data_js140_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H48 B F6 N6 O6 S2' _chemical_formula_weight 873.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 31.1770(19) _cell_length_b 16.2710(9) _cell_length_c 18.0874(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.572(4) _cell_angle_gamma 90.00 _cell_volume 8838.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4932 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 24.08 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3656 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9480 _exptl_absorpt_correction_T_max 0.9955 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 76713 _diffrn_reflns_av_R_equivalents 0.1315 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.31 _reflns_number_total 11013 _reflns_number_gt 5837 _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. ; _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^)+(0.0606P)^2^+7.5295P] 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 11013 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1400 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.06856(10) 0.63156(19) 0.17762(17) 0.0326(7) Uani 1 1 d . . . C2 C 0.19828(11) -0.0286(2) 0.42407(18) 0.0394(8) Uani 1 1 d . . . C11 C 0.14686(9) 0.31979(17) 0.45663(15) 0.0241(6) Uani 1 1 d . . . H11 H 0.1265 0.3522 0.4749 0.029 Uiso 1 1 calc R . . C12 C 0.12165(9) 0.50506(17) 0.39609(15) 0.0233(6) Uani 1 1 d . . . H12 H 0.1522 0.5183 0.4037 0.028 Uiso 1 1 calc R . . C13 C 0.19637(9) 0.44091(16) 0.30973(15) 0.0220(6) Uani 1 1 d . . . H13 H 0.2113 0.4324 0.3623 0.026 Uiso 1 1 calc R . . C14 C 0.08688(9) 0.31397(18) 0.26121(15) 0.0252(6) Uani 1 1 d . . . C21 C 0.18471(9) 0.26630(17) 0.38301(16) 0.0256(6) Uani 1 1 d . . . H21 H 0.1956 0.2551 0.3398 0.031 Uiso 1 1 calc R . . C22 C 0.05700(9) 0.44575(18) 0.35706(16) 0.0276(7) Uani 1 1 d . . . H22 H 0.0340 0.4092 0.3318 0.033 Uiso 1 1 calc R . . C23 C 0.18195(9) 0.48087(18) 0.18979(16) 0.0276(6) Uani 1 1 d . . . H23 H 0.1849 0.5052 0.1436 0.033 Uiso 1 1 calc R . . C24 C 0.08705(11) 0.22817(19) 0.27358(18) 0.0350(7) Uani 1 1 d . . . C31 C 0.19754(10) 0.22864(18) 0.45134(16) 0.0284(7) Uani 1 1 d . . . H31 H 0.2191 0.1861 0.4655 0.034 Uiso 1 1 calc R . . C32 C 0.05269(9) 0.50867(18) 0.40324(16) 0.0292(7) Uani 1 1 d . . . H32 H 0.0264 0.5246 0.4166 0.035 Uiso 1 1 calc R . . C33 C 0.14638(10) 0.43941(18) 0.19943(15) 0.0263(6) Uani 1 1 d . . . H33 H 0.1196 0.4291 0.1607 0.032 Uiso 1 1 calc R . . C34 C 0.05685(12) 0.1760(2) 0.2244(2) 0.0458(9) Uani 1 1 d . . . C41 C 0.17390(11) 0.23619(18) 0.57445(16) 0.0323(7) Uani 1 1 d . . . H41A H 0.1606 0.2797 0.5996 0.039 Uiso 1 1 calc R . . H41B H 0.2051 0.2281 0.6051 0.039 Uiso 1 1 calc R . . C42 C 0.10590(11) 0.61505(18) 0.48077(16) 0.0332(7) Uani 1 1 d . . . H42A H 0.1378 0.6283 0.4882 0.040 Uiso 1 1 calc R . . H42B H 0.1018 0.5986 0.5311 0.040 Uiso 1 1 calc R . . C43 C 0.25587(9) 0.52515(18) 0.28005(16) 0.0262(6) Uani 1 1 d . . . H43A H 0.2716 0.5143 0.2403 0.031 Uiso 1 1 calc R . . H43B H 0.2746 0.5039 0.3295 0.031 Uiso 1 1 calc R . . C44 C 0.02543(11) 0.2085(2) 0.1607(2) 0.0457(9) Uani 1 1 d . . . C51 C 0.14817(10) 0.15652(18) 0.57375(16) 0.0301(7) Uani 1 1 d . . . H51 H 0.1631 0.1124 0.5511 0.036 Uiso 1 1 calc . . . C52 C 0.07841(10) 0.69148(18) 0.45318(17) 0.0308(7) Uani 1 1 d . . . H52 H 0.0465 0.6776 0.4485 0.037 Uiso 1 1 calc . . . C53 C 0.25010(10) 0.61761(17) 0.28676(15) 0.0261(6) Uani 1 1 d . . . H53 H 0.2328 0.6390 0.2356 0.031 Uiso 1 1 calc . . . C54 C 0.02452(10) 0.2931(2) 0.14662(17) 0.0364(8) Uani 1 1 d . . . C61 C 0.09975(11) 0.1624(2) 0.52616(18) 0.0378(8) Uani 1 1 d . . . H61A H 0.0852 0.2092 0.5449 0.045 Uiso 1 1 calc R . . H61B H 0.0989 0.1735 0.4720 0.045 Uiso 1 1 calc R . . C62 C 0.09201(13) 0.7594(2) 0.5132(2) 0.0480(9) Uani 1 1 d . . . H62A H 0.0885 0.7397 0.5630 0.058 Uiso 1 1 calc R . . H62B H 0.1238 0.7734 0.5201 0.058 Uiso 1 1 calc R . . C63 C 0.22470(11) 0.63865(18) 0.34576(17) 0.0334(7) Uani 1 1 d . . . H63A H 0.2391 0.6111 0.3949 0.040 Uiso 1 1 calc R . . H63B H 0.1939 0.6176 0.3276 0.040 Uiso 1 1 calc R . . C64 C 0.05451(9) 0.3452(2) 0.19719(16) 0.0303(7) Uani 1 1 d . . . C71 C 0.07383(12) 0.0841(2) 0.5303(2) 0.0468(9) Uani 1 1 d . . . H71A H 0.0863 0.0384 0.5064 0.056 Uiso 1 1 calc R . . H71B H 0.0423 0.0918 0.5011 0.056 Uiso 1 1 calc R . . C72 C 0.06373(15) 0.8354(2) 0.4886(2) 0.0625(11) Uani 1 1 d . . . H72A H 0.0738 0.8792 0.5274 0.075 Uiso 1 1 calc R . . H72B H 0.0323 0.8224 0.4860 0.075 Uiso 1 1 calc R . . C73 C 0.22339(12) 0.7314(2) 0.3592(2) 0.0453(9) Uani 1 1 d . . . H73A H 0.2089 0.7422 0.4007 0.054 Uiso 1 1 calc R . . H73B H 0.2054 0.7583 0.3119 0.054 Uiso 1 1 calc R . . C81 C 0.07610(12) 0.0621(2) 0.6132(2) 0.0522(10) Uani 1 1 d . . . H81A H 0.0611 0.1053 0.6357 0.063 Uiso 1 1 calc R . . H81B H 0.0603 0.0096 0.6145 0.063 Uiso 1 1 calc R . . C82 C 0.06664(15) 0.8664(2) 0.4108(2) 0.0608(11) Uani 1 1 d . . . H82A H 0.0975 0.8842 0.4143 0.073 Uiso 1 1 calc R . . H82B H 0.0467 0.9143 0.3952 0.073 Uiso 1 1 calc R . . C83 C 0.27042(13) 0.7681(2) 0.3812(2) 0.0500(9) Uani 1 1 d . . . H83A H 0.2686 0.8283 0.3876 0.060 Uiso 1 1 calc R . . H83B H 0.2877 0.7445 0.4307 0.060 Uiso 1 1 calc R . . C91 C 0.12431(12) 0.0541(2) 0.6604(2) 0.0489(9) Uani 1 1 d . . . H91A H 0.1384 0.0074 0.6407 0.059 Uiso 1 1 calc R . . H91B H 0.1252 0.0423 0.7144 0.059 Uiso 1 1 calc R . . C92 C 0.05316(17) 0.7984(2) 0.3513(2) 0.0709(13) Uani 1 1 d . . . H92A H 0.0568 0.8180 0.3015 0.085 Uiso 1 1 calc R . . H92B H 0.0214 0.7847 0.3441 0.085 Uiso 1 1 calc R . . C93 C 0.29366(12) 0.7496(2) 0.3198(2) 0.0451(9) Uani 1 1 d . . . H93A H 0.3242 0.7726 0.3352 0.054 Uiso 1 1 calc R . . H93B H 0.2773 0.7763 0.2712 0.054 Uiso 1 1 calc R . . C101 C 0.15070(11) 0.1326(2) 0.65683(17) 0.0392(8) Uani 1 1 d . . . H10A H 0.1822 0.1242 0.6855 0.047 Uiso 1 1 calc R . . H10B H 0.1387 0.1780 0.6818 0.047 Uiso 1 1 calc R . . C102 C 0.08144(15) 0.7215(2) 0.37618(19) 0.0547(10) Uani 1 1 d . . . H10C H 0.0712 0.6777 0.3375 0.066 Uiso 1 1 calc R . . H10D H 0.1129 0.7341 0.3788 0.066 Uiso 1 1 calc R . . C103 C 0.29601(10) 0.65737(18) 0.30731(18) 0.0351(7) Uani 1 1 d . . . H10E H 0.3147 0.6317 0.3546 0.042 Uiso 1 1 calc R . . H10F H 0.3103 0.6471 0.2655 0.042 Uiso 1 1 calc R . . N11 N 0.15273(7) 0.32450(13) 0.38617(12) 0.0216(5) Uani 1 1 d . . . N12 N 0.10056(7) 0.44348(13) 0.35270(12) 0.0203(5) Uani 1 1 d . . . N13 N 0.15551(7) 0.41439(13) 0.27515(12) 0.0207(5) Uani 1 1 d . . . N21 N 0.17358(8) 0.26320(14) 0.49695(12) 0.0252(5) Uani 1 1 d . . . N22 N 0.09391(8) 0.54499(14) 0.42695(12) 0.0244(5) Uani 1 1 d . . . N23 N 0.21331(7) 0.48099(14) 0.26015(12) 0.0227(5) Uani 1 1 d . . . O1 O 0.04952(7) 0.50818(12) 0.08711(11) 0.0334(5) Uani 1 1 d . . . O2 O 0.10914(7) 0.59751(14) 0.07515(11) 0.0386(5) Uani 1 1 d . . . O3 O 0.03263(7) 0.64514(14) 0.03369(12) 0.0453(6) Uani 1 1 d . . . O4 O 0.25294(7) 0.07919(13) 0.39958(11) 0.0352(5) Uani 1 1 d . . . O5 O 0.28385(7) -0.03914(13) 0.47778(12) 0.0378(5) Uani 1 1 d . . . O6 O 0.24434(7) 0.06571(13) 0.52805(10) 0.0333(5) Uani 1 1 d . . . F1 F 0.09699(7) 0.58919(13) 0.23210(10) 0.0539(6) Uani 1 1 d . . . F2 F 0.02966(6) 0.62915(14) 0.19422(11) 0.0566(6) Uani 1 1 d . . . F3 F 0.08176(8) 0.70927(12) 0.18493(11) 0.0626(6) Uani 1 1 d . . . F4 F 0.16428(6) 0.02362(14) 0.40875(12) 0.0593(6) Uani 1 1 d . . . F5 F 0.19124(7) -0.08339(15) 0.47406(13) 0.0690(7) Uani 1 1 d . . . F6 F 0.19727(7) -0.06894(13) 0.35953(11) 0.0576(6) Uani 1 1 d . . . S1 S 0.06439(2) 0.59109(5) 0.08216(4) 0.02758(18) Uani 1 1 d . . . S2 S 0.25093(2) 0.02485(4) 0.46120(4) 0.02617(17) Uani 1 1 d . . . B1 B 0.12262(10) 0.37284(19) 0.31639(17) 0.0212(7) 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 0.0375(18) 0.0335(18) 0.0272(16) 0.0030(14) 0.0092(14) -0.0021(15) C2 0.0399(19) 0.043(2) 0.0324(18) 0.0031(16) 0.0045(15) 0.0028(17) C11 0.0297(15) 0.0239(15) 0.0190(14) -0.0015(12) 0.0071(12) 0.0032(13) C12 0.0203(14) 0.0252(15) 0.0228(14) 0.0028(12) 0.0031(11) 0.0030(12) C13 0.0236(15) 0.0223(14) 0.0195(14) 0.0009(12) 0.0048(11) 0.0008(12) C14 0.0258(15) 0.0286(16) 0.0213(14) 0.0001(12) 0.0066(12) 0.0008(13) C21 0.0272(15) 0.0240(15) 0.0272(15) -0.0009(13) 0.0099(12) 0.0042(13) C22 0.0234(15) 0.0294(16) 0.0298(16) 0.0011(13) 0.0070(13) 0.0004(13) C23 0.0272(15) 0.0370(17) 0.0186(14) 0.0030(13) 0.0064(12) 0.0028(14) C24 0.0392(18) 0.0271(17) 0.0377(18) -0.0037(14) 0.0085(15) -0.0022(15) C31 0.0290(16) 0.0241(16) 0.0310(16) 0.0012(13) 0.0062(13) 0.0061(13) C32 0.0255(15) 0.0353(18) 0.0281(16) 0.0044(14) 0.0095(13) 0.0054(13) C33 0.0288(16) 0.0335(17) 0.0154(14) 0.0030(12) 0.0038(12) 0.0060(13) C34 0.044(2) 0.040(2) 0.047(2) -0.0106(17) 0.0019(17) -0.0095(17) C41 0.0407(18) 0.0337(18) 0.0198(15) 0.0074(13) 0.0036(13) 0.0093(15) C42 0.0430(19) 0.0314(17) 0.0250(16) -0.0076(13) 0.0089(14) 0.0019(15) C43 0.0226(14) 0.0313(16) 0.0254(15) 0.0004(13) 0.0079(12) -0.0037(13) C44 0.041(2) 0.052(2) 0.043(2) -0.0134(18) 0.0080(17) -0.0068(17) C51 0.0388(18) 0.0242(16) 0.0270(16) 0.0042(13) 0.0084(14) 0.0093(14) C52 0.0269(16) 0.0271(16) 0.0375(18) -0.0044(14) 0.0069(14) 0.0009(13) C53 0.0338(16) 0.0236(15) 0.0217(14) 0.0024(12) 0.0087(12) 0.0001(13) C54 0.0330(17) 0.048(2) 0.0284(17) -0.0076(15) 0.0082(14) -0.0016(16) C61 0.047(2) 0.0353(19) 0.0309(17) 0.0036(15) 0.0093(15) 0.0028(16) C62 0.069(3) 0.036(2) 0.043(2) -0.0078(17) 0.0228(19) 0.0039(18) C63 0.0407(18) 0.0312(17) 0.0316(17) -0.0018(14) 0.0157(14) 0.0018(15) C64 0.0239(15) 0.0431(19) 0.0227(15) -0.0034(14) 0.0043(12) -0.0021(14) C71 0.044(2) 0.042(2) 0.052(2) 0.0017(18) 0.0089(17) -0.0033(17) C72 0.083(3) 0.035(2) 0.076(3) -0.011(2) 0.032(2) 0.009(2) C73 0.056(2) 0.0340(19) 0.052(2) -0.0065(17) 0.0246(19) 0.0008(17) C81 0.052(2) 0.049(2) 0.061(2) 0.0172(19) 0.024(2) 0.0026(19) C82 0.081(3) 0.027(2) 0.064(3) 0.0012(19) 0.003(2) 0.005(2) C83 0.065(3) 0.034(2) 0.054(2) -0.0124(17) 0.0203(19) -0.0079(18) C91 0.057(2) 0.046(2) 0.047(2) 0.0207(18) 0.0195(18) 0.0086(18) C92 0.112(4) 0.039(2) 0.049(2) 0.0054(19) 0.000(2) 0.010(2) C93 0.051(2) 0.0322(19) 0.055(2) -0.0002(16) 0.0180(18) -0.0082(16) C101 0.047(2) 0.039(2) 0.0322(17) 0.0128(15) 0.0116(15) 0.0124(16) C102 0.094(3) 0.036(2) 0.0332(19) -0.0005(16) 0.016(2) 0.011(2) C103 0.0396(18) 0.0287(17) 0.0404(18) -0.0007(14) 0.0165(15) -0.0061(14) N11 0.0227(12) 0.0215(12) 0.0197(11) -0.0002(10) 0.0039(9) 0.0026(10) N12 0.0190(12) 0.0221(12) 0.0189(11) 0.0033(10) 0.0037(9) 0.0028(10) N13 0.0237(12) 0.0219(12) 0.0160(11) 0.0008(10) 0.0044(9) 0.0026(10) N21 0.0296(13) 0.0249(13) 0.0193(12) 0.0034(10) 0.0033(10) 0.0055(11) N22 0.0264(13) 0.0250(13) 0.0211(12) 0.0008(10) 0.0052(10) 0.0065(10) N23 0.0246(12) 0.0234(13) 0.0201(12) 0.0020(10) 0.0060(10) 0.0012(10) O1 0.0355(12) 0.0340(12) 0.0318(11) -0.0017(9) 0.0107(9) -0.0066(10) O2 0.0343(12) 0.0550(15) 0.0287(11) 0.0059(10) 0.0120(9) -0.0084(11) O3 0.0498(14) 0.0485(15) 0.0295(12) 0.0068(11) -0.0032(11) 0.0120(12) O4 0.0469(13) 0.0349(12) 0.0264(11) 0.0034(10) 0.0142(10) 0.0040(10) O5 0.0338(12) 0.0337(13) 0.0433(13) -0.0044(10) 0.0057(10) 0.0105(10) O6 0.0409(12) 0.0385(12) 0.0177(10) -0.0017(9) 0.0028(9) 0.0130(10) F1 0.0662(14) 0.0674(14) 0.0229(9) 0.0022(10) 0.0031(9) 0.0247(12) F2 0.0462(12) 0.0834(16) 0.0465(12) -0.0180(11) 0.0231(10) -0.0027(11) F3 0.1027(18) 0.0413(12) 0.0446(12) -0.0078(10) 0.0215(12) -0.0247(12) F4 0.0292(10) 0.0705(15) 0.0691(14) -0.0004(12) -0.0027(10) 0.0095(11) F5 0.0594(14) 0.0775(17) 0.0640(15) 0.0235(13) 0.0062(11) -0.0268(12) F6 0.0654(14) 0.0501(13) 0.0470(12) -0.0172(10) -0.0027(10) -0.0103(11) S1 0.0283(4) 0.0329(4) 0.0207(4) 0.0047(3) 0.0050(3) -0.0013(3) S2 0.0275(4) 0.0283(4) 0.0216(4) -0.0015(3) 0.0047(3) 0.0044(3) B1 0.0239(16) 0.0217(17) 0.0179(15) 0.0024(13) 0.0053(13) 0.0030(13) _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 F3 1.325(4) . ? C1 F2 1.326(3) . ? C1 F1 1.328(3) . ? C1 S1 1.820(3) . ? C2 F4 1.328(4) . ? C2 F5 1.330(4) . ? C2 F6 1.332(4) . ? C2 S2 1.819(3) . ? C11 N21 1.322(3) . ? C11 N11 1.337(3) . ? C11 H11 0.9500 . ? C12 N22 1.319(3) . ? C12 N12 1.332(3) . ? C12 H12 0.9500 . ? C13 N23 1.328(3) . ? C13 N13 1.331(3) . ? C13 H13 0.9500 . ? C14 C64 1.411(4) . ? C14 C24 1.414(4) . ? C14 B1 1.599(4) . ? C21 C31 1.341(4) . ? C21 N11 1.387(3) . ? C21 H21 0.9500 . ? C22 C32 1.351(4) . ? C22 N12 1.382(3) . ? C22 H22 0.9500 . ? C23 C33 1.349(4) . ? C23 N23 1.381(3) . ? C23 H23 0.9500 . ? C24 C34 1.395(4) . ? C31 N21 1.373(3) . ? C31 H31 0.9500 . ? C32 N22 1.374(4) . ? C32 H32 0.9500 . ? C33 N13 1.383(3) . ? C33 H33 0.9500 . ? C34 C44 1.400(5) . ? C41 N21 1.467(3) . ? C41 C51 1.523(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N22 1.480(4) . ? C42 C52 1.517(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 N23 1.466(3) . ? C43 C53 1.524(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C54 1.398(5) . ? C51 C61 1.527(4) . ? C51 C101 1.534(4) . ? C51 H51 1.0000 . ? C52 C102 1.503(4) . ? C52 C62 1.527(4) . ? C52 H52 1.0000 . ? C53 C103 1.523(4) . ? C53 C63 1.529(4) . ? C53 H53 1.0000 . ? C54 C64 1.404(4) . ? C61 C71 1.521(5) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C72 1.514(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C73 1.531(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C71 C81 1.524(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C82 1.520(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C83 1.533(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C81 C91 1.522(5) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C92 1.522(5) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C93 1.510(5) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C91 C101 1.531(5) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C102 1.527(5) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C103 1.523(4) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? N11 B1 1.568(4) . ? N12 B1 1.571(4) . ? N13 B1 1.573(4) . ? O1 S1 1.437(2) . ? O2 S1 1.438(2) . ? O3 S1 1.434(2) . ? O4 S2 1.437(2) . ? O5 S2 1.436(2) . ? O6 S2 1.4420(19) . ? 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 F3 C1 F2 106.5(3) . . ? F3 C1 F1 107.1(3) . . ? F2 C1 F1 106.6(2) . . ? F3 C1 S1 112.4(2) . . ? F2 C1 S1 111.6(2) . . ? F1 C1 S1 112.3(2) . . ? F4 C2 F5 107.6(3) . . ? F4 C2 F6 107.6(3) . . ? F5 C2 F6 107.2(3) . . ? F4 C2 S2 111.2(2) . . ? F5 C2 S2 111.5(2) . . ? F6 C2 S2 111.5(2) . . ? N21 C11 N11 109.8(2) . . ? N21 C11 H11 125.1 . . ? N11 C11 H11 125.1 . . ? N22 C12 N12 110.1(2) . . ? N22 C12 H12 124.9 . . ? N12 C12 H12 124.9 . . ? N23 C13 N13 110.2(2) . . ? N23 C13 H13 124.9 . . ? N13 C13 H13 124.9 . . ? C64 C14 C24 117.2(3) . . ? C64 C14 B1 121.4(3) . . ? C24 C14 B1 121.3(3) . . ? C31 C21 N11 108.3(2) . . ? C31 C21 H21 125.9 . . ? N11 C21 H21 125.9 . . ? C32 C22 N12 108.5(3) . . ? C32 C22 H22 125.7 . . ? N12 C22 H22 125.7 . . ? C33 C23 N23 106.5(2) . . ? C33 C23 H23 126.7 . . ? N23 C23 H23 126.7 . . ? C34 C24 C14 121.7(3) . . ? C21 C31 N21 106.9(2) . . ? C21 C31 H31 126.5 . . ? N21 C31 H31 126.5 . . ? C22 C32 N22 106.2(2) . . ? C22 C32 H32 126.9 . . ? N22 C32 H32 126.9 . . ? C23 C33 N13 108.5(2) . . ? C23 C33 H33 125.7 . . ? N13 C33 H33 125.7 . . ? C24 C34 C44 119.9(3) . . ? N21 C41 C51 112.3(2) . . ? N21 C41 H41A 109.2 . . ? C51 C41 H41A 109.2 . . ? N21 C41 H41B 109.2 . . ? C51 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? N22 C42 C52 113.2(2) . . ? N22 C42 H42A 108.9 . . ? C52 C42 H42A 108.9 . . ? N22 C42 H42B 108.9 . . ? C52 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? N23 C43 C53 112.6(2) . . ? N23 C43 H43A 109.1 . . ? C53 C43 H43A 109.1 . . ? N23 C43 H43B 109.1 . . ? C53 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C54 C44 C34 119.8(3) . . ? C41 C51 C61 112.9(2) . . ? C41 C51 C101 108.6(2) . . ? C61 C51 C101 110.6(3) . . ? C41 C51 H51 108.2 . . ? C61 C51 H51 108.2 . . ? C101 C51 H51 108.2 . . ? C102 C52 C42 113.6(3) . . ? C102 C52 C62 110.4(3) . . ? C42 C52 C62 109.6(3) . . ? C102 C52 H52 107.7 . . ? C42 C52 H52 107.7 . . ? C62 C52 H52 107.7 . . ? C103 C53 C43 108.4(2) . . ? C103 C53 C63 111.3(2) . . ? C43 C53 C63 111.8(2) . . ? C103 C53 H53 108.4 . . ? C43 C53 H53 108.4 . . ? C63 C53 H53 108.4 . . ? C44 C54 C64 119.9(3) . . ? C71 C61 C51 112.1(3) . . ? C71 C61 H61A 109.2 . . ? C51 C61 H61A 109.2 . . ? C71 C61 H61B 109.2 . . ? C51 C61 H61B 109.2 . . ? H61A C61 H61B 107.9 . . ? C72 C62 C52 110.7(3) . . ? C72 C62 H62A 109.5 . . ? C52 C62 H62A 109.5 . . ? C72 C62 H62B 109.5 . . ? C52 C62 H62B 109.5 . . ? H62A C62 H62B 108.1 . . ? C53 C63 C73 111.9(2) . . ? C53 C63 H63A 109.2 . . ? C73 C63 H63A 109.2 . . ? C53 C63 H63B 109.2 . . ? C73 C63 H63B 109.2 . . ? H63A C63 H63B 107.9 . . ? C54 C64 C14 121.4(3) . . ? C61 C71 C81 111.1(3) . . ? C61 C71 H71A 109.4 . . ? C81 C71 H71A 109.4 . . ? C61 C71 H71B 109.4 . . ? C81 C71 H71B 109.4 . . ? H71A C71 H71B 108.0 . . ? C62 C72 C82 111.6(3) . . ? C62 C72 H72A 109.3 . . ? C82 C72 H72A 109.3 . . ? C62 C72 H72B 109.3 . . ? C82 C72 H72B 109.3 . . ? H72A C72 H72B 108.0 . . ? C63 C73 C83 111.1(3) . . ? C63 C73 H73A 109.4 . . ? C83 C73 H73A 109.4 . . ? C63 C73 H73B 109.4 . . ? C83 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? C91 C81 C71 110.5(3) . . ? C91 C81 H81A 109.6 . . ? C71 C81 H81A 109.6 . . ? C91 C81 H81B 109.6 . . ? C71 C81 H81B 109.6 . . ? H81A C81 H81B 108.1 . . ? C72 C82 C92 109.9(3) . . ? C72 C82 H82A 109.7 . . ? C92 C82 H82A 109.7 . . ? C72 C82 H82B 109.7 . . ? C92 C82 H82B 109.7 . . ? H82A C82 H82B 108.2 . . ? C93 C83 C73 110.3(3) . . ? C93 C83 H83A 109.6 . . ? C73 C83 H83A 109.6 . . ? C93 C83 H83B 109.6 . . ? C73 C83 H83B 109.6 . . ? H83A C83 H83B 108.1 . . ? C81 C91 C101 111.5(3) . . ? C81 C91 H91A 109.3 . . ? C101 C91 H91A 109.3 . . ? C81 C91 H91B 109.3 . . ? C101 C91 H91B 109.3 . . ? H91A C91 H91B 108.0 . . ? C82 C92 C102 111.0(3) . . ? C82 C92 H92A 109.4 . . ? C102 C92 H92A 109.4 . . ? C82 C92 H92B 109.4 . . ? C102 C92 H92B 109.4 . . ? H92A C92 H92B 108.0 . . ? C83 C93 C103 110.9(3) . . ? C83 C93 H93A 109.5 . . ? C103 C93 H93A 109.5 . . ? C83 C93 H93B 109.5 . . ? C103 C93 H93B 109.5 . . ? H93A C93 H93B 108.1 . . ? C91 C101 C51 111.4(3) . . ? C91 C101 H10A 109.3 . . ? C51 C101 H10A 109.3 . . ? C91 C101 H10B 109.3 . . ? C51 C101 H10B 109.3 . . ? H10A C101 H10B 108.0 . . ? C52 C102 C92 111.4(3) . . ? C52 C102 H10C 109.3 . . ? C92 C102 H10C 109.3 . . ? C52 C102 H10D 109.3 . . ? C92 C102 H10D 109.3 . . ? H10C C102 H10D 108.0 . . ? C93 C103 C53 112.0(3) . . ? C93 C103 H10E 109.2 . . ? C53 C103 H10E 109.2 . . ? C93 C103 H10F 109.2 . . ? C53 C103 H10F 109.2 . . ? H10E C103 H10F 107.9 . . ? C11 N11 C21 106.5(2) . . ? C11 N11 B1 126.2(2) . . ? C21 N11 B1 126.2(2) . . ? C12 N12 C22 106.5(2) . . ? C12 N12 B1 126.5(2) . . ? C22 N12 B1 126.2(2) . . ? C13 N13 C33 106.6(2) . . ? C13 N13 B1 125.4(2) . . ? C33 N13 B1 127.5(2) . . ? C11 N21 C31 108.5(2) . . ? C11 N21 C41 125.3(2) . . ? C31 N21 C41 125.9(2) . . ? C12 N22 C32 108.7(2) . . ? C12 N22 C42 125.4(2) . . ? C32 N22 C42 125.9(2) . . ? C13 N23 C23 108.1(2) . . ? C13 N23 C43 124.9(2) . . ? C23 N23 C43 126.7(2) . . ? O3 S1 O1 115.62(13) . . ? O3 S1 O2 115.38(13) . . ? O1 S1 O2 114.23(13) . . ? O3 S1 C1 102.71(14) . . ? O1 S1 C1 102.87(13) . . ? O2 S1 C1 103.50(13) . . ? O5 S2 O4 115.50(13) . . ? O5 S2 O6 114.45(12) . . ? O4 S2 O6 114.35(12) . . ? O5 S2 C2 104.71(14) . . ? O4 S2 C2 103.33(14) . . ? O6 S2 C2 102.27(14) . . ? N11 B1 N12 105.4(2) . . ? N11 B1 N13 105.8(2) . . ? N12 B1 N13 107.3(2) . . ? N11 B1 C14 111.6(2) . . ? N12 B1 C14 112.9(2) . . ? N13 B1 C14 113.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C64 C14 C24 C34 0.5(4) . . . . ? B1 C14 C24 C34 -178.0(3) . . . . ? N11 C21 C31 N21 0.1(3) . . . . ? N12 C22 C32 N22 0.1(3) . . . . ? N23 C23 C33 N13 0.3(3) . . . . ? C14 C24 C34 C44 0.3(5) . . . . ? C24 C34 C44 C54 0.1(5) . . . . ? N21 C41 C51 C61 -57.5(3) . . . . ? N21 C41 C51 C101 179.4(2) . . . . ? N22 C42 C52 C102 -57.7(4) . . . . ? N22 C42 C52 C62 178.3(3) . . . . ? N23 C43 C53 C103 -179.9(2) . . . . ? N23 C43 C53 C63 57.1(3) . . . . ? C34 C44 C54 C64 -1.3(5) . . . . ? C41 C51 C61 C71 -176.3(3) . . . . ? C101 C51 C61 C71 -54.4(3) . . . . ? C102 C52 C62 C72 56.5(4) . . . . ? C42 C52 C62 C72 -177.6(3) . . . . ? C103 C53 C63 C73 52.2(3) . . . . ? C43 C53 C63 C73 173.6(3) . . . . ? C44 C54 C64 C14 2.1(4) . . . . ? C24 C14 C64 C54 -1.7(4) . . . . ? B1 C14 C64 C54 176.9(3) . . . . ? C51 C61 C71 C81 56.0(4) . . . . ? C52 C62 C72 C82 -57.1(4) . . . . ? C53 C63 C73 C83 -54.4(4) . . . . ? C61 C71 C81 C91 -56.4(4) . . . . ? C62 C72 C82 C92 56.6(5) . . . . ? C63 C73 C83 C93 57.1(4) . . . . ? C71 C81 C91 C101 56.4(4) . . . . ? C72 C82 C92 C102 -55.8(5) . . . . ? C73 C83 C93 C103 -58.0(4) . . . . ? C81 C91 C101 C51 -55.7(4) . . . . ? C41 C51 C101 C91 178.3(3) . . . . ? C61 C51 C101 C91 53.9(3) . . . . ? C42 C52 C102 C92 180.0(3) . . . . ? C62 C52 C102 C92 -56.4(4) . . . . ? C82 C92 C102 C52 56.8(5) . . . . ? C83 C93 C103 C53 56.7(4) . . . . ? C43 C53 C103 C93 -176.7(2) . . . . ? C63 C53 C103 C93 -53.3(3) . . . . ? N21 C11 N11 C21 0.8(3) . . . . ? N21 C11 N11 B1 169.4(2) . . . . ? C31 C21 N11 C11 -0.5(3) . . . . ? C31 C21 N11 B1 -169.1(2) . . . . ? N22 C12 N12 C22 0.1(3) . . . . ? N22 C12 N12 B1 -169.7(2) . . . . ? C32 C22 N12 C12 -0.1(3) . . . . ? C32 C22 N12 B1 169.7(2) . . . . ? N23 C13 N13 C33 0.0(3) . . . . ? N23 C13 N13 B1 -173.0(2) . . . . ? C23 C33 N13 C13 -0.2(3) . . . . ? C23 C33 N13 B1 172.6(2) . . . . ? N11 C11 N21 C31 -0.7(3) . . . . ? N11 C11 N21 C41 -174.8(2) . . . . ? C21 C31 N21 C11 0.4(3) . . . . ? C21 C31 N21 C41 174.4(3) . . . . ? C51 C41 N21 C11 98.9(3) . . . . ? C51 C41 N21 C31 -74.1(4) . . . . ? N12 C12 N22 C32 0.0(3) . . . . ? N12 C12 N22 C42 177.6(2) . . . . ? C22 C32 N22 C12 -0.1(3) . . . . ? C22 C32 N22 C42 -177.7(2) . . . . ? C52 C42 N22 C12 123.4(3) . . . . ? C52 C42 N22 C32 -59.3(4) . . . . ? N13 C13 N23 C23 0.2(3) . . . . ? N13 C13 N23 C43 173.9(2) . . . . ? C33 C23 N23 C13 -0.3(3) . . . . ? C33 C23 N23 C43 -173.8(2) . . . . ? C53 C43 N23 C13 -100.2(3) . . . . ? C53 C43 N23 C23 72.3(3) . . . . ? F3 C1 S1 O3 -59.1(3) . . . . ? F2 C1 S1 O3 60.4(2) . . . . ? F1 C1 S1 O3 -180.0(2) . . . . ? F3 C1 S1 O1 -179.5(2) . . . . ? F2 C1 S1 O1 -60.0(2) . . . . ? F1 C1 S1 O1 59.6(2) . . . . ? F3 C1 S1 O2 61.3(3) . . . . ? F2 C1 S1 O2 -179.2(2) . . . . ? F1 C1 S1 O2 -59.6(2) . . . . ? F4 C2 S2 O5 177.7(2) . . . . ? F5 C2 S2 O5 57.6(3) . . . . ? F6 C2 S2 O5 -62.2(2) . . . . ? F4 C2 S2 O4 -61.0(2) . . . . ? F5 C2 S2 O4 178.9(2) . . . . ? F6 C2 S2 O4 59.1(3) . . . . ? F4 C2 S2 O6 58.0(2) . . . . ? F5 C2 S2 O6 -62.1(3) . . . . ? F6 C2 S2 O6 178.1(2) . . . . ? C11 N11 B1 N12 25.8(3) . . . . ? C21 N11 B1 N12 -167.7(2) . . . . ? C11 N11 B1 N13 139.3(2) . . . . ? C21 N11 B1 N13 -54.2(3) . . . . ? C11 N11 B1 C14 -97.1(3) . . . . ? C21 N11 B1 C14 69.4(3) . . . . ? C12 N12 B1 N11 63.3(3) . . . . ? C22 N12 B1 N11 -104.6(3) . . . . ? C12 N12 B1 N13 -49.1(3) . . . . ? C22 N12 B1 N13 143.0(2) . . . . ? C12 N12 B1 C14 -174.7(2) . . . . ? C22 N12 B1 C14 17.5(4) . . . . ? C13 N13 B1 N11 -32.1(3) . . . . ? C33 N13 B1 N11 156.3(2) . . . . ? C13 N13 B1 N12 80.0(3) . . . . ? C33 N13 B1 N12 -91.5(3) . . . . ? C13 N13 B1 C14 -154.7(2) . . . . ? C33 N13 B1 C14 33.8(4) . . . . ? C64 C14 B1 N11 176.2(2) . . . . ? C24 C14 B1 N11 -5.3(4) . . . . ? C64 C14 B1 N12 57.7(3) . . . . ? C24 C14 B1 N12 -123.8(3) . . . . ? C64 C14 B1 N13 -64.6(3) . . . . ? C24 C14 B1 N13 113.9(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.702 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.065 _iucr_refine_instruction_details ; TITL js140_0m in C2/c CELL 0.71073 31.1770 16.2710 18.0874 90.000 105.572 90.000 ZERR 8.00 0.0019 0.0009 0.0009 0.000 0.004 0.000 LATT 7 SYMM -x, y, -z+1/2 SFAC C H N O F S B UNIT 304 384 48 48 48 16 8 TEMP -123.000 SIZE 0.023 0.023 0.276 ACTA CONF OMIT 1 1 0 OMIT 2 0 0 L.S. 10 FMAP 2 PLAN 10 BOND $H WGHT 0.060600 7.529500 FVAR 0.05006 C1 1 0.068564 0.631555 0.177616 11.00000 0.03751 0.03347 = 0.02720 0.00302 0.00916 -0.00214 C2 1 0.198283 -0.028587 0.424065 11.00000 0.03994 0.04295 = 0.03242 0.00311 0.00448 0.00278 C11 1 0.146860 0.319793 0.456629 11.00000 0.02972 0.02385 = 0.01899 -0.00147 0.00713 0.00320 AFIX 43 H11 2 0.126541 0.352240 0.474948 11.00000 -1.20000 AFIX 0 C12 1 0.121649 0.505060 0.396091 11.00000 0.02030 0.02518 = 0.02283 0.00281 0.00309 0.00301 AFIX 43 H12 2 0.152206 0.518287 0.403702 11.00000 -1.20000 AFIX 0 C13 1 0.196374 0.440913 0.309726 11.00000 0.02361 0.02226 = 0.01947 0.00088 0.00476 0.00083 AFIX 43 H13 2 0.211269 0.432386 0.362315 11.00000 -1.20000 AFIX 0 C14 1 0.086875 0.313973 0.261215 11.00000 0.02583 0.02857 = 0.02129 0.00008 0.00664 0.00079 C21 1 0.184706 0.266304 0.383015 11.00000 0.02720 0.02398 = 0.02724 -0.00086 0.00988 0.00415 AFIX 43 H21 2 0.195638 0.255063 0.339836 11.00000 -1.20000 AFIX 0 C22 1 0.056999 0.445750 0.357059 11.00000 0.02339 0.02939 = 0.02980 0.00108 0.00702 0.00041 AFIX 43 H22 2 0.033952 0.409191 0.331815 11.00000 -1.20000 AFIX 0 C23 1 0.181950 0.480869 0.189788 11.00000 0.02723 0.03700 = 0.01859 0.00299 0.00642 0.00284 AFIX 43 H23 2 0.184860 0.505219 0.143643 11.00000 -1.20000 AFIX 0 C24 1 0.087053 0.228167 0.273577 11.00000 0.03919 0.02708 = 0.03767 -0.00374 0.00850 -0.00217 C31 1 0.197538 0.228635 0.451345 11.00000 0.02905 0.02409 = 0.03103 0.00116 0.00617 0.00611 AFIX 43 H31 2 0.219088 0.186149 0.465502 11.00000 -1.20000 AFIX 0 C32 1 0.052694 0.508674 0.403240 11.00000 0.02555 0.03533 = 0.02814 0.00441 0.00953 0.00539 AFIX 43 H32 2 0.026442 0.524625 0.416641 11.00000 -1.20000 AFIX 0 C33 1 0.146385 0.439410 0.199430 11.00000 0.02882 0.03350 = 0.01543 0.00298 0.00379 0.00605 AFIX 43 H33 2 0.119576 0.429119 0.160730 11.00000 -1.20000 AFIX 0 C34 1 0.056852 0.176043 0.224422 11.00000 0.04364 0.04042 = 0.04728 -0.01055 0.00189 -0.00948 C41 1 0.173899 0.236189 0.574446 11.00000 0.04072 0.03369 = 0.01980 0.00737 0.00356 0.00931 AFIX 23 H41A 2 0.160610 0.279692 0.599561 11.00000 -1.20000 H41B 2 0.205083 0.228141 0.605074 11.00000 -1.20000 AFIX 0 C42 1 0.105903 0.615049 0.480766 11.00000 0.04299 0.03136 = 0.02501 -0.00758 0.00891 0.00191 AFIX 23 H42A 2 0.137778 0.628289 0.488242 11.00000 -1.20000 H42B 2 0.101847 0.598559 0.531142 11.00000 -1.20000 AFIX 0 C43 1 0.255869 0.525152 0.280050 11.00000 0.02260 0.03129 = 0.02545 0.00042 0.00792 -0.00375 AFIX 23 H43A 2 0.271620 0.514275 0.240263 11.00000 -1.20000 H43B 2 0.274622 0.503898 0.329479 11.00000 -1.20000 AFIX 0 C44 1 0.025434 0.208537 0.160724 11.00000 0.04085 0.05166 = 0.04287 -0.01344 0.00803 -0.00676 C51 1 0.148168 0.156515 0.573745 11.00000 0.03884 0.02425 = 0.02697 0.00418 0.00839 0.00931 AFIX 11 H51 2 0.163072 0.112445 0.551102 11.00000 -1.20000 AFIX 0 C52 1 0.078409 0.691479 0.453179 11.00000 0.02693 0.02706 = 0.03751 -0.00437 0.00694 0.00095 AFIX 11 H52 2 0.046545 0.677603 0.448514 11.00000 -1.20000 AFIX 0 C53 1 0.250098 0.617613 0.286764 11.00000 0.03380 0.02356 = 0.02169 0.00237 0.00871 0.00008 AFIX 11 H53 2 0.232798 0.639014 0.235621 11.00000 -1.20000 AFIX 0 C54 1 0.024521 0.293106 0.146616 11.00000 0.03301 0.04776 = 0.02845 -0.00757 0.00824 -0.00164 C61 1 0.099747 0.162446 0.526156 11.00000 0.04653 0.03529 = 0.03092 0.00355 0.00928 0.00280 AFIX 23 H61A 2 0.085248 0.209166 0.544940 11.00000 -1.20000 H61B 2 0.098924 0.173518 0.471973 11.00000 -1.20000 AFIX 0 C62 1 0.092013 0.759442 0.513157 11.00000 0.06913 0.03594 = 0.04341 -0.00777 0.02280 0.00390 AFIX 23 H62A 2 0.088481 0.739698 0.562962 11.00000 -1.20000 H62B 2 0.123759 0.773392 0.520121 11.00000 -1.20000 AFIX 0 C63 1 0.224698 0.638648 0.345761 11.00000 0.04070 0.03119 = 0.03164 -0.00176 0.01566 0.00185 AFIX 23 H63A 2 0.239140 0.611053 0.394923 11.00000 -1.20000 H63B 2 0.193868 0.617552 0.327601 11.00000 -1.20000 AFIX 0 C64 1 0.054508 0.345247 0.197186 11.00000 0.02392 0.04309 = 0.02269 -0.00338 0.00434 -0.00211 C71 1 0.073830 0.084147 0.530326 11.00000 0.04425 0.04161 = 0.05209 0.00171 0.00889 -0.00331 AFIX 23 H71A 2 0.086257 0.038429 0.506434 11.00000 -1.20000 H71B 2 0.042340 0.091776 0.501096 11.00000 -1.20000 AFIX 0 C72 1 0.063733 0.835368 0.488572 11.00000 0.08340 0.03469 = 0.07566 -0.01081 0.03192 0.00852 AFIX 23 H72A 2 0.073794 0.879162 0.527355 11.00000 -1.20000 H72B 2 0.032337 0.822399 0.485967 11.00000 -1.20000 AFIX 0 C73 1 0.223387 0.731376 0.359199 11.00000 0.05566 0.03403 = 0.05217 -0.00655 0.02458 0.00077 AFIX 23 H73A 2 0.208935 0.742164 0.400739 11.00000 -1.20000 H73B 2 0.205403 0.758310 0.311928 11.00000 -1.20000 AFIX 0 C81 1 0.076102 0.062129 0.613174 11.00000 0.05207 0.04859 = 0.06089 0.01723 0.02352 0.00265 AFIX 23 H81A 2 0.061113 0.105333 0.635665 11.00000 -1.20000 H81B 2 0.060316 0.009583 0.614500 11.00000 -1.20000 AFIX 0 C82 1 0.066638 0.866386 0.410794 11.00000 0.08134 0.02745 = 0.06394 0.00120 0.00281 0.00498 AFIX 23 H82A 2 0.097473 0.884236 0.414258 11.00000 -1.20000 H82B 2 0.046686 0.914292 0.395152 11.00000 -1.20000 AFIX 0 C83 1 0.270421 0.768052 0.381206 11.00000 0.06453 0.03353 = 0.05432 -0.01245 0.02025 -0.00794 AFIX 23 H83A 2 0.268631 0.828274 0.387605 11.00000 -1.20000 H83B 2 0.287737 0.744521 0.430704 11.00000 -1.20000 AFIX 0 C91 1 0.124310 0.054084 0.660364 11.00000 0.05717 0.04594 = 0.04672 0.02068 0.01950 0.00860 AFIX 23 H91A 2 0.138386 0.007367 0.640736 11.00000 -1.20000 H91B 2 0.125154 0.042289 0.714432 11.00000 -1.20000 AFIX 0 C92 1 0.053161 0.798430 0.351272 11.00000 0.11244 0.03887 = 0.04903 0.00537 0.00048 0.00998 AFIX 23 H92A 2 0.056837 0.817967 0.301497 11.00000 -1.20000 H92B 2 0.021367 0.784736 0.344111 11.00000 -1.20000 AFIX 0 C93 1 0.293662 0.749646 0.319811 11.00000 0.05066 0.03222 = 0.05470 -0.00019 0.01804 -0.00816 AFIX 23 H93A 2 0.324175 0.772630 0.335180 11.00000 -1.20000 H93B 2 0.277350 0.776277 0.271174 11.00000 -1.20000 AFIX 0 C101 1 0.150704 0.132629 0.656832 11.00000 0.04701 0.03888 = 0.03224 0.01282 0.01159 0.01235 AFIX 23 H10A 2 0.182228 0.124153 0.685488 11.00000 -1.20000 H10B 2 0.138712 0.178043 0.681784 11.00000 -1.20000 AFIX 0 C102 1 0.081443 0.721536 0.376182 11.00000 0.09408 0.03631 = 0.03322 -0.00047 0.01598 0.01128 AFIX 23 H10C 2 0.071215 0.677671 0.337534 11.00000 -1.20000 H10D 2 0.112886 0.734055 0.378755 11.00000 -1.20000 AFIX 0 C103 1 0.296011 0.657371 0.307306 11.00000 0.03957 0.02871 = 0.04041 -0.00073 0.01650 -0.00613 AFIX 23 H10E 2 0.314736 0.631660 0.354626 11.00000 -1.20000 H10F 2 0.310320 0.647130 0.265487 11.00000 -1.20000 AFIX 0 N11 3 0.152734 0.324496 0.386174 11.00000 0.02270 0.02153 = 0.01965 -0.00021 0.00391 0.00260 N12 3 0.100560 0.443480 0.352700 11.00000 0.01896 0.02208 = 0.01894 0.00335 0.00366 0.00277 N13 3 0.155510 0.414393 0.275147 11.00000 0.02373 0.02186 = 0.01595 0.00082 0.00436 0.00259 N21 3 0.173583 0.263196 0.496945 11.00000 0.02961 0.02491 = 0.01929 0.00339 0.00326 0.00545 N22 3 0.093913 0.544994 0.426950 11.00000 0.02637 0.02504 = 0.02106 0.00083 0.00519 0.00650 N23 3 0.213312 0.480988 0.260146 11.00000 0.02457 0.02340 = 0.02007 0.00204 0.00602 0.00119 O1 4 0.049525 0.508181 0.087107 11.00000 0.03550 0.03398 = 0.03176 -0.00168 0.01073 -0.00656 O2 4 0.109143 0.597506 0.075152 11.00000 0.03425 0.05498 = 0.02866 0.00592 0.01199 -0.00842 O3 4 0.032630 0.645142 0.033686 11.00000 0.04978 0.04854 = 0.02954 0.00678 -0.00318 0.01197 O4 4 0.252943 0.079191 0.399577 11.00000 0.04692 0.03493 = 0.02641 0.00336 0.01425 0.00403 O5 4 0.283852 -0.039138 0.477779 11.00000 0.03384 0.03375 = 0.04327 -0.00437 0.00572 0.01054 O6 4 0.244343 0.065711 0.528048 11.00000 0.04091 0.03852 = 0.01769 -0.00174 0.00284 0.01295 F1 5 0.096994 0.589192 0.232102 11.00000 0.06619 0.06737 = 0.02288 0.00224 0.00308 0.02470 F2 5 0.029661 0.629151 0.194224 11.00000 0.04616 0.08336 = 0.04645 -0.01796 0.02310 -0.00268 F3 5 0.081763 0.709267 0.184929 11.00000 0.10272 0.04129 = 0.04464 -0.00781 0.02149 -0.02469 F4 5 0.164279 0.023625 0.408749 11.00000 0.02923 0.07050 = 0.06906 -0.00043 -0.00266 0.00947 F5 5 0.191241 -0.083391 0.474060 11.00000 0.05941 0.07752 = 0.06398 0.02354 0.00617 -0.02675 F6 5 0.197273 -0.068939 0.359531 11.00000 0.06545 0.05013 = 0.04700 -0.01720 -0.00269 -0.01025 S1 6 0.064392 0.591092 0.082159 11.00000 0.02830 0.03286 = 0.02066 0.00466 0.00497 -0.00132 S2 6 0.250933 0.024852 0.461205 11.00000 0.02752 0.02828 = 0.02159 -0.00147 0.00467 0.00442 B1 7 0.122619 0.372840 0.316386 11.00000 0.02387 0.02168 = 0.01788 0.00244 0.00531 0.00297 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM js140_0m in C2/c REM R1 = 0.0598 for 5837 Fo > 4sig(Fo) and 0.1400 for all 11013 data REM 532 parameters refined using 0 restraints END WGHT 0.0606 7.5407 REM Highest difference peak 0.702, deepest hole -0.374, 1-sigma level 0.065 Q1 1 0.0010 0.3167 0.1018 11.00000 0.05 0.70 Q2 1 0.1108 0.2042 0.3216 11.00000 0.05 0.63 Q3 1 0.0553 0.4053 0.1826 11.00000 0.05 0.61 Q4 1 0.0069 0.1718 0.1253 11.00000 0.05 0.55 Q5 1 0.0552 0.1137 0.2409 11.00000 0.05 0.53 Q6 1 0.1038 0.3432 0.2907 11.00000 0.05 0.33 Q7 1 0.0214 0.2472 0.1633 11.00000 0.05 0.31 Q8 1 0.0630 0.6190 0.1305 11.00000 0.05 0.29 Q9 1 0.0912 0.8061 0.3387 11.00000 0.05 0.28 Q10 1 0.0950 0.2698 0.2689 11.00000 0.05 0.25 ; data_jsnmsu111213_0m _vrf_PLAT710_jsnmsu111213_0m ; RESPONSE: These angles relate to the terminal nitrosyl ligand. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 B N7 Ni O2' _chemical_formula_weight 566.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 '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 13.9653(8) _cell_length_b 17.0466(10) _cell_length_c 23.6430(13) _cell_angle_alpha 85.049(3) _cell_angle_beta 76.475(3) _cell_angle_gamma 88.960(3) _cell_volume 5452.