Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Karl Wieghardt' _publ_contact_author_address ; Max-Planck-Inst. for Bioinorganic Chemistry Stiftstr. 34-36 Muelheim 45470 GERMANY ; _publ_contact_author_email WIEGHARDT@MPI-MUELHEIM.MPG.DE _publ_section_title ; Neutral Bis(1,4-diaza-1,3-butadiene)nickel Complexes and their Corresponding Monocations: Molecular and Electronic Structures. A Combined Experimental and Density Functional Theoretical Study ; loop_ _publ_author_name 'Karl Wieghardt' 'Nicoleta Muresan' 'Thomas Weyhermuller' data_1 _database_code_depnum_ccdc_archive 'CCDC 650249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N4 Ni' _chemical_formula_weight 615.48 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' 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 11.3674(8) _cell_length_b 11.8340(8) _cell_length_c 13.8385(9) _cell_angle_alpha 65.052(5) _cell_angle_beta 80.316(5) _cell_angle_gamma 77.999(5) _cell_volume 1644.17(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent crystal fragment' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9258 _exptl_absorpt_correction_T_max 0.9599 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '1032 images at 1.0 deg. stepwise rotation in omega and phi, 80 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42057 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9582 _reflns_number_gt 7568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.8819P] 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 9582 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.753139(19) 0.73538(2) 0.738499(16) 0.02228(6) Uani 1 1 d . . . N1 N 0.64469(13) 0.75473(14) 0.85729(11) 0.0276(3) Uani 1 1 d . . . C2 C 0.52793(17) 0.78232(18) 0.83984(15) 0.0324(4) Uani 1 1 d . . . C3 C 0.50652(16) 0.78838(17) 0.74060(15) 0.0314(4) Uani 1 1 d . . . H3 H 0.4271 0.8001 0.7214 0.038 Uiso 1 1 calc R . . N4 N 0.60376(13) 0.77671(13) 0.67500(11) 0.0259(3) Uani 1 1 d . . . C5 C 0.58417(15) 0.77705(16) 0.57493(14) 0.0271(3) Uani 1 1 d . . . C6 C 0.62684(16) 0.87058(17) 0.48010(14) 0.0304(4) Uani 1 1 d . . . C7 C 0.60815(18) 0.8723(2) 0.38214(15) 0.0372(4) Uani 1 1 d . . . H7 H 0.6347 0.9366 0.3174 0.045 Uiso 1 1 calc R . . C8 C 0.55187(18) 0.7820(2) 0.37814(16) 0.0407(5) Uani 1 1 d . . . H8 H 0.5401 0.7839 0.3111 0.049 Uiso 1 1 calc R . . C9 C 0.51263(17) 0.6887(2) 0.47237(17) 0.0381(4) Uani 1 1 d . . . H9 H 0.4756 0.6256 0.4691 0.046 Uiso 1 1 calc R . . C10 C 0.52611(16) 0.68476(17) 0.57231(15) 0.0311(4) Uani 1 1 d . . . C11 C 0.67453(16) 0.75743(18) 0.95313(14) 0.0308(4) Uani 1 1 d . . . C12 C 0.69449(18) 0.64317(19) 1.04214(14) 0.0361(4) Uani 1 1 d . . . C13 C 0.7292(2) 0.6445(2) 1.13391(16) 0.0447(5) Uani 1 1 d . . . H13 H 0.7432 0.5678 1.1950 0.054 Uiso 1 1 calc R . . C14 C 0.7432(2) 0.7561(2) 1.13659(17) 0.0490(5) Uani 1 1 d . . . H14 H 0.7686 0.7556 1.1988 0.059 Uiso 1 1 calc R . . C15 C 0.7203(2) 0.8685(2) 1.04913(18) 0.0456(5) Uani 1 1 d . . . H15 H 0.7293 0.9449 1.0523 0.055 Uiso 1 1 calc R . . C16 C 0.68413(18) 0.87209(19) 0.95579(15) 0.0364(4) Uani 1 1 d . . . C17 C 0.69029(18) 0.96810(18) 0.48326(15) 0.0362(4) Uani 1 1 d . . . H17A H 0.6346 1.0194 0.5166 0.054 Uiso 1 1 calc R . . H17B H 0.7176 1.0224 0.4102 0.054 Uiso 1 1 calc R . . H17C H 0.7601 0.9262 0.5251 0.054 Uiso 1 1 calc R . . C18 C 0.48019(18) 0.58170(19) 0.67201(17) 0.0388(4) Uani 1 1 d . . . H18A H 0.3973 0.6112 0.6943 0.058 Uiso 1 1 calc R . . H18B H 0.5320 0.5595 0.7293 0.058 Uiso 1 1 calc R . . H18C H 0.4814 0.5073 0.6574 0.058 Uiso 1 1 calc R . . C19 C 0.42644(19) 0.8043(2) 0.91785(17) 0.0442(5) Uani 1 1 d . . . H19A H 0.4313 0.7316 0.9869 0.066 Uiso 1 1 calc R . . H19B H 0.3490 0.8153 0.8903 0.066 Uiso 1 1 calc R . . H19C H 0.4328 0.8803 0.9272 0.066 Uiso 1 1 calc R . . C20 C 0.6791(2) 0.52150(19) 1.03911(16) 0.0406(4) Uani 1 1 d . . . H20A H 0.5966 0.5276 1.0233 0.061 Uiso 1 1 calc R . . H20B H 0.6941 0.4521 1.1087 0.061 Uiso 1 1 calc R . . H20C H 0.7367 0.5055 0.9834 0.061 Uiso 1 1 calc R . . C21 C 0.6541(2) 0.99626(19) 0.86366(17) 0.0438(5) Uani 1 1 d . . . H21A H 0.6674 0.9835 0.7969 0.066 Uiso 1 1 calc R . . H21B H 0.7059 1.0550 0.8596 0.066 Uiso 1 1 calc R . . H21C H 0.5693 1.0312 0.8745 0.066 Uiso 1 1 calc R . . N31 N 0.90749(12) 0.78451(12) 0.73537(10) 0.0232(3) Uani 1 1 d . . . C32 C 1.00066(15) 0.72590(16) 0.69217(13) 0.0264(3) Uani 1 1 d . . . C33 C 0.96901(15) 0.64299(16) 0.65652(14) 0.0278(3) Uani 1 1 d . . . H33 H 1.0266 0.6014 0.6193 0.033 Uiso 1 1 calc R . . N34 N 0.85412(12) 0.62523(13) 0.67731(11) 0.0244(3) Uani 1 1 d . . . C35 C 0.82149(15) 0.54854(16) 0.63180(14) 0.0268(3) Uani 1 1 d . . . C36 C 0.83463(16) 0.58397(17) 0.52021(14) 0.0291(4) Uani 1 1 d . . . C37 C 0.79665(17) 0.50774(19) 0.48087(16) 0.0355(4) Uani 1 1 d . . . H37 H 0.8008 0.5323 0.4057 0.043 Uiso 1 1 calc R . . C38 C 0.75358(17) 0.3983(2) 0.54826(18) 0.0397(5) Uani 1 1 d . . . H38 H 0.7306 0.3468 0.5195 0.048 Uiso 1 1 calc R . . C39 C 0.74345(18) 0.36251(19) 0.65754(18) 0.0390(4) Uani 1 1 d . . . H39 H 0.7139 0.2862 0.7036 0.047 Uiso 1 1 calc R . . C40 C 0.77623(16) 0.43752(17) 0.70132(15) 0.0320(4) Uani 1 1 d . . . C41 C 0.94091(15) 0.85890(15) 