Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Kevin Smith' 'Jack Fajer' 'Daniel J. Nurco' _publ_contact_author_name 'Prof Kevin Smith' _publ_contact_author_address ; Office of Research & Grad. Studies Louisiana State University 130 David Boyd Hall Baton Rouge LA 70803 UNITED STATES OF AMERICA ; _publ_contact_author_email KMSMITH@LSU.EDU _publ_section_title ; Conformational Landscape Surfing Induced by Off-On p-p Stacking in a Porphyrin-Quinone Dyad ; data_djn202ll _database_code_CSD 194212 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ni PQ' _chemical_melting_point ? _chemical_formula_moiety '2[C51 H13 Cl2 F15 N6 Ni O2], 1.5[C6 H14]' _chemical_formula_sum 'C111 H47 Cl4 F30 N12 Ni2 O4' _chemical_formula_weight 2468 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.037(5) _cell_length_b 22.693(4) _cell_length_c 30.799(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.047(4) _cell_angle_gamma 90.00 _cell_volume 21359(6) _cell_formula_units_Z 8 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 5969 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.09 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9690 _exptl_absorpt_coefficient_mu 0.56 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7657 _exptl_absorpt_correction_T_max 0.8491 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were grown from methylene chloride / n-hexane. ; _diffrn_ambient_temperature 91(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ; 50 frames measured at the beginning and end of the data collection. ; _diffrn_standards_interval_time ? _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 13875 _diffrn_reflns_av_R_equivalents 0.2375 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 22.46 _reflns_number_total 13875 _reflns_number_gt 9065 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5, XP (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+778.6161P] 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 13875 _refine_ls_number_parameters 1248 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1741 _refine_ls_R_factor_gt 0.1233 _refine_ls_wR_factor_ref 0.3487 _refine_ls_wR_factor_gt 0.3019 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.10883(5) -0.01418(8) 0.30058(5) 0.0397(5) Uani 1 1 d . . . N1 N -0.0713(3) -0.0807(5) 0.3194(3) 0.035(2) Uani 1 1 d U . . C1 C -0.0270(4) -0.0827(6) 0.3242(4) 0.040(3) Uani 1 1 d . . . F1 F -0.1276(3) -0.1900(3) 0.4170(2) 0.056(2) Uani 1 1 d . . . Cl1 Cl 0.01458(15) -0.0783(2) 0.56736(13) 0.0761(13) Uani 1 1 d . . . O1 O 0.0020(4) -0.1040(5) 0.4728(3) 0.058(3) Uani 1 1 d . . . Cl2 Cl 0.08006(16) 0.0291(2) 0.59085(13) 0.0797(14) Uani 1 1 d . . . O2 O 0.1203(4) 0.0656(5) 0.5168(3) 0.073(3) Uani 1 1 d . . . N2 N -0.1591(3) -0.0652(5) 0.2940(3) 0.038(3) Uani 1 1 d . . . F2 F -0.1399(3) -0.3025(4) 0.4410(3) 0.068(2) Uani 1 1 d . . . C2 C -0.0111(5) -0.1420(6) 0.3355(5) 0.051(4) Uani 1 1 d . . . H2 H 0.0184 -0.1551 0.3393 0.062 Uiso 1 1 calc R . . N3 N -0.1460(3) 0.0520(5) 0.2779(4) 0.042(3) Uani 1 1 d . . . F3 F -0.1527(3) -0.3898(4) 0.3784(4) 0.079(3) Uani 1 1 d . . . C3 C -0.0469(5) -0.1751(7) 0.3397(5) 0.053(4) Uani 1 1 d . . . H3 H -0.0471 -0.2154 0.3479 0.063 Uiso 1 1 calc R . . N4 N -0.0580(3) 0.0375(5) 0.3099(3) 0.042(3) Uani 1 1 d . . . C4 C -0.0841(4) -0.1369(6) 0.3295(4) 0.041(3) Uani 1 1 d . . . F4 F -0.1554(3) -0.3612(4) 0.2921(3) 0.086(3) Uani 1 1 d . . . N5 N 0.0454(3) -0.0707(4) 0.4110(3) 0.033(2) Uani 1 1 d D . . H5A H 0.024(3) -0.097(4) 0.412(4) 0.040 Uiso 1 1 d D . . F5 F -0.1424(3) -0.2497(4) 0.2686(3) 0.076(3) Uani 1 1 d . . . C5 C -0.1261(5) -0.1555(6) 0.3283(4) 0.045(4) Uani 1 1 d . . . C5A C -0.13440(13) -0.21725(18) 0.34223(17) 0.044(3) Uani 1 1 d G . . C5B C -0.13353(14) -0.2315(2) 0.38627(18) 0.045(3) Uani 1 1 d G . . C5C C -0.13958(16) -0.2895(2) 0.3983(2) 0.049(4) Uani 1 1 d G . . C5D C -0.14650(17) -0.33333(19) 0.3663(3) 0.069(5) Uani 1 1 d G . . C5E C -0.14736(16) -0.31911(18) 0.3223(2) 0.056(4) Uani 1 1 d G . . C5F C -0.14131(14) -0.26107(19) 0.3102(2) 0.059(4) Uani 1 1 d G . . F6 F -0.28349(15) 0.0373(2) 0.2953(2) 0.078(3) Uani 1 1 d G . . N6 N 0.11683(17) 0.0637(4) 0.4048(4) 0.064(4) Uani 1 1 d G . . C6 C -0.16217(12) -0.12096(19) 0.31022(14) 0.040(3) Uani 1 1 d G . . F7 F -0.36822(15) 0.0346(3) 0.2574(3) 0.090(3) Uani 1 1 d G . . C7 C -0.20564(12) -0.14317(19) 0.30256(15) 0.051(4) Uani 1 1 d G . . H7 H -0.2155 -0.1797 0.3123 0.062 Uiso 1 1 calc R . . C8 C -0.2303(4) -0.1006(6) 0.2782(5) 0.047(3) Uani 1 1 d U . . H8 H -0.2607 -0.1024 0.2668 0.056 Uiso 1 1 calc R . . F8 F -0.3914(3) 0.0007(4) 0.1725(4) 0.084(3) Uani 1 1 d . . . F9 F -0.3284(3) -0.0320(5) 0.1253(3) 0.089(3) Uani 1 1 d . . . C9 C -0.2013(4) -0.0529(6) 0.2731(4) 0.045(3) Uani 1 1 d . . . F10 F -0.2439(3) -0.0316(4) 0.1636(3) 0.064(2) Uani 1 1 d . . . C10 C -0.2144(4) -0.0014(6) 0.2531(4) 0.045(3) Uani 1 1 d . . . C10A C -0.26174(16) 0.0036(2) 0.23053(18) 0.054(4) Uani 1 1 d G . . C10B C -0.29369(17) 0.0201(3) 0.2547(2) 0.055(4) Uani 1 1 d G . . C10C C -0.33760(16) 0.0184(3) 0.2352(3) 