# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address J.Crowley ;Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; S.Scott ;Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; E.Gavey '' S.Lind '' K.Gordon '' _publ_contact_author_name 'Dr James Crowley' _publ_contact_author_address ;Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email jcrowley@chemistry.otago.ac.nz _publ_contact_author_phone +64-3-04797731 _publ_contact_author_fax +64-3-04797731 _publ_section_title ; Self-Assembled Palladium(II) "Click" Cages: Synthesis, Structural Modification and Stability. ; # Attachment '- seg242.cif' data_seg242 _database_code_depnum_ccdc_archive 'CCDC 819051' #TrackingRef '- seg242.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common "Pd ''click'' cage" _chemical_melting_point ? _chemical_formula_moiety 'C128 H120 B4 F16 N33 O16 Pd2' _chemical_formula_sum 'C128 H120 B4 F16 N33 O16 Pd2' _chemical_formula_weight 2936.61 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 27.9204(17) _cell_length_b 22.5838(14) _cell_length_c 24.610(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.689(3) _cell_angle_gamma 90.00 _cell_volume 13060.2(20) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6819 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 21.16 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6012 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8891 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43487 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 21.29 _reflns_number_total 7217 _reflns_number_gt 5761 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008)' _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^ > 2\s(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. ; 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 -0.028 -0.250 0.222 1281.8 354.4 2 -0.004 0.250 0.746 1281.7 354.4 _platon_squeeze_details ; The unit cell contains 32 acetonitrile molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.0997P)^2^+35.7097P] 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 7217 _refine_ls_number_parameters 826 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1495 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3019(3) 0.4885(3) 0.1915(3) 0.059(2) Uani 1 1 d . . . H1A H 0.2830 0.4528 0.1688 0.088 Uiso 1 1 calc R . . H1B H 0.3424 0.4830 0.2139 0.088 Uiso 1 1 calc R . . H1C H 0.2906 0.5205 0.1613 0.088 Uiso 1 1 calc R . . C2 C 0.2964(3) 0.4605(3) 0.2809(3) 0.0368(16) Uani 1 1 d . . . C3 C 0.2756(2) 0.4768(3) 0.3234(3) 0.0309(15) Uani 1 1 d . . . C4 C 0.2390(2) 0.5247(3) 0.3091(3) 0.0299(15) Uani 1 1 d . . . H4 H 0.2289 0.5488 0.2738 0.036 Uiso 1 1 calc R . . C5 C 0.2180(2) 0.5360(3) 0.3469(3) 0.0293(15) Uani 1 1 d . . . H5 H 0.1935 0.5678 0.3369 0.035 Uiso 1 1 calc R . . C6 C 0.2907(3) 0.4418(3) 0.3770(3) 0.0343(16) Uani 1 1 d . . . H6 H 0.3154 0.4101 0.3872 0.041 Uiso 1 1 calc R . . C7 C 0.2700(3) 0.4532(3) 0.4145(3) 0.0327(15) Uani 1 1 d . . . H7 H 0.2806 0.4293 0.4500 0.039 Uiso 1 1 calc R . . C8 C 0.2327(2) 0.5009(2) 0.4003(3) 0.0261(14) Uani 1 1 d . . . C9 C 0.2081(2) 0.5122(3) 0.4399(3) 0.0300(14) Uani 1 1 d . . . H9A H 0.2025 0.5544 0.4413 0.036 Uiso 1 1 calc R . . H9B H 0.2345 0.4987 0.4837 0.036 Uiso 1 1 calc R . . C10 C 0.1353(2) 0.4463(2) 0.4433(3) 0.0234(13) Uani 1 1 d . . . H10 H 0.1556 0.4361 0.4868 0.028 Uiso 1 1 calc R . . C11 C 0.0812(2) 0.4290(2) 0.3964(2) 0.0177(13) Uani 1 1 d . . . C12 C 0.0407(2) 0.3931(2) 0.4031(2) 0.0195(13) Uani 1 1 d . . . C13 C 0.0275(2) 0.4116(3) 0.4474(3) 0.0303(15) Uani 1 1 d . . . H13 H 0.0456 0.4444 0.4733 0.036 Uiso 1 1 calc R . . C14 C -0.0127(3) 0.3809(3) 0.4527(3) 0.0372(16) Uani 1 1 d . . . H14 H -0.0228 0.3942 0.4810 0.045 Uiso 1 1 calc R . . C15 C -0.0381(2) 0.3307(3) 0.4163(3) 0.0339(16) Uani 1 1 d . . . H15 H -0.0651 0.3105 0.4203 0.041 Uiso 1 1 calc R . . C16 C -0.0235(2) 0.3100(2) 0.3737(2) 0.0212(13) Uani 1 1 d . . . C17 C 0.0153(2) 0.3423(2) 0.3669(2) 0.0164(12) Uani 1 1 d . . . H17 H 0.0244 0.3298 0.3376 0.020 Uiso 1 1 calc R . . C18 C -0.0502(2) 0.2544(2) 0.3388(3) 0.0214(13) Uani 1 1 d . . . C19 C -0.0852(2) 0.2177(3) 0.3471(3) 0.0282(14) Uani 1 1 d . . . H19 H -0.0984 0.2237 0.3743 0.034 Uiso 1 1 calc R . . C20 C -0.1328(3) 0.1188(3) 0.2965(3) 0.0389(17) Uani 1 1 d . . . H20A H -0.1252 0.0884 0.2743 0.047 Uiso 1 1 calc R . . H20B H -0.1725 0.1300 0.2691 0.047 Uiso 1 1 calc R . . C21 C -0.1217(2) 0.0941(3) 0.3597(3) 0.0324(16) Uani 1 1 d . . . C22 C -0.1510(2) 0.1173(3) 0.3859(3) 0.0346(16) Uani 1 1 d . . . H22 H -0.1758 0.1489 0.3660 0.042 Uiso 1 1 calc R . . C23 C -0.1428(2) 