1 C -0.03966(14) 0.41513(14) 0.09358(16) 0.0197(5) Uani 1 1 d . . . C2 C -0.09711(15) 0.41580(16) 0.11273(18) 0.0223(5) Uani 1 1 d . . . H2 H -0.1290 0.4066 0.0750 0.027 Uiso 1 1 calc R . . C3 C -0.10931(13) 0.42956(14) 0.18568(17) 0.0189(5) Uani 1 1 d . . . C4 C -0.02837(15) 0.40449(15) 0.01429(17) 0.0219(5) Uani 1 1 d . . . C5 C 0.0084(2) 0.3747(2) -0.00112(18) 0.0331(8) Uani 1 1 d . . . H5 H 0.0257 0.3607 0.0383 0.040 Uiso 1 1 calc R . . C6 C 0.0195(2) 0.3656(2) -0.0760(2) 0.0375(9) Uani 1 1 d . . . H6 H 0.0442 0.3446 -0.0864 0.045 Uiso 1 1 calc R . . C7 C -0.03761(16) 0.41485(16) -0.11797(18) 0.0241(5) Uani 1 1 d . . . H7 H -0.0534 0.4293 -0.1584 0.029 Uiso 1 1 calc R . . C8 C -0.05128(15) 0.42545(16) -0.04577(17) 0.0230(5) Uani 1 1 d . . . H8 H -0.0760 0.4467 -0.0371 0.028 Uiso 1 1 calc R . . C9 C -0.16808(14) 0.43566(14) 0.20063(18) 0.0205(5) Uani 1 1 d . . . C10 C -0.18890(16) 0.43299(16) 0.27422(19) 0.0237(6) Uani 1 1 d . . . H10 H -0.1664 0.4268 0.3147 0.028 Uiso 1 1 calc R . . C11 C -0.24413(17) 0.4398(2) 0.2869(2) 0.0304(7) Uani 1 1 d . . . H11 H -0.2583 0.4378 0.3371 0.036 Uiso 1 1 calc R . . C12 C -0.25837(17) 0.4499(2) 0.1636(2) 0.0321(7) Uani 1 1 d . . . H12 H -0.2828 0.4551 0.1246 0.038 Uiso 1 1 calc R . . C13 C -0.20429(15) 0.44390(17) 0.14425(19) 0.0257(6) Uani 1 1 d . . . H13 H -0.1922 0.4454 0.0933 0.031 Uiso 1 1 calc R . . C14 C 0.05985(13) 0.33225(14) 0.2536(3) 0.0276(6) Uani 1 1 d . . . C15 C 0.0000 0.27387(18) 0.2500 0.0455(13) Uani 1 2 d S . . H15 H 0.0000 0.2335 0.2500 0.055 Uiso 1 2 calc SR . . C16 C 0.12232(14) 0.33035(15) 0.2579(3) 0.0296(7) Uani 1 1 d . . . C17 C 0.17788(16) 0.38403(17) 0.2862(2) 0.0331(8) Uani 1 1 d . . . H17 H 0.1759 0.4207 0.3051 0.040 Uiso 1 1 calc R . . C18 C 0.23592(17) 0.38360(19) 0.2868(3) 0.0373(8) Uani 1 1 d . . . H18 H 0.2735 0.4207 0.3070 0.045 Uiso 1 1 calc R . . C21 C -0.1588(3) 0.5513(3) -0.1041(3) 0.0662(16) Uani 1 1 d . . . H21A H -0.1283 0.5357 -0.0919 0.099 Uiso 1 1 calc R . . H21B H -0.1339 0.5972 -0.1202 0.099 Uiso 1 1 calc R . . H21C H -0.1881 0.5245 -0.1446 0.099 Uiso 1 1 calc R . . C19 C 0.1901(2) 0.2836(2) 0.2294(4) 0.0560(17) Uani 1 1 d . . . H19 H 0.1945 0.2491 0.2078 0.067 Uiso 1 1 calc R . . C20 C 0.12892(18) 0.2793(2) 0.2274(3) 0.0506(13) Uani 1 1 d . . . H20 H 0.0923 0.2422 0.2056 0.061 Uiso 1 1 calc R . . C22 C -0.2432(4) 0.5900(4) -0.0601(9) 0.127(5) Uani 1 1 d . . . H22A H -0.2140 0.6216 -0.0975 0.190 Uiso 1 1 calc R . . H22B H -0.2505 0.6134 -0.0193 0.190 Uiso 1 1 calc R . . H22C H -0.2853 0.5594 -0.0835 0.190 Uiso 1 1 calc R . . B1 B 0.0638(9) 0.2361(6) 0.0213(9) 0.088(6) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02090(13) 0.02711(12) 0.01794(13) 0.00059(7) 0.00118(14) 0.01045(6) Fe1 0.0166(2) 0.01895(16) 0.0170(2) -0.00090(14) -0.0018(3) 0.00832(10) S1 0.0393(5) 0.0520(6) 0.0575(8) 0.0054(5) 0.0020(5) 0.0225(5) F1 0.108(6) 0.109(6) 0.134(7) 0.004(5) -0.031(5) 0.071(5) F2 0.57(4) 0.57(4) 0.57(4) 0.007(8) -0.013(8) 0.28(2) F4 0.174(9) 0.177(9) 0.178(10) 0.008(7) -0.017(7) 0.081(7) F3 0.220(10) 0.116(7) 0.241(10) 0.012(6) -0.012(7) 0.109(7) O1 0.0176(8) 0.0211(8) 0.0331(12) 0.0018(11) -0.0001(11) 0.0092(7) O3 0.0201(10) 0.0284(10) 0.0184(8) -0.0014(7) -0.0012(9) 0.0123(9) O2 0.0210(8) 0.0261(9) 0.0203(13) -0.0043(9) -0.0019(8) 0.0141(7) O4 0.0455(17) 0.0521(17) 0.0489(18) 0.0115(14) 0.0058(15) 0.0213(15) O5 0.0374(14) 0.0521(17) 0.0423(17) -0.0060(14) -0.0076(12) 0.0196(14) N1 0.0335(12) 0.0377(16) 0.0190(10) -0.0021(11) 0.0007(14) 0.0236(15) N2 0.0239(12) 0.0424(15) 0.039(2) -0.0040(12) 0.0018(11) 0.0191(12) N3 0.0218(11) 0.0340(13) 0.056(2) -0.0067(14) -0.0060(14) 0.0179(10) C1 0.0178(11) 0.0235(12) 0.0190(12) -0.0015(10) -0.0002(9) 0.0111(10) C2 0.0190(12) 0.0313(14) 0.0197(14) -0.0062(11) -0.0030(10) 0.0150(11) C3 0.0184(11) 0.0189(12) 0.0188(13) -0.0027(10) -0.0003(9) 0.0089(9) C4 0.0208(12) 0.0276(13) 0.0181(13) -0.0022(10) -0.0012(10) 0.0127(11) C5 0.043(2) 0.059(2) 0.0179(12) -0.0019(13) -0.0009(14) 0.041(2) C6 0.052(2) 0.065(2) 0.0215(15) -0.0052(15) -0.0030(14) 0.049(2) C7 0.0268(14) 0.0302(14) 0.0192(13) 0.0024(11) -0.0006(11) 0.0171(12) C8 0.0246(13) 0.0273(14) 0.0213(13) -0.0013(11) -0.0012(10) 0.0160(12) C9 0.0187(12) 0.0197(12) 0.0214(14) -0.0032(10) 0.0006(10) 0.0083(10) C10 0.0219(13) 0.0284(14) 0.0209(13) -0.0015(11) 0.0019(10) 0.0125(12) C11 0.0253(14) 0.0410(18) 0.0284(18) 0.0012(14) 0.0075(12) 0.0194(14) C12 0.0233(14) 0.0424(19) 0.0350(18) -0.0015(14) -0.0036(13) 0.0198(14) C13 0.0221(13) 0.0342(15) 0.0245(15) -0.0018(12) -0.0011(11) 0.0169(12) C14 0.0183(10) 0.0236(11) 0.0420(17) -0.0010(16) -0.0047(16) 0.0112(9) C15 0.0220(18) 0.0202(12) 0.095(4) -0.0044(18) -0.009(4) 0.0110(9) C16 0.0178(11) 0.0243(12) 0.047(2) 0.0022(16) -0.0029(15) 0.0106(10) C17 0.0203(14) 0.0264(15) 0.053(2) -0.0077(14) -0.0087(14) 0.0122(12) C18 0.0197(14) 0.0292(16) 0.062(3) -0.0091(16) -0.0088(15) 0.0113(13) C21 0.039(2) 0.081(4) 0.054(3) 0.019(3) 0.001(2) 0.012(3) C19 0.0315(18) 0.0379(19) 0.109(5) -0.022(2) -0.017(2) 0.0250(16) C20 0.0228(15) 0.0324(18) 0.096(4) -0.020(2) -0.0155(18) 0.0135(14) C22 0.071(4) 0.077(5) 0.252(16) 0.048(7) 0.011(6) 0.053(4) B1 0.147(17) 0.037(6) 0.090(11) -0.016(7) -0.023(12) 0.053(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 Ag1 N1 2.256(2) 5_554 ? Ag1 N1 2.256(2) . ? Ag1 N3 2.357(3) 10 ? Ag1 N3 2.357(3) 9 ? Fe1 O3 1.985(2) . ? Fe1 O3 1.985(2) 5 ? Fe1 O1 1.9909(19) . ? Fe1 O1 1.9910(19) 5 ? Fe1 O2 1.9926(19) . ? Fe1 O2 1.993(2) 5 ? S1 O4 1.520(3) . ? S1 C21 1.781(6) . ? S1 C22 1.797(7) . ? F1 B1 1.251(13) . ? F2 B1 1.422(18) . ? F4 B1 1.254(15) . ? F3 B1 1.295(16) . ? O1 C14 1.272(3) . ? O3 C1 1.280(4) . ? O2 C3 1.272(4) . ? N1 C6 1.340(4) . ? N1 C7 1.344(4) . ? N2 C11 1.320(5) . ? N2 C12 1.324(5) . ? N3 C19 1.333(5) . ? N3 C18 1.341(5) . ? N3 Ag1 2.357(3) 8 ? C1 C2 1.402(4) . ? C1 C4 1.486(4) . ? C2 C3 1.407(4) . ? C3 C9 1.484(4) . ? C4 C5 1.388(4) . ? C4 C8 1.397(4) . ? C5 C6 1.399(5) . ? C7 C8 1.382(4) . ? C9 C10 1.394(5) . ? C9 C13 1.394(4) . ? C10 C11 1.404(4) . ? C12 C13 1.392(4) . ? C14 C15 1.393(3) . ? C14 C16 1.494(4) . ? C15 C14 1.392(3) 5 ? C16 C17 1.382(5) . ? C16 C20 1.397(5) . ? C17 C18 1.370(5) . ? C19 C20 1.392(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 N1 Ag1 N1 134.50(13) 5_554 . ? N1 Ag1 N3 106.70(14) 5_554 10 ? N1 Ag1 N3 100.62(13) . 10 ? N1 Ag1 N3 100.62(13) 5_554 9 ? N1 Ag1 N3 106.70(14) . 9 ? N3 Ag1 N3 104.86(15) 10 9 ? O3 Fe1 O3 176.30(12) . 5 ? O3 Fe1 O1 91.58(12) . . ? O3 Fe1 O1 91.12(12) 5 . ? O3 Fe1 O1 91.11(12) . 5 ? O3 Fe1 O1 91.58(12) 5 5 ? O1 Fe1 O1 86.60(11) . 5 ? O3 Fe1 O2 86.90(10) . . ? O3 Fe1 O2 90.62(11) 5 . ? O1 Fe1 O2 175.04(9) . . ? O1 Fe1 O2 88.71(8) 5 . ? O3 Fe1 O2 90.62(11) . 5 ? O3 Fe1 O2 86.90(10) 5 5 ? O1 Fe1 O2 88.71(8) . 5 ? O1 Fe1 O2 175.05(9) 5 5 ? O2 Fe1 O2 96.02(12) . 5 ? O4 S1 C21 105.0(3) . . ? O4 S1 C22 103.9(4) . . ? C21 S1 C22 97.2(5) . . ? C14 O1 Fe1 130.17(17) . . ? C1 O3 Fe1 126.9(2) . . ? C3 O2 Fe1 128.4(2) . . ? C6 N1 C7 117.7(3) . . ? C6 N1 Ag1 119.4(2) . . ? C7 N1 Ag1 121.7(2) . . ? C11 N2 C12 117.4(3) . . ? C19 N3 C18 117.2(3) . . ? C19 N3 Ag1 123.3(3) . 8 ? C18 N3 Ag1 118.4(2) . 8 ? O3 C1 C2 125.5(3) . . ? O3 C1 C4 115.2(2) . . ? C2 C1 C4 119.3(3) . . ? C1 C2 C3 122.5(3) . . ? O2 C3 C2 124.1(3) . . ? O2 C3 C9 116.1(3) . . ? C2 C3 C9 119.7(3) . . ? C5 C4 C8 118.3(3) . . ? C5 C4 C1 118.9(3) . . ? C8 C4 C1 122.7(3) . . ? C4 C5 C6 118.6(3) . . ? N1 C6 C5 123.2(3) . . ? N1 C7 C8 123.0(3) . . ? C7 C8 C4 119.2(3) . . ? C10 C9 C13 117.6(3) . . ? C10 C9 C3 119.3(3) . . ? C13 C9 C3 123.2(3) . . ? C9 C10 C11 118.1(3) . . ? N2 C11 C10 124.1(3) . . ? N2 C12 C13 123.5(3) . . ? C12 C13 C9 119.2(3) . . ? O1 C14 C15 125.3(3) . . ? O1 C14 C16 114.9(2) . . ? C15 C14 C16 119.8(3) . . ? C14 C15 C14 122.5(4) 5 . ? C17 C16 C20 117.9(3) . . ? C17 C16 C14 119.1(3) . . ? C20 C16 C14 122.7(3) . . ? C18 C17 C16 119.1(3) . . ? N3 C18 C17 123.9(3) . . ? N3 C19 C20 122.9(4) . . ? C19 C20 C16 118.9(4) . . ? F1 B1 F4 125.5(14) . . ? F1 B1 F3 109.8(11) . . ? F4 B1 F3 109.4(12) . . ? F1 B1 F2 102.7(13) . . ? F4 B1 F2 104.1(13) . . ? F3 B1 F2 102.4(13) . . ? 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 O3 Fe1 O1 C14 -90.1(4) . . . . ? O3 Fe1 O1 C14 92.4(4) 5 . . . ? O1 Fe1 O1 C14 0.9(4) 5 . . . ? O2 Fe1 O1 C14 -18.1(17) . . . . ? O2 Fe1 O1 C14 179.3(4) 5 . . . ? O3 Fe1 O3 C1 -71.8(2) 5 . . . ? O1 Fe1 O3 C1 151.5(2) . . . . ? O1 Fe1 O3 C1 64.9(2) 5 . . . ? O2 Fe1 O3 C1 -23.8(2) . . . . ? O2 Fe1 O3 C1 -119.8(2) 5 . . . ? O3 Fe1 O2 C3 23.1(2) . . . . ? O3 Fe1 O2 C3 -159.6(2) 5 . . . ? O1 Fe1 O2 C3 -49.1(15) . . . . ? O1 Fe1 O2 C3 -68.0(3) 5 . . . ? O2 Fe1 O2 C3 113.5(3) 5 . . . ? N1 Ag1 N1 C6 -155.2(4) 5_554 . . . ? N3 Ag1 N1 C6 -28.8(4) 10 . . . ? N3 Ag1 N1 C6 80.4(4) 9 . . . ? N1 Ag1 N1 C7 37.6(3) 5_554 . . . ? N3 Ag1 N1 C7 164.0(3) 10 . . . ? N3 Ag1 N1 C7 -86.8(3) 9 . . . ? Fe1 O3 C1 C2 15.8(4) . . . . ? Fe1 O3 C1 C4 -164.4(2) . . . . ? O3 C1 C2 C3 3.8(5) . . . . ? C4 C1 C2 C3 -176.0(3) . . . . ? Fe1 O2 C3 C2 -13.8(4) . . . . ? Fe1 O2 C3 C9 167.00(19) . . . . ? C1 C2 C3 O2 -5.0(5) . . . . ? C1 C2 C3 C9 174.3(3) . . . . ? O3 C1 C4 C5 29.4(4) . . . . ? C2 C1 C4 C5 -150.8(3) . . . . ? O3 C1 C4 C8 -148.2(3) . . . . ? C2 C1 C4 C8 31.6(5) . . . . ? C8 C4 C5 C6 -1.5(6) . . . . ? C1 C4 C5 C6 -179.2(4) . . . . ? C7 N1 C6 C5 0.3(7) . . . . ? Ag1 N1 C6 C5 -167.5(4) . . . . ? C4 C5 C6 N1 0.9(7) . . . . ? C6 N1 C7 C8 -0.7(6) . . . . ? Ag1 N1 C7 C8 166.7(3) . . . . ? N1 C7 C8 C4 0.0(5) . . . . ? C5 C4 C8 C7 1.1(5) . . . . ? C1 C4 C8 C7 178.7(3) . . . . ? O2 C3 C9 C10 -16.5(4) . . . . ? C2 C3 C9 C10 164.2(3) . . . . ? O2 C3 C9 C13 163.6(3) . . . . ? C2 C3 C9 C13 -15.6(4) . . . . ? C13 C9 C10 C11 -1.0(5) . . . . ? C3 C9 C10 C11 179.2(3) . . . . ? C12 N2 C11 C10 1.5(6) . . . . ? C9 C10 C11 N2 -0.2(6) . . . . ? C11 N2 C12 C13 -1.6(6) . . . . ? N2 C12 C13 C9 0.5(6) . . . . ? C10 C9 C13 C12 0.8(5) . . . . ? C3 C9 C13 C12 -179.3(3) . . . . ? Fe1 O1 C14 C15 -1.8(7) . . . . ? Fe1 O1 C14 C16 179.4(3) . . . . ? O1 C14 C15 C14 0.9(4) . . . 