0.78293(13) 0.0250(3) Uani 1 1 d . . . C42 C 0.98666(16) 0.79762(17) 0.88351(13) 0.0292(4) Uani 1 1 d . . . C43 C 1.02689(19) 0.87009(19) 0.92508(15) 0.0376(4) Uani 1 1 d . . . H43 H 1.0595 0.8301 0.9925 0.045 Uiso 1 1 calc R . . C44 C 1.0201(2) 0.99912(19) 0.86974(15) 0.0399(4) Uani 1 1 d . . . H44 H 1.0481 1.0471 0.8991 0.048 Uiso 1 1 calc R . . C45 C 0.97251(19) 1.05854(18) 0.77159(15) 0.0360(4) Uani 1 1 d . . . H45 H 0.9669 1.1475 0.7346 0.043 Uiso 1 1 calc R . . C46 C 0.93269(17) 0.98946(16) 0.72630(13) 0.0290(3) Uani 1 1 d . . . C47 C 0.88948(18) 0.69679(18) 0.44199(15) 0.0361(4) Uani 1 1 d . . . H47A H 0.9765 0.6720 0.4293 0.054 Uiso 1 1 calc R . . H47B H 0.8755 0.7614 0.4711 0.054 Uiso 1 1 calc R . . H47C H 0.8523 0.7308 0.3744 0.054 Uiso 1 1 calc R . . C48 C 0.7651(2) 0.3988(2) 0.82016(16) 0.0425(5) Uani 1 1 d . . . H48A H 0.8419 0.4006 0.8423 0.064 Uiso 1 1 calc R . . H48B H 0.7449 0.3131 0.8562 0.064 Uiso 1 1 calc R . . H48C H 0.7012 0.4572 0.8396 0.064 Uiso 1 1 calc R . . C49 C 1.12897(16) 0.74792(19) 0.67865(15) 0.0335(4) Uani 1 1 d . . . H49A H 1.1329 0.8381 0.6388 0.050 Uiso 1 1 calc R . . H49B H 1.1796 0.7007 0.6392 0.050 Uiso 1 1 calc R . . H49C H 1.1581 0.7193 0.7492 0.050 Uiso 1 1 calc R . . C50 C 0.99519(18) 0.65715(17) 0.94381(14) 0.0351(4) Uani 1 1 d . . . H50A H 1.0665 0.6153 0.9144 0.053 Uiso 1 1 calc R . . H50B H 0.9225 0.6299 0.9368 0.053 Uiso 1 1 calc R . . H50C H 1.0022 0.6347 1.0196 0.053 Uiso 1 1 calc R . . C51 C 0.88515(19) 1.05420(17) 0.61753(14) 0.0339(4) Uani 1 1 d . . . H51A H 0.9251 1.0091 0.5727 0.051 Uiso 1 1 calc R . . H51B H 0.9016 1.1413 0.5839 0.051 Uiso 1 1 calc R . . H51C H 0.7978 1.0543 0.6253 0.051 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 0.02367(11) 0.02289(11) 0.02124(10) -0.01028(8) -0.00115(7) -0.00314(7) N1 0.0306(7) 0.0295(7) 0.0232(7) -0.0122(6) 0.0008(6) -0.0047(6) C2 0.0310(9) 0.0340(9) 0.0309(9) -0.0145(7) 0.0036(7) -0.0037(7) C3 0.0261(8) 0.0332(9) 0.0348(9) -0.0153(8) -0.0016(7) -0.0018(7) N4 0.0260(7) 0.0257(7) 0.0265(7) -0.0114(6) -0.0033(5) -0.0018(5) C5 0.0232(8) 0.0301(8) 0.0288(8) -0.0132(7) -0.0054(6) -0.0001(6) C6 0.0275(8) 0.0341(9) 0.0298(9) -0.0128(7) -0.0058(7) -0.0023(7) C7 0.0373(10) 0.0439(11) 0.0276(9) -0.0121(8) -0.0062(7) -0.0029(8) C8 0.0374(10) 0.0555(13) 0.0364(10) -0.0252(10) -0.0119(8) 0.0001(9) C9 0.0305(9) 0.0448(11) 0.0500(12) -0.0289(10) -0.0103(8) -0.0024(8) C10 0.0236(8) 0.0347(9) 0.0381(9) -0.0181(8) -0.0046(7) -0.0018(7) C11 0.0320(9) 0.0390(10) 0.0242(8) -0.0171(7) 0.0041(7) -0.0067(7) C12 0.0385(10) 0.0448(11) 0.0250(8) -0.0155(8) 0.0028(7) -0.0077(8) C13 0.0509(12) 0.0582(13) 0.0240(9) -0.0156(9) -0.0003(8) -0.0110(10) C14 0.0526(13) 0.0744(16) 0.0309(10) -0.0311(11) 0.0006(9) -0.0144(12) C15 0.0468(12) 0.0614(14) 0.0449(12) -0.0383(11) 0.0075(9) -0.0142(10) C16 0.0371(10) 0.0432(11) 0.0332(9) -0.0223(8) 0.0072(8) -0.0087(8) C17 0.0387(10) 0.0348(10) 0.0337(9) -0.0102(8) -0.0044(8) -0.0097(8) C18 0.0320(10) 0.0365(10) 0.0503(12) -0.0193(9) -0.0002(8) -0.0089(8) C19 0.0345(10) 0.0607(14) 0.0404(11) -0.0284(10) 0.0063(8) -0.0039(9) C20 0.0495(12) 0.0389(11) 0.0299(9) -0.0096(8) -0.0024(8) -0.0096(9) C21 0.0503(12) 0.0381(11) 0.0456(12) -0.0225(9) 0.0062(10) -0.0080(9) N31 0.0279(7) 0.0228(6) 0.0204(6) -0.0096(5) -0.0032(5) -0.0043(5) C32 0.0269(8) 0.0289(8) 0.0248(8) -0.0118(7) -0.0017(6) -0.0056(6) C33 0.0260(8) 0.0310(9) 0.0294(8) -0.0168(7) -0.0021(7) -0.0008(7) N34 0.0268(7) 0.0239(7) 0.0255(7) -0.0129(5) -0.0031(5) -0.0030(5) C35 0.0234(8) 0.0266(8) 0.0342(9) -0.0174(7) -0.0032(7) -0.0002(6) C36 0.0258(8) 0.0336(9) 0.0321(9) -0.0199(7) -0.0056(7) 0.0041(7) C37 0.0297(9) 0.0455(11) 0.0411(10) -0.0301(9) -0.0067(8) 0.0040(8) C38 0.0305(9) 0.0489(12) 0.0569(12) -0.0394(10) -0.0049(9) -0.0016(8) C39 0.0328(10) 0.0341(10) 0.0565(12) -0.0248(9) 0.0009(9) -0.0078(8) C40 0.0299(9) 0.0311(9) 0.0378(10) -0.0175(8) -0.0004(7) -0.0046(7) C41 0.0283(8) 0.0263(8) 0.0231(7) -0.0120(6) -0.0020(6) -0.0059(6) C42 0.0343(9) 0.0315(9) 0.0239(8) -0.0119(7) -0.0037(7) -0.0066(7) C43 0.0491(12) 0.0430(11) 0.0261(9) -0.0156(8) -0.0096(8) -0.0092(9) C44 0.0555(13) 0.0420(11) 0.0333(10) -0.0211(9) -0.0054(9) -0.0168(9) C45 0.0512(12) 0.0290(9) 0.0325(9) -0.0142(8) -0.0032(8) -0.0125(8) C46 0.0374(9) 0.0277(8) 0.0235(8) -0.0110(7) -0.0027(7) -0.0070(7) C47 0.0380(10) 0.0392(10) 0.0289(9) -0.0136(8) -0.0037(8) -0.0009(8) C48 0.0515(12) 0.0379(11) 0.0374(10) -0.0124(9) 0.0031(9) -0.0166(9) C49 0.0273(9) 0.0437(10) 0.0351(9) -0.0208(8) -0.0004(7) -0.0083(7) C50 0.0417(10) 0.0335(9) 0.0259(8) -0.0062(7) -0.0069(7) -0.0064(8) C51 0.0481(11) 0.0268(9) 0.0270(8) -0.0093(7) -0.0063(8) -0.0072(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.9206(14) . ? Ni1 N34 1.9276(14) . ? Ni1 N1 1.9475(14) . ? Ni1 N31 1.9483(14) . ? N1 C2 1.337(2) . ? N1 C11 1.438(2) . ? C2 C3 1.405(3) . ? C2 C19 1.502(3) . ? C3 N4 1.330(2) . ? N4 C5 1.437(2) . ? C5 C6 1.402(2) . ? C5 C10 1.404(2) . ? C6 C7 1.398(2) . ? C6 C17 1.501(3) . ? C7 C8 1.378(3) . ? C8 C9 1.384(3) . ? C9 C10 1.397(3) . ? C10 C18 1.505(3) . ? C11 C12 1.399(3) . ? C11 C16 1.400(3) . ? C12 C13 1.399(3) . ? C12 C20 1.504(3) . ? C13 