0.0928(3) 0.4423(3) 0.0343(16) Uani 1 1 d . . . H23 H -0.1619 0.1086 0.4603 0.041 Uiso 1 1 calc R . . C24 C -0.0846(3) 0.0472(3) 0.3897(3) 0.0404(17) Uani 1 1 d . . . H24 H -0.0644 0.0320 0.3727 0.049 Uiso 1 1 calc R . . C25 C -0.0775(3) 0.0228(3) 0.4464(3) 0.0422(17) Uani 1 1 d . . . H25 H -0.0528 -0.0088 0.4667 0.051 Uiso 1 1 calc R . . C26 C -0.1070(3) 0.0455(3) 0.4715(3) 0.0350(16) Uani 1 1 d . . . C27 C -0.1005(3) 0.0161(3) 0.5298(3) 0.0476(19) Uani 1 1 d . . . C28 C -0.1295(5) 0.0170(4) 0.6044(4) 0.092(3) Uani 1 1 d . . . H28A H -0.0915 0.0211 0.6415 0.137 Uiso 1 1 calc R . . H28B H -0.1394 -0.0242 0.5967 0.137 Uiso 1 1 calc R . . H28C H -0.1555 0.0374 0.6120 0.137 Uiso 1 1 calc R . . C29 C -0.2609(5) 0.8136(5) 0.1462(7) 0.161(6) Uani 1 1 d . . . H29A H -0.2848 0.7947 0.1050 0.241 Uiso 1 1 calc R . . H29B H -0.2419 0.8467 0.1414 0.241 Uiso 1 1 calc R . . H29C H -0.2837 0.8272 0.1620 0.241 Uiso 1 1 calc R . . C30 C -0.2357(5) 0.7323(5) 0.2194(6) 0.101(4) Uani 1 1 d U . . C31 C -0.1908(3) 0.6898(4) 0.2634(6) 0.087(4) Uani 1 1 d . . . C32 C -0.1425(3) 0.6816(4) 0.2587(4) 0.079(3) Uani 1 1 d . . . H32 H -0.1377 0.7039 0.2302 0.095 Uiso 1 1 calc R . . C33 C -0.1032(3) 0.6395(4) 0.2981(5) 0.076(3) Uani 1 1 d . . . H33 H -0.0720 0.6323 0.2949 0.092 Uiso 1 1 calc R . . C34 C -0.1957(4) 0.6583(5) 0.3078(6) 0.092(4) Uani 1 1 d . . . H34 H -0.2267 0.6652 0.3115 0.110 Uiso 1 1 calc R . . C35 C -0.1564(3) 0.6175(4) 0.3465(4) 0.070(3) Uani 1 1 d . . . H35 H -0.1610 0.5963 0.3758 0.084 Uiso 1 1 calc R . . C36 C -0.1090(3) 0.6072(4) 0.3425(5) 0.065(3) Uani 1 1 d . . . C37 C -0.0657(3) 0.5628(4) 0.3843(4) 0.065(2) Uani 1 1 d . . . H37A H -0.0723 0.5495 0.4171 0.078 Uiso 1 1 calc R . . H37B H -0.0281 0.5805 0.4057 0.078 Uiso 1 1 calc R . . C38 C -0.1059(3) 0.4669(3) 0.3214(3) 0.0370(16) Uani 1 1 d . . . H38 H -0.1342 0.4597 0.3297 0.044 Uiso 1 1 calc R . . C39 C -0.0943(2) 0.4343(2) 0.2830(3) 0.0230(14) Uani 1 1 d . . . C40 C -0.1254(2) 0.3826(2) 0.2439(3) 0.0225(13) Uani 1 1 d . . . C41 C -0.1767(2) 0.3684(2) 0.2382(3) 0.0335(16) Uani 1 1 d . . . H41 H -0.1886 0.3903 0.2609 0.040 Uiso 1 1 calc R . . C42 C -0.1074(2) 0.3473(2) 0.2117(3) 0.0194(13) Uani 1 1 d . . . H42 H -0.0729 0.3552 0.2159 0.023 Uiso 1 1 calc R . . C43 C -0.2096(3) 0.3226(3) 0.1996(4) 0.0420(18) Uani 1 1 d . . . H43 H -0.2442 0.3146 0.1951 0.050 Uiso 1 1 calc R . . C44 C -0.1922(2) 0.2882(2) 0.1672(3) 0.0346(16) Uani 1 1 d . . . H44 H -0.2148 0.2570 0.1413 0.041 Uiso 1 1 calc R . . C45 C -0.1406(2) 0.3003(2) 0.1736(3) 0.0197(13) Uani 1 1 d . . . C46 C -0.1239(2) 0.2628(2) 0.1369(3) 0.0197(13) Uani 1 1 d . . . C47 C -0.1566(2) 0.2454(2) 0.0743(3) 0.0255(14) Uani 1 1 d . . . H47 H -0.1936 0.2572 0.0438 0.031 Uiso 1 1 calc R . . C48 C -0.1377(2) 0.1742(3) 0.0068(3) 0.0331(15) Uani 1 1 d . . . H48A H -0.1762 0.1834 -0.0283 0.040 Uiso 1 1 calc R . . H48B H -0.1356 0.1319 0.0150 0.040 Uiso 1 1 calc R . . C49 C -0.0965(3) 0.1906(3) -0.0120(3) 0.0318(15) Uani 1 1 d . . . C50 C -0.0481(3) 0.1564(3) 0.0087(3) 0.0380(16) Uani 1 1 d . . . H50 H -0.0426 0.1217 0.0318 0.046 Uiso 1 1 calc R . . C51 C -0.0082(3) 0.1736(3) -0.0048(3) 0.0455(18) Uani 1 1 d . . . H51 H 0.0242 0.1507 0.0095 0.055 Uiso 1 1 calc R . . C52 C -0.0165(3) 0.2253(3) -0.0399(3) 0.0462(18) Uani 1 1 d . . . C53 C -0.0656(3) 0.2584(3) -0.0615(3) 0.0485(19) Uani 1 1 d . . . H53 H -0.0716 0.2928 -0.0852 0.058 Uiso 1 1 calc R . . C54 C -0.1055(3) 0.2410(3) -0.0482(3) 0.0396(17) Uani 1 1 d . . . H54 H -0.1385 0.2632 -0.0637 0.047 Uiso 1 1 calc R . . C55 C 0.0267(4) 0.2470(4) -0.0515(4) 0.070(3) Uani 1 1 d . . . C56 C 0.1159(8) 0.2341(9) -0.0346(14) 0.323(18) Uani 1 1 d . . . H56A H 0.1309 0.2736 -0.0230 0.484 Uiso 1 1 calc R . . H56B H 0.0964 0.2294 -0.0805 0.484 Uiso 1 1 calc R . . H56C H 0.1466 0.2061 -0.0136 0.484 Uiso 1 1 calc R . . N1 N 0.15274(18) 0.48106(19) 0.4127(2) 0.0237(11) Uani 1 1 d . . . N2 N 0.11366(19) 0.48635(19) 0.3508(2) 0.0251(11) Uani 1 1 d . . . N3 N 0.07021(17) 0.45453(18) 0.3393(2) 0.0211(11) Uani 1 1 d . . . N4 N -0.04403(17) 0.22742(18) 0.2929(2) 0.0182(11) Uani 1 1 d . . . N5 N -0.07281(18) 0.1763(2) 0.2740(2) 0.0229(11) Uani 1 1 d . . . N6 N -0.09631(19) 0.1714(2) 0.3075(2) 0.0298(12) Uani 1 1 d . . . N7 N -0.0684(2) 0.5113(2) 0.3447(2) 0.0408(14) Uani 1 1 d . . . N8 N -0.03303(19) 0.5090(2) 0.3245(2) 0.0337(13) Uani 1 1 d . . . N9 N -0.04854(18) 0.46153(19) 0.2870(2) 0.0218(11) Uani 1 1 d . . . N10 N -0.07365(17) 0.23381(17) 0.1634(2) 0.0154(10) Uani 1 1 d . . . N11 N -0.07340(18) 0.19959(19) 0.1191(2) 0.0222(11) Uani 1 1 d . . . N12 N -0.12420(19) 0.2073(2) 0.0657(2) 