# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 900349' #TrackingRef 'CIF-060912.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H44 Cd7.50 N51 O6.50' _chemical_formula_weight 2216.29 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.4565(2) _cell_length_b 28.6559(3) _cell_length_c 16.8825(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.2664(6) _cell_angle_gamma 90.00 _cell_volume 7475.77(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80904 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'weak yellow' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 2.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details '(Blessing, 1995, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD Diffractometer' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 0.76 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 77942 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.49 _reflns_number_total 17034 _reflns_number_gt 9361 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (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^)+(0.0309P)^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 SHELXL _refine_ls_extinction_coef 0.00004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17034 _refine_ls_number_parameters 966 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.49699(2) 0.178996(13) 0.263803(19) 0.04127(11) Uani 1 1 d . . . Cd2 Cd 0.50456(2) 0.123725(12) 0.483798(18) 0.03443(10) Uani 1 1 d . . . Cd3 Cd 0.48341(2) 0.204511(13) 0.66927(2) 0.04123(11) Uani 1 1 d . . . Cd4 Cd 0.38095(2) 0.072821(12) 0.646721(19) 0.03582(10) Uani 1 1 d . . . Cd5 Cd 0.5000 0.0000 0.5000 0.03268(13) Uani 1 2 d S . . Cd6 Cd 0.39542(2) -0.052202(12) 0.672156(19) 0.03650(10) Uani 1 1 d . . . Cd7 Cd 0.15754(2) 0.010775(13) 0.73448(2) 0.03996(10) Uani 1 1 d . . . Cd8 Cd 0.09515(3) 0.000407(15) 0.93911(2) 0.05233(12) Uani 1 1 d . . . O1 O 0.4679(3) 0.26390(15) 0.2670(2) 0.0669(11) Uani 1 1 d . . . O2 O 0.5020(2) 0.18783(13) 0.1201(2) 0.0602(11) Uani 1 1 d . . . O3 O 0.5078(2) 0.28508(12) 0.6292(2) 0.0582(10) Uani 1 1 d . . . O4 O 0.4713(3) 0.25287(15) 0.7920(2) 0.0732(12) Uani 1 1 d . . . O5 O 0.0219(2) 0.05427(13) 0.7156(2) 0.0629(11) Uani 1 1 d . . . N1 N 0.6197(3) 0.22117(16) 0.2888(2) 0.0459(11) Uani 1 1 d . . . N2 N 0.3611(3) 0.17166(15) 0.2064(2) 0.0472(11) Uani 1 1 d . . . N3 N 0.4522(3) 0.17723(15) 0.3897(2) 0.0444(11) Uani 1 1 d . . . N4 N 0.4332(3) 0.21427(19) 0.4187(2) 0.0593(13) Uani 1 1 d . . . N5 N 0.4161(5) 0.2498(2) 0.4466(3) 0.113(3) Uani 1 1 d . . . N6 N 0.6327(3) 0.11212(14) 0.4166(2) 0.0451(11) Uani 1 1 d . . . N7 N 0.7008(3) 0.12436(16) 0.4436(3) 0.0561(12) Uani 1 1 d . . . N8 N 0.7654(4) 0.1368(2) 0.4683(4) 0.105(2) Uani 1 1 d . . . N9 N 0.5593(3) 0.18256(15) 0.5626(2) 0.0454(11) Uani 1 1 d . . . N10 N 0.6042(3) 0.21106(18) 0.5319(3) 0.0613(13) Uani 1 1 d . . . N11 N 0.6489(4) 0.2373(2) 0.5027(4) 0.113(2) Uani 1 1 d . . . N12 N 0.3552(3) 0.23897(15) 0.6313(2) 0.0398(10) Uani 1 1 d . . . N13 N 0.6098(3) 0.20568(16) 0.7489(2) 0.0528(12) Uani 1 1 d . . . N14 N 0.4694(2) 0.05704(13) 0.4029(2) 0.0353(10) Uani 1 1 d . . . N15 N 0.3988(3) 0.05963(15) 0.3707(2) 0.0472(11) Uani 1 1 d . . . N16 N 0.3322(4) 0.0626(2) 0.3408(3) 0.099(2) Uani 1 1 d . . . N17 N 0.3684(3) 0.12365(14) 0.5408(2) 0.0436(11) Uani 1 1 d . . . N18 N 0.3065(3) 0.13704(16) 0.5022(2) 0.0472(11) Uani 1 1 d . . . N19 N 0.2489(3) 0.1511(2) 0.4665(3) 0.0780(17) Uani 1 1 d . . . N20 N 0.5275(2) 0.06535(13) 0.5818(2) 0.0349(10) Uani 1 1 d . . . N21 N 0.5889(3) 0.06643(15) 0.6275(2) 0.0471(11) Uani 1 1 d . . . N22 N 0.6443(4) 0.0681(2) 0.6725(3) 0.0917(19) Uani 1 1 d . . . N23 N 0.4345(3) 0.13611(14) 0.7189(2) 0.0458(11) Uani 1 1 d . . . N24 N 0.4709(3) 0.12735(17) 0.7809(3) 0.0621(13) Uani 1 1 d . . . N25 N 0.5062(4) 0.1190(2) 0.8401(3) 0.107(2) Uani 1 1 d . . . N26 N 0.3687(2) 0.00338(13) 0.5650(2) 0.0340(9) Uani 1 1 d . . . N27 N 0.3022(3) -0.00469(16) 0.5274(3) 0.0518(12) Uani 1 1 d . . . N28 N 0.2418(4) -0.0150(3) 0.4940(4) 0.119(3) Uani 1 1 d . . . N29 N 0.2333(3) 0.06774(16) 0.6699(2) 0.0481(11) Uani 1 1 d . . . N30 N 0.1872(3) 0.10062(19) 0.6534(3) 0.0560(13) Uani 1 1 d . . . N31 N 0.1423(4) 0.1318(2) 0.6378(4) 0.099(2) Uani 1 1 d . . . N32 N 0.4250(3) 0.01659(14) 0.7354(2) 0.0439(11) Uani 1 1 d . . . N33 N 0.4095(3) 0.01838(15) 0.8057(3) 0.0557(12) Uani 1 1 d . . . N34 N 0.3956(4) 0.0194(2) 0.8715(3) 