5 ? C16 C14 C15 C14 179.6(5) . . . 5 ? O1 C14 C16 C17 20.5(7) . . . . ? C15 C14 C16 C17 -158.3(4) . . . . ? O1 C14 C16 C20 -152.8(5) . . . . ? C15 C14 C16 C20 28.4(7) . . . . ? C20 C16 C17 C18 -3.3(7) . . . . ? C14 C16 C17 C18 -176.8(4) . . . . ? C19 N3 C18 C17 2.7(7) . . . . ? Ag1 N3 C18 C17 171.0(4) 8 . . . ? C16 C17 C18 N3 0.7(7) . . . . ? C18 N3 C19 C20 -3.6(8) . . . . ? Ag1 N3 C19 C20 -171.3(4) 8 . . . ? N3 C19 C20 C16 1.1(9) . . . . ? C17 C16 C20 C19 2.4(8) . . . . ? C14 C16 C20 C19 175.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.75 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.422 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.132 #===end data_compound10_bath267 _database_code_depnum_ccdc_archive 'CCDC 853063' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45.56 H56.28 Ag F6 Fe N6 O9.28 P S3.28' _chemical_formula_weight 1250.29 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' 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.378(2) _cell_length_b 23.544(3) _cell_length_c 18.052(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.387(2) _cell_angle_gamma 90.00 _cell_volume 5553.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2953 _cell_measurement_theta_min 2.296 _cell_measurement_theta_max 22.624 _exptl_crystal_description block _exptl_crystal_colour Dark-red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2561 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ; SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7848 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8516 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 20.39 _reflns_number_total 2722 _reflns_number_gt 2242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0685P)^2^+51.8309P] 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 2722 _refine_ls_number_parameters 367 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.126 _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 0.5000 0.14107(4) 0.2500 0.0445(4) Uani 1 2 d S . . Fe1 Fe 0.5000 0.08267(7) -0.2500 0.0368(5) Uani 1 2 d S . . S1 S 0.1693(4) 0.1701(2) -0.4944(2) 0.0975(14) Uani 0.84 1 d P . . F1 F 0.3451(8) 0.2578(4) 0.0745(5) 0.147(4) Uani 1 1 d . . . O1 O 0.6139(4) 0.0268(2) -0.2243(3) 0.0405(15) Uani 1 1 d . . . N1 N 0.9361(8) -0.0858(4) -0.1675(6) 0.082(3) Uani 1 1 d . . . C1 C 0.9035(11) -0.0768(7) -0.1048(8) 0.117(6) Uani 1 1 d . . . H1 H 0.9405 -0.0934 -0.0606 0.141 Uiso 1 1 calc R . . O4A O 0.1278(18) 0.1227(13) -0.4669(17) 0.171(14) Uani 0.42 1 d P . . S2A S 0.8396(12) -0.0757(6) 0.0870(9) 0.113(4) Uani 0.30 1 d P A 2 P2 P 0.2500 0.2500 0.0000 0.134(3) Uani 1 2 d S . . F2 F 0.3294(7) 0.2257(4) -0.0460(5) 0.142(4) Uani 1 1 d . . . O2 O 0.4959(5) 0.0811(2) -0.1399(3) 0.0399(15) Uani 1 1 d . . . N2 N 0.5003(6) 0.1048(3) 0.1345(4) 0.0401(18) Uani 1 1 d . . . C2 C 0.8202(11) -0.0451(6) -0.0991(7) 0.105(5) Uani 1 1 d . . . H2 H 0.8021 -0.0410 -0.0524 0.126 Uiso 1 1 calc R . . S2 S 0.8761(7) -0.0436(4) 0.1444(5) 0.110(3) Uani 0.50 1 d P A 1 F3 F 0.2292(8) 0.1874(3) 0.0269(5) 0.143(4) Uani 1 1 d . . . O3 O 0.3939(4) 0.1442(3) -0.2617(3) 0.0427(15) Uani 1 1 d . . . N3 N 0.1370(7) 0.2952(3) -0.2494(5) 0.052(2) Uani 1 1 d . . . C3 C 0.7643(7) -0.0197(4) -0.1611(5) 0.050(3) Uani 1 1 d . . . O4 O 0.2712(18) 0.1904(11) -0.4552(11) 0.114(7) Uani 0.42 1 d P . . C4 C 0.7938(8) -0.0291(4) -0.2263(6) 0.059(3) Uani 1 1 d . . . H4 H 0.7575 -0.0131 -0.2711 0.071 Uiso 1 1 calc R . . O5 O 0.8158(8) -0.0101(5) 0.0827(5) 0.094(4) Uani 0.80 1 d P . . C5 C 0.8789(9) -0.0628(6) -0.2269(7) 0.076(3) Uani 1 1 d . . . H5 H 0.8960 -0.0694 -0.2734 0.091 Uiso 1 1 calc R . . C6 C 0.6716(7) 0.0160(4) -0.1592(5) 0.046(2) Uani 1 1 d . . . C7 C 0.6516(7) 0.0347(4) -0.0900(5) 0.048(2) Uani 1 1 d . . . H7 H 0.6995 0.0267 -0.0457 0.057 Uiso 1 1 calc R . . C8 C 0.5637(8) 0.0645(4) -0.0841(5) 0.044(2) Uani 1 1 d . . . C9 C 0.5627(7) 0.0618(4) 0.1261(5) 0.048(2) Uani 1 1 d . . . H9 H 0.5913 0.0404 0.1687 0.058 Uiso 1 1 calc R . . C10 C 0.5871(7) 0.0473(4) 0.0576(5) 0.046(2) Uani 1 1 d . . . H10 H 0.6315 0.0174 0.0549 0.056 Uiso 1 1 calc R . . C11 C 0.5438(7) 0.0785(4) -0.0071(4) 0.038(2) Uani 1 1 d . . . C12 C 0.4789(9) 0.1202(4) 0.0006(5) 0.071(3) Uani 1 1 d . . . H12 H 0.4459 0.1406 -0.0417 0.085 Uiso 1 1 calc R . . C13 C 0.4600(9) 0.1333(5) 0.0725(5) 0.075(4) Uani 1 1 d . . . H13 H 0.4169 0.1637 0.0764 0.090 Uiso 1 1 calc R . . C14 C 0.2294(9) 0.3124(5) -0.2121(6) 0.071(3) Uani 1 1 d . . . H14 H 0.2341 0.3455 -0.1836 0.085 Uiso 1 1 calc R . . C15 C 0.3183(8) 0.2831(4) -0.2142(6) 0.067(3) Uani 1 1 d . . . H15 H 0.3813 0.2975 -0.1893 0.080 Uiso 1 1 calc R . . C16 C 0.3131(7) 0.2315(4) -0.2539(5) 0.045(2) Uani 1 1 d . . . C17 C 0.2182(8) 0.2137(4) -0.2899(6) 0.057(3) Uani 1 1 d . . . H17 H 0.2099 0.1798 -0.3170 0.068 Uiso 1 1 calc R . . C18 C 0.1326(8) 0.2475(5) -0.2854(6) 0.061(3) Uani 1 1 d . . . H18 H 0.0684 0.2345 -0.3100 0.073 Uiso 1 1 calc R . . C19 C 0.4072(7) 0.1978(4) -0.2549(5) 0.044(2) Uani 1 1 d . . . C20 C 0.5000 0.2261(5) -0.2500 0.058(4) Uani 1 2 d S . . H20 H 0.5000 0.2656 -0.2500 0.069 Uiso 1 2 calc SR . . C21 C 0.0756(14) 0.2233(8) -0.5230(11) 0.134(7) Uani 0.84 1 d P . . H21A H 0.0180 0.2074 -0.5579 0.201 Uiso 0.84 1 calc PR . . H21B H 0.1042 0.2537 -0.5472 0.201 Uiso 0.84 1 calc PR . . H21C H 0.0536 0.2377 -0.4793 0.201 Uiso 0.84 1 calc PR . . C22 C 0.1837(13) 0.1536(8) -0.5863(8) 0.109(6) Uani 0.84 1 d P . . H22A H 0.2145 0.1168 -0.5862 0.164 Uiso 0.84 1 calc PR . . H22B H 0.2267 0.1815 -0.6026 0.164 Uiso 0.84 1 calc PR . . H22C H 0.1178 0.1535 -0.6203 0.164 Uiso 0.84 1 calc PR . . C24 C 0.9549(17) -0.0907(12) 0.1373(18) 0.274(16) Uani 0.80 1 d PU . . H24A H 1.0176 -0.0734 0.1312 0.411 Uiso 0.80 1 calc PR A 1 H24B H 0.9280 -0.1140 0.0940 0.411 Uiso 0.80 1 calc PR A 1 H24C H 0.9676 -0.1137 0.1823 0.411 Uiso 0.80 1 calc PR A 1 H24D H 0.9245 -0.1273 0.1405 0.411 Uiso 0.80 1 calc PR A 1 H24E H 1.0142 -0.0867 0.1777 0.411 Uiso 0.80 1 calc PR A 1 H24F H 0.9745 -0.0871 0.0894 0.411 Uiso 0.80 1 calc PR A 1 C23 C 0.7888(17) -0.1065(7) 0.1492(10) 0.146(9) Uani 0.80 1 d P . . H23A H 0.7265 -0.0934 0.1616 0.218 Uiso 0.80 1 calc PR A 1 H23B H 0.8224 -0.1326 0.1874 0.218 Uiso 0.80 1 calc PR A 1 H23C H 0.7734 -0.1253 0.1009 0.218 Uiso 0.80 1 calc PR A 1 H23D H 0.8217 -0.1408 0.1383 0.218 Uiso 0.80 1 calc PR A 1 H23E H 0.7258 -0.1016 0.1125 0.218 Uiso 0.80 1 calc PR A 1 H23F H 0.7748 -0.1088 0.1990 0.218 Uiso 0.80 1 calc PR A 1 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 0.0586(7) 0.0562(7) 0.0238(6) 0.000 0.0203(5) 0.000 Fe1 0.0559(12) 0.0364(11) 0.0216(10) 0.000 0.0162(9) 0.000 S1 0.103(3) 0.126(4) 0.068(3) 0.007(2) 0.026(3) -0.014(3) F1 0.190(9) 0.146(8) 0.105(7) 0.047(6) 0.036(7) 0.094(7) O1 0.054(4) 0.044(4) 0.027(4) 0.005(3) 0.018(3) 0.008(3) N1 0.093(7) 0.101(8) 0.063(7) 0.018(6) 0.041(6) 0.035(6) C1 0.117(12) 0.175(15) 0.065(9) 0.021(9) 0.031(9) 0.072(11) O4A 0.094(17) 0.21(3) 0.18(3) 0.12(2) -0.018(17) -0.074(19) S2A 0.153(13) 0.091(9) 0.102(10) -0.017(8) 0.043(9) 0.011(9) P2 0.194(8) 0.102(5) 0.131(6) 0.055(4) 0.092(6) 0.085(5) F2 0.183(8) 0.132(7) 0.135(7) 0.047(6) 0.085(7) 0.095(7) O2 0.059(4) 0.045(4) 0.017(3) 0.001(3) 0.011(3) 0.007(3) N2 0.058(5) 0.040(4) 0.023(4) 0.003(4) 0.009(4) 0.009(4) C2 0.124(11) 0.143(12) 0.066(9) 0.019(8) 0.058(9) 0.077(11) S2 0.124(7) 0.135(7) 0.079(5) -0.008(5) 0.040(5) 0.028(6) F3 0.205(10) 0.097(6) 0.142(7) 0.056(6) 0.073(7) 0.070(6) O3 0.057(4) 0.044(4) 0.029(3) -0.003(3) 0.013(3) 0.000(3) N3 0.064(6) 0.047(5) 0.049(5) -0.011(4) 0.020(5) -0.001(4) C3 0.055(6) 0.068(7) 0.027(5) 0.006(5) 0.012(5) 0.018(5) O4 0.118(18) 0.15(2) 0.068(13) -0.031(14) 0.007(13) -0.010(16) C4 0.053(7) 0.075(7) 0.056(7) -0.010(6) 0.022(5) 0.010(6) O5 0.095(8) 0.129(9) 0.047(6) 0.000(6) -0.009(5) 0.062(7) C5 0.077(8) 0.103(9) 0.054(8) -0.015(7) 0.029(7) 0.006(8) C6 0.062(7) 0.040(6) 0.041(7) 0.004(5) 0.021(6) -0.006(5) C7 0.061(7) 0.060(6) 0.025(5) -0.004(5) 0.016(5) 0.011(5) C8 0.068(7) 0.036(5) 0.034(6) -0.002(5) 0.021(6) 0.000(5) C9 0.062(6) 0.055(7) 0.031(6) 0.006(5) 0.015(5) 0.005(6) C10 0.054(6) 0.050(6) 0.038(6) -0.003(5) 0.016(5) 0.001(5) C11 0.051(6) 0.040(5) 0.023(5) 0.008(4) 0.009(4) 0.008(5) C12 0.109(9) 0.070(8) 0.034(6) 0.015(5) 0.014(6) 0.038(7) C13 0.126(10) 0.071(7) 0.027(6) -0.006(6) 0.018(6) 0.050(7) C14 0.073(9) 0.064(7) 0.077(8) -0.027(6) 0.018(7) 0.008(7) C15 0.058(7) 0.065(8) 0.077(8) -0.015(6) 0.011(6) 0.004(6) C16 0.057(7) 0.049(6) 0.034(5) -0.002(5) 0.021(5) -0.001(5) C17 0.064(8) 0.056(7) 0.052(6) -0.006(5) 0.013(6) 0.005(6) C18 0.051(7) 0.073(8) 0.054(7) -0.003(6) 0.005(6) -0.006(6) C19 0.066(7) 0.041(6) 0.029(5) 0.006(5) 0.017(5) -0.003(6) C20 0.079(11) 0.011(7) 0.093(11) 0.000 0.039(9) 0.000 C21 0.125(15) 0.156(18) 0.125(15) -0.049(14) 0.035(13) 0.015(14) C22 0.106(13) 0.157(17) 0.064(10) -0.012(10) 0.014(9) 0.022(11) C24 0.136(17) 0.26(2) 0.35(3) -0.03(2) -0.115(18) 0.147(18) C23 0.25(3) 0.116(15) 0.101(14) 0.058(12) 0.113(16) 0.081(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 Ag1 N2 2.255(6) . ? Ag1 N2 2.255(6) 2_655 ? Ag1 N3 2.367(8) 7 ? Ag1 N3 2.367(8) 8_556 ? Fe1 O1 1.991(6) 2_654 ? Fe1 O1 1.991(6) . ? Fe1 O2 2.000(5) 2_654 ? Fe1 O2 2.000(5) . ? Fe1 O3 2.008(6) . ? Fe1 O3 2.008(6) 2_654 ? S1 O4A 1.39(2) . ? S1 O4 1.47(2) . ? S1 C22 1.754(14) . ? S1 C21 1.771(19) . ? F1 P2 1.651(10) . ? O1 C6 1.285(10) . ? N1 C5 1.294(14) . ? N1 C1 1.315(15) . ? C1 C2 1.364(16) . ? S2A O5 1.575(17) . ? S2A C23 1.60(2) . ? S2A C24 1.65(2) . ? P2 F2 1.588(7) 7 ? P2 F2 1.588(7) . ? P2 F3 1.596(8) . ? P2 F3 1.596(8) 7 ? P2 F1 1.651(10) 7 ? O2 C8 1.263(10) . ? N2 C13 1.316(11) . ? N2 C9 1.342(11) . ? C2 C3 1.346(14) . ? S2 O5 1.458(12) . ? S2 C24 1.55(2) . ? S2 C23 1.90(2) . ? O3 C19 1.276(10) . ? N3 C18 1.292(12) . ? N3 C14 1.337(13) . ? N3 Ag1 2.367(8) 7 ? C3 C4 1.337(13) . ? C3 C6 1.505(13) . ? C4 C5 1.390(14) . ? C6 C7 1.403(12) . ? C7 C8 1.394(12) . ? C8 C11 1.507(12) . ? C9 C10 1.386(12) . ? C10 C11 1.397(12) . ? C11 C12 1.337(13) . ? C12 C13 1.409(13) . ? C14 C15 1.382(14) . ? C15 C16 1.405(13) . ? C16 C17 1.362(13) . ? C16 C19 1.491(13) . ? C17 C18 1.410(14) . ? C19 C20 1.395(10) . ? C20 C19 1.395(10) 2_654 ? 