0.0257(11) Uani 1 1 d . . . O1 O 0.3185(2) 0.4135(2) 0.2838(2) 0.0586(14) Uani 1 1 d . . . O2 O 0.28643(18) 0.50238(18) 0.2380(2) 0.0430(11) Uani 1 1 d . . . O3 O -0.0724(2) -0.0271(2) 0.5551(2) 0.0683(15) Uani 1 1 d . . . O4 O -0.1325(2) 0.0425(2) 0.5483(2) 0.0609(14) Uani 1 1 d . . . O5 O -0.2181(3) 0.7707(3) 0.1924(5) 0.136(4) Uani 1 1 d . . . O6 O -0.2841(3) 0.7325(3) 0.2085(4) 0.117(3) Uani 1 1 d . . . O7 O 0.0172(2) 0.2887(3) -0.0881(3) 0.091(2) Uani 1 1 d . . . O8 O 0.0772(3) 0.2242(3) -0.0148(4) 0.126(3) Uani 1 1 d . . . B1 B 0.7592(3) 0.1367(3) 0.0774(4) 0.041(2) Uani 1 1 d . . . F1 F 0.7259(2) 0.0927(2) 0.0807(2) 0.0970(19) Uani 1 1 d . . . F2 F 0.72884(16) 0.18852(19) 0.0582(2) 0.0696(12) Uani 1 1 d . . . F3 F 0.80773(15) 0.14438(15) 0.13770(18) 0.0537(11) Uani 1 1 d . . . F4 F 0.7714(2) 0.1217(2) 0.0334(3) 0.1010(18) Uani 1 1 d . . . Pd1 Pd 0.0000 0.45367(2) 0.2500 0.0193(2) Uani 1 2 d S . . Pd2 Pd 0.0000 0.23573(2) 0.2500 0.0158(2) Uani 1 2 d S . . B2 B 0.1393(5) 0.5658(6) 0.5480(7) 0.072(3) Uani 1 1 d . . . F21 F 0.1749(11) 0.5670(11) 0.5237(11) 0.064(6) Uani 0.584(14) 1 d PU A 1 F22 F 0.0834(4) 0.5547(6) 0.4908(6) 0.075(3) Uani 0.584(14) 1 d P A 1 F23 F 0.1243(4) 0.6261(4) 0.5397(7) 0.079(3) Uani 0.584(14) 1 d P A 1 F24 F 0.1737(5) 0.5642(6) 0.6176(7) 0.103(5) Uani 0.584(14) 1 d P A 1 F31 F 0.1415(8) 0.5060(8) 0.5767(8) 0.081(7) Uani 0.416(14) 1 d P A 2 F32 F 0.1401(6) 0.6024(7) 0.5869(9) 0.071(5) Uani 0.416(14) 1 d P A 2 F33 F 0.1075(10) 0.5236(11) 0.5389(15) 0.084(9) Uani 0.416(14) 1 d P A 2 F34 F 0.1858(14) 0.5524(14) 0.5440(14) 0.048(6) Uani 0.416(14) 1 d P A 2 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 C1 0.073(5) 0.075(5) 0.040(5) 0.001(4) 0.037(4) -0.017(4) C2 0.038(4) 0.040(4) 0.029(4) -0.006(3) 0.016(3) -0.018(3) C3 0.025(3) 0.035(4) 0.028(4) 0.000(3) 0.010(3) -0.009(3) C4 0.023(3) 0.032(4) 0.024(4) 0.008(3) 0.006(3) -0.010(3) C5 0.019(3) 0.029(3) 0.029(4) 0.004(3) 0.006(3) -0.007(3) C6 0.036(4) 0.032(4) 0.029(4) 0.012(3) 0.014(3) 0.008(3) C7 0.037(4) 0.035(4) 0.023(4) 0.010(3) 0.014(3) 0.000(3) C8 0.015(3) 0.037(4) 0.015(3) -0.003(3) 0.000(3) -0.016(3) C9 0.017(3) 0.039(4) 0.019(3) -0.001(3) 0.000(3) -0.010(3) C10 0.023(3) 0.030(3) 0.018(3) -0.001(3) 0.012(3) -0.001(3) C11 0.015(3) 0.022(3) 0.012(3) -0.002(3) 0.004(3) 0.004(2) C12 0.014(3) 0.026(3) 0.015(3) 0.000(3) 0.006(3) 0.002(3) C13 0.026(3) 0.043(4) 0.019(3) -0.013(3) 0.010(3) -0.007(3) C14 0.039(4) 0.061(4) 0.026(4) -0.020(3) 0.027(3) -0.010(3) C15 0.026(3) 0.059(4) 0.022(4) -0.009(3) 0.017(3) -0.013(3) C16 0.021(3) 0.035(3) 0.010(3) -0.002(3) 0.010(3) -0.004(3) C17 0.016(3) 0.029(3) 0.009(3) 0.003(3) 0.010(3) 0.004(2) C18 0.017(3) 0.037(3) 0.011(3) 0.004(3) 0.009(3) 0.003(3) C19 0.026(3) 0.045(4) 0.021(3) -0.006(3) 0.017(3) -0.011(3) C20 0.033(4) 0.048(4) 0.036(4) -0.004(3) 0.019(3) -0.028(3) C21 0.032(4) 0.037(4) 0.031(4) -0.008(3) 0.019(3) -0.027(3) C22 0.028(4) 0.040(4) 0.035(4) 0.010(3) 0.016(3) -0.011(3) C23 0.028(4) 0.040(4) 0.030(4) -0.001(3) 0.012(3) -0.017(3) C24 0.042(4) 0.038(4) 0.043(5) -0.013(4) 0.025(4) -0.017(3) C25 0.051(4) 0.033(4) 0.035(4) -0.003(3) 0.019(4) -0.011(3) C26 0.045(4) 0.033(4) 0.021(4) -0.004(3) 0.013(4) -0.016(3) C27 0.069(5) 0.036(4) 0.028(4) -0.003(4) 0.019(4) -0.021(4) C28 0.143(9) 0.105(7) 0.053(6) 0.019(5) 0.070(6) -0.007(6) C29 0.101(9) 0.088(8) 0.200(15) -0.013(9) 0.020(10) 0.051(7) C30 0.092(7) 0.064(6) 0.107(7) -0.063(5) 0.027(6) 0.008(6) C31 0.033(5) 0.059(6) 0.095(8) -0.063(6) -0.014(5) 0.023(5) C32 0.056(6) 0.059(5) 0.078(7) -0.040(5) 0.007(5) 0.012(5) C33 0.049(5) 0.075(6) 0.068(7) -0.053(5) 0.008(5) 0.018(5) C34 0.047(6) 0.087(8) 0.097(9) -0.067(7) 0.010(7) 0.003(6) C35 0.043(5) 0.075(6) 0.066(6) -0.054(5) 0.013(5) 0.004(5) C36 0.039(5) 0.072(6) 0.060(6) -0.056(5) 0.010(5) 0.008(4) C37 0.045(5) 0.085(6) 0.046(5) -0.052(5) 0.012(4) 0.001(4) C38 0.021(4) 0.064(4) 0.019(4) -0.010(3) 0.006(3) 0.009(3) C39 0.017(3) 0.039(4) 0.011(3) 0.001(3) 0.006(3) 0.012(3) C40 0.020(3) 0.028(3) 0.016(3) 0.006(3) 0.008(3) 0.011(3) C41 0.040(4) 0.026(3) 0.057(5) -0.004(3) 0.041(4) 0.004(3) C42 0.015(3) 0.032(3) 0.013(3) 0.002(3) 0.008(3) 0.002(3) C43 0.034(4) 0.031(4) 0.077(5) -0.001(4) 0.040(4) 0.000(3) C44 0.029(4) 0.025(3) 0.051(4) -0.001(3) 0.022(4) -0.005(3) C45 0.014(3) 0.024(3) 0.017(3) 0.005(3) 0.006(3) 0.004(2) C46 0.013(3) 0.024(3) 0.014(3) 0.001(3) 0.002(3) -0.001(3) C47 0.015(3) 0.029(3) 0.024(4) 0.005(3) 0.004(3) 0.001(3) C48 0.029(4) 0.041(4) 0.014(3) -0.007(3) 0.002(3) 0.001(3) C49 0.036(4) 0.036(4) 0.013(3) -0.012(3) 0.007(3) 0.003(3) C50 0.047(4) 0.036(4) 0.023(4) 