0.097(2) Uani 1 1 d . . . N35 N 0.1711(3) 0.04704(17) 0.8533(2) 0.0552(12) Uani 1 1 d . . . N36 N 0.2177(3) 0.07822(19) 0.8739(3) 0.0593(13) Uani 1 1 d . . . N37 N 0.2615(4) 0.1087(2) 0.8929(4) 0.109(2) Uani 1 1 d . . . N38 N 0.4562(3) -0.10543(14) 0.7603(2) 0.0435(11) Uani 1 1 d . . . N39 N 0.4985(3) -0.08849(16) 0.8152(3) 0.0533(12) Uani 1 1 d . . . N40 N 0.5384(3) -0.0734(2) 0.8682(3) 0.0833(17) Uani 1 1 d . . . N41 N 0.2536(3) -0.04961(15) 0.7189(2) 0.0454(11) Uani 1 1 d . . . N42 N 0.2212(3) -0.08565(19) 0.7399(3) 0.0560(13) Uani 1 1 d . . . N43 N 0.1882(4) -0.11948(19) 0.7600(3) 0.0907(19) Uani 1 1 d . . . N44 N 0.0658(3) -0.02154(15) 0.6340(2) 0.0461(11) Uani 1 1 d . . . N45 N 0.0691(3) -0.03432(16) 0.8213(2) 0.0502(12) Uani 1 1 d . . . N46 N 0.0146(3) -0.0610(2) 0.7994(3) 0.0582(13) Uani 1 1 d . . . N47 N -0.0348(4) -0.0877(2) 0.7762(3) 0.109(2) Uani 1 1 d . . . N48 N -0.0213(3) 0.04638(17) 0.9682(3) 0.0565(13) Uani 1 1 d . . . N49 N -0.0681(4) 0.06677(19) 0.9233(3) 0.0638(14) Uani 1 1 d . . . N50 N -0.1146(4) 0.0872(2) 0.8819(4) 0.102(2) Uani 1 1 d . . . C1 C 0.6950(4) 0.2011(2) 0.2973(3) 0.0576(15) Uani 1 1 d . . . H1 H 0.6986 0.1690 0.2890 0.069 Uiso 1 1 calc R . . C2 C 0.7698(4) 0.2250(3) 0.3179(3) 0.0732(19) Uani 1 1 d . . . H2 H 0.8226 0.2097 0.3236 0.088 Uiso 1 1 calc R . . C3 C 0.7633(5) 0.2718(3) 0.3294(3) 0.082(2) Uani 1 1 d . . . H3 H 0.8125 0.2891 0.3427 0.098 Uiso 1 1 calc R . . C4 C 0.6853(5) 0.2938(2) 0.3218(3) 0.0718(19) Uani 1 1 d . . . H4 H 0.6806 0.3257 0.3304 0.086 Uiso 1 1 calc R . . C5 C 0.6133(4) 0.2675(2) 0.3012(3) 0.0499(14) Uani 1 1 d . . . C6 C 0.5273(5) 0.2886(2) 0.2901(4) 0.0658(18) Uani 1 1 d . . . C7 C 0.5131(5) 0.3386(2) 0.3071(5) 0.119(3) Uani 1 1 d . . . H7A H 0.4537 0.3464 0.2955 0.178 Uiso 1 1 calc R . . H7B H 0.5501 0.3572 0.2749 0.178 Uiso 1 1 calc R . . H7C H 0.5260 0.3446 0.3621 0.178 Uiso 1 1 calc R . . C8 C 0.2908(4) 0.1659(2) 0.2479(4) 0.0632(16) Uani 1 1 d . . . H8 H 0.2958 0.1638 0.3028 0.076 Uiso 1 1 calc R . . C9 C 0.2091(4) 0.1629(2) 0.2117(5) 0.092(2) Uani 1 1 d . . . H9 H 0.1602 0.1588 0.2421 0.110 Uiso 1 1 calc R . . C10 C 0.2015(5) 0.1659(3) 0.1321(5) 0.113(3) Uani 1 1 d . . . H10 H 0.1472 0.1657 0.1072 0.135 Uiso 1 1 calc R . . C11 C 0.2742(4) 0.1692(3) 0.0891(4) 0.092(2) Uani 1 1 d . . . H11 H 0.2702 0.1689 0.0341 0.110 Uiso 1 1 calc R . . C12 C 0.3530(3) 0.17278(19) 0.1262(3) 0.0543(15) Uani 1 1 d . . . C13 C 0.4361(4) 0.1790(2) 0.0837(3) 0.0614(16) Uani 1 1 d . . . C14 C 0.4360(5) 0.1724(3) -0.0049(3) 0.116(3) Uani 1 1 d . . . H14A H 0.4030 0.1969 -0.0299 0.174 Uiso 1 1 calc R . . H14B H 0.4105 0.1428 -0.0181 0.174 Uiso 1 1 calc R . . H14C H 0.4943 0.1733 -0.0231 0.174 Uiso 1 1 calc R . . C15 C 0.2791(3) 0.21710(19) 0.6326(3) 0.0451(13) Uani 1 1 d . . . H15 H 0.2778 0.1862 0.6494 0.054 Uiso 1 1 calc R . . C16 C 0.2035(4) 0.2378(2) 0.6104(3) 0.0553(15) Uani 1 1 d . . . H16 H 0.1517 0.2214 0.6118 0.066 Uiso 1 1 calc R . . C17 C 0.2046(4) 0.2826(2) 0.5862(3) 0.0624(17) Uani 1 1 d . . . H17 H 0.1531 0.2973 0.5713 0.075 Uiso 1 1 calc R . . C18 C 0.2815(4) 0.3065(2) 0.5835(3) 0.0546(15) Uani 1 1 d . . . H18 H 0.2831 0.3375 0.5669 0.065 Uiso 1 1 calc R . . C19 C 0.3562(3) 0.28324(19) 0.6063(3) 0.0442(13) Uani 1 1 d . . . C20 C 0.4462(4) 0.30520(19) 0.6028(3) 0.0506(14) Uani 1 1 d . . . C21 C 0.4522(4) 0.3522(2) 0.5645(4) 0.0753(18) Uani 1 1 d . . . H21A H 0.4171 0.3741 0.5925 0.113 Uiso 1 1 calc R . . H21B H 0.4321 0.3502 0.5104 0.113 Uiso 1 1 calc R . . H21C H 0.5113 0.3625 0.5661 0.113 Uiso 1 1 calc R . . C22 C 0.6738(4) 0.1766(2) 0.7345(4) 0.081(2) Uani 1 1 d . . . H22 H 0.6711 0.1579 0.6894 0.097 Uiso 1 1 calc R . . C23 C 0.7464(4) 0.1734(3) 0.7867(5) 0.120(3) Uani 1 1 d . . . H23 H 0.7896 0.1517 0.7771 0.144 Uiso 1 1 calc R . . C24 C 0.7534(5) 0.2016(3) 0.8497(5) 0.113(3) Uani 1 1 d . . . H24 H 0.8022 0.2008 0.8829 0.135 Uiso 1 1 calc R . . C25 C 0.6881(4) 0.2311(3) 0.8636(3) 0.078(2) Uani 1 1 d . . . H25 H 0.6913 0.2507 0.9074 0.093 Uiso 1 1 calc R . . C26 C 0.6158(4) 0.2326(2) 0.8135(3) 0.0539(15) Uani 1 1 d . . . C27 C 0.5371(4) 0.2612(2) 0.8275(3) 0.0645(18) Uani 1 1 d . . . C28 C 0.5410(5) 0.3002(3) 0.8858(5) 0.143(4) Uani 1 1 d . . . H28A H 0.5032 0.3249 0.8682 0.215 Uiso 1 1 calc R . . H28B H 0.5992 0.3117 0.8902 0.215 Uiso 1 1 calc R . . H28C H 0.5230 0.2892 0.9365 0.215 Uiso 1 1 calc R . . C29 C 0.0865(4) -0.0580(2) 0.5921(3) 