# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Leonard F. Lindoy' _publ_contact_author_address ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; _publ_contact_author_email Lindoy@chem.usyd.edu.au _publ_contact_author_fax '+61 2 9351 3329' _publ_contact_author_phone '+61 2 9351 4400' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Inherent helicity in an extended tris-bipyridyl molecular cage ; loop_ _publ_author_name _publ_author_address 'David F. Perkins' ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'Leonard F. Lindoy' ; The Centre for Heavy Metal Research, School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; 'George V. Meehan' ; School of Pharmacy and Molecular Sciences, James Cook University, Queensland 4811, Australia ; 'Peter Turner' ; Crystal Structure Analysis Facility School of Chemistry, University of Sydney, Sydney 2006, NSW, Australia. ; #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_lfl8 _database_code_depnum_ccdc_archive 'CCDC 222140' _audit_creation_method SHELXL-97 _publ_section_experimental ; In a cold room, a colourless hexagonal crystal was transferred from the growth solution to a mixture of mother liquor and Dupont Krytox GPL106 perfluoropolyalkylether. The crystal was attached to a mohair fibre glued to a short length of copper wire inserted in a copper pin, and cooled with dry ice. The crystal was then mounted on a Bruker SMART 1000 diffractometer equipped with an Oxford Cryosystem Cryostream. Diffraction data were collected at 173 Kelvin, with graphite monochromated MoKa radiation generated from a sealed tube. Cell constants were obtained from a least squares refinement against 1014 reflections located between 5 and 50\% 2\q. Data were collected with 0.3\% increment \w scans, with the CCD camera at two 2\q positions, to provide data coverage from 2 to 64\% 2\q, 6.45 cm from the crystal . A full sphere of reciprocal space was collected at the hight 2\q camera position, however an ice blockage restricted the low two theta position collection to a quartant. An empirical absorption correction determined with SADABS^1^ was applied to the data. The data integration and reduction were undertaken with SAINT and XPREP,^2^ and subsequent computations were carried out with the teXsan3 graphical user interface. The data reduction included the application of Lorentz and polarisation corrections. The structure was solved in the space group P\-3(#147) by direct methods with SIR97^4^, and extended and refined with SHELXL-97.^5^ Refinement with isotropic displacement parameters factors halted with R1 around 0.24 until the twin law (y,x,-z) was applied, and the residual then fell to about 0.14. The (y,x,-z) twin fraction converged to 0.364(1). The asymmetric unit contains two crystallographically independent complex molecules, each of which resides on a three fold axis (1/3,2/3,z for complex molecule 1 and 2/3,1/3,z for complex molecule 2). The C(27) and C(65) tertiary butyl residues exhibit orientational disorder and the associated sites were modelled with 50% occupancies. The counterions partially occupy three sites in the asymmetric unit, such that there are two hexafluorophosphate counterions per complex molecule. The P(2) and P(3) counterions are centred on the same three fold axis (0,0,z), and the P(1) and P(3) counterions were modelled with 7/9 and 2/3 site occupancies respectively. The asymmetric unit also contains partially occupied acetonitrile and sites assumed to be partially occupied water oxygen sites. The acetonitrile sites C(69), C(70) and N(9) were modelled with 2/3 occupancies and the C(71), C(72) and N(10) acetonitrile sites were modelled with 1/6 occupancies. The water molecule O(9), which bridges the two actonitrile positions, was also modelled with an occupancy of 1/6. The water molecule O(8), O(10) and O(12) sites are on three fold axes and O(11) is on a three fold roto-inversion site. The O(8), O(10), O(11) and O(12) water atoms were modelled with 0.125 occupancies and O(9) was modelled with a 1/6 occupancy. The refinement model formulation is then formulated as [Ni(L)3]2PF6.1.25CH3CN.2H20, however no hydrogens were included in the refinement model for the water molecules. The solvate, water and partially occupied ligand sites were modelled with isotropic displacement parameters, and the rest of the non-hydrogen atoms were modelled with anisotropic displacement parameters. A riding atom model was used for hydrogen atoms. 1. Blessing, R.H.; Acta Cryst. (1995) A51 33 - 38. Sheldrick, G.M.; SADABS. Empirical absorption correction program for area detector data. University of Gottingen, Germany, 1996. 2. Bruker (1995). SMART, SAINT and XPREP. Area detector control and data integration and reduction software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 3. Molecular Structure Corporation (1997-1998). teXsan for Windows: Single Crystal Structure Analysis Software, MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. 4. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. J. Appl. Cryst.,(1993), 26, 343. 5. Sheldrick, G.M.; SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany, 1997. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104.50 H117.75 F12 N9.25 Ni O8 P2' _chemical_formula_weight 1979.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_space_group_name_H-M 'P -3 ' _symmetry_Int_Tables_number 147 _symmetry_cell_setting trigonal loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 15.9763(19) _cell_length_b 15.9763(19) _cell_length_c 51.131(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11302(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1014 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.96 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.292 _exptl_crystal_size_min 0.144 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4158 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 18 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 136109 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -75 _diffrn_reflns_limit_l_max 75 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 31.61 _reflns_number_total 24406 _reflns_number_gt 18113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1408P)^2^+5.3903P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24406 _refine_ls_number_parameters 849 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2426 _refine_ls_wR_factor_gt 0.2061 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.3333 0.6667 0.223321(10) 0.02844(12) Uani 1 3 d S . . Ni2 Ni 0.6667 0.3333 0.270392(10) 0.02819(12) Uani 1 3 d S . . P1 P 0.11144(13) 0.23299(12) 0.23390(4) 0.0707(4) Uani 0.78 1 d P . . P2 P 0.0000 0.0000 0.37130(4) 0.0548(4) Uani 1 3 d S . . P3 P 0.0000 0.0000 0.07540(12) 0.1035(13) Uani 0.67 3 d SPD . . F1 F 0.0353(4) 0.2255(4) 0.21274(13) 0.117(2) Uani 0.78 1 d P . . F2 F 0.1976(5) 0.3121(6) 0.21846(13) 0.136(2) Uani 0.78 1 d P . . F3 F 0.1884(4) 0.2427(4) 0.25521(11) 0.1085(18) Uani 0.78 1 d P . . F4 F 0.0226(7) 0.1563(8) 0.2504(3) 0.213(5) Uani 0.78 1 d P . . F5 F 0.0939(6) 0.3082(6) 0.24884(17) 0.156(3) Uani 0.78 1 d P . . F6 F 0.1156(7) 0.1502(6) 0.22087(19) 0.183(4) Uani 0.78 1 d P . . F7 F 0.0468(3) 0.09418(19) 0.35322(6) 0.0772(7) Uani 1 1 d . . . F8 F -0.0470(3) -0.0939(2) 0.38899(6) 0.0915(9) Uani 1 1 d . . . F9 F -0.0886(7) -0.0619(8) 0.09350(19) 0.157(3) Uani 0.67 1 d P . . F10 F 0.0925(7) 0.0633(8) 0.0587(2) 0.190(4) Uani 0.67 1 d PD . . O1 O 0.2307(2) 0.45457(16) 0.31776(4) 0.0503(6) Uani 1 1 d . . . O2 O 0.56958(17) 0.7946(2) 0.13364(4) 0.0475(6) Uani 1 1 d . . . O3 O 0.4912(2) 0.3669(2) 0.36102(5) 0.0505(6) Uani 1 1 d . . . O4 O 0.90470(19) 0.49134(18) 0.18505(5) 0.0467(5) Uani 1 1 d . . . O5 O 0.2262(6) 0.1255(7) 0.14522(16) 0.0561(19) Uiso 0.33 1 d P . . O6 O 0.2961(13) 0.1409(14) 0.1324(3) 0.114(4) Uiso 0.33 1 d P . . O7 O 0.3092(8) 0.1252(8) 0.1550(2) 0.072(3) Uiso 0.33 1 d P . . O8 O 0.0000 0.0000 0.0071(9) 0.082(14) Uiso 0.12 3 d SP . . O9 O 0.2063(9) 0.1083(11) 0.3063(2) 0.039(2) Uiso 0.17 1 d P . . O10 O 0.0000 0.0000 0.4534(7) 0.057(8) Uiso 0.12 3 d SP . . O11 O 0.0000 0.0000 0.5000 0.106(13) Uiso 0.25 6 d SP . . O12 O 0.6667 0.3333 0.5828(13) 0.103(18) Uiso 0.12 3 d SP . . N1 N 0.3333 0.6667 0.35743(8) 0.0333(7) Uani 1 3 d S . . N2 N 0.3333 0.6667 0.09445(7) 0.0320(7) Uani 1 3 d S . . N3 N 0.34622(18) 0.56348(18) 0.24552(4) 0.0316(4) Uani 1 1 d . . . N4 N 0.44421(18) 0.65998(19) 0.20298(5) 0.0335(5) Uani 1 1 d . . . N5 N 0.6667 0.3333 0.40003(8) 0.0353(7) Uani 1 3 d S . . N6 N 0.6667 0.3333 0.15417(8) 0.0369(8) Uani 1 3 d S . . N7 N 0.63359(18) 0.42684(17) 0.29140(5) 0.0326(5) Uani 1 1 d . . . N8 N 0.74318(18) 0.46311(17) 0.24908(4) 0.0315(4) Uani 1 1 d . . . C1 C 0.2339(2) 0.6007(2) 0.34804(6) 0.0360(6) Uani 1 1 d . . . H1A H 0.2341 0.5998 0.3287 0.043 Uiso 1 1 calc R . . H1B H 0.1914 0.6260 0.3537 0.043 Uiso 1 1 calc R . . C2 C 0.1929(2) 0.4984(2) 0.35805(6) 0.0346(5) Uani 1 1 d . . . C3 C 0.1528(2) 0.4737(2) 0.38305(6) 0.0388(6) Uani 1 1 d . . . H3 H 0.1529 0.5226 0.3937 0.047 Uiso 1 1 calc R . . C4 C 0.1126(3) 0.3803(3) 0.39315(6) 0.0450(7) Uani 1 1 d . A . C5 C 0.1158(3) 0.3114(2) 0.37721(7) 0.0427(7) Uani 1 1 d . . . H5 H 0.0913 0.2477 0.3838 0.051 Uiso 1 1 calc R . . C6 C 0.1534(2) 0.3325(2) 0.35198(6) 0.0390(6) Uani 1 1 d . . . H6 H 0.1528 0.2834 0.3414 0.047 Uiso 1 1 calc R . . C7 C 0.1919(2) 0.4259(2) 0.34236(6) 0.0361(6) Uani 1 1 d . . . C8 C 0.2381(3) 0.3870(2) 0.30165(6) 0.0385(6) Uani 1 1 d . . . H8A H 0.1735 0.3382 0.2951 0.046 Uiso 1 1 calc R . . H8B H 0.2658 0.3534 0.3116 0.046 Uiso 1 1 calc R . . C9 C 0.3037(2) 0.4431(2) 0.27901(5) 0.0359(6) Uani 1 1 d . . . C10 C 0.3756(3) 0.4261(3) 0.27080(7) 0.0435(7) Uani 1 1 d . . . H10 H 0.3854 0.3786 0.2792 0.052 Uiso 1 1 calc R . . C11 C 0.4342(3) 0.4795(3) 0.24988(7) 0.0451(7) Uani 1 1 d . . . H11 H 0.4848 0.4693 0.2440 0.054 Uiso 1 1 calc R . . C12 C 0.4179(2) 0.5479(2) 0.23769(5) 0.0349(6) Uani 1 1 d . . . C13 C 0.2909(2) 0.5122(2) 0.26584(5) 0.0332(5) Uani 1 1 d . . . H13 H 0.2408 0.5235 0.2715 0.040 Uiso 1 1 calc R . . C14 C 0.4765(2) 0.6065(2) 0.21531(5) 0.0354(6) Uani 1 1 d . . . C15 C 0.5596(3) 0.6073(3) 0.20729(7) 0.0451(7) Uani 1 1 d . . . H15 H 0.5828 0.5717 0.2168 0.054 Uiso 1 1 calc R . . C16 C 0.6093(3) 0.6603(3) 0.18528(6) 0.0471(8) Uani 1 1 d . . . H16 H 0.6662 0.6610 0.1795 0.057 Uiso 1 1 calc R . . C17 C 0.5745(2) 0.7119(3) 0.17195(6) 0.0411(6) Uani 1 1 d . . . C18 C 0.4924(2) 0.7111(2) 0.18160(6) 0.0373(6) Uani 1 1 d . . . H18 H 0.4694 0.7479 0.1728 0.045 Uiso 1 1 calc R . . C19 C 0.6288(3) 0.7683(4) 0.14821(7) 0.0598(11) Uani 1 1 d . . . H19A H 0.6889 0.8272 0.1536 0.072 Uiso 1 1 calc R . . H19B H 0.6467 0.7286 0.1372 0.072 Uiso 1 1 calc R . . C20 C 0.5845(2) 0.8042(2) 0.10679(5) 0.0386(6) Uani 1 1 d . . . C21 C 0.6727(2) 0.8296(3) 0.09516(6) 0.0474(7) Uani 1 1 d . . . H21 H 0.7269 0.8418 0.1056 0.057 Uiso 1 1 calc R . . C22 C 0.6806(2) 0.8369(3) 0.06776(6) 0.0484(7) Uani 1 1 d . . . H22 H 0.7409 0.8543 0.0598 0.058 Uiso 1 1 calc R . . C23 C 0.6025(3) 0.8193(2) 0.05208(6) 0.0446(7) Uani 1 1 d . . . C24 C 0.5157(3) 0.7960(2) 0.06444(6) 0.0408(6) Uani 1 1 d . . . H24 H 0.4619 0.7848 0.0540 0.049 Uiso 1 1 calc R . . C25 C 0.5051(2) 0.7886(2) 0.09171(6) 0.0353(5) Uani 1 1 d . . . C26 C 0.4090(2) 0.7611(2) 0.10384(6) 0.0365(6) Uani 1 1 d . . . H26A H 0.4140 0.7591 0.1231 0.044 Uiso 1 1 calc R . . H26B H 0.3913 0.8106 0.0995 0.044 Uiso 1 1 calc R . . C27 C 0.0681(4) 0.3552(4) 0.42053(7) 0.0643(12) Uani 1 1 d D . . C28A C 0.0270(10) 0.4122(10) 0.4306(3) 0.084(3) Uiso 0.50 1 d P A 1 H28A H 0.0063 0.4372 0.4160 0.126 Uiso 0.50 1 calc PR A 1 H28B H 0.0758 0.4663 0.4410 0.126 Uiso 0.50 1 calc PR A 1 H28C H -0.0288 0.3713 0.4417 0.126 Uiso 0.50 1 calc PR A 1 C29A C -0.0325(7) 0.2707(10) 0.4176(4) 0.123(5) Uiso 0.50 1 d PD A 1 H29A H -0.0701 0.2886 0.4061 0.185 Uiso 0.50 1 calc PR A 1 H29B H -0.0636 0.2523 0.4348 0.185 Uiso 0.50 1 calc PR A 1 H29C H -0.0295 0.2160 0.4100 0.185 Uiso 0.50 1 calc PR A 1 C30A C 0.1063(9) 0.3098(9) 0.4369(2) 0.076(3) Uiso 0.50 1 d P A 1 H30A H 0.1265 0.2724 0.4260 0.114 Uiso 0.50 1 calc PR A 1 H30B H 0.0566 0.2666 0.4493 0.114 Uiso 0.50 1 calc PR A 1 H30C H 0.1622 0.3594 0.4465 0.114 Uiso 0.50 1 calc PR A 1 C28B C -0.0233(8) 0.3567(9) 0.4206(2) 0.070(2) Uiso 0.50 1 d P A 2 H28D H -0.0519 0.3404 0.4382 0.105 Uiso 0.50 1 calc PR A 2 H28E H -0.0681 0.3094 0.4080 0.105 Uiso 0.50 1 calc PR A 2 H28F H -0.0106 0.4214 0.4158 0.105 Uiso 0.50 1 calc PR A 2 C29B C 0.1380(8) 0.4338(7) 0.4385(2) 0.080(3) Uiso 0.50 1 d PD A 2 H29D H 0.1993 0.4337 0.4388 0.121 Uiso 0.50 1 calc PR A 2 H29E H 0.1109 0.4222 0.4562 0.121 Uiso 0.50 1 calc PR A 2 H29F H 0.1492 0.4965 0.4322 0.121 Uiso 0.50 1 calc PR A 2 C30B C 0.0622(8) 0.2641(8) 0.4314(2) 0.066(2) Uiso 0.50 1 d P A 2 H30D H 0.1258 0.2691 0.4302 0.099 Uiso 0.50 1 calc PR A 2 H30E H 0.0149 0.2081 0.4214 0.099 Uiso 0.50 1 calc PR A 2 H30F H 0.0423 0.2564 0.4498 0.099 Uiso 0.50 1 calc PR A 2 C31 C 0.6087(3) 0.8247(3) 0.02202(7) 0.0523(9) Uani 1 1 d . . . C32 C 0.5316(5) 0.7299(4) 0.01034(9) 0.0774(15) Uani 1 1 d . . . H32A H 0.5416 0.6773 0.0163 0.116 Uiso 1 1 calc R . . H32B H 0.5358 0.7338 -0.0088 0.116 Uiso 1 1 calc R . . H32C H 0.4676 0.7173 0.0159 0.116 Uiso 1 1 calc R . . C33 C 0.5925(5) 0.9067(4) 0.01262(9) 0.0776(15) Uani 1 1 d . . . H33A H 0.6421 0.9681 0.0202 0.116 Uiso 1 1 calc R . . H33B H 0.5284 0.8938 0.0182 0.116 Uiso 1 1 calc R . . H33C H 0.5966 0.9107 -0.0065 0.116 Uiso 1 1 calc R . . C34 C 0.7085(4) 0.8469(6) 0.01213(8) 0.0859(17) Uani 1 1 d . . . H34A H 0.7584 0.9082 0.0196 0.129 Uiso 1 1 calc R . . H34B H 0.7104 0.8517 -0.0070 0.129 Uiso 1 1 calc R . . H34C H 0.7205 0.7948 0.0175 0.129 Uiso 1 1 calc R . . C35 C 0.5667(2) 0.2734(2) 0.39090(6) 0.0360(5) Uani 1 1 d . . . H35A H 0.5426 0.2055 0.3961 0.043 Uiso 1 1 calc R . . H35B H 0.5654 0.2758 0.3716 0.043 Uiso 1 1 calc R . . C36 C 0.5009(2) 0.3069(2) 0.40198(6) 0.0390(6) Uani 1 1 d . . . C37 C 0.4778(3) 0.2934(3) 0.42843(7) 0.0468(7) Uani 1 1 d . . . H37 H 0.5037 0.2628 0.4389 0.056 Uiso 1 1 calc R . . C38 C 0.4174(3) 0.3233(3) 0.44033(7) 0.0549(9) Uani 1 1 d . . . C39 C 0.3779(3) 0.3635(3) 0.42402(8) 0.0531(9) Uani 1 1 d . . . H39 H 0.3339 0.3809 0.4312 0.064 Uiso 1 1 calc R . . C40 C 0.4001(3) 0.3796(3) 0.39740(7) 0.0497(8) Uani 1 1 d . . . H40 H 0.3732 0.4091 0.3868 0.060 Uiso 1 1 calc R . . C41 C 0.4622(2) 0.3517(3) 0.38677(6) 0.0403(6) Uani 1 1 d . . . C42 C 0.4834(3) 0.4389(3) 0.34691(6) 0.0427(7) Uani 1 1 d . . . H42A H 0.5020 0.4958 0.3582 0.051 Uiso 1 1 calc R . . H42B H 0.4159 0.4135 0.3411 0.051 Uiso 1 1 calc R . . C43 C 0.5491(3) 0.4672(3) 0.32371(6) 0.0397(6) Uani 1 1 d . . . C44 C 0.5843(3) 0.5570(3) 0.31207(8) 0.0511(8) Uani 1 1 d . . . H44 H 0.5669 0.6016 0.3189 0.061 Uiso 1 1 calc R . . C45 C 0.6446(3) 0.5818(3) 0.29055(8) 0.0497(8) Uani 1 1 d . . . H45 H 0.6693 0.6435 0.2826 0.060 Uiso 1 1 calc R . . C46 C 0.6686(2) 0.5156(2) 0.28069(6) 0.0376(6) Uani 1 1 d . . . C47 C 0.5748(2) 0.4037(2) 0.31221(5) 0.0355(6) Uani 1 1 d . . . H47 H 0.5493 0.3409 0.3195 0.043 Uiso 1 1 calc R . . C48 C 0.7344(2) 0.5375(2) 0.25816(6) 0.0370(6) Uani 1 1 d . . . C49 C 0.7846(3) 0.6287(2) 0.24659(8) 0.0519(9) Uani 1 1 d . . . H49 H 0.7772 0.6803 0.2531 0.062 Uiso 1 1 calc R . . C50 C 0.8444(3) 0.6437(3) 0.22581(8) 0.0528(9) Uani 1 1 d . . . H50 H 0.8792 0.7059 0.2180 0.063 Uiso 1 1 calc R . . C51 C 0.8543(2) 0.5676(2) 0.21611(6) 0.0381(6) Uani 1 1 d . . . C52 C 0.8017(2) 0.4786(2) 0.22851(6) 0.0345(5) Uani 1 1 d . . . H52 H 0.8073 0.4258 0.2221 0.041 Uiso 1 1 calc R . . C53 C 0.9193(3) 0.5827(3) 0.19322(7) 0.0461(7) Uani 1 1 d . . . H53A H 0.9041 0.6140 0.1787 0.055 Uiso 1 1 calc R . . H53B H 0.9877 0.6253 0.1983 0.055 Uiso 1 1 calc R . . C54 C 0.9112(2) 0.4793(3) 0.15836(7) 0.0432(7) Uani 1 1 d . B . C55 C 0.9866(3) 0.5465(3) 0.14306(8) 0.0546(9) Uani 1 1 d . . . H55 H 1.0376 0.6035 0.1507 0.065 Uiso 1 1 calc R . . C56 C 0.9867(3) 0.5292(3) 0.11634(8) 0.0593(10) Uani 1 1 d . B . H56 H 1.0377 0.5760 0.1058 0.071 Uiso 1 1 calc R . . C57 C 0.9159(3) 0.4473(4) 0.10480(7) 0.0608(11) Uani 1 1 d . . . C58 C 0.8419(3) 0.3794(3) 0.12074(7) 0.0529(9) Uani 1 1 d . B . H58 H 0.7933 0.3207 0.1132 0.064 Uiso 1 1 calc R . . C59 C 0.8375(2) 0.3952(2) 0.14724(7) 0.0416(7) Uani 1 1 d . . . C60 C 0.7493(2) 0.3239(2) 0.16246(7) 0.0391(6) Uani 1 1 d . B . H60A H 0.7359 0.2573 0.1592 0.047 Uiso 1 1 calc R . . H60B H 0.7607 0.3372 0.1814 0.047 Uiso 1 1 calc R . . C61 C 0.4049(5) 0.3150(4) 0.47033(9) 0.0837(18) Uani 1 1 d D . . C62 C 0.3489(8) 0.3581(8) 0.48006(11) 0.132(4) Uani 1 1 d . . . H62A H 0.3702 0.4200 0.4712 0.199 Uiso 1 1 calc R . . H62B H 0.3588 0.3688 0.4989 0.199 Uiso 1 1 calc R . . H62C H 0.2801 0.3145 0.4765 0.199 Uiso 1 1 calc R . . C63 C 0.3826(9) 0.2182(6) 0.47993(12) 0.136(4) Uani 1 1 d . . . H63A H 0.4258 0.1994 0.4715 0.203 Uiso 1 1 calc R . . H63B H 0.3154 0.1706 0.4758 0.203 Uiso 1 1 calc R . . H63C H 0.3920 0.2206 0.4989 0.203 Uiso 1 1 calc R . . C64 C 0.5005(6) 0.3806(7) 0.48317(12) 0.134(3) Uani 1 1 d D . . H64A H 0.5473 0.3608 0.4782 0.200 Uiso 1 1 calc R . . H64B H 0.4924 0.3764 0.5022 0.200 Uiso 1 1 calc R . . H64C H 0.5240 0.4473 0.4775 0.200 Uiso 1 1 calc R . . C65A C 0.9178(6) 0.4091(7) 0.07536(17) 0.0531(18) Uiso 0.50 1 d PD B 1 C66A C 1.0131(7) 0.4684(8) 0.06251(18) 0.058(2) Uiso 0.50 1 d PD B 1 H66A H 1.0625 0.4619 0.0722 0.087 Uiso 0.50 1 calc PR B 1 H66B H 1.0298 0.5363 0.0624 0.087 Uiso 0.50 1 calc PR B 1 H66C H 1.0099 0.4460 0.0445 0.087 Uiso 0.50 1 calc PR B 1 C67A C 0.9046(10) 0.3036(10) 0.0736(3) 0.088(3) Uiso 0.50 1 d P B 1 H67A H 0.8430 0.2570 0.0817 0.132 Uiso 0.50 1 calc PR B 1 H67B H 0.9578 0.3026 0.0828 0.132 Uiso 0.50 1 calc PR B 1 H67C H 0.9047 0.2863 0.0552 0.132 Uiso 0.50 1 calc PR B 1 C68A C 0.8325(9) 0.4047(11) 0.0618(2) 0.085(3) Uiso 0.50 1 d P B 1 H68A H 0.8349 0.4669 0.0636 0.128 Uiso 0.50 1 calc PR B 1 H68B H 0.7727 0.3536 0.0696 0.128 Uiso 0.50 1 calc PR B 1 H68C H 0.8341 0.3907 0.0432 0.128 Uiso 0.50 1 calc PR B 1 C65B C 0.9164(5) 0.4458(6) 0.07450(13) 0.0435(14) Uiso 0.50 1 d P B 2 C66B C 1.0038(8) 0.4316(9) 0.0677(2) 0.064(2) Uiso 0.50 1 d P B 2 H66D H 1.0639 0.4878 0.0737 0.096 Uiso 0.50 1 calc PR B 2 H66E H 1.0069 0.4250 0.0487 0.096 Uiso 0.50 1 calc PR B 2 H66F H 0.9956 0.3732 0.0763 0.096 Uiso 0.50 1 calc PR B 2 C67B C 0.9194(8) 0.5345(8) 0.0622(2) 0.071(2) Uiso 0.50 1 d P B 2 H67D H 0.9771 0.5931 0.0683 0.106 Uiso 0.50 1 calc PR B 2 H67E H 0.8615 0.5368 0.0673 0.106 Uiso 0.50 1 calc PR B 2 H67F H 0.9215 0.5303 0.0431 0.106 Uiso 0.50 1 calc PR B 2 C68B C 0.8250(6) 0.3552(7) 0.06509(17) 0.0543(17) Uiso 0.50 1 d P B 2 H68D H 0.8179 0.3595 0.0462 0.081 Uiso 0.50 1 calc PR B 2 H68E H 0.7685 0.3503 0.0741 0.081 Uiso 0.50 1 calc PR B 2 H68F H 0.8302 0.2979 0.0690 0.081 Uiso 0.50 1 calc PR B 2 N9 N 0.3538(3) 0.2428(3) 0.31063(9) 0.0457(9) Uiso 0.67 1 d P C 1 C69 C 0.3079(5) 0.1793(5) 0.32327(13) 0.0595(14) Uiso 0.67 1 d P C 1 C70 C 0.3009(6) 0.1322(6) 0.34929(14) 0.0691(18) Uiso 0.67 1 d P C 1 H70A H 0.2395 0.0710 0.3503 0.104 Uiso 0.67 1 calc PR C 1 H70B H 0.3039 0.1752 0.3634 0.104 Uiso 0.67 1 calc PR C 1 H70C H 0.3547 0.1196 0.3511 0.104 Uiso 0.67 1 calc PR C 1 N10 N 0.1791(13) -0.0203(13) 0.2851(3) 0.042(3) Uiso 0.17 1 d P C -2 C71 C 0.1272(17) 0.0041(18) 0.2876(5) 0.053(3) Uiso 0.17 1 d PD C -2 C72 C 0.0652(16) 0.0461(17) 0.2900(5) 0.053(3) Uiso 0.17 1 d PD C -2 H72A H 0.0772 0.0796 0.3068 0.080 Uiso 0.17 1 calc PR C -2 H72B H -0.0026 -0.0053 0.2890 0.080 Uiso 0.17 1 calc PR C -2 H72C H 0.0793 0.0922 0.2758 0.080 Uiso 0.17 1 calc PR C -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 Ni1 0.03077(17) 0.03077(17) 0.0238(2) 0.000 0.000 0.01538(8) Ni2 0.02742(16) 0.02742(16) 0.0297(2) 0.000 0.000 0.01371(8) P1 0.0593(9) 0.0678(9) 0.0951(11) -0.0176(8) -0.0195(9) 0.0395(8) P2 0.0528(5) 0.0528(5) 0.0589(9) 0.000 0.000 0.0264(3) P3 0.0924(18) 0.0924(18) 0.126(4) 0.000 0.000 0.0462(9) F1 0.106(4) 0.118(4) 0.159(5) -0.053(4) -0.064(4) 0.079(3) F2 0.103(4) 0.199(7) 0.121(4) 0.036(5) 0.004(3) 0.088(5) F3 0.119(4) 0.105(4) 0.132(4) -0.041(3) -0.064(3) 0.080(3) F4 0.114(6) 0.206(10) 0.296(13) 0.112(10) 0.032(7) 0.062(6) F5 0.158(6) 0.188(7) 0.191(7) -0.098(6) -0.092(5) 0.139(6) F6 0.206(8) 0.162(6) 0.249(9) -0.125(7) -0.139(7) 0.143(6) F7 0.0786(19) 0.0535(13) 0.0873(17) 0.0086(12) 0.0111(18) 0.0240(15) F8 0.110(3) 0.0739(18) 0.0801(17) 0.0218(14) 0.003(2) 0.038(2) F9 0.113(6) 0.173(9) 0.177(7) 0.003(7) -0.001(5) 0.065(6) F10 0.204(10) 0.152(8) 0.190(8) 0.049(7) 0.048(8) 0.070(8) O1 0.0723(17) 0.0345(10) 0.0412(10) 0.0075(8) 0.0194(13) 0.0245(12) O2 0.0446(12) 0.0712(18) 0.0330(9) 0.0095(11) 0.0061(8) 0.0337(13) O3 0.0718(17) 0.0681(17) 0.0362(11) 0.0065(11) 0.0128(11) 0.0533(15) O4 0.0453(13) 0.0436(12) 0.0484(12) 0.0028(10) 0.0144(10) 0.0201(11) N1 0.0273(10) 0.0273(10) 0.0452(19) 0.000 0.000 0.0137(5) N2 0.0321(11) 0.0321(11) 0.0317(16) 0.000 0.000 0.0161(5) N3 0.0357(12) 0.0355(12) 0.0264(10) 0.0003(8) -0.0001(8) 0.0199(10) N4 0.0337(11) 0.0389(12) 0.0286(10) -0.0005(9) 0.0019(9) 0.0188(10) N5 0.0333(11) 0.0333(11) 0.0393(19) 0.000 0.000 0.0167(6) N6 0.0360(12) 0.0360(12) 0.0386(19) 0.000 0.000 0.0180(6) N7 0.0352(11) 0.0301(10) 0.0345(11) -0.0012(8) 0.0000(9) 0.0178(9) N8 0.0304(11) 0.0287(10) 0.0341(10) -0.0011(8) -0.0005(8) 0.0138(9) C1 0.0298(12) 0.0318(13) 0.0451(14) -0.0007(10) -0.0012(10) 0.0145(10) C2 0.0287(12) 0.0318(13) 0.0399(14) -0.0008(10) -0.0016(10) 0.0124(10) C3 0.0399(15) 0.0434(16) 0.0354(13) -0.0033(12) -0.0023(11) 0.0225(13) C4 0.0527(19) 0.0504(18) 0.0360(14) 0.0079(13) 0.0062(13) 0.0288(16) C5 0.0451(17) 0.0386(15) 0.0425(15) 0.0083(12) 0.0056(13) 0.0194(13) C6 0.0434(16) 0.0271(12) 0.0392(13) 0.0018(10) 0.0033(12) 0.0122(11) C7 0.0366(14) 0.0321(13) 0.0348(12) 0.0010(10) 0.0030(10) 0.0136(11) C8 0.0499(17) 0.0354(14) 0.0318(12) 0.0029(11) 0.0035(12) 0.0226(13) C9 0.0468(16) 0.0368(14) 0.0271(11) 0.0009(10) 0.0002(11) 0.0231(13) C10 0.0527(19) 0.0445(17) 0.0422(15) 0.0081(13) 0.0041(13) 0.0310(15) C11 0.0539(19) 0.0546(19) 0.0422(15) 0.0092(14) 0.0077(14) 0.0387(17) C12 0.0407(15) 0.0369(14) 0.0306(11) -0.0001(10) 0.0017(10) 0.0220(13) C13 0.0391(14) 0.0331(13) 0.0287(11) -0.0010(10) -0.0003(10) 0.0191(12) C14 0.0374(14) 0.0424(15) 0.0308(12) 0.0002(11) 0.0008(10) 0.0233(13) C15 0.0443(17) 0.058(2) 0.0418(16) 0.0066(14) 0.0051(13) 0.0328(16) C16 0.0452(17) 0.068(2) 0.0372(15) 0.0050(15) 0.0074(13) 0.0348(17) C17 0.0353(14) 0.0547(18) 0.0312(13) 0.0025(12) 0.0023(11) 0.0210(14) C18 0.0358(14) 0.0467(16) 0.0306(12) 0.0049(11) 0.0023(10) 0.0215(13) C19 0.0436(18) 0.102(3) 0.0401(16) 0.0209(19) 0.0105(14) 0.041(2) C20 0.0354(13) 0.0414(16) 0.0342(12) 0.0047(11) 0.0041(10) 0.0156(12) C21 0.0378(14) 0.061(2) 0.0378(13) 0.0053(15) 0.0077(11) 0.0201(16) C22 0.0449(16) 0.057(2) 0.0378(13) 0.0099(16) 0.0130(12) 0.0216(17) C23 0.0538(18) 0.0432(17) 0.0342(13) 0.0038(11) 0.0062(12) 0.0224(14) C24 0.0468(17) 0.0410(16) 0.0329(13) 0.0016(11) 0.0014(12) 0.0205(14) C25 0.0352(13) 0.0323(13) 0.0346(13) 0.0026(10) 0.0016(10) 0.0141(11) C26 0.0384(14) 0.0397(14) 0.0336(12) -0.0026(11) 0.0002(10) 0.0212(12) C27 0.092(3) 0.081(3) 0.0398(17) 0.0179(18) 0.0205(19) 0.058(3) C31 0.072(2) 0.057(2) 0.0344(14) 0.0082(13) 0.0125(15) 0.0371(19) C32 0.115(4) 0.068(3) 0.0397(18) -0.0072(18) 0.002(2) 0.038(3) C33 0.126(5) 0.076(3) 0.044(2) 0.018(2) 0.014(2) 0.061(3) C34 0.096(4) 0.133(5) 0.0435(19) 0.012(3) 0.027(2) 0.069(4) C35 0.0335(12) 0.0348(14) 0.0408(13) -0.0050(11) -0.0008(10) 0.0178(11) C36 0.0350(14) 0.0397(15) 0.0388(14) -0.0008(11) 0.0040(11) 0.0161(12) C37 0.0531(19) 0.0536(19) 0.0401(15) 0.0028(14) 0.0063(14) 0.0315(16) C38 0.069(2) 0.065(2) 0.0378(16) 0.0018(15) 0.0126(16) 0.039(2) C39 0.055(2) 0.069(2) 0.0482(18) 0.0031(17) 0.0127(16) 0.041(2) C40 0.0486(18) 0.065(2) 0.0453(17) -0.0020(16) 0.0057(14) 0.0358(18) C41 0.0397(15) 0.0473(17) 0.0364(14) -0.0028(12) 0.0035(11) 0.0235(13) C42 0.0470(17) 0.0518(18) 0.0405(15) 0.0012(13) 0.0078(13) 0.0330(15) C43 0.0403(16) 0.0446(17) 0.0393(13) -0.0018(13) 0.0022(12) 0.0250(13) C44 0.060(2) 0.0387(16) 0.062(2) 0.0002(15) 0.0168(17) 0.0304(16) C45 0.061(2) 0.0374(16) 0.0559(19) 0.0055(14) 0.0188(16) 0.0286(16) C46 0.0416(15) 0.0345(14) 0.0385(14) -0.0010(11) 0.0032(11) 0.0204(12) C47 0.0367(15) 0.0393(15) 0.0355(12) 0.0004(11) 0.0014(11) 0.0227(13) C48 0.0391(14) 0.0302(13) 0.0414(14) 0.0012(11) 0.0037(11) 0.0170(12) C49 0.064(2) 0.0296(14) 0.059(2) 0.0041(13) 0.0187(17) 0.0219(15) C50 0.060(2) 0.0330(15) 0.0566(19) 0.0065(13) 0.0162(16) 0.0169(14) C51 0.0320(13) 0.0301(13) 0.0426(15) -0.0003(11) 0.0043(11) 0.0084(11) C52 0.0309(13) 0.0327(13) 0.0370(13) -0.0010(10) 0.0006(10) 0.0137(11) C53 0.0387(16) 0.0379(16) 0.0494(17) -0.0003(13) 0.0112(13) 0.0100(13) C54 0.0373(15) 0.0473(17) 0.0452(16) 0.0032(13) 0.0102(12) 0.0213(13) C55 0.0364(16) 0.053(2) 0.056(2) -0.0039(16) 0.0127(15) 0.0090(15) C56 0.0407(18) 0.071(3) 0.053(2) 0.0071(18) 0.0156(15) 0.0178(18) C57 0.0404(17) 0.081(3) 0.0470(17) 0.000(2) 0.0078(13) 0.020(2) C58 0.0389(17) 0.063(2) 0.0475(18) -0.0039(16) 0.0022(14) 0.0185(16) C59 0.0341(14) 0.0447(16) 0.0455(15) 0.0042(12) 0.0075(12) 0.0192(12) C60 0.0349(14) 0.0376(15) 0.0463(16) 0.0054(12) 0.0048(12) 0.0192(12) C61 0.135(5) 0.099(4) 0.047(2) 0.014(2) 0.030(3) 0.081(4) C62 0.229(11) 0.179(9) 0.047(3) 0.011(4) 0.039(4) 0.146(9) C63 0.261(12) 0.116(6) 0.061(3) 0.032(3) 0.062(5) 0.118(7) C64 0.190(10) 0.193(10) 0.049(3) -0.027(4) -0.016(4) 0.119(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.095(2) 3_565 ? Ni1 N3 2.095(2) 2_665 ? Ni1 N3 2.095(2) . ? Ni1 N4 2.103(2) 2_665 ? Ni1 N4 2.103(2) 3_565 ? Ni1 N4 2.103(2) . ? Ni2 N8 2.109(2) 3_665 ? Ni2 N8 2.109(2) . ? Ni2 N8 2.109(2) 2_655 ? Ni2 N7 2.110(2) 3_665 ? Ni2 N7 2.110(2) 2_655 ? Ni2 N7 2.110(2) . ? P1 F6 1.512(6) . ? P1 F2 1.541(7) . ? P1 F5 1.562(6) . ? P1 F4 1.577(9) . ? P1 F1 1.587(5) . ? P1 F3 1.591(5) . ? P2 F8 1.583(3) 2 ? P2 F8 1.583(3) 3 ? P2 F8 1.583(3) . ? P2 F7 1.598(3) 3 ? P2 F7 1.598(3) 2 ? P2 F7 1.598(3) . ? P3 F9 1.562(10) 2 ? P3 F9 1.562(10) 3 ? P3 F9 1.562(10) . ? P3 F10 1.564(7) 3 ? P3 F10 1.564(7) . ? P3 F10 1.564(7) 2 ? O1 C7 1.376(3) . ? O1 C8 1.409(4) . ? O2 C20 1.389(3) . ? O2 C19 1.422(5) . ? O3 C41 1.376(4) . ? O3 C42 1.415(4) . ? O4 C54 1.390(4) . ? O4 C53 1.421(4) . ? O5 O6 1.211(18) . ? O5 O7 1.420(14) . ? O6 O7 1.223(17) . ? O8 O8 0.72(9) 4 ? O9 C69 1.684(14) . ? O9 C71 1.78(3) . ? N1 C1 1.480(3) . ? N1 C1 1.480(3) 3_565 ? N1 C1 1.480(3) 2_665 ? N2 C26 1.464(3) 2_665 ? N2 C26 1.464(3) . ? N2 C26 1.464(3) 3_565 ? N3 C13 1.345(4) . ? N3 C12 1.349(4) . ? N4 C18 1.351(4) . ? N4 C14 1.354(4) . ? N5 C35 1.468(3) 2_655 ? N5 C35 1.468(3) . ? N5 C35 1.468(3) 3_665 ? N6 C60 1.463(3) . ? N6 C60 1.463(3) 3_665 ? N6 C60 1.463(3) 2_655 ? N7 C47 1.343(4) . ? N7 C46 1.353(4) . ? N8 C52 1.345(4) . ? N8 C48 1.347(4) . ? C1 C2 1.514(4) . ? C2 C3 1.395(4) . ? C2 C7 1.403(4) . ? C3 C4 1.396(5) . ? C4 C5 1.391(5) . ? C4 C27 1.530(5) . ? C5 C6 1.392(4) . ? C6 C7 1.388(4) . ? C8 C9 1.518(4) . ? C9 C10 1.372(5) . ? C9 C13 1.392(4) . ? C10 C11 1.396(5) . ? C11 C12 1.390(4) . ? C12 C14 1.478(4) . ? C14 C15 1.385(4) . ? C15 C16 1.393(5) . ? C16 C17 1.382(5) . ? C17 C18 1.397(4) . ? C17 C19 1.502(5) . ? C20 C21 1.389(4) . ? C20 C25 1.396(4) . ? C21 C22 1.406(4) . ? C22 C23 1.389(5) . ? C23 C24 1.395(5) . ? C23 C31 1.540(4) . ? C24 C25 1.402(4) . ? C25 C26 1.505(4) . ? C27 C30A 1.428(12) . ? C27 C28A 1.458(14) . ? C27 C28B 1.471(12) . ? C27 C29A 1.503(2) . ? C27 C29B 1.504(2) . ? C27 C30B 1.517(11) . ? C31 C32 1.518(7) . ? C31 C33 1.534(6) . ? C31 C34 1.536(7) . ? C35 C36 1.509(4) . ? C36 C37 1.390(5) . ? C36 C41 1.393(5) . ? C37 C38 1.410(5) . ? C38 C39 1.382(6) . ? C38 C61 1.544(6) . ? C39 C40 1.398(5) . ? C40 C41 1.385(5) . ? C42 C43 1.496(4) . ? C43 C44 1.386(5) . ? C43 C47 1.400(4) . ? C44 C45 1.384(5) . ? C45 C46 1.387(4) . ? C46 C48 1.479(4) . ? C48 C49 1.395(4) . ? C49 C50 1.368(5) . ? C50 C51 1.393(5) . ? C51 C52 1.392(4) . ? C51 C53 1.502(4) . ? C54 C55 1.387(5) . ? C54 C59 1.390(5) . ? C55 C56 1.394(6) . ? C56 C57 1.364(6) . ? C57 C58 1.399(5) . ? C57 C65B 1.550(8) . ? C57 C65A 1.630(10) . ? C58 C59 1.387(5) . ? C59 C60 1.512(4) . ? C61 C62 1.463(9) . ? C61 C63 1.486(9) . ? C61 C64 1.504(2) . ? C65A C66A 1.485(13) . ? C65A C68A 1.500(16) . ? C65A C67A 1.593(17) . ? C65B C67B 1.529(14) . ? C65B C68B 1.530(11) . ? C65B C66B 1.563(13) . ? N9 C69 1.114(8) . ? C69 C70 1.505(10) . ? N10 C71 1.08(3) . ? C71 C72 1.453(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 N3 Ni1 N3 93.41(9) 3_565 2_665 ? N3 Ni1 N3 93.41(9) 3_565 . ? N3 Ni1 N3 93.41(9) 2_665 . ? N3 Ni1 N4 90.17(9) 3_565 2_665 ? N3 Ni1 N4 79.12(9) 2_665 2_665 ? N3 Ni1 N4 171.91(10) . 