0.006(3) 0.013(3) 0.018(3) C51 0.045(4) 0.053(4) 0.037(4) 0.010(4) 0.022(4) 0.025(4) C52 0.049(4) 0.062(5) 0.033(4) 0.016(4) 0.026(4) 0.025(4) C53 0.049(5) 0.061(5) 0.034(4) 0.021(4) 0.022(4) 0.022(4) C54 0.041(4) 0.044(4) 0.032(4) 0.009(3) 0.019(4) 0.020(3) C55 0.070(6) 0.085(6) 0.075(6) 0.047(5) 0.052(6) 0.044(5) C56 0.23(2) 0.27(2) 0.62(5) 0.29(3) 0.33(3) 0.123(17) N1 0.017(3) 0.028(3) 0.016(3) -0.002(2) 0.003(3) -0.003(2) N2 0.024(3) 0.027(3) 0.018(3) 0.000(2) 0.007(3) -0.006(2) N3 0.012(3) 0.018(2) 0.018(3) 0.001(2) -0.002(2) -0.002(2) N4 0.014(2) 0.021(3) 0.020(3) 0.000(2) 0.009(2) -0.007(2) N5 0.022(3) 0.032(3) 0.018(3) 0.002(2) 0.012(2) -0.005(2) N6 0.028(3) 0.041(3) 0.022(3) -0.003(3) 0.014(3) -0.015(2) N7 0.030(3) 0.060(4) 0.021(3) -0.025(3) 0.006(3) 0.009(3) N8 0.021(3) 0.044(3) 0.022(3) -0.014(3) 0.002(3) 0.006(2) N9 0.016(3) 0.027(3) 0.012(3) -0.005(2) 0.001(2) 0.006(2) N10 0.012(3) 0.018(2) 0.014(3) 0.000(2) 0.006(2) -0.0021(19) N11 0.022(3) 0.028(3) 0.015(3) -0.008(2) 0.009(3) -0.006(2) N12 0.021(3) 0.033(3) 0.019(3) -0.006(2) 0.008(3) -0.005(2) O1 0.091(4) 0.040(3) 0.068(4) 0.007(3) 0.058(3) 0.006(3) O2 0.056(3) 0.045(3) 0.032(3) 0.006(2) 0.027(2) -0.008(2) O3 0.099(4) 0.049(3) 0.044(3) 0.016(3) 0.031(3) 0.004(3) O4 0.094(4) 0.064(3) 0.034(3) 0.009(2) 0.040(3) -0.005(3) O5 0.070(5) 0.062(5) 0.182(9) -0.028(5) 0.008(5) 0.035(4) O6 0.054(4) 0.100(5) 0.132(6) -0.073(5) 0.007(4) 0.024(4) O7 0.051(3) 0.156(6) 0.078(4) 0.065(5) 0.043(3) 0.031(4) O8 0.088(5) 0.145(6) 0.184(8) 0.091(6) 0.098(6) 0.067(5) B1 0.040(5) 0.043(5) 0.026(5) -0.001(4) 0.010(4) -0.014(4) F1 0.091(3) 0.104(4) 0.035(3) 0.013(2) -0.006(3) -0.071(3) F2 0.041(2) 0.079(3) 0.053(3) 0.008(2) 0.001(2) 0.009(2) F3 0.040(2) 0.042(2) 0.036(2) -0.0007(18) -0.008(2) -0.0071(17) F4 0.119(4) 0.117(4) 0.093(4) -0.065(3) 0.074(4) -0.051(3) Pd1 0.0158(4) 0.0237(4) 0.0130(4) 0.000 0.0042(3) 0.000 Pd2 0.0147(4) 0.0211(4) 0.0119(4) 0.000 0.0074(3) 0.000 B2 0.054(7) 0.091(10) 0.088(10) -0.039(8) 0.051(8) -0.010(7) F21 0.069(10) 0.063(11) 0.080(14) -0.017(8) 0.053(10) 0.000(7) F22 0.037(5) 0.111(8) 0.057(7) -0.034(6) 0.011(5) 0.002(5) F23 0.070(6) 0.080(7) 0.116(10) -0.007(6) 0.069(7) 0.005(5) F24 0.087(8) 0.109(9) 0.156(13) -0.013(9) 0.094(9) -0.018(7) F31 0.081(12) 0.120(14) 0.067(12) 0.017(10) 0.057(11) 0.035(10) F32 0.054(9) 0.073(11) 0.098(13) -0.061(11) 0.049(10) -0.015(8) F33 0.066(13) 0.095(15) 0.11(2) -0.089(15) 0.064(14) -0.052(12) F34 0.046(11) 0.059(14) 0.056(14) -0.006(9) 0.038(11) 0.003(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O2 1.458(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.210(7) . ? C2 O2 1.330(7) . ? C2 C3 1.493(9) . ? C3 C6 1.393(8) . ? C3 C4 1.396(8) . ? C4 C5 1.366(8) . ? C4 H4 0.9300 . ? C5 C8 1.393(8) . ? C5 H5 0.9300 . ? C6 C7 1.351(8) . ? C6 H6 0.9300 . ? C7 C8 1.405(8) . ? C7 H7 0.9300 . ? C8 C9 1.486(8) . ? C9 N1 1.488(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N1 1.348(7) . ? C10 C11 1.373(7) . ? C10 H10 0.9300 . ? C11 N3 1.391(7) . ? C11 C12 1.472(7) . ? C12 C17 1.388(7) . ? C12 C13 1.389(7) . ? C13 C14 1.385(8) . ? C13 H13 0.9300 . ? C14 C15 1.379(8) . ? C14 H14 0.9300 . ? C15 C16 1.395(8) . ? C15 H15 0.9300 . ? C16 C17 1.389(7) . ? C16 C18 1.477(8) . ? C17 H17 0.9300 . ? C18 N4 1.373(7) . ? C18 C19 1.378(7) . ? C19 N6 1.347(7) . ? C19 H19 0.9300 . ? C20 N6 1.491(7) . ? C20 C21 1.521(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C24 1.383(9) . ? C21 C22 1.387(8) . ? C22 C23 1.394(8) . ? C22 H22 0.9300 . ? C23 C26 1.371(8) . ? C23 H23 0.9300 . ? C24 C25 1.412(9) . ? C24 H24 0.9300 . ? C25 C26 1.367(9) . ? C25 H25 0.9300 . ? C26 C27 1.498(9) . ? C27 O3 1.196(8) . ? C27 O4 1.343(9) . ? C28 O4 1.455(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O5 1.481(13) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O6 1.228(13) . ? C30 O5 1.335(15) . ? C30 C31 1.483(15) . ? C31 C34 1.373(14) . ? C31 C32 1.427(13) . ? C32 C33 1.379(12) . ? C32 H32 0.9300 . ? C33 C36 1.393(12) . ? C33 H33 0.9300 . ? C34 C35 1.353(13) . ? C34 H34 0.9300 . ? C35 C36 1.400(10) . ? C35 H35 0.9300 . ? C36 C37 1.478(11) . ? C37 N7 1.492(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 N7 1.333(8) . ? C38 C39 1.370(8) . ? C38 H38 0.9300 . ? C39 N9 1.372(7) . ? C39 C40 1.462(8) . ? C40 C42 1.395(7) . ? C40 C41 1.401(7) . ? C41 C43 1.369(9) . ? C41 H41 0.9300 . ? C42 C45 1.388(7) . ? C42 H42 0.9300 . ? C43 C44 1.376(8) . ? C43 H43 0.9300 . ? C44 C45 1.389(7) . ? C44 H44 0.9300 . ? C45 C46 1.485(8) . ? C46 N10 1.353(6) . ? C46 C47 1.357(8) . ? C47 N12 1.344(7) . ? C47 H47 0.9300 . ? C48 N12 1.488(7) . ? C48 