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 24.39 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7061 _exptl_absorpt_correction_T_max 0.9113 _exptl_absorpt_process_details 'multi-scan' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 86603 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.10 _reflns_number_total 24003 _reflns_number_gt 16267 _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. ; _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^)+(0.0503P)^2^+1.3919P] 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 24003 _refine_ls_number_parameters 1429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.42631(2) 0.350838(19) 0.057707(14) 0.02798(8) Uani 1 1 d . . . Ni2 Ni 0.47830(2) 0.860550(18) 0.447095(14) 0.02560(8) Uani 1 1 d . . . Ni3 Ni 1.00309(2) 0.869879(19) 0.591765(14) 0.02747(8) Uani 1 1 d . . . Ni4 Ni 0.07099(2) 0.378163(19) 0.906145(15) 0.03064(9) Uani 1 1 d . . . B1 B 0.4634(2) 0.17291(18) 0.05665(12) 0.0276(6) Uani 1 1 d . . . H1A H 0.4774(19) 0.1077(15) 0.0549(11) 0.033 Uiso 1 1 d . . . B2 B 0.5246(2) 0.68371(17) 0.44951(12) 0.0259(6) Uani 1 1 d . . . H2A H 0.5423(18) 0.6175(15) 0.4503(11) 0.031 Uiso 1 1 d . . . B3 B 0.9748(2) 0.69115(18) 0.61816(12) 0.0264(6) Uani 1 1 d . . . H3B H 0.9655(18) 0.6297(15) 0.6273(11) 0.032 Uiso 1 1 d . . . B4 B 0.0283(2) 0.20339(17) 0.90073(12) 0.0258(6) Uani 1 1 d . . . H4B H 0.0116(18) 0.1388(15) 0.9006(11) 0.031 Uiso 1 1 d . . . N1 N 0.42142(15) 0.20701(12) 0.00443(9) 0.0261(5) Uani 1 1 d . . . N2 N 0.37759(15) 0.30000(12) -0.05388(9) 0.0284(5) Uani 1 1 d . . . N3 N 0.38780(15) 0.19489(12) 0.11275(9) 0.0271(5) Uani 1 1 d . . . N4 N 0.29685(15) 0.27319(14) 0.17143(9) 0.0332(5) Uani 1 1 d . . . N5 N 0.55809(15) 0.22042(12) 0.05404(9) 0.0269(5) Uani 1 1 d . . . N6 N 0.64419(15) 0.32600(13) 0.05312(9) 0.0308(5) Uani 1 1 d . . . N7 N 0.41784(16) 0.44631(13) 0.06371(10) 0.0358(5) Uani 1 1 d . . . N8 N 0.44037(14) 0.70368(11) 0.50192(8) 0.0239(4) Uani 1 1 d . . . N9 N 0.34304(14) 0.78074(12) 0.55861(9) 0.0267(5) Uani 1 1 d . . . N10 N 0.49050(14) 0.71493(12) 0.39388(8) 0.0247(4) Uani 1 1 d . . . N11 N 0.43843(15) 0.80304(13) 0.33531(9) 0.0304(5) Uani 1 1 d . . . N12 N 0.61493(14) 0.73515(11) 0.45153(8) 0.0242(4) Uani 1 1 d . . . N13 N 0.69563(14) 0.84478(12) 0.44733(9) 0.0250(4) Uani 1 1 d . . . N14 N 0.46070(15) 0.95623(13) 0.44435(9) 0.0287(5) Uani 1 1 d . . . N15 N 1.05471(14) 0.71341(12) 0.56154(8) 0.0252(4) Uani 1 1 d . . . N16 N 1.14361(15) 0.79290(12) 0.49253(9) 0.0268(5) Uani 1 1 d . . . N17 N 1.00664(15) 0.73059(12) 0.66797(9) 0.0261(5) Uani 1 1 d . . . N18 N 1.05172(16) 0.82744(13) 0.71064(9) 0.0316(5) Uani 1 1 d . . . N19 N 0.87899(14) 0.73368(12) 0.61029(9) 0.0262(5) Uani 1 1 d . . . N20 N 0.78701(15) 0.83513(13) 0.59599(9) 0.0308(5) Uani 1 1 d . . . N21 N 1.02087(16) 0.96460(13) 0.57323(10) 0.0342(5) Uani 1 1 d . . . N22 N 0.07068(14) 0.21845(11) 0.95365(9) 0.0248(4) Uani 1 1 d . . . N23 N 0.12092(15) 0.28892(12) 1.01387(9) 0.0291(5) Uani 1 1 d . . . N24 N 0.10552(15) 0.23714(12) 0.84627(9) 0.0287(5) Uani 1 1 d . . . N25 N 0.20101(16) 0.32610(14) 0.79020(10) 0.0377(6) Uani 1 1 d . . . N26 N -0.06511(14) 0.25595(11) 0.90393(9) 0.0248(4) Uani 1 1 d . . . N27 N -0.14575(15) 0.36693(12) 0.90311(9) 0.0291(5) Uani 1 1 d . . . N28 N 0.09202(18) 0.46964(14) 0.91670(11) 0.0427(6) Uani 1 1 d . . . O1 O 0.42363(18) 0.51336(13) 0.07282(12) 0.0679(7) Uani 1 1 d . . . O2 O 0.45585(17) 1.02625(12) 0.44127(10) 0.0528(6) Uani 1 1 d . . . O3 O 1.0370(2) 1.03107(13) 0.55508(12) 0.0737(8) Uani 1 1 d . . . O4 O 0.1037(2) 0.53251(14) 0.93199(13) 0.0854(9) Uani 1 1 d . . . O5 O 0.32564(19) 0.90294(19) 0.72510(11) 0.0851(9) Uani 1 1 d . . . O6 O 0.17321(19) 0.8413(2) 0.30721(11) 0.0977(11) Uani 1 1 d . . . O7 O 0.5908(2) 0.44392(15) 0.19465(11) 0.0717(7) Uani 1 1 d . . . O8 O 0.1136(3) 0.5566(2) 0.24351(13) 0.1064(11) Uani 1 1 d . . . C1 C 0.40340(18) 0.28536(15) -0.00200(11) 0.0280(6) Uani 1 1 d . . . C2 C 0.40748(18) 0.17145(15) -0.04372(11) 0.0286(6) Uani 1 1 d . . . C3 C 0.4200(2) 0.09489(17) -0.05918(12) 0.0395(7) Uani 1 1 d . . . H3 H 0.4384 0.0540 -0.0339 0.047 Uiso 1 1 calc R . . C4 C 0.4046(3) 0.08050(19) -0.11328(14) 0.0500(8) Uani 1 1 d . . . H4 H 0.4139 0.0287 -0.1255 0.060 Uiso 1 1 calc R . . C5 C 0.3757(2) 0.14009(19) -0.15020(13) 0.0464(8) Uani 1 1 d . . . H5 H 0.3644 0.1277 -0.1865 0.056 Uiso 1 1 calc R . . C6 C 0.3633(2) 0.21619(18) -0.13507(12) 0.0387(7) Uani 1 1 d . . . H6 H 0.3444 0.2570 -0.1602 0.046 Uiso 1 1 calc R . . C7 C 0.37964(18) 0.23067(15) -0.08125(11) 0.0296(6) Uani 1 1 d . . . C8 C 0.36295(18) 0.27129(15) 0.11937(11) 0.0288(6) Uani 1 1 d . . . C9 C 0.33662(18) 0.14727(16) 0.16071(11) 0.0311(6) Uani 1 1 d . . . C10 C 0.3341(2) 0.06662(17) 0.17410(12) 0.0388(7) Uani 1 1 d . . . H10 H 0.3739 0.0322 0.1489 0.047 Uiso 1 1 calc R . . C11 C 0.2708(2) 0.0381(2) 0.22613(13) 0.0477(8) Uani 1 1 d . . . H11 H 0.2673 -0.0170 0.2368 0.057 Uiso 1 1 calc R . . C12 C 0.2123(2) 0.0890(2) 0.26307(13) 0.0518(9) Uani 1 1 d . . . H12 H 0.1693 0.0674 0.2980 0.062 Uiso 1 1 calc R . . C13 C 0.2152(2) 0.1692(2) 0.25034(12) 0.0453(8) Uani 1 1 d . . . H13 H 0.1760 0.2036 0.2759 0.054 Uiso 1 1 calc R . . C14 C 0.27833(19) 0.19743(18) 0.19811(11) 0.0348(6) Uani 1 1 d . . . C15 C 0.55333(18) 0.29999(15) 0.05338(10) 0.0267(5) Uani 1 1 d . . . C16 C 0.65309(18) 0.19547(16) 0.05491(10) 0.0287(6) Uani 1 1 d . . . C17 C 0.6960(2) 0.12185(18) 0.05571(11) 0.0379(7) Uani 1 1 d . . . H17 H 0.6599 0.0756 0.0543 0.045 Uiso 1 1 calc R . . C18 C 0.7943(2) 0.1183(2) 0.05861(13) 0.0506(9) Uani 1 1 d . . . H18 H 0.8254 0.0684 0.0601 0.061 Uiso 1 1 calc R . . C19 C 0.8483(2) 0.1858(2) 0.05940(13) 0.0522(9) Uani 1 1 d . . . H19 H 0.9151 0.1808 0.0619 0.063 Uiso 1 1 calc R . . C20 C 0.8074(2) 0.2600(2) 0.05665(12) 0.0428(7) Uani 1 1 d . . . H20 H 0.8445 0.3063 0.0561 0.051 Uiso 1 1 calc R . . C21 C 0.70802(19) 0.26294(17) 0.05475(11) 0.0331(6) Uani 1 1 d . . . C22 C 0.3572(2) 0.37734(16) -0.07939(12) 0.0386(7) Uani 1 1 d . . . H22A H 0.3607 0.4169 -0.0523 0.058 Uiso 1 1 calc R . . H22B H 0.2911 0.3775 -0.0870 0.058 Uiso 1 1 calc R . . H22C H 0.4060 0.3897 -0.1161 0.058 Uiso 1 1 calc R . . C23 C 0.2505(2) 0.34428(19) 0.19536(14) 0.0493(8) Uani 1 1 d . . . H23A H 0.2782 0.3905 0.1695 0.074 Uiso 1 1 calc R . . H23B H 0.2628 0.3482 0.2342 0.074 Uiso 1 1 calc R . . H23C H 0.1794 0.3419 0.1985 0.074 Uiso 1 1 calc R . . C24 C 0.6714(2) 0.40893(17) 0.05235(13) 0.0441(7) Uani 1 1 d . . . H24A H 0.6246 0.4426 0.0364 0.066 Uiso 1 1 calc R . . H24B H 0.7379 0.4179 0.0279 0.066 Uiso 1 1 calc R . . H24C H 0.6697 0.4216 0.0922 0.066 Uiso 1 1 calc R . . C25 C 0.41416(17) 0.78009(15) 0.50847(11) 0.0271(5) Uani 1 1 d . . . C26 C 0.38436(17) 0.65508(15) 0.54714(10) 0.0254(5) Uani 1 1 d . . . C27 C 0.38137(19) 0.57372(15) 0.55986(11) 0.0303(6) Uani 1 1 d . . . H27 H 0.4233 0.5398 0.5353 0.036 Uiso 1 1 calc R . . C28 C 0.3148(2) 0.54442(17) 0.60978(12) 0.0357(6) Uani 1 1 d . . . H28 H 0.3110 0.4891 0.6195 0.043 Uiso 1 1 calc R . . C29 C 0.2530(2) 0.59382(17) 0.64628(12) 0.0374(7) Uani 1 1 d . . . H29 H 0.2081 0.5714 0.6802 0.045 Uiso 1 1 calc R . . C30 C 0.25581(19) 0.67439(17) 0.63415(11) 0.0339(6) Uani 1 1 d . . . H30 H 0.2142 0.7081 0.6591 0.041 Uiso 1 1 calc R . . C31 C 0.32227(17) 0.70427(15) 0.58368(10) 0.0261(5) Uani 1 1 d . . . C32 C 0.46586(17) 0.79230(15) 0.38683(11) 0.0271(5) Uani 1 1 d . . . C33 C 0.47748(17) 0.67633(15) 0.34674(11) 0.0279(6) Uani 1 1 d . . . C34 C 0.49185(19) 0.59850(17) 0.33362(12) 0.0349(6) Uani 1 1 d . . . H34 H 0.5146 0.5600 0.3589 0.042 Uiso 1 1 calc R . . C35 C 0.4712(2) 0.5799(2) 0.28166(14) 0.0476(8) Uani 1 1 d . . . H35 H 0.4799 0.5272 0.2713 0.057 Uiso 1 1 calc R . . C36 C 0.4382(2) 0.6360(2) 0.24433(13) 0.0489(8) Uani 1 1 d . . . H36 H 0.4252 0.6206 0.2092 0.059 Uiso 1 1 calc R . . C37 C 0.4239(2) 0.7134(2) 0.25716(12) 0.0439(7) Uani 1 1 d . . . H37 H 0.4012 0.7518 0.2318 0.053 Uiso 1 1 calc R . . C38 C 0.44442(18) 0.73230(16) 0.30909(11) 0.0314(6) Uani 1 1 d . . . C39 C 0.60607(18) 0.81453(14) 0.44873(10) 0.0255(5) Uani 1 1 d . . . C40 C 0.71205(17) 0.71433(14) 0.45250(10) 0.0241(5) Uani 1 1 d . . . C41 C 0.75854(18) 0.64202(15) 0.45674(11) 0.0293(6) Uani 1 1 d . . . H41 H 0.7239 0.5939 0.4594 0.035 Uiso 1 1 calc R . . C42 C 0.85735(19) 0.64328(16) 0.45698(12) 0.0351(6) Uani 1 1 d . . . H42 H 0.8914 0.5948 0.4592 0.042 Uiso 1 1 calc R . . C43 C 0.90886(19) 0.71372(16) 0.45400(12) 0.0348(6) Uani 1 1 d . . . H43 H 0.9767 0.7120 0.4545 0.042 Uiso 1 1 calc R . . C44 C 0.86256(18) 0.78576(15) 0.45038(11) 0.0296(6) Uani 1 1 d . . . H44 H 0.8970 0.8338 0.4486 0.035 Uiso 1 1 calc R . . C45 C 0.76373(18) 0.78470(14) 0.44946(10) 0.0251(5) Uani 1 1 d . . . C46 C 0.2971(2) 0.85126(16) 0.58363(12) 0.0346(6) Uani 1 1 d . . . H46A H 0.3300 0.8981 0.5609 0.052 Uiso 1 1 calc R . . H46B H 0.3031 0.8510 0.6241 0.052 Uiso 1 1 calc R . . H46C H 0.2273 0.8521 0.5827 0.052 Uiso 1 1 calc R . . C47 C 0.4082(2) 0.87800(17) 0.31020(13) 0.0417(7) Uani 1 1 d . . . H47A H 0.4147 0.9198 0.3351 0.063 Uiso 1 1 calc R . . H47B H 0.3395 0.8744 0.3076 0.063 Uiso 1 1 calc R . . H47C H 0.4502 0.8902 0.2711 0.063 Uiso 1 1 calc R . . C48 C 0.7204(2) 0.92804(14) 0.43613(12) 0.0331(6) Uani 1 1 d . . . H48A H 0.7549 0.9392 0.3951 0.050 Uiso 1 1 calc R . . H48B H 0.7630 0.9417 0.4614 0.050 Uiso 1 1 calc R . . H48C H 0.6599 0.9593 0.4443 0.050 Uiso 1 1 calc R . . C49 C 1.07453(17) 0.79010(15) 0.54353(11) 0.0267(5) Uani 1 1 d . . . C50 C 1.11191(17) 0.66630(15) 0.52123(10) 0.0257(5) Uani 1 1 d . . . C51 C 1.11862(19) 0.58536(15) 0.51857(11) 0.0317(6) Uani 1 1 d . . . H51 H 1.0803 0.5503 0.5484 0.038 Uiso 1 1 calc R . . C52 C 1.1834(2) 0.55772(17) 0.47070(12) 0.0366(6) Uani 1 1 d . . . H52 H 1.1901 0.5026 0.4678 0.044 Uiso 1 1 calc R . . C53 C 1.2392(2) 0.60921(17) 0.42659(12) 0.0382(7) Uani 1 1 d . . . H53 H 1.2823 0.5882 0.3942 0.046 Uiso 1 1 calc R . . C54 C 1.23349(18) 0.68956(17) 0.42882(11) 0.0328(6) Uani 1 1 d . . . H54 H 1.2719 0.7245 0.3990 0.039 Uiso 1 1 calc R . . C55 C 1.16849(17) 0.71685(15) 0.47700(10) 0.0261(5) Uani 1 1 d . . . C56 C 1.02347(18) 0.80952(15) 0.66211(11) 0.0290(6) Uani 1 1 d . . . C57 C 1.02328(17) 0.69816(15) 0.72084(11) 0.0274(6) Uani 1 1 d . . . C58 C 1.01660(19) 0.62149(16) 0.74659(11) 0.0328(6) Uani 1 1 d . . . H58 H 0.9958 0.5793 0.7285 0.039 Uiso 1 1 calc R . . C59 C 1.0420(2) 0.60959(19) 0.80028(12) 0.0416(7) Uani 1 1 d . . . H59 H 1.0386 0.5579 0.8192 0.050 Uiso 1 1 calc R . . C60 C 1.0721(2) 0.6712(2) 0.82692(13) 0.0466(8) Uani 1 1 d . . . H60 H 1.0893 0.6604 0.8634 0.056 Uiso 1 1 calc R . . C61 C 1.0777(2) 0.74744(19) 0.80185(12) 0.0420(7) Uani 1 1 d . . . H61 H 1.0976 0.7896 0.8203 0.050 Uiso 1 1 calc R . . C62 C 1.05270(18) 0.75972(16) 0.74833(11) 0.0320(6) Uani 1 1 d . . . C63 C 0.87929(18) 0.81295(15) 0.59960(10) 0.0278(6) Uani 1 1 d . . . C64 C 0.78549(18) 0.70474(16) 0.61286(10) 0.0304(6) Uani 1 1 d . . . C65 C 0.7471(2) 0.62875(18) 0.62152(12) 0.0392(7) Uani 1 1 d . . . H65 H 0.7864 0.5842 0.6277 0.047 Uiso 1 1 calc R . . C66 C 0.6487(2) 0.6211(2) 0.62075(13) 0.0523(9) Uani 1 1 d . . . H66 H 0.6203 0.5699 0.6266 0.063 Uiso 1 1 calc R . . C67 C 0.5901(2) 0.6857(2) 0.61166(14) 0.0564(9) Uani 1 1 d . . . H67 H 0.5230 0.6776 0.6116 0.068 Uiso 1 1 calc R . . C68 C 0.6276(2) 0.7613(2) 0.60269(12) 0.0458(8) Uani 1 1 d . . . H68 H 0.5882 0.8056 0.5960 0.055 Uiso 1 1 calc R . . C69 C 0.72637(19) 0.76936(17) 0.60389(11) 0.0334(6) Uani 1 1 d . . . C70 C 1.1881(2) 0.86481(16) 0.45932(12) 0.0351(6) Uani 1 1 d . . . H70A H 1.1510 0.9106 0.4749 0.053 Uiso 1 1 calc R . . H70B H 1.1868 0.8632 0.4182 0.053 Uiso 1 1 calc R . . H70C H 1.2565 0.8688 0.4626 0.053 Uiso 1 1 calc R . . C71 C 1.0756(2) 0.90615(17) 0.72270(14) 0.0445(7) Uani 1 1 d . . . H71A H 1.0702 0.9438 0.6898 0.067 Uiso 1 1 calc R . . H71B H 1.1431 0.9068 0.7281 0.067 Uiso 1 1 calc R . . H71C H 1.0297 0.9209 0.7583 0.067 Uiso 1 1 calc R . . C72 C 0.7553(2) 0.91578(18) 0.58771(13) 0.0452(8) Uani 1 1 d . . . H72A H 0.7201 0.9334 0.6254 0.068 Uiso 1 1 calc R . . H72B H 0.7114 0.9190 0.5607 0.068 Uiso 1 1 calc R . . H72C H 0.8129 0.9495 0.5714 0.068 Uiso 1 1 calc R . . C73 C 0.09023(17) 0.29316(15) 0.96341(11) 0.0276(6) Uani 1 1 d . . . C74 C 0.09113(17) 0.16605(15) 0.99751(11) 0.0278(6) Uani 1 1 d . . . C75 C 0.0828(2) 0.08514(16) 1.00720(14) 0.0411(7) Uani 1 1 d . . . H75 H 0.0630 0.0542 0.9803 0.049 Uiso 1 1 calc R . . C76 C 0.1046(3) 0.05143(19) 1.05819(16) 0.0587(10) Uani 1 1 d . . . H76 H 0.0988 -0.0040 1.0666 0.070 Uiso 1 1 calc R . . C77 C 0.1348(3) 0.0962(2) 1.09732(17) 0.0641(10) Uani 1 1 d . . . H77 H 0.1487 0.0708 1.1319 0.077 Uiso 1 1 calc R . . C78 C 0.1448(2) 0.17675(19) 1.08695(14) 0.0475(8) Uani 1 1 d . . . H78 H 0.1662 0.2075 1.1134 0.057 Uiso 1 1 calc R . . C79 C 0.12251(18) 0.21099(16) 1.03644(11) 0.0311(6) Uani 1 1 d . . . C80 C 0.13145(18) 0.31400(16) 0.84184(11) 0.0327(6) Uani 1 1 d . . . C81 C 0.15978(18) 0.19952(17) 0.79936(11) 0.0322(6) Uani 1 1 d . . . C82 C 0.16353(19) 0.12133(18) 0.78650(12) 0.0387(7) Uani 1 1 d . . . H82 H 0.1218 0.0825 0.8109 0.046 Uiso 1 1 calc R . . C83 C 0.2309(2) 0.1025(2) 0.73645(13) 0.0484(8) Uani 1 1 d . . . H83 H 0.2361 0.0495 0.7266 0.058 Uiso 1 1 calc R . . C84 C 0.2912(2) 0.1598(2) 0.70026(13) 0.0549(9) Uani 1 1 d . . . H84 H 0.3364 0.1448 0.6663 0.066 Uiso 1 1 calc R . . C85 C 0.2870(2) 0.2376(2) 0.71240(12) 0.0513(9) Uani 1 1 d . . . H85 H 0.3278 0.2765 0.6874 0.062 Uiso 1 1 calc R . . C86 C 0.21986(19) 0.25668(19) 0.76320(11) 0.0379(7) Uani 1 1 d . . . C87 C -0.05677(19) 0.33499(15) 0.90484(10) 0.0276(6) Uani 1 1 d . . . C88 C -0.16035(17) 0.23717(15) 0.90153(10) 0.0254(5) Uani 1 1 d . . . C89 C -0.20709(19) 0.16617(16) 0.90048(11) 0.0321(6) Uani 1 1 d . . . H89 H -0.1733 0.1175 0.9020 0.038 Uiso 1 1 calc R . . C90 C -0.3049(2) 0.16919(17) 0.89720(12) 0.0388(7) Uani 1 1 d . . . H90 H -0.3384 0.1215 0.8964 0.047 Uiso 1 1 calc R . . C91 C -0.3551(2) 0.23974(17) 0.89510(12) 0.0388(7) Uani 1 1 d . . . H91 H -0.4219 0.2394 0.8924 0.047 Uiso 1 1 calc R . . C92 C -0.30994(19) 0.31070(17) 0.89687(11) 0.0343(6) Uani 1 1 d . . . H92 H -0.3444 0.3592 0.8958 0.041 Uiso 1 1 calc R . . C93 C -0.21218(18) 0.30794(15) 0.90027(10) 0.0277(6) Uani 1 1 d . . . C94 C 0.1455(2) 0.35668(16) 1.04188(12) 0.0367(6) Uani 1 1 d . . . H94A H 0.1417 0.4050 1.0168 0.055 Uiso 1 1 calc R . . H94B H 0.2124 0.3506 1.0479 0.055 Uiso 1 1 calc R . . H94C H 0.0988 0.3598 1.0796 0.055 Uiso 1 1 calc R . . C95 C 0.2497(2) 0.4014(2) 0.76852(14) 0.0550(9) Uani 1 1 d . . . H95A H 0.3209 0.3953 0.7640 0.083 Uiso 1 1 calc R . . H95B H 0.2249 0.4406 0.7963 0.083 Uiso 1 1 calc R . . H95C H 0.2359 0.4188 0.7306 0.083 Uiso 1 1 calc R . . C96 C -0.1660(2) 0.45112(15) 0.89958(13) 0.0408(7) Uani 1 1 d . . . H96A H -0.1145 0.4792 0.9117 0.061 Uiso 1 1 calc R . . H96B H -0.2301 0.4612 0.9253 0.061 Uiso 1 1 calc R . . H96C H -0.1668 0.4696 0.8593 0.061 Uiso 1 1 calc R . . C97 C 0.4198(3) 0.9272(4) 0.6923(2) 0.1083(18) Uani 1 1 d . . . H97A H 0.4221 0.9852 0.6847 0.130 Uiso 1 1 calc R . . H97B H 0.4351 0.9036 0.6544 0.130 Uiso 1 1 calc R . . C98 C 0.4914(3) 0.9006(3) 0.72687(17) 0.0709(11) Uani 1 1 d . . . H98A H 0.5488 0.9365 0.7188 0.085 Uiso 1 1 calc R . . H98B H 0.5145 0.8465 0.7190 0.085 Uiso 1 1 calc R . . C99 C 0.4326(3) 0.9033(3) 0.78744(19) 0.1014(17) Uani 1 1 d . . . H99A H 0.4454 0.9530 0.8033 0.122 Uiso 1 1 calc R . . H99B H 0.4498 0.8586 0.8128 0.122 Uiso 1 1 calc R . . C100 C 0.3273(3) 0.8985(3) 0.78509(16) 0.0769(12) Uani 1 1 d . . . H10A H 0.2979 0.8482 0.8053 0.092 Uiso 1 1 calc R . . H10B H 0.2895 0.9425 0.8042 0.092 Uiso 1 1 calc R . . C101 C 0.1692(3) 0.8151(3) 0.2548(2) 0.0917(15) Uani 1 1 d . . . H10C H 0.1703 0.7568 0.2569 0.110 Uiso 1 1 calc R . . H10D H 0.2256 0.8356 0.2236 0.110 Uiso 1 1 calc R . . C102 C 0.0732(3) 0.8462(4) 0.2430(2) 0.131(2) Uani 1 1 d . . . H10E H 0.0836 0.8965 0.2182 0.157 Uiso 1 1 calc R . . H10F H 0.0427 0.8078 0.2234 0.157 Uiso 1 1 calc R . . C103 C 0.0128(3) 0.8575(4) 0.29944(19) 0.115(2) Uani 1 1 d . . . H10G H -0.0225 0.9084 0.2990 0.138 Uiso 1 1 calc R . . H10H H -0.0361 0.8145 0.3125 0.138 Uiso 1 1 calc R . . C104 C 0.0793(3) 0.8570(5) 0.3365(2) 0.178(4) Uani 1 1 d . . . H10I H 0.0778 0.9089 0.3526 0.213 Uiso 1 1 calc R . . H10J H 0.0582 0.8167 0.3697 0.213 Uiso 1 1 calc R . . C105 C 0.6482(4) 0.3983(3) 0.2262(3) 0.1118(19) Uani 1 1 d . . . H10K H 0.6424 0.4191 0.2647 0.134 Uiso 1 1 calc R . . H10L H 0.7182 0.4018 0.2049 0.134 Uiso 1 1 calc R . . C106 C 0.6177(4) 0.3189(3) 0.2344(3) 0.124(2) Uani 1 1 d . . . H10M H 0.6116 0.2982 0.2755 0.149 Uiso 1 1 calc R . . H10N H 0.6660 0.2864 0.2090 0.149 Uiso 1 1 calc R . . C107 C 0.5194(4) 0.3171(3) 0.2189(2) 0.0996(16) Uani 1 1 d . . . H10O H 0.5213 0.2825 0.1871 0.119 Uiso 1 1 calc R . . H10P H 0.4671 0.2983 0.2531 0.119 Uiso 1 1 calc R . . C108 C 0.5023(3) 0.4006(2) 0.19944(19) 0.0744(12) Uani 1 1 d . . . H10Q H 0.4844 0.4035 0.1612 0.089 Uiso 1 1 calc R . . H10R H 0.4476 0.4230 0.2281 0.089 Uiso 1 1 calc R . . C109 C 0.1484(3) 0.5677(3) 0.29278(19) 0.0840(13) Uani 1 1 d . . . H10S H 0.1943 0.6130 0.2849 0.101 Uiso 1 1 calc R . . H10T H 0.1839 0.5202 0.3039 0.101 Uiso 1 1 calc R . . C110 C 0.0620(3) 0.5828(3) 0.34022(18) 0.0926(15) Uani 1 1 d . . . H11A H 0.0728 0.6303 0.3593 0.111 Uiso 1 1 calc R . . H11B H 0.0494 0.5374 0.3700 0.111 Uiso 1 1 calc R . . C111 C 0.0265(4) 0.6002(3) 0.24740(18) 0.0850(13) Uani 1 1 d . . . H11C H -0.0159 0.5776 0.2247 0.102 Uiso 1 1 calc R . . H11D H 0.0415 0.6556 0.2323 0.102 Uiso 1 1 calc R . . C112 C -0.0238(3) 0.5949(3) 0.31139(18) 0.0833(13) Uani 1 1 d . . . H11E H -0.0702 0.5500 0.3220 0.100 Uiso 1 1 calc R . . H11F H -0.0597 0.6441 0.3222 0.100 Uiso 1 1 calc R . . 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 0.02543(18) 0.02725(18) 0.03246(18) -0.00482(14) -0.00848(14) 0.00192(14) Ni2 0.02199(17) 0.02405(17) 0.03037(18) -0.00227(14) -0.00543(13) 0.00100(13) Ni3 0.02455(17) 0.02520(18) 0.03177(18) -0.00060(14) -0.00540(14) -0.00044(13) Ni4 0.02756(18) 0.02606(18) 0.0386(2) 0.00631(15) -0.01110(15) -0.00563(14) B1 0.0283(16) 0.0288(16) 0.0257(15) -0.0022(12) -0.0061(12) -0.0011(12) B2 0.0213(14) 0.0272(16) 0.0285(15) -0.0037(12) -0.0036(12) -0.0023(12) B3 0.0245(15) 0.0262(16) 0.0269(15) 0.0005(12) -0.0040(12) -0.0021(12) B4 0.0198(14) 0.0293(16) 0.0261(14) 0.0027(12) -0.0028(11) -0.0034(12) N1 0.0260(11) 0.0270(11) 0.0259(11) -0.0035(9) -0.0067(9) -0.0029(9) N2 0.0228(11) 0.0331(12) 0.0309(12) -0.0006(10) -0.0103(9) 0.0014(9) N3 0.0226(11) 0.0318(12) 0.0261(11) -0.0003(9) -0.0048(9) -0.0030(9) N4 0.0237(11) 0.0463(14) 0.0292(12) -0.0073(11) -0.0044(9) 0.0036(10) N5 0.0228(11) 0.0320(12) 0.0253(11) -0.0037(9) -0.0043(9) 0.0017(9) N6 0.0254(12) 0.0390(13) 0.0285(11) -0.0038(10) -0.0064(9) -0.0058(10) N7 0.0300(13) 0.0317(13) 0.0460(14) -0.0044(11) -0.0100(11) 0.0083(10) N8 0.0178(10) 0.0251(11) 0.0277(11) -0.0016(9) -0.0034(8) -0.0022(8) N9 0.0216(11) 0.0308(12) 0.0272(11) -0.0048(9) -0.0037(9) 0.0017(9) N10 0.0209(10) 0.0277(11) 0.0254(11) -0.0044(9) -0.0041(8) -0.0014(9) N11 0.0252(11) 0.0370(13) 0.0288(11) 0.0005(10) -0.0066(9) -0.0035(9) N12 0.0195(10) 0.0254(11) 0.0269(11) -0.0008(9) -0.0043(8) -0.0006(8) N13 0.0224(11) 0.0252(11) 0.0273(11) -0.0029(9) -0.0050(9) -0.0028(8) N14 0.0243(11) 0.0314(13) 0.0306(12) -0.0025(10) -0.0073(9) 0.0048(9) N15 0.0224(11) 0.0265(11) 0.0258(11) -0.0013(9) -0.0042(9) -0.0002(9) N16 0.0213(11) 0.0308(12) 0.0267(11) 0.0012(9) -0.0033(9) -0.0041(9) N17 0.0229(11) 0.0295(12) 0.0247(11) -0.0002(9) -0.0037(9) -0.0007(9) N18 0.0288(12) 0.0345(13) 0.0319(12) -0.0051(10) -0.0072(10) -0.0012(10) N19 0.0228(11) 0.0292(12) 0.0256(11) -0.0017(9) -0.0036(9) -0.0042(9) N20 0.0250(12) 0.0414(13) 0.0263(11) -0.0014(10) -0.0073(9) 0.0054(10) N21 0.0300(12) 0.0299(13) 0.0441(14) -0.0016(11) -0.0117(10) -0.0019(10) N22 0.0204(10) 0.0242(11) 0.0278(11) 0.0042(9) -0.0040(8) -0.0013(8) N23 0.0252(11) 0.0312(12) 0.0319(12) -0.0002(10) -0.0098(9) -0.0029(9) N24 0.0218(11) 0.0361(13) 0.0262(11) 0.0016(10) -0.0027(9) -0.0029(9) N25 0.0260(12) 0.0500(15) 0.0342(13) 0.0136(11) -0.0066(10) -0.0104(11) N26 0.0199(10) 0.0255(11) 0.0280(11) 0.0012(9) -0.0046(8) -0.0028(8) N27 0.0252(11) 0.0299(12) 0.0312(12) -0.0003(9) -0.0056(9) 0.0012(9) N28 0.0438(15) 0.0294(13) 0.0616(17) 0.0094(12) -0.0300(13) -0.0092(11) O1 0.0635(16) 0.0293(12) 0.114(2) -0.0199(13) -0.0227(15) 0.0104(11) O2 0.0683(16) 0.0278(12) 0.0652(15) -0.0049(10) -0.0222(12) 0.0135(10) O3 0.086(2) 0.0292(13) 0.111(2) 0.0105(13) -0.0382(17) -0.0175(12) O4 0.121(2) 0.0334(14) 0.125(2) -0.0008(15) -0.075(2) -0.0199(14) O5 0.0512(16) 0.152(3) 0.0548(16) -0.0181(17) -0.0123(13) -0.0224(17) O6 0.0429(16) 0.199(4) 0.0534(16) -0.0077(19) -0.0164(13) -0.0065(18) O7 0.086(2) 0.0681(17) 0.0669(17) -0.0230(14) -0.0233(15) -0.0010(15) O8 0.094(2) 0.158(3) 0.0642(19) -0.010(2) -0.0148(18) 0.014(2) C1 0.0218(13) 0.0314(14) 0.0303(14) -0.0014(11) -0.0051(11) -0.0012(11) C2 0.0223(13) 0.0349(15) 0.0288(13) -0.0037(11) -0.0055(11) -0.0066(11) C3 0.0484(18) 0.0365(16) 0.0350(15) -0.0043(13) -0.0118(13) -0.0061(13) C4 0.067(2) 0.0428(19) 0.0462(18) -0.0159(15) -0.0198(16) -0.0046(16) C5 0.054(2) 0.056(2) 0.0354(16) -0.0123(15) -0.0193(14) -0.0037(16) C6 0.0341(16) 0.0517(19) 0.0323(15) -0.0004(13) -0.0130(12) -0.0035(13) C7 0.0226(13) 0.0362(15) 0.0305(14) -0.0026(12) -0.0069(11) -0.0034(11) C8 0.0211(13) 0.0374(15) 0.0281(13) -0.0057(12) -0.0053(10) 0.0015(11) C9 0.0221(13) 0.0459(17) 0.0266(13) 0.0017(12) -0.0095(11) -0.0040(12) C10 0.0314(15) 0.0473(18) 0.0385(16) 0.0079(14) -0.0135(12) -0.0064(13) C11 0.0459(19) 0.055(2) 0.0431(18) 0.0195(15) -0.0188(15) -0.0133(15) C12 0.0340(17) 0.083(3) 0.0346(17) 0.0143(17) -0.0060(14) -0.0113(17) C13 0.0279(15) 0.078(2) 0.0276(15) 0.0009(15) -0.0035(12) -0.0010(15) C14 0.0230(14) 0.0562(19) 0.0265(14) -0.0028(13) -0.0084(11) -0.0001(12) C15 0.0252(13) 0.0309(14) 0.0249(13) -0.0042(11) -0.0067(10) -0.0030(11) C16 0.0251(13) 0.0408(16) 0.0197(12) -0.0032(11) -0.0044(10) 0.0047(11) C17 0.0361(16) 0.0468(18) 0.0298(14) -0.0034(13) -0.0064(12) 0.0101(13) C18 0.0420(19) 0.072(2) 0.0361(17) -0.0084(16) -0.0057(14) 0.0290(17) C19 0.0220(15) 0.097(3) 0.0374(17) -0.0092(18) -0.0064(13) 0.0147(17) C20 0.0253(15) 0.075(2) 0.0284(15) -0.0070(15) -0.0046(12) -0.0030(15) C21 0.0237(13) 0.0550(18) 0.0199(13) -0.0048(12) -0.0032(10) 0.0002(12) C22 0.0364(16) 0.0391(17) 0.0408(16) 0.0017(13) -0.0121(13) 0.0040(13) C23 0.0368(17) 0.062(2) 0.0481(18) -0.0191(16) -0.0029(14) 0.0108(15) C24 0.0420(18) 0.0436(18) 0.0471(18) -0.0037(14) -0.0101(14) -0.0155(14) C25 0.0195(12) 0.0312(14) 0.0311(14) -0.0041(11) -0.0066(10) 0.0015(10) C26 0.0175(12) 0.0343(14) 0.0252(13) -0.0009(11) -0.0072(10) -0.0029(10) C27 0.0256(14) 0.0339(15) 0.0311(14) -0.0005(12) -0.0068(11) -0.0007(11) C28 0.0322(15) 0.0355(16) 0.0374(15) 0.0088(13) -0.0080(12) -0.0057(12) C29 0.0280(15) 0.0481(18) 0.0318(15) 0.0081(13) -0.0021(12) -0.0057(13) C30 0.0222(13) 0.0507(18) 0.0277(14) -0.0026(13) -0.0039(11) 0.0018(12) C31 0.0176(12) 0.0350(15) 0.0268(13) -0.0014(11) -0.0078(10) -0.0009(10) C32 0.0172(12) 0.0342(15) 0.0286(13) -0.0009(11) -0.0030(10) -0.0011(10) C33 0.0162(12) 0.0389(15) 0.0273(13) -0.0076(12) -0.0002(10) -0.0053(11) C34 0.0238(14) 0.0418(16) 0.0383(15) -0.0112(13) -0.0024(12) -0.0016(12) C35 0.0367(17) 0.058(2) 0.0491(19) -0.0270(17) -0.0032(14) -0.0037(15) C36 0.0439(18) 0.071(2) 0.0355(17) -0.0229(17) -0.0093(14) -0.0063(16) C37 0.0344(16) 0.068(2) 0.0301(15) -0.0077(15) -0.0068(12) -0.0051(15) C38 0.0229(13) 0.0409(16) 0.0288(14) -0.0027(12) -0.0022(11) -0.0060(11) C39 0.0236(13) 0.0277(14) 0.0253(13) -0.0051(10) -0.0050(10) -0.0011(10) C40 0.0229(13) 0.0287(13) 0.0199(12) -0.0026(10) -0.0032(10) 0.0001(10) C41 0.0253(13) 0.0286(14) 0.0322(14) 0.0006(11) -0.0042(11) -0.0006(11) C42 0.0280(14) 0.0337(15) 0.0417(16) 0.0000(13) -0.0059(12) 0.0050(12) C43 0.0216(13) 0.0457(17) 0.0384(15) -0.0014(13) -0.0103(11) 0.0008(12) C44 0.0231(13) 0.0332(15) 0.0329(14) -0.0030(12) -0.0073(11) -0.0047(11) C45 0.0242(13) 0.0281(14) 0.0218(12) -0.0019(10) -0.0031(10) -0.0018(10) C46 0.0304(15) 0.0363(16) 0.0359(15) -0.0109(12) -0.0032(12) 0.0057(12) C47 0.0415(17) 0.0459(18) 0.0393(16) 0.0076(14) -0.0164(13) -0.0012(14) C48 0.0319(15) 0.0254(14) 0.0414(16) -0.0041(12) -0.0064(12) -0.0058(11) C49 0.0189(12) 0.0306(14) 0.0304(13) 0.0005(11) -0.0065(10) -0.0011(10) C50 0.0203(12) 0.0344(15) 0.0226(12) -0.0017(11) -0.0056(10) 0.0013(10) C51 0.0326(15) 0.0318(15) 0.0290(14) 0.0000(11) -0.0051(11) 0.0014(11) C52 0.0370(16) 0.0352(16) 0.0376(16) -0.0098(13) -0.0066(13) 0.0044(12) C53 0.0308(15) 0.0490(18) 0.0336(15) -0.0140(14) -0.0020(12) 0.0044(13) C54 0.0212(13) 0.0471(17) 0.0281(14) -0.0034(12) -0.0017(11) -0.0024(12) C55 0.0198(12) 0.0341(15) 0.0250(13) -0.0011(11) -0.0069(10) 0.0006(10) C56 0.0215(13) 0.0338(15) 0.0306(14) -0.0049(11) -0.0032(11) 0.0006(11) C57 0.0160(12) 0.0383(15) 0.0264(13) -0.0021(11) -0.0021(10) 0.0014(10) C58 0.0267(14) 0.0397(16) 0.0292(14) 0.0003(12) -0.0020(11) 0.0005(12) C59 0.0361(16) 0.0524(19) 0.0319(15) 0.0095(14) -0.0040(13) 0.0015(14) C60 0.0428(18) 0.070(2) 0.0291(15) 0.0047(15) -0.0149(13) -0.0014(16) C61 0.0381(17) 0.057(2) 0.0331(15) -0.0059(14) -0.0123(13) -0.0034(14) C62 0.0216(13) 0.0427(16) 0.0308(14) -0.0044(12) -0.0037(11) 0.0011(11) C63 0.0265(13) 0.0361(15) 0.0201(12) -0.0020(11) -0.0042(10) 0.0031(11) C64 0.0237(13) 0.0460(17) 0.0206(12) -0.0058(12) -0.0017(10) -0.0075(12) C65 0.0362(16) 0.0483(18) 0.0310(15) -0.0055(13) -0.0023(12) -0.0102(13) C66 0.0446(19) 0.072(2) 0.0398(17) -0.0097(17) -0.0054(15) -0.0284(18) C67 0.0297(17) 0.099(3) 0.0429(18) -0.0099(19) -0.0102(14) -0.0140(18) C68 0.0291(16) 0.077(2) 0.0329(16) -0.0074(15) -0.0100(12) 0.0003(15) C69 0.0235(13) 0.0534(18) 0.0235(13) -0.0050(12) -0.0050(11) -0.0017(12) C70 0.0307(15) 0.0354(16) 0.0351(15) 0.0053(12) -0.0022(12) -0.0047(12) C71 0.0454(18) 0.0420(18) 0.0507(18) -0.0126(15) -0.0168(15) -0.0053(14) C72 0.0420(18) 0.0511(19) 0.0428(17) 0.0040(15) -0.0145(14) 0.0149(14) C73 0.0193(12) 0.0297(14) 0.0324(14) 0.0013(11) -0.0046(10) -0.0021(10) C74 0.0159(12) 0.0320(14) 0.0336(14) 0.0053(11) -0.0048(10) 0.0020(10) C75 0.0347(16) 0.0314(16) 0.060(2) 0.0029(14) -0.0200(14) 0.0008(12) C76 0.057(2) 0.0392(18) 0.088(3) 0.0234(18) -0.043(2) -0.0032(16) C77 0.065(2) 0.060(2) 0.076(3) 0.0333(19) -0.047(2) -0.0117(18) C78 0.0424(18) 0.056(2) 0.0494(18) 0.0088(16) -0.0258(15) -0.0075(15) C79 0.0201(13) 0.0387(16) 0.0339(14) 0.0058(12) -0.0084(11) -0.0021(11) C80 0.0218(13) 0.0409(16) 0.0341(14) 0.0115(12) -0.0086(11) -0.0059(11) C81 0.0185(13) 0.0567(18) 0.0219(13) -0.0024(12) -0.0059(10) -0.0034(12) C82 0.0254(14) 0.061(2) 0.0311(15) -0.0119(14) -0.0059(12) -0.0017(13) C83 0.0326(16) 0.077(2) 0.0401(17) -0.0252(17) -0.0108(14) -0.0018(16) C84 0.0306(17) 0.105(3) 0.0290(16) -0.0195(18) -0.0019(13) -0.0049(18) C85 0.0293(16) 0.094(3) 0.0273(15) 0.0033(17) -0.0030(12) -0.0135(17) C86 0.0253(14) 0.062(2) 0.0257(14) 0.0041(14) -0.0075(11) -0.0051(13) C87 0.0305(14) 0.0274(14) 0.0235(13) 0.0018(11) -0.0046(11) -0.0016(11) C88 0.0192(12) 0.0330(14) 0.0211(12) 0.0024(10) -0.0002(10) -0.0009(10) C89 0.0284(14) 0.0316(15) 0.0343(15) 0.0026(12) -0.0053(11) -0.0022(11) C90 0.0282(15) 0.0413(17) 0.0462(17) -0.0015(14) -0.0073(13) -0.0101(12) C91 0.0206(14) 0.0522(19) 0.0419(16) -0.0002(14) -0.0052(12) -0.0030(13) C92 0.0235(14) 0.0433(17) 0.0341(15) -0.0003(13) -0.0043(11) 0.0055(12) C93 0.0237(13) 0.0334(15) 0.0232(13) 0.0007(11) -0.0010(10) 0.0007(11) C94 0.0319(15) 0.0412(17) 0.0397(16) -0.0089(13) -0.0115(12) -0.0051(12) C95 0.0421(19) 0.065(2) 0.0512(19) 0.0248(17) -0.0057(15) -0.0205(16) C96 0.0415(17) 0.0293(15) 0.0499(18) -0.0020(13) -0.0082(14) 0.0074(13) C97 0.054(3) 0.198(6) 0.070(3) -0.001(3) -0.010(2) -0.032(3) C98 0.055(2) 0.087(3) 0.069(3) -0.020(2) -0.005(2) -0.014(2) C99 0.065(3) 0.177(5) 0.075(3) -0.064(3) -0.024(2) 0.012(3) C100 0.064(3) 0.109(3) 0.054(2) -0.008(2) -0.0054(19) 0.004(2) C101 0.053(3) 0.120(4) 0.112(4) -0.058(3) -0.025(2) 0.017(2) C102 0.061(3) 0.259(7) 0.092(4) -0.081(4) -0.038(3) 0.052(4) C103 0.068(3) 0.221(6) 0.068(3) -0.048(4) -0.032(2) 0.045(4) C104 0.047(3) 0.424(12) 0.068(3) -0.060(5) -0.014(2) 0.027(5) C105 0.111(4) 0.099(4) 0.151(5) 0.001(4) -0.087(4) -0.004(3) C106 0.113(4) 0.085(4) 0.204(7) -0.010(4) -0.096(5) -0.002(3) C107 0.110(4) 0.110(4) 0.088(3) 0.014(3) -0.048(3) -0.026(3) C108 0.072(3) 0.080(3) 0.088(3) -0.047(3) -0.038(2) 0.011(2) C109 0.072(3) 0.104(4) 0.082(3) -0.005(3) -0.033(3) 0.007(3) C110 0.076(3) 0.144(4) 0.062(3) -0.012(3) -0.022(2) 0.005(3) C111 0.098(4) 0.098(3) 0.068(3) -0.011(2) -0.038(3) 0.018(3) C112 0.070(3) 0.111(4) 0.075(3) -0.027(3) -0.022(2) 0.008(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 Ni1 N7 1.646(2) . ? Ni1 C15 1.945(3) . ? Ni1 C1 1.959(3) . ? Ni1 C8 1.961(3) . ? Ni2 N14 1.643(2) . ? Ni2 C39 1.944(2) . ? Ni2 C32 1.955(3) . ? Ni2 C25 1.970(3) . ? Ni3 N21 1.644(2) . ? Ni3 C56 1.955(3) . ? Ni3 C49 1.958(2) . ? Ni3 C63 1.961(3) . ? Ni4 N28 1.643(2) . ? Ni4 C87 1.950(3) . ? Ni4 C73 1.955(3) . ? Ni4 C80 1.968(3) . ? B1 N5 1.549(4) . ? B1 N1 1.552(4) . ? B1 N3 1.559(3) . ? B2 N10 1.550(3) . ? B2 N8 1.553(3) . ? B2 N12 1.562(3) . ? B3 N15 1.552(3) . ? B3 N19 1.553(3) . ? B3 N17 1.558(3) . ? B4 N22 1.545(3) . ? B4 N24 1.548(3) . ? B4 N26 1.560(3) . ? N1 C1 1.357(3) . ? N1 C2 1.389(3) . ? N2 C1 1.359(3) . ? N2 C7 1.392(3) . ? N2 C22 1.453(3) . ? N3 C8 1.354(3) . ? N3 C9 1.392(3) . ? N4 C8 1.357(3) . ? N4 C14 1.388(4) . ? N4 C23 1.458(3) . ? N5 C15 1.356(3) . ? N5 C16 1.390(3) . ? N6 C15 1.350(3) . ? N6 C21 1.388(3) . ? N6 C24 1.468(3) . ? N7 O1 1.189(3) . ? N8 C25 1.359(3) . ? N8 C26 1.386(3) . ? N9 C25 1.358(3) . ? N9 C31 1.391(3) . ? N9 C46 1.457(3) . ? N10 C32 1.363(3) . ? N10 C33 1.391(3) . ? N11 C32 1.357(3) . ? N11 C38 1.395(3) . ? N11 C47 1.459(3) . ? N12 C39 1.354(3) . ? N12 C40 1.401(3) . ? N13 C39 1.354(3) . ? N13 C45 1.391(3) . ? N13 C48 1.454(3) . ? N14 O2 1.191(3) . ? N15 C49 1.352(3) . ? N15 C50 1.394(3) . ? N16 C49 1.354(3) . ? N16 C55 1.394(3) . ? N16 C70 1.463(3) . ? N17 C56 1.360(3) . ? N17 C57 1.391(3) . ? N18 C56 1.357(3) . ? N18 C62 1.398(3) . ? N18 C71 1.456(3) . ? N19 C63 1.353(3) . ? N19 C64 1.390(3) . ? N20 C63 1.356(3) . ? N20 C69 1.390(3) . ? N20 C72 1.448(3) . ? N21 O3 1.183(3) . ? N22 C73 1.357(3) . ? N22 C74 1.387(3) . ? N23 C73 1.355(3) . ? N23 C79 1.390(3) . ? N23 C94 1.464(3) . ? N24 C80 1.354(3) . ? N24 C81 1.388(3) . ? N25 C80 1.373(3) . ? N25 C86 1.385(4) . ? N25 C95 1.459(4) . ? N26 C87 1.357(3) . ? N26 C88 1.389(3) . ? N27 C87 1.356(3) . ? N27 C93 1.397(3) . ? N27 C96 1.457(3) . ? N28 O4 1.186(3) . ? O5 C97 1.410(5) . ? O5 C100 1.419(4) . ? O6 C104 1.367(5) . ? O6 C101 1.367(5) . ? O7 C105 1.401(5) . ? O7 C108 1.429(4) . ? O8 C109 1.391(5) . ? O8 C111 1.402(5) . ? C2 C3 1.383(4) . ? C2 C7 1.397(4) . ? C3 C4 1.388(4) . ? C4 C5 1.398(4) . ? C5 C6 1.372(4) . ? C6 C7 1.387(4) . ? C9 C10 1.383(4) . ? C9 C14 1.394(4) . ? C10 C11 1.391(4) . ? C11 C12 1.398(5) . ? C12 C13 1.374(5) . ? C13 C14 1.392(4) . ? C16 C17 1.381(4) . ? C16 C21 1.393(4) . ? C17 C18 1.391(4) . ? C18 C19 1.392(5) . ? C19 C20 1.382(4) . ? C20 C21 1.398(4) . ? C26 C27 1.393(3) . ? C26 C31 1.396(3) . ? C27 C28 1.381(4) . ? C28 C29 1.396(4) . ? C29 C30 1.378(4) . ? C30 C31 1.392(3) . ? C33 C34 1.389(4) . ? C33 C38 1.395(4) . ? C34 C35 1.389(4) . ? C35 C36 1.391(5) . ? C36 C37 1.381(4) . ? C37 C38 1.389(4) . ? C40 C41 1.390(3) . ? C40 C45 1.399(3) . ? C41 C42 1.382(4) . ? C42 C43 1.399(4) . ? C43 C44 1.383(4) . ? C44 C45 1.386(3) . ? C50 C51 1.387(3) . ? C50 C55 1.394(3) . ? C51 C52 1.386(4) . ? C52 C53 1.397(4) . ? C53 C54 1.375(4) . ? C54 C55 1.389(3) . ? C57 C58 1.388(4) . ? C57 C62 1.397(4) . ? C58 C59 1.393(4) . ? C59 C60 1.389(4) . ? C60 C61 1.377(4) . ? C61 C62 1.387(4) . ? C64 C65 1.391(4) . ? C64 C69 1.396(4) . ? C65 C66 1.387(4) . ? C66 C67 1.392(5) . ? C67 C68 1.380(5) . ? C68 C69 1.396(4) . ? C74 C75 1.381(4) . ? C74 C79 1.396(4) . ? C75 C76 1.387(4) . ? C76 C77 1.390(5) . ? C77 C78 1.378(4) . ? C78 C79 1.383(4) . ? C81 C82 1.390(4) . ? C81 C86 1.391(4) . ? C82 C83 1.386(4) . ? C83 C84 1.394(5) . ? C84 C85 1.378(5) . ? C85 C86 1.399(4) . ? C88 C89 1.390(4) . ? C88 C93 1.397(3) . ? C89 C90 1.386(4) . ? C90 C91 1.384(4) . ? C91 C92 1.383(4) . ? C92 C93 1.386(3) . ? C97 C98 1.475(6) . ? C98 C99 1.479(5) . ? C99 C100 1.489(5) . ? C101 C102 1.509(6) . ? C102 C103 1.429(6) . ? C103 C104 1.417(6) . ? C105 C106 1.410(6) . ? C106 C107 1.503(6) . ? C107 C108 1.489(6) . ? C109 C110 1.479(6) . ? C110 C112 1.513(6) . ? C111 C112 1.507(6) . ? 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 N7 Ni1 C15 118.85(11) . . ? N7 Ni1 C1 132.30(11) . . ? C15 Ni1 C1 89.23(10) . . ? N7 Ni1 C8 123.90(11) . . ? C15 Ni1 C8 90.66(10) . . ? C1 Ni1 C8 90.42(10) . . ? N14 Ni2 C39 121.83(10) . . ? N14 Ni2 C32 125.64(11) . . ? C39 Ni2 C32 89.87(10) . . ? N14 Ni2 C25 127.91(10) . . ? C39 Ni2 C25 90.05(10) . . ? C32 Ni2 C25 90.45(10) . . ? N21 Ni3 C56 127.98(11) . . ? N21 Ni3 C49 121.92(11) . . ? C56 Ni3 C49 90.32(10) . . ? N21 Ni3 C63 125.72(11) . . ? C56 Ni3 C63 89.61(10) . . ? C49 Ni3 C63 90.20(10) . . ? N28 Ni4 C87 125.49(11) . . ? N28 Ni4 C73 119.54(11) . . ? C87 Ni4 C73 90.91(10) . . ? N28 Ni4 C80 130.56(12) . . ? C87 Ni4 C80 88.55(10) . . ? C73 Ni4 C80 90.60(11) . . ? N5 B1 N1 106.6(2) . . ? N5 B1 N3 106.0(2) . . ? N1 B1 N3 106.0(2) . . ? N10 B2 N8 106.0(2) . . ? N10 B2 N12 106.4(2) . . ? N8 B2 N12 106.51(19) . . ? N15 B3 N19 106.5(2) . . ? N15 B3 N17 106.3(2) . . ? N19 B3 N17 105.9(2) . . ? N22 B4 N24 105.6(2) . . ? N22 B4 N26 107.3(2) . . ? N24 B4 N26 106.1(2) . . ? C1 N1 C2 109.8(2) . . ? C1 N1 B1 119.5(2) . . ? C2 N1 B1 130.2(2) . . ? C1 N2 C7 110.2(2) . . ? C1 N2 C22 125.3(2) . . ? C7 N2 C22 124.4(2) . . ? C8 N3 C9 110.0(2) . . ? C8 N3 B1 119.6(2) . . ? C9 N3 B1 130.4(2) . . ? C8 N4 C14 110.1(2) . . ? C8 N4 C23 125.0(2) . . ? C14 N4 C23 124.9(2) . . ? C15 N5 C16 109.7(2) . . ? C15 N5 B1 119.4(2) . . ? C16 N5 B1 130.8(2) . . ? C15 N6 C21 110.3(2) . . ? C15 N6 C24 125.0(2) . . ? C21 N6 C24 124.7(2) . . ? O1 N7 Ni1 169.3(2) . . ? C25 N8 C26 110.2(2) . . ? C25 N8 B2 119.3(2) . . ? C26 N8 B2 130.5(2) . . ? C25 N9 C31 110.1(2) . . ? C25 N9 C46 125.1(2) . . ? C31 N9 C46 124.8(2) . . ? C32 N10 C33 109.7(2) . . ? C32 N10 B2 119.4(2) . . ? C33 N10 B2 130.8(2) . . ? C32 N11 C38 110.4(2) . . ? C32 N11 C47 125.1(2) . . ? C38 N11 C47 124.5(2) . . ? C39 N12 C40 109.5(2) . . ? C39 N12 B2 119.3(2) . . ? C40 N12 B2 131.1(2) . . ? C39 N13 C45 110.4(2) . . ? C39 N13 C48 124.4(2) . . ? C45 N13 C48 124.5(2) . . ? O2 N14 Ni2 174.8(2) . . ? C49 N15 C50 109.4(2) . . ? C49 N15 B3 119.7(2) . . ? C50 N15 B3 130.8(2) . . ? C49 N16 C55 110.0(2) . . ? C49 N16 C70 125.3(2) . . ? C55 N16 C70 124.7(2) . . ? C56 N17 C57 110.0(2) . . ? C56 N17 B3 119.4(2) . . ? C57 N17 B3 130.7(2) . . ? C56 N18 C62 110.4(2) . . ? C56 N18 C71 125.1(2) . . ? C62 N18 C71 124.5(2) . . ? C63 N19 C64 109.4(2) . . ? C63 N19 B3 119.4(2) . . ? C64 N19 B3 131.3(2) . . ? C63 N20 C69 110.1(2) . . ? C63 N20 C72 124.9(2) . . ? C69 N20 C72 125.0(2) . . ? O3 N21 Ni3 174.3(2) . . ? C73 N22 C74 109.9(2) . . ? C73 N22 B4 119.9(2) . . ? C74 N22 B4 130.2(2) . . ? C73 N23 C79 110.2(2) . . ? C73 N23 C94 125.0(2) . . ? C79 N23 C94 124.7(2) . . ? C80 N24 C81 110.8(2) . . ? C80 N24 B4 119.2(2) . . ? C81 N24 B4 129.9(2) . . ? C80 N25 C86 110.4(2) . . ? C80 N25 C95 124.0(3) . . ? C86 N25 C95 125.5(2) . . ? C87 N26 C88 109.7(2) . . ? C87 N26 B4 119.2(2) . . ? C88 N26 B4 130.9(2) . . ? C87 N27 C93 110.1(2) . . ? C87 N27 C96 124.5(2) . . ? C93 N27 C96 125.2(2) . . ? O4 N28 Ni4 171.3(3) . . ? C97 O5 C100 107.9(3) . . ? C104 O6 C101 108.1(3) . . ? C105 O7 C108 106.7(3) . . ? C109 O8 C111 107.5(3) . . ? N1 C1 N2 107.1(2) . . ? N1 C1 Ni1 118.10(18) . . ? N2 C1 Ni1 134.70(19) . . ? C3 C2 N1 132.4(3) . . ? C3 C2 C7 120.6(2) . . ? N1 C2 C7 107.0(2) . . ? C2 C3 C4 117.0(3) . . ? C3 C4 C5 121.8(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 116.8(3) . . ? C6 C7 N2 131.6(3) . . ? C6 C7 C2 122.4(2) . . ? N2 C7 C2 105.9(2) . . ? N3 C8 N4 107.0(2) . . ? N3 C8 Ni1 118.04(17) . . ? N4 C8 Ni1 134.9(2) . . ? C10 C9 N3 132.4(2) . . ? C10 C9 C14 121.1(3) . . ? N3 C9 C14 106.4(2) . . ? C9 C10 C11 117.1(3) . . ? C10 C11 C12 121.2(3) . . ? C13 C12 C11 122.0(3) . . ? C12 C13 C14 116.6(3) . . ? N4 C14 C13 131.6(3) . . ? N4 C14 C9 106.4(2) . . ? C13 C14 C9 122.0(3) . . ? N6 C15 N5 107.2(2) . . ? N6 C15 Ni1 134.02(19) . . ? N5 C15 Ni1 118.63(17) . . ? C17 C16 N5 132.6(3) . . ? C17 C16 C21 120.7(3) . . ? N5 C16 C21 106.6(2) . . ? C16 C17 C18 117.2(3) . . ? C17 C18 C19 121.8(3) . . ? C20 C19 C18 121.7(3) . . ? C19 C20 C21 116.1(3) . . ? N6 C21 C16 106.2(2) . . ? N6 C21 C20 131.3(3) . . ? C16 C21 C20 122.5(3) . . ? N9 C25 N8 106.8(2) . . ? N9 C25 Ni2 135.10(19) . . ? N8 C25 Ni2 118.02(17) . . ? N8 C26 C27 132.7(2) . . ? N8 C26 C31 106.5(2) . . ? C27 C26 C31 120.8(2) . . ? C28 C27 C26 117.2(2) . . ? C27 C28 C29 121.8(3) . . ? C30 C29 C28 121.4(2) . . ? C29 C30 C31 117.1(2) . . ? N9 C31 C30 132.0(2) . . ? N9 C31 C26 106.3(2) . . ? C30 C31 C26 121.7(2) . . ? N11 C32 N10 106.9(2) . . ? N11 C32 Ni2 134.92(19) . . ? N10 C32 Ni2 118.17(18) . . ? C34 C33 N10 131.9(3) . . ? C34 C33 C38 121.1(2) . . ? N10 C33 C38 107.0(2) . . ? C33 C34 C35 116.6(3) . . ? C34 C35 C36 122.1(3) . . ? C37 C36 C35 121.6(3) . . ? C36 C37 C38 116.5(3) . . ? C37 C38 C33 122.2(3) . . ? C37 C38 N11 131.9(3) . . ? C33 C38 N11 106.0(2) . . ? N13 C39 N12 107.5(2) . . ? N13 C39 Ni2 133.96(18) . . ? N12 C39 Ni2 118.58(17) . . ? C41 C40 C45 120.8(2) . . ? C41 C40 N12 132.5(2) . . ? C45 C40 N12 106.7(2) . . ? C42 C41 C40 117.0(2) . . ? C41 C42 C43 122.1(3) . . ? C44 C43 C42 121.0(2) . . ? C43 C44 C45 117.0(2) . . ? C44 C45 N13 132.0(2) . . ? C44 C45 C40 122.1(2) . . ? N13 C45 C40 105.9(2) . . ? N15 C49 N16 107.6(2) . . ? N15 C49 Ni3 118.20(17) . . ? N16 C49 Ni3 134.18(19) . . ? C51 C50 C55 120.5(2) . . ? C51 C50 N15 132.5(2) . . ? C55 C50 N15 107.0(2) . . ? C52 C51 C50 117.3(2) . . ? C51 C52 C53 121.4(3) . . ? C54 C53 C52 121.8(2) . . ? C53 C54 C55 116.4(2) . . ? C54 C55 N16 131.5(2) . . ? C54 C55 C50 122.5(2) . . ? N16 C55 C50 106.0(2) . . ? N18 C56 N17 106.9(2) . . ? N18 C56 Ni3 134.9(2) . . ? N17 C56 Ni3 118.23(18) . . ? C58 C57 N17 132.0(2) . . ? C58 C57 C62 121.0(2) . . ? N17 C57 C62 106.9(2) . . ? C57 C58 C59 116.6(3) . . ? C60 C59 C58 121.9(3) . . ? C61 C60 C59 121.7(3) . . ? C60 C61 C62 116.7(3) . . ? C61 C62 C57 122.1(3) . . ? C61 C62 N18 132.1(3) . . ? C57 C62 N18 105.8(2) . . ? N19 C63 N20 107.5(2) . . ? N19 C63 Ni3 118.42(18) . . ? N20 C63 Ni3 134.0(2) . . ? N19 C64 C65 132.3(3) . . ? N19 C64 C69 107.1(2) . . ? C65 C64 C69 120.6(3) . . ? C66 C65 C64 116.9(3) . . ? C65 C66 C67 122.3(3) . . ? C68 C67 C66 121.3(3) . . ? C67 C68 C69 116.6(3) . . ? N20 C69 C68 131.8(3) . . ? N20 C69 C64 105.9(2) . . ? C68 C69 C64 122.3(3) . . ? N23 C73 N22 107.0(2) . . ? N23 C73 Ni4 135.11(19) . . ? N22 C73 Ni4 117.85(18) . . ? C75 C74 N22 131.8(3) . . ? C75 C74 C79 121.4(2) . . ? N22 C74 C79 106.7(2) . . ? C74 C75 C76 116.5(3) . . ? C75 C76 C77 122.1(3) . . ? C78 C77 C76 121.2(3) . . ? C77 C78 C79 117.1(3) . . ? C78 C79 N23 132.3(3) . . ? C78 C79 C74 121.6(3) . . ? N23 C79 C74 106.1(2) . . ? N24 C80 N25 105.8(2) . . ? N24 C80 Ni4 118.37(18) . . ? N25 C80 Ni4 135.8(2) . . ? N24 C81 C82 131.9(2) . . ? N24 C81 C86 106.5(2) . . ? C82 C81 C86 121.6(2) . . ? C83 C82 C81 117.0(3) . . ? C82 C83 C84 121.4(3) . . ? C85 C84 C83 121.8(3) . . ? C84 C85 C86 117.0(3) . . ? N25 C86 C81 106.4(2) . . ? N25 C86 C85 132.3(3) . . ? C81 C86 C85 121.2(3) . . ? N27 C87 N26 107.3(2) . . ? N27 C87 Ni4 134.22(19) . . ? N26 C87 Ni4 118.44(18) . . ? N26 C88 C89 132.9(2) . . ? N26 C88 C93 107.0(2) . . ? C89 C88 C93 120.2(2) . . ? C90 C89 C88 117.5(2) . . ? C91 C90 C89 121.9(3) . . ? C92 C91 C90 121.3(3) . . ? C91 C92 C93 117.0(3) . . ? C92 C93 N27 132.0(2) . . ? C92 C93 C88 122.2(2) . . ? N27 C93 C88 105.9(2) . . ? O5 C97 C98 107.3(4) . . ? C97 C98 C99 102.2(4) . . ? C98 C99 C100 106.6(3) . . ? O5 C100 C99 106.6(3) . . ? O6 C101 C102 105.1(3) . . ? C103 C102 C101 104.6(4) . . ? C104 C103 C102 104.8(4) . . ? O6 C104 C103 111.4(4) . . ? O7 C105 C106 110.8(4) . . ? C105 C106 C107 106.6(4) . . ? C108 C107 C106 104.0(4) . . ? O7 C108 C107 108.3(3) . . ? O8 C109 C110 107.2(4) . . ? C109 C110 C112 105.7(3) . . ? O8 C111 C112 105.7(3) . . ? C111 C112 C110 102.