C14 1.378(3) . ? C14 C15 1.381(3) . ? C15 C16 1.402(3) . ? C16 C21 1.503(3) . ? N31 C32 1.338(2) . ? N31 C41 1.437(2) . ? C32 C33 1.397(2) . ? C32 C49 1.502(2) . ? C33 N34 1.330(2) . ? N34 C35 1.435(2) . ? C35 C40 1.402(2) . ? C35 C36 1.409(2) . ? C36 C37 1.397(2) . ? C36 C47 1.498(3) . ? C37 C38 1.371(3) . ? C38 C39 1.379(3) . ? C39 C40 1.400(3) . ? C40 C48 1.500(3) . ? C41 C46 1.398(2) . ? C41 C42 1.403(2) . ? C42 C43 1.394(2) . ? C42 C50 1.503(2) . ? C43 C44 1.381(3) . ? C44 C45 1.384(3) . ? C45 C46 1.396(2) . ? C46 C51 1.508(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N34 103.83(6) . . ? N4 Ni1 N1 81.99(6) . . ? N34 Ni1 N1 148.75(6) . . ? N4 Ni1 N31 147.48(6) . . ? N34 Ni1 N31 82.14(6) . . ? N1 Ni1 N31 109.61(6) . . ? C2 N1 C11 117.12(15) . . ? C2 N1 Ni1 113.86(12) . . ? C11 N1 Ni1 128.59(12) . . ? N1 C2 C3 113.93(16) . . ? N1 C2 C19 124.35(17) . . ? C3 C2 C19 121.71(17) . . ? N4 C3 C2 116.23(16) . . ? C3 N4 C5 117.18(14) . . ? C3 N4 Ni1 113.67(12) . . ? C5 N4 Ni1 128.39(11) . . ? C6 C5 C10 120.98(16) . . ? C6 C5 N4 118.13(15) . . ? C10 C5 N4 120.88(15) . . ? C7 C6 C5 118.77(17) . . ? C7 C6 C17 120.42(17) . . ? C5 C6 C17 120.82(16) . . ? C8 C7 C6 120.98(18) . . ? C7 C8 C9 119.59(18) . . ? C8 C9 C10 121.67(18) . . ? C9 C10 C5 117.97(17) . . ? C9 C10 C18 119.20(17) . . ? C5 C10 C18 122.83(17) . . ? C12 C11 C16 121.49(17) . . ? C12 C11 N1 118.33(16) . . ? C16 C11 N1 120.18(17) . . ? C13 C12 C11 118.56(19) . . ? C13 C12 C20 120.74(18) . . ? C11 C12 C20 120.70(17) . . ? C14 C13 C12 120.7(2) . . ? C13 C14 C15 120.16(19) . . ? C14 C15 C16 121.2(2) . . ? C11 C16 C15 117.81(19) . . ? C11 C16 C21 121.98(18) . . ? C15 C16 C21 120.19(19) . . ? C32 N31 C41 114.52(14) . . ? C32 N31 Ni1 113.45(11) . . ? C41 N31 Ni1 131.47(11) . . ? N31 C32 C33 114.33(15) . . ? N31 C32 C49 124.27(15) . . ? C33 C32 C49 121.37(15) . . ? N34 C33 C32 116.61(15) . . ? C33 N34 C35 115.54(14) . . ? C33 N34 Ni1 113.11(11) . . ? C35 N34 Ni1 129.96(11) . . ? C40 C35 C36 120.94(16) . . ? C40 C35 N34 118.22(15) . . ? C36 C35 N34 120.84(15) . . ? C37 C36 C35 117.94(17) . . ? C37 C36 C47 118.37(16) . . ? C35 C36 C47 123.68(16) . . ? C38 C37 C36 121.49(18) . . ? C37 C38 C39 120.29(17) . . ? C38 C39 C40 120.68(19) . . ? C39 C40 C35 118.59(17) . . ? C39 C40 C48 120.69(17) . . ? C35 C40 C48 120.71(16) . . ? C46 C41 C42 121.42(15) . . ? C46 C41 N31 119.58(14) . . ? C42 C41 N31 118.93(14) . . ? C43 C42 C41 118.23(16) . . ? C43 C42 C50 120.70(16) . . ? C41 C42 C50 121.05(15) . . ? C44 C43 C42 121.00(17) . . ? C43 C44 C45 120.08(17) . . ? C44 C45 C46 120.84(17) . . ? C45 C46 C41 118.40(16) . . ? C45 C46 C51 120.56(16) . . ? C41 C46 C51 121.02(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.437 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.058 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 650250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C54 H76 N4 Ni], (C6 H14)' _chemical_formula_sum 'C60 H90 N4 Ni' _chemical_formula_weight 926.07 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' 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 13.1901(6) _cell_length_b 13.8920(6) _cell_length_c 14.9786(6) _cell_angle_alpha 93.853(3) _cell_angle_beta 93.563(3) _cell_angle_gamma 94.205(3) _cell_volume 2724.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 0.396 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.8902 _exptl_absorpt_correction_T_max 0.9821 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '720 images at 1.0 deg. stepwise rotation in omega and phi, 85 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35076 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9590 _reflns_number_gt 7841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+3.9433P] 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 9590 _refine_ls_number_parameters 626 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.17767(3) 0.23732(3) 0.23321(2) 0.01762(11) Uani 1 1 d . . . C5 C 0.3911(2) 0.2147(2) 0.3406(2) 0.0280(7) Uani 1 1 d . . . C6 C 0.3954(2) 0.1240(2) 0.3755(2) 0.0297(7) Uani 1 1 d . A . C7 C 0.4908(2) 0.0905(3) 0.3966(2) 0.0368(8) Uani 1 1 d . . . H7 H 0.4947 0.0296 0.4214 0.044 Uiso 1 1 calc R A . C8 C 0.5794(2) 0.1444(3) 0.3821(2) 0.0406(9) Uani 1 1 d . A . H8 H 0.6436 0.1208 0.3972 0.049 Uiso 1 1 calc R . . C9 C 0.5750(2) 0.2323(3) 0.3459(2) 0.0399(9) Uani 1 1 d . . . H9 H 0.6366 0.2682 0.3350 0.048 Uiso 1 1 calc R A . C10 C 0.4819(2) 0.2698(2) 0.3248(2) 0.0339(8) Uani 1 1 d . A . C11 C 0.0299(2) 0.3851(2) 0.30920(18) 0.0208(6) Uani 1 1 d . . . C12 C -0.0461(2) 0.3495(2) 0.36342(19) 0.0219(6) Uani 1 1 d . A . C13 C -0.1325(2) 0.4006(2) 0.3707(2) 0.0292(7) Uani 1 1 d . . . H13 H -0.1845 0.3777 0.4070 0.035 Uiso 1 1 calc R A . C14 C -0.1448(2) 0.4834(2) 0.3268(2) 0.0333(8) Uani 1 1 d . A . H14 H -0.2037 0.5179 0.3341 0.040 Uiso 1 1 calc R . . C15 C -0.0712(3) 0.5159(2) 0.2725(2) 0.0328(8) Uani 1 1 d . . . H15 H -0.0808 0.5720 0.2410 0.039 Uiso 1 1 calc R A . C16 C 0.0172(2) 0.4681(2) 0.2626(2) 0.0262(7) Uani 1 1 d . A . C17 C 0.2991(2) 0.0640(2) 0.3964(2) 0.0335(8) Uani 1 1 d . . . H17 H 0.2410 0.0845 0.3579 0.040 Uiso 1 1 calc R A . C18 C 