C49 1.501(8) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C54 1.382(9) . ? C49 C50 1.394(8) . ? C50 C51 1.378(9) . ? C50 H50 0.9300 . ? C51 C52 1.397(9) . ? C51 H51 0.9300 . ? C52 C53 1.391(9) . ? C52 C55 1.464(10) . ? C53 C54 1.375(9) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 O7 1.230(9) . ? C55 O8 1.302(9) . ? C56 O8 1.425(15) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? N1 N2 1.316(6) . ? N2 N3 1.303(6) . ? N3 Pd1 2.005(4) . ? N4 N5 1.338(6) . ? N4 Pd2 2.015(4) . ? N5 N6 1.305(6) . ? N7 N8 1.325(7) . ? N8 N9 1.325(6) . ? N9 Pd1 2.008(4) . ? N10 N11 1.339(6) . ? N10 Pd2 2.009(4) . ? N11 N12 1.325(6) . ? B1 F4 1.342(9) . ? B1 F2 1.372(9) . ? B1 F3 1.377(8) . ? B1 F1 1.392(8) . ? Pd1 N3 2.005(4) 2 ? Pd1 N9 2.008(4) 2 ? Pd2 N10 2.009(4) 2 ? Pd2 N4 2.015(4) 2 ? B2 F33 1.236(17) . ? B2 F32 1.257(16) . ? B2 F34 1.39(4) . ? B2 F23 1.406(15) . ? B2 F21 1.41(3) . ? B2 F24 1.443(17) . ? B2 F22 1.451(17) . ? B2 F31 1.51(2) . ? F31 F33 0.99(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 O2 123.5(6) . . ? O1 C2 C3 123.7(6) . . ? O2 C2 C3 112.7(6) . . ? C6 C3 C4 119.0(6) . . ? C6 C3 C2 119.4(6) . . ? C4 C3 C2 121.5(6) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C8 121.4(6) . . ? C4 C5 H5 119.3 . . ? C8 C5 H5 119.3 . . ? C7 C6 C3 121.0(6) . . ? C7 C6 H6 119.5 . . ? C3 C6 H6 119.5 . . ? C6 C7 C8 120.6(5) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C5 C8 C7 118.1(5) . . ? C5 C8 C9 121.1(5) . . ? C7 C8 C9 120.8(5) . . ? C8 C9 N1 111.0(4) . . ? C8 C9 H9A 109.4 . . ? N1 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? N1 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N1 C10 C11 105.1(5) . . ? N1 C10 H10 127.4 . . ? C11 C10 H10 127.4 . . ? C10 C11 N3 105.9(4) . . ? C10 C11 C12 128.8(5) . . ? N3 C11 C12 125.3(4) . . ? C17 C12 C13 119.5(5) . . ? C17 C12 C11 122.7(5) . . ? C13 C12 C11 117.8(5) . . ? C14 C13 C12 119.6(5) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.5(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C18 124.0(5) . . ? C15 C16 C18 117.5(5) . . ? C12 C17 C16 121.2(5) . . ? C12 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? N4 C18 C19 105.7(5) . . ? N4 C18 C16 127.4(4) . . ? C19 C18 C16 126.8(5) . . ? N6 C19 C18 105.2(5) . . ? N6 C19 H19 127.4 . . ? C18 C19 H19 127.4 . . ? N6 C20 C21 111.5(5) . . ? N6 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N6 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C24 C21 C22 120.1(6) . . ? C24 C21 C20 120.4(6) . . ? C22 C21 C20 119.5(6) . . ? C21 C22 C23 119.5(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C26 C23 C22 120.8(6) . . ? C26 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C21 C24 C25 119.3(6) . . ? C21 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.2(6) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C23 120.1(6) . . ? C25 C26 C27 118.3(6) . . ? C23 C26 C27 121.6(6) . . ? O3 C27 O4 123.7(6) . . ? O3 C27 C26 124.5(7) . . ? O4 C27 C26 111.7(7) . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 H29A 109.5 . . ? O5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C30 O5 123.1(12) . . ? O6 C30 C31 123.9(14) . . ? O5 C30 C31 112.9(12) . . ? C34 C31 C32 120.2(9) . . ? C34 C31 C30 120.6(12) . . ? C32 C31 C30 119.2(13) . . ? C33 C32 C31 117.4(10) . . ? C33 C32 H32 121.3 . . ? C31 C32 H32 121.3 . . ? C32 C33 C36 121.9(9) . . ? C32 C33 H33 119.1 . . ? C36 C33 H33 119.1 . . ? C35 C34 C31 121.5(10) . . ? C35 C34 H34 119.3 . . ? C31 C34 H34 119.3 . . ? C34 C35 C36 120.2(11) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C33 C36 C35 118.9(9) . . ? C33 C36 C37 120.2(7) . . ? C35 C36 C37 120.9(10) . . ? C36 C37 N7 109.9(6) . . ? C36 C37 H37A 109.7 . . ? N7 C37 H37A 109.7 . . ? C36 C37 H37B 109.7 . . ? N7 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? N7 C38 C39 106.1(5) . . ? N7 C38 H38 126.9 . . ? C39 C38 H38 126.9 . . ? C38 C39 N9 105.5(5) . . ? C38 C39 C40 127.4(5) . . ? N9 C39 C40 127.1(5) . . ? C42 C40 C41 118.3(5) . . ? C42 C40 C39 124.3(5) . . ? C41 C40 C39 117.4(5) . . ? C43 C41 C40 120.6(5) . . ? C43 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C45 C42 C40 120.5(5) . . ? C45 C42 H42 119.7 . . ? C40 C42 H42 119.7 . . ? C41 C43 C44 121.0(5) . . ? C41 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C45 119.5(6) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C42 C45 C44 120.0(5) . . ? C42 C45 C46 122.2(4) . . ? C44 C45 C46 117.8(5) . . ? N10 C46 C47 107.1(5) . . ? N10 C46 C45 124.5(5) . . ? C47 C46 C45 128.0(5) . . ? N12 C47 C46 105.4(5) . . ? N12 C47 H47 127.3 . . ? C46 C47 H47 127.3 . . ? N12 C48 C49 110.0(5) . . ? N12 C48 H48A 109.7 . . ? C49 C48 H48A 109.7 . . ? N12 C48 H48B 109.7 . . ? C49 C48 H48B 109.7 . . ? H48A C48 H48B 108.2 . . ? C54 C49 C50 119.7(6) . . ? C54 C49 C48 120.1(5) . . ? C50 C49 C48 120.2(6) . . ? C51 C50 C49 120.3(6) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C52 120.1(6) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 119.0(6) . . ? C53 C52 C55 119.4(6) . . ? C51 C52 C55 121.5(6) . . ? C54 C53 C52 120.9(6) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C53 C54 C49 120.0(6) . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? O7 C55 O8 122.3(8) . . ? O7 C55 C52 121.7(7) . . ? O8 C55 C52 115.4(7) . . ? O8 C56 H56A 109.5 . . ? O8 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O8 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N2 N1 C10 112.1(4) . . ? N2 N1 C9 119.3(4) . . ? C10 N1 C9 128.6(5) . . ? N3 N2 N1 107.1(4) . . ? N2 N3 C11 109.8(4) . . ? N2 N3 Pd1 119.2(3) . . ? C11 N3 Pd1 130.9(3) . . ? N5 N4 C18 110.4(4) . . ? N5 N4 Pd2 108.7(3) . . ? C18 N4 Pd2 140.6(3) . . ? N6 N5 N4 105.5(4) . . ? N5 N6 C19 113.2(4) . . ? N5 N6 C20 118.7(5) . . ? C19 N6 C20 128.1(5) . . ? N8 N7 C38 112.4(5) . . ? N8 N7 C37 119.3(6) . . ? C38 N7 C37 128.2(6) . . ? N9 N8 N7 105.3(4) . . ? N8 N9 C39 110.7(4) . . ? N8 N9 Pd1 109.9(3) . . ? C39 N9 Pd1 139.2(4) . . ? N11 N10 C46 110.2(4) . . ? N11 N10 Pd2 115.0(3) . . ? C46 N10 Pd2 134.6(4) . . ? N12 N11 N10 105.0(4) . . ? N11 N12 C47 112.3(4) . . ? N11 N12 C48 118.2(4) . . ? C47 N12 C48 129.5(5) . . ? C2 O2 C1 116.4(5) . . ? C27 O4 C28 116.0(6) . . ? C30 O5 C29 116.5(10) . . ? C55 O8 C56 116.0(10) . . ? F4 B1 F2 108.4(6) . . ? F4 B1 F3 111.8(6) . . ? F2 B1 F3 109.2(6) . . ? F4 B1 F1 109.6(6) . . ? F2 B1 F1 108.7(6) . . ? F3 B1 F1 109.1(6) . . ? N3 Pd1 N3 178.9(2) 2 . ? N3 Pd1 N9 89.81(17) 2 . ? N3 Pd1 N9 90.09(17) . . ? N3 Pd1 N9 90.09(17) 2 2 ? N3 Pd1 N9 89.81(17) . 2 ? N9 Pd1 N9 169.9(2) . 2 ? N10 Pd2 N10 177.5(2) . 2 ? N10 Pd2 N4 89.37(16) . . ? N10 Pd2 N4 90.40(17) 2 . ? N10 Pd2 N4 90.40(17) . 2 ? N10 Pd2 N4 89.37(16) 2 2 ? N4 Pd2 N4 169.3(2) . 2 ? F33 B2 F32 111.1(12) . . ? F33 B2 F34 115.3(18) . . ? F32 B2 F34 124.4(18) . . ? F33 B2 F23 126.2(16) . . ? F32 B2 F23 49.8(10) . . ? F34 B2 F23 114.7(16) . . ? F33 B2 F21 122.6(15) . . ? F32 B2 F21 125.7(16) . . ? F34 B2 F21 22.0(14) . . ? F23 B2 F21 98.3(13) . . ? F33 B2 F24 98.5(18) . . ? F32 B2 F24 52.0(11) . . ? F34 B2 F24 91.7(15) . . ? F23 B2 F24 98.7(11) . . ? F21 B2 F24 109.5(13) . . ? F33 B2 F22 53.3(15) . . ? F32 B2 F22 114.9(11) . . ? F34 B2 F22 116.8(17) . . ? F23 B2 F22 86.9(11) . . ? F21 B2 F22 103.1(14) . . ? F24 B2 F22 145.6(11) . . ? F33 B2 F31 40.5(14) . . ? F32 B2 F31 104.6(15) . . ? F34 B2 F31 92.0(15) . . ? F23 B2 F31 150.1(10) . . ? F21 B2 F31 110.8(12) . . ? F24 B2 F31 65.7(10) . . ? F22 B2 F31 92.9(12) . . ? F33 F31 B2 54.6(13) . . ? F31 F33 B2 84.8(18) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 21.29 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.850 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.091 # Attachment '- sos004.cif' data_test1 _database_code_depnum_ccdc_archive 'CCDC 819052' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common di-triazole _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N6 O2' _chemical_formula_sum 'C26 H24 N6 O2' _chemical_formula_weight 452.51 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc _symmetry_space_group_name_Hall 'P -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 20.910(6) _cell_length_b 5.727(4) _cell_length_c 9.4091(12) _cell_angle_alpha 90.000(0) _cell_angle_beta 101.318(33) _cell_angle_gamma 90.000(0) _cell_volume 1104.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 20729 _cell_measurement_theta_min 2.982 _cell_measurement_theta_max 24.379 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31245 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4074 _reflns_number_gt 3734 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006) ; _computing_publication_materia ; SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0517P)^2^+0.0070P] 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 -0.4(10) _refine_ls_number_reflns 4074 _refine_ls_number_parameters 309 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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 C1 C 0.44434(10) 0.9698(4) 0.7045(2) 0.0319(5) Uani 1 1 d . . . H1A H 0.4463 1.1116 0.6511 0.048 Uiso 1 1 calc R . . H1B H 0.4825 0.9577 0.7799 0.048 Uiso 1 1 calc R . . H1C H 0.4061 0.9714 0.7468 0.048 Uiso 1 1 calc R . . C2 C 0.38776(8) 0.7593(3) 0.50030(19) 0.0219(4) Uani 1 1 d . . . C3 C 0.38508(9) 0.5671(3) 