2_665 ? N3 Ni1 N4 79.12(9) 3_565 3_565 ? N3 Ni1 N4 171.91(10) 2_665 3_565 ? N3 Ni1 N4 90.17(10) . 3_565 ? N4 Ni1 N4 97.63(9) 2_665 3_565 ? N3 Ni1 N4 171.91(10) 3_565 . ? N3 Ni1 N4 90.17(10) 2_665 . ? N3 Ni1 N4 79.12(9) . . ? N4 Ni1 N4 97.63(9) 2_665 . ? N4 Ni1 N4 97.63(9) 3_565 . ? N8 Ni2 N8 95.70(8) 3_665 . ? N8 Ni2 N8 95.70(8) 3_665 2_655 ? N8 Ni2 N8 95.70(8) . 2_655 ? N8 Ni2 N7 78.13(9) 3_665 3_665 ? N8 Ni2 N7 90.28(9) . 3_665 ? N8 Ni2 N7 171.83(10) 2_655 3_665 ? N8 Ni2 N7 90.28(9) 3_665 2_655 ? N8 Ni2 N7 171.83(10) . 2_655 ? N8 Ni2 N7 78.13(9) 2_655 2_655 ? N7 Ni2 N7 96.41(9) 3_665 2_655 ? N8 Ni2 N7 171.83(10) 3_665 . ? N8 Ni2 N7 78.13(9) . . ? N8 Ni2 N7 90.28(9) 2_655 . ? N7 Ni2 N7 96.41(9) 3_665 . ? N7 Ni2 N7 96.41(9) 2_655 . ? F6 P1 F2 94.6(6) . . ? F6 P1 F5 172.4(6) . . ? F2 P1 F5 92.9(5) . . ? F6 P1 F4 88.4(6) . . ? F2 P1 F4 177.0(6) . . ? F5 P1 F4 84.1(6) . . ? F6 P1 F1 90.0(3) . . ? F2 P1 F1 92.8(4) . . ? F5 P1 F1 88.1(3) . . ? F4 P1 F1 87.0(5) . . ? F6 P1 F3 91.0(3) . . ? F2 P1 F3 86.6(4) . . ? F5 P1 F3 91.0(3) . . ? F4 P1 F3 93.5(5) . . ? F1 P1 F3 178.9(3) . . ? F8 P2 F8 90.59(19) 2 3 ? F8 P2 F8 90.59(19) 2 . ? F8 P2 F8 90.59(19) 3 . ? F8 P2 F7 89.60(19) 2 3 ? F8 P2 F7 179.4(2) 3 3 ? F8 P2 F7 89.9(2) . 3 ? F8 P2 F7 179.4(2) 2 2 ? F8 P2 F7 89.9(2) 3 2 ? F8 P2 F7 89.60(19) . 2 ? F7 P2 F7 89.86(17) 3 2 ? F8 P2 F7 89.9(2) 2 . ? F8 P2 F7 89.60(19) 3 . ? F8 P2 F7 179.4(2) . . ? F7 P2 F7 89.86(17) 3 . ? F7 P2 F7 89.86(17) 2 . ? F9 P3 F9 88.5(6) 2 3 ? F9 P3 F9 88.5(6) 2 . ? F9 P3 F9 88.5(6) 3 . ? F9 P3 F10 89.8(6) 2 3 ? F9 P3 F10 176.8(7) 3 3 ? F9 P3 F10 88.7(6) . 3 ? F9 P3 F10 88.7(6) 2 . ? F9 P3 F10 89.8(6) 3 . ? F9 P3 F10 176.8(7) . . ? F10 P3 F10 92.9(7) 3 . ? F9 P3 F10 176.8(7) 2 2 ? F9 P3 F10 88.7(6) 3 2 ? F9 P3 F10 89.8(6) . 2 ? F10 P3 F10 92.9(7) 3 2 ? F10 P3 F10 92.9(7) . 2 ? C7 O1 C8 118.4(2) . . ? C20 O2 C19 116.6(3) . . ? C41 O3 C42 118.2(3) . . ? C54 O4 C53 116.4(3) . . ? O6 O5 O7 54.7(9) . . ? O5 O6 O7 71.4(11) . . ? O6 O7 O5 53.9(10) . . ? C69 O9 C71 154.1(12) . . ? C1 N1 C1 110.00(19) . 3_565 ? C1 N1 C1 110.00(19) . 2_665 ? C1 N1 C1 110.00(19) 3_565 2_665 ? C26 N2 C26 109.80(18) 2_665 . ? C26 N2 C26 109.80(18) 2_665 3_565 ? C26 N2 C26 109.80(18) . 3_565 ? C13 N3 C12 118.5(2) . . ? C13 N3 Ni1 127.2(2) . . ? C12 N3 Ni1 114.28(18) . . ? C18 N4 C14 118.5(3) . . ? C18 N4 Ni1 127.5(2) . . ? C14 N4 Ni1 113.44(18) . . ? C35 N5 C35 110.39(18) 2_655 . ? C35 N5 C35 110.39(18) 2_655 3_665 ? C35 N5 C35 110.39(18) . 3_665 ? C60 N6 C60 111.97(18) . 3_665 ? C60 N6 C60 111.97(18) . 2_655 ? C60 N6 C60 111.97(18) 3_665 2_655 ? C47 N7 C46 118.3(3) . . ? C47 N7 Ni2 126.6(2) . . ? C46 N7 Ni2 114.69(19) . . ? C52 N8 C48 118.4(3) . . ? C52 N8 Ni2 126.4(2) . . ? C48 N8 Ni2 115.12(19) . . ? N1 C1 C2 113.0(2) . . ? C3 C2 C7 118.4(3) . . ? C3 C2 C1 120.3(3) . . ? C7 C2 C1 121.2(3) . . ? C2 C3 C4 122.8(3) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C27 121.7(3) . . ? C3 C4 C27 121.6(3) . . ? C4 C5 C6 122.2(3) . . ? C7 C6 C5 119.7(3) . . ? O1 C7 C6 124.4(3) . . ? O1 C7 C2 115.5(3) . . ? C6 C7 C2 120.1(3) . . ? O1 C8 C9 106.9(2) . . ? C10 C9 C13 118.6(3) . . ? C10 C9 C8 121.0(3) . . ? C13 C9 C8 120.3(3) . . ? C9 C10 C11 118.9(3) . . ? C12 C11 C10 119.5(3) . . ? N3 C12 C11 121.4(3) . . ? N3 C12 C14 116.1(3) . . ? C11 C12 C14 122.5(3) . . ? N3 C13 C9 123.0(3) . . ? N4 C14 C15 121.5(3) . . ? N4 C14 C12 116.1(3) . . ? C15 C14 C12 122.4(3) . . ? C14 C15 C16 119.8(3) . . ? C17 C16 C15 119.0(3) . . ? C16 C17 C18 118.5(3) . . ? C16 C17 C19 118.2(3) . . ? C18 C17 C19 123.3(3) . . ? N4 C18 C17 122.7(3) . . ? O2 C19 C17 109.3(3) . . ? O2 C20 C21 123.3(3) . . ? O2 C20 C25 115.8(3) . . ? C21 C20 C25 120.9(3) . . ? C20 C21 C22 119.1(3) . . ? C23 C22 C21 121.6(3) . . ? C22 C23 C24 117.7(3) . . ? C22 C23 C31 122.6(3) . . ? C24 C23 C31 119.7(3) . . ? C23 C24 C25 122.4(3) . . ? C20 C25 C24 118.3(3) . . ? C20 C25 C26 121.9(3) . . ? C24 C25 C26 119.8(3) . . ? N2 C26 C25 111.2(2) . . ? C30A C27 C28A 123.4(8) . . ? C30A C27 C28B 133.3(7) . . ? C28A C27 C28B 39.5(6) . . ? C30A C27 C29A 98.0(10) . . ? C28A C27 C29A 89.0(10) . . ? C28B C27 C29A 52.5(9) . . ? C30A C27 C29B 74.9(8) . . ? C28A C27 C29B 69.0(8) . . ? C28B C27 C29B 108.2(7) . . ? C29A C27 C29B 145.6(10) . . ? C30A C27 C30B 30.1(5) . . ? C28A C27 C30B 129.6(7) . . ? C28B C27 C30B 115.4(7) . . ? C29A C27 C30B 69.5(9) . . ? C29B C27 C30B 103.9(7) . . ? C30A C27 C4 114.0(6) . . ? C28A C27 C4 117.2(6) . . ? C28B C27 C4 109.6(5) . . ? C29A C27 C4 107.0(8) . . ? C29B C27 C4 106.6(6) . . ? C30B C27 C4 112.7(5) . . ? C32 C31 C33 109.3(5) . . ? C32 C31 C34 109.4(4) . . ? C33 C31 C34 107.4(4) . . ? C32 C31 C23 109.9(3) . . ? C33 C31 C23 109.1(3) . . ? C34 C31 C23 111.8(4) . . ? N5 C35 C36 111.9(2) . . ? C37 C36 C41 118.1(3) . . ? C37 C36 C35 119.2(3) . . ? C41 C36 C35 122.7(3) . . ? C36 C37 C38 122.7(3) . . ? C39 C38 C37 116.4(3) . . ? C39 C38 C61 124.8(4) . . ? C37 C38 C61 118.7(4) . . ? C38 C39 C40 122.7(3) . . ? C41 C40 C39 118.6(3) . . ? O3 C41 C40 123.4(3) . . ? O3 C41 C36 115.3(3) . . ? C40 C41 C36 121.3(3) . . ? O3 C42 C43 108.5(3) . . ? C44 C43 C47 117.1(3) . . ? C44 C43 C42 120.9(3) . . ? C47 C43 C42 121.9(3) . . ? C45 C44 C43 120.1(3) . . ? C44 C45 C46 119.3(3) . . ? N7 C46 C45 121.7(3) . . ? N7 C46 C48 115.8(3) . . ? C45 C46 C48 122.5(3) . . ? N7 C47 C43 123.5(3) . . ? N8 C48 C49 121.1(3) . . ? N8 C48 C46 115.8(3) . . ? C49 C48 C46 123.1(3) . . ? C50 C49 C48 119.9(3) . . ? C49 C50 C51 119.9(3) . . ? C52 C51 C50 117.1(3) . . ? C52 C51 C53 122.4(3) . . ? C50 C51 C53 120.5(3) . . ? N8 C52 C51 123.6(3) . . ? O4 C53 C51 108.6(3) . . ? C55 C54 O4 122.9(3) . . ? C55 C54 C59 120.4(3) . . ? O4 C54 C59 116.7(3) . . ? C54 C55 C56 119.1(4) . . ? C57 C56 C55 122.1(4) . . ? C56 C57 C58 117.8(3) . . ? C56 C57 C65B 116.1(4) . . ? C58 C57 C65B 125.4(4) . . ? C56 C57 C65A 126.7(4) . . ? C58 C57 C65A 114.5(5) . . ? C65B C57 C65A 21.5(3) . . ? C59 C58 C57 121.9(4) . . ? C58 C59 C54 118.7(3) . . ? C58 C59 C60 118.6(3) . . ? C54 C59 C60 122.5(3) . . ? N6 C60 C59 108.8(3) . . ? C62 C61 C63 119.6(6) . . ? C62 C61 C64 99.8(7) . . ? C63 C61 C64 102.3(7) . . ? C62 C61 C38 112.3(5) . . ? C63 C61 C38 111.8(4) . . ? C64 C61 C38 109.3(4) . . ? C66A C65A C68A 116.3(9) . . ? C66A C65A C67A 101.6(9) . . ? C68A C65A C67A 106.7(10) . . ? C66A C65A C57 112.0(7) . . ? C68A C65A C57 105.0(8) . . ? C67A C65A C57 115.4(8) . . ? C67B C65B C68B 108.7(7) . . ? C67B C65B C57 113.3(7) . . ? C68B C65B C57 108.6(6) . . ? C67B C65B C66B 115.2(8) . . ? C68B C65B C66B 107.0(7) . . ? C57 C65B C66B 103.7(6) . . ? N9 C69 C70 145.0(7) . . ? N9 C69 O9 106.7(7) . . ? C70 C69 O9 108.3(7) . . ? N10 C71 C72 174(3) . . ? N10 C71 O9 95.1(19) . . ? C72 C71 O9 81.5(15) . . ? 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 N3 Ni1 N3 C13 1.5(2) 3_565 . . . ? N3 Ni1 N3 C13 95.15(19) 2_665 . . . ? N4 Ni1 N3 C13 117.7(7) 2_665 . . . ? N4 Ni1 N3 C13 -77.6(2) 3_565 . . . ? N4 Ni1 N3 C13 -175.3(3) . . . . ? N3 Ni1 N3 C12 -179.5(2) 3_565 . . . ? N3 Ni1 N3 C12 -85.9(2) 2_665 . . . ? N4 Ni1 N3 C12 -63.3(7) 2_665 . . . ? N4 Ni1 N3 C12 101.4(2) 3_565 . . . ? N4 Ni1 N3 C12 3.6(2) . . . . ? N3 Ni1 N4 C18 157.7(6) 3_565 . . . ? N3 Ni1 N4 C18 -85.9(3) 2_665 . . . ? N3 Ni1 N4 C18 -179.3(3) . . . . ? N4 Ni1 N4 C18 -6.9(3) 2_665 . . . ? N4 Ni1 N4 C18 92.0(2) 3_565 . . . ? N3 Ni1 N4 C14 -31.0(8) 3_565 . . . ? N3 Ni1 N4 C14 85.3(2) 2_665 . . . ? N3 Ni1 N4 C14 -8.1(2) . . . . ? N4 Ni1 N4 C14 164.4(2) 2_665 . . . ? N4 Ni1 N4 C14 -96.8(3) 3_565 . . . ? N8 Ni2 N7 C47 -141.1(6) 3_665 . . . ? N8 Ni2 N7 C47 177.5(3) . . . . ? N8 Ni2 N7 C47 81.7(2) 2_655 . . . ? N7 Ni2 N7 C47 -93.58(19) 3_665 . . . ? N7 Ni2 N7 C47 3.6(3) 2_655 . . . ? N8 Ni2 N7 C46 45.9(7) 3_665 . . . ? N8 Ni2 N7 C46 4.5(2) . . . . ? N8 Ni2 N7 C46 -91.2(2) 2_655 . . . ? N7 Ni2 N7 C46 93.5(3) 3_665 . . . ? N7 Ni2 N7 C46 -169.3(2) 2_655 . . . ? N8 Ni2 N8 C52 1.8(2) 3_665 . . . ? N8 Ni2 N8 C52 -94.56(19) 2_655 . . . ? N7 Ni2 N8 C52 79.9(2) 3_665 . . . ? N7 Ni2 N8 C52 -135.1(6) 2_655 . . . ? N7 Ni2 N8 C52 176.4(3) . . . . ? N8 Ni2 N8 C48 -175.1(2) 3_665 . . . ? N8 Ni2 N8 C48 88.5(3) 2_655 . . . ? N7 Ni2 N8 C48 -97.0(2) 3_665 . . . ? N7 Ni2 N8 C48 48.0(7) 2_655 . . . ? N7 Ni2 N8 C48 -0.5(2) . . . . ? C1 N1 C1 C2 -177.1(2) 3_565 . . . ? C1 N1 C1 C2 61.6(4) 2_665 . . . ? N1 C1 C2 C3 81.6(4) . . . . ? N1 C1 C2 C7 -99.9(3) . . . . ? C7 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 C4 179.0(3) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? C2 C3 C4 C27 -179.2(4) . . . . ? C3 C4 C5 C6 -2.5(5) . . . . ? C27 C4 C5 C6 178.0(4) . . . . ? C4 C5 C6 C7 1.8(5) . . . . ? C8 O1 C7 C6 -4.4(5) . . . . ? C8 O1 C7 C2 175.7(3) . . . . ? C5 C6 C7 O1 -179.8(3) . . . . ? C5 C6 C7 C2 0.1(5) . . . . ? C3 C2 C7 O1 178.7(3) . . . . ? C1 C2 C7 O1 0.2(4) . . . . ? C3 C2 C7 C6 -1.2(5) . . . . ? C1 C2 C7 C6 -179.7(3) . . . . ? C7 O1 C8 C9 -166.7(3) . . . . ? O1 C8 C9 C10 135.1(3) . . . . ? O1 C8 C9 C13 -46.0(4) . . . . ? C13 C9 C10 C11 1.1(5) . . . . ? C8 C9 C10 C11 180.0(3) . . . . ? C9 C10 C11 C12 -0.7(6) . . . . ? C13 N3 C12 C11 1.0(4) . . . . ? Ni1 N3 C12 C11 -178.1(3) . . . . ? C13 N3 C12 C14 -179.8(3) . . . . ? Ni1 N3 C12 C14 1.1(3) . . . . ? C10 C11 C12 N3 -0.4(5) . . . . ? C10 C11 C12 C14 -179.5(3) . . . . ? C12 N3 C13 C9 -0.6(4) . . . . ? Ni1 N3 C13 C9 178.4(2) . . . . ? C10 C9 C13 N3 -0.5(5) . . . . ? C8 C9 C13 N3 -179.4(3) . . . . ? C18 N4 C14 C15 3.3(5) . . . . ? Ni1 N4 C14 C15 -168.8(3) . . . . ? C18 N4 C14 C12 -176.7(3) . . . . ? Ni1 N4 C14 C12 11.2(3) . . . . ? N3 C12 C14 N4 -8.3(4) . . . . ? C11 C12 C14 N4 170.8(3) . . . . ? N3 C12 C14 C15 171.6(3) . . . . ? C11 C12 C14 C15 -9.2(5) . . . . ? N4 C14 C15 C16 -3.1(5) . . . . ? C12 C14 C15 C16 176.9(3) . . . . ? C14 C15 C16 C17 0.4(6) . . . . ? C15 C16 C17 C18 1.9(6) . . . . ? C15 C16 C17 C19 -179.8(4) . . . . ? C14 N4 C18 C17 -0.8(5) . . . . ? Ni1 N4 C18 C17 170.0(3) . . . . ? C16 C17 C18 N4 -1.8(5) . . . . ? C19 C17 C18 N4 180.0(4) . . . . ? C20 O2 C19 C17 -150.3(3) . . . . ? C16 C17 C19 O2 164.9(4) . . . . ? C18 C17 C19 O2 -16.9(6) . . . . ? C19 O2 C20 C21 -27.7(5) . . . . ? C19 O2 C20 C25 153.5(4) . . . . ? O2 C20 C21 C22 179.6(4) . . . . ? C25 C20 C21 C22 -1.7(6) . . . . ? C20 C21 C22 C23 0.0(7) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C21 C22 C23 C31 -178.7(4) . . . . ? C22 C23 C24 C25 -1.0(5) . . . . ? C31 C23 C24 C25 179.0(3) . . . . ? O2 C20 C25 C24 -179.1(3) . . . . ? C21 C20 C25 C24 2.1(5) . . . . ? O2 C20 C25 C26 -1.2(5) . . . . ? C21 C20 C25 C26 -180.0(3) . . . . ? C23 C24 C25 C20 -0.7(5) . . . . ? C23 C24 C25 C26 -178.7(3) . . . . ? C26 N2 C26 C25 -172.5(2) 2_665 . . . ? C26 N2 C26 C25 66.6(4) 3_565 . . . ? C20 C25 C26 N2 -118.9(3) . . . . ? C24 C25 C26 N2 59.1(4) . . . . ? C5 C4 C27 C30A 53.2(8) . . . . ? C3 C4 C27 C30A -126.3(7) . . . . ? C5 C4 C27 C28A -151.9(7) . . . . ? C3 C4 C27 C28A 28.6(9) . . . . ? C5 C4 C27 C28B -109.5(6) . . . . ? C3 C4 C27 C28B 71.0(7) . . . . ? C5 C4 C27 C29A -54.0(10) . . . . ? C3 C4 C27 C29A 126.5(9) . . . . ? C5 C4 C27 C29B 133.6(6) . . . . ? C3 C4 C27 C29B -45.9(7) . . . . ? C5 C4 C27 C30B 20.3(7) . . . . ? C3 C4 C27 C30B -159.2(6) . . . . ? C22 C23 C31 C32 124.1(5) . . . . ? C24 C23 C31 C32 -55.9(5) . . . . ? C22 C23 C31 C33 -116.1(5) . . . . ? C24 C23 C31 C33 63.9(5) . . . . ? C22 C23 C31 C34 2.5(6) . . . . ? C24 C23 C31 C34 -177.5(4) . . . . ? C35 N5 C35 C36 174.7(2) 2_655 . . . ? C35 N5 C35 C36 -63.0(4) 3_665 . . . ? N5 C35 C36 C37 -70.3(4) . . . . ? N5 C35 C36 C41 109.3(4) . . . . ? C41 C36 C37 C38 -0.2(6) . . . . ? C35 C36 C37 C38 179.5(4) . . . . ? C36 C37 C38 C39 2.9(6) . . . . ? C36 C37 C38 C61 -173.6(4) . . . . ? C37 C38 C39 C40 -3.7(7) . . . . ? C61 C38 C39 C40 172.5(5) . . . . ? C38 C39 C40 C41 1.8(7) . . . . ? C42 O3 C41 C40 20.4(5) . . . . ? C42 O3 C41 C36 -158.7(3) . . . . ? C39 C40 C41 O3 -177.9(4) . . . . ? C39 C40 C41 C36 1.1(6) . . . . ? C37 C36 C41 O3 177.2(3) . . . . ? C35 C36 C41 O3 -2.4(5) . . . . ? C37 C36 C41 C40 -1.9(5) . . . . ? C35 C36 C41 C40 178.4(3) . . . . ? C41 O3 C42 C43 160.0(3) . . . . ? O3 C42 C43 C44 -155.8(3) . . . . ? O3 C42 C43 C47 26.7(5) . . . . ? C47 C43 C44 C45 -2.1(6) . . . . ? C42 C43 C44 C45 -179.7(4) . . . . ? C43 C44 C45 C46 0.6(7) . . . . ? C47 N7 C46 C45 -0.5(5) . . . . ? Ni2 