0.3052(3) -0.0440(3) 0.3760(3) 0.0436(9) Uani 1 1 d . A . H18A H 0.3209 -0.0564 0.3134 0.065 Uiso 1 1 calc R . . H18B H 0.2398 -0.0783 0.3860 0.065 Uiso 1 1 calc R . . H18C H 0.3590 -0.0668 0.4155 0.065 Uiso 1 1 calc R . . C19 C 0.2765(3) 0.0854(3) 0.4939(3) 0.0547(11) Uani 1 1 d . A . H19A H 0.3330 0.0672 0.5333 0.082 Uiso 1 1 calc R . . H19B H 0.2136 0.0480 0.5063 0.082 Uiso 1 1 calc R . . H19C H 0.2682 0.1546 0.5049 0.082 Uiso 1 1 calc R . . C20 C 0.4831(3) 0.3697(3) 0.2888(3) 0.0495(10) Uani 1 1 d . . . H20 H 0.4126 0.3802 0.2649 0.059 Uiso 1 1 calc R A . C21 C 0.5556(3) 0.3807(3) 0.2128(3) 0.0536(11) Uani 1 1 d . A . H21A H 0.6264 0.3834 0.2378 0.080 Uiso 1 1 calc R . . H21B H 0.5441 0.4405 0.1838 0.080 Uiso 1 1 calc R . . H21C H 0.5426 0.3252 0.1686 0.080 Uiso 1 1 calc R . . C22 C 0.5168(4) 0.4497(3) 0.3639(4) 0.0827(17) Uani 1 1 d . A . H22A H 0.4707 0.4453 0.4126 0.124 Uiso 1 1 calc R . . H22B H 0.5147 0.5133 0.3396 0.124 Uiso 1 1 calc R . . H22C H 0.5865 0.4411 0.3871 0.124 Uiso 1 1 calc R . . N1 N 0.12550(16) 0.34072(16) 0.30919(15) 0.0179(9) Uani 0.721(5) 1 d PD A 1 N4 N 0.29288(17) 0.25394(17) 0.32751(15) 0.0270(10) Uani 0.721(5) 1 d PD A 1 C2 C 0.1902(2) 0.3729(2) 0.37794(19) 0.0270(12) Uani 0.721(5) 1 d PD A 1 C3 C 0.2808(2) 0.3265(2) 0.38712(19) 0.0332(14) Uani 0.721(5) 1 d PD A 1 H3 H 0.3313 0.3462 0.4340 0.040 Uiso 0.721(5) 1 calc PR A 1 C23 C 0.1814(3) 0.4607(3) 0.4414(3) 0.0297(10) Uani 0.721(5) 1 d PD A 1 H23A H 0.1155 0.4870 0.4290 0.045 Uiso 0.721(5) 1 calc PR A 1 H23B H 0.2364 0.5099 0.4329 0.045 Uiso 0.721(5) 1 calc PR A 1 H23C H 0.1867 0.4421 0.5034 0.045 Uiso 0.721(5) 1 calc PR A 1 N1X N 0.29288(17) 0.25394(17) 0.32751(15) 0.0179(9) Uani 0.279(5) 1 d PD A 2 N4X N 0.12550(16) 0.34072(16) 0.30919(15) 0.0270(10) Uani 0.279(5) 1 d PD A 2 C2X C 0.2808(2) 0.3265(2) 0.38712(19) 0.0270(12) Uani 0.279(5) 1 d PD A 2 C3X C 0.1902(2) 0.3729(2) 0.37794(19) 0.0332(14) Uani 0.279(5) 1 d PD A 2 H3X H 0.1759 0.4246 0.4188 0.040 Uiso 0.279(5) 1 calc PR A 2 C23X C 0.3354(7) 0.3470(8) 0.4793(5) 0.0297(10) Uani 0.279(5) 1 d PD A 2 H23D H 0.3979 0.3129 0.4821 0.045 Uiso 0.279(5) 1 calc PR A 2 H23E H 0.2909 0.3246 0.5249 0.045 Uiso 0.279(5) 1 calc PR A 2 H23F H 0.3528 0.4168 0.4904 0.045 Uiso 0.279(5) 1 calc PR A 2 C24 C -0.0351(2) 0.2594(2) 0.4151(2) 0.0270(7) Uani 1 1 d . . . H24 H 0.0111 0.2176 0.3824 0.032 Uiso 1 1 calc R A . C25 C -0.1369(2) 0.2007(2) 0.4193(2) 0.0280(7) Uani 1 1 d . A . H25A H -0.1796 0.2354 0.4598 0.042 Uiso 1 1 calc R . . H25B H -0.1250 0.1375 0.4416 0.042 Uiso 1 1 calc R . . H25C H -0.1715 0.1915 0.3592 0.042 Uiso 1 1 calc R . . C26 C 0.0122(3) 0.2831(3) 0.5104(3) 0.0626(13) Uani 1 1 d . A . H26A H 0.0827 0.3101 0.5081 0.094 Uiso 1 1 calc R . . H26B H 0.0114 0.2240 0.5425 0.094 Uiso 1 1 calc R . . H26C H -0.0270 0.3306 0.5416 0.094 Uiso 1 1 calc R . . C27 C 0.0977(3) 0.5088(2) 0.2039(2) 0.0336(8) Uani 1 1 d . . . H27 H 0.1583 0.4699 0.2096 0.040 Uiso 1 1 calc R A . C28 C 0.0577(3) 0.5008(3) 0.1058(2) 0.0469(10) Uani 1 1 d . A . H28A H 0.0397 0.4327 0.0861 0.070 Uiso 1 1 calc R . . H28B H 0.1104 0.5274 0.0691 0.070 Uiso 1 1 calc R . . H28C H -0.0029 0.5373 0.0992 0.070 Uiso 1 1 calc R . . C29 C 0.1319(3) 0.6148(3) 0.2329(3) 0.0526(11) Uani 1 1 d . A . H29A H 0.0754 0.6552 0.2212 0.079 Uiso 1 1 calc R . . H29B H 0.1896 0.6360 0.1989 0.079 Uiso 1 1 calc R . . H29C H 0.1528 0.6208 0.2971 0.079 Uiso 1 1 calc R . . N31 N 0.23418(17) 0.21000(17) 0.11649(15) 0.0202(5) Uani 1 1 d . A . C32 C 0.1685(2) 0.1583(2) 0.05672(19) 0.0228(6) Uani 1 1 d . . . C33 C 0.0746(2) 0.1306(2) 0.08924(19) 0.0226(6) Uani 1 1 d . A . H33 H 0.0225 0.0947 0.0515 0.027 Uiso 1 1 calc R . . N34 N 0.06001(16) 0.15568(16) 0.17418(15) 0.0169(5) Uani 1 1 d . A . C35 C -0.0425(2) 0.1250(2) 0.19586(18) 0.0179(6) Uani 1 1 d . . . C36 C -0.1270(2) 0.1679(2) 0.15703(18) 0.0197(6) Uani 1 1 d . A . C37 C -0.2247(2) 0.1277(2) 0.17065(19) 0.0230(7) Uani 1 1 d . . . H37 H -0.2823 0.1559 0.1452 0.028 Uiso 1 1 calc R A . C38 C -0.2394(2) 0.0483(2) 0.2201(2) 0.0243(7) Uani 1 1 d . A . H38 H -0.3064 0.0215 0.2279 0.029 Uiso 1 1 calc R . . C39 C -0.1560(2) 0.0078(2) 0.25831(19) 0.0228(6) Uani 1 1 d . . . H39 H -0.1664 -0.0466 0.2927 0.027 Uiso 1 1 calc R A . C40 C -0.0569(2) 0.0451(2) 0.24739(18) 0.0192(6) Uani 1 1 d . A . C41 C 0.3338(2) 0.2278(2) 0.0834(2) 0.0278(7) Uani 1 1 d . . . C42 C 0.4022(2) 0.1549(3) 0.0876(2) 0.0331(8) Uani 1 1 d . A . C43 C 0.4909(3) 0.1671(3) 0.0413(3) 0.0525(11) Uani 1 1 d . . . H43 H 0.5383 0.1188 0.0427 0.063 Uiso 1 1 calc R A . C44 C 0.5113(3) 0.2465(4) -0.0059(3) 0.0652(14) Uani 1 1 d . A . H44 H 0.5708 0.2515 -0.0385 0.078 Uiso 1 1 calc R . . C45 C 0.4457(3) 0.3191(3) -0.0060(3) 0.0561(12) Uani 1 1 d . . . H45 H 0.4613 0.3749 -0.0374 0.067 Uiso 1 1 calc R A . C46 C 0.3561(3) 0.3118(3) 0.0396(2) 0.0384(8) Uani 1 1 d . A . C47 C -0.1152(2) 0.2545(2) 0.1006(2) 0.0265(7) Uani 1 1 d . . . H47 H -0.0438 0.2844 0.1119 0.032 Uiso 1 1 calc R A . C48 C -0.1877(2) 0.3308(2) 0.1257(2) 0.0335(8) Uani 1 1 d . A . H48A H -0.2576 0.3069 0.1054 0.050 Uiso 1 1 calc R . . H48B H -0.1691 0.3903 0.0970 0.050 Uiso 1 1 calc R . . H48C H -0.1830 0.3442 0.1910 0.050 Uiso 