0.4086(2) 0.0253(4) Uani 1 1 d . . . H3 H 0.4184 0.4570 0.4244 0.030 Uiso 1 1 calc R . . C4 C 0.33299(9) 0.5400(3) 0.2944(2) 0.0254(4) Uani 1 1 d . . . H4 H 0.3318 0.4115 0.2335 0.030 Uiso 1 1 calc R . . C5 C 0.28219(8) 0.7017(3) 0.26875(19) 0.0209(4) Uani 1 1 d . . . C6 C 0.28532(9) 0.8906(3) 0.3630(2) 0.0266(4) Uani 1 1 d . . . H6 H 0.2516 0.9992 0.3485 0.032 Uiso 1 1 calc R . . C7 C 0.33732(9) 0.9211(3) 0.4776(2) 0.0255(4) Uani 1 1 d . . . H7 H 0.3385 1.0489 0.5390 0.031 Uiso 1 1 calc R . . C8 C 0.22445(9) 0.6719(3) 0.1453(2) 0.0243(4) Uani 1 1 d . . . H8A H 0.2057 0.8235 0.1160 0.029 Uiso 1 1 calc R . . H8B H 0.2388 0.6025 0.0629 0.029 Uiso 1 1 calc R . . C9 C 0.12700(8) 0.5789(3) 0.26080(19) 0.0220(4) Uani 1 1 d . . . H9 H 0.1136 0.7281 0.2807 0.026 Uiso 1 1 calc R . . C10 C 0.10251(8) 0.3710(3) 0.29791(19) 0.0207(4) Uani 1 1 d . . . C11 C 0.05075(8) 0.3138(3) 0.37868(19) 0.0205(4) Uani 1 1 d . . . C12 C -0.00152(9) 0.4652(3) 0.3808(2) 0.0217(4) Uani 1 1 d . . . H12 H -0.0041 0.6054 0.3302 0.026 Uiso 1 1 calc R . . C13 C 0.05452(9) 0.1047(3) 0.4556(2) 0.0234(4) Uani 1 1 d . . . H13 H 0.0893 0.0036 0.4556 0.028 Uiso 1 1 calc R . . C14 C 0.00640(9) 0.0472(3) 0.5323(2) 0.0251(4) Uani 1 1 d . . . H14 H 0.0091 -0.0926 0.5835 0.030 Uiso 1 1 calc R . . C15 C -0.04533(9) 0.1957(3) 0.53311(19) 0.0245(4) Uani 1 1 d . . . H15 H -0.0775 0.1543 0.5840 0.029 Uiso 1 1 calc R . . C16 C -0.04996(9) 0.4076(3) 0.45839(19) 0.0216(4) Uani 1 1 d . . . C17 C -0.10539(9) 0.5636(3) 0.4622(2) 0.0227(4) Uani 1 1 d . . . C18 C -0.13112(9) 0.7421(3) 0.3714(2) 0.0250(4) Uani 1 1 d . . . H18 H -0.1165 0.7950 0.2899 0.030 Uiso 1 1 calc R . . C19 C -0.23000(9) 0.9990(3) 0.3623(2) 0.0269(4) Uani 1 1 d . . . H19A H -0.2088 1.1178 0.3144 0.032 Uiso 1 1 calc R . . H19B H -0.2469 1.0739 0.4398 0.032 Uiso 1 1 calc R . . C20 C -0.28651(9) 0.8962(3) 0.2541(2) 0.0226(4) Uani 1 1 d . . . C21 C -0.28214(9) 0.6885(3) 0.1810(2) 0.0245(4) Uani 1 1 d . . . H21 H -0.2439 0.6017 0.2023 0.029 Uiso 1 1 calc R . . C22 C -0.33385(9) 0.6071(3) 0.0763(2) 0.0242(4) Uani 1 1 d . . . H22 H -0.3301 0.4672 0.0284 0.029 Uiso 1 1 calc R . . C23 C -0.39090(9) 0.7358(3) 0.04395(19) 0.0238(4) Uani 1 1 d . . . C24 C -0.39608(9) 0.9434(3) 0.1182(2) 0.0265(4) Uani 1 1 d . . . H24 H -0.4345 1.0298 0.0977 0.032 Uiso 1 1 calc R . . C25 C -0.34483(10) 1.0206(3) 0.2213(2) 0.0261(4) Uani 1 1 d . . . H25 H -0.3490 1.1588 0.2705 0.031 Uiso 1 1 calc R . . C26 C -0.44082(10) 0.4698(4) -0.1408(2) 0.0325(5) Uani 1 1 d . . . H26A H -0.4034 0.4791 -0.1855 0.049 Uiso 1 1 calc R . . H26B H -0.4795 0.4556 -0.2144 0.049 Uiso 1 1 calc R . . H26C H -0.4369 0.3359 -0.0783 0.049 Uiso 1 1 calc R . . N1 N 0.17450(7) 0.5215(2) 0.18956(17) 0.0208(3) Uani 1 1 d . . . N2 N 0.18040(7) 0.2887(3) 0.18129(17) 0.0262(4) Uani 1 1 d . . . N3 N 0.13655(7) 0.1958(3) 0.24673(16) 0.0254(4) Uani 1 1 d . . . N4 N -0.14210(8) 0.5455(3) 0.56627(18) 0.0361(4) Uani 1 1 d . . . N5 N -0.18878(9) 0.7041(3) 0.54319(19) 0.0355(4) Uani 1 1 d . . . N6 N -0.18178(7) 0.8243(3) 0.42467(17) 0.0233(3) Uani 1 1 d . . . O1 O 0.44155(6) 0.7748(2) 0.60910(13) 0.0276(3) Uani 1 1 d . . . O2 O -0.44476(6) 0.6758(2) -0.05798(14) 0.0313(3) 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 C1 0.0304(11) 0.0362(12) 0.0270(11) -0.0049(9) 0.0004(9) -0.0033(8) C2 0.0189(9) 0.0278(10) 0.0198(10) 0.0035(8) 0.0059(8) -0.0010(7) C3 0.0229(9) 0.0241(10) 0.0294(11) 0.0025(8) 0.0064(8) 0.0064(8) C4 0.0251(10) 0.0245(10) 0.0277(11) -0.0053(9) 0.0079(8) 0.0001(8) C5 0.0199(9) 0.0219(9) 0.0217(10) 0.0045(8) 0.0063(7) -0.0006(7) C6 0.0225(9) 0.0261(10) 0.0310(11) 0.0002(9) 0.0048(8) 0.0075(8) C7 0.0275(10) 0.0250(10) 0.0241(11) -0.0039(8) 0.0056(8) 0.0035(8) C8 0.0223(10) 0.0263(11) 0.0239(10) 0.0044(8) 0.0037(8) 0.0012(8) C9 0.0236(10) 0.0195(10) 0.0217(10) -0.0012(8) 0.0019(8) 0.0034(7) C10 0.0171(8) 0.0225(10) 0.0203(10) -0.0013(8) -0.0014(7) 0.0021(7) C11 0.0217(9) 0.0203(9) 0.0180(10) -0.0045(8) 0.0008(7) -0.0026(7) C12 0.0235(9) 0.0218(9) 0.0189(10) 0.0021(8) 0.0022(7) -0.0013(7) C13 0.0252(9) 0.0222(10) 0.0205(9) -0.0026(8) -0.0013(8) 0.0003(8) C14 0.0314(10) 0.0206(10) 0.0202(10) 0.0025(8) -0.0024(8) -0.0035(8) C15 0.0274(10) 0.0276(10) 0.0184(10) -0.0026(8) 0.0047(8) -0.0059(8) C16 0.0223(9) 0.0227(10) 0.0179(9) -0.0033(8) -0.0007(7) -0.0047(7) C17 0.0225(9) 0.0268(10) 0.0191(9) -0.0018(8) 0.0046(7) -0.0047(8) C18 0.0257(10) 0.0302(11) 0.0211(10) -0.0017(8) 0.0096(8) -0.0021(8) C19 0.0290(10) 0.0255(10) 0.0267(10) -0.0031(8) 0.0068(8) 0.0023(8) C20 0.0250(9) 0.0237(10) 0.0206(10) 0.0019(8) 0.0084(8) -0.0005(7) C21 0.0235(9) 0.0255(10) 