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 B1 N1 C1 -54.4(3) . . . . ? N3 B1 N1 C1 58.2(3) . . . . ? N5 B1 N1 C2 117.4(3) . . . . ? N3 B1 N1 C2 -130.0(2) . . . . ? N5 B1 N3 C8 57.0(3) . . . . ? N1 B1 N3 C8 -56.0(3) . . . . ? N5 B1 N3 C9 -123.6(3) . . . . ? N1 B1 N3 C9 123.4(3) . . . . ? N1 B1 N5 C15 55.2(3) . . . . ? N3 B1 N5 C15 -57.4(3) . . . . ? N1 B1 N5 C16 -128.3(2) . . . . ? N3 B1 N5 C16 119.1(3) . . . . ? C15 Ni1 N7 O1 -30.9(13) . . . . ? C1 Ni1 N7 O1 -149.6(12) . . . . ? C8 Ni1 N7 O1 81.8(13) . . . . ? N10 B2 N8 C25 -59.9(3) . . . . ? N12 B2 N8 C25 53.1(3) . . . . ? N10 B2 N8 C26 121.8(3) . . . . ? N12 B2 N8 C26 -125.2(2) . . . . ? N8 B2 N10 C32 56.3(3) . . . . ? N12 B2 N10 C32 -56.8(3) . . . . ? N8 B2 N10 C33 -122.3(2) . . . . ? N12 B2 N10 C33 124.6(2) . . . . ? N10 B2 N12 C39 54.0(3) . . . . ? N8 B2 N12 C39 -58.7(3) . . . . ? N10 B2 N12 C40 -121.7(2) . . . . ? N8 B2 N12 C40 125.6(2) . . . . ? C39 Ni2 N14 O2 13(2) . . . . ? C32 Ni2 N14 O2 -103(2) . . . . ? C25 Ni2 N14 O2 132(2) . . . . ? N19 B3 N15 C49 55.2(3) . . . . ? N17 B3 N15 C49 -57.3(3) . . . . ? N19 B3 N15 C50 -121.7(3) . . . . ? N17 B3 N15 C50 125.7(2) . . . . ? N15 B3 N17 C56 55.2(3) . . . . ? N19 B3 N17 C56 -57.8(3) . . . . ? N15 B3 N17 C57 -124.0(2) . . . . ? N19 B3 N17 C57 123.0(2) . . . . ? N15 B3 N19 C63 -57.5(3) . . . . ? N17 B3 N19 C63 55.4(3) . . . . ? N15 B3 N19 C64 123.4(3) . . . . ? N17 B3 N19 C64 -123.7(3) . . . . ? C56 Ni3 N21 O3 139(2) . . . . ? C49 Ni3 N21 O3 20(2) . . . . ? C63 Ni3 N21 O3 -97(2) . . . . ? N24 B4 N22 C73 59.7(3) . . . . ? N26 B4 N22 C73 -53.1(3) . . . . ? N24 B4 N22 C74 -122.8(2) . . . . ? N26 B4 N22 C74 124.3(2) . . . . ? N22 B4 N24 C80 -57.7(3) . . . . ? N26 B4 N24 C80 56.0(3) . . . . ? N22 B4 N24 C81 118.8(3) . . . . ? N26 B4 N24 C81 -127.6(3) . . . . ? N22 B4 N26 C87 57.3(3) . . . . ? N24 B4 N26 C87 -55.2(3) . . . . ? N22 B4 N26 C88 -128.5(2) . . . . ? N24 B4 N26 C88 119.0(3) . . . . ? C87 Ni4 N28 O4 85.4(16) . . . . ? C73 Ni4 N28 O4 -29.8(17) . . . . ? C80 Ni4 N28 O4 -149.9(16) . . . . ? C2 N1 C1 N2 0.3(3) . . . . ? B1 N1 C1 N2 173.6(2) . . . . ? C2 N1 C1 Ni1 -176.00(16) . . . . ? B1 N1 C1 Ni1 -2.7(3) . . . . ? C7 N2 C1 N1 -0.4(3) . . . . ? C22 N2 C1 N1 -176.5(2) . . . . ? C7 N2 C1 Ni1 175.0(2) . . . . ? C22 N2 C1 Ni1 -1.1(4) . . . . ? N7 Ni1 C1 N1 176.98(17) . . . . ? C15 Ni1 C1 N1 47.17(19) . . . . ? C8 Ni1 C1 N1 -43.49(19) . . . . ? N7 Ni1 C1 N2 2.0(3) . . . . ? C15 Ni1 C1 N2 -127.8(3) . . . . ? C8 Ni1 C1 N2 141.5(3) . . . . ? C1 N1 C2 C3 177.0(3) . . . . ? B1 N1 C2 C3 4.6(4) . . . . ? C1 N1 C2 C7 0.0(3) . . . . ? B1 N1 C2 C7 -172.4(2) . . . . ? N1 C2 C3 C4 -176.2(3) . . . . ? C7 C2 C3 C4 0.6(4) . . . . ? C2 C3 C4 C5 -1.3(5) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C4 C5 C6 C7 -0.7(4) . . . . ? C5 C6 C7 N2 177.1(3) . . . . ? C5 C6 C7 C2 0.0(4) . . . . ? C1 N2 C7 C6 -177.0(3) . . . . ? C22 N2 C7 C6 -0.9(4) . . . . ? C1 N2 C7 C2 0.4(3) . . . . ? C22 N2 C7 C2 176.5(2) . . . . ? C3 C2 C7 C6 0.0(4) . . . . ? N1 C2 C7 C6 177.5(2) . . . . ? C3 C2 C7 N2 -177.7(2) . . . . ? N1 C2 C7 N2 -0.2(3) . . . . ? C9 N3 C8 N4 0.5(3) . . . . ? B1 N3 C8 N4 -180.0(2) . . . . ? C9 N3 C8 Ni1 179.40(16) . . . . ? B1 N3 C8 Ni1 -1.1(3) . . . . ? C14 N4 C8 N3 -0.7(3) . . . . ? C23 N4 C8 N3 -179.5(2) . . . . ? C14 N4 C8 Ni1 -179.3(2) . . . . ? C23 N4 C8 Ni1 1.8(4) . . . . ? N7 Ni1 C8 N3 -169.91(17) . . . . ? C15 Ni1 C8 N3 -43.8(2) . . . . ? C1 Ni1 C8 N3 45.4(2) . . . . ? N7 Ni1 C8 N4 8.6(3) . . . . ? C15 Ni1 C8 N4 134.7(3) . . . . ? C1 Ni1 C8 N4 -136.1(3) . . . . ? C8 N3 C9 C10 178.2(3) . . . . ? B1 N3 C9 C10 -1.3(5) . . . . ? C8 N3 C9 C14 -0.2(3) . . . . ? B1 N3 C9 C14 -179.6(2) . . . . ? N3 C9 C10 C11 -177.9(3) . . . . ? C14 C9 C10 C11 0.3(4) . . . . ? C9 C10 C11 C12 0.1(4) . . . . ? C10 C11 C12 C13 -0.8(5) . . . . ? C11 C12 C13 C14 1.0(4) . . . . ? C8 N4 C14 C13 -178.0(3) . . . . ? C23 N4 C14 C13 0.8(5) . . . . ? C8 N4 C14 C9 0.5(3) . . . . ? C23 N4 C14 C9 179.4(2) . . . . ? C12 C13 C14 N4 177.8(3) . . . . ? C12 C13 C14 C9 -0.6(4) . . . . ? C10 C9 C14 N4 -178.8(2) . . . . ? N3 C9 C14 N4 -0.2(3) . . . . ? C10 C9 C14 C13 -0.1(4) . . . . ? N3 C9 C14 C13 178.5(2) . . . . ? C21 N6 C15 N5 -1.1(3) . . . . ? C24 N6 C15 N5 179.9(2) . . . . ? C21 N6 C15 Ni1 174.4(2) . . . . ? C24 N6 C15 Ni1 -4.5(4) . . . . ? C16 N5 C15 N6 0.7(3) . . . . ? B1 N5 C15 N6 177.9(2) . . . . ? C16 N5 C15 Ni1 -175.68(16) . . . . ? B1 N5 C15 Ni1 1.5(3) . . . . ? N7 Ni1 C15 N6 -1.4(3) . . . . ? C1 Ni1 C15 N6 138.2(3) . . . . ? C8 Ni1 C15 N6 -131.4(3) . . . . ? N7 Ni1 C15 N5 173.80(18) . . . . ? C1 Ni1 C15 N5 -46.6(2) . . . . ? C8 Ni1 C15 N5 43.8(2) . . . . ? C15 N5 C16 C17 -179.9(3) . . . . ? B1 N5 C16 C17 3.4(4) . . . . ? C15 N5 C16 C21 0.0(3) . . . . ? B1 N5 C16 C21 -176.8(2) . . . . ? N5 C16 C17 C18 -177.7(3) . . . . ? C21 C16 C17 C18 2.4(4) . . . . ? C16 C17 C18 C19 -1.4(4) . . . . ? C17 C18 C19 C20 -0.7(5) . . . . ? C18 C19 C20 C21 1.8(4) . . . . ? C15 N6 C21 C16 1.1(3) . . . . ? C24 N6 C21 C16 -179.9(2) . . . . ? C15 N6 C21 C20 -178.1(3) . . . . ? C24 N6 C21 C20 0.8(4) . . . . ? C17 C16 C21 N6 179.2(2) . . . . ? N5 C16 C21 N6 -0.7(3) . . . . ? C17 C16 C21 C20 -1.4(4) . . . . ? N5 C16 C21 C20 178.7(2) . . . . ? C19 C20 C21 N6 178.5(3) . . . . ? C19 C20 C21 C16 -0.7(4) . . . . ? C31 N9 C25 N8 -1.2(3) . . . . ? C46 N9 C25 N8 177.1(2) . . . . ? C31 N9 C25 Ni2 176.4(2) . . . . ? C46 N9 C25 Ni2 -5.3(4) . . . . ? C26 N8 C25 N9 1.4(3) . . . . ? B2 N8 C25 N9 -177.2(2) . . . . ? C26 N8 C25 Ni2 -176.64(16) . . . . ? B2 N8 C25 Ni2 4.7(3) . . . . ? N14 Ni2 C25 N9 2.9(3) . . . . ? C39 Ni2 C25 N9 134.9(3) . . . . ? C32 Ni2 C25 N9 -135.3(3) . . . . ? N14 Ni2 C25 N8 -179.73(16) . . . . ? C39 Ni2 C25 N8 -47.73(19) . . . . ? C32 Ni2 C25 N8 42.14(19) . . . . ? C25 N8 C26 C27 178.8(3) . . . . ? B2 N8 C26 C27 -2.8(4) . . . . ? C25 N8 C26 C31 -1.2(3) . . . . ? B2 N8 C26 C31 177.3(2) . . . . ? N8 C26 C27 C28 -179.9(3) . . . . ? C31 C26 C27 C28 0.0(4) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? C28 C29 C30 C31 0.5(4) . . . . ? C25 N9 C31 C30 -179.5(3) . . . . ? C46 N9 C31 C30 2.2(4) . . . . ? C25 N9 C31 C26 0.5(3) . . . . ? C46 N9 C31 C26 -177.8(2) . . . . ? C29 C30 C31 N9 179.2(3) . . . . ? C29 C30 C31 C26 -0.7(4) . . . . ? N8 C26 C31 N9 0.4(3) . . . . ? C27 C26 C31 N9 -179.5(2) . . . . ? N8 C26 C31 C30 -179.6(2) . . . . ? C27 C26 C31 C30 0.5(4) . . . . ? C38 N11 C32 N10 0.5(3) . . . . ? C47 N11 C32 N10 -178.6(2) . . . . ? C38 N11 C32 Ni2 179.24(19) . . . . ? C47 N11 C32 Ni2 0.1(4) . . . . ? C33 N10 C32 N11 -0.7(3) . . . . ? B2 N10 C32 N11 -179.5(2) . . . . ? C33 N10 C32 Ni2 -179.62(16) . . . . ? B2 N10 C32 Ni2 1.5(3) . . . . ? N14 Ni2 C32 N11 -3.6(3) . . . . ? C39 Ni2 C32 N11 -133.9(3) . . . . ? C25 Ni2 C32 N11 136.0(3) . . . . ? N14 Ni2 C32 N10 174.97(16) . . . . ? C39 Ni2 C32 N10 44.64(19) . . . . ? C25 Ni2 C32 N10 -45.41(19) . . . . ? C32 N10 C33 C34 -179.8(3) . . . . ? B2 N10 C33 C34 -1.1(4) . . . . ? C32 N10 C33 C38 0.5(3) . . . . ? B2 N10 C33 C38 179.2(2) . . . . ? N10 C33 C34 C35 -179.9(3) . . . . ? C38 C33 C34 C35 -0.3(4) . . . . ? C33 C34 C35 C36 0.2(4) . . . . ? C34 C35 C36 C37 -0.2(5) . . . . ? C35 C36 C37 C38 0.2(4) . . . . ? C36 C37 C38 C33 -0.2(4) . . . . ? C36 C37 C38 N11 -180.0(3) . . . . ? C34 C33 C38 C37 0.3(4) . . . . ? N10 C33 C38 C37 -180.0(2) . . . . ? C34 C33 C38 N11 -179.9(2) . . . . ? N10 C33 C38 N11 -0.2(3) . . . . ? C32 N11 C38 C37 179.6(3) . . . . ? C47 N11 C38 C37 -1.3(4) . . . . ? C32 N11 C38 C33 -0.2(3) . . . . ? C47 N11 C38 C33 179.0(2) . . . . ? C45 N13 C39 N12 -0.2(3) . . . . ? C48 N13 C39 N12 171.0(2) . . . . ? C45 N13 C39 Ni2 -179.81(19) . . . . ? C48 N13 C39 Ni2 -8.6(4) . . . . ? C40 N12 C39 N13 0.6(3) . . . . ? B2 N12 C39 N13 -175.95(19) . . . . ? C40 N12 C39 Ni2 -179.77(15) . . . . ? B2 N12 C39 Ni2 3.7(3) . . . . ? N14 Ni2 C39 N13 -1.1(3) . . . . ? C32 Ni2 C39 N13 132.1(2) . . . . ? C25 Ni2 C39 N13 -137.4(2) . . . . ? N14 Ni2 C39 N12 179.40(17) . . . . ? C32 Ni2 C39 N12 -47.41(19) . . . . ? C25 Ni2 C39 N12 43.04(19) . . . . ? C39 N12 C40 C41 178.0(3) . . . . ? B2 N12 C40 C41 -6.1(4) . . . . ? C39 N12 C40 C45 -0.7(3) . . . . ? B2 N12 C40 C45 175.3(2) . . . . ? C45 C40 C41 C42 -0.9(4) . . . . ? N12 C40 C41 C42 -179.4(2) . . . . ? C40 C41 C42 C43 0.9(4) . . . . ? C41 C42 C43 C44 -0.3(4) . . . . ? C42 C43 C44 C45 -0.4(4) . . . . ? C43 C44 C45 N13 178.5(2) . . . . ? C43 C44 C45 C40 0.5(4) . . . . ? C39 N13 C45 C44 -178.4(3) . . . . ? C48 N13 C45 C44 10.3(4) . . . . ? C39 N13 C45 C40 -0.2(3) . . . . ? C48 N13 C45 C40 -171.4(2) . . . . ? C41 C40 C45 C44 0.2(4) . . . . ? N12 C40 C45 C44 179.0(2) . . . . ? C41 C40 C45 N13 -178.3(2) . . . . ? N12 C40 C45 N13 0.5(2) . . . . ? C50 N15 C49 N16 -0.2(3) . . . . ? B3 N15 C49 N16 -177.8(2) . . . . ? C50 N15 C49 Ni3 179.35(16) . . . . ? B3 N15 C49 Ni3 1.8(3) . . . . ? C55 N16 C49 N15 0.4(3) . . . . ? C70 N16 C49 N15 -177.8(2) . . . . ? C55 N16 C49 Ni3 -179.03(19) . . . . ? C70 N16 C49 Ni3 2.7(4) . . . . ? N21 Ni3 C49 N15 -179.22(17) . . . . ? C56 Ni3 C49 N15 44.0(2) . . . . ? C63 Ni3 C49 N15 -45.6(2) . . . . ? N21 Ni3 C49 N16 0.2(3) . . . . ? C56 Ni3 C49 N16 -136.6(3) . . . . ? C63 Ni3 C49 N16 133.8(3) . . . . ? C49 N15 C50 C51 -178.9(3) . . . . ? B3 N15 C50 C51 -1.7(4) . . . . ? C49 N15 C50 C55 -0.1(3) . . . . ? B3 N15 C50 C55 177.1(2) . . . . ? C55 C50 C51 C52 0.2(4) . . . . ? N15 C50 C51 C52 178.9(3) . . . . ? C50 C51 C52 C53 -0.5(4) . . . . ? C51 C52 C53 C54 0.8(4) . . . . ? C52 C53 C54 C55 -0.6(4) . . . . ? C53 C54 C55 N16 -178.9(3) . . . . ? C53 C54 C55 C50 0.3(4) . . . . ? C49 N16 C55 C54 178.8(3) . . . . ? C70 N16 C55 C54 -2.9(4) . . . . ? C49 N16 C55 C50 -0.5(3) . . . . ? C70 N16 C55 C50 177.8(2) . . . . ? C51 C50 C55 C54 -0.1(4) . . . . ? N15 C50 C55 C54 -179.1(2) . . . . ? C51 C50 C55 N16 179.3(2) . . . . ? N15 C50 C55 N16 0.3(3) . . . . ? C62 N18 C56 N17 -0.3(3) . . . . ? C71 N18 C56 N17 -179.0(2) . . . . ? C62 N18 C56 Ni3 179.2(2) . . . . ? C71 N18 C56 Ni3 0.5(4) . . . . ? C57 N17 C56 N18 0.6(3) . . . . ? B3 N17 C56 N18 -178.7(2) . . . . ? C57 N17 C56 Ni3 -178.98(16) . . . . ? B3 N17 C56 Ni3 1.7(3) . . . . ? N21 Ni3 C56 N18 2.3(3) . . . . ? C49 Ni3 C56 N18 134.8(3) . . . . ? C63 Ni3 C56 N18 -135.0(3) . . . . ? N21 Ni3 C56 N17 -178.18(17) . . . . ? C49 Ni3 C56 N17 -45.72(19) . . . . ? C63 Ni3 C56 N17 44.47(19) . . . . ? C56 N17 C57 C58 -179.8(3) . . . . ? B3 N17 C57 C58 -0.5(4) . . . . ? C56 N17 C57 C62 -0.7(3) . . . . ? B3 N17 C57 C62 178.6(2) . . . . ? N17 C57 C58 C59 178.1(2) . . . . ? C62 C57 C58 C59 -0.9(4) . . . . ? C57 C58 C59 C60 0.2(4) . . . . ? C58 C59 C60 C61 0.6(5) . . . . ? C59 C60 C61 C62 -0.7(4) . . . . ? C60 C61 C62 C57 0.0(4) . . . . ? C60 C61 C62 N18 -178.6(3) . . . . ? C58 C57 C62 C61 0.8(4) . . . . ? N17 C57 C62 C61 -178.4(2) . . . . ? C58 C57 C62 N18 179.7(2) . . . . ? N17 C57 C62 N18 0.5(3) . . . . ? C56 N18 C62 C61 178.6(3) . . . . ? C71 N18 C62 C61 -2.6(4) . . . . ? C56 N18 C62 C57 -0.1(3) . . . . ? C71 N18 C62 C57 178.6(2) . . . . ? C64 N19 C63 N20 0.7(3) . . . . ? B3 N19 C63 N20 -178.6(2) . . . . ? C64 N19 C63 Ni3 -178.55(16) . . . . ? B3 N19 C63 Ni3 2.2(3) . . . . ? C69 N20 C63 N19 -0.6(3) . . . . ? C72 N20 C63 N19 176.9(2) . . . . ? C69 N20 C63 Ni3 178.52(19) . . . . ? C72 N20 C63 Ni3 -4.0(4) . . . . ? N21 Ni3 C63 N19 174.35(17) . . . . ? C56 Ni3 C63 N19 -46.79(19) . . . . ? C49 Ni3 C63 N19 43.53(19) . . . . ? N21 Ni3 C63 N20 -4.7(3) . . . . ? C56 Ni3 C63 N20 134.2(2) . . . . ? C49 Ni3 C63 N20 -135.5(2) . . . . ? C63 N19 C64 C65 178.7(3) . . . . ? B3 N19 C64 C65 -2.2(4) . . . . ? C63 N19 C64 C69 -0.6(3) . . . . ? B3 N19 C64 C69 178.6(2) . . . . ? N19 C64 C65 C66 -179.2(3) . . . . ? C69 C64 C65 C66 0.0(4) . . . . ? C64 C65 C66 C67 0.1(4) . . . . ? C65 C66 C67 C68 0.2(5) . . . . ? C66 C67 C68 C69 -0.7(4) . . . . ? C63 N20 C69 C68 -178.2(3) . . . . ? C72 N20 C69 C68 4.3(4) . . . . ? C63 N20 C69 C64 0.2(3) . . . . ? C72 N20 C69 C64 -177.3(2) . . . . ? C67 C68 C69 N20 179.1(3) . . . . ? C67 C68 C69 C64 0.9(4) . . . . ? N19 C64 C69 N20 0.2(3) . . . . ? C65 C64 C69 N20 -179.1(2) . . . . ? N19 C64 C69 C68 178.8(2) . . . . ? C65 C64 C69 C68 -0.5(4) . . . . ? C79 N23 C73 N22 0.8(3) . . . . ? C94 N23 C73 N22 -177.1(2) . . . . ? C79 N23 C73 Ni4 -178.6(2) . . . . ? C94 N23 C73 Ni4 3.4(4) . . . . ? C74 N22 C73 N23 -1.3(3) . . . . ? B4 N22 C73 N23 176.6(2) . . . . ? C74 N22 C73 Ni4 178.23(16) . . . . ? B4 N22 C73 Ni4 -3.8(3) . . . . ? N28 Ni4 C73 N23 -1.6(3) . . . . ? C87 Ni4 C73 N23 -134.1(3) . . . . ? C80 Ni4 C73 N23 137.3(3) . . . . ? N28 Ni4 C73 N22 179.02(18) . . . . ? C87 Ni4 C73 N22 46.45(19) . . . . ? C80 Ni4 C73 N22 -42.10(19) . . . . ? C73 N22 C74 C75 179.5(3) . . . . ? B4 N22 C74 C75 1.8(4) . . . . ? C73 N22 C74 C79 1.3(3) . . . . ? B4 N22 C74 C79 -176.4(2) . . . . ? N22 C74 C75 C76 -176.3(3) . . . . ? C79 C74 C75 C76 1.6(4) . . . . ? C74 C75 C76 C77 -0.9(5) . . . . ? C75 C76 C77 C78 -0.3(6) . . . . ? C76 C77 C78 C79 0.8(5) . . . . ? C77 C78 C79 N23 177.3(3) . . . . ? C77 C78 C79 C74 0.0(4) . . . . ? C73 N23 C79 C78 -177.6(3) . . . . ? C94 N23 C79 C78 0.3(4) . . . . ? C73 N23 C79 C74 0.0(3) . . . . ? C94 N23 C79 C74 177.9(2) . . . . ? C75 C74 C79 C78 -1.2(4) . . . . ? N22 C74 C79 C78 177.1(2) . . . . ? C75 C74 C79 N23 -179.2(2) . . . . ? N22 C74 C79 N23 -0.8(3) . . . . ? C81 N24 C80 N25 2.0(3) . . . . ? B4 N24 C80 N25 179.2(2) . . . . ? C81 N24 C80 Ni4 -175.87(17) . . . . ? B4 N24 C80 Ni4 1.2(3) . . . . ? C86 N25 C80 N24 -1.3(3) . . . . ? C95 N25 C80 N24 -179.5(2) . . . . ? C86 N25 C80 Ni4 176.1(2) . . . . ? C95 N25 C80 Ni4 -2.1(4) . . . . ? N28 Ni4 C80 N24 174.82(18) . . . . ? C87 Ni4 C80 N24 -47.2(2) . . . . ? C73 Ni4 C80 N24 43.7(2) . . . . ? N28 Ni4 C80 N25 -2.3(3) . . . . ? C87 Ni4 C80 N25 135.7(3) . . . . ? C73 Ni4 C80 N25 -133.4(3) . . . . ? C80 N24 C81 C82 175.8(3) . . . . ? B4 N24 C81 C82 -0.9(4) . . . . ? C80 N24 C81 C86 -2.0(3) . . . . ? B4 N24 C81 C86 -178.7(2) . . . . ? N24 C81 C82 C83 -176.6(3) . . . . ? C86 C81 C82 C83 0.9(4) . . . . ? C81 C82 C83 C84 -0.9(4) . . . . ? C82 C83 C84 C85 0.1(5) . . . . ? C83 C84 C85 C86 0.5(5) . . . . ? C80 N25 C86 C81 0.1(3) . . . . ? C95 N25 C86 C81 178.2(3) . . . . ? C80 N25 C86 C85 -176.1(3) . . . . ? C95 N25 C86 C85 2.0(5) . . . . ? N24 C81 C86 N25 1.2(3) . . . . ? C82 C81 C86 N25 -177.0(2) . . . . ? N24 C81 C86 C85 177.8(2) . . . . ? C82 C81 C86 C85 -0.3(4) . . . . ? C84 C85 C86 N25 175.2(3) . . . . ? C84 C85 C86 C81 -0.5(4) . . . . ? C93 N27 C87 N26 -0.8(3) . . . . ? C96 N27 C87 N26 -175.8(2) . . . . ? C93 N27 C87 Ni4 177.36(19) . . . . ? C96 N27 C87 Ni4 2.3(4) . . . . ? C88 N26 C87 N27 0.1(3) . . . . ? B4 N26 C87 N27 175.4(2) . . . . ? C88 N26 C87 Ni4 -178.42(16) . . . . ? B4 N26 C87 Ni4 -3.1(3) . . . . ? N28 Ni4 C87 N27 11.3(3) . . . . ? C73 Ni4 C87 N27 139.4(3) . . . . ? C80 Ni4 C87 N27 -130.1(3) . . . . ? N28 Ni4 C87 N26 -170.76(18) . . . . ? C73 Ni4 C87 N26 -42.67(19) . . . . ? C80 Ni4 C87 N26 47.91(19) . . . . ? C87 N26 C88 C89 -179.1(3) . . . . ? B4 N26 C88 C89 6.3(4) . . . . ? C87 N26 C88 C93 0.7(3) . . . . ? B4 N26 C88 C93 -173.9(2) . . . . ? N26 C88 C89 C90 -179.2(3) . . . . ? C93 C88 C89 C90 1.0(4) . . . . ? C88 C89 C90 C91 -0.1(4) . . . . ? C89 C90 C91 C92 -0.8(4) . . . . ? C90 C91 C92 C93 0.6(4) . . . . ? C91 C92 C93 N27 -179.6(3) . . . . ? C91 C92 C93 C88 0.4(4) . . . . ? C87 N27 C93 C92 -178.9(3) . . . . ? C96 N27 C93 C92 -3.9(4) . . . . ? C87 N27 C93 C88 1.2(3) . . . . ? C96 N27 C93 C88 176.2(2) . . . . ? N26 C88 C93 C92 179.0(2) . . . . ? C89 C88 C93 C92 -1.2(4) . . . . ? N26 C88 C93 N27 -1.1(3) . . . . ? C89 C88 C93 N27 178.7(2) . . . . ? C100 O5 C97 C98 27.8(5) . . . . ? O5 C97 C98 C99 -30.9(5) . . . . ? C97 C98 C99 C100 22.5(5) . . . . ? C97 O5 C100 C99 -12.7(5) . . . . ? C98 C99 C100 O5 -7.0(5) . . . . ? C104 O6 C101 C102 22.4(7) . . . . ? O6 C101 C102 C103 -24.5(6) . . . . ? C101 C102 C103 C104 16.8(8) . . . . ? C101 O6 C104 C103 -12.4(8) . . . . ? C102 C103 C104 O6 -3.9(9) . . . . ? C108 O7 C105 C106 19.6(6) . . . . ? O7 C105 C106 C107 -13.6(7) . . . . ? C105 C106 C107 C108 2.4(7) . . . . ? C105 O7 C108 C107 -17.5(5) . . . . ? C106 C107 C108 O7 9.2(5) . . . . ? C111 O8 C109 C110 28.9(5) . . . . ? O8 C109 C110 C112 -10.5(6) . . . . ? C109 O8 C111 C112 -35.5(5) . . . . ? O8 C111 C112 C110 27.1(5) . . . . ? C109 C110 C112 C111 -10.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.499 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.061 _iucr_refine_instruction_details ; TITL jsNMSU111213_0m in P-1 CELL 0.71073 13.9653 17.0466 23.6430 85.049 76.475 88.960 ZERR 8.00 0.0008 0.0010 0.0013 0.003 0.003 0.003 LATT 1 SFAC C H N O B Ni UNIT 224 240 56 16 8 8 OMIT 0 -1 2 OMIT 0 2 1 OMIT -1 1 1 OMIT -1 0 2 OMIT 1 1 1 OMIT -1 1 2 OMIT 1 -1 2 OMIT 1 1 2 OMIT 1 0 2 OMIT 0 0 2 OMIT 0 2 0 OMIT 1 1 0 OMIT 1 -1 1 OMIT 0 1 2 OMIT 1 2 1 OMIT -1 -1 1 OMIT -1 1 0 OMIT 0 -2 1 OMIT -1 0 1 OMIT 2 0 1 OMIT 1 2 0 L.S. 5 ACTA BOND FMAP 2 PLAN 10 CONF SIZE 0.126 0.179 0.498 WGHT 0.050300 1.391900 FVAR 0.060450 TEMP -100.150 Ni1 6 0.426310 0.350838 0.057707 11.000000 0.025430 = 0.027250 0.032460 -0.004820 -0.008480 0.001920 Ni2 6 0.478299 0.860550 0.447095 11.000000 0.021990 = 0.024050 0.030370 -0.002270 -0.005430 0.001000 Ni3 6 1.003088 0.869879 0.591765 11.000000 0.024550 = 0.025200 0.031770 -0.000600 -0.005400 -0.000440 Ni4 6 0.070993 0.378163 0.906145 11.000000 0.027560 = 0.026060 0.038570 0.006310 -0.011100 -0.005630 B1 5 0.463426 0.172909 0.056648 11.000000 0.028320 = 0.028840 0.025700 -0.002150 -0.006130 -0.001080 H1A 2 0.477385 0.107667 0.054861 11.000000 -1.200000 B2 5 0.524560 0.683705 0.449509 11.000000 0.021250 = 0.027240 0.028520 -0.003690 -0.003650 -0.002340 H2A 2 0.542254 0.617459 0.450311 11.000000 -1.200000 B3 5 0.974848 0.691152 0.618164 11.000000 0.024540 = 0.026210 0.026910 0.000460 -0.003970 -0.002090 H3B 2 0.965453 0.629702 0.627332 11.000000 -1.200000 B4 5 0.028306 0.203390 0.900735 11.000000 0.019800 = 0.029330 0.026070 0.002730 -0.002760 -0.003430 H4B 2 0.011645 0.138817 0.900590 11.000000 -1.200000 N1 3 0.421420 0.207007 0.004427 11.000000 0.026020 = 0.027010 0.025940 -0.003470 -0.006680 -0.002920 N2 3 0.377593 0.300004 -0.053878 11.000000 0.022800 = 0.033130 0.030870 -0.000630 -0.010310 0.001380 N3 3 0.387804 0.194887 0.112754 11.000000 0.022610 = 0.031780 0.026080 -0.000270 -0.004830 -0.003030 N4 3 0.296851 0.273186 0.171430 11.000000 0.023710 = 0.046340 0.029220 -0.007270 -0.004420 0.003650 N5 3 0.558094 0.220424 0.054040 11.000000 0.022770 = 0.032050 0.025310 -0.003720 -0.004260 0.001720 N6 3 0.644187 0.326004 0.053117 11.000000 0.025420 = 0.038970 0.028540 -0.003760 -0.006430 -0.005840 N7 3 0.417838 0.446307 0.063712 11.000000 0.030000 = 0.031730 0.046030 -0.004420 -0.010010 0.008280 N8 3 0.440374 0.703676 0.501921 11.000000 0.017840 = 0.025130 0.027670 -0.001610 -0.003390 -0.002200 N9 3 0.343041 0.780743 0.558612 11.000000 0.021630 = 0.030810 0.027150 -0.004810 -0.003720 0.001680 N10 3 0.490504 0.714927 0.393877 11.000000 0.020940 = 0.027660 0.025380 -0.004360 -0.004140 -0.001400 N11 3 0.438430 0.803043 0.335311 11.000000 0.025190 = 0.037040 0.028810 0.000500 -0.006600 -0.003510 N12 3 0.614925 0.735147 0.451529 11.000000 0.019460 = 0.025390 0.026900 -0.000790 -0.004290 -0.000590 N13 3 0.695627 0.844785 0.447330 11.000000 0.022450 = 0.025200 0.027320 -0.002910 -0.005040 -0.002840 N14 3 0.460695 0.956232 0.444353 11.000000 0.024350 = 0.031360 0.030630 -0.002520 -0.007300 0.004810 N15 3 1.054710 0.713415 0.561541 11.000000 0.022430 = 0.026530 0.025820 -0.001270 -0.004180 -0.000180 N16 3 1.143609 0.792903 0.492531 11.000000 0.021250 = 0.030800 0.026730 0.001210 -0.003270 -0.004100 N17 3 1.006636 0.730592 0.667967 11.000000 0.022870 = 0.029500 0.024700 -0.000220 -0.003720 -0.000750 N18 3 1.051721 0.827442 0.710644 11.000000 0.028790 = 0.034470 0.031940 -0.005140 -0.007220 -0.001190 N19 3 0.878987 0.733682 0.610287 11.000000 0.022750 = 0.029240 0.025560 -0.001700 -0.003570 -0.004220 N20 3 0.787012 0.835127 0.595991 11.000000 0.025020 = 0.041420 0.026300 -0.001390 -0.007330 0.005350 N21 3 1.020867 0.964595 0.573232 11.000000 0.030020 = 0.029880 0.044100 -0.001590 -0.011740 -0.001940 N22 3 0.070677 0.218450 0.953651 11.000000 0.020420 = 0.024230 0.027840 0.004170 -0.003960 -0.001270 N23 3 0.120920 0.288921 1.013870 11.000000 0.025240 = 0.031250 0.031930 -0.000160 -0.009780 -0.002920 N24 3 0.105519 0.237136 0.846270 11.000000 0.021810 = 0.036080 0.026220 0.001630 -0.002700 -0.002880 N25 3 0.201007 0.326097 0.790202 11.000000 0.025960 = 0.049950 0.034240 0.013640 -0.006560 -0.010390 N26 3 -0.065110 0.255950 0.903926 11.000000 0.019860 = 0.025530 0.027970 0.001250 -0.004580 -0.002820 N27 3 -0.145748 0.366928 0.903107 11.000000 0.025200 = 0.029930 0.031250 -0.000300 -0.005570 0.001220 N28 3 0.092023 0.469639 0.916699 11.000000 0.043750 = 0.029410 0.061610 0.009370 -0.030000 -0.009220 O1 4 0.423630 0.513361 0.072819 11.000000 0.063500 = 0.029300 0.113870 -0.019930 -0.022690 0.010350 O2 4 0.455851 1.026246 0.441269 11.000000 0.068270 = 0.027840 0.065160 -0.004950 -0.022240 0.013520 O3 4 1.037035 1.031071 0.555081 11.000000 0.086280 = 0.029200 0.111020 0.010530 -0.038210 -0.017490 O4 4 0.103659 0.532509 0.931989 11.000000 0.120610 = 0.033380 0.124800 -0.000800 -0.074700 -0.019950 O5 4 0.325638 0.902935 0.725105 11.000000 0.051200 = 0.151980 0.054760 -0.018150 -0.012310 -0.022440 O6 4 0.173205 0.841264 0.307212 11.000000 0.042890 = 0.199080 0.053420 -0.007670 -0.016400 -0.006490 O7 4 0.590829 0.443919 0.194646 11.000000 0.085960 = 0.068090 0.066880 -0.023040 -0.023290 -0.001020 O8 4 0.113639 0.556592 0.243512 11.000000 0.094160 = 0.158480 0.064190 -0.010030 -0.014790 0.014370 C1 1 0.403399 0.285363 -0.002002 11.000000 0.021810 = 0.031400 0.030260 -0.001410 -0.005080 -0.001190 C2 1 0.407484 0.171448 -0.043718 11.000000 0.022340 = 0.034850 0.028800 -0.003660 -0.005500 -0.006570 C3 1 0.420013 0.094889 -0.059184 11.000000 0.048390 = 0.036470 0.035020 -0.004310 -0.011760 -0.006090 AFIX 43 H3 2 0.438375 0.053958 -0.033923 11.000000 -1.200000 AFIX 0 C4 1 0.404563 0.080498 -0.113276 11.000000 0.066730 = 0.042750 0.046200 -0.015920 -0.019750 -0.004580 AFIX 43 H4 2 0.413879 0.028713 -0.125531 11.000000 -1.200000 AFIX 0 C5 1 0.375685 0.140088 -0.150202 11.000000 0.053830 = 0.056030 0.035420 -0.012300 -0.019320 -0.003740 AFIX 43 H5 2 0.364421 0.127664 -0.186515 11.000000 -1.200000 AFIX 0 C6 1 0.363267 0.216188 -0.135075 11.000000 0.034120 = 0.051730 0.032330 -0.000380 -0.013020 -0.003480 AFIX 43 H6 2 0.344373 0.256977 -0.160242 11.000000 -1.200000 AFIX 0 C7 1 0.379641 0.230667 -0.081252 11.000000 0.022620 = 0.036210 0.030450 -0.002630 -0.006880 -0.003410 C8 1 0.362951 0.271288 0.119369 11.000000 0.021130 = 0.037400 0.028090 -0.005650 -0.005340 0.001510 C9 1 0.336623 0.147266 0.160707 11.000000 0.022080 = 0.045930 0.026570 0.001680 -0.009470 -0.004010 C10 1 0.334136 0.066623 0.174104 11.000000 0.031380 = 0.047340 0.038520 0.007890 -0.013460 -0.006400 AFIX 43 H10 2 0.373939 0.032219 0.148862 11.000000 -1.200000 AFIX 0 C11 1 0.270847 0.038051 0.226130 11.000000 0.045910 = 0.054540 0.043090 0.019460 -0.018820 -0.013310 AFIX 43 H11 2 0.267329 -0.017036 0.236754 11.000000 -1.200000 AFIX 0 C12 1 0.212316 0.088959 0.263068 11.000000 0.033990 = 0.082840 0.034560 0.014300 -0.005950 -0.011320 AFIX 43 H12 2 0.169279 0.067421 0.298028 11.000000 -1.200000 AFIX 0 C13 1 0.215153 0.169170 0.250342 11.000000 0.027910 = 0.077870 0.027610 0.000850 -0.003510 -0.000990 AFIX 43 H13 2 0.176018 0.203593 0.275869 11.000000 -1.200000 AFIX 0 C14 1 0.278330 0.197432 0.198110 11.000000 0.022970 = 0.056180 0.026510 -0.002840 -0.008430 -0.000090 C15 1 0.553325 0.299988 0.053377 11.000000 0.025210 = 0.030940 0.024850 -0.004250 -0.006660 -0.003000 C16 1 0.653087 0.195467 0.054908 11.000000 0.025130 = 0.040780 0.019720 -0.003200 -0.004430 0.004740 C17 1 0.695982 0.121851 0.055705 11.000000 0.036060 = 0.046840 0.029800 -0.003410 -0.006440 0.010120 AFIX 43 H17 2 0.659866 0.075642 0.054326 11.000000 -1.200000 AFIX 0 C18 1 0.794313 0.118268 0.058615 11.000000 0.041960 = 0.071630 0.036110 -0.008420 -0.005730 0.029010 AFIX 43 H18 2 0.825440 0.068363 0.060110 11.000000 -1.200000 AFIX 0 C19 1 0.848339 0.185810 0.059395 11.000000 0.021980 = 0.096980 0.037390 -0.009250 -0.006380 0.014660 AFIX 43 H19 2 0.915123 0.180761 0.061876 11.000000 -1.200000 AFIX 0 C20 1 0.807352 0.260011 0.056655 11.000000 0.025350 = 0.074550 0.028380 -0.007010 -0.004580 -0.003010 AFIX 43 H20 2 0.844482 0.306335 0.056100 11.000000 -1.200000 AFIX 0 C21 1 0.708022 0.262941 0.054745 11.000000 0.023720 = 0.055010 0.019900 -0.004800 -0.003200 0.000160 C22 1 0.357198 0.377338 -0.079392 11.000000 0.036370 = 0.039060 0.040820 0.001650 -0.012090 0.004040 AFIX 137 H22A 2 0.360702 0.416936 -0.052253 11.000000 -1.500000 H22B 2 0.291144 0.377532 -0.086983 11.000000 -1.500000 H22C 2 0.405996 0.389691 -0.116142 11.000000 -1.500000 AFIX 0 C23 1 0.250518 0.344277 0.195363 11.000000 0.036750 = 0.061600 0.048130 -0.019090 -0.002860 0.010780 AFIX 137 H23A 2 0.278227 0.390487 0.169547 11.000000 -1.500000 H23B 2 0.262786 0.348244 0.234170 11.000000 -1.500000 H23C 2 0.179400 0.341881 0.198458 11.000000 -1.500000 AFIX 0 C24 1 0.671363 0.408929 0.052346 11.000000 0.041980 = 0.043610 0.047080 -0.003680 -0.010070 -0.015500 AFIX 137 H24A 2 0.624646 0.442565 0.036414 11.000000 -1.500000 H24B 2 0.737930 0.417944 0.027901 11.000000 -1.500000 H24C 2 0.669659 0.421644 0.092209 11.000000 -1.500000 AFIX 0 C25 1 0.414155 0.780086 0.508475 11.000000 0.019510 = 0.031190 0.031080 -0.004080 -0.006610 0.001510 C26 1 0.384361 0.655077 0.547141 11.000000 0.017480 = 0.034280 0.025220 -0.000850 -0.007170 -0.002910 C27 1 0.381367 0.573724 0.559864 11.000000 0.025640 = 0.033910 0.031120 -0.000490 -0.006750 -0.000710 AFIX 43 H27 2 0.423339 0.539811 0.535256 11.000000 -1.200000 AFIX 0 C28 1 0.314796 0.544421 0.609775 11.000000 0.032230 = 0.035460 0.037430 0.008790 -0.008040 -0.005680 AFIX 43 H28 2 0.310951 0.489144 0.619527 11.000000 -1.200000 AFIX 0 C29 1 0.253005 0.593823 0.646280 11.000000 0.028050 = 0.048150 0.031840 0.008090 -0.002060 -0.005710 AFIX 43 H29 2 0.208099 0.571425 0.680189 11.000000 -1.200000 AFIX 0 C30 1 0.255806 0.674395 0.634146 11.000000 0.022190 = 0.050670 0.027730 -0.002590 -0.003890 0.001830 AFIX 43 H30 2 0.214197 0.708096 0.659129 11.000000 -1.200000 AFIX 0 C31 1 0.322267 0.704270 0.583677 11.000000 0.017610 = 0.035020 0.026810 -0.001380 -0.007830 -0.000940 C32 1 0.465857 0.792304 0.386833 11.000000 0.017210 = 0.034200 0.028580 -0.000940 -0.003040 -0.001070 C33 1 0.477485 0.676325 0.346738 11.000000 0.016170 = 0.038890 0.027290 -0.007560 -0.000180 -0.005300 C34 1 0.491850 0.598496 0.333623 11.000000 0.023810 = 0.041760 0.038300 -0.011190 -0.002400 -0.001580 AFIX 43 H34 2 0.514615 0.559981 0.358888 11.000000 -1.200000 AFIX 0 C35 1 0.471214 0.579876 0.281657 11.000000 0.036700 = 0.057750 0.049080 -0.026990 -0.003200 -0.003720 AFIX 43 H35 2 0.479912 0.527160 0.271289 11.000000 -1.200000 AFIX 0 C36 1 0.438226 0.635964 0.244334 11.000000 0.043900 = 0.070820 0.035470 -0.022860 -0.009290 -0.006340 AFIX 43 H36 2 0.425235 0.620622 0.209166 11.000000 -1.200000 AFIX 0 C37 1 0.423892 0.713437 0.257161 11.000000 0.034360 = 0.067650 0.030080 -0.007730 -0.006790 -0.005120 AFIX 43 H37 2 0.401173 0.751827 0.231788 11.000000 -1.200000 AFIX 0 C38 1 0.444425 0.732299 0.309089 11.000000 0.022860 = 0.040940 0.028790 -0.002740 -0.002190 -0.005970 C39 1 0.606074 0.814527 0.448728 11.000000 0.023620 = 0.027730 0.025310 -0.005070 -0.005020 -0.001140 C40 1 0.712047 0.714327 0.452503 11.000000 0.022860 = 0.028730 0.019900 -0.002630 -0.003180 0.000140 C41 1 0.758543 0.642017 0.456743 11.000000 0.025270 = 0.028600 0.032190 0.000580 -0.004200 -0.000580 AFIX 43 H41 2 0.723946 0.593871 0.459362 11.000000 -1.200000 AFIX 0 C42 1 0.857350 0.643283 0.456980 11.000000 0.028000 = 0.033730 0.041730 -0.000030 -0.005920 0.005030 AFIX 43 H42 2 0.891387 0.594777 0.459240 11.000000 -1.200000 AFIX 0 C43 1 0.908862 0.713721 0.453998 11.000000 0.021580 = 0.045730 0.038380 -0.001440 -0.010310 0.000810 AFIX 43 H43 2 0.976706 0.712037 0.454468 11.000000 -1.200000 AFIX 0 C44 1 0.862558 0.785765 0.450378 11.000000 0.023100 = 0.033240 0.032930 -0.003010 -0.007310 -0.004650 AFIX 43 H44 2 0.896951 0.833823 0.448599 11.000000 -1.200000 AFIX 0 C45 1 0.763730 0.784699 0.449463 11.000000 0.024150 = 0.028120 0.021790 -0.001890 -0.003070 -0.001840 C46 1 0.297091 0.851261 0.583632 11.000000 0.030420 = 0.036340 0.035920 -0.010940 -0.003230 0.005720 AFIX 137 H46A 2 0.329979 0.898062 0.560884 11.000000 -1.500000 H46B 2 0.303111 0.851008 0.624121 11.000000 -1.500000 H46C 2 0.227283 0.852132 0.582715 11.000000 -1.500000 AFIX 0 C47 1 0.408234 0.877999 0.310196 11.000000 0.041520 = 0.045910 0.039270 0.007570 -0.016380 -0.001180 AFIX 137 H47A 2 0.414710 0.919762 0.335073 11.000000 -1.500000 H47B 2 0.339473 0.874372 0.307577 11.000000 -1.500000 H47C 2 0.450241 0.890200 0.271074 11.000000 -1.500000 AFIX 0 C48 1 0.720392 0.928036 0.436129 11.000000 0.031930 = 0.025370 0.041420 -0.004060 -0.006380 -0.005790 AFIX 137 H48A 2 0.754920 0.939164 0.395147 11.000000 -1.500000 H48B 2 0.763029 0.941722 0.461370 11.000000 -1.500000 H48C 2 0.659919 0.959336 0.444320 11.000000 -1.500000 AFIX 0 C49 1 1.074526 0.790097 0.543528 11.000000 0.018940 = 0.030580 0.030390 0.000480 -0.006470 -0.001120 C50 1 1.111910 0.666299 0.521228 11.000000 0.020300 = 0.034380 0.022590 -0.001730 -0.005610 0.001260 C51 1 1.118624 0.585361 0.518568 11.000000 0.032640 = 0.031750 0.029050 0.000000 -0.005150 0.001370 AFIX 43 H51 2 1.080320 0.550292 0.548366 11.000000 -1.200000 AFIX 0 C52 1 1.183450 0.557717 0.470699 11.000000 0.037050 = 0.035180 0.037580 -0.009760 -0.006630 0.004440 AFIX 43 H52 2 1.190111 0.502554 0.467811 11.000000 -1.200000 AFIX 0 C53 1 1.239226 0.609212 0.426592 11.000000 0.030840 = 0.049050 0.033570 -0.014020 -0.001990 0.004440 AFIX 43 H53 2 1.282300 0.588152 0.394164 11.000000 -1.200000 AFIX 0 C54 1 1.233494 0.689559 0.428823 11.000000 0.021220 = 0.047150 0.028130 -0.003410 -0.001730 -0.002420 AFIX 43 H54 2 1.271931 0.724534 0.399011 11.000000 -1.200000 AFIX 0 C55 1 1.168494 0.716848 0.477001 11.000000 0.019840 = 0.034060 0.024990 -0.001150 -0.006920 0.000550 C56 1 1.023466 0.809522 0.662114 11.000000 0.021500 = 0.033780 0.030590 -0.004950 -0.003240 0.000610 C57 1 1.023278 0.698157 0.720844 11.000000 0.016050 = 0.038310 0.026390 -0.002120 -0.002080 0.001420 C58 1 1.016601 0.621486 0.746586 11.000000 0.026690 = 0.039660 0.029220 0.000340 -0.002010 0.000480 AFIX 43 H58 2 0.995810 0.579304 0.728517 11.000000 -1.200000 AFIX 0 C59 1 1.041960 0.609591 0.800280 11.000000 0.036120 = 0.052450 0.031930 0.009530 -0.003980 0.001460 AFIX 43 H59 2 1.038556 0.557899 0.819208 11.000000 -1.200000 AFIX 0 C60 1 1.072082 0.671184 0.826925 11.000000 0.042790 = 0.069580 0.029140 0.004670 -0.014890 -0.001430 AFIX 43 H60 2 1.089282 0.660411 0.863386 11.000000 -1.200000 AFIX 0 C61 1 1.077655 0.747443 0.801854 11.000000 0.038070 = 0.057440 0.033070 -0.005900 -0.012300 -0.003420 AFIX 43 H61 2 1.097617 0.789587 0.820310 11.000000 -1.200000 AFIX 0 C62 1 1.052696 0.759722 0.748332 11.000000 0.021580 = 0.042710 0.030770 -0.004420 -0.003690 0.001070 C63 1 0.879291 0.812953 0.599600 11.000000 0.026530 = 0.036090 0.020060 -0.001960 -0.004220 0.003090 C64 1 0.785485 0.704741 0.612861 11.000000 0.023720 = 0.045970 0.020600 -0.005810 -0.001710 -0.007450 C65 1 0.747074 0.628753 0.621524 11.000000 0.036240 = 0.048290 0.031000 -0.005520 -0.002340 -0.010220 AFIX 43 H65 2 0.786398 0.584211 0.627685 11.000000 -1.200000 AFIX 0 C66 1 0.648675 0.621052 0.620748 11.000000 0.044620 = 0.072150 0.039830 -0.009690 -0.005430 -0.028440 AFIX 43 H66 2 0.620285 0.569907 0.626621 11.000000 -1.200000 AFIX 0 C67 1 0.590094 0.685705 0.611658 11.000000 0.029740 = 0.098660 0.042860 -0.009940 -0.010250 -0.014040 AFIX 43 H67 2 0.522979 0.677632 0.611625 11.000000 -1.200000 AFIX 0 C68 1 0.627607 0.761290 0.602694 11.000000 0.029060 = 0.077250 0.032940 -0.007410 -0.010040 0.000320 AFIX 43 H68 2 0.588200 0.805579 0.596044 11.000000 -1.200000 AFIX 0 C69 1 0.726368 0.769357 0.603895 11.000000 0.023460 = 0.053370 0.023520 -0.004980 -0.005010 -0.001660 C70 1 1.188137 0.864808 0.459316 11.000000 0.030700 = 0.035360 0.035080 0.005280 -0.002160 -0.004690 AFIX 137 H70A 2 1.150989 0.910629 0.474891 11.000000 -1.500000 H70B 2 1.186759 0.863164 0.418184 11.000000 -1.500000 H70C 2 1.256501 0.868815 0.462618 11.000000 -1.500000 AFIX 0 C71 1 1.075626 0.906154 0.722699 11.000000 0.045400 = 0.041960 0.050700 -0.012550 -0.016760 -0.005290 AFIX 137 H71A 2 1.070239 0.943760 0.689823 11.000000 -1.500000 H71B 2 1.143054 0.906755 0.728128 11.000000 -1.500000 H71C 2 1.029677 0.920926 0.758260 11.000000 -1.500000 AFIX 0 C72 1 0.755284 0.915775 0.587708 11.000000 0.042010 = 0.051100 0.042840 0.004020 -0.014540 0.014900 AFIX 137 H72A 2 0.720074 0.933412 0.625351 11.000000 -1.500000 H72B 2 0.711405 0.918967 0.560744 11.000000 -1.500000 H72C 2 0.812899 0.949530 0.571422 11.000000 -1.500000 AFIX 0 C73 1 0.090232 0.293163 0.963405 11.000000 0.019330 = 0.029690 0.032420 0.001250 -0.004570 -0.002120 C74 1 0.091125 0.166051 0.997514 11.000000 0.015890 = 0.032030 0.033590 0.005270 -0.004750 0.001970 C75 1 0.082755 0.085136 1.007200 11.000000 0.034720 = 0.031430 0.060390 0.002900 -0.020020 0.000820 AFIX 43 H75 2 0.063045 0.054185 0.980335 11.000000 -1.200000 AFIX 0 C76 1 0.104625 0.051432 1.058189 11.000000 0.056630 = 0.039210 0.088130 0.023390 -0.042820 -0.003210 AFIX 43 H76 2 0.098799 -0.004014 1.066640 11.000000 -1.200000 AFIX 0 C77 1 0.134797 0.096194 1.097320 11.000000 0.065140 = 0.059670 0.075870 0.033330 -0.046550 -0.011670 AFIX 43 H77 2 0.148749 0.070778 1.131851 11.000000 -1.200000 AFIX 0 C78 1 0.144847 0.176754 1.086952 11.000000 0.042430 = 0.056040 0.049430 0.008760 -0.025810 -0.007490 AFIX 43 H78 2 0.166207 0.207457 1.113376 11.000000 -1.200000 AFIX 0 C79 1 0.122506 0.210987 1.036437 11.000000 0.020150 = 0.038740 0.033910 0.005800 -0.008370 -0.002100 C80 1 0.131452 0.313997 0.841838 11.000000 0.021770 = 0.040940 0.034130 0.011480 -0.008630 -0.005950 C81 1 0.159782 0.199517 0.799357 11.000000 0.018460 = 0.056690 0.021870 -0.002350 -0.005910 -0.003390 C82 1 0.163534 0.121329 0.786496 11.000000 0.025410 = 0.060720 0.031110 -0.011860 -0.005860 -0.001730 AFIX 43 H82 2 0.121783 0.082481 0.810921 11.000000 -1.200000 AFIX 0 C83 1 0.230896 0.102548 0.736450 11.000000 0.032610 = 0.077470 0.040070 -0.025160 -0.010830 -0.001850 AFIX 43 H83 2 0.236089 0.049519 0.726615 11.000000 -1.200000 AFIX 0 C84 1 0.291165 0.159803 0.700256 11.000000 0.030570 = 0.105210 0.029030 -0.019520 -0.001910 -0.004910 AFIX 43 H84 2 0.336392 0.144795 0.666263 11.000000 -1.200000 AFIX 0 C85 1 0.286982 0.237586 0.712403 11.000000 0.029290 = 0.094470 0.027270 0.003310 -0.003040 -0.013530 AFIX 43 H85 2 0.327827 0.276478 0.687412 11.000000 -1.200000 AFIX 0 C86 1 0.219857 0.256679 0.763205 11.000000 0.025260 = 0.062370 0.025720 0.004080 -0.007470 -0.005100 C87 1 -0.056766 0.334989 0.904845 11.000000 0.030520 = 0.027430 0.023500 0.001790 -0.004640 -0.001600 C88 1 -0.160346 0.237167 0.901526 11.000000 0.019210 = 0.032960 0.021130 0.002420 -0.000210 -0.000930 C89 1 -0.207086 0.166173 0.900479 11.000000 0.028420 = 0.031570 0.034280 0.002610 -0.005270 -0.002170 AFIX 43 H89 2 -0.173273 0.117450 0.901955 11.000000 -1.200000 AFIX 0 C90 1 -0.304885 0.169195 0.897198 11.000000 0.028240 = 0.041280 0.046150 -0.001520 -0.007270 -0.010100 AFIX 43 H90 2 -0.338422 0.121470 0.896367 11.000000 -1.200000 AFIX 0 C91 1 -0.355122 0.239736 0.895098 11.000000 0.020620 = 0.052240 0.041910 -0.000230 -0.005230 -0.002970 AFIX 43 H91 2 -0.421917 0.239388 0.892388 11.000000 -1.200000 AFIX 0 C92 1 -0.309944 0.310697 0.896870 11.000000 0.023530 = 0.043310 0.034120 -0.000330 -0.004340 0.005500 AFIX 43 H92 2 -0.344375 0.359179 0.895805 11.000000 -1.200000 AFIX 0 C93 1 -0.212183 0.307936 0.900269 11.000000 0.023720 = 0.033400 0.023210 0.000710 -0.001040 0.000710 C94 1 0.145473 0.356675 1.041877 11.000000 0.031900 = 0.041170 0.039710 -0.008860 -0.011530 -0.005110 AFIX 137 H94A 2 0.141711 0.405002 1.016849 11.000000 -1.500000 H94B 2 0.212395 0.350597 1.047885 11.000000 -1.500000 H94C 2 0.098752 0.359788 1.079648 11.000000 -1.500000 AFIX 0 C95 1 0.249669 0.401400 0.768521 11.000000 0.042120 = 0.064650 0.051150 0.024770 -0.005660 -0.020510 AFIX 137 H95A 2 0.320904 0.395342 0.764036 11.000000 -1.500000 H95B 2 0.224937 0.440648 0.796325 11.000000 -1.500000 H95C 2 0.235859 0.418803 0.730635 11.000000 -1.500000 AFIX 0 C96 1 -0.165956 0.451117 0.899576 11.000000 0.041530 = 0.029260 0.049890 -0.002020 -0.008190 0.007430 AFIX 137 H96A 2 -0.114524 0.479204 0.911726 11.000000 -1.500000 H96B 2 -0.230103 0.461197 0.925343 11.000000 -1.500000 H96C 2 -0.166836 0.469590 0.859283 11.000000 -1.500000 AFIX 0 C97 1 0.419751 0.927201 0.692327 11.000000 0.053990 = 0.198400 0.069640 -0.001150 -0.009710 -0.032400 AFIX 23 H97A 2 0.422134 0.985236 0.684659 11.000000 -1.200000 H97B 2 0.435139 0.903589 0.654429 11.000000 -1.200000 AFIX 0 C98 1 0.491355 0.900585 0.726871 11.000000 0.054900 = 0.086730 0.069420 -0.019630 -0.005180 -0.013640 AFIX 23 H98A 2 0.548782 0.936487 0.718751 11.000000 -1.200000 H98B 2 0.514550 0.846508 0.718979 11.000000 -1.200000 AFIX 0 C99 1 0.432604 0.903328 0.787445 11.000000 0.064810 = 0.177280 0.075270 -0.064180 -0.024130 0.011930 AFIX 23 H99A 2 0.445381 0.953010 0.803252 11.000000 -1.200000 H99B 2 0.449818 0.858586 0.812779 11.000000 -1.200000 AFIX 0 C100 1 0.327277 0.898482 0.785093 11.000000 0.063760 = 0.109450 0.053530 -0.007640 -0.005440 0.004140 AFIX 23 H10A 2 0.297855 0.848244 0.805252 11.000000 -1.200000 H10B 2 0.289486 0.942545 0.804233 11.000000 -1.200000 AFIX 0 C101 1 0.169191 0.815072 0.254756 11.000000 0.053250 = 0.120250 0.112470 -0.057730 -0.025190 0.016980 AFIX 23 H10C 2 0.170298 0.756815 0.256928 11.000000 -1.200000 H10D 2 0.225590 0.835616 0.223585 11.000000 -1.200000 AFIX 0 C102 1 0.073204 0.846199 0.243017 11.000000 0.060930 = 0.259500 0.091920 -0.081060 -0.038480 0.051860 AFIX 23 H10E 2 0.083606 0.896538 0.218172 11.000000 -1.200000 H10F 2 0.042749 0.807813 0.223360 11.000000 -1.200000 AFIX 0 C103 1 0.012783 0.857522 0.299444 11.000000 0.068030 = 0.220910 0.068230 -0.047530 -0.032470 0.045360 AFIX 23 H10G 2 -0.022527 0.908375 0.298986 11.000000 -1.200000 H10H 2 -0.036113 0.814492 0.312496 11.000000 -1.200000 AFIX 0 C104 1 0.079250 0.857012 0.336523 11.000000 0.047250 = 0.423990 0.067520 -0.059970 -0.013780 0.026620 AFIX 23 H10I 2 0.077761 0.908902 0.352557 11.000000 -1.200000 H10J 2 0.058170 0.816651 0.369654 11.000000 -1.200000 AFIX 0 C105 1 0.648226 0.398304 0.226239 11.000000 0.111060 = 0.099090 0.151350 0.001490 -0.086910 -0.003780 AFIX 23 H10K 2 0.642399 0.419148 0.264705 11.000000 -1.200000 H10L 2 0.718245 0.401788 0.204925 11.000000 -1.200000 AFIX 0 C106 1 0.617678 0.318934 0.234436 11.000000 0.113230 = 0.084900 0.204010 -0.009790 -0.095600 -0.001990 AFIX 23 H10M 2 0.611641 0.298229 0.275549 11.000000 -1.200000 H10N 2 0.665964 0.286353 0.208961 11.000000 -1.200000 AFIX 0 C107 1 0.519406 0.317145 0.218859 11.000000 0.110430 = 0.109510 0.088230 0.014250 -0.048380 -0.026200 AFIX 23 H10O 2 0.521327 0.282526 0.187078 11.000000 -1.200000 H10P 2 0.467137 0.298292 0.253148 11.000000 -1.200000 AFIX 0 C108 1 0.502304 0.400555 0.199438 11.000000 0.072100 = 0.079760 0.087750 -0.047200 -0.037790 0.011170 AFIX 23 H10Q 2 0.484369 0.403542 0.161202 11.000000 -1.200000 H10R 2 0.447619 0.422955 0.228094 11.000000 -1.200000 AFIX 0 C109 1 0.148421 0.567693 0.292778 11.000000 0.072320 = 0.104410 0.081980 -0.005230 -0.033140 0.007270 AFIX 23 H10S 2 0.194325 0.613026 0.284874 11.000000 -1.200000 H10T 2 0.183877 0.520194 0.303939 11.000000 -1.200000 AFIX 0 C110 1 0.061966 0.582781 0.340222 11.000000 0.075830 = 0.143700 0.061830 -0.011930 -0.022410 0.004610 AFIX 23 H11A 2 0.072776 0.630271 0.359269 11.000000 -1.200000 H11B 2 0.049435 0.537364 0.370042 11.000000 -1.200000 AFIX 0 C111 1 0.026530 0.600152 0.247400 11.000000 0.098160 = 0.098060 0.067850 -0.011160 -0.037700 0.017870 AFIX 23 H11C 2 -0.015854 0.577614 0.224651 11.000000 -1.200000 H11D 2 0.041462 0.655645 0.232275 11.000000 -1.200000 AFIX 0 C112 1 -0.023753 0.594937 0.311389 11.000000 0.070140 = 0.110840 0.074870 -0.026910 -0.022500 0.007790 AFIX 23 H11E 2 -0.070226 0.549983 0.322012 11.000000 -1.200000 H11F 2 -0.059669 0.644076 0.322177 11.000000 -1.200000 AFIX HKLF 4 1 1 0 0 0 1 0 0 0 1 END Q1 1 0.041800 0.802100 0.279300 11.000000 0.050000 0.500000 Q2 1 0.403200 0.301900 0.039700 11.000000 0.050000 0.440000 Q3 1 1.021500 0.917300 0.610600 11.000000 0.050000 0.420000 Q4 1 0.445400 0.381300 0.090400 11.000000 0.050000 0.410000 Q5 1 0.465900 0.809700 0.432000 11.000000 0.050000 0.390000 Q6 1 0.158200 0.519000 0.901400 11.000000 0.050000 0.380000 Q7 1 0.150900 0.783300 0.299200 11.000000 0.050000 0.350000 Q8 1 0.076200 0.797600 0.329900 11.000000 0.050000 0.350000 Q9 1 1.162500 0.755900 0.482300 11.000000 0.050000 0.350000 Q10 1 0.423300 0.864700 0.697100 11.000000 0.050000 0.340000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM jsNMSU111213_0m in P-1 REM R1= 0.0445 for 16267 Fo > 4sig(Fo) and 0.0814 for all 24003 data REM 1429 parameters refined using 0 restraints ; data_jsnmsu030712 _audit_update_record ; 2012-09-06 # Formatted by publCIF ; _vrf_PLAT220_jsnmsu030712 ; RESPONSE: This is part of a cyclohexyl ring with large thermal motion. Attempts to model the ring as disordered did not improve the structure ; _vrf_PLAT222_jsnmsu030712 ; RESPONSE: This is part of a cyclohexyl ring with large thermal motion. Attempts to model the ring as disordered did not improve the structure ; _vrf_PLAT241_jsnmsu030712 ; 2 RESPONSE: This is part of a cyclohexyl ring with large thermal motion. Attempts to model the ring as disordered did not improve the structure ; _vrf_PLAT341_jsnmsu030712 ; RESPONSE: Very weakly diffracting crystal ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 B N7 Ni O' _chemical_formula_weight 740.43 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' 'B' 'B' 0.0013 0.0007 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.241(4) _cell_length_b 10.847(3) _cell_length_c 22.885(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.991(14) _cell_angle_gamma 90.00 _cell_volume 3960.