N7 C46 C45 173.1(3) . . . . ? C47 N7 C46 C48 178.8(3) . . . . ? Ni2 N7 C46 C48 -7.6(3) . . . . ? C44 C45 C46 N7 0.8(6) . . . . ? C44 C45 C46 C48 -178.5(4) . . . . ? C46 N7 C47 C43 -1.2(4) . . . . ? Ni2 N7 C47 C43 -173.9(2) . . . . ? C44 C43 C47 N7 2.4(5) . . . . ? C42 C43 C47 N7 -180.0(3) . . . . ? C52 N8 C48 C49 0.0(5) . . . . ? Ni2 N8 C48 C49 177.2(3) . . . . ? C52 N8 C48 C46 179.6(3) . . . . ? Ni2 N8 C48 C46 -3.2(4) . . . . ? N7 C46 C48 N8 7.3(4) . . . . ? C45 C46 C48 N8 -173.4(3) . . . . ? N7 C46 C48 C49 -173.2(3) . . . . ? C45 C46 C48 C49 6.2(6) . . . . ? N8 C48 C49 C50 -0.5(6) . . . . ? C46 C48 C49 C50 179.9(4) . . . . ? C48 C49 C50 C51 0.6(7) . . . . ? C49 C50 C51 C52 -0.2(6) . . . . ? C49 C50 C51 C53 179.7(4) . . . . ? C48 N8 C52 C51 0.4(4) . . . . ? Ni2 N8 C52 C51 -176.4(2) . . . . ? C50 C51 C52 N8 -0.3(5) . . . . ? C53 C51 C52 N8 179.8(3) . . . . ? C54 O4 C53 C51 144.9(3) . . . . ? C52 C51 C53 O4 8.5(5) . . . . ? C50 C51 C53 O4 -171.4(3) . . . . ? C53 O4 C54 C55 47.9(5) . . . . ? C53 O4 C54 C59 -132.2(3) . . . . ? O4 C54 C55 C56 -179.2(4) . . . . ? C59 C54 C55 C56 1.0(6) . . . . ? C54 C55 C56 C57 -1.4(7) . . . . ? C55 C56 C57 C58 -0.3(8) . . . . ? C55 C56 C57 C65B 170.2(5) . . . . ? C55 C56 C57 C65A -167.7(6) . . . . ? C56 C57 C58 C59 2.4(7) . . . . ? C65B C57 C58 C59 -167.2(5) . . . . ? C65A C57 C58 C59 171.3(5) . . . . ? C57 C58 C59 C54 -2.7(6) . . . . ? C57 C58 C59 C60 172.9(4) . . . . ? C55 C54 C59 C58 1.0(5) . . . . ? O4 C54 C59 C58 -178.8(3) . . . . ? C55 C54 C59 C60 -174.5(4) . . . . ? O4 C54 C59 C60 5.7(5) . . . . ? C60 N6 C60 C59 164.5(3) 3_665 . . . ? C60 N6 C60 C59 -68.8(5) 2_655 . . . ? C58 C59 C60 N6 -69.7(4) . . . . ? C54 C59 C60 N6 105.8(4) . . . . ? C39 C38 C61 C62 -2.3(9) . . . . ? C37 C38 C61 C62 173.9(7) . . . . ? C39 C38 C61 C63 135.4(7) . . . . ? C37 C38 C61 C63 -48.5(8) . . . . ? C39 C38 C61 C64 -112.1(7) . . . . ? C37 C38 C61 C64 64.1(7) . . . . ? C56 C57 C65A C66A 7.0(11) . . . . ? C58 C57 C65A C66A -160.8(7) . . . . ? C65B C57 C65A C66A 73.8(13) . . . . ? C56 C57 C65A C68A -120.1(8) . . . . ? C58 C57 C65A C68A 72.1(9) . . . . ? C65B C57 C65A C68A -53.3(12) . . . . ? C56 C57 C65A C67A 122.6(9) . . . . ? C58 C57 C65A C67A -45.1(9) . . . . ? C65B C57 C65A C67A -170.5(17) . . . . ? C56 C57 C65B C67B -51.7(8) . . . . ? C58 C57 C65B C67B 118.0(8) . . . . ? C65A C57 C65B C67B -176.5(16) . . . . ? C56 C57 C65B C68B -172.5(6) . . . . ? C58 C57 C65B C68B -2.8(9) . . . . ? C65A C57 C65B C68B 62.7(12) . . . . ? C56 C57 C65B C66B 74.0(8) . . . . ? C58 C57 C65B C66B -116.3(7) . . . . ? C65A C57 C65B C66B -50.8(12) . . . . ? C71 O9 C69 N9 106(3) . . . . ? C71 O9 C69 C70 -73(3) . . . . ? C69 O9 C71 N10 -10(4) . . . . ? C69 O9 C71 C72 174(2) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 31.61 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.115 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.101 #===END data_lfl38 _database_code_depnum_ccdc_archive 'CCDC 222141' _audit_creation_method SHELXL-97 _publ_section_experimental ; Data for this small crystal were obtained at the ChemMatCARS facility at the Advanced Photon Source of the Argonne National Laboratory, Argonne USA. Double diamond (111) reflections were used to obtain monochromated 0.56356 \%A radiation from the synchrotron source, and harmonics were eliminated with mirrors. A colourless columnar crystal was attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Diffraction Cryojet. A Bruker Kappa with 4 chip mosaic CCD detector was used for the data collection. Cell constants were obtained from a least squares refinement against 1000 reflections located between 5.44 and 40\% 2\q. Data were collected at 123(2) Kelvin with \f scans to 37\% 2\q. The data integration and reduction were undertaken with SAINT and XPREP^1^, and subsequent computations were carried out with the teXsan^2^, WinGX^3^ and XTAL^4^ graphical user interfaces. The intensities of 146 standard reflections recollected at the end of the experiment changed by 11%. A multi-scan empirial correction for absorption, decay and any beam inhomogeneity determined with SADABS^5^ was applied to the data. The structure was solved in the space group P\-1 (#2) by direct methods with SIR97^6^, and extended and refined with SHELXL-97.^7^ The asymmetric unit contains the cage molecule, and three toluene solvate sites with populations refined and then fixed at the first decimal place (0.5). Two sites were treated as partial occupancy water sites. The three pyridyl links in the cage each have two orientations with occupancies of 0.5 (there may be further unresolved orientational disorder), and one of the toluene sites is in the centre of the cage cavity. Neighbouring molecules nestle into the helical groves defined by the bi-pyridyl links, and it may be that the nestling of a helical molecule into the groves of another containing a bound toluene molecule precludes solvate binding in both molecules. That is, toluene binding may be marginal and sensitive to subtle changes in the bi-pyridyl residue orientation and dictated by the grove interactions. The fully occupied atom sites were modelled with anisotropic displacement parameters and the rest were modelled with isotropic displacement parameters. Rigid bodies were used to model the pyridyl residues and toluene solvates. The pyridyl nitrogen assignment was based on a comparison of displacment parameters and may be erroneous. A riding atom model with group displacement parameters was used for the hydrogen atoms. No hydrogens were included for the sites treated as partial occupancy water oxygen sites. 1. Bruker (1995); SMART, SAINT and XPREP. Area detector control and data integration and reduction software. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 2. Molecular Structure Corporation (1997-1998). teXsan for Windows: Single Crystal Structure Analysis Software, MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. 3. WinGX, Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. 4. Hall, S.R., du Boulay, D.J. & Olthof-Hazekamp, R. (1999) Eds. Xtal3.6 System . University of Western Australia. 5. Blessing, R.H.; Acta Cryst. (1995) A51 33 - 38. Sheldrick, G.M.; SADABS. Empirical absorption correction program for area detector data. University of Gottingen, Germany, 1996. 6. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G., Spagna R. J. Appl. Cryst. 1998, 32, 115-119. 7. Sheldrick, G.M.; SHELX97 Programs for Crystal Structure Analysis. University of Gottingen. Institut fur Anorganische Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1998. ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112.50 H126 N8 O6.50' _chemical_formula_weight 1694.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.555(4) _cell_length_b 16.622(2) _cell_length_c 23.495(6) _cell_angle_alpha 71.105(11) _cell_angle_beta 78.998(8) _cell_angle_gamma 70.890(11) _cell_volume 5406(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 19.92 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1818 _exptl_absorpt_coefficient_mu 0.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.734 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; SADABS (Sheldrick, 1996) ; _diffrn_crystal_treatment ; attached with Exxon Paratone N, to a short length of fibre supported on a thin piece of copper wire inserted in a copper mounting pin. The crystal was quenched in a cold nitrogen gas stream from an Oxford Diffraction Cryojet. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.56356 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ChemMatCARS, APS, Argonne National Lab, USA' _diffrn_radiation_monochromator 'Double Diamond 111' _diffrn_measurement_device_type 'Bruker Kappa with 4 chip CCD detector' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 146 _diffrn_standards_interval_count ; First 50 frames recollected at of data collection ; _diffrn_standards_interval_time ? _diffrn_standards_decay_% 10.77 _diffrn_reflns_number 101066 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 18.24 _reflns_number_total 14377 _reflns_number_gt 10853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker,1995)' _computing_cell_refinement 'SAINT (Bruker,1995)' _computing_data_reduction 'SAINT and XPREP (Bruker 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; teXsan for Windows (MSC, 1997) xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999) ORTEPII (Johnson,C.K., 1976). WinGX (Farrugia, 1999) ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14377 _refine_ls_number_parameters 895 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1905 _refine_ls_R_factor_gt 0.1613 _refine_ls_wR_factor_ref 0.4376 _refine_ls_wR_factor_gt 0.4067 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.006 _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 O1 O 0.2542(3) 0.0200(3) 0.7024(2) 0.0580(12) Uani 1 1 d . B . O2 O 0.7701(3) 0.2001(3) 0.35673(18) 0.0545(12) Uani 1 1 d . . . O3 O 0.2232(3) 0.4332(3) 0.69865(18) 0.0593(12) Uani 1 1 d . D . O4 O 0.4979(4) 0.6119(3) 0.23330(19) 0.0703(15) Uani 1 1 d . . . O5 O -0.0670(4) 0.3901(4) 0.5651(2) 0.092(2) Uani 1 1 d . F . O6 O 0.4399(3) 0.2306(3) 0.2139(2) 0.0597(12) Uani 1 1 d . . . N1 N 0.0746(3) 0.2607(3) 0.7156(2) 0.0444(12) Uani 1 1 d . . . N2 N 0.6258(3) 0.3628(3) 0.2080(2) 0.0408(11) Uani 1 1 d . . . C1 C 0.1481(4) 0.1771(4) 0.7188(3) 0.0463(14) Uani 1 1 d . . . H1A H 0.1940 0.1731 0.7443 0.056 Uiso 1 1 calc R . . H1B H 0.1789 0.1780 0.6777 0.056 Uiso 1 1 calc R . . C2 C 0.1145(4) 0.0961(4) 0.7441(3) 0.0466(14) Uani 1 1 d . . . C3 C 0.0298(4) 0.0969(4) 0.7758(3) 0.0509(15) Uani 1 1 d . . . H3 H -0.0083 0.1510 0.7832 0.061 Uiso 1 1 calc R . . C4 C -0.0027(4) 0.0221(4) 0.7978(3) 0.0532(16) Uani 1 1 d . . . C5 C 0.0556(4) -0.0558(4) 0.7871(3) 0.0554(16) Uani 1 1 d . . . H5 H 0.0361 -0.1080 0.8010 0.067 Uiso 1 1 calc R . . C6 C 0.1420(4) -0.0596(4) 0.7565(3) 0.0535(16) Uani 1 1 d . . . H6 H 0.1809 -0.1144 0.7506 0.064 Uiso 1 1 calc R . . C7 C 0.1715(4) 0.0147(4) 0.7346(3) 0.0482(15) Uani 1 1 d . . . C8 C 0.3189(4) -0.0596(5) 0.6943(3) 0.0537(15) Uiso 1 1 d . . . H8A H 0.2911 -0.0877 0.6742 0.064 Uiso 1 1 calc R A 1 H8B H 0.3344 -0.1014 0.7344 0.064 Uiso 1 1 calc R A 1 C9A C 0.4073(5) -0.0432(6) 0.6562(4) 0.041(3) Uiso 0.50 1 d PG B 1 N3A N 0.5265(5) -0.0620(6) 0.5750(4) 0.067(3) Uiso 0.50 1 d PG B 1 C10A C 0.4400(7) 0.0212(7) 0.6640(4) 0.089(5) Uiso 0.50 1 d PG B 1 H10A H 0.4110 0.0498 0.6946 0.107 Uiso 0.50 1 calc PR B 1 C11A C 0.5151(6) 0.0435(6) 0.6272(4) 0.068(4) Uiso 0.50 1 d PG B 1 H11A H 0.5367 0.0875 0.6326 0.082 Uiso 0.50 1 calc PR B 1 C12A C 0.5583(5) 0.0021(6) 0.5827(4) 0.054(3) Uiso 0.50 1 d PG B 1 C13A C 0.4513(5) -0.0846(5) 0.6117(4) 0.044(3) Uiso 0.50 1 d PG B 1 H13A H 0.4300 -0.1288 0.6061 0.053 Uiso 0.50 1 calc PR B 1 C14A C 0.6300(9) 0.0359(9) 0.5444(6) 0.066(4) Uiso 0.50 1 d PG B 1 N4A N 0.6742(12) -0.0045(9) 0.4994(8) 0.152(12) Uiso 0.50 1 d PG B 1 C15A C 0.6522(10) 0.1098(9) 0.5468(6) 0.110(6) Uiso 0.50 1 d PG B 1 H15A H 0.6229 0.1378 0.5776 0.132 Uiso 0.50 1 calc PR B 1 C16A C 0.7172(10) 0.1423(9) 0.5041(7) 0.121(7) Uiso 0.50 1 d PG B 1 H16A H 0.7317 0.1926 0.5058 0.146 Uiso 0.50 1 calc PR B 1 C17A C 0.7608(10) 0.1019(12) 0.4592(7) 0.088(7) Uiso 0.50 1 d PG B 1 C18A C 0.7393(13) 0.0284(12) 0.4569(7) 0.160(15) Uiso 0.50 1 d PG B 1 H18A H 0.7691 0.0004 0.4262 0.192 Uiso 0.50 1 calc PR B 1 C9B C 0.3854(6) -0.0270(7) 0.6484(4) 0.060(5) Uiso 0.50 1 d PG B 2 N3B N 0.5380(5) -0.0659(6) 0.5990(5) 0.082(4) Uiso 0.50 1 d PG B 2 C10B C 0.3777(6) 0.0624(6) 0.6182(5) 0.098(6) Uiso 0.50 1 d PG B 2 H10B H 0.3231 0.1068 0.6247 0.118 Uiso 0.50 1 calc PR B 2 C11B C 0.4498(7) 0.0864(5) 0.5787(5) 0.094(5) Uiso 0.50 1 d PG B 2 H11B H 0.4440 0.1472 0.5581 0.113 Uiso 0.50 1 calc PR B 2 C12B C 0.5299(6) 0.0227(6) 0.5690(4) 0.047(3) Uiso 0.50 1 d PG B 2 C13B C 0.4660(7) -0.0906(5) 0.6387(4) 0.066(4) Uiso 0.50 1 d PG B 2 H13B H 0.4723 -0.1515 0.6592 0.079 Uiso 0.50 1 calc PR B 2 C14B C 0.6052(5) 0.0432(5) 0.5297(4) 0.051(3) Uiso 0.50 1 d PG B 2 N4B N 0.6020(5) 0.1329(5) 0.5127(4) 0.075(3) Uiso 0.50 1 d PG B 2 C15B C 0.6783(5) -0.0154(4) 0.5066(4) 0.031(3) Uiso 0.50 1 d PG B 2 H15B H 0.6815 -0.0765 0.5180 0.037 Uiso 0.50 1 calc PR B 2 C16B C 0.7474(5) 0.0146(5) 0.4667(4) 0.041(3) Uiso 0.50 1 d PG B 2 H16B H 0.7972 -0.0261 0.4510 0.049 Uiso 0.50 1 calc PR B 2 C17B C 0.7438(6) 0.1036(6) 0.4497(4) 0.044(4) Uiso 0.50 1 d PG B 2 C18B C 0.6712(6) 0.1624(4) 0.4728(4) 0.071(4) Uiso 0.50 1 d PG B 2 H18B H 0.6685 0.2234 0.4613 0.085 Uiso 0.50 1 calc PR B 2 C19 C 0.8176(5) 0.1397(5) 0.4074(3) 0.0687(19) Uiso 1 1 d . . . H19A H 0.8508 0.1712 0.4206 0.082 Uiso 1 1 calc R B 1 H19B H 0.8638 0.0906 0.3939 0.082 Uiso 1 1 calc R B 1 C20 C 0.8176(4) 0.2460(4) 0.3090(3) 0.0485(15) Uani 1 1 d . . . C21 C 0.9081(4) 0.2456(5) 0.3097(3) 0.0602(18) Uani 1 1 d . B . H21 H 0.9396 0.2137 0.3449 0.072 Uiso 1 1 calc R . . C22 C 0.9505(4) 0.2925(5) 0.2585(3) 0.0557(17) Uani 1 1 d . . . H22 H 1.0116 0.2918 0.2592 0.067 Uiso 1 1 calc R B . C23 C 0.9074(4) 0.3406(4) 0.2060(3) 0.0475(15) Uani 1 1 d . B . C24 C 0.8172(4) 0.3412(4) 0.2067(2) 0.0421(13) Uani 1 1 d . . . H24 H 0.7861 0.3735 0.1715 0.050 Uiso 1 1 calc R B . C25 C 0.7709(4) 0.2954(4) 0.2579(2) 0.0417(13) Uani 1 1 d . B . C26 C 0.6749(4) 0.2935(4) 0.2579(2) 0.0418(13) Uani 1 1 d . . . H26A H 0.6769 0.2347 0.2553 0.050 Uiso 1 1 calc R B . H26B H 0.6402 0.3008 0.2968 0.050 Uiso 1 1 calc R . . C27 C -0.0980(5) 0.0290(5) 0.8324(3) 0.0654(19) Uani 1 1 d . . . C28 C -0.1698(5) 0.1049(6) 0.7942(5) 0.092(3) Uani 1 1 d . . . H28A H -0.2300 0.1113 0.8173 0.138 Uiso 1 1 calc R . . H28B H -0.1716 0.0914 0.7569 0.138 Uiso 1 1 