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 N2 Ag1 N2 135.5(4) . 2_655 ? N2 Ag1 N3 113.0(3) . 7 ? N2 Ag1 N3 95.1(3) 2_655 7 ? N2 Ag1 N3 95.1(3) . 8_556 ? N2 Ag1 N3 113.0(3) 2_655 8_556 ? N3 Ag1 N3 101.3(4) 7 8_556 ? O1 Fe1 O1 97.2(3) 2_654 . ? O1 Fe1 O2 86.5(2) 2_654 2_654 ? O1 Fe1 O2 92.1(2) . 2_654 ? O1 Fe1 O2 92.1(2) 2_654 . ? O1 Fe1 O2 86.5(2) . . ? O2 Fe1 O2 177.9(3) 2_654 . ? O1 Fe1 O3 88.0(2) 2_654 . ? O1 Fe1 O3 171.8(2) . . ? O2 Fe1 O3 94.5(2) 2_654 . ? O2 Fe1 O3 87.0(2) . . ? O1 Fe1 O3 171.8(2) 2_654 2_654 ? O1 Fe1 O3 88.0(2) . 2_654 ? O2 Fe1 O3 87.0(2) 2_654 2_654 ? O2 Fe1 O3 94.5(2) . 2_654 ? O3 Fe1 O3 87.6(3) . 2_654 ? O4A S1 O4 119.4(14) . . ? O4A S1 C22 107.1(17) . . ? O4 S1 C22 104.4(10) . . ? O4A S1 C21 111.2(14) . . ? O4 S1 C21 115.7(12) . . ? C22 S1 C21 95.5(8) . . ? C6 O1 Fe1 128.5(5) . . ? C5 N1 C1 113.6(10) . . ? N1 C1 C2 125.5(12) . . ? O5 S2A C23 111.4(11) . . ? O5 S2A C24 113.0(14) . . ? C23 S2A C24 90.2(16) . . ? F2 P2 F2 180.0(8) 7 . ? F2 P2 F3 89.6(4) 7 . ? F2 P2 F3 90.4(4) . . ? F2 P2 F3 90.4(4) 7 7 ? F2 P2 F3 89.6(4) . 7 ? F3 P2 F3 180.0(6) . 7 ? F2 P2 F1 88.9(5) 7 7 ? F2 P2 F1 91.1(5) . 7 ? F3 P2 F1 89.5(5) . 7 ? F3 P2 F1 90.5(5) 7 7 ? F2 P2 F1 91.1(5) 7 . ? F2 P2 F1 88.9(5) . . ? F3 P2 F1 90.5(5) . . ? F3 P2 F1 89.5(5) 7 . ? F1 P2 F1 180.0(9) 7 . ? C8 O2 Fe1 129.1(5) . . ? C13 N2 C9 116.2(7) . . ? C13 N2 Ag1 120.7(6) . . ? C9 N2 Ag1 121.0(6) . . ? C3 C2 C1 119.8(11) . . ? O5 S2 C24 126.6(13) . . ? O5 S2 C23 102.1(9) . . ? C24 S2 C23 83.2(14) . . ? C19 O3 Fe1 128.5(6) . . ? C18 N3 C14 117.0(9) . . ? C18 N3 Ag1 126.6(7) . 7 ? C14 N3 Ag1 116.2(7) . 7 ? C4 C3 C2 116.3(9) . . ? C4 C3 C6 120.8(9) . . ? C2 C3 C6 122.9(9) . . ? C3 C4 C5 119.9(10) . . ? S2 O5 S2A 50.2(7) . . ? N1 C5 C4 124.9(10) . . ? O1 C6 C7 124.1(8) . . ? O1 C6 C3 115.2(8) . . ? C7 C6 C3 120.7(9) . . ? C8 C7 C6 123.4(9) . . ? O2 C8 C7 124.6(8) . . ? O2 C8 C11 115.4(8) . . ? C7 C8 C11 119.9(9) . . ? N2 C9 C10 123.8(8) . . ? C9 C10 C11 118.9(9) . . ? C12 C11 C10 117.4(8) . . ? C12 C11 C8 120.3(8) . . ? C10 C11 C8 122.2(8) . . ? C11 C12 C13 120.4(9) . . ? N2 C13 C12 123.3(9) . . ? N3 C14 C15 122.9(10) . . ? C14 C15 C16 119.8(10) . . ? C17 C16 C15 116.6(9) . . ? C17 C16 C19 122.3(9) . . ? C15 C16 C19 121.1(9) . . ? C16 C17 C18 119.0(9) . . ? N3 C18 C17 124.6(10) . . ? O3 C19 C20 125.6(9) . . ? O3 C19 C16 115.2(8) . . ? C20 C19 C16 119.2(9) . . ? C19 C20 C19 122.9(12) . 2_654 ? S2 C24 S2A 47.4(7) . . ? S2A C23 S2 42.2(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.39 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.065 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.083 #===end data_compound11_k06adb12 _database_code_depnum_ccdc_archive 'CCDC 853064' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.50 H35.50 Ag F6 Fe N6 O7.25 S1.25 Sb' _chemical_formula_weight 1173.80 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.0850(1) _cell_length_b 24.2820(2) _cell_length_c 18.1190(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.126(1) _cell_angle_gamma 90.00 _cell_volume 5303.20(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 161652 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2330 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.79 _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 kappaCCD _diffrn_measurement_method kappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96145 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12131 _reflns_number_gt 9778 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Early refinements of the structural model indicated that there was diffuse electron density in the lattice. Subsequent examination with PLATON showed that this centred on 2 regions namely in the middle of the A and C faces of the unit cell. It appeared that these regions contained highly disordered fragments of DMSO but disorder was so extensive that a sensible atomic model could not be developed. Hence the solvent was modelled using the SQUEEZE procedure in PLATON. This yielded an estimate of the solvent content (based on the approximate number of electrons contained in the voids) as being in the region of 30 electrons (close to 1 DMSO molecules). Thus, F(000) and related parameters, as presented, are derived on the basis of inclusion of an additional DMSO in the unit cell. The anion (SBF6) in this structure is disordered over 2 sites in a ratio of 55:45. There exists, within each fragment considerable disorder also. Optimum convergence was attained by restraining all Sb-F and F-F distances to being respectively similar. Partial fluorines were treated isotropically. Electron density maxima/minima in the final difference Fourier map are located at chemically insignificant distances from the partial Sb atoms. Indeed, it is highly likely that the partial anions are positionally disordered with fragments of DMSO. Strenuous efforts (>150 runs!) were undertaken in an effort to model such disorder, but the problem could not be satisfactorily resolved - and hence abandoned. ; _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^)+(0.1483P)^2^+26.7272P] 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 12131 _refine_ls_number_parameters 589 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2544 _refine_ls_wR_factor_gt 0.2414 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 393.9 14.6 2 0.500 0.500 1.000 393.8 15.1 _platon_squeeze_details ; Early refinements of the structural model indicated that there was diffuse electron density in the lattice. Subsequent examination with PLATON showed that this centred on 2 regions namely in the middle of the A and C faces of the unit cell. It appeared that these regions contained highly disordered fragments of DMSO but disorder was so extensive that a sensible atomic model could not be developed. Hence the solvent was modelled using the SQUEEZE procedure in PLATON. This yielded an estimate of the solvent content (based on the approximate number of electrons contained in the voids) as being in the region of 30 electrons (close to 1 DMSO molecules). Thus, F(000) and related parameters, as presented, are derived on the basis of inclusion of an additional DMSO in the unit cell. ; 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 Sb1 Sb 0.58018(9) 0.40638(5) 0.45710(6) 0.0617(3) Uani 0.55 1 d PD A 1 Ag1 Ag 0.19857(4) 0.067797(18) -0.22239(2) 0.03181(16) Uani 1 1 d . . . Fe1 Fe 0.09705(6) 0.05987(3) 0.26912(4) 0.02365(19) Uani 1 1 d . C . S1 S 0.9149(3) 0.18739(15) 0.47826(19) 0.0693(9) Uani 0.70 1 d P B 1 S1A S 0.8434(16) 0.2044(8) 0.4313(8) 0.142(6) Uani 0.30 1 d P B 2 F1 F 0.5081(11) 0.4710(5) 0.4758(7) 0.138(6) Uiso 0.55 1 d PD . 1 F2 F 0.6490(10) 0.4428(5) 0.3873(6) 0.107(4) Uiso 0.55 1 d PD A 1 F3 F 0.6449(12) 0.3448(5) 0.4428(8) 0.183(8) Uiso 0.55 1 d PD A 1 F4 F 0.5066(10) 0.3752(5) 0.5306(6) 0.114(4) Uiso 0.55 1 d PD A 1 F5 F 0.6878(10) 0.4267(5) 0.5250(7) 0.128(5) Uiso 0.55 1 d PD A 1 F6 F 0.4664(11) 0.3898(6) 0.3923(7) 0.146(6) Uiso 0.55 1 d PD A 1 O1 O 0.2583(3) 0.04224(16) 0.2735(2) 0.0285(8) Uani 1 1 d . . . O2 O 0.1451(3) 0.13832(16) 0.2741(2) 0.0305(8) Uani 1 1 d . . . O3 O 0.0904(3) 0.05680(16) 0.3780(2) 0.0282(8) Uani 1 1 d . . . O4 O 0.0759(3) -0.02143(15) 0.2694(2) 0.0275(8) Uani 1 1 d . . . O5 O -0.0587(3) 0.08658(16) 0.25392(19) 0.0263(8) Uani 1 1 d . . . O6 O 0.0975(3) 0.05622(17) 0.1593(2) 0.0305(8) Uani 1 1 d . . . O7 O 0.8198(10) 0.1514(4) 0.4677(6) 0.121(3) Uani 1 1 d . . . N1 N 0.6333(4) -0.0182(2) 0.2232(3) 0.0374(11) Uani 1 1 d . . . N2 N 0.2340(5) 0.3358(2) 0.2731(3) 0.0388(12) Uani 1 1 d . . . N3 N 0.1633(4) 0.0548(2) 0.6515(3) 0.0291(10) Uani 1 1 d . . . N4 N 0.1649(8) -0.2194(3) 0.2519(5) 0.074(2) Uani 1 1 d . C . N5 N -0.4045(5) 0.1981(3) 0.2343(4) 0.0560(17) Uani 1 1 d . C . N6 N 0.1299(5) 0.0578(2) -0.1113(3) 0.0355(11) Uani 1 1 d . C . C1 C 0.3370(5) 0.0725(2) 0.2539(3) 0.0296(11) Uani 1 1 d . . . C2 C 0.3320(5) 0.1294(2) 0.2460(4) 0.0339(12) Uani 1 1 d . . . H2 H 0.3946 0.1484 0.2297 0.041 Uiso 1 1 calc R . . C3 C 0.2380(5) 0.1598(2) 0.2613(3) 0.0296(11) Uani 1 1 d . . . C4 C 0.4425(5) 0.0420(2) 0.2431(3) 0.0302(11) Uani 1 1 d . . . C5 C 0.4647(6) -0.0061(3) 0.2821(4) 0.0470(17) Uani 1 1 d . . . H5 H 0.4138 -0.0197 0.3153 0.056 Uiso 1 1 calc R . . C6 C 0.5612(6) -0.0339(3) 0.2723(4) 0.0496(18) Uani 1 1 d . . . H6 H 0.5780 -0.0658 0.3015 0.059 Uiso 1 1 calc R . . C7 C 0.6087(5) 0.0267(3) 0.1832(4) 0.0373(13) Uani 1 1 d . . . H7 H 0.6577 0.0377 0.1472 0.045 Uiso 1 1 calc R . . C8 C 0.5145(6) 0.0581(2) 0.1918(4) 0.0380(14) Uani 1 1 d . . . H8 H 0.5001 0.0902 0.1627 0.046 Uiso 1 1 calc R . . C9 C 0.2409(5) 0.2210(2) 0.2630(3) 0.0321(12) Uani 1 1 d . . . C10 C 0.3355(5) 0.2519(3) 0.2644(5) 0.0489(18) Uani 1 1 d . . . H10 H 0.4055 0.2345 0.2614 0.059 Uiso 1 1 calc R . . C11 C 0.3285(6) 0.3094(3) 0.2702(5) 0.0496(18) Uani 1 1 d . . . H11 H 0.3952 0.3303 0.2720 0.060 Uiso 1 1 calc R . . C12 C 0.1407(6) 0.3057(3) 0.2688(5) 0.0517(19) Uani 1 1 d . . . H12 H 0.0716 0.3243 0.2692 0.062 Uiso 1 1 calc R . . C13 C 0.1406(5) 0.2488(3) 0.2637(4) 0.0453(16) Uani 1 1 d . . . H13 H 0.0726 0.2291 0.2607 0.054 Uiso 1 1 calc R . . C14 C 0.1213(4) 0.0163(2) 0.4202(3) 0.0266(11) Uani 1 1 d . C 2 C15 C 0.1375(5) -0.0374(2) 0.3942(3) 0.0295(11) Uani 1 1 d . . . H15 H 0.1664 -0.0643 0.4284 0.035 Uiso 1 1 calc R C 2 C16 C 0.1137(4) -0.0532(2) 0.3214(3) 0.0257(10) Uani 1 1 d . C . C17 C 0.1378(4) 0.0289(2) 0.5010(3) 0.0256(10) Uani 1 1 d . . . C18 C 0.1442(6) 0.0835(3) 0.5247(3) 0.0363(13) Uani 1 1 d . C . H18 H 0.1406 0.1128 0.4899 0.044 Uiso 1 1 calc R . . C19 C 0.1559(6) 0.0943(2) 0.6007(3) 0.0350(13) Uani 1 1 d . . . H19 H 0.1588 0.1316 0.6167 0.042 Uiso 1 1 calc R C . C20 C 0.1585(5) 0.0032(2) 0.6281(3) 0.0309(12) Uani 1 1 d . . . H20 H 0.1635 -0.0252 0.6642 0.037 Uiso 1 1 calc R C . C21 C 0.1466(5) -0.0119(2) 0.5549(3) 0.0322(12) Uani 1 1 d . C . H21 H 0.1444 -0.0497 