0.066(5) Uani 1 1 d G . . C10D C -0.34956(17) 0.0002(3) 0.1917(3) 0.057(4) Uani 1 1 d GU . . C10E C -0.3176(2) -0.0162(3) 0.1676(2) 0.057(4) Uani 1 1 d G . . C10F C -0.27370(19) -0.0145(3) 0.1870(2) 0.052(4) Uani 1 1 d G . . F11 F -0.1384(2) 0.1931(3) 0.3588(2) 0.088(3) Uani 1 1 d G . . C11 C -0.18832(15) 0.0487(3) 0.2556(2) 0.048(4) Uani 1 1 d G . . F12 F -0.1322(3) 0.3081(3) 0.3744(3) 0.136(5) Uani 1 1 d G . . C12 C -0.20275(18) 0.1075(2) 0.24255(16) 0.055(4) Uani 1 1 d G . . H12 H -0.2302 0.1177 0.2253 0.066 Uiso 1 1 calc R . . F13 F -0.0847(4) 0.3785(4) 0.3288(4) 0.115(4) Uani 1 1 d . . . C13 C -0.1721(5) 0.1438(7) 0.2584(5) 0.058(4) Uani 1 1 d . . . H13 H -0.1735 0.1855 0.2560 0.069 Uiso 1 1 calc R . . F14 F -0.0428(3) 0.3290(4) 0.2676(4) 0.091(3) Uani 1 1 d . . . C14 C -0.1353(4) 0.1104(6) 0.2801(4) 0.042(3) Uani 1 1 d . . . F15 F -0.0482(3) 0.2119(4) 0.2509(3) 0.065(2) Uani 1 1 d . . . C15 C -0.0951(4) 0.1335(6) 0.2994(4) 0.045(3) Uani 1 1 d . . . C15A C -0.09242(18) 0.1997(3) 0.3062(2) 0.052(4) Uani 1 1 d G . . C15B C -0.1139(3) 0.2253(3) 0.3374(3) 0.069(5) Uani 1 1 d G . . C15C C -0.1111(4) 0.2858(4) 0.3446(3) 0.091(6) Uani 1 1 d G . . C15D C -0.0869(3) 0.3206(3) 0.3206(4) 0.084(6) Uani 1 1 d G . . C15E C -0.0654(3) 0.2949(3) 0.2894(4) 0.073(5) Uani 1 1 d G . . C15F C -0.0681(3) 0.2345(3) 0.2822(2) 0.061(5) Uani 1 1 d G . . C16 C -0.0581(3) 0.0983(3) 0.3117(3) 0.042(3) Uani 1 1 d G . . C17 C -0.0159(2) 0.1213(3) 0.3249(3) 0.048(4) Uani 1 1 d G . . H17 H -0.0081 0.1614 0.3300 0.058 Uiso 1 1 calc R . . C18 C 0.0111(4) 0.0744(6) 0.3286(4) 0.041(3) Uani 1 1 d U . . H18 H 0.0421 0.0758 0.3358 0.049 Uiso 1 1 calc R . . C19 C -0.0148(4) 0.0220(6) 0.3200(4) 0.040(3) Uani 1 1 d . . . C20 C 0.0006(4) -0.0343(7) 0.3244(4) 0.047(4) Uani 1 1 d . . . C20A C 0.0498(2) -0.0458(4) 0.3351(3) 0.048(4) Uani 1 1 d G . . C20B C 0.0697(2) -0.0650(4) 0.3766(2) 0.041(3) Uani 1 1 d G . . C20C C 0.1141(3) -0.0783(4) 0.3847(2) 0.046(3) Uani 1 1 d G . . H20C H 0.1276 -0.0915 0.4131 0.056 Uiso 1 1 calc R . . C20D C 0.1386(2) -0.0724(5) 0.3513(3) 0.061(4) Uani 1 1 d G . . H20D H 0.1689 -0.0814 0.3568 0.073 Uiso 1 1 calc R . . C20E C 0.1187(3) -0.0531(5) 0.3097(3) 0.082(6) Uani 1 1 d G . . H20E H 0.1354 -0.0490 0.2869 0.099 Uiso 1 1 calc R . . C20F C 0.0743(3) -0.0398(5) 0.3017(2) 0.060(4) Uani 1 1 d GU . . H20F H 0.0607 -0.0267 0.2733 0.073 Uiso 1 1 calc R . . C20G C 0.0563(5) -0.0436(6) 0.4504(4) 0.045(3) Uani 1 1 d . . . C20H C 0.0307(5) -0.0676(6) 0.4844(4) 0.043(3) Uani 1 1 d . . . C20I C 0.0409(5) -0.0464(7) 0.5295(4) 0.050(4) Uani 1 1 d . . . C20J C 0.0698(5) -0.0009(7) 0.5397(4) 0.056(4) Uani 1 1 d . . . C20K C 0.0936(5) 0.0254(7) 0.5065(5) 0.056(4) Uani 1 1 d . . . C20L C 0.0838(5) 0.0019(6) 0.4615(4) 0.049(4) Uani 1 1 d . . . C20M C 0.1042(5) 0.0348(7) 0.4301(5) 0.054(4) Uani 1 1 d . . . Ni2 Ni 0.13596(5) 0.36610(7) 0.43056(6) 0.0442(5) Uani 1 1 d . . . Cl3 Cl 0.03845(12) 0.31085(18) 0.33483(14) 0.0613(10) Uani 1 1 d . . . O3 O 0.0757(3) 0.1944(4) 0.3559(3) 0.053(2) Uani 1 1 d . . . Cl4 Cl 0.10807(12) 0.39668(16) 0.30136(13) 0.0566(10) Uani 1 1 d . . . O4 O 0.1872(3) 0.3337(4) 0.2940(4) 0.060(3) Uani 1 1 d . . . N7 N 0.1978(3) 0.3506(4) 0.4327(3) 0.039(3) Uani 1 1 d . . . N8 N 0.1441(3) 0.4463(5) 0.4124(4) 0.046(3) Uani 1 1 d . . . N9 N 0.0747(4) 0.3810(5) 0.4285(4) 0.054(3) Uani 1 1 d . . . N10 N 0.1285(3) 0.2865(5) 0.4488(3) 0.040(3) Uani 1 1 d . . . N11 N 0.1593(3) 0.1609(4) 0.3703(3) 0.036(2) Uani 1 1 d D . . H11A H 0.140(3) 0.135(4) 0.378(4) 0.044 Uiso 1 1 d D . . N12 N 0.2560(4) 0.2158(5) 0.3276(4) 0.055(3) Uani 1 1 d . . . F16 F 0.2746(3) 0.4766(4) 0.3629(3) 0.079(3) Uani 1 1 d . . . F17 F 0.3385(4) 0.5584(5) 0.3723(4) 0.099(4) Uani 1 1 d . . . F18 F 0.3620(3) 0.6137(5) 0.4499(4) 0.110(4) Uani 1 1 d . . . F19 F 0.3195(4) 0.5916(5) 0.5172(4) 0.108(4) Uani 1 1 d . . . F20 F 0.2535(4) 0.5126(4) 0.5079(3) 0.083(3) Uani 1 1 d . . . F21 F 0.0162(3) 0.4568(5) 0.3044(4) 0.089(3) Uani 1 1 d . . . C21 C 0.2176(4) 0.2963(6) 0.4317(4) 0.042(3) Uani 1 1 d . . . C22 C 0.2632(4) 0.3043(6) 0.4299(4) 0.040(3) Uani 1 1 d . . . H22 H 0.2837 0.2742 0.4270 0.048 Uiso 1 1 calc R . . F22 F -0.0428(3) 0.5353(6) 0.2649(4) 0.114(4) Uani 1 1 d . . . F23 F -0.0580(4) 0.6367(6) 0.3047(6) 0.148(6) Uani 1 1 d . . . C23 C 0.2713(4) 0.3623(6) 0.4332(4) 0.043(3) Uani 1 1 d . . . H23 H 0.2991 0.3805 0.4348 0.051 Uiso 1 1 calc R . . F24 F -0.0098(5) 0.6632(5) 0.3839(5) 0.136(5) Uani 1 1 d . . . C24 C 0.2307(4) 0.3920(6) 0.4337(4) 0.040(3) Uani 1 1 d U . . F25 F 0.0512(4) 0.5886(5) 0.4238(4) 0.101(4) Uani 1 1 d . . . C25 C 0.2247(4) 0.4517(6) 0.4296(4) 0.041(3) Uani 1 1 d . . . C25A C 0.26255(14) 0.4926(2) 0.43506(19) 0.045(3) Uani 1 1 d G . . C25B C 0.28435(17) 0.5044(3) 0.4002(2) 0.049(4) Uani 1 1 d G . . C25C C 0.31794(17) 0.5457(3) 0.4053(2) 0.061(4) Uani 1 1 d G . . C25D C 0.32974(16) 0.5752(3) 0.4451(2) 0.071(5) Uani 1 1 d G . . C25E C 0.3079(2) 0.5634(3) 0.4800(2) 0.069(5) Uani 1 1 d G . . C25F C 0.27435(18) 0.5221(3) 0.47492(18) 0.052(4) Uani 1 1 d G . . F26 F -0.0201(2) 