calc R . . H28C H -0.1535 0.1604 0.7842 0.138 Uiso 1 1 calc R . . C29 C -0.1253(6) -0.0559(6) 0.8471(5) 0.092(3) Uani 1 1 d . . . H29A H -0.0818 -0.1048 0.8727 0.138 Uiso 1 1 calc R . . H29B H -0.1250 -0.0697 0.8095 0.138 Uiso 1 1 calc R . . H29C H -0.1868 -0.0478 0.8685 0.138 Uiso 1 1 calc R . . C30 C -0.0992(6) 0.0504(7) 0.8921(4) 0.089(3) Uani 1 1 d . . . H30A H -0.0554 0.0016 0.9176 0.134 Uiso 1 1 calc R . . H30B H -0.1607 0.0577 0.9134 0.134 Uiso 1 1 calc R . . H30C H -0.0823 0.1054 0.8830 0.134 Uiso 1 1 calc R . . C31 C 0.9608(4) 0.3862(5) 0.1491(3) 0.0514(16) Uani 1 1 d . . . C32 C 1.0423(5) 0.3152(6) 0.1306(4) 0.077(2) Uani 1 1 d . B . H32A H 1.0773 0.3432 0.0947 0.116 Uiso 1 1 calc R . . H32B H 1.0205 0.2721 0.1216 0.116 Uiso 1 1 calc R . . H32C H 1.0816 0.2848 0.1638 0.116 Uiso 1 1 calc R . . C33 C 0.9962(5) 0.4526(5) 0.1640(3) 0.0620(18) Uani 1 1 d . B . H33A H 0.9443 0.4982 0.1762 0.093 Uiso 1 1 calc R . . H33B H 1.0314 0.4805 0.1283 0.093 Uiso 1 1 calc R . . H33C H 1.0354 0.4212 0.1972 0.093 Uiso 1 1 calc R . . C34 C 0.9017(5) 0.4353(5) 0.0961(3) 0.0613(18) Uani 1 1 d . B . H34A H 0.9361 0.4682 0.0624 0.092 Uiso 1 1 calc R . . H34B H 0.8460 0.4768 0.1088 0.092 Uiso 1 1 calc R . . H34C H 0.8853 0.3923 0.0830 0.092 Uiso 1 1 calc R . . C35 C 0.1118(4) 0.3341(4) 0.7067(2) 0.0474(15) Uani 1 1 d . . . H35A H 0.0637 0.3907 0.6934 0.057 Uiso 1 1 calc R . . H35B H 0.1625 0.3321 0.6740 0.057 Uiso 1 1 calc R . . C36 C 0.1469(4) 0.3327(4) 0.7630(3) 0.0464(14) Uani 1 1 d . . . C37 C 0.1209(4) 0.2847(4) 0.8203(3) 0.0485(15) Uani 1 1 d . . . H37 H 0.0807 0.2505 0.8242 0.058 Uiso 1 1 calc R . . C38 C 0.1513(5) 0.2844(5) 0.8730(3) 0.0561(17) Uani 1 1 d . . . C39 C 0.2094(5) 0.3352(5) 0.8658(3) 0.0652(19) Uani 1 1 d . . . H39 H 0.2322 0.3357 0.9004 0.078 Uiso 1 1 calc R . . C40 C 0.2357(5) 0.3861(5) 0.8088(3) 0.0631(18) Uani 1 1 d . . . H40 H 0.2751 0.4211 0.8051 0.076 Uiso 1 1 calc R . . C41 C 0.2036(4) 0.3853(4) 0.7570(3) 0.0501(15) Uani 1 1 d . . . C42 C 0.2749(5) 0.4918(5) 0.6900(3) 0.0637(18) Uiso 1 1 d . . . H42A H 0.3305 0.4615 0.7118 0.076 Uiso 1 1 calc R C 1 H42B H 0.2386 0.5431 0.7053 0.076 Uiso 1 1 calc R C 1 N5A N 0.3343(7) 0.6362(5) 0.5353(4) 0.077(3) Uiso 0.50 1 d PG D 1 C47A C 0.3083(6) 0.6078(5) 0.5967(4) 0.080(4) Uiso 0.50 1 d PG D 1 H47A H 0.2959 0.6468 0.6211 0.096 Uiso 0.50 1 calc PR D 1 C43A C 0.3004(6) 0.5222(5) 0.6226(3) 0.028(2) Uiso 0.50 1 d PG D 1 C44A C 0.3186(6) 0.4651(5) 0.5869(4) 0.070(4) Uiso 0.50 1 d PG D 1 H44A H 0.3133 0.4066 0.6046 0.085 Uiso 0.50 1 calc PR D 1 C45A C 0.3447(7) 0.4935(7) 0.5255(4) 0.069(4) Uiso 0.50 1 d PG D 1 H45A H 0.3571 0.4544 0.5011 0.083 Uiso 0.50 1 calc PR D 1 C46A C 0.3525(7) 0.5790(7) 0.4997(3) 0.083(8) Uiso 0.50 1 d PG D 1 N5B N 0.2543(6) 0.6338(7) 0.5267(4) 0.081(4) Uiso 0.50 1 d PG D 2 C47B C 0.2327(6) 0.6055(9) 0.5887(4) 0.089(5) Uiso 0.50 1 d PG D 2 H47B H 0.1736 0.6304 0.6062 0.107 Uiso 0.50 1 calc PR D 2 C43B C 0.2976(9) 0.5407(10) 0.6251(3) 0.090 Uiso 0.50 1 d PG D 2 C44B C 0.3840(8) 0.5042(9) 0.5995(5) 0.112(7) Uiso 0.50 1 d PG D 2 H44B H 0.4283 0.4599 0.6244 0.134 Uiso 0.50 1 calc PR D 2 C45B C 0.4056(5) 0.5325(9) 0.5375(5) 0.115(7) Uiso 0.50 1 d PG D 2 H45B H 0.4647 0.5075 0.5200 0.138 Uiso 0.50 1 calc PR D 2 C46B C 0.3407(6) 0.5973(7) 0.5010(3) 0.028(3) Uiso 0.50 1 d PG D 2 C48A C 0.3827(9) 0.6144(8) 0.4387(3) 0.063(5) Uiso 0.50 1 d PG D 1 N6A N 0.4219(8) 0.6847(8) 0.4149(4) 0.105(5) Uiso 0.50 1 d PG D 1 C49A C 0.3697(8) 0.5728(7) 0.3999(5) 0.082(5) Uiso 0.50 1 d PG D 1 H49A H 0.3436 0.5248 0.4155 0.099 Uiso 0.50 1 calc PR D 1 C50A C 0.3946(9) 0.6010(8) 0.3380(4) 0.097(5) Uiso 0.50 1 d PG D 1 H50A H 0.3852 0.5721 0.3118 0.116 Uiso 0.50 1 calc PR D 1 C51A C 0.4329(9) 0.6708(8) 0.3146(3) 0.066(4) Uiso 0.50 1 d PG D 1 C52A C 0.4464(8) 0.7124(7) 0.3530(5) 0.082(5) Uiso 0.50 1 d PG D 1 H52A H 0.4726 0.7603 0.3371 0.099 Uiso 0.50 1 calc PR D 1 C48B C 0.3568(7) 0.6295(6) 0.4354(3) 0.029(3) Uiso 0.50 1 d PG D 2 N6B N 0.2928(6) 0.6899(7) 0.3968(4) 0.109(5) Uiso 0.50 1 d PG D 2 C49B C 0.4435(7) 0.5898(8) 0.4106(4) 0.108(6) Uiso 0.50 1 d PG D 2 H49B H 0.4879 0.5479 0.4365 0.129 Uiso 0.50 1 calc PR D 2 C50B C 0.4649(6) 0.6117(8) 0.3483(4) 0.125(8) Uiso 0.50 1 d PG D 2 H50B H 0.5240 0.5847 0.3318 0.149 Uiso 0.50 1 calc PR D 2 C51B C 0.4009(7) 0.6722(6) 0.3101(3) 0.036(3) Uiso 0.50 1 d PG D 2 C52B C 0.3147(6) 0.7113(7) 0.3343(4) 0.079(4) Uiso 0.50 1 d PG D 2 H52B H 0.2704 0.7529 0.3083 0.094 Uiso 0.50 1 calc PR D 2 C53 C 0.4423(6) 0.6943(6) 0.2454(4) 0.082(2) Uiso 1 1 d . . . H53A H 0.3819 0.7138 0.2297 0.098 Uiso 1 1 calc R D 1 H53B H 0.4728 0.7418 0.2271 0.098 Uiso 1 1 calc R D 1 C54 C 0.5278(5) 0.6112(5) 0.1738(3) 0.0590(18) Uani 1 1 d . . . C55 C 0.5147(6) 0.6869(5) 0.1238(3) 0.077(2) Uani 1 1 d . D . H55 H 0.4818 0.7436 0.1291 0.092 Uiso 1 1 calc R . . C56 C 0.5504(6) 0.6779(5) 0.0668(3) 0.075(2) Uani 1 1 d . . . H56 H 0.5418 0.7293 0.0331 0.090 Uiso 1 1 calc R D . C57 C 0.5985(5) 0.5957(5) 0.0573(3) 0.0565(17) Uani 1 1 d . D . C58 C 0.6100(4) 0.5220(4) 0.1085(3) 0.0474(14) Uani 1 1 d . . . H58 H 0.6429 0.4652 0.1034 0.057 Uiso 1 1 calc R D . C59 C 0.5756(4) 0.5285(4) 0.1664(2) 0.0450(14) Uani 1 1 d . B . C60 C 0.5930(4) 0.4483(4) 0.2216(2) 0.0438(14) Uani 1 1 d . . . H60A H 0.6386 0.4525 0.2438 0.053 Uiso 1 1 calc R B . H60B H 0.5356 0.4503 0.2486 0.053 Uiso 1 1 calc R . . C61 C 0.1201(6) 0.2316(6) 0.9362(3) 0.076(2) Uani 1 1 d . . . C62 C 0.0580(6) 0.1768(6) 0.9338(3) 0.081(2) Uani 1 1 d . . . H62A H 0.0892 0.1385 0.9075 0.121 Uiso 1 1 calc R . . H62B H 0.0006 0.2171 0.9178 0.121 Uiso 1 1 calc R . . H62C H 0.0449 0.1401 0.9746 0.121 Uiso 1 1 calc R . . C63 C 0.2051(10) 0.1625(12) 0.9669(6) 0.173(8) Uani 1 1 d . . . H63A H 0.2403 0.1933 0.9783 0.260 Uiso 1 1 calc R . . H63B H 0.2435 0.1301 0.9385 0.260 Uiso 1 1 calc R . . H63C H 0.1851 0.1207 1.0030 0.260 Uiso 1 1 calc R . . C64 C 0.0629(12) 0.2968(10) 0.9720(5) 0.163(7) Uani 1 1 d . . . H64A H 0.0265 0.3501 0.9447 0.245 Uiso 1 1 calc R . . H64B H 0.1035 0.3132 0.9907 0.245 Uiso 1 1 calc R . . H64C H 0.0220 0.2688 1.0036 0.245 Uiso 1 1 calc R . . C65 C 0.6360(5) 0.5879(5) -0.0072(3) 0.066(2) Uani 1 1 d . . . C66 C 0.5588(8) 0.6239(9) -0.0470(4) 0.123(4) Uani 1 1 d . D . H66A H 0.5311 0.6873 -0.0507 0.184 Uiso 1 1 calc R . . H66B H 0.5127 0.5922 -0.0291 0.184 Uiso 1 1 calc R . . H66C H 0.5825 0.6158 -0.0871 0.184 Uiso 1 1 calc R . . C67 C 0.6832(8) 0.4916(7) -0.0065(4) 0.107(4) Uani 1 1 d . D . H67A H 0.6394 0.4569 0.0100 0.161 Uiso 1 1 calc R . . H67B H 0.7343 0.4675 0.0187 0.161 Uiso 1 1 calc R . . H67C H 0.7062 0.4886 -0.0478 0.161 Uiso 1 1 calc R . . C68 C 0.7045(11) 0.6402(13) -0.0317(5) 0.176(8) Uani 1 1 d . D . H68A H 0.7276 0.6471 0.0020 0.265 Uiso 1 1 calc R . . H68B H 0.6751 0.6988 -0.0576 0.265 Uiso 1 1 calc R . . H68C H 0.7555 0.6086 -0.0553 0.265 Uiso 1 1 calc R . . C69 C 0.0188(4) 0.2796(4) 0.6658(3) 0.0502(15) Uani 1 1 d . . . H69A H 0.0064 0.2245 0.6666 0.060 Uiso 1 1 calc R . . H69B H 0.0535 0.2999 0.6266 0.060 Uiso 1 1 calc R . . C70 C -0.0718(4) 0.3508(4) 0.6709(3) 0.0510(15) Uani 1 1 d . . . C71 C -0.1140(4) 0.3609(4) 0.7269(3) 0.0502(15) Uani 1 1 d . . . H71 H -0.0861 0.3219 0.7622 0.060 Uiso 1 1 calc R . . C72 C -0.1956(4) 0.4261(5) 0.7331(3) 0.0582(17) Uani 1 1 d . . . C73 C -0.2339(6) 0.4806(6) 0.6799(4) 0.085(3) Uani 1 1 d . . . H73 H -0.2893 0.5263 0.6823 0.102 Uiso 1 1 calc R . . C74 C -0.1940(6) 0.4707(7) 0.6235(4) 0.100(4) Uani 1 1 d . . . H74 H -0.2219 0.5092 0.5881 0.120 Uiso 1 1 calc R . . C75 C -0.1139(5) 0.4050(6) 0.6194(3) 0.074(2) Uani 1 1 d . . . C76 C -0.1028(6) 0.4416(6) 0.5093(4) 0.079(2) Uiso 1 1 d . . . H76A H -0.1126 0.5056 0.5036 0.095 Uiso 1 1 calc R E 1 H76B H -0.1615 0.4321 0.5072 0.095 Uiso 1 1 calc R E 1 C77A C -0.0281(7) 0.4079(7) 0.4609(3) 0.051(4) Uiso 0.50 1 d PG F 1 N7A N 0.0171(6) 0.4000(6) 0.3583(3) 0.065(3) Uiso 0.50 1 d PG F 1 C78A C 0.0530(8) 0.3419(7) 0.4783(3) 0.107(6) Uiso 0.50 1 d PG F 1 H78A H 0.0656 0.3215 0.5194 0.128 Uiso 0.50 1 calc PR F 1 C79A C 0.1152(6) 0.3063(7) 0.4355(4) 0.068(4) Uiso 0.50 1 d PG F 1 H79A H 0.1702 0.2618 0.4475 0.082 Uiso 0.50 1 calc PR F 1 C80A C 0.0975(6) 0.3350(7) 0.3756(4) 0.089(7) Uiso 0.50 1 d PG F 1 C81A C -0.0455(5) 0.4362(6) 0.4009(3) 0.049(3) Uiso 0.50 1 d PG F 1 H81A H -0.1005 0.4806 0.3886 0.059 Uiso 0.50 1 calc PR F 1 C77B C -0.0511(6) 0.4053(6) 0.4619(4) 0.064(5) Uiso 0.50 1 d PG F 2 N7B N 0.0396(6) 0.2765(4) 0.4288(4) 0.071(3) Uiso 0.50 1 d PG F 2 C78B C -0.0113(7) 0.4579(4) 0.4124(4) 0.065(4) Uiso 0.50 1 d PG F 2 H78B H -0.0285 0.5203 0.4064 0.078 Uiso 0.50 1 calc PR F 2 C79B C 0.0537(6) 0.4202(5) 0.3715(3) 0.061(3) Uiso 0.50 1 d PG F 2 H79B H 0.0807 0.4569 0.3378 0.073 Uiso 0.50 1 calc PR F 2 C80B C 0.0792(5) 0.3294(5) 0.3797(3) 0.033(3) Uiso 0.50 1 d PG F 2 C81B C -0.0255(6) 0.3136(6) 0.4698(4) 0.075(4) Uiso 0.50 1 d PG F 2 H81B H -0.0525 0.2767 0.5033 0.090 Uiso 0.50 1 calc PR F 2 C82A C 0.1649(6) 0.2898(6) 0.3378(3) 0.034(3) Uiso 0.50 1 d PG F 1 N8A N 0.1535(5) 0.3178(6) 0.2767(3) 0.057(3) Uiso 0.50 1 d PG F 1 C83A C 0.2453(7) 0.2252(7) 0.3580(3) 0.080(4) Uiso 0.50 1 d PG F 1 H83A H 0.2539 0.2050 0.3998 0.096 Uiso 0.50 1 calc PR F 1 C84A C 0.3128(5) 0.1906(7) 0.3170(4) 0.083(5) Uiso 0.50 1 d PG F 1 H84A H 0.3674 0.1470 0.3310 0.099 Uiso 0.50 1 calc PR F 1 C85A C 0.3011(5) 0.2191(7) 0.2561(4) 0.052(4) Uiso 0.50 1 d PG F 1 C86A C 0.2214(6) 0.2826(6) 0.2359(3) 0.055(3) Uiso 0.50 1 d PG F 1 H86A H 0.2130 0.3024 0.1941 0.066 Uiso 0.50 1 calc PR F 1 C82B C 0.1450(5) 0.2808(6) 0.3441(4) 0.073(6) Uiso 0.50 1 d PG F 2 N8B N 0.1705(6) 0.3314(4) 0.2876(4) 0.051(3) Uiso 0.50 1 d PG F 2 C83B C 0.1961(6) 0.1921(5) 0.3648(3) 0.055(3) Uiso 0.50 1 d PG F 2 H83B H 0.1791 0.1564 0.4032 0.066 Uiso 0.50 1 calc PR F 2 C84B C 0.2717(6) 0.1559(4) 0.3290(4) 0.058(3) Uiso 0.50 1 d PG F 2 H84B H 0.3063 0.0957 0.3434 0.069 Uiso 0.50 1 calc PR F 2 C85B C 0.2969(5) 0.2068(5) 0.2728(4) 0.049(4) Uiso 0.50 1 d PG F 2 C86B C 0.2463(6) 0.2945(5) 0.2521(3) 0.060(3) Uiso 0.50 1 d PG F 2 H86B H 0.2632 0.3298 0.2134 0.072 Uiso 0.50 1 calc PR F 2 C87 C 0.3780(5) 0.1789(6) 0.2232(4) 0.079(2) Uiso 1 1 d . . . H87A H 0.3622 0.1798 0.1841 0.095 Uiso 1 1 calc R F 1 H87B H 0.4052 0.1166 0.2461 0.095 Uiso 1 1 calc R F 1 C88 C 0.5207(4) 0.2089(4) 0.1788(3) 0.0495(15) Uani 1 1 d . . . C89 C 0.5479(5) 0.1391(5) 0.1529(4) 0.069(2) Uani 1 1 d . F . H89 H 0.5104 0.1011 0.1602 0.082 Uiso 1 1 calc R . . C90 C 0.6289(5) 0.1248(5) 0.1169(3) 0.067(2) Uani 1 1 d . . . H90 H 0.6463 0.0769 0.0994 0.081 Uiso 1 1 calc R F . C91 C 0.6863(4) 0.1788(5) 0.1052(3) 0.0544(16) Uani 1 1 d . F . C92 C 0.6587(4) 0.2462(4) 0.1329(3) 0.0477(15) Uani 1 1 d . . . H92 H 0.6972 0.2830 0.1266 0.057 Uiso 1 1 calc R F . C93 C 0.5777(4) 0.2623(4) 0.1695(2) 0.0421(13) Uani 1 1 d . B . C94 C 0.5483(4) 0.3390(4) 0.1977(3) 0.0422(13) Uani 1 1 d . . . H94A H 0.5087 0.3914 0.1707 0.051 Uiso 1 1 calc R B . H94B H 0.5117 0.3225 0.2367 0.051 Uiso 1 1 calc R . . C95 C -0.2355(4) 0.4340(5) 0.7962(3) 0.0592(18) Uani 1 1 d . . . C96 C -0.2519(7) 0.3451(7) 0.8370(4) 0.104(3) Uani 1 1 d . . . H96A H -0.2788 0.3515 0.8771 0.156 Uiso 1 1 calc R . . H96B H -0.1935 0.2983 0.8407 0.156 Uiso 1 1 calc R . . H96C H -0.2937 0.3293 0.8189 0.156 Uiso 1 1 calc R . . C97 C -0.1671(5) 0.4549(6) 0.8239(3) 0.067(2) Uani 1 1 d . . . H97A H -0.1912 0.4586 0.8650 0.100 Uiso 1 1 calc R . . H97B H -0.1571 0.5118 0.7992 0.100 Uiso 1 1 calc R . . H97C H -0.1090 0.4079 0.8253 0.100 Uiso 1 1 calc R . . C98 C -0.3265(5) 0.5084(8) 0.7950(4) 0.098(3) Uani 1 1 d . . . H98A H -0.3166 0.5650 0.7696 0.148 Uiso 1 1 calc R . . H98B H -0.3489 0.5125 0.8361 0.148 Uiso 1 1 calc R . . H98C H -0.3717 0.4949 0.7783 0.148 Uiso 1 1 calc R . . C99 C 0.7723(5) 0.1655(5) 0.0608(3) 0.072(2) Uani 1 1 d . . . C100 C 0.7422(8) 0.1999(8) -0.0038(4) 0.130(5) Uani 1 1 d . F . H100 H 0.7051 0.1646 -0.0078 0.195 Uiso 1 1 calc R . . H200 H 0.7963 0.1946 -0.0331 0.195 Uiso 1 1 calc R . . H300 H 0.7059 0.2623 -0.0115 0.195 Uiso 1 1 calc R . . C101 C 0.8273(5) 0.0666(5) 0.0744(4) 0.076(2) Uani 1 1 d . F . H101 H 0.7890 0.0320 0.0712 0.114 Uiso 1 1 calc R . . H201 H 0.8464 0.0456 0.1153 0.114 Uiso 1 1 calc R . . H301 H 0.8814 0.0594 0.0452 0.114 Uiso 1 1 calc R . . C102 C 0.8364(6) 0.2174(6) 0.0662(4) 0.095(3) Uani 1 1 d . F . H102 H 0.8932 0.2040 0.0401 0.143 Uiso 1 1 calc R . . H202 H 0.8505 0.1994 0.1082 0.143 Uiso 1 1 calc R . . H303 H 0.8058 0.2812 0.0538 0.143 Uiso 1 1 calc R . . C103 C 0.9340(5) -0.0356(6) 0.5868(5) 0.109(6) Uiso 0.50 1 d PG G -1 C104 C 0.9318(5) -0.0061(7) 0.6364(4) 0.107(6) Uiso 0.50 1 d PG G -1 H104 H 0.9051 -0.0333 0.6747 0.128 Uiso 0.50 1 calc PR G -1 C105 C 0.9680(5) 0.0622(8) 0.6307(4) 0.097(6) Uiso 0.50 1 d PG G -1 H105 H 0.9660 0.0815 0.6649 0.117 Uiso 0.50 1 calc PR G -1 C106 C 1.0070(5) 0.1026(7) 0.5753(5) 0.128(8) Uiso 0.50 1 d PG G -1 H106 H 1.0321 0.1493 0.5714 0.154 Uiso 0.50 1 calc PR G -1 C107 C 1.0091(4) 0.0746(7) 0.5256(4) 0.092(5) Uiso 0.50 1 d PG G -1 H107 H 1.0354 0.1024 0.4874 0.111 Uiso 0.50 1 calc PR G -1 C108 C 0.9729(4) 0.0060(7) 0.5313(4) 0.091(5) Uiso 0.50 1 d PG G -1 H108 H 0.9747 -0.0127 0.4968 0.110 Uiso 0.50 1 calc PR G -1 C109 C 0.8978(6) -0.1123(5) 0.5934(6) 0.209(16) Uiso 0.50 1 d PG G -1 H109 H 0.8314 -0.0908 0.5918 0.313 Uiso 0.50 1 calc PR G -1 H209 H 0.9122 -0.1567 0.6322 0.313 Uiso 0.50 1 calc PR G -1 H309 H 0.9263 -0.1392 0.5604 0.313 Uiso 0.50 1 calc PR G -1 C110 C 0.3878(6) 0.3253(6) 0.4425(8) 0.114(7) Uiso 0.50 1 d PR . . C111 C 0.3794(6) 0.3586(6) 0.4913(8) 0.124(8) Uiso 0.50 1 d PR . . H111 H 0.4210 0.3893 0.4920 0.149 Uiso 0.50 1 calc PR . . C112 C 0.3106(5) 0.3481(8) 0.5398(5) 0.141(9) Uiso 0.50 1 d