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 846 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 17.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8871 _exptl_absorpt_correction_T_max 0.9434 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19853 _diffrn_reflns_av_R_equivalents 0.1401 _diffrn_reflns_av_sigmaI/netI 0.2085 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7776 _reflns_number_gt 3260 _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. ; _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^)+(0.1108P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7776 _refine_ls_number_parameters 509 _refine_ls_number_restraints 224 _refine_ls_R_factor_all 0.2134 _refine_ls_R_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.2528 _refine_ls_wR_factor_gt 0.1976 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.965 _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 Ni1 Ni 0.28686(5) 0.54361(9) 1.03707(4) 0.0370(3) Uani 1 1 d . . . O1 O 0.2989(5) 0.6872(8) 0.9432(4) 0.118(3) Uani 1 1 d . . . N1 N 0.1744(3) 0.4077(5) 1.0566(3) 0.0312(7) Uani 1 1 d . . . N2 N 0.1040(3) 0.4607(6) 0.9463(3) 0.0491(15) Uani 1 1 d . . . N3 N 0.3265(3) 0.3451(5) 1.1345(2) 0.0312(7) Uani 1 1 d . . . N4 N 0.4166(3) 0.3318(5) 1.1051(3) 0.0349(14) Uani 1 1 d . A . N5 N 0.2762(3) 0.5433(5) 1.1568(2) 0.0312(7) Uani 1 1 d . . . N6 N 0.3057(3) 0.7312(6) 1.1443(2) 0.0333(13) Uani 1 1 d . . . N7 N 0.3020(4) 0.6270(6) 0.9821(3) 0.0465(16) Uani 1 1 d . . . B1 B 0.2510(4) 0.4021(8) 1.1348(4) 0.0312(7) Uani 1 1 d D . . H1 H 0.242(3) 0.348(4) 1.165(2) 0.037 Uiso 1 1 d D . . C1 C 0.1796(4) 0.4651(7) 1.0072(3) 0.0403(17) Uani 1 1 d . . . C2 C 0.0930(4) 0.3661(7) 1.0267(4) 0.0446(19) Uani 1 1 d . . . C3 C 0.0540(4) 0.3095(7) 1.0544(5) 0.058(2) Uani 1 1 d . . . H3 H 0.0848 0.2891 1.1031 0.069 Uiso 1 1 calc R . . C4 C -0.0301(5) 0.2823(8) 1.0115(6) 0.076(3) Uani 1 1 d . . . H4 H -0.0576 0.2424 1.0302 0.091 Uiso 1 1 calc R . . C5 C -0.0736(5) 0.3131(9) 0.9420(7) 0.090(4) Uani 1 1 d . . . H5 H -0.1314 0.2926 0.9131 0.108 Uiso 1 1 calc R . . C6 C -0.0380(5) 0.3730(8) 0.9107(5) 0.075(3) Uani 1 1 d . . . H6 H -0.0695 0.3935 0.8620 0.090 Uiso 1 1 calc R . . C7 C 0.0474(4) 0.4007(7) 0.9563(4) 0.053(2) Uani 1 1 d . . . C8 C 0.0806(5) 0.5231(9) 0.8809(4) 0.070(3) Uani 1 1 d . . . H8A H 0.1201 0.5918 0.8924 0.083 Uiso 1 1 calc R . . H8B H 0.0239 0.5588 0.8588 0.083 Uiso 1 1 calc R . . C9 C 0.0809(8) 0.4337(15) 0.8254(5) 0.139(5) Uani 1 1 d U . . H9 H 0.0361 0.3698 0.8089 0.166 Uiso 1 1 calc R . . C10 C 0.0622(11) 0.5149(18) 0.7608(6) 0.215(7) Uani 1 1 d DU . . H10A H 0.0075 0.5568 0.7399 0.258 Uiso 1 1 calc R . . H10B H 0.1060 0.5791 0.7775 0.258 Uiso 1 1 calc R . . C11 C 0.0604(13) 0.437(2) 0.7051(8) 0.245(9) Uani 1 1 d DU . . H11A H 0.0108 0.3822 0.6831 0.294 Uiso 1 1 calc R . . H11B H 0.0544 0.4917 0.6679 0.294 Uiso 1 1 calc R . . C12 C 0.1346(15) 0.363(2) 0.7332(9) 0.279(10) Uani 1 1 d DU . . H12A H 0.1819 0.4187 0.7456 0.334 Uiso 1 1 calc R . . H12B H 0.1262 0.3070 0.6958 0.334 Uiso 1 1 calc R . . C13 C 0.1584(12) 0.2886(18) 0.7965(8) 0.222(8) Uani 1 1 d U . . H13A H 0.2142 0.2507 0.8167 0.266 Uiso 1 1 calc R . . H13B H 0.1171 0.2219 0.7833 0.266 Uiso 1 1 calc R . . C14 C 0.1606(8) 0.3738(13) 0.8506(6) 0.139(5) Uani 1 1 d U . . H14A H 0.1777 0.3253 0.8933 0.167 Uiso 1 1 calc R . . H14B H 0.2038 0.4380 0.8644 0.167 Uiso 1 1 calc R . . C15 C 0.3486(4) 0.3962(7) 1.0927(3) 0.0348(16) Uani 1 1 d . . . C16 C 0.3803(4) 0.2490(6) 1.1735(3) 0.0324(16) Uani 1 1 d . . . C17 C 0.3853(4) 0.1716(7) 1.2240(3) 0.0387(17) Uani 1 1 d . . . H17 H 0.3470 0.1775 1.2376 0.046 Uiso 1 1 calc R . . C18 C 0.4493(4) 0.0852(7) 1.2534(3) 0.048(2) Uani 1 1 d . . . H18 H 0.4552 0.0313 1.2887 0.058 Uiso 1 1 calc R . . C19 C 0.5058(4) 0.0742(7) 1.2332(4) 0.0445(19) Uani 1 1 d . . . H19 H 0.5480 0.0126 1.2542 0.053 Uiso 1 1 calc R . . C20 C 0.5005(4) 0.1523(7) 1.1832(3) 0.0441(19) Uani 1 1 d . . . H20 H 0.5386 0.1460 1.1694 0.053 Uiso 1 1 calc R . . C21 C 0.4376(4) 0.2399(6) 1.1541(3) 0.0338(16) Uani 1 1 d . . . C22 C 0.4597(4) 0.3608(7) 1.0704(3) 0.0417(18) Uani 1 1 d . . . H22A H 0.5203 0.3442 1.1035 0.050 Uiso 1 1 calc R A . H22B H 0.4528 0.4497 1.0585 0.050 Uiso 1 1 calc R . . C23 C 0.427(3) 0.287(5) 1.005(3) 0.069(6) Uani 0.504(12) 1 d PU A -1 H23 H 0.3641 0.2952 0.9758 0.083 Uiso 0.504(12) 1 calc PR A -1 C24 C 0.4444(11) 0.1622(19) 1.0093(9) 0.064(4) Uani 0.504(12) 1 d PU A -1 H24A H 0.4200 0.1202 1.0323 0.076 Uiso 0.504(12) 1 calc PR A -1 H24B H 0.5060 0.1513 1.0401 0.076 Uiso 0.504(12) 1 calc PR A -1 C25 C 0.4116(14) 0.098(2) 0.9381(11) 0.076(5) Uani 0.504(12) 1 d PU A -1 H25A H 0.4245 0.0092 0.9453 0.091 Uiso 0.504(12) 1 calc PR A -1 H25B H 0.3500 0.1086 0.9061 0.091 Uiso 0.504(12) 1 calc PR A -1 C26 C 0.4554(19) 0.160(3) 0.9062(15) 0.095(7) Uani 0.504(12) 1 d PU A -1 H26A H 0.5170 0.1513 0.9388 0.114 Uiso 0.504(12) 1 calc PR A -1 H26B H 0.4374 0.1200 0.8609 0.114 Uiso 0.504(12) 1 calc PR A -1 C27 C 0.4307(19) 0.295(2) 0.8948(12) 0.108(6) Uani 0.504(12) 1 d PU A -1 H27A H 0.3689 0.3014 0.8626 0.130 Uiso 0.504(12) 1 calc PR A -1 H27B H 0.4555 0.3358 0.8720 0.130 Uiso 0.504(12) 1 calc PR A -1 C28 C 0.4600(15) 0.361(2) 0.9642(12) 0.084(6) Uani 0.504(12) 1 d PU A -1 H28A H 0.4380 0.4461 0.9545 0.101 Uiso 0.504(12) 1 calc PR A -1 H28B H 0.5220 0.3646 0.9942 0.101 Uiso 0.504(12) 1 calc PR A -1 C23A C 0.446(3) 0.272(6) 1.012(3) 0.070(7) Uani 0.496(12) 1 d PU A -2 H23A H 0.4674 0.1918 1.0375 0.084 Uiso 0.496(12) 1 calc PR A -2 C24A C 0.3586(12) 0.246(2) 0.9574(10) 0.087(6) Uani 0.496(12) 1 d PU A -2 H24C H 0.3312 0.3234 0.9314 0.104 Uiso 0.496(12) 1 calc PR A -2 H24D H 0.3296 0.2183 0.9796 0.104 Uiso 0.496(12) 1 calc PR A -2 C25A C 0.3483(17) 0.148(3) 0.9052(13) 0.109(7) Uani 0.496(12) 1 d PU A -2 H25C H 0.2884 0.1412 0.8662 0.131 Uiso 0.496(12) 1 calc PR A -2 H25D H 0.3672 0.0675 0.9291 0.131 Uiso 0.496(12) 1 calc PR A -2 C26A C 0.4011(16) 0.185(3) 0.8749(13) 0.096(6) Uani 0.496(12) 1 d PU A -2 H26C H 0.3969 0.1183 0.8433 0.115 Uiso 0.496(12) 1 calc PR A -2 H26D H 0.3783 0.2612 0.8469 0.115 Uiso 0.496(12) 1 calc PR A -2 C27A C 0.4874(17) 0.203(3) 0.9310(15) 0.102(7) Uani 0.496(12) 1 d PU A -2 H27C H 0.5185 0.2310 0.9106 0.122 Uiso 0.496(12) 1 calc PR A -2 H27D H 0.5116 0.1227 0.9545 0.122 Uiso 0.496(12) 1 calc PR A -2 C28A C 0.5010(15) 0.298(2) 0.9874(13) 0.080(6) Uani 0.496(12) 1 d PU A -2 H28C H 0.5603 0.2950 1.0280 0.096 Uiso 0.496(12) 1 calc PR A -2 H28D H 0.4893 0.3817 0.9670 0.096 Uiso 0.496(12) 1 calc PR A -2 C29 C 0.2924(3) 0.6168(7) 1.1181(3) 0.0322(16) Uani 1 1 d . . . C30 C 0.2777(4) 0.6127(7) 1.2080(3) 0.0386(17) Uani 1 1 d . . . C31 C 0.2654(4) 0.5822(8) 1.2609(4) 0.052(2) Uani 1 1 d . . . H31 H 0.2524 0.5004 1.2665 0.062 Uiso 1 1 calc R . . C32 C 0.2733(5) 0.6771(9) 1.3048(4) 0.062(2) Uani 1 1 d . . . H32 H 0.2657 0.6593 1.3415 0.074 Uiso 1 1 calc R . . C33 C 0.2918(5) 0.7970(8) 1.2970(4) 0.058(2) Uani 1 1 d . . . H33 H 0.2962 0.8590 1.3282 0.069 Uiso 1 1 calc R . . C34 C 0.3041(4) 0.8283(8) 1.2452(4) 0.050(2) Uani 1 1 d . . . H34 H 0.3172 0.9103 1.2399 0.060 Uiso 1 1 calc R . . C35 C 0.2964(4) 0.7341(7) 1.2010(3) 0.0382(17) Uani 1 1 d . . . C36 C 0.3265(4) 0.8371(7) 1.1169(3) 0.0374(17) Uani 1 1 d . . . H36A H 0.3663 0.8098 1.1049 0.045 Uiso 1 1 calc R . . H36B H 0.3553 0.9000 1.1545 0.045 Uiso 1 1 calc R . . C37 C 0.2508(4) 0.8964(7) 1.0520(4) 0.0384(17) Uani 1 1 d . . . H37 H 0.2151 0.8290 1.0189 0.046 Uiso 1 1 calc R . . C38 C 0.2774(5) 0.9794(7) 1.0140(4) 0.058(2) Uani 1 1 d . . . H38A H 0.3137 1.0462 1.0461 0.070 Uiso 1 1 calc R . . H38B H 0.3105 0.9306 1.0011 0.070 Uiso 1 1 calc R . . C39 C 0.2027(6) 1.0352(9) 0.9481(4) 0.077(3) Uani 1 1 d . . . H39A H 0.1675 0.9687 0.9149 0.093 Uiso 1 1 calc R . . H39B H 0.2222 1.0881 0.9248 0.093 Uiso 1 1 calc R . . C40 C 0.1510(6) 1.1112(9) 0.9660(5) 0.075(3) Uani 1 1 d . . . H40A H 0.1014 1.1452 0.9223 0.091 Uiso 1 1 calc R . . H40B H 0.1849 1.1809 0.9968 0.091 Uiso 1 1 calc R . . C41 C 0.1231(5) 1.0298(8) 1.0035(5) 0.064(2) Uani 1 1 d . . . H41A H 0.0910 1.0799 1.0167 0.077 Uiso 1 1 calc R . . H41B H 0.0858 0.9640 0.9711 0.077 Uiso 1 1 calc R . . C42 C 0.1968(4) 0.9728(7) 1.0682(4) 0.0490(19) Uani 1 1 d . . . H42A H 0.1766 0.9193 1.0908 0.059 Uiso 1 1 calc R . . H42B H 0.2316 1.0388 1.1020 0.059 Uiso 1 1 calc R . . 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 0.0451(5) 0.0375(6) 0.0306(5) 0.0014(5) 0.0224(4) -0.0032(5) O1 0.182(7) 0.109(7) 0.113(6) 0.004(5) 0.114(6) -0.025(6) N1 0.0332(15) 0.0340(19) 0.0297(16) 0.0033(14) 0.0196(13) 0.0013(14) N2 0.040(3) 0.038(4) 0.044(4) 0.001(3) 0.009(3) 0.003(3) N3 0.0332(15) 0.0340(19) 0.0297(16) 0.0033(14) 0.0196(13) 0.0013(14) N4 0.034(3) 0.041(4) 0.027(3) -0.003(3) 0.015(3) -0.005(3) N5 0.0332(15) 0.0340(19) 0.0297(16) 0.0033(14) 0.0196(13) 0.0013(14) N6 0.031(3) 0.047(4) 0.022(3) 0.003(3) 0.015(2) 0.001(3) N7 0.080(4) 0.036(4) 0.021(3) 0.002(3) 0.027(3) 0.002(3) B1 0.0332(15) 0.0340(19) 0.0297(16) 0.0033(14) 0.0196(13) 0.0013(14) C1 0.038(4) 0.036(5) 0.039(4) -0.005(4) 0.017(3) 0.001(4) C2 0.035(4) 0.030(5) 0.065(5) 0.001(4) 0.025(4) 0.002(3) C3 0.045(5) 0.032(5) 0.096(6) 0.005(5) 0.040(5) 0.000(4) C4 0.045(5) 0.038(6) 0.142(10) 0.010(6) 0.050(6) 0.002(4) C5 0.033(5) 0.035(6) 0.167(11) -0.010(7) 0.033(6) -0.009(4) C6 0.048(5) 0.035(6) 0.093(7) 0.009(5) 0.009(5) 0.003(4) C7 0.035(4) 0.022(4) 0.074(6) -0.002(4) 0.014(4) -0.002(3) C8 0.043(4) 0.070(7) 0.056(5) 0.005(5) 0.004(4) 0.003(4) C9 0.139(9) 0.209(15) 0.063(6) 0.039(8) 0.054(7) 0.085(9) C10 0.273(15) 0.279(19) 0.067(8) 0.055(8) 0.079(9) 0.123(13) C11 0.296(18) 0.36(2) 0.089(10) 0.038(10) 0.116(12) 0.137(15) C12 0.36(2) 0.32(2) 0.098(11) -0.010(12) 0.091(14) 0.142(16) C13 0.310(17) 0.206(17) 0.119(11) -0.041(9) 0.101(13) 0.097(13) C14 0.177(10) 0.124(11) 0.111(8) -0.012(7) 0.077(9) 0.053(9) C15 0.033(4) 0.041(5) 0.024(3) -0.003(3) 0.012(3) -0.007(3) C16 0.028(3) 0.035(5) 0.025(3) -0.004(3) 0.010(3) -0.003(3) C17 0.047(4) 0.037(5) 0.031(4) 0.000(3) 0.021(3) -0.002(4) C18 0.053(4) 0.047(6) 0.028(4) 0.010(4) 0.013(3) -0.004(4) C19 0.032(4) 0.040(5) 0.044(4) 0.000(4) 0.010(3) 0.000(3) C20 0.036(4) 0.047(5) 0.036(4) -0.009(4) 0.012(3) -0.006(4) C21 0.033(4) 0.031(4) 0.024(4) -0.002(3) 0.008(3) -0.005(3) C22 0.042(4) 0.046(5) 0.044(4) -0.006(4) 0.029(4) -0.008(4) C23 0.091(16) 0.080(11) 0.071(13) -0.034(10) 0.066(13) -0.034(12) C24 0.073(10) 0.084(11) 0.067(9) -0.013(9) 0.059(8) -0.016(9) C25 0.109(13) 0.063(10) 0.079(11) -0.023(9) 0.067(11) -0.011(10) C26 0.141(18) 0.109(13) 0.071(14) -0.044(11) 0.081(13) -0.042(13) C27 0.174(16) 0.107(12) 0.077(11) -0.020(10) 0.091(12) -0.046(13) C28 0.120(15) 0.092(12) 0.081(12) -0.024(10) 0.082(12) -0.035(11) C23A 0.083(13) 0.089(16) 0.063(11) -0.025(10) 0.057(9) -0.035(13) C24A 0.087(10) 0.124(15) 0.063(10) -0.049(10) 0.050(9) -0.050(11) C25A 0.147(14) 0.125(17) 0.091(13) -0.063(11) 0.089(12) -0.070(13) C26A 0.149(14) 0.097(15) 0.077(12) -0.038(10) 0.085(10) -0.052(12) C27A 0.125(13) 0.115(17) 0.103(15) -0.045(12) 0.087(12) -0.009(12) C28A 0.097(12) 0.094(16) 0.092(13) -0.039(11) 0.079(11) -0.032(10) C29 0.031(3) 0.036(5) 0.033(4) 0.001(3) 0.020(3) -0.003(3) C30 0.042(4) 0.043(5) 0.037(4) 0.006(4) 0.027(3) 0.008(4) C31 0.067(5) 0.051(6) 0.047(5) 0.009(4) 0.038(4) 0.008(4) C32 0.081(6) 0.080(8) 0.047(5) 0.002(5) 0.049(5) 0.004(5) C33 0.081(6) 0.058(6) 0.047(5) -0.007(4) 0.044(5) 0.000(5) C34 0.057(4) 0.052(6) 0.045(4) -0.005(4) 0.032(4) -0.002(4) C35 0.031(3) 0.053(5) 0.027(4) 0.000(4) 0.014(3) 0.008(3) C36 0.046(4) 0.038(5) 0.035(4) -0.007(3) 0.027(4) -0.009(3) C37 0.046(4) 0.029(4) 0.048(4) -0.001(4) 0.031(4) -0.003(3) C38 0.087(6) 0.038(5) 0.070(6) -0.002(4) 0.056(5) -0.009(5) C39 0.113(7) 0.053(6) 0.068(6) 0.034(5) 0.052(6) 0.018(6) C40 0.089(6) 0.038(6) 0.102(7) 0.018(5) 0.056(6) 0.010(5) C41 0.072(5) 0.036(5) 0.091(6) 0.006(5) 0.049(5) 0.016(5) C42 0.057(4) 0.034(5) 0.059(5) -0.005(4) 0.034(4) -0.009(4) _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 N7 1.702(6) . ? Ni1 C29 1.965(6) . ? Ni1 C1 1.969(7) . ? Ni1 C15 1.973(7) . ? O1 N7 1.079(8) . ? N1 C1 1.341(8) . ? N1 C2 1.388(8) . ? N1 B1 1.560(9) . ? N2 C1 1.339(8) . ? N2 C7 1.393(9) . ? N2 C8 1.466(10) . ? N3 C15 1.363(7) . ? N3 C16 1.386(8) . ? N3 B1 1.583(8) . ? N4 C15 1.365(8) . ? N4 C21 1.381(8) . ? N4 C22 1.467(7) . ? N5 C29 1.352(8) . ? N5 C30 1.378(8) . ? N5 B1 1.600(10) . ? N6 C29 1.338(8) . ? N6 C35 1.406(7) . ? N6 C36 1.468(8) . ? C2 C3 1.370(10) . ? C2 C7 1.389(10) . ? C3 C4 1.376(11) . ? C4 C5 1.361(13) . ? C5 C6 1.398(13) . ? C6 C7 1.401(10) . ? C8 C9 1.601(14) . ? C9 C14 1.456(14) . ? C9 C10 1.579(18) . ? C10 C11 1.513(16) . ? C11 C12 1.436(16) . ? C12 C13 1.49(2) . ? C13 C14 1.526(16) . ? C16 C17 1.388(9) . ? C16 C21 1.404(8) . ? C17 C18 1.386(9) . ? C18 C19 1.404(9) . ? C19 C20 1.380(9) . ? C20 C21 1.382(9) . ? C22 C23 1.50(5) . ? C22 C23A 1.54(6) . ? C23 C24 1.38(6) . ? C23 C28 1.61(6) . ? C24 C25 1.54(2) . ? C25 C26 1.54(3) . ? C26 C27 1.52(4) . ? C27 C28 1.54(3) . ? C23A C24A 1.46(5) . ? C23A C28A 1.48(5) . ? C24A C25A 1.53(3) . ? C25A C26A 1.57(3) . ? C26A C27A 1.44(4) . ? C27A C28A 1.55(3) . ? C30 C31 1.396(9) . ? C30 C35 1.398(10) . ? C31 C32 1.387(11) . ? C32 C33 1.386(11) . ? C33 C34 1.374(9) . ? C34 C35 1.386(10) . ? C36 C37 1.524(9) . ? C37 C38 1.525(9) . ? C37 C42 1.528(9) . ? C38 C39 1.510(10) . ? C39 C40 1.512(11) . ? C40 C41 1.523(11) . ? C41 C42 1.496(10) . ? 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 N7 Ni1 C29 122.8(3) . . ? N7 Ni1 C1 123.6(3) . . ? C29 Ni1 C1 89.8(3) . . ? N7 Ni1 C15 128.1(3) . . ? C29 Ni1 C15 91.3(3) . . ? C1 Ni1 C15 90.5(3) . . ? C1 N1 C2 109.3(5) . . ? C1 N1 B1 121.2(5) . . ? C2 N1 B1 129.4(5) . . ? C1 N2 C7 109.9(6) . . ? C1 N2 C8 125.6(6) . . ? C7 N2 C8 124.1(6) . . ? C15 N3 C16 110.2(5) . . ? C15 N3 B1 119.4(5) . . ? C16 N3 B1 130.3(5) . . ? C15 N4 C21 110.6(5) . . ? C15 N4 C22 122.9(6) . . ? C21 N4 C22 126.6(5) . . ? C29 N5 C30 109.3(6) . . ? C29 N5 B1 120.0(5) . . ? C30 N5 B1 130.4(5) . . ? C29 N6 C35 110.0(6) . . ? C29 N6 C36 124.3(5) . . ? C35 N6 C36 125.6(6) . . ? O1 N7 Ni1 168.2(7) . . ? N1 B1 N3 106.9(5) . . ? N1 B1 N5 104.4(5) . . ? N3 B1 N5 105.0(5) . . ? N2 C1 N1 108.2(6) . . ? N2 C1 Ni1 134.0(5) . . ? N1 C1 Ni1 117.7(4) . . ? C3 C2 N1 132.7(7) . . ? C3 C2 C7 120.3(7) . . ? N1 C2 C7 106.9(6) . . ? C2 C3 C4 119.7(9) . . ? C5 C4 C3 119.4(9) . . ? C4 C5 C6 123.8(8) . . ? C5 C6 C7 115.1(9) . . ? C2 C7 N2 105.8(6) . . ? C2 C7 C6 121.6(8) . . ? N2 C7 C6 132.6(8) . . ? N2 C8 C9 113.3(8) . . ? C14 C9 C10 105.0(11) . . ? C14 C9 C8 115.2(9) . . ? C10 C9 C8 107.7(11) . . ? C11 C10 C9 111.3(14) . . ? C12 C11 C10 112.6(15) . . ? C11 C12 C13 115(2) . . ? C12 C13 C14 108.2(15) . . ? C9 C14 C13 113.8(12) . . ? N3 C15 N4 106.4(6) . . ? N3 C15 Ni1 118.1(4) . . ? N4 C15 Ni1 135.3(5) . . ? N3 C16 C17 132.2(6) . . ? N3 C16 C21 106.5(5) . . ? C17 C16 C21 121.3(6) . . ? C18 C17 C16 116.3(6) . . ? C17 C18 C19 122.5(7) . . ? C20 C19 C18 120.6(7) . . ? C19 C20 C21 117.5(6) . . ? N4 C21 C20 132.0(6) . . ? N4 C21 C16 106.3(6) . . ? C20 C21 C16 121.7(6) . . ? N4 C22 C23 112(2) . . ? N4 C22 C23A 117(2) . . ? C24 C23 C22 120(4) . . ? C24 C23 C28 112(3) . . ? C22 C23 C28 103(3) . . ? C23 C24 C25 115(2) . . ? C26 C25 C24 107.3(17) . . ? C27 C26 C25 107(2) . . ? C26 C27 C28 112(2) . . ? C27 C28 C23 109(2) . . ? C24A C23A C28A 116(4) . . ? C24A C23A C22 115(3) . . ? C28A C23A C22 114(4) . . ? C23A C24A C25A 113(3) . . ? C24A C25A C26A 109.9(18) . . ? C27A C26A C25A 111(2) . . ? C26A C27A C28A 114(2) . . ? C23A C28A C27A 112(3) . . ? N6 C29 N5 108.1(5) . . ? N6 C29 Ni1 133.9(5) . . ? N5 C29 Ni1 118.0(5) . . ? N5 C30 C31 132.3(7) . . ? N5 C30 C35 107.6(5) . . ? C31 C30 C35 120.1(7) . . ? C32 C31 C30 116.7(8) . . ? C33 C32 C31 122.3(7) . . ? C34 C33 C32 121.6(8) . . ? C33 C34 C35 116.6(8) . . ? C34 C35 C30 122.7(6) . . ? C34 C35 N6 132.3(7) . . ? C30 C35 N6 105.0(6) . . ? N6 C36 C37 114.0(5) . . ? C36 C37 C38 111.3(5) . . ? C36 C37 C42 113.7(5) . . ? C38 C37 C42 108.0(6) . . ? C39 C38 C37 111.7(6) . . ? C38 C39 C40 110.6(7) . . ? C39 C40 C41 109.1(7) . . ? C42 C41 C40 111.1(7) . . ? C41 C42 C37 112.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C29 Ni1 N7 O1 -74(3) . . . . ? C1 Ni1 N7 O1 41(3) . . . . ? C15 Ni1 N7 O1 163(3) . . . . ? C1 N1 B1 N3 -54.6(8) . . . . ? C2 N1 B1 N3 129.7(6) . . . . ? C1 N1 B1 N5 56.3(7) . . . . ? C2 N1 B1 N5 -119.4(7) . . . . ? C15 N3 B1 N1 53.2(7) . . . . ? C16 N3 B1 N1 -129.9(6) . . . . ? C15 N3 B1 N5 -57.3(7) . . . . ? C16 N3 B1 N5 119.6(7) . . . . ? C29 N5 B1 N1 -54.9(6) . . . . ? C30 N5 B1 N1 118.4(6) . . . . ? C29 N5 B1 N3 57.4(7) . . . . ? C30 N5 B1 N3 -129.3(6) . . . . ? C7 N2 C1 N1 1.0(8) . . . . ? C8 N2 C1 N1 173.6(7) . . . . ? C7 N2 C1 Ni1 -174.4(6) . . . . ? C8 N2 C1 Ni1 -1.8(12) . . . . ? C2 N1 C1 N2 -0.5(8) . . . . ? B1 N1 C1 N2 -177.0(6) . . . . ? C2 N1 C1 Ni1 175.8(5) . . . . ? B1 N1 C1 Ni1 -0.7(8) . . . . ? N7 Ni1 C1 N2 -1.2(9) . . . . ? C29 Ni1 C1 N2 129.1(7) . . . . ? C15 Ni1 C1 N2 -139.6(7) . . . . ? N7 Ni1 C1 N1 -176.3(5) . . . . ? C29 Ni1 C1 N1 -45.9(6) . . . . ? C15 Ni1 C1 N1 45.4(5) . . . . ? C1 N1 C2 C3 -175.6(8) . . . . ? B1 N1 C2 C3 0.5(13) . . . . ? C1 N1 C2 C7 -0.3(8) . . . . ? B1 N1 C2 C7 175.9(6) . . . . ? N1 C2 C3 C4 177.5(8) . . . . ? C7 C2 C3 C4 2.7(11) . . . . ? C2 C3 C4 C5 -0.6(13) . . . . ? C3 C4 C5 C6 -0.7(15) . . . . ? C4 C5 C6 C7 -0.2(14) . . . . ? C3 C2 C7 N2 176.9(7) . . . . ? N1 C2 C7 N2 0.9(8) . . . . ? C3 C2 C7 C6 -3.7(12) . . . . ? N1 C2 C7 C6 -179.7(7) . . . . ? C1 N2 C7 C2 -1.2(8) . . . . ? C8 N2 C7 C2 -173.9(7) . . . . ? C1 N2 C7 C6 179.5(8) . . . . ? C8 N2 C7 C6 6.8(14) . . . . ? C5 C6 C7 C2 2.3(12) . . . . ? C5 C6 C7 N2 -178.4(8) . . . . ? C1 N2 C8 C9 100.3(10) . . . . ? C7 N2 C8 C9 -88.1(10) . . . . ? N2 C8 C9 C14 -58.5(15) . . . . ? N2 C8 C9 C10 -175.3(10) . . . . ? C14 C9 C10 C11 57.4(19) . . . . ? C8 C9 C10 C11 -179.4(14) . . . . ? C9 C10 C11 C12 -53(3) . . . . ? C10 C11 C12 C13 51(3) . . . . ? C11 C12 C13 C14 -51(3) . . . . ? C10 C9 C14 C13 -62.1(19) . . . . ? C8 C9 C14 C13 179.6(13) . . . . ? C12 C13 C14 C9 60(2) . . . . ? C16 N3 C15 N4 0.3(7) . . . . ? B1 N3 C15 N4 177.8(5) . . . . ? C16 N3 C15 Ni1 -175.3(4) . . . . ? B1 N3 C15 Ni1 2.1(7) . . . . ? C21 N4 C15 N3 0.3(7) . . . . ? C22 N4 C15 N3 -179.0(5) . . . . ? C21 N4 C15 Ni1 174.8(5) . . . . ? C22 N4 C15 Ni1 -4.6(9) . . . . ? N7 Ni1 C15 N3 178.9(4) . . . . ? C29 Ni1 C15 N3 43.9(5) . . . . ? C1 Ni1 C15 N3 -45.8(5) . . . . ? N7 Ni1 C15 N4 4.9(8) . . . . ? C29 Ni1 C15 N4 -130.1(6) . . . . ? C1 Ni1 C15 N4 140.1(6) . . . . ? C15 N3 C16 C17 178.1(7) . . . . ? B1 N3 C16 C17 1.0(11) . . . . ? C15 N3 C16 C21 -0.7(7) . . . . ? B1 N3 C16 C21 -177.9(6) . . . . ? N3 C16 C17 C18 -179.0(7) . . . . ? C21 C16 C17 C18 -0.3(9) . . . . ? C16 C17 C18 C19 -0.9(10) . . . . ? C17 C18 C19 C20 1.2(11) . . . . ? C18 C19 C20 C21 -0.4(10) . . . . ? C15 N4 C21 C20 -180.0(7) . . . . ? C22 N4 C21 C20 -0.6(11) . . . . ? C15 N4 C21 C16 -0.8(7) . . . . ? C22 N4 C21 C16 178.6(5) . . . . ? C19 C20 C21 N4 178.3(7) . . . . ? C19 C20 C21 C16 -0.8(10) . . . . ? N3 C16 C21 N4 0.9(7) . . . . ? C17 C16 C21 N4 -178.1(6) . . . . ? N3 C16 C21 C20 -179.8(6) . . . . ? C17 C16 C21 C20 1.2(10) . . . . ? C15 N4 C22 C23 -93(2) . . . . ? C21 N4 C22 C23 88(2) . . . . ? C15 N4 C22 C23A -106(2) . . . . ? C21 N4 C22 C23A 74(2) . . . . ? N4 C22 C23 C24 -72(3) . . . . ? C23A C22 C23 C24 44(17) . . . . ? N4 C22 C23 C28 163.0(16) . . . . ? C23A C22 C23 C28 -81(19) . . . . ? C22 C23 C24 C25 -176(3) . . . . ? C28 C23 C24 C25 -55(4) . . . . ? C23 C24 C25 C26 62(3) . . . . ? C24 C25 C26 C27 -62(3) . . . . ? C25 C26 C27 C28 62(3) . . . . ? C26 C27 C28 C23 -54(3) . . . . ? C24 C23 C28 C27 50(4) . . . . ? C22 C23 C28 C27 180(2) . . . . ? N4 C22 C23A C24A 52(5) . . . . ? C23 C22 C23A C24A -18(16) . . . . ? N4 C22 C23A C28A -172(2) . . . . ? C23 C22 C23A C28A 119(22) . . . . ? C28A C23A C24A C25A 50(5) . . . . ? C22 C23A C24A C25A -174(3) . . . . ? C23A C24A C25A C26A -53(4) . . . . ? C24A C25A C26A C27A 56(3) . . . . ? C25A C26A C27A C28A -55(4) . . . . ? C24A C23A C28A C27A -46(5) . . . . ? C22 C23A C28A C27A 178(3) . . . . ? C26A C27A C28A C23A 50(4) . . . . ? C35 N6 C29 N5 -1.1(7) . . . . ? C36 N6 C29 N5 179.1(5) . . . . ? C35 N6 C29 Ni1 175.3(5) . . . . ? C36 N6 C29 Ni1 -4.5(9) . . . . ? C30 N5 C29 N6 1.0(7) . . . . ? B1 N5 C29 N6 175.6(5) . . . . ? C30 N5 C29 Ni1 -176.1(4) . . . . ? B1 N5 C29 Ni1 -1.5(7) . . . . ? N7 Ni1 C29 N6 1.3(7) . . . . ? C1 Ni1 C29 N6 -129.6(6) . . . . ? C15 Ni1 C29 N6 139.8(6) . . . . ? N7 Ni1 C29 N5 177.4(4) . . . . ? C1 Ni1 C29 N5 46.5(5) . . . . ? C15 Ni1 C29 N5 -44.0(5) . . . . ? C29 N5 C30 C31 -179.8(7) . . . . ? B1 N5 C30 C31 6.4(11) . . . . ? C29 N5 C30 C35 -0.5(7) . . . . ? B1 N5 C30 C35 -174.3(5) . . . . ? N5 C30 C31 C32 178.9(7) . . . . ? C35 C30 C31 C32 -0.3(10) . . . . ? C30 C31 C32 C33 0.4(12) . . . . ? C31 C32 C33 C34 -0.5(13) . . . . ? C32 C33 C34 C35 0.4(11) . . . . ? C33 C34 C35 C30 -0.4(10) . . . . ? C33 C34 C35 N6 -178.9(6) . . . . ? N5 C30 C35 C34 -179.0(6) . . . . ? C31 C30 C35 C34 0.4(10) . . . . ? N5 C30 C35 N6 -0.2(7) . . . . ? C31 C30 C35 N6 179.2(6) . . . . ? C29 N6 C35 C34 179.5(7) . . . . ? C36 N6 C35 C34 -0.7(10) . . . . ? C29 N6 C35 C30 0.8(7) . . . . ? C36 N6 C35 C30 -179.4(5) . . . . ? C29 N6 C36 C37 81.4(7) . . . . ? C35 N6 C36 C37 -98.4(7) . . . . ? N6 C36 C37 C38 -163.6(6) . . . . ? N6 C36 C37 C42 74.2(8) . . . . ? C36 C37 C38 C39 178.0(6) . . . . ? C42 C37 C38 C39 -56.5(8) . . . . ? C37 C38 C39 C40 59.4(10) . . . . ? C38 C39 C40 C41 -57.8(10) . . . . ? C39 C40 C41 C42 57.1(10) . . . . ? C40 C41 C42 C37 -57.7(9) . . . . ? C36 C37 C42 C41 180.0(6) . . . . ? C38 C37 C42 C41 56.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.089 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.091 _iucr_refine_instruction_details ; TITL jsNMSU030712 in P21/c CELL 0.71073 19.2410 10.8470 22.8850 90.000 123.991 90.000 ZERR 4 0.0040 0.0030 0.0050 0.000 0.014 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H B N Ni O UNIT 168 208 4 28 4 4 L.S. 10 TEMP -100.150 SIZE 0.111 0.170 0.231 FMAP 2 PLAN 10 DFIX 1.04 B1 H1 SADI c11 c12 c11 c10 EADP B1 N1 N3 N5 SIMU c9 c10 c11 c12 c13 c14 DELU c9 c10 c11 c12 c13 c14 SIMU c23 c24 c25 c26 c27 c28 c23a c24a c25a c26a c27a c28a DELU c23 c24 c25 c26 c27 c28 c23a c24a c25a c26a c27a c28a OMIT -1 1 1 OMIT -1 1 2 OMIT 2 0 0 OMIT 0 0 2 OMIT -3 0 2 OMIT 0 1 1 OMIT -2 1 1 OMIT -2 0 2 OMIT -1 0 2 OMIT 1 0 0 OMIT 1 0 2 OMIT -2 1 2 OMIT 0 1 2 OMIT 2 1 0 OMIT -3 1 1 OMIT 1 1 0 BOND CONF ACTA WGHT 0.110800 FVAR 0.11310 0.50353 NI1 5 0.286859 0.543609 1.037071 11.00000 0.04513 0.03751 = 0.03057 0.00138 0.02244 -0.00319 O1 6 0.298877 0.687193 0.943177 11.00000 0.18218 0.10864 = 0.11332 0.00384 0.11352 -0.02460 N1 4 0.174423 0.407743 1.056582 11.00000 0.03323 0.03401 = 0.02974 0.00335 0.01963 0.00134 N2 4 0.104029 0.460711 0.946316 11.00000 0.04043 0.03783 = 0.04431 0.00059 0.00854 0.00340 N3 4 0.326541 0.345055 1.134458 11.00000 0.03323 0.03401 = 0.02974 0.00335 0.01963 0.00134 N4 4 0.416556 0.331804 1.105110 11.00000 0.03383 0.04107 = 0.02705 -0.00309 0.01524 -0.00526 N5 4 0.276152 0.543281 1.156789 11.00000 0.03323 0.03401 = 0.02974 0.00335 0.01963 0.00134 N6 4 0.305689 0.731195 1.144282 11.00000 0.03134 0.04664 = 0.02184 0.00295 0.01487 0.00135 N7 4 0.301984 0.627008 0.982096 11.00000 0.07992 0.03643 = 0.02097 0.00229 0.02693 0.00197 B1 3 0.251050 0.402070 1.134849 11.00000 0.03323 0.03401 = 0.02974 0.00335 0.01963 0.00134 H1 2 0.241652 0.348308 1.165488 11.00000 -1.20000 C1 1 0.179600 0.465061 1.007214 11.00000 0.03795 0.03560 = 0.03938 -0.00509 0.01676 0.00085 C2 1 0.093042 0.366110 1.026744 11.00000 0.03522 0.02957 = 0.06486 0.00067 0.02547 0.00196 C3 1 0.053981 0.309507 1.054440 11.00000 0.04544 0.03212 = 0.09626 0.00473 0.03993 0.00007 AFIX 43 H3 2 0.084829 0.289107 1.103106 11.00000 -1.20000 AFIX 0 C4 1 -0.030117 0.282319 1.011488 11.00000 0.04506 0.03762 = 0.14206 0.01001 0.04986 0.00197 AFIX 43 H4 2 -0.057604 0.242424 1.030166 11.00000 -1.20000 AFIX 0 C5 1 -0.073585 0.313087 0.941995 11.00000 0.03295 0.03469 = 0.16655 -0.00966 0.03335 -0.00913 AFIX 43 H5 2 -0.131437 0.292631 0.913116 11.00000 -1.20000 AFIX 0 C6 1 -0.038014 0.373040 0.910675 11.00000 0.04808 0.03478 = 0.09255 0.00922 0.00933 0.00291 AFIX 43 H6 2 -0.069470 0.393523 0.862005 11.00000 -1.20000 AFIX 0 C7 1 0.047413 0.400732 0.956283 11.00000 0.03494 0.02181 = 0.07423 -0.00199 0.01355 -0.00237 C8 1 0.080588 0.523080 0.880889 11.00000 0.04347 0.07021 = 0.05643 0.00536 0.00432 0.00275 AFIX 23 H8A 2 0.120124 0.591825 0.892392 11.00000 -1.20000 H8B 2 0.023866 0.558823 0.858801 11.00000 -1.20000 AFIX 0 C9 1 0.080895 0.433653 0.825374 11.00000 0.13906 0.20856 = 0.06323 0.03851 0.05358 0.08519 AFIX 13 H9 2 0.036136 0.369818 0.808851 11.00000 -1.20000 AFIX 0 C10 1 0.062217 0.514887 0.760817 11.00000 0.27340 0.27897 = 0.06677 0.05456 0.07859 0.12264 AFIX 23 H10A 2 0.007514 0.556755 0.739942 11.00000 -1.20000 H10B 2 0.105979 0.579079 0.777507 11.00000 -1.20000 AFIX 0 C11 1 0.060387 0.437046 0.705133 11.00000 0.29637 0.36124 = 0.08916 0.03847 0.11565 0.13653 AFIX 23 H11A 2 0.010842 0.382152 0.683119 11.00000 -1.20000 H11B 2 0.054356 0.491720 0.667916 11.00000 -1.20000 AFIX 0 C12 1 0.134577 0.363430 0.733183 11.00000 0.36008 0.31722 = 0.09849 -0.00968 0.09138 0.14242 AFIX 23 H12A 2 0.181908 0.418661 0.745559 11.00000 -1.20000 H12B 2 0.126203 0.306966 0.695764 11.00000 -1.20000 AFIX 0 C13 1 0.158444 0.288626 0.796537 11.00000 0.31011 0.20597 = 0.11948 -0.04113 0.10124 0.09659 AFIX 23 H13A 2 0.214203 0.250676 0.816664 11.00000 -1.20000 H13B 2 0.117057 0.221912 0.783340 11.00000 -1.20000 AFIX 0 C14 1 0.160649 0.373783 0.850604 11.00000 0.17736 0.12398 = 0.11052 -0.01181 0.07722 0.05343 AFIX 23 H14A 2 0.177674 0.325296 0.893282 11.00000 -1.20000 H14B 2 0.203758 0.437985 0.864362 11.00000 -1.20000 AFIX 0 C15 1 0.348585 0.396237 1.092652 11.00000 0.03286 0.04140 = 0.02356 -0.00292 0.01169 -0.00694 C16 1 0.380334 0.249040 1.173512 11.00000 0.02845 0.03510 = 0.02498 -0.00438 0.00965 -0.00346 C17 1 0.385332 0.171590 1.223991 11.00000 0.04730 0.03667 = 0.03091 0.00050 0.02103 -0.00230 AFIX 43 H17 2 0.346991 0.177468 1.237610 11.00000 -1.20000 AFIX 0 C18 1 0.449315 0.085194 1.253449 11.00000 0.05297 0.04740 = 0.02814 0.00955 0.01325 -0.00383 AFIX 43 H18 2 0.455185 0.031303 1.288674 11.00000 -1.20000 AFIX 0 C19 1 0.505781 0.074245 1.233247 11.00000 0.03151 0.04002 = 0.04419 0.00038 0.01027 0.00042 AFIX 43 H19 2 0.548044 0.012585 1.254178 11.00000 -1.20000 AFIX 0 C20 1 0.500457 0.152268 1.183238 11.00000 0.03584 0.04725 = 0.03647 -0.00874 0.01229 -0.00563 AFIX 43 H20 2 0.538574 0.145952 1.169402 11.00000 -1.20000 AFIX 0 C21 1 0.437609 0.239888 1.154067 11.00000 0.03296 0.03113 = 0.02414 -0.00200 0.00791 -0.00489 C22 1 0.459671 0.360818 1.070447 11.00000 0.04243 0.04647 = 0.04426 -0.00620 0.02919 -0.00825 AFIX 23 H22A 2 0.520332 0.344165 1.103533 11.00000 -1.20000 H22B 2 0.452791 0.449662 1.058544 11.00000 -1.20000 AFIX 0 PART -1 C23 1 0.426503 0.286827 1.004639 21.00000 0.09113 0.07960 = 0.07105 -0.03402 0.06649 -0.03437 AFIX 13 H23 2 0.364080 0.295175 0.975774 21.00000 -1.20000 AFIX 0 C24 1 0.444429 0.162212 1.009317 21.00000 0.07321 0.08421 = 0.06654 -0.01315 0.05929 -0.01639 AFIX 23 H24A 2 0.420047 0.120235 1.032304 21.00000 -1.20000 H24B 2 0.505989 0.151347 1.040069 21.00000 -1.20000 AFIX 0 C25 1 0.411559 0.098467 0.938144 21.00000 0.10912 0.06341 = 0.07870 -0.02312 0.06687 -0.01109 AFIX 23 H25A 2 0.424531 0.009244 0.945337 21.00000 -1.20000 H25B 2 0.350047 0.108615 0.906140 21.00000 -1.20000 AFIX 0 C26 1 0.455380 0.159668 0.906247 21.00000 0.14069 0.10892 = 0.07082 -0.04396 0.08062 -0.04160 AFIX 23 H26A 2 0.516961 0.151298 0.938768 21.00000 -1.20000 H26B 2 0.437419 0.119990 0.860913 21.00000 -1.20000 AFIX 0 C27 1 0.430663 0.294670 0.894774 21.00000 0.17418 0.10743 = 0.07659 -0.02039 0.09111 -0.04578 AFIX 23 H27A 2 0.368938 0.301368 0.862614 21.00000 -1.20000 H27B 2 0.455538 0.335815 0.871964 21.00000 -1.20000 AFIX 0 C28 1 0.459997 0.360756 0.964244 21.00000 0.12010 0.09166 = 0.08137 -0.02387 0.08172 -0.03496 AFIX 23 H28A 2 0.438041 0.446115 0.954465 21.00000 -1.20000 H28B 2 0.521987 0.364637 0.994157 21.00000 -1.20000 AFIX 0 PART -2 C23A 1 0.446080 0.272391 1.012391 -21.00000 0.08318 0.08890 = 0.06320 -0.02488 0.05660 -0.03515 AFIX 13 H23A 2 0.467420 0.191769 1.037516 -21.00000 -1.20000 AFIX 0 C24A 1 0.358571 0.246368 0.957351 -21.00000 0.08742 0.12374 = 0.06272 -0.04921 0.04995 -0.04965 AFIX 23 H24C 2 0.331190 0.323449 0.931356 -21.00000 -1.20000 H24D 2 0.329613 0.218346 0.979622 -21.00000 -1.20000 AFIX 0 C25A 1 0.348262 0.148425 0.905156 -21.00000 0.14717 0.12533 = 0.09127 -0.06272 0.08897 -0.07001 AFIX 23 H25C 2 0.288387 0.141203 0.866168 -21.00000 -1.20000 H25D 2 0.367236 0.067534 0.929122 -21.00000 -1.20000 AFIX 0 C26A 1 0.401087 0.184506 0.874874 -21.00000 0.14921 0.09723 = 0.07680 -0.03750 0.08460 -0.05225 AFIX 23 H26C 2 0.396911 0.118334 0.843259 -21.00000 -1.20000 H26D 2 0.378346 0.261195 0.846897 -21.00000 -1.20000 AFIX 0 C27A 1 0.487441 0.202784 0.931028 -21.00000 0.12521 0.11479 = 0.10330 -0.04528 0.08715 -0.00945 AFIX 23 H27C 2 0.518457 0.230990 0.910604 -21.00000 -1.20000 H27D 2 0.511586 0.122675 0.954476 -21.00000 -1.20000 AFIX 0 C28A 1 0.501014 0.297717 0.987413 -21.00000 0.09661 0.09408 = 0.09172 -0.03894 0.07879 -0.03207 AFIX 23 H28C 2 0.560312 0.295032 1.027977 -21.00000 -1.20000 H28D 2 0.489348 0.381667 0.967031 -21.00000 -1.20000 AFIX 0 PART 0 C29 1 0.292425 0.616848 1.118129 11.00000 0.03090 0.03635 = 0.03319 0.00068 0.02034 -0.00326 C30 1 0.277710 0.612667 1.207965 11.00000 0.04249 0.04347 = 0.03740 0.00614 0.02704 0.00824 C31 1 0.265434 0.582151 1.260853 11.00000 0.06679 0.05086 = 0.04728 0.00911 0.03827 0.00819 AFIX 43 H31 2 0.252356 0.500392 1.266471 11.00000 -1.20000 AFIX 0 C32 1 0.273272 0.677069 1.304781 11.00000 0.08114 0.07983 = 0.04694 0.00170 0.04936 0.00376 AFIX 43 H32 2 0.265658 0.659306 1.341504 11.00000 -1.20000 AFIX 0 C33 1 0.291830 0.796967 1.296966 11.00000 0.08079 0.05839 = 0.04661 -0.00674 0.04359 -0.00041 AFIX 43 H33 2 0.296162 0.858974 1.328164 11.00000 -1.20000 AFIX 0 C34 1 0.304111 0.828290 1.245180 11.00000 0.05702 0.05236 = 0.04453 -0.00513 0.03153 -0.00192 AFIX 43 H34 2 0.317193 0.910282 1.239937 11.00000 -1.20000 AFIX 0 C35 1 0.296428 0.734089 1.201001 11.00000 0.03098 0.05287 = 0.02729 0.00039 0.01412 0.00812 C36 1 0.326539 0.837100 1.116898 11.00000 0.04647 0.03796 = 0.03455 -0.00698 0.02678 -0.00863 AFIX 23 H36A 2 0.366254 0.809828 1.104942 11.00000 -1.20000 H36B 2 0.355322 0.899992 1.154515 11.00000 -1.20000 AFIX 0 C37 1 0.250841 0.896448 1.051994 11.00000 0.04590 0.02946 = 0.04785 -0.00100 0.03117 -0.00336 AFIX 13 H37 2 0.215083 0.828992 1.018884 11.00000 -1.20000 AFIX 0 C38 1 0.277369 0.979384 1.013953 11.00000 0.08716 0.03797 = 0.06966 -0.00174 0.05648 -0.00851 AFIX 23 H38A 2 0.313653 1.046235 1.046095 11.00000 -1.20000 H38B 2 0.310478 0.930628 1.001149 11.00000 -1.20000 AFIX 0 C39 1 0.202656 1.035211 0.948121 11.00000 0.11329 0.05313 = 0.06758 0.03405 0.05182 0.01764 AFIX 23 H39A 2 0.167506 0.968726 0.914926 11.00000 -1.20000 H39B 2 0.222157 1.088117 0.924764 11.00000 -1.20000 AFIX 0 C40 1 0.151043 1.111195 0.965961 11.00000 0.08896 0.03845 = 0.10223 0.01813 0.05552 0.01014 AFIX 23 H40A 2 0.101381 1.145203 0.922294 11.00000 -1.20000 H40B 2 0.184870 1.180931 0.996789 11.00000 -1.20000 AFIX 0 C41 1 0.123147 1.029800 1.003487 11.00000 0.07160 0.03595 = 0.09064 0.00635 0.04895 0.01641 AFIX 23 H41A 2 0.090978 1.079879 1.016741 11.00000 -1.20000 H41B 2 0.085828 0.963964 0.971084 11.00000 -1.20000 AFIX 0 C42 1 0.196812 0.972806 1.068176 11.00000 0.05709 0.03370 = 0.05900 -0.00535 0.03413 -0.00892 AFIX 23 H42A 2 0.176596 0.919271 1.090751 11.00000 -1.20000 H42B 2 0.231585 1.038775 1.102018 11.00000 -1.20000 HKLF 4 1 0.0000 1.0000 0.0000 -1.0000 0.0000 0.0000 0.0000 -1.0000 1.0000 REM triclinic in P21/c REM R1 = 0.0876 for 3260 Fo > 4sig(Fo) and 0.2134 for all 7776 data REM 509 parameters refined using 224 restraints END WGHT 0.1108 0.0000 REM Highest difference peak 1.089, deepest hole -0.392, 1-sigma level 0.091 Q1 1 0.1026 0.5397 0.7306 11.00000 0.05 0.56 Q2 1 0.0432 0.3236 0.7312 11.00000 0.05 0.55 Q3 1 0.3516 0.6499 0.9913 11.00000 0.05 0.46 Q4 1 0.3630 0.5457 1.0745 11.00000 0.05 0.39 Q5 1 0.2188 0.5444 1.0166 11.00000 0.05 0.38 Q6 1 -0.0093 0.4458 0.7543 11.00000 0.05 0.38 Q7 1 0.5321 0.3669 1.1358 11.00000 0.05 0.37 Q8 1 0.1699 0.4459 0.7854 11.00000 0.05 0.34 Q9 1 0.5682 0.3009 1.1788 11.00000 0.05 0.33 Q10 1 0.0534 0.3653 0.7014 11.00000 0.05 0.32 ; data_mar15p1 _vrf_RINTA01_mar15p1 ; RESPONSE: Crystal was very weakly diffracting. Several others were tested and this proved to be the best one. ; _vrf_PLAT020_mar15p1 ; RESPONSE: See previous response. ; _vrf_PLAT213_mar15p1 ; RESPONSE: Atoms C9 and C8 are part of a cyclohexyl ring with large thermal motion. Attempts to model the ring as disordered did not improve the structure. The cause of the error with N16 is not immediately apparent, but it is correctly identified as nitrogen. ; _vrf_RFACR01_mar15p1 ; RESPONSE: Crystal was very weakly diffracting. Several others were tested and this proved to be the best one. ; _vrf_PLAT026_mar15p1 ; RESPONSE: See previous response ; _vrf_PLAT084_mar15p1 ; RESPONSE: No twin laws were detected. Likely due to overall poor crystal quality. ; _vrf_PLAT220_mar15p1 ; RESPONSE: See previous response ; _vrf_PLAT241_mar15p1 ; RESPONSE: See previous response ; _vrf_PLAT341_mar15p1 ; RESPONSE: Crystal was very weakly diffracting. Several others were tested and this proved to be the best one. ; _vrf_PLAT710_mar15p1 ; RESPONSE: Linear torsion angles involving N7, N14 and N21 are related to the terminal nitrosyl ligand and are correct. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C112 H160 B3 N21 Ni3 O4' _chemical_formula_weight 2073.17 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' 'B' 'B' 0.0013 0.0007 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 26.345(6) _cell_length_b 37.425(7) _cell_length_c 11.4322(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.762(13) _cell_angle_gamma 90.00 _cell_volume 11109(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 18.28 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4440 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8076 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 111284 _diffrn_reflns_av_R_equivalents 0.4876 _diffrn_reflns_av_sigmaI/netI 0.4313 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 26.37 _reflns_number_total 22708 _reflns_number_gt 6775 _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. ; _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^)+(0.1656P)^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 22708 _refine_ls_number_parameters 1342 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.3409 _refine_ls_R_factor_gt 0.1126 _refine_ls_wR_factor_ref 0.3866 _refine_ls_wR_factor_gt 0.2475 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.954 _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 Ni1 Ni 0.23299(6) 0.98669(4) 0.36063(13) 0.0266(4) Uani 1 1 d . . . Ni2 Ni 0.21387(6) 0.83266(4) 0.83752(12) 0.0233(4) Uani 1 1 d . . . Ni3 Ni 0.25365(6) 1.15886(4) 0.86829(14) 0.0335(4) Uani 1 1 d . . . B1 B 0.1620(6) 0.9719(3) 0.1165(11) 0.028(3) Uani 1 1 d . . . B2 B 0.1468(5) 0.8537(3) 0.5957(11) 0.024(3) Uani 1 1 d . . . B3 B 0.1877(6) 1.1845(4) 0.6313(12) 0.030(3) Uani 1 1 d . . . N1 N 0.1969(4) 0.9388(2) 0.1632(8) 0.025(2) Uani 1 1 d . . . N2 N 0.2500(4) 0.9085(3) 0.2913(9) 0.033(3) Uani 1 1 d . . . N3 N 0.1997(4) 1.0042(2) 0.1166(8) 0.028(2) Uani 1 1 d . . . N4 N 0.2588(4) 1.0423(2) 0.1854(8) 0.029(2) Uani 1 1 d . . . N5 N 0.1313(4) 0.9790(2) 0.2234(8) 0.028(2) Uani 1 1 d . . . N6 N 0.1216(4) 0.9884(2) 0.4061(8) 0.024(2) Uani 1 1 d . . . N7 N 0.2743(4) 0.9932(3) 0.4835(9) 0.035(3) Uani 1 1 d . . . N8 N 0.1784(3) 0.8180(2) 0.5921(7) 0.024(2) Uani 1 1 d . . . N9 N 0.2282(4) 0.7735(2) 0.6586(8) 0.027(2) Uani 1 1 d . . . N10 N 0.1897(3) 0.8824(2) 0.6428(7) 0.021(2) Uani 1 1 d . . . N11 N 0.2472(3) 0.9076(2) 0.7750(7) 0.021(2) Uani 1 1 d . C . N12 N 0.1150(4) 0.8503(2) 0.6998(7) 0.023(2) Uani 1 1 d . . . N13 N 0.1027(4) 0.8420(2) 0.8794(8) 0.024(2) Uani 1 1 d . . . N14 N 0.2525(4) 0.8238(2) 0.9615(8) 0.023(2) Uani 1 1 d . . . N15 N 0.1554(4) 1.1821(2) 0.7354(9) 0.032(3) Uani 1 1 d . . . N16 N 0.1451(4) 1.1749(2) 0.9168(8) 0.026(2) Uani 1 1 d . . . N17 N 0.2132(4) 1.1466(2) 0.6245(8) 0.025(2) Uani 1 1 d . . . N18 N 0.2566(4) 1.0988(3) 0.6845(9) 0.032(2) Uani 1 1 d . . . N19 N 0.2321(4) 1.2117(2) 0.6786(9) 0.030(2) Uani 1 1 d . . . N20 N 0.2958(4) 1.2315(3) 0.8044(9) 0.040(3) Uani 1 1 d . . . N21 N 0.2906(4) 1.1465(3) 0.9951(10) 0.049(3) Uani 1 1 d . . . O1 O 0.3071(5) 0.9959(3) 0.5668(10) 0.081(4) Uani 1 1 d . . . O2 O 0.2851(4) 0.8186(3) 1.0462(8) 0.059(3) Uani 1 1 d . . . O3 O 0.3179(6) 1.1381(4) 1.0827(11) 0.123(6) Uani 1 1 d . . . O4 O 0.3878(8) 0.3244(6) 0.884(2) 0.183(10) Uani 1 1 d . . . C1 C 0.2291(4) 0.9413(3) 0.2702(10) 0.026(3) Uani 1 1 d . . . C2 C 0.1988(5) 0.9038(3) 0.1206(11) 0.034(3) Uani 1 1 d . . . H2 H 0.1799 0.8948 0.0483 0.041 Uiso 1 1 calc R . . C3 C 0.2323(5) 0.8848(3) 0.2007(11) 0.034(3) Uani 1 1 d . . . H3 H 0.2417 0.8605 0.1956 0.040 Uiso 1 1 calc R . . C4 C 0.2865(5) 0.8977(4) 0.4002(11) 0.046(4) Uani 1 1 d . . . H4A H 0.2730 0.8759 0.4338 0.055 Uiso 1 1 calc R . . H4B H 0.2881 0.9169 0.4601 0.055 Uiso 1 1 calc R . . C5 C 0.3410(6) 0.8901(5) 0.3762(14) 0.069(5) Uani 1 1 d . . . H5 H 0.3378 0.8741 0.3052 0.083 Uiso 1 1 calc R . . C6 C 0.3687(7) 0.8697(7) 0.480(2) 0.138(10) Uani 1 1 d . . . H6A H 0.3516 0.8465 0.4885 0.165 Uiso 1 1 calc R . . H6B H 0.3695 0.8835 0.5545 0.165 Uiso 1 1 calc R . . C7 C 0.4283(10) 0.8634(8) 0.453(2) 0.183(14) Uani 1 1 d . . . H7A H 0.4494 0.8511 0.5206 0.220 Uiso 1 1 calc R . . H7B H 0.4271 0.8482 0.3814 0.220 Uiso 1 1 calc R . . C8 C 0.4513(8) 0.8977(7) 0.433(2) 0.172(15) Uani 1 1 d . . . H8A H 0.4497 0.9139 0.5006 0.207 Uiso 1 1 calc R . . H8B H 0.4878 0.8945 0.4249 0.207 Uiso 1 1 calc R . . C9 C 0.4232(7) 0.9120(8) 0.328(2) 0.171(14) Uani 1 1 d . . . H9A H 0.4202 0.8939 0.2641 0.205 Uiso 1 1 calc R . . H9B H 0.4415 0.9331 0.3035 0.205 Uiso 1 1 calc R . . C10 C 0.3688(8) 0.9230(5) 0.3494(18) 0.098(6) Uani 1 1 d . . . H10A H 0.3716 0.9400 0.4167 0.117 Uiso 1 1 calc R . . H10B H 0.3498 0.9349 0.2778 0.117 Uiso 1 1 calc R . . C11 C 0.2338(4) 1.0139(3) 0.2166(10) 0.024(3) Uani 1 1 d . . . C12 C 0.2052(5) 1.0272(3) 0.0248(10) 0.028(3) Uani 1 1 d . . . H12 H 0.1866 1.0263 -0.0540 0.034 Uiso 1 1 calc R . . C13 C 0.2416(5) 1.0508(3) 0.0674(11) 0.035(3) Uani 1 1 d . . . H13 H 0.2535 1.0699 0.0247 0.042 Uiso 1 1 calc R . . C14 C 0.3008(5) 1.0603(3) 0.2632(10) 0.036(3) Uani 1 1 d . . . H14A H 0.2906 1.0646 0.3414 0.044 Uiso 1 1 calc R . . H14B H 0.3073 1.0837 0.2286 0.044 Uiso 1 1 calc R . . C15 C 0.3502(5) 1.0382(4) 0.2801(12) 0.044(3) Uani 1 1 d . . . H15 H 0.3409 1.0132 0.2992 0.053 Uiso 1 1 calc R . . C16 C 0.3729(6) 1.0367(4) 0.1717(14) 0.071(5) Uani 1 1 d . . . H16A H 0.3793 1.0613 0.1460 0.085 Uiso 1 1 calc R . . H16B H 0.3482 1.0252 0.1077 0.085 Uiso 1 1 calc R . . C17 C 0.4238(7) 1.0156(5) 0.1904(15) 0.079(5) Uani 1 1 d . . . H17A H 0.4165 0.9901 0.2034 0.095 Uiso 1 1 calc R . . H17B H 0.4395 1.0173 0.1178 0.095 Uiso 1 1 calc R . . C18 C 0.4620(7) 1.0293(5) 0.2953(18) 0.094(6) Uani 1 1 d . . . H18A H 0.4723 1.0540 0.2783 0.113 Uiso 1 1 calc R . . H18B H 0.4932 1.0142 0.3058 0.113 Uiso 1 1 calc R . . C19 C 0.4398(7) 1.0294(5) 0.4106(15) 0.084(6) Uani 1 1 d . . . H19A H 0.4644 1.0404 0.4756 0.101 Uiso 1 1 calc R . . H19B H 0.4325 1.0047 0.4339 0.101 Uiso 1 1 calc R . . C20 C 0.3881(6) 1.0519(5) 0.3845(14) 0.075(5) Uani 1 1 d . . . H20A H 0.3715 1.0517 0.4560 0.090 Uiso 1 1 calc R . . H20B H 0.3968 1.0770 0.3690 0.090 Uiso 1 1 calc R . . C21 C 0.1570(5) 0.9881(3) 0.3315(10) 0.029(3) Uani 1 1 d . . . C22 C 0.0799(5) 0.9728(3) 0.2316(10) 0.030(3) Uani 1 1 d . . . H22 H 0.0537 0.9657 0.1682 0.036 Uiso 1 1 calc R . . C23 C 0.0735(5) 0.9787(3) 0.3434(11) 0.033(3) Uani 1 1 d . . . H23 H 0.0423 0.9766 0.3741 0.040 Uiso 1 1 calc R . . C24 C 0.1322(5) 0.9969(3) 0.5316(10) 0.028(3) Uani 1 1 d . . . H24A H 0.1691 0.9923 0.5614 0.034 Uiso 1 1 calc R . . H24B H 0.1121 0.9804 0.5738 0.034 Uiso 1 1 calc R . . C25 C 0.1199(5) 1.0350(3) 0.5631(9) 0.028(3) Uani 1 1 d . . . H25 H 0.1387 1.0516 0.5169 0.033 Uiso 1 1 calc R . . C26 C 0.1395(5) 1.0411(3) 0.6954(10) 0.033(3) Uani 1 1 d . . . H26A H 0.1772 1.0370 0.7120 0.039 Uiso 1 1 calc R . . H26B H 0.1232 1.0235 0.7420 0.039 Uiso 1 1 calc R . . C27 C 0.1279(5) 1.0790(3) 0.7353(11) 0.037(3) Uani 1 1 d . . . H27A H 0.1469 1.0967 0.6948 0.045 Uiso 1 1 calc R . . H27B H 0.1396 1.0814 0.8219 0.045 Uiso 1 1 calc R . . C28 C 0.0697(5) 1.0867(3) 0.7056(12) 0.045(4) Uani 1 1 d . . . H28A H 0.0510 1.0707 0.7525 0.054 Uiso 1 1 calc R . . H28B H 0.0630 1.1117 0.7270 0.054 Uiso 1 1 calc R . . C29 C 0.0507(5) 1.0810(3) 0.5759(11) 0.041(3) Uani 1 1 d . . . H29A H 0.0670 1.0988 0.5301 0.049 Uiso 1 1 calc R . . H29B H 0.0130 1.0852 0.5593 0.049 Uiso 1 1 calc R . . C30 C 0.0618(5) 1.0437(3) 0.5333(11) 0.037(3) Uani 1 1 d . . . H30A H 0.0502 1.0421 0.4464 0.044 Uiso 1 1 calc R . . H30B H 0.0421 1.0259 0.5716 0.044 Uiso 1 1 calc R . . C31 C 0.1253(4) 0.9670(3) -0.0070(10) 0.026(3) Uani 1 1 d . . . C32 C 0.1398(5) 0.9474(3) -0.0990(10) 0.032(3) Uani 1 1 d . . . H32 H 0.1732 0.9371 -0.0876 0.038 Uiso 1 1 calc R . . C33 C 0.1081(5) 0.9421(3) -0.2052(11) 0.040(3) Uani 1 1 d . . . H33 H 0.1187 0.9270 -0.2633 0.048 Uiso 1 1 calc R . . C34 C 0.0606(6) 0.9587(3) -0.2280(12) 0.045(4) Uani 1 1 d . . . H34 H 0.0381 0.9550 -0.3012 0.054 Uiso 1 1 calc R . . C35 C 0.0467(5) 0.9808(3) -0.1417(11) 0.039(3) Uani 1 1 d . . . H35 H 0.0144 0.9927 -0.1567 0.046 Uiso 1 1 calc R . . C36 C 0.0784(5) 0.9857(3) -0.0353(11) 0.036(3) Uani 1 1 d . . . H36 H 0.0687 1.0021 0.0205 0.044 Uiso 1 1 calc R . . C37 C 0.327(2) 0.3266(14) 1.005(4) 0.065(12) Uani 0.49(3) 1 d PDU A -1 H37A H 0.3008 0.3428 1.0280 0.097 Uiso 0.49(3) 1 calc PR A -1 H37B H 0.3523 0.3207 1.0747 0.097 Uiso 0.49(3) 1 calc PR A -1 H37C H 0.3098 0.3047 0.9712 0.097 Uiso 0.49(3) 1 calc PR A -1 C38 C 0.352(2) 0.3444(13) 0.915(5) 0.091(12) Uani 0.49(3) 1 d PDU A -1 H38A H 0.3266 0.3500 0.8437 0.109 Uiso 0.49(3) 1 calc PR A -1 H38B H 0.3679 0.3671 0.9474 0.109 Uiso 0.49(3) 1 calc PR A -1 C39 C 0.422(2) 0.3386(18) 0.868(6) 0.133(16) Uani 0.49(3) 1 d PDU A -1 H39A H 0.4384 0.3482 0.9459 0.160 Uiso 0.49(3) 1 calc PR A -1 H39B H 0.4091 0.3595 0.8187 0.160 Uiso 0.49(3) 1 calc PR A -1 C40 C 0.4637(17) 0.3229(14) 0.813(5) 0.102(15) Uani 0.49(3) 1 d PDU A -1 H40A H 0.4912 0.3406 0.8138 0.153 Uiso 0.49(3) 1 calc PR A -1 H40B H 0.4502 0.3159 0.7314 0.153 Uiso 0.49(3) 1 calc PR A -1 H40C H 0.4775 0.3018 0.8586 0.153 Uiso 0.49(3) 1 calc PR A -1 C37A C 0.3172(14) 0.3361(16) 0.955(5) 0.081(14) Uani 0.51(3) 1 d PDU A -2 H37D H 0.3038 0.3440 1.0255 0.122 Uiso 0.51(3) 1 calc PR A -2 H37E H 0.3042 0.3121 0.9324 0.122 Uiso 0.51(3) 1 calc PR A -2 H37F H 0.3058 0.3527 0.8893 0.122 Uiso 0.51(3) 1 calc PR A -2 C38A C 0.3743(13) 0.3354(14) 0.981(4) 0.081(11) Uani 0.51(3) 1 d PDU A -2 H38C H 0.3882 0.3595 1.0019 0.098 Uiso 0.51(3) 1 calc PR A -2 H38D H 0.3866 0.3189 1.0473 0.098 Uiso 0.51(3) 1 calc PR A -2 C39A C 0.454(2) 0.3235(15) 0.901(5) 0.132(15) Uani 0.51(3) 1 d PDU A -2 H39C H 0.4725 0.3346 0.9750 0.158 Uiso 0.51(3) 1 calc PR A -2 H39D H 0.4690 0.2997 0.8878 0.158 Uiso 0.51(3) 1 calc PR A -2 C40A C 0.448(2) 0.3474(14) 0.796(4) 0.139(17) Uani 0.51(3) 1 d PDU A -2 H40D H 0.4818 0.3524 0.7743 0.208 Uiso 0.51(3) 1 calc PR A -2 H40E H 0.4319 0.3698 0.8145 0.208 Uiso 0.51(3) 1 calc PR A -2 H40F H 0.4260 0.3357 0.7289 0.208 Uiso 0.51(3) 1 calc PR A -2 C41 C 0.2080(4) 0.8050(3) 0.6908(10) 0.025(3) Uani 1 1 d . . . C42 C 0.1801(5) 0.7947(3) 0.4963(10) 0.029(3) Uani 1 1 d . . . H42 H 0.1629 0.7978 0.4170 0.034 Uiso 1 1 calc R . . C43 C 0.2104(5) 0.7674(3) 0.5379(10) 0.029(3) Uani 1 1 d . . . H43 H 0.2185 0.7474 0.4934 0.034 Uiso 1 1 calc R . . C44 C 0.2616(4) 0.7511(3) 0.7397(10) 0.027(3) Uani 1 1 d . B . H44A H 0.2547 0.7258 0.7168 0.033 Uiso 1 1 calc R . . H44B H 0.2533 0.7543 0.8203 0.033 Uiso 1 1 calc R . . C45 C 0.3162(6) 0.7583(5) 0.7436(17) 0.079(5) Uani 1 1 d U . . H45 H 0.3186 0.7508 0.6607 0.095 Uiso 1 1 calc R B . C46 C 0.3503(17) 0.7290(10) 0.809(4) 0.077(9) Uani 0.575(17) 1 d PU B -1 H46A H 0.3354 0.7054 0.7833 0.093 Uiso 0.575(17) 1 calc PR B -1 H46B H 0.3497 0.7312 0.8954 0.093 Uiso 0.575(17) 1 calc PR B -1 C47 C 0.4078(11) 0.7301(9) 0.789(3) 0.093(8) Uani 0.575(17) 1 d PU B -1 H47A H 0.4286 0.7145 0.8490 0.112 Uiso 0.575(17) 1 calc PR B -1 H47B H 0.4095 0.7200 0.7099 0.112 Uiso 0.575(17) 1 calc PR B -1 C50 C 0.3377(11) 0.7905(8) 0.741(3) 0.077(7) Uani 0.575(17) 1 d PU B -1 H50A H 0.3382 0.8021 0.8195 0.092 Uiso 0.575(17) 1 calc PR B -1 H50B H 0.3158 0.8053 0.6810 0.092 Uiso 0.575(17) 1 calc PR B -1 C46A C 0.349(2) 0.7422(14) 0.853(5) 0.079(10) Uani 0.425(17) 1 d PU B -2 H46C H 0.3503 0.7161 0.8394 0.095 Uiso 0.425(17) 1 calc PR B -2 H46D H 0.3299 0.7457 0.9198 0.095 Uiso 0.425(17) 1 calc PR B -2 C47A C 0.4051(14) 0.7560(12) 0.892(4) 0.087(9) Uani 0.425(17) 1 d PU B -2 H47C H 0.4044 0.7776 0.9422 0.104 Uiso 0.425(17) 1 calc PR B -2 H47D H 0.4253 0.7374 0.9419 0.104 Uiso 0.425(17) 1 calc PR B -2 C50A C 0.3398(13) 0.7704(11) 0.653(4) 0.063(7) Uani 0.425(17) 1 d PU B -2 H50C H 0.3173 0.7879 0.6040 0.076 Uiso 0.425(17) 1 calc PR B -2 H50D H 0.3463 0.7502 0.6016 0.076 Uiso 0.425(17) 1 calc PR B -2 C48 C 0.4299(7) 0.7642(5) 0.7969(19) 0.098(6) Uani 1 1 d U . . H48A H 0.4648 0.7630 0.7760 0.118 Uiso 1 1 calc R B . H48B H 0.4331 0.7732 0.8793 0.118 Uiso 1 1 calc R . . C49 C 0.3963(7) 0.7901(5) 0.7120(18) 0.098(6) Uani 1 1 d U B . H49A H 0.3957 0.7824 0.6289 0.118 Uiso 1 1 calc R . . H49B H 0.4111 0.8144 0.7213 0.118 Uiso 1 1 calc R . . C51 C 0.2210(4) 0.8775(3) 0.7522(9) 0.018(2) Uani 1 1 d . . . C52 C 0.1984(5) 0.9170(3) 0.6049(10) 0.027(3) Uani 1 1 d . . . H52 H 0.1815 0.9280 0.5340 0.032 Uiso 1 1 calc R . . C53 C 0.2357(5) 0.9323(3) 0.6885(10) 0.030(3) Uani 1 1 d . . . H53 H 0.2503 0.9554 0.6859 0.036 Uiso 1 1 calc R . . C54 C 0.2839(4) 0.9134(3) 0.8840(9) 0.028(3) Uani 1 1 d . . . H54A H 0.2721 0.9004 0.9497 0.034 Uiso 1 1 calc R C . H54B H 0.2847 0.9392 0.9037 0.034 Uiso 1 1 calc R . . C55 C 0.3387(10) 0.9011(6) 0.874(2) 0.046(2) Uani 0.677(9) 1 d P C -1 H55 H 0.3359 0.8755 0.8493 0.055 Uiso 0.677(9) 1 calc PR C -1 C56 C 0.3746(7) 0.9022(6) 0.9937(16) 0.046(2) Uani 0.677(9) 1 d P C -1 H56A H 0.3763 0.9270 1.0236 0.055 Uiso 0.677(9) 1 calc PR C -1 H56B H 0.3596 0.8873 1.0508 0.055 Uiso 0.677(9) 1 calc PR C -1 C57 C 0.4280(8) 0.8895(6) 0.9903(17) 0.046(2) Uani 0.677(9) 1 d P C -1 H57A H 0.4273 0.8642 0.9649 0.055 Uiso 0.677(9) 1 calc PR C -1 H57B H 0.4491 0.8912 1.0705 0.055 Uiso 0.677(9) 1 calc PR C -1 C58 C 0.4521(8) 0.9129(6) 0.9020(17) 0.046(2) Uani 0.677(9) 1 d P C -1 H58A H 0.4539 0.9382 0.9279 0.055 Uiso 0.677(9) 1 calc PR C -1 H58B H 0.4874 0.9045 0.8973 0.055 Uiso 0.677(9) 1 calc PR C -1 C59 C 0.4181(7) 0.9093(6) 0.7840(16) 0.046(2) Uani 0.677(9) 1 d P C -1 H59A H 0.4186 0.8841 0.7575 0.055 Uiso 0.677(9) 1 calc PR C -1 H59B H 0.4320 0.9242 0.7254 0.055 Uiso 0.677(9) 1 calc PR C -1 C60 C 0.3633(7) 0.9201(6) 0.7863(16) 0.046(2) Uani 0.677(9) 1 d P C -1 H60A H 0.3626 0.9460 0.8027 0.055 Uiso 0.677(9) 1 calc PR C -1 H60B H 0.3428 0.9160 0.7066 0.055 Uiso 0.677(9) 1 calc PR C -1 C55A C 0.339(2) 0.9154(12) 0.866(5) 0.046(2) Uani 0.323(9) 1 d P C -2 H55A H 0.3404 0.9297 0.7924 0.055 Uiso 0.323(9) 1 calc PR C -2 C56A C 0.3581(17) 0.8825(12) 0.851(4) 0.046(2) Uani 0.323(9) 1 d P C -2 H56C H 0.3390 0.8724 0.7763 0.055 Uiso 0.323(9) 1 calc PR C -2 H56D H 0.3506 0.8672 0.9166 0.055 Uiso 0.323(9) 1 calc PR C -2 C57A C 0.4118(15) 0.8798(12) 0.847(3) 0.046(2) Uani 0.323(9) 1 d P C -2 H57C H 0.4184 0.8894 0.7705 0.055 Uiso 0.323(9) 1 calc PR C -2 H57D H 0.4218 0.8542 0.8512 0.055 Uiso 0.323(9) 1 calc PR C -2 C58A C 0.4462(18) 0.9003(13) 0.951(4) 0.046(2) Uani 0.323(9) 1 d P C -2 H58C H 0.4490 0.8860 1.0242 0.055 Uiso 0.323(9) 1 calc PR C -2 H58D H 0.4812 0.9031 0.9314 0.055 Uiso 0.323(9) 1 calc PR C -2 C59A C 0.4245(15) 0.9374(11) 0.972(3) 0.046(2) Uani 0.323(9) 1 d P C -2 H59C H 0.4446 0.9473 1.0462 0.055 Uiso 0.323(9) 1 calc PR C -2 H59D H 0.4298 0.9533 0.9064 0.055 Uiso 0.323(9) 1 calc PR C -2 C60A C 0.3694(15) 0.9381(12) 0.983(3) 0.046(2) Uani 0.323(9) 1 d P C -2 H60C H 0.3567 0.9630 0.9812 0.055 Uiso 0.323(9) 1 calc PR C -2 H60D H 0.3638 0.9267 1.0575 0.055 Uiso 0.323(9) 1 calc PR C -2 C61 C 0.1396(5) 0.8398(3) 0.8083(9) 0.025(3) Uani 1 1 d . . . C62 C 0.0639(4) 0.8600(3) 0.7026(10) 0.026(3) Uani 1 1 d . . . H62 H 0.0392 0.8684 0.6383 0.031 Uiso 1 1 calc R . . C63 C 0.0571(5) 0.8548(3) 0.8170(10) 0.030(3) Uani 1 1 d . . . H63 H 0.0264 0.8591 0.8479 0.036 Uiso 1 1 calc R . . C64 C 0.1124(5) 0.8330(3) 1.0048(8) 0.027(3) Uani 1 1 d . . . H64A H 0.0949 0.8507 1.0485 0.033 Uiso 1 1 calc R . . H64B H 0.1499 0.8347 1.0345 0.033 Uiso 1 1 calc R . . C65 C 0.0941(5) 0.7955(3) 1.0323(9) 0.029(3) Uani 1 1 d . . . H65 H 0.1094 0.7780 0.9819 0.034 Uiso 1 1 calc R . . C66 C 0.1153(5) 0.7870(3) 1.1633(10) 0.031(3) Uani 1 1 d . . . H66A H 0.1535 0.7877 1.1762 0.038 Uiso 1 1 calc R . . H66B H 0.1034 0.8054 1.2146 0.038 Uiso 1 1 calc R . . C67 C 0.0978(5) 0.7505(3) 1.1981(10) 0.039(3) Uani 1 1 d . . . H67A H 0.1098 0.7466 1.2840 0.047 Uiso 1 1 calc R . . H67B H 0.1135 0.7318 1.1542 0.047 Uiso 1 1 calc R . . C68 C 0.0390(5) 0.7472(3) 1.1707(12) 0.047(4) Uani 1 1 d . . . H68A H 0.0290 0.7228 1.1911 0.056 Uiso 1 1 calc R . . H68B H 0.0236 0.7643 1.2208 0.056 Uiso 1 1 calc R . . C69 C 0.0176(5) 0.7546(3) 1.0400(11) 0.042(3) Uani 1 1 d . . . H69A H 0.0298 0.7361 0.9897 0.050 Uiso 1 1 calc R . . H69B H -0.0205 0.7537 1.0270 0.050 Uiso 1 1 calc R . . C70 C 0.0352(4) 0.7912(3) 1.0054(10) 0.029(3) Uani 1 1 d . . . H70A H 0.0192 0.8098 1.0491 0.035 Uiso 1 1 calc R . . H70B H 0.0231 0.7950 0.9195 0.035 Uiso 1 1 calc R . . C71 C 0.1123(4) 0.8602(3) 0.4665(9) 0.022(3) Uani 1 1 d . . . C72 C 0.1253(5) 0.8807(3) 0.3758(10) 0.029(3) Uani 1 1 d . . . H72 H 0.1575 0.8927 0.3869 0.034 Uiso 1 1 calc R . . C73 C 0.0920(5) 0.8842(3) 0.2687(10) 0.035(3) Uani 1 1 d . . . H73 H 0.1022 0.8984 0.2077 0.042 Uiso 1 1 calc R . . C74 C 0.0450(5) 0.8678(3) 0.2482(10) 0.026(3) Uani 1 1 d . . . H74 H 0.0221 0.8714 0.1756 0.031 Uiso 1 1 calc R . . C75 C 0.0318(5) 0.8462(3) 0.3344(10) 0.034(3) Uani 1 1 d . . . H75 H -0.0001 0.8339 0.3204 0.041 Uiso 1 1 calc R . . C76 C 0.0640(4) 0.8422(3) 0.4407(10) 0.025(3) Uani 1 1 d . . . H76 H 0.0539 0.8269 0.4991 0.030 Uiso 1 1 calc R . . C81 C 0.1780(6) 1.1711(3) 0.8460(12) 0.049(4) Uani 1 1 d . . . C82 C 0.1074(4) 1.1951(3) 0.7447(10) 0.026(3) Uani 1 1 d . . . H82 H 0.0832 1.2055 0.6829 0.031 Uiso 1 1 calc R . . C83 C 0.1015(5) 1.1905(3) 0.8555(12) 0.039(3) Uani 1 1 d . . . H83 H 0.0719 1.1969 0.8878 0.046 Uiso 1 1 calc R . . C84 C 0.1560(5) 1.1665(3) 1.0433(10) 0.033(3) Uani 1 1 d . . . H84A H 0.1388 1.1843 1.0873 0.039 Uiso 1 1 calc R . . H84B H 0.1935 1.1682 1.0717 0.039 Uiso 1 1 calc R . . C85 C 0.1370(4) 1.1283(3) 1.0701(10) 0.031(3) Uani 1 1 d . . . H85 H 0.1531 1.1109 1.0208 0.037 Uiso 1 1 calc R . . C86 C 0.0786(5) 1.1242(3) 1.0376(11) 0.038(3) Uani 1 1 d . . . H86A H 0.0681 1.1275 0.9510 0.046 Uiso 1 1 calc R . . H86B H 0.0617 1.1430 1.0781 0.046 Uiso 1 1 calc R . . C87 C 0.0603(5) 1.0875(3) 1.0729(12) 0.045(4) Uani 1 1 d . . . H87A H 0.0223 1.0867 1.0546 0.054 Uiso 1 1 calc R . . H87B H 0.0738 1.0689 1.0248 0.054 Uiso 1 1 calc R . . C88 C 0.0776(6) 1.0793(3) 1.2029(12) 0.051(4) Uani 1 1 d . . . H88A H 0.0668 1.0548 1.2201 0.061 Uiso 1 1 calc R . . H88B H 0.0611 1.0962 1.2517 0.061 Uiso 1 1 calc R . . C89 C 0.1367(6) 1.0825(3) 1.2352(11) 0.043(4) Uani 1 1 d . . . H89A H 0.1473 1.0788 1.3216 0.052 Uiso 1 1 calc R . . H89B H 0.1529 1.0636 1.1936 0.052 Uiso 1 1 calc R . . C90 C 0.1556(5) 1.1186(3) 1.2014(10) 0.040(3) Uani 1 1 d . . . H90A H 0.1937 1.1188 1.2175 0.048 Uiso 1 1 calc R . . H90B H 0.1434 1.1371 1.2520 0.048 Uiso 1 1 calc R . . C91 C 0.2426(4) 1.1314(3) 0.7202(10) 0.028(3) Uani 1 1 d . . . C92 C 0.2101(4) 1.1220(3) 0.5297(11) 0.029(3) Uani 1 1 d . . . H92 H 0.1921 1.1258 0.4515 0.034 Uiso 1 1 calc R . . C93 C 0.2358(5) 1.0933(3) 0.5661(11) 0.036(3) Uani 1 1 d . . . H93 H 0.2397 1.0726 0.5205 0.043 Uiso 1 1 calc R . . C94 C 0.2865(5) 1.0732(3) 0.7676(11) 0.036(3) Uani 1 1 d . . . H94A H 0.2681 1.0500 0.7620 0.043 Uiso 1 1 calc R . . H94B H 0.2885 1.0822 0.8497 0.043 Uiso 1 1 calc R . . C95 C 0.3402(5) 1.0673(3) 0.7430(11) 0.037(3) Uani 1 1 d . . . H95 H 0.3372 1.0601 0.6578 0.045 Uiso 1 1 calc R . . C96 C 0.3658(6) 1.0356(4) 0.8201(13) 0.053(4) Uani 1 1 d . . . H96A H 0.3693 1.0420 0.9051 0.064 Uiso 1 1 calc R . . H96B H 0.3433 1.0143 0.8060 0.064 Uiso 1 1 calc R . . C97 C 0.4200(6) 1.0264(4) 0.7904(16) 0.075(5) Uani 1 1 d . . . H97A H 0.4354 1.0064 0.8410 0.090 Uiso 1 1 calc R . . H97B H 0.4166 1.0189 0.7064 0.090 Uiso 1 1 calc R . . C98 C 0.4541(6) 1.0587(5) 0.8117(15) 0.074(5) Uani 1 1 d . . . H98A H 0.4883 1.0530 0.7915 0.089 Uiso 1 1 calc R . . H98B H 0.4589 1.0652 0.8967 0.089 Uiso 1 1 calc R . . C99 C 0.4304(5) 1.0905(4) 0.7360(16) 0.069(5) Uani 1 1 d . . . H99A H 0.4529 1.1117 0.7537 0.083 Uiso 1 1 calc R . . H99B H 0.4281 1.0847 0.6508 0.083 Uiso 1 1 calc R . . C100 C 0.3763(5) 1.0991(4) 0.7626(14) 0.056(4) Uani 1 1 d . . . H10C H 0.3793 1.1071 0.8460 0.067 Uiso 1 1 calc R . . H10D H 0.3614 1.1190 0.7109 0.067 Uiso 1 1 calc R . . C101 C 0.2626(5) 1.2029(3) 0.7782(11) 0.030(3) Uani 1 1 d . . . C102 C 0.2432(5) 1.2450(3) 0.6427(13) 0.040(3) Uani 1 1 d . . . H102 H 0.2253 1.2573 0.5754 0.048 Uiso 1 1 calc R . . C103 C 0.2830(6) 1.2574(3) 0.7174(12) 0.046(4) Uani 1 1 d . . . H103 H 0.2996 1.2798 0.7126 0.056 Uiso 1 1 calc R . . C104 C 0.3392(6) 1.2320(4) 0.9035(12) 0.048(4) Uani 1 1 d . . . H10E H 0.3271 1.2234 0.9760 0.058 Uiso 1 1 calc R . . H10F H 0.3510 1.2570 0.9179 0.058 Uiso 1 1 calc R . . C105 C 0.3845(5) 1.2091(4) 0.8827(12) 0.049(4) Uani 1 1 d . . . H105 H 0.3704 1.1849 0.8586 0.058 Uiso 1 1 calc R . . C106 C 0.4246(6) 1.2040(4) 0.9989(13) 0.063(4) Uani 1 1 d . . . H10G H 0.4387 1.2276 1.0276 0.075 Uiso 1 1 calc R . . H10H H 0.4073 1.1935 1.0612 0.075 Uiso 1 1 calc R . . C107 C 0.4684(6) 1.1797(5) 0.9771(15) 0.081(5) Uani 1 1 d . . . H10I H 0.4549 1.1555 0.9554 0.097 Uiso 1 1 calc R . . H10J H 0.4943 1.1778 1.0505 0.097 Uiso 1 1 calc R . . C108 C 0.4943(7) 1.1952(5) 0.8749(17) 0.090(6) Uani 1 1 d . . . H10K H 0.5098 1.2187 0.8993 0.108 Uiso 1 1 calc R . . H10L H 0.5222 1.1790 0.8602 0.108 Uiso 1 1 calc R . . C109 C 0.4548(6) 1.1997(4) 0.7584(15) 0.070(5) Uani 1 1 d . . . H10M H 0.4718 1.2109 0.6968 0.083 Uiso 1 1 calc R . . H10N H 0.4417 1.1760 0.7290 0.083 Uiso 1 1 calc R . . C110 C 0.4099(6) 1.2230(4) 0.7815(13) 0.060(4) Uani 1 1 d . . . H11A H 0.4226 1.2476 0.8005 0.073 Uiso 1 1 calc R . . H11B H 0.3838 1.2242 0.7083 0.073 Uiso 1 1 calc R . . C111 C 0.1523(5) 1.1938(3) 0.5059(11) 0.033(3) Uani 1 1 d . . . C112 C 0.1039(5) 1.1800(3) 0.4765(11) 0.042(3) Uani 1 1 d . . . H112 H 0.0911 1.1655 0.5331 0.050 Uiso 1 1 calc R . . C113 C 0.0721(5) 1.1862(3) 0.3662(11) 0.037(3) Uani 1 1 d . . . H113 H 0.0383 1.1764 0.3498 0.045 Uiso 1 1 calc R . . C114 C 0.0914(5) 1.2073(3) 0.2799(11) 0.040(3) Uani 1 1 d . . . H114 H 0.0708 1.2121 0.2050 0.048 Uiso 1 1 calc R . . C115 C 0.1405(5) 1.2206(3) 0.3077(11) 0.038(3) Uani 1 1 d . . . H115 H 0.1534 1.2354 0.2519 0.046 Uiso 1 1 calc R . . C116 C 0.1710(5) 1.2132(3) 0.4126(12) 0.044(4) Uani 1 1 d . . . H116 H 0.2057 1.2211 0.4252 0.053 Uiso 1 1 calc R . . 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 0.0220(9) 0.0317(9) 0.0274(9) 0.0000(7) 0.0077(7) -0.0009(7) Ni2 0.0237(10) 0.0262(8) 0.0206(8) 0.0016(7) 0.0059(7) 0.0022(7) Ni3 0.0261(10) 0.0417(10) 0.0340(9) 0.0021(8) 0.0088(8) 0.0003(8) B1 0.037(9) 0.021(7) 0.025(8) 0.005(6) 0.008(7) 0.004(6) B2 0.012(7) 0.033(8) 0.028(8) 0.010(6) 0.005(6) -0.005(6) B3 0.023(9) 0.036(8) 0.037(9) 0.002(7) 0.017(7) 0.003(7) N1 0.020(6) 0.027(5) 0.028(6) -0.006(4) 0.006(5) 0.004(4) N2 0.018(6) 0.032(6) 0.051(7) 0.004(5) 0.009(5) 0.006(5) N3 0.027(6) 0.025(5) 0.035(6) 0.010(4) 0.016(5) 0.002(4) N4 0.030(7) 0.031(6) 0.028(6) 0.003(5) 0.010(5) -0.008(5) N5 0.029(6) 0.031(6) 0.027(6) 0.002(4) 0.013(5) 0.013(5) N6 0.020(6) 0.026(5) 0.029(6) 0.004(4) 0.014(5) 0.006(4) N7 0.045(7) 0.039(6) 0.020(6) 0.000(5) 0.004(5) -0.020(5) N8 0.020(6) 0.036(6) 0.016(5) 0.004(4) 0.006(4) 0.005(4) N9 0.029(6) 0.021(5) 0.034(6) 0.001(4) 0.015(5) 0.004(4) N10 0.020(6) 0.027(5) 0.020(5) 0.003(4) 0.013(4) 0.002(4) N11 0.020(6) 0.023(5) 0.020(5) 0.005(4) 0.001(4) 0.000(4) N12 0.027(6) 0.025(5) 0.015(5) 0.001(4) 0.003(4) -0.003(4) N13 0.025(6) 0.026(5) 0.024(5) -0.001(4) 0.013(5) 0.000(4) N14 0.019(6) 0.030(6) 0.020(5) -0.002(4) 0.000(5) 0.010(4) N15 0.035(7) 0.026(5) 0.042(7) 0.005(5) 0.025(5) 0.008(5) N16 0.017(6) 0.029(5) 0.039(6) 0.002(5) 0.024(5) -0.003(4) N17 0.024(6) 0.027(5) 0.025(6) 0.005(4) 0.006(5) -0.002(4) N18 0.019(6) 0.039(6) 0.042(7) -0.005(5) 0.014(5) -0.001(5) N19 0.030(7) 0.024(6) 0.037(6) 0.001(5) 0.007(5) -0.011(5) N20 0.045(8) 0.036(6) 0.041(7) -0.018(5) 0.014(6) -0.004(6) N21 0.038(8) 0.059(8) 0.045(7) 0.013(6) -0.007(6) -0.013(6) O1 0.090(10) 0.087(8) 0.054(7) 0.005(6) -0.026(7) -0.045(7) O2 0.055(7) 0.067(7) 0.046(6) 0.011(5) -0.018(6) 0.013(5) O3 0.117(13) 0.155(13) 0.073(9) 0.055(9) -0.051(9) -0.043(10) O4 0.100(16) 0.23(2) 0.26(2) -0.060(17) 0.129(17) -0.053(14) C1 0.018(7) 0.024(6) 0.040(8) -0.009(6) 0.020(6) -0.007(5) C2 0.031(8) 0.028(7) 0.044(8) -0.004(6) 0.007(7) -0.003(6) C3 0.024(8) 0.032(7) 0.050(8) -0.006(7) 0.020(7) 0.001(6) C4 0.041(9) 0.053(9) 0.041(8) 0.010(7) 0.004(7) 0.012(7) C5 0.027(9) 0.125(15) 0.054(10) 0.018(10) 0.003(8) 0.029(10) C6 0.038(13) 0.22(3) 0.15(2) 0.07(2) -0.003(13) 0.022(15) C7 0.10(2) 0.27(4) 0.16(3) 0.06(3) -0.01(2) 0.12(2) C8 0.047(14) 0.24(3) 0.21(3) 0.17(3) -0.026(16) -0.059(18) C9 0.019(11) 0.31(4) 0.19(3) 0.17(3) 0.047(14) 0.028(16) C10 0.085(17) 0.105(16) 0.099(16) 0.022(13) 0.003(13) 0.015(13) C11 0.024(7) 0.022(6) 0.028(7) -0.004(5) 0.007(6) 0.005(5) C12 0.032(8) 0.039(7) 0.015(6) 0.006(5) 0.007(6) -0.002(6) C13 0.040(9) 0.031(7) 0.039(8) 0.000(6) 0.019(7) -0.004(6) C14 0.042(9) 0.044(8) 0.023(7) -0.004(6) 0.007(6) -0.010(7) C15 0.028(8) 0.051(9) 0.053(9) -0.006(7) 0.009(7) -0.004(7) C16 0.058(12) 0.087(12) 0.072(12) -0.016(10) 0.022(10) 0.007(10) C17 0.055(12) 0.110(14) 0.075(12) -0.025(11) 0.020(10) -0.003(11) C18 0.045(12) 0.106(15) 0.138(19) -0.007(13) 0.034(13) 0.006(10) C19 0.049(13) 0.114(15) 0.089(14) -0.011(12) 0.016(11) 0.001(11) C20 0.051(12) 0.102(14) 0.074(12) -0.018(10) 0.021(10) -0.020(10) C21 0.023(7) 0.038(7) 0.029(7) 0.005(6) 0.013(6) 0.013(6) C22 0.026(8) 0.035(7) 0.027(7) 0.006(6) -0.001(6) 0.004(6) C23 0.021(7) 0.031(7) 0.049(8) 0.007(6) 0.010(6) -0.006(5) C24 0.026(7) 0.035(7) 0.028(7) 0.009(5) 0.015(6) 0.009(5) C25 0.026(8) 0.035(7) 0.022(6) 0.003(5) 0.004(5) 0.012(5) C26 0.031(8) 0.039(7) 0.032(7) 0.004(6) 0.014(6) 0.004(6) C27 0.038(9) 0.041(8) 0.036(8) 0.005(6) 0.013(6) 0.003(6) C28 0.040(9) 0.044(8) 0.052(9) -0.009(7) 0.007(7) 0.012(7) C29 0.031(8) 0.037(7) 0.054(9) -0.003(7) 0.003(7) 0.013(6) C30 0.023(8) 0.044(8) 0.040(8) -0.009(6) -0.003(6) 0.010(6) C31 0.016(7) 0.024(6) 0.041(7) 0.006(6) 0.012(6) 0.008(5) C32 0.025(8) 0.035(7) 0.036(8) 0.009(6) 0.008(6) 0.019(6) C33 0.045(10) 0.038(8) 0.041(8) -0.001(6) 0.021(7) -0.004(7) C34 0.055(11) 0.037(8) 0.045(9) -0.005(7) 0.012(8) -0.016(7) C35 0.022(8) 0.049(8) 0.046(9) 0.009(7) 0.008(7) 0.011(6) C36 0.036(8) 0.045(8) 0.031(7) 0.005(6) 0.017(7) -0.008(7) C37 0.07(3) 0.05(3) 0.07(3) 0.00(2) 0.01(2) 0.01(2) C38 0.06(2) 0.11(3) 0.12(3) 0.01(2) 0.05(2) 0.00(2) C39 0.07(3) 0.17(4) 0.17(4) -0.04(3) 0.06(3) 0.02(2) C40 0.06(2) 0.13(4) 0.12(3) -0.03(3) 0.04(2) 0.02(2) C37A 0.056(19) 0.10(3) 0.10(4) 0.00(3) 0.03(3) 0.03(2) C38A 0.053(19) 0.11(3) 0.09(3) 0.01(2) 0.02(2) 0.00(2) C39A 0.06(3) 0.16(4) 0.18(4) -0.07(3) 0.04(3) -0.02(3) C40A 0.09(4) 0.16(4) 0.16(4) -0.08(3) 0.01(3) -0.02(3) C41 0.015(7) 0.029(7) 0.034(7) 0.000(6) 0.011(6) -0.002(5) C42 0.031(8) 0.027(7) 0.033(7) -0.002(6) 0.019(6) 0.011(6) C43 0.028(8) 0.035(7) 0.024(7) -0.005(6) 0.009(6) -0.004(6) C44 0.015(7) 0.039(7) 0.031(7) 0.002(6) 0.011(5) 0.006(6) C45 0.037(8) 0.091(11) 0.100(12) 0.049(9) -0.014(8) 0.006(7) C46 0.032(11) 0.096(17) 0.09(2) 0.039(16) -0.012(16) 0.019(12) C47 0.038(11) 0.114(14) 0.12(2) 0.025(16) -0.006(15) 0.021(11) C50 0.043(10) 0.070(12) 0.108(19) 0.000(15) -0.014(13) 0.016(10) C46A 0.024(12) 0.10(2) 0.11(2) 0.029(18) -0.020(13) 0.021(17) C47A 0.025(13) 0.11(2) 0.118(18) 0.020(16) -0.013(11) 0.020(16) C50A 0.026(12) 0.071(18) 0.094(17) -0.001(14) 0.010(10) 0.017(12) C48 0.032(9) 0.130(13) 0.128(14) 0.008(12) -0.001(9) 0.009(8) C49 0.047(9) 0.107(12) 0.132(14) 0.026(10) -0.009(9) -0.015(8) C51 0.014(6) 0.021(6) 0.020(6) -0.002(5) 0.008(5) 0.005(5) C52 0.025(7) 0.026(7) 0.034(7) 0.009(6) 0.016(6) 0.003(5) C53 0.032(8) 0.023(6) 0.036(7) 0.004(6) 0.008(6) -0.005(6) C54 0.033(8) 0.026(6) 0.026(7) -0.009(5) 0.006(6) -0.013(6) C55 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C56 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C57 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C58 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C59 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C60 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C55A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C56A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C57A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C58A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C59A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C60A 0.027(4) 0.077(6) 0.032(4) 0.010(4) -0.003(3) 0.000(4) C61 0.029(8) 0.025(6) 0.021(6) -0.007(5) 0.004(6) -0.005(5) C62 0.016(7) 0.027(6) 0.036(7) 0.002(5) 0.007(6) 0.003(5) C63 0.022(7) 0.034(7) 0.038(8) 0.003(6) 0.018(6) 0.002(6) C64 0.040(9) 0.033(7) 0.011(6) -0.005(5) 0.011(5) -0.004(6) C65 0.040(8) 0.025(6) 0.022(6) 0.000(5) 0.009(6) 0.006(6) C66 0.030(8) 0.038(7) 0.028(7) -0.002(6) 0.011(6) 0.001(6) C67 0.053(10) 0.040(8) 0.025(7) -0.001(6) 0.005(6) 0.019(7) C68 0.047(10) 0.045(8) 0.050(9) 0.011(7) 0.014(7) -0.007(7) C69 0.043(9) 0.039(8) 0.045(8) 0.012(6) 0.014(7) 0.006(7) C70 0.028(8) 0.036(7) 0.026(7) 0.003(5) 0.012(6) -0.002(6) C71 0.029(7) 0.022(6) 0.015(6) 0.004(5) 0.008(5) 0.004(5) C72 0.027(8) 0.031(7) 0.031(7) -0.007(6) 0.014(6) -0.014(6) C73 0.064(11) 0.030(7) 0.012(6) 0.001(5) 0.011(7) 0.019(7) C74 0.025(8) 0.032(7) 0.021(6) -0.006(5) 0.005(6) 0.015(6) C75 0.043(9) 0.036(7) 0.027(7) -0.007(6) 0.015(6) 0.010(6) C76 0.016(7) 0.039(7) 0.021(6) 0.002(5) 0.007(5) -0.006(5) C81 0.074(12) 0.036(8) 0.049(9) 0.004(7) 0.046(9) -0.006(7) C82 0.019(7) 0.022(6) 0.036(7) 0.009(5) 0.006(6) 0.010(5) C83 0.021(8) 0.040(8) 0.059(9) 0.005(7) 0.017(7) 0.010(6) C84 0.037(9) 0.036(7) 0.031(7) -0.011(6) 0.021(6) -0.008(6) C85 0.021(7) 0.038(7) 0.037(7) -0.007(6) 0.016(6) 0.003(6) C86 0.039(9) 0.028(7) 0.047(8) 0.001(6) 0.004(7) 0.001(6) C87 0.034(9) 0.039(8) 0.060(10) 0.002(7) 0.005(7) -0.020(6) C88 0.073(12) 0.030(8) 0.053(10) 0.003(7) 0.021(9) -0.013(7) C89 0.063(11) 0.024(7) 0.044(8) 0.008(6) 0.013(8) 0.002(7) C90 0.045(9) 0.043(8) 0.033(8) 0.003(6) 0.011(7) 0.015(7) C91 0.015(7) 0.037(7) 0.034(7) 0.001(6) 0.010(6) 0.000(5) C92 0.013(7) 0.040(7) 0.035(7) -0.002(6) 0.008(6) -0.004(6) C93 0.032(8) 0.032(7) 0.048(9) -0.009(6) 0.018(7) 0.007(6) C94 0.022(8) 0.034(7) 0.052(9) 0.005(6) 0.008(6) 0.005(6) C95 0.039(9) 0.039(8) 0.033(7) -0.002(6) 0.002(6) 0.002(6) C96 0.041(10) 0.057(9) 0.064(10) 0.005(8) 0.015(8) 0.010(7) C97 0.047(12) 0.067(11) 0.109(15) -0.006(10) 0.008(10) 0.028(9) C98 0.023(9) 0.108(14) 0.091(13) -0.012(11) 0.013(9) -0.001(10) C99 0.015(8) 0.068(11) 0.129(15) 0.002(10) 0.028(9) -0.005(7) C100 0.034(9) 0.049(9) 0.087(12) -0.003(8) 0.015(8) 0.003(7) C101 0.025(8) 0.033(7) 0.036(8) -0.002(6) 0.016(6) -0.009(6) C102 0.033(9) 0.028(7) 0.064(10) -0.001(7) 0.023(8) -0.001(6) C103 0.074(12) 0.027(7) 0.048(9) 0.013(7) 0.038(9) -0.004(7) C104 0.057(11) 0.049(9) 0.043(9) -0.015(7) 0.023(8) -0.010(8) C105 0.038(9) 0.058(9) 0.053(9) -0.026(7) 0.016(8) -0.020(7) C106 0.031(10) 0.098(12) 0.055(10) -0.014(9) -0.007(8) -0.014(9) C107 0.038(12) 0.112(15) 0.092(14) -0.002(11) 0.012(10) -0.015(10) C108 0.041(12) 0.118(16) 0.116(16) 0.000(13) 0.030(12) -0.003(11) C109 0.051(12) 0.076(11) 0.085(13) -0.023(10) 0.021(10) -0.025(9) C110 0.063(12) 0.069(11) 0.055(10) -0.002(8) 0.025(9) -0.012(9) C111 0.021(8) 0.029(7) 0.049(8) 0.006(6) 0.007(6) 0.005(6) C112 0.047(10) 0.045(8) 0.034(8) 0.013(6) 0.006(7) 0.006(7) C113 0.027(8) 0.030(7) 0.054(9) -0.007(7) 0.007(7) -0.001(6) C114 0.040(9) 0.035(7) 0.041(8) 0.003(6) -0.006(7) 0.027(7) C115 0.047(10) 0.029(7) 0.037(8) 0.011(6) 0.004(7) 0.007(6) C116 0.040(9) 0.037(8) 0.057(10) -0.001(7) 0.013(8) -0.001(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 N7 1.643(11) . ? Ni1 C11 1.941(11) . ? Ni1 C21 1.974(12) . ? Ni1 C1 1.981(10) . ? Ni2 N14 1.633(9) . ? Ni2 C61 1.946(12) . ? Ni2 C41 1.954(11) . ? Ni2 C51 1.965(10) . ? Ni3 N21 1.668(12) . ? Ni3 C91 1.960(12) . ? Ni3 C101 1.980(11) . ? Ni3 C81 2.019(16) . ? B1 N3 1.566(16) . ? B1 C31 1.581(18) . ? B1 N1 1.582(15) . ? B1 N5 1.598(15) . ? B2 N12 1.574(15) . ? B2 N8 1.580(15) . ? B2 N10 1.586(15) . ? B2 C71 1.615(17) . ? B3 N19 1.574(17) . ? B3 N15 1.577(16) . ? B3 N17 1.578(16) . ? B3 C111 1.610(19) . ? N1 C1 1.369(14) . ? N1 C2 1.401(14) . ? N2 C1 1.351(14) . ? N2 C3 1.383(15) . ? N2 C4 1.493(15) . ? N3 C11 1.378(14) . ? N3 C12 1.382(13) . ? N4 C11 1.327(13) . ? N4 C13 1.385(14) . ? N4 C14 1.462(15) . ? N5 C21 1.348(14) . ? N5 C22 1.393(14) . ? N6 C21 1.367(13) . ? N6 C23 1.393(14) . ? N6 C24 1.449(13) . ? N7 O1 1.176(13) . ? N8 C41 1.348(14) . ? N8 C42 1.407(13) . ? N9 C41 1.370(13) . ? N9 C43 1.399(13) . ? N9 C44 1.436(14) . ? N10 C51 1.389(13) . ? N10 C52 1.394(13) . ? N11 C51 1.325(13) . ? N11 C53 1.348(13) . ? N11 C54 1.458(13) . ? N12 C61 1.357(13) . ? N12 C62 1.398(14) . ? N13 C63 1.373(14) . ? N13 C61 1.373(13) . ? N13 C64 1.453(13) . ? N14 O2 1.197(11) . ? N15 C81 1.366(16) . ? N15 C82 1.378(14) . ? N16 C81 1.290(14) . ? N16 C83 1.371(15) . ? N16 C84 1.459(14) . ? N17 C91 1.354(14) . ? N17 C92 1.414(14) . ? N18 C91 1.356(14) . ? N18 C93 1.386(15) . ? N18 C94 1.479(14) . ? N19 C101 1.319(15) . ? N19 C102 1.362(14) . ? N20 C101 1.381(15) . ? N20 C103 1.390(15) . ? N20 C104 1.467(17) . ? N21 O3 1.174(14) . ? O4 C39 1.08(6) . ? O4 C38A 1.28(5) . ? O4 C38 1.29(5) . ? O4 C39A 1.73(6) . ? C2 C3 1.360(16) . ? C4 C5 1.534(18) . ? C5 C10 1.49(2) . ? C5 C6 1.50(2) . ? C6 C7 1.67(3) . ? C7 C8 1.45(3) . ? C8 C9 1.40(3) . ? C9 C10 1.55(3) . ? C12 C13 1.334(16) . ? C14 C15 1.527(18) . ? C15 C16 1.466(18) . ? C15 C20 1.511(19) . ? C16 C17 1.54(2) . ? C17 C18 1.52(2) . ? C18 C19 1.53(2) . ? C19 C20 1.59(2) . ? C22 C23 1.334(16) . ? C24 C25 1.519(15) . ? C25 C26 1.530(15) . ? C25 C30 1.545(16) . ? C26 C27 1.539(15) . ? C27 C28 1.539(17) . ? C28 C29 1.498(17) . ? C29 C30 1.523(15) . ? C31 C32 1.390(15) . ? C31 C36 1.408(16) . ? C32 C33 1.365(17) . ? C33 C34 1.382(18) . ? C34 C35 1.383(17) . ? C35 C36 1.368(17) . ? C37 C38 1.48(3) . ? C38 C39 2.00(6) . ? C39 C40 1.48(3) . ? C37A C38A 1.48(3) . ? C39A C40A 1.49(3) . ? C42 C43 1.331(15) . ? C44 C45 1.456(19) . ? C45 C50 1.33(3) . ? C45 C50A 1.37(4) . ? C45 C46A 1.51(5) . ? C45 C46 1.53(4) . ? C46 C47 1.57(5) . ? C47 C48 1.40(3) . ? C50 C49 1.64(3) . ? C46A C47A 1.57(7) . ? C47A C48 1.40(5) . ? C50A C49 1.69(4) . ? C48 C49 1.54(2) . ? C52 C53 1.375(16) . ? C54 C55A 1.50(6) . ? C54 C55 1.54(3) . ? C55 C60 1.47(3) . ? C55 C56 1.52(3) . ? C56 C57 1.49(3) . ? C57 C58 1.55(3) . ? C58 C59 1.49(3) . ? C59 C60 1.50(3) . ? C55A C56A 1.35(7) . ? C55A C60A 1.67(6) . ? C56A C57A 1.43(5) . ? C57A C58A 1.56(6) . ? C58A C59A 1.54(6) . ? C59A C60A 1.48(5) . ? C62 C63 1.364(15) . ? C64 C65 1.532(15) . ? C65 C70 1.539(16) . ? C65 C66 1.541(15) . ? C66 C67 1.514(16) . ? C67 C68 1.533(18) . ? C68 C69 1.530(17) . ? C69 C70 1.519(15) . ? C71 C72 1.380(14) . ? C71 C76 1.425(15) . ? C72 C73 1.385(16) . ? C73 C74 1.365(17) . ? C74 C75 1.364(15) . ? C75 C76 1.368(16) . ? C82 C83 1.313(15) . ? C84 C85 1.563(15) . ? C85 C86 1.528(16) . ? C85 C90 1.541(16) . ? C86 C87 1.529(16) . ? C87 C88 1.510(17) . ? C88 C89 1.543(19) . ? C89 C90 1.512(16) . ? C92 C93 1.299(16) . ? C94 C95 1.506(17) . ? C95 C100 1.516(18) . ? C95 C96 1.562(17) . ? C96 C97 1.56(2) . ? C97 C98 1.50(2) . ? C98 C99 1.54(2) . ? C99 C100 1.541(18) . ? C102 C103 1.319(18) . ? C104 C105 1.519(18) . ? C105 C110 1.523(18) . ? C105 C106 1.563(19) . ? C106 C107 1.52(2) . ? C107 C108 1.56(2) . ? C108 C109 1.55(2) . ? C109 C110 1.53(2) . ? C111 C112 1.362(17) . ? C111 C116 1.446(17) . ? C112 C113 1.411(17) . ? C113 C114 1.424(17) . ? C114 C115 1.373(18) . ? C115 C116 1.354(17) . ? 