# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hong Wang' _publ_contact_author_email wangh3@muohio.edu loop_ _publ_author_name 'Lin Jiang' 'Ross Zaenglein' 'James Engle' 'Chris Mittal' 'Christopher Hartley' 'Christopher Ziegler' 'Hong Wang' data_p1bar _database_code_depnum_ccdc_archive 'CCDC 865552' #TrackingRef '- 4a-r-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C149.50 H121.50 N19.50 Ni' _chemical_formula_weight 2249.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6976(4) _cell_length_b 21.9195(5) _cell_length_c 22.0585(5) _cell_angle_alpha 97.683(2) _cell_angle_beta 101.995(2) _cell_angle_gamma 96.078(2) _cell_volume 5894.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9321 _cell_measurement_theta_min 5.83 _cell_measurement_theta_max 65.52 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2366 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8157 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details 'SADABS; [Sheldrick, G. M. (2004)]' _exptl_special_details ; Estimated minimum and maximum transmission: 0.8467 1.0000 Data collected was from a poorly defracting crystal sample; this resulted in a lower than ideal theta(max) value. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60475 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.19 _diffrn_reflns_theta_max 61.00 _reflns_number_total 17351 _reflns_number_gt 12877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Hydrogen atoms were assigned ideal positions and refined isotropically as riding atoms. The Platon program was used to remove disordered solvent molecules, approximately 0.5 pyridine molecules per unit cell were modeled without specific atom positions using the SQUEEZE program. However, the formula weight, F(OOO), density and other parameters reflect the full formula. Nitrogen atoms in the assigned pyridine solvent molecules were assigned to the position that provided the best refinement. ; _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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17351 _refine_ls_number_parameters 1512 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2723 _refine_ls_wR_factor_gt 0.2499 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4205(3) 0.21899(15) 0.40973(15) 0.0330(9) Uani 1 1 d . . . C2 C 0.4008(3) 0.25516(16) 0.46584(16) 0.0343(9) Uani 1 1 d . . . C3 C 0.4066(3) 0.24339(17) 0.52747(15) 0.0350(9) Uani 1 1 d . . . H3 H 0.4244 0.2046 0.5381 0.042 Uiso 1 1 calc R . . C4 C 0.3864(3) 0.28781(17) 0.57253(16) 0.0373(9) Uani 1 1 d . . . C5 C 0.3879(4) 0.27056(16) 0.63585(16) 0.0398(10) Uani 1 1 d . . . C6 C 0.4691(4) 0.23880(17) 0.66357(16) 0.0415(10) Uani 1 1 d . . . H6 H 0.5252 0.2287 0.6430 0.050 Uiso 1 1 calc R . . C7 C 0.4669(4) 0.22188(18) 0.72199(18) 0.0468(11) Uani 1 1 d . . . H7 H 0.5224 0.1995 0.7399 0.056 Uiso 1 1 calc R . . C8 C 0.3172(4) 0.2659(2) 0.7277(2) 0.0555(12) Uani 1 1 d . . . H8 H 0.2641 0.2767 0.7503 0.067 Uiso 1 1 calc R . . C9 C 0.3102(4) 0.2838(2) 0.6692(2) 0.0510(11) Uani 1 1 d . . . H9 H 0.2524 0.3051 0.6523 0.061 Uiso 1 1 calc R . . C10 C 0.3629(3) 0.34637(17) 0.55676(16) 0.0385(9) Uani 1 1 d . . . C11 C 0.3588(3) 0.40039(17) 0.60491(16) 0.0392(9) Uani 1 1 d . . . C12 C 0.4387(4) 0.41691(17) 0.66021(16) 0.0399(9) Uani 1 1 d . . . H12 H 0.4953 0.3922 0.6694 0.048 Uiso 1 1 calc R . . C13 C 0.4352(4) 0.46969(19) 0.70180(17) 0.0479(11) Uani 1 1 d . . . H13 H 0.4909 0.4799 0.7391 0.058 Uiso 1 1 calc R . . C14 C 0.2824(4) 0.4911(2) 0.6391(2) 0.0538(12) Uani 1 1 d . . . H14 H 0.2269 0.5167 0.6312 0.065 Uiso 1 1 calc R . . C15 C 0.2800(4) 0.43973(19) 0.59475(18) 0.0465(11) Uani 1 1 d . . . H15 H 0.2245 0.4313 0.5573 0.056 Uiso 1 1 calc R . . C16 C 0.3498(3) 0.35636(16) 0.49489(15) 0.0336(9) Uani 1 1 d . . . H16 H 0.3293 0.3945 0.4838 0.040 Uiso 1 1 calc R . . C17 C 0.3668(3) 0.30997(15) 0.44865(16) 0.0322(8) Uani 1 1 d . . . C18 C 0.3595(3) 0.30508(16) 0.38080(15) 0.0314(8) Uani 1 1 d . . . C19 C 0.3309(3) 0.34986(15) 0.34319(15) 0.0302(8) Uani 1 1 d . . . C20 C 0.3188(3) 0.41294(15) 0.37616(14) 0.0315(9) Uani 1 1 d . . . C21 C 0.4082(3) 0.45706(17) 0.40232(15) 0.0374(9) Uani 1 1 d . . . H21 H 0.4791 0.4483 0.4002 0.045 Uiso 1 1 calc R . . C22 C 0.3928(4) 0.51576(17) 0.43244(17) 0.0458(11) Uani 1 1 d . . . H22 H 0.4544 0.5461 0.4507 0.055 Uiso 1 1 calc R . . C23 C 0.2898(4) 0.53009(19) 0.43596(19) 0.0475(11) Uani 1 1 d . . . C24 C 0.2030(4) 0.48436(18) 0.41018(18) 0.0465(10) Uani 1 1 d . . . H24 H 0.1320 0.4923 0.4131 0.056 Uiso 1 1 calc R . . C25 C 0.2164(4) 0.42746(17) 0.38031(16) 0.0393(10) Uani 1 1 d . . . H25 H 0.1544 0.3974 0.3621 0.047 Uiso 1 1 calc R . . C26 C 0.2705(5) 0.5931(2) 0.4657(2) 0.0697(15) Uani 1 1 d . . . H26 H 0.1909 0.5910 0.4640 0.084 Uiso 1 1 calc R . . C27 C 0.3284(7) 0.6113(3) 0.5325(2) 0.097(2) Uani 1 1 d . . . H27A H 0.3131 0.5776 0.5558 0.145 Uiso 1 1 calc R . . H27B H 0.3036 0.6490 0.5505 0.145 Uiso 1 1 calc R . . H27C H 0.4068 0.6193 0.5353 0.145 Uiso 1 1 calc R . . C28 C 0.2998(10) 0.6419(3) 0.4303(3) 0.139(4) Uani 1 1 d . . . H28A H 0.2854 0.6819 0.4502 0.209 Uiso 1 1 calc R . . H28B H 0.2564 0.6321 0.3871 0.209 Uiso 1 1 calc R . . H28C H 0.3772 0.6442 0.4300 0.209 Uiso 1 1 calc R . . C29 C 0.3084(3) 0.34178(15) 0.27696(15) 0.0300(8) Uani 1 1 d . . . C30 C 0.2828(3) 0.38934(15) 0.23756(15) 0.0312(8) Uani 1 1 d . . . C31 C 0.2863(3) 0.45348(15) 0.24920(15) 0.0317(8) Uani 1 1 d . . . H31 H 0.3040 0.4745 0.2913 0.038 Uiso 1 1 calc R . . C32 C 0.2643(3) 0.48740(16) 0.20005(16) 0.0338(9) Uani 1 1 d . . . C33 C 0.2756(3) 0.55609(16) 0.21409(15) 0.0364(9) Uani 1 1 d . . . C34 C 0.2227(4) 0.58620(18) 0.25552(18) 0.0462(10) Uani 1 1 d . . . H34 H 0.1782 0.5631 0.2765 0.055 Uiso 1 1 calc R . . C35 C 0.2356(4) 0.6504(2) 0.2659(2) 0.0552(12) Uani 1 1 d . . . H35 H 0.1967 0.6700 0.2936 0.066 Uiso 1 1 calc R . . C36 C 0.3500(4) 0.65748(19) 0.2015(2) 0.0551(12) Uani 1 1 d . . . H36 H 0.3962 0.6822 0.1828 0.066 Uiso 1 1 calc R . . C37 C 0.3414(4) 0.59387(17) 0.18671(18) 0.0438(10) Uani 1 1 d . . . H37 H 0.3800 0.5758 0.1580 0.053 Uiso 1 1 calc R . . C38 C 0.2367(3) 0.45535(16) 0.13665(15) 0.0321(8) Uani 1 1 d . . . C39 C 0.2076(3) 0.48754(16) 0.08145(16) 0.0373(9) Uani 1 1 d . . . C40 C 0.1346(3) 0.53001(17) 0.07777(17) 0.0399(10) Uani 1 1 d . . . H40 