0.0597(16) Uani 1 1 d . . . H29 H 0.1440 -0.0676 0.5922 0.072 Uiso 1 1 calc R . . C30 C 0.0256(5) -0.0829(2) 0.5474(4) 0.083(2) Uani 1 1 d . . . H30 H 0.0423 -0.1088 0.5184 0.100 Uiso 1 1 calc R . . C31 C -0.0579(6) -0.0691(3) 0.5463(4) 0.103(3) Uani 1 1 d . . . H31 H -0.0996 -0.0853 0.5168 0.124 Uiso 1 1 calc R . . C32 C -0.0792(4) -0.0311(3) 0.5893(4) 0.084(2) Uani 1 1 d . . . H32 H -0.1363 -0.0209 0.5898 0.101 Uiso 1 1 calc R . . C33 C -0.0166(4) -0.0077(2) 0.6320(3) 0.0531(15) Uani 1 1 d . . . C34 C -0.0355(4) 0.0349(2) 0.6781(3) 0.0601(16) Uani 1 1 d . . . C35 C -0.1276(4) 0.0539(3) 0.6778(4) 0.107(3) Uani 1 1 d . . . H35A H -0.1325 0.0771 0.7185 0.160 Uiso 1 1 calc R . . H35B H -0.1674 0.0289 0.6875 0.160 Uiso 1 1 calc R . . H35C H -0.1410 0.0677 0.6272 0.160 Uiso 1 1 calc R . . O6 O 0.2111(6) -0.0622(3) 0.9332(4) 0.058(2) Uiso 0.50 1 d PD . . O6' O 0.1510(6) 0.0421(3) 1.0644(6) 0.087(3) Uiso 0.50 1 d PD . . N51 N 0.1951(6) 0.0085(3) 1.0412(5) 0.046(2) Uiso 0.50 1 d P . . N51' N 0.2235(7) -0.0318(4) 0.9774(6) 0.069(3) Uiso 0.50 1 d P . . C36 C 0.1893(8) 0.0346(4) 1.0979(6) 0.041(3) Uiso 0.50 1 d P . . C36' C 0.2579(9) -0.0607(4) 0.9394(7) 0.052(3) Uiso 0.50 1 d P . . C37 C 0.2426(11) 0.0434(6) 1.1641(10) 0.068(6) Uiso 0.50 1 d P . . C37' C 0.3466(10) -0.0818(6) 0.9520(9) 0.066(5) Uiso 0.50 1 d P . . C38 C 0.3066(9) 0.0118(5) 1.1734(7) 0.071(4) Uiso 0.50 1 d P . . C38' C 0.3890(10) -0.0638(6) 1.0200(9) 0.096(5) Uiso 0.50 1 d P . . C39 C 0.3258(8) -0.0202(5) 1.1128(8) 0.064(4) Uiso 0.50 1 d P . . C39' C 0.3506(10) -0.0304(5) 1.0750(9) 0.085(4) Uiso 0.50 1 d P . . C40 C 0.2750(11) -0.0207(5) 1.0491(9) 0.038(5) Uiso 0.50 1 d P . . C40' C 0.2545(13) -0.0157(7) 1.0433(11) 0.058(7) Uiso 0.50 1 d P . . C41 C 0.2802(7) -0.0552(4) 0.9874(6) 0.050(3) Uiso 0.50 1 d PD . . C41' C 0.2313(12) 0.0167(7) 1.0903(13) 0.127(7) Uiso 0.50 1 d PD . . C42 C 0.3577(12) -0.0849(7) 0.9810(11) 0.082(6) Uiso 0.50 1 d P . . C42' C 0.2394(13) 0.0296(7) 1.1782(11) 0.080(7) Uiso 0.50 1 d P . . O7 O 0.8756(5) 0.2175(3) 0.5228(4) 0.076(2) Uiso 0.50 1 d PD . . C43 C 0.8975(8) 0.1938(4) 0.5935(6) 0.070(3) Uiso 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 Cd1 0.0410(2) 0.0453(3) 0.0376(2) 0.00107(18) 0.00120(16) -0.00141(19) Cd2 0.0370(2) 0.0332(2) 0.03316(19) -0.00084(16) 0.00360(15) 0.00055(17) Cd3 0.0391(2) 0.0406(2) 0.0440(2) -0.00329(18) 0.00064(16) 0.00200(18) Cd4 0.0381(2) 0.0345(2) 0.0350(2) 0.00008(16) 0.00480(15) -0.00056(17) Cd5 0.0340(3) 0.0333(3) 0.0309(3) -0.0004(2) 0.0041(2) 0.0012(2) Cd6 0.0391(2) 0.0360(2) 0.0346(2) -0.00074(16) 0.00460(15) 0.00349(17) Cd7 0.0364(2) 0.0385(2) 0.0454(2) 0.00084(18) 0.01040(16) -0.00117(18) Cd8 0.0449(2) 0.0726(3) 0.0397(2) 0.0042(2) 0.00675(17) -0.0054(2) O1 0.059(3) 0.065(3) 0.076(3) 0.013(2) 0.008(2) 0.011(2) O2 0.050(3) 0.081(3) 0.049(2) 0.010(2) -0.0007(19) -0.008(2) O3 0.043(2) 0.043(2) 0.088(3) 0.008(2) -0.009(2) 0.0037(19) O4 0.056(3) 0.091(3) 0.073(3) -0.032(2) 0.001(2) 0.004(2) O5 0.050(3) 0.058(3) 0.081(3) -0.011(2) 0.000(2) 0.006(2) N1 0.045(3) 0.045(3) 0.049(3) 0.001(2) 0.010(2) 0.000(2) N2 0.037(3) 0.051(3) 0.054(3) -0.001(2) 0.002(2) -0.002(2) N3 0.058(3) 0.041(3) 0.034(2) 0.001(2) 0.0051(19) 0.011(2) N4 0.083(4) 0.063(4) 0.032(3) 0.009(3) 0.002(2) 0.024(3) N5 0.207(7) 0.083(5) 0.049(3) -0.009(3) -0.002(4) 0.078(5) N6 0.036(3) 0.045(3) 0.055(3) -0.015(2) 0.007(2) -0.007(2) N7 0.048(3) 0.047(3) 0.073(3) -0.016(2) 0.002(3) 0.003(3) N8 0.053(4) 0.099(5) 0.161(6) -0.051(4) -0.024(4) 0.000(4) N9 0.044(3) 0.048(3) 0.044(3) -0.006(2) 0.008(2) -0.014(2) N10 0.064(4) 0.058(4) 0.062(3) -0.020(3) 0.016(3) -0.020(3) N11 0.134(6) 0.091(5) 0.116(5) -0.029(4) 0.065(4) -0.056(4) N12 0.043(3) 0.035(3) 0.041(2) -0.002(2) 0.0013(19) 0.002(2) N13 0.042(3) 0.057(3) 0.059(3) -0.009(2) -0.005(2) 0.001(2) N14 0.033(2) 0.040(3) 0.033(2) -0.0016(18) -0.0028(18) 0.004(2) N15 0.049(3) 0.046(3) 0.046(3) -0.004(2) -0.009(2) 0.002(2) N16 0.080(4) 0.111(5) 0.103(4) -0.021(4) -0.044(4) 0.014(4) N17 0.038(3) 0.050(3) 0.044(2) 0.011(2) 0.007(2) 0.007(2) N18 0.043(3) 0.056(3) 0.043(3) 0.003(2) 0.009(2) 0.005(3) N19 0.055(3) 0.113(5) 0.065(3) 0.007(3) -0.010(3) 0.025(3) N20 0.034(2) 0.038(3) 0.032(2) -0.0023(18) -0.0035(18) 0.002(2) N21 0.045(3) 0.049(3) 0.047(3) -0.008(2) -0.004(2) 0.003(2) N22 0.074(4) 0.103(5) 0.097(4) -0.021(3) -0.041(3) 0.011(3) N23 0.058(3) 0.040(3) 0.040(2) 