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 N7 Ni1 C11 123.2(5) . . ? N7 Ni1 C21 130.2(5) . . ? C11 Ni1 C21 90.0(5) . . ? N7 Ni1 C1 122.8(5) . . ? C11 Ni1 C1 90.8(5) . . ? C21 Ni1 C1 88.5(5) . . ? N14 Ni2 C61 129.6(4) . . ? N14 Ni2 C41 125.7(4) . . ? C61 Ni2 C41 89.6(4) . . ? N14 Ni2 C51 120.4(5) . . ? C61 Ni2 C51 88.6(4) . . ? C41 Ni2 C51 91.5(4) . . ? N21 Ni3 C91 125.7(5) . . ? N21 Ni3 C101 125.5(5) . . ? C91 Ni3 C101 90.1(5) . . ? N21 Ni3 C81 126.2(6) . . ? C91 Ni3 C81 90.7(5) . . ? C101 Ni3 C81 86.9(5) . . ? N3 B1 C31 112.5(9) . . ? N3 B1 N1 105.8(10) . . ? C31 B1 N1 116.3(9) . . ? N3 B1 N5 105.9(9) . . ? C31 B1 N5 112.9(10) . . ? N1 B1 N5 102.3(8) . . ? N12 B2 N8 107.5(8) . . ? N12 B2 N10 103.8(9) . . ? N8 B2 N10 103.5(9) . . ? N12 B2 C71 114.5(9) . . ? N8 B2 C71 108.7(9) . . ? N10 B2 C71 117.9(9) . . ? N19 B3 N15 104.1(10) . . ? N19 B3 N17 107.4(10) . . ? N15 B3 N17 105.9(9) . . ? N19 B3 C111 116.8(10) . . ? N15 B3 C111 112.3(10) . . ? N17 B3 C111 109.7(10) . . ? C1 N1 C2 108.8(9) . . ? C1 N1 B1 118.9(9) . . ? C2 N1 B1 131.9(10) . . ? C1 N2 C3 111.9(10) . . ? C1 N2 C4 125.6(11) . . ? C3 N2 C4 122.5(10) . . ? C11 N3 C12 109.2(9) . . ? C11 N3 B1 121.9(9) . . ? C12 N3 B1 128.9(10) . . ? C11 N4 C13 110.5(10) . . ? C11 N4 C14 124.3(10) . . ? C13 N4 C14 125.1(10) . . ? C21 N5 C22 108.8(9) . . ? C21 N5 B1 120.2(10) . . ? C22 N5 B1 130.4(10) . . ? C21 N6 C23 109.5(10) . . ? C21 N6 C24 125.6(10) . . ? C23 N6 C24 125.0(9) . . ? O1 N7 Ni1 173.6(12) . . ? C41 N8 C42 109.8(9) . . ? C41 N8 B2 121.0(9) . . ? C42 N8 B2 129.2(9) . . ? C41 N9 C43 108.9(9) . . ? C41 N9 C44 123.6(10) . . ? C43 N9 C44 127.5(9) . . ? C51 N10 C52 107.5(9) . . ? C51 N10 B2 119.7(8) . . ? C52 N10 B2 131.8(10) . . ? C51 N11 C53 113.1(9) . . ? C51 N11 C54 122.9(9) . . ? C53 N11 C54 124.0(9) . . ? C61 N12 C62 111.6(9) . . ? C61 N12 B2 118.8(9) . . ? C62 N12 B2 129.3(9) . . ? C63 N13 C61 111.0(9) . . ? C63 N13 C64 125.9(9) . . ? C61 N13 C64 123.1(10) . . ? O2 N14 Ni2 172.7(10) . . ? C81 N15 C82 107.2(10) . . ? C81 N15 B3 120.7(11) . . ? C82 N15 B3 131.1(10) . . ? C81 N16 C83 108.6(11) . . ? C81 N16 C84 124.0(12) . . ? C83 N16 C84 127.2(10) . . ? C91 N17 C92 107.2(9) . . ? C91 N17 B3 121.9(10) . . ? C92 N17 B3 130.9(10) . . ? C91 N18 C93 110.2(10) . . ? C91 N18 C94 122.1(10) . . ? C93 N18 C94 127.5(10) . . ? C101 N19 C102 110.9(11) . . ? C101 N19 B3 116.4(10) . . ? C102 N19 B3 132.3(11) . . ? C101 N20 C103 108.5(11) . . ? C101 N20 C104 124.0(11) . . ? C103 N20 C104 127.4(12) . . ? O3 N21 Ni3 177.8(13) . . ? C39 O4 C38A 110(4) . . ? C39 O4 C38 115(4) . . ? C38A O4 C39A 110(3) . . ? C38 O4 C39A 138(4) . . ? N2 C1 N1 105.6(9) . . ? N2 C1 Ni1 134.6(9) . . ? N1 C1 Ni1 119.7(8) . . ? C3 C2 N1 108.0(11) . . ? C2 C3 N2 105.6(10) . . ? N2 C4 C5 112.9(11) . . ? C10 C5 C6 113.2(16) . . ? C10 C5 C4 113.1(15) . . ? C6 C5 C4 107.3(13) . . ? C5 C6 C7 105.5(17) . . ? C8 C7 C6 110(2) . . ? C9 C8 C7 107(2) . . ? C8 C9 C10 109.7(19) . . ? C5 C10 C9 108.1(17) . . ? N4 C11 N3 105.7(9) . . ? N4 C11 Ni1 136.5(9) . . ? N3 C11 Ni1 117.8(8) . . ? C13 C12 N3 107.2(10) . . ? C12 C13 N4 107.4(10) . . ? N4 C14 C15 111.6(10) . . ? C16 C15 C20 111.7(13) . . ? C16 C15 C14 112.1(12) . . ? C20 C15 C14 110.5(11) . . ? C15 C16 C17 111.9(14) . . ? C18 C17 C16 112.5(14) . . ? C17 C18 C19 112.5(15) . . ? C18 C19 C20 106.2(15) . . ? C15 C20 C19 113.5(13) . . ? N5 C21 N6 106.5(10) . . ? N5 C21 Ni1 119.0(8) . . ? N6 C21 Ni1 132.5(9) . . ? C23 C22 N5 108.6(11) . . ? C22 C23 N6 106.6(11) . . ? N6 C24 C25 115.3(9) . . ? C24 C25 C26 108.9(9) . . ? C24 C25 C30 112.9(10) . . ? C26 C25 C30 110.0(9) . . ? C25 C26 C27 112.3(10) . . ? C26 C27 C28 110.4(11) . . ? C29 C28 C27 110.2(10) . . ? C28 C29 C30 113.4(10) . . ? C29 C30 C25 111.1(10) . . ? C32 C31 C36 115.6(11) . . ? C32 C31 B1 122.1(10) . . ? C36 C31 B1 121.9(10) . . ? C33 C32 C31 123.0(12) . . ? C32 C33 C34 120.0(12) . . ? C33 C34 C35 118.4(13) . . ? C36 C35 C34 121.3(13) . . ? C35 C36 C31 121.1(12) . . ? O4 C38 C37 111(5) . . ? C37 C38 C39 133(5) . . ? O4 C39 C40 125(6) . . ? C40 C39 C38 160(5) . . ? O4 C38A C37A 105(4) . . ? C40A C39A O4 86(4) . . ? N8 C41 N9 106.3(9) . . ? N8 C41 Ni2 118.6(8) . . ? N9 C41 Ni2 135.1(9) . . ? C43 C42 N8 107.0(11) . . ? C42 C43 N9 108.0(10) . . ? N9 C44 C45 113.9(10) . . ? C50 C45 C50A 55.9(19) . . ? C50 C45 C44 125.9(19) . . ? C50A C45 C44 128(2) . . ? C50 C45 C46A 101(3) . . ? C50A C45 C46A 119(3) . . ? C44 C45 C46A 112(3) . . ? C50 C45 C46 116(2) . . ? C50A C45 C46 108(3) . . ? C44 C45 C46 112(2) . . ? C45 C46 C47 114(3) . . ? C48 C47 C46 114(3) . . ? C45 C50 C49 114(2) . . ? C45 C46A C47A 119(4) . . ? C48 C47A C46A 113(4) . . ? C45 C50A C49 109(3) . . ? C47A C48 C47 67(2) . . ? C47A C48 C49 110(2) . . ? C47 C48 C49 110.3(19) . . ? C48 C49 C50 109.8(17) . . ? C48 C49 C50A 110.5(18) . . ? N11 C51 N10 105.9(9) . . ? N11 C51 Ni2 136.0(8) . . ? N10 C51 Ni2 117.9(7) . . ? C53 C52 N10 107.8(10) . . ? N11 C53 C52 105.7(10) . . ? N11 C54 C55A 114(2) . . ? N11 C54 C55 113.0(13) . . ? C60 C55 C56 108.7(19) . . ? C60 C55 C54 115.6(17) . . ? C56 C55 C54 112.1(19) . . ? C57 C56 C55 114.5(18) . . ? C56 C57 C58 109.2(16) . . ? C59 C58 C57 106.7(17) . . ? C58 C59 C60 113.0(17) . . ? C55 C60 C59 114.7(17) . . ? C56A C55A C54 111(4) . . ? C56A C55A C60A 115(4) . . ? C54 C55A C60A 105(4) . . ? C55A C56A C57A 117(4) . . ? C56A C57A C58A 113(4) . . ? C59A C58A C57A 112(4) . . ? C60A C59A C58A 115(4) . . ? C59A C60A C55A 106(3) . . ? N12 C61 N13 104.2(10) . . ? N12 C61 Ni2 120.5(8) . . ? N13 C61 Ni2 134.4(8) . . ? C63 C62 N12 105.6(10) . . ? C62 C63 N13 107.6(10) . . ? N13 C64 C65 114.0(9) . . ? C64 C65 C70 113.4(9) . . ? C64 C65 C66 108.3(9) . . ? C70 C65 C66 111.1(9) . . ? C67 C66 C65 111.4(10) . . ? C66 C67 C68 111.2(10) . . ? C69 C68 C67 112.2(10) . . ? C70 C69 C68 109.8(11) . . ? C69 C70 C65 112.6(10) . . ? C72 C71 C76 115.7(10) . . ? C72 C71 B2 126.8(10) . . ? C76 C71 B2 117.6(9) . . ? C71 C72 C73 121.1(11) . . ? C74 C73 C72 121.9(11) . . ? C75 C74 C73 118.5(12) . . ? C74 C75 C76 120.8(12) . . ? C75 C76 C71 122.0(11) . . ? N16 C81 N15 108.4(13) . . ? N16 C81 Ni3 134.4(11) . . ? N15 C81 Ni3 116.8(8) . . ? C83 C82 N15 106.7(11) . . ? C82 C83 N16 108.9(11) . . ? N16 C84 C85 112.1(9) . . ? C86 C85 C90 110.7(10) . . ? C86 C85 C84 112.8(10) . . ? C90 C85 C84 110.3(10) . . ? C85 C86 C87 112.0(10) . . ? C88 C87 C86 112.8(11) . . ? C87 C88 C89 110.0(11) . . ? C90 C89 C88 111.8(11) . . ? C89 C90 C85 113.3(11) . . ? N17 C91 N18 106.4(10) . . ? N17 C91 Ni3 117.3(8) . . ? N18 C91 Ni3 136.3(9) . . ? C93 C92 N17 109.5(11) . . ? C92 C93 N18 106.7(11) . . ? N18 C94 C95 112.9(10) . . ? C94 C95 C100 116.3(11) . . ? C94 C95 C96 109.6(10) . . ? C100 C95 C96 108.2(11) . . ? C97 C96 C95 111.6(11) . . ? C98 C97 C96 109.3(12) . . ? C97 C98 C99 111.0(13) . . ? C100 C99 C98 110.5(12) . . ? C95 C100 C99 112.7(11) . . ? N19 C101 N20 105.4(10) . . ? N19 C101 Ni3 123.2(9) . . ? N20 C101 Ni3 131.2(10) . . ? C103 C102 N19 108.4(12) . . ? C102 C103 N20 106.7(12) . . ? N20 C104 C105 113.7(10) . . ? C104 C105 C110 112.7(12) . . ? C104 C105 C106 111.8(11) . . ? C110 C105 C106 111.5(12) . . ? C107 C106 C105 110.8(12) . . ? C106 C107 C108 109.9(15) . . ? C109 C108 C107 111.6(14) . . ? C110 C109 C108 109.8(13) . . ? C105 C110 C109 112.9(13) . . ? C112 C111 C116 115.4(12) . . ? C112 C111 B3 121.0(11) . . ? C116 C111 B3 123.2(11) . . ? C111 C112 C113 123.3(12) . . ? C112 C113 C114 118.8(12) . . ? C115 C114 C113 118.3(12) . . ? C116 C115 C114 121.7(13) . . ? C115 C116 C111 122.2(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 B1 N1 C1 54.9(12) . . . . ? C31 B1 N1 C1 -179.4(10) . . . . ? N5 B1 N1 C1 -55.8(12) . . . . ? N3 B1 N1 C2 -132.2(11) . . . . ? C31 B1 N1 C2 -6.5(18) . . . . ? N5 B1 N1 C2 117.1(12) . . . . ? C31 B1 N3 C11 177.8(9) . . . . ? N1 B1 N3 C11 -54.2(13) . . . . ? N5 B1 N3 C11 54.0(13) . . . . ? C31 B1 N3 C12 -1.9(16) . . . . ? N1 B1 N3 C12 126.1(11) . . . . ? N5 B1 N3 C12 -125.7(11) . . . . ? N3 B1 N5 C21 -48.2(13) . . . . ? C31 B1 N5 C21 -171.7(10) . . . . ? N1 B1 N5 C21 62.4(12) . . . . ? N3 B1 N5 C22 141.7(11) . . . . ? C31 B1 N5 C22 18.1(15) . . . . ? N1 B1 N5 C22 -107.7(12) . . . . ? C11 Ni1 N7 O1 -81(9) . . . . ? C21 Ni1 N7 O1 155(9) . . . . ? C1 Ni1 N7 O1 35(9) . . . . ? N12 B2 N8 C41 -51.4(13) . . . . ? N10 B2 N8 C41 58.1(12) . . . . ? C71 B2 N8 C41 -175.8(9) . . . . ? N12 B2 N8 C42 126.5(11) . . . . ? N10 B2 N8 C42 -124.0(11) . . . . ? C71 B2 N8 C42 2.1(15) . . . . ? N12 B2 N10 C51 53.6(12) . . . . ? N8 B2 N10 C51 -58.5(11) . . . . ? C71 B2 N10 C51 -178.5(9) . . . . ? N12 B2 N10 C52 -113.4(11) . . . . ? N8 B2 N10 C52 134.4(10) . . . . ? C71 B2 N10 C52 14.4(17) . . . . ? N8 B2 N12 C61 49.9(12) . . . . ? N10 B2 N12 C61 -59.4(11) . . . . ? C71 B2 N12 C61 170.7(9) . . . . ? N8 B2 N12 C62 -137.3(10) . . . . ? N10 B2 N12 C62 113.4(11) . . . . ? C71 B2 N12 C62 -16.5(15) . . . . ? C61 Ni2 N14 O2 -160(7) . . . . ? C41 Ni2 N14 O2 74(7) . . . . ? C51 Ni2 N14 O2 -43(7) . . . . ? N19 B3 N15 C81 -59.0(13) . . . . ? N17 B3 N15 C81 54.1(14) . . . . ? C111 B3 N15 C81 173.7(10) . . . . ? N19 B3 N15 C82 107.8(13) . . . . ? N17 B3 N15 C82 -139.1(11) . . . . ? C111 B3 N15 C82 -19.4(17) . . . . ? N19 B3 N17 C91 55.9(13) . . . . ? N15 B3 N17 C91 -54.8(14) . . . . ? C111 B3 N17 C91 -176.1(10) . . . . ? N19 B3 N17 C92 -126.6(11) . . . . ? N15 B3 N17 C92 122.7(12) . . . . ? C111 B3 N17 C92 1.3(16) . . . . ? N15 B3 N19 C101 59.0(13) . . . . ? N17 B3 N19 C101 -52.9(13) . . . . ? C111 B3 N19 C101 -176.6(10) . . . . ? N15 B3 N19 C102 -113.6(13) . . . . ? N17 B3 N19 C102 134.5(12) . . . . ? C111 B3 N19 C102 10.8(18) . . . . ? C91 Ni3 N21 O3 77(35) . . . . ? C101 Ni3 N21 O3 -44(35) . . . . ? C81 Ni3 N21 O3 -160(34) . . . . ? C3 N2 C1 N1 0.1(12) . . . . ? C4 N2 C1 N1 -177.6(10) . . . . ? C3 N2 C1 Ni1 176.1(9) . . . . ? C4 N2 C1 Ni1 -1.7(18) . . . . ? C2 N1 C1 N2 0.2(12) . . . . ? B1 N1 C1 N2 174.6(9) . . . . ? C2 N1 C1 Ni1 -176.5(7) . . . . ? B1 N1 C1 Ni1 -2.1(13) . . . . ? N7 Ni1 C1 N2 10.1(13) . . . . ? C11 Ni1 C1 N2 141.4(11) . . . . ? C21 Ni1 C1 N2 -128.6(11) . . . . ? N7 Ni1 C1 N1 -174.4(8) . . . . ? C11 Ni1 C1 N1 -43.1(9) . . . . ? C21 Ni1 C1 N1 46.9(9) . . . . ? C1 N1 C2 C3 -0.4(13) . . . . ? B1 N1 C2 C3 -173.9(11) . . . . ? N1 C2 C3 N2 0.5(13) . . . . ? C1 N2 C3 C2 -0.4(13) . . . . ? C4 N2 C3 C2 177.4(11) . . . . ? C1 N2 C4 C5 -111.6(14) . . . . ? C3 N2 C4 C5 70.9(16) . . . . ? N2 C4 C5 C10 70.7(18) . . . . ? N2 C4 C5 C6 -163.8(15) . . . . ? C10 C5 C6 C7 -53(3) . . . . ? C4 C5 C6 C7 -178.0(19) . . . . ? C5 C6 C7 C8 56(3) . . . . ? C6 C7 C8 C9 -66(3) . . . . ? C7 C8 C9 C10 70(3) . . . . ? C6 C5 C10 C9 57(2) . . . . ? C4 C5 C10 C9 179.4(15) . . . . ? C8 C9 C10 C5 -64(3) . . . . ? C13 N4 C11 N3 -0.4(12) . . . . ? C14 N4 C11 N3 -176.6(10) . . . . ? C13 N4 C11 Ni1 -177.6(9) . . . . ? C14 N4 C11 Ni1 6.1(18) . . . . ? C12 N3 C11 N4 0.6(12) . . . . ? B1 N3 C11 N4 -179.1(9) . . . . ? C12 N3 C11 Ni1 178.5(7) . . . . ? B1 N3 C11 Ni1 -1.2(14) . . . . ? N7 Ni1 C11 N4 -7.8(14) . . . . ? C21 Ni1 C11 N4 132.7(12) . . . . ? C1 Ni1 C11 N4 -138.8(12) . . . . ? N7 Ni1 C11 N3 175.2(8) . . . . ? C21 Ni1 C11 N3 -44.3(9) . . . . ? C1 Ni1 C11 N3 44.2(9) . . . . ? C11 N3 C12 C13 -0.6(13) . . . . ? B1 N3 C12 C13 179.1(11) . . . . ? N3 C12 C13 N4 0.4(13) . . . . ? C11 N4 C13 C12 0.0(14) . . . . ? C14 N4 C13 C12 176.2(11) . . . . ? C11 N4 C14 C15 73.0(14) . . . . ? C13 N4 C14 C15 -102.7(13) . . . . ? N4 C14 C15 C16 70.0(15) . . . . ? N4 C14 C15 C20 -164.7(11) . . . . ? C20 C15 C16 C17 53.1(19) . . . . ? C14 C15 C16 C17 177.7(13) . . . . ? C15 C16 C17 C18 -53(2) . . . . ? C16 C17 C18 C19 56(2) . . . . ? C17 C18 C19 C20 -55(2) . . . . ? C16 C15 C20 C19 -56.6(18) . . . . ? C14 C15 C20 C19 177.9(13) . . . . ? C18 C19 C20 C15 55.9(19) . . . . ? C22 N5 C21 N6 -1.2(12) . . . . ? B1 N5 C21 N6 -173.3(9) . . . . ? C22 N5 C21 Ni1 164.6(7) . . . . ? B1 N5 C21 Ni1 -7.5(13) . . . . ? C23 N6 C21 N5 1.0(12) . . . . ? C24 N6 C21 N5 -179.8(9) . . . . ? C23 N6 C21 Ni1 -162.0(9) . . . . ? C24 N6 C21 Ni1 17.1(17) . . . . ? N7 Ni1 C21 N5 -174.8(8) . . . . ? C11 Ni1 C21 N5 49.4(9) . . . . ? C1 Ni1 C21 N5 -41.4(9) . . . . ? N7 Ni1 C21 N6 -13.4(14) . . . . ? C11 Ni1 C21 N6 -149.2(11) . . . . ? C1 Ni1 C21 N6 120.0(11) . . . . ? C21 N5 C22 C23 1.0(13) . . . . ? B1 N5 C22 C23 172.0(10) . . . . ? N5 C22 C23 N6 -0.3(12) . . . . ? C21 N6 C23 C22 -0.4(12) . . . . ? C24 N6 C23 C22 -179.6(10) . . . . ? C21 N6 C24 C25 97.9(13) . . . . ? C23 N6 C24 C25 -83.0(13) . . . . ? N6 C24 C25 C26 -172.7(9) . . . . ? N6 C24 C25 C30 64.7(13) . . . . ? C24 C25 C26 C27 -179.2(10) . . . . ? C30 C25 C26 C27 -54.9(13) . . . . ? C25 C26 C27 C28 56.4(13) . . . . ? C26 C27 C28 C29 -55.7(13) . . . . ? C27 C28 C29 C30 56.4(15) . . . . ? C28 C29 C30 C25 -55.6(15) . . . . ? C24 C25 C30 C29 175.2(10) . . . . ? C26 C25 C30 C29 53.2(13) . . . . ? N3 B1 C31 C32 86.4(13) . . . . ? N1 B1 C31 C32 -35.9(16) . . . . ? N5 B1 C31 C32 -153.8(10) . . . . ? N3 B1 C31 C36 -86.1(13) . . . . ? N1 B1 C31 C36 151.6(11) . . . . ? N5 B1 C31 C36 33.8(15) . . . . ? C36 C31 C32 C33 -8.9(17) . . . . ? B1 C31 C32 C33 178.3(11) . . . . ? C31 C32 C33 C34 4.6(19) . . . . ? C32 C33 C34 C35 0.7(18) . . . . ? C33 C34 C35 C36 -1.1(19) . . . . ? C34 C35 C36 C31 -3.5(18) . . . . ? C32 C31 C36 C35 8.2(17) . . . . ? B1 C31 C36 C35 -178.9(11) . . . . ? C39 O4 C38 C37 -143(6) . . . . ? C38A O4 C38 C37 -49(4) . . . . ? C39A O4 C38 C37 -111(5) . . . . ? C38A O4 C38 C39 94(6) . . . . ? C39A O4 C38 C39 32(6) . . . . ? C38A O4 C39 C40 145(7) . . . . ? C38 O4 C39 C40 -169(7) . . . . ? C39A O4 C39 C40 49(6) . . . . ? C38A O4 C39 C38 -46(3) . . . . ? C39A O4 C39 C38 -141(6) . . . . ? C37 C38 C39 O4 50(7) . . . . ? O4 C38 C39 C40 26(16) . . . . ? C37 C38 C39 C40 76(21) . . . . ? C39 O4 C38A C37A 141(6) . . . . ? C38 O4 C38A C37A 37(4) . . . . ? C39A O4 C38A C37A 178(4) . . . . ? C39 O4 C39A C40A -26(6) . . . . ? C38A O4 C39A C40A -123(4) . . . . ? C38 O4 C39A C40A -84(6) . . . . ? C42 N8 C41 N9 -0.5(12) . . . . ? B2 N8 C41 N9 177.8(9) . . . . ? C42 N8 C41 Ni2 178.8(7) . . . . ? B2 N8 C41 Ni2 -2.9(13) . . . . ? C43 N9 C41 N8 0.1(12) . . . . ? C44 N9 C41 N8 -179.2(9) . . . . ? C43 N9 C41 Ni2 -179.0(9) . . . . ? C44 N9 C41 Ni2 1.7(17) . . . . ? N14 Ni2 C41 N8 -172.9(8) . . . . ? C61 Ni2 C41 N8 45.8(9) . . . . ? C51 Ni2 C41 N8 -42.9(9) . . . . ? N14 Ni2 C41 N9 6.1(13) . . . . ? C61 Ni2 C41 N9 -135.2(11) . . . . ? C51 Ni2 C41 N9 136.2(11) . . . . ? C41 N8 C42 C43 0.7(13) . . . . ? B2 N8 C42 C43 -177.4(10) . . . . ? N8 C42 C43 N9 -0.6(12) . . . . ? C41 N9 C43 C42 0.3(12) . . . . ? C44 N9 C43 C42 179.6(10) . . . . ? C41 N9 C44 C45 -92.6(15) . . . . ? C43 N9 C44 C45 88.2(16) . . . . ? N9 C44 C45 C50 41(3) . . . . ? N9 C44 C45 C50A -31(3) . . . . ? N9 C44 C45 C46A 163(2) . . . . ? N9 C44 C45 C46 -168(2) . . . . ? C50 C45 C46 C47 -40(4) . . . . ? C50A C45 C46 C47 20(4) . . . . ? C44 C45 C46 C47 165(3) . . . . ? C46A C45 C46 C47 -100(9) . . . . ? C45 C46 C47 C48 45(4) . . . . ? C50A C45 C50 C49 -50(3) . . . . ? C44 C45 C50 C49 -164.8(18) . . . . ? C46A C45 C50 C49 68(4) . . . . ? C46 C45 C50 C49 44(4) . . . . ? C50 C45 C46A C47A -26(5) . . . . ? C50A C45 C46A C47A 31(6) . . . . ? C44 C45 C46A C47A -162(4) . . . . ? C46 C45 C46A C47A 101(10) . . . . ? C45 C46A C47A C48 -36(6) . . . . ? C50 C45 C50A C49 45(2) . . . . ? C44 C45 C50A C49 157.2(18) . . . . ? C46A C45 C50A C49 -38(4) . . . . ? C46 C45 C50A C49 -65(3) . . . . ? C46A C47A C48 C47 -51(3) . . . . ? C46A C47A C48 C49 53(4) . . . . ? C46 C47 C48 C47A 49(3) . . . . ? C46 C47 C48 C49 -54(4) . . . . ? C47A C48 C49 C50 -15(3) . . . . ? C47 C48 C49 C50 56(3) . . . . ? C47A C48 C49 C50A -63(3) . . . . ? C47 C48 C49 C50A 8(3) . . . . ? C45 C50 C49 C48 -53(3) . . . . ? C45 C50 C49 C50A 47(3) . . . . ? C45 C50A C49 C48 55(3) . . . . ? C45 C50A C49 C50 -43(2) . . . . ? C53 N11 C51 N10 -0.2(12) . . . . ? C54 N11 C51 N10 178.8(9) . . . . ? C53 N11 C51 Ni2 -175.0(9) . . . . ? C54 N11 C51 Ni2 4.1(17) . . . . ? C52 N10 C51 N11 -1.1(11) . . . . ? B2 N10 C51 N11 -171.0(9) . . . . ? C52 N10 C51 Ni2 174.8(7) . . . . ? B2 N10 C51 Ni2 4.9(12) . . . . ? N14 Ni2 C51 N11 -10.5(13) . . . . ? C61 Ni2 C51 N11 126.0(11) . . . . ? C41 Ni2 C51 N11 -144.4(11) . . . . ? N14 Ni2 C51 N10 175.2(7) . . . . ? C61 Ni2 C51 N10 -48.3(8) . . . . ? C41 Ni2 C51 N10 41.3(8) . . . . ? C51 N10 C52 C53 2.0(12) . . . . ? B2 N10 C52 C53 170.2(10) . . . . ? C51 N11 C53 C52 1.4(13) . . . . ? C54 N11 C53 C52 -177.6(10) . . . . ? N10 C52 C53 N11 -2.0(12) . . . . ? C51 N11 C54 C55A 111(2) . . . . ? C53 N11 C54 C55A -70(2) . . . . ? C51 N11 C54 C55 88.6(14) . . . . ? C53 N11 C54 C55 -92.4(15) . . . . ? N11 C54 C55 C60 63(2) . . . . ? C55A C54 C55 C60 -34(7) . . . . ? N11 C54 C55 C56 -171.5(14) . . . . ? C55A C54 C55 C56 91(8) . . . . ? C60 C55 C56 C57 -52(3) . . . . ? C54 C55 C56 C57 178.4(17) . . . . ? C55 C56 C57 C58 59(2) . . . . ? C56 C57 C58 C59 -59(2) . . . . ? C57 C58 C59 C60 58(2) . . . . ? C56 C55 C60 C59 49(3) . . . . ? C54 C55 C60 C59 176.2(18) . . . . ? C58 C59 C60 C55 -56(3) . . . . ? N11 C54 C55A C56A -78(4) . . . . ? C55 C54 C55A C56A 14(5) . . . . ? N11 C54 C55A C60A 157(2) . . . . ? C55 C54 C55A C60A -111(9) . . . . ? C54 C55A C56A C57A -172(4) . . . . ? C60A C55A C56A C57A -53(6) . . . . ? C55A C56A C57A C58A 48(6) . . . . ? C56A C57A C58A C59A -43(5) . . . . ? C57A C58A C59A C60A 49(5) . . . . ? C58A C59A C60A C55A -50(4) . . . . ? C56A C55A C60A C59A 52(5) . . . . ? C54 C55A C60A C59A 175(3) . . . . ? C62 N12 C61 N13 1.7(11) . . . . ? B2 N12 C61 N13 175.7(9) . . . . ? C62 N12 C61 Ni2 -169.4(7) . . . . ? B2 N12 C61 Ni2 4.6(13) . . . . ? C63 N13 C61 N12 -2.0(12) . . . . ? C64 N13 C61 N12 179.7(9) . . . . ? C63 N13 C61 Ni2 167.1(9) . . . . ? C64 N13 C61 Ni2 -11.1(16) . . . . ? N14 Ni2 C61 N12 173.9(7) . . . . ? C41 Ni2 C61 N12 -47.3(9) . . . . ? C51 Ni2 C61 N12 44.2(9) . . . . ? N14 Ni2 C61 N13 6.1(13) . . . . ? C41 Ni2 C61 N13 144.9(11) . . . . ? C51 Ni2 C61 N13 -123.6(11) . . . . ? C61 N12 C62 C63 -0.7(12) . . . . ? B2 N12 C62 C63 -173.9(10) . . . . ? N12 C62 C63 N13 -0.6(12) . . . . ? C61 N13 C63 C62 1.7(13) . . . . ? C64 N13 C63 C62 179.9(9) . . . . ? C63 N13 C64 C65 82.8(13) . . . . ? C61 N13 C64 C65 -99.2(12) . . . . ? N13 C64 C65 C70 -66.3(12) . . . . ? N13 C64 C65 C66 169.9(9) . . . . ? C64 C65 C66 C67 178.7(10) . . . . ? C70 C65 C66 C67 53.6(12) . . . . ? C65 C66 C67 C68 -54.7(13) . . . . ? C66 C67 C68 C69 56.4(14) . . . . ? C67 C68 C69 C70 -55.8(14) . . . . ? C68 C69 C70 C65 55.0(13) . . . . ? C64 C65 C70 C69 -176.6(9) . . . . ? C66 C65 C70 C69 -54.4(12) . . . . ? N12 B2 C71 C72 145.1(11) . . . . ? N8 B2 C71 C72 -94.7(12) . . . . ? N10 B2 C71 C72 22.6(16) . . . . ? N12 B2 C71 C76 -36.9(14) . . . . ? N8 B2 C71 C76 83.3(12) . . . . ? N10 B2 C71 C76 -159.4(10) . . . . ? C76 C71 C72 C73 2.1(16) . . . . ? B2 C71 C72 C73 -179.9(11) . . . . ? C71 C72 C73 C74 0.5(17) . . . . ? C72 C73 C74 C75 -3.0(17) . . . . ? C73 C74 C75 C76 2.6(16) . . . . ? C74 C75 C76 C71 0.2(17) . . . . ? C72 C71 C76 C75 -2.5(16) . . . . ? B2 C71 C76 C75 179.3(10) . . . . ? C83 N16 C81 N15 -3.7(14) . . . . ? C84 N16 C81 N15 -178.9(9) . . . . ? C83 N16 C81 Ni3 167.8(10) . . . . ? C84 N16 C81 Ni3 -7.3(19) . . . . ? C82 N15 C81 N16 4.0(13) . . . . ? B3 N15 C81 N16 173.6(10) . . . . ? C82 N15 C81 Ni3 -169.3(8) . . . . ? B3 N15 C81 Ni3 0.4(14) . . . . ? N21 Ni3 C81 N16 6.4(16) . . . . ? C91 Ni3 C81 N16 143.5(13) . . . . ? C101 Ni3 C81 N16 -126.5(13) . . . . ? N21 Ni3 C81 N15 177.4(8) . . . . ? C91 Ni3 C81 N15 -45.5(10) . . . . ? C101 Ni3 C81 N15 44.5(10) . . . . ? C81 N15 C82 C83 -2.6(13) . . . . ? B3 N15 C82 C83 -170.8(12) . . . . ? N15 C82 C83 N16 0.4(13) . . . . ? C81 N16 C83 C82 2.1(14) . . . . ? C84 N16 C83 C82 177.0(10) . . . . ? C81 N16 C84 C85 -96.3(13) . . . . ? C83 N16 C84 C85 89.5(13) . . . . ? N16 C84 C85 C86 -63.2(13) . . . . ? N16 C84 C85 C90 172.4(9) . . . . ? C90 C85 C86 C87 -51.7(13) . . . . ? C84 C85 C86 C87 -175.8(10) . . . . ? C85 C86 C87 C88 55.4(15) . . . . ? C86 C87 C88 C89 -55.6(15) . . . . ? C87 C88 C89 C90 54.7(14) . . . . ? C88 C89 C90 C85 -54.0(14) . . . . ? C86 C85 C90 C89 52.1(14) . . . . ? C84 C85 C90 C89 177.6(10) . . . . ? C92 N17 C91 N18 -0.1(12) . . . . ? B3 N17 C91 N18 177.9(9) . . . . ? C92 N17 C91 Ni3 -179.3(7) . . . . ? B3 N17 C91 Ni3 -1.3(14) . . . . ? C93 N18 C91 N17 -0.4(12) . . . . ? C94 N18 C91 N17 -176.0(9) . . . . ? C93 N18 C91 Ni3 178.6(10) . . . . ? C94 N18 C91 Ni3 3.0(17) . . . . ? N21 Ni3 C91 N17 -176.9(8) . . . . ? C101 Ni3 C91 N17 -41.2(9) . . . . ? C81 Ni3 C91 N17 45.8(9) . . . . ? N21 Ni3 C91 N18 4.3(15) . . . . ? C101 Ni3 C91 N18 140.0(12) . . . . ? C81 Ni3 C91 N18 -133.1(12) . . . . ? C91 N17 C92 C93 0.5(13) . . . . ? B3 N17 C92 C93 -177.2(11) . . . . ? N17 C92 C93 N18 -0.7(13) . . . . ? C91 N18 C93 C92 0.7(13) . . . . ? C94 N18 C93 C92 176.0(11) . . . . ? C91 N18 C94 C95 -112.1(12) . . . . ? C93 N18 C94 C95 73.1(15) . . . . ? N18 C94 C95 C100 66.1(15) . . . . ? N18 C94 C95 C96 -170.8(10) . . . . ? C94 C95 C96 C97 175.4(12) . . . . ? C100 C95 C96 C97 -56.8(15) . . . . ? C95 C96 C97 C98 59.0(18) . . . . ? C96 C97 C98 C99 -58.2(18) . . . . ? C97 C98 C99 C100 57.2(19) . . . . ? C94 C95 C100 C99 179.6(12) . . . . ? C96 C95 C100 C99 55.8(16) . . . . ? C98 C99 C100 C95 -56.6(18) . . . . ? C102 N19 C101 N20 -2.3(13) . . . . ? B3 N19 C101 N20 -176.5(9) . . . . ? C102 N19 C101 Ni3 173.0(8) . . . . ? B3 N19 C101 Ni3 -1.2(14) . . . . ? C103 N20 C101 N19 1.0(13) . . . . ? C104 N20 C101 N19 -174.9(10) . . . . ? C103 N20 C101 Ni3 -173.8(9) . . . . ? C104 N20 C101 Ni3 10.3(18) . . . . ? N21 Ni3 C101 N19 -179.5(9) . . . . ? C91 Ni3 C101 N19 44.6(10) . . . . ? C81 Ni3 C101 N19 -46.1(10) . . . . ? N21 Ni3 C101 N20 -5.5(14) . . . . ? C91 Ni3 C101 N20 -141.4(11) . . . . ? C81 Ni3 C101 N20 127.9(12) . . . . ? C101 N19 C102 C103 2.9(15) . . . . ? B3 N19 C102 C103 175.8(12) . . . . ? N19 C102 C103 N20 -2.1(14) . . . . ? C101 N20 C103 C102 0.7(14) . . . . ? C104 N20 C103 C102 176.4(12) . . . . ? C101 N20 C104 C105 74.1(15) . . . . ? C103 N20 C104 C105 -101.0(14) . . . . ? N20 C104 C105 C110 65.4(15) . . . . ? N20 C104 C105 C106 -168.1(11) . . . . ? C104 C105 C106 C107 177.5(12) . . . . ? C110 C105 C106 C107 -55.3(17) . . . . ? C105 C106 C107 C108 56.5(18) . . . . ? C106 C107 C108 C109 -57.8(19) . . . . ? C107 C108 C109 C110 55.9(19) . . . . ? C104 C105 C110 C109 -178.7(12) . . . . ? C106 C105 C110 C109 54.5(17) . . . . ? C108 C109 C110 C105 -54.5(17) . . . . ? N19 B3 C111 C112 -157.3(11) . . . . ? N15 B3 C111 C112 -37.2(16) . . . . ? N17 B3 C111 C112 80.2(14) . . . . ? N19 B3 C111 C116 30.2(16) . . . . ? N15 B3 C111 C116 150.3(11) . . . . ? N17 B3 C111 C116 -92.3(13) . . . . ? C116 C111 C112 C113 -4.6(18) . . . . ? B3 C111 C112 C113 -177.6(11) . . . . ? C111 C112 C113 C114 1.2(19) . . . . ? C112 C113 C114 C115 0.4(17) . . . . ? C113 C114 C115 C116 2.0(18) . . . . ? C114 C115 C116 C111 -5.9(19) . . . . ? C112 C111 C116 C115 7.0(18) . . . . ? B3 C111 C116 C115 179.9(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.721 _refine_diff_density_min -1.448 _refine_diff_density_rms 0.225 _iucr_refine_instruction_details ; TITL mar15p1 in P21/c CELL 0.71073 26.3450 37.4250 11.4322 90.000 99.762 90.000 ZERR 4 0.0060 0.0070 0.0019 0.000 0.013 0.000 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H B N Ni O UNIT 448 640 12 84 12 16 L.S. 10 ACTA BOND FMAP 2 PLAN 10 SIZE 0.08 0.159 0.396 CONF SADI c37 c38 c37a c38a c39 c40 c39a c40a EADP c55 c56 c57 c58 c59 c60 c55a c56a c57a c58a c59a c60a DELU C37 C38 C39 C40 C37A C38A C39A C40A DELU C45 C46 C47 C48 C49 C50 C46A C47A C50A SIMU C37 C38 C39 C40 C37A C38A C39A C40A SIMU C45 C46 C47 C48 C49 C50 C46A C47A C50A TEMP -100.150 WGHT 0.165600 FVAR 0.04178 0.57477 0.67703 0.49115 NI1 5 0.232987 0.986687 0.360633 11.00000 0.02200 0.03170 = 0.02736 0.00003 0.00771 -0.00090 NI2 5 0.213869 0.832664 0.837520 11.00000 0.02369 0.02623 = 0.02062 0.00165 0.00593 0.00218 NI3 5 0.253650 1.158856 0.868286 11.00000 0.02605 0.04166 = 0.03400 0.00207 0.00879 0.00027 B1 3 0.161993 0.971906 0.116505 11.00000 0.03735 0.02086 = 0.02543 0.00488 0.00763 0.00426 B2 3 0.146814 0.853717 0.595661 11.00000 0.01217 0.03254 = 0.02770 0.00952 0.00513 -0.00522 B3 3 0.187683 1.184519 0.631334 11.00000 0.02264 0.03568 = 0.03707 0.00238 0.01687 0.00278 N1 4 0.196902 0.938775 0.163171 11.00000 0.02048 0.02721 = 0.02778 -0.00563 0.00594 0.00385 N2 4 0.250049 0.908533 0.291315 11.00000 0.01806 0.03209 = 0.05087 0.00416 0.00943 0.00593 N3 4 0.199715 1.004232 0.116588 11.00000 0.02656 0.02480 = 0.03493 0.01009 0.01570 0.00184 N4 4 0.258772 1.042266 0.185364 11.00000 0.02972 0.03148 = 0.02819 0.00315 0.00953 -0.00751 N5 4 0.131292 0.979006 0.223440 11.00000 0.02889 0.03068 = 0.02692 0.00189 0.01344 0.01304 N6 4 0.121564 0.988370 0.406139 11.00000 0.01964 0.02639 = 0.02872 0.00359 0.01380 0.00649 N7 4 0.274275 0.993188 0.483533 11.00000 0.04548 0.03860 = 0.02012 -0.00040 0.00394 -0.01966 N8 4 0.178378 0.817956 0.592124 11.00000 0.01962 0.03638 = 0.01613 0.00408 0.00613 0.00541 N9 4 0.228201 0.773501 0.658629 11.00000 0.02944 0.02093 = 0.03373 0.00051 0.01516 0.00363 N10 4 0.189741 0.882417 0.642808 11.00000 0.02022 0.02654 = 0.02018 0.00260 0.01294 0.00201 N11 4 0.247180 0.907639 0.775028 11.00000 0.01990 0.02251 = 0.02028 0.00478 0.00058 -0.00043 N12 4 0.114973 0.850262 0.699817 11.00000 0.02744 0.02546 = 0.01520 0.00082 0.00315 -0.00305 N13 4 0.102661 0.842041 0.879388 11.00000 0.02539 0.02642 = 0.02419 -0.00064 0.01272 -0.00046 N14 4 0.252503 0.823768 0.961493 11.00000 0.01903 0.03020 = 0.01962 -0.00211 0.00044 0.01040 N15 4 0.155447 1.182074 0.735374 11.00000 0.03488 0.02612 = 0.04202 0.00457 0.02450 0.00766 N16 4 0.145140 1.174904 0.916837 11.00000 0.01659 0.02904 = 0.03851 0.00223 0.02365 -0.00297 N17 4 0.213211 1.146601 0.624505 11.00000 0.02390 0.02726 = 0.02530 0.00518 0.00570 -0.00161 N18 4 0.256626 1.098836 0.684467 11.00000 0.01929 0.03886 = 0.04188 -0.00457 0.01416 -0.00078 N19 4 0.232101 1.211658 0.678557 11.00000 0.03000 0.02412 = 0.03650 0.00107 0.00699 -0.01081 N20 4 0.295793 1.231488 0.804410 11.00000 0.04531 0.03650 = 0.04110 -0.01826 0.01372 -0.00380 N21 4 0.290559 1.146481 0.995075 11.00000 0.03757 0.05860 = 0.04500 0.01280 -0.00744 -0.01345 O1 6 0.307087 0.995862 0.566780 11.00000 0.08966 0.08689 = 0.05393 0.00538 -0.02578 -0.04498 O2 6 0.285137 0.818629 1.046245 11.00000 0.05480 0.06661 = 0.04601 0.01080 -0.01776 0.01325 O3 6 0.317922 1.138072 1.082738 11.00000 0.11732 0.15496 = 0.07282 0.05469 -0.05091 -0.04347 O4 6 0.387819 0.324401 0.884436 11.00000 0.10034 0.22857 = 0.25562 -0.05996 0.12856 -0.05253 C1 1 0.229114 0.941330 0.270160 11.00000 0.01844 0.02393 = 0.03977 -0.00899 0.02031 -0.00690 C2 1 0.198761 0.903769 0.120566 11.00000 0.03113 0.02816 = 0.04408 -0.00397 0.00667 -0.00288 AFIX 43 H2 2 0.179868 0.894825 0.048323 11.00000 -1.20000 AFIX 0 C3 1 0.232336 0.884849 0.200724 11.00000 0.02418 0.03155 = 0.05039 -0.00552 0.02034 0.00115 AFIX 43 H3 2 0.241675 0.860453 0.195571 11.00000 -1.20000 AFIX 0 C4 1 0.286458 0.897660 0.400177 11.00000 0.04128 0.05339 = 0.04099 0.00953 0.00360 0.01187 AFIX 23 H4A 2 0.273011 0.875935 0.433758 11.00000 -1.20000 H4B 2 0.288109 0.916899 0.460138 11.00000 -1.20000 AFIX 0 C5 1 0.340990 0.890102 0.376162 11.00000 0.02651 0.12516 = 0.05430 0.01767 0.00278 0.02925 AFIX 13 H5 2 0.337829 0.874127 0.305176 11.00000 -1.20000 AFIX 0 C6 1 0.368714 0.869729 0.480396 11.00000 0.03795 0.22331 = 0.14515 0.07168 -0.00345 0.02214 AFIX 23 H6A 2 0.351570 0.846537 0.488504 11.00000 -1.20000 H6B 2 0.369522 0.883543 0.554539 11.00000 -1.20000 AFIX 0 C7 1 0.428261 0.863428 0.452577 11.00000 0.10280 0.26888 = 0.16458 0.05771 -0.01357 0.12113 AFIX 23 H7A 2 0.449408 0.851123 0.520588 11.00000 -1.20000 H7B 2 0.427062 0.848179 0.381400 11.00000 -1.20000 AFIX 0 C8 1 0.451277 0.897676 0.432955 11.00000 0.04722 0.24386 = 0.20868 0.16866 -0.02595 -0.05887 AFIX 23 H8A 2 0.449650 0.913909 0.500594 11.00000 -1.20000 H8B 2 0.487833 0.894496 0.424913 11.00000 -1.20000 AFIX 0 C9 1 0.423245 0.911962 0.328262 11.00000 0.01899 0.31033 = 0.19302 0.16727 0.04703 0.02791 AFIX 23 H9A 2 0.420232 0.893943 0.264057 11.00000 -1.20000 H9B 2 0.441476 0.933050 0.303462 11.00000 -1.20000 AFIX 0 C10 1 0.368799 0.923050 0.349397 11.00000 0.08493 0.10452 = 0.09879 0.02200 0.00311 0.01493 AFIX 23 H10A 2 0.371595 0.939972 0.416747 11.00000 -1.20000 H10B 2 0.349770 0.934938 0.277799 11.00000 -1.20000 AFIX 0 C11 1 0.233831 1.013940 0.216558 11.00000 0.02378 0.02205 = 0.02833 -0.00353 0.00720 0.00486 C12 1 0.205235 1.027157 0.024782 11.00000 0.03196 0.03897 = 0.01479 0.00628 0.00662 -0.00154 AFIX 43 H12 2 0.186605 1.026253 -0.053956 11.00000 -1.20000 AFIX 0 C13 1 0.241616 1.050793 0.067404 11.00000 0.03991 0.03062 = 0.03925 0.00040 0.01915 -0.00431 AFIX 43 H13 2 0.253549 1.069939 0.024713 11.00000 -1.20000 AFIX 0 C14 1 0.300787 1.060266 0.263163 11.00000 0.04197 0.04435 = 0.02349 -0.00418 0.00666 -0.00972 AFIX 23 H14A 2 0.290554 1.064559 0.341394 11.00000 -1.20000 H14B 2 0.307271 1.083744 0.228616 11.00000 -1.20000 AFIX 0 C15 1 0.350194 1.038162 0.280081 11.00000 0.02816 0.05138 = 0.05271 -0.00562 0.00945 -0.00440 AFIX 13 H15 2 0.340909 1.013183 0.299250 11.00000 -1.20000 AFIX 0 C16 1 0.372938 1.036650 0.171666 11.00000 0.05753 0.08684 = 0.07183 -0.01635 0.02221 0.00686 AFIX 23 H16A 2 0.379341 1.061265 0.145983 11.00000 -1.20000 H16B 2 0.348247 1.025195 0.107719 11.00000 -1.20000 AFIX 0 C17 1 0.423810 1.015619 0.190423 11.00000 0.05495 0.11016 = 0.07472 -0.02499 0.02030 -0.00331 AFIX 23 H17A 2 0.416497 0.990112 0.203393 11.00000 -1.20000 H17B 2 0.439453 1.017307 0.117755 11.00000 -1.20000 AFIX 0 C18 1 0.461957 1.029330 0.295306 11.00000 0.04549 0.10566 = 0.13757 -0.00685 0.03429 0.00650 AFIX 23 H18A 2 0.472326 1.053957 0.278264 11.00000 -1.20000 H18B 2 0.493184 1.014158 0.305794 11.00000 -1.20000 AFIX 0 C19 1 0.439768 1.029367 0.410628 11.00000 0.04925 0.11435 = 0.08944 -0.01106 0.01560 0.00143 AFIX 23 H19A 2 0.464361 1.040430 0.475627 11.00000 -1.20000 H19B 2 0.432533 1.004651 0.433929 11.00000 -1.20000 AFIX 0 C20 1 0.388125 1.051934 0.384471 11.00000 0.05143 0.10196 = 0.07431 -0.01802 0.02085 -0.01994 AFIX 23 H20A 2 0.371548 1.051673 0.455974 11.00000 -1.20000 H20B 2 0.396759 1.077045 0.368950 11.00000 -1.20000 AFIX 0 C21 1 0.156974 0.988116 0.331543 11.00000 0.02322 0.03819 = 0.02914 0.00528 0.01287 0.01350 C22 1 0.079879 0.972846 0.231617 11.00000 0.02596 0.03488 = 0.02734 0.00645 -0.00117 0.00350 AFIX 43 H22 2 0.053708 0.965701 0.168234 11.00000 -1.20000 AFIX 0 C23 1 0.073532 0.978659 0.343353 11.00000 0.02091 0.03056 = 0.04930 0.00674 0.01018 -0.00569 AFIX 43 H23 2 0.042348 0.976582 0.374103 11.00000 -1.20000 AFIX 0 C24 1 0.132159 0.996873 0.531560 11.00000 0.02564 0.03468 = 0.02763 0.00911 0.01545 0.00853 AFIX 23 H24A 2 0.169107 0.992334 0.561384 11.00000 -1.20000 H24B 2 0.112088 0.980379 0.573777 11.00000 -1.20000 AFIX 0 C25 1 0.119853 1.034955 0.563092 11.00000 0.02596 0.03524 = 0.02222 0.00252 0.00433 0.01172 AFIX 13 H25 2 0.138681 1.051571 0.516930 11.00000 -1.20000 AFIX 0 C26 1 0.139523 1.041066 0.695363 11.00000 0.03097 0.03872 = 0.03160 0.00390 0.01403 0.00367 AFIX 23 H26A 2 0.177197 1.037026 0.712029 11.00000 -1.20000 H26B 2 0.123233 1.023467 0.742016 11.00000 -1.20000 AFIX 0 C27 1 0.127870 1.079021 0.735290 11.00000 0.03758 0.04068 = 0.03573 0.00465 0.01319 0.00263 AFIX 23 H27A 2 0.146869 1.096670 0.694767 11.00000 -1.20000 H27B 2 0.139632 1.081390 0.821894 11.00000 -1.20000 AFIX 0 C28 1 0.069717 1.086730 0.705578 11.00000 0.03994 0.04366 = 0.05152 -0.00901 0.00681 0.01175 AFIX 23 H28A 2 0.050994 1.070718 0.752514 11.00000 -1.20000 H28B 2 0.062991 1.111713 0.726969 11.00000 -1.20000 AFIX 0 C29 1 0.050655 1.081001 0.575853 11.00000 0.03067 0.03678 = 0.05394 -0.00273 0.00276 0.01252 AFIX 23 H29A 2 0.067016 1.098808 0.530090 11.00000 -1.20000 H29B 2 0.013009 1.085168 0.559263 11.00000 -1.20000 AFIX 0 C30 1 0.061769 1.043696 0.533314 11.00000 0.02326 0.04351 = 0.04045 -0.00853 -0.00259 0.01039 AFIX 23 H30A 2 0.050239 1.042114 0.446428 11.00000 -1.20000 H30B 2 0.042133 1.025898 0.571637 11.00000 -1.20000 AFIX 0 C31 1 0.125265 0.967039 -0.006980 11.00000 0.01595 0.02420 = 0.04055 0.00629 0.01170 0.00805 C32 1 0.139759 0.947381 -0.099030 11.00000 0.02527 0.03506 = 0.03558 0.00914 0.00830 0.01877 AFIX 43 H32 2 0.173234 0.937144 -0.087571 11.00000 -1.20000 AFIX 0 C33 1 0.108109 0.942101 -0.205184 11.00000 0.04484 0.03803 = 0.04090 -0.00149 0.02120 -0.00376 AFIX 43 H33 2 0.118747 0.927016 -0.263340 11.00000 -1.20000 AFIX 0 C34 1 0.060613 0.958691 -0.228047 11.00000 0.05455 0.03689 = 0.04471 -0.00468 0.01194 -0.01642 AFIX 43 H34 2 0.038093 0.955035 -0.301237 11.00000 -1.20000 AFIX 0 C35 1 0.046653 0.980756 -0.141749 11.00000 0.02199 0.04893 = 0.04615 0.00872 0.00834 0.01111 AFIX 43 H35 2 0.014373 0.992687 -0.156735 11.00000 -1.20000 AFIX 0 C36 1 0.078403 0.985738 -0.035270 11.00000 0.03604 0.04541 = 0.03131 0.00513 0.01682 -0.00791 AFIX 43 H36 2 0.068678 1.002087 0.020538 11.00000 -1.20000 PART -1 AFIX 0 C37 1 0.326634 0.326634 1.004841 41.00000 0.06863 0.05389 = 0.07251 -0.00232 0.01463 0.00621 AFIX 33 H37A 2 0.300791 0.342782 1.028048 41.00000 -1.50000 H37B 2 0.352262 0.320700 1.074716 41.00000 -1.50000 H37C 2 0.309786 0.304703 0.971242 41.00000 -1.50000 AFIX 0 C38 1 0.352476 0.344381 0.914751 41.00000 0.05930 0.10576 = 0.11906 0.00688 0.04804 0.00192 AFIX 23 H38A 2 0.326615 0.349998 0.843726 41.00000 -1.20000 H38B 2 0.367949 0.367148 0.947423 41.00000 -1.20000 AFIX 0 C39 1 0.421788 0.338557 0.868139 41.00000 0.07427 0.17189 = 0.16837 -0.03799 0.06238 0.02446 AFIX 23 H39A 2 0.438413 0.348176 0.945922 41.00000 -1.20000 H39B 2 0.409092 0.359474 0.818694 41.00000 -1.20000 AFIX 0 C40 1 0.463717 0.322872 0.813344 41.00000 0.06344 0.13302 = 0.11928 -0.03205 0.04207 0.01741 AFIX 33 H40A 2 0.491187 0.340554 0.813799 41.00000 -1.50000 H40B 2 0.450173 0.315912 0.731351 41.00000 -1.50000 H40C 2 0.477545 0.301768 0.858612 41.00000 -1.50000 PART -2 AFIX 0 C37A 1 0.317159 0.336081 0.954815 -41.00000 0.05557 0.09650 = 0.09869 -0.00129 0.03369 0.03420 AFIX 33 H37D 2 0.303795 0.343955 1.025506 -41.00000 -1.50000 H37E 2 0.304193 0.312066 0.932408 -41.00000 -1.50000 H37F 2 0.305764 0.352673 0.889303 -41.00000 -1.50000 AFIX 0 C38A 1 0.374251 0.335396 0.980888 -41.00000 0.05313 0.10582 = 0.08946 0.00911 0.02356 0.00439 AFIX 23 H38C 2 0.388210 0.359549 1.001913 -41.00000 -1.20000 H38D 2 0.386609 0.318884 1.047277 -41.00000 -1.20000 AFIX 0 C39A 1 0.454489 0.323463 0.900902 -41.00000 0.05752 0.16402 = 0.17935 -0.06531 0.03790 -0.01991 AFIX 23 H39C 2 0.472456 0.334596 0.975048 -41.00000 -1.20000 H39D 2 0.469041 0.299697 0.887783 -41.00000 -1.20000 AFIX 0 C40A 1 0.447993 0.347358 0.795693 -41.00000 0.08927 0.16290 = 0.16170 -0.07643 0.01296 -0.01774 AFIX 33 H40D 2 0.481754 0.352401 0.774286 -41.00000 -1.50000 H40E 2 0.431939 0.369790 0.814451 -41.00000 -1.50000 H40F 2 0.426000 0.335651 0.728920 -41.00000 -1.50000 PART 0 AFIX 0 C41 1 0.207998 0.805023 0.690797 11.00000 0.01463 0.02863 = 0.03406 -0.00034 0.01091 -0.00203 C42 1 0.180069 0.794661 0.496311 11.00000 0.03110 0.02734 = 0.03259 -0.00169 0.01938 0.01101 AFIX 43 H42 2 0.162851 0.797764 0.416967 11.00000 -1.20000 AFIX 0 C43 1 0.210371 0.767438 0.537881 11.00000 0.02847 0.03474 = 0.02435 -0.00486 0.00908 -0.00381 AFIX 43 H43 2 0.218464 0.747416 0.493384 11.00000 -1.20000 AFIX 0 C44 1 0.261627 0.751068 0.739724 11.00000 0.01529 0.03899 = 0.03052 0.00245 0.01089 0.00587 AFIX 23 H44A 2 0.254692 0.725803 0.716763 11.00000 -1.20000 H44B 2 0.253334 0.754293 0.820346 11.00000 -1.20000 AFIX 0 C45 1 0.316202 0.758270 0.743603 11.00000 0.03674 0.09145 = 0.10016 0.04941 -0.01445 0.00631 AFIX 13 H45 2 0.318588 0.750813 0.660713 11.00000 -1.20000 PART -1 AFIX 0 C46 1 0.350280 0.728985 0.809390 21.00000 0.03247 0.09603 = 0.09472 0.03936 -0.01242 0.01859 AFIX 23 H46A 2 0.335418 0.705423 0.783330 21.00000 -1.20000 H46B 2 0.349702 0.731232 0.895438 21.00000 -1.20000 AFIX 0 C47 1 0.407809 0.730054 0.789305 21.00000 0.03816 0.11384 = 0.11993 0.02502 -0.00635 0.02062 AFIX 23 H47A 2 0.428632 0.714468 0.849009 21.00000 -1.20000 H47B 2 0.409539 0.720024 0.709946 21.00000 -1.20000 AFIX 0 C50 1 0.337671 0.790515 0.741447 21.00000 0.04333 0.06984 = 0.10849 0.00024 -0.01359 0.01564 AFIX 23 H50A 2 0.338214 0.802084 0.819526 21.00000 -1.20000 H50B 2 0.315817 0.805302 0.681021 21.00000 -1.20000 PART -2 AFIX 0 C46A 1 0.348527 0.742177 0.852551 -21.00000 0.02417 0.09671 = 0.10535 0.02908 -0.02019 0.02135 AFIX 23 H46C 2 0.350261 0.716091 0.839393 -21.00000 -1.20000 H46D 2 0.329852 0.745746 0.919846 -21.00000 -1.20000 AFIX 0 C47A 1 0.405140 0.755969 0.892499 -21.00000 0.02518 0.10864 = 0.11809 0.01967 -0.01330 0.01951 AFIX 23 H47C 2 0.404420 0.777558 0.942232 -21.00000 -1.20000 H47D 2 0.425257 0.737419 0.941880 -21.00000 -1.20000 AFIX 0 C50A 1 0.339820 0.770401 0.653041 -21.00000 0.02556 0.07088 = 0.09369 -0.00143 0.00950 0.01655 AFIX 23 H50C 2 0.317299 0.787852 0.604000 -21.00000 -1.20000 H50D 2 0.346263 0.750195 0.601616 -21.00000 -1.20000 PART 0 AFIX 0 C48 1 0.429862 0.764225 0.796882 11.00000 0.03178 0.12983 = 0.12754 0.00825 -0.00132 0.00913 AFIX 23 H48A 2 0.464789 0.763000 0.776018 11.00000 -1.20000 H48B 2 0.433109 0.773168 0.879314 11.00000 -1.20000 AFIX 0 C49 1 0.396305 0.790057 0.712033 11.00000 0.04657 0.10741 = 0.13240 0.02632 -0.00911 -0.01526 AFIX 23 H49A 2 0.395660 0.782376 0.628927 11.00000 -1.20000 H49B 2 0.411116 0.814409 0.721292 11.00000 -1.20000 AFIX 0 C51 1 0.221036 0.877479 0.752193 11.00000 0.01351 0.02092 = 0.02018 -0.00222 0.00760 0.00544 C52 1 0.198366 0.916961 0.604893 11.00000 0.02464 0.02623 = 0.03405 0.00863 0.01568 0.00346 AFIX 43 H52 2 0.181475 0.927955 0.533962 11.00000 -1.20000 AFIX 0 C53 1 0.235680 0.932261 0.688509 11.00000 0.03241 0.02264 = 0.03557 0.00442 0.00824 -0.00471 AFIX 43 H53 2 0.250324 0.955383 0.685880 11.00000 -1.20000 AFIX 0 C54 1 0.283924 0.913444 0.883955 11.00000 0.03272 0.02606 = 0.02609 -0.00931 0.00601 -0.01276 AFIX 23 H54A 2 0.272091 0.900372 0.949657 11.00000 -1.20000 H54B 2 0.284724 0.939214 0.903729 11.00000 -1.20000 PART -1 AFIX 0 C55 1 0.338663 0.901096 0.874419 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 13 H55 2 0.335923 0.875472 0.849346 31.00000 -1.20000 AFIX 0 C56 1 0.374559 0.902178 0.993682 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H56A 2 0.376282 0.927045 1.023624 31.00000 -1.20000 H56B 2 0.359626 0.887257 1.050800 31.00000 -1.20000 AFIX 0 C57 1 0.428039 0.889486 0.990312 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H57A 2 0.427266 0.864175 0.964894 31.00000 -1.20000 H57B 2 0.449121 0.891181 1.070493 31.00000 -1.20000 AFIX 0 C58 1 0.452127 0.912882 0.901985 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H58A 2 0.453939 0.938154 0.927945 31.00000 -1.20000 H58B 2 0.487396 0.904549 0.897341 31.00000 -1.20000 AFIX 0 C59 1 0.418063 0.909259 0.783961 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H59A 2 0.418581 0.884098 0.757455 31.00000 -1.20000 H59B 2 0.431960 0.924230 0.725353 31.00000 -1.20000 AFIX 0 C60 1 0.363346 0.920095 0.786286 31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H60A 2 0.362582 0.946045 0.802700 31.00000 -1.20000 H60B 2 0.342785 0.915978 0.706579 31.00000 -1.20000 PART -2 AFIX 0 C55A 1 0.338958 0.915433 0.865650 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 13 H55A 2 0.340366 0.929741 0.792396 -31.00000 -1.20000 AFIX 0 C56A 1 0.358099 0.882482 0.851040 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H56C 2 0.339006 0.872414 0.776255 -31.00000 -1.20000 H56D 2 0.350596 0.867158 0.916608 -31.00000 -1.20000 AFIX 0 C57A 1 0.411789 0.879764 0.847262 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H57C 2 0.418381 0.889368 0.770549 -31.00000 -1.20000 H57D 2 0.421772 0.854234 0.851152 -31.00000 -1.20000 AFIX 0 C58A 1 0.446168 0.900281 0.950552 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H58C 2 0.449007 0.885965 1.024196 -31.00000 -1.20000 H58D 2 0.481216 0.903066 0.931380 -31.00000 -1.20000 AFIX 0 C59A 1 0.424474 0.937352 0.972338 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H59C 2 0.444587 0.947252 1.046244 -31.00000 -1.20000 H59D 2 0.429778 0.953295 0.906368 -31.00000 -1.20000 AFIX 0 C60A 1 0.369396 0.938124 0.982565 -31.00000 0.02738 0.07692 = 0.03172 0.00977 -0.00258 -0.00027 AFIX 23 H60C 2 0.356694 0.963042 0.981224 -31.00000 -1.20000 H60D 2 0.363845 0.926700 1.057478 -31.00000 -1.20000 PART 0 AFIX 0 C61 1 0.139634 0.839769 0.808273 11.00000 0.02889 0.02506 = 0.02138 -0.00691 0.00425 -0.00525 C62 1 0.063943 0.859956 0.702634 11.00000 0.01578 0.02699 = 0.03584 0.00243 0.00724 0.00267 AFIX 43 H62 2 0.039201 0.868395 0.638334 11.00000 -1.20000 AFIX 0 C63 1 0.057124 0.854760 0.817019 11.00000 0.02226 0.03364 = 0.03819 0.00293 0.01829 0.00152 AFIX 43 H63 2 0.026432 0.859147 0.847924 11.00000 -1.20000 AFIX 0 C64 1 0.112390 0.832954 1.004796 11.00000 0.04030 0.03278 = 0.01071 -0.00521 0.01125 -0.00421 AFIX 23 H64A 2 0.094934 0.850704 1.048483 11.00000 -1.20000 H64B 2 0.149852 0.834737 1.034493 11.00000 -1.20000 AFIX 0 C65 1 0.094096 0.795498 1.032269 11.00000 0.03970 0.02530 = 0.02213 -0.00035 0.00932 0.00554 AFIX 13 H65 2 0.109401 0.778032 0.981911 11.00000 -1.20000 AFIX 0 C66 1 0.115346 0.786951 1.163329 11.00000 0.03048 0.03780 = 0.02812 -0.00247 0.01095 0.00104 AFIX 23 H66A 2 0.153452 0.787653 1.176225 11.00000 -1.20000 H66B 2 0.103429 0.805386 1.214572 11.00000 -1.20000 AFIX 0 C67 1 0.097839 0.750519 1.198060 11.00000 0.05265 0.03960 = 0.02471 -0.00126 0.00472 0.01924 AFIX 23 H67A 2 0.109827 0.746646 1.283967 11.00000 -1.20000 H67B 2 0.113464 0.731834 1.154181 11.00000 -1.20000 AFIX 0 C68 1 0.039020 0.747193 1.170690 11.00000 0.04682 0.04478 = 0.05021 0.01112 0.01409 -0.00661 AFIX 23 H68A 2 0.028967 0.722784 