0.2455(4) 0.4083(2) 0.098(4) Uani 1 1 d G . . C26 C 0.18373(14) 0.4754(2) 0.41611(17) 0.039(3) Uani 1 1 d G . . F27 F -0.0889(2) 0.2001(5) 0.4370(3) 0.145(6) Uani 1 1 d G . . C27 C 0.17557(15) 0.5334(2) 0.3986(3) 0.058(4) Uani 1 1 d G . . H27 H 0.1970 0.5632 0.3983 0.069 Uiso 1 1 calc R . . F28 F -0.0892(3) 0.1898(5) 0.5256(4) 0.092(3) Uani 1 1 d . . . C28 C 0.1328(5) 0.5388(6) 0.3828(5) 0.058(4) Uani 1 1 d . . . H28 H 0.1188 0.5720 0.3677 0.069 Uiso 1 1 calc R . . F29 F -0.0207(3) 0.2247(5) 0.5830(3) 0.095(3) Uani 1 1 d . . . C29 C 0.1121(5) 0.4857(6) 0.3927(5) 0.051(4) Uani 1 1 d U . . F30 F 0.0490(3) 0.2744(5) 0.5551(3) 0.086(3) Uani 1 1 d . . . C30 C 0.0687(5) 0.4758(6) 0.3888(5) 0.054(4) Uani 1 1 d . . . C30A C 0.0358(2) 0.5206(3) 0.3662(3) 0.064(5) Uani 1 1 d G . . C30B C 0.0113(3) 0.5073(4) 0.3252(3) 0.067(5) Uani 1 1 d G . . C30C C -0.0198(3) 0.5470(5) 0.3046(3) 0.085(6) Uani 1 1 d G . . C30D C -0.0264(3) 0.6000(4) 0.3250(4) 0.088(6) Uani 1 1 d GU . . C30E C -0.0020(4) 0.6133(3) 0.3661(4) 0.095(7) Uani 1 1 d G . . C30F C 0.0291(3) 0.5736(3) 0.3867(3) 0.084(6) Uani 1 1 d G . . C31 C 0.0505(3) 0.4272(4) 0.4084(4) 0.064(4) Uani 1 1 d G . . C32 C 0.0057(3) 0.4233(4) 0.4125(4) 0.075(5) Uani 1 1 d G . . H32 H -0.0174 0.4493 0.4008 0.090 Uiso 1 1 calc R . . C33 C 0.0033(5) 0.3741(8) 0.4370(6) 0.069(5) Uani 1 1 d U . . H33 H -0.0222 0.3603 0.4469 0.083 Uiso 1 1 calc R . . C34 C 0.0446(4) 0.3471(6) 0.4453(5) 0.053(4) Uani 1 1 d . . . C35 C 0.0539(5) 0.2940(7) 0.4637(5) 0.051(4) Uani 1 1 d . . . C35A C 0.01638(19) 0.2617(2) 0.4815(2) 0.055(4) Uani 1 1 d G . . C35B C -0.0194(2) 0.2422(4) 0.4514(2) 0.068(5) Uani 1 1 d G . . C35C C -0.05548(19) 0.2184(4) 0.4663(3) 0.077(5) Uani 1 1 d G . . C35D C -0.0557(2) 0.2140(4) 0.5112(3) 0.065(5) Uani 1 1 d G . . C35E C -0.0199(2) 0.2335(5) 0.5414(2) 0.061(4) Uani 1 1 d G . . C35F C 0.0162(2) 0.2574(4) 0.5265(2) 0.056(4) Uani 1 1 d G . . C36 C 0.0929(2) 0.2638(4) 0.4648(3) 0.046(3) Uani 1 1 d G . . C37 C 0.1002(2) 0.2029(4) 0.4766(3) 0.048(4) Uani 1 1 d G . . H37 H 0.0809 0.1780 0.4890 0.057 Uiso 1 1 calc R . . C38 C 0.1398(5) 0.1875(7) 0.4669(4) 0.050(4) Uani 1 1 d . . . H38 H 0.1535 0.1500 0.4707 0.060 Uiso 1 1 calc R . . C39 C 0.1567(4) 0.2400(6) 0.4494(4) 0.037(3) Uani 1 1 d . . . C40 C 0.1982(4) 0.2423(6) 0.4372(4) 0.041(3) Uani 1 1 d . . . C40A C 0.22009(19) 0.1846(2) 0.4293(2) 0.040(3) Uani 1 1 d G . . C40B C 0.20030(18) 0.1465(2) 0.39644(18) 0.045(3) Uani 1 1 d G . . C40C C 0.21958(18) 0.0926(2) 0.39034(18) 0.043(3) Uani 1 1 d G . . H40C H 0.2061 0.0665 0.3679 0.052 Uiso 1 1 calc R . . C40D C 0.25866(18) 0.0767(3) 0.4171(2) 0.053(4) Uani 1 1 d G . . H40D H 0.2718 0.0398 0.4130 0.063 Uiso 1 1 calc R . . C40E C 0.27845(18) 0.1147(3) 0.45000(19) 0.048(3) Uani 1 1 d G . . H40E H 0.3052 0.1039 0.4683 0.057 Uiso 1 1 calc R . . C40F C 0.25917(19) 0.1687(3) 0.45610(19) 0.050(4) Uani 1 1 d G . . H40F H 0.2727 0.1947 0.4786 0.060 Uiso 1 1 calc R . . C40G C 0.1498(4) 0.2108(6) 0.3493(4) 0.038(3) Uani 1 1 d . . . C40H C 0.1023(5) 0.2290(7) 0.3452(4) 0.050(4) Uani 1 1 d . . . C40I C 0.0905(4) 0.2903(6) 0.3313(5) 0.043(3) Uani 1 1 d . . . C40J C 0.1189(5) 0.3252(6) 0.3166(5) 0.048(3) Uani 1 1 d . . . C40K C 0.1644(4) 0.3047(6) 0.3136(4) 0.042(3) Uani 1 1 d . . . C40L C 0.1773(4) 0.2474(6) 0.3317(5) 0.047(4) Uani 1 1 d . . . C40M C 0.2211(5) 0.2305(6) 0.3294(4) 0.039(3) Uani 1 1 d . . . C41 C -0.3163(12) -0.1486(16) 0.0012(12) 0.192(7) Uiso 1 1 d . A 1 H41A H -0.3026 -0.1221 -0.0176 0.287 Uiso 1 1 calc R A 1 H41B H -0.3263 -0.1844 -0.0154 0.287 Uiso 1 1 calc R A 1 H41C H -0.2950 -0.1591 0.0274 0.287 Uiso 1 1 calc R A 1 C42 C -0.3571(4) -0.1162(9) 0.0158(5) 0.192(7) Uiso 1 1 d G A 1 H42A H -0.3832 -0.1352 -0.0017 0.230 Uiso 1 1 calc R A 1 H42B H -0.3566 -0.1287 0.0467 0.230 Uiso 1 1 calc R A 1 C43 C -0.3663(3) -0.0610(9) 0.0152(5) 0.192(7) Uiso 1 1 d G A 1 H43A H -0.3689 -0.0486 -0.0159 0.230 Uiso 1 1 calc R A 1 H43B H -0.3399 -0.0413 0.0314 0.230 Uiso 1 1 calc R A 1 C44 C -0.4030(3) -0.0344(9) 0.0312(5) 0.192(7) Uiso 1 1 d G A 1 H44A H -0.4305 -0.0477 0.0126 0.230 Uiso 1 1 calc R A 1 H44B H -0.4032 -0.0479 0.0617 0.230 Uiso 1 1 calc R A 1 C45 C -0.4009(3) 0.0284(9) 0.0304(5) 0.192(7) Uiso 0.80 1 d PG A 1 H45A H -0.4019 0.0412 -0.0004 0.230 Uiso 0.80 1 calc PR A 1 H45B H -0.3724 0.0409 0.0475 0.230 Uiso 0.80 1 calc PR A 1 C46 C -0.4372(3) 0.0604(9) 0.0489(6) 0.192(7) Uiso 0.80 1 d PG A 1 H46A H -0.4658 0.0465 0.0337 0.287 Uiso 0.80 1 calc PR A 1 H46B H -0.4347 0.1029 0.0443 0.287 Uiso 0.80 1 calc PR A 1 H46C H -0.4343 0.0522 0.0805 0.287 Uiso 0.80 1 calc PR A 1 C45' C -0.3006(4) -0.2034(8) 0.0070(5) 0.192(7) Uiso 0.20 1 d PG B 2 C46' C -0.2550(4) -0.2157(8) 0.0068(5) 0.192(7) Uiso 0.20 1 d PG . 