H 0.1032 0.5417 0.1123 0.048 Uiso 1 1 calc R . . C41 C 0.1073(4) 0.55558(18) 0.02309(18) 0.0478(11) Uani 1 1 d . . . H41 H 0.0566 0.5845 0.0216 0.057 Uiso 1 1 calc R . . C42 C 0.2172(4) 0.5007(2) -0.02352(18) 0.0495(11) Uani 1 1 d . . . H42 H 0.2468 0.4898 -0.0590 0.059 Uiso 1 1 calc R . . C43 C 0.2495(4) 0.47230(19) 0.02828(18) 0.0452(10) Uani 1 1 d . . . H43 H 0.2993 0.4429 0.0278 0.054 Uiso 1 1 calc R . . C44 C 0.2314(3) 0.39183(16) 0.12576(15) 0.0335(9) Uani 1 1 d . . . H44 H 0.2117 0.3704 0.0838 0.040 Uiso 1 1 calc R . . C45 C 0.2543(3) 0.35810(16) 0.17497(15) 0.0331(9) Uani 1 1 d . . . C46 C 0.2620(3) 0.29232(15) 0.17787(15) 0.0323(9) Uani 1 1 d . . . C47 C 0.2325(3) 0.24333(16) 0.12665(15) 0.0341(9) Uani 1 1 d . . . C48 C 0.1669(3) 0.25796(15) 0.06619(16) 0.0375(10) Uani 1 1 d . . . C49 C 0.0607(4) 0.26709(17) 0.06124(18) 0.0449(11) Uani 1 1 d . . . H49 H 0.0284 0.2638 0.0960 0.054 Uiso 1 1 calc R . . C50 C -0.0014(4) 0.2812(2) 0.0059(2) 0.0586(13) Uani 1 1 d . . . H50 H -0.0753 0.2868 0.0035 0.070 Uiso 1 1 calc R . . C51 C 0.0432(5) 0.2872(2) -0.0450(2) 0.0600(14) Uani 1 1 d . . . C52 C 0.1515(5) 0.27843(19) -0.04041(18) 0.0566(14) Uani 1 1 d . . . H52 H 0.1838 0.2827 -0.0750 0.068 Uiso 1 1 calc R . . C53 C 0.2142(4) 0.26312(17) 0.01526(16) 0.0445(11) Uani 1 1 d . . . H53 H 0.2876 0.2565 0.0177 0.053 Uiso 1 1 calc R . . C54 C -0.0242(6) 0.3022(3) -0.1049(2) 0.090(2) Uani 1 1 d D . . H54 H -0.0868 0.3203 -0.0920 0.108 Uiso 1 1 calc R . . C55 C 0.0328(5) 0.3529(3) -0.1309(2) 0.0702(15) Uani 1 1 d . . . H55A H 0.0974 0.3391 -0.1431 0.105 Uiso 1 1 calc R . . H55B H 0.0546 0.3902 -0.0988 0.105 Uiso 1 1 calc R . . H55C H -0.0165 0.3626 -0.1678 0.105 Uiso 1 1 calc R . . C56 C -0.0722(7) 0.2488(3) -0.1496(3) 0.115(3) Uani 1 1 d D . . H56A H -0.1231 0.2609 -0.1844 0.172 Uiso 1 1 calc R . . H56B H -0.1115 0.2192 -0.1297 0.172 Uiso 1 1 calc R . . H56C H -0.0154 0.2294 -0.1657 0.172 Uiso 1 1 calc R . . C57 C 0.2577(3) 0.18252(15) 0.12662(15) 0.0318(8) Uani 1 1 d . . . C58 C 0.2226(3) 0.13115(15) 0.07387(15) 0.0309(8) Uani 1 1 d . . . C59 C 0.1438(3) 0.12131(16) 0.01726(15) 0.0329(9) Uani 1 1 d . . . H59 H 0.1010 0.1530 0.0067 0.040 Uiso 1 1 calc R . . C60 C 0.1280(3) 0.06483(16) -0.02375(15) 0.0322(8) Uani 1 1 d . . . C61 C 0.0407(3) 0.05538(16) -0.08152(14) 0.0319(8) Uani 1 1 d . . . C62 C 0.0198(4) 0.10188(18) -0.11717(16) 0.0425(10) Uani 1 1 d . . . H62 H 0.0633 0.1414 -0.1052 0.051 Uiso 1 1 calc R . . C63 C -0.0643(4) 0.0910(2) -0.17031(17) 0.0477(11) Uani 1 1 d . . . H63 H -0.0771 0.1243 -0.1932 0.057 Uiso 1 1 calc R . . C64 C -0.1078(3) -0.0080(2) -0.15699(17) 0.0430(10) Uani 1 1 d . . . H64 H -0.1515 -0.0474 -0.1710 0.052 Uiso 1 1 calc R . . C65 C -0.0278(3) -0.00136(18) -0.10278(16) 0.0373(9) Uani 1 1 d . . . H65 H -0.0192 -0.0350 -0.0799 0.045 Uiso 1 1 calc R . . C66 C 0.1929(3) 0.01842(16) -0.00755(16) 0.0333(9) Uani 1 1 d . . . C67 C 0.1900(3) -0.04103(17) -0.04943(17) 0.0366(9) Uani 1 1 d . . . C68 C 0.1769(3) -0.09836(18) -0.02753(19) 0.0441(10) Uani 1 1 d . . . H68 H 0.1647 -0.0997 0.0133 0.053 Uiso 1 1 calc R . . C69 C 0.1821(4) -0.15228(19) -0.0661(2) 0.0507(11) Uani 1 1 d . . . H69 H 0.1716 -0.1906 -0.0510 0.061 Uiso 1 1 calc R . . C70 C 0.2157(4) -0.1004(2) -0.1439(2) 0.0511(11) Uani 1 1 d . . . H70 H 0.2318 -0.1009 -0.1841 0.061 Uiso 1 1 calc R . . C71 C 0.2089(3) -0.0423(2) -0.10909(18) 0.0444(10) Uani 1 1 d . . . H71 H 0.2171 -0.0051 -0.1264 0.053 Uiso 1 1 calc R . . C72 C 0.2671(3) 0.02735(16) 0.04985(15) 0.0324(8) Uani 1 1 d . . . H72 H 0.3074 -0.0051 0.0614 0.039 Uiso 1 1 calc R . . C73 C 0.2828(3) 0.08341(15) 0.09058(15) 0.0306(8) Uani 1 1 d . . . C74 C 0.3495(3) 0.10577(15) 0.15458(15) 0.0295(8) Uani 1 1 d . . . C75 C 0.4205(3) 0.07279(15) 0.18938(15) 0.0306(8) Uani 1 1 d . . . C76 C 0.4455(3) 0.01310(16) 0.15602(15) 0.0322(9) Uani 1 1 d . . . C77 C 0.3970(3) -0.04369(16) 0.16589(16) 0.0342(9) Uani 1 1 d . . . H77 H 0.3534 -0.0449 0.1960 0.041 Uiso 1 1 calc R . . C78 C 0.4128(3) -0.09852(17) 0.13139(16) 0.0390(10) Uani 1 1 d . . . H78 H 0.3791 -0.1370 0.1383 0.047 Uiso 1 1 calc R . . C79 C 0.4766(3) -0.09879(17) 0.08700(16) 0.0378(9) Uani 1 1 d . . . C80 C 0.5256(3) -0.04187(17) 0.07874(16) 0.0362(9) Uani 1 1 d . . . H80 H 0.5705 -0.0405 0.0493 0.043 Uiso 1 1 calc R . . C81 C 0.5100(3) 0.01369(16) 0.11320(15) 0.0326(9) Uani 1 1 d . . . H81 H 0.5444 0.0522 0.1068 0.039 Uiso 1 1 calc R . . C82 C 0.4901(4) -0.15965(18) 0.04993(17) 0.0434(10) Uani 1 1 d . . . H82 H 0.4253 -0.1902 0.0491 0.052 Uiso 1 1 calc R . . C83 C 0.4925(4) -0.1547(2) -0.01904(18) 0.0529(12) Uani 1 1 d . . . H83A H 0.4276 -0.1379 -0.0387 0.079 Uiso 1 1 calc R . . H83B H 0.4938 -0.1960 -0.0420 0.079 Uiso 1 1 calc R . . H83C H 0.5577 -0.1270 -0.0202 0.079 Uiso 1 1 calc R . . C84 C 0.5878(5) -0.1848(2) 0.0815(2) 0.0616(14) Uani 1 1 d . . . H84A H 0.6532 -0.1560 0.0830 0.092 Uiso 1 1 calc R . . H84B H 0.5921 -0.2253 0.0580 0.092 Uiso 1 1 calc R . . H84C H 0.5823 -0.1896 0.1243 0.092 Uiso 1 1 calc R . . C85 C 0.4708(3) 0.08929(15) 0.25401(15) 0.0306(8) Uani 1 1 d . . . C86 C 0.5520(3) 0.05767(16) 0.28902(15) 0.0322(8) Uani 1 1 d . . . C87 C 0.6191(3) 0.01517(16) 0.27220(16) 0.0327(8) Uani 1 1 d . . . H87 H 0.6130 0.0000 0.2290 0.039 Uiso 1 1 calc R . . C88 C 0.6949(3) -0.00543(16) 0.31711(17) 0.0365(9) Uani 1 1 d . . . C89 C 0.7690(3) -0.04738(16) 0.29592(16) 0.0350(9) Uani 1 1 d . . . C90 C 0.7299(3) -0.09827(17) 0.24805(17) 0.0395(9) Uani 1 1 d . . . H90 H 0.6550 -0.1064 0.2278 0.047 Uiso 1 1 calc R . . C91 C 0.8018(4) -0.13665(19) 0.23049(19) 0.0448(10) Uani 1 1 d . . . H91 H 0.7733 -0.1714 0.1985 0.054 Uiso 1 1 calc R . . C92 C 0.9449(4) -0.07816(18) 0.30043(19) 0.0443(10) Uani 1 1 d . . . H92 H 1.0208 -0.0703 0.3185 0.053 Uiso 1 1 calc R . . C93 C 0.8808(3) -0.03790(18) 0.32192(17) 0.0398(9) Uani 1 1 d . . . H93 H 0.9120 -0.0037 0.3542 0.048 Uiso 1 1 calc R . . C94 C 0.6995(3) 0.01559(18) 0.38145(16) 0.0390(9) Uani 1 1 d . . . C95 C 0.7682(4) -0.0093(2) 0.43318(18) 0.0515(12) Uani 1 1 d . . . C96 C 0.7677(4) -0.0727(3) 0.4338(2) 0.0631(14) Uani 1 1 d . . . H96 H 0.7270 -0.1021 0.3991 0.076 Uiso 1 1 calc R . . C97 C 0.8273(6) -0.0921(3) 0.4857(3) 0.088(2) Uani 1 1 d . . . H97 H 0.8235 -0.1355 0.4863 0.105 Uiso 1 1 calc R . . C98 C 0.8927(6) 0.0069(4) 