PG . . H112 H 0.3066 0.3710 0.5727 0.169 Uiso 0.50 1 calc PR . . C113 C 0.2492(4) 0.3044(9) 0.5389(5) 0.150(10) Uiso 0.50 1 d PG . . H113 H 0.2023 0.2976 0.5710 0.180 Uiso 0.50 1 calc PR . . C114 C 0.2567(5) 0.2706(7) 0.4912(6) 0.133(8) Uiso 0.50 1 d PG . . H114 H 0.2150 0.2402 0.4905 0.160 Uiso 0.50 1 calc PR . . C115 C 0.3249(5) 0.2810(7) 0.4441(5) 0.098(6) Uiso 0.50 1 d PG . . H115 H 0.3289 0.2570 0.4117 0.117 Uiso 0.50 1 calc PR . . C116 C 0.4587(5) 0.3394(7) 0.3919(4) 0.078(4) Uiso 0.50 1 d PG . . H116 H 0.4503 0.3179 0.3597 0.117 Uiso 0.50 1 calc PR . . H216 H 0.5192 0.3069 0.4061 0.117 Uiso 0.50 1 calc PR . . H316 H 0.4537 0.4029 0.3762 0.117 Uiso 0.50 1 calc PR . . C117 C 0.5636(8) 0.0905(9) 0.7502(5) 0.098(6) Uiso 0.50 1 d PG . . C118 C 0.5473(8) 0.0684(10) 0.8130(5) 0.123(7) Uiso 0.50 1 d PG . . H118 H 0.5950 0.0287 0.8371 0.147 Uiso 0.50 1 calc PR . . C119 C 0.4627(9) 0.1033(11) 0.8408(5) 0.103(6) Uiso 0.50 1 d PG . . H119 H 0.4527 0.0875 0.8837 0.124 Uiso 0.50 1 calc PR . . C120 C 0.3925(8) 0.1612(11) 0.8065(7) 0.121(7) Uiso 0.50 1 d PG . . H120 H 0.3343 0.1849 0.8256 0.145 Uiso 0.50 1 calc PR . . C121 C 0.4077(9) 0.1843(13) 0.7443(7) 0.146 Uiso 0.50 1 d PG . . H121 H 0.3598 0.2243 0.7205 0.175 Uiso 0.50 1 calc PR . . C122 C 0.4926(10) 0.1493(12) 0.7163(5) 0.170 Uiso 0.50 1 d PG . . H122 H 0.5022 0.1656 0.6734 0.204 Uiso 0.50 1 calc PR . . C123 C 0.6547(10) 0.0500(15) 0.7197(8) 0.155(10) Uiso 0.50 1 d PG . . H123 H 0.6458 0.0458 0.6807 0.232 Uiso 0.50 1 calc PR . . H223 H 0.6823 -0.0095 0.7454 0.232 Uiso 0.50 1 calc PR . . H323 H 0.6951 0.0873 0.7133 0.232 Uiso 0.50 1 calc PR . . O100 O 0.4637(17) 0.0673(18) 0.0184(11) 0.095(7) Uiso 0.25 1 d P H 1 O200 O 0.584(2) 0.013(2) -0.0164(14) 0.121(9) Uiso 0.25 1 d P I 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 O1 0.061(3) 0.037(3) 0.071(3) -0.017(2) 0.011(2) -0.016(2) O2 0.047(2) 0.056(3) 0.050(2) 0.0055(19) 0.0005(18) -0.024(2) O3 0.080(3) 0.066(3) 0.044(2) -0.021(2) 0.013(2) -0.043(2) O4 0.121(4) 0.035(3) 0.048(3) -0.0140(19) 0.009(2) -0.020(3) O5 0.111(4) 0.088(4) 0.036(2) -0.016(2) -0.015(3) 0.029(3) O6 0.047(2) 0.057(3) 0.091(3) -0.040(2) 0.004(2) -0.023(2) N1 0.056(3) 0.035(3) 0.040(3) -0.011(2) 0.001(2) -0.013(2) N2 0.043(3) 0.040(3) 0.041(3) -0.015(2) 0.002(2) -0.016(2) C1 0.056(3) 0.036(3) 0.043(3) -0.011(2) 0.002(3) -0.011(3) C2 0.055(4) 0.040(4) 0.045(3) -0.014(3) -0.005(3) -0.012(3) C3 0.055(4) 0.040(4) 0.051(4) -0.012(3) -0.003(3) -0.007(3) C4 0.056(4) 0.045(4) 0.056(4) -0.011(3) -0.001(3) -0.018(3) C5 0.064(4) 0.039(4) 0.065(4) -0.015(3) 0.001(3) -0.020(3) C6 0.059(4) 0.040(4) 0.062(4) -0.019(3) 0.000(3) -0.014(3) C7 0.056(4) 0.038(4) 0.049(3) -0.010(3) 0.001(3) -0.016(3) C20 0.043(3) 0.048(4) 0.050(3) -0.008(3) 0.008(3) -0.020(3) C21 0.055(4) 0.067(5) 0.054(4) -0.004(3) -0.001(3) -0.026(3) C22 0.047(3) 0.065(5) 0.055(4) -0.010(3) 0.006(3) -0.028(3) C23 0.053(4) 0.047(4) 0.046(3) -0.015(3) 0.007(3) -0.022(3) C24 0.047(3) 0.042(4) 0.039(3) -0.015(2) 0.005(2) -0.016(3) C25 0.050(3) 0.040(3) 0.039(3) -0.016(2) 0.009(2) -0.019(3) C26 0.044(3) 0.042(4) 0.042(3) -0.011(2) 0.004(2) -0.020(3) C27 0.066(4) 0.045(4) 0.078(5) -0.015(3) 0.010(4) -0.018(3) C28 0.058(5) 0.076(6) 0.129(8) -0.011(5) -0.006(5) -0.022(4) C29 0.077(5) 0.065(6) 0.122(7) -0.023(5) 0.030(5) -0.030(4) C30 0.083(6) 0.096(7) 0.089(6) -0.044(5) 0.031(5) -0.031(5) C31 0.057(4) 0.057(4) 0.047(3) -0.018(3) 0.014(3) -0.032(3) C32 0.072(5) 0.084(6) 0.069(5) -0.025(4) 0.031(4) -0.032(4) C33 0.061(4) 0.077(5) 0.056(4) -0.012(3) 0.009(3) -0.043(4) C34 0.076(4) 0.073(5) 0.042(3) -0.011(3) 0.011(3) -0.046(4) C35 0.058(4) 0.038(3) 0.040(3) -0.011(2) 0.009(3) -0.014(3) C36 0.056(3) 0.040(4) 0.042(3) -0.017(3) 0.013(3) -0.015(3) C37 0.057(4) 0.043(4) 0.042(3) -0.015(3) 0.010(3) -0.016(3) C38 0.070(4) 0.057(4) 0.042(3) -0.018(3) 0.011(3) -0.025(3) C39 0.082(5) 0.082(6) 0.039(3) -0.028(3) 0.007(3) -0.029(4) C40 0.078(5) 0.067(5) 0.055(4) -0.030(3) 0.014(3) -0.035(4) C41 0.064(4) 0.049(4) 0.040(3) -0.019(3) 0.016(3) -0.026(3) C54 0.089(5) 0.045(4) 0.041(3) -0.010(3) 0.008(3) -0.027(3) C55 0.116(6) 0.042(4) 0.059(4) -0.010(3) 0.016(4) -0.022(4) C56 0.114(6) 0.057(5) 0.046(4) -0.003(3) 0.003(4) -0.031(4) C57 0.063(4) 0.057(4) 0.046(4) -0.014(3) 0.004(3) -0.018(3) C58 0.051(3) 0.048(4) 0.046(3) -0.015(3) -0.003(3) -0.017(3) C59 0.051(3) 0.044(4) 0.043(3) -0.013(3) 0.002(3) -0.019(3) C60 0.056(3) 0.040(3) 0.042(3) -0.015(2) 0.000(3) -0.021(3) C61 0.115(6) 0.078(6) 0.041(4) -0.014(3) 0.005(4) -0.047(5) C62 0.107(6) 0.077(6) 0.052(4) -0.014(4) 0.024(4) -0.041(5) C63 0.164(12) 0.225(18) 0.096(8) 0.068(10) -0.046(8) -0.104(12) C64 0.294(18) 0.162(12) 0.075(7) -0.070(7) 0.100(9) -0.148(13) C65 0.071(4) 0.082(6) 0.039(3) -0.013(3) 0.002(3) -0.022(4) C66 0.136(9) 0.139(10) 0.071(6) -0.045(6) -0.033(6) 0.017(7) C67 0.129(8) 0.105(8) 0.052(5) -0.025(4) 0.010(5) 0.008(6) C68 0.212(15) 0.30(2) 0.083(7) -0.090(10) 0.088(9) -0.182(16) C69 0.060(4) 0.043(4) 0.042(3) -0.015(3) 0.003(3) -0.008(3) C70 0.063(4) 0.043(4) 0.044(3) -0.018(3) -0.002(3) -0.008(3) C71 0.057(4) 0.050(4) 0.043(3) -0.013(3) -0.004(3) -0.016(3) C72 0.051(4) 0.064(5) 0.058(4) -0.027(3) -0.002(3) -0.006(3) C73 0.074(5) 0.093(6) 0.070(5) -0.039(4) -0.017(4) 0.020(4) C74 0.098(6) 0.106(7) 0.057(5) -0.022(4) -0.029(4) 0.035(5) C75 0.083(5) 0.075(5) 0.045(4) -0.022(3) -0.009(3) 0.009(4) C88 0.051(3) 0.045(4) 0.060(4) -0.021(3) -0.011(3) -0.013(3) C89 0.060(4) 0.061(5) 0.105(6) -0.052(4) -0.005(4) -0.018(3) C90 0.071(5) 0.059(5) 0.082(5) -0.043(4) -0.010(4) -0.008(4) C91 0.062(4) 0.051(4) 0.049(4) -0.020(3) -0.004(3) -0.010(3) C92 0.055(4) 0.044(4) 0.043(3) -0.014(3) -0.003(3) -0.012(3) C93 0.047(3) 0.042(4) 0.038(3) -0.014(2) -0.003(2) -0.012(3) C94 0.043(3) 0.044(4) 0.046(3) -0.022(3) 0.005(2) -0.018(3) C95 0.047(3) 0.069(5) 0.059(4) -0.026(3) 0.007(3) -0.012(3) C96 0.121(8) 0.100(8) 0.099(7) -0.046(6) 0.050(6) -0.058(6) C97 0.057(4) 0.083(6) 0.065(4) -0.039(4) 0.005(3) -0.013(4) C98 0.053(4) 0.137(9) 0.102(7) -0.066(6) -0.003(4) 0.007(5) C99 0.077(5) 0.068(5) 0.059(4) -0.030(4) 0.011(4) -0.003(4) C100 0.140(9) 0.131(9) 0.058(5) -0.029(5) 0.010(5) 0.033(7) C101 0.065(4) 0.065(5) 0.096(6) -0.042(4) 0.006(4) -0.005(4) C102 0.086(6) 0.076(6) 0.117(7) -0.048(5) 0.060(5) -0.034(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 O1 C7 1.377(7) . ? O1 C8 1.420(8) . ? O2 C20 1.373(7) . ? O2 C19 1.430(8) . ? O3 C41 1.379(7) . ? O3 C42 1.400(9) . ? O4 C54 1.389(8) . ? O4 C53 1.444(10) . ? O5 C75 1.398(8) . ? O5 C76 1.413(9) . ? O6 C88 1.376(7) . ? O6 C87 1.433(9) . ? N1 C35 1.457(8) . ? N1 C1 1.473(7) . ? N1 C69 1.481(8) . ? N2 C60 1.463(7) . ? N2 C94 1.469(7) . ? N2 C26 1.475(7) . ? C1 C2 1.504(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.383(9) . ? C2 C7 1.415(9) . ? C3 C4 1.402(9) . ? C3 H3 0.9500 . ? C4 C5 1.386(9) . ? C4 C27 1.536(9) . ? C5 C6 1.389(9) . ? C5 H5 0.9500 . ? C6 C7 1.368(9) . ? C6 H6 0.9500 . ? C8 C9B 1.446(9) . ? C8 C9A 1.546(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9A C13A 1.3859 . ? C9A C10A 1.4000 . ? N3A C12A 1.3856 . ? N3A C13A 1.3950 . ? C10A C11A 1.3924 . ? C10A H10A 0.9500 . ? C11A C12A 1.3819 . ? C11A H11A 0.9500 . ? C12A C14A 1.438(12) . ? C13A H13A 0.9500 . ? C14A N4A 1.3859 . ? C14A C15A 1.4001 . ? N4A C18A 1.3949 . ? C15A C16A 1.3924 . ? C15A H15A 0.9500 . ? C16A C17A 1.3820 . ? C16A H16A 0.9500 . ? C17A C18A 1.3857 . ? C17A C19 1.455(13) . ? C18A H18A 0.9500 . ? C9B C13B 1.3859 . ? C9B C10B 1.4000 . ? N3B C12B 1.3857 . ? N3B C13B 1.3949 . ? C10B C11B 1.3924 . ? C10B H10B 0.9500 . ? C11B C12B 1.3820 . ? C11B H11B 0.9500 . ? C12B C14B 1.409(9) . ? C13B H13B 0.9500 . ? C14B C15B 1.3859 . ? C14B N4B 1.4000 . ? N4B C18B 1.3924 . ? C15B C16B 1.3949 . ? C15B H15B 0.9500 . ? C16B C17B 1.3857 . ? C16B H16B 0.9500 . ? C17B C18B 1.3820 . ? C17B C19 1.516(9) . ? C18B H18B 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.393(8) . ? C20 C21 1.411(9) . ? C21 C22 1.384(9) . ? C21 H21 0.9500 . ? C22 C23 1.391(9) . ? C22 H22 0.9500 . ? C23 C24 1.397(8) . ? C23 C31 1.543(8) . ? C24 C25 1.407(8) . ? C24 H24 0.9500 . ? C25 C26 1.504(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C29 1.520(11) . ? C27 C28 1.540(11) . ? C27 C30 1.550(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.527(10) . ? C31 C34 1.533(9) . ? C31 C33 1.538(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.516(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.385(8) . ? C36 C41 1.393(9) . ? C37 C38 1.405(9) . ? C37 H37 0.9500 . ? C38 C39 1.382(10) . ? C38 C61 1.540(9) . ? C39 C40 1.400(10) . ? C39 H39 0.9500 . ? C40 C41 1.404(9) . ? C40 H40 0.9500 . ? C42 C43B 1.513(10) . ? C42 C43A 1.516(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N5A C47A 1.3900 . ? N5A C46A 1.3900 . ? C47A C43A 1.3900 . ? C47A H47A 0.9500 . ? C43A C44A 1.3900 . ? C44A C45A 1.3900 . ? C44A H44A 0.9500 . ? C45A C46A 1.3900 . ? C45A H45A 0.9500 . ? C46A C48A 1.413(9) . ? N5B C47B 1.3900 . ? N5B C46B 1.3900 . ? C47B C43B 1.3900 . ? C47B H47B 0.9500 . ? C43B C44B 1.3900 . ? C44B C45B 1.3900 . ? C44B H44B 0.9500 . ? C45B C46B 1.3900 . ? C45B H45B 0.9500 . ? C46B C48B 1.461(9) . ? C48A C49A 1.3860 . ? C48A N6A 1.4000 . ? N6A C52A 1.3924 . ? C49A C50A 1.3949 . ? C49A H49A 0.9500 . ? C50A C51A 1.3857 . ? C50A H50A 0.9500 . ? C51A C52A 1.3820 . ? C51A C53 1.534(11) . ? C52A H52A 0.9500 . ? C48B N6B 1.3860 . ? C48B C49B 1.4000 . ? N6B C52B 1.3949 . ? C49B C50B 1.3924 . ? C49B H49B 0.9500 . ? C50B C51B 1.3820 . ? C50B H50B 0.9500 . ? C51B C52B 1.3856 . ? C51B C53 1.510(10) . ? C52B H52B 0.9500 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C59 1.382(9) . ? C54 C55 1.404(10) . ? C55 C56 1.385(10) . ? C55 H55 0.9500 . ? C56 C57 1.392(11) . ? C56 H56 0.9500 . ? C57 C58 1.400(9) . ? C57 C65 1.548(9) . ? C58 C59 1.389(8) . ? C58 H58 0.9500 . ? C59 C60 1.519(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C64 1.532(14) . ? C61 C62 1.549(12) . ? C61 C63 1.555(16) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C68 1.506(14) . ? C65 C66 1.506(12) . ? C65 C67 1.523(13) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.527(8) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C75 1.385(9) . ? C70 C71 1.390(8) . ? C71 C72 1.393(9) . ? C71 H71 0.9500 . ? C72 C73 1.391(10) . ? C72 C95 1.524(9) . ? C73 C74 1.389(11) . ? C73 H73 0.9500 . ? C74 C75 1.373(11) . ? C74 H74 0.9500 . ? C76 C77B 1.425(10) . ? C76 C77A 1.562(11) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77A C81A 1.3859 . ? C77A C78A 1.4001 . ? N7A C80A 1.3857 . ? N7A C81A 1.3949 . ? C78A C79A 1.3924 . ? C78A H78A 0.9500 . ? C79A C80A 1.3819 . ? C79A H79A 0.9500 . ? C80A C82A 1.420(9) . ? C81A H81A 0.9500 . ? C77B C78B 1.3859 . ? C77B C81B 1.4000 . ? N7B C80B 1.3820 . ? N7B C81B 1.3924 . ? C78B C79B 1.3949 . ? C78B H78B 0.9500 . ? C79B C80B 1.3857 . ? C79B H79B 0.9500 . ? C80B C82B 1.402(8) . ? C81B H81B 0.9500 . ? C82A N8A 1.3859 . ? C82A C83A 1.4000 . ? N8A C86A 1.3949 . ? C83A C84A 1.3924 . ? C83A H83A 0.9500 . ? C84A C85A 1.3820 . ? C84A H84A 0.9500 . ? C85A C86A 1.3857 . ? C85A C87 1.390(10) . ? C86A H86A 0.9500 . ? C82B N8B 1.3859 . ? C82B C83B 1.4000 . ? N8B C86B 1.3949 . ? C83B C84B 1.3924 . ? C83B H83B 0.9500 . ? C84B C85B 1.3820 . ? C84B H84B 0.9500 . ? C85B C86B 1.3857 . ? C85B C87 1.603(10) . ? C86B H86B 0.9500 . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.388(9) . ? C88 C93 1.393(9) . ? C89 C90 1.374(10) . ? C89 H89 0.9500 . ? C90 C91 1.397(10) . ? C90 H90 0.9500 . ? C91 C92 1.383(9) . ? C91 C99 1.534(9) . ? C92 C93 1.383(8) . ? C92 H92 0.9500 . ? C93 C94 1.523(8) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C97 1.527(10) . ? C95 C98 1.542(10) . ? C95 C96 1.549(12) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C99 C101 1.543(11) . ? C99 C100 1.544(12) . ? C99 C102 1.561(13) . ? C100 H100 0.9800 . ? C100 H200 0.9800 . ? C100 H300 0.9800 . ? C101 H101 0.9800 . ? C101 H201 0.9800 . ? C101 H301 0.9800 . ? C102 H102 0.9800 . ? C102 H202 0.9800 . ? C102 H303 0.9800 . ? C103 C108 1.3908 . ? C103 C104 1.3960 . ? C103 C109 1.5073 . ? C104 C105 1.3833 . ? C104 H104 0.9500 . ? C105 C106 1.3829 . ? C105 H105 0.9500 . ? C106 C107 1.3797 . ? C106 H106 0.9500 . ? C107 C108 1.3887 . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 H109 0.9800 . ? C109 H209 0.9800 . ? C109 H309 0.9800 . ? C110 C115 1.3929(14) . ? C110 C111 1.3957 . ? C110 C116 1.474(17) . ? C111 C112 1.415(17) . ? C111 H111 0.9500 . ? C112 C113 1.3829 . ? C112 H112 0.9500 . ? C113 C114 1.3797 . ? C113 H113 0.9500 . ? C114 C115 1.3886 . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 H116 0.9800 . ? C116 H216 0.9800 . ? C116 H316 0.9800 . ? C117 C122 1.3907 . ? C117 C118 1.3959 . ? C117 C123 1.5074 . ? C118 C119 1.3833 . ? C118 H118 0.9500 . ? C119 C120 1.3830 . ? C119 H119 0.9500 . ? C120 C121 1.3797 . ? C120 H120 0.9500 . ? C121 C122 1.3886 . ? C121 H121 0.9500 . ? C122 H122 0.9500 . ? C123 H123 0.9800 . ? C123 H223 0.9800 . ? C123 H323 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 O1 C8 118.1(5) . . ? C20 O2 C19 118.8(5) . . ? C41 O3 C42 117.7(5) . . ? C54 O4 C53 118.9(5) . . ? C75 O5 C76 120.6(6) . . ? C88 O6 C87 117.6(5) . . ? C35 N1 C1 111.0(5) . . ? C35 N1 C69 110.0(5) . . ? C1 N1 C69 109.8(5) . . ? C60 N2 C94 109.7(4) . . ? C60 N2 C26 110.4(4) . . ? C94 N2 C26 110.6(5) . . ? N1 C1 C2 113.2(5) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C7 117.7(6) . . ? C3 C2 C1 123.5(5) . . ? C7 C2 C1 118.8(5) . . ? C2 C3 C4 123.5(6) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C5 C4 C3 116.4(6) . . ? C5 C4 C27 123.5(6) . . ? C3 C4 C27 120.1(6) . . ? C4 C5 C6 121.7(6) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 120.7(6) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 O1 126.2(6) . . ? C6 C7 C2 120.0(6) . . ? O1 C7 C2 113.9(5) . . ? O1 C8 C9B 102.4(7) . . ? O1 C8 C9A 112.3(6) . . ? C9B C8 C9A 14.6(6) . . ? O1 C8 H8A 109.2 . . ? C9B C8 H8A 104.1 . . ? C9A C8 H8A 109.2 . . ? O1 C8 H8B 109.2 . . ? C9B C8 H8B 123.5 . . ? C9A C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C13A C9A C10A 118.9 . . ? C13A C9A C8 122.7(6) . . ? C10A C9A C8 118.2(6) . . ? C12A N3A C13A 120.4 . . ? C11A C10A C9A 120.2 . . ? C11A C10A H10A 119.9 . . ? C9A C10A H10A 119.9 . . ? C12A C11A C10A 120.6 . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C11A C12A N3A 119.5 . . ? C11A C12A C14A 115.3(8) . . ? N3A C12A C14A 125.0(8) . . ? C9A C13A N3A 120.5 . . ? C9A C13A H13A 119.7 . . ? N3A C13A H13A 119.7 . . ? N4A C14A C15A 118.9 . . ? N4A C14A C12A 116.3(11) . . ? C15A C14A C12A 124.6(11) . . ? C14A N4A C18A 120.5 . . ? C16A C15A C14A 120.2 . . ? C16A C15A H15A 119.9 . . ? C14A C15A H15A 119.9 . . ? C17A C16A C15A 120.6 . . ? C17A C16A H16A 119.7 . . ? C15A C16A H16A 119.7 . . ? C16A C17A C18A 119.5 . . ? C16A C17A C19 123.8(12) . . ? C18A C17A C19 115.9(12) . . ? C17A C18A N4A 120.4 . . ? C17A C18A H18A 119.8 . . ? N4A C18A H18A 119.8 . . ? C13B C9B C10B 118.9 . . ? C13B C9B C8 115.5(8) . . ? C10B C9B C8 125.3(7) . . ? C12B N3B C13B 120.4 . . ? C11B C10B C9B 120.2 . . ? C11B C10B H10B 119.9 . . ? C9B C10B H10B 119.9 . . ? C12B C11B C10B 120.6 . . ? C12B C11B H11B 119.7 . . ? C10B C11B H11B 119.7 . . ? C11B C12B N3B 119.5 . . ? C11B C12B C14B 123.0(7) . . ? N3B C12B C14B 117.6(7) . . ? C9B C13B N3B 120.5 . . ? C9B C13B H13B 119.7 . . ? N3B C13B H13B 119.7 . . ? C15B C14B N4B 118.9 . . ? C15B C14B C12B 126.6(6) . . ? N4B C14B C12B 114.5(6) . . ? C18B N4B C14B 120.2 . . ? C14B C15B C16B 120.5 . . ? C14B C15B H15B 119.7 . . ? C16B C15B H15B 119.7 . . ? C17B C16B C15B 120.4 . . ? C17B C16B H16B 119.8 . . ? C15B C16B H16B 119.8 . . ? C18B C17B C16B 119.5 . . ? C18B C17B C19 117.8(6) . . ? C16B C17B C19 122.7(6) . . ? C17B C18B N4B 120.6 . . ? C17B C18B H18B 119.7 . . ? N4B C18B H18B 119.7 . . ? O2 C19 C17A 115.6(9) . . ? O2 C19 C17B 103.2(6) . . ? C17A C19 C17B 13.9(9) . . ? O2 C19 H19A 108.4 . . ? C17A C19 H19A 108.4 . . ? C17B C19 H19A 120.4 . . ? O2 C19 H19B 108.4 . . ? C17A C19 H19B 108.4 . . ? C17B C19 H19B 108.6 . . ? H19A C19 H19B 107.4 . . ? O2 C20 C25 116.3(5) . . ? O2 C20 C21 123.6(5) . . ? C25 C20 C21 120.1(5) . . ? C22 C21 C20 118.9(6) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 122.8(6) . . ? C21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C22 C23 C24 117.1(5) . . ? C22 C23 C31 120.1(5) . . ? C24 C23 C31 122.7(5) . . ? C23 C24 C25 122.1(5) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C20 C25 C24 118.8(5) . . ? C20 C25 C26 119.0(5) . . ? C24 C25 C26 122.0(5) . . ? N2 C26 C25 113.9(5) . . ? N2 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? N2 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C29 C27 C4 112.5(6) . . ? C29 C27 C28 108.0(7) . . ? C4 C27 C28 109.6(6) . . ? C29 C27 C30 109.0(7) . . ? C4 C27 C30 109.2(6) . . ? C28 C27 C30 108.3(7) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C34 108.9(6) . . ? C32 C31 C33 108.9(6) . . ? C34 C31 C33 109.1(6) . . ? C32 C31 C23 108.4(6) . . ? C34 C31 C23 112.2(5) . . ? C33 C31 C23 109.3(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 C36 113.3(5) . . ? N1 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? N1 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C41 119.0(6) . . ? C37 C36 C35 122.4(6) . . ? C41 C36 C35 118.5(5) . . ? C36 C37 C38 123.0(6) . . ? C36 C37 H37 118.5 . . ? C38 C37 H37 118.5 . . ? C39 C38 C37 117.0(6) . . ? C39 C38 C61 121.1(6) . . ? C37 C38 C61 121.9(7) . . ? C38 C39 C40 121.6(6) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C39 C40 C41 119.9(7) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? O3 C41 C36 115.0(5) . . ? O3 C41 C40 125.6(6) . . ? C36 C41 C40 119.4(6) . . ? O3 C42 C43B 116.0(8) . . ? O3 C42 C43A 106.4(6) . . ? C43B C42 C43A 12.1(7) . . ? O3 C42 H42A 110.4 . . ? C43B C42 H42A 111.4 . . ? C43A C42 H42A 110.4 . . ? O3 C42 H42B 110.4 . . ? C43B C42 H42B 99.3 . . ? C43A C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C47A N5A C46A 120.0 . . ? C43A C47A N5A 120.0 . . ? C43A C47A H47A 120.0 . . ? N5A C47A H47A 120.0 . . ? C44A C43A C47A 120.0 . . ? C44A C43A C42 120.9(6) . . ? C47A C43A C42 119.0(6) . . ? C43A C44A C45A 120.0 . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C46A C45A C44A 120.0 . . ? C46A C45A H45A 120.0 . . ? C44A C45A H45A 120.0 . . ? C45A C46A N5A 120.0 . . ? C45A C46A C48A 125.6(8) . . ? N5A C46A C48A 114.4(8) . . ? C47B N5B C46B 120.0 . . ? N5B C47B C43B 120.0 . . ? N5B C47B H47B 120.0 . . ? C43B C47B H47B 120.0 . . ? C44B C43B C47B 120.0 . . ? C44B C43B C42 115.2(8) . . ? C47B C43B C42 123.5(8) . . ? C45B C44B C43B 120.0 . . ? C45B C44B H44B 120.0 . . ? C43B C44B H44B 120.0 . . ? C44B C45B C46B 120.0 . . ? C44B C45B H45B 120.0 . . ? C46B C45B H45B 120.0 . . ? C45B C46B N5B 120.0 . . ? C45B C46B C48B 123.7(8) . . ? N5B C46B C48B 116.3(8) . . ? C49A C48A N6A 118.9 . . ? C49A C48A C46A 113.5(8) . . ? N6A C48A C46A 127.6(8) . . ? C52A N6A C48A 120.2 . . ? C48A C49A C50A 120.5 . . ? C48A C49A H49A 119.7 . . ? C50A C49A H49A 119.7 . . ? C51A C50A C49A 120.4 . . ? C51A C50A H50A 119.8 . . ? C49A C50A H50A 119.8 . . ? C52A C51A C50A 119.5 . . ? C52A C51A C53 131.3(8) . . ? C50A C51A C53 108.8(8) . . ? C51A C52A N6A 120.6 . . ? C51A C52A H52A 119.7 . . ? N6A C52A H52A 119.7 . . ? N6B C48B C49B 118.9 . . ? N6B C48B C46B 125.9(8) . . ? C49B C48B C46B 115.1(8) . . ? C48B N6B C52B 120.5 . . ? C50B C49B C48B 120.2 . . ? C50B C49B H49B 119.9 . . ? C48B C49B H49B 119.9 . . ? C51B C50B C49B 120.6 . . ? C51B C50B H50B 119.7 . . ? C49B C50B H50B 119.7 . . ? C50B C51B C52B 119.5 . . ? C50B C51B C53 111.3(7) . . ? C52B C51B C53 128.7(7) . . ? C51B C52B N6B 120.4 . . ? C51B C52B H52B 119.8 . . ? N6B C52B H52B 119.8 . . ? O4 C53 C51B 107.5(7) . . ? O4 C53 C51A 103.2(7) . . ? C51B C53 C51A 19.7(5) . . ? O4 C53 H53A 111.1 . . ? C51B C53 H53A 92.0 . . ? C51A C53 H53A 111.1 . . ? O4 C53 H53B 111.1 . . ? C51B C53 H53B 124.4 . . ? C51A C53 H53B 111.1 . . ? H53A C53 H53B 109.1 . . ? C59 C54 O4 114.8(5) . . ? C59 C54 C55 120.5(6) . . ? O4 C54 C55 124.7(6) . . ? C56 C55 C54 119.3(7) . . ? C56 C55 H55 120.4 . . ? C54 C55 H55 120.4 . . ? C55 C56 C57 122.0(7) . . ? C55 C56 H56 119.0 . . ? C57 C56 H56 119.0 . . ? C56 C57 C58 116.8(6) . . ? C56 C57 C65 120.5(6) . . ? C58 C57 C65 122.6(6) . . ? C59 C58 C57 122.8(6) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C54 C59 C58 118.6(6) . . ? C54 C59 C60 119.5(5) . . ? C58 C59 C60 121.9(6) . . ? N2 C60 C59 114.5(5) . . ? N2 C60 H60A 108.6 . . ? C59 C60 H60A 108.6 . . ? N2 C60 H60B 108.6 . . ? C59 C60 H60B 108.6 . . ? H60A C60 H60B 107.6 . . ? C64 C61 C38 108.9(8) . . ? C64 C61 C62 106.3(8) . . ? C38 C61 C62 112.6(6) . . ? C64 C61 C63 114.4(11) . . ? C38 C61 C63 109.2(7) . . ? C62 C61 C63 105.5(9) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C68 C65 C66 110.3(10) . . ? C68 C65 C67 108.9(10) . . ? C66 C65 C67 108.5(8) . . ? C68 C65 C57 108.2(7) . . ? C66 C65 C57 109.9(6) . . ? C67 C65 C57 111.1(6) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N1 C69 C70 111.6(5) . . ? N1 C69 H69A 109.3 . . ? C70 C69 H69A 109.3 . . ? N1 C69 H69B 109.3 . . ? C70 C69 H69B 109.3 . . ? H69A C69 H69B 108.0 . . ? C75 C70 C71 119.0(6) . . ? C75 C70 C69 120.0(5) . . ? C71 C70 C69 121.0(5) . . ? C70 C71 C72 122.5(6) . . ? C70 C71 H71 118.8 . . ? C72 C71 H71 118.8 . . ? C73 C72 C71 116.3(6) . . ? C73 C72 C95 124.9(6) . . ? C71 C72 C95 118.8(6) . . ? C74 C73 C72 122.3(7) . . ? C74 C73 H73 118.8 . . ? C72 C73 H73 118.8 . . ? C75 C74 C73 119.6(7) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C70 120.2(6) . . ? C74 C75 O5 124.4(6) . . ? C70 C75 O5 115.3(6) . . ? O5 C76 C77B 110.1(7) . . ? O5 C76 C77A 104.2(6) . . ? C77B C76 C77A 13.2(6) . . ? O5 C76 H76A 110.9 . . ? C77B C76 H76A 117.5 . . ? C77A C76 H76A 110.9 . . ? O5 C76 H76B 110.9 . . ? C77B C76 H76B 97.7 . . ? C77A C76 H76B 110.9 . . ? H76A C76 H76B 108.9 . . ? C81A C77A C78A 118.9 . . ? C81A C77A C76 120.1(6) . . ? C78A C77A C76 120.7(6) . . ? C80A N7A C81A 120.4 . . ? C79A C78A C77A 120.2 . . ? C79A C78A H78A 119.9 . . ? C77A C78A H78A 119.9 . . ? C80A C79A C78A 120.6 . . ? C80A C79A H79A 119.7 . . ? C78A C79A H79A 119.7 . . ? C79A C80A N7A 119.5 . . ? C79A C80A C82A 114.2(7) . . ? N7A C80A C82A 126.3(7) . . ? C77A C81A N7A 120.5 . . ? C77A C81A H81A 119.7 . . ? N7A C81A H81A 119.7 . . ? C78B C77B C81B 118.9 . . ? C78B C77B C76 119.5(7) . . ? C81B C77B C76 120.4(7) . . ? C80B N7B C81B 120.6 . . ? C77B C78B C79B 120.5 . . ? C77B C78B H78B 119.7 . . ? C79B C78B H78B 119.7 . . ? C80B C79B C78B 120.4 . . ? C80B C79B H79B 119.8 . . ? C78B C79B H79B 119.8 . . ? N7B C80B C79B 119.5 . . ? N7B C80B C82B 113.0(7) . . ? C79B C80B C82B 127.5(7) . . ? N7B C81B C77B 120.2 . . ? N7B C81B H81B 119.9 . . ? C77B C81B H81B 119.9 . . ? N8A C82A C83A 118.9 . . ? N8A C82A C80A 117.3(6) . . ? C83A C82A C80A 123.5(6) . . ? C82A N8A C86A 120.5 . . ? C84A C83A C82A 120.2 . . ? C84A C83A H83A 119.9 . . ? C82A C83A H83A 119.9 . . ? C85A C84A C83A 120.6 . . ? C85A C84A H84A 119.7 . . ? C83A C84A H84A 119.7 . . ? C84A C85A C86A 119.5 . . ? C84A C85A C87 111.0(7) . . ? C86A C85A C87 129.4(7) . . ? C85A C86A N8A 120.4 . . ? C85A C86A H86A 119.8 . . ? N8A C86A H86A 119.8 . . ? N8B C82B C83B 118.9 . . ? N8B C82B C80B 114.7(6) . . ? C83B C82B C80B 125.3(6) . . ? C82B N8B C86B 120.5 . . ? C84B C83B C82B 120.2 . . ? C84B C83B H83B 119.9 . . ? C82B C83B H83B 119.9 . . ? C85B C84B C83B 120.6 . . ? C85B C84B H84B 119.7 . . ? C83B C84B H84B 119.7 . . ? C84B C85B C86B 119.5 . . ? C84B C85B C87 129.4(6) . . ? C86B C85B C87 111.1(6) . . ? C85B C86B N8B 120.3 . . ? C85B C86B H86B 119.8 . . ? N8B C86B H86B 119.8 . . ? C85A C87 O6 104.9(8) . . ? C85A C87 C85B 12.3(5) . . ? O6 C87 C85B 108.3(7) . . ? C85A C87 H87A 110.8 . . ? O6 C87 H87A 110.8 . . ? C85B C87 H87A 118.8 . . ? C85A C87 H87B 110.8 . . ? O6 C87 H87B 110.8 . . ? C85B C87 H87B 98.7 . . ? H87A C87 H87B 108.8 . . ? O6 C88 C89 124.9(6) . . ? O6 C88 C93 115.7(5) . . ? C89 C88 C93 119.4(6) . . ? C90 C89 C88 120.3(7) . . ? C90 C89 H89 119.8 . . ? C88 C89 H89 119.8 . . ? C89 C90 C91 121.7(6) . . ? C89 C90 H90 119.2 . . ? C91 C90 H90 119.2 . . ? C92 C91 C90 116.7(6) . . ? C92 C91 C99 123.0(6) . . ? C90 C91 C99 120.2(6) . . ? C91 C92 C93 123.0(6) . . ? C91 C92 H92 118.5 . . ? C93 C92 H92 118.5 . . ? C92 C93 C88 118.8(5) . . ? C92 C93 C94 121.5(5) . . ? C88 C93 C94 119.7(5) . . ? N2 C94 C93 112.9(4) . . ? N2 C94 H94A 109.0 . . ? C93 C94 H94A 109.0 . . ? N2 C94 H94B 109.0 . . ? C93 C94 H94B 109.0 . . ? H94A C94 H94B 107.8 . . ? C72 C95 C97 108.6(5) . . ? C72 C95 C98 112.0(6) . . ? C97 C95 C98 108.5(7) . . ? C72 C95 C96 110.4(6) . . ? C97 C95 C96 108.4(7) . . ? C98 C95 C96 108.9(7) . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C95 C97 H97A 109.5 . . ? C95 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C95 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C95 C98 H98A 109.5 . . ? C95 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C95 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C91 C99 C101 110.7(6) . . ? C91 C99 C100 108.1(7) . . ? C101 C99 C100 110.2(7) . . ? C91 C99 C102 110.7(6) . . ? C101 C99 C102 107.3(7) . . ? C100 C99 C102 109.8(8) . . ? C99 C100 H100 109.5 . . ? C99 C100 H200 109.5 . . ? H100 C100 H200 109.5 . . ? C99 C100 H300 109.5 . . ? H100 C100 H300 109.5 . . ? H200 C100 H300 109.5 . . ? C99 C101 H101 109.5 . . ? C99 C101 H201 109.5 . . ? H101 C101 H201 109.5 . . ? C99 C101 H301 109.5 . . ? H101 C101 H301 109.5 . . ? H201 C101 H301 109.5 . . ? C99 C102 H102 109.5 . . ? C99 C102 H202 109.5 . . ? H102 C102 H202 109.5 . . ? C99 C102 H303 109.5 . . ? H102 C102 H303 109.5 . . ? H202 C102 H303 109.5 . . ? C108 C103 C104 118.1 . . ? C108 C103 C109 120.8 . . ? C104 C103 C109 121.1 . . ? C105 C104 C103 120.9 . . ? C105 C104 H104 119.6 . . ? C103 C104 H104 119.6 . . ? C106 C105 C104 120.3 . . ? C106 C105 H105 119.8 . . ? C104 C105 H105 119.8 . . ? C107 C106 C105 119.5 . . ? C107 C106 H106 120.2 . . ? C105 C106 H106 120.2 . . ? C106 C107 C108 120.3 . . ? C106 C107 H107 119.9 . . ? C108 C107 H107 119.9 . . ? C107 C108 C103 120.9 . . ? C107 C108 H108 119.6 . . ? C103 C108 H108 119.6 . . ? C115 C110 C111 116.4(9) . . ? C115 C110 C116 123.1(12) . . ? C111 C110 C116 120.4(3) . . ? C110 C111 C112 121.8(4) . . ? C110 C111 H111 119.1 . . ? C112 C111 H111 119.1 . . ? C113 C112 C111 119.5(4) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C114 C113 C112 119.5 . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C113 C114 C115 120.3 . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C114 C115 C110 122.4(8) . . ? C114 C115 H115 118.8 . . ? C110 C115 H115 118.8 . . ? C110 C116 H116 109.5 . . ? C110 C116 H216 109.5 . . ? H116 C116 H216 109.5 . . ? C110 C116 H316 109.5 . . ? H116 C116 H316 109.5 . . ? H216 C116 H316 109.5 . . ? C122 C117 C118 118.1 . . ? C122 C117 C123 120.8 . . ? C118 C117 C123 121.1 . . ? C119 C118 C117 120.9 . . ? C119 C118 H118 119.6 . . ? C117 C118 H118 119.6 . . ? C120 C119 C118 120.3 . . ? C120 C119 H119 119.8 . . ? C118 C119 H119 119.8 . . ? C121 C120 C119 119.5 . . ? C121 C120 H120 120.2 . . ? C119 C120 H120 120.2 . . ? C120 C121 C122 120.3 . . ? C120 C121 H121 119.9 . . ? C122 C121 H121 119.9 . . ? C121 C122 C117 120.9 . . ? C121 C122 H122 119.6 . . ? C117 C122 H122 119.6 . . ? C117 C123 H123 109.5 . . ? C117 C123 H223 109.5 . . ? H123 C123 H223 109.5 . . ? C117 C123 H323 109.5 . . ? H123 C123 H323 109.5 . . ? H223 C123 H323 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 N1 C1 C2 164.6(5) . . . . ? C69 N1 C1 C2 -73.5(6) . . . . ? N1 C1 C2 C3 -16.3(8) . . . . ? N1 C1 C2 C7 162.9(5) . . . . ? C7 C2 C3 C4 -1.4(9) . . . . ? C1 C2 C3 C4 177.8(6) . . . . ? C2 C3 C4 C5 1.1(9) . . . . ? C2 C3 C4 C27 -179.8(6) . . . . ? C3 C4 C5 C6 0.2(10) . . . . ? C27 C4 C5 C6 -178.8(6) . . . . ? C4 C5 C6 C7 -1.4(10) . . . . ? C5 C6 C7 O1 -178.2(6) . . . . ? C5 C6 C7 C2 1.1(10) . . . . ? C8 O1 C7 C6 -5.2(9) . . . . ? C8 O1 C7 C2 175.5(5) . . . . ? C3 C2 C7 C6 0.2(9) . . . . ? C1 C2 C7 C6 -179.0(6) . . . . ? C3 C2 C7 O1 179.6(5) . . . . ? C1 C2 C7 O1 0.4(8) . . . . ? C7 O1 C8 C9B 167.5(6) . . . . ? C7 O1 C8 C9A 178.8(6) . . . . ? O1 C8 C9A C13A -137.8(7) . . . . ? C9B C8 C9A C13A -88(2) . . . . ? O1 C8 C9A C10A 37.3(8) . . . . ? C9B C8 C9A C10A 87(2) . . . . ? C13A C9A C10A C11A 0.6 . . . . ? C8 C9A C10A C11A -174.7(9) . . . . ? C9A C10A C11A C12A -0.4 . . . . ? C10A C11A C12A N3A 0.0 . . . . ? C10A C11A C12A C14A 175.1(10) . . . . ? C13A N3A C12A C11A 0.1 . . . . ? C13A N3A C12A C14A -174.5(11) . . . . ? C10A C9A C13A N3A -0.5 . . . . ? C8 C9A C13A N3A 174.5(9) . . . . ? C12A N3A C13A C9A 0.2 . . . . ? C11A C12A C14A N4A -179.8(8) . . . . ? N3A C12A C14A N4A -5.1(13) . . . . ? C11A C12A C14A C15A -5.1(13) . . . . ? N3A C12A C14A C15A 169.7(8) . . . . ? C15A C14A N4A C18A -0.5 . . . . ? C12A C14A N4A C18A 174.6(12) . . . . ? N4A C14A C15A C16A 0.6 . . . . ? C12A C14A C15A C16A -174.0(13) . . . . ? C14A C15A C16A C17A -0.4 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C15A C16A C17A C19 169.4(14) . . . . ? C16A C17A C18A N4A 0.1 . . . . ? C19 C17A C18A N4A -170.1(13) . . . . ? C14A N4A C18A C17A 0.2 . . . . ? O1 C8 C9B C13B 169.0(6) . . . . ? C9A C8 C9B C13B 35(2) . . . . ? O1 C8 C9B C10B -4.9(9) . . . . ? C9A C8 C9B C10B -139(3) . . . . ? C13B C9B C10B C11B 0.6 . . . . ? C8 C9B C10B C11B 174.3(10) . . . . ? C9B C10B C11B C12B -0.4 . . . . ? C10B C11B C12B N3B 0.0 . . . . ? C10B C11B C12B C14B -179.8(10) . . . . ? C13B N3B C12B C11B 0.1 . . . . ? C13B N3B C12B C14B 179.9(9) . . . . ? C10B C9B C13B N3B -0.5 . . . . ? C8 C9B C13B N3B -174.8(9) . . . . ? C12B N3B C13B C9B 0.1 . . . . ? C11B C12B C14B C15B -164.0(7) . . . . ? N3B C12B C14B C15B 16.2(11) . . . . ? C11B C12B C14B N4B 14.9(10) . . . . ? N3B C12B C14B N4B -164.8(6) . . . . ? C15B C14B N4B C18B 0.6 . . . . ? C12B C14B N4B C18B -178.4(9) . . . . ? N4B C14B C15B C16B -0.5 . . . . ? C12B C14B C15B C16B 178.4(10) . . . . ? C14B C15B C16B C17B 0.2 . . . . ? C15B C16B C17B C18B 0.1 . . . . ? C15B C16B C17B C19 179.0(9) . . . . ? C16B C17B C18B N4B 0.0 . . . . ? C19 C17B C18B N4B -178.9(9) . . . . ? C14B N4B C18B C17B -0.4 . . . . ? C20 O2 C19 C17A 172.7(10) . . . . ? C20 O2 C19 C17B 179.6(6) . . . . ? C16A C17A C19 O2 -86.2(13) . . . . ? C18A C17A C19 O2 83.5(11) . . . . ? C16A C17A C19 C17B -115(4) . . . . ? C18A C17A C19 C17B 55(4) . . . . ? C18B C17B C19 O2 -63.7(8) . . . . ? C16B C17B C19 O2 117.4(7) . . . . ? C18B C17B C19 C17A 90(4) . . . . ? C16B C17B C19 C17A -89(4) . . . . ? C19 O2 C20 C25 172.5(6) . . . . ? C19 O2 C20 C21 -8.1(10) . . . . ? O2 C20 C21 C22 178.4(7) . . . . ? C25 C20 C21 C22 -2.2(11) . . . . ? C20 C21 C22 C23 0.3(12) . . . . ? C21 C22 C23 C24 0.8(10) . . . . ? C21 C22 C23 C31 -175.9(7) . . . . ? C22 C23 C24 C25 0.0(9) . . . . ? C31 C23 C24 C25 176.6(6) . . . . ? O2 C20 C25 C24 -177.6(6) . . . . ? C21 C20 C25 C24 2.9(9) . . . . ? O2 C20 C25 C26 -1.5(8) . . . . ? C21 C20 C25 C26 179.1(6) . . . . ? C23 C24 C25 C20 -1.8(9) . . . . ? C23 C24 C25 C26 -177.9(6) . . . . ? C60 N2 C26 C25 -78.5(6) . . . . ? C94 N2 C26 C25 160.0(5) . . . . ? C20 C25 C26 N2 167.0(5) . . . . ? C24 C25 C26 N2 -16.9(8) . . . . ? C5 C4 C27 C29 -6.8(10) . . . . ? C3 C4 C27 C29 174.2(7) . . . . ? C5 C4 C27 C28 -127.0(8) . . . . ? C3 C4 C27 C28 54.0(9) . . . . ? C5 C4 C27 C30 114.5(8) . . . . ? C3 C4 C27 C30 -64.5(8) . . . . ? C22 C23 C31 C32 59.4(8) . . . . ? C24 C23 C31 C32 -117.1(7) . . . . ? C22 C23 C31 C34 179.7(6) . . . . ? C24 C23 C31 C34 3.2(9) . . . . ? C22 C23 C31 C33 -59.2(8) . . . . ? C24 C23 C31 C33 124.4(7) . . . . ? C1 N1 C35 C36 -74.3(6) . . . . ? C69 N1 C35 C36 163.9(5) . . . . ? N1 C35 C36 C37 -19.0(8) . . . . ? N1 C35 C36 C41 164.5(5) . . . . ? C41 C36 C37 C38 -2.0(9) . . . . ? C35 C36 C37 C38 -178.5(6) . . . . ? C36 C37 C38 C39 0.3(10) . . . . ? C36 C37 C38 C61 179.0(6) . . . . ? C37 C38 C39 C40 1.1(11) . . . . ? C61 C38 C39 C40 -177.6(7) . . . . ? C38 C39 C40 C41 -0.8(11) . . . . ? C42 O3 C41 C36 175.9(6) . . . . ? C42 O3 C41 C40 -4.1(10) . . . . ? C37 C36 C41 O3 -177.7(5) . . . . ? C35 C36 C41 O3 -1.0(8) . . . . ? C37 C36 C41 C40 2.3(9) . . . . ? C35 C36 C41 C40 178.9(6) . . . . ? C39 C40 C41 O3 179.0(6) . . . . ? C39 C40 C41 C36 -0.9(10) . . . . ? C41 O3 C42 C43B 178.0(7) . . . . ? C41 O3 C42 C43A 170.0(6) . . . . ? C46A N5A C47A C43A 0.0 . . . . ? N5A C47A C43A C44A 0.0 . . . . ? N5A C47A C43A C42 178.0(8) . . . . ? O3 C42 C43A C44A -34.9(8) . . . . ? C43B C42 C43A C44A -178(4) . . . . ? O3 C42 C43A C47A 147.1(6) . . . . ? C43B C42 C43A C47A 4(3) . . . . ? C47A C43A C44A C45A 0.0 . . . . ? C42 C43A C44A C45A -178.0(8) . . . . ? C43A C44A C45A C46A 0.0 . . . . ? C44A C45A C46A N5A 0.0 . . . . ? C44A C45A C46A C48A 176.6(11) . . . . ? C47A N5A C46A C45A 0.0 . . . . ? C47A N5A C46A C48A -177.0(10) . . . . ? C46B N5B C47B C43B 0.0 . . . . ? N5B C47B C43B C44B 0.0 . . . . ? N5B C47B C43B C42 -166.2(13) . . . . ? O3 C42 C43B C44B -98.1(9) . . . . ? C43A C42 C43B C44B -59(3) . . . . ? O3 C42 C43B C47B 68.7(12) . . . . ? C43A C42 C43B C47B 108(4) . . . . ? C47B C43B C44B C45B 0.0 . . . . ? C42 C43B C44B C45B 167.3(12) . . . . ? C43B C44B C45B C46B 0.0 . . . . ? C44B C45B C46B N5B 0.0 . . . . ? C44B C45B C46B C48B -178.6(10) . . . . ? C47B N5B C46B C45B 0.0 . . . . ? C47B N5B C46B C48B 178.7(9) . . . . ? C45A C46A C48A C49A 24.8(12) . . . . ? N5A C46A C48A C49A -158.4(6) . . . . ? C45A C46A C48A N6A -155.7(7) . . . . ? N5A C46A C48A N6A 21.1(13) . . . . ? C49A C48A N6A C52A 0.6 . . . . ? C46A C48A N6A C52A -178.8(13) . . . . ? N6A C48A C49A C50A -0.5 . . . . ? C46A C48A C49A C50A 179.0(11) . . . . ? C48A C49A C50A C51A 0.1 . . . . ? C49A C50A C51A C52A 0.1 . . . . ? C49A C50A C51A C53 -173.2(10) . . . . ? C50A C51A C52A N6A 0.0 . . . . ? C53 C51A C52A N6A 171.5(13) . . . . ? C48A N6A C52A C51A -0.4 . . . . ? C45B C46B C48B N6B 175.9(8) . . . . ? N5B C46B C48B N6B -2.8(12) . . . . ? C45B C46B C48B C49B 0.4(11) . . . . ? N5B C46B C48B C49B -178.3(8) . . . . ? C49B C48B N6B C52B -0.5 . . . . ? C46B C48B N6B C52B -175.8(9) . . . . ? N6B C48B C49B C50B 0.6 . . . . ? C46B C48B C49B C50B 176.4(8) . . . . ? C48B C49B C50B C51B -0.4 . . . . ? C49B C50B C51B C52B 0.0 . . . . ? C49B C50B C51B C53 172.8(8) . . . . ? C50B C51B C52B N6B 0.1 . . . . ? C53 C51B C52B N6B -171.3(10) . . . . ? C48B N6B C52B C51B 0.2 . . . . ? C54 O4 C53 C51B 166.2(7) . . . . ? C54 O4 C53 C51A -173.8(7) . . . . ? C50B C51B C53 O4 44.7(9) . . . . ? C52B C51B C53 O4 -143.4(8) . . . . ? C50B C51B C53 C51A -35.6(18) . . . . ? C52B C51B C53 C51A 136(2) . . . . ? C52A C51A C53 O4 130.3(9) . . . . ? C50A C51A C53 O4 -57.5(8) . . . . ? C52A C51A C53 C51B -125(2) . . . . ? C50A C51A C53 C51B 47.5(17) . . . . ? C53 O4 C54 C59 -176.1(7) . . . . ? C53 O4 C54 C55 5.8(12) . . . . ? C59 C54 C55 C56 -0.1(13) . . . . ? O4 C54 C55 C56 177.9(8) . . . . ? C54 C55 C56 C57 0.4(14) . . . . ? C55 C56 C57 C58 -0.6(12) . . . . ? C55 C56 C57 C65 179.0(8) . . . . ? C56 C57 C58 C59 0.3(10) . . . . ? C65 C57 C58 C59 -179.2(6) . . . . ? O4 C54 C59 C58 -178.4(6) . . . . ? C55 C54 C59 C58 -0.2(11) . . . . ? O4 C54 C59 C60 -1.3(9) . . . . ? C55 C54 C59 C60 176.8(7) . . . . ? C57 C58 C59 C54 0.0(10) . . . . ? C57 C58 C59 C60 -176.9(6) . . . . ? C94 N2 C60 C59 -80.8(6) . . . . ? C26 N2 C60 C59 157.2(5) . . . . ? C54 C59 C60 N2 167.2(6) . . . . ? C58 C59 C60 N2 -15.9(8) . . . . ? C39 C38 C61 C64 64.3(11) . . . . ? C37 C38 C61 C64 -114.3(10) . . . . ? C39 C38 C61 C62 -178.0(7) . . . . ? C37 C38 C61 C62 3.3(11) . . . . ? C39 C38 C61 C63 -61.2(12) . . . . ? C37 C38 C61 C63 120.1(10) . . . . ? C56 C57 C65 C68 62.4(12) . . . . ? C58 C57 C65 C68 -118.0(11) . . . . ? C56 C57 C65 C66 -58.0(11) . . . . ? C58 C57 C65 C66 121.5(9) . . . . ? C56 C57 C65 C67 -178.1(8) . . . . ? C58 C57 C65 C67 1.4(10) . . . . ? C35 N1 C69 C70 -72.6(6) . . . . ? C1 N1 C69 C70 164.9(5) . . . . ? N1 C69 C70 C75 151.5(7) . . . . ? N1 C69 C70 C71 -29.9(9) . . . . ? C75 C70 C71 C72 -2.6(11) . . . . ? C69 C70 C71 C72 178.7(7) . . . . ? C70 C71 C72 C73 0.7(11) . . . . ? C70 C71 C72 C95 -178.3(6) . . . . ? C71 C72 C73 C74 0.5(14) . . . . ? C95 C72 C73 C74 179.5(9) . . . . ? C72 C73 C74 C75 0.1(17) . . . . ? C73 C74 C75 C70 -2.0(17) . . . . ? C73 C74 C75 O5 -178.7(10) . . . . ? C71 C70 C75 C74 3.2(13) . . . . ? C69 C70 C75 C74 -178.1(9) . . . . ? C71 C70 C75 O5 -179.8(7) . . . . ? C69 C70 C75 O5 -1.1(11) . . . . ? C76 O5 C75 C74 -2.7(15) . . . . ? C76 O5 C75 C70 -179.6(8) . . . . ? C75 O5 C76 C77B -170.8(9) . . . . ? C75 O5 C76 C77A 176.9(8) . . . . ? O5 C76 C77A C81A 171.8(7) . . . . ? C77B C76 C77A C81A 53(2) . . . . ? O5 C76 C77A C78A -1.4(10) . . . . ? C77B C76 C77A C78A -120(3) . . . . ? C81A C77A C78A C79A 0.6 . . . . ? C76 C77A C78A C79A 173.8(11) . . . . ? C77A C78A C79A C80A -0.4 . . . . ? C78A C79A C80A N7A 0.0 . . . . ? C78A C79A C80A C82A -177.2(11) . . . . ? C81A N7A C80A C79A 0.1 . . . . ? C81A N7A C80A C82A 177.0(13) . . . . ? C78A C77A C81A N7A -0.5 . . . . ? C76 C77A C81A N7A -173.8(11) . . . . ? C80A N7A C81A C77A 0.1 . . . . ? O5 C76 C77B C78B -123.5(7) . . . . ? C77A C76 C77B C78B -58(2) . . . . ? O5 C76 C77B C81B 44.2(10) . . . . ? C77A C76 C77B C81B 109(3) . . . . ? C81B C77B C78B C79B -0.5 . . . . ? C76 C77B C78B C79B 167.4(9) . . . . ? C77B C78B C79B C80B 0.2 . . . . ? C81B N7B C80B C79B 0.0 . . . . ? C81B N7B C80B C82B 178.3(8) . . . . ? C78B C79B C80B N7B 0.1 . . . . ? C78B C79B C80B C82B -178.0(10) . . . . ? C80B N7B C81B C77B -0.4 . . . . ? C78B C77B C81B N7B 0.6 . . . . ? C76 C77B C81B N7B -167.2(10) . . . . ? C79A C80A C82A N8A -177.4(6) . . . . ? N7A C80A C82A N8A 5.6(14) . . . . ? C79A C80A C82A C83A -3.6(11) . . . . ? N7A C80A C82A C83A 179.4(7) . . . . ? C83A C82A N8A C86A -0.5 . . . . ? C80A C82A N8A C86A 173.6(11) . . . . ? N8A C82A C83A C84A 0.6 . . . . ? C80A C82A C83A C84A -173.1(11) . . . . ? C82A C83A C84A C85A -0.4 . . . . ? C83A C84A C85A C86A 0.0 . . . . ? C83A C84A C85A C87 177.5(9) . . . . ? C84A C85A C86A N8A 0.1 . . . . ? C87 C85A C86A N8A -176.8(11) . . . . ? C82A N8A C86A C85A 0.1 . . . . ? N7B C80B C82B N8B 165.4(5) . . . . ? C79B C80B C82B N8B -16.4(10) . . . . ? N7B C80B C82B C83B -26.5(10) . . . . ? C79B C80B C82B C83B 151.7(6) . . . . ? C83B C82B N8B C86B -0.5 . . . . ? C80B C82B N8B C86B 168.4(9) . . . . ? N8B C82B C83B C84B 0.6 . . . . ? C80B C82B C83B C84B -167.0(10) . . . . ? C82B C83B C84B C85B -0.3 . . . . ? C83B C84B C85B C86B 0.0 . . . . ? C83B C84B C85B C87 -177.4(9) . . . . ? C84B C85B C86B N8B 0.1 . . . . ? C87 C85B C86B N8B 177.9(8) . . . . ? C82B N8B C86B C85B 0.2 . . . . ? C84A C85A C87 O6 -82.7(8) . . . . ? C86A C85A C87 O6 94.4(10) . . . . ? C84A C85A C87 C85B 25(3) . . . . ? C86A C85A C87 C85B -158(3) . . . . ? C88 O6 C87 C85A -176.0(6) . . . . ? C88 O6 C87 C85B 171.7(6) . . . . ? C84B C85B C87 C85A 166(3) . . . . ? C86B C85B C87 C85A -12(3) . . . . ? C84B C85B C87 O6 -118.3(8) . . . . ? C86B C85B C87 O6 64.1(7) . . . . ? C87 O6 C88 C89 -1.8(10) . . . . ? C87 O6 C88 C93 178.3(6) . . . . ? O6 C88 C89 C90 177.8(6) . . . . ? C93 C88 C89 C90 -2.2(11) . . . . ? C88 C89 C90 C91 0.3(12) . . . . ? C89 C90 C91 C92 1.5(10) . . . . ? C89 C90 C91 C99 -175.1(7) . . . . ? C90 C91 C92 C93 -1.5(9) . . . . ? C99 C91 C92 C93 175.1(6) . . . . ? C91 C92 C93 C88 -0.4(9) . . . . ? C91 C92 C93 C94 -178.0(5) . . . . ? O6 C88 C93 C92 -177.8(5) . . . . ? C89 C88 C93 C92 2.3(9) . . . . ? O6 C88 C93 C94 -0.1(8) . . . . ? C89 C88 C93 C94 179.9(6) . . . . ? C60 N2 C94 C93 166.9(5) . . . . ? C26 N2 C94 C93 -71.1(6) . . . . ? C92 C93 C94 N2 -28.3(8) . . . . ? C88 C93 C94 N2 154.1(5) . . . . ? C73 C72 C95 C97 -117.9(9) . . . . ? C71 C72 C95 C97 61.0(9) . . . . ? C73 C72 C95 C98 1.9(12) . . . . ? C71 C72 C95 C98 -179.1(8) . . . . ? C73 C72 C95 C96 123.4(9) . . . . ? C71 C72 C95 C96 -57.7(9) . . . . ? C92 C91 C99 C101 135.5(7) . . . . ? C90 C91 C99 C101 -48.0(9) . . . . ? C92 C91 C99 C100 -103.7(9) . . . . ? C90 C91 C99 C100 72.8(10) . . . . ? C92 C91 C99 C102 16.6(10) . . . . ? C90 C91 C99 C102 -166.9(7) . . . . ? C108 C103 C104 C105 -0.5 . . . . ? C109 C103 C104 C105 177.7 . . . . ? C103 C104 C105 C106 0.1 . . . . ? C104 C105 C106 C107 0.4 . . . . ? C105 C106 C107 C108 -0.4 . . . . ? C106 C107 C108 C103 0.0 . . . . ? C104 C103 C108 C107 0.4 . . . . ? C109 C103 C108 C107 -177.8 . . . . ? C115 C110 C111 C112 -0.1(2) . . . . ? C116 C110 C111 C112 178.4(3) . . . . ? C110 C111 C112 C113 -0.6(3) . . . . ? C111 C112 C113 C114 0.8(2) . . . . ? C112 C113 C114 C115 -0.4 . . . . ? C113 C114 C115 C110 -0.25(13) . . . . ? C111 C110 C115 C114 0.5 . . . . ? C116 C110 C115 C114 -177.89(7) . . . . ? C122 C117 C118 C119 0.5 . . . . ? C123 C117 C118 C119 -177.7 . . . . ? C117 C118 C119 C120 -0.1 . . . . ? C118 C119 C120 C121 -0.4 . . . . ? C119 C120 C121 C122 0.4 . . . . ? C120 C121 C122 C117 0.0 . . . . ? C118 C117 C122 C121 -0.4 . . . . ? C123 C117 C122 C121 177.8 . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 18.24 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.266 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.117