0.000(2) -0.004(2) -0.008(2) N24 0.083(4) 0.064(4) 0.040(3) -0.005(3) 0.001(3) -0.025(3) N25 0.149(6) 0.122(6) 0.049(3) 0.014(3) -0.024(4) -0.036(4) N26 0.030(2) 0.038(3) 0.034(2) -0.0006(18) 0.0036(18) 0.0018(19) N27 0.044(3) 0.062(3) 0.049(3) 0.006(2) -0.002(2) -0.004(3) N28 0.072(4) 0.179(7) 0.105(5) 0.030(4) -0.043(4) -0.027(4) N29 0.037(3) 0.043(3) 0.065(3) 0.011(2) 0.013(2) -0.001(2) N30 0.045(3) 0.050(4) 0.074(3) 0.008(3) 0.023(3) -0.013(3) N31 0.072(4) 0.060(4) 0.166(6) 0.043(4) 0.029(4) 0.013(3) N32 0.064(3) 0.035(3) 0.033(2) 0.000(2) 0.003(2) -0.004(2) N33 0.076(4) 0.041(3) 0.049(3) 0.000(3) 0.002(3) 0.008(2) N34 0.165(6) 0.084(5) 0.043(3) 0.002(3) 0.017(3) 0.024(4) N35 0.056(3) 0.062(4) 0.048(3) -0.004(2) 0.005(2) -0.017(3) N36 0.064(4) 0.047(4) 0.067(3) 0.007(3) -0.010(3) -0.001(3) N37 0.126(6) 0.056(4) 0.143(6) -0.005(4) -0.046(4) -0.025(4) N38 0.052(3) 0.041(3) 0.037(2) -0.004(2) -0.010(2) 0.003(2) N39 0.054(3) 0.050(3) 0.056(3) 0.002(3) 0.003(3) 0.013(3) N40 0.076(4) 0.095(5) 0.078(4) -0.026(3) -0.025(3) 0.004(3) N41 0.041(3) 0.041(3) 0.055(3) 0.002(2) 0.016(2) 0.003(2) N42 0.057(3) 0.045(3) 0.067(3) 0.004(3) 0.020(2) 0.012(3) N43 0.112(5) 0.048(4) 0.114(5) 0.005(3) 0.054(4) 0.009(3) N44 0.051(3) 0.044(3) 0.043(3) -0.002(2) 0.006(2) 0.002(2) N45 0.059(3) 0.047(3) 0.045(3) -0.005(2) 0.017(2) -0.015(3) N46 0.053(4) 0.073(4) 0.049(3) 0.009(3) 0.008(2) -0.009(3) N47 0.093(5) 0.146(6) 0.087(4) -0.003(4) 0.003(3) -0.066(5) N48 0.065(4) 0.055(3) 0.050(3) 0.007(2) 0.017(2) 0.007(3) N49 0.071(4) 0.062(4) 0.059(4) 0.009(3) 0.020(3) -0.013(3) N50 0.084(5) 0.122(6) 0.101(5) 0.057(4) 0.000(4) -0.014(4) C1 0.044(4) 0.065(4) 0.064(4) 0.004(3) 0.009(3) 0.000(4) C2 0.053(5) 0.093(6) 0.074(4) 0.018(4) 0.002(3) -0.006(4) C3 0.069(5) 0.117(7) 0.060(4) -0.002(4) 0.001(3) -0.042(5) C4 0.085(5) 0.060(5) 0.071(4) -0.015(3) 0.020(4) -0.013(4) C5 0.051(4) 0.052(4) 0.047(3) -0.001(3) 0.014(3) -0.008(3) C6 0.067(5) 0.052(5) 0.079(4) 0.007(3) 0.028(4) -0.006(4) C7 0.109(6) 0.037(5) 0.212(9) -0.016(5) 0.048(6) 0.007(4) C8 0.049(4) 0.063(4) 0.078(4) -0.005(3) 0.012(3) -0.005(3) C9 0.039(4) 0.101(6) 0.137(7) -0.029(5) 0.016(4) -0.008(4) C10 0.049(5) 0.157(9) 0.131(7) -0.028(6) -0.034(5) 0.009(5) C11 0.053(5) 0.130(7) 0.091(5) -0.007(5) -0.025(4) 0.014(5) C12 0.041(4) 0.059(4) 0.062(4) 0.006(3) -0.017(3) 0.008(3) C13 0.062(4) 0.079(5) 0.043(3) 0.009(3) -0.008(3) -0.001(4) C14 0.109(6) 0.203(9) 0.037(4) 0.002(5) -0.005(4) -0.005(6) C15 0.039(3) 0.050(4) 0.047(3) -0.004(3) 0.003(2) -0.006(3) C16 0.038(4) 0.061(4) 0.068(4) -0.011(3) 0.001(3) -0.002(3) C17 0.045(4) 0.079(5) 0.063(4) -0.007(4) 0.003(3) 0.018(4) C18 0.053(4) 0.048(4) 0.063(4) 0.000(3) 0.004(3) 0.011(3) C19 0.045(4) 0.048(4) 0.040(3) -0.011(3) 0.003(2) 0.006(3) C20 0.056(4) 0.038(4) 0.059(4) -0.008(3) 0.008(3) -0.007(3) C21 0.071(5) 0.054(4) 0.101(5) 0.019(4) -0.002(4) -0.010(3) C22 0.054(4) 0.083(5) 0.104(5) -0.023(4) -0.013(4) 0.024(4) C23 0.056(5) 0.152(9) 0.150(8) -0.024(7) -0.033(5) 0.043(5) C24 0.081(6) 0.156(9) 0.099(6) -0.033(6) -0.036(5) 0.000(6) C25 0.066(5) 0.105(6) 0.063(4) -0.024(4) -0.007(4) -0.006(4) C26 0.049(4) 0.064(4) 0.048(3) -0.009(3) -0.001(3) -0.012(3) C27 0.067(5) 0.073(5) 0.054(4) -0.022(3) 0.014(3) -0.021(4) C28 0.088(6) 0.176(9) 0.166(8) -0.125(7) 0.022(5) -0.008(6) C29 0.072(4) 0.059(4) 0.048(3) -0.003(3) 0.004(3) 0.002(3) C30 0.125(7) 0.062(5) 0.062(4) -0.013(4) -0.009(4) 0.003(5) C31 0.108(7) 0.091(7) 0.108(6) -0.017(5) -0.059(5) 0.002(5) C32 0.070(5) 0.074(5) 0.107(5) -0.014(4) -0.033(4) 0.008(4) C33 0.055(4) 0.056(4) 0.048(3) 0.003(3) -0.004(3) 0.000(3) C34 0.048(4) 0.062(5) 0.070(4) 0.009(3) 0.002(3) 0.012(3) C35 0.054(4) 0.145(8) 0.120(6) -0.029(5) -0.021(4) 0.035(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 Cd1 N3 2.251(4) . ? Cd1 N38 2.268(4) 3_656 ? Cd1 N1 2.281(4) . ? Cd1 N2 2.303(4) . ? Cd1 O2 2.443(3) . ? Cd1 O1 2.475(4) . ? Cd2 N9 2.298(4) . ? Cd2 N6 2.327(4) . ? Cd2 N17 2.333(4) . ? Cd2 N3 2.339(4) . ? Cd2 N20 2.374(4) . ? Cd2 N14 2.404(4) . ? Cd3 N9 2.260(4) . ? Cd3 N23 2.268(4) . ? Cd3 N12 2.292(4) . ? Cd3 N13 2.347(4) . ? Cd3 O3 2.437(4) . ? Cd3 O4 2.503(4) . ? Cd4 N32 2.292(4) . ? Cd4 N17 2.311(4) . ? Cd4 N23 2.327(4) . ? Cd4 N29 2.329(4) . ? Cd4 N26 2.427(4) . ? Cd4 N20 2.547(4) . ? Cd5 N26 2.330(4) . ? Cd5 N26 2.330(4) 3_656 ? Cd5 N14 2.355(4) . ? Cd5 N14 2.355(4) 3_656 ? Cd5 N20 2.360(4) 3_656 ? Cd5 N20 