0.5338(2) 0.102(3) Uani 1 1 d . . . H98 H 0.9379 0.0351 0.5680 0.122 Uiso 1 1 calc R . . C99 C 0.8331(4) 0.0307(3) 0.48541(19) 0.0713(17) Uani 1 1 d . . . H99 H 0.8360 0.0744 0.4874 0.086 Uiso 1 1 calc R . . C100 C 0.6375(3) 0.05993(17) 0.39855(16) 0.0401(10) Uani 1 1 d . . . H100 H 0.6446 0.0754 0.4418 0.048 Uiso 1 1 calc R . . C101 C 0.5638(3) 0.08267(16) 0.35307(16) 0.0348(9) Uani 1 1 d . . . C102 C 0.4921(3) 0.13045(15) 0.35435(15) 0.0331(9) Uani 1 1 d . . . C103 C 0.4743(3) 0.16639(16) 0.40833(15) 0.0344(9) Uani 1 1 d . . . C104 C 0.5236(3) 0.14817(17) 0.47021(16) 0.0375(9) Uani 1 1 d . . . C105 C 0.6200(4) 0.18106(18) 0.50720(16) 0.0424(10) Uani 1 1 d . . . H105 H 0.6554 0.2148 0.4927 0.051 Uiso 1 1 calc R . . C106 C 0.6658(4) 0.1655(2) 0.56527(18) 0.0527(12) Uani 1 1 d . . . H106 H 0.7317 0.1889 0.5898 0.063 Uiso 1 1 calc R . . C107 C 0.6161(5) 0.11608(19) 0.58783(18) 0.0597(14) Uani 1 1 d . . . C108 C 0.5202(4) 0.08319(18) 0.55035(18) 0.0543(13) Uani 1 1 d . . . H108 H 0.4850 0.0491 0.5644 0.065 Uiso 1 1 calc R . . C109 C 0.4745(4) 0.09898(17) 0.49267(16) 0.0411(10) Uani 1 1 d . . . H109 H 0.4085 0.0757 0.4682 0.049 Uiso 1 1 calc R . . C110 C 0.6578(7) 0.0985(2) 0.6517(2) 0.103(3) Uani 1 1 d D . . H110 H 0.5901 0.0921 0.6678 0.124 Uiso 1 1 calc R . . C111 C 0.6931(4) 0.0350(2) 0.64735(19) 0.0574(13) Uani 1 1 d . . . H11A H 0.7504 0.0336 0.6237 0.086 Uiso 1 1 calc R . . H11B H 0.6309 0.0037 0.6258 0.086 Uiso 1 1 calc R . . H11C H 0.7210 0.0261 0.6897 0.086 Uiso 1 1 calc R . . C112 C 0.7249(6) 0.1450(2) 0.6986(2) 0.089(2) Uani 1 1 d D . . H12A H 0.7465 0.1277 0.7374 0.134 Uiso 1 1 calc R . . H12B H 0.6848 0.1799 0.7066 0.134 Uiso 1 1 calc R . . H12C H 0.7899 0.1595 0.6844 0.134 Uiso 1 1 calc R . . C113 C 0.5778(3) 0.30123(17) 0.30086(17) 0.0405(10) Uani 1 1 d . . . H113 H 0.5417 0.3210 0.3301 0.049 Uiso 1 1 calc R . . C114 C 0.6819(4) 0.3251(2) 0.3027(2) 0.0508(11) Uani 1 1 d . . . H114 H 0.7165 0.3609 0.3321 0.061 Uiso 1 1 calc R . . C115 C 0.7373(4) 0.2965(2) 0.2612(2) 0.0547(12) Uani 1 1 d . . . H115 H 0.8109 0.3114 0.2625 0.066 Uiso 1 1 calc R . . C116 C 0.6825(4) 0.24597(19) 0.2184(2) 0.0522(12) Uani 1 1 d . . . H116 H 0.7171 0.2255 0.1887 0.063 Uiso 1 1 calc R . . C117 C 0.5760(4) 0.22541(18) 0.21917(18) 0.0435(10) Uani 1 1 d . . . H117 H 0.5383 0.1909 0.1890 0.052 Uiso 1 1 calc R . . C118 C 0.1160(3) 0.18653(19) 0.25130(18) 0.0452(11) Uani 1 1 d . . . H118 H 0.1214 0.2237 0.2337 0.054 Uiso 1 1 calc R . . C119 C 0.0138(4) 0.1580(2) 0.2512(2) 0.0567(13) Uani 1 1 d . . . H119 H -0.0496 0.1749 0.2340 0.068 Uiso 1 1 calc R . . C120 C 0.0067(4) 0.1041(2) 0.2770(2) 0.0562(13) Uani 1 1 d . . . H120 H -0.0623 0.0818 0.2759 0.067 Uiso 1 1 calc R . . C121 C 0.0991(4) 0.0833(2) 0.3039(2) 0.0533(12) Uani 1 1 d . . . H121 H 0.0957 0.0477 0.3240 0.064 Uiso 1 1 calc R . . C122 C 0.1972(4) 0.11400(18) 0.30181(19) 0.0448(10) Uani 1 1 d . . . H122 H 0.2611 0.0985 0.3206 0.054 Uiso 1 1 calc R . . C123 C 0.0017(7) 0.2366(5) 0.6394(5) 0.125(3) Uani 1 1 d . . . H123 H -0.0090 0.1936 0.6422 0.150 Uiso 1 1 calc R . . C124 C -0.0095(9) 0.2588(6) 0.5822(4) 0.150(4) Uani 1 1 d . . . H124 H -0.0225 0.2308 0.5439 0.180 Uiso 1 1 calc R . . C125 C -0.0013(8) 0.3213(5) 0.5825(4) 0.129(3) Uani 1 1 d . . . H125 H -0.0170 0.3372 0.5441 0.154 Uiso 1 1 calc R . . C126 C 0.0280(6) 0.3592(4) 0.6357(3) 0.102(2) Uani 1 1 d . . . H126 H 0.0385 0.4023 0.6330 0.123 Uiso 1 1 calc R . . C127 C 0.0440(6) 0.3457(4) 0.6897(3) 0.093(2) Uani 1 1 d . . . H127 H 0.0643 0.3770 0.7258 0.111 Uiso 1 1 calc R . . C128 C 0.5123(5) 0.6590(2) 0.8917(2) 0.0588(12) Uani 1 1 d . . . H128 H 0.5847 0.6701 0.8878 0.071 Uiso 1 1 calc R . . C129 C 0.4396(6) 0.6259(2) 0.8408(2) 0.0777(18) Uani 1 1 d . . . H129 H 0.4606 0.6124 0.8028 0.093 Uiso 1 1 calc R . . C130 C 0.3320(6) 0.6123(3) 0.8468(3) 0.090(2) Uani 1 1 d . . . H130 H 0.2776 0.5904 0.8122 0.108 Uiso 1 1 calc R . . C131 C 0.3067(5) 0.6306(3) 0.9017(4) 0.092(2) Uani 1 1 d . . . H131 H 0.2344 0.6217 0.9067 0.110 Uiso 1 1 calc R . . C132 C 0.3855(5) 0.6618(3) 0.9498(3) 0.0797(16) Uani 1 1 d . . . H132 H 0.3666 0.6740 0.9887 0.096 Uiso 1 1 calc R . . C133 C 1.0498(6) 0.2746(3) 0.4188(3) 0.097(2) Uani 1 1 d . . . H133 H 1.1105 0.3052 0.4220 0.117 Uiso 1 1 calc R . . C134 C 1.0663(5) 0.2156(3) 0.4222(3) 0.0827(18) Uani 1 1 d . . . H134 H 1.1383 0.2054 0.4291 0.099 Uiso 1 1 calc R . . C135 C 0.9815(6) 0.1702(3) 0.4159(3) 0.0797(17) Uani 1 1 d . . . H135 H 0.9935 0.1284 0.4177 0.096 Uiso 1 1 calc R . . C136 C 0.8790(6) 0.1856(3) 0.4068(3) 0.0845(18) Uani 1 1 d . . . H136 H 0.8185 0.1546 0.4022 0.101 Uiso 1 1 calc R . . C137 C 0.8640(6) 0.2454(3) 0.4044(3) 0.096(2) Uani 1 1 d . . . H137 H 0.7917 0.2551 0.3979 0.115 Uiso 1 1 calc R . . C138 C 0.9775(5) 0.4231(4) 0.1702(3) 0.0828(18) Uani 1 1 d . . . H138 H 0.9854 0.4097 0.1288 0.099 Uiso 1 1 calc R . . C139 C 0.9958(6) 0.3861(4) 0.2130(6) 0.141(4) Uani 1 1 d . . . H139 H 1.0236 0.3482 0.2042 0.169 Uiso 1 1 calc R . . C140 C 0.9735(9) 0.4041(8) 0.2700(7) 0.207(10) Uani 1 1 d D . . H140 H 0.9758 0.3752 0.2987 0.248 Uiso 1 1 calc R . . C141 C 0.9506(10) 0.4555(9) 0.2857(4) 0.187(9) Uani 1 1 d D . . H141 H 0.9464 0.4684 0.3279 0.225 Uiso 1 1 calc R . . C142 C 0.9322(7) 0.4925(6) 0.2448(5) 0.161(5) Uani 1 1 d . . . H142 H 0.9065 0.5305 0.2568 0.193 Uiso 1 1 calc R . . C143 C 0.6050(5) 0.6265(3) 0.0831(3) 0.0763(16) Uani 1 1 d . . . H143 H 0.5901 0.6572 0.0572 0.092 Uiso 1 1 calc R . . C144 C 0.6883(5) 0.6409(2) 0.1323(2) 0.0716(16) Uani 1 1 d . . . H144 H 0.7362 0.6788 0.1396 0.086 Uiso 1 1 calc R . . C145 C 0.7010(6) 0.5986(3) 0.1715(3) 0.090(2) Uani 1 1 d . . . H145 H 0.7569 0.6084 0.2087 0.107 Uiso 1 1 calc R . . C146 C 0.6372(5) 0.5425(3) 0.1598(3) 0.0757(16) Uani 1 1 d . . . H146 H 0.6484 0.5135 0.1881 0.091 Uiso 1 1 calc R . . C147 C 0.5561(5) 0.5286(3) 0.1060(3) 0.0735(15) Uani 1 1 d . . . H147 H 0.5120 0.4893 0.0963 0.088 Uiso 1 1 calc R . . N1 N 0.3889(3) 0.24907(13) 0.35984(12) 0.0320(7) Uani 1 1 d . . . N2 N 0.3004(3) 0.28574(12) 0.23890(12) 0.0314(7) Uani 1 1 d . . . N3 N 0.3283(3) 0.16421(12) 0.17405(12) 0.0315(7) Uani 1 1 d . . . N4 N 0.4420(3) 0.13442(12) 0.29398(12) 0.0321(7) Uani 1 1 d . . . N5 N 0.5234(3) 0.25153(12) 0.26018(12) 0.0332(7) Uani 1 1 d . . . N6 N 0.2082(3) 0.16463(13) 