1 1 calc R . . C49 C -0.1340(3) 0.2261(3) -0.0011(2) 0.0453(9) Uani 1 1 d . A . H49A H -0.0872 0.1778 -0.0190 0.068 Uiso 1 1 calc R . . H49B H -0.1223 0.2836 -0.0346 0.068 Uiso 1 1 calc R . . H49C H -0.2044 0.1988 -0.0139 0.068 Uiso 1 1 calc R . . C50 C 0.0334(2) -0.0046(2) 0.28671(19) 0.0222(6) Uani 1 1 d . . . H50 H 0.0959 0.0403 0.2846 0.027 Uiso 1 1 calc R A . C51 C 0.0210(3) -0.0242(3) 0.3843(2) 0.0474(10) Uani 1 1 d . A . H51A H -0.0401 -0.0678 0.3884 0.071 Uiso 1 1 calc R . . H51B H 0.0143 0.0370 0.4192 0.071 Uiso 1 1 calc R . . H51C H 0.0810 -0.0542 0.4081 0.071 Uiso 1 1 calc R . . C52 C 0.0484(3) -0.0965(3) 0.2305(3) 0.0560(12) Uani 1 1 d . A . H52A H -0.0134 -0.1405 0.2289 0.084 Uiso 1 1 calc R . . H52B H 0.1062 -0.1277 0.2570 0.084 Uiso 1 1 calc R . . H52C H 0.0620 -0.0807 0.1694 0.084 Uiso 1 1 calc R . . C53 C 0.1870(2) 0.1299(3) -0.0396(2) 0.0396(9) Uani 1 1 d . A . H53A H 0.1809 0.1860 -0.0754 0.059 Uiso 1 1 calc R . . H53B H 0.1365 0.0777 -0.0632 0.059 Uiso 1 1 calc R . . H53C H 0.2555 0.1076 -0.0428 0.059 Uiso 1 1 calc R . . C54 C 0.3813(2) 0.0659(2) 0.1386(2) 0.0339(8) Uani 1 1 d . . . H54 H 0.3442 0.0863 0.1920 0.041 Uiso 1 1 calc R A . C55 C 0.3142(3) -0.0170(3) 0.0856(3) 0.0456(10) Uani 1 1 d . A . H55A H 0.2443 0.0018 0.0774 0.068 Uiso 1 1 calc R . . H55B H 0.3147 -0.0754 0.1189 0.068 Uiso 1 1 calc R . . H55C H 0.3411 -0.0302 0.0268 0.068 Uiso 1 1 calc R . . C56 C 0.4802(3) 0.0243(3) 0.1739(3) 0.0540(11) Uani 1 1 d . A . H56A H 0.5128 -0.0067 0.1236 0.081 Uiso 1 1 calc R . . H56B H 0.4640 -0.0236 0.2170 0.081 Uiso 1 1 calc R . . H56C H 0.5267 0.0768 0.2034 0.081 Uiso 1 1 calc R . . C57 C 0.2845(3) 0.3927(3) 0.0368(2) 0.0434(9) Uani 1 1 d . . . H57 H 0.2263 0.3749 0.0737 0.052 Uiso 1 1 calc R A . C58 C 0.3370(4) 0.4879(3) 0.0783(4) 0.0739(15) Uani 1 1 d . A . H58A H 0.3965 0.5057 0.0452 0.111 Uiso 1 1 calc R . . H58B H 0.3588 0.4807 0.1411 0.111 Uiso 1 1 calc R . . H58C H 0.2893 0.5387 0.0753 0.111 Uiso 1 1 calc R . . C59 C 0.2403(5) 0.4034(4) -0.0590(3) 0.0809(16) Uani 1 1 d . A . H59A H 0.2954 0.4229 -0.0965 0.121 Uiso 1 1 calc R . . H59B H 0.1908 0.4527 -0.0578 0.121 Uiso 1 1 calc R . . H59C H 0.2064 0.3413 -0.0838 0.121 Uiso 1 1 calc R . . C61 C -0.6378(15) -0.308(2) 0.4039(13) 0.081(3) Uani 0.676(4) 1 d PD B 1 H61A H -0.6451 -0.3136 0.4682 0.121 Uiso 0.676(4) 1 calc PR B 1 H61B H -0.6538 -0.3722 0.3720 0.121 Uiso 0.676(4) 1 calc PR B 1 H61C H -0.6847 -0.2629 0.3812 0.121 Uiso 0.676(4) 1 calc PR B 1 C62 C -0.5335(5) -0.2739(5) 0.3897(5) 0.0658(18) Uani 0.676(4) 1 d PD B 1 H62A H -0.4869 -0.3191 0.4157 0.079 Uiso 0.676(4) 1 calc PR B 1 H62B H -0.5182 -0.2101 0.4232 0.079 Uiso 0.676(4) 1 calc PR B 1 C63 C -0.5101(6) -0.2638(7) 0.2911(5) 0.073(3) Uani 0.676(4) 1 d PD B 1 H63A H -0.5261 -0.3271 0.2570 0.087 Uiso 0.676(4) 1 calc PR B 1 H63B H -0.5548 -0.2171 0.2652 0.087 Uiso 0.676(4) 1 calc PR B 1 C64 C -0.4019(5) -0.2304(5) 0.2806(4) 0.0630(17) Uani 0.676(4) 1 d PD B 1 H64A H -0.3864 -0.1689 0.3180 0.076 Uiso 0.676(4) 1 calc PR B 1 H64B H -0.3961 -0.2154 0.2174 0.076 Uiso 0.676(4) 1 calc PR B 1 C65 C -0.3199(5) -0.2974(4) 0.3041(4) 0.0527(15) Uani 0.676(4) 1 d PD B 1 H65A H -0.3269 -0.3153 0.3664 0.063 Uiso 0.676(4) 1 calc PR B 1 H65B H -0.3321 -0.3575 0.2643 0.063 Uiso 0.676(4) 1 calc PR B 1 C66 C -0.2126(5) -0.2569(5) 0.2965(5) 0.0531(16) Uani 0.676(4) 1 d PD B 1 H66A H -0.1653 -0.3048 0.3134 0.080 Uiso 0.676(4) 1 calc PR B 1 H66B H -0.1987 -0.1980 0.3365 0.080 Uiso 0.676(4) 1 calc PR B 1 H66C H -0.2035 -0.2413 0.2345 0.080 Uiso 0.676(4) 1 calc PR B 1 C61X C -0.653(3) -0.326(5) 0.413(2) 0.081(3) Uani 0.324(4) 1 d PD B 2 H61D H -0.7245 -0.3523 0.4044 0.121 Uiso 0.324(4) 1 calc PR B 2 H61E H -0.6490 -0.2664 0.4528 0.121 Uiso 0.324(4) 1 calc PR B 2 H61F H -0.6119 -0.3733 0.4401 0.121 Uiso 0.324(4) 1 calc PR B 2 C62X C -0.6157(8) -0.3037(10) 0.3265(9) 0.0658(18) Uani 0.324(4) 1 d PD B 2 H62C H -0.6606 -0.2586 0.2985 0.079 Uiso 0.324(4) 1 calc PR B 2 H62D H -0.6207 -0.3642 0.2871 0.079 Uiso 0.324(4) 1 calc PR B 2 C63X C -0.5053(11) -0.2589(19) 0.3312(10) 0.073(3) Uani 0.324(4) 1 d PD B 2 H63C H -0.5037 -0.1907 0.3555 0.087 Uiso 0.324(4) 1 calc PR B 2 H63D H -0.4633 -0.2938 0.3733 0.087 Uiso 0.324(4) 1 calc PR B 2 C64X C -0.4593(8) -0.2617(11) 0.2431(7) 0.0630(17) Uani 0.324(4) 1 d PD B 2 H64C H -0.5043 -0.2299 0.2006 0.076 Uiso 0.324(4) 1 calc PR B 2 H64D H -0.4594 -0.3303 0.2205 0.076 Uiso 0.324(4) 1 calc PR B 2 C65X C -0.3516(8) -0.2151(7) 0.2403(9) 0.0527(15) Uani 0.324(4) 1 d PD B 2 H65C H -0.3397 -0.2036 0.1771 0.063 Uiso 0.324(4) 1 calc PR B 2 H65D H -0.3477 -0.1511 0.2742 0.063 Uiso 0.324(4) 1 calc PR B 2 C66X C -0.2671(9) -0.2700(10) 0.2765(12) 0.0531(16) Uani 0.324(4) 1 d PD B 2 H66D H -0.2017 -0.2337 0.2703 0.080 Uiso 0.324(4) 1 calc PR B 2 H66E H -0.2687 -0.3332 0.2429 0.080 Uiso 0.324(4) 1 calc PR B 2 H66F H -0.2755 -0.2793 0.3400 0.080 Uiso 0.324(4) 1 calc PR B 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 0.01084(18) 0.0240(2) 0.0172(2) -0.00330(14) 0.00192(13) -0.00056(14) C5 0.0151(15) 0.041(2) 0.0254(17) -0.0118(14) -0.0014(12) 0.0017(13) C6 0.0173(15) 0.042(2) 0.0271(17) -0.0099(15) -0.0051(13) 0.0028(14) C7 