2.360(4) . ? Cd6 N32 2.283(4) . ? Cd6 N6 2.314(4) 3_656 ? Cd6 N38 2.316(4) . ? Cd6 N41 2.347(4) . ? Cd6 N26 2.439(4) . ? Cd6 N14 2.472(4) 3_656 ? Cd7 N35 2.265(4) . ? Cd7 N29 2.298(4) . ? Cd7 N41 2.299(4) . ? Cd7 N44 2.374(4) . ? Cd7 N45 2.404(4) . ? Cd7 O5 2.454(4) . ? Cd8 N45 2.252(4) . ? Cd8 N51' 2.269(11) . ? Cd8 N48 2.293(5) . ? Cd8 N51 2.301(9) . ? Cd8 N35 2.311(4) . ? Cd8 N48 2.373(4) 3_557 ? Cd8 O6 2.539(8) . ? Cd8 O6' 2.564(10) . ? O1 C6 1.216(7) . ? O2 C13 1.204(6) . ? O3 C20 1.191(6) . ? O4 C27 1.193(6) . ? O5 C34 1.212(6) . ? N1 C1 1.304(6) . ? N1 C5 1.349(6) . ? N2 C8 1.317(6) . ? N2 C12 1.357(6) . ? N3 N4 1.208(6) . ? N4 N5 1.155(6) . ? N6 N7 1.192(6) . ? N6 Cd6 2.314(4) 3_656 ? N7 N8 1.131(6) . ? N9 N10 1.198(6) . ? N10 N11 1.139(6) . ? N12 C15 1.334(6) . ? N12 C19 1.337(6) . ? N13 C22 1.321(7) . ? N13 C26 1.338(6) . ? N14 N15 1.211(5) . ? N14 Cd6 2.472(4) 3_656 ? N15 N16 1.139(6) . ? N17 N18 1.209(5) . ? N18 N19 1.137(5) . ? N20 N21 1.210(5) . ? N21 N22 1.132(6) . ? N23 N24 1.204(5) . ? N24 N25 1.154(6) . ? N26 N27 1.217(5) . ? N27 N28 1.119(6) . ? N29 N30 1.210(6) . ? N30 N31 1.159(6) . ? N32 N33 1.217(5) . ? N33 N34 1.136(6) . ? N35 N36 1.194(6) . ? N36 N37 1.146(6) . ? N38 N39 1.222(5) . ? N38 Cd1 2.268(4) 3_656 ? N39 N40 1.160(6) . ? N41 N42 1.204(6) . ? N42 N43 1.150(6) . ? N44 C29 1.305(6) . ? N44 C33 1.334(6) . ? N45 N46 1.191(6) . ? N46 N47 1.143(6) . ? N48 N49 1.189(6) . ? N48 Cd8 2.373(4) 3_557 ? N49 N50 1.151(7) . ? C1 C2 1.382(8) . ? C2 C3 1.360(9) . ? C3 C4 1.363(9) . ? C4 C5 1.381(8) . ? C5 C6 1.467(8) . ? C6 C7 1.479(8) . ? C8 C9 1.394(8) . ? C9 C10 1.348(9) . ? C10 C11 1.353(9) . ? C11 C12 1.361(7) . ? C12 C13 1.496(7) . ? C13 C14 1.508(7) . ? C15 C16 1.356(7) . ? C16 C17 1.345(7) . ? C17 C18 1.374(7) . ? C18 C19 1.381(7) . ? C19 C20 1.531(7) . ? C20 C21 1.498(7) . ? C22 C23 1.415(8) . ? C23 C24 1.338(9) . ? C24 C25 1.340(9) . ? C25 C26 1.388(7) . ? C26 C27 1.489(8) . ? C27 C28 1.491(8) . ? C29 C30 1.391(8) . ? C30 C31 1.348(9) . ? C31 C32 1.355(9) . ? C32 C33 1.369(8) . ? C33 C34 1.481(8) . ? C34 C35 1.525(7) . ? O6 C36' 0.730(13) . ? O6 N51' 1.160(12) . ? O6 C41 1.404(12) . ? O6' C36 0.838(12) . ? O6' N51 1.249(12) . ? O6' C41' 1.496(16) . ? N51 C41' 1.02(2) . ? N51 C40' 1.152(18) . ? N51 C36 1.219(13) . ? N51 C40 1.50(2) . ? N51 N51' 1.645(14) . ? N51' C41 1.113(13) . ? N51' C36' 1.182(14) . ? N51' C40' 1.286(19) . ? N51' C40 1.47(2) . ? C36 C41' 0.839(18) . ? C36 C37 1.40(2) . ? C36 C42' 1.55(2) . ? C36 C40' 2.00(2) . ? C36' C41 0.887(13) . ? C36' C37' 1.509(19) . ? C36' C42 1.82(2) . ? C37 C38 1.35(2) . ? C37 C41' 1.47(3) . ? C37' C42 0.52(2) . ? C37' C38' 1.41(2) . ? C37' C41 1.421(19) . ? C38 C42' 1.16(2) . ? C38 C39 1.410(16) . ? C38 C41' 1.81(2) . ? C38' C42 1.008(19) . ? C38' C39' 1.470(19) . ? C38' C41 1.776(18) . ? C39 C39' 0.806(16) . ? C39 C40 1.318(19) . ? C39 C40' 1.60(2) . ? C39 C41' 1.84(2) . ? C39' C40 1.269(18) . ? C39' C40' 1.62(2) . ? C39' C41 1.952(18) . ? C40 C41 1.440(18) . ? C40 C41' 1.45(3) . ? C40' C41' 1.28(3) . ? C40' C41 1.53(2) . ? C41 C42 1.47(2) . ? C41' C42' 1.53(3) . ? O7 C43 1.407(11) . ? 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 N3 Cd1 N38 104.76(15) . 3_656 ? N3 Cd1 N1 96.25(14) . . ? N38 Cd1 N1 104.98(16) 3_656 . ? N3 Cd1 N2 95.68(15) . . ? N38 Cd1 N2 97.52(15) 3_656 . ? N1 Cd1 N2 150.84(15) . . ? N3 Cd1 O2 163.28(14) . . ? N38 Cd1 O2 84.29(13) 3_656 . ? N1 Cd1 O2 94.85(13) . . ? N2 Cd1 O2 68.89(13) . . ? N3 Cd1 O1 86.66(14) . . ? N38 Cd1 O1 167.47(13) 3_656 . ? N1 Cd1 O1 68.01(15) . . ? N2 Cd1 O1 86.26(14) . . ? O2 Cd1 O1 85.96(12) . . ? N9 Cd2 N6 94.62(14) . . ? N9 Cd2 N17 94.91(14) . . ? N6 Cd2 N17 170.29(15) . . ? N9 Cd2 N3 91.70(15) . . ? N6 Cd2 N3 92.76(15) . . ? N17 Cd2 N3 88.81(14) . . ? N9 Cd2 N20 93.78(14) . . ? N6 Cd2 N20 97.08(14) . . ? N17 Cd2 N20 80.44(13) . . ? N3 Cd2 N20 168.31(14) . . ? N9 Cd2 N14 171.12(14) . . ? N6 Cd2 N14 78.11(13) . . ? N17 Cd2 N14 92.23(13) . . ? N3 Cd2 N14 93.73(14) . . ? N20 Cd2 N14 82.19(13) . . ? N9 Cd3 N23 103.70(15) . . ? N9 Cd3 N12 110.96(14) . . ? N23 Cd3 N12 100.51(15) . . ? N9 Cd3 N13 91.16(15) . . ? N23 Cd3 N13 94.64(15) . . ? N12 Cd3 N13 149.01(15) . . ? N9 Cd3 O3 87.50(14) . . ? N23 Cd3 O3 167.43(14) . . ? N12 Cd3 O3 69.67(14) . . ? N13 Cd3 O3 90.76(14) . . ? N9 Cd3 O4 149.68(14) . . ? N23 Cd3 O4 98.12(14) . . ? N12 Cd3 O4 85.00(13) . . ? N13 Cd3 O4 66.09(14) . . ? O3 Cd3 O4 73.74(13) . . ? N32 Cd4 N17 165.20(14) . . ? N32 Cd4 N23 96.26(14) . . ? N17 Cd4 N23 86.35(14) . . ? N32 Cd4 N29 97.12(15) . . ? N17 Cd4 N29 95.97(15) . . ? N23 Cd4 N29 107.41(15) . . ? N32 Cd4 N26 79.24(13) . . ? N17 Cd4 N26 94.18(13) . . ? N23 Cd4 N26 163.61(14) . . ? N29 Cd4 N26 88.85(14) . . ? N32 Cd4 N20 88.16(13) . . ? N17 Cd4 N20 77.31(13) . . ? N23 Cd4 N20 88.93(13) . . ? N29 Cd4 N20 162.06(13) . . ? N26 Cd4 N20 75.26(12) . . ? N26 Cd5 N26 180.0 . 