0.27484(12) 0.0343(8) Uani 1 1 d . . . N7 N 0.3939(4) 0.23458(16) 0.75394(16) 0.0537(10) Uani 1 1 d . . . N8 N 0.3593(3) 0.50679(16) 0.69285(15) 0.0501(9) Uani 1 1 d . . . N9 N 0.2974(4) 0.68633(16) 0.24048(19) 0.0598(11) Uani 1 1 d . . . N10 N 0.1481(3) 0.54191(17) -0.02729(15) 0.0519(10) Uani 1 1 d . . . N11 N -0.1278(3) 0.03726(17) -0.19111(14) 0.0482(9) Uani 1 1 d . . . N12 N 0.2010(3) -0.15356(18) -0.12375(17) 0.0552(10) Uani 1 1 d . . . N13 N 0.9081(3) -0.12809(16) 0.25550(16) 0.0500(9) Uani 1 1 d . . . N14 N 0.8906(5) -0.0533(4) 0.5354(2) 0.112(2) Uani 1 1 d . . . N15 N 0.0316(7) 0.2855(8) 0.6948(4) 0.180(5) Uani 1 1 d . . . N16 N 0.4884(4) 0.67678(19) 0.9462(2) 0.0679(12) Uani 1 1 d . . . N17 N 0.9457(6) 0.2923(2) 0.4106(3) 0.1002(18) Uani 1 1 d . . . N18 N 0.9479(5) 0.4797(4) 0.1848(3) 0.114(2) Uani 1 1 d . . . N19 N 0.5388(5) 0.5705(3) 0.0668(3) 0.0985(17) Uani 1 1 d . . . Ni1 Ni 0.36530(5) 0.20858(2) 0.26682(2) 0.0303(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(2) 0.0248(17) 0.0215(16) -0.0027(13) -0.0021(15) 0.0042(15) C2 0.044(2) 0.0312(19) 0.0229(17) -0.0011(14) -0.0017(16) 0.0091(16) C3 0.046(2) 0.0333(19) 0.0213(17) 0.0017(14) -0.0013(16) 0.0072(16) C4 0.048(3) 0.036(2) 0.0231(17) -0.0018(14) 0.0004(16) 0.0072(17) C5 0.061(3) 0.0301(19) 0.0240(18) -0.0011(14) 0.0033(18) 0.0056(17) C6 0.059(3) 0.038(2) 0.0240(18) -0.0006(15) 0.0041(17) 0.0095(18) C7 0.067(3) 0.042(2) 0.0270(19) 0.0040(16) 0.002(2) 0.003(2) C8 0.078(4) 0.051(3) 0.043(2) 0.0065(19) 0.025(2) 0.008(2) C9 0.065(3) 0.049(2) 0.043(2) 0.0079(18) 0.017(2) 0.015(2) C10 0.052(3) 0.037(2) 0.0234(18) 0.0004(15) 0.0044(17) 0.0078(17) C11 0.056(3) 0.039(2) 0.0229(18) 0.0042(15) 0.0092(17) 0.0082(18) C12 0.059(3) 0.036(2) 0.0268(18) 0.0023(15) 0.0137(18) 0.0075(18) C13 0.067(3) 0.049(2) 0.0243(19) -0.0043(16) 0.0095(19) 0.007(2) C14 0.071(3) 0.049(2) 0.046(2) 0.0047(19) 0.017(2) 0.020(2) C15 0.063(3) 0.048(2) 0.0269(19) 0.0014(16) 0.0060(18) 0.016(2) C16 0.045(2) 0.0315(18) 0.0226(17) 0.0017(14) 0.0013(16) 0.0117(16) C17 0.039(2) 0.0276(18) 0.0248(17) -0.0016(13) -0.0009(15) 0.0060(15) C18 0.038(2) 0.0345(19) 0.0164(16) -0.0036(13) -0.0009(14) 0.0033(15) C19 0.039(2) 0.0256(17) 0.0197(16) -0.0040(13) -0.0024(15) 0.0057(14) C20 0.047(2) 0.0283(18) 0.0141(15) -0.0024(13) -0.0015(15) 0.0056(16) C21 0.048(3) 0.041(2) 0.0185(16) -0.0017(14) 0.0014(16) 0.0033(17) C22 0.066(3) 0.032(2) 0.0270(18) 0.0009(15) -0.0066(18) -0.0104(19) C23 0.062(3) 0.041(2) 0.037(2) 0.0002(17) 0.005(2) 0.015(2) C24 0.061(3) 0.041(2) 0.034(2) -0.0026(17) 0.0066(19) 0.014(2) C25 0.054(3) 0.0306(19) 0.0298(19) 0.0014(14) 0.0010(17) 0.0102(17) C26 0.081(4) 0.044(3) 0.069(3) -0.014(2) -0.006(3) 0.015(2) C27 0.195(8) 0.065(3) 0.046(3) -0.001(2) 0.046(4) 0.057(4) C28 0.328(13) 0.043(3) 0.052(3) 0.003(2) 0.043(5) 0.047(5) C29 0.041(2) 0.0263(17) 0.0187(16) -0.0009(13) -0.0002(15) 0.0084(15) C30 0.036(2) 0.0308(18) 0.0207(16) -0.0029(13) -0.0030(15) 0.0047(15) C31 0.041(2) 0.0299(18) 0.0197(16) -0.0008(13) -0.0022(15) 0.0072(15) C32 0.041(2) 0.0308(18) 0.0263(17) -0.0004(14) 0.0013(16) 0.0072(15) C33 0.051(3) 0.0290(18) 0.0222(17) -0.0030(14) -0.0052(16) 0.0074(16) C34 0.062(3) 0.037(2) 0.035(2) -0.0026(16) 0.0045(19) 0.0088(19) C35 0.066(3) 0.044(3) 0.049(2) -0.010(2) 0.006(2) 0.016(2) C36 0.072(3) 0.035(2) 0.050(3) -0.0002(19) 0.002(2) 0.001(2) C37 0.056(3) 0.032(2) 0.037(2) 0.0005(16) 0.0015(19) 0.0018(18) C38 0.040(2) 0.0300(18) 0.0213(16) 0.0006(13) -0.0010(15) 0.0041(15) C39 0.050(3) 0.0290(18) 0.0257(18) -0.0021(14) -0.0008(16) 0.0007(16) C40 0.056(3) 0.035(2) 0.0263(18) 0.0013(15) 0.0027(17) 0.0104(18) C41 0.067(3) 0.039(2) 0.035(2) 0.0060(16) 0.003(2) 0.014(2) C42 0.065(3) 0.055(3) 0.029(2) 0.0065(18) 0.0130(19) 0.006(2) C43 0.056(3) 0.047(2) 0.033(2) 0.0052(17) 0.0110(19) 0.0095(19) C44 0.048(2) 0.0301(18) 0.0178(16) -0.0028(13) -0.0015(15) 0.0087(16) C45 0.041(2) 0.0331(19) 0.0198(16) -0.0036(14) -0.0031(15) 0.0096(15) C46 0.045(2) 0.0271(18) 0.0193(16) -0.0018(13) -0.0020(15) 0.0075(15) C47 0.045(2) 0.0347(19) 0.0179(16) -0.0003(14) -0.0014(15) 0.0066(16) C48 0.058(3) 0.0232(18) 0.0225(18) -0.0038(13) -0.0058(17) 0.0054(16) C49 0.058(3) 0.032(2) 0.033(2) -0.0015(15) -0.0095(19) 0.0057(18) C50 0.065(3) 0.055(3) 0.040(2) 0.0075(19) -0.021(2) 0.002(2) C51 0.070(4) 0.054(3) 0.043(3) 0.012(2) -0.016(2) 0.001(2) C52 0.096(4) 0.042(2) 0.0229(19) -0.0015(16) 0.003(2) -0.004(2) C53 0.075(3) 0.0309(19) 0.0202(18) -0.0010(14) -0.0014(18) 0.0077(18) C54 0.104(5) 0.091(4) 0.052(3) 0.022(3) -0.029(3) -0.005(3) C55 0.086(4) 0.077(3) 0.046(3) 0.022(2) -0.001(3) 0.023(3) C56 0.155(7) 0.081(4) 0.072(4) 0.018(3) -0.049(4) -0.005(4) C57 0.047(2) 0.0262(18) 0.0176(16) -0.0029(13) -0.0009(15) 0.0070(15) C58 0.041(2) 0.0301(18) 0.0162(15) -0.0009(13) -0.0032(15) 0.0065(15) C59 0.045(2) 0.0288(18) 0.0217(17) -0.0015(13) 0.0009(16) 0.0082(15) C60 0.041(2) 0.0330(19) 0.0181(16) -0.0026(13) 0.0003(15) 0.0035(16) C61 0.036(2) 0.040(2) 0.0151(15) -0.0048(14) 0.0013(15) 0.0075(16) C62 0.056(3) 0.040(2) 0.0225(18) -0.0027(15) -0.0055(17) 0.0077(18) C63 0.056(3) 0.061(3) 0.0263(19) 0.0124(18) 0.0007(18) 0.016(2) C64 0.035(2) 0.063(3) 0.0254(18) 0.0008(17) 0.0018(16) -0.0014(19) C65 0.038(2) 0.044(2) 0.0254(18) -0.0038(15) 0.0051(16) 0.0024(17) C66 0.033(2) 0.0348(19) 0.0248(17) -0.0068(14) -0.0036(15) 0.0049(15) C67 0.033(2) 0.038(2) 0.0305(19) -0.0103(15) -0.0049(16) 0.0099(16) C68 0.046(3) 0.038(2) 0.038(2) -0.0058(16) -0.0042(18) 0.0023(17) C69 0.049(3) 0.037(2) 0.053(3) -0.0121(18) -0.006(2) 0.0070(18) C70 0.043(3) 0.060(3) 0.038(2) -0.014(2) -0.0024(19) 0.003(2) C71 0.036(2) 0.051(2) 0.035(2) -0.0161(17) -0.0016(17) 0.0023(18) C72 0.038(2) 0.0294(18) 0.0247(17) -0.0026(14) -0.0014(15) 0.0053(15) C73 0.041(2) 0.0262(17) 0.0195(16) -0.0036(13) 0.0001(15) 0.0047(15) C74 0.036(2) 0.0261(17) 0.0200(16) -0.0053(13) -0.0018(15) 0.0034(14) C75 0.039(2) 0.0293(18) 0.0177(16) -0.0037(13) -0.0016(15) 0.0020(15) C76 0.037(2) 0.0309(18) 0.0206(17) -0.0016(13) -0.0073(16) 0.0058(15) C77 0.039(2) 0.0337(19) 0.0244(17) -0.0012(14) -0.0021(16) 0.0064(16) C78 0.053(3) 0.0292(19) 0.0287(18) -0.0018(14) -0.0010(18) 0.0066(16) C79 0.046(2) 0.037(2) 0.0249(18) -0.0021(15) -0.0020(17) 0.0114(17) C80 0.039(2) 0.038(2) 0.0276(18) -0.0012(15) 