0.0204(17) 0.047(2) 0.042(2) -0.0070(16) -0.0041(15) 0.0068(15) C8 0.0143(16) 0.058(2) 0.046(2) -0.0156(19) -0.0057(15) 0.0065(15) C9 0.0125(16) 0.053(2) 0.050(2) -0.0211(19) 0.0017(15) -0.0043(15) C10 0.0238(17) 0.041(2) 0.0346(19) -0.0111(15) 0.0036(14) 0.0009(14) C11 0.0219(15) 0.0211(15) 0.0178(15) -0.0063(12) 0.0004(12) -0.0014(12) C12 0.0191(15) 0.0250(16) 0.0206(16) -0.0017(12) -0.0007(12) 0.0000(12) C13 0.0211(16) 0.0396(19) 0.0261(17) -0.0013(15) 0.0037(13) -0.0009(14) C14 0.0282(18) 0.0323(19) 0.040(2) -0.0030(15) 0.0025(15) 0.0106(14) C15 0.039(2) 0.0229(17) 0.0362(19) 0.0024(14) -0.0026(15) 0.0053(14) C16 0.0302(17) 0.0237(16) 0.0241(16) -0.0003(13) 0.0012(13) -0.0001(13) C17 0.0163(15) 0.040(2) 0.043(2) 0.0002(16) -0.0052(14) 0.0070(14) C18 0.0251(18) 0.046(2) 0.056(2) -0.0134(18) -0.0011(17) 0.0017(16) C19 0.048(2) 0.054(3) 0.061(3) -0.015(2) 0.025(2) -0.0065(19) C20 0.0250(19) 0.053(2) 0.071(3) 0.000(2) 0.0182(18) -0.0004(17) C21 0.029(2) 0.068(3) 0.062(3) 0.000(2) 0.0107(18) -0.0085(18) C22 0.089(4) 0.047(3) 0.113(4) -0.018(3) 0.058(3) -0.008(2) N1 0.021(2) 0.015(2) 0.018(2) -0.0019(17) 0.0055(17) 0.0019(16) N4 0.011(2) 0.043(3) 0.025(2) -0.005(2) -0.0034(17) -0.0008(19) C2 0.033(3) 0.023(3) 0.024(3) -0.009(2) 0.008(2) 0.004(2) C3 0.027(3) 0.043(4) 0.026(3) -0.005(3) -0.015(2) 0.003(3) C23 0.023(2) 0.035(2) 0.030(2) -0.0075(19) 0.0002(17) 0.0068(18) N1X 0.021(2) 0.015(2) 0.018(2) -0.0019(17) 0.0055(17) 0.0019(16) N4X 0.011(2) 0.043(3) 0.025(2) -0.005(2) -0.0034(17) -0.0008(19) C2X 0.033(3) 0.023(3) 0.024(3) -0.009(2) 0.008(2) 0.004(2) C3X 0.027(3) 0.043(4) 0.026(3) -0.005(3) -0.015(2) 0.003(3) C23X 0.023(2) 0.035(2) 0.030(2) -0.0075(19) 0.0002(17) 0.0068(18) C24 0.0219(16) 0.0344(18) 0.0248(17) 0.0078(14) -0.0001(13) -0.0013(13) C25 0.0232(16) 0.0305(17) 0.0301(18) 0.0005(14) 0.0071(13) -0.0012(13) C26 0.068(3) 0.071(3) 0.042(2) 0.027(2) -0.024(2) -0.035(2) C27 0.0312(18) 0.0351(19) 0.0351(19) 0.0119(15) 0.0049(15) -0.0039(14) C28 0.053(2) 0.053(2) 0.032(2) 0.0036(18) 0.0062(17) -0.0202(19) C29 0.059(3) 0.052(2) 0.042(2) 0.0060(19) -0.0044(19) -0.025(2) N31 0.0126(12) 0.0271(13) 0.0210(13) -0.0014(10) 0.0048(10) 0.0014(10) C32 0.0190(15) 0.0316(17) 0.0179(15) -0.0002(13) 0.0021(12) 0.0041(13) C33 0.0160(15) 0.0313(17) 0.0189(16) -0.0049(13) -0.0008(12) -0.0002(12) N34 0.0118(11) 0.0204(12) 0.0183(12) -0.0007(10) 0.0011(9) 0.0017(9) C35 0.0136(14) 0.0220(15) 0.0171(14) -0.0045(12) 0.0019(11) -0.0010(11) C36 0.0170(14) 0.0225(15) 0.0192(15) -0.0021(12) 0.0013(11) 0.0023(12) C37 0.0147(14) 0.0281(17) 0.0253(16) -0.0021(13) -0.0032(12) 0.0041(12) C38 0.0122(14) 0.0326(17) 0.0270(17) -0.0013(14) 0.0029(12) -0.0031(12) C39 0.0214(15) 0.0236(16) 0.0232(16) 0.0022(13) 0.0021(12) -0.0010(12) C40 0.0182(14) 0.0232(15) 0.0155(14) -0.0025(12) 0.0002(11) 0.0017(12) C41 0.0148(15) 0.0426(19) 0.0236(17) -0.0101(14) 0.0047(12) -0.0052(13) C42 0.0140(15) 0.053(2) 0.0288(18) -0.0183(16) -0.0005(13) 0.0005(14) C43 0.0175(18) 0.085(3) 0.051(2) -0.030(2) 0.0088(17) 0.0015(19) C44 0.024(2) 0.108(4) 0.061(3) -0.020(3) 0.028(2) -0.014(2) C45 0.039(2) 0.080(3) 0.048(2) 0.000(2) 0.0247(19) -0.022(2) C46 0.0279(18) 0.050(2) 0.036(2) -0.0019(17) 0.0089(15) -0.0112(16) C47 0.0191(15) 0.0278(17) 0.0330(18) 0.0061(14) 0.0003(13) 0.0013(13) C48 0.0287(18) 0.0310(18) 0.040(2) 0.0021(15) -0.0051(15) 0.0052(14) C49 0.062(3) 0.043(2) 0.034(2) 0.0123(17) 0.0082(18) 0.0149(19) C50 0.0161(14) 0.0270(16) 0.0235(16) 0.0043(13) 0.0010(12) 0.0005(12) C51 0.033(2) 0.076(3) 0.040(2) 0.028(2) 0.0066(16) 0.0223(19) C52 0.042(2) 0.059(3) 0.063(3) -0.024(2) -0.019(2) 0.029(2) C53 0.0235(17) 0.061(2) 0.0329(19) -0.0065(17) 0.0056(14) 0.0008(16) C54 0.0217(16) 0.043(2) 0.0353(19) -0.0157(16) -0.0030(14) 0.0121(14) C55 0.041(2) 0.039(2) 0.054(2) -0.0179(18) -0.0091(18) 0.0142(17) C56 0.034(2) 0.074(3) 0.052(2) -0.028(2) -0.0108(18) 0.028(2) C57 0.044(2) 0.044(2) 0.044(2) 0.0127(17) 0.0112(17) -0.0093(17) C58 0.059(3) 0.056(3) 0.103(4) -0.011(3) 0.027(3) -0.019(2) C59 0.125(5) 0.066(3) 0.055(3) 0.014(2) -0.002(3) 0.022(3) C61 0.044(6) 0.064(11) 0.125(7) -0.040(5) -0.016(4) -0.002(5) C62 0.048(4) 0.064(4) 0.080(5) -0.034(4) -0.003(3) 0.012(3) C63 0.056(3) 0.069(4) 0.082(8) -0.056(6) -0.007(5) -0.003(3) C64 0.073(5) 0.074(5) 0.040(4) -0.008(3) -0.004(3) 0.016(4) C65 0.065(4) 0.030(3) 0.065(4) 0.002(3) 0.021(3) -0.001(3) C66 0.045(4) 0.041(3) 0.073(5) 0.004(3) 0.014(4) -0.013(3) C61X 0.044(6) 0.064(11) 0.125(7) -0.040(5) -0.016(4) -0.002(5) C62X 0.048(4) 0.064(4) 0.080(5) -0.034(4) -0.003(3) 0.012(3) C63X 0.056(3) 0.069(4) 0.082(8) -0.056(6) -0.007(5) -0.003(3) C64X 0.073(5) 0.074(5) 0.040(4) -0.008(3) -0.004(3) 0.016(4) C65X 0.065(4) 0.030(3) 0.065(4) 0.002(3) 0.021(3) -0.001(3) C66X 0.045(4) 0.041(3) 0.073(5) 0.004(3) 0.014(4) -0.013(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 N1 1.963(2) . ? Ni1 N31 1.967(2) . ? Ni1 N34 1.978(2) . ? Ni1 N4 1.999(2) . ? C5 C6 1.400(5) . ? C5 C10 1.415(4) . ? C5 N4 1.449(4) . ? C6 C7 1.399(4) . ? C6 C17 1.528(4) . ? C7 C8 1.377(5) . ? C8 C9 1.372(5) . ? C9 C10 1.396(5) . ? C10 C20 1.522(5) . ? C11 C16 1.402(4) . ? C11 C12 1.412(4) . ? C11 