3_656 ? N26 Cd5 N14 97.76(13) . . ? N26 Cd5 N14 82.24(13) 3_656 . ? N26 Cd5 N14 82.24(13) . 3_656 ? N26 Cd5 N14 97.76(13) 3_656 3_656 ? N14 Cd5 N14 180.00(13) . 3_656 ? N26 Cd5 N20 99.25(13) . 3_656 ? N26 Cd5 N20 80.75(13) 3_656 3_656 ? N14 Cd5 N20 96.47(13) . 3_656 ? N14 Cd5 N20 83.53(13) 3_656 3_656 ? N26 Cd5 N20 80.75(13) . . ? N26 Cd5 N20 99.25(13) 3_656 . ? N14 Cd5 N20 83.53(13) . . ? N14 Cd5 N20 96.47(13) 3_656 . ? N20 Cd5 N20 180.00(11) 3_656 . ? N32 Cd6 N6 167.49(14) . 3_656 ? N32 Cd6 N38 101.18(14) . . ? N6 Cd6 N38 89.74(15) 3_656 . ? N32 Cd6 N41 89.67(15) . . ? N6 Cd6 N41 94.46(15) 3_656 . ? N38 Cd6 N41 100.00(15) . . ? N32 Cd6 N26 79.16(13) . . ? N6 Cd6 N26 88.72(14) 3_656 . ? N38 Cd6 N26 165.16(13) . . ? N41 Cd6 N26 94.84(14) . . ? N32 Cd6 N14 97.22(14) . 3_656 ? N6 Cd6 N14 76.98(13) 3_656 3_656 ? N38 Cd6 N14 87.55(13) . 3_656 ? N41 Cd6 N14 168.65(13) . 3_656 ? N26 Cd6 N14 77.73(12) . 3_656 ? N35 Cd7 N29 93.20(16) . . ? N35 Cd7 N41 113.55(16) . . ? N29 Cd7 N41 98.24(16) . . ? N35 Cd7 N44 148.64(16) . . ? N29 Cd7 N44 103.93(14) . . ? N41 Cd7 N44 90.07(15) . . ? N35 Cd7 N45 75.49(15) . . ? N29 Cd7 N45 166.89(15) . . ? N41 Cd7 N45 92.45(15) . . ? N44 Cd7 N45 83.54(14) . . ? N35 Cd7 O5 86.82(15) . . ? N29 Cd7 O5 91.16(14) . . ? N41 Cd7 O5 156.84(14) . . ? N44 Cd7 O5 67.06(14) . . ? N45 Cd7 O5 81.76(14) . . ? N45 Cd8 N51' 102.1(3) . . ? N45 Cd8 N48 108.47(17) . . ? N51' Cd8 N48 149.1(3) . . ? N45 Cd8 N51 144.1(3) . . ? N51' Cd8 N51 42.2(4) . . ? N48 Cd8 N51 107.4(3) . . ? N45 Cd8 N35 77.61(15) . . ? N51' Cd8 N35 87.7(3) . . ? N48 Cd8 N35 102.37(16) . . ? N51 Cd8 N35 93.9(2) . . ? N45 Cd8 N48 104.68(16) . 3_557 ? N51' Cd8 N48 90.7(3) . 3_557 ? N48 Cd8 N48 78.00(19) . 3_557 ? N51 Cd8 N48 83.6(2) . 3_557 ? N35 Cd8 N48 177.47(17) . 3_557 ? N45 Cd8 O6 76.5(2) . . ? N51' Cd8 O6 27.2(3) . . ? N48 Cd8 O6 166.6(2) . . ? N51 Cd8 O6 68.8(3) . . ? N35 Cd8 O6 90.8(2) . . ? N48 Cd8 O6 88.7(2) 3_557 . ? N45 Cd8 O6' 170.2(2) . . ? N51' Cd8 O6' 71.2(4) . . ? N48 Cd8 O6' 78.9(2) . . ? N51 Cd8 O6' 29.1(3) . . ? N35 Cd8 O6' 94.6(2) . . ? N48 Cd8 O6' 83.0(2) 3_557 . ? O6 Cd8 O6' 97.9(3) . . ? C6 O1 Cd1 116.3(4) . . ? C13 O2 Cd1 116.1(3) . . ? C20 O3 Cd3 115.8(4) . . ? C27 O4 Cd3 116.6(4) . . ? C34 O5 Cd7 116.6(4) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Cd1 121.5(4) . . ? C5 N1 Cd1 119.1(4) . . ? C8 N2 C12 118.4(5) . . ? C8 N2 Cd1 122.9(4) . . ? C12 N2 Cd1 118.7(3) . . ? N4 N3 Cd1 116.5(3) . . ? N4 N3 Cd2 112.6(3) . . ? Cd1 N3 Cd2 123.17(18) . . ? N5 N4 N3 179.2(7) . . ? N7 N6 Cd6 128.1(3) . 3_656 ? N7 N6 Cd2 121.8(3) . . ? Cd6 N6 Cd2 105.80(17) 3_656 . ? N8 N7 N6 178.5(7) . . ? N10 N9 Cd3 118.1(3) . . ? N10 N9 Cd2 117.3(3) . . ? Cd3 N9 Cd2 118.33(18) . . ? N11 N10 N9 178.0(7) . . ? C15 N12 C19 117.8(4) . . ? C15 N12 Cd3 123.4(4) . . ? C19 N12 Cd3 118.8(3) . . ? C22 N13 C26 118.4(5) . . ? C22 N13 Cd3 120.2(4) . . ? C26 N13 Cd3 121.1(4) . . ? N15 N14 Cd5 121.4(3) . . ? N15 N14 Cd2 113.4(3) . . ? Cd5 N14 Cd2 96.73(13) . . ? N15 N14 Cd6 122.4(3) . 3_656 ? Cd5 N14 Cd6 99.13(14) . 3_656 ? Cd2 N14 Cd6 98.78(14) . 3_656 ? N16 N15 N14 179.0(6) . . ? N18 N17 Cd4 132.0(3) . . ? N18 N17 Cd2 119.2(3) . . ? Cd4 N17 Cd2 105.02(16) . . ? N19 N18 N17 177.8(6) . . ? N21 N20 Cd5 121.5(3) . . ? N21 N20 Cd2 122.0(3) . . ? Cd5 N20 Cd2 97.40(13) . . ? N21 N20 Cd4 114.6(3) . . ? Cd5 N20 Cd4 99.67(13) . . ? Cd2 N20 Cd4 96.88(13) . . ? N22 N21 N20 177.3(6) . . ? N24 N23 Cd3 110.4(3) . . ? N24 N23 Cd4 116.5(3) . . ? Cd3 N23 Cd4 126.73(18) . . ? N25 N24 N23 179.7(7) . . ? N27 N26 Cd5 118.7(3) . . ? N27 N26 Cd4 120.4(3) . . ? Cd5 N26 Cd4 104.11(15) . . ? N27 N26 Cd6 112.9(3) . . ? Cd5 N26 Cd6 100.78(14) . . ? Cd4 N26 Cd6 95.95(13) . . ? N28 N27 N26 175.6(6) . . ? N30 N29 Cd7 111.0(3) . . ? N30 N29 Cd4 119.1(3) . . ? Cd7 N29 Cd4 129.5(2) . . ? N31 N30 N29 179.3(6) . . ? N33 N32 Cd6 116.8(3) . . ? N33 N32 Cd4 123.1(3) . . ? Cd6 N32 Cd4 104.37(15) . . ? N34 N33 N32 179.0(6) . . ? N36 N35 Cd7 130.2(4) . . ? N36 N35 Cd8 124.1(4) . . ? Cd7 N35 Cd8 104.56(19) . . ? N37 N36 N35 178.8(6) . . ? N39 N38 Cd1 109.8(3) . 