2 C53 C 0.0000(4) -0.2506(4) 0.2500(5) 0.094(13) Uiso 0.25 2 d SPG . . C54 C 0.0396(4) -0.2789(3) 0.2865(6) 0.094(13) Uiso 0.25 1 d PG . . C55 C 0.0856(5) -0.3165(3) 0.3073(7) 0.094(13) Uiso 0.25 1 d PG . . C56 C 0.1068(4) -0.2784(3) 0.3549(6) 0.094(13) Uiso 0.25 1 d PG . . C47 C 0.2467(4) -0.2003(3) 0.3648(6) 0.075(9) Uiso 0.25 1 d PG C 1 C48 C 0.2575(3) -0.1850(4) 0.3259(5) 0.075(9) Uiso 0.25 1 d PG C 1 C49 C 0.2596(4) -0.2388(5) 0.3010(6) 0.075(9) Uiso 0.15 1 d PG C 1 C50 C 0.2329(4) -0.2907(4) 0.3127(7) 0.075(9) Uiso 0.15 1 d PG C 1 C51 C 0.2401(5) -0.3149(4) 0.3292(7) 0.075(9) Uiso 0.25 1 d PG C 1 C52 C 0.2478(5) -0.3063(3) 0.3790(7) 0.075(9) Uiso 0.25 1 d PG C 1 C49' C 0.2670(4) -0.2242(5) 0.3084(6) 0.075(9) Uiso 0.10 1 d PG D 2 C50' C 0.2428(4) -0.2593(5) 0.3023(6) 0.075(9) Uiso 0.10 1 d PG D 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 0.0357(9) 0.0511(10) 0.0350(9) 0.0019(8) 0.0136(7) -0.0076(8) N1 0.020(5) 0.051(6) 0.036(5) -0.006(4) 0.011(4) -0.009(4) C1 0.041(8) 0.050(9) 0.031(7) -0.009(6) 0.015(6) 0.000(7) F1 0.068(5) 0.051(5) 0.048(5) -0.001(4) 0.009(4) -0.019(4) Cl1 0.083(3) 0.111(4) 0.042(2) 0.013(2) 0.031(2) 0.019(3) O1 0.070(7) 0.065(7) 0.043(6) 0.003(5) 0.021(5) -0.006(6) Cl2 0.105(3) 0.094(3) 0.038(2) -0.020(2) 0.007(2) 0.020(3) O2 0.122(10) 0.050(6) 0.040(6) 0.001(5) -0.007(6) -0.028(7) N2 0.043(7) 0.046(7) 0.032(6) 0.005(5) 0.023(5) -0.008(5) F2 0.076(6) 0.062(6) 0.068(6) 0.006(4) 0.020(5) -0.019(5) C2 0.035(8) 0.054(9) 0.068(10) -0.009(7) 0.018(7) -0.009(7) N3 0.037(6) 0.044(7) 0.048(7) 0.015(5) 0.012(5) 0.001(5) F3 0.074(6) 0.037(5) 0.131(9) 0.001(5) 0.032(6) -0.011(4) C3 0.056(10) 0.049(9) 0.054(9) -0.017(7) 0.012(7) -0.004(8) N4 0.040(7) 0.063(8) 0.024(6) 0.008(5) 0.009(5) -0.007(6) C4 0.041(8) 0.039(8) 0.047(8) -0.015(6) 0.022(6) -0.009(7) F4 0.097(8) 0.067(6) 0.094(7) -0.040(6) 0.017(6) -0.009(5) N5 0.039(6) 0.033(6) 0.030(6) -0.002(5) 0.015(5) 0.001(5) F5 0.106(8) 0.079(6) 0.045(5) -0.019(5) 0.019(5) -0.019(6) C5 0.057(9) 0.047(8) 0.034(8) -0.012(6) 0.019(7) -0.020(7) C5A 0.034(8) 0.041(8) 0.058(9) -0.010(7) 0.016(6) -0.009(6) C5B 0.044(8) 0.045(9) 0.049(9) -0.004(7) 0.013(7) -0.005(7) C5C 0.029(8) 0.060(10) 0.058(10) 0.001(8) 0.006(7) -0.012(7) C5D 0.037(9) 0.055(11) 0.113(16) -0.006(10) 0.002(9) -0.005(7) C5E 0.045(9) 0.041(9) 0.083(12) -0.019(9) 0.010(8) -0.007(7) C5F 0.052(9) 0.060(11) 0.065(11) -0.014(8) 0.013(8) -0.006(8) F6 0.062(6) 0.108(8) 0.069(6) 0.003(6) 0.022(5) 0.020(5) N6 0.082(10) 0.063(9) 0.043(8) 0.011(7) -0.001(7) -0.028(7) C6 0.020(7) 0.052(9) 0.050(8) -0.002(7) 0.011(6) 0.004(6) F7 0.038(5) 0.100(8) 0.137(9) 0.020(7) 0.029(6) 0.017(5) C7 0.046(9) 0.057(9) 0.055(9) 0.003(7) 0.019(7) -0.015(7) C8 0.027(6) 0.057(7) 0.056(7) 0.007(6) 0.009(5) -0.002(6) F8 0.040(5) 0.080(7) 0.126(9) 0.023(6) 0.000(5) -0.002(5) F9 0.065(6) 0.105(8) 0.088(8) 0.004(6) -0.012(5) -0.007(6) C9 0.032(8) 0.055(9) 0.049(8) 0.003(7) 0.008(6) -0.011(7) F10 0.052(5) 0.088(7) 0.052(5) 0.011(5) 0.007(4) 0.000(5) C10 0.034(7) 0.057(9) 0.049(8) 0.008(7) 0.020(6) 0.000(7) C10A 0.049(9) 0.045(9) 0.069(11) 0.027(8) 0.016(8) -0.001(7) C10B 0.039(9) 0.057(10) 0.068(11) 0.012(8) 0.007(8) 0.005(7) C10C 0.046(10) 0.055(10) 0.099(14) 0.016(9) 0.020(9) 0.013(8) C10D 0.040(7) 0.052(7) 0.075(8) 0.011(6) -0.001(6) -0.003(6) C10E 0.044(9) 0.068(10) 0.052(10) 0.001(8) -0.016(7) -0.014(8) C10F 0.037(8) 0.055(9) 0.069(11) 0.021(8) 0.021(8) -0.004(7) F11 0.121(9) 0.076(7) 0.083(7) -0.012(5) 0.057(7) -0.013(6) C11 0.038(8) 0.064(10) 0.041(8) 0.011(7) 0.007(6) -0.005(7) F12 0.198(15) 0.093(9) 0.135(11) -0.038(8) 0.079(11) -0.009(9) C12 0.047(9) 0.043(9) 0.073(11) 0.026(8) 0.002(8) -0.006(7) F13 0.138(11) 0.051(7) 0.147(11) -0.014(6) 0.003(8) -0.010(6) C13 0.061(10) 0.052(9) 0.059(10) 0.012(8) 0.011(8) 0.002(8) F14 0.077(7) 0.064(6) 0.118(9) 0.033(6) -0.018(6) -0.015(5) C14 0.040(8) 0.045(8) 0.045(8) 0.014(6) 0.023(7) -0.001(7) F15 0.053(5) 0.068(6) 0.079(6) 0.023(5) 0.029(5) 0.000(4) C15 0.040(8) 0.046(8) 0.050(9) -0.006(7) 0.013(6) -0.008(7) C15A 0.041(8) 0.066(10) 0.048(9) -0.001(7) 0.004(7) -0.004(7) C15B 0.084(12) 0.049(10) 0.076(12) 0.003(9) 0.026(10) -0.012(9) C15C 0.116(17) 0.066(13) 0.098(16) -0.020(11) 0.036(13) -0.010(12) C15D 0.094(15) 0.064(13) 0.084(14) -0.003(11) -0.012(11) -0.013(11) C15E 0.073(12) 0.055(11) 0.082(13) 0.010(9) -0.010(10) -0.022(9) C15F 0.053(10) 0.041(9) 0.082(12) 0.025(8) -0.012(9) -0.011(7) C16 0.038(8) 0.053(9) 0.041(8) 0.002(6) 0.025(6) -0.015(7) C17 0.049(9) 0.049(9) 0.045(9) 0.010(7) 0.004(7) -0.019(7) C18 0.040(6) 0.053(7) 0.032(6) 0.008(5) 0.014(5) -0.016(6) C19 0.041(8) 0.058(9) 0.023(7) 0.003(6) 0.010(6) -0.008(7) C20 0.044(8) 0.073(11) 0.024(7) 0.003(7) 0.011(6) -0.004(8) C20A 0.052(9) 0.058(9) 0.035(8) -0.001(7) 0.011(7) -0.011(7) C20B 0.048(9) 0.042(8) 0.035(8) 0.002(6) 0.014(6) -0.011(6) C20C 0.046(9) 0.049(9) 0.045(8) 0.004(7) 0.010(7) -0.008(7) C20D 0.038(8) 0.095(13) 0.050(10) 0.007(9) 0.008(7) -0.006(8) C20E 0.061(11) 0.138(18) 0.054(11) 0.005(11) 0.027(9) -0.001(11) C20F 0.047(7) 0.092(8) 0.047(7) 0.008(6) 0.019(6) -0.001(6) C20G 0.054(9) 0.045(8) 0.038(8) 0.010(7) 0.016(7) 0.019(7) C20H 0.048(9) 0.044(8) 0.043(8) 0.005(7) 0.019(7) 0.006(7) C20I 0.056(9) 0.069(10) 0.029(8) 0.002(7) 0.016(7) 0.032(8) C20J 0.078(11) 0.065(11) 0.028(8) -0.001(7) 0.019(7) 0.025(9) C20K 0.064(10) 0.058(10) 0.043(9) -0.006(8) -0.003(7) 