0.5412 0.039 Uiso 1 1 calc R . . C22 C 0.1336(5) -0.1111(2) 0.2991(3) 0.0323(12) Uani 1 1 d . . . C23 C 0.1803(7) -0.1221(3) 0.2334(4) 0.0529(18) Uani 1 1 d . C . H23 H 0.2026 -0.0928 0.2031 0.063 Uiso 1 1 calc R . . C24 C 0.1943(10) -0.1762(4) 0.2122(5) 0.074(3) Uani 1 1 d . . . H24 H 0.2267 -0.1830 0.1668 0.089 Uiso 1 1 calc R C . C25 C 0.1199(8) -0.2087(3) 0.3144(5) 0.059(2) Uani 1 1 d . . . H25 H 0.0976 -0.2390 0.3430 0.071 Uiso 1 1 calc R C . C26 C 0.1028(7) -0.1559(3) 0.3413(4) 0.0484(17) Uani 1 1 d . C . H26 H 0.0709 -0.1505 0.3871 0.058 Uiso 1 1 calc R . . C27 C -0.1084(4) 0.1077(2) 0.1954(3) 0.0248(10) Uani 1 1 d . C . C28 C -0.0697(5) 0.1032(2) 0.1242(3) 0.0309(12) Uani 1 1 d . . . H28 H -0.1130 0.1188 0.0837 0.037 Uiso 1 1 calc R C 2 C29 C 0.0296(5) 0.0767(2) 0.1101(3) 0.0263(11) Uani 1 1 d . C 2 C30 C -0.2126(4) 0.1384(2) 0.2075(3) 0.0280(11) Uani 1 1 d . . . C31 C -0.2738(5) 0.1652(3) 0.1512(4) 0.0349(12) Uani 1 1 d . C . H31 H -0.2517 0.1640 0.1020 0.042 Uiso 1 1 calc R . . C32 C -0.3682(6) 0.1939(3) 0.1676(4) 0.0500(18) Uani 1 1 d . . . H32 H -0.4097 0.2117 0.1280 0.060 Uiso 1 1 calc R C . C33 C -0.3443(6) 0.1726(4) 0.2885(4) 0.0512(18) Uani 1 1 d . . . H33 H -0.3681 0.1753 0.3372 0.061 Uiso 1 1 calc R C . C34 C -0.2493(5) 0.1424(3) 0.2784(4) 0.0363(13) Uani 1 1 d . C . H34 H -0.2099 0.1247 0.3190 0.044 Uiso 1 1 calc R . . C35 C 0.0611(5) 0.0709(2) 0.0327(3) 0.0286(11) Uani 1 1 d . . . C36 C -0.0133(5) 0.0733(3) -0.0298(3) 0.0342(12) Uani 1 1 d . C . H36 H -0.0898 0.0798 -0.0244 0.041 Uiso 1 1 calc R . . C37 C 0.0240(5) 0.0663(3) -0.0989(3) 0.0352(13) Uani 1 1 d . . . H37 H -0.0289 0.0677 -0.1403 0.042 Uiso 1 1 calc R C . C38 C 0.2015(6) 0.0530(4) -0.0511(4) 0.0489(18) Uani 1 1 d . . . H38 H 0.2769 0.0449 -0.0582 0.059 Uiso 1 1 calc R C . C39 C 0.1706(6) 0.0594(3) 0.0207(4) 0.0458(17) Uani 1 1 d . C . H39 H 0.2243 0.0560 0.0614 0.055 Uiso 1 1 calc R . . C45 C 0.8625(17) 0.2561(6) 0.4877(11) 0.151(7) Uani 1 1 d . . . H45A H 0.8244 0.2588 0.5335 0.226 Uiso 0.50 1 calc PR B 1 H45B H 0.8102 0.2646 0.4453 0.226 Uiso 0.50 1 calc PR B 1 H45C H 0.9242 0.2823 0.4893 0.226 Uiso 0.50 1 calc PR B 1 H45D H 0.8815 0.2783 0.4453 0.226 Uiso 0.50 1 calc PR B 1 H45E H 0.8956 0.2725 0.5334 0.226 Uiso 0.50 1 calc PR B 1 H45F H 0.7816 0.2548 0.4894 0.226 Uiso 0.50 1 calc PR B 1 C46 C 0.9718(10) 0.1963(5) 0.3970(6) 0.080(3) Uani 1 1 d . . . H46A H 1.0060 0.1617 0.3823 0.120 Uiso 0.50 1 calc PR B 1 H46B H 1.0285 0.2251 0.4022 0.120 Uiso 0.50 1 calc PR B 1 H46C H 0.9141 0.2072 0.3590 0.120 Uiso 0.50 1 calc PR B 1 H46D H 0.9598 0.2343 0.3801 0.120 Uiso 0.50 1 calc PR B 1 H46E H 0.9372 0.1709 0.3602 0.120 Uiso 0.50 1 calc PR B 1 H46F H 1.0516 0.1889 0.4034 0.120 Uiso 0.50 1 calc PR B 1 Sb1A Sb 0.2622(2) 0.27603(7) 0.52162(10) 0.0964(6) Uani 0.45 1 d PD D 1 F1A F 0.1628(15) 0.2309(8) 0.5527(11) 0.151(8) Uiso 0.45 1 d PD D 1 F2A F 0.289(2) 0.2278(10) 0.4541(12) 0.264(18) Uiso 0.45 1 d PD D 1 F3A F 0.360(2) 0.3197(11) 0.4904(15) 0.65(8) Uiso 0.45 1 d PD D 1 F4A F 0.232(2) 0.3216(9) 0.5891(12) 0.260(17) Uiso 0.45 1 d PD D 1 F5A F 0.1638(18) 0.3056(9) 0.4608(12) 0.232(15) Uiso 0.45 1 d PD D 1 F6A F 0.3629(16) 0.2453(9) 0.5803(12) 0.180(10) Uiso 0.45 1 d PD D 1 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 Sb1 0.0643(6) 0.0695(7) 0.0501(6) 0.0036(5) -0.0046(5) 0.0076(5) Ag1 0.0445(3) 0.0283(2) 0.0234(2) -0.00066(15) 0.00802(17) 0.00930(17) Fe1 0.0282(4) 0.0222(4) 0.0207(4) 0.0021(3) 0.0030(3) 0.0040(3) S1 0.086(2) 0.067(2) 0.0552(18) -0.0017(15) 0.0085(16) 0.0164(18) S1A 0.176(15) 0.158(15) 0.091(9) 0.011(9) -0.003(9) 0.057(12) O1 0.0265(19) 0.0269(19) 0.032(2) 0.0061(15) 0.0026(15) 0.0054(15) O2 0.033(2) 0.0217(18) 0.037(2) 0.0032(15) 0.0067(16) 0.0034(15) O3 0.038(2) 0.0241(18) 0.0224(18) 0.0009(14) 0.0015(15) 0.0038(15) O4 0.034(2) 0.0230(18) 0.0249(18) -0.0003(14) 0.0004(15) 0.0017(15) O5 0.0285(19) 0.032(2) 0.0190(17) 0.0036(14) 0.0042(14) 0.0039(15) O6 0.034(2) 0.036(2) 0.0206(18) 0.0029(15) 0.0022(15) 0.0099(16) O7 0.177(10) 0.074(6) 0.113(7) 0.011(5) 0.027(7) -0.012(6) N1 0.034(3) 0.038(3) 0.040(3) 0.004(2) 0.006(2) 0.010(2) N2 0.040(3) 0.029(3) 0.048(3) 0.003(2) 0.008(2) -0.001(2) N3 0.033(2) 0.033(2) 0.022(2) 0.0012(18) 0.0030(18) -0.0015(19) N4 0.118(7) 0.034(3) 0.067(5) -0.014(3) -0.011(5) 0.017(4) N5 0.036(3) 0.070(4) 0.063(4) 0.001(3) 0.010(3) 0.023(3) N6 0.042(3) 0.042(3) 0.023(2) 0.000(2) 0.005(2) 0.001(2) C1 0.032(3) 0.030(3) 0.027(3) 0.001(2) 0.004(2) 0.005(2) C2 0.027(3) 0.029(3) 0.047(3) 0.003(2) 0.010(2) 0.004(2) C3 0.035(3) 0.027(3) 0.028(3) 0.003(2) 0.005(2) 0.003(2) C4 0.029(3) 0.028(3) 0.034(3) -0.003(2) 0.005(2) 0.005(2) C5 0.042(4) 0.043(4) 0.058(4) 0.018(3) 0.019(3) 0.015(3) C6 0.043(4) 0.050(4) 0.058(4) 0.024(3) 0.015(3) 0.021(3) C7 0.038(3) 0.031(3) 0.045(3) -0.003(2) 0.017(3) 0.001(2) C8 0.044(3) 0.021(3) 0.050(4) 0.003(2) 0.013(3) 0.007(2) C9 0.038(3) 0.025(3) 0.034(3) 0.001(2) 0.007(2) 0.002(2) C10 0.030(3) 0.030(3) 0.088(6) -0.008(3) 0.014(3) 0.002(3) C11 0.039(4) 0.029(3) 0.082(5) 0.000(3) 0.010(3) -0.001(3) C12 0.033(3) 0.027(3) 0.094(6) 0.006(3) 0.005(3) 0.003(3) C13 0.032(3) 0.030(3) 0.074(5) 0.002(3) 0.006(3) 0.002(3) C14 0.030(3) 0.026(3) 0.024(2) 0.002(2) 0.002(2) 0.001(2) C15 0.037(3) 0.027(3) 0.025(3) 0.002(2) 0.000(2) 0.005(2) C16 0.028(3) 0.022(2) 0.027(3) 0.0025(19) 0.002(2) 0.001(2) C17 0.030(3) 0.027(3) 0.020(2) 0.002(2) 0.0037(19) 0.000(2) C18 0.058(4) 0.029(3) 0.023(3) -0.001(2) 0.001(3) 0.004(3) C19 0.051(4) 0.027(3) 0.026(3) 0.001(2) 0.002(2) 0.003(2) C20 0.044(3) 0.026(3) 0.022(3) 0.002(2) 0.002(2) 0.000(2) C21 0.049(3) 0.023(3) 0.024(3) -0.001(2) 0.002(2) -0.005(2) C22 0.039(3) 0.027(3) 0.031(3) -0.002(2) 0.000(2) 0.005(2) C23 0.076(5) 0.041(4) 0.042(4) -0.003(3) 0.008(3) 0.012(4) C24 0.122(8) 0.048(5) 0.053(5) -0.016(4) 0.013(5) 0.028(5) C25 0.078(6) 0.030(3) 0.069(5) 0.001(3) -0.004(4) 0.006(3) C26 0.068(5) 0.032(3) 0.046(4) 0.003(3) 0.007(3) 0.006(3) C27 0.028(3) 0.020(2) 0.027(3) 0.0020(19) 0.006(2) 0.0005(19) C28 0.032(3) 0.035(3) 0.025(3) 0.006(2) 0.002(2) 0.009(2) C29 0.032(3) 0.025(3) 0.022(2) -0.0004(19) 0.003(2) 0.001(2) C30 0.028(3) 0.023(3) 0.033(3) 0.001(2) 0.003(2) -0.001(2) C31 0.029(3) 0.039(3) 0.037(3) 0.006(2) 0.003(2) 0.005(2) C32 0.033(3) 0.068(5) 0.048(4) 0.008(3) 0.001(3) 0.016(3) C33 0.043(4) 0.067(5) 0.046(4) -0.001(3) 0.015(3) 0.013(3) C34 0.033(3) 0.039(3) 0.038(3) 0.000(3) 0.009(2) 0.005(2) C35 0.036(3) 0.030(3) 0.020(2) 0.001(2) 0.006(2) 0.004(2) C36 0.036(3) 0.041(3) 0.025(3) 0.003(2) -0.001(2) -0.001(2) C37 0.041(3) 0.039(3) 0.026(3) -0.001(2) 0.001(2) 0.001(2) C38 0.034(3) 0.085(5) 0.029(3) -0.005(3) 0.007(3) 0.013(3) C39 0.035(3) 0.077(5) 0.026(3) 0.002(3) 0.004(2) 0.015(3) C45 0.22(2) 0.083(10) 0.156(17) -0.010(10) 0.062(14) 0.048(11) C46 0.081(7) 0.073(7) 0.086(7) -0.018(5) 0.005(5) -0.001(5) Sb1A 0.1411(17) 0.0668(10) 0.0752(11) -0.0009(8) -0.0347(11) -0.0148(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 Sb1 F3 1.716(12) . ? Sb1 F6 1.788(12) . ? Sb1 F5 1.794(11) . ? Sb1 F2 1.795(11) . ? Sb1 F4 1.818(11) . ? Sb1 F1 1.837(11) . ? Ag1 N6 2.245(5) . ? Ag1 N3 2.315(5) 1_554 ? Ag1 N1 2.364(5) 3_655 ? Ag1 N2 2.381(5) 4_565 ? Fe1 O3 1.981(4) . ? Fe1 O4 1.991(4) . ? Fe1 O5 1.991(4) . ? Fe1 O1 1.991(4) . ? Fe1 O2 1.991(4) . ? Fe1 O6 1.992(4) . ? S1 O7 1.445(12) . ? S1 C46 1.684(12) . ? S1 C45 1.797(14) . ? S1A O7 1.48(2) . ? S1A C45 1.62(2) . ? S1A C46 1.72(2) . ? F1 F1 1.68(2) 3_666 ? O1 C1 1.272(7) . ? O2 C3 1.275(7) . ? O3 C14 1.285(6) . ? O4 C16 1.277(6) . ? O5 C27 1.288(6) . ? O6 C29 1.269(7) . ? N1 C7 1.330(8) . ? N1 C6 1.344(9) . ? N1 Ag1 2.364(5) 3_655 ? N2 C11 1.314(9) . ? N2 C12 1.341(9) . ? N2 Ag1 2.381(5) 4_566 ? N3 C20 1.323(7) . ? N3 C19 1.329(7) . ? N3 Ag1 2.315(5) 1_556 ? N4 C25 1.316(13) . ? N4 C24 1.335(13) . ? N5 C32 1.320(10) . ? N5 C33 1.332(10) . ? N6 C37 1.332(8) . ? N6 C38 1.347(9) . ? C1 C2 1.392(8) . ? C1 C4 1.499(8) . ? C2 C3 1.398(8) . ? C3 C9 1.486(8) . ? C4 C8 1.375(9) . ? C4 C5 1.382(9) . ? C5 C6 1.371(9) . ? C7 C8 1.389(8) . ? C9 C10 1.366(9) . ? C9 C13 1.389(9) . ? C10 C11 1.405(9) . ? C12 C13 1.384(9) . ? C14 C15 1.403(8) . ? C14 C17 1.496(7) . ? C15 C16 1.384(8) . ? C16 C22 1.487(7) . ? C17 C21 1.389(8) . ? C17 C18 1.394(8) . ? C18 C19 1.399(8) . ? C20 C21 1.375(8) . ? C22 C23 1.380(10) . ? C22 C26 1.394(9) . ? C23 C24 1.383(11) . ? C25 C26 1.393(10) . ? C27 C28 1.408(8) . ? C27 C30 1.493(7) . ? C28 C29 1.401(8) . ? C29 C35 1.486(7) . ? C30 C31 1.378(8) . ? C30 C34 1.393(8) . ? C31 C32 1.388(9) . ? C33 C34 1.387(9) . ? C35 C39 1.385(9) . ? C35 C36 1.394(8) . ? C36 C37 1.371(9) . ? C38 C39 1.388(9) . ? Sb1A F4A 1.709(19) . ? Sb1A F3A 1.72(2) . ? Sb1A F5A 1.72(2) . ? Sb1A F6A 1.726(18) . ? Sb1A F2A 1.740(19) . ? Sb1A F1A 1.749(17) . ? 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 F3 Sb1 F6 92.4(5) . . ? F3 Sb1 F5 91.6(5) . . ? F6 Sb1 F5 175.7(6) . . ? F3 Sb1 F2 94.8(5) . . ? F6 Sb1 F2 91.2(5) . . ? F5 Sb1 F2 89.9(5) . . ? F3 Sb1 F4 90.0(5) . . ? F6 Sb1 F4 89.6(5) . . ? F5 Sb1 F4 88.9(5) . . ? F2 Sb1 F4 175.1(5) . . ? F3 Sb1 F1 177.6(6) . . ? F6 Sb1 F1 87.7(5) . . ? F5 Sb1 F1 88.2(5) . . ? F2 Sb1 F1 87.7(5) . . ? F4 Sb1 F1 87.5(5) . . ? N6 Ag1 N3 144.69(18) . 1_554 ? N6 Ag1 N1 108.89(19) . 3_655 ? N3 Ag1 N1 91.24(18) 1_554 3_655 ? N6 Ag1 N2 102.47(19) . 4_565 ? N3 Ag1 N2 96.98(18) 1_554 4_565 ? N1 Ag1 N2 110.14(19) 3_655 4_565 ? O3 Fe1 O4 86.89(16) . . ? O3 Fe1 O5 92.54(16) . . ? O4 Fe1 O5 101.70(16) . . ? O3 Fe1 O1 93.57(16) . . ? O4 Fe1 O1 84.97(16) . . ? O5 Fe1 O1 171.19(16) . . ? O3 Fe1 O2 91.34(16) . . ? O4 Fe1 O2 170.24(16) . . ? O5 Fe1 O2 87.96(16) . . ? O1 Fe1 O2 85.56(16) . . ? O3 Fe1 O6 174.81(17) . . ? O4 Fe1 O6 88.17(16) . . ? O5 Fe1 O6 86.94(15) . . ? O1 Fe1 O6 87.54(16) . . ? O2 Fe1 O6 93.80(17) . . ? O7 S1 C46 109.4(6) . . ? O7 S1 C45 106.9(9) . . ? C46 S1 C45 97.6(7) . . ? O7 S1A C45 114.5(12) . . ? O7 S1A C46 105.5(11) . . ? C45 S1A C46 103.0(14) . . ? F1 F1 Sb1 152.6(13) 3_666 . ? C1 O1 Fe1 127.9(4) . . ? C3 O2 Fe1 129.9(4) . . ? C14 O3 Fe1 126.2(3) . . ? C16 O4 Fe1 124.2(3) . . ? C27 O5 Fe1 128.6(3) . . ? C29 O6 Fe1 129.5(4) . . ? S1 O7 S1A 50.0(8) . . ? C7 N1 C6 117.7(5) . . ? C7 N1 Ag1 124.9(4) . 