3_656 ? N39 N38 Cd6 115.3(3) . . ? Cd1 N38 Cd6 128.53(17) 3_656 . ? N40 N39 N38 178.5(6) . . ? N42 N41 Cd7 109.8(3) . . ? N42 N41 Cd6 118.0(3) . . ? Cd7 N41 Cd6 132.3(2) . . ? N43 N42 N41 178.1(6) . . ? C29 N44 C33 117.9(5) . . ? C29 N44 Cd7 123.4(4) . . ? C33 N44 Cd7 117.2(3) . . ? N46 N45 Cd8 132.1(3) . . ? N46 N45 Cd7 124.3(3) . . ? Cd8 N45 Cd7 102.00(18) . . ? N47 N46 N45 176.8(7) . . ? N49 N48 Cd8 128.0(4) . . ? N49 N48 Cd8 113.8(4) . 3_557 ? Cd8 N48 Cd8 102.00(19) . 3_557 ? N50 N49 N48 177.9(7) . . ? N1 C1 C2 123.2(6) . . ? C3 C2 C1 117.5(7) . . ? C2 C3 C4 120.6(7) . . ? C3 C4 C5 118.6(7) . . ? N1 C5 C4 120.9(6) . . ? N1 C5 C6 117.0(5) . . ? C4 C5 C6 122.1(6) . . ? O1 C6 C5 118.5(6) . . ? O1 C6 C7 120.7(6) . . ? C5 C6 C7 120.8(6) . . ? N2 C8 C9 121.6(6) . . ? C10 C9 C8 119.4(6) . . ? C9 C10 C11 118.9(7) . . ? C10 C11 C12 120.3(7) . . ? N2 C12 C11 121.2(6) . . ? N2 C12 C13 114.8(4) . . ? C11 C12 C13 124.0(6) . . ? O2 C13 C12 120.5(5) . . ? O2 C13 C14 121.0(6) . . ? C12 C13 C14 118.5(5) . . ? N12 C15 C16 123.0(5) . . ? C17 C16 C15 119.1(5) . . ? C16 C17 C18 120.1(6) . . ? C17 C18 C19 117.9(6) . . ? N12 C19 C18 122.1(5) . . ? N12 C19 C20 114.7(5) . . ? C18 C19 C20 123.1(5) . . ? O3 C20 C21 122.7(5) . . ? O3 C20 C19 120.4(5) . . ? C21 C20 C19 116.8(5) . . ? N13 C22 C23 120.9(6) . . ? C24 C23 C22 120.3(7) . . ? C23 C24 C25 118.2(7) . . ? C24 C25 C26 120.9(6) . . ? N13 C26 C25 121.2(5) . . ? N13 C26 C27 113.8(5) . . ? C25 C26 C27 124.8(6) . . ? O4 C27 C26 120.1(5) . . ? O4 C27 C28 120.2(6) . . ? C26 C27 C28 119.7(6) . . ? N44 C29 C30 122.2(6) . . ? C31 C30 C29 119.6(6) . . ? C30 C31 C32 118.1(7) . . ? C31 C32 C33 119.9(7) . . ? N44 C33 C32 122.1(6) . . ? N44 C33 C34 115.5(5) . . ? C32 C33 C34 122.4(6) . . ? O5 C34 C33 120.1(5) . . ? O5 C34 C35 120.7(6) . . ? C33 C34 C35 119.2(6) . . ? C36' O6 N51' 73.5(13) . . ? C36' O6 C41 33.1(11) . . ? N51' O6 C41 50.4(6) . . ? C36' O6 Cd8 130.8(14) . . ? N51' O6 Cd8 63.3(7) . . ? C41 O6 Cd8 113.7(7) . . ? C36 O6' N51 68.3(11) . . ? C36 O6' C41' 26.9(12) . . ? N51 O6' C41' 42.3(9) . . ? C36 O6' Cd8 131.0(12) . . ? N51 O6' Cd8 63.7(6) . . ? C41' O6' Cd8 106.0(11) . . ? C41' N51 C40' 72.0(15) . . ? C41' N51 C36 42.9(11) . . ? C40' N51 C36 114.7(14) . . ? C41' N51 O6' 82.0(12) . . ? C40' N51 O6' 153.7(14) . . ? C36 N51 O6' 39.7(7) . . ? C41' N51 C40 67.6(16) . . ? C40' N51 C40 4.5(15) . . ? C36 N51 C40 110.4(11) . . ? O6' N51 C40 149.3(11) . . ? C41' N51 N51' 123.1(16) . . ? C40' N51 N51' 51.1(11) . . ? C36 N51 N51' 165.8(12) . . ? O6' N51 N51' 154.5(10) . . ? C40 N51 N51' 55.5(8) . . ? C41' N51 Cd8 169.1(15) . . ? C40' N51 Cd8 118.9(12) . . ? C36 N51 Cd8 126.2(10) . . ? O6' N51 Cd8 87.2(7) . . ? C40 N51 Cd8 123.4(8) . . ? N51' N51 Cd8 67.9(5) . . ? C41 N51' O6 76.3(9) . . ? C41 N51' C36' 45.3(8) . . ? O6 N51' C36' 36.3(7) . . ? C41 N51' C40' 78.9(13) . . ? O6 N51' C40' 151.4(14) . . ? C36' N51' C40' 123.8(15) . . ? C41 N51' C40 66.2(10) . . ? O6 N51' C40 140.5(12) . . ? C36' N51' C40 110.9(12) . . ? C40' N51' C40 12.9(13) . . ? C41 N51' N51 123.0(11) . . ? O6 N51' N51 154.9(11) . . ? C36' N51' N51 167.8(13) . . ? C40' N51' N51 44.2(9) . . ? C40 N51' N51 57.0(9) . . ? C41 N51' Cd8 165.5(11) . . ? O6 N51' Cd8 89.5(8) . . ? C36' N51' Cd8 122.1(11) . . ? C40' N51' Cd8 114.1(11) . . ? C40 N51' Cd8 127.0(10) . . ? N51 N51' Cd8 69.9(5) . . ? O6' C36 C41' 126(2) . . ? O6' C36 N51 72.0(11) . . ? C41' C36 N51 55.6(16) . . ? O6' C36 C37 152.7(17) . . ? C41' C36 C37 78(2) . . ? N51 C36 C37 133.4(15) . . ? O6' C36 C42' 160.7(17) . . ? C41' C36 C42' 73(2) . . ? N51 C36 C42' 125.9(14) . . ? C37 C36 C42' 17.0(11) . . ? O6' C36 C40' 103.4(13) . . ? C41' C36 C40' 24.2(17) . . ? N51 C36 C40' 31.6(7) . . ? C37 C36 C40' 101.8(12) . . ? C42' C36 C40' 95.2(12) . . ? O6 C36' C41 120.3(19) . . ? O6 C36' N51' 70.2(13) . . ? C41 C36' N51' 63.2(11) . . ? O6 C36' C37' 153.2(19) . . ? C41 C36' C37' 67.0(13) . . ? N51' C36' C37' 128.5(14) . . ? O6 C36' C42 149.8(17) . . ? C41 C36' C42 53.6(13) . . ? N51' C36' C42 116.4(13) . . ? C37' C36' C42 14.6(9) . . ? C38 C37 C36 113.0(14) . . ? C38 C37 C41' 79.8(12) . . ? C36 C37 C41' 33.9(8) . . ? C42 C37' C38' 33(3) . . ? C42 C37' C41 86(3) . . ? C38' C37' C41 77.9(10) . . ? C42 C37' C36' 119(4) . . ? C38' C37' C36' 