1.191118 11.00000 -1.20000 H68B 2 0.023632 0.764273 1.220813 11.00000 -1.20000 AFIX 0 C69 1 0.017577 0.754608 1.039994 11.00000 0.04286 0.03927 = 0.04522 0.01158 0.01355 0.00603 AFIX 23 H69A 2 0.029842 0.736057 0.989691 11.00000 -1.20000 H69B 2 -0.020522 0.753727 1.027031 11.00000 -1.20000 AFIX 0 C70 1 0.035158 0.791204 1.005422 11.00000 0.02788 0.03562 = 0.02623 0.00329 0.01163 -0.00234 AFIX 23 H70A 2 0.019183 0.809764 1.049091 11.00000 -1.20000 H70B 2 0.023062 0.795016 0.919524 11.00000 -1.20000 AFIX 0 C71 1 0.112325 0.860182 0.466533 11.00000 0.02900 0.02230 = 0.01507 0.00413 0.00768 0.00378 C72 1 0.125270 0.880709 0.375772 11.00000 0.02728 0.03127 = 0.03068 -0.00673 0.01368 -0.01366 AFIX 43 H72 2 0.157537 0.892670 0.386902 11.00000 -1.20000 AFIX 0 C73 1 0.092027 0.884182 0.268667 11.00000 0.06445 0.02986 = 0.01203 0.00111 0.01145 0.01876 AFIX 43 H73 2 0.102220 0.898354 0.207711 11.00000 -1.20000 AFIX 0 C74 1 0.045034 0.867818 0.248218 11.00000 0.02489 0.03218 = 0.02096 -0.00640 0.00466 0.01520 AFIX 43 H74 2 0.022064 0.871386 0.175622 11.00000 -1.20000 AFIX 0 C75 1 0.031819 0.846239 0.334360 11.00000 0.04350 0.03586 = 0.02667 -0.00693 0.01464 0.00997 AFIX 43 H75 2 -0.000128 0.833871 0.320363 11.00000 -1.20000 AFIX 0 C76 1 0.064042 0.842195 0.440714 11.00000 0.01568 0.03918 = 0.02120 0.00227 0.00660 -0.00569 AFIX 43 H76 2 0.053930 0.826942 0.499091 11.00000 -1.20000 AFIX 0 C81 1 0.178014 1.171139 0.846008 11.00000 0.07389 0.03604 = 0.04869 0.00403 0.04607 -0.00612 C82 1 0.107393 1.195145 0.744680 11.00000 0.01903 0.02245 = 0.03574 0.00871 0.00629 0.00963 AFIX 43 H82 2 0.083206 1.205521 0.682938 11.00000 -1.20000 AFIX 0 C83 1 0.101516 1.190476 0.855451 11.00000 0.02123 0.03968 = 0.05860 0.00478 0.01700 0.00972 AFIX 43 H83 2 0.071850 1.196854 0.887794 11.00000 -1.20000 AFIX 0 C84 1 0.155967 1.166492 1.043261 11.00000 0.03689 0.03552 = 0.03064 -0.01071 0.02100 -0.00815 AFIX 23 H84A 2 0.138823 1.184332 1.087280 11.00000 -1.20000 H84B 2 0.193534 1.168164 1.071724 11.00000 -1.20000 AFIX 0 C85 1 0.136992 1.128281 1.070135 11.00000 0.02102 0.03767 = 0.03718 -0.00657 0.01633 0.00331 AFIX 13 H85 2 0.153065 1.110943 1.020759 11.00000 -1.20000 AFIX 0 C86 1 0.078588 1.124165 1.037648 11.00000 0.03939 0.02786 = 0.04672 0.00073 0.00421 0.00131 AFIX 23 H86A 2 0.068111 1.127466 0.950994 11.00000 -1.20000 H86B 2 0.061675 1.143016 1.078109 11.00000 -1.20000 AFIX 0 C87 1 0.060344 1.087550 1.072917 11.00000 0.03433 0.03857 = 0.06047 0.00225 0.00459 -0.01966 AFIX 23 H87A 2 0.022264 1.086687 1.054593 11.00000 -1.20000 H87B 2 0.073829 1.068930 1.024841 11.00000 -1.20000 AFIX 0 C88 1 0.077561 1.079294 1.202896 11.00000 0.07339 0.03010 = 0.05286 0.00325 0.02077 -0.01253 AFIX 23 H88A 2 0.066786 1.054775 1.220080 11.00000 -1.20000 H88B 2 0.061094 1.096170 1.251673 11.00000 -1.20000 AFIX 0 C89 1 0.136686 1.082507 1.235172 11.00000 0.06350 0.02443 = 0.04363 0.00778 0.01272 0.00169 AFIX 23 H89A 2 0.147276 1.078828 1.321624 11.00000 -1.20000 H89B 2 0.152917 1.063564 1.193610 11.00000 -1.20000 AFIX 0 C90 1 0.155550 1.118614 1.201402 11.00000 0.04476 0.04313 = 0.03254 0.00278 0.01077 0.01528 AFIX 23 H90A 2 0.193677 1.118758 1.217510 11.00000 -1.20000 H90B 2 0.143442 1.137145 1.252015 11.00000 -1.20000 AFIX 0 C91 1 0.242601 1.131381 0.720180 11.00000 0.01531 0.03669 = 0.03436 0.00126 0.00966 -0.00002 C92 1 0.210127 1.121977 0.529703 11.00000 0.01287 0.03950 = 0.03510 -0.00168 0.00804 -0.00372 AFIX 43 H92 2 0.192052 1.125810 0.451487 11.00000 -1.20000 AFIX 0 C93 1 0.235840 1.093303 0.566143 11.00000 0.03232 0.03228 = 0.04760 -0.00891 0.01836 0.00732 AFIX 43 H93 2 0.239656 1.072561 0.520520 11.00000 -1.20000 AFIX 0 C94 1 0.286457 1.073200 0.767557 11.00000 0.02162 0.03426 = 0.05225 0.00492 0.00781 0.00541 AFIX 23 H94A 2 0.268053 1.050037 0.762000 11.00000 -1.20000 H94B 2 0.288478 1.082193 0.849657 11.00000 -1.20000 AFIX 0 C95 1 0.340214 1.067311 0.742952 11.00000 0.03881 0.03880 = 0.03337 -0.00192 0.00222 0.00204 AFIX 13 H95 2 0.337227 1.060099 0.657832 11.00000 -1.20000 AFIX 0 C96 1 0.365808 1.035609 0.820124 11.00000 0.04090 0.05665 = 0.06430 0.00462 0.01541 0.00951 AFIX 23 H96A 2 0.369324 1.042003 0.905148 11.00000 -1.20000 H96B 2 0.343321 1.014308 0.806017 11.00000 -1.20000 AFIX 0 C97 1 0.419981 1.026394 0.790373 11.00000 0.04724 0.06739 = 0.10920 -0.00638 0.00770 0.02755 AFIX 23 H97A 2 0.435383 1.006399 0.841009 11.00000 -1.20000 H97B 2 0.416599 1.018885 0.706371 11.00000 -1.20000 AFIX 0 C98 1 0.454066 1.058658 0.811666 11.00000 0.02334 0.10846 = 0.09062 -0.01219 0.01288 -0.00122 AFIX 23 H98A 2 0.488263 1.052981 0.791533 11.00000 -1.20000 H98B 2 0.458949 1.065195 0.896750 11.00000 -1.20000 AFIX 0 C99 1 0.430417 1.090517 0.736039 11.00000 0.01515 0.06810 = 0.12881 0.00156 0.02763 -0.00465 AFIX 23 H99A 2 0.452903 1.111709 0.753664 11.00000 -1.20000 H99B 2 0.428091 1.084728 0.650796 11.00000 -1.20000 AFIX 0 C100 1 0.376309 1.099095 0.762595 11.00000 0.03393 0.04899 = 0.08743 -0.00319 0.01508 0.00320 AFIX 23 H10C 2 0.379348 1.107102 0.846028 11.00000 -1.20000 H10D 2 0.361380 1.119007 0.710929 11.00000 -1.20000 AFIX 0 C101 1 0.262589 1.202932 0.778211 11.00000 0.02546 0.03300 = 0.03591 -0.00198 0.01576 -0.00872 C102 1 0.243166 1.245041 0.642712 11.00000 0.03325 0.02817 = 0.06384 -0.00069 0.02331 -0.00053 AFIX 43 H102 2 0.225267 1.257313 0.575394 11.00000 -1.20000 AFIX 0 C103 1 0.282962 1.257433 0.717371 11.00000 0.07386 0.02654 = 0.04795 0.01260 0.03766 -0.00403 AFIX 43 H103 2 0.299634 1.279765 0.712602 11.00000 -1.20000 AFIX 0 C104 1 0.339176 1.231987 0.903516 11.00000 0.05736 0.04931 = 0.04299 -0.01457 0.02271 -0.01011 AFIX 23 H10E 2 0.327056 1.223444 0.975975 11.00000 -1.20000 H10F 2 0.351034 1.256953 0.917852 11.00000 -1.20000 AFIX 0 C105 1 0.384494 1.209147 0.882733 11.00000 0.03779 0.05764 = 0.05348 -0.02593 0.01620 -0.01961 AFIX 13 H105 2 0.370432 1.184932 0.858595 11.00000 -1.20000 AFIX 0 C106 1 0.424589 1.204026 0.998941 11.00000 0.03109 0.09802 = 0.05466 -0.01377 -0.00685 -0.01422 AFIX 23 H10G 2 0.438686 1.227569 1.027557 11.00000 -1.20000 H10H 2 0.407310 1.193470 1.061219 11.00000 -1.20000 AFIX 0 C107 1 0.468417 1.179715 0.977058 11.00000 0.03791 0.11220 = 0.09245 -0.00163 0.01219 -0.01451 AFIX 23 H10I 2 0.454876 1.155499 0.955373 11.00000 -1.20000 H10J 2 0.494292 1.177769 1.050457 11.00000 -1.20000 AFIX 0 C108 1 0.494256 1.195186 0.874890 11.00000 0.04144 0.11847 = 0.11552 -0.00031 0.03034 -0.00293 AFIX 23 H10K 2 0.509803 1.218680 0.899331 11.00000 -1.20000 H10L 2 0.522199 1.178969 0.860242 11.00000 -1.20000 AFIX 0 C109 1 0.454753 1.199684 0.758392 11.00000 0.05113 0.07612 = 0.08460 -0.02342 0.02104 -0.02511 AFIX 23 H10M 2 0.471768 1.210915 0.696819 11.00000 -1.20000 H10N 2 0.441716 1.175960 0.728991 11.00000 -1.20000 AFIX 0 C110 1 0.409915 1.223000 0.781501 11.00000 0.06274 0.06918 = 0.05474 -0.00223 0.02504 -0.01227 AFIX 23 H11A 2 0.422637 1.247566 0.800499 11.00000 -1.20000 H11B 2 0.383816 1.224162 0.708285 11.00000 -1.20000 AFIX 0 C111 1 0.152276 1.193766 0.505911 11.00000 0.02086 0.02946 = 0.04917 0.00649 0.00723 0.00525 C112 1 0.103944 1.179994 0.476507 11.00000 0.04662 0.04498 = 0.03370 0.01272 0.00566 0.00562 AFIX 43 H112 2 0.091059 1.165493 0.533079 11.00000 -1.20000 AFIX 0 C113 1 0.072067 1.186195 0.366211 11.00000 0.02717 0.03006 = 0.05426 -0.00700 0.00740 -0.00050 AFIX 43 H113 2 0.038315 1.176443 0.349802 11.00000 -1.20000 AFIX 0 C114 1 0.091368 1.207329 0.279888 11.00000 0.03982 0.03460 = 0.04100 0.00291 -0.00593 0.02662 AFIX 43 H114 2 0.070766 1.212096 0.204960 11.00000 -1.20000 AFIX 0 C115 1 0.140487 1.220638 0.307672 11.00000 0.04673 0.02883 = 0.03710 0.01061 0.00371 0.00670 AFIX 43 H115 2 0.153426 1.235417 0.251891 11.00000 -1.20000 AFIX 0 C116 1 0.170954 1.213233 0.412551 11.00000 0.03951 0.03657 = 0.05726 -0.00077 0.01321 -0.00050 AFIX 43 H116 2 0.205747 1.221085 0.425225 11.00000 -1.20000 HKLF 4 1 0.0000 -1.0000 0.0000 0.0000 0.0000 1.0000 -1.0000 0.0000 0.0000 REM mar15p1 in P21/c REM R1 = 0.1126 for 6775 Fo > 4sig(Fo) and 0.3409 for all 22708 data REM 1342 parameters refined using 192 restraints END WGHT 0.1652 0.0000 REM Highest difference peak 0.721, deepest hole -1.448, 1-sigma level 0.225 Q1 1 0.3108 0.7858 0.4968 11.00000 0.05 0.72 Q2 1 0.2623 1.0143 0.8455 11.00000 0.05 0.71 Q3 1 0.3042 0.7055 0.8790 11.00000 0.05 0.69 Q4 1 0.5126 1.1645 1.0036 11.00000 0.05 0.69 Q5 1 0.2797 0.3034 0.8471 11.00000 0.05 0.66 Q6 1 0.2349 0.7066 0.8170 11.00000 0.05 0.66 Q7 1 0.2415 0.9744 0.8127 11.00000 0.05 0.63 Q8 1 0.2889 1.0145 0.8146 11.00000 0.05 0.63 Q9 1 0.2858 0.9721 0.9127 11.00000 0.05 0.63 Q10 1 0.1844 0.7970 0.3235 11.00000 0.05 0.61 ; data_twin4 _vrf_PLAT220_twin4 ; RESPONSE: Free rotation of t-butyl groups can lead to large thermal ellipsoids, but in this case the motion was not large enough to warrant modeling as disordered. ; _vrf_PLAT710_twin4 ; RESPONSE: Linear torsion angles involving N10 are related to the terminal nitrosyl ligand and are correct. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H67 B N10 Ni O4' _chemical_formula_weight 917.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 '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 13.8677(4) _cell_length_b 14.0829(4) _cell_length_c 14.1333(4) _cell_angle_alpha 107.976(2) _cell_angle_beta 101.760(2) _cell_angle_gamma 97.862(2) _cell_volume 2510.56(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3381 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.93 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.9372 _exptl_absorpt_process_details 'Bruker, TWINABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16578 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.44 _reflns_number_total 10272 _reflns_number_gt 8444 _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. ; _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^)+(0.0655P)^2^+1.7408P] 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 10272 _refine_ls_number_parameters 612 _refine_ls_number_restraints 152 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1280 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.068 _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 Ni1 Ni 0.81099(3) 0.72081(3) 0.67730(3) 0.01962(11) Uani 1 1 d . . . B1 B 0.7277(2) 0.8313(3) 0.5317(3) 0.0210(7) Uani 1 1 d . . . H1 H 0.700(2) 0.866(3) 0.477(3) 0.025 Uiso 1 1 d . . . N1 N 0.84465(18) 0.8492(2) 0.5602(2) 0.0211(5) Uani 1 1 d . . . N2 N 0.90746(19) 0.9084(2) 0.5259(2) 0.0269(6) Uani 1 1 d . . . N3 N 0.99327(18) 0.8401(2) 0.6283(2) 0.0233(6) Uani 1 1 d . . . N4 N 0.68894(19) 0.71321(19) 0.4857(2) 0.0201(6) Uani 1 1 d . . . N5 N 0.6209(2) 0.6614(2) 0.3905(2) 0.0242(6) Uani 1 1 d . . . N6 N 0.6624(2) 0.55711(19) 0.4738(2) 0.0223(6) Uani 1 1 d . . . N7 N 0.70008(19) 0.86559(19) 0.6361(2) 0.0207(6) Uani 1 1 d . . . N8 N 0.6481(2) 0.9425(2) 0.6664(2) 0.0266(6) Uani 1 1 d . . . N9 N 0.6942(2) 0.87905(19) 0.7890(2) 0.0226(6) Uani 1 1 d . . . N10 N 0.8611(2) 0.6653(2) 0.7557(3) 0.0352(7) Uani 1 1 d . . . O1 O 0.9007(3) 0.6277(4) 0.8107(4) 0.1102(18) Uani 1 1 d . . . C1 C 0.8941(2) 0.8071(2) 0.6227(2) 0.0210(6) Uani 1 1 d . . . C2 C 0.9972(2) 0.9004(3) 0.5682(3) 0.0285(8) Uani 1 1 d . . . H2 H 1.0578 0.9321 0.5587 0.034 Uiso 1 1 calc R . . C3 C 1.0784(2) 0.8166(2) 0.6859(2) 0.0242(7) Uani 1 1 d . . . C4 C 1.0819(2) 0.8163(2) 0.7844(3) 0.0267(7) Uani 1 1 d . . . H4 H 1.0268 0.8294 0.8132 0.032 Uiso 1 1 calc R . . C5 C 1.1664(3) 0.7969(3) 0.8409(3) 0.0290(8) Uani 1 1 d . . . H5 H 1.1675 0.7949 0.9076 0.035 Uiso 1 1 calc R . . C6 C 1.2496(2) 0.7803(2) 0.8022(3) 0.0272(7) Uani 1 1 d . . . C7 C 1.2431(3) 0.7793(3) 0.7024(3) 0.0356(8) Uani 1 1 d . . . H7 H 1.2980 0.7664 0.6733 0.043 Uiso 1 1 calc R . . C8 C 1.1582(3) 0.7966(3) 0.6445(3) 0.0321(8) Uani 1 1 d . . . H8 H 1.1552 0.7947 0.5762 0.039 Uiso 1 1 calc R . . C9 C 1.3470(3) 0.7654(3) 0.8654(3) 0.0376(9) Uani 1 1 d . . . C10 C 1.3746(4) 0.6664(4) 0.8070(4) 0.0627(14) Uani 1 1 d . . . H10A H 1.4350 0.6567 0.8496 0.094 Uiso 1 1 calc R . . H10B H 1.3878 0.6704 0.7427 0.094 Uiso 1 1 calc R . . H10C H 1.3185 0.6086 0.7913 0.094 Uiso 1 1 calc R . . C11 C 1.4318(3) 0.8561(4) 0.8856(4) 0.0582(13) Uani 1 1 d . . . H11A H 1.4142 0.9194 0.9235 0.087 Uiso 1 1 calc R . . H11B H 1.4416 0.8593 0.8197 0.087 Uiso 1 1 calc R . . H11C H 1.4943 0.8480 0.9263 0.087 Uiso 1 1 calc R . . C12 C 1.3361(3) 0.7601(4) 0.9694(4) 0.0606(13) Uani 1 1 d . . . H12A H 1.3986 0.7484 1.0065 0.091 Uiso 1 1 calc R . . H12B H 1.2800 0.7038 0.9580 0.091 Uiso 1 1 calc R . . H12C H 1.3226 0.8246 1.0103 0.091 Uiso 1 1 calc R . . C13 C 0.7158(2) 0.6523(2) 0.5386(2) 0.0213(7) Uani 1 1 d . . . C14 C 0.6069(2) 0.5673(3) 0.3861(3) 0.0276(7) Uani 1 1 d . . . H14 H 0.5637 0.5118 0.3293 0.033 Uiso 1 1 calc R . . C15 C 0.6618(2) 0.4629(2) 0.4936(2) 0.0229(7) Uani 1 1 d . . . C16 C 0.5731(2) 0.3899(2) 0.4617(3) 0.0273(7) Uani 1 1 d . . . H16 H 0.5124 0.4019 0.4266 0.033 Uiso 1 1 calc R . . C17 C 0.5732(2) 0.2991(3) 0.4812(3) 0.0300(7) Uani 1 1 d . . . H17 H 0.5123 0.2488 0.4575 0.036 Uiso 1 1 calc R . . C18 C 0.6602(2) 0.2799(2) 0.5345(3) 0.0260(7) Uani 1 1 d . . . C19 C 0.7490(2) 0.3544(2) 0.5649(3) 0.0267(7) Uani 1 1 d . . . H19 H 0.8098 0.3430 0.6006 0.032 Uiso 1 1 calc R . . C20 C 0.7504(2) 0.4451(2) 0.5439(3) 0.0259(7) Uani 1 1 d . . . H20 H 0.8117 0.4944 0.5641 0.031 Uiso 1 1 calc R . . C21 C 0.6562(3) 0.1806(3) 0.5587(3) 0.0341(8) Uani 1 1 d . . . C22 C 0.5798(3) 0.1739(3) 0.6218(4) 0.0551(12) Uani 1 1 d . . . H22A H 0.5993 0.2337 0.6853 0.083 Uiso 1 1 calc R . . H22B H 0.5783 0.1115 0.6390 0.083 Uiso 1 1 calc R . . H22C H 0.5127 0.1722 0.5814 0.083 Uiso 1 1 calc R . . C23 C 0.6232(3) 0.0884(3) 0.4576(4) 0.0487(11) Uani 1 1 d . . . H23A H 0.5591 0.0922 0.4157 0.073 Uiso 1 1 calc R . . H23B H 0.6146 0.0251 0.4731 0.073 Uiso 1 1 calc R . . H23C H 0.6747 0.0893 0.4195 0.073 Uiso 1 1 calc R . . C24 C 0.7590(3) 0.1748(3) 0.6200(4) 0.0453(10) Uani 1 1 d . . . H24A H 0.8087 0.1785 0.5802 0.068 Uiso 1 1 calc R . . H24B H 0.7531 0.1102 0.6332 0.068 Uiso 1 1 calc R . . H24C H 0.7809 0.2320 0.6857 0.068 Uiso 1 1 calc R . . C25 C 0.7294(2) 0.8257(2) 0.7091(2) 0.0202(6) Uani 1 1 d . . . C26 C 0.6467(3) 0.9484(2) 0.7589(3) 0.0281(7) Uani 1 1 d . . . H26 H 0.6164 0.9951 0.8012 0.034 Uiso 1 1 calc R . . C27 C 0.7027(2) 0.8650(2) 0.8867(2) 0.0237(7) Uani 1 1 d . . . C28 C 0.6797(3) 0.7680(3) 0.8901(3) 0.0296(7) Uani 1 1 d . . . H28 H 0.6627 0.7099 0.8288 0.036 Uiso 1 1 calc R . . C29 C 0.6817(3) 0.7565(3) 0.9843(3) 0.0334(8) Uani 1 1 d . . . H29 H 0.6667 0.6895 0.9866 0.040 Uiso 1 1 calc R . . C30 C 0.7050(3) 0.8397(3) 1.0756(3) 0.0288(8) Uani 1 1 d . . . C31 C 0.7284(3) 0.9357(3) 1.0691(3) 0.0357(9) Uani 1 1 d . . . H31 H 0.7453 0.9941 1.1301 0.043 Uiso 1 1 calc R . . C32 C 0.7280(3) 0.9491(3) 0.9756(3) 0.0311(8) Uani 1 1 d . . . H32 H 0.7450 1.0158 0.9732 0.037 Uiso 1 1 calc R . . C33 C 0.7009(3) 0.8273(3) 1.1790(3) 0.0412(9) Uani 1 1 d . . . C34 C 0.7029(7) 0.7187(4) 1.1759(4) 0.106(3) Uani 1 1 d . . . H34A H 0.7595 0.6972 1.1498 0.159 Uiso 1 1 calc R . . H34B H 0.6396 0.6728 1.1305 0.159 Uiso 1 1 calc R . . H34C H 0.7108 0.7162 1.2456 0.159 Uiso 1 1 calc R . . C35 C 0.7888(4) 0.8982(4) 1.2658(4) 0.0741(17) Uani 1 1 d . . . H35A H 0.8522 0.8825 1.2513 0.111 Uiso 1 1 calc R . . H35B H 0.7837 0.8889 1.3306 0.111 Uiso 1 1 calc R . . H35C H 0.7876 0.9692 1.2716 0.111 Uiso 1 1 calc R . . C36 C 0.6045(4) 0.8522(7) 1.2038(4) 0.107(3) Uani 1 1 d . . . H36A H 0.6032 0.8477 1.2714 0.160 Uiso 1 1 calc R . . H36B H 0.5467 0.8033 1.1511 0.160 Uiso 1 1 calc R . . H36C H 0.6011 0.9216 1.2051 0.160 Uiso 1 1 calc R . . O2 O 0.4258(2) 0.4682(2) 0.1893(2) 0.0524(8) Uani 1 1 d . . . C37 C 0.3518(4) 0.5150(4) 0.2314(4) 0.0683(15) Uani 1 1 d . . . H37A H 0.3845 0.5778 0.2916 0.082 Uiso 1 1 calc R . . H37B H 0.3101 0.4675 0.2538 0.082 Uiso 1 1 calc R . . C38 C 0.2882(6) 0.5401(6) 0.1475(6) 0.117(3) Uani 1 1 d . . . H38A H 0.2622 0.6021 0.1755 0.140 Uiso 1 1 calc R . . H38B H 0.2309 0.4825 0.1047 0.140 Uiso 1 1 calc R . . C39 C 0.3628(8) 0.5581(7) 0.0874(8) 0.142(4) Uani 1 1 d . . . H39A H 0.3342 0.5187 0.0130 0.170 Uiso 1 1 calc R . . H39B H 0.3805 0.6316 0.0967 0.170 Uiso 1 1 calc R . . C40 C 0.4533(5) 0.5231(5) 0.1291(5) 0.098(2) Uani 1 1 d . . . H40A H 0.4762 0.4794 0.0721 0.118 Uiso 1 1 calc R . . H40B H 0.5091 0.5825 0.1712 0.118 Uiso 1 1 calc R . . O3 O 1.0045(4) 0.6688(4) 0.4065(5) 0.135(2) Uani 1 1 d . . . C41 C 0.9502(9) 0.6468(11) 0.3070(11) 0.267(10) Uani 1 1 d . . . H41A H 0.9965 0.6428 0.2617 0.321 Uiso 1 1 calc R . . H41B H 0.9141 0.7019 0.3029 0.321 Uiso 1 1 calc R . . C42 C 0.8798(10) 0.5526(10) 0.2731(12) 0.275(11) Uani 1 1 d . . . H42A H 0.8817 0.5090 0.2038 0.330 Uiso 1 1 calc R . . H42B H 0.8106 0.5638 0.2704 0.330 Uiso 1 1 calc R . . C43 C 0.9111(9) 0.5065(7) 0.3479(7) 0.159(5) Uani 1 1 d . . . H43A H 0.9542 0.4583 0.3247 0.191 Uiso 1 1 calc R . . H43B H 0.8519 0.4690 0.3604 0.191 Uiso 1 1 calc R . . C44 C 0.9668(7) 0.5906(5) 0.4396(7) 0.133(3) Uani 1 1 d . . . H44A H 0.9223 0.6138 0.4846 0.159 Uiso 1 1 calc R . . H44B H 1.0228 0.5698 0.4787 0.159 Uiso 1 1 calc R . . O4 O 0.1377(5) 0.8680(6) 0.0829(7) 0.093(3) Uani 0.551(8) 1 d PGU A 1 C45 C 0.0608(7) 0.9254(6) 0.0721(7) 0.138(5) Uani 0.551(8) 1 d PGU A 1 H45A H 0.0227 0.9041 -0.0010 0.165 Uiso 0.551(8) 1 calc PR A 1 H45B H 0.0911 0.9994 0.0970 0.165 Uiso 0.551(8) 1 calc PR A 1 C46 C -0.0055(6) 0.9034(7) 0.1343(8) 0.149(5) Uani 0.551(8) 1 d PGU A 1 H46A H 0.0180 0.9526 0.2058 0.179 Uiso 0.551(8) 1 calc PR A 1 H46B H -0.0755 0.9065 0.1044 0.179 Uiso 0.551(8) 1 calc PR A 1 C47 C 0.0008(7) 0.8008(7) 0.1315(10) 0.149(6) Uani 0.551(8) 1 d PGU A 1 H47A H -0.0635 0.7520 0.0904 0.179 Uiso 0.551(8) 1 calc PR A 1 H47B H 0.0160 0.7981 0.2021 0.179 Uiso 0.551(8) 1 calc PR A 1 C48 C 0.0864(7) 0.7754(4) 0.0813(8) 0.122(4) Uani 0.551(8) 1 d PGU A 1 H48A H 0.1318 0.7443 0.1206 0.147 Uiso 0.551(8) 1 calc PR A 1 H48B H 0.0591 0.7271 0.0096 0.147 Uiso 0.551(8) 1 calc PR A 1 O4A O 0.0490(6) 0.8037(5) 0.0404(6) 0.234(8) Uani 0.449(8) 1 d PGU A 2 C45A C -0.0112(6) 0.8803(8) 0.0425(7) 0.151(7) Uani 0.449(8) 1 d PGU A 2 H45C H -0.0819 0.8525 0.0387 0.181 Uiso 0.449(8) 1 calc PR A 2 H45D H -0.0101 0.9053 -0.0157 0.181 Uiso 0.449(8) 1 calc PR A 2 C46A C 0.0369(7) 0.9622(5) 0.1410(9) 0.114(5) Uani 0.449(8) 1 d PGU A 2 H46C H 0.0896 1.0120 0.1331 0.137 Uiso 0.449(8) 1 calc PR A 2 H46D H -0.0135 0.9985 0.1678 0.137 Uiso 0.449(8) 1 calc PR A 2 C47A C 0.0808(8) 0.9137(9) 0.2097(5) 0.139(7) Uani 0.449(8) 1 d PGU A 2 H47C H 0.1347 0.9633 0.2682 0.167 Uiso 0.449(8) 1 calc PR A 2 H47D H 0.0291 0.8830 0.2370 0.167 Uiso 0.449(8) 1 calc PR A 2 C48A C 0.1198(6) 0.8389(7) 0.1489(6) 0.148(7) Uani 0.449(8) 1 d PGU A 2 H48C H 0.1213 0.7811 0.1747 0.177 Uiso 0.449(8) 1 calc PR A 2 H48D H 0.1892 0.8672 0.1488 0.177 Uiso 0.449(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02087(18) 0.0205(2) 0.0207(2) 0.01150(16) 0.00457(17) 0.00568(17) B1 0.0232(15) 0.0189(18) 0.0221(19) 0.0106(13) 0.0022(15) 0.0053(14) N1 0.0228(12) 0.0221(14) 0.0226(14) 0.0130(11) 0.0071(11) 0.0043(11) N2 0.0261(13) 0.0326(16) 0.0251(15) 0.0168(12) 0.0067(12) 0.0003(12) N3 0.0192(12) 0.0283(14) 0.0241(15) 0.0131(12) 0.0045(10) 0.0034(10) N4 0.0231(13) 0.0206(13) 0.0170(13) 0.0084(11) 0.0035(11) 0.0040(11) N5 0.0258(14) 0.0255(14) 0.0195(14) 0.0067(11) 0.0030(11) 0.0061(11) N6 0.0249(13) 0.0173(13) 0.0230(14) 0.0053(11) 0.0055(11) 0.0043(10) N7 0.0220(13) 0.0191(13) 0.0225(14) 0.0093(11) 0.0044(11) 0.0068(10) N8 0.0289(14) 0.0250(14) 0.0296(16) 0.0114(12) 0.0085(12) 0.0120(12) N9 0.0267(14) 0.0212(13) 0.0225(14) 0.0099(11) 0.0078(11) 0.0062(11) N10 0.0302(14) 0.0386(18) 0.0402(19) 0.0264(14) -0.0001(14) 0.0029(14) O1 0.080(3) 0.139(4) 0.142(4) 0.122(3) -0.016(3) 0.015(3) C1 0.0208(14) 0.0221(16) 0.0198(16) 0.0082(12) 0.0036(12) 0.0037(12) C2 0.0251(15) 0.0345(19) 0.0279(19) 0.0174(16) 0.0062(14) -0.0011(14) C3 0.0184(14) 0.0254(17) 0.0286(18) 0.0119(14) 0.0028(12) 0.0027(12) C4 0.0234(16) 0.0299(17) 0.0282(17) 0.0117(14) 0.0073(13) 0.0056(13) C5 0.0315(18) 0.0327(18) 0.0216(17) 0.0118(14) 0.0019(14) 0.0043(14) C6 0.0205(15) 0.0258(17) 0.0314(19) 0.0070(14) 0.0034(13) 0.0045(13) C7 0.0234(17) 0.049(2) 0.036(2) 0.0133(18) 0.0089(15) 0.0123(16) C8 0.0282(17) 0.046(2) 0.0244(18) 0.0119(16) 0.0101(14) 0.0106(16) C9 0.0282(18) 0.042(2) 0.039(2) 0.0128(18) 0.0000(15) 0.0126(15) C10 0.055(3) 0.055(3) 0.069(3) 0.010(2) -0.002(2) 0.034(2) C11 0.0246(18) 0.059(3) 0.081(4) 0.023(3) -0.004(2) 0.0064(19) C12 0.044(2) 0.096(4) 0.051(3) 0.037(3) 0.001(2) 0.032(2) C13 0.0216(15) 0.0201(15) 0.0249(17) 0.0105(13) 0.0065(13) 0.0057(12) C14 0.0267(17) 0.0286(18) 0.0235(17) 0.0067(14) 0.0030(14) 0.0043(14) C15 0.0287(16) 0.0173(15) 0.0234(17) 0.0058(13) 0.0089(13) 0.0069(13) C16 0.0251(16) 0.0228(16) 0.0330(18) 0.0073(14) 0.0081(14) 0.0071(13) C17 0.0256(15) 0.0220(17) 0.041(2) 0.0085(14) 0.0108(15) 0.0025(14) C18 0.0290(15) 0.0202(16) 0.0319(19) 0.0083(14) 0.0142(14) 0.0076(13) C19 0.0267(16) 0.0239(16) 0.0316(18) 0.0106(14) 0.0087(14) 0.0086(13) C20 0.0257(16) 0.0199(16) 0.0306(18) 0.0079(14) 0.0073(14) 0.0026(13) C21 0.0315(18) 0.0229(17) 0.054(2) 0.0187(17) 0.0145(17) 0.0070(14) C22 0.060(3) 0.041(2) 0.097(4) 0.047(2) 0.046(3) 0.022(2) C23 0.047(2) 0.0229(19) 0.070(3) 0.0118(19) 0.007(2) 0.0077(17) C24 0.043(2) 0.037(2) 0.064(3) 0.032(2) 0.009(2) 0.0090(18) C25 0.0200(14) 0.0192(15) 0.0213(16) 0.0079(13) 0.0046(12) 0.0030(12) C26 0.0345(18) 0.0243(17) 0.0288(18) 0.0085(14) 0.0118(15) 0.0137(14) C27 0.0249(16) 0.0280(17) 0.0205(17) 0.0095(14) 0.0086(13) 0.0067(13) C28 0.0398(19) 0.0234(17) 0.0221(17) 0.0036(14) 0.0089(15) 0.0037(14) C29 0.042(2) 0.0271(18) 0.030(2) 0.0111(16) 0.0089(16) 0.0029(15) C30 0.0304(18) 0.0328(18) 0.0230(17) 0.0092(14) 0.0087(14) 0.0043(14) C31 0.050(2) 0.0287(19) 0.0208(18) 0.0017(15) 0.0083(16) 0.0001(16) C32 0.041(2) 0.0214(16) 0.0271(18) 0.0060(14) 0.0074(15) 0.0033(14) C33 0.048(2) 0.052(2) 0.0231(19) 0.0159(18) 0.0095(17) -0.0013(19) C34 0.225(9) 0.059(3) 0.045(3) 0.032(3) 0.049(4) 0.011(4) C35 0.079(4) 0.092(4) 0.032(2) 0.029(3) -0.010(2) -0.023(3) C36 0.062(4) 0.234(9) 0.045(3) 0.064(5) 0.031(3) 0.039(5) O2 0.0561(18) 0.0452(17) 0.0459(17) 0.0070(14) 0.0124(14) 0.0000(14) C37 0.050(3) 0.067(3) 0.073(4) 0.003(3) 0.016(3) 0.013(2) C38 0.109(6) 0.100(5) 0.108(6) 0.021(5) -0.022(5) 0.025(5) C39 0.171(8) 0.135(7) 0.141(8) 0.110(7) 0.002(7) 0.016(7) C40 0.110(5) 0.109(5) 0.061(4) 0.044(4) 0.007(3) -0.036(4) O3 0.102(4) 0.115(4) 0.175(6) 0.061(4) 0.008(4) -0.004(3) C41 0.187(11) 0.269(15) 0.279(16) 0.217(14) -0.155(12) -0.129(11) C42 0.212(13) 0.218(14) 0.309(19) 0.173(15) -0.139(13) -0.113(11) C43 0.212(11) 0.095(6) 0.120(8) 0.032(6) -0.012(7) -0.035(7) C44 0.156(8) 0.067(4) 0.161(8) 0.004(5) 0.089(7) -0.007(5) O4 0.091(5) 0.113(6) 0.096(6) 0.046(5) 0.059(5) 0.019(4) C45 0.120(9) 0.124(10) 0.218(14) 0.090(10) 0.099(10) 0.031(7) C46 0.139(11) 0.152(11) 0.205(14) 0.083(11) 0.103(10) 0.054(9) C47 0.159(12) 0.161(11) 0.194(14) 0.118(11) 0.103(10) 0.031(9) C48 0.149(11) 0.139(9) 0.111(11) 0.076(9) 0.037(9) 0.057(8) O4A 0.278(15) 0.193(12) 0.158(11) -0.025(10) -0.001(11) 0.107(10) C45A 0.138(14) 0.176(14) 0.105(10) -0.004(10) 0.034(10) 0.046(11) C46A 0.149(13) 0.077(8) 0.101(10) 0.016(7) 0.051(9) -0.017(7) C47A 0.089(11) 0.109(12) 0.157(11) -0.015(9) -0.026(10) 0.048(9) C48A 0.161(14) 0.165(14) 0.110(12) 0.018(10) 0.054(10) 0.049(10) _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 N10 1.640(2) . ? Ni1 C25 1.980(3) . ? Ni1 C13 1.986(3) . ? Ni1 C1 1.990(3) . ? B1 N7 1.549(5) . ? B1 N1 1.554(4) . ? B1 N4 1.557(4) . ? B1 H1 1.07(3) . ? N1 C1 1.338(3) . ? N1 N2 1.382(3) . ? N2 C2 1.303(4) . ? N3 C1 1.368(4) . ? N3 C2 1.377(4) . ? N3 C3 1.431(4) . ? N4 C13 1.343(4) . ? N4 N5 1.386(4) . ? N5 C14 1.293(4) . ? N6 C13 1.371(4) . ? N6 C14 1.378(4) . ? N6 C15 1.437(4) . ? N7 C25 1.339(4) . ? N7 N8 1.389(4) . ? N8 C26 1.288(4) . ? N9 C25 1.370(4) . ? N9 C26 1.374(4) . ? N9 C27 1.439(4) . ? N10 O1 1.161(4) . ? C2 H2 0.9500 . ? C3 C8 1.376(5) . ? C3 C4 1.384(5) . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 H5 0.9500 . ? C6 C7 1.389(5) . ? C6 C9 1.539(4) . ? C7 C8 1.387(5) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C11 1.524(6) . ? C9 C10 1.528(6) . ? C9 C12 1.532(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C14 H14 0.9500 . ? C15 C16 1.383(4) . ? C15 C20 1.384(4) . ? C16 C17 1.389(4) . ? C16 H16 0.9500 . ? C17 C18 1.393(4) . ? C17 H17 0.9500 . ? C18 C19 1.398(4) . ? C18 C21 1.537(4) . ? C19 C20 1.397(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.528(6) . ? C21 C24 1.537(5) . ? C21 C23 1.537(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 H26 0.9500 . ? C27 C32 1.375(5) . ? C27 C28 1.378(5) . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C29 C30 1.392(5) . ? C29 H29 0.9500 . ? C30 C31 1.383(5) . ? C30 C33 1.535(5) . ? C31 C32 1.389(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C36 1.509(7) . ? C33 C35 1.513(6) . ? C33 C34 1.520(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O2 C40 1.387(6) . ? O2 C37 1.427(6) . ? C37 C38 1.492(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.509(12) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.488(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O3 C41 1.370(11) . ? O3 C44 1.402(9) . ? C41 C42 1.416(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.428(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.440(11) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O4 C48 1.3893 . ? O4 C45 1.4345 . ? C45 C46 1.4604 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.4487 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.5313 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O4A C45A 1.4488 . ? O4A C48A 1.5313 . ? C45A C46A 1.4605 . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? C46A C47A 1.4346 . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C47A C48A 1.3892 . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? 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 N10 Ni1 C25 126.00(16) . . ? N10 Ni1 C13 126.78(15) . . ? C25 Ni1 C13 90.00(12) . . ? N10 Ni1 C1 122.42(13) . . ? C25 Ni1 C1 90.03(13) . . ? C13 Ni1 C1 90.74(12) . . ? N7 B1 N1 105.2(2) . . ? N7 B1 N4 105.4(2) . . ? N1 B1 N4 105.6(3) . . ? N7 B1 H1 117(2) . . ? N1 B1 H1 111.8(17) . . ? N4 B1 H1 110.8(19) . . ? C1 N1 N2 113.5(2) . . ? C1 N1 B1 121.4(2) . . ? N2 N1 B1 125.1(2) . . ? C2 N2 N1 103.4(2) . . ? C1 N3 C2 107.9(2) . . ? C1 N3 C3 126.6(2) . . ? C2 N3 C3 125.6(3) . . ? C13 N4 N5 113.7(2) . . ? C13 N4 B1 121.9(2) . . ? N5 N4 B1 124.3(2) . . ? C14 N5 N4 103.3(2) . . ? C13 N6 C14 108.0(3) . . ? C13 N6 C15 126.6(3) . . ? C14 N6 C15 125.4(3) . . ? C25 N7 N8 113.1(3) . . ? C25 N7 B1 122.0(3) . . ? N8 N7 B1 124.8(2) . . ? C26 N8 N7 103.6(3) . . ? C25 N9 C26 107.8(3) . . ? C25 N9 C27 127.0(3) . . ? C26 N9 C27 125.2(3) . . ? O1 N10 Ni1 176.9(3) . . ? N1 C1 N3 103.7(2) . . ? N1 C1 Ni1 116.9(2) . . ? N3 C1 Ni1 139.4(2) . . ? N2 C2 N3 111.5(3) . . ? N2 C2 H2 124.3 . . ? N3 C2 H2 124.3 . . ? C8 C3 C4 119.8(3) . . ? C8 C3 N3 120.1(3) . . ? C4 C3 N3 120.1(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 117.3(3) . . ? C7 C6 C9 119.7(3) . . ? C5 C6 C9 123.0(3) . . ? C8 C7 C6 121.5(3) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C3 C8 C7 120.1(3) . . ? C3 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C11 C9 C10 109.7(4) . . ? C11 C9 C12 108.3(4) . . ? C10 C9 C12 107.8(4) . . ? C11 C9 C6 108.6(3) . . ? C10 C9 C6 110.6(3) . . ? C12 C9 C6 111.7(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 N6 103.2(3) . . ? N4 C13 Ni1 116.3(2) . . ? N6 C13 Ni1 140.5(2) . . ? N5 C14 N6 111.8(3) . . ? N5 C14 H14 124.1 . . ? N6 C14 H14 124.1 . . ? C16 C15 C20 120.2(3) . . ? C16 C15 N6 120.1(3) . . ? C20 C15 N6 119.7(3) . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 121.7(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 117.4(3) . . ? C17 C18 C21 120.2(3) . . ? C19 C18 C21 122.4(3) . . ? C20 C19 C18 121.4(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C15 C20 C19 119.5(3) . . ? C15 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C18 109.2(3) . . ? C22 C21 C24 108.6(3) . . ? C18 C21 C24 112.3(3) . . ? C22 C21 C23 109.1(3) . . ? C18 C21 C23 109.5(3) . . ? C24 C21 C23 108.0(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 N9 103.6(3) . . ? N7 C25 Ni1 116.6(2) . . ? N9 C25 Ni1 139.8(2) . . ? N8 C26 N9 112.0(3) . . ? N8 C26 H26 124.0 . . ? N9 C26 H26 124.0 . . ? C32 C27 C28 120.5(3) . . ? C32 C27 N9 119.6(3) . . ? C28 C27 N9 119.8(3) . . ? C27 C28 C29 119.0(3) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 122.2(3) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 117.0(3) . . ? C31 C30 C33 120.7(3) . . ? C29 C30 C33 122.3(3) . . ? C30 C31 C32 121.8(3) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C27 C32 C31 119.5(3) . . ? C27 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C36 C33 C35 108.4(5) . . ? C36 C33 C34 108.1(5) . . ? C35 C33 C34 107.7(4) . . ? C36 C33 C30 109.2(4) . . ? C35 C33 C30 111.5(3) . . ? C34 C33 C30 111.8(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40 O2 C37 104.9(5) . . ? O2 C37 C38 106.3(5) . . ? O2 C37 H37A 110.5 . . ? C38 C37 H37A 110.5 . . ? O2 C37 H37B 110.5 . . ? C38 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? C37 C38 C39 101.5(6) . . ? C37 C38 H38A 111.5 . . ? C39 C38 H38A 111.5 . . ? C37 C38 H38B 111.5 . . ? C39 C38 H38B 111.5 . . ? H38A C38 H38B 109.3 . . ? C40 C39 C38 105.9(5) . . ? C40 C39 H39A 110.6 . . ? C38 C39 H39A 110.6 . . ? C40 C39 H39B 110.6 . . ? C38 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? O2 C40 C39 107.2(6) . . ? O2 C40 H40A 110.3 . . ? C39 C40 H40A 110.3 . . ? O2 C40 H40B 110.3 . . ? C39 C40 H40B 110.3 . . ? H40A C40 H40B 108.5 . . ? C41 O3 C44 107.3(7) . . ? O3 C41 C42 110.1(8) . . ? O3 C41 H41A 109.6 . . ? C42 C41 H41A 109.6 . . ? O3 C41 H41B 109.6 . . ? C42 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? C41 C42 C43 104.7(9) . . ? C41 C42 H42A 110.8 . . ? C43 C42 H42A 110.8 . . ? C41 C42 H42B 110.8 . . ? C43 C42 H42B 110.8 . . ? H42A C42 H42B 108.9 . . ? C42 C43 C44 104.9(9) . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43B 110.8 . . ? C44 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? O3 C44 C43 106.3(8) . . ? O3 C44 H44A 110.5 . . ? C43 C44 H44A 110.5 . . ? O3 C44 H44B 110.5 . . ? C43 C44 H44B 110.5 . . ? H44A C44 H44B 108.7 . . ? C48 O4 C45 104.1 . . ? O4 C45 C46 106.1 . . ? O4 C45 H45A 110.5 . . ? C46 C45 H45A 110.5 . . ? O4 C45 H45B 110.5 . . ? C46 C45 H45B 110.5 . . ? H45A C45 H45B 108.7 . . ? C47 C46 C45 104.2 . . ? C47 C46 H46A 110.9 . . ? C45 C46 H46A 110.9 . . ? C47 C46 H46B 110.9 . . ? C45 C46 H46B 110.9 . . ? H46A C46 H46B 108.9 . . ? C46 C47 C48 105.4 . . ? C46 C47 H47A 110.7 . . ? C48 C47 H47A 110.7 . . ? C46 C47 H47B 110.7 . . ? C48 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? O4 C48 C47 105.6 . . ? O4 C48 H48A 110.6 . . ? C47 C48 H48A 110.6 . . ? O4 C48 H48B 110.6 . . ? C47 C48 H48B 110.6 . . ? H48A C48 H48B 108.8 . . ? C45A O4A C48A 105.4 . . ? O4A C45A C46A 104.2 . . ? O4A C45A H45C 110.9 . . ? C46A C45A H45C 110.9 . . ? O4A C45A H45D 110.9 . . ? C46A C45A H45D 110.9 . . ? H45C C45A H45D 108.9 . . ? C47A C46A C45A 106.1 . . ? C47A C46A H46C 110.5 . . ? C45A C46A H46C 110.5 . . ? C47A C46A H46D 110.5 . . ? C45A C46A H46D 110.5 . . ? H46C C46A H46D 108.7 . . ? C48A C47A C46A 104.1 . . ? C48A C47A H47C 110.9 . . ? C46A C47A H47C 110.9 . . ? C48A C47A H47D 110.9 . . ? C46A C47A H47D 110.9 . . ? H47C C47A H47D 109.0 . . ? C47A C48A O4A 105.6 . . ? C47A C48A H48C 110.6 . . ? O4A C48A H48C 110.6 . . ? C47A C48A H48D 110.6 . . ? O4A C48A H48D 110.6 . . ? H48C C48A H48D 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 B1 N1 C1 55.7(4) . . . . ? N4 B1 N1 C1 -55.5(4) . . . . ? N7 B1 N1 N2 -124.0(3) . . . . ? N4 B1 N1 N2 124.8(3) . . . . ? C1 N1 N2 C2 0.8(4) . . . . ? B1 N1 N2 C2 -179.5(3) . . . . ? N7 B1 N4 C13 -54.2(3) . . . . ? N1 B1 N4 C13 56.8(4) . . . . ? N7 B1 N4 N5 122.5(3) . . . . ? N1 B1 N4 N5 -126.5(3) . . . . ? C13 N4 N5 C14 -0.2(4) . . . . ? B1 N4 N5 C14 -177.2(3) . . . . ? N1 B1 N7 C25 -56.2(3) . . . . ? N4 B1 N7 C25 55.1(3) . . . . ? N1 B1 N7 N8 120.4(3) . . . . ? N4 B1 N7 N8 -128.3(3) . . . . ? C25 N7 N8 C26 0.1(4) . . . . ? B1 N7 N8 C26 -176.8(3) . . . . ? C25 Ni1 N10 O1 -121(9) . . . . ? C13 Ni1 N10 O1 116(9) . . . . ? C1 Ni1 N10 O1 -3(9) . . . . ? N2 N1 C1 N3 -0.4(4) . . . . ? B1 N1 C1 N3 179.9(3) . . . . ? N2 N1 C1 Ni1 179.7(2) . . . . ? B1 N1 C1 Ni1 0.0(4) . . . . ? C2 N3 C1 N1 -0.1(4) . . . . ? C3 N3 C1 N1 -180.0(3) . . . . ? C2 N3 C1 Ni1 179.8(3) . . . . ? C3 N3 C1 Ni1 -0.1(6) . . . . ? N10 Ni1 C1 N1 -179.3(2) . . . . ? C25 Ni1 C1 N1 -45.2(3) . . . . ? C13 Ni1 C1 N1 44.8(3) . . . . ? N10 Ni1 C1 N3 0.8(5) . . . . ? C25 Ni1 C1 N3 135.0(4) . . . . ? C13 Ni1 C1 N3 -135.0(4) . . . . ? N1 N2 C2 N3 -0.8(4) . . . . ? C1 N3 C2 N2 0.6(4) . . . . ? C3 N3 C2 N2 -179.5(3) . . . . ? C1 N3 C3 C8 140.0(3) . . . . ? C2 N3 C3 C8 -39.9(5) . . . . ? C1 N3 C3 C4 -41.6(5) . . . . ? C2 N3 C3 C4 138.5(3) . . . . ? C8 C3 C4 C5 0.6(5) . . . . ? N3 C3 C4 C5 -177.8(3) . . . . ? C3 C4 C5 C6 1.8(5) . . . . ? C4 C5 C6 C7 -2.9(5) . . . . ? C4 C5 C6 C9 176.0(3) . . . . ? C5 C6 C7 C8 1.6(5) . . . . ? C9 C6 C7 C8 -177.3(3) . . . . ? C4 C3 C8 C7 -1.9(5) . . . . ? N3 C3 C8 C7 176.5(3) . . . . ? C6 C7 C8 C3 0.8(6) . . . . ? C7 C6 C9 C11 65.4(5) . . . . ? C5 C6 C9 C11 -113.4(4) . . . . ? C7 C6 C9 C10 -55.1(5) . . . . ? C5 C6 C9 C10 126.1(4) . . . . ? C7 C6 C9 C12 -175.2(4) . . . . ? C5 C6 C9 C12 5.9(5) . . . . ? N5 N4 C13 N6 0.1(4) . . . . ? B1 N4 C13 N6 177.1(3) . . . . ? N5 N4 C13 Ni1 -178.7(2) . . . . ? B1 N4 C13 Ni1 -1.7(4) . . . . ? C14 N6 C13 N4 0.0(3) . . . . ? C15 N6 C13 N4 -178.7(3) . . . . ? C14 N6 C13 Ni1 178.4(3) . . . . ? C15 N6 C13 Ni1 -0.4(6) . . . . ? N10 Ni1 C13 N4 -176.4(2) . . . . ? C25 Ni1 C13 N4 46.4(2) . . . . ? C1 Ni1 C13 N4 -43.6(3) . . . . ? N10 Ni1 C13 N6 5.3(5) . . . . ? C25 Ni1 C13 N6 -131.9(4) . . . . ? C1 Ni1 C13 N6 138.1(4) . . . . ? N4 N5 C14 N6 0.3(4) . . . . ? C13 N6 C14 N5 -0.2(4) . . . . ? C15 N6 C14 N5 178.6(3) . . . . ? C13 N6 C15 C16 141.5(3) . . . . ? C14 N6 C15 C16 -37.1(5) . . . . ? C13 N6 C15 C20 -39.0(5) . . . . ? C14 N6 C15 C20 142.4(3) . . . . ? C20 C15 C16 C17 0.6(5) . . . . ? N6 C15 C16 C17 -179.9(3) . . . . ? C15 C16 C17 C18 1.5(6) . . . . ? C16 C17 C18 C19 -2.1(5) . . . . ? C16 C17 C18 C21 177.3(3) . . . . ? C17 C18 C19 C20 0.8(5) . . . . ? C21 C18 C19 C20 -178.6(3) . . . . ? C16 C15 C20 C19 -1.8(5) . . . . ? N6 C15 C20 C19 178.6(3) . . . . ? C18 C19 C20 C15 1.2(5) . . . . ? C17 C18 C21 C22 -58.1(5) . . . . ? C19 C18 C21 C22 121.3(4) . . . . ? C17 C18 C21 C24 -178.7(4) . . . . ? C19 C18 C21 C24 0.7(5) . . . . ? C17 C18 C21 C23 61.3(4) . . . . ? C19 C18 C21 C23 -119.3(4) . . . . ? N8 N7 C25 N9 0.3(3) . . . . ? B1 N7 C25 N9 177.3(3) . . . . ? N8 N7 C25 Ni1 -176.6(2) . . . . ? B1 N7 C25 Ni1 0.4(4) . . . . ? C26 N9 C25 N7 -0.5(3) . . . . ? C27 N9 C25 N7 178.3(3) . . . . ? C26 N9 C25 Ni1 175.2(3) . . . . ? C27 N9 C25 Ni1 -6.0(5) . . . . ? N10 Ni1 C25 N7 176.4(2) . . . . ? C13 Ni1 C25 N7 -45.9(2) . . . . ? C1 Ni1 C25 N7 44.9(2) . . . . ? N10 Ni1 C25 N9 1.1(4) . . . . ? C13 Ni1 C25 N9 138.8(4) . . . . ? C1 Ni1 C25 N9 -130.5(4) . . . . ? N7 N8 C26 N9 -0.4(4) . . . . ? C25 N9 C26 N8 0.6(4) . . . . ? C27 N9 C26 N8 -178.2(3) . . . . ? C25 N9 C27 C32 137.2(3) . . . . ? C26 N9 C27 C32 -44.2(5) . . . . ? C25 N9 C27 C28 -46.7(5) . . . . ? C26 N9 C27 C28 132.0(4) . . . . ? C32 C27 C28 C29 0.4(5) . . . . ? N9 C27 C28 C29 -175.7(3) . . . . ? C27 C28 C29 C30 0.8(6) . . . . ? C28 C29 C30 C31 -1.3(6) . . . . ? C28 C29 C30 C33 176.2(3) . . . . ? C29 C30 C31 C32 0.6(6) . . . . ? C33 C30 C31 C32 -176.9(4) . . . . ? C28 C27 C32 C31 -1.1(5) . . . . ? N9 C27 C32 C31 175.0(3) . . . . ? C30 C31 C32 C27 0.6(6) . . . . ? C31 C30 C33 C36 76.2(5) . . . . ? C29 C30 C33 C36 -101.1(5) . . . . ? C31 C30 C33 C35 -43.5(5) . . . . ? C29 C30 C33 C35 139.1(4) . . . . ? C31 C30 C33 C34 -164.2(5) . . . . ? C29 C30 C33 C34 18.4(6) . . . . ? C40 O2 C37 C38 39.4(6) . . . . ? O2 C37 C38 C39 -29.8(7) . . . . ? C37 C38 C39 C40 10.4(9) . . . . ? C37 O2 C40 C39 -31.9(7) . . . . ? C38 C39 C40 O2 12.8(9) . . . . ? C44 O3 C41 C42 -2.3(18) . . . . ? O3 C41 C42 C43 -14(2) . . . . ? C41 C42 C43 C44 24.0(18) . . . . ? C41 O3 C44 C43 17.6(13) . . . . ? C42 C43 C44 O3 -25.9(14) . . . . ? C48 O4 C45 C46 39.7 . . . . ? O4 C45 C46 C47 -29.8 . . . . ? C45 C46 C47 C48 9.4 . . . . ? C45 O4 C48 C47 -32.5 . . . . ? C46 C47 C48 O4 14.3 . . . . ? C48A O4A C45A C46A 9.4 . . . . ? O4A C45A C46A C47A -29.8 . . . . ? C45A C46A C47A C48A 39.6 . . . . ? C46A C47A C48A O4A -32.5 . . . . ? C45A O4A C48A C47A 14.3 . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.636 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.077 _iucr_refine_instruction_details ; TITL twin4 in P-1 CELL 0.71073 13.8677 14.0829 14.1333 107.976 101.760 97.862 ZERR 2.00 0.0004 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H N O B Ni UNIT 96 134 20 8 2 2 MERG 0 L.S. 10 ACTA OMIT 0 -1 1 OMIT -1 1 0 OMIT 0 0 -1 OMIT 1 0 1 OMIT 0 0 1 OMIT -1 0 1 OMIT 1 1 0 OMIT 0 1 0 BOND $H CONF FMAP 2 PLAN -10 SIZE 0.150 0.303 0.525 DELU O4 C45 C46 C47 C48 O4A C45A C46A C47A C48A SIMU O4 C45 C46 C47 C48 O4A C45A C46A C47A C48A TEMP -100.140 WGHT 0.065500 1.740800 BASF 0.46611 FVAR 0.43782 0.55112 NI1 6 0.810986 0.720806 0.677303 11.00000 0.02087 0.02046 = 0.02067 0.01150 0.00457 0.00568 B1 5 0.727720 0.831348 0.531704 11.00000 0.02321 0.01891 = 0.02205 0.01061 0.00220 0.00533 H1 2 0.700057 0.866136 0.477097 11.00000 -1.20000 N1 3 0.844649 0.849215 0.560168 11.00000 0.02284 0.02209 = 0.02259 0.01297 0.00706 0.00429 N2 3 0.907457 0.908378 0.525881 11.00000 0.02611 0.03261 = 0.02506 0.01677 0.00667 0.00030 N3 3 0.993267 0.840081 0.628286 11.00000 0.01921 0.02827 = 0.02415 0.01307 0.00449 0.00338 N4 3 0.688941 0.713214 0.485738 11.00000 0.02307 0.02064 = 0.01698 0.00836 0.00347 0.00400 N5 3 0.620855 0.661407 0.390533 11.00000 0.02577 0.02545 = 0.01947 0.00673 0.00299 0.00605 N6 3 0.662387 0.557105 0.473844 11.00000 0.02492 0.01726 = 0.02300 0.00530 0.00551 0.00427 N7 3 0.700076 0.865593 0.636136 11.00000 0.02200 0.01910 = 0.02251 0.00926 0.00435 0.00678 N8 3 0.648125 0.942501 0.666406 11.00000 0.02887 0.02503 = 0.02956 0.01144 0.00853 0.01204 N9 3 0.694226 0.879052 0.788974 11.00000 0.02668 0.02121 = 0.02251 0.00993 0.00778 0.00624 N10 3 0.861050 0.665275 0.755666 11.00000 0.03019 0.03859 = 0.04021 0.02636 -0.00012 0.00290 O1 4 0.900736 0.627654 0.810699 11.00000 0.07954 0.13926 = 0.14151 0.12199 -0.01581 0.01541 C1 1 0.894101 0.807078 0.622665 11.00000 0.02082 0.02208 = 0.01982 0.00818 0.00359 0.00371 C2 1 0.997229 0.900364 0.568173 11.00000 0.02511 0.03454 = 0.02787 0.01740 0.00619 -0.00109 AFIX 43 H2 2 1.057792 0.932095 0.558746 11.00000 -1.20000 AFIX 0 C3 1 1.078446 0.816589 0.685910 11.00000 0.01835 0.02538 = 0.02863 0.01186 0.00282 0.00274 C4 1 1.081922 0.816348 0.784415 11.00000 0.02341 0.02986 = 0.02824 0.01165 0.00728 0.00556 AFIX 43 H4 2 1.026809 0.829415 0.813199 11.00000 -1.20000 AFIX 0 C5 1 1.166403 0.796901 0.840860 11.00000 0.03147 0.03267 = 0.02160 0.01182 0.00187 0.00431 AFIX 43 H5 2 1.167472 0.794856 0.907620 11.00000 -1.20000 AFIX 0 C6 1 1.249598 0.780317 0.802173 11.00000 0.02052 0.02581 = 0.03138 0.00702 0.00338 0.00451 C7 1 1.243110 0.779296 0.702448 11.00000 0.02337 0.04870 = 0.03561 0.01328 0.00894 0.01231 AFIX 43 H7 2 1.298030 0.766431 0.673276 11.00000 -1.20000 AFIX 0 C8 1 1.158239 0.796640 0.644507 11.00000 0.02815 0.04593 = 0.02439 0.01190 0.01007 0.01059 AFIX 43 H8 2 1.155210 0.794741 0.576170 11.00000 -1.20000 AFIX 0 C9 1 1.347047 0.765429 0.865398 11.00000 0.02821 0.04208 = 0.03897 0.01282 -0.00004 0.01265 C10 1 1.374576 0.666391 0.807007 11.00000 0.05504 0.05466 = 0.06889 0.01049 -0.00247 0.03424 AFIX 137 H10A 2 1.435018 0.656682 0.849622 11.00000 -1.50000 H10B 2 1.387836 0.670363 0.742673 11.00000 -1.50000 H10C 2 1.318528 0.608622 0.791283 11.00000 -1.50000 AFIX 0 C11 1 1.431834 0.856111 0.885551 11.00000 0.02462 0.05909 = 0.08097 0.02306 -0.00390 0.00640 AFIX 137 H11A 2 1.414154 0.919386 0.923521 11.00000 -1.50000 H11B 2 1.441568 0.859290 0.819747 11.00000 -1.50000 H11C 2 1.494302 0.847968 0.926344 11.00000 -1.50000 AFIX 0 C12 1 1.336064 0.760061 0.969418 11.00000 0.04394 0.09556 = 0.05094 0.03739 0.00062 0.03239 AFIX 137 H12A 2 1.398580 0.748414 1.006542 11.00000 -1.50000 H12B 2 1.280004 0.703757 0.957999 11.00000 -1.50000 H12C 2 1.322584 0.824580 1.010255 11.00000 -1.50000 AFIX 0 C13 1 0.715801 0.652295 0.538623 11.00000 0.02155 0.02011 = 0.02492 0.01053 0.00650 0.00572 C14 1 0.606935 0.567270 0.386138 11.00000 0.02674 0.02863 = 0.02352 0.00667 0.00304 0.00433 AFIX 43 H14 2 0.563710 0.511832 0.329318 11.00000 -1.20000 AFIX 0 C15 1 0.661761 0.462872 0.493574 11.00000 0.02873 0.01731 = 0.02345 0.00582 0.00889 0.00690 C16 1 0.573101 0.389936 0.461664 11.00000 0.02512 0.02281 = 0.03298 0.00726 0.00809 0.00711 AFIX 43 H16 2 0.512424 0.401887 0.426569 11.00000 -1.20000 AFIX 0 C17 1 0.573189 0.299143 0.481167 11.00000 0.02560 0.02195 = 0.04089 0.00850 0.01084 0.00245 AFIX 43 H17 2 0.512299 0.248789 0.457547 11.00000 -1.20000 AFIX 0 C18 1 0.660227 0.279949 0.534462 11.00000 0.02899 0.02018 = 0.03192 0.00827 0.01419 0.00759 C19 1 0.749046 0.354391 0.564895 11.00000 0.02667 0.02392 = 0.03164 0.01058 0.00866 0.00857 AFIX 43 H19 2 0.809762 0.343031 0.600584 11.00000 -1.20000 AFIX 0 C20 1 0.750390 0.445141 0.543922 11.00000 0.02570 0.01989 = 0.03064 0.00791 0.00733 0.00259 AFIX 43 H20 2 0.811697 0.494351 0.564068 11.00000 -1.20000 AFIX 0 C21 1 0.656209 0.180571 0.558738 11.00000 0.03150 0.02294 = 0.05381 0.01874 0.01445 0.00700 C22 1 0.579779 0.173906 0.621755 11.00000 0.06037 0.04069 = 0.09668 0.04747 0.04616 0.02173 AFIX 137 H22A 2 0.599314 0.233658 0.685321 11.00000 -1.50000 H22B 2 0.578269 0.111544 0.639007 11.00000 -1.50000 H22C 2 0.512734 0.172240 0.581355 11.00000 -1.50000 AFIX 0 C23 1 0.623172 0.088431 0.457575 11.00000 0.04661 0.02285 = 0.06964 0.01181 0.00652 0.00768 AFIX 137 H23A 2 0.559104 0.092202 0.415703 11.00000 -1.50000 H23B 2 0.614599 0.025067 0.473057 11.00000 -1.50000 H23C 2 0.674750 0.089283 0.419473 11.00000 -1.50000 AFIX 0 C24 1 0.759048 0.174814 0.620026 11.00000 0.04342 0.03682 = 0.06388 0.03205 0.00857 0.00904 AFIX 137 H24A 2 0.808728 0.178542 0.580213 11.00000 -1.50000 H24B 2 0.753070 0.110182 0.633209 11.00000 -1.50000 H24C 2 0.780919 0.232047 0.685737 11.00000 -1.50000 AFIX 0 C25 1 0.729391 0.825722 0.709140 11.00000 0.02001 0.01918 = 0.02127 0.00787 0.00464 0.00304 C26 1 0.646707 0.948375 0.758864 11.00000 0.03452 0.02432 = 0.02882 0.00850 0.01176 0.01366 AFIX 43 H26 2 0.616404 0.995091 0.801192 11.00000 -1.20000 AFIX 0 C27 1 0.702701 0.865019 0.886742 11.00000 0.02494 0.02802 = 0.02054 0.00949 0.00858 0.00668 C28 1 0.679673 0.768015 0.890119 11.00000 0.03978 0.02338 = 0.02212 0.00364 0.00891 0.00367 AFIX 43 H28 2 0.662669 0.709923 0.828785 11.00000 -1.20000 AFIX 0 C29 1 0.681686 0.756453 0.984298 11.00000 0.04181 0.02714 = 0.03031 0.01106 0.00894 0.00292 AFIX 43 H29 2 0.666656 0.689469 0.986619 11.00000 -1.20000 AFIX 0 C30 1 0.704984 0.839670 1.075623 11.00000 0.03039 0.03280 = 0.02296 0.00921 0.00869 0.00431 C31 1 0.728434 0.935689 1.069056 11.00000 0.04951 0.02866 = 0.02083 0.00168 0.00831 0.00010 AFIX 43 H31 2 0.745317 0.994085 1.130098 11.00000 -1.20000 AFIX 0 C32 1 0.727973 0.949075 0.975630 11.00000 0.04125 0.02145 = 0.02714 0.00596 0.00738 0.00333 AFIX 43 H32 2 0.744985 1.015786 0.973155 11.00000 -1.20000 AFIX 0 C33 1 0.700916 0.827302 1.179035 11.00000 0.04755 0.05151 = 0.02314 0.01587 0.00947 -0.00130 C34 1 0.702882 0.718731 1.175936 11.00000 0.22542 0.05872 = 0.04500 0.03177 0.04919 0.01134 AFIX 137 H34A 2 0.759545 0.697227 1.149768 11.00000 -1.50000 H34B 2 0.639580 0.672764 1.130475 11.00000 -1.50000 H34C 2 0.710787 0.716212 1.245567 11.00000 -1.50000 AFIX 0 C35 1 0.788823 0.898226 1.265756 11.00000 0.07882 0.09193 = 0.03229 0.02879 -0.01038 -0.02332 AFIX 137 H35A 2 0.852152 0.882520 1.251292 11.00000 -1.50000 H35B 2 0.783679 0.888916 1.330599 11.00000 -1.50000 H35C 2 0.787591 0.969189 1.271559 11.00000 -1.50000 AFIX 0 C36 1 0.604523 0.852160 1.203838 11.00000 0.06250 0.23430 = 0.04508 0.06364 0.03108 0.03892 AFIX 137 H36A 2 0.603159 0.847716 1.271415 11.00000 -1.50000 H36B 2 0.546668 0.803347 1.151148 11.00000 -1.50000 H36C 2 0.601120 0.921565 1.205063 11.00000 -1.50000 AFIX 0 O2 4 0.425809 0.468223 0.189252 11.00000 0.05606 0.04519 = 0.04593 0.00700 0.01240 0.00003 C37 1 0.351757 0.514973 0.231394 11.00000 0.04966 0.06685 = 0.07326 0.00314 0.01612 0.01325 AFIX 23 H37A 2 0.384462 0.577799 0.291551 11.00000 -1.20000 H37B 2 0.310104 0.467476 0.253753 11.00000 -1.20000 AFIX 0 C38 1 0.288192 0.540094 0.147527 11.00000 0.10946 0.09974 = 0.10845 0.02111 -0.02195 0.02485 AFIX 23 H38A 2 0.262177 0.602087 0.175532 11.00000 -1.20000 H38B 2 0.230880 0.482521 0.104706 11.00000 -1.20000 AFIX 0 C39 1 0.362808 0.558141 0.087374 11.00000 0.17131 0.13484 = 0.14051 0.11002 0.00157 0.01556 AFIX 23 H39A 2 0.334236 0.518695 0.013000 11.00000 -1.20000 H39B 2 0.380461 0.631573 0.096714 11.00000 -1.20000 AFIX 0 C40 1 0.453342 0.523127 0.129119 11.00000 0.11005 0.10905 = 0.06149 0.04435 0.00712 -0.03597 AFIX 23 H40A 2 0.476161 0.479361 0.072105 11.00000 -1.20000 H40B 2 0.509098 0.582535 0.171224 11.00000 -1.20000 AFIX 0 O3 4 1.004484 0.668799 0.406506 11.00000 0.10155 0.11516 = 0.17507 0.06070 0.00803 -0.00450 C41 1 0.950201 0.646771 0.306975 11.00000 0.18654 0.26901 = 0.27941 0.21698 -0.15450 -0.12873 AFIX 23 H41A 2 0.996508 0.642773 0.261703 11.00000 -1.20000 H41B 2 0.914099 0.701938 0.302853 11.00000 -1.20000 AFIX 0 C42 1 0.879850 0.552557 0.273079 11.00000 0.21228 0.21821 = 0.30915 0.17338 -0.13870 -0.11349 AFIX 23 H42A 2 0.881664 0.508952 0.203778 11.00000 -1.20000 H42B 2 0.810586 0.563848 0.270433 11.00000 -1.20000 AFIX 0 C43 1 0.911061 0.506474 0.347879 11.00000 0.21202 0.09451 = 0.11955 0.03161 -0.01247 -0.03493 AFIX 23 H43A 2 0.954244 0.458311 0.324678 11.00000 -1.20000 H43B 2 0.851943 0.469009 0.360389 11.00000 -1.20000 AFIX 0 C44 1 0.966829 0.590565 0.439609 11.00000 0.15636 0.06746 = 0.16144 0.00432 0.08935 -0.00705 AFIX 23 H44A 2 0.922251 0.613787 0.484571 11.00000 -1.20000 H44B 2 1.022829 0.569832 0.478686 11.00000 -1.20000 AFIX 6 PART 1 O4 4 0.137740 0.868035 0.082926 21.00000 0.09101 0.11294 = 0.09608 0.04578 0.05908 0.01943 C45 1 0.060837 0.925361 0.072085 21.00000 0.11971 0.12415 = 0.21792 0.08997 0.09885 0.03069 AFIX 23 H45A 2 0.022732 0.904134 -0.001036 21.00000 -1.20000 H45B 2 0.091061 0.999386 0.097047 21.00000 -1.20000 AFIX 5 C46 1 -0.005472 0.903436 0.134279 21.00000 0.13898 0.15185 = 0.20520 0.08339 0.10274 0.05441 AFIX 23 H46A 2 0.018008 0.952626 0.205825 21.00000 -1.20000 H46B 2 -0.075536 0.906544 0.104399 21.00000 -1.20000 AFIX 5 C47 1 0.000789 0.800818 0.131541 21.00000 0.15902 0.16121 = 0.19402 0.11776 0.10335 0.03139 AFIX 23 H47A 2 -0.063512 0.752000 0.090399 21.00000 -1.20000 H47B 2 0.016032 0.798065 0.202073 21.00000 -1.20000 AFIX 5 C48 1 0.086414 0.775399 0.081316 21.00000 0.14948 0.13942 = 0.11125 0.07622 0.03689 0.05685 AFIX 23 H48A 2 0.131816 0.744293 0.120627 21.00000 -1.20000 H48B 2 0.059096 0.727117 0.009635 21.00000 -1.20000 AFIX 5 PART 2 O4A 4 0.048962 0.803665 0.040420 -21.00000 0.27815 0.19295 = 0.15801 -0.02527 -0.00061 0.10695 C45A 1 -0.011161 0.880345 0.042475 -21.00000 0.13754 0.17568 = 0.10532 -0.00415 0.03360 0.04645 AFIX 23 H45C 2 -0.081925 0.852527 0.038723 -21.00000 -1.20000 H45D 2 -0.010115 0.905265 -0.015667 -21.00000 -1.20000 AFIX 5 C46A 1 0.036914 0.962159 0.141031 -21.00000 0.14872 0.07667 = 0.10123 0.01596 0.05066 -0.01695 AFIX 23 H46C 2 0.089589 1.011990 0.133118 -21.00000 -1.20000 H46D 2 -0.013496 0.998531 0.167773 -21.00000 -1.20000 AFIX 5 C47A 1 0.080754 0.913748 0.209715 -21.00000 0.08915 0.10882 = 0.15675 -0.01510 -0.02645 0.04850 AFIX 23 H47C 2 0.134730 0.963348 0.268221 -21.00000 -1.20000 H47D 2 0.029070 0.882984 0.236954 -21.00000 -1.20000 AFIX 5 C48A 1 0.119803 0.838899 0.148892 -21.00000 0.16064 0.16497 = 0.10968 0.01837 0.05433 0.04926 AFIX 23 H48C 2 0.121326 0.781150 0.174731 -21.00000 -1.20000 H48D 2 0.189177 0.867221 0.148846 -21.00000 -1.20000 PART 0 HKLF 5 1 1 0 0 0 1 0 0 0 1 REM twin4 in P-1 REM R1 = 0.0524 for 8444 Fo > 4sig(Fo) and 0.0709 for all 10272 data REM 612 parameters refined using 152 restraints END WGHT 0.0655 1.7442 REM Highest difference peak 0.636, deepest hole -0.524, 1-sigma level 0.077 Q1 1 0.0991 0.9400 0.1438 11.00000 0.05 0.64 Q2 1 0.0083 0.5548 0.0353 11.00000 0.05 0.56 Q3 1 -0.0178 0.4880 0.0088 11.00000 0.05 0.53 Q4 1 -0.0180 0.7732 0.0639 11.00000 0.05 0.45 Q5 1 -0.0291 0.8091 0.0306 11.00000 0.05 0.45 Q6 1 0.9174 0.6440 0.3778 11.00000 0.05 0.44 Q7 1 0.9297 0.6594 0.3514 11.00000 0.05 0.41 Q8 1 0.8797 0.5762 0.3795 11.00000 0.05 0.39 Q9 1 0.0444 0.8634 0.1892 11.00000 0.05 0.37 Q10 1 0.9558 0.5549 0.2253 11.00000 0.05 0.37 ; data_jsnmsusal1072_0m-sr _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Smith, Jeremy M.' _publ_contact_author_address ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; _publ_contact_author_email jesmith@nmsu.edu loop_ _publ_author_name _publ_author_address 'Smith, Jeremy M.' ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; 'Munoz, Salvador B.' ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; 'Foster, Wallace K.' ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; 'Lin, Hsui-Jung' ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; 'Margarit, Charles G.' ;Department of Chemistry and Biochemistry New Mexico State University Las Cruces, NM, 88003 USA ; 'Dickie, Diane A.' ;Department of Chemistry and Chemical Biology University of New Mexico Albuquerque, NM, 87131 USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H37 B N10 Ni O' _chemical_formula_weight 659.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 8.7177(17) _cell_length_b 12.974(3) _cell_length_c 17.960(4) _cell_angle_alpha 74.731(4) _cell_angle_beta 77.159(4) _cell_angle_gamma 72.128(3) _cell_volume 1842.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.81 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7794 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41686 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 27.10 _reflns_number_total 8112 _reflns_number_gt 6478 _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. ; _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^)+(0.0598P)^2^+0.3175P] 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 8112 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ni1 Ni 0.27975(3) 0.37659(2) 0.280818(14) 0.02254(9) Uani 1 1 d . . . B1 B -0.0439(2) 0.37000(18) 0.39306(13) 0.0251(5) Uani 1 1 d . . . H1 H -0.1483 0.3674 0.4295 0.030 Uiso 1 1 calc R . . O1 O 0.5447(2) 0.3377(2) 0.16102(12) 0.0683(6) Uani 1 1 d . . . N1 N 0.00574(18) 0.47874(13) 0.38222(9) 0.0235(3) Uani 1 1 d . . . N2 N -0.07596(18) 0.56256(13) 0.42249(10) 0.0259(4) Uani 1 1 d . . . N3 N 0.15484(17) 0.59089(13) 0.35083(9) 0.0231(3) Uani 1 1 d . . . N4 N 0.10644(17) 0.27495(13) 0.42014(9) 0.0229(3) Uani 1 1 d . . . N5 N 0.10261(18) 0.19403(13) 0.48823(9) 0.0239(3) Uani 1 1 d . . . N6 N 0.35273(17) 0.18008(12) 0.42351(9) 0.0224(3) Uani 1 1 d . . . N7 N -0.04817(18) 0.36050(14) 0.30909(10) 0.0265(4) Uani 1 1 d . . . N8 N -0.1813(2) 0.35554(15) 0.28172(11) 0.0343(4) Uani 1 1 d . . . N9 N 0.0317(2) 0.36101(15) 0.18802(10) 0.0318(4) Uani 1 1 d . . . N10 N 0.4421(2) 0.36324(15) 0.21316(10) 0.0315(4) Uani 1 1 d . . . C1 C 0.1463(2) 0.49375(15) 0.33822(11) 0.0229(4) Uani 1 1 d . . . C2 C 0.0182(2) 0.62843(16) 0.40205(12) 0.0272(4) Uani 1 1 d . . . H2 H -0.0042 0.6948 0.4202 0.033 Uiso 1 1 calc R . . C3 C 0.2915(2) 0.63938(16) 0.32426(12) 0.0251(4) Uani 1 1 d . . . C4 C 0.4368(2) 0.58048(17) 0.35375(13) 0.0298(4) Uani 1 1 d . . . C5 C 0.5673(2) 0.62821(19) 0.32825(14) 0.0373(5) Uani 1 1 d . . . H5 H 0.6678 0.5899 0.3469 0.045 Uiso 1 1 calc R . . C6 C 0.5557(3) 0.72879(19) 0.27707(15) 0.0395(5) Uani 1 1 d . . . C7 C 0.4080(3) 0.78533(18) 0.25058(14) 0.0378(5) Uani 1 1 d . . . H7 H 0.3982 0.8559 0.2164 0.045 Uiso 1 1 calc R . . C8 C 0.2744(2) 0.74114(17) 0.27289(13) 0.0304(4) Uani 1 1 d . . . C9 C 0.1167(3) 0.80180(19) 0.24081(15) 0.0422(6) Uani 1 1 d . . . H9A H 0.1313 0.8684 0.2020 0.063 Uiso 1 1 calc R . . H9B H 0.0301 0.8230 0.2835 0.063 Uiso 1 1 calc R . . H9C H 0.0867 0.7533 0.2162 0.063 Uiso 1 1 calc R . . C10 C 0.7037(3) 0.7758(2) 0.2503(2) 0.0658(9) Uani 1 1 d . . . H10A H 0.7153 0.8094 0.2909 0.099 Uiso 1 1 calc R . . H10B H 0.6891 0.8321 0.2020 0.099 Uiso 1 1 calc R . . H10C H 0.8018 0.7160 0.2407 0.099 Uiso 1 1 calc R . . C11 C 0.4541(2) 0.47146(18) 0.41132(13) 0.0356(5) Uani 1 1 d . . . H11A H 0.4739 0.4119 0.3835 0.053 Uiso 1 1 calc R . . H11B H 0.3537 0.4735 0.4492 0.053 Uiso 1 1 calc R . . H11C H 0.5460 0.4580 0.4388 0.053 Uiso 1 1 calc R . . C12 C 0.2564(2) 0.26834(15) 0.37978(11) 0.0227(4) Uani 1 1 d . . . C13 C 0.2548(2) 0.13824(15) 0.48823(12) 0.0247(4) Uani 1 1 d . . . H13 H 0.2932 0.0765 0.5279 0.030 Uiso 1 1 calc R . . C14 C 0.5284(2) 0.14168(15) 0.40706(11) 0.0230(4) Uani 1 1 d . . . C15 C 0.6219(2) 0.15742(15) 0.45488(12) 0.0247(4) Uani 1 1 d . . . C16 C 0.7910(2) 0.12276(16) 0.43580(12) 0.0272(4) Uani 1 1 d . . . H16 H 0.8573 0.1326 0.4674 0.033 Uiso 1 1 calc R . . C17 C 0.8652(2) 0.07447(16) 0.37215(13) 0.0293(4) Uani 1 1 d . . . C18 C 0.7675(2) 0.05954(16) 0.32649(12) 0.0284(4) Uani 1 1 d . . . H18 H 0.8178 0.0264 0.2828 0.034 Uiso 1 1 calc R . . C19 C 0.5973(2) 0.09203(16) 0.34319(12) 0.0257(4) Uani 1 1 d . . . C20 C 0.4942(2) 0.07212(18) 0.29418(14) 0.0350(5) Uani 1 1 d . . . H20A H 0.4209 0.0287 0.3277 0.053 Uiso 1 1 calc R . . H20B H 0.5650 0.0314 0.2549 0.053 Uiso 1 1 calc R . . H20C H 0.4298 0.1433 0.2680 0.053 Uiso 1 1 calc R . . C21 C 1.0490(2) 0.0396(2) 0.35312(15) 0.0429(6) Uani 1 1 d . . . H21A H 1.0810 -0.0002 0.3103 0.064 Uiso 1 1 calc R . . H21B H 1.0944 -0.0090 0.3993 0.064 Uiso 1 1 calc R . . H21C H 1.0909 0.1054 0.3373 0.064 Uiso 1 1 calc R . . C22 C 0.5476(3) 0.20746(18) 0.52549(13) 0.0331(5) Uani 1 1 d . . . H22A H 0.5247 0.1495 0.5705 0.050 Uiso 1 1 calc R . . H22B H 0.4458 0.2641 0.5155 0.050 Uiso 1 1 calc R . . H22C H 0.6239 0.2415 0.5365 0.050 Uiso 1 1 calc R . . C23 C 0.0819(2) 0.36455(16) 0.25355(12) 0.0261(4) Uani 1 1 d . . . C24 C -0.1283(3) 0.3556(2) 0.20836(14) 0.0387(5) Uani 1 1 d . . . H24 H -0.1919 0.3523 0.1728 0.046 Uiso 1 1 calc R . . C25 C 0.1299(3) 0.36747(19) 0.11190(13) 0.0351(5) Uani 1 1 d . . . C26 C 0.1536(3) 0.4704(2) 0.07030(13) 0.0389(5) Uani 1 1 d . . . C27 C 0.2564(3) 0.4735(2) -0.00076(14) 0.0461(6) Uani 1 1 d . . . H27 H 0.2753 0.5424 -0.0294 0.055 Uiso 1 1 calc R . . C28 C 0.3321(4) 0.3805(2) -0.03123(15) 0.0557(7) Uani 1 1 d . . . C29 C 0.3037(4) 0.2808(2) 0.01140(16) 0.0593(8) Uani 1 1 d . . . H29 H 0.3540 0.2163 -0.0096 0.071 Uiso 1 1 calc R . . C30 C 0.2047(3) 0.2711(2) 0.08374(14) 0.0455(6) Uani 1 1 d . . . C31 C 0.1842(4) 0.1598(2) 0.13141(18) 0.0655(8) Uani 1 1 d . . . H31A H 0.2292 0.1427 0.1800 0.098 Uiso 1 1 calc R . . H31B H 0.2420 0.1024 0.1013 0.098 Uiso 1 1 calc R . . H31C H 0.0680 0.1623 0.1438 0.098 Uiso 1 1 calc R . . C32 C 0.4465(5) 0.3878(3) -0.10875(17) 0.0836(11) Uani 1 1 d . . . H32A H 0.5157 0.3137 -0.1135 0.125 Uiso 1 1 calc R . . H32B H 0.5152 0.4362 -0.1110 0.125 Uiso 1 1 calc R . . H32C H 0.3823 0.4183 -0.1517 0.125 Uiso 1 1 calc R . . C33 C 0.0726(3) 0.5731(2) 0.10229(16) 0.0507(6) Uani 1 1 d . . . H33A H 0.1266 0.5719 0.1450 0.076 Uiso 1 1 calc R . . H33B H -0.0426 0.5761 0.1220 0.076 Uiso 1 1 calc R . . H33C H 0.0808 0.6385 0.0608 0.076 Uiso 1 1 calc R . . 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 0.01611(12) 0.02510(14) 0.02710(15) -0.00761(10) -0.00332(9) -0.00466(9) B1 0.0151(9) 0.0276(11) 0.0302(12) -0.0064(9) -0.0021(8) -0.0031(8) O1 0.0376(10) 0.1186(18) 0.0594(12) -0.0478(12) 0.0203(9) -0.0312(11) N1 0.0170(7) 0.0242(8) 0.0282(9) -0.0076(7) -0.0049(6) -0.0012(6) N2 0.0202(8) 0.0251(8) 0.0292(9) -0.0082(7) -0.0041(7) 0.0011(6) N3 0.0172(7) 0.0230(8) 0.0298(9) -0.0084(7) -0.0049(6) -0.0032(6) N4 0.0185(7) 0.0220(8) 0.0272(9) -0.0047(7) -0.0039(6) -0.0041(6) N5 0.0210(8) 0.0210(8) 0.0297(9) -0.0050(7) -0.0039(7) -0.0058(6) N6 0.0163(7) 0.0201(8) 0.0298(9) -0.0063(7) -0.0042(6) -0.0022(6) N7 0.0176(7) 0.0310(9) 0.0333(9) -0.0072(7) -0.0083(7) -0.0065(6) N8 0.0247(8) 0.0413(11) 0.0424(11) -0.0067(9) -0.0148(8) -0.0114(7) N9 0.0283(9) 0.0393(10) 0.0329(10) -0.0085(8) -0.0104(7) -0.0115(7) N10 0.0229(8) 0.0425(10) 0.0342(10) -0.0136(8) -0.0011(7) -0.0135(7) C1 0.0177(8) 0.0246(10) 0.0272(10) -0.0049(8) -0.0084(7) -0.0035(7) C2 0.0240(9) 0.0250(10) 0.0311(11) -0.0093(8) -0.0073(8) 0.0005(8) C3 0.0200(9) 0.0252(10) 0.0340(11) -0.0134(8) -0.0041(8) -0.0057(7) C4 0.0245(9) 0.0300(11) 0.0389(12) -0.0141(9) -0.0083(9) -0.0048(8) C5 0.0219(10) 0.0395(13) 0.0569(15) -0.0207(11) -0.0103(10) -0.0056(9) C6 0.0256(10) 0.0396(13) 0.0607(16) -0.0233(12) 0.0003(10) -0.0132(9) C7 0.0367(12) 0.0288(11) 0.0497(14) -0.0107(10) -0.0023(10) -0.0124(9) C8 0.0270(10) 0.0270(10) 0.0399(12) -0.0117(9) -0.0058(9) -0.0064(8) C9 0.0369(12) 0.0310(12) 0.0567(16) 0.0023(11) -0.0181(11) -0.0083(9) C10 0.0377(14) 0.0572(18) 0.108(3) -0.0199(17) 0.0023(15) -0.0275(13) C11 0.0274(10) 0.0382(12) 0.0420(13) -0.0090(10) -0.0152(9) -0.0024(9) C12 0.0188(8) 0.0221(9) 0.0289(10) -0.0088(8) -0.0057(7) -0.0034(7) C13 0.0227(9) 0.0203(9) 0.0299(11) -0.0040(8) -0.0053(8) -0.0041(7) C14 0.0160(8) 0.0185(9) 0.0321(11) -0.0034(8) -0.0054(7) -0.0018(7) C15 0.0252(9) 0.0174(9) 0.0316(11) -0.0028(8) -0.0068(8) -0.0062(7) C16 0.0219(9) 0.0236(10) 0.0375(12) -0.0019(9) -0.0096(8) -0.0083(8) C17 0.0186(9) 0.0258(10) 0.0399(12) -0.0018(9) -0.0040(8) -0.0056(8) C18 0.0212(9) 0.0260(10) 0.0338(11) -0.0068(9) -0.0013(8) -0.0017(8) C19 0.0207(9) 0.0219(9) 0.0343(11) -0.0063(8) -0.0067(8) -0.0030(7) C20 0.0276(10) 0.0373(12) 0.0447(13) -0.0195(10) -0.0116(9) -0.0013(9) C21 0.0191(10) 0.0534(15) 0.0544(15) -0.0125(12) -0.0022(10) -0.0087(10) C22 0.0328(11) 0.0337(11) 0.0349(12) -0.0099(9) -0.0082(9) -0.0074(9) C23 0.0261(9) 0.0246(10) 0.0294(11) -0.0080(8) -0.0073(8) -0.0054(8) C24 0.0298(11) 0.0502(14) 0.0446(14) -0.0100(11) -0.0159(10) -0.0152(10) C25 0.0353(11) 0.0454(13) 0.0301(11) -0.0107(10) -0.0122(9) -0.0114(10) C26 0.0395(12) 0.0457(14) 0.0332(12) -0.0087(10) -0.0120(10) -0.0087(10) C27 0.0548(15) 0.0495(15) 0.0316(13) -0.0022(11) -0.0105(11) -0.0128(12) C28 0.0682(18) 0.0630(18) 0.0308(13) -0.0107(13) -0.0069(12) -0.0097(14) C29 0.080(2) 0.0563(18) 0.0418(15) -0.0235(14) -0.0095(14) -0.0069(15) C30 0.0592(15) 0.0458(14) 0.0372(14) -0.0143(11) -0.0121(12) -0.0142(12) C31 0.092(2) 0.0527(17) 0.0581(19) -0.0198(15) -0.0093(17) -0.0222(16) C32 0.111(3) 0.080(2) 0.0389(17) -0.0136(16) 0.0075(17) -0.008(2) C33 0.0580(16) 0.0424(14) 0.0490(16) -0.0101(12) -0.0045(13) -0.0114(12) _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 N10 1.6448(17) . ? Ni1 C23 1.9549(19) . ? Ni1 C12 1.968(2) . ? Ni1 C1 1.9834(19) . ? B1 N1 1.552(3) . ? B1 N7 1.555(3) . ? B1 N4 1.565(2) . ? B1 H1 1.0000 . ? O1 N10 1.182(2) . ? N1 C1 1.341(2) . ? N1 N2 1.387(2) . ? N2 C2 1.292(3) . ? N3 C1 1.364(2) . ? N3 C2 1.377(2) . ? N3 C3 1.447(2) . ? N4 C12 1.336(2) . ? N4 N5 1.388(2) . ? N5 C13 1.302(2) . ? N6 C12 1.365(2) . ? N6 C13 1.373(2) . ? N6 C14 1.445(2) . ? N7 C23 1.338(3) . ? N7 N8 1.382(2) . ? N8 C24 1.296(3) . ? N9 C23 1.359(2) . ? N9 C24 1.380(3) . ? N9 C25 1.439(3) . ? C2 H2 0.9500 . ? C3 C8 1.384(3) . ? C3 C4 1.400(3) . ? C4 C5 1.392(3) . ? C4 C11 1.503(3) . ? C5 C6 1.373(3) . ? C5 H5 0.9500 . ? C6 C7 1.389(3) . ? C6 C10 1.523(3) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.513(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 H13 0.9500 . ? C14 C19 1.392(3) . ? C14 C15 1.396(3) . ? C15 C16 1.394(3) . ? C15 C22 1.503(3) . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 C21 1.511(3) . ? C18 C19 1.399(3) . ? C18 H18 0.9500 . ? C19 C20 1.504(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 H24 0.9500 . ? C25 C30 1.390(3) . ? C25 C26 1.400(3) . ? C26 C27 1.386(3) . ? C26 C33 1.500(3) . ? C27 C28 1.375(4) . ? C27 H27 0.9500 . ? C28 C29 1.382(4) . ? C28 C32 1.521(4) . ? C29 C30 1.390(4) . ? C29 H29 0.9500 . ? C30 C31 1.512(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Ni1 C23 116.03(8) . . ? N10 Ni1 C12 124.24(8) . . ? C23 Ni1 C12 91.46(8) . . ? N10 Ni1 C1 135.73(8) . . ? C23 Ni1 C1 89.87(8) . . ? C12 Ni1 C1 87.57(8) . . ? N1 B1 N7 105.04(16) . . ? N1 B1 N4 105.02(14) . . ? N7 B1 N4 105.12(15) . . ? N1 B1 H1 113.6 . . ? N7 B1 H1 113.6 . . ? N4 B1 H1 113.6 . . ? C1 N1 N2 113.22(15) . . ? C1 N1 B1 121.35(15) . . ? N2 N1 B1 125.01(15) . . ? C2 N2 N1 103.36(15) . . ? C1 N3 C2 107.77(15) . . ? C1 N3 C3 126.74(15) . . ? C2 N3 C3 125.02(16) . . ? C12 N4 N5 113.08(14) . . ? C12 N4 B1 121.48(16) . . ? N5 N4 B1 125.35(15) . . ? C13 N5 N4 103.53(15) . . ? C12 N6 C13 108.13(15) . . ? C12 N6 C14 125.88(16) . . ? C13 N6 C14 125.88(15) . . ? C23 N7 N8 113.14(16) . . ? C23 N7 B1 120.40(15) . . ? N8 N7 B1 126.30(16) . . ? C24 N8 N7 103.36(16) . . ? C23 N9 C24 107.34(18) . . ? C23 N9 C25 124.46(17) . . ? C24 N9 C25 128.14(17) . . ? O1 N10 Ni1 165.59(17) . . ? N1 C1 N3 103.73(15) . . ? N1 C1 Ni1 117.32(13) . . ? N3 C1 Ni1 138.88(14) . . ? N2 C2 N3 111.92(17) . . ? N2 C2 H2 124.0 . . ? N3 C2 H2 124.0 . . ? C8 C3 C4 122.69(18) . . ? C8 C3 N3 119.94(16) . . ? C4 C3 N3 117.36(17) . . ? C5 C4 C3 116.9(2) . . ? C5 C4 C11 120.37(18) . . ? C3 C4 C11 122.71(18) . . ? C6 C5 C4 122.27(19) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 118.80(19) . . ? C5 C6 C10 119.8(2) . . ? C7 C6 C10 121.4(2) . . ? C8 C7 C6 121.6(2) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C3 C8 C7 117.72(19) . . ? C3 C8 C9 121.46(18) . . ? C7 C8 C9 120.8(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.5 . . ? C4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N6 103.94(16) . . ? N4 C12 Ni1 117.53(13) . . ? N6 C12 Ni1 138.53(14) . . ? N5 C13 N6 111.32(17) . . ? N5 C13 H13 124.3 . . ? N6 C13 H13 124.3 . . ? C19 C14 C15 122.77(17) . . ? C19 C14 N6 118.36(16) . . ? C15 C14 N6 118.86(17) . . ? C16 C15 C14 117.36(18) . . ? C16 C15 C22 119.80(18) . . ? C14 C15 C22 122.82(17) . . ? C17 C16 C15 121.99(18) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 118.75(17) . . ? C16 C17 C21 120.11(19) . . ? C18 C17 C21 121.1(2) . . ? C17 C18 C19 121.72(19) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C14 C19 C18 117.39(18) . . ? C14 C19 C20 121.89(17) . . ? C18 C19 C20 120.71(18) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N7 C23 N9 104.30(16) . . ? N7 C23 Ni1 118.90(14) . . ? N9 C23 Ni1 136.78(15) . . ? N8 C24 N9 111.86(18) . . ? N8 C24 H24 124.1 . . ? N9 C24 H24 124.1 . . ? C30 C25 C26 122.1(2) . . ? C30 C25 N9 119.3(2) . . ? C26 C25 N9 118.6(2) . . ? C27 C26 C25 117.6(2) . . ? C27 C26 C33 121.3(2) . . ? C25 C26 C33 121.1(2) . . ? C28 C27 C26 122.4(3) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 118.1(3) . . ? C27 C28 C32 120.4(3) . . ? C29 C28 C32 121.5(3) . . ? C28 C29 C30 122.7(3) . . ? C28 C29 H29 118.7 . . ? C30 C29 H29 118.7 . . ? C25 C30 C29 117.2(2) . . ? C25 C30 C31 121.2(2) . . ? C29 C30 C31 121.6(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 B1 N1 C1 -58.5(2) . . . . ? N4 B1 N1 C1 52.1(2) . . . . ? N7 B1 N1 N2 129.54(17) . . . . ? N4 B1 N1 N2 -119.86(17) . . . . ? C1 N1 N2 C2 -0.1(2) . . . . ? B1 N1 N2 C2 172.46(17) . . . . ? N1 B1 N4 C12 -52.9(2) . . . . ? N7 B1 N4 C12 57.6(2) . . . . ? N1 B1 N4 N5 123.54(17) . . . . ? N7 B1 N4 N5 -125.92(17) . . . . ? C12 N4 N5 C13 0.2(2) . . . . ? B1 N4 N5 C13 -176.47(17) . . . . ? N1 B1 N7 C23 54.2(2) . . . . ? N4 B1 N7 C23 -56.3(2) . . . . ? N1 B1 N7 N8 -120.84(19) . . . . ? N4 B1 N7 N8 128.64(18) . . . . ? C23 N7 N8 C24 0.6(2) . . . . ? B1 N7 N8 C24 175.96(19) . . . . ? C23 Ni1 N10 O1 -34.6(8) . . . . ? C12 Ni1 N10 O1 76.9(8) . . . . ? C1 Ni1 N10 O1 -154.4(7) . . . . ? N2 N1 C1 N3 0.0(2) . . . . ? B1 N1 C1 N3 -172.86(16) . . . . ? N2 N1 C1 Ni1 177.60(11) . . . . ? B1 N1 C1 Ni1 4.7(2) . . . . ? C2 N3 C1 N1 0.09(19) . . . . ? C3 N3 C1 N1 172.47(17) . . . . ? C2 N3 C1 Ni1 -176.65(16) . . . . ? C3 N3 C1 Ni1 -4.3(3) . . . . ? N10 Ni1 C1 N1 170.48(13) . . . . ? C23 Ni1 C1 N1 41.71(15) . . . . ? C12 Ni1 C1 N1 -49.76(14) . . . . ? N10 Ni1 C1 N3 -13.1(3) . . . . ? C23 Ni1 C1 N3 -141.9(2) . . . . ? C12 Ni1 C1 N3 126.7(2) . . . . ? N1 N2 C2 N3 0.2(2) . . . . ? C1 N3 C2 N2 -0.2(2) . . . . ? C3 N3 C2 N2 -172.71(17) . . . . ? C1 N3 C3 C8 117.3(2) . . . . ? C2 N3 C3 C8 -71.5(3) . . . . ? C1 N3 C3 C4 -63.9(3) . . . . ? C2 N3 C3 C4 107.2(2) . . . . ? C8 C3 C4 C5 -0.8(3) . . . . ? N3 C3 C4 C5 -179.55(17) . . . . ? C8 C3 C4 C11 178.21(19) . . . . ? N3 C3 C4 C11 -0.5(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C11 C4 C5 C6 -178.5(2) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C4 C5 C6 C10 -179.0(2) . . . . ? C5 C6 C7 C8 -1.8(3) . . . . ? C10 C6 C7 C8 177.9(2) . . . . ? C4 C3 C8 C7 -0.2(3) . . . . ? N3 C3 C8 C7 178.52(18) . . . . ? C4 C3 C8 C9 178.8(2) . . . . ? N3 C3 C8 C9 -2.5(3) . . . . ? C6 C7 C8 C3 1.5(3) . . . . ? C6 C7 C8 C9 -177.5(2) . . . . ? N5 N4 C12 N6 -0.1(2) . . . . ? B1 N4 C12 N6 176.75(15) . . . . ? N5 N4 C12 Ni1 179.01(11) . . . . ? B1 N4 C12 Ni1 -4.2(2) . . . . ? C13 N6 C12 N4 -0.07(19) . . . . ? C14 N6 C12 N4 -176.53(16) . . . . ? C13 N6 C12 Ni1 -178.86(16) . . . . ? C14 N6 C12 Ni1 4.7(3) . . . . ? N10 Ni1 C12 N4 -163.83(13) . . . . ? C23 Ni1 C12 N4 -40.58(15) . . . . ? C1 Ni1 C12 N4 49.23(15) . . . . ? N10 Ni1 C12 N6 14.8(2) . . . . ? C23 Ni1 C12 N6 138.1(2) . . . . ? C1 Ni1 C12 N6 -132.1(2) . . . . ? N4 N5 C13 N6 -0.3(2) . . . . ? C12 N6 C13 N5 0.2(2) . . . . ? C14 N6 C13 N5 176.68(16) . . . . ? C12 N6 C14 C19 -70.1(2) . . . . ? C13 N6 C14 C19 114.1(2) . . . . ? C12 N6 C14 C15 108.9(2) . . . . ? C13 N6 C14 C15 -66.9(2) . . . . ? C19 C14 C15 C16 1.0(3) . . . . ? N6 C14 C15 C16 -177.90(16) . . . . ? C19 C14 C15 C22 -177.84(19) . . . . ? N6 C14 C15 C22 3.2(3) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C22 C15 C16 C17 178.88(19) . . . . ? C15 C16 C17 C18 -0.5(3) . . . . ? C15 C16 C17 C21 179.17(19) . . . . ? C16 C17 C18 C19 0.1(3) . . . . ? C21 C17 C18 C19 -179.6(2) . . . . ? C15 C14 C19 C18 -1.4(3) . . . . ? N6 C14 C19 C18 177.49(16) . . . . ? C15 C14 C19 C20 177.72(19) . . . . ? N6 C14 C19 C20 -3.3(3) . . . . ? C17 C18 C19 C14 0.9(3) . . . . ? C17 C18 C19 C20 -178.30(19) . . . . ? N8 N7 C23 N9 -0.6(2) . . . . ? B1 N7 C23 N9 -176.25(16) . . . . ? N8 N7 C23 Ni1 178.09(13) . . . . ? B1 N7 C23 Ni1 2.4(2) . . . . ? C24 N9 C23 N7 0.3(2) . . . . ? C25 N9 C23 N7 177.61(19) . . . . ? C24 N9 C23 Ni1 -177.97(18) . . . . ? C25 N9 C23 Ni1 -0.7(3) . . . . ? N10 Ni1 C23 N7 171.58(14) . . . . ? C12 Ni1 C23 N7 41.88(16) . . . . ? C1 Ni1 C23 N7 -45.69(16) . . . . ? N10 Ni1 C23 N9 -10.3(2) . . . . ? C12 Ni1 C23 N9 -140.0(2) . . . . ? C1 Ni1 C23 N9 132.4(2) . . . . ? N7 N8 C24 N9 -0.4(2) . . . . ? C23 N9 C24 N8 0.0(3) . . . . ? C25 N9 C24 N8 -177.1(2) . . . . ? C23 N9 C25 C30 101.7(2) . . . . ? C24 N9 C25 C30 -81.6(3) . . . . ? C23 N9 C25 C26 -75.0(3) . . . . ? C24 N9 C25 C26 101.7(3) . . . . ? C30 C25 C26 C27 -0.4(3) . . . . ? N9 C25 C26 C27 176.19(19) . . . . ? C30 C25 C26 C33 -179.4(2) . . . . ? N9 C25 C26 C33 -2.8(3) . . . . ? C25 C26 C27 C28 1.0(4) . . . . ? C33 C26 C27 C28 180.0(2) . . . . ? C26 C27 C28 C29 -0.2(4) . . . . ? C26 C27 C28 C32 -178.8(3) . . . . ? C27 C28 C29 C30 -1.1(4) . . . . ? C32 C28 C29 C30 177.5(3) . . . . ? C26 C25 C30 C29 -0.7(3) . . . . ? N9 C25 C30 C29 -177.4(2) . . . . ? C26 C25 C30 C31 176.9(2) . . . . ? N9 C25 C30 C31 0.3(3) . . . . ? C28 C29 C30 C25 1.5(4) . . . . ? C28 C29 C30 C31 -176.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.562 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.054 # 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 -0.009 0.000 0.000 274 79 ' ' _platon_squeeze_details ; ; _iucr_refine_instructions_details ; TITL jsNMSUsal1072_0m in P-1 CELL 0.71073 8.7177 12.9737 17.9604 74.731 77.159 72.128 ZERR 2.00 0.0017 0.0025 0.0035 0.004 0.004 0.003 LATT 1 SFAC C H N O B NI UNIT 66 74 20 2 2 2 TEMP -100.080 SIZE 0.216 0.299 0.464 ACTA OMIT 0 -1 1 OMIT 1 0 1 OMIT 1 1 0 OMIT 0 1 1 OMIT 1 1 1 OMIT 0 1 0 OMIT 0 1 2 OMIT 0 0 2 OMIT 1 0 2 L.S. 10 FMAP 2 PLAN 10 BOND $H CONF WGHT 0.059800 0.317500 FVAR 1.40806 NI1 6 0.279751 0.376593 0.280818 11.00000 0.01611 0.02510 = 0.02710 -0.00761 -0.00332 -0.00466 B1 5 -0.043909 0.370005 0.393061 11.00000 0.01508 0.02761 = 0.03020 -0.00637 -0.00205 -0.00314 AFIX 13 H1 2 -0.148291 0.367370 0.429492 11.00000 -1.20000 AFIX 0 O1 4 0.544694 0.337670 0.161016 11.00000 0.03763 0.11859 = 0.05945 -0.04777 0.02034 -0.03120 N1 3 0.005739 0.478737 0.382217 11.00000 0.01704 0.02423 = 0.02821 -0.00761 -0.00492 -0.00122 N2 3 -0.075956 0.562561 0.422494 11.00000 0.02018 0.02505 = 0.02917 -0.00824 -0.00407 0.00113 N3 3 0.154842 0.590893 0.350831 11.00000 0.01719 0.02304 = 0.02984 -0.00840 -0.00491 -0.00324 N4 3 0.106437 0.274949 0.420137 11.00000 0.01848 0.02197 = 0.02722 -0.00467 -0.00394 -0.00412 N5 3 0.102610 0.194027 0.488232 11.00000 0.02100 0.02098 = 0.02969 -0.00502 -0.00388 -0.00576 N6 3 0.352732 0.180079 0.423508 11.00000 0.01634 0.02007 = 0.02980 -0.00630 -0.00421 -0.00221 N7 3 -0.048175 0.360505 0.309094 11.00000 0.01760 0.03098 = 0.03331 -0.00722 -0.00828 -0.00650 N8 3 -0.181332 0.355543 0.281721 11.00000 0.02466 0.04130 = 0.04238 -0.00666 -0.01482 -0.01140 N9 3 0.031698 0.361012 0.188015 11.00000 0.02825 0.03932 = 0.03293 -0.00853 -0.01040 -0.01147 N10 3 0.442087 0.363236 0.213165 11.00000 0.02291 0.04251 = 0.03417 -0.01356 -0.00114 -0.01354 C1 1 0.146260 0.493748 0.338220 11.00000 0.01765 0.02458 = 0.02719 -0.00493 -0.00839 -0.00348 C2 1 0.018197 0.628431 0.402048 11.00000 0.02398 0.02503 = 0.03109 -0.00930 -0.00728 0.00053 AFIX 43 H2 2 -0.004207 0.694820 0.420193 11.00000 -1.20000 AFIX 0 C3 1 0.291535 0.639382 0.324256 11.00000 0.02000 0.02522 = 0.03401 -0.01341 -0.00410 -0.00574 C4 1 0.436838 0.580477 0.353748 11.00000 0.02451 0.03004 = 0.03885 -0.01409 -0.00832 -0.00482 C5 1 0.567274 0.628214 0.328252 11.00000 0.02188 0.03953 = 0.05693 -0.02069 -0.01032 -0.00557 AFIX 43 H5 2 0.667795 0.589905 0.346895 11.00000 -1.20000 AFIX 0 C6 1 0.555656 0.728790 0.277073 11.00000 0.02561 0.03959 = 0.06071 -0.02326 0.00034 -0.01319 C7 1 0.407983 0.785329 0.250576 11.00000 0.03674 0.02878 = 0.04972 -0.01068 -0.00227 -0.01237 AFIX 43 H7 2 0.398214 0.855920 0.216367 11.00000 -1.20000 AFIX 0 C8 1 0.274360 0.741139 0.272894 11.00000 0.02697 0.02705 = 0.03988 -0.01173 -0.00575 -0.00639 C9 1 0.116718 0.801803 0.240808 11.00000 0.03693 0.03100 = 0.05670 0.00232 -0.01807 -0.00833 AFIX 137 H9A 2 0.131345 0.868418 0.201965 11.00000 -1.50000 H9B 2 0.030053 0.823019 0.283494 11.00000 -1.50000 H9C 2 0.086654 0.753264 0.216182 11.00000 -1.50000 AFIX 0 C10 1 0.703672 0.775764 0.250278 11.00000 0.03774 0.05717 = 0.10773 -0.01994 0.00229 -0.02749 AFIX 137 H10A 2 0.715272 0.809429 0.290880 11.00000 -1.50000 H10B 2 0.689125 0.832073 0.201983 11.00000 -1.50000 H10C 2 0.801849 0.716013 0.240731 11.00000 -1.50000 AFIX 0 C11 1 0.454100 0.471462 0.411317 11.00000 0.02735 0.03819 = 0.04199 -0.00903 -0.01522 -0.00241 AFIX 137 H11A 2 0.473851 0.411859 0.383514 11.00000 -1.50000 H11B 2 0.353672 0.473472 0.449184 11.00000 -1.50000 H11C 2 0.546030 0.457994 0.438777 11.00000 -1.50000 AFIX 0 C12 1 0.256401 0.268342 0.379782 11.00000 0.01875 0.02211 = 0.02893 -0.00878 -0.00571 -0.00341 C13 1 0.254841 0.138242 0.488228 11.00000 0.02269 0.02027 = 0.02990 -0.00403 -0.00530 -0.00414 AFIX 43 H13 2 0.293250 0.076509 0.527917 11.00000 -1.20000 AFIX 0 C14 1 0.528406 0.141676 0.407057 11.00000 0.01599 0.01849 = 0.03214 -0.00341 -0.00545 -0.00176 C15 1 0.621857 0.157416 0.454877 11.00000 0.02522 0.01738 = 0.03162 -0.00279 -0.00676 -0.00617 C16 1 0.790974 0.122763 0.435804 11.00000 0.02187 0.02364 = 0.03752 -0.00186 -0.00962 -0.00829 AFIX 43 H16 2 0.857321 0.132570 0.467425 11.00000 -1.20000 AFIX 0 C17 1 0.865204 0.074472 0.372153 11.00000 0.01864 0.02577 = 0.03989 -0.00178 -0.00398 -0.00559 C18 1 0.767549 0.059538 0.326487 11.00000 0.02121 0.02598 = 0.03380 -0.00681 -0.00133 -0.00172 AFIX 43 H18 2 0.817758 0.026386 0.282775 11.00000 -1.20000 AFIX 0 C19 1 0.597270 0.092032 0.343186 11.00000 0.02067 0.02188 = 0.03434 -0.00633 -0.00667 -0.00304 C20 1 0.494249 0.072118 0.294175 11.00000 0.02758 0.03731 = 0.04466 -0.01954 -0.01162 -0.00132 AFIX 137 H20A 2 0.420855 0.028693 0.327677 11.00000 -1.50000 H20B 2 0.564984 0.031351 0.254906 11.00000 -1.50000 H20C 2 0.429776 0.143332 0.268007 11.00000 -1.50000 AFIX 0 C21 1 1.049034 0.039609 0.353118 11.00000 0.01909 0.05344 = 0.05439 -0.01250 -0.00218 -0.00867 AFIX 137 H21A 2 1.081014 -0.000198 0.310332 11.00000 -1.50000 H21B 2 1.094389 -0.008994 0.399345 11.00000 -1.50000 H21C 2 1.090937 0.105406 0.337332 11.00000 -1.50000 AFIX 0 C22 1 0.547609 0.207460 0.525489 11.00000 0.03282 0.03366 = 0.03487 -0.00991 -0.00817 -0.00739 AFIX 137 H22A 2 0.524676 0.149475 0.570539 11.00000 -1.50000 H22B 2 0.445823 0.264071 0.515490 11.00000 -1.50000 H22C 2 0.623926 0.241461 0.536471 11.00000 -1.50000 AFIX 0 C23 1 0.081870 0.364545 0.253545 11.00000 0.02612 0.02459 = 0.02940 -0.00795 -0.00728 -0.00537 C24 1 -0.128313 0.355581 0.208357 11.00000 0.02978 0.05020 = 0.04457 -0.01005 -0.01586 -0.01521 AFIX 43 H24 2 -0.191932 0.352269 0.172846 11.00000 -1.20000 AFIX 0 C25 1 0.129855 0.367468 0.111901 11.00000 0.03526 0.04545 = 0.03012 -0.01069 -0.01217 -0.01138 C26 1 0.153577 0.470381 0.070298 11.00000 0.03951 0.04567 = 0.03322 -0.00871 -0.01199 -0.00869 C27 1 0.256437 0.473506 -0.000756 11.00000 0.05483 0.04948 = 0.03157 -0.00217 -0.01053 -0.01279 AFIX 43 H27 2 0.275342 0.542439 -0.029448 11.00000 -1.20000 AFIX 0 C28 1 0.332096 0.380500 -0.031225 11.00000 0.06822 0.06295 = 0.03078 -0.01074 -0.00693 -0.00969 C29 1 0.303738 0.280812 0.011396 11.00000 0.07995 0.05630 = 0.04183 -0.02348 -0.00950 -0.00693 AFIX 43 H29 2 0.354012 0.216315 -0.009623 11.00000 -1.20000 AFIX 0 C30 1 0.204686 0.271058 0.083745 11.00000 0.05917 0.04581 = 0.03722 -0.01428 -0.01214 -0.01415 C31 1 0.184158 0.159823 0.131405 11.00000 0.09167 0.05274 = 0.05806 -0.01984 -0.00928 -0.02220 AFIX 137 H31A 2 0.229176 0.142680 0.179961 11.00000 -1.50000 H31B 2 0.242030 0.102446 0.101337 11.00000 -1.50000 H31C 2 0.067965 0.162261 0.143801 11.00000 -1.50000 AFIX 0 C32 1 0.446491 0.387817 -0.108748 11.00000 0.11145 0.07959 = 0.03890 -0.01359 0.00747 -0.00783 AFIX 137 H32A 2 0.515698 0.313681 -0.113477 11.00000 -1.50000 H32B 2 0.515152 0.436196 -0.110992 11.00000 -1.50000 H32C 2 0.382328 0.418290 -0.151724 11.00000 -1.50000 AFIX 0 C33 1 0.072570 0.573138 0.102286 11.00000 0.05798 0.04241 = 0.04896 -0.01009 -0.00445 -0.01145 AFIX 137 H33A 2 0.126604 0.571940 0.144996 11.00000 -1.50000 H33B 2 -0.042610 0.576084 0.121960 11.00000 -1.50000 H33C 2 0.080807 0.638505 0.060795 11.00000 -1.50000 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM jsNMSUsal1072_0m in P-1 REM R1 = 0.0402 for 6478 Fo > 4sig(Fo) and 0.0545 for all 8112 data REM 424 parameters refined using 0 restraints END WGHT 0.0597 0.3193 REM Highest difference peak 0.562, deepest hole -0.462, 1-sigma level 0.054 Q1 1 0.2371 0.4441 0.3135 11.00000 0.05 0.56 Q2 1 0.3221 0.3199 0.2480 11.00000 0.05 0.46 Q3 1 0.2684 0.3336 0.3482 11.00000 0.05 0.36 Q4 1 0.2708 0.4201 0.2298 11.00000 0.05 0.35 Q5 1 0.5082 0.4083 0.1642 11.00000 0.05 0.34 Q6 1 1.1018 0.0606 0.3831 11.00000 0.05 0.31 Q7 1 -0.0375 0.5154 0.4025 11.00000 0.05 0.28 Q8 1 1.0964 -0.0425 0.3617 11.00000 0.05 0.28 Q9 1 0.5266 0.0049 0.2817 11.00000 0.05 0.28 Q10 1 0.1970 0.3167 0.1114 11.00000 0.05 0.27 ;