3_655 ? C6 N1 Ag1 117.2(4) . 3_655 ? C11 N2 C12 117.4(6) . . ? C11 N2 Ag1 129.7(4) . 4_566 ? C12 N2 Ag1 112.7(4) . 4_566 ? C20 N3 C19 117.6(5) . . ? C20 N3 Ag1 116.5(4) . 1_556 ? C19 N3 Ag1 125.7(4) . 1_556 ? C25 N4 C24 116.8(7) . . ? C32 N5 C33 116.0(6) . . ? C37 N6 C38 116.5(5) . . ? C37 N6 Ag1 123.8(4) . . ? C38 N6 Ag1 118.5(4) . . ? O1 C1 C2 125.0(5) . . ? O1 C1 C4 114.3(5) . . ? C2 C1 C4 120.6(5) . . ? C1 C2 C3 122.3(5) . . ? O2 C3 C2 124.0(5) . . ? O2 C3 C9 115.1(5) . . ? C2 C3 C9 120.9(5) . . ? C8 C4 C5 118.5(5) . . ? C8 C4 C1 122.2(5) . . ? C5 C4 C1 119.1(5) . . ? C6 C5 C4 119.1(6) . . ? N1 C6 C5 122.9(6) . . ? N1 C7 C8 122.8(6) . . ? C4 C8 C7 118.9(6) . . ? C10 C9 C13 117.5(6) . . ? C10 C9 C3 124.5(6) . . ? C13 C9 C3 117.9(6) . . ? C9 C10 C11 119.5(6) . . ? N2 C11 C10 123.1(6) . . ? N2 C12 C13 123.0(6) . . ? C12 C13 C9 119.3(6) . . ? O3 C14 C15 123.6(5) . . ? O3 C14 C17 115.9(5) . . ? C15 C14 C17 120.5(5) . . ? C16 C15 C14 123.6(5) . . ? O4 C16 C15 125.0(5) . . ? O4 C16 C22 115.3(5) . . ? C15 C16 C22 119.7(5) . . ? C21 C17 C18 117.5(5) . . ? C21 C17 C14 122.6(5) . . ? C18 C17 C14 119.9(5) . . ? C17 C18 C19 118.8(5) . . ? N3 C19 C18 122.9(6) . . ? N3 C20 C21 124.2(5) . . ? C20 C21 C17 119.0(5) . . ? C23 C22 C26 117.7(6) . . ? C23 C22 C16 120.0(6) . . ? C26 C22 C16 122.2(6) . . ? C22 C23 C24 119.2(8) . . ? N4 C24 C23 123.7(8) . . ? N4 C25 C26 124.3(8) . . ? C25 C26 C22 118.3(7) . . ? O5 C27 C28 123.9(5) . . ? O5 C27 C30 115.2(5) . . ? C28 C27 C30 120.9(5) . . ? C29 C28 C27 123.3(5) . . ? O6 C29 C28 124.8(5) . . ? O6 C29 C35 115.5(5) . . ? C28 C29 C35 119.7(5) . . ? C31 C30 C34 117.4(5) . . ? C31 C30 C27 122.7(5) . . ? C34 C30 C27 119.8(5) . . ? C30 C31 C32 118.9(6) . . ? N5 C32 C31 124.7(6) . . ? N5 C33 C34 124.2(7) . . ? C33 C34 C30 118.7(6) . . ? C39 C35 C36 116.7(5) . . ? C39 C35 C29 118.6(5) . . ? C36 C35 C29 124.6(5) . . ? C37 C36 C35 120.1(6) . . ? N6 C37 C36 123.8(6) . . ? N6 C38 C39 123.3(6) . . ? C35 C39 C38 119.6(6) . . ? S1A C45 S1 42.1(6) . . ? S1 C46 S1A 42.6(6) . . ? F4A Sb1A F3A 91.5(7) . . ? F4A Sb1A F5A 90.8(7) . . ? F3A Sb1A F5A 89.6(7) . . ? F4A Sb1A F6A 91.0(7) . . ? F3A Sb1A F6A 89.8(7) . . ? F5A Sb1A F6A 178.1(8) . . ? F4A Sb1A F2A 177.6(9) . . ? F3A Sb1A F2A 91.0(7) . . ? F5A Sb1A F2A 89.1(7) . . ? F6A Sb1A F2A 89.0(7) . . ? F4A Sb1A F1A 89.3(7) . . ? F3A Sb1A F1A 179.3(9) . . ? F5A Sb1A F1A 90.5(7) . . ? F6A Sb1A F1A 90.0(6) . . ? F2A Sb1A F1A 88.3(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.838 _refine_diff_density_min -1.962 _refine_diff_density_rms 0.193 #===end data_compound12_k07adb11 _database_code_depnum_ccdc_archive 'CCDC 853065' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 Ag2 Cl2 Fe N9 O12' _chemical_formula_weight 1197.26 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' Fe Fe 0.3463 0.8444 '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' Cl Cl 0.1484 0.1585 '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 11.7140(3) _cell_length_b 14.0930(5) _cell_length_c 15.5890(6) _cell_angle_alpha 100.969(2) _cell_angle_beta 109.712(2) _cell_angle_gamma 103.542(2) _cell_volume 2251.11(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 151495 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1194 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.93 _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32276 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 32276 _reflns_number_gt 25177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0507P)^2^+37.8924P] 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 SHELXL _refine_ls_extinction_coef 0.0118(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 32276 _refine_ls_number_parameters 616 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.1066 _refine_ls_wR_factor_ref 0.2594 _refine_ls_wR_factor_gt 0.2402 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.91434(5) 0.50038(5) 0.27677(4) 0.0432(2) Uani 1 1 d . . . Ag2 Ag 0.84249(5) 0.82285(5) 0.25576(4) 0.0444(2) Uani 1 1 d . . . Fe1 Fe 0.55878(9) 0.78887(8) 0.58869(7) 0.0317(2) Uani 1 1 d . . . Cl1 Cl 0.5158(3) 0.4890(3) 0.1568(2) 0.0897(9) Uani 1 1 d . . . Cl2 Cl 0.3697(3) 0.6306(2) 0.1557(2) 0.0795(7) Uani 1 1 d . . . O1 O 0.6885(4) 0.7222(4) 0.5794(3) 0.0358(11) Uani 1 1 d . . . O2 O 0.4291(4) 0.6602(4) 0.4933(3) 0.0352(11) Uani 1 1 d . . . O3 O 0.5813(4) 0.8487(4) 0.4870(3) 0.0363(11) Uani 1 1 d . . . O4 O 0.4194(4) 0.8504(4) 0.5763(3) 0.0348(11) Uani 1 1 d . . . O5 O 0.5197(4) 0.7436(4) 0.6913(3) 0.0368(11) Uani 1 1 d . . . O6 O 0.7037(4) 0.9004(4) 0.6910(3) 0.0313(10) Uani 1 1 d . . . O7 O 0.8446(7) 0.6440(5) 0.2240(5) 0.0677(17) Uani 1 1 d . . . O8 O 0.8216(7) 0.5309(5) 0.0982(5) 0.0738(18) Uani 1 1 d . . . O9 O 0.7326(7) 0.6491(5) 0.0853(5) 0.081(2) Uani 1 1 d . . . O10 O 0.7325(7) 1.0254(5) 1.0657(4) 0.0740(19) Uani 1 1 d . . . O11 O 0.7861(8) 1.1182(6) 1.2087(5) 0.085(2) Uani 1 1 d . . . O12 O 0.9003(9) 1.1597(6) 1.1340(7) 0.127(4) Uani 1 1 d . . . N1 N 0.9246(5) 0.5863(5) 0.4227(4) 0.0390(14) Uani 1 1 d . . . N2 N 0.0981(5) 0.4787(4) 0.2721(4) 0.0350(13) Uani 1 1 d . . . N3 N 0.6656(5) 0.8568(5) 0.2566(4) 0.0368(13) Uani 1 1 d . . . N4 N 0.0018(5) 0.8555(5) 0.4086(4) 0.0410(14) Uani 1 1 d . . . N5 N 0.2689(6) 0.6429(5) 0.8049(5) 0.0436(15) Uani 1 1 d . . . N6 N 1.0580(6) 1.1109(5) 0.8335(4) 0.0497(16) Uani 1 1 d . . . N7 N 0.7996(7) 0.6086(5) 0.1367(6) 0.0564(18) Uani 1 1 d . . . N8 N 0.1465(10) 0.7420(9) 0.2047(7) 0.093(3) Uani 1 1 d . . . N9 N 0.8117(8) 1.1047(6) 1.1379(6) 0.066(2) Uani 1 1 d . . . C1 C 1.0264(6) 0.6217(6) 0.5064(5) 0.0399(17) Uani 1 1 d . . . H1 H 1.1030 0.6092 0.5072 0.048 Uiso 1 1 calc R . . C2 C 1.0288(7) 0.6748(6) 0.5911(5) 0.0386(16) Uani 1 1 d . . . H2 H 1.1055 0.7020 0.6474 0.046 Uiso 1 1 calc R . . C3 C 0.9160(6) 0.6868(6) 0.5911(5) 0.0365(16) Uani 1 1 d . . . H3 H 0.9139 0.7231 0.6482 0.044 Uiso 1 1 calc R . . C4 C 0.8042(6) 0.6463(5) 0.5080(4) 0.0301(14) Uani 1 1 d . . . C5 C 0.8153(6) 0.5992(6) 0.4240(5) 0.0372(16) Uani 1 1 d . . . H5 H 0.7417 0.5754 0.3656 0.045 Uiso 1 1 calc R . . C6 C 0.6803(6) 0.6571(5) 0.5055(5) 0.0336(15) Uani 1 1 d . . . C7 C 0.5652(7) 0.5972(6) 0.4317(5) 0.0409(17) Uani 1 1 d . . . H7 H 0.5680 0.5538 0.3783 0.049 Uiso 1 1 calc R . . C8 C 0.4432(6) 0.5958(5) 0.4299(5) 0.0326(15) Uani 1 1 d . . . C9 C 0.3268(6) 0.5202(5) 0.3528(5) 0.0323(15) Uani 1 1 d . . . C10 C 0.3230(7) 0.4317(5) 0.2986(5) 0.0371(17) Uani 1 1 d . . . H10 H 0.3994 0.4151 0.3069 0.045 Uiso 1 1 calc R . . C11 C 0.2060(7) 0.3654(6) 0.2306(6) 0.0482(19) Uani 1 1 d . . . H11 H 0.2023 0.3029 0.1919 0.058 Uiso 1 1 calc R . . C12 C 0.0951(8) 0.3888(6) 0.2186(6) 0.0467(19) Uani 1 1 d . . . H12 H 0.0155 0.3418 0.1725 0.056 Uiso 1 1 calc R . . C13 C 0.2095(6) 0.5422(6) 0.3357(5) 0.0366(16) Uani 1 1 d . . . H13 H 0.2120 0.6056 0.3719 0.044 Uiso 1 1 calc R . . C14 C 0.4952(6) 0.8627(5) 0.4190(5) 0.0290(14) Uani 1 1 d . . . C15 C 0.5273(6) 0.8768(5) 0.3380(5) 0.0330(15) Uani 1 1 d . . . C16 C 0.6235(7) 0.8453(6) 0.3261(5) 0.0380(16) Uani 1 1 d . . . H16 H 0.6643 0.8128 0.3698 0.046 Uiso 1 1 calc R . . C17 C 0.6065(6) 0.9034(6) 0.1964(5) 0.0410(17) Uani 1 1 d . . . H17 H 0.6343 0.9137 0.1473 0.049 Uiso 1 1 calc R . . C18 C 0.5080(7) 0.9369(6) 0.2025(5) 0.0363(16) Uani 1 1 d . . . H18 H 0.4679 0.9678 0.1570 0.044 Uiso 1 1 calc R . . C19 C 0.4673(7) 0.9262(6) 0.2732(6) 0.0445(18) Uani 1 1 d . . . H19 H 0.4007 0.9510 0.2791 0.053 Uiso 1 1 calc R . . C20 C 0.3774(7) 0.8670(6) 0.4224(5) 0.0418(17) Uani 1 1 d . . . H20 H 0.3158 0.8741 0.3680 0.050 Uiso 1 1 calc R . . C21 C 0.3449(6) 0.8615(5) 0.5013(5) 0.0366(16) Uani 1 1 d . . . C22 C 0.2191(6) 0.8705(5) 0.4967(5) 0.0326(15) Uani 1 1 d . . . C23 C 0.1160(6) 0.8486(5) 0.4131(5) 0.0377(16) Uani 1 1 d . . . H23 H 0.1255 0.8275 0.3550 0.045 Uiso 1 1 calc R . . C24 C -0.0126(7) 0.8834(5) 0.4902(5) 0.0361(16) Uani 1 1 d . . . H24 H -0.0927 0.8888 0.4883 0.043 Uiso 1 1 calc R . . C25 C 0.0874(6) 0.9047(5) 0.5776(5) 0.0370(16) Uani 1 1 d . . . H25 H 0.0751 0.9241 0.6348 0.044 Uiso 1 1 calc R . . C26 C 0.2041(7) 0.8977(5) 0.5820(5) 0.0339(15) Uani 1 1 d . . . H26 H 0.2727 0.9111 0.6415 0.041 Uiso 1 1 calc R . . C27 C 0.5577(7) 0.7949(6) 0.7789(5) 0.0376(16) Uani 1 1 d . . . C28 C 0.4694(6) 0.7595(5) 0.8252(5) 0.0364(16) Uani 1 1 d . . . C29 C 0.3540(6) 0.6799(5) 0.7693(5) 0.0350(16) Uani 1 1 d . . . H29 H 0.3352 0.6511 0.7039 0.042 Uiso 1 1 calc R . . C30 C 0.2928(8) 0.6858(7) 0.8947(6) 0.057(2) Uani 1 1 d . . . H30 H 0.2332 0.6593 0.9200 0.068 Uiso 1 1 calc R . . C31 C 0.3994(9) 0.7666(8) 0.9527(7) 0.074(3) Uani 1 1 d . . . H31 H 0.4113 0.7965 1.0164 0.089 Uiso 1 1 calc R . . C32 C 0.4911(8) 0.8057(8) 0.9191(6) 0.063(3) Uani 1 1 d . . . H32 H 0.5660 0.8619 0.9589 0.076 Uiso 1 1 calc R . . C33 C 0.6644(6) 0.8806(5) 0.8251(5) 0.0323(15) Uani 1 1 d . . . H33 H 0.6893 0.9108 0.8913 0.039 Uiso 1 1 calc R . . C34 C 0.7389(6) 0.9261(5) 0.7805(5) 0.0334(15) Uani 1 1 d . . . C35 C 0.8643(7) 1.0097(6) 0.8376(5) 0.0388(16) Uani 1 1 d . . . C36 C 0.9419(6) 1.0380(6) 0.7902(5) 0.0397(17) Uani 1 1 d . . . H36 H 0.9119 1.0045 0.7240 0.048 Uiso 1 1 calc R . . C37 C 1.0998(8) 1.1554(7) 0.9274(6) 0.066(3) Uani 1 1 d . . . H37 H 1.1830 1.2046 0.9592 0.080 Uiso 1 1 calc R . . C38 C 1.0274(9) 1.1334(8) 0.9813(6) 0.071(3) Uani 1 1 d . . . H38 H 1.0592 1.1673 1.0475 0.085 Uiso 1 1 calc R . . C39 C 0.9070(8) 1.0596(7) 0.9331(6) 0.060(2) Uani 1 1 d . . . H39 H 0.8538 1.0435 0.9663 0.072 Uiso 1 1 calc R . . C40 C 0.0429(14) 0.6443(11) 0.0238(8) 0.099(4) Uani 1 1 d . . . H40A H 0.0415 0.5732 0.0146 0.148 Uiso 1 1 calc R . . H40B H 0.0939 0.6775 -0.0072 0.148 Uiso 1 1 calc R . . H40C H -0.0449 0.6459 -0.0044 0.148 Uiso 1 1 calc R . . C41 C 0.1021(13) 0.7006(14) 0.1302(12) 0.112(5) Uani 1 1 d . . . C42 C 0.4517(10) 0.5724(9) 0.0987(7) 0.072(3) Uani 1 1 d . . . H42A H 0.5222 0.6258 0.0970 0.087 Uiso 1 1 calc R . . H42B H 0.3924 0.5335 0.0321 0.087 