0.0010(16) 0.0097(16) C81 0.038(2) 0.0290(18) 0.0246(17) -0.0017(13) -0.0032(16) 0.0050(15) C82 0.060(3) 0.035(2) 0.033(2) -0.0041(15) 0.0103(19) 0.0076(18) C83 0.080(3) 0.042(2) 0.031(2) -0.0063(17) 0.005(2) 0.015(2) C84 0.094(4) 0.046(2) 0.041(2) -0.0016(19) 0.004(2) 0.029(2) C85 0.041(2) 0.0261(17) 0.0192(16) -0.0016(13) -0.0036(15) 0.0071(15) C86 0.039(2) 0.0297(18) 0.0234(17) -0.0001(13) -0.0005(15) 0.0062(15) C87 0.040(2) 0.0296(18) 0.0234(17) -0.0016(13) -0.0005(15) 0.0065(15) C88 0.041(2) 0.0323(19) 0.0309(19) 0.0022(15) -0.0030(16) 0.0051(16) C89 0.046(2) 0.0326(19) 0.0234(17) 0.0040(14) 0.0012(16) 0.0076(16) C90 0.044(2) 0.036(2) 0.0325(19) -0.0019(15) -0.0011(17) 0.0046(17) C91 0.050(3) 0.038(2) 0.041(2) -0.0050(16) 0.005(2) 0.0106(18) C92 0.043(3) 0.045(2) 0.042(2) 0.0012(17) 0.0065(19) 0.0086(18) C93 0.043(3) 0.043(2) 0.0286(18) 0.0020(15) -0.0010(17) 0.0056(18) C94 0.045(2) 0.046(2) 0.0244(18) 0.0020(15) 0.0018(17) 0.0142(18) C95 0.060(3) 0.068(3) 0.033(2) 0.0117(19) 0.008(2) 0.036(2) C96 0.074(4) 0.080(3) 0.056(3) 0.032(2) 0.029(3) 0.045(3) C97 0.095(5) 0.122(5) 0.085(4) 0.063(4) 0.050(4) 0.074(4) C98 0.122(6) 0.165(7) 0.030(3) 0.008(3) 0.005(3) 0.105(5) C99 0.079(4) 0.105(4) 0.024(2) -0.005(2) -0.013(2) 0.052(3) C100 0.055(3) 0.040(2) 0.0207(17) 0.0007(14) -0.0030(17) 0.0136(18) C101 0.044(2) 0.0325(19) 0.0227(17) -0.0036(14) -0.0008(16) 0.0066(16) C102 0.044(2) 0.0287(18) 0.0212(17) -0.0026(13) -0.0022(15) 0.0085(15) C103 0.044(2) 0.0335(19) 0.0200(16) -0.0001(14) -0.0023(15) 0.0049(16) C104 0.050(3) 0.036(2) 0.0228(17) -0.0028(15) 0.0000(17) 0.0150(17) C105 0.058(3) 0.038(2) 0.0247(18) -0.0020(15) -0.0043(18) 0.0159(18) C106 0.070(3) 0.045(2) 0.030(2) -0.0065(17) -0.015(2) 0.021(2) C107 0.109(4) 0.035(2) 0.0238(19) -0.0054(17) -0.012(2) 0.024(2) C108 0.103(4) 0.031(2) 0.0275(19) -0.0003(16) 0.008(2) 0.020(2) C109 0.064(3) 0.033(2) 0.0232(17) -0.0015(14) 0.0034(18) 0.0147(18) C110 0.199(7) 0.048(3) 0.033(2) -0.009(2) -0.041(3) 0.041(4) C111 0.088(4) 0.046(2) 0.031(2) 0.0030(17) -0.008(2) 0.022(2) C112 0.162(6) 0.063(3) 0.029(2) -0.002(2) -0.020(3) 0.046(4) C113 0.047(3) 0.035(2) 0.0303(19) -0.0101(15) -0.0006(17) 0.0020(17) C114 0.050(3) 0.046(2) 0.044(2) -0.0121(18) 0.001(2) -0.005(2) C115 0.052(3) 0.048(3) 0.060(3) -0.005(2) 0.020(2) -0.006(2) C116 0.065(3) 0.038(2) 0.056(3) -0.0061(19) 0.027(2) 0.006(2) C117 0.059(3) 0.034(2) 0.034(2) -0.0100(16) 0.0170(19) -0.0001(18) C118 0.046(3) 0.044(2) 0.038(2) 0.0090(17) -0.0083(18) 0.0013(19) C119 0.049(3) 0.059(3) 0.052(3) 0.016(2) -0.013(2) -0.001(2) C120 0.051(3) 0.053(3) 0.055(3) 0.013(2) -0.006(2) -0.009(2) C121 0.056(3) 0.046(2) 0.057(3) 0.016(2) 0.007(2) 0.005(2) C122 0.054(3) 0.036(2) 0.042(2) 0.0058(17) 0.0046(19) 0.0140(19) C123 0.112(7) 0.145(8) 0.119(7) 0.037(6) 0.022(6) 0.002(5) C124 0.161(9) 0.179(10) 0.081(6) -0.017(6) -0.017(6) 0.022(8) C125 0.175(9) 0.120(7) 0.079(5) 0.020(5) -0.009(5) 0.032(6) C126 0.113(6) 0.113(5) 0.072(4) 0.007(4) 0.012(4) 0.006(4) C127 0.095(5) 0.135(6) 0.048(3) 0.013(4) 0.008(3) 0.029(4) C128 0.072(3) 0.048(3) 0.053(3) 0.003(2) 0.012(2) 0.005(2) C129 0.118(6) 0.065(3) 0.042(3) 0.006(2) 0.005(3) 0.005(3) C130 0.092(5) 0.079(4) 0.079(4) 0.029(3) -0.020(4) -0.025(3) C131 0.069(4) 0.116(5) 0.095(5) 0.058(4) 0.012(4) -0.005(4) C132 0.066(4) 0.087(4) 0.089(4) 0.021(3) 0.023(3) 0.005(3) C133 0.106(6) 0.077(4) 0.088(4) 0.028(3) -0.024(4) -0.010(4) C134 0.071(4) 0.099(5) 0.078(4) 0.026(3) 0.002(3) 0.026(4) C135 0.090(5) 0.083(4) 0.067(3) 0.022(3) 0.006(3) 0.028(4) C136 0.083(5) 0.078(4) 0.081(4) 0.015(3) -0.005(3) 0.006(3) C137 0.085(5) 0.098(5) 0.096(5) 0.012(4) -0.005(4) 0.030(4) C138 0.056(4) 0.110(5) 0.080(4) 0.008(4) 0.021(3) -0.002(3) C139 0.053(5) 0.123(6) 0.228(12) 0.084(8) -0.036(6) -0.005(4) C140 0.073(8) 0.38(2) 0.145(11) 0.200(14) -0.060(8) -0.109(11) C141 0.072(7) 0.43(3) 0.022(3) -0.017(8) -0.002(4) -0.058(12) C142 0.073(6) 0.259(13) 0.096(7) -0.094(8) -0.022(5) 0.024(6) C143 0.102(5) 0.067(3) 0.058(3) 0.004(3) 0.018(3) 0.008(3) C144 0.106(5) 0.057(3) 0.040(3) 0.001(2) 0.000(3) 0.003(3) C145 0.125(6) 0.095(5) 0.041(3) -0.005(3) 0.008(3) 0.021(4) C146 0.104(5) 0.074(4) 0.061(3) 0.008(3) 0.040(3) 0.024(3) C147 0.073(4) 0.077(4) 0.078(4) 0.021(3) 0.022(3) 0.021(3) N1 0.0430(19) 0.0276(15) 0.0203(13) -0.0001(11) -0.0031(12) 0.0068(13) N2 0.0456(19) 0.0251(14) 0.0181(13) -0.0026(11) -0.0032(12) 0.0078(12) N3 0.0424(19) 0.0263(15) 0.0197(14) -0.0035(11) -0.0023(13) 0.0044(12) N4 0.0432(19) 0.0274(15) 0.0188(14) -0.0036(11) -0.0051(13) 0.0078(13) N5 0.049(2) 0.0253(15) 0.0200(14) -0.0014(11) -0.0014(13) 0.0056(13) N6 0.049(2) 0.0301(15) 0.0162(13) -0.0018(11) -0.0058(13) 0.0033(13) N7 0.078(3) 0.045(2) 0.0346(18) 0.0059(15) 0.0106(19) 0.0004(19) N8 0.071(3) 0.045(2) 0.0336(18) -0.0022(14) 0.0124(17) 0.0131(18) N9 0.073(3) 0.0343(19) 0.060(2) -0.0034(17) -0.002(2) 0.0051(19) N10 0.073(3) 0.050(2) 0.0298(18) 0.0099(15) 0.0032(17) 0.0070(19) N11 0.041(2) 0.068(2) 0.0282(16) 0.0019(16) -0.0029(15) 0.0011(17) N12 0.053(2) 0.057(2) 0.046(2) -0.0121(17) -0.0014(18) 0.0147(18) N13 0.053(2) 0.050(2) 0.0438(19) -0.0015(16) 0.0075(17) 0.0119(17) N14 0.132(5) 0.193(7) 0.045(3) 0.050(4) 0.031(3) 0.119(5) N15 0.118(7) 0.373(16) 0.114(6) 0.119(9) 0.069(5) 0.134(9) N16 0.078(3) 0.060(2) 0.060(3) -0.0086(19) 0.019(2) 0.002(2) N17 0.122(5) 0.071(3) 0.094(4) 0.008(3) -0.008(3) 0.025(3) N18 0.090(4) 0.139(6) 0.092(4) 0.021(4) -0.018(3) -0.003(4) N19 0.105(5) 0.097(4) 0.097(4) 0.011(3) 0.034(3) 0.018(3) Ni1 0.0438(4) 0.0252(3) 0.0156(3) -0.0036(2) -0.0044(3) 0.0068(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.369(4) . ? C1 C103 1.402(5) . ? C1 C2 1.460(5) . ? C2 C17 1.392(5) . ? C2 C3 1.406(5) . ? C3 C4 1.379(5) . ? C3 H3 0.9500 . ? C4 C10 1.419(5) . ? C4 C5 1.492(5) . ? C5 C9 1.380(6) . ? C5 C6 1.387(6) . ? C6 C7 1.393(6) . ? C6 H6 0.9500 . ? C7 N7 1.307(6) . ? C7 H7 0.9500 . ? C8 N7 1.330(6) . ? C8 C9 1.385(6) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C16 1.390(5) . ? C10 C11 1.494(5) . ? C11 C15 1.392(6) . ? C11 C12 1.392(5) . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 N8 1.327(6) . ? C13 H13 0.9500 . ? C14 N8 1.348(6) . ? C14 C15 1.381(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.408(5) . ? C16 H16 0.9500 . ? C17 C18 1.469(5) . ? C18 N1 1.370(5) . ? C18 C19 1.397(5) . ? C19 C29 1.412(5) . ? C19 C20 1.512(5) . ? C20 C21 1.380(5) . ? C20 C25 1.388(6) . ? C21 C22 1.419(6) . ? C21 H21 0.9500 . ? C22 C23 1.392(7) . ? C22 H22 0.9500 . ? C23 C24 1.377(6) . ? C23 C26 1.515(6) . ? C24 C25 1.375(5) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C28 1.467(9) . ? C26 C27 1.483(8) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N2 1.374(4) . ? C29 C30 1.464(5) . ? C30 C31 1.389(5) . ? C30 C45 1.412(5) . ? C31 C32 1.393(5) . ? C31 H31 0.9500 . ? C32 C38 1.433(5) . ? C32 C33 1.481(5) . ? C33 C34 1.382(6) . ? C33 C37 1.394(6) . ? C34 C35 1.381(6) . ? C34 H34 0.9500 . ? C35 N9 1.312(7) . ? C35 H35 0.9500 . ? C36 N9 1.329(6) . ? C36 C37 1.376(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C44 1.373(5) . ? C38 C39 1.488(5) . ? C39 C40 1.379(6) . ? C39 C43 1.401(6) . ? C40 C41 1.392(5) . ? C40 H40 0.9500 . ? C41 N10 1.333(6) . ? C41 H41 0.9500 . ? C42 N10 1.322(6) . ? C42 C43 1.382(6) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.392(5) . ? C44 H44 0.9500 . ? C45 C46 1.464(5) . ? C46 N2 1.366(4) . ? C46 C47 1.409(5) . ? C47 C57 1.403(5) . ? C47 C48 1.512(5) . ? C48 C49 1.368(6) . ? C48 C53 1.391(6) . ? C49 C50 1.401(6) . ? C49 H49 0.9500 . ? C50 C51 1.373(8) . ? C50 H50 0.9500 . ? C51 C52 1.394(8) . ? C51 C54 1.513(6) . ? C52 C53 1.419(6) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C56 1.415(8) . ? C54 C55 1.505(8) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N3 1.363(4) . ? C57 C58 1.466(4) . ? C58 C73 1.403(5) . ? C58 C59 1.404(5) . ? C59 C60 1.401(5) . ? C59 H59 0.9500 . ? C60 C66 1.411(5) . ? C60 C61 1.480(5) . ? C61 C62 1.383(5) . ? C61 C65 1.404(5) . ? C62 C63 1.386(5) . ? C62 H62 0.9500 . ? C63 N11 1.323(6) . ? C63 H63 0.9500 . ? C64 N11 1.338(5) . ? C64 C65 1.378(5) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 C72 1.389(5) . ? C66 C67 1.486(5) . ? C67 C71 1.383(6) . ? C67 C68 1.411(6) . ? C68 C69 1.377(6) . ? C68 H68 0.9500 . ? C69 N12 1.340(6) . ? C69 H69 0.9500 . ? C70 N12 1.309(6) . ? C70 C71 1.417(6) . ? C70 H70 0.9500 . ? C71 H71 0.9500 . ? C72 C73 1.391(5) . ? C72 H72 0.9500 . ? C73 C74 1.477(4) . ? C74 N3 1.368(4) . ? C74 C75 1.387(5) . ? C75 C85 1.416(4) . ? C75 C76 1.511(5) . ? C76 C81 1.373(6) . ? C76 C77 1.394(5) . ? C77 C78 1.391(5) . ? C77 H77 0.9500 . ? C78 C79 1.394(6) . ? C78 H78 0.9500 . ? C79 C80 1.386(6) . ? C79 C82 1.514(5) . ? C80 C81 1.402(5) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 C84 1.488(6) . ? C82 C83 1.546(6) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 N4 1.366(4) . ? C85 C86 1.450(5) . ? C86 C87 1.393(5) . ? C86 C101 1.416(5) . ? C87 C88 1.388(5) . ? C87 H87 0.9500 . ? C88 C94 1.419(5) . ? C88 C89 1.483(6) . ? C89 C90 1.398(5) . ? C89 C93 1.399(6) . ? C90 C91 1.383(6) . ? C90 H90 0.9500 . ? C91 N13 1.332(6) . ? C91 H91 0.9500 . ? C92 N13 1.344(5) . ? C92 C93 1.366(6) . ? C92 H92 0.9500 . ? C93 H93 0.9500 . ? C94 C100 1.377(6) . ? C94 C95 1.488(5) . ? C95 C96 1.391(7) . ? C95 C99 1.400(7) . ? C96 C97 1.379(7) . ? C96 H96 0.9500 . ? C97 N14 1.346(10) . ? C97 H97 0.9500 . ? C98 N14 1.322(10) . ? C98 C99 1.372(7) . ? C98 H98 0.9500 . ? C99 H99 0.9500 . ? C100 C101 1.404(5) . ? C100 H100 0.9500 . ? C101 C102 1.460(5) . ? C102 N4 1.370(4) . ? C102 C103 1.410(5) . ? C103 C104 1.503(5) . ? C104 C109 1.387(6) . ? C104 C105 1.387(6) . ? C105 C106 1.394(5) . ? C105 H105 0.9500 . ? C106 C107 1.397(7) . ? C106 H106 0.9500 . ? C107 C108 1.386(7) . ? C107 C110 1.514(6) . ? C108 C109 1.389(5) . ? C108 H108 0.9500 . ? C109 H109 0.9500 . ? C110 C112 1.414(7) . ? C110 C111 1.506(7) . ? C110 H110 1.0000 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H12A 0.9800 . ? C112 H12B 0.9800 . ? C112 H12C 0.9800 . ? C113 N5 1.338(4) . ? C113 C114 1.359(6) . ? C113 H113 0.9500 . ? C114 C115 1.390(6) . ? C114 H114 0.9500 . ? C115 C116 1.374(6) . ? C115 H115 0.9500 . ? C116 C117 1.384(6) . ? C116 H116 0.9500 . ? C117 N5 1.336(5) . ? C117 H117 0.9500 . ? C118 N6 1.343(5) . ? C118 C119 1.379(6) . ? C118 H118 0.9500 . ? C119 C120 1.380(6) . ? C119 H119 0.9500 . ? C120 C121 1.353(7) . ? C120 H120 0.9500 . ? C121 C122 1.363(6) . ? C121 H121 0.9500 . ? C122 N6 1.335(5) . ? C122 H122 0.9500 . ? C123 C124 1.397(13) . ? C123 N15 1.470(15) . ? C123 H123 0.9500 . ? C124 C125 1.363(13) . ? C124 H124 0.9500 . ? C125 C126 1.302(11) . ? C125 H125 0.9500 . ? C126 C127 1.248(9) . ? C126 H126 0.9500 . ? C127 N15 1.335(14) . ? C127 H127 0.9500 . ? C128 N16 1.320(6) . ? C128 C129 1.361(7) . ? C128 H128 0.9500 . ? C129 C130 1.404(9) . ? C129 H129 0.9500 . ? C130 C131 1.337(10) . ? C130 H130 0.9500 . ? C131 C132 1.347(9) . ? C131 H131 0.9500 . ? C132 N16 1.334(7) . ? C132 H132 0.9500 . ? C133 C134 1.342(9) . ? C133 N17 1.401(10) . ? C133 H133 0.9500 . ? C134 C135 1.357(9) . ? C134 H134 0.9500 . ? C135 C136 1.361(9) . ? C135 H135 0.9500 . ? C136 C137 1.350(9) . ? C136 H136 0.9500 . ? C137 N17 1.353(9) . ? C137 H137 0.9500 . ? C138 C139 1.325(11) . ? C138 N18 1.351(9) . ? C138 H138 0.9500 . ? C139 C140 1.361(19) . ? C139 H139 0.9500 . ? C140 C141 1.217(16) . ? C140 H140 0.9500 . ? C141 C142 1.30(2) . ? C141 H141 0.9500 . ? C142 N18 1.375(12) . ? C142 H142 0.9500 . ? C143 C144 1.325(8) . ? C143 N19 1.371(8) . ? C143 H143 0.9500 . ? C144 C145 1.348(8) . ? C144 H144 0.9500 . ? C145 C146 1.362(9) . ? C145 H145 0.9500 . ? C146 C147 1.375(8) . ? C146 H146 0.9500 . ? C147 N19 1.345(8) . ? C147 H147 0.9500 . ? N1 Ni1 2.071(3) . ? N2 Ni1 2.069(3) . ? N3 Ni1 2.080(3) . ? N4 Ni1 2.074(3) . ? N5 Ni1 2.167(3) . ? N6 Ni1 2.174(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C103 125.4(3) . . ? N1 C1 C2 108.5(3) . . ? C103 C1 C2 125.7(3) . . ? C17 C2 C3 120.1(3) . . ? C17 C2 C1 106.9(3) . . ? C3 C2 C1 132.9(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C10 119.5(3) . . ? C3 C4 C5 117.2(3) . . ? C10 C4 C5 123.2(3) . . ? C9 C5 C6 116.7(4) . . ? C9 C5 C4 123.1(4) . . ? C6 C5 C4 120.1(4) . . ? C5 C6 C7 118.9(4) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N7 C7 C6 124.6(4) . . ? N7 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N7 C8 C9 123.9(5) . . ? N7 C8 H8 118.1 . . ? C9 C8 H8 118.1 . . ? C5 C9 C8 119.6(4) . . ? C5 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C16 C10 C4 119.9(3) . . ? C16 C10 