0.018(9) C20L 0.066(10) 0.040(8) 0.039(8) 0.005(6) 0.004(7) -0.014(7) C20M 0.074(11) 0.045(9) 0.041(9) -0.007(7) 0.002(8) -0.014(8) Ni2 0.0375(10) 0.0394(10) 0.0560(11) -0.0056(8) 0.0087(8) -0.0059(8) Cl3 0.039(2) 0.064(2) 0.080(3) -0.003(2) 0.0085(18) -0.0050(18) O3 0.044(6) 0.056(6) 0.060(6) 0.004(5) 0.013(5) -0.013(5) Cl4 0.049(2) 0.046(2) 0.074(3) 0.0010(18) 0.0078(18) -0.0034(17) O4 0.036(5) 0.061(7) 0.086(8) 0.016(6) 0.016(5) -0.004(5) N7 0.047(7) 0.037(6) 0.031(6) -0.006(5) 0.003(5) 0.003(5) N8 0.037(6) 0.039(6) 0.062(8) -0.002(6) 0.010(5) 0.009(5) N9 0.041(7) 0.052(8) 0.069(8) -0.011(6) 0.013(6) 0.002(6) N10 0.046(7) 0.041(6) 0.032(6) -0.007(5) 0.001(5) -0.002(6) N11 0.045(7) 0.029(6) 0.036(6) -0.003(5) 0.010(5) -0.008(5) N12 0.056(9) 0.047(7) 0.066(9) 0.002(6) 0.015(7) -0.009(6) F16 0.103(8) 0.086(7) 0.056(6) -0.010(5) 0.034(5) -0.013(6) F17 0.095(8) 0.098(8) 0.120(9) 0.025(7) 0.062(7) -0.005(6) F18 0.070(7) 0.079(7) 0.175(12) 0.025(7) 0.008(7) -0.037(6) F19 0.145(11) 0.084(8) 0.080(8) -0.008(6) -0.025(7) -0.045(7) F20 0.127(9) 0.070(6) 0.055(6) -0.003(5) 0.025(6) -0.030(6) F21 0.044(5) 0.085(7) 0.130(9) -0.013(6) -0.009(5) 0.011(5) C21 0.047(8) 0.043(8) 0.033(7) -0.009(6) -0.005(6) -0.009(7) C22 0.039(8) 0.039(8) 0.042(8) -0.001(6) 0.003(6) -0.002(6) F22 0.051(6) 0.147(11) 0.139(11) 0.031(9) 0.001(6) 0.037(7) F23 0.086(9) 0.123(11) 0.238(17) 0.054(11) 0.039(9) 0.068(8) C23 0.034(7) 0.046(9) 0.050(8) -0.002(6) 0.010(6) -0.014(6) F24 0.127(11) 0.078(8) 0.212(15) -0.016(9) 0.050(10) 0.046(8) C24 0.033(6) 0.037(6) 0.044(6) -0.004(5) -0.004(5) -0.013(5) F25 0.110(9) 0.072(7) 0.120(10) -0.021(7) 0.019(7) 0.018(6) C25 0.041(8) 0.043(8) 0.040(8) -0.004(6) 0.004(6) -0.010(6) C25A 0.046(8) 0.051(9) 0.039(8) 0.000(7) 0.010(6) -0.007(7) C25B 0.055(9) 0.045(8) 0.049(9) 0.008(7) 0.010(7) 0.004(7) C25C 0.051(9) 0.071(11) 0.066(11) 0.029(9) 0.023(8) 0.003(8) C25D 0.048(10) 0.059(11) 0.099(15) 0.003(10) -0.008(9) -0.010(8) C25E 0.060(11) 0.060(10) 0.077(12) 0.007(9) -0.019(9) -0.028(9) C25F 0.061(10) 0.042(8) 0.047(9) 0.008(7) -0.008(7) -0.018(7) F26 0.093(7) 0.155(10) 0.044(6) 0.000(6) 0.007(5) -0.074(7) C26 0.030(7) 0.036(8) 0.050(8) -0.008(6) 0.008(6) 0.002(6) F27 0.129(11) 0.173(13) 0.122(10) 0.012(9) -0.007(8) -0.113(10) C27 0.051(10) 0.046(9) 0.079(11) -0.004(8) 0.020(8) -0.005(7) F28 0.078(7) 0.101(8) 0.099(8) 0.024(6) 0.022(6) -0.030(6) C28 0.048(10) 0.043(9) 0.085(12) -0.005(8) 0.018(8) -0.006(7) F29 0.081(7) 0.142(10) 0.067(7) 0.002(6) 0.028(5) -0.013(7) C29 0.052(7) 0.042(7) 0.061(7) -0.010(6) 0.011(6) -0.019(6) F30 0.063(6) 0.140(9) 0.056(6) -0.028(6) 0.016(5) -0.027(6) C30 0.043(9) 0.043(9) 0.076(11) -0.001(8) 0.007(7) -0.007(7) C30A 0.039(9) 0.040(9) 0.114(15) 0.001(9) 0.019(9) -0.008(7) C30B 0.046(10) 0.045(10) 0.112(15) 0.006(10) 0.018(10) 0.008(8) C30C 0.038(10) 0.102(15) 0.110(16) 0.008(13) -0.004(10) 0.007(10) C30D 0.075(9) 0.090(9) 0.101(10) 0.004(8) 0.024(8) 0.018(8) C30E 0.066(13) 0.074(14) 0.15(2) 0.002(13) 0.033(13) 0.024(11) C30F 0.077(13) 0.071(13) 0.105(16) -0.003(12) 0.019(12) 0.026(11) C31 0.045(9) 0.047(9) 0.099(13) -0.008(9) 0.011(9) -0.007(8) C32 0.024(8) 0.060(11) 0.141(17) 0.006(11) 0.014(9) 0.002(7) C33 0.049(7) 0.074(8) 0.085(8) 0.010(7) 0.013(7) -0.012(7) C34 0.031(8) 0.030(8) 0.094(12) -0.003(8) 0.001(7) -0.009(6) C35 0.048(9) 0.056(10) 0.049(9) -0.017(7) 0.014(7) -0.012(7) C35A 0.054(9) 0.048(9) 0.066(11) -0.001(8) 0.021(8) -0.014(7) C35B 0.067(11) 0.062(11) 0.073(12) -0.004(9) 0.009(9) -0.038(9) C35C 0.070(12) 0.079(12) 0.077(13) -0.014(10) -0.001(10) -0.035(10) C35D 0.051(10) 0.071(11) 0.079(12) 0.021(9) 0.023(9) -0.021(8) C35E 0.040(9) 0.082(12) 0.064(11) 0.003(9) 0.012(8) -0.009(8) C35F 0.032(8) 0.083(11) 0.053(10) -0.017(8) 0.005(7) 0.007(8) C36 0.056(9) 0.040(8) 0.044(8) -0.010(6) 0.011(7) -0.010(7) C37 0.056(10) 0.046(9) 0.041(8) 0.000(6) 0.008(7) -0.018(7) C38 0.055(9) 0.052(9) 0.041(8) -0.017(7) 0.002(7) -0.008(7) C39 0.036(7) 0.040(8) 0.035(7) -0.007(6) 0.005(6) -0.011(6) C40 0.045(8) 0.037(8) 0.036(8) -0.004(6) -0.004(6) -0.015(6) C40A 0.043(8) 0.041(8) 0.036(7) -0.003(6) 0.004(6) -0.004(6) C40B 0.052(9) 0.044(8) 0.042(8) 0.006(7) 0.013(7) -0.014(7) C40C 0.055(9) 0.041(8) 0.038(8) 0.003(6) 0.023(7) -0.007(7) C40D 0.070(11) 0.034(8) 0.063(10) 0.001(7) 0.034(8) 0.001(7) C40E 0.045(8) 0.045(9) 0.053(9) 0.004(7) 0.007(7) 0.001(7) C40F 0.057(9) 0.049(9) 0.042(8) 0.007(7) 0.006(7) -0.005(7) C40G 0.038(8) 0.040(8) 0.035(7) -0.003(6) 0.004(6) -0.004(6) C40H 0.051(9) 0.058(10) 0.038(8) -0.006(7) 0.004(7) -0.017(8) C40I 0.029(7) 0.036(8) 0.062(9) -0.006(7) -0.001(6) -0.003(6) C40J 0.052(9) 0.040(8) 0.050(9) 0.002(7) 0.007(7) 0.001(7) C40K 0.040(8) 0.037(8) 0.051(9) 0.000(6) 0.016(7) -0.014(6) C40L 0.047(9) 0.047(9) 0.049(9) -0.013(7) 0.012(7) -0.009(7) C40M 0.040(9) 0.040(8) 0.038(8) -0.004(6) 0.012(6) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.925(10) . ? Ni1 N1 1.933(10) . ? Ni1 N3 1.948(10) . ? Ni1 N4 1.948(11) . ? N1 C1 1.360(16) . ? N1 C4 1.386(16) . ? C1 C20 1.391(19) . ? C1 C2 