N1 1.443(4) . ? C12 C13 1.392(4) . ? C12 C24 1.526(4) . ? C13 C14 1.378(4) . ? C14 C15 1.375(5) . ? C15 C16 1.394(4) . ? C16 C27 1.521(4) . ? C17 C18 1.519(5) . ? C17 C19 1.523(5) . ? C20 C21 1.540(5) . ? C20 C22 1.549(6) . ? N1 C2 1.327(3) . ? N4 C3 1.326(3) . ? C2 C3 1.402(4) . ? C2 C23 1.512(4) . ? C24 C25 1.526(4) . ? C24 C26 1.527(5) . ? C27 C28 1.524(5) . ? C27 C29 1.533(5) . ? N31 C32 1.340(4) . ? N31 C41 1.443(4) . ? C32 C33 1.396(4) . ? C32 C53 1.510(4) . ? C33 N34 1.326(3) . ? N34 C35 1.451(3) . ? C35 C40 1.401(4) . ? C35 C36 1.414(4) . ? C36 C37 1.398(4) . ? C36 C47 1.521(4) . ? C37 C38 1.379(4) . ? C38 C39 1.381(4) . ? C39 C40 1.394(4) . ? C40 C50 1.526(4) . ? C41 C46 1.399(5) . ? C41 C42 1.408(5) . ? C42 C43 1.403(5) . ? C42 C54 1.513(5) . ? C43 C44 1.369(6) . ? C44 C45 1.376(6) . ? C45 C46 1.401(5) . ? C46 C57 1.521(5) . ? C47 C48 1.523(4) . ? C47 C49 1.547(5) . ? C50 C52 1.513(4) . ? C50 C51 1.521(4) . ? C54 C55 1.543(5) . ? C54 C56 1.543(4) . ? C57 C58 1.522(5) . ? C57 C59 1.535(6) . ? C61 C62 1.457(14) . ? C62 C63 1.541(9) . ? C63 C64 1.489(9) . ? C64 C65 1.518(8) . ? C65 C66 1.498(8) . ? C61X C62X 1.460(15) . ? C62X C63X 1.537(9) . ? C63X C64X 1.486(9) . ? C64X C65X 1.521(9) . ? C65X C66X 1.491(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N31 142.76(10) . . ? N1 Ni1 N34 108.27(9) . . ? N31 Ni1 N34 81.81(9) . . ? N1 Ni1 N4 82.03(10) . . ? N31 Ni1 N4 108.25(9) . . ? N34 Ni1 N4 148.61(10) . . ? C6 C5 C10 120.2(3) . . ? C6 C5 N4 118.8(3) . . ? C10 C5 N4 120.8(3) . . ? C7 C6 C5 118.7(3) . . ? C7 C6 C17 119.4(3) . . ? C5 C6 C17 121.7(3) . . ? C8 C7 C6 121.1(3) . . ? C9 C8 C7 120.1(3) . . ? C8 C9 C10 121.2(3) . . ? C9 C10 C5 118.6(3) . . ? C9 C10 C20 118.3(3) . . ? C5 C10 C20 123.1(3) . . ? C16 C11 C12 120.7(3) . . ? C16 C11 N1 120.0(3) . . ? C12 C11 N1 119.0(2) . . ? C13 C12 C11 117.9(3) . . ? C13 C12 C24 119.8(3) . . ? C11 C12 C24 122.3(3) . . ? C14 C13 C12 121.8(3) . . ? C15 C14 C13 119.6(3) . . ? C14 C15 C16 121.4(3) . . ? C15 C16 C11 118.6(3) . . ? C15 C16 C27 119.2(3) . . ? C11 C16 C27 122.2(3) . . ? C18 C17 C19 110.5(3) . . ? C18 C17 C6 113.0(3) . . ? C19 C17 C6 110.0(3) . . ? C10 C20 C21 112.3(3) . . ? C10 C20 C22 111.0(4) . . ? C21 C20 C22 107.8(3) . . ? C2 N1 C11 113.3(2) . . ? C2 N1 Ni1 112.79(17) . . ? C11 N1 Ni1 133.75(17) . . ? C3 N4 C5 112.5(2) . . ? C3 N4 Ni1 111.27(18) . . ? C5 N4 Ni1 135.75(18) . . ? N1 C2 C3 116.5(2) . . ? N1 C2 C23 126.6(3) . . ? C3 C2 C23 116.5(2) . . ? N4 C3 C2 117.2(2) . . ? C12 C24 C25 112.0(2) . . ? C12 C24 C26 112.6(3) . . ? C25 C24 C26 108.9(3) . . ? C16 C27 C28 110.6(3) . . ? C16 C27 C29 111.7(3) . . ? C28 C27 C29 109.4(3) . . ? C32 N31 C41 112.8(2) . . ? C32 N31 Ni1 113.40(18) . . ? C41 N31 Ni1 133.59(19) . . ? N31 C32 C33 114.7(2) . . ? N31 C32 C53 126.2(3) . . ? C33 C32 C53 119.1(3) . . ? N34 C33 C32 118.2(3) . . ? C33 N34 C35 111.1(2) . . ? C33 N34 Ni1 111.68(18) . . ? C35 N34 Ni1 136.77(17) . . ? C40 C35 C36 120.6(2) . . ? C40 C35 N34 118.8(2) . . ? C36 C35 N34 120.2(2) . . ? C37 C36 C35 118.2(3) . . ? C37 C36 C47 119.4(2) . . ? C35 C36 C47 122.5(2) . . ? C38 C37 C36 121.5(3) . . ? C37 C38 C39 119.5(3) . . ? C38 C39 C40 121.4(3) . . ? C39 C40 C35 118.7(3) . . ? C39 C40 C50 119.8(3) . . ? C35 C40 C50 121.3(2) . . ? C46 C41 C42 121.4(3) . . ? C46 C41 N31 119.6(3) . . ? C42 C41 N31 118.6(3) . . ? C43 C42 C41 117.2(4) . . ? C43 C42 C54 120.8(3) . . ? C41 C42 C54 122.0(3) . . ? C44 C43 C42 122.0(4) . . ? C43 C44 C45 119.9(3) . . ? C44 C45 C46 120.9(4) . . ? C41 C46 C45 118.3(4) . . ? C41 C46 C57 122.1(3) . . ? C45 C46 C57 119.5(3) . . ? C36 C47 C48 111.7(2) . . ? C36 C47 C49 112.5(3) . . ? C48 C47 C49 108.0(3) . . ? C52 C50 C51 111.5(3) . . ? C52 C50 C40 110.5(2) . . ? C51 C50 C40 111.4(2) . . ? C42 C54 C55 114.8(3) . . ? C42 C54 C56 112.2(3) . . ? C55 C54 C56 107.9(3) . . ? C46 C57 C58 111.2(3) . . ? C46 C57 C59 111.6(3) . . ? C58 C57 C59 111.2(4) . . ? C61 C62 C63 115.3(10) . . ? C64 C63 C62 112.9(5) . . ? C63 C64 C65 118.4(6) . . ? C66 C65 C64 115.4(5) . . ? C61X C62X C63X 114.7(14) . . ? C64X C63X C62X 113.6(8) . . ? C63X C64X C65X 117.5(7) . . ? C66X C65X C64X 116.8(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.527 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.057 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 650251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 I2 N2 Ni' _chemical_formula_weight 590.90 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 7.0556(6) _cell_length_b 8.2305(6) _cell_length_c 18.0170(12) _cell_angle_alpha 94.370(4) _cell_angle_beta 98.977(4) _cell_angle_gamma 98.200(4) _cell_volume 1017.69(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 3.990 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.611 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50 kV, 80 mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '625 images at 1.0 deg. stepwise rotation in omega and phi, 115 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7093 _diffrn_reflns_av_R_equivalents 0.1173 _diffrn_reflns_av_sigmaI/netI 0.0940 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 22.49 _reflns_number_total 2161 _reflns_number_gt 