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 0.0307(3) 0.0479(4) 0.0463(4) 0.0017(3) 0.0195(3) 0.0080(3) Ag2 0.0300(3) 0.0584(4) 0.0466(4) 0.0137(3) 0.0204(3) 0.0113(3) Fe1 0.0316(5) 0.0357(6) 0.0269(5) 0.0040(4) 0.0141(4) 0.0102(4) Cl1 0.099(2) 0.112(2) 0.087(2) 0.0443(19) 0.0440(18) 0.064(2) Cl2 0.0878(18) 0.0742(17) 0.0763(17) 0.0088(14) 0.0368(15) 0.0309(15) O1 0.034(2) 0.043(3) 0.030(3) 0.005(2) 0.014(2) 0.016(2) O2 0.035(2) 0.041(3) 0.031(3) 0.005(2) 0.017(2) 0.013(2) O3 0.029(2) 0.042(3) 0.040(3) 0.010(2) 0.019(2) 0.012(2) O4 0.032(2) 0.045(3) 0.027(3) 0.006(2) 0.011(2) 0.019(2) O5 0.036(3) 0.039(3) 0.034(3) 0.001(2) 0.020(2) 0.009(2) O6 0.032(2) 0.039(3) 0.021(2) 0.004(2) 0.012(2) 0.010(2) O7 0.090(5) 0.054(4) 0.049(4) 0.011(3) 0.020(4) 0.019(3) O8 0.101(5) 0.045(4) 0.065(4) 0.005(3) 0.032(4) 0.017(4) O9 0.100(5) 0.046(4) 0.080(5) 0.026(4) 0.017(4) 0.016(4) O10 0.089(5) 0.060(4) 0.047(4) -0.005(3) 0.031(4) -0.010(4) O11 0.108(6) 0.077(5) 0.045(4) 0.004(3) 0.029(4) -0.003(4) O12 0.118(7) 0.074(5) 0.152(9) -0.037(5) 0.101(7) -0.046(5) N1 0.028(3) 0.045(4) 0.044(4) 0.009(3) 0.017(3) 0.013(3) N2 0.033(3) 0.040(3) 0.030(3) 0.002(3) 0.015(3) 0.012(3) N3 0.033(3) 0.046(4) 0.033(3) 0.009(3) 0.018(3) 0.011(3) N4 0.025(3) 0.057(4) 0.043(4) 0.009(3) 0.018(3) 0.016(3) N5 0.035(3) 0.044(4) 0.051(4) 0.007(3) 0.024(3) 0.008(3) N6 0.037(3) 0.064(5) 0.033(4) 0.011(3) 0.009(3) -0.001(3) N7 0.069(5) 0.037(4) 0.055(5) 0.015(4) 0.018(4) 0.014(4) N8 0.087(7) 0.127(9) 0.036(5) -0.008(5) 0.012(5) 0.025(6) N9 0.076(6) 0.060(5) 0.061(5) 0.015(4) 0.033(5) 0.014(5) C1 0.026(3) 0.049(5) 0.041(4) 0.002(3) 0.016(3) 0.009(3) C2 0.038(4) 0.041(4) 0.038(4) 0.009(3) 0.016(3) 0.016(3) C3 0.038(4) 0.042(4) 0.034(4) 0.015(3) 0.017(3) 0.014(3) C4 0.035(4) 0.030(4) 0.024(3) 0.004(3) 0.013(3) 0.011(3) C5 0.026(3) 0.043(4) 0.047(4) 0.011(3) 0.023(3) 0.007(3) C6 0.034(4) 0.040(4) 0.035(4) 0.017(3) 0.020(3) 0.014(3) C7 0.033(4) 0.046(4) 0.035(4) -0.008(3) 0.018(3) 0.007(3) C8 0.037(4) 0.041(4) 0.026(4) 0.005(3) 0.018(3) 0.019(3) C9 0.031(3) 0.035(4) 0.034(4) 0.008(3) 0.022(3) 0.007(3) C10 0.040(4) 0.037(4) 0.048(5) 0.017(4) 0.027(4) 0.020(3) C11 0.038(4) 0.036(4) 0.061(5) -0.002(4) 0.018(4) 0.010(3) C12 0.044(4) 0.047(5) 0.047(5) 0.002(4) 0.025(4) 0.009(4) C13 0.028(4) 0.041(4) 0.040(4) 0.009(3) 0.019(3) 0.005(3) C14 0.022(3) 0.024(3) 0.029(4) 0.000(3) 0.001(3) 0.008(3) C15 0.024(3) 0.037(4) 0.028(4) -0.002(3) 0.009(3) 0.006(3) C16 0.036(4) 0.044(4) 0.039(4) 0.014(3) 0.018(3) 0.016(3) C17 0.030(4) 0.046(5) 0.039(4) 0.005(3) 0.015(3) 0.002(3) C18 0.043(4) 0.044(4) 0.019(3) 0.008(3) 0.008(3) 0.015(3) C19 0.048(4) 0.038(4) 0.053(5) 0.010(4) 0.024(4) 0.021(4) C20 0.031(4) 0.059(5) 0.037(4) 0.013(4) 0.016(3) 0.016(4) C21 0.026(3) 0.035(4) 0.038(4) -0.004(3) 0.009(3) 0.008(3) C22 0.031(3) 0.036(4) 0.038(4) 0.013(3) 0.018(3) 0.014(3) C23 0.033(4) 0.039(4) 0.044(4) 0.006(3) 0.022(4) 0.013(3) C24 0.041(4) 0.035(4) 0.045(4) 0.012(3) 0.025(4) 0.024(3) C25 0.036(4) 0.040(4) 0.037(4) 0.005(3) 0.023(3) 0.007(3) C26 0.039(4) 0.029(4) 0.034(4) 0.004(3) 0.016(3) 0.013(3) C27 0.037(4) 0.049(5) 0.035(4) 0.015(4) 0.021(3) 0.017(4) C28 0.032(4) 0.037(4) 0.032(4) 0.005(3) 0.014(3) -0.001(3) C29 0.028(3) 0.038(4) 0.037(4) 0.003(3) 0.019(3) 0.005(3) C30 0.062(5) 0.054(5) 0.037(5) -0.003(4) 0.028(4) -0.011(4) C31 0.065(6) 0.080(7) 0.045(5) -0.010(5) 0.034(5) -0.029(5) C32 0.045(5) 0.075(6) 0.040(5) -0.012(4) 0.023(4) -0.019(4) C33 0.033(4) 0.029(4) 0.036(4) 0.003(3) 0.020(3) 0.005(3) C34 0.029(3) 0.035(4) 0.039(4) 0.015(3) 0.014(3) 0.012(3) C35 0.038(4) 0.039(4) 0.032(4) 0.009(3) 0.014(3) 0.000(3) C36 0.028(4) 0.048(5) 0.040(4) 0.014(4) 0.014(3) 0.007(3) C37 0.044(5) 0.069(6) 0.044(5) 0.006(4) 0.007(4) -0.033(4) C38 0.058(5) 0.084(7) 0.034(5) 0.004(4) 0.015(4) -0.026(5) C39 0.051(5) 0.066(6) 0.050(5) 0.009(4) 0.027(4) -0.007(4) C40 0.130(11) 0.126(11) 0.059(7) 0.025(7) 0.044(8) 0.067(9) C41 0.080(9) 0.180(16) 0.103(12) 0.049(11) 0.053(9) 0.059(10) C42 0.063(6) 0.105(9) 0.051(6) 0.023(6) 0.022(5) 0.031(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 N2 2.267(5) 1_655 ? Ag1 N1 2.315(6) . ? Ag1 N5 2.335(6) 2_666 ? Ag1 O7 2.528(6) . ? Ag2 N3 2.237(5) . ? Ag2 N6 2.291(6) 2_776 ? Ag2 N4 2.356(6) 1_655 ? Ag2 O7 2.483(6) . ? Fe1 O6 1.966(5) . ? Fe1 O5 1.979(5) . ? Fe1 O2 1.992(5) . ? Fe1 O4 1.992(4) . ? Fe1 O1 1.994(4) . ? Fe1 O3 1.996(5) . ? Cl1 C42 1.768(10) . ? Cl2 C42 1.748(9) . ? O1 C6 1.289(8) . ? O2 C8 1.291(7) . ? O3 C14 1.278(7) . ? O4 C21 1.264(8) . ? O5 C27 1.285(8) . ? O6 C34 1.264(8) . ? O7 N7 1.231(9) . ? O8 N7 1.269(9) . ? O9 N7 1.243(9) . ? O10 N9 1.307(10) . ? O11 N9 1.231(9) . ? O12 N9 1.168(10) . ? N1 C1 1.340(9) . ? N1 C5 1.340(8) . ? N2 C13 1.314(9) . ? N2 C12 1.364(9) . ? N2 Ag1 2.267(5) 1_455 ? N3 C17 1.342(9) . ? N3 C16 1.353(8) . ? N4 C24 1.337(9) . ? N4 C23 1.343(8) . ? N4 Ag2 2.356(6) 1_455 ? N5 C30 1.320(10) . ? N5 C29 1.346(8) . ? N5 Ag1 2.335(6) 2_666 ? N6 C37 1.341(11) . ? N6 C36 1.350(10) . ? N6 Ag2 2.291(6) 2_776 ? N8 C41 1.073(17) . ? C1 C2 1.377(10) . ? C1 H1 0.9500 . ? C2 C3 1.371(9) . ? C2 H2 0.9500 . ? C3 C4 1.394(10) . ? C3 H3 0.9500 . ? C4 C5 1.413(9) . ? C4 C6 1.482(9) . ? C5 H5 0.9500 . ? C6 C7 1.381(10) . ? C7 C8 1.415(9) . ? C7 H7 0.9500 . ? C8 C9 1.472(10) . ? C9 C10 1.350(10) . ? C9 C13 1.428(9) . ? C10 C11 1.385(11) . ? C10 H10 0.9500 . ? C11 C12 1.375(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C20 1.414(9) . ? C14 C15 1.468(9) . ? C15 C16 1.359(9) . ? C15 C19 1.420(10) . ? C16 H16 0.9500 . ? C17 C18 1.369(9) . ? C17 H17 0.9500 . ? C18 C19 1.360(10) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.416(10) . ? C20 H20 0.9500 . ? C21 C22 1.488(9) . ? C22 C23 1.364(10) . ? C22 C26 1.394(9) . ? C23 H23 0.9500 . ? C24 C25 1.387(10) . ? C24 H24 0.9500 . ? C25 C26 1.373(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C33 1.376(10) . ? C27 C28 1.496(9) . ? C28 C32 1.393(10) . ? C28 C29 1.402(10) . ? C29 H29 0.9500 . ? C30 C31 1.361(12) . ? C30 H30 0.9500 . ? C31 C32 1.395(11) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.405(9) . ? C33 H33 0.9500 . ? C34 C35 1.499(10) . ? C35 C39 1.376(11) . ? C35 C36 1.389(9) . ? C36 H36 0.9500 . ? C37 C38 1.407(11) . ? C37 H37 0.9500 . ? C38 C39 1.392(12) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.53(2) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 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 N2 Ag1 N1 117.0(2) 1_655 . ? N2 Ag1 N5 115.5(2) 1_655 2_666 ? N1 Ag1 N5 112.5(2) . 2_666 ? N2 Ag1 O7 119.7(2) 1_655 . ? N1 Ag1 O7 83.8(2) . . ? N5 Ag1 O7 104.0(2) 2_666 . ? N3 Ag2 N6 119.4(2) . 2_776 ? N3 Ag2 N4 114.22(19) . 1_655 ? N6 Ag2 N4 107.3(2) 2_776 1_655 ? N3 Ag2 O7 120.1(2) . . ? N6 Ag2 O7 103.5(2) 2_776 . ? N4 Ag2 O7 87.2(2) 1_655 . ? O6 Fe1 O5 86.50(19) . . ? O6 Fe1 O2 170.04(18) . . ? O5 Fe1 O2 89.78(19) . . ? O6 Fe1 O4 99.95(19) . . ? O5 Fe1 O4 85.65(18) . . ? O2 Fe1 O4 88.96(19) . . ? O6 Fe1 O1 85.91(19) . . ? O5 Fe1 O1 101.33(19) . . ? O2 Fe1 O1 85.77(19) . . ? O4 Fe1 O1 171.22(19) . . ? O6 Fe1 O3 92.94(19) . . ? O5 Fe1 O3 170.89(18) . . ? O2 Fe1 O3 92.18(19) . . ? O4 Fe1 O3 85.50(18) . . ? O1 Fe1 O3 87.69(18) . . ? C6 O1 Fe1 126.9(4) . . ? C8 O2 Fe1 128.2(4) . . ? C14 O3 Fe1 127.5(4) . . ? C21 O4 Fe1 127.2(4) . . ? C27 O5 Fe1 128.4(5) . . ? C34 O6 Fe1 131.6(4) . . ? N7 O7 Ag2 105.8(5) . . ? N7 O7 Ag1 101.5(5) . . ? Ag2 O7 Ag1 152.0(3) . . ? C1 N1 C5 116.6(6) . . ? C1 N1 Ag1 127.2(4) . . ? C5 N1 Ag1 116.1(5) . . ? C13 N2 C12 118.4(6) . . ? C13 N2 Ag1 120.0(4) . 1_455 ? C12 N2 Ag1 120.0(5) . 1_455 ? C17 N3 C16 116.1(6) . . ? C17 N3 Ag2 121.4(4) . . ? C16 N3 Ag2 121.8(5) . . ? C24 N4 C23 118.4(6) . . ? C24 N4 Ag2 124.6(4) . 1_455 ? C23 N4 Ag2 117.0(5) . 1_455 ? C30 N5 C29 118.6(7) . . ? C30 N5 Ag1 116.0(5) . 2_666 ? C29 N5 Ag1 125.3(5) . 2_666 ? C37 N6 C36 117.4(6) . . ? C37 N6 Ag2 121.3(5) . 2_776 ? C36 N6 Ag2 120.1(5) . 2_776 ? O7 N7 O9 120.2(7) . . ? O7 N7 O8 120.5(7) . . ? O9 N7 O8 119.4(8) . . ? O12 N9 O11 122.7(9) . . ? O12 N9 O10 121.3(8) . . ? O11 N9 O10 116.0(8) . . ? N1 C1 C2 125.1(6) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C3 C2 C1 117.3(7) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C2 C3 C4 120.6(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 116.9(6) . . ? C3 C4 C6 122.1(6) . . ? C5 C4 C6 120.9(6) . . ? N1 C5 C4 123.1(7) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? O1 C6 C7 123.2(6) . . ? O1 C6 C4 114.9(6) . . ? C7 C6 C4 121.9(6) . . ? C6 C7 C8 124.6(6) . . ? C6 C7 H7 117.7 . . ? C8 C7 H7 117.7 . . ? O2 C8 C7 122.4(7) . . ? O2 C8 C9 117.7(5) . . ? C7 C8 C9 119.9(5) . . ? C10 C9 C13 118.1(7) . . ? C10 C9 C8 124.8(6) . . ? C13 C9 C8 117.1(6) . . ? C9 C10 C11 118.9(6) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 120.8(7) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? N2 C12 C11 120.8(8) . . ? N2 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? N2 C13 C9 123.0(6) . . ? N2 C13 H13 118.5 . . ? C9 C13 H13 118.5 . . ? O3 C14 C20 122.1(6) . . ? O3 C14 C15 115.9(5) . . ? C20 C14 C15 121.9(6) . . ? C16 C15 C19 117.5(6) . . ? C16 C15 C14 118.8(6) . . ? C19 C15 C14 123.6(5) . . ? N3 C16 C15 124.8(7) . . ? N3 C16 H16 117.6 . . ? C15 C16 H16 117.6 . . ? N3 C17 C18 123.1(6) . . ? N3 C17 H17 118.5 . . ? C18 C17 H17 118.5 . . ? C19 C18 C17 120.4(7) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C15 118.0(6) . . ? C18 C19 H19 121.0 . . ? C15 C19 H19 121.0 . . ? C14 C20 C21 124.5(7) . . ? C14 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? O4 C21 C20 122.5(6) . . ? O4 C21 C22 118.6(6) . . ? C20 C21 C22 118.9(6) . . ? C23 C22 C26 118.4(6) . . ? C23 C22 C21 123.3(6) . . ? C26 C22 C21 118.2(6) . . ? N4 C23 C22 123.5(6) . . ? N4 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? N4 C24 C25 121.1(6) . . ? N4 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 120.4(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C22 118.2(7) . . ? C25 C26 H26 120.9 . . ? C22 C26 H26 120.9 . . ? O5 C27 C33 123.6(6) . . ? O5 C27 C28 114.3(6) . . ? C33 C27 C28 121.9(6) . . ? C32 C28 C29 