C11 117.3(3) . . ? C4 C10 C11 122.7(3) . . ? C15 C11 C12 116.3(3) . . ? C15 C11 C10 121.8(3) . . ? C12 C11 C10 121.7(4) . . ? C13 C12 C11 119.6(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? N8 C13 C12 124.3(4) . . ? N8 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? N8 C14 C15 123.6(4) . . ? N8 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C11 120.0(4) . . ? C14 C15 H15 120.0 . . ? C11 C15 H15 120.0 . . ? C10 C16 C17 120.1(3) . . ? C10 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C2 C17 C16 119.5(3) . . ? C2 C17 C18 106.5(3) . . ? C16 C17 C18 134.0(3) . . ? N1 C18 C19 124.7(3) . . ? N1 C18 C17 108.4(3) . . ? C19 C18 C17 126.9(3) . . ? C18 C19 C29 126.6(3) . . ? C18 C19 C20 117.2(3) . . ? C29 C19 C20 116.1(3) . . ? C21 C20 C25 118.8(3) . . ? C21 C20 C19 121.1(4) . . ? C25 C20 C19 120.1(3) . . ? C20 C21 C22 119.1(4) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 121.7(4) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C24 C23 C22 117.3(4) . . ? C24 C23 C26 119.8(4) . . ? C22 C23 C26 122.9(4) . . ? C25 C24 C23 121.7(4) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C20 121.4(4) . . ? C24 C25 H25 119.3 . . ? C20 C25 H25 119.3 . . ? C28 C26 C27 109.2(5) . . ? C28 C26 C23 111.2(5) . . ? C27 C26 C23 113.8(4) . . ? C28 C26 H26 107.4 . . ? C27 C26 H26 107.4 . . ? C23 C26 H26 107.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 C19 124.3(3) . . ? N2 C29 C30 108.8(3) . . ? C19 C29 C30 126.7(3) . . ? C31 C30 C45 119.3(3) . . ? C31 C30 C29 134.4(3) . . ? C45 C30 C29 106.1(3) . . ? C30 C31 C32 121.0(3) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C38 119.2(3) . . ? C31 C32 C33 119.5(3) . . ? C38 C32 C33 121.2(3) . . ? C34 C33 C37 116.4(3) . . ? C34 C33 C32 121.9(4) . . ? C37 C33 C32 121.7(4) . . ? C35 C34 C33 119.0(4) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N9 C35 C34 125.1(5) . . ? N9 C35 H35 117.5 . . ? C34 C35 H35 117.5 . . ? N9 C36 C37 123.8(5) . . ? N9 C36 H36 118.1 . . ? C37 C36 H36 118.1 . . ? C36 C37 C33 119.6(4) . . ? C36 C37 H37 120.2 . . ? C33 C37 H37 120.2 . . ? C44 C38 C32 119.2(3) . . ? C44 C38 C39 117.8(3) . . ? C32 C38 C39 122.8(3) . . ? C40 C39 C43 116.7(3) . . ? C40 C39 C38 123.1(4) . . ? C43 C39 C38 120.0(4) . . ? C39 C40 C41 119.6(4) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? N10 C41 C40 124.0(4) . . ? N10 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? N10 C42 C43 124.8(4) . . ? N10 C42 H42 117.6 . . ? C43 C42 H42 117.6 . . ? C42 C43 C39 118.9(4) . . ? C42 C43 H43 120.5 . . ? C39 C43 H43 120.5 . . ? C38 C44 C45 121.4(3) . . ? C38 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C44 C45 C30 119.8(3) . . ? C44 C45 C46 133.6(3) . . ? C30 C45 C46 106.5(3) . . ? N2 C46 C47 125.2(3) . . ? N2 C46 C45 108.8(3) . . ? C47 C46 C45 126.0(3) . . ? C57 C47 C46 126.3(3) . . ? C57 C47 C48 117.2(3) . . ? C46 C47 C48 116.5(3) . . ? C49 C48 C53 119.3(3) . . ? C49 C48 C47 120.4(4) . . ? C53 C48 C47 120.4(4) . . ? C48 C49 C50 121.3(5) . . ? C48 C49 H49 119.3 . . ? C50 C49 H49 119.3 . . ? C51 C50 C49 120.8(5) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C50 C51 C52 118.4(4) . . ? C50 C51 C54 120.7(5) . . ? C52 C51 C54 120.9(5) . . ? C51 C52 C53 121.0(4) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C48 C53 C52 119.2(5) . . ? C48 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C56 C54 C55 114.5(6) . . ? C56 C54 C51 113.4(5) . . ? C55 C54 C51 113.2(5) . . ? C56 C54 H54 104.8 . . ? C55 C54 H54 104.8 . . ? C51 C54 H54 104.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N3 C57 C47 124.3(3) . . ? N3 C57 C58 109.5(3) . . ? C47 C57 C58 125.8(3) . . ? C73 C58 C59 119.9(3) . . ? C73 C58 C57 105.9(3) . . ? C59 C58 C57 134.1(3) . . ? C60 C59 C58 120.2(3) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C66 119.2(3) . . ? C59 C60 C61 118.3(3) . . ? C66 C60 C61 122.5(3) . . ? C62 C61 C65 115.8(3) . . ? C62 C61 C60 122.5(3) . . ? C65 C61 C60 121.7(3) . . ? C61 C62 C63 120.3(4) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? N11 C63 C62 124.1(4) . . ? N11 C63 H63 117.9 . . ? C62 C63 H63 117.9 . . ? N11 C64 C65 124.2(4) . . ? N11 C64 H64 117.9 . . ? C65 C64 H64 117.9 . . ? C64 C65 C61 119.6(4) . . ? C64 C65 H65 120.2 . . ? C61 C65 H65 120.2 . . ? C72 C66 C60 120.3(3) . . ? C72 C66 C67 115.6(3) . . ? C60 C66 C67 124.0(3) . . ? C71 C67 C68 117.4(3) . . ? C71 C67 C66 121.7(4) . . ? C68 C67 C66 120.7(3) . . ? C69 C68 C67 119.2(4) . . ? C69 C68 H68 120.4 . . ? C67 C68 H68 120.4 . . ? N12 C69 C68 123.4(4) . . ? N12 C69 H69 118.3 . . ? C68 C69 H69 118.3 . . ? N12 C70 C71 123.8(4) . . ? N12 C70 H70 118.1 . . ? C71 C70 H70 118.1 . . ? C67 C71 C70 118.4(4) . . ? C67 C71 H71 120.8 . . ? C70 C71 H71 120.8 . . ? C66 C72 C73 120.4(3) . . ? C66 C72 H72 119.8 . . ? C73 C72 H72 119.8 . . ? C72 C73 C58 119.9(3) . . ? C72 C73 C74 133.4(3) . . ? C58 C73 C74 106.6(3) . . ? N3 C74 C75 125.8(3) . . ? N3 C74 C73 108.4(3) . . ? C75 C74 C73 125.8(3) . . ? C74 C75 C85 126.0(3) . . ? C74 C75 C76 117.5(3) . . ? C85 C75 C76 116.5(3) . . ? C81 C76 C77 119.2(3) . . ? C81 C76 C75 121.2(3) . . ? C77 C76 C75 119.5(4) . . ? C78 C77 C76 119.6(4) . . ? C78 C77 H77 120.2 . . ? C76 C77 H77 120.2 . . ? C77 C78 C79 122.1(4) . . ? C77 C78 H78 119.0 . . ? C79 C78 H78 119.0 . . ? C80 C79 C78 117.4(3) . . ? C80 C79 C82 122.4(4) . . ? C78 C79 C82 120.1(3) . . ? C79 C80 C81 121.0(4) . . ? C79 C80 H80 119.5 . . ? C81 C80 H80 119.5 . . ? C76 C81 C80 120.8(3) . . ? C76 C81 H81 119.6 . . ? C80 C81 H81 119.6 . . ? C84 C82 C79 111.2(3) . . ? C84 C82 C83 111.1(4) . . ? C79 C82 C83 112.8(3) . . ? C84 C82 H82 107.1 . . ? C79 C82 H82 107.1 . . ? C83 C82 H82 107.1 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N4 C85 C75 124.2(3) . . ? N4 C85 C86 109.7(3) . . ? C75 C85 C86 125.8(3) . . ? C87 C86 C101 119.7(3) . . ? C87 C86 C85 134.2(3) . . ? C101 C86 C85 106.0(3) . . ? C88 C87 C86 121.5(3) . . ? C88 C87 H87 119.3 . . ? C86 C87 H87 119.3 . . ? C87 C88 C94 118.5(4) . . ? C87 C88 C89 118.7(3) . . ? C94 C88 C89 122.8(3) . . ? C90 C89 C93 116.7(4) . . ? C90 C89 C88 121.2(3) . . ? C93 C89 C88 122.1(3) . . ? C91 C90 C89 119.2(4) . . ? C91 C90 H90 120.4 . . ? C89 C90 H90 120.4 . . ? N13 C91 C90 124.4(4) . . ? N13 C91 H91 117.8 . . ? C90 C91 H91 117.8 . . ? N13 C92 C93 124.6(4) . . ? N13 C92 H92 117.7 . . ? C93 