1577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+68.6515P] 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 2161 _refine_ls_number_parameters 112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1178 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1688 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.8258(4) -0.1365(3) -0.26936(14) 0.0143(7) Uani 1 1 d . . . I1 I -0.5465(2) 0.10121(18) -0.23032(8) 0.0203(4) Uani 1 1 d . . . I2 I -0.7376(3) -0.3837(2) -0.33389(11) 0.0463(6) Uani 1 1 d . . . N1 N -0.966(2) -0.216(2) -0.1879(9) 0.014(4) Uiso 1 1 d . . . C2 C -1.152(3) -0.239(2) -0.2051(11) 0.013(4) Uiso 1 1 d . . . C3 C -1.227(3) -0.199(2) -0.2807(11) 0.013(4) Uiso 1 1 d . . . H3 H -1.3625 -0.2141 -0.2994 0.016 Uiso 1 1 calc R . . N4 N -1.100(2) -0.1411(18) -0.3213(8) 0.006(3) Uiso 1 1 d . . . C5 C -1.168(3) -0.105(2) -0.3983(11) 0.015(5) Uiso 1 1 d . . . C6 C -1.241(3) -0.235(2) -0.4526(11) 0.013(5) Uiso 1 1 d . . . C7 C -1.307(3) -0.192(2) -0.5261(11) 0.014(5) Uiso 1 1 d . . . H7 H -1.3638 -0.2754 -0.5658 0.016 Uiso 1 1 calc R . . C8 C -1.289(3) -0.023(2) -0.5401(11) 0.014(5) Uiso 1 1 d . . . H8 H -1.3328 0.0042 -0.5895 0.016 Uiso 1 1 calc R . . C9 C -1.211(3) 0.099(3) -0.4854(11) 0.016(5) Uiso 1 1 d . . . H9 H -1.1926 0.2104 -0.4971 0.019 Uiso 1 1 calc R . . C10 C -1.154(3) 0.062(2) -0.4087(11) 0.010(4) Uiso 1 1 d . . . C11 C -1.070(3) 0.193(2) -0.3469(11) 0.013(5) Uiso 1 1 d . . . H11A H -1.0714 0.3012 -0.3659 0.020 Uiso 1 1 calc R . . H11B H -0.9359 0.1799 -0.3276 0.020 Uiso 1 1 calc R . . H11C H -1.1468 0.1846 -0.3060 0.020 Uiso 1 1 calc R . . C12 C -1.260(3) -0.411(2) -0.4398(12) 0.018(5) Uiso 1 1 d . . . H12A H -1.3201 -0.4784 -0.4870 0.027 Uiso 1 1 calc R . . H12B H -1.3417 -0.4321 -0.4012 0.027 Uiso 1 1 calc R . . H12C H -1.1312 -0.4390 -0.4228 0.027 Uiso 1 1 calc R . . C13 C -0.870(3) -0.257(2) -0.1127(11) 0.014(5) Uiso 1 1 d . . . C14 C -0.852(3) -0.429(2) -0.1077(11) 0.013(4) Uiso 1 1 d . . . C15 C -0.751(3) -0.457(3) -0.0375(12) 0.020(5) Uiso 1 1 d . . . H15 H -0.7321 -0.5662 -0.0288 0.024 Uiso 1 1 calc R . . C16 C -0.676(3) -0.331(3) 0.0196(13) 0.022(5) Uiso 1 1 d . . . H16 H -0.6074 -0.3559 0.0659 0.027 Uiso 1 1 calc R . . C17 C -0.700(3) -0.174(2) 0.0107(11) 0.012(4) Uiso 1 1 d . . . H17 H -0.6454 -0.0915 0.0509 0.014 Uiso 1 1 calc R . . C18 C -0.802(3) -0.127(2) -0.0565(10) 0.009(4) Uiso 1 1 d . . . C19 C -0.838(3) 0.042(2) -0.0661(12) 0.020(5) Uiso 1 1 d . . . H19A H -0.7829 0.1133 -0.0193 0.030 Uiso 1 1 calc R . . H19B H -0.9778 0.0434 -0.0777 0.030 Uiso 1 1 calc R . . H19C H -0.7756 0.0830 -0.1075 0.030 Uiso 1 1 calc R . . C20 C -0.931(3) -0.568(3) -0.1668(12) 0.022(5) Uiso 1 1 d . . . H20A H -0.8998 -0.6712 -0.1480 0.033 Uiso 1 1 calc R . . H20B H -0.8725 -0.5493 -0.2120 0.033 Uiso 1 1 calc R . . H20C H -1.0722 -0.5747 -0.1796 0.033 Uiso 1 1 calc R . . C21 C -1.297(3) -0.304(3) -0.1579(12) 0.023(5) Uiso 1 1 d . . . H21A H -1.2282 -0.3274 -0.1093 0.034 Uiso 1 1 calc R . . H21B H -1.3765 -0.4050 -0.1842 0.034 Uiso 1 1 calc R . . H21C H -1.3799 -0.2208 -0.1495 0.034 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 0.0153(14) 0.0178(15) 0.0084(14) 0.0038(12) -0.0020(11) 0.0006(11) I1 0.0225(8) 0.0214(8) 0.0144(8) -0.0034(6) 0.0020(6) -0.0012(6) I2 0.0414(11) 0.0476(12) 0.0494(12) -0.0006(9) 0.0105(9) 0.0047(9) _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 N1 1.996(16) . ? Ni1 N4 2.008(14) . ? Ni1 I2 2.471(3) . ? Ni1 I1 2.542(3) . ? N1 C2 1.28(2) . ? N1 C13 1.50(2) . ? C2 C3 1.46(3) . ? C2 C21 1.49(3) . ? C3 N4 1.30(2) . ? N4 C5 1.46(2) . ? C5 C6 1.37(3) . ? C5 C10 1.40(3) . ? C6 C7 1.42(3) . ? C6 C12 1.47(3) . ? C7 C8 1.42(3) . ? C8 C9 1.35(3) . ? C9 C10 1.44(3) . ? C10 C11 1.48(3) . ? C13 C18 1.39(3) . ? C13 C14 1.45(3) . ? C14 C15 1.40(3) . ? C14 C20 1.48(3) . ? C15 C16 1.39(3) . ? C16 C17 1.34(3) . ? C17 C18 1.42(3) . ? C18 C19 1.47(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 80.8(6) . . ? N1 Ni1 I2 106.2(5) . . ? N4 Ni1 I2 101.7(4) . . ? N1 Ni1 I1 116.5(5) . . ? N4 Ni1 I1 131.1(4) . . ? I2 Ni1 I1 114.47(11) . . ? C2 N1 C13 120.2(16) . . ? C2 N1 Ni1 114.9(13) . . ? C13 N1 Ni1 124.8(12) . . ? N1 C2 C3 114.9(17) . . ? N1 C2 C21 127.8(18) . . ? C3 C2 C21 117.3(17) . . ? N4 C3 C2 117.1(17) . . ? C3 N4 C5 119.1(16) . . ? C3 N4 Ni1 112.2(12) . . ? C5 N4 Ni1 128.4(12) . . ? C6 C5 C10 126.2(18) . . ? C6 C5 N4 118.6(17) . . ? C10 C5 N4 115.2(17) . . ? C5 C6 C7 115.9(17) . . ? C5 C6 C12 125.3(18) . . ? C7 C6 C12 118.8(18) . . ? C8 C7 C6 119.9(18) . . ? C9 C8 C7 121.8(19) . . ? C8 C9 C10 120.2(18) . . ? C5 C10 C9 115.7(18) . . ? C5 C10 C11 122.2(17) . . ? C9 C10 C11 121.8(17) . . ? C18 C13 C14 126.9(18) . . ? C18 C13 N1 117.3(16) . . ? C14 C13 N1 115.7(17) . . ? C15 C14 C13 112.6(18) . . ? C15 C14 C20 120.8(18) . . ? C13 C14 C20 126.7(17) . . ? C16 C15 C14 123(2) . . ? C17 C16 C15 121(2) . . ? C16 C17 C18 122.8(19) . . ? C13 C18 C17 113.9(17) . . ? C13 C18 C19 122.5(17) . . ? C17 C18 C19 123.6(18) . . ? _diffrn_measured_fraction_theta_max 0.811 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.811 _refine_diff_density_max 1.206 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.264 #===END