117.9(6) . . ? C32 C28 C27 123.6(7) . . ? C29 C28 C27 118.4(6) . . ? N5 C29 C28 122.5(6) . . ? N5 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? N5 C30 C31 122.7(7) . . ? N5 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C30 C31 C32 120.3(8) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C28 C32 C31 117.8(8) . . ? C28 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C27 C33 C34 124.1(6) . . ? C27 C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? O6 C34 C33 122.4(6) . . ? O6 C34 C35 116.6(6) . . ? C33 C34 C35 121.1(6) . . ? C39 C35 C36 118.3(7) . . ? C39 C35 C34 124.5(6) . . ? C36 C35 C34 117.2(6) . . ? N6 C36 C35 123.2(7) . . ? N6 C36 H36 118.4 . . ? C35 C36 H36 118.4 . . ? N6 C37 C38 123.7(7) . . ? N6 C37 H37 118.2 . . ? C38 C37 H37 118.2 . . ? C39 C38 C37 116.9(8) . . ? C39 C38 H38 121.6 . . ? C37 C38 H38 121.6 . . ? C35 C39 C38 120.5(7) . . ? C35 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N8 C41 C40 177.9(17) . . ? Cl2 C42 Cl1 112.1(5) . . ? Cl2 C42 H42A 109.2 . . ? Cl1 C42 H42A 109.2 . . ? Cl2 C42 H42B 109.2 . . ? Cl1 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.928 _refine_diff_density_min -2.073 _refine_diff_density_rms 0.208 #===end data_compound13_bath331 _database_code_depnum_ccdc_archive 'CCDC 853066' #TrackingRef '- dppd-strucs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46.75 H32 Ag2 Cl0.50 F6 Fe N8 O10' _chemical_formula_weight 1269.12 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' Fe Fe 0.3463 0.8444 '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' Cl Cl 0.1484 0.1585 '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 11.789(2) _cell_length_b 13.259(3) _cell_length_c 16.790(3) _cell_angle_alpha 102.365(2) _cell_angle_beta 91.136(2) _cell_angle_gamma 104.490(2) _cell_volume 2474.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4924 _cell_measurement_theta_min 2.194 _cell_measurement_theta_max 25.573 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 1.188 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; SADABS ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6907 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17689 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 23.97 _reflns_number_total 17694 _reflns_number_gt 12220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Small crystal, diffraction fall off above 23o. Network voids filled with 2 molecules of CH3CN and 1/4 of a CH2Cl2 fragment per asymmetric unit (proximate to an inversion centre). Residual electron density maximum is in the region of the disordered solvent. Successful refinement was achieved after accounting for 14% pseudo-merohedral twinning along the reciprocal 0 0 1 direction. ; _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^)+(0.0952P)^2^+1.3130P] 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 0.0143(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17694 _refine_ls_number_parameters 679 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 -0.05727(4) 0.34244(4) 0.30116(3) 0.03630(17) Uani 1 1 d . . . Ag2 Ag 0.00065(4) 0.05712(4) 0.29072(3) 0.03676(17) Uani 1 1 d . . . Fe1 Fe 0.49934(7) 0.27314(7) 0.58101(5) 0.0243(2) Uani 1 1 d . . . Cl1 Cl 0.4207(5) 0.4167(5) 0.0392(4) 0.100(2) Uani 0.50 1 d PD . . F1 F 0.0979(7) 0.0891(5) 0.0971(4) 0.125(3) Uani 1 1 d . . . F2 F 0.1480(8) 0.2402(6) 0.0720(4) 0.130(3) Uani 1 1 d . . . F3 F 0.2687(6) 0.1699(8) 0.1160(4) 0.144(3) Uani 1 1 d . . . F4 F 0.7527(6) 0.0946(4) -0.0180(4) 0.107(2) Uani 1 1 d . . . F5 F 0.9024(5) 0.2169(6) -0.0277(4) 0.114(2) Uani 1 1 d . . . F6 F 0.8377(5) 0.2043(4) 0.0908(3) 0.0895(17) Uani 1 1 d . . . O1 O 0.3757(3) 0.3479(3) 0.5733(2) 0.0284(9) Uani 1 1 d . . . O2 O 0.5732(3) 0.3464(3) 0.4945(2) 0.0284(9) Uani 1 1 d . . . O3 O 0.4046(3) 0.1498(3) 0.4930(2) 0.0282(9) Uani 1 1 d . . . O4 O 0.6235(3) 0.1925(3) 0.5703(2) 0.0272(9) Uani 1 1 d . . . O5 O 0.6075(3) 0.3777(3) 0.6696(2) 0.0260(9) Uani 1 1 d . . . O6 O 0.4137(3) 0.2124(3) 0.6674(2) 0.0278(9) Uani 1 1 d . . . O7 O 0.0415(4) 0.2117(4) 0.2302(3) 0.0477(13) Uani 1 1 d . . . O8 O 0.2330(5) 0.2980(5) 0.2520(3) 0.0604(15) Uani 1 1 d . . . O9 O 0.7747(5) 0.3686(4) 0.0417(3) 0.0588(14) Uani 1 1 d . . . O10 O 0.6420(5) 0.2358(5) -0.0438(4) 0.0697(17) Uani 1 1 d . . . N1 N 0.0310(4) 0.3609(4) 0.4309(3) 0.0317(12) Uani 1 1 d . . . N2 N 0.7568(4) 0.3595(4) 0.2949(3) 0.0300(11) Uani 1 1 d . . . N3 N 0.1792(4) 0.0241(4) 0.2889(3) 0.0288(11) Uiso 1 1 d . . . N4 N 0.9311(4) 0.0992(4) 0.4186(3) 0.0324(12) Uani 1 1 d . . . N5 N 0.9350(4) 0.5401(4) 0.7689(3) 0.0331(12) Uani 1 1 d . . . N6 N 0.1635(4) 0.0512(4) 0.7874(3) 0.0369(13) Uani 1 1 d . . . N7 N 1.0364(13) 0.2916(9) 0.7563(6) 0.130(5) Uani 1 1 d . A . N8 N 0.6449(7) 0.0996(5) 0.2424(4) 0.0594(18) Uani 1 1 d . . . C1 C 0.3990(5) 0.3668(5) 0.4379(4) 0.0271(13) Uani 1 1 d . . . H1 H 0.3603 0.3730 0.3897 0.033 Uiso 1 1 calc R . . C2 C 0.3356(5) 0.3623(5) 0.5051(4) 0.0259(13) Uani 1 1 d . . . C3 C 0.2111(5) 0.3717(4) 0.5052(4) 0.0250(13) Uani 1 1 d . . . C4 C 0.1597(5) 0.3905(5) 0.5786(4) 0.0291(14) Uani 1 1 d . . . H4 H 0.2030 0.3987 0.6289 0.035 Uiso 1 1 calc R . . C5 C 0.0432(5) 0.3972(5) 0.5774(4) 0.0315(14) Uani 1 1 d . . . H5 H 0.0063 0.4123 0.6267 0.038 Uiso 1 1 calc R . . C6 C -0.0160(5) 0.3816(5) 0.5032(4) 0.0283(14) Uani 1 1 d . . . H6 H -0.0954 0.3854 0.5025 0.034 Uiso 1 1 calc R . . C7 C 0.1434(5) 0.3568(5) 0.4332(4) 0.0290(14) Uani 1 1 d . . . H7 H 0.1783 0.3430 0.3829 0.035 Uiso 1 1 calc R . . C8 C 0.5157(5) 0.3628(4) 0.4348(3) 0.0243(13) Uani 1 1 d . . . C9 C 0.5806(5) 0.3736(5) 0.3610(4) 0.0291(14) Uani 1 1 d . . . C10 C 0.6889(5) 0.3501(5) 0.3564(4) 0.0276(13) Uani 1 1 d . . . H10 H 0.7164 0.3256 0.4004 0.033 Uiso 1 1 calc R . . C11 C 0.7151(6) 0.3896(7) 0.2316(4) 0.050(2) Uani 1 1 d . . . H11 H 0.7609 0.3956 0.1861 0.059 Uiso 1 1 calc R . . C12 C 0.6055(7) 0.4126(9) 0.2309(5) 0.080(3) Uani 1 1 d . . . H12 H 0.5784 0.4346 0.1854 0.096 Uiso 1 1 calc R . . C13 C 0.5377(7) 0.4036(8) 0.2945(5) 0.067(3) Uani 1 1 d . . . H13 H 0.4625 0.4175 0.2937 0.081 Uiso 1 1 calc R . . C14 C 0.5650(5) 0.0924(5) 0.4343(4) 0.0299(14) Uani 1 1 d . . . H14 H 0.5905 0.0549 0.3862 0.036 Uiso 1 1 calc R . . C15 C 0.4476(5) 0.0976(4) 0.4338(4) 0.0236(13) Uani 1 1 d . . . C16 C 0.3673(5) 0.0417(5) 0.3602(4) 0.0254(13) Uani 1 1 d . . . C17 C 0.2625(5) 0.0710(5) 0.3518(4) 0.0264(13) Uani 1 1 d . . . H17 H 0.2488 0.1274 0.3927 0.032 Uiso 1 1 calc R . . C18 C 0.2018(5) -0.0553(5) 0.2312(4) 0.0361(15) Uani 1 1 d . . . H18 H 0.1452 -0.0898 0.1863 0.043 Uiso 1 1 calc R . . C19 C 0.3037(6) -0.0883(5) 0.2348(4) 0.0369(15) Uani 1 1 d . . . H19 H 0.3173 -0.1434 0.1927 0.044 Uiso 1 1 calc R . . C20 C 0.3853(5) -0.0397(5) 0.3005(4) 0.0321(14) Uani 1 1 d . . . H20 H 0.4547 -0.0630 0.3044 0.039 Uiso 1 1 calc R . . C21 C 0.6468(5) 0.1400(5) 0.5024(4) 0.0249(13) Uani 1 1 d . . . C22 C 0.7701(5) 0.1293(4) 0.4983(4) 0.0269(13) Uani 1 1 d . . . C23 C 0.8190(5) 0.1067(5) 0.4247(4) 0.0285(14) Uani 1 1 d . . . H23 H 0.7715 0.0959 0.3756 0.034 Uiso 1 1 calc R . . C24 C 0.9966(5) 0.1157(4) 0.4889(4) 0.0308(14) Uani 1 1 d . . . H24 H 1.0751 0.1096 0.4859 0.037 Uiso 1 1 calc R . . C25 C 0.9562(5) 0.1406(5) 0.5644(4) 0.0312(14) Uani 1 1 d . . . H25 H 1.0060 0.1522 0.6124 0.037 Uiso 1 1 calc R . . C26 C 0.8405(5) 0.1487(5) 0.5700(4) 0.0295(14) Uani 1 1 d . . . H26 H 0.8107 0.1670 0.6218 0.035 Uiso 1 1 calc R . . C27 C 0.5437(5) 0.3005(5) 0.7818(4) 0.0324(14) Uani 1 1 d . . . H27 H 0.5617 0.3028 0.8377 0.039 Uiso 1 1 calc R . . C28 C 0.6253(5) 0.3684(5) 0.7419(4) 0.0291(14) Uani 1 1 d . . . C29 C 0.7429(5) 0.4311(5) 0.7838(4) 0.0264(13) Uani 1 1 d . . . C30 C 0.8263(5) 0.4847(5) 0.7382(4) 0.0293(14) Uani 1 1 d . . . H30 H 0.8045 0.4814 0.6828 0.035 Uiso 1 1 calc R . . C31 C 0.9648(6) 0.5435(6) 0.8480(4) 0.0429(17) Uani 1 1 d . . . H31 H 1.0414 0.5830 0.8711 0.051 Uiso 1 1 calc R . . C32 C 0.8888(5) 0.4922(6) 0.8955(4) 0.0423(17) Uani 1 1 d . . . H32 H 0.9132 0.4960 0.9506 0.051 Uiso 1 1 calc R . . C33 C 0.7769(5) 0.4348(5) 0.8641(4) 0.0372(15) Uani 1 1 d . . . H33 H 0.7240 0.3983 0.8969 0.045 Uiso 1 1 calc R . . C34 C 0.4408(5) 0.2325(5) 0.7439(4) 0.0286(14) Uani 1 1 d . . . C35 C 0.3558(5) 0.1702(5) 0.7905(4) 0.0276(13) Uani 1 1 d . . . C36 C 0.2471(5) 0.1121(5) 0.7527(4) 0.0275(13) Uani 1 1 d . . . H36 H 0.2304 0.1155 0.6979 0.033 Uiso 1 1 calc R . . C37 C 0.1854(6) 0.0470(6) 0.8652(4) 0.0435(17) Uani 1 1 d . . . H37 H 0.1264 0.0051 0.8911 0.052 Uiso 1 1 calc R . . C38 C 0.2938(5) 0.1030(6) 0.9095(4) 0.0395(16) Uani 1 1 d . . . H38 H 0.3079 0.0980 0.9643 0.047 Uiso 1 1 calc R . . C39 C 0.3797(5) 0.1656(5) 0.8725(4) 0.0348(15) Uani 1 1 d . . . H39 H 0.4529 0.2045 0.9015 0.042 Uiso 1 1 calc R . . C40 C 0.1463(6) 0.2374(6) 0.2116(4) 0.0422(17) Uani 1 1 d . . . C41 C 0.1628(7) 0.1879(8) 0.1247(5) 0.060(2) Uani 1 1 d . . . C42 C 0.7317(6) 0.2752(7) 0.0032(4) 0.0491(19) Uani 1 1 d . . . C43 C 0.8029(8) 0.1967(7) 0.0124(6) 0.065(2) Uani 1 1 d . . . C44 C 1.0871(12) 0.3194(9) 0.8158(8) 0.091(4) Uani 1 1 d . . . C45 C 1.1599(14) 0.3538(12) 0.8917(8) 0.050(4) Uani 0.50 1 d P A 2 H45A H 1.2255 0.3203 0.8866 0.075 Uiso 0.50 1 calc PR A 2 H45B H 1.1130 0.3325 0.9358 0.075 Uiso 0.50 1 calc PR A 2 H45C H 1.1905 0.4317 0.9043 0.075 Uiso 0.50 1 calc PR A 2 C46 C 0.5497(19) 0.482(3) 0.014(3) 0.081(11) Uiso 0.25 1 d PD . -1 H46A H 0.5835 0.4256 -0.0173 0.097 Uiso 0.25 1 calc PR . -1 H46B H 0.5991 0.5116 0.0661 0.097 Uiso 0.25 1 calc PR . -1 C47 C 0.5055(11) 0.0894(13) 0.1191(8) 0.141(6) Uani 1 1 d . . . H47A H 0.5530 0.1071 0.0743 0.212 Uiso 1 1 calc R . . H47B H 0.4554 0.1386 0.1324 0.212 Uiso 1 1 calc R . . H47C H 0.4562 0.0158 0.1023 0.212 Uiso 1 1 calc R . . C48 C 0.5838(8) 0.0994(8) 0.1918(6) 0.065(2) 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 0.0174(3) 0.0496(3) 0.0442(3) 0.0178(3) 0.0017(2) 0.0071(2) Ag2 0.0178(3) 0.0452(3) 0.0455(3) 0.0119(2) 0.0004(2) 0.0038(2) Fe1 0.0168(4) 0.0290(5) 0.0264(5) 0.0065(4) -0.0021(3) 0.0047(3) Cl1 0.078(3) 0.094(4) 0.117(4) -0.021(3) -0.048(3) 0.047(3) F1 