C92 H92 117.7 . . ? C92 C93 C89 119.4(4) . . ? C92 C93 H93 120.3 . . ? C89 C93 H93 120.3 . . ? C100 C94 C88 120.4(3) . . ? C100 C94 C95 116.8(3) . . ? C88 C94 C95 122.7(4) . . ? C96 C95 C99 116.8(4) . . ? C96 C95 C94 122.4(4) . . ? C99 C95 C94 120.8(4) . . ? C97 C96 C95 118.8(6) . . ? C97 C96 H96 120.6 . . ? C95 C96 H96 120.6 . . ? N14 C97 C96 124.0(6) . . ? N14 C97 H97 118.0 . . ? C96 C97 H97 118.0 . . ? N14 C98 C99 123.6(6) . . ? N14 C98 H98 118.2 . . ? C99 C98 H98 118.2 . . ? C98 C99 C95 120.0(6) . . ? C98 C99 H99 120.0 . . ? C95 C99 H99 120.0 . . ? C94 C100 C101 121.0(3) . . ? C94 C100 H100 119.5 . . ? C101 C100 H100 119.5 . . ? C100 C101 C86 118.6(3) . . ? C100 C101 C102 135.1(3) . . ? C86 C101 C102 106.3(3) . . ? N4 C102 C103 124.6(3) . . ? N4 C102 C101 109.0(3) . . ? C103 C102 C101 126.4(3) . . ? C1 C103 C102 126.2(3) . . ? C1 C103 C104 117.4(3) . . ? C102 C103 C104 116.2(3) . . ? C109 C104 C105 117.8(3) . . ? C109 C104 C103 121.8(3) . . ? C105 C104 C103 120.4(4) . . ? C104 C105 C106 121.2(4) . . ? C104 C105 H105 119.4 . . ? C106 C105 H105 119.4 . . ? C105 C106 C107 120.9(4) . . ? C105 C106 H106 119.6 . . ? C107 C106 H106 119.6 . . ? C108 C107 C106 117.6(4) . . ? C108 C107 C110 118.5(5) . . ? C106 C107 C110 123.9(5) . . ? C107 C108 C109 121.4(4) . . ? C107 C108 H108 119.3 . . ? C109 C108 H108 119.3 . . ? C104 C109 C108 121.2(4) . . ? C104 C109 H109 119.4 . . ? C108 C109 H109 119.4 . . ? C112 C110 C111 116.0(5) . . ? C112 C110 C107 117.6(5) . . ? C111 C110 C107 112.5(4) . . ? C112 C110 H110 102.6 . . ? C111 C110 H110 102.6 . . ? C107 C110 H110 102.6 . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C110 C112 H12A 109.5 . . ? C110 C112 H12B 109.5 . . ? H12A C112 H12B 109.5 . . ? C110 C112 H12C 109.5 . . ? H12A C112 H12C 109.5 . . ? H12B C112 H12C 109.5 . . ? N5 C113 C114 123.6(4) . . ? N5 C113 H113 118.2 . . ? C114 C113 H113 118.2 . . ? C113 C114 C115 119.4(4) . . ? C113 C114 H114 120.3 . . ? C115 C114 H114 120.3 . . ? C116 C115 C114 118.0(4) . . ? C116 C115 H115 121.0 . . ? C114 C115 H115 121.0 . . ? C115 C116 C117 118.7(4) . . ? C115 C116 H116 120.6 . . ? C117 C116 H116 120.6 . . ? N5 C117 C116 123.5(3) . . ? N5 C117 H117 118.2 . . ? C116 C117 H117 118.2 . . ? N6 C118 C119 123.6(4) . . ? N6 C118 H118 118.2 . . ? C119 C118 H118 118.2 . . ? C118 C119 C120 117.8(4) . . ? C118 C119 H119 121.1 . . ? C120 C119 H119 121.1 . . ? C121 C120 C119 119.2(4) . . ? C121 C120 H120 120.4 . . ? C119 C120 H120 120.4 . . ? C120 C121 C122 119.4(4) . . ? C120 C121 H121 120.3 . . ? C122 C121 H121 120.3 . . ? N6 C122 C121 123.6(4) . . ? N6 C122 H122 118.2 . . ? C121 C122 H122 118.2 . . ? C124 C123 N15 114.2(9) . . ? C124 C123 H123 122.9 . . ? N15 C123 H123 122.9 . . ? C125 C124 C123 118.8(9) . . ? C125 C124 H124 120.6 . . ? C123 C124 H124 120.6 . . ? C126 C125 C124 119.8(8) . . ? C126 C125 H125 120.1 . . ? C124 C125 H125 120.1 . . ? C127 C126 C125 127.6(9) . . ? C127 C126 H126 116.2 . . ? C125 C126 H126 116.2 . . ? C126 C127 N15 117.4(8) . . ? C126 C127 H127 121.3 . . ? N15 C127 H127 121.3 . . ? N16 C128 C129 124.0(6) . . ? N16 C128 H128 118.0 . . ? C129 C128 H128 118.0 . . ? C128 C129 C130 117.0(6) . . ? C128 C129 H129 121.5 . . ? C130 C129 H129 121.5 . . ? C131 C130 C129 119.4(6) . . ? C131 C130 H130 120.3 . . ? C129 C130 H130 120.3 . . ? C130 C131 C132 118.8(7) . . ? C130 C131 H131 120.6 . . ? C132 C131 H131 120.6 . . ? N16 C132 C131 124.2(7) . . ? N16 C132 H132 117.9 . . ? C131 C132 H132 117.9 . . ? C134 C133 N17 121.8(6) . . ? C134 C133 H133 119.1 . . ? N17 C133 H133 119.1 . . ? C133 C134 C135 120.9(6) . . ? C133 C134 H134 119.6 . . ? C135 C134 H134 119.6 . . ? C134 C135 C136 118.9(6) . . ? C134 C135 H135 120.6 . . ? C136 C135 H135 120.6 . . ? C137 C136 C135 119.5(7) . . ? C137 C136 H136 120.3 . . ? C135 C136 H136 120.3 . . ? C136 C137 N17 124.0(7) . . ? C136 C137 H137 118.0 . . ? N17 C137 H137 118.0 . . ? C139 C138 N18 120.7(8) . . ? C139 C138 H138 119.7 . . ? N18 C138 H138 119.7 . . ? C138 C139 C140 118.1(11) . . ? C138 C139 H139 120.9 . . ? C140 C139 H139 120.9 . . ? C141 C140 C139 122.8(10) . . ? C141 C140 H140 118.6 . . ? C139 C140 H140 118.6 . . ? C140 C141 C142 119.8(10) . . ? C140 C141 H141 120.1 . . ? C142 C141 H141 120.1 . . ? C141 C142 N18 123.3(11) . . ? C141 C142 H142 118.4 . . ? N18 C142 H142 118.4 . . ? C144 C143 N19 124.9(6) . . ? C144 C143 H143 117.6 . . ? N19 C143 H143 117.6 . . ? C143 C144 C145 116.1(6) . . ? C143 C144 H144 121.9 . . ? C145 C144 H144 121.9 . . ? C144 C145 C146 122.7(6) . . ? C144 C145 H145 118.7 . . ? C146 C145 H145 118.7 . . ? C145 C146 C147 118.5(6) . . ? C145 C146 H146 120.8 . . ? C147 C146 H146 120.8 . . ? N19 C147 C146 120.4(6) . . ? N19 C147 H147 119.8 . . ? C146 C147 H147 119.8 . . ? C1 N1 C18 109.3(3) . . ? C1 N1 Ni1 124.1(2) . . ? C18 N1 Ni1 125.8(2) . . ? C46 N2 C29 109.4(3) . . ? C46 N2 Ni1 124.4(2) . . ? C29 N2 Ni1 125.1(2) . . ? C57 N3 C74 109.3(3) . . ? C57 N3 Ni1 124.1(2) . . ? C74 N3 Ni1 124.9(2) . . ? C85 N4 C102 108.8(3) . . ? C85 N4 Ni1 124.9(2) . . ? C102 N4 Ni1 124.9(2) . . ? C117 N5 C113 116.7(4) . . ? C117 N5 Ni1 121.0(2) . . ? C113 N5 Ni1 122.0(3) . . ? C122 N6 C118 116.3(4) . . ? C122 N6 Ni1 122.5(3) . . ? C118 N6 Ni1 121.2(3) . . ? C7 N7 C8 116.3(4) . . ? C13 N8 C14 116.1(3) . . ? C35 N9 C36 116.0(4) . . ? C42 N10 C41 116.0(3) . . ? C63 N11 C64 115.9(3) . . ? C70 N12 C69 117.7(4) . . ? C91 N13 C92 115.8(4) . . ? C98 N14 C97 116.7(5) . . ? C127 N15 C123 121.9(7) . . ? C128 N16 C132 116.5(5) . . ? C137 N17 C133 115.0(6) . . ? C138 N18 C142 114.6(8) . . ? C147 N19 C143 117.2(6) . . ? N2 Ni1 N1 89.82(11) . . ? N2 Ni1 N4 175.52(13) . . ? N1 Ni1 N4 90.52(11) . . ? N2 Ni1 N3 90.35(11) . . ? N1 Ni1 N3 174.92(13) . . ? N4 Ni1 N3 89.71(11) . . ? N2 Ni1 N5 88.81(12) . . ? N1 Ni1 N5 92.16(11) . . ? N4 Ni1 N5 86.72(12) . . ? N3 Ni1 N5 92.91(12) . . ? N2 Ni1 N6 92.10(12) . . ? N1 Ni1 N6 87.31(11) . . ? N4 Ni1 N6 92.37(12) . . ? N3 Ni1 N6 87.61(11) . . ? N5 Ni1 N6 178.94(11) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 61.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.831 _refine_diff_density_min -0.584 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 81 17 ' ' 2 0.274 0.744 0.079 24 2 ' ' 3 0.726 0.256 0.920 24 2 ' ' _platon_squeeze_details ; ; _refine_diff_density_rms 0.080