1.453(19) . ? F1 C5B 1.325(9) . ? Cl1 C20I 1.697(15) . ? O1 C20H 1.221(16) . ? Cl2 C20J 1.695(14) . ? O2 C20K 1.235(18) . ? N2 C6 1.370(11) . ? N2 C9 1.383(16) . ? F2 C5C 1.350(10) . ? C2 C3 1.365(19) . ? C2 H2 0.9500 . ? N3 C14 1.366(17) . ? N3 C11 1.372(12) . ? F3 C5D 1.357(9) . ? C3 C4 1.436(19) . ? C3 H3 0.9500 . ? N4 C19 1.367(16) . ? N4 C16 1.379(13) . ? C4 C5 1.362(18) . ? F4 C5E 1.326(10) . ? N5 C20G 1.349(17) . ? N5 C20B 1.408(11) . ? N5 H5A 0.91(2) . ? F5 C5F 1.303(10) . ? C5 C6 1.401(15) . ? C5 C5A 1.501(14) . ? C5A C5B 1.3900 . ? C5A C5F 1.3900 . ? C5B C5C 1.3900 . ? C5C C5D 1.3900 . ? C5D C5E 1.3900 . ? C5E C5F 1.3900 . ? F6 C10B 1.297(8) . ? N6 C20M 1.139(17) . ? C6 C7 1.4210 . ? F7 C10C 1.316(9) . ? C7 C8 1.372(14) . ? C7 H7 0.9500 . ? C8 C9 1.433(18) . ? C8 H8 0.9500 . ? F8 C10D 1.329(10) . ? F9 C10E 1.337(12) . ? C9 C10 1.350(19) . ? F10 C10F 1.325(10) . ? C10 C11 1.391(15) . ? C10 C10A 1.516(14) . ? C10A C10B 1.3900 . ? C10A C10F 1.3900 . ? C10B C10C 1.3900 . ? C10C C10D 1.3900 . ? C10D C10E 1.3900 . ? C10E C10F 1.3900 . ? F11 C15B 1.312(10) . ? C11 C12 1.4405 . ? F12 C15C 1.319(11) . ? C12 C13 1.289(16) . ? C12 H12 0.9500 . ? F13 C15D 1.337(12) . ? C13 C14 1.434(19) . ? C13 H13 0.9500 . ? F14 C15E 1.304(12) . ? C14 C15 1.387(18) . ? F15 C15F 1.333(11) . ? C15 C16 1.399(16) . ? C15 C15A 1.516(15) . ? C15A C15B 1.3900 . ? C15A C15F 1.3900 . ? C15B C15C 1.3900 . ? C15C C15D 1.3900 . ? C15D C15E 1.3900 . ? C15E C15F 1.3900 . ? C16 C17 1.4001 . ? C17 C18 1.346(15) . ? C17 H17 0.9500 . ? C18 C19 1.434(18) . ? C18 H18 0.9500 . ? C19 C20 1.362(19) . ? C20 C20A 1.527(15) . ? C20A C20B 1.3900 . ? C20A C20F 1.3900 . ? C20B C20C 1.3900 . ? C20C C20D 1.3900 . ? C20C H20C 0.9500 . ? C20D C20E 1.3900 . ? C20D H20D 0.9500 . ? C20E C20F 1.3900 . ? C20E H20E 0.9500 . ? C20F H20F 0.9500 . ? C20G C20L 1.346(19) . ? C20G C20H 1.522(18) . ? C20H C20I 1.453(19) . ? C20I C20J 1.37(2) . ? C20J C20K 1.49(2) . ? C20K C20L 1.47(2) . ? C20L C20M 1.45(2) . ? Ni2 N10 1.917(11) . ? Ni2 N9 1.922(11) . ? Ni2 N8 1.934(11) . ? Ni2 N7 1.941(11) . ? Cl3 C40I 1.704(13) . ? O3 C40H 1.225(16) . ? Cl4 C40J 1.706(14) . ? O4 C40K 1.203(15) . ? N7 C21 1.379(16) . ? N7 C24 1.385(16) . ? N8 C26 1.383(12) . ? N8 C29 1.392(18) . ? N9 C31 1.373(13) . ? N9 C34 1.379(18) . ? N10 C39 1.369(16) . ? N10 C36 1.387(12) . ? N11 C40G 1.313(16) . ? N11 C40B 1.420(12) . ? N11 H11A 0.91(2) . ? N12 C40M 1.144(16) . ? F16 C25B 1.299(11) . ? F17 C25C 1.322(11) . ? F18 C25D 1.318(10) . ? F19 C25E 1.308(12) . ? F20 C25F 1.314(11) . ? F21 C30B 1.332(13) . ? C21 C40 1.389(18) . ? C21 C22 1.437(18) . ? C22 C23 1.341(18) . ? C22 H22 0.9500 . ? F22 C30C 1.328(15) . ? F23 C30D 1.352(13) . ? C23 C24 1.431(18) . ? C23 H23 0.9500 . ? F24 C30E 1.299(14) . ? C24 C25 1.368(18) . ? F25 C30F 1.272(14) . ? C25 C26 1.378(14) . ? C25 C25A 1.484(13) . ? C25A C25B 1.3900 . ? C25A C25F 1.3900 . ? C25B C25C 1.3900 . ? C25C C25D 1.3900 . ? C25D C25E 1.3900 . ? C25E C25F 1.3900 . ? F26 C35B 1.325(9) . ? C26 C27 1.4266 . ? F27 C35C 1.317(9) . ? C27 C28 1.337(16) . ? C27 H27 0.9500 . ? F28 C35D 1.320(10) . ? C28 C29 1.42(2) . ? C28 H28 0.9500 . ? F29 C35E 1.304(11) . ? C29 C30 1.350(19) . ? F30 C35F 1.285(11) . ? C30 C31 1.419(16) . ? C30 C30A 1.522(16) . ? C30A C30B 1.3900 . ? C30A C30F 1.3900 . ? C30B C30C 1.3900 . ? C30C C30D 1.3900 . ? C30D C30E 1.3900 . ? C30E C30F 1.3900 . ? C31 C32 1.4202 . ? C32 C33 1.356(18) . ? C32 H32 0.9500 . ? C33 C34 1.40(2) . ? C33 H33 0.9500 . ? C34 C35 1.34(2) . ? C35 C36 1.387(16) . ? C35 C35A 1.553(15) . ? C35A C35B 1.3900 . ? C35A C35F 1.3900 . ? C35B C35C 1.3900 . ? C35C C35D 1.3900 . ? C35D C35E 1.3900 . ? C35E C35F 1.3900 . ? C36 C37 1.4354 . ? C37 C38 1.362(16) . ? C37 H37 0.9500 . ? C38 C39 1.444(19) . ? C38 H38 0.9500 . ? C39 C40 1.403(18) . ? C40 C40A 1.516(14) . ? C40A C40B 1.3900 . ? C40A C40F 1.3900 . ? C40B C40C 1.3900 . ? C40C C40D 1.3900 . ? C40C H40C 0.9500 . ? C40D C40E 1.3900 . ? C40D H40D 0.9500 . ? C40E C40F 1.3900 . ? C40E H40E 0.9500 . ? C40F H40F 0.9500 . ? C40G C40L 1.367(18) . ? C40G C40H 1.516(19) . ? C40H C40I 1.48(2) . ? C40I C40J 1.321(19) . ? C40J C40K 1.504(19) . ? C40K C40L 1.444(19) . ? C40L C40M 1.43(2) . ? C41 C42 1.60(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.2833 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.4470 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.4270 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.5293 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45' C46' 1.4440 . ? C46' C46' 1.65(4) 7_445 ? C53 C54 1.64(2) 2 ? C53 C54 1.6449 . ? C54 C55 1.6892 . ? C55 C56 1.7307 . ? C47 C48 1.3428 . ? C48 C49 1.4512 . ? C49 C50 1.5202 . ? C50 C51 0.7551 . ? C51 C52 1.5236 . ? C49' C50' 1.0884 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 89.8(4) . . ? N2 Ni1 N3 90.4(4) . . ? N1 Ni1 N3 176.4(4) . . ? N2 Ni1 N4 177.6(4) . . ? N1 Ni1 N4 89.8(4) . . ? N3 Ni1 N4 90.2(5) . . ? C1 N1 C4 105.7(11) . . ? C1 N1 Ni1 127.2(9) . . ? C4 N1 Ni1 127.1(8) . . ? N1 C1 C20 125.7(12) . . ? N1 C1 C2 110.5(11) . . ? C20 C1 