0.142(6) 0.081(4) 0.103(5) -0.032(4) 0.028(4) -0.013(4) F2 0.230(9) 0.151(6) 0.055(4) 0.040(4) 0.023(4) 0.116(6) F3 0.098(5) 0.261(10) 0.079(4) -0.012(5) 0.021(4) 0.104(6) F4 0.132(5) 0.058(4) 0.119(5) 0.015(3) -0.047(4) 0.010(3) F5 0.083(4) 0.144(6) 0.128(5) 0.031(5) 0.036(4) 0.049(4) F6 0.122(5) 0.079(4) 0.069(4) 0.017(3) -0.033(3) 0.032(3) O1 0.023(2) 0.038(2) 0.024(2) 0.0044(19) -0.0029(17) 0.0095(18) O2 0.021(2) 0.031(2) 0.037(2) 0.0145(19) 0.0002(18) 0.0063(17) O3 0.018(2) 0.031(2) 0.038(2) 0.014(2) 0.0001(18) 0.0048(17) O4 0.023(2) 0.032(2) 0.027(2) 0.0068(19) -0.0001(17) 0.0088(18) O5 0.0156(19) 0.033(2) 0.032(2) 0.0135(19) 0.0017(17) 0.0059(17) O6 0.020(2) 0.029(2) 0.031(2) 0.0078(19) -0.0048(17) 0.0002(17) O7 0.036(3) 0.045(3) 0.075(4) 0.033(3) 0.021(2) 0.016(2) O8 0.046(3) 0.077(4) 0.050(3) 0.007(3) 0.003(3) 0.008(3) O9 0.067(4) 0.057(4) 0.046(3) 0.015(3) -0.010(3) 0.002(3) O10 0.041(3) 0.093(5) 0.069(4) 0.018(3) -0.018(3) 0.010(3) N1 0.023(3) 0.029(3) 0.043(3) 0.012(2) -0.004(2) 0.003(2) N2 0.024(3) 0.037(3) 0.028(3) 0.006(2) -0.003(2) 0.007(2) N4 0.024(3) 0.027(3) 0.046(3) 0.006(2) 0.003(2) 0.008(2) N5 0.022(3) 0.032(3) 0.042(3) 0.013(3) -0.002(2) -0.003(2) N6 0.021(3) 0.045(3) 0.037(3) 0.012(3) -0.005(2) -0.008(2) N7 0.238(14) 0.103(8) 0.058(6) 0.001(6) -0.028(7) 0.080(9) N8 0.069(5) 0.051(4) 0.056(5) 0.016(4) 0.010(4) 0.008(4) C1 0.017(3) 0.042(4) 0.024(3) 0.005(3) -0.003(2) 0.013(3) C2 0.019(3) 0.025(3) 0.034(4) 0.005(3) 0.000(3) 0.010(2) C3 0.017(3) 0.020(3) 0.038(4) 0.010(3) -0.003(3) 0.003(2) C4 0.018(3) 0.027(3) 0.040(4) 0.005(3) -0.002(3) 0.004(2) C5 0.018(3) 0.031(3) 0.045(4) 0.011(3) 0.007(3) 0.003(3) C6 0.015(3) 0.028(3) 0.041(4) 0.006(3) 0.000(3) 0.005(2) C7 0.022(3) 0.031(3) 0.035(4) 0.013(3) 0.005(3) 0.003(3) C8 0.027(3) 0.020(3) 0.023(3) 0.003(2) -0.007(2) 0.002(2) C9 0.020(3) 0.033(3) 0.037(4) 0.012(3) 0.003(3) 0.009(3) C10 0.020(3) 0.027(3) 0.033(4) 0.011(3) 0.001(3) -0.001(2) C11 0.026(4) 0.087(6) 0.043(4) 0.024(4) 0.015(3) 0.019(4) C12 0.058(5) 0.174(11) 0.048(5) 0.065(6) 0.020(4) 0.066(6) C13 0.049(5) 0.128(8) 0.057(5) 0.056(6) 0.027(4) 0.050(5) C14 0.014(3) 0.030(3) 0.041(4) -0.002(3) 0.003(3) 0.005(2) C15 0.025(3) 0.018(3) 0.032(3) 0.013(3) 0.007(3) 0.006(2) C16 0.020(3) 0.025(3) 0.030(3) 0.007(3) 0.001(2) 0.004(2) C17 0.023(3) 0.023(3) 0.031(3) 0.004(3) 0.005(2) 0.004(2) C18 0.023(3) 0.049(4) 0.032(4) 0.000(3) -0.005(3) 0.008(3) C19 0.037(4) 0.041(4) 0.032(4) 0.001(3) -0.001(3) 0.014(3) C20 0.019(3) 0.036(4) 0.042(4) 0.003(3) -0.001(3) 0.012(3) C21 0.018(3) 0.025(3) 0.034(4) 0.014(3) 0.000(2) 0.003(2) C22 0.019(3) 0.021(3) 0.040(4) 0.014(3) 0.001(3) 0.000(2) C23 0.015(3) 0.030(3) 0.042(4) 0.009(3) -0.003(3) 0.008(2) C24 0.017(3) 0.019(3) 0.055(4) 0.011(3) -0.001(3) 0.000(2) C25 0.023(3) 0.025(3) 0.047(4) 0.012(3) -0.004(3) 0.005(3) C26 0.028(3) 0.030(3) 0.036(4) 0.013(3) 0.003(3) 0.011(3) C27 0.032(3) 0.038(4) 0.022(3) 0.009(3) -0.003(3) -0.003(3) C28 0.017(3) 0.034(4) 0.033(4) 0.003(3) -0.002(3) 0.006(3) C29 0.014(3) 0.030(3) 0.032(3) 0.005(3) -0.001(2) 0.004(2) C30 0.024(3) 0.031(3) 0.032(3) 0.011(3) -0.001(3) 0.004(3) C31 0.032(4) 0.048(4) 0.041(4) 0.014(3) -0.007(3) -0.005(3) C32 0.026(3) 0.065(5) 0.033(4) 0.015(4) -0.005(3) 0.004(3) C33 0.030(3) 0.040(4) 0.036(4) 0.012(3) 0.002(3) -0.002(3) C34 0.018(3) 0.024(3) 0.042(4) 0.008(3) -0.001(3) 0.004(2) C35 0.019(3) 0.026(3) 0.039(4) 0.008(3) 0.003(3) 0.006(2) C36 0.020(3) 0.026(3) 0.034(4) 0.011(3) -0.002(2) 0.000(2) C37 0.028(4) 0.054(5) 0.041(4) 0.014(4) 0.000(3) -0.007(3) C38 0.022(3) 0.057(5) 0.040(4) 0.020(3) 0.001(3) 0.002(3) C39 0.030(3) 0.039(4) 0.032(4) 0.007(3) -0.003(3) 0.002(3) C40 0.038(4) 0.045(4) 0.047(4) 0.017(4) 0.004(3) 0.012(3) C41 0.048(5) 0.081(7) 0.049(5) 0.015(5) 0.015(4) 0.013(5) C42 0.040(4) 0.062(5) 0.039(4) 0.022(4) -0.011(3) -0.005(4) C43 0.058(5) 0.056(6) 0.068(6) 0.011(5) -0.020(5) -0.002(4) C44 0.140(11) 0.064(7) 0.092(9) 0.037(7) 0.043(8) 0.054(7) C45 0.089(12) 0.045(9) 0.024(7) -0.008(6) -0.014(7) 0.045(8) C47 0.097(9) 0.208(16) 0.119(10) 0.082(11) -0.045(8) 0.007(9) C48 0.058(6) 0.074(6) 0.065(6) 0.026(5) 0.006(5) 0.012(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 Ag1 N2 2.262(5) 1_455 ? Ag1 N1 2.334(5) . ? Ag1 N5 2.370(5) 2_666 ? Ag1 O7 2.441(5) . ? Ag2 N3 2.254(5) . ? Ag2 N6 2.287(5) 2_556 ? Ag2 N4 2.319(5) 1_455 ? Ag2 O7 2.426(4) . ? Fe1 O1 1.974(4) . ? Fe1 O5 1.979(4) . ? Fe1 O6 1.980(4) . ? Fe1 O4 2.007(4) . ? Fe1 O2 2.010(4) . ? Fe1 O3 2.022(4) . ? Cl1 C46 1.663(10) . ? Cl1 C46 1.74(3) 2_665 ? F1 C41 1.319(10) . ? F2 C41 1.270(10) . ? F3 C41 1.334(9) . ? F4 C43 1.317(10) . ? F5 C43 1.361(10) . ? F6 C43 1.346(9) . ? O1 C2 1.300(7) . ? O2 C8 1.285(7) . ? O3 C15 1.274(7) . ? O4 C21 1.277(7) . ? O5 C28 1.266(7) . ? O6 C34 1.271(7) . ? O7 C40 1.261(8) . ? O8 C40 1.216(8) . ? O9 C42 1.241(9) . ? O10 C42 1.237(8) . ? N1 C7 1.339(7) . ? N1 C6 1.347(8) . ? N2 C10 1.326(7) . ? N2 C11 1.338(8) . ? N2 Ag1 2.262(5) 1_655 ? N3 C18 1.354(8) . ? N3 C17 1.355(7) . ? N4 C24 1.343(8) . ? N4 C23 1.355(7) . ? N4 Ag2 2.319(5) 1_655 ? N5 C30 1.337(7) . ? N5 C31 1.354(8) . ? N5 Ag1 2.370(5) 2_666 ? N6 C36 1.338(7) . ? N6 C37 1.342(8) . ? N6 Ag2 2.287(5) 2_556 ? N7 C44 1.094(14) . ? N8 C48 1.102(10) . ? C1 C2 1.370(8) . ? C1 C8 1.392(8) . ? C2 C3 1.504(7) . ? C3 C7 1.384(8) . ? C3 C4 1.386(8) . ? C4 C5 1.399(8) . ? C5 C6 1.365(9) . ? C8 C9 1.484(8) . ? C9 C10 1.388(8) . ? C9 C13 1.388(9) . ? C11 C12 1.400(10) . ? C12 C13 1.354(10) . ? C14 C15 1.403(8) . ? C14 C21 1.407(8) . ? C15 C16 1.478(8) . ? C16 C20 1.369(8) . ? C16 C17 1.397(8) . ? C18 C19 1.382(8) . ? C19 C20 1.379(9) . ? C21 C22 1.497(7) . ? C22 C23 1.380(8) . ? C22 C26 1.388(8) . ? C24 C25 1.367(9) . ? C25 C26 1.399(8) . ? C27 C34 1.366(8) . ? C27 C28 1.426(8) . ? C28 C29 1.497(8) . ? C29 C33 1.386(8) . ? C29 C30 1.404(8) . ? C31 C32 1.364(9) . ? C32 C33 1.377(9) . ? C34 C35 1.481(8) . ? C35 C36 1.379(8) . ? C35 C39 1.418(8) . ? C37 C38 1.411(9) . ? C38 C39 1.387(9) . ? C40 C41 1.503(11) . ? C42 C43 1.521(12) . ? C44 C45 1.442(19) . ? C46 Cl1 1.74(3) 2_665 ? C47 C48 1.478(14) . ? 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 N2 Ag1 N1 116.82(18) 1_455 . ? N2 Ag1 N5 110.40(17) 1_455 2_666 ? N1 Ag1 N5 109.86(17) . 2_666 ? N2 Ag1 O7 134.44(18) 1_455 . ? N1 Ag1 O7 95.88(17) . . ? N5 Ag1 O7 84.30(16) 2_666 . ? N3 Ag2 N6 124.76(19) . 2_556 ? N3 Ag2 N4 116.14(17) . 1_455 ? N6 Ag2 N4 102.85(18) 2_556 1_455 ? N3 Ag2 O7 99.67(16) . . ? N6 Ag2 O7 101.87(18) 2_556 . ? N4 Ag2 O7 110.14(17) 1_455 . ? O1 Fe1 O5 100.60(16) . . ? O1 Fe1 O6 87.77(16) . . ? O5 Fe1 O6 87.39(16) . . ? O1 Fe1 O4 171.36(16) . . ? O5 Fe1 O4 85.57(16) . . ? O6 Fe1 O4 98.62(16) . . ? O1 Fe1 O2 85.46(16) . . ? O5 Fe1 O2 92.60(16) . . ? O6 Fe1 O2 173.11(16) . . ? O4 Fe1 O2 88.24(16) . . ? O1 Fe1 O3 88.55(16) . . ? O5 Fe1 O3 170.67(15) . . ? O6 Fe1 O3 91.17(16) . . ? O4 Fe1 O3 85.53(15) . . ? O2 Fe1 O3 89.94(16) . . ? C46 Cl1 C46 51(2) . 2_665 ? C2 O1 Fe1 123.8(3) . . ? C8 O2 Fe1 124.6(4) . . ? C15 O3 Fe1 124.9(3) . . ? C21 O4 Fe1 123.8(3) . . ? C28 O5 Fe1 127.1(4) . . ? C34 O6 Fe1 129.8(4) . . ? C40 O7 Ag2 112.6(4) . . ? C40 O7 Ag1 122.7(4) . . ? Ag2 O7 Ag1 109.63(17) . . ? C7 N1 C6 117.0(5) . . ? C7 N1 Ag1 115.5(4) . . ? C6 N1 Ag1 127.3(4) . . ? C10 N2 C11 117.3(5) . . ? C10 N2 Ag1 121.9(4) . 1_655 ? C11 N2 Ag1 120.6(4) . 1_655 ? C18 N3 C17 116.5(5) . . ? C18 N3 Ag2 121.1(4) . . ? C17 N3 Ag2 121.7(4) . . ? C24 N4 C23 117.0(5) . . ? C24 N4 Ag2 123.1(4) . 1_655 ? C23 N4 Ag2 119.8(4) . 1_655 ? C30 N5 C31 117.6(5) . . ? C30 N5 Ag1 121.3(4) . 2_666 ? C31 N5 Ag1 119.9(4) . 2_666 ? C36 N6 C37 118.1(5) . . ? C36 N6 Ag2 119.5(4) . 2_556 ? C37 N6 Ag2 122.0(4) . 2_556 ? C2 C1 C8 125.0(5) . . ? O1 C2 C1 123.8(5) . . ? O1 C2 C3 114.1(5) . . ? C1 C2 C3 122.1(5) . . ? C7 C3 C4 118.4(5) . . ? C7 C3 C2 121.7(5) . . ? C4 C3 C2 119.8(5) . . ? C3 C4 C5 119.0(6) . . ? C6 C5 C4 118.1(6) . . ? N1 C6 C5 124.2(5) . . ? N1 C7 C3 123.3(6) . . ? O2 C8 C1 122.4(5) . . ? O2 C8 C9 115.7(5) . . ? C1 C8 C9 121.9(5) . . ? C10 C9 C13 117.5(6) . . ? C10 C9 C8 118.8(5) . . ? C13 C9 C8 123.6(5) . . ? N2 C10 C9 124.6(5) . . ? N2 C11 C12 121.5(6) . . ? C13 C12 C11 120.5(7) . . ? C12 C13 C9 118.5(6) . . ? C15 C14 C21 123.3(5) . . ? O3 C15 C14 124.2(5) . . ? O3 C15 C16 116.6(5) . . ? C14 C15 C16 119.2(5) . . ? C20 C16 C17 116.9(5) . . ? C20 C16 C15 125.1(5) . . ? C17 C16 C15 117.9(5) . . ? N3 C17 C16 124.2(5) . . ? N3 C18 C19 122.8(6) . . ? C20 C19 C18 118.9(6) . . ? C16 C20 C19 120.7(5) . . ? O4 C21 C14 124.3(5) . . ? O4 C21 C22 115.7(5) . . ? C14 C21 C22 119.9(5) . . ? C23 C22 C26 118.4(5) . . ? C23 C22 C21 121.8(5) . . ? C26 C22 C21 119.7(5) . . ? N4 C23 C22 123.5(5) . . ? N4 C24 C25 123.4(5) . . ? C24 C25 C26 119.1(6) . . ? C22 C26 C25 118.5(6) . . ? C34 C27 C28 123.4(6) . . ? O5 C28 C27 124.1(5) . . ? O5 C28 C29 115.2(5) . . ? C27 C28 C29 120.6(5) . . ? C33 C29 C30 117.7(5) . . ? C33 C29 C28 123.8(5) . . ? C30 C29 C28 118.4(5) . . ? N5 C30 C29 123.3(6) . . ? N5 C31 C32 122.3(6) . . ? C31 C32 C33 120.3(6) . . ? C32 C33 C29 118.8(6) . . ? O6 C34 C27 124.1(5) . . ? O6 C34 C35 115.2(5) . . ? C27 C34 C35 120.6(6) . . ? C36 C35 C39 117.3(5) . . ? C36 C35 C34 119.0(5) . . ? C39 C35 C34 123.7(5) . . ? N6 C36 C35 124.8(6) . . ? N6 C37 C38 121.7(6) . . ? C39 C38 C37 119.4(6) . . ? C38 C39 C35 118.6(6) . . ? O8 C40 O7 129.8(7) . . ? O8 C40 C41 116.6(6) . . ? O7 C40 C41 113.6(7) . . ? F2 C41 F1 106.8(8) . . ? F2 C41 F3 106.5(7) . . ? F1 C41 F3 98.7(8) . . ? F2 C41 C40 115.8(8) . . ? F1 C41 C40 114.8(7) . . ? F3 C41 C40 112.7(7) . . ? O10 C42 O9 130.5(8) . . ? O10 C42 C43 114.3(7) . . ? O9 C42 C43 115.1(6) . . ? F4 C43 F6 106.0(7) . . ? F4 C43 F5 104.2(8) . . ? F6 C43 F5 106.6(7) . . ? F4 C43 C42 116.8(7) . . ? F6 C43 C42 112.8(7) . . ? F5 C43 C42 109.7(7) . . ? N7 C44 C45 176.4(14) . . ? Cl1 C46 Cl1 129(2) . 2_665 ? N8 C48 C47 174.0(12) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.97 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.729 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.137 #===end