0.0261(11) 0.0008(8) 0.0089(8) 0.0023(8) C22 0.0278(9) 0.0221(10) 0.0238(10) -0.0015(8) 0.0078(8) 0.0002(8) C23 0.0237(9) 0.0286(10) 0.0198(10) 0.0031(8) 0.0059(8) 0.0000(8) C24 0.0261(10) 0.0292(10) 0.0257(11) 0.0056(8) 0.0090(8) 0.0082(8) C25 0.0349(10) 0.0212(10) 0.0237(10) -0.0006(8) 0.0096(8) 0.0054(8) C26 0.0324(11) 0.0334(12) 0.0308(12) -0.0033(9) 0.0041(9) -0.0070(9) N1 0.0187(7) 0.0187(8) 0.0243(8) -0.0001(7) 0.0028(6) 0.0008(6) N2 0.0237(8) 0.0234(9) 0.0316(9) -0.0013(7) 0.0055(7) 0.0030(7) N3 0.0219(8) 0.0222(9) 0.0330(9) -0.0027(7) 0.0073(7) -0.0003(6) N4 0.0306(9) 0.0455(11) 0.0360(10) 0.0139(8) 0.0157(8) 0.0099(8) N5 0.0335(9) 0.0458(11) 0.0305(10) 0.0124(8) 0.0144(8) 0.0090(8) N6 0.0217(8) 0.0279(8) 0.0209(8) -0.0008(7) 0.0056(6) -0.0006(6) O1 0.0242(7) 0.0326(8) 0.0242(7) -0.0012(6) 0.0006(6) 0.0033(6) O2 0.0266(7) 0.0368(8) 0.0283(8) -0.0032(6) -0.0002(6) 0.0025(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 O1 1.427(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.367(2) . ? C2 C7 1.388(3) . ? C2 C3 1.393(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9300 . ? C4 C5 1.394(3) . ? C4 H4 0.9300 . ? C5 C6 1.392(3) . ? C5 C8 1.512(3) . ? C6 C7 1.384(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.475(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.344(2) . ? C9 C10 1.368(3) . ? C9 H9 0.9300 . ? C10 N3 1.371(2) . ? C10 C11 1.476(2) . ? C11 C13 1.393(3) . ? C11 C12 1.398(3) . ? C12 C16 1.399(3) . ? C12 H12 0.9300 . ? C13 C14 1.388(3) . ? C13 H13 0.9300 . ? C14 C15 1.377(3) . ? C14 H14 0.9300 . ? C15 C16 1.397(3) . ? C15 H15 0.9300 . ? C16 C17 1.469(3) . ? C17 N4 1.362(2) . ? C17 C18 1.372(3) . ? C18 N6 1.343(2) . ? C18 H18 0.9300 . ? C19 N6 1.459(2) . ? C19 C20 1.519(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.386(3) . ? C20 C25 1.394(3) . ? C21 C22 1.392(3) . ? C21 H21 0.9300 . ? C22 C23 1.385(3) . ? C22 H22 0.9300 . ? C23 O2 1.372(2) . ? C23 C24 1.394(3) . ? C24 C25 1.370(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 O2 1.425(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N1 N2 1.343(2) . ? N2 N3 1.313(2) . ? N4 N5 1.320(2) . ? N5 N6 1.343(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C7 124.08(17) . . ? O1 C2 C3 116.25(16) . . ? C7 C2 C3 119.67(17) . . ? C4 C3 C2 120.04(17) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.21(17) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 117.83(17) . . ? C6 C5 C8 120.50(15) . . ? C4 C5 C8 121.65(16) . . ? C7 C6 C5 121.71(16) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C2 119.52(17) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? N1 C8 C5 110.60(14) . . ? N1 C8 H8A 109.5 . . ? C5 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N1 C9 C10 105.37(16) . . ? N1 C9 H9 127.3 . . ? C10 C9 H9 127.3 . . ? C9 C10 N3 107.53(16) . . ? C9 C10 C11 132.33(17) . . ? N3 C10 C11 120.13(16) . . ? C13 C11 C12 119.34(16) . . ? C13 C11 C10 119.06(16) . . ? C12 C11 C10 121.60(16) . . ? C11 C12 C16 120.61(17) . . ? C11 C12 H12 119.7 . . ? C16 C12 H12 119.7 . . ? C14 C13 C11 120.08(17) . . ? C14 C13 H13 120.0 . . ? C11 C13 H13 120.0 . . ? C15 C14 C13 120.44(17) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.71(17) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C12 118.80(16) . . ? C15 C16 C17 119.55(16) . . ? C12 C16 C17 121.64(16) . . ? N4 C17 C18 107.26(16) . . ? N4 C17 C16 121.99(16) . . ? C18 C17 C16 130.74(17) . . ? N6 C18 C17 105.71(17) . . ? N6 C18 H18 127.1 . . ? C17 C18 H18 127.1 . . ? N6 C19 C20 112.90(16) . . ? N6 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N6 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C21 C20 C25 117.98(17) . . ? C21 C20 C19 123.16(16) . . ? C25 C20 C19 118.80(17) . . ? C20 C21 C22 121.39(17) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C23 C22 C21 119.55(17) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? O2 C23 C22 125.03(17) . . ? O2 C23 C24 115.47(16) . . ? C22 C23 C24 119.50(17) . . ? C25 C24 C23 120.21(17) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 121.36(18) . . ? C24 C25 H25 119.3 . . ? C20 C25 H25 119.3 . . ? O2 C26 H26A 109.5 . . ? O2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 N1 C9 110.91(14) . . ? N2 N1 C8 119.02(15) . . ? C9 N1 C8 129.19(16) . . ? N3 N2 N1 107.15(14) . . ? N2 N3 C10 109.04(15) . . ? N5 N4 C17 109.42(16) . . ? N4 N5 N6 106.97(15) . . ? C18 N6 N5 110.64(15) . . ? C18 N6 C19 128.60(16) . . ? N5 N6 C19 120.40(15) . . ? C2 O1 C1 116.62(14) . . ? C23 O2 C26 117.51(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.129 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.041