C2 123.2(12) . . ? C6 N2 C9 103.6(9) . . ? C6 N2 Ni1 128.6(7) . . ? C9 N2 Ni1 127.7(9) . . ? C3 C2 C1 106.6(12) . . ? C3 C2 H2 126.7 . . ? C1 C2 H2 126.7 . . ? C14 N3 C11 106.3(9) . . ? C14 N3 Ni1 127.3(9) . . ? C11 N3 Ni1 126.4(7) . . ? C2 C3 C4 106.5(13) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C19 N4 C16 105.0(10) . . ? C19 N4 Ni1 127.9(9) . . ? C16 N4 Ni1 126.9(8) . . ? C5 C4 N1 126.1(13) . . ? C5 C4 C3 123.2(13) . . ? N1 C4 C3 110.6(11) . . ? C20G N5 C20B 123.4(10) . . ? C20G N5 H5A 110(8) . . ? C20B N5 H5A 126(8) . . ? C4 C5 C6 122.1(11) . . ? C4 C5 C5A 119.6(12) . . ? C6 C5 C5A 118.0(9) . . ? C5B C5A C5F 120.0 . . ? C5B C5A C5 121.4(5) . . ? C5F C5A C5 118.6(5) . . ? F1 C5B C5A 120.7(4) . . ? F1 C5B C5C 119.3(4) . . ? C5A C5B C5C 120.0 . . ? F2 C5C C5B 119.4(5) . . ? F2 C5C C5D 120.6(5) . . ? C5B C5C C5D 120.0 . . ? F3 C5D C5C 119.5(6) . . ? F3 C5D C5E 120.5(6) . . ? C5C C5D C5E 120.0 . . ? F4 C5E C5F 120.8(6) . . ? F4 C5E C5D 119.1(6) . . ? C5F C5E C5D 120.0 . . ? F5 C5F C5E 118.0(4) . . ? F5 C5F C5A 122.0(4) . . ? C5E C5F C5A 120.0 . . ? N2 C6 C5 124.1(7) . . ? N2 C6 C7 113.1(5) . . ? C5 C6 C7 122.6(5) . . ? C8 C7 C6 105.3(6) . . ? C8 C7 H7 127.4 . . ? C6 C7 H7 127.4 . . ? C7 C8 C9 106.9(10) . . ? C7 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? C10 C9 N2 124.9(12) . . ? C10 C9 C8 124.0(12) . . ? N2 C9 C8 111.0(12) . . ? C9 C10 C11 123.8(12) . . ? C9 C10 C10A 117.7(11) . . ? C11 C10 C10A 118.1(10) . . ? C10B C10A C10F 120.0 . . ? C10B C10A C10 120.0(6) . . ? C10F C10A C10 119.6(6) . . ? F6 C10B C10A 121.4(4) . . ? F6 C10B C10C 118.6(4) . . ? C10A C10B C10C 120.0 . . ? F7 C10C C10D 119.2(5) . . ? F7 C10C C10B 120.8(5) . . ? C10D C10C C10B 120.0 . . ? F8 C10D C10C 120.1(7) . . ? F8 C10D C10E 119.8(7) . . ? C10C C10D C10E 120.0 . . ? F9 C10E C10D 120.9(6) . . ? F9 C10E C10F 119.1(6) . . ? C10D C10E C10F 120.0 . . ? F10 C10F C10E 118.9(5) . . ? F10 C10F C10A 121.1(5) . . ? C10E C10F C10A 120.0 . . ? N3 C11 C10 124.6(9) . . ? N3 C11 C12 108.3(5) . . ? C10 C11 C12 126.3(6) . . ? C13 C12 C11 108.2(8) . . ? C13 C12 H12 125.9 . . ? C11 C12 H12 125.9 . . ? C12 C13 C14 108.3(12) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? N3 C14 C15 125.6(12) . . ? N3 C14 C13 108.8(12) . . ? C15 C14 C13 125.6(13) . . ? C14 C15 C16 122.4(12) . . ? C14 C15 C15A 117.2(11) . . ? C16 C15 C15A 120.4(10) . . ? C15B C15A C15F 120.0 . . ? C15B C15A C15 119.2(6) . . ? C15F C15A C15 120.8(6) . . ? F11 C15B C15A 120.3(5) . . ? F11 C15B C15C 119.7(5) . . ? C15A C15B C15C 120.0 . . ? F12 C15C C15D 122.2(7) . . ? F12 C15C C15B 117.8(7) . . ? C15D C15C C15B 120.0 . . ? F13 C15D C15C 118.1(9) . . ? F13 C15D C15E 121.9(9) . . ? C15C C15D C15E 120.0 . . ? F14 C15E C15F 121.8(8) . . ? F14 C15E C15D 118.2(8) . . ? C15F C15E C15D 120.0 . . ? F15 C15F C15E 118.1(5) . . ? F15 C15F C15A 121.9(6) . . ? C15E C15F C15A 120.0 . . ? N4 C16 C15 124.6(9) . . ? N4 C16 C17 112.0(7) . . ? C15 C16 C17 123.2(6) . . ? C18 C17 C16 105.5(7) . . ? C18 C17 H17 127.3 . . ? C16 C17 H17 127.3 . . ? C17 C18 C19 108.6(11) . . ? C17 C18 H18 125.7 . . ? C19 C18 H18 125.7 . . ? C20 C19 N4 125.3(12) . . ? C20 C19 C18 125.7(13) . . ? N4 C19 C18 108.8(12) . . ? C19 C20 C1 122.4(12) . . ? C19 C20 C20A 120.1(12) . . ? C1 C20 C20A 117.1(12) . . ? C20B C20A C20F 120.0 . . ? C20B C20A C20 121.3(7) . . ? C20F C20A C20 118.6(7) . . ? C20A C20B C20C 120.0 . . ? C20A C20B N5 120.7(7) . . ? C20C C20B N5 119.3(7) . . ? C20D C20C C20B 120.0 . . ? C20D C20C H20C 120.0 . . ? C20B C20C H20C 120.0 . . ? C20E C20D C20C 120.0 . . ? C20E C20D H20D 120.0 . . ? C20C C20D H20D 120.0 . . ? C20D C20E C20F 120.0 . . ? C20D C20E H20E 120.0 . . ? C20F C20E H20E 120.0 . . ? C20E C20F C20A 120.0 . . ? C20E C20F H20F 120.0 . . ? C20A C20F H20F 120.0 . . ? C20L C20G N5 128.8(12) . . ? C20L C20G C20H 119.0(13) . . ? N5 C20G C20H 112.1(12) . . ? O1 C20H C20I 122.1(13) . . ? O1 C20H C20G 118.8(12) . . ? C20I C20H C20G 119.2(14) . . ? C20J C20I C20H 119.5(13) . . ? C20J C20I Cl1 122.7(11) . . ? C20H C20I Cl1 117.7(13) . . ? C20I C20J C20K 122.1(13) . . ? C20I C20J Cl2 121.6(11) . . ? C20K C20J Cl2 116.3(13) . . ? O2 C20K C20L 122.0(14) . . ? O2 C20K C20J 120.7(13) . . ? C20L C20K C20J 117.3(15) . . ? C20G C20L C20M 123.8(13) . . ? C20G C20L C20K 122.4(13) . . ? C20M C20L C20K 113.7(13) . . ? N6 C20M C20L 173.8(17) . . ? N10 Ni2 N9 90.4(5) . . ? N10 Ni2 N8 179.4(5) . . ? N9 Ni2 N8 90.2(5) . . ? N10 Ni2 N7 89.3(4) . . ? N9 Ni2 N7 179.7(5) . . ? N8 Ni2 N7 90.1(4) . . ? C21 N7 C24 106.1(10) . . ? C21 N7 Ni2 127.1(9) . . ? C24 N7 Ni2 126.7(8) . . ? C26 N8 C29 106.6(9) . . ? C26 N8 Ni2 125.8(7) . . ? C29 N8 Ni2 127.6(9) . . ? C31 N9 C34 104.1(10) . . ? C31 N9 Ni2 127.6(9) . . ? C34 N9 Ni2 128.3(10) . . ? C39 N10 C36 104.8(9) . . ? C39 N10 Ni2 128.3(9) . . ? C36 N10 Ni2 126.8(8) . . ? C40G N11 C40B 125.4(9) . . ? C40G N11 H11A 127(8) . . ? C40B N11 H11A 105(8) . . ? N7 C21 C40 125.4(12) . . ? N7 C21 C22 109.5(11) . . ? C40 C21 C22 124.6(13) . . ? C23 C22 C21 107.1(12) . . ? C23 C22 H22 126.5 . . ? C21 C22 H22 126.5 . . ? C22 C23 C24 108.0(11) . . ? C22 C23 H23 126.0 . . ? C24 C23 H23 126.0 . . ? C25 C24 N7 125.6(12) . . ? C25 C24 C23 124.7(12) . . ? N7 C24 C23 109.1(11) . . ? C24 C25 C26 121.2(11) . . ? C24 C25 C25A 121.2(11) . . ? C26 C25 C25A 117.3(10) . . ? C25B C25A C25F 120.0 . . ? C25B C25A C25 121.0(5) . . ? C25F C25A C25 118.9(5) . . ? F16 C25B C25C 118.7(5) . . ? F16 C25B C25A 121.3(5) . . ? C25C C25B C25A 120.0 . . ? F17 C25C C25B 120.9(6) . . ? F17 C25C C25D 119.1(6) . . ? C25B C25C C25D 120.0 . . ? F18 C25D C25E 120.3(7) . . ? F18 C25D C25C 119.7(7) . . ? C25E C25D C25C 120.0 . . ? F19 C25E C25F 121.0(6) . . ? F19 C25E C25D 119.0(6) . . ? C25F C25E C25D 120.0 . . ? F20 C25F C25E 119.1(5) . . ? F20 C25F C25A 120.8(5) . . ? C25E C25F C25A 120.0 . . ? C25 C26 N8 126.8(8) . . ? C25 C26 C27 124.7(6) . . ? N8 C26 C27 108.2(5) . . ? C28 C27 C26 108.8(7) . . ? C28 C27 H27 125.6 . . ? C26 C27 H27 125.6 . . ? C27 C28 C29 107.4(13) . . ? C27 C28 H28 126.3 . . ? C29 C28 H28 126.3 . . ? C30 C29 N8 123.8(13) . . ? C30 C29 C28 127.0(15) . . ? N8 C29 C28 108.8(12) . . ? C29 C30 C31 123.8(13) . . ? C29 C30 C30A 120.7(12) . . ? C31 C30 C30A 115.2(10) . . ? C30B C30A C30F 120.0 . . ? C30B C30A C30 119.2(7) . . ? C30F C30A C30 120.8(7) . . ? F21 C30B C30A 122.2(7) . . ? F21 C30B C30C 117.8(7) . . ? C30A C30B C30C 120.0 . . ? F22 C30C C30D 119.5(8) . . ? F22 C30C C30B 120.5(9) . . ? C30D C30C C30B 120.0 . . ? F23 C30D C30C 118.4(11) . . ? F23 C30D C30E 121.5(11) . . ? C30C C30D C30E 120.0 . . ? F24 C30E C30D 117.5(10) . . ? F24 C30E C30F 122.5(10) . . ? C30D C30E C30F 120.0 . . ? F25 C30F C30E 117.3(7) . . ? F25 C30F C30A 122.6(7) . . ? C30E C30F C30A 120.0 . . ? N9 C31 C30 123.8(10) . . ? N9 C31 C32 112.2(7) . . ? C30 C31 C32 123.8(6) . . ? C33 C32 C31 104.6(9) . . ? C33 C32 H32 127.7 . . ? C31 C32 H32 127.7 . . ? C32 C33 C34 108.8(13) . . ? C32 C33 H33 125.6 . . ? C34 C33 H33 125.6 . . ? C35 C34 N9 123.4(13) . . ? C35 C34 C33 126.3(14) . . ? N9 C34 C33 110.1(13) . . ? C34 C35 C36 125.2(13) . . ? C34 C35 C35A 117.0(12) . . ? C36 C35 C35A 117.6(11) . . ? C35B C35A C35F 120.0 . . ? C35B C35A C35 118.4(6) . . ? C35F C35A C35 121.3(6) . . ? F26 C35B C35A 121.4(5) . . ? F26 C35B C35C 118.6(5) . . ? C35A C35B C35C 120.0 . . ? F27 C35C C35D 121.4(6) . . ? F27 C35C C35B 118.6(6) . . ? C35D C35C C35B 120.0 . . ? F28 C35D C35C 120.3(8) . . ? F28 C35D C35E 119.6(8) . . ? C35C C35D C35E 120.0 . . ? F29 C35E C35F 122.6(7) . . ? F29 C35E C35D 117.2(7) . . ? C35F C35E C35D 120.0 . . ? F30 C35F C35E 118.5(6) . . ? F30 C35F C35A 121.5(6) . . ? C35E C35F C35A 120.0 . . ? N10 C36 C35 123.6(10) . . ? N10 C36 C37 110.4(7) . . ? C35 C36 C37 125.5(6) . . ? C38 C37 C36 107.4(8) . . ? C38 C37 H37 126.3 . . ? C36 C37 H37 126.3 . . ? C37 C38 C39 105.7(12) . . ? C37 C38 H38 127.1 . . ? C39 C38 H38 127.1 . . ? N10 C39 C40 125.6(12) . . ? N10 C39 C38 111.6(11) . . ? C40 C39 C38 122.7(12) . . ? C21 C40 C39 120.3(12) . . ? C21 C40 C40A 121.8(11) . . ? C39 C40 C40A 117.9(10) . . ? C40B C40A C40F 120.0 . . ? C40B C40A C40 120.1(5) . . ? C40F C40A C40 119.9(5) . . ? C40C C40B C40A 120.0 . . ? C40C C40B N11 119.3(5) . . ? C40A C40B N11 120.6(5) . . ? C40D C40C C40B 120.0 . . ? C40D C40C H40C 120.0 . . ? C40B C40C H40C 120.0 . . ? C40C C40D C40E 120.0 . . ? C40C C40D H40D 120.0 . . ? C40E C40D H40D 120.0 . . ? C40F C40E C40D 120.0 . . ? C40F C40E H40E 120.0 . . ? C40D C40E H40E 120.0 . . ? C40E C40F C40A 120.0 . . ? C40E C40F H40F 120.0 . . ? C40A C40F H40F 120.0 . . ? N11 C40G C40L 128.2(13) . . ? N11 C40G C40H 114.0(11) . . ? C40L C40G C40H 117.8(12) . . ? O3 C40H C40I 122.4(13) . . ? O3 C40H C40G 119.7(13) . . ? C40I C40H C40G 117.8(12) . . ? C40J C40I C40H 121.1(12) . . ? C40J C40I Cl3 123.7(11) . . ? C40H C40I Cl3 115.3(10) . . ? C40I C40J C40K 121.7(12) . . ? C40I C40J Cl4 123.6(11) . . ? C40K C40J Cl4 114.7(10) . . ? O4 C40K C40L 122.5(13) . . ? O4 C40K C40J 120.3(12) . . ? C40L C40K C40J 117.0(11) . . ? C40G C40L C40M 121.4(13) . . ? C40G C40L C40K 123.4(13) . . ? C40M C40L C40K 115.2(12) . . ? N12 C40M C40L 178.7(15) . . ? C43 C42 C41 129.1(15) . . ? C43 C42 H42A 105.0 . . ? C41 C42 H42A 105.0 . . ? C43 C42 H42B 105.0 . . ? C41 C42 H42B 105.0 . . ? H42A C42 H42B 105.9 . . ? C42 C43 C44 126.0 . . ? C42 C43 H43A 105.8 . . ? C44 C43 H43A 105.8 . . ? C42 C43 H43B 105.8 . . ? C44 C43 H43B 105.8 . . ? H43A C43 H43B 106.2 . . ? C45 C44 C43 111.8 . . ? C45 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C45 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 115.5 . . ? C44 C45 H45A 108.4 . . ? C46 C45 H45A 108.4 . . ? C44 C45 H45B 108.4 . . ? C46 C45 H45B 108.4 . . ? H45A C45 H45B 107.5 . . ? C45' C46' C46' 114.3(10) . 7_445 ? C54 C53 C54 134.1(3) 2 . ? C53 C54 C55 159.6 . . ? C54 C55 C56 103.9 . . ? C47 C48 C49 107.2 . . ? C48 C49 C50 116.6 . . ? C51 C50 C49 127.8 . . ? C50 C51 C52 124.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11A N6 0.91(2) 2.00(5) 2.868(12) 160(11) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.028 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.139