112.0(12) . . ? C41 C37' C36' 35.1(6) . . ? C42' C38 C37 19.5(13) . . ? C42' C38 C39 122.6(15) . . ? C37 C38 C39 121.1(12) . . ? C42' C38 C41' 57.2(13) . . ? C37 C38 C41' 53.0(10) . . ? C39 C38 C41' 68.3(10) . . ? C42 C38' C37' 16.3(15) . . ? C42 C38' C39' 127(2) . . ? C37' C38' C39' 124.5(14) . . ? C42 C38' C41 56.1(14) . . ? C37' C38' C41 51.5(8) . . ? C39' C38' C41 73.2(10) . . ? C39' C39 C40 68.6(15) . . ? C39' C39 C38 157(2) . . ? C40 C39 C38 117.9(14) . . ? C39' C39 C40' 77.2(18) . . ? C40 C39 C40' 8.9(13) . . ? C38 C39 C40' 109.2(12) . . ? C39' C39 C41' 115.7(19) . . ? C40 C39 C41' 51.7(11) . . ? C38 C39 C41' 66.2(10) . . ? C40' C39 C41' 43.0(9) . . ? C39 C39' C40 75.2(17) . . ? C39 C39' C38' 160(2) . . ? C40 C39' C38' 107.9(15) . . ? C39 C39' C40' 73.8(17) . . ? C40 C39' C40' 2.5(14) . . ? C38' C39' C40' 109.9(13) . . ? C39 C39' C41 117.8(19) . . ? C40 C39' C41 47.5(10) . . ? C38' C39' C41 60.6(9) . . ? C40' C39' C41 49.7(9) . . ? C39' C40 C39 36.2(9) . . ? C39' C40 C41 91.9(14) . . ? C39 C40 C41 123.8(15) . . ? C39' C40 C41' 115.5(16) . . ? C39 C40 C41' 82.9(13) . . ? C41 C40 C41' 152.5(16) . . ? C39' C40 N51' 135.6(16) . . ? C39 C40 N51' 167.8(15) . . ? C41 C40 N51' 45.0(7) . . ? C41' C40 N51' 107.8(14) . . ? C39' C40 N51 154.8(15) . . ? C39 C40 N51 122.9(13) . . ? C41 C40 N51 112.3(12) . . ? C41' C40 N51 40.3(8) . . ? N51' C40 N51 67.4(9) . . ? N51 C40' C41' 49.1(12) . . ? N51 C40' N51' 84.7(15) . . ? C41' C40' N51' 134(2) . . ? N51 C40' C41 130.1(17) . . ? C41' C40' C41 178.5(19) . . ? N51' C40' C41 45.5(8) . . ? N51 C40' C39 127.4(17) . . ? C41' C40' C39 78.5(13) . . ? N51' C40' C39 147.6(18) . . ? C41 C40' C39 102.1(14) . . ? N51 C40' C39' 152.8(18) . . ? C41' C40' C39' 104.5(16) . . ? N51' C40' C39' 120.9(16) . . ? C41 C40' C39' 76.4(11) . . ? C39 C40' C39' 29.0(6) . . ? N51 C40' C36 33.7(8) . . ? C41' C40' C36 15.6(10) . . ? N51' C40' C36 118.4(15) . . ? C41 C40' C36 163.4(14) . . ? C39 C40' C36 93.7(12) . . ? C39' C40' C36 120.1(13) . . ? C36' C41 N51' 71.4(12) . . ? C36' C41 O6 26.7(10) . . ? N51' C41 O6 53.4(7) . . ? C36' C41 C37' 77.9(14) . . ? N51' C41 C37' 146.5(13) . . ? O6 C41 C37' 101.4(10) . . ? C36' C41 C40 139.1(16) . . ? N51' C41 C40 68.8(11) . . ? O6 C41 C40 121.0(11) . . ? C37' C41 C40 136.4(12) . . ? C36' C41 C42 97.5(16) . . ? N51' C41 C42 166.9(14) . . ? O6 C41 C42 118.6(13) . . ? C37' C41 C42 20.6(9) . . ? C40 C41 C42 120.4(13) . . ? C36' C41 C40' 126.4(16) . . ? N51' C41 C40' 55.5(10) . . ? O6 C41 C40' 107.6(11) . . ? C37' C41 C40' 148.7(13) . . ? C40 C41 C40' 13.4(11) . . ? C42 C41 C40' 133.8(14) . . ? C36' C41 C38' 127.1(16) . . ? N51' C41 C38' 150.1(13) . . ? O6 C41 C38' 152.0(11) . . ? C37' C41 C38' 50.7(9) . . ? C40 C41 C38' 86.5(10) . . ? C42 C41 C38' 34.6(8) . . ? C40' C41 C38' 99.7(11) . . ? C36' C41 C39' 162.8(15) . . ? N51' C41 C39' 108.6(11) . . ? O6 C41 C39' 161.5(10) . . ? C37' C41 C39' 96.7(10) . . ? C40 C41 C39' 40.5(8) . . ? C42 C41 C39' 79.9(10) . . ? C40' C41 C39' 53.9(10) . . ? C38' C41 C39' 46.1(6) . . ? C36 C41' N51 81.5(17) . . ? C36 C41' C40' 140(3) . . ? N51 C41' C40' 58.9(15) . . ? C36 C41' C40 153(3) . . ? N51 C41' C40 72.1(18) . . ? C40' C41' C40 13.2(13) . . ? C36 C41' C37 68(2) . . ? N51 C41' C37 150(2) . . ? C40' C41' C37 151.1(19) . . ? C40 C41' C37 138.0(16) . . ? C36 C41' O6' 26.8(12) . . ? N51 C41' O6' 55.7(10) . . ? C40' C41' O6' 114.6(17) . . ? C40 C41' O6' 127.7(18) . . ? C37 C41' O6' 94.4(15) . . ? C36 C41' C42' 76(2) . . ? N51 C41' C42' 151(2) . . ? C40' C41' C42' 139.4(18) . . ? C40 C41' C42' 127.9(15) . . ? C37 C41' C42' 17.6(11) . . ? O6' C41' C42' 102.4(17) . . ? C36 C41' C38 115(2) . . ? N51 C41' C38 161(2) . . ? C40' C41' C38 103.9(15) . . ? C40 C41' C38 90.9(11) . . ? C37 C41' C38 47.2(10) . . ? O6' C41' C38 141.2(18) . . ? C42' C41' C38 39.7(8) . . ? C36 C41' C39 159(3) . . ? N51 C41' C39 117(2) . . ? C40' C41' C39 58.5(13) . . ? C40 C41' C39 45.4(8) . . ? C37 C41' C39 92.6(13) . . ? O6' C41' C39 172.8(18) . . ? C42' C41' C39 83.8(11) . . ? C38 C41' C39 45.5(7) . . ? C37' C42 C38' 131(4) . . ? C37' C42 C41 74(3) . . ? C38' C42 C41 89.3(18) . . ? C37' C42 C36' 47(3) . . ? C38' C42 C36' 114.6(19) . . ? C41 C42 C36' 28.9(6) . . ? C38 C42' C41' 83